PIM International December 2021

CataMIM® • A direct replacement for all current commercially available catalytic debind feedstocks • Improved flow • Stronger green and brown parts • More materials available and better surface finish

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• Custom scale-up factors available • Faster cycle times • 65°C / 150°F mold temperature

AquaMIM® • Water Debind • Custom scale-up factors available • Large selection of available materials

MIM/PIM

SolvMIM® • Solvent, Super Critical Fluid Extraction (SFE) or Thermal Debind methods • Hundreds of materials available • Custom scale-up factors available

FEEDSTOCKS • At RYER, all our feedstocks are manufactured to the highest level of quality, with excellent batch-to-batch repeatability.

• RYER is the ONLY commercially available feedstock manufacturer to offer all five debind methods.

• RYER offers the largest material selections of any commercially available feedstock manufacturer.

• RYER offers technical support for feedstock selection, injection molding, debinding and sintering.

RYER, Inc. | 42625 Rio Nedo Unit B | Temecula, CA 92590 | USA | Tel: +1 951 296 2203 Email: dave@ryerinc.com | www.ryerinc.com

Publisher & Editorial Offices Inovar Communications Ltd 11 Park Plaza Battlefield Enterprise Park Shrewsbury SY1 3AF United Kingdom Tel: +44 (0)1743 469909 www.pim-international.com Managing Director & Editor Nick Williams nick@inovar-communications.com Group News Editor Paul Whittaker paul@inovar-communications.com

For the MIM, CIM and sinter-based AM industries

Deputy Editor Emily-Jo Hopson-VandenBos emily-jo@inovar-communications.com Assistant Editors Kim Hayes kim@inovar-communications.com Charlie Hopson-VandenBos charlie@inovar-communications.com Advertising Sales Director Jon Craxford, Advertising Sales Director Tel: +44 (0)207 1939 749 jon@inovar-communications.com Digital Marketer Swetha Akshita swetha@inovar-communications.com Production Manager Hugo Ribeiro hugo@inovar-communications.com Consulting Editors Prof Randall M German Former Professor of Mechanical Engineering, San Diego State University, USA Dr Yoshiyuki Kato Kato Professional Engineer Office, Yokohama, Japan Professor Dr Frank Petzoldt Deputy Director, Fraunhofer IFAM, Bremen, Germany Dr David Whittaker DWA Consulting, Wolverhampton, UK Bernard Williams Consultant, Shrewsbury, UK Subscriptions Powder Injection Moulding International is published on a quarterly basis as either a free digital publication or via a paid print subscription. The annual print subscription charge for four issues is £145.00 including shipping.

Accuracy of contents Whilst every effort has been made to ensure the accuracy of the information in this publication, the publisher accepts no responsibility for errors or omissions or for any consequences arising there from.

Inovar Communications Ltd cannot be held responsible for views or claims expressed by contributors or advertisers, which are not necessarily those of the publisher.

Advertisements Although all advertising material is expected to conform to ethical standards, inclusion in this publication does not constitute a guarantee or endorsement of the quality or value of such product or of the claims made by its manufacturer.

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Printed by Cambrian Printers, Aberystwyth, United Kingdom ISSN 1753-1497 (print) ISSN 2055-6667 (online) Vol. 15 No. 4 December 2021 © 2021 Inovar Communications Ltd

A positive force that works two ways Over the last few years it has felt that there has been only one way traffic when it came to talent and expertise moving between the MIM industry and the sinter-based AM industry, most notably the Binder Jetting industry. Nonetheless, I was sure that having MIM experts embedded in the dynamic, high-profile AM industry would, in due course, lead to a greater awareness of the promise of MIM technology outside of the small global family of the initiated.

Recently, it seems as if the traffic has started to flow in both directions, and MIM is now getting a lift from the attention around Binder Jetting. Once people are excited about the prospect of making parts from powder and binder, and ready to embrace issues such as shrinkage during the debinding and sintering process, MIM almost starts to look like the easiest, and certainly the most mature, of several technology options – so long as the part can be moulded and the production volumes warrant the tooling investment.

This is certainly the case at FreeFORM Technologies, the US-based Binder Jetting firm that we profiled in our June 2021 issue. The company has just purchased two injection moulding machines and a furnace to service the high level of interest it is seeing in MIM. One of the two companies that we visited for this issue of PIM International is SSI Sintered Specialties, also based in the US. SSI is not only diversifying from its core expertise in press and sinter PM by installing Binder Jetting technology, but it is also embracing MIM with renewed enthusiasm.

Nick Williams, Managing Director & Editor

Cover image

Component for a noise-reducing water fitting designed for use in a hotel, made from 316L and partly machine finished (Courtesy Hansgrohe SE)

December 2021 PIM International

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December 2021

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Headmade Materials and Cold Metal Fusion: An innovative approach to sinter-based Additive Manufacturing

In recent years there has been a surge in interest in sinterbased metal Additive Manufacturing, with many of these technologies adapting the materials used in Metal Injection Moulding. Whilst Binder Jetting (BJT) and Material Extrusion (MEX) processes lead the field in terms of market penetration, sometimes something radically different comes along. This is certainly the case with Germany’s Headmade Materials, whose Cold Metal Fusion (CMF) AM process takes a completely new approach. Dr Georg Schlieper visited the company and reports for PIM International on the company and its technology. >>>

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SSI Sintered Specialties: Expanding horizons through ‘next-generation’ MIM materials and Binder Jetting

SSI Sintered Specialties, LLC can trace its roots back to the earliest days of Powder Metallurgy in the US. True to its name, that company has over the decades found success through specialisation, in particular stainless steel PM products. This is a theme that continues today, with the company now expanding its horizons through the development of large MIM parts using innovative feedstock technology, and the adoption of metal Binder Jetting. Bernard North visited the company on behalf of PIM International and reports on its plans to remain at the forefront of metal powder based parts production. >>>

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Exploring the subtleties of the formulation and preparation of MIM feedstocks

A technical session, comprising three papers, at the Euro PM2021 Virtual Congress, organised by the European Powder Metallurgy Association (EPMA) and held from October 18–22, 2021, assessed various aspects of the formulation and preparation of feedstocks for Metal Injection Moulding.

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Dr David Whittaker reports on three papers that addressed solvent debinding efficiency, strategies for enhancing the debinding of polyacetal (POM) feedstocks, and, lastly, an analytical method for enhancing the understanding of the homogeneity of MIM feedstocks and green parts. >>>

December 2021 PIM International

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© 2021 by 3D Systems, Inc. All rights reserved. Specifications subject to change without notice.

3D Systems and the 3D Systems logo are registered trademarks of 3D Systems, Inc.

Learn more at 3dsystems.com/3d-printers/metal

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What drives the success of an industry: chance or strategy?

Lessons from the growth of MIM in China

In March 2007, the very first issue of PIM International featured a review of MIM in Asia.

China’s MIM industry was estimated as having around twenty MIM firms, many modest in size and of limited capability, with Taiwan accounting for another fifteen.

Fast forward less than fifteen years, and Greater China now accounts for half of global MIM production, is a leader in MIM-grade powder production, and is home to a host of production equipment manufacturers.

Industry consultant Dr Chiou Yau Hung (Dr Q) assesses just what happened to drive this success: good fortune, good strategy, or a slice of both? >>>

105 A microstructural investigation of 420 martensitic stainless steel processed by MIM

Type 420 martensitic stainless steel covers a wide carbon range of 0.15% to 0.45%.

Demand for this material from the 3C, automotive, biomedical and aerospace industries has been increasing thanks to its combination of moderate corrosion resistance, high hardness, and good tensile properties.

In this study, Shu-Hsu Hsieh, Dr ChungHuei Chueh, and I-Shiuan Chen, from Chenming Electronic Technology Corp.

(UNEEC), Taiwan, investigated Nb-alloyed 420 produced using BASF SE’s Catamold 420 W feedstock. Decarburisation was examined in samples processed in both a graphite furnace and a molybdenum lined furnace. Microstructure, phase and hardness variations from the sintered state to each specific stage in heat treatment were also explored. Additionally, the influence of niobium on the formation of intergranular compounds, carbides, and carbonitrides was also assessed in each heat treatment stage for comparison. >>>

Regular features...

09 News

123 Advertisers’ index & buyer’s guide

Discover the leading suppliers of materials and equipment for MIM, CIM and sinterbased AM, as well as part manufacturing partners and more. >>>

126 Events guide

View a list of upcoming events for the MIM, CIM & sinter-based AM industries. >>>

Vol. 15 No. 4 © 2021 Inovar Communications Ltd

December 2021 PIM International

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MIM POWDER MANUFACTURER CHARACTERISTICS

APPLICATIONS

Plasma Quality Powder

Metal Injection Molding

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Additive Manufacturing

Industrial Capacity

Hot and Cold Isostatic Pressing

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Thermal and Cold Spray

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Industry News FreeFORM expands technology offering with addition of MIM services FreeFORM Technologies, St Marys, Pennsylvania, USA, reports that it has expanded its offering to provide Metal Injection Moulding services, in addition to its metal Binder Jetting (BJT) capacity, thanks to the recent acquisition of two fully automated Arburg Allrounder 320 C injection moulding machines and a vacuum debinding and sintering furnace for MIM and sinter-based AM from Centorr Vacuum Industries.

Founded in 2020, FreeFORM has developed a strong presence in the metal BJT service bureau landscape.

The company has worked to educate customers of the benefits of Binder Jetting, especially during the current supply chain crisis. FreeFORM explains that the current market has led to nearly all industries looking for new or secondary suppliers for their products and the impact of the COVID-19 pandemic has revitalised the drive for companies to explore tool-less technologies such as metal Additive Manufacturing.

In the company’s first twelve months of business, it delivered over 45,000 additively manufactured parts to more than twenty-five customers worldwide. “AM 2.0 is alive and well,” stated Nathan Higgins, president of FreeFORM Technologies. “We have seen a great increase in customer and prospect RFQ activity for new and conversion products. FreeFORM strives to operate as a function of the customers’ engineering teams, solving their most complex problems.

Along with our customers, equipment manufacturers, and powder suppliers, we have helped customers launch products in several new binder jetted materials in 25% of the typical time for traditional manufacturing.”

“Volume is a still a recurring question from our customers when it comes to Additive Manufacturing and some still prefer to manufacture high volumes of parts with traditional technologies like Metal Injection Moulding,” Higgins continued. “Our goal at FreeFORM is to continue to

build on the acceleration of the AM 2.0 movement, but as a customer first business the message was loud and clear, we needed to offer additional technology.”

FreeFORM finished the installation of the injection moulding machines, along with additional sintering capacity, in Q3 2021. With this new capacity and additional technology, the company anticipates that it can continue to serve its customers from ideation through production with or without tooling.

Chris Aiello, vice president of Business Development, FreeFORM Technologies, added, “When we were presented with the opportunity to acquire these assets and the transfer tooling that came along with them, it was a no brainer for us. MIM is a natural fit to complement our existing capacity, plus people know our team as ‘MIM guys’ from our past roles, so it feels right to add this offering. Over the past twelve months, we have had countless requests from customers to offer MIM. We had explored some alternatives, but, to Nate’s point, the writing was on the wall – we needed to offer this to our customers.” www.freeformtech.com

FreeFORM Technologies can offer MIM services thanks to the acquisition of two fully automated Arburg injection moulding machines (left) and a vacuum furnace from Centorr Vacuum Industries (Courtesy FreeFORM Technologies)

Vol. 15 No. 4 © 2021 Inovar Communications Ltd

December 2021 PIM International

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WHEN CONSISTENCY IS KEY THE RIGHT PARTNER IS EVERYTHING History is important – as are innovations. Just imagine what 159 years of materials expertise and nearly half a century in powder atomization could do for you. Sandvik adds true value to your business through world leading R&D and the widest range of metal powders on the market — including Osprey® nickel-free stainless steel, aluminum, and premium titanium powder, tailored to perfection for technologies such as metal injection molding and binder jetting. Our in-house atomizing facilities produce customized and highly consistent metal powders with excellent morphology, at any fraction your process requires. So, when you expect more than just a material... The right partner is everything.

MEET OUR METAL POWDER AND ADDITIVE MANUFACTURING EXPERTS AT MIM 2022 | February 21-23 | mpif.org/events/MIM2022 Additive by Sandvik: Material Matters | Interactive webinar series | metalpowder.sandvik/webinar

EXPLORE OUR MARKET-LEADING RANGE OF FINE METAL POWDERS metalpowder.sandvik

Industry News

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Visottica Comotec acquires majority stake in Ookii and Matrix Visottica Comotec, an eyewear components company based in the Veneto region of Italy, has completed the acquisition of a majority stake in Ookii, a specialist in precision micromechanics headquartered in the Belluno eyewear district in Italy.

The deal will also see the company gain a majority stake in Matrix s.r.l., a leading producer of Metal Injection Moulding and microfusion components, of which Ookii holds 100% of the capital.

Visottica Comotec’s share in Ookii has risen to 83.8%, up from a 50% share which it has held since 2017.

Established in 1994, Ookii specialises in the production of moulds and small metal parts, operating mainly in the eyewear and precision engineering sectors. Among the main

structure, we can support our traditional customers even more effectively thanks to our leadership in the eyewear sector, while also empowering our presence in rapidly developing markets like industrial and fashion accessories.

Technological integration and the combination of the different know-how of the group’s companies guarantees tailor-made products with maximum flexibility and speed, integrating them into Visottica Comotec global strategy and offer.

This operation also confirms the strategic vision of the Group to maintain a strong manufacturing presence in Italy to support Asian production.”

The agreement between the two companies provides for the acquisition by Visottica of 100% of the Ookii shares in 2024. www.visotticacomotec.com www.matrix-mim.com

processes used are cold moulding, die-casting of zamak, aluminium and magnesium, and moulding of plastic materials. Matrix primarily uses MIM stainless steel (316L and 17-4PH) for the production of components for the biomedical, automotive, fashion and aerospace sectors.

Visottica Comotec also recently acquired 50% of Eurodecori, a company specialising in the production and processing of zamak parts. Through a policy of strategic acquisitions, Visottica Comotec explains that it has progressively expanded its offerings, creating a high-level technological hub.

Rinaldo Montalban, president of Visottica Comotec, stated, “With this consolidation of the corporate

Ti-MIM specialist Element22 adopts Headmade’s Cold Metal Fusion AM process Titanium Metal Injection Moulding specialist Element22, Kiel, Germany, has purchased a Formiga P110 SLS machine from EOS as part of its implementation of the Cold Metal Fusion (CMF) Additive Manufacturing process developed by Headmade Materials, Würzberg, Germany.

“We are innovation drivers and always on the lookout for better, more effective solutions,” stated Matthias Scharvogel, CEO of Element22.

“During technology screening, we came across the Cold Metal Fusion technology. The projects that we have already been able to realise with Headmade Materials in the past few months then completely convinced us.”

CMF technology has recently been demonstrated in titanium series components for high-end bicycles,

Cold Metal Fusion is based on integrating metal powder into a functional binder system (Courtesy Element22)

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which, among other things, offers new possibilities in frame construction.

New part designs and functional integrations can be implemented, while production costs can be reduced.

The demand for additively manufactured titanium components also comes from other sectors such as medical, aerospace and other highend consumer goods. Utilising the CMF technology, Element22 now also serves these sectors.

When processing the titanium feedstock from Headmade Materials on the EOS Formiga P110, the included polymeric binder is melted layer by layer to form strong green parts. These are then debound and

sintered to produce components which are reportedly comparable to MIM parts.

Christian Fischer, Managing Director, Headmade Materials, concluded, “We are pleased about the expansion of our partnership with Element22 and that the titanium specialist is relying in-house on our Cold Metal Fusion technology to move into industrial titanium 3D printing.

This also underlines our technology leadership in sinter-based titanium 3D printing.”

Read more about Headmade Materials in our article on page 63. www.headmade-materials.com www.element22.de

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Industry News

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Epeire 3D releases new T-Titane AM machine

Registration opens for MIM2022 International conference on metals, ceramics and carbides

Epeire 3D, a start-up Additive Manufacturing machine maker based in Haubourdin, France, has released the Epeire T-Titane®, its newest machine intended for small to medium industrial production runs.

Based on the company’s pellet extrusion technology, a form of Material Extrusion (MEX), the T-Titane uses titanium MIM feedstock to additively manufacture the part, followed by a debinding and sintering stage.

The T-Titane joins the company’s T-MIM machine for stainless steel, Inconel, copper and aluminium processing, as well as its T-600 for polymer materials. It comes installed with a titanium and titanium alloy head which offers an accuracy of a 50 μm tolerance, a repeatability of +/-100 μm and flow rate of up to 2,500 cm3/hour.

With a build chamber of 500 x 450 x 500 mm, the T-Titane is said to open a wide range of manufacturing applications, including automotive, medical, sports and mould production. www.epeire3d.com

Registration is now open for MIM2022: International Conference on Injection Molding of Metals, Ceramics and Carbides, scheduled to take place February 21–23 in West Palm Beach, Florida, USA. Organised by the Metal Powder Industries Federation (MPIF), the annual event will showcase the latest innovations in MIM part design, tooling, moulding, debinding and sintering.

The two-day conference will include the following presentations: • Plasma powder production for MIM applications - Jérôme Pollak, Tekna • Exploring automated bending process for MIM part dimensional correction - Douglas Kaercher, The Arc Group Worldwide • Reduction in shrinkage of binder jet printed large stainless-steel parts using novel metal powders - Kyle Myers, ExOne • 17-4PH stainless past and present Tim McCabe, OptiMIM • The 1st ever direct jetting for highdefinition Additive Manufacturing of metals & ceramics - Dror Danai, XJet LTD. • A review of state-of-the-art Vacuum Induction Melting Inert Gas Atomisation (VIGA) technology and the fine metal powders possible from this technology Ralf Carlström, Höganäs AB • Powder production and Metal Injection Moulding of a novel light-weight, high-strength, nonmagnetic steel, compared with Ti6Al4V alloy alternative - Paul A Davies, Sandvik Osprey Ltd • Mitigating post-sinter distortion in MIM via machining in the green state - Levi M Rust, ARC Group Worldwide

The T-Titane uses titanium MIM feedstock to additively manufacture components (Courtesy Epeire 3D)

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• Application of hot disk transient plane source for thermal conductivity evaluation during Metal Injection Moulding: Case of metal

December 2021

powders - Artem A Trofimov, Orton Ceramic Foundation • Impact of gas guiding in an improved debinding and sintering furnace for AM Parts: CFD simulations and initial experimental results - Tim Ohnweile, Carbolite Gero • Sintering behaviour of binder-jet printed H-13 - James W. Sears, Amaero • Comparison of binder-jet and MIM - Animesh Bose, FAPMI, Desktop Metal, Inc. • Dry ice cleaning in MIM – Who needs it? - Steve Wilson, Cold Jet LLC • Metal Injection Moulding of F75 (Co-28Cr-6Mo) - John L Johnson, FAPMI, Novamet/Ultra Fine Specialty Products • Effect of Nb addition and sinter conditions on AISI-420 martensitic stainless steels produced by Powder Injection Molding: Microstructural, mechanical and corrosion properties - Prof Ozkan Gulsoy, Marmara University • Two component micro Powder Injection Molding of bi-material stainless steel 17-PH and yttria stabilised zirconia - Sulong Abu Baker, Universiti Kebangsaan Malaysia A tabletop exhibition and reception for all delegates will take place following the technical presentations on February 22.

Prior to the main conference, an optional Powder Injection Moulding tutorial will be hosted by Matthew Bulger, former MIMA president, on February 21. The tutorial provides a basis for determining options, uses, properties, applications, and opportunities for cost-effective PIM manufacturing solutions.

Early registration discounts apply until January 7, 2022. www.mpif.org

© 2021 Inovar Communications Ltd

Vol. 15 No. 4

EPSON ATMIX CORPORATION

Finer Powder Production Cleaner Powder Production Shape Control of Powders • Low Alloy Steel • High Alloy Steel • Stainless Steel • Magnetic Materials • Granulated Powder

JAPAN Mr. Ryo Numasawa Numasawa.Ryo@exc.epson.co.jp ASIA and OCEANIA Ms. Jenny Wong jenny-w@pacificsowa.co.jp CHINA Mr. Hideki Kobayashi kobayashi-h@pacificsowa.co.jp

U.S.A and SOUTH AMERICA Mr. Tom Pelletiers tpelletiers@scmmetals.com EU Dr. Dieter Pyraseh Dieter.Pyrasch@thyssenkrupp.com KOREA Mr. John Yun dkico@hanafos.com

Industry News

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Sandvik to list Sandvik Materials Technology in 2022, appoints first members of SMT Board The Sandvik Board of Directors has confirmed its previous decision to proceed with the preparation to distribute Sandvik Materials Technology (SMT) to Sandvik’s shareholders and list the company’s shares on the Nasdaq Stockholm Exchange. The board’s current target

PIMI Island Half Page Ad – Grow Profits – C Series.indd 1

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for a distribution and listing remain relevant. We believe that both Sandvik and Sandvik Materials Technology can develop more favourably on their own,” stated Johan Molin, chairman of the Sandvik Board of Directors.

The Sandvik Board intends to formally propose the distribution and listing of SMT at a shareholders’ meeting next year.

As part of this process, the Sandvik Board of Directors has appointed Andreas Nordbrandt as chairman of the board of SMT. Additionally, Claes Boustedt and Karl Åberg have been appointed as members of the SMT Board of Directors. Additional members of the SMT Board will be appointed at a later stage to fulfil any requirements and ensure a suitable board composition.

Nordbrandt holds an MSc in Mechanical Engineering and Hydraulics and is a member of the Sandvik AB Board of Directors.

He has operative experience from a global industrial environment, particularly within international mining. He previously worked at Atlas Copco Group and Epiroc Group from 1995–2018, where he held several leading positions.

Boustedt has an MSc in Business and Economics and is a member of the Sandvik AB Board of Directors, as well as chairman of the Audit Committee. He has been executive vice president of LE Lundbergföretagen AB since 1997, and president of LE Lundberg Kapitalförvaltning AB since 1995.

He is also a board member of Hufvudstaden AB and Förvaltnings AB Lunden. Åberg holds an MSc in Economics and Business Administration and has been Head of Investments and Analysis at Industrivärden AB since 2017. His previous experience includes being a partner at Zeres Capital, where he was also a co-founder, and partner at Capman Public Market. www.home.sandvik/en

is to complete the listing on the Nasdaq Stockholm Exchange during the second or third quarter 2022, subject to approval by Sandvik’s shareholders.

“The internal separation of SMT is proceeding as planned and the previously communicated reasons

December 2021

2/8/21 2:45 PM

© 2021 Inovar Communications Ltd

Vol. 15 No. 4

Industry News

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Bloemacher and Neubert receive EPMA Distinguished Service Award The European Powder Metallurgy Association (EPMA) announced the recipients of its 2021 Distinguished Service Award during the opening session of Euro PM2021, held as a digital event for the second year due to the coronavirus pandemic.The EPMA’s Distinguished Service Awards are presented in recognition of individuals who make an outstanding contribution to the European PM industry. This year, the Distinguished Service Award was presented to Martin Bloemacher and Harald Neubert.

Metal Injection Moulding as a part of his research. He went on to co-invent the Catamold system for MIM and was a founding member of the Catamold group at BASF in 1990.

Bloemacher was instrumental in building Catamold production and application services in Ludwigshafen and the company’s site in Asia. He was a recipient of BASF’s innovation award in 1996 and has been a member of the EPMA Council since 2000. He retired from BASF in March 2021.

Martin Bloemacher After studying physics at the University of Duisburg, Germany, Martin Bloemacher joined BASF, Ludwigshafen, Germany, in 1987 and began work within the Carbonyl Iron Powder (CIP) Plant. Having built up an application lab for CIP, he started to work on

Harald Neubert Harald Neubert received his diploma and PhD from the University of Essen, Germany, and went on to join Krebsöge Group in 1988, which later became part of the GKN group. He began working in Powder Forging at the Pulverschmiede Hueckeswagen

Thermal Process Equipment for PIM Applications Continuous Plants

Martin Bloemacher (left) and Harald Neubert (right) (Courtesy EPMA) facility and became plant manager in 1989. During his time at the company he progressed to several senior management positions, becoming President, Asian Pacific and South American Operations in 2005.

In 2007 he joined Miba Sinter Group, Laakirchen, Austria, and was responsible for the group’s technology and R&D. He became its CEO in 2008, retiring in January 2021. Neubert holds a number of patents and is a long-serving member of the EPMA Board and Council. www.epma.com

Thermoprozessanlagen GmbH

Batch Furnaces (Debinding, Sintering, HIP/CIP)

CREMER HIP Innovations GmbH

50

Years

Designed, developed and made in Germany

Vol. 15 No. 4 © 2021 Inovar Communications Ltd

www.cremer-polyfour.de

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Industry News

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LightForce Orthodontics closes Series C funding with $50 million investment LightForce Orthodontics, Cambridge, Massachusetts, USA, has closed its Series C funding round with a $50 million investment from new investor Kleiner Perkins and existing investors Matrix Partners, Tyche Partners and AM Ventures, reports TechCrunch.

LightForce technology provides additively manufactured bracket systems for orthodontics using a ceramic material said to be virtually identical to that used for familiar injection moulded brackets. The company has seen large-scale growth since the closing of its Series B funding in October 2020, including a 500% increase in revenue and 300% team growth.

“We raised a little bit earlier than we had planned. There were some very well-known VCs that were keeping tabs on us that had seen us in the past, but we were a bit too early for them. Kleiner Perkins was always one that was on my mind, as one that I would love to work with – especially with Wen Hsieh himself. He has a deep background in 3D printing and hard tech. He’s done a lot of the best hard-tech deals,” stated Dr Alfred Griffin III, DMD, PhD, MMSc, CEO and co-founder of Lightforce.

“Kleiner Perkins is one of the only venture capital groups that has done anything significant in orthodontics – it was twenty years ago, but Align

The additively manufactured bracket (left) can be placed and aligned with precision reputedly to the micrometre, in addition to being customised for each tooth; (right) a traditional bracket (Courtesy LightForce Orthodontics)

MPIF names new president and officers The Metal Powder Industries Federation (MPIF) has elected Rodney Brennen, vice president/CFO, Metco Industries, Inc, as the 31st president of the MPIF, succeeding Dean Howard, PMT, North American Höganäs Co, a subsidiary of Höganäs AB. Brennen’s two-year term began at the conclusion of the MPIF’s annual Powder Metallurgy Management Summit and 76th Annual MPIF Business Meeting, October 23–25,

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2021, in Nashville, Tennessee, USA. Brennen has worked for Metco Industries for more than twenty-five years, starting as Finance and Personnel Manager and progressing to his current position as vice president/ CFO. He most recently served as president of the Powder Metallurgy Parts Association. He is active in APMI International, a past chairman of the West Penn Chapter (1999– 2001), and currently serves on the APMI Board of Directors. He received

December 2021

Technology changed orthodontics, for the better in my opinion. Two value props came out of Align Technology: one was the aesthetic benefits, which unlocked the adult segment. The second thing is the digital nature of what they do.”

“Alfred is an orthodontist himself,” Wen Hsieh, the Kleiner Perkins partner who led the investment, commented. “He already knows where to insert into their workflow.

What part of their normal workflow is eliminated, what part is enhanced, how they can spend more or less time, how it impacts the dental tech, how it impacts the footprint of the office, how it impacts how often the patient has to come in, and so on.”

This latest $50 million investment will be used by LightForce to scale operations and market efforts, something which may prove a challenge due to the necessarily bespoke nature of these hybrid ceramic braces.

“Scaling – mass customisation – is a very unique problem that most talk about in theory, but very few have dealt with in practice. There’s around 200 of us in the company right now, and we will probably double that over the next year. Sales and engineering are probably going to be the biggest expenses, but in terms of headcount, we will need to grow the most in manufacturing technicians, both in terms of physical and digital manufacturing,” Griffin added. www.lightforceortho.com

the Distinguished Service to Powder Metallurgy Award in 2021.

Two of the federation’s six associations also instated new presidents following the Summit.

Nicola Gismondi, PMT, vice president, Sales & Marketing, MPP, has been elected president of the Powder Metallurgy Parts Association (PMPA) and will serve a two-year term.

Christopher Adam, PMT, president & CEO, Valimet Inc, has been elected president of the Association for Metal Additive Manufacturing (AMAM) and will also serve a two-year term. www.mpif.org

© 2021 Inovar Communications Ltd

Vol. 15 No. 4

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Industry News

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HP announces commercial availability of its Metal Jet AM machine in 2022 HP has confirmed it intends to move towards broader commercial availability of its Metal Jet Additive Manufacturing machine in 2022, as it continues to validate production applications with partners and customers.

“3D printing is unlocking new levels of personalisation, business resiliency, sustainability, and market disruption,” stated Didier Deltort, president of Personalization & 3D Printing, HP Inc. “Together with our partners and customers, we will

HP has confirmed it intends to move towards broader commercial availability of its Metal Jet AM machine in 2022 (Courtesy HP)

Digital Metal and Etteplan partner to advance transition to AM Digital Metal, part of Sweden’s Höganäs Group, and global engineering company Etteplan, Espoo, Finland, have announced that they will enter a strategic partnership to offer guidance to existing and new customers looking to make the transition to Additive Manufacturing.

The companies aim to provide design optimisation solutions for Digital Metal’s Binder Jetting (BJT) processes and to offer manufacturing companies the full benefit of the technology – from idea to complete component with volume production in mind.

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“Together with Etteplan we will be able to offer a stronger value proposition, covering a complete design and manufacturing process, to our customers,” stated Christian Lönne, CEO at Digital Metal. “The partnership gives us access to a world-class design team that complements our business very well.”

Etteplan provides solutions for software and embedded solutions, industrial equipment and plant engineering and technical documentation solutions to leading companies in the manufacturing industry. In 2020, it had a turnover of approximately €260 million and

December 2021

continue to pave the path to mass production with advancements to our Multi Jet Fusion platform, the commercial launch of HP Metal Jet, and investments in software, services, and partner capabilities.”

HP displayed a number of new parts built on its Metal Jet platform at the recent Formnext exhibition, where it highlighted progress with partners such as GKN and Volkswagen.

Volkswagen is integrating HP Metal Jet produced final parts for the A pillar of its T-Roc convertible. The structural parts were reported to have passed crash test certification and weigh almost 50% less than conventional components.

“Our early Metal Jet partners and customers such as GKN, Parmatech, Volkswagen, Cobra Golf, and others, are successfully demonstrating our metals mass production advantage,” commented Ramon Pastor, Global Head of HP’s 3D metals business. “As we continue to advance our technology, materials, and capabilities, we remain on track to launch in 2022. We look forward to delivering industry leading efficiency, cost savings, and design freedom to help the industry accelerate and scale digital manufacturing.” www.hp.com/go/3Dmetals

currently has over 3,500 employees.

The companies explain that by combining Digital Metal’s expertise in BJT with Etteplan’s knowledge in the design of components for AM, their goal is to accelerate the transition from traditional manufacturing to Additive Manufacturing.

Riku Riikonen, SVP, Engineering Solutions, Etteplan, commented, “Etteplan has invested heavily in Additive Manufacturing and has been involved in groundbreaking engineering already for a long time. We look forward to exploring and create synergies together with Digital Metal. The partnership will strengthen both Etteplan’s as well as Digital Metal’s offerings towards existing and future customers.” www.digitalmetal.tech www.etteplan.com

© 2021 Inovar Communications Ltd

Vol. 15 No. 4

More than a Global Leader.

A Trusted Partner.

Elnik’s innovations and experiences in all areas of temperature and atmosphere management have led us to become the benchmark for the Batch-based Debind and Sinter equipment industry. We have applied these core competencies across a wide variety of industries through our 50 year history and look forward to the emergence of new technologies that will continue to drive demand for new innovative products.

Innovation drives our manufacturing and design solutions Quality takes precedence in all areas of our business Experience motivates our team to always do what’s right Excellence is the benchmark for all customer relationships From First Stage Debind Equipment (Catalytic, Solvent, Water) and Second Stage Debind & Sinter Furnaces (All Metal or Graphite) to support with ancillary utility equipment, Elnik’s experienced team is driven to be the only partner you need for all your MIM and Metal AM equipment for 2021 and beyond.

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Industry News

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AIM3D premieres ExAM 510 prototype at Formnext 2021 AIM3D GmbH, a spin-off company of the German University of Rostock, has developed a new Additive Manufacturing machine for its pelletbased Composite Extrusion Modelling (CEM) process, a Material Extrusion (MEX) process. The new ExAM 510 is a multi-material machine for AM that can additively manufacture up to three different materials in parallel and is suitable for 316L, 17-4PH, 8620,

42CrMo4, 304, 420 W, WcCo, Ti64, Cu99 metals; Al2O3, ZrO2, SiC, Si3N4 ceramics; and plastics.

As the latest addition to the Rostock company’s product offerings, the ExAM 510 machine is intended as a further development of the smaller ExAM 255 model. The multimaterial machine can process up to three materials, which allows for two building materials and a support

MIM debind and sinter vacuum furnaces Over 6,500 production and laboratory furnaces manufactured since 1954 • Metal or graphite hot zones • Processes all binders and feedstocks • Sizes from 8.5 to 340 liters (0.3–12 cu ft.)

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MIM-VacTM Injectavac® Centorr Vacuum Industries 55 Northeastern Blvd Nashua, NH 03062 USA Tel: +1 603 595 7233 Fax: +1 603 595 9220 Email: sales@centorr.com

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PIM International

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The ExAM 510 prototype was on show at Formnext 2021 (Courtesy AIM3D GmbH) material. The extended build platform of 510 x 510 x 400 mm enables a multitude of applications.

The build area can be heated up to 200°C in order to reduce stresses in the component and to process high-performance materials. It also features a reportedly increased build rate, depending on the material, of up to 250 cm³/h (when using a 0.4 mm nozzle).

The ExAM 510 concept aims to enable significantly increased precision for additively manufactured components. The objective of developing the machine was to get more out of the patented AIM3D extruder technology; this extruder class can enable an output up to ten times higher than standard filament extruders. The use of linear motors and a stable mineral cast bed makes extremely precise operation possible even at high speeds, thus fully exploiting the potential of the technology.

Clemens Lieberwirth, CTO at AIM3D, stated, “The further development of our patented ExAM 255 machine into the ExAM 510 is a technological leap for us. So you could say we are now offering a faster, bigger, hotter and more precise CEM process technology for Additive Manufacturing.”

The ExAM 510 model was on show as a prototype at Formnext 2021. After a beta phase with pilot processors, AlphaSTAR anticipates that the ExAM 510 will be ready for series production in time for Formnext 2022. www.aim3d.de

© 2021 Inovar Communications Ltd

Vol. 15 No. 4

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Industry News

Solar Atmospheres retrofits vacuum furnace for sinterbased AM and MIM The as-purchased VFS HL50 vacuum furnace (left) and the upgraded furnace (right) with a new hot zone and pumping technology (Courtesy Solar Atmospheres of Western PA) Sellersville, Pennsylvania, and led by owner and CEO William Jones, designed the apparatus needed to consolidate the binders into one central location, thus minimising the cleaning downtime often experienced.

The update included a completely new hot zone, a binder pumping port and a second vacuum pump.

The company stated that, by mid-October, high-volume MIM

EFFICIENT STEEL AND ALUMINIUM PARTS DEVELOPMENT.

sinter jobs will be fully transferred from current Solar vacuum furnaces to this dedicated and refurbished vacuum furnace. After multiple sintering runs, Solar will then have the data to compare the downtime of a traditional vacuum furnace versus the newly designed debind & sinter modifications. Solar added that it intends to share its findings after the completion of these test runs. www.solaratm.com

ISO/TS 16949:2016/EN 9100:2018 ISO14001:2015/AD 2000 WO Certiield Company

Solar Atmospheres of Western PA, Hermitage, Pennsylvania, USA, reports it has successfully retrofitted a pre-owned vacuum furnace with a new hot zone and pumping technology to enable the furnace to be used for Metal Injection Moulding and sinter-based Additive Manufacturing processing. The upgrade is designed to minimise the impact of detrimental binders on the furnace during sintering cycles.

For the project, the company purchased a used VFS HL50 external quench vacuum furnace at auction, with the specific goal of retrofitting an older furnace with new technology.

Solar Manufacturing, based in

New additive manufacturing facilites for prototypes and short batches.

— Investment Casting — MIM — Machining — Additive manufacturing www.ecrimesagroup.com Avda. Parayas, 32 39011 Santander - España (Spain) ecrimesa@ecrimesa.es (+34) 942 334 511

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December 2021 PIM International

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DIGITAL METAL

OUR MATERIALS • Stainless steel 316L and 17-4PH • Tool steel DM D2 • Super alloys DM 625 & DM 247 (equivalent to Inconel 625 & MAR M247) • Titanium Ti6Al4V • DM Cu, pure copper

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Industry News

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NRC Canada installs Admatec AM machine to aid VPP development The Advanced Materials for Additive Manufacturing group at the National Research Council in Canada (NRC) has installed an Admaflex 130 Additive Manufacturing machine from Dutch company Admatec, to aid in its activities developing new photoresins for Vat Photopolymerisation (VPP) to process ceramics and metals.

Dr Chantal Paquet, head of the Advanced Materials for Additive Manufacturing group, has expressed excitement about the opportunities that lie ahead in developing new

materials, AM material architectures and the technologies these materials and architectures will enable.

The Admaflex 130 uses VPP to produce metal AM and ceramic AM parts. The group states that its ability to innovate in the material space has been helped by the Admaflex 130’s open platform, which enables users to adjust the build parameters in order to maintain good build quality with new materials. www.admateceurope.com nrc.canada.ca

Incus AM technology in project for producing spare parts in space Incus GmbH, Vienna, Austria, has partnered with the European Space Agency (ESA), OHB System AG, Bremen, Germany, and Lithoz GmbH, Vienna, Austria, on a collaborative project that aims to develop and test Additive Manufacturing in a microgravity environment. Incus provides lithography-based metal manufacturing (LMM) technology, defined as a Vat Photopolymerisation (VPP) process by ISO/ASTM, which is said to produce parts with excellent surface aesthetics and similar material properties to those found in Metal Injection Moulding.

One of the major challenges in maintaining a lunar station is ensuring a constant supply of goods.

In addition to supplies, research materials and equipment, spare parts are also needed in the event of any failure of individual components.

Since long-term missions have to be self sufficient, space experts from the ESA have shown interest in the use and reuse of both existing lunar surface materials and recycling of lunar base materials, derived from production waste and end-of-life items. The ability to manufacture necessary items and spare parts, on board and on demand, will reportedly help to reduce the cost and volume of

Vol. 15 No. 4 © 2021 Inovar Communications Ltd

cargo missions from Earth, as well as minimise production waste.

The LMM technology is said to offer a potential solution as it can produce spare parts from recycled metal waste, which could enable the utilisation of recycled powders from scrap metals that are available on the moon.

The LMM process uses a paste or suspension as feedstock and does not rely on the use of highly spherical gas atomised powders or support structures. The production of dimensionally accurate components separated by the thermal demoulding process does not require any time-consuming, mostly manual, reworking and is completely safe for the operator.

“We at Incus are excited to be a part of a project that will test the capabilities of our LMM technology for use in space,” commented Dr Gerald Mitteramskogler, Incus CEO. “Our solution could be a great fit to meet the challenging requirements of producing parts in such an environment.”

The goal of the eighteen-month project is to assess the feasibility of processing scrap metals available on the moon’s surface to produce a highquality final product via a zero-waste process. The assessment will take into account the constraints of a space

The Advanced Materials for Additive Manufacturing group at the National Research Council in Canada has installed an Admaflex 130 for researching materials (Courtesy Admatec)

environment – for example, considering the potential contamination of the metal powder with lunar dust.

Further evaluation of the influence of impurities on the sintering and result of the final microstructure will lead to optimisation of the binder quantity and type, as well as the development of a sustainable manufacturing chain in space.

Dr Martin Schwentenwein, Head of Material Development at Lithoz, stated, “Lithographic techniques such as the ones developed by Incus and Lithoz allow the combination of high precision 3D printing with highperformance metals and ceramics, while still remaining extremely resource-efficient. While these concepts have been successfully demonstrated on Earth, the activities of such projects are crucial for filling technological gaps and enabling the implementation of Additive Manufacturing in a space environment.”

Dr Martina Meisnar, Materials and Processes Engineer at ESA, added, “Out-of-Earth manufacturing is a very interesting topic that is being investigated by the European Space Agency with great effort. The goal is to refine these manufacturing concepts towards demonstration on Earth and ultimately for implementation in space.” www.incus3d.com | www.esa.int www.lithoz.com www.ohb-system.de

December 2021 PIM International

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Industry News

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PM Tooling System

Hyperion Metals to acquire Blacksand Technology

The EROWA PM Tooling System is the standard interface of the press tools between the toolshop and the powder press machine.

Its unrivalled resetting time also enables you to produce small series profitably. www.erowa.com

more info

Hyperion Metals, Charlotte, North Carolina, USA, has executed a one-year option to acquire Blacksand Technology LLC, West Valley City, Utah. The two companies have been collaborating on an investigation into the commercial development of spherical titanium metal powders.

“The combination of Hyperion and Blacksand Technology is transformational, bringing together two highly complementary organisations, supported by the world-class metallurgical engineering department at the University of Utah, to create a leader in sustainable low carbon titanium metal and powders,” stated Anastasios Arima, CEO and Managing Director, Hyperion.

“Hyperion’s Titan Project in Tennessee will supply low carbon titanium mineral feedstock to produce low carbon, low-cost titanium metal and powders using the HAMR and GSD technologies. We aim to build on Blacksand’s strengths in material science and innovation to scale and commercialise these breakthrough American technologies and make the US, once again, the leader in titanium metal.”

Since the founding of Blacksand in 2013, it has developed the hydrogen assisted metallothermic reduction (HAMR) technology and developed over forty patents worldwide relating to titanium manufacturing, from the supply chain to specific technologies. Over the years, the company has seen a reported investment of around $12 million into these technologies from government agencies including the Advanced Research Projects Agency – Energy and the Office of Energy Efficiency and Renewable Energy of the US Department of Energy; the National Science Foundation; and the Naval Air Systems Command of the US Department of Defense.

Dr Z Zak Fang, Professor of the University of Utah and founder of Blacksand, added, “Blacksand is excited about the prospects of commercialising its suite of titanium technologies through Hyperion Metals.

Hyperion recognises the potential of the breakthrough HAMR process based on a simple and elegant scientific principle to lead the titanium production industry away from the old, energy-intensive, and environmentallychallenging Kroll process. This is a historical opportunity to change how titanium is made with an energy-efficient, potentially zero-emission, and low-cost technology.” www.hyperionmetals.us www.blacksandtechllc.com

Check out our Buyer’s guide...

Find new suppliers of materials, production equipment and finished MIM or sinter-based AM parts on pages 123-125

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Vol. 15 No. 4

Industry News

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Triditive introduces two Amcell industrial AM machines Triditive, Gijón, Spain, has released two new industrial Additive Manufacturing machines, the Amcell 8300® and Amcell 1400®, for both metals and polymers. The machines are intended to allow the development of flexible technology to manufacture complex parts at a reduced time to market.

The Amcell 1400 is a large format Additive Manufacturing machine, suitable for metals, composites and polymers. It makes use of a Material Extrusion (MEX) process to additively manufacture titanium and stainless steel parts.

The Amcell 8300 is aimed at high-volume production and

Both of Triditive’s new Additive Manufacturing machines, the Amcell 8300 (left) and Amcell 1400 (right), can process metal and polymer materials (Courtesy Triditive) utilises what the company refers to as Automated Multimaterial Deposition (AMD) Technology®, a multi material MEX process, capable of manufacturing parts in polymers, composites and metals at the same time.

Both machines feature EVAM Software®, a manufacturing execution system (MES) that

supports the creation and management of digital warehouses and to scale production on demand. The software also works to calculate the prices of the parts produced through its quotation engine, enabling the centralisation and arrangement of all production orders. www.triditive.com

It’s a matter of choice High temp lab and industrial furnace manufacturer to the world www.cmfurnaces.com info@cmfurnaces.com 103 Dewey Street Bloomfield, NJ 07003-4237 | Tel: 973-338-6500 | Fax: 973-338-1625

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December 2021 PIM International

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Industry News

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Digital Metal adds low-alloy steel and superalloy to range of BJT materials Digital Metal, part of Sweden’s Höganäs Group, has added DM 4140 low-alloy steel and DM 718 nickel-chromium-based superalloy to the range of materials that can be processed on its Binder Jetting (BJT) AM machine. Other materials in the range already include pure copper DM Cu, stainless steel 316L and 17-4PH, tool steel DM D2, superalloys DM 625 (equivalent to Inconel 625) and DM 247 (equivalent to MAR M247), and titanium Ti6Al4V. DM 4140, a low-alloy steel powder, was developed within Hyundai Motors in order to manufacture gearbox Control Fingers using BJT. By adding carbon steel to its BJT technology, Digital Metal is said to have expanded its offer of tool-free design freedom, shortened lead times, and potential weight savings.

exposed to high loads, such as gear wheels, connecting rods, fasteners, couplings, gears, belt pulleys and shafts. With adjustment to curing conditions, DM 4140 is also available as a turnkey solution for customers who already have Digital Metal systems processing other steels and superalloys.

DM 718 is a nickel-chromiumbased precipitation-hardening superalloy, reportedly equivalent to UNS N07718 (Inconel alloy 718).

It is said to offer high strength, as well as creep and corrosion resistance, in cryogenic and elevated temperatures (up to about 650°C).

This alloy composition is thought to be the most used nickel-chromium superalloy in metal AM, in addition to being one of the most commonly used superalloys overall.

The alloy can be strengthened using industry-standard treatments, consisting of solution annealing and quenching, followed by ageing steps. www.digitalmetal.tech

The material is additively manufactured with an ink that is commonly used for other steel and nickel-base alloys, although the process has been modified to reach properties that are consistent with MIM standards (ISO22068). By alternatively applying quenching and subsequent tempering treatment in an as-sintered state, tensile properties may be tuned toward application requirements.

Low-alloy steel components, manufactured by Metal Injection Moulding, have been used in general engineering and automotive manufacturing since the early 1980s. Its strength, toughness, and resistance to deformation during quenching are said to have made DM 4140 a popular grade. DM 4140 is well suited to producing components

500 Park East Drive Woonsocket, RI 02895 USA

www.ultrafinepowder.com

MIM & BINDER-JET AM METAL POWDERS Unique inert gas atomizing technology produces highly specified, spherical metal powders for MIM and AM applications. Team with history of developing and producing fine gas atomized powders since 1990.

Specializing in sub 30 micron powders, Ultra Fine has the technical capability to work with you to develop and produce the powder to suit your application.

Ultrafine offers flexibility and quick turn-around times.

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With partner Novamet Specialty Products Corp., Ultra Fine provides various after treatments, coatings and other capabilities using Ultra Fine’s high quality powders.

1420 Toshiba Drive, Suite E Lebanon, TN 37087 USA

www.novametcorp.com

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Vol. 15 No. 4

Industry News

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Pfeiffer Vacuum offers cloudbased service management Pfeiffer Vacuum GmbH, Asslar, Germany, has introduced a new Virtual Service Management (VSM) web-based app that makes it possible to manage vacuum equipment from different manufacturers. The app is integrated into Pfeiffer Vacuum’s new Select & Request Portal, allowing interested parties who register in the portal to access the new service directly. The app allows users to create their own locations, departments and machines, to which the various vacuum components are assigned, enabling management of the vacuum equipment more easily.

The corresponding product data and operating instructions are stored and made available in the system.

A clear display of organisational units and vacuum components is expected to make planning and documentation (such as service activities, maintenance and repairs) over the entire service life much easier. Customers can store additional information, such as maintenance intervals, the average running time and the last service date. This makes it possible for the software to organise servicing and maintenance intervals and to involve the relevant Pfeiffer Vacuum service center in good time.

System downtimes can also be minimised by synchronising maintenance activities. Creating a service request is also quick, since the data can be filled in automatically.

Each vacuum component is uniquely identified via an ID code and QR code. The tool offers the option of exporting QR codes in several formats (e.g. for a label printer). With the mobile app (Android and iOS), the QR code can be scanned by smartphones or tablets, providing an instant overview of the most important data (such as the article number, operating manual or service tickets). www.pfeiffer-vacuum.com

Vol. 15 No. 4 © 2021 Inovar Communications Ltd

JPMA celebrates 65 years and moves headquarters The Japan Powder Metallurgy Association (JPMA) has relocated to a new address within the Matsudashoji Building in Tokyo, Japan. The move comes as the association celebrates its sixtyfifth year since its founding in April, 1956.

The JPMA consists of over sixty member companies that represent a number of product areas across the Powder Metallurgy supply chain, including PM equipment manufacturing, powder makers and parts manufacturers. www.jpma.gr.jp

Anzeige_PIM Magazin_120x175_1121_R02.indd 1

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Industry News

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The Japanese Metal Injection Moulding industry has seen a decrease in output for 2020, reporting total sales of JPY 10.22 billion ($90 million), a 6.8% drop from the previous year. The Japan Powder Metallurgy Association (JPMA) collected data through questionnaires from nineteen Japan-based companies involved in MIM production.

The JPMA stated that the drop can mainly be attributed to the COVID-19 pandemic, adding that sales of medical and aerospace parts, the main users of MIM technology in the region, accounted for a 10% decrease. However, sales of MIM components in the Information Equipment category were reported to have increased more than 20% due to the demand for semiconductor components.

The JPMA forecasts that 2021 will see sales increase to the same level reported in 2018, boosted by a recovery following the pandemic.

12000 11500

(Million Yen)

Japan’s 2020 MIM output impacted by pandemic

11000 10500 10000 9500 9000

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2015

2016

2017

2018

2019

2020

Sales of MIM products in Japan (FY2014–2020) (Courtesy JPMA)

The report also identified the main markets for MIM in Japan, with the largest market remaining the industrial machine parts sector. This accounted for 29.3% of production (previous year: 26.5%), medical appliance parts accounted for 18.2% of production (previous year: 19.2%) and automotive parts accounted for 14.6% of production (previous year: 16.2%). The total percentage of these MIM markets was 62.1%.

The JPMA added that it is seeing a trend for some low-cost MIM parts being imported from developing countries, with the higher-quality parts being supplied by domestic manufacturers.

Distribution ratio of MIM markets in Japan (FY2020) (Courtesy JPMA)

View our Advertisers’ index & buyer’s guide on pages 123-125

2014

Stainless steel remained the most widely used material in Japan’s MIM industry in 2020, accounting for 73.2% of production (previous year: 74.8%). Together, stainless steels, Fe-Ni materials, low-alloy steels and magnetic materials accounted for over 89% of production. Magnetic material saw an increase after two years of continuous decrease.

Titanium continued to fluctuate, with the majority of demand coming from the medical device sector.

The JPMA believes that the use of stainless steel will continue to dominate the market, being suited to a wide range of applications. www.jpma.gr.jp

Distribution ratio of materials used for MIM production in Japan (FY2020) (Courtesy JPMA)

Looking for suppliers of materials, production equipment and finished MIM or sinter-based AM parts?

December 2021

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Vol. 15 No. 4

CATAMOLD® MOTION 8620 feedstock for Automotive applications Catamold® motion is BASF’s new MIM feedstock suitable for the production of eRocker Arms for Cylinder Deactivation (CDA), thus contribution to reduce NOx and CO2 emissions for a more sustainable world.

Catamold® motion enters a new era of pre-alloyed, low alloy MIM feedstocks for enhanced and reliable metal parts production in all industries.

Catamold® motion 8620 keeps the wheels in motion

www.catamold.com

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Desktop Metal qualifies 420 stainless steel, nickel alloy IN625 and D2 tool steel for its Production System Desktop Metal, Inc., Boston, Massachusetts, USA, has qualified 420 stainless steel, nickel alloy IN625 and D2 tool steel for use in its Production SystemTM Additive Manufacturing platform. The high-speed Binder Jetting (BJT) machine is based on the company’s bi-directional Single Pass Jetting™ (SPJ) technology.

420 stainless steel A martensitic heat-treatable stainless steel, 420 stainless steel is characterised by its high strength and hardness, as well as its corrosion resistance when exposed to the atmosphere, foods, fresh water, and mild acids when in a fully hardened condition. It is a common material used extensively across a variety of

applications such as surgical and dental instruments, ball bearings, gear shafts, pump and valve components, fasteners, gauges, hand tools, and high-end cutlery.

“Engineers continue to seek out metal Additive Manufacturing as a leading option to drive innovation in design and manufacturing,” stated Jonah Myerberg, CTO and co-founder of Desktop Metal. “We believe our qualification of 420 SS and other high-strength alloys will accelerate the deployment of our AM 2.0 solutions among customers looking to successfully mass-produce critical parts at scale.”

The company’s materials science team has qualified and fully characterised 420 stainless steel additively manufactured on the Production

System and found that it meets MPIF 35 standards for structural Powder Metallurgy parts set by the Metal Powder Industries Federation (MPIF).

Producing 420 stainless steel parts on the Production System platform eliminates the use of tooling and minimises material waste, as well offering shorter production times and part cost compared to conventional manufacturing methods.

Nickel alloy IN625 IN625 is a nickel-chromium superalloy characterised by its high strength, resistance to corrosion and oxidation, excellent weldability, and ability to withstand extreme, elevated temperatures for parts under load.

As such, IN625 is a critical material in high temperature aerospace applications, while its corrosion resistance under a range of temperatures and pressures makes it well suited to applications across marine, power generation, and chemical processing.

sinterbased additive manufacturing next dimension of heat treatment

mut-jena.de integrated sintering furnace for high volume production

MUT ADVANCED HEATING 30

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Industry News

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Cams used in oil and gas or chemical processing applications convert rotary motion into reciprocating linear motion in a machine. D2 tool steel is critical for this application because of its hardness and corrosion resistance (Courtesy Desktop Metal)

“As Desktop Metal continues to drive our internal R&D efforts to qualify more materials for the Production System platform, we are excited to offer customers an all-inclusive Binder Jetting solution to print fully characterised IN625 with excellent properties,” added Myerberg.

Jason Harjo, Director, Mechanical & Electrical Design (Americas), Koch Engineered Solutions, added, “As a transformative combustion equipment company, we are very excited about the release of IN625 for its high temperature and corrosion-resistant properties in flaring and sulfur incineration applications. This will give us much more flexibility in innovative, Additive Manufacturing designs for some of our most difficult applications.”

Desktop Metal’s materials science team has qualified and fully characterised IN625 manufactured on its Production System technology in accordance with ASTM testing requirements. IN625 parts additively manufactured on the Production System platform were reported to eliminate the use of tooling and minimise material waste at a significantly decreased production time and part cost compared to conventional manufacturing methods.

D2 tool steel D2 is used for a wide variety of cold work tools that require a combination of wear resistance and moderate toughness, such as coining and sizing tools, blanking and forming dies, shear cutting tools, gauges, burnishing tools, and other wear parts.

“Our materials science team is constantly working to develop new materials and processes to make 3D printing accessible to all industries and applications,” explained Myerberg. “We are responding to the demand from our customers across manufacturing and industrial industries for materials like D2 tool steel that enable the production of critical forming and cutting tools and in various other applications where high hardness is valued.”

One such application are rotating cams, used in oil & gas or chemicalprocessing applications to convert rotary motion into reciprocating linear motion in a machine. Typically, these parts require multiple manufacturing steps, beginning with CNC machining and following on with broaching of the spline on a separate machine. BJT enables the production of cams in a single build step, reducing both the cost and lead time of the part, while also supporting the production of numerous cam sizes in a single build to accommodate different machines, all without any fixturing or tooling required.

D2 tool steel is critical for this application because of its hardness and corrosion resistance, which ensures a longer lifetime as the cam mechanically interacts with a sliding pin. In addition, because these components are often integrated into machines operating in harsh environments, the corrosion resistance provided by D2 ensures that the parts will perform as intended and not deteriorate.

Desktop Metal’s materials science team has qualified and fully characterised D2 tool steel additively manufactured on Production System technology in accordance with ASTM testing requirements. www.desktopmetal.com

Vol. 15 No. 4 © 2021 Inovar Communications Ltd

• Low weight • Good mechanical stability • Low heat capacity • Solvent and acid resistant • high open porosity • dust- and particle-free surface • homogeneous shrinkage • Absorbtion of the binder into the pores during the debindering process • Very smooth surface finish • Compatibility to Molybdenum, CFC, RSiC • Good to very good thermal shock resistance • Handling and assembly with robots possible

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December 2021 PIM International

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Industry News

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Schunk to offer Additive Manufacturing series production from ExOne Following the recent purchase of an X1 25Pro from The ExOne Company, North Huntingdon, Pennsylvania, USA, Schunk Group, headquartered in Heuchelheim, Germany, has announced that it will integrate metal Binder Jetting (BJT) Additive Manufacturing into its existing series production technologies. Depending on the component, application and quantity, Schunk customers can now choose between metal BJT, Metal Injection Moulding and press & sinter Powder Metallurgy.

Prior to the integration of BJT, Schunk Sinter Metals production

quantities started at 100,000 units from its location in Thale, Germany.

With the increasing move away from the traditional Internal Combustion Engines (ICEs) and the shift to new types of drive, production quantities may vary. The company’s aim is to increase its flexibility in testing and production with both new and existing series equipment and facilities, and to be able to produce new geometries for any type of drive.

“If we still want to be an attractive development partner tomorrow, we have to use and further develop technologies that move our customers

Left to right: Eric Bader (Managing Director, ExOne); Tobias Heusel (Global Account Manager), Daniel Alfonso (Global Business Development Manager), Alexander Gatej (Innovation Manager), Schunk; and Frank Betzler (Regional Sales Manager, ExOne) (Courtesy The Schunk Group)

NanoE €2 million facility expansion for ceramic and metal AM NanoE SAS, Ballainvilliers, France, will invest €2 million in a new facility dedicated to metal and ceramic Additive Manufacturing, doubling its production volume.

This 1000 m2 facility will feature offices, demonstration centre and a manufacturing facility. The investment will be supported by the France Relance recovery plan, which provides up to 50% of the cost.

For three years, the company has been promoting its Zetamix technology – which includes AM machines, furnaces and filaments – to

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democratise ceramic and metal AM. Through this brand, the company markets ceramic and metal filaments compatible with any machines utilising Fused Filament Fabrication (FFF), a Material Extrusion (MEX) process.

“This government support plan allows us to make the investment in one year instead of the two or three we expected,” stated Guillaume de Calan, CEO. The latest additions to the Zetamix line include thermal zirconia, a technical ceramic filament that does not require chemical

December 2021

forward,” stated Tobias Heusel, Global Account Manager, Schunk Mobility.

“We can no longer do this with our existing sintered metal components for combustion engines alone. That’s why we want to integrate innovative 3D printing technologies into our existing series production and open up new applications and markets with new products.”

Eric Bader, Managing Director, ExOne GmbH, added “The combination of our strength in Binder Jetting and Schunk’s extremely sound understanding of Powder Metallurgy and sintering experience creates exactly the intersection that is needed to be a sustainable partner and supplier to future customers together. It takes a fair amount of vision to enter 3D printing here and now. Schunk is clearly demonstrating its commitment to new developments.”

In the future, Schunk intends to continue to focus on automotive and aerospace markets. In addition, it is expected that AM will bring increased flexibility, thus opening the possibility of producing complex components for a wide range of industries. There is already interest reported from a machine manufacturer, for example, but components for the consumer sector, for white goods or the medical industry are also conceivable. www.exone.com www.schunk-group.com debinding, and silicon carbide. Both of these are expected to be available for sale in 2022.

To better achieve its goal of democratisation, NanoE relies on a wide reseller network. In 2021, resellers numbers have increased from five to twenty-five, with over fifty Zetamix systems installed. Zetamix expects to hire twenty-five further resellers to expand its reach and double the number of installed users.

“Our partners around the globe are a key aspect of Zetamix strategy; thanks to their fine knowledge of their respective market and the training we provide, they are able to promote the technology in their countries,” de Calan concluded. www.nanoe.com

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Vol. 15 No. 4

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FuseLab 3D releases new FFF metal AM machine with rotary extruders FuseLab 3D, Peer, Belgium, has launched its new FL300M Additive Manufacturing machine, incorporating a novel rotary extruder for enhanced metal powder based Fused Filament Fabrication (FFF).

The FL300M features a highperformance and high-precision motion system, coupled with FuseLab’s unique extruder design, which is said to result in more reliable builds with better surface qualities and increased densities.

Traditional FFF extruders feed the filament into the melt zone via one or two drive gears, thus limiting the number of points of contact between the drive system and the filament to two, at most. At higher speeds, or increased extrusion forces, this can result in slipping and subsequent under-extrusion. FuseLab believes it has resolved this with a design

based on three drive rollers each offering twelve points of contact: a total of thirty-six engagement points between the drive mechanism and the filament.

The increase in points of contact is said to be particularly beneficial for additively manufacturing with metal-powder-based filaments, which are more fragile due to high metal powder/low binder makeup. The distributed contact of the FL300M’s rotary extruder is intended to minimise the risk of filament failure.

In addition, the non-slip characteristic of the extruder reportedly eliminates under-extrusion, resulting in higher densities, something especially desirable in metal parts.

While the FL300M is optimised for metal powder filaments, it is multi-material capable, with an open filament system allowing for

FuseLab’s rotary Fused Filament Fabrication extruders offer a total of thirty-six engagement points between the drive mechanism and the filament (Courtesy FuseLab)

filaments up to 2.85 mm in diameter.

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December 2021

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Vol. 15 No. 4

Industry News

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BASF’s Forward AM opens new technology centre in Detroit Forward AM, an Additive Manufacturing solutions brand of BASF 3D Printing Solutions GmbH, headquartered in Heidelberg, Germany, has opened a new Additive Manufacturing Applications Technology Center (ATC) in Detroit, Michigan, USA, in cooperation with Michigan State University (MSU). This follows the opening of the company’s AMTC in Shanghai, China in August. The ATC will reportedly serve as the hub of expertise for solutions in the North American AM market. The cooperation is said to combine the strengths of the company and the university in order to offer customers fully integrated AM solutions. Forward AM contributes with a wide range of high-performance Additive Manufacturing materials and rich engineering expertise, while MSU brings years of technical expertise and the motivation to be on the cutting edge of new ideas to support the next generations of AM services and design solutions.

“With this step we are significantly strengthening our offerings in North America,” stated François Minec, Managing Director BASF 3D Printing Solutions. “By collaborating with Michigan State University, we create a unique combination of science and industry expertise – ideal conditions to drive innovation in Additive Manufacturing together with our customers.”

Through the ATC, new value-adding technical services are available to customers, such predictive modelling, increasing innovation potential with customers across North America.

Forward AM has installed more than twenty AM machines of various AM technologies such as Laser Beam Powder Bed Fusion (PBF-LB) and Fused Filament Fabrication (FFF), a Material Extrusion (MEX) based technology, at the ATC. The cooperation between Forward AM and MSU is complemented with an investment by BASF Corporation

Vol. 15 No. 4 © 2021 Inovar Communications Ltd

in the Scale-up Research Facility (SuRF) space. This investment is said to be strengthening BASF’s strategy in Additive Manufacturing and its pursuit toward more sustainable industrial solutions. The ATC is expected to enable shared resources that combine education and industry to drive the industrialisation of AM in the Americas.

Doug Gage, vice president for Research and Innovation at Michigan State University, commented, “MSU is committed to strong industry

partnerships as an engine to drive innovation, economic opportunities, and skills development that meet emerging technology needs. The Scale-up Research Facility (SuRF) in Detroit, established with funding from the Michigan Economic Development Corporation and Department of Energy through the Institute for Advanced Composite Manufacturing Innovation, is a prime example of the effectiveness of place-based innovation.” www.forward-am.com www.msu.edu

December 2021 PIM International

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Industry News

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Lithoz remotely installs CeraFab ceramic AM machine at Australian University Lithoz GmbH, Vienna, Austria, reports that it has remotely installed a Lithoz CeraFab ceramic AM machine at the University of Wollongong (UOW), Australia. A partnership between Lithoz, UOW and Australiabased AM provider Objective3D enabled the remote installation of the machine, which will be used for a range of applications in the development of bioprinting hardware.

Purchased by the Australian National Fabrication Facility (ANFF) Materials Node, based at UOW, the machine is intended for use at the Translational Research Initiative for Cellular Engineering and Printing (TRICEP). TRICEP works with research institutions and industry to develop innovative technologies using what it calls ‘3D bioprinting’ – the use of AM for biomedical applications. pim international 2016-09.pdf

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Dr Johannes Homa, Lithoz CEO, explained that the installation project highlighted the importance of agile working. “We are world and industry technology providers for ceramic 3D printing systems and materials, and have been working in research and industry for more than ten years. After the past year, it has become clear to us just how critical flexibility in the manufacturing world is, and we are very happy that this remote installation has been a success.”

The investment from ANFF will reportedly give TRICEP a highly flexible means of customising and producing devices to support material development research globally.

TRICEP Associate Director A/Prof Stephen Beirne stated that the team was thrilled to have access to this exciting new technology.

A partnership between Lithoz, the University of Wollongong and Objective3D enabled the remote installation of the CeraFab ceramic AM machine in Australia (Courtesy Lithoz GmbH) “The CeraFab 3D printer provides us with access to new families of materials with properties and printing characteristics that greatly expand our service and research capabilities.

The system will be immediately put to use in the development of nextgeneration biofabrication hardware and implantable structures.” www.lithoz.com www.uow.edu.au

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December 2021

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Sandvik releases interim report for third quarter 2021 Sandvik AB, headquartered in Stockholm, Sweden, has released its interim report for the third quarter of 2021. The company stated that revenues increased organically by 13%, while adjusted operating profit was reported at SEK 3,817 million (Q3 2020: 2,626 million). Order intake saw organic growth of 21% to SEK 26,292 million.

Sandvik Materials Technology Sandvik Materials Technology saw order intake increase 29%, with a 1% increase in revenue. Strong order intake development was noted in all major regions, compared against the corresponding period in the preceding year, with the strongest development seen in North America.

Optimism in oil & gas and aerospace segments continued to improve, with an increase in the number of orders being placed, though levels were still said to remain low.

Sandvik Manufacturing and Machining Solutions Sandvik Manufacturing and Machining Solutions saw order intake grow 16% and revenues up 18% year on year, driven by the automotive and engineering sectors. Regional order intake growth was seen at 16% in Europe, 19% in Asia and 13% in North America, although lower production volumes in the automotive sector due to semi-conductor shortages were noted.

Sandvik Machining Solutions acquired a majority stake in the solid round tools company Chuzhou Yongpu. Sandvik Manufacturing Solutions increased the pace of its M&A activities, resulting in three strategically important acquisitions in and after the quarter.

Sandvik Mining and Rock Technology Sandvik Mining and Rock Technology reported order intake and revenue increases of 26% and 12%, respectively. There has been a reported all-time high order intake in aftermarket, with organic order growth of 38%, and strong equipment growth of 13% year on year. Broadbased underlying demand in both infrastructure and mining with order intake growth of 68% in North America; 19%, Europe; and 10%, Asia.

During the quarter, Sandvik Rock Processing Solutions expanded its offering within crushing and screening with the launch of the track-mobile impact crusher QI353.

Based on a new modular platform it can operate in both primary or secondary crushing applications, providing a sustainable solution at reportedly lower operational costs.

“Sandvik has become a more growth-oriented company. We deliver on strong organic growth and have already added over SEK 8 billion in annual revenues from strategic acquisitions. At the same time, we have taken important steps to become a more digitally focused company,” stated Stefan Widing, president and CEO. “With our leading positions, Sandvik has a strong and obvious role in supporting our customers’ digital transformation; a shift that will improve productivity, and lead to significant sustainability gains. As a growth-focused, resilient and high-performing company, and with an underlying demand for our solutions, Sandvik is well positioned to execute on profitable growth, and to deliver long-term shareholder value.” www.sandvik.com

Send us your news Submitting news to PIM International is free of charge and reaches a global audience. For more information, contact Paul Whittaker: paul@inovar-communications.com

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Fitbit’s Luxe fitness Formnext + PM South China reports tracker enhanced successful debut event through use of After three days of activity across + PM South China, and had a pleasant MIM 15,000 m of fair ground, the first experience networking with them.

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Fitbit, San Francisco, California, USA, recently launched Fitbit Luxe™, a fitness and wellness tracker that features a stainless steel case produced using Metal Injection Moulding. The use of MIM continues to gain success in the 3C (computers, communications and consumer electronics) sector, particularly where aesthetics and precision are a priority.

The Luxe’s design features a profile that sits lightly on the wearer’s wrist, creating a jewellery-like appearance and feel. Fitbit applied a modern take on traditional jewellery-making techniques by using MIM to create the case, providing the aesthetics expected of handcrafted jewellery, while delivering the precision required to enable its advanced sensor technology. The company states that the design has resulted in one of its most fashionable and comfortable devices yet.

James Park, VP, GM and co-founder of Fitbit, commented, “We’ve made major technological advancements with Luxe, creating a smaller, slimmer, beautifully designed tracker packed with advanced features – some that were previously only available with our smartwatches – making these tools accessible to even more people around the globe.” www.fitbit.com

The recently launched Fitbit Luxe features a stainless steel MIM case (Courtesy Fitbit)

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Formnext + PM South China is reported to have ended with much enthusiasm, following an event which the organisers believe will cement its place as one of the leading fairs in the region for Additive Manufacturing, Powder Metallurgy, design, software and processing technologies. Leveraging the success of Formnext in Frankfurt and PM China in Shanghai, Formnext + PM South China took place in Shenzhen, September 9–11, 2021, and welcomed some 199 exhibitors from around the world.

Jointly organised by Guangzhou Guangya Messe Frankfurt Co Ltd and Uniris Exhibition Shanghai Co Ltd, Formnext + PM South China held a series of over eighty concurrent events, featuring academics and experts discussing the emerging trends within the industry both in China and worldwide.

Aiping Sun, Senior Engineer, New Materials Applications, OPPO, stated, “I was delighted to see a large selection of Powder Metallurgy suppliers gathered here at Formnext

In addition to the exhibition, I also found the concurrent programme presentations to be extremely useful, specifically how key industry players share their latest technological findings and market insights within the Powder Metallurgy space.”

Jerry Ma, General Manager – Asia Pacific, SLM Solutions (Shanghai), added, “We’ve been exhibiting at Formnext in Frankfurt for years, and when we learnt that the fair will be held in China, we decided to join as it is a trusted platform for the industry. Additive Manufacturing is an emerging sector in China and has seen rapid growth over the past five years. The market has a lot of potential, especially as the 14th Five-Year Plan calls for cultivating advanced manufacturing industry clusters, and, together with the government’s increased investment into aerospace technology, these will provide ample opportunities for the Additive Manufacturing industry.” www.formnext-pm. hk.messefrankfurt.com

EPHJ trade show reports positive outing for 2021 After a twenty-seven month break, the EPHJ trade show returned in September, with 530 exhibitors from thirteen countries showcasing their products and technology to some 12,000 visitors. While 90% of exhibitors declared a watchmaking activity and 59% a microtechnology activity, nearly half of all exhibitors now also listed a medtech activity, illustrating an increasing diversification into this sector.

Travel restrictions meant that the majority of exhibitors this year were more local, with just 25% of exhibitors from outside of Switzerland. The Swiss cantons most represented among the exhibitors were Neuchâtel

December 2021

(94), Jura (66), Bern (64), Geneva (55), Vaud (45) and Zürich (16).

The 2021 Exhibitors’ Grand Prize was awarded to the STS based in Le Sentier, Switzerland. Elected by its peers, STS was rewarded for its alternative solution to rhodium, which has reportedly become the most expensive metal in the world. The company’s alternative, developed with white platinum, allows certain parts of the watch’s movement to feature the same properties and look as rhodium, without the use of the prohibitively costly element.

The next EPHJ trade show is scheduled to take place from June 14–17, 2022, in Geneva, Switzerland. www.ephj.ch

© 2021 Inovar Communications Ltd

Vol. 15 No. 4

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XJet launches automated postprocessing system for AM parts XJet Ltd, Rehovot, Israel, has launched a new system to automate the post-processing of XJet parts called SMART (Support Material Automatic Removal Technology).

The equipment is said to provide the last link in the chain for automated end-to-end Additive Manufacturing using XJet NanoParticle Jetting™ (NPJ).

XJet has launched its SMART system to automate the post-processing of XJet parts (Courtesy XJet Ltd)

SMART is reported to work seamlessly with all XJet Carmel AM machines, automating the removal of the soluble support material and eliminating the dependency on operator expertise. The water-based system has a selection of programs – differing by water level, flow rate and other parameters – to suit any given tray of parts. Using intelligent algorithms, the SMART system suggests the appropriate program.

“The SMART station delivers the final missing link in AM,” stated Dror Danai, XJet CBO. “Now XJet’s awardwinning soluble support material becomes even easier to remove, making part production really easy and allowing virtually any geometry as water can access even the smallest channels that XJet ultrahigh-quality printing enables.”

“This is all part of XJet’s drive to support manufacturers in a true production environment,” Danai continued. “XJet technology is designed for manufacturers who want to build better parts for realworld applications. We examine

the whole workflow to see what can be done to reduce production time, minimise operational costs, and ensure the premium quality of parts is repeatable.”

XJet explains that its soluble support material works with all its ceramic and metal build materials and the ability to melt away the support ensures any ultra-fine details and complex geometries of parts are preserved throughout the postprocessing process. The introduction of end-to-end automation – from support generation to support removal – allows manufacturers to produce premium quality parts, with all the benefits of AM. Danai added, “One of our beta customers has reported a 90% reduction in cleaning time and hassle using the XJet SMART station, so we’re delighted with the results!

Additive Manufacturing is supposed to offer true design freedom and complex geometries with zero additional cost. Our soluble support material delivers those capabilities – even for tiny cavities. Now with the SMART station, our customers can benefit from simple, predictable, low-cost operation.” www.xjet3d.com

Plansee receives award from Tyrolean government for its 100-year anniversary The Plansee Group, headquartered in Reutte, Austria, has received an award from the Tyrolean government in recognition of the group’s 100-year anniversary. Michael Schwarzkopf, chairman of the Plansee Group Supervisory Board, accepted the certificate, which was presented by Sonja Ledl-Rossmann, president of the Tyrolean Parliament, and Christoph Walser, president of the Tyrolean Chamber of Commerce.

Governor Günther Platter commented, “As a special recognition of the success story, the company will in future bear the Tyrolean coat of arms, with which the state of Tyrol honours individuals and companies for outstanding services.”

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Founded in 1921, the Plansee Group is a world leader in the fields of refractory metals and hardmetals, covering the entire production process from the ore through to customerspecific components. It has over fifty global production locations and over 13,000 employees.

The group also hosts the well respected Plansee Seminar, an international conference on refractory metals and hard materials. Now in its 20th edition, the seminar will take place at the group’s Reutte headquarters on May 30–June 3, 2022.

The presentations at the 20th Plansee Seminar will include topics where products based on refractory metals and hard materials play

December 2021

The Plansee Group has received an award from the Tyrolean government in recognition of its 100th anniversary (Courtesy Plansee Group) an important role, or where they are promising alternatives to present material solutions. Applications, materials, processes, digital transformation, and testing methods will be addressed in keynote lectures and contributed papers. www.plansee.com

© 2021 Inovar Communications Ltd

Vol. 15 No. 4

Industry News

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Altair launches consortium to support Material Data Center Altair, Troy, Michigan, USA, has The AMDC consortium is intended announced the launch of the Altair® to shape the growth of this cloudMaterial Data Center™ consortium, based database, which gives designed to help make its Altair engineers and designers instant Material Data Center (AMDC) a access to accurate data on a vast best-in-class materials information array of metals, plastics, and composresource to support innovative ites for use with CAE applications. product design and manufacturing.

“We are delighted to welcome The development of sustainable, industry leaders such as Nikola efficient, minimum-weight Motors and the National Institute for designs requires accurate, multiAviation Research to the consortium,” domain material properties; the stated Stephanie Buckner, senior vice selection of these materials is a president of customer engagement vital step in product development. and corporate development, Altair.

The AMDC furnishes users with “Members will play a central role in the material properties needed for driving AMDC, maximising its value tasks such as virtual prototyping to engineers and designers as they and simulation, enabling pursue new engineering challenges.” users to browse, search, and Consortium members will share compare materials in a standalone real-world experiences and best pracapplication or through the interface tices, working to ensure the AMDC Mixer Extruders of their simulation and optimisation roadmap reflects the needs of its tools. customer base. By enhancing the

breadth and scale of the AMDC, the consortium is expected to make a valuable contribution to an asset that serves global engineering and manufacturing communities.

In addition to providing strategic guidance, organisations serving on the consortium’s steering committee will have early access to the latest software and innovations from Altair.

“The foundation of predictable CAE structural simulations lays in the proper definition of standardised building block testing procedures for material characterisation and processing the experimental data into verified and validated CAE material cards,” added Dr Gerardo Olivares, Director and Senior Research Scientist at the Wichita State University’s National Institute for Aviation Research. “NIAR’s Advanced Virtual Engineering and Testing research group is proud to be a steering committee member of Altair’s MateZ Blade Mixers rial Data Center consortium.” www.altair.com

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December 2021 PIM International

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3DGBIRE and MIM specialist CMG Technologies to provide AM debinding & sintering services in UK The sole distributor of BASF Forward AM products in the UK and Ireland, 3DGBIRE, Chorley, Lancashire, UK, and legacy user of BASF Catamold feedstock for Metal Injection Moulding, CMG Technologies, Woodbridge, Suffolk, have announced a partnership to provide UK-based debinding and sintering options for parts manufactured from BASF Forward AM’s Ultrafuse metal filaments.

Additional aims of the partnership will include finishing services for debound and sintered AM parts, as well as encouraging the adoption of AM by facilitating the training, upskilling and professional development of staff within customer organisations.

Because the service debinds and sinters additively manufactured and MIM parts in the same furnaces at the same time, it is stated that costs are reduced, along with lead times for customers using these services.

“3DGBIRE and CMG Technologies have merged two industries in their service offering: conventional Metal Injection Moulding based on Catamold technology and

3DGBIRE and CMG Technologies have partnered to process parts manufactured from BASF Forward AM metal filaments (Courtesy CMG/3DGBIRE)

3D printing with metal Fused Filament Fabrication [FFF] using Ultrafuse 316L or 17-4PH,” stated Tobias Rödlmeier, Business Development Manager for Metal Filaments at BASF Forward AM. “We are very pleased that this efficient solution is now open to our UK Ultrafuse metal filament customers.”

Previously, parts had to be shipped to Germany, which has become an increasingly costly and prolonged process according to Paul Croft, 3DGBIRE Director. “Before Brexit you could quickly and costeffectively ship parts and goods to Germany, that is no longer the case so we were very keen to establish a debinding and sintering offering in the UK that enables customers to realise the huge cost saving opportunities of Additive Manufacturing.”

Rachel Garret, Managing Director, CMG, added, “CMG is thrilled to be expanding our relationship with BASF into the AM market. We have over twenty years of experience within the MIM industry and our extensive knowledge developed over the last two decades means that this is a very natural progression for us. We can apply our skills within debinding and sintering of MIM parts directly to the debinding and sintering of 3D metal printed parts to ensure we are processing parts to the highest quality and accuracy.” www.3dgbire.com www.cmgtechnologies.co.uk

Example parts produced using BASF’s ultrafuse filament (Courtesy CMG/3DGBIRE)

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Sandvik AM announces additions to powder sales teams Sandvik Additive Manufacturing, a division of Sandvik AB, headquartered in Stockholm, Sweden, has strengthened its Osprey® metal powders sales team with the appointment of Dr Martin McMahon has Head of Global Powder Sales. The company also announced that Manuel Winkler and Dr Olesia Khafizova have joined as sales representatives, reinforcing the EMEA metal powder sales team.

McMahon has a PhD in Materials Science and Engineering from Liverpool University, UK, and has gained extensive experience from the metal Additive Manufacturing sector, where he’s held several senior positions with companies such as Renishaw and 3T Additive Manufacturing. Joining Sandvik from his most recent position as Business Development Director at Aluminium Materials Technologies, McMahon has reportedly played a key role in introducing AM to a number of industrial sectors such as aerospace, automotive, defence, oil & gas, energy, medical, and food.

Winkler has a master’s degree in technical management from Clausthal University of Technology, Germany, and started his career in quality management, consulting and sales related roles at international enterprises and global manufacturers for automotive and the processing industry. Formerly, he entered Sandvik Hyperion as a Sales Specialist in metal machining and built up a successful customer portfolio which he previously pursued at Hyperion Materials and Technologies.

Dr Olesia Khafizova has a PhD in Mechanical Engineering from Saint Petersburg Mining University, Russia, where she majored in improving mechanical properties of welded joints. Since 2016, she has been a Market Manager for Composites and Additive Manufacturing at Shimadzu Europe GmbH, where she managed R&D projects on material testing solutions in collaboration with the global headquarter and international industrial and research partners. Khafizova successfully supported the sales of products for AM materials assessment and handled aspects of the sales and postsales process, and has also been involved in regulatory requirements such as DIN, ISO, ASTM and Nadcap. www.additive.sandvik

Dr Martin McMahon (left), Manuel Winkler (centre) and Dr Olesia Khafizova (right) have joined Sandvik Additive Manufacturing (Courtesy Sandvik AB)

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Ti6Al4V alloy parts produced by metal Fused Filament Fabrication (FFF) compared to MIM and other processes Fused Filament Fabrication is an Additive Manufacturing process pioneered by researchers at Rutgers University in the USA in the mid 1990s, initially using 17-4PH stainless steel and Si3N4 ceramic powders.

The FFF process, which today is categorised as a Material Extrusion (MEX) AM process, is described as a technology that uses a suitable metal-polymer feedstock to produce fused metal filaments which are extruded during a layer by layer Additive Manufacturing process to create green parts. The green parts can then be thermally processed to debind and sinter the parts using technology similar to Metal Injection Moulding.

Early research on Fused Filament Fabrication lacked detailed knowledge of metal filament properties, effect of processing and build parameters, sintered properties, etc.

This has, to a large extent, been rectified with a resultant surge in interest in FFF technology in recent years.

Currently, a number of polymer-metal feedstock systems are reported, and commercial FFF AM machines available on the market including those from Markforged (ADAM™: Atomic Diffusion Additive Manufacturing), Desktop Metal (BMD™: Bound Metal Deposition) and Pulse 3D Printer

(Matterhackers) with claimed capabilities to process 17-4PH, 316L, H13, A2, D2 tool steels, Cu, and Inconel 625 alloy parts.

There remains, however, a lack of basic understanding of the materials and parameters at each step of the FFF process (Fig. 1), and a group of researchers at the Materials Innovation Guild, University of Louisville, Louisville, Kentucky, USA, in collaboration with researchers at CSIR-Central Glass and Ceramic Research Institute, Kolkata, India, and Sakarya University of Applied Sciences, Sakarya, Turkey, have undertaken a detailed study into the feasibility of using FFF to produce Ti6Al4V alloy parts.

The results of this study were recently published in a paper entitled ‘Additive manufacturing of Ti6Al4V alloy by metal fused filament fabrication (MF3): producing parts comparable to that of metal injection molding’ in Progress in Additive Manufacturing, February 11, 2021.

The paper outlines effective powderbinder feedstock preparation for filament fabrication; the Additive Manufacturing of high-density green parts followed by binder removal and sintering to achieve properties and microstructures comparable to other

manufacturing processes, such as MIM, correlated with FFF processed Ti6Al4V alloy properties.

The authors used a Ti6Al4V powder having a median particle size of 30 µm which was mixed with a binder consisting of three components: a backbone polymer (30–50 wt.%), an elastomer (20–30 wt.%), and a plasticising phase (20–40 wt.%).

The backbone component is said to provide the necessary strength and stiffness to the filament, as well as assisting component shape retention during thermal debinding. The elastomer provides flexibility to the filament so that it can be spooled into coils for the ease of manufacture and storage, and the plasticising phase helps decrease feedstock viscosity and improve overall metal powder loading into the binder matrix. The critical solids loading of 59 vol.% was selected for preparing the feedstock filaments for further FFF. The authors reported that a constant shear rate of 50 s−1 at 160°C was used to evaluate the variations in feedstock viscosity to measure its homogeneity. Additionally, powder concentration post mixing was also evaluated by measuring the feedstock’s pycnometer density in granule and filament forms.

The Ti6Al4V feedstock was then extruded into filaments having a consistent diameter of 1.75 ± 0.05 mm using a capillary die with an L/D ratio of 30/1.75 mm on a capillary rheometer. The extrusion temperature was

Fig. 1 Overview of the Fused Filament Fabrication process used in the present study to fabricate Ti6Al4V parts (From paper: ‘Additive Manufacturing of Ti6Al4V alloy by metal Fused Filament Fabrication (MF3): producing parts comparable to that of Metal Injection Molding’ in ‘Progress in Additive Manufacturing’ by Paramjot Singh, et al., February 11, 2021)

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Shrinkage (%) X

Y

Z

Yield strength (MPa)

14 ± 0.5

15 ± 0.5

15 ± 0.5

745 ± 10

Density (%) 94.2 ± 0.1

Ultimate tensile strength (MPa)

Elongation (%)

875 ± 15

17 ± 3

Table 1 Physical and mechanical properties of sintered FFF Ti6Al4V parts (n = 4) (From paper: ‘Additive Manufacturing of Ti6Al4V alloy by metal Fused Filament Fabrication (MF3): producing parts comparable to that of Metal Injection Molding’ in ‘Progress in Additive Manufacturing’ by Paramjot Singh, et al., February 11, 2021)

Relative density (%)

Yield strength (MPa)

Ultimate tensile strength (MPa)

Elongation (%)

Source

MIM

97.3 ± 1.2

750 ± 25

860 ± 40

14 ± 4

[18–22]

L-PBF

99.7 ± 0.15

1150 ± 80

1270 ± 70

6±2

[23–25]

100

830 ± 10

930 ± 10

13 ± 1.5

[26]

Process

Wrought (annealed)

Table 2 Properties of Ti6Al4V components produced using different manufacturing routes. (From paper: ‘Additive Manufacturing of Ti6Al4V alloy by metal Fused Filament Fabrication (MF3): producing parts comparable to that of Metal Injection Molding’ in ‘Progress in Additive Manufacturing’ by Paramjot Singh, et al., February 11, 2021)

105°C with a uniform extrusion speed of 0.1 mm/s with pressure measured at the capillary entrance corresponding to 40 ± 3 MPa. The resulting continuous filament with 59 vol.% of Ti6Al4V powder was found to exhibit a density of 2.96 ± 0.002 g/cm3, and Modulus and UTS of 170 ± 20 MPa, 1.15 ± 0.15 MPa, respectively. These stable properties resulted in continuous material extrusion to produce dense green parts with a density of 2.92 ± 0.002 g/cm3 (98.5 ± 0.6% relative to that of feedstock density of 2.96 g/cm3).

Several FFF experiments were done using the developed Ti6Al4V alloy feedstock system. Initial results showed that an extrusion temperature of 240°C enabled consistent material flow due to optimal feedstock viscosity during additive manufacturing. Similarly, a bed temperature of 65°C resulted in good adhesion of the part to the build plat

form during the entire build process.

A layer height of 150 μm with 100% infill was selected to achieve close packing of printed beads leading to dense green parts. The selected bead deposition angle of alternating 0° and 90° resulted in sound and dense parts. A build speed of 10 mm/ s−1 resulted in good infill, consistent material flow (at extrusion multiplier of 115%), and strong inter-bead and inter-layer bonding.

The researchers stated that the FFF green parts were debound using a two-step debinding procedure conventionally used in MIM part processing. The parts were first solvent debound in n-heptane at 64°C for 4 h, followed by thermal debinding in partial vacuum at four holding temperatures of 250°C, 330°C, 440°C and 550°C, respectively, for complete polymer binder removal. Sintering was done in the same furnace at a temperature of 1250°C for 4 h with

partial vacuum and continuous argon flow to minimise oxidation.

Table 1 shows as-sintered part properties, with current conditions achieving a relative density of 94.2 ± 0.1% with an average shrinkage of 14.5 ± 0.5% in all three directions (X–Y-Z). The authors attribute isotropic shrinkage in all three directions to the uniform powder distribution in the green parts as a result of homogeneous feedstock/filament use in addition to optimal build parameters.

The authors concluded that optimal FFF build parameters can produce Ti6Al4V parts with mechanical properties comparable to those of MIM parts. The Laser Beam Powder Bed Fusion (PBF-LB) data for ultimate tensile strength was 45% higher than FFF, but 65% lower in elongation. www. https://www.springer.com/ journal/40964

Advertisers’ index & buyer’s guide Find new suppliers of materials, production equipment and finished MIM or sinter-based AM parts on pages 123-125

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Sintering and creep properties of MIM titanium aluminides (Ti(43-47) Al5Nb0.2B-0.2C) Titanium aluminides show outstanding high temperature mechanical properties with low density, making them attractive light materials for aerospace and automotive applications. However, conventional processing methods that involve solidification (e.g., casting), can result in segregation which can be eliminated only through thermomechanical treatments. Powder metallurgical processes, including

Metal Injection Moulding, can offer both near-net shape fabrication to substantially reduce manufacturing costs, as well as providing a fine and isotropic microstructure in small to medium complex shaped parts.

Some research has already indicated that MIM produced titanium aluminides have good mechanical properties at room temperature achieving a tensile strength of >600 MPa. There is, however,

(a)

(b)

(c)

(d)

(e)

(f)

Fig.1 Microstructures of sintered specimens at different temperatures. a) 43Al sintered at 1450°C. b) 43Al sintered at 1500°C. c) 45Al sintered at 1450°C. d) 45Al sintered at 1500°C. e) 47Al sintered at 1450°C. f ) 47Al sintered at 1500°C. (From paper: ‘Sintering and creep resistance of Powder Metallurgy processed Ti-(43-47)Al-5Nb-0.2B-0.2C’ by J Soyama, et al., Journal of Advanced Engineering Materials (Vol. 22, 2020, 2000377)

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only limited information available on the creep properties of these sintered materials, and how the different microstructural features of sintered TiAl (such as colony size, lamellar spacing, presence of precipitates, porosity, etc.) influence creep properties. Understanding these unique microstructural characteristics is important to allow wider application of MIM titanium aluminides.

Recent collaborative research undertaken at Universidade Estadual de Campinas, Brazil, and HelmholtzZentrum Hereon, Germany, has been investigating the effect of Al variations on the sintering behaviour and creep resistance in MIM processed titanium aluminides based on the alloy TNB-V5 (Ti45Al5N0.2B-0.2 C at%). The results of this work have recently been published in a paper by J Soyama, W Limberg, T Ebel, and F Pyczak in the journal Advanced Engineering Materials (Vol.22, 2020, 2000377, 7pp).

The authors reported that an argon gas atomised prealloyed Ti45Al5Nb0.2B-0.2C (TNB-V5) powder (<45 µm) was used as the starting material, and to achieve the aluminium variations high-purity elemental titanium and aluminium powders with particle size also of <45 μm were added to the prealloyed TNB-V5 powder. The titanium addition was used to decrease the aluminium content to 43 at% designated 43Al, whereas addition of elemental aluminium increased it to 47 at% and was designated 47Al. In addition, high-purity niobium and boron powders were added in small amounts to keep the relative composition constant at the TNB-V5 value.

The binder system used to prepare MIM feedstocks from these powder mixtures was composed of paraffin waxes, polyethylene-vinyl-acetate, and stearic acid. The paraffin waxes and stearic acid were removed chemically in a bath of hexane for 15 h at 45°C. The remaining backbone polymer was removed thermally inside the sintering furnace. The feedstock was injection moulded to produce tensile test bars from which

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were cut cylindrical specimens of about 8 mm in length and 4.1 mm diameter.

The sintering temperatures investigated were 1450°C and 1500°C with a dwell time of 2 h in a high vacuum of ≈10-4 mbar. After sintering, the

(a)

8

cooling rates were in the order of 10°C min-1 from the sintering temperature. The authors stated that the process of sintering is very sensitive and based on the dilatometry results, it was possible to consider the two sintering temperatures of 1450°C and

Sintered at 1500°C / 2 h Compression creep test at 800°C / 350 MPa

7

43 Al

6 Strain (%)

5 47 Al

4 3

45 Al

2 1 0

0

5

10

15

20

25

30

Time (hours) (b)

1E-3

Sintered at 1500°C / 2 h Compression creep test at 800°C / 350 MPa

Creep rate (s-1)

1E-4 1E-5 1E-6

43 Al 47 Al

45 Al

1E-7 1E-8 0

1

2

3

4

5

6

7

8

Strain (%)

Fig. 2 Compression creep curves of different aluminium variations measured at 800°C and 350 MPa loading: (a) Creep strain (b) Creep rate. (From paper: ‘Sintering and creep resistance of Powder Metallurgy processed Ti-(43-47) Al-5Nb-0.2B-0.2C’ by J Soyama, et al., Journal of Advanced Engineering Materials (Vol. 22, 2020, 2000377)

Alloy

Ultimate tensile strength [MPa]

Strain at break [%]

43Al

527 ± 34

0.5 ± 0.1

TNB-V5 (45Al)

622 ± 30

0.5 ± 0.1

47Al

341 ± 90

0.3 ± 0.1

Table 1 Room temperature tensile properties of specimens sintered at 1500°C for 2 h. (From paper: ‘Sintering and creep resistance of Powder Metallurgy processed Ti-(43-47)Al-5Nb-0.2B-0.2C’ by J Soyama, et al., Journal of Advanced Engineering Materials (Vol. 22, 2020, 2000377)

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1500°C. In the case of 43Al and 47Al, a lower temperature could suffice for proper sintering as densification took place below 1500°C. However, the higher sintering temperature of 1500°C could improve densification due to the presence of liquid phase, as in the case of TNB-V5 (45Al).

Fig. 1 shows SEM images of specimens with the three aluminium variations sintered at 1450 and 1500°C for 2 h. In all cases, a fully lamellar microstructure was achieved with different colony sizes. From the SEM images it was possible to identify pores, represented by the dark (mostly circular features) elongated particles that correspond to borides and areas of increased Nb content, as shown in Fig.1b. It was also established that colony size and porosity were influenced by the sintering temperatures.

Sintering at 1450°C led to higher porosity of ≈10% in the case of the most porous 47Al, whereas sintering at 1500°C could significantly decrease the porosity to values <1% for the alloys with 43Al and 45Al, whereas for 47Al, a value of about 7% was achieved.

The researchers also investigated the mechanical properties of the MIM TiAl alloys. They established that, at room temperature, high tensile strength of around 500–600 MPa was achieved for Ti45Al5Nb0.2B0.2C and Ti43Al5Nb0.2B-0.2C, whereas Ti47Al5Nb0.2B-0.2C resulted in reduced tensile strength due to higher porosity (Table 1).

The most creep-resistant alloy was Ti45Al5Nb0.2B-0.2C, which could be sintered to very low porosity and showed serrated colony boundaries.

For the same sintering parameters, Ti47Al5Nb0.2B-0.2C showed higher creep resistance in comparison to Ti43Al5Nb0.2B-0.2C (Fig. 2), which was attributed to the larger colony size achieved after sintering induced by the higher Al content. This, they state, indicates that the effect of porosity was secondary to colony size in compressive creep at 800°C and 350 MPa loading. www.onlinelibrary.wiley.com/ journal/15272648

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Potential of using MIM Ti and Ti alloys for aircraft components Metal Injection Moulding has been receiving increasing attention as a promising technique for the manufacture of complex shaped parts from Ti and Ti alloys for a range of applications in biomedical, aerospace, automotive and other industries.

However, few applications currently exist due to the need to use high cost, fine (<45 μm), low oxygen, spherical titanium powder. Using less expensive hydride-dehydride (HDH) Ti powder could improve the competitiveness of MIM-Ti and Ti alloys for larger parts, but processing issues remain.

A review paper on the possibilities and problems of using MIM for Ti and Ti alloy aircraft parts, including 131 references from researchers around the world spanning the past two decades, was recently presented

by Dmitry M Krotov from the Bauman Moscow State Technical University, Moscow, at the XLIV Academic

(a)

Space Conference held in Moscow.

The paper, which was published in the AIP Conference Proceedings in October 2021, discusses the potential of using MIM technology to manufacture small to medium Ti part in sizes up to 50 mm, wall thickness up to < 5.0 mm and < 50 g in weight, with complex geometries. Aspects covered by the author include: Ti powder type and particle size and shape, impurity contents of the powder (especially oxygen, which reduces the sintered materials tensile ductility), cold processability, fatigue resistance and corrosion resistance. The author also covered the influence of small additions of alloying elements such as iron, nickel or boron on final sintered density and microstructures of MIM-Ti and Ti alloy parts.

The author stated that the use of lower-cost titanium hydride powder (TiH2) as an alternative to more

(b)

150 μm (c)

200 μm (d)

40 μm

150 μm

Fig.1 Microstructures of MIM-Ti samples: (a) commercially pure Ti with a density of 96.5%; (b) Ti6Al4V with a sintered density of 96.4% (c) Ti6Al4V0.5B with a density of 97.7%, and (d) T16Nb with a density of 95%. (From paper: ‘Possibilities and problems of using MIM technology in manufacturing part of aircraft elements made of titanium and titanium alloys’ by D M Krotov, published in the AIP Conference Proceedings, October 2021)

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expensive spherical Ti and Ti alloy powders is an important development for MIM-Ti components with resulting good mechanical properties.

Releasing hydrogen atoms during thermal debinding and sintering of MIM-Ti parts prevents the absorption of Ti oxygen, which, in turn, maintains the final oxygen level as low as in the starting powder.

A lot of research work has been published on the MIM of the commonly used Ti6Al4V alloys, mainly for biomedical applications. Studies have shown that the room temperature tensile strength of these MIM Ti6Al4V alloys can reach 800 MPa with elongation up to 15%, which are said to be promising properties for the aerospace industry. Fig. 1 shows examples of microstructures for MIM Ti6Al4V which indicate that there is a typical plate structure with small fractions of remaining porosity. Fig. 1(c) shows a significant improvement in the microstructure and density of Ti6Al4V alloy by adding 0.5% boron to the starting powder.

The Ti10V2Fe3Al alloy developed for aerospace applications has also been investigated using MIM. This alloy attained a sintered density of 97%, a tensile strength of 1050 MPa, and elongation of 5% under optimised MIM conditions. There is considered to be scope to increase these properties further by post-processing methods such as Hot Isostatic Pressing (HIP).

Titanium aluminides are another group of Ti alloys which have been investigated using MIM processing because their high strength-todensity ratio and excellent resistance to creep and oxidation at high temperatures. However, mechanical properties of the MIM TiAl parts were low even after HIP compared with cast alloys. The biggest problem remains the high oxygen uptake during the debinding and sintering processes. https://aip.scitation.org/journal/ apc

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CHINA’S LEADING SUPPLIER OF MIM POWDERS ADOPTING ADVANCED GAS AND WATER COMBINED ATOMIZATION TECHNOLOGY

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New design of PIM system applied to different powder feedstocks Researchers at Hitit University, the Materials Research Development Centre (MARGEM) and Karabuk University, all located in Turkey, have developed a newly designed machine (‘newPIM’) to mould metal and ceramic feedstocks. Details of the newPIM system and the powder feedstocks processed have been published in a paper by Bunyamin Cicek, et al., in the Journal of Polymer Engineering, Vol. 41, No. 4, 2021, pp 299-309. The authors of the paper stated that this automated PIM system has been developed to overcome some of the homogeneity distribution problems that can arise using different polymer and powder feedstock structures.

(a)

(b)

(c)

Fig. 1 (a) and (b) sketch and design of the newPIM system and (c) image of the actual newPIM equipment. (From paper: ‘Applicability of different powder and polymer recipes in a new design powder injection moulding system’, by B Cicek, et al., in the Journal of Polymer Engineering, Vol. 41, No. 4 2021, pp 299-309)

Simplifying the complex

Solving the impossible PolyMIM® - Water soluble binder system PolyPOM - Catalytic binder system GranuPrint - 3D-Printing Materials Three systems with excellent characteristics during production.

Global presence and application support.

PolyMIM GmbH Am Gefach 55566 Bad Sobernheim Phone: +49 6751 857 69-0 Fax: +49 6751 85769-5300 Mail: info@polymim.com PolyMIM GmbH a subsidiary of the Polymer-Group www.polymer-gruppe.de

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Feedstock (FS) Binder component

Name 60% Main (filler binder)

35% Secondary (stick binder)

5% Lubricator

Powder

FS binder/powder rate (%)

newPIM-A

PW

EVA

SA

Mg

(35/65 wt) (45/55 vol)

newPIM-B

PW

PP

SA

SiO2

(20/80 wt) (40/60 vol)

newPIM-C

PW

LDPE

SA

SiC

(20/80 wt) (45/55 vol)

newPIM-D

PEG

PMMA

SA

316L

(12/88 wt) (50/50 vol)

Table 1 Feedstock mixture recipes and percentage (wt/vol) powder loading rates. ((From paper: ‘Applicability of different powder and polymer recipes in a new design powder injection moulding system’, by B Cicek, et al., in the Journal of Polymer Engineering, Vol. 41, No. 4 2021, pp 299-309)

The design of the newPIM system is shown in Fig. 1 and the basic elements involve the heating of the feedstock to 180°C to reach a fluid gel consistency, and charging this gel-like feedstock into a heated mould (60-65°C) under argon gas at a pressure of 40 bar through a chamber nozzle having 4 mm diameter. The mould is held closed after injection for 10 sec with a hydraulic bearing system under approx. 7000 N load (also shown in Fig. 1(b) and (c). The heating and temperature of the feedstock prior to moulding is controlled by specially manufactured resistance and thermocouple mechanisms. After the newPIM moulding process, the hydraulic mechanism separates the mould from two sides, allowing the two green PIM samples having Ø35 and 10 mm thickness to be removed. The inner surfaces of the mould were then cleaned with compressed air and alcohol ready for the next injection.

The researchers focused on four feedstock mixtures involving metal and ceramic powders for application in the newPIM system, and these are listed in Table 1 together with the binder compositions. It was established that the best feedstock and resulting green parts were achieved using PEG+PMMA composition with spherical powder having a particle size below 40 µm.

The green parts produced from the feedstocks investigated are shown in Fig. 2 together with the densities and porosities obtained. For

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example, samples made using the newPIM system showed a maximum porosity of 2.2% (newPIM-C) and in the newPIM-D sample involving 316L stainless steel, only 0.63% porosity was detected. No cracks or unfilled areas were observed in the green parts after moulding. The researchers concluded that when the mould

surfaces and broken surfaces were examined in green products moulded in the newPIM system, the most suitable structure was obtained in PEG + PMMA + SA + spherical powder (316L) composition based on porosity calculations.

The authors reported separately that work of the research team on

this subject continues. The sintering process of the moulded samples has been completed and the metallic materials obtained and are being studied. Thus, they stated, the suitability of the new production method for different industries will be proven. https://www.degruyter.com/ journal/key/polyeng/html

Density (g/cm3)

Porosity (%)

Density Porosity Rates

Theoretical

FS

GP

FS

GP

newPIM-A

1.29865

1.25861

1.27852

3.083202

1.550071

newPIM-B

1.75226

1.69902

1.72552

3.038362

1.526029

newPIM-C

2.02998

1.97608

1.98523

2.655199

2.204455

newPIM-D

4.69958

4.64592

4.66985

1.141804

0.63261

Fig. 2 Moulded newPIM parts from the four feedstocks with their density and porosity rate results. (From paper: ‘Applicability of different powder and polymer recipes in a new design powder injection moulding system’, by B Cicek, et al., in the Journal of Polymer Engineering, Vol. 41, No. 4 2021, pp 299-309)

From the archive The PIM International archive gives free access to all our back issues, offering the most comprehensive insight into the world of MIM, CIM and sinter-based AM. Our June 2020 issue includes the following articles and technical reviews: • Element 22: A leader in titanium MIM leverages its expertise to advance sinterbased Ti Additive Manufacturing

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June 2020 • Digitising part production: A new approach to creating unique part IDs for MIM components • Making the business case: How sinter-based Additive Manufacturing can compete with PIM • Reducing MIM part costs with more expensive materials? The re-evaluation of a major 3C application • The production and evaluation of alumina sinter supports for MIM by ceramic AM

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Promoting grain growth to improve creep properties in MIM Ni-base superalloy IN713 Inconel 713 (IN713) is a typical γ’-phase precipitation-strengthened nickel-base superalloy applied widely in components used at high temperatures in aero engines and gas turbines used for power generation. Examples of IN713 parts include turbine nozzles and turbine blades, which have traditionally been produced by precision casting. Some of these parts, however, have small, complex shapes with thin walls and fine structures which makes them difficult to manufacture by casting, and Metal Injection Moulding has recently been attracting attention as an alternative and more economic

fabrication process. Only a limited amount of research data is currently available on the properties of MIM IN713 superalloy parts, and this data has shown that some properties particularly high temperature tensile strength and creep strength are significantly lower than those obtained in castings.

Researchers at the Technical Institute, Corporate Technology Division, Kawasaki Heavy Industries Ltd, in Akashi, Japan, have undertaken work to clarify the causes for low creep strength in MIM IN713 by conducting detailed analyses of microstructure, high-temperature mechanical proper-

Carbon content (mass%) Powder

Sintered

Increase

Powder C

0.10

0.12

0.02

Powder ULC

0.01

0.05

0.04

Horke et al.

0.03-0.07

0.12

0.05-0.09

Table 1 Comparison of carbon contents in starting powders and sintered IN713 materials; included is data from paper by K Horke [1] as referenced.

(From paper: ‘Development of Grain Growth Promotion Technique of Ni-Based Superalloy IN713 Fabricated by Metal Injection Molding’, by Shinya Hibino, et al., Materials Transactions Vol. 62, No. 3 , 2021, pp 436-441)

1400

25 20

1000

Elongation (%)

Strength, σ/MPa

1200 800 600 400 200 0

0

200

400 600 800 Temperature, T/Υ

1000

15 10 5 0

0 200 400 600 8001000 Temperature, T/Υ

Powder C-SHA materials : 0.2% Yield Strength㻌 㻌 Ultimate Tensile Strength 㻌㻌 Elongation 0.2% Yield Strength㻌 㻌 㻌 Ultimate Tensile Strength㻌 㻌 㻌 Elongation Castings8) :

Fig. 1 Tensile test results of ‘Powder C’ materials compared with castings (From paper: ‘Development of Grain Growth Promotion Technique of Ni-Based Superalloy IN713 Fabricated by Metal Injection Molding’, by Shinya Hibino, et al., Materials Transactions Vol. 62, No. 3 , 2021, pp 436-441)

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ties, creep deformation mechanism, and carbide precipitation of MIM IN713 materials. The results of their work have been published in a paper: ‘Development of Grain Growth Promotion Technique of Ni-Based Superalloy IN713 Fabricated by Metal Injection Molding’,

by Shinya Hibino, et al., Materials Transactions Vol. 62, No. 3, 2021, 436-441.

The authors investigated the two known types of IN713: IN713C (carbon content: 0.08%-0.20%) and IN713LC (carbon content: 0.03%0.07%), both of which have excellent high-temperature tensile strength, creep strength, and oxidation resistance when produced as castings.

For their research into the MIM of these superalloys, the authors used gas atomized IN713C powder which was designated as ‘Powder C’ (0.10 mass%), and a powder which contained lower carbon (0.01 mass% ) than the composition equivalent to IN713C, designated as ‘Powder ULC’ (Ultra Low Carbon).

Conventional mixing, injection moulding, debinding, and sintering was applied to both Powder C and Powder ULC. Powder C was injection moulded to a round bar shape with a length of 100 mm and a diameter of 10 mm, whilst Powder ULC was moulded to a thin plate shape with a length of 80 mm, a width of 30 mm, and a thickness of 3 mm in order to improve debinding.

The temperature and the holding time during vacuum sintering were set at 1280°C for 3 h for Powder C, and at 1300°C for 3 h for Powder ULC. Hot Isostatic Pressing (HIP) was applied to remove any residual porosity after sintering. The temperature, holding time, and the pressure of the HIP step were fixed at 1204°C for 4 h at 104 MPa respectively in an Ar gas. In some samples, additional heat treatments were also attempted to promote grain growth either after the sintering or after HIP. The samples used in creep tests were subjected to solution treatment and ageing (STA). Table 1 shows that the carbon content after sintering increases

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1000 Applied Stress, σ/MPa

by 0.02% to 0.12% compared with that of the starting Powder C, but the authors stated that this is still within the composition range of IN713C. Tensile properties were evaluated at room temperature (23°C) and high temperatures of 650°C, 775°C, and 900°C, and creep rupture was done at 927°C in accordance with ASTM E112. Fig. 1 shows the tensile properties of the HIPed and heat treated Powder C. Above 700°C both tensile strength and elongation can be seen to be decreasing, and, at 900°C, the 0.2% yield strength, tensile strength and elongation all fell below the properties of castings. Creep strength at 927°C was more than 10 times shorter than that of castings based on logarithm of rupture time (Fig. 2).

The authors reported that the main cause of the low creep strength of the IN713C-MIM materials can be attributed to the grain refinement, that the grain boundary area existing on the stress-loaded surface is extremely large, and that the progress of grain boundary diffusion creep deformation is much faster.

This suggests that it is necessary to lower the creep strain rate by means of reducing the number of grain boundaries through grain growth in order to improve the creep strength in the IN713C-MIM materials. To achieve this, they subjected HIPed and heat treated the IN713-MIM to an additional heat treatment at 1280°C for 12 hr.

To the best of their knowledge, the authors stated that this is first time that promotion of grain growth in IN713C-MIM materials has been successfully demonstrated by an additional heat treatment step.

100 㻌 Powder C-SHA materials 㻌 Horke et al.7) 㻌 Castings8) 10

18

20 22 24 26 28 Larson-Miller Parameter (/1000)

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Fig. 2 Creep test results of ‘Powder C’ HIPed and subjected to STA; included is data from paper by K Horke, reference [1] (From paper: ‘Development of Grain Growth Promotion Technique of Ni-Based Superalloy IN713 Fabricated by Metal Injection Molding’, by Shinya Hibino, et al., Materials Transactions Vol. 62, No. 3, 2021, pp 436-441)

This is said to weaken the pinning effect on grain boundary migration by decreasing the amount of the MC carbides which are stable at high temperature. Using this approach experiments were also conducted on Powder ULC, aimed at the reduction of the grain boundary carbides that exhibit the pinning effect on the grain growth, and it was found that the carbon content of the sintered Powder ULC materials could be suppressed to 0.05%.

The authors are confident that this new approach could lead to the expansion of the application of the MIM process for IN713 superalloys. It also possibly leads to the solution of the high-temperature strength issues in MIM materials not only for IN713, but also other γ’-phase precipitation strengthened Ni-based superalloys.

The authors also consider that

the developed technology could be applied to the metal Additive Manufacturing (AM) process using Binder Jetting (BJT) methods.

Further detailed research is planned to evaluate the strength properties of MIM IN713C and IN713LC superalloys, and to optimise the heat treatment conditions to promote grain growth in order to optimise grain size. In particular, since it is expected that both the positive effects of the grain growth and the negative effects of the partial loss of the grain boundary strengthening by carbides are included, it will be necessary to determine the optimal conditions by balancing these two factors.

[1] K Horke, et al.: Published in Proceedings PM2016 World Congress, (2016) 3296472 https://www.jim.or.jp/journal/e/

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Headmade Materials

Headmade Materials and Cold Metal Fusion: An innovative approach to sinter-based Additive Manufacturing In recent years there has been a surge in interest in sinter-based metal Additive Manufacturing, with many of these technologies adapting the materials used in Metal Injection Moulding. Whilst Binder Jetting (BJT) and Material Extrusion (MEX) processes lead the field in terms of market penetration, sometimes something radically different comes along. This is certainly the case with Germany's Headmade Materials, whose Cold Metal Fusion (CMF) AM process takes a completely new approach. Dr Georg Schlieper visited the company and reports for PIM International on the company and its technology.

Headmade Materials GmbH is a start-up based in northern Bavaria, Germany. Founded at the beginning of 2019 by Christian Staudigel and Christian Fischer, the inventors of the unique Cold Metal Fusion process, the company is backed with VC-funding from btov’s Industrial Technologies fund, and currently employs thirteen. In 2020, it moved into its current premises in Unterpleichfeld, a small town near Würzburg.

The Cold Metal Fusion (CMF) process is, in part, a radical departure from other sinter-based AM processes, although the metal powders and debinding and sinter processes that are used will be familiar. The process uses a feedstock made of a thermoplastic binder filled with metal powder, developed

by Staudigel and Fischer, that is processed on commercially available Laser Beam Powder Bed Fusion (PBF-LB) AM machines for polymers to create green parts.

The seed for the invention was planted when the pair became friends while studying mechanical

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engineering, with a focus on polymer engineering, at the University of Applied Sciences in Stuttgart. After completing their master’s degrees, they went on to study at the SKZ Kunststoffzentrum research institute in Würzburg. One research topic the pair studied at SKZ was the processing of highly

filled polymers using Additive Manufacturing. In order to produce flame-resistant or electrically conductive plastics, the materials are filled with certain substances.

The higher the degree of filling, the stronger the effect of the filler material on the material’s properties.

Fig. 1 Headmade Materials’ premises in Unterpleichfeld, near Würzburg

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Fig. 2 View of a build underway using the Cold Metal Fusion process

During this work, Staudigel and Fischer came up with the idea of creating green AM parts with metal powder-filled polymers before sintering them into finished components, as in the Metal Injection Moulding process.

Initially, they used filaments filled with metal powder using Fused Filament Fabrication (FFF), a Material Extrusion (MEX) process.

Based on their experience with FFF, the pair learned more about metal powders and the requirements for the binder. Finally, they developed a micro-granulate that could be processed on polymer PBF-LB machines.

The Cold Metal Fusion process As with many sinter-based Additive Manufacturing process, Cold Metal Fusion uses the same metal powders as MIM. Headmade Materials’s proprietary binder system is used to produce a microgranulate that behaves like a highly filled polymer and, as such, can be processed like a plastic feedstock in the polymer PBF-LB process, with the difference being that the manufacturing temperature and energy is much lower than for plastics such as polyamide.

At the beginning of a build, a layer of the ‘powdered’ polymer-metal feedstock is first spread over the base plate in the build chamber of the polymer PBF-LB machine. The green parts are not built directly onto the build plate, as in metal PBF-LB, but onto this initial powder layer.

A laser beam selectively melts the polymer element of the feedstock with the effect that the feedstock granules bond. Once the first layer is created, the base plate is lowered by a layer thickness and the next layer of powder applied with a blade or roller. The next layer is then selectively melted with the laser beam (see Figs. 2 and 3). In this way, the

Fig. 3 A schematic representation of Cold Metal Fusion

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green parts are built up layer by layer. The temperatures in the build space do not exceed 80°C. The usual layer thickness for additively manufacturing with CMF feedstock is 0.1 mm, significantly larger than with other AM processes. This leads to a comparatively higher build speed while still allowing parts to be additively manufactured at a suitably high resolution for many technical applications.

In contrast to metal PBF-LB, the green parts produced by Cold Metal Fusion do not require support structures during the PBF-LB process itself; support is provided by the surrounding powder. This means that the green parts do not have to be laboriously separated from support structures and the build plate during post-processing.

This also means that the entire volume of the build chamber can be used for parts, as no space is taken up by supports (Fig. 4). Up to several hundred green parts can be manufactured in a single build job, depending on the component size and the size of the build chamber.

Thanks to these advantages, Staudigel stated that production volumes of up to 100,000 parts per year can be possible and economically viable with CMF. In this way, it is believed that this technology can close the gap between those Additive Manufacturing processes that are attractive for single parts and low build quantities, such as in common in metal PBF-LB, and the MIM process, which is primarily used for large-to-very large production volumes.

Regardless of the process used, Additive Manufacturing offers unprecedented design freedom that is far superior to the MIM process.

In principle, the size of CMF green parts is limited only by the size of the build space of the AM machine, but, in most cases, it is the sintering step that is the limiting process.

Even with this in mind, the CMF process still allows the production of much larger components than the MIM process.

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Fig. 4 CMF green parts manufactured without supports

Fig. 5 CMF green parts after depowdering, prior to sintering (Courtesy Titanium GmbH)

The advantages of high green strength A crucial feature is the high strength of green parts produced by CMF (Fig. 5). This strength makes it possible to depowder a build with water and thereby facilitates automatic depowdering (Fig. 6).

Unmelted feedstock can be recycled and reused for the next build. It is

even possible to perform machining operations on the green parts and to significantly improve the surface quality via common postprocessing steps such as vibratory grinding and blasting. There is also an option to assemble two or more green CMF parts via sinter joining – a proven technique from the MIM industry.

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Fig. 6 Depowdering of a CMF green part with water

Debinding and sintering The internal structure of the green CMF parts is very similar to that of green parts produced by MIM and, as with MIM parts, they are further processed by initial debinding in a solvent and then second stage thermal debinding and sintering. The binder content of the CMF feedstock is, however, slightly lower than that of typical MIM feedstocks, thus shrinkage during sintering is also slightly lower than with MIM parts. The shrinkage in the X, Y and Z directions is much the same, which is not the case with all sinter-based Additive Manufacturing processes; this enables a high dimensional accuracy. In the sintered state, the density, microstructure and material properties are identical to those of MIM components (Fig. 7).

Fig. 7 Microstructure of 316L stainless steel made by CMF

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Metal powder specifications and material availability Metal powders with particle sizes from 5–25 μm are best suited for the CMF process, but coarser

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Fig. 8 Working with CMF feedstock requires respiratory protection, but, thanks to the metal powders being agglomerated in the feedstock, it is comparatively much safer to use than with pure metal powders

and finer powders have also been successfully processed. The flowability of the metal powder itself is not of high importance, as integrating the powder into the CMF feedstock adds a certain level of flowability. Both pure and pre-alloyed metal powders, as well as metal powder blends, can be used as the raw material. Since the metal powder is agglomerated in the CMF feedstock, there are fewer safety issues in a CMF manufacturing facility than with other AM processes that work with exposed powder; when processed into CMF feedstock, the powder particles are fully enclosed by the binder and are, therefore, far less sensitive to oxidation and moisture, which is particularly advantageous for such oxygen-affine materials as titanium. Nevertheless, respiratory protection is required when working with CMF feedstock (Fig. 8).

As with MIM, the potential range of materials that can be processed

by CMF is considerably greater than with the conventional metal PBF-LB process, although only a select range of alloys have been qualified to date.

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In principle, all materials that can be processed via MIM can also be processed via CMF. So far, in addition to 316L stainless steel and Ti6Al4V, Headmade Materials offers a cobaltchromium alloy, pure titanium grade 1, and a tungsten alloy. 17-4PH stainless steel will be released at the end of 2021, and tool steels, copper alloy, aluminium and a superalloy are also under development.

Headmade has yet to attempt the processing of ceramic materials using CMF. "We are focusing on metals for the time being, because we see a larger market there in the near term," explained Staudigel.

"Ceramic powders are considerably finer than metal powders. As this requires additional development work, this is a lower priority for the time being."

“As with MIM, the potential range of materials that can be processed by CMF is considerably greater than with the conventional metal PBF-LB process, although only a select range of alloys have been qualified to date. In principle, all materials that can be processed via MIM can also be processed via CMF.”

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Comparisons with metal PBF-LB Staudigel admits that metal PBF-LB has its strengths in comparison to sinter-based processes, particularly when it comes to the production of parts in small quantities. He also stated that metal PBF-LB is significantly more advanced than sinter-based AM processes in terms of process simulation, and in the ability to manufacture very fine cooling channels and remove the powder from them; sinter-based processes are at a disadvantage here.

The issue of density was also raised, particularly in relation to tool inserts with internal cooling channels.

The surface of these tools has to be absolutely pore-free, because even the smallest pores become visible on a polished surface and lead to the rejection of a component. “It is very difficult to produce tool steels to an entirely pore-free structure using sinter-based processes. For highquality components, therefore, an additional Hot Isostatic Press (HIP) operation is usually necessary after sintering,” stated Staudigel.

Application development

Fig. 9 Component for a noise-reducing water fitting designed for use in a hotel, made from 316L and partly machine finished (Courtesy Hansgrohe SE)

“An example of the type of part Hansgrohe is investigating for CMF, a component for a water fitting designed for use in hotels, is shown in Fig. 9. Here, the channels are designed in such a way that flowing water produces as little noise as possible.”

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Application development can either be carried out in-house, in close cooperation with the customer, or at a customer’s own facility. So far, the focus has been on components made of 316L, tungsten heavy metal and Ti6Al4V. Bathroom components One customer is Hansgrohe SE, a specialist in high-quality bathroom fittings, which is showing great interest in CMF technology because the process enables the production of complex components with integrated water channels. An example of the type of part Hansgrohe is investigating for CMF, a component for a water fitting designed for use in hotels, is shown in Fig. 9. Here, the channels are designed in such a way that flowing water produces as little noise as possible; in this way, hotel guests are shielded against plumbing noises from neighbouring rooms.

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Fig. 10 Pedal crank (top) and various bike parts made of titanium Ti6Al4V (Courtesy Sturdy Cycles)

The bicycle industry In order to apply its CMF technology to titanium and titanium alloys, Headmade has entered into a close cooperation with Element22 GmbH, a leading manufacturer of titanium MIM products based in Kiel, Germany. The first applications being prepared for market are components for the bicycle industry.

This industry is showing great

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interest in the potential for complex, lightweight titanium components for bicycle frames, pedal cranks and clipless pedals (Fig. 10).

A number of bike frame builders are exploring titanium products made with Cold Metal Fusion technology, thanks to its cost advantages and the better, more uniform surface that can be created. A few thousand bike frame components

are expected to be manufactured with CMF technology in the coming year.

Motorsport The oil separator shown in Fig. 11 is used in the Stallardo ’21 race car, produced for the Formula Student racing team Rennstall Esslingen.

The Ti6Al4V part features a complex inner helix. The connection thread

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Fig. 11 Oil-air separator made of Ti6Al4V, produced for the Stallardo ’21 Formula Student race car (Courtesy Rennstall Esslingen)

Fig. 12 Tungsten heavy alloy part (Courtesy Plansee SE)

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was additively manufactured as a separate part and joined with the oil separator in the sintering process.

Further applications are under development in areas including medical technology.

internal cooling channels (Fig. 12).

The part measures about 50 x 50 x 50 mm and weighs 1.2 kg.

Heavy metal components In cooperation with Plansee SE in Reutte, Austria, Headmade has also developed a component made of a heavy metal alloy that contains

Although Additive Manufacturing offers an unprecedented freedom of design, CMF technology, like all industrial manufacturing processes, requires process-oriented product

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design. For this purpose, Headmade Materials has created a guide with instructions for the design of CMF parts, incorporating experiences from both polymer PBF-LB and MIM technologies into the guidelines.

The limiting factor for CMF technology is less the build process for green parts – which can additively manufacture almost every structure possible in a polymer PBF-LB machine – but the required debinding and sintering steps that follow, and which impose strong limits on possible part designs.

It should always be borne in mind that these parts go through a relatively unstable state in the sintering phase, where gravity can have an unwelcome influence. This critical stage is the main limiting factor. Headmade is, together with partners, working on simulations to make trial-and-error iterations more predictable.

Dimensional tolerances are generally given as +/-0.3 mm for larger and heavier parts. Depending on the part geometry, dimensional tolerances of up to +/-0.1 mm are also possible.

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Flat surfaces and part positioning The first fundamental principle for the design of CMF parts is that they should have a flat surface on which they rest during sintering.

Otherwise, there is a risk that the part will be deformed on the sinter plate and warping will occur due to a part’s own weight. If a flat surface is not possible, distortion can possibly be counteracted by a sinter support adapted to the geometry of the part – however such solutions add cost.

In addition, parts should be positioned during sintering in such a way that the largest masses rest on the sinter plate. Overhanging parts are particularly susceptible to distortion and may need to be supported during sintering.

Wall thickness Wall thicknesses should be between 1 and 10 mm; with wall thicknesses above 10 mm, it is difficult and time consuming to completely debind the green parts. On the other hand, it is not necessary to design a uniform wall thickness, as is recommended with MIM. Free-standing walls that are connected to the base body on one side only should be at least 2 mm thick and no longer than 20 mm tall, otherwise the risk of distortion increases.

Through holes and threads Through holes should have a diameter of between 1 and 20 mm.

Larger diameters are possible, but require additional measures – for example, a larger wall thickness in order to improve the stability, or less weight above the bore. Because of the layer-by-layer process, with manufacturing steps of 0.1 mm, circular holes should preferably be aligned vertically. Horizontal holes usually have to be reworked.

Through holes are easier to depowder than blind holes.

Threads can be additively manufactured up to a minimum size of M4. When manufacturing, the thread should be oriented in the Z direction. Finer threads should be recut to ensure a good fit.

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Fig. 13 An EOS Formiga P110 Laser Beam Powder Bed Fusion machine used for additively manufacturing green parts from CMF feedstock

Headmade’s business strategy "The focus of our business activities lies on the production and marketing of the feedstock for Cold Metal Fusion," explained Staudigel. "We are not a manufacturer of production equipment, but provide our customers with the material and know-how for processing the feedstock into high-quality components."

To demonstrate the capabilities of the process and to get new customers to a point from which they can manufacture their applications themselves, Headmade Materials has an in-house application centre with all the necessary equipment for part design and optimisation, building, debinding and

sintering. Fig. 13 shows a commercial polymer PBF-LB machine which is used at Headmade Materials.

For understandable reasons, the equipment and technology used to produce the feedstock is not shown to the public. There are three polymer PBF-LB machines for production of parts. Solvent debinding takes place in a commercially available system and a vacuum furnace is available for sintering. In case of larger quantities, external partners with higher sintering capacities are involved in the production process (Fig. 14).

One of the first manufacturers of MIM parts to have implemented Cold Metal Fusion in its production was MIMplus Technologies, Ispringen, Germany. For MIMplus' decision in favour of CMF technology, the high

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Fig. 14 First stage debound, or 'brown', CMF parts being transferred to vacuum sintering

component quality, cost effectiveness and easy integration into the company's production were of particular importance.

Christian Staudigel believes that Powder Metallurgy and MIM companies considering the implementation of AM in-house usually need to change their business model, because most of them are set up for mass production. AM, on the other hand, is not particularly economical for mass production, but for smaller quantities.

Fortunately, however, the trend today is towards smaller quantities and a greater diversity of variants of industrial products.

Marius Geldner, CFO of Headmade Materials, stated, "A lot of work is still needed to bring the benefits of our process closer to customers. Often, a design change is necessary to take full advantage of Additive Manufacturing."

"For customers who have no experience of sintering, it is not easy to select the appropriate systems from the wide range of sintering furnaces that are available, as they do not know exactly what requirements they have to meet," explained Staudigel. "We at Headmade

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Materials help them overcome this hurdle."

The company is striving to make its process known to experts through presentations at symposia and through participation in technical exhibitions such as those at Fraunhofer IFAM, the Hagen Symposium and Formnext. In addition, the company cooperates closely with the leading manufacturers of polymer PBF-LB machines. These company’s customers are often interested in setting up a production line for metal AM parts in addition to plastic ones. Furthermore, cooperation is being developed with the manufacturers of MIM sintering furnaces so that they can develop tailor-made solutions for CMF.

Outlook In the coming years, Staudigel believes that the most important task for his company is the expansion of feedstock production capabilities and the diversification of the material portfolio in close cooperation with customers and their needs.

As the investment in a polymer PBF-LB machine for use with the

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CMF process is comparatively low, and the manufacturing speed is higher than is possible with many other metal AM processes, the costeffectiveness of this step is attractive.

Staudigel, therefore, expects that the CMF process will soon penetrate new markets that are currently still closed to Additive Manufacturing for cost reasons. The first steps have been taken in the bicycle applications sector, and more will follow.

Author Georg Schlieper Harscheidweg 89 D-45149 Essen Germany info@gammatec.com

Contact Christian Staudigel Headmade Materials GmbH Langhausstrasse 9 D-97294 Unterpleichfeld Germany c.staudigel@headmade-materials.de www.headmade-materials.de

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THE EVOLVING STORY OF METAL BINDER JETTING: THE PAIN AND THE PROMISE Binder Jetting – at once the new kid on the block yet one of the industry’s earliest processes – holds the promise of taking metal Additive Manufacturing into the territory of true highvolume production. Yet progress towards this goal appears to be struggling, with machine sales lower than many hoped and two new ‘big players’ appearing to be holding back on full commercialisation.

In this report, Joseph Kowen considers the development of this industry to date, the obstacles facing its growth, and, of course, the recent announcement of two of Binder Jetting’s biggest rivals coming together in the most unexpected acquisition.

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Expanding horizons at SSI

SSI Sintered Specialties: Expanding horizons through ‘next-generation’ MIM materials and Binder Jetting SSI Sintered Specialties, LLC can trace its roots back to the earliest days of Powder Metallurgy in the US. True to its name, that company has over the decades found success through specialisation, in particular stainless steel PM products. This is a theme that continues today, with the company now expanding its horizons through the development of large MIM parts using innovative feedstock technology, and the adoption of metal Binder Jetting.

Bernard North visited the company on behalf of PIM International and reports on its plans to remain at the forefront of metal powder based parts production.

Janesville, in the Midwest of the USA, lies ninety-five miles from Chicago’s O’Hare Airport along Interstate 90.

This modestly sized Wisconsin city, with a population of around 65,000, is home to SSI Sintered Specialties, LLC, a major player in the Powder Metallurgy parts business, and one with a long and distinguished history.

In October, I visited the company on behalf of PIM International magazine and met with three members of SSI’s team: Paul Hauck, Chief Operating Officer, Joe Lange, Vice President, Manufacturing, and Kayla Varicalli, Marketing Manager, to discuss some major developments at the company, including an expansion of its Metal Injection Moulding capabilities and a move into sinter-based metal Additive Manufacturing.

Pen Company opened its Panoramic sintering division for porous Powder Metallurgy components for pens.

During the following decade the product line diversified into initial automotive applications, and in the 1970s sintered stainless steel parts for mounting rear-view

mirrors were developed and introduced. In 1982, Parker Pen sold the operation to a group of six private investors, who named the company SSI Technologies, Inc. In 1987, one of those investors became the sole owner and remains as such to this day.

Innovation past and present: the story of SSI The history of SSI can be traced back to the earliest days of PM component production in North America. In the 1950s, the Parker

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Fig. 1 A continuous sintering furnace in operation at SSI (Courtesy SSI Sintered Specialties)

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Fig. 2 A Dorst hydraulic CNC multi-platen powder compaction press at SSI, used for the production of large PM components for the automotive industry (Courtesy SSI Sintered Specialties)

“A very high proportion - around 85% - of the company’s PM output is for stainless steel product, with many applications being large components.

As a result, SSI is one of the world’s largest consumers of stainless steel powders.”

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Over the next four decades the company grew by expanding its product range in terms of materials, markets, and product complexity, enabled by successive (and contiguous) increases in manufacturing space up to the present 23,000 m2 (250,000 ft2). During this time, major upgrades were implemented in manufacturing equipment and processes, workflow efficiency, forward integration into machining and other finishing processes, and quality systems. The workforce level currently sits at approximately 400 employees.

In relation to press and sinter PM production, the company’s rather unique expertise lies in the production of stainless steel components. A very high proportion - around 85% - of the company’s PM output is for stainless steel product, with many applications being large components. As a result, SSI is one of the world’s largest consumers of stainless steel powders.

With an eye to efficient and sustainable manufacturing, there is an emphasis on net or near-net shaping, with extensive use of multi-level press tooling. Thus, around 40% of SSI’s PM production volume does not require finishing processes. There is a high level of forward integration – of the 60% of SSI’s production that requires finishing operations, more than 95% of those operations (machining, grinding, coining, infiltration, heat treatment, brushing, burnishing, and assembly) are done in-house.

This increases control over costs, lead times, delivery performance, and quality, and puts SSI closer to the final customer. Total production volume varies by market conditions, but it is typically about 100 million parts annually.

MIM and AM: driving diversification In 2019, the associated automotive and industrial sensor and systems business, SSI Controls Technologies, was sold to Amphenol

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Corporation, and SSI Sintered Specialties became its own standalone business, with a focus on sustainable solutions using Powder Metallurgy.

This presented an opportunity to reposition the company to compete in a rapidly evolving global market and to leverage its expertise in sintering – particularly high-temperature sintering. As a result, 2021 has become a year of transformation for the company, resulting in a major expansion of production capabilities as well as a new sales and engineering office in Novi, Michigan.

Whilst innovation in press and sinter PM parts production remains a focus at SSI, the company is also diversifying its product portfolio – and market reach - through two forming technologies that are closely related to each other: Metal Injection Moulding and metal Binder Jetting (BJT).

MIM has been offered in-house at SSI since the 1980s; however, strategic technology upgrades will offer access to a broader range of customers who are looking for the ability to produce higher performance, larger and more complex geometries in volume production.

SSI’s non-automotive target markets for these newly introduced technologies include aerospace, defence, electronics, medical, industrial, and sports equipment.

At the heart of SSI’s MIM technology upgrades is a partnership with Tundra Innovations, a material additives company based in White Bear Lake, Minnesota, USA, to explore the high-volume production of large, complex components

by MIM. SSI will operate as the preferred production partner of parts made with Tundra’s Dynamik® materials platform. The intention is that, by leveraging SSI's metallurgical production expertise and Tundra’s expertise in specialist binder systems, larger and more complex parts can be produced that were previously considered economically or technically unviable for MIM. Hauck explained that, with traditional MIM materials, the uncertainty

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Expanding horizons at SSI

Fig. 3 SSI is using feedstock from Tundra Innovations to produce large, complex parts previously not considered economically or technically feasible with MIM (Courtesy Tundra Innovations)

of non-isotropic shrinkage significantly increases with larger parts, often resulting in high part variability, low dimensional stability and expensive material processing.

These obstacles have kept most MIM components around 25 g or less.

Tundra’s binder technology offers the ability to produce parts with an average isotropic shrinkage of 10-12%, compared to conventional shrinkage of 16-20%. This improves dimensional stability for the production of parts with near-wrought properties. The feedstock can be processed using conventional

MIM equipment and enables large, complex part production – including parts that are 100 g or larger.

“It takes a strong partnership between dedicated materials and engineering experts to solve the challenging obstacles that are present in the Metal Injection Moulding space today,” Hauck stated at the time of the partnership announcement.

“Partnering with Tundra, a company with a background in leveraging advanced technical insights to reinvent what’s possible, advances our strategy to design and produce MIM components with properties and possibilities that the market has

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never seen before. MIM has had a successful history in delivering very complex metal parts for demanding applications, but its scope has been limited to small parts. Our partnership with Tundra enables us to address a broader range of applications that were not economically possible with traditional MIM operations, expanding how our customers can leverage the technology for their applications.”

The partnership with Tundra coincides with other MIM-related technology investment announcements that include the addition of a high-temperature refractory metal lined vacuum furnace from Elnik Systems, Cedar Grove, New Jersey, and a new automated injection moulding cell from Arburg GmbH & Co KG, Lossburg, Germany, offering customers the capabilities needed to lead the development of what are described as ‘non-traditional’ MIM applications.

Embracing metal Binder Jetting In September, SSI announced its purchase of the X1 160Pro and InnoventPro 3L metal Binder Jetting (BJT) machines from The ExOne Company, North Huntingdon, Pennsylvania, USA. Delivery of the two machines is expected in the first half of 2022.

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The addition of metal Binder Jetting to SSI’s technology portfolio is regarded as a natural next step in providing customers with the most advanced technology on the market to produce complex geometries in volume production. “Our expertise and lengthy heritage in hightemperature metallurgy processing is a perfect fit for Binder Jetting technology, and we are thrilled to be working with ExOne to offer our customers the future of metal 3D printing,” Hauck stated.

With Binder Jetting, SSI intends to offer components with increased complexity and size for volume production in a variety of metals, without the need for tooling. The investment in this technology is, states Hauck, just one of the steps in SSI’s business strategy to embrace AM and bring new manufacturing solutions for volume production.

SSI and ExOne will collaborate on BJT material, automation, and process development, with the InnoventPro being used for material and application development, and the 160Pro dedicated to volume production through a fully automated cell with continuous sintering equipment.

Hauck stated that the main reasons for the selection of metal Binder Jetting as the ‘AM process of choice’ at SSI are lower capital cost and higher build rates of the

“SSI and ExOne will collaborate on BJT material, automation, and process development, with the InnoventPro being used for material and application development, and the 160Pro dedicated to volume production through a fully automated cell with continuous sintering equipment.”

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machines compared to Laser Beam Powder Bed Fusion (PBF-LB) and Electron Beam Powder Bed Fusion (PBF-EB). In addition, the sintering processes for MIM and binder jet AM parts are very close, and offer invaluable synergies.

Hauck stated that, of the small number of companies currently offering BJT machines, ExOne was selected for a number of reasons.

“Their long history with sand machines for the foundry industry has given them a firm market base, as well as great experience in operating in demanding industrial environments. They have developed a lot of experience with different metals and user industries.” Hauck also commented that ExOne’s Triple Advanced Compaction Technology (ACT) gives higher and more uniform green densities, and hence lower and more uniform shrinkage during sintering. “Transitioning between the smaller and larger units should be straightforward as the units have the same print jet configurations.”

Pros and cons of MIM and AM: part complexity, dimensional control, and production volume The adoption of metal Binder Jetting to date, although modest, has been driven in large part by the MIM industry – suggesting that the technology is primarily seen as an opportunity rather than a threat by the MIM industry. Hauck believes that component design will be a big factor in determining what process is the best fit for the application.

“While many people view AM as suitable for low volume work because it obviates the need for tooling, our focus at SSI with both MIM and AM will be on volume production.

We are already in discussion with several potential customers on some very exciting possibilities,” stated Hauck.

Just as the activity of MIM firms around the world is starting to create a rather fluid ‘border’ between MIM and the sinter-based

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Expanding horizons at SSI

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AM industry, experienced MIM professionals are also moving freely between the industries, taking with them the necessary expertise in debinding and sintering.

Hauck himself made the switch to working on sinter-based Additive Manufacturing technologies in 2018, joining HP’s metal Binder Jetting program as product manager of the company’s Metal Jet hardware division. In 2020, Hauck took on his current position as Chief Operating Officer back at his former employer, SSI. He is therefore able to promote both MIM and BJT technologies with the experience of operating in both industries.

When it comes to the size capabilities of the new MIM technology being introduced at SSI, Hauck explained that the maximum practical sintered cross-section thickness is around 12.5 mm, and that whilst the maximum practical weight of MIM parts using this technology appears to be about 500 g, 100 g could be an optimum ‘routine’ weight, far higher than that of typical MIM parts, which rarely exceed 25 g.

“SSI’s partnership with Tundra has enabled the production of physically large, complex components with solid dimensional control at a more efficient cost in MIM. Tundra’s Dynamik® feedstock achieves extremely high powder packing densities - upwards of 80% by volume - through the use of a bimodal coarse/fine particle size distribution and proprietary organic binder technology, greatly reducing both the absolute shrinkage down to a linear 10-12% during sintering to high densities, as well as substantially reducing the degree of shrinkage anisotropy. Modern high temperature sintering technology is also very helpful, which SSI has an abundance of in its facility.”

In terms of the materials available as part of the new process, Hauck explained, “SSI’s focus for MIM will be on components that can best leverage the new technology – like complex design features at nearly any size - for high volume production in both stainless steel and other materials."

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Fig. 4 An Elnik Systems batch vacuum debinding and sintering furnace recently installed at SSI to support its MIM and BJT development program (Courtesy SSI Sintered Specialties)

Fig. 5 In September, SSI announced its purchase of X1 160Pro and InnoventPro 3L metal Binder Jetting machines from ExOne. Delivery of the two machines is expected in the first half of 2022 (Courtesy SSI Sintered Specialties)

Conventional PM manufacturing capabilities enhanced SSI has more than forty presses for press and sinter PM parts production, ranging from 20 to 880 US tons (tonnes) in capacity. The company recently invested in a new SACMI 200

ton fully automatic hydraulic CNC press. Equipped with integrated automation for part removal, the MPH 200 press is scheduled for installation in 2022.

The press, stated SSI, provides process and productivity improvements compared to traditional mechanical press technologies and will enable the company to produce

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Fig. 6 Continuous sintering furnaces for high-volume PM part production at SSI (Courtesy SSI Sintered Specialties)

more PM components without the need for secondary operations.

SSI’s Janesville plant has fortyseven sintering furnaces with operating temperatures between 1150 and 1600°C; thirty-two of these furnaces are capable of sintering above 1300°C, helping to achieve relatively high densities for press and sinter PM parts in

the range 88-94% theoretical, compared to standard PM parts which are commonly in the 82-88% range. As previously mentioned, SSI does most of its post-processing in-house, and the plant has forty-six CNC machine tools of various kinds, again with a high level of materials handling automation.

“SSI’s Janesville plant has forty-seven sintering furnaces with operating temperatures between 1150°C and 1600°C; thirty-two of these furnaces are capable of sintering above 1300°C, helping to achieve relatively high densities for press and sinter PM parts in the range 88-94% theoretical...”

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Powder management, quality and environmental SSI does not manufacture powder, and processing of powders prior to part production is limited to V-blending to adjust certain compositions. Major grades are dual-sourced, with pre-qualified primary and secondary suppliers, and are delivered in super-sacks or appropriate sealed containers and inventoried thus.

Qualified powder suppliers provide data directly into SSI’s quality management system, thus avoiding needless duplication of effort.

However, the plant also has extensive analytical and property measurement capabilities, which are also used by development staff in their process and product improvement work.

Quality system data are integrated with process control and control plans into the company’s ERP (Enterprise Resource Planning) system. Furthermore, SSI’s phase

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Expanding horizons at SSI

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gate system for process and product development is incorporated into the ERP system. SSI was first certified to the international ISO 9001 quality systems standard in 1998, and it is currently certified to ISO 9001:2015 as well as the automotive quality standards ISO/TS 16949:2009 and IATF 16949:2016.

The company was first certified to the environmental standard ISO 14001 in 2011, and it is currently certified to ISO 14001-2015. In addition, the company is compliant with ITAR (International Traffic in Arms Regulations) and US Conflict-Free Minerals policy.

The role of professional bodies Hauck believes that professional bodies such as the Metal Powder Industries Federation (MPIF) and APMI play a critical role, especially in standards development, information exchange, and networking. At the Orlando PowderMet2021 conference he was particularly impressed with the number of doctoral students present and with the resume and job vacancy boards to facilitate placement. From 1999 to 2005, Hauck was President of the MPIF's Metal Injection Molding Association (MIMA).

In 2013, Hauck was recognised by the MPIF with its Distinguished

Service to Powder Metallurgy award – an award in which nominations and selections are made by industry peers on having contributed a minimum of twenty-five years of service to the industry and technology of Powder Metallurgy.

He is also a co-chair of the MPIF PowderMet2022 conference, to be held in Portland, Oregon, and has been encouraging his contacts in the industry to submit presentations for the event.

Outlook SSI Sintered Specialties is without doubt a significant player in the powder metallurgical parts manufacturing space, and one with a blend of technical and industry experts from within the organisation as well as recently drawn from external sources. As with many PM producers around the world, navigating a path through the uncertain waters ahead, in part as a result of vehicle electrification, will require vision and tenacity. It will be fascinating to see how quickly, and in what directions, the company develops new products and business as it integrates its new technologies into its manufacturing and commercial operations.

Hauck agrees with the assessment of Edwin Pope, IHS Markit, in his plenary presentation at

PowderMet2021, that the reality of the EV revolution may in fact be a relatively slow market shift, especially in North America, due to challenges with the overall infrastructure needed for large scale BEV or fuel cell vehicle adoption. That said, SSI is pursuing PM applications for full electric vehicles, as well as continuing to diversify into non-automotive markets.

Author Bernard North North Technical Management, LLC Greater Pittsburgh Area Pennsylvania, USA bnorth524@msn.com

Contact Kayla Varicalli Marketing Manager SSI Sintered Specialties kvaricalli@ssisintered.com www.ssisintered.com

Read all back issues of PIM International for free www.pim-international.com

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Euro PM2021: Advances in MIM feedstocks

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Exploring the subtleties of the formulation and preparation of MIM feedstocks A technical session, comprising three papers, at the Euro PM2021 Virtual Congress, organised by the European Powder Metallurgy Association (EPMA) and held from October 18–22, 2021, assessed various aspects of the formulation and preparation of feedstocks for Metal Injection Moulding. Dr David Whittaker reports on three papers that addressed solvent debinding efficiency, strategies for enhancing the debinding of polyacetal (POM) feedstocks, and, lastly, an analytical method for enhancing the understanding of the homogeneity of MIM feedstocks and green parts.

Effect of backbone selection on the solvent debinding of Metal Injection Moulding feedstocks The first paper featured in this review came from Christian Kukla, Santiago Cano, Stephan Schuschnigg, Clemens Holzer and Joamin Gonzalez-Gutierrez (Montanuniversitaet Leoben, Austria).

It considered the effect of backbone selection in MIM feedstocks on the efficiency of solvent debinding [1].

At least two components are necessary in MIM feedstock binders: the backbone, to provide strength and shape retention during the removal of the other binder components, and the main binder component to provide flowability during the injection moulding process.

Organic solvents or water can be used to remove a portion of the binder, followed by thermal debinding to eliminate the remaining binder components. During solvent debinding, interconnected pore channels are left, allowing the

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decomposition products in thermal debinding to leave the part. If the binder components are not adequately selected, defects – such as cracking, distortions or slumping – can be encountered during solvent debinding. The binder component to be removed in thermal debinding is the backbone. The backbone must be low cost, chemically resistant to solvents used in solvent debinding and easily removable by thermal degradation. These requirements are fulfilled by polyolefins, the most commonly used being high-density polyethylene (HDPE), low-density polyethylene (LDPE), and polypropylene (PP).

For high performance, the binder should show good adhesion to the powder. In many cases, an additive

achieves this. Stearic acid (SA) is commonly used for this purpose in PIM. Another possibility is the use of grafted polyolefins; grafting introduces suitable polar sites onto the chains of the polymers, thus improving the adhesion between polymers and particles with different polarities. The use of grafted polymers as PIM feedstocks has not, to date, been extensively studied.

Therefore, the reported work looked at the behaviour of different backbones and grafted polyolefins, comparing the debinding performance, morphology and thermal degradation of feedstocks with grafted backbones.

The major fraction of the binder in the studied feedstocks was composed of two waxes, added to

Composition (wt.%) Fe

C

Si

Mn

P

S

Cr

Ni

Mo

Cu

Balance

0.017

0.55

1.28

0.019

0.006

16.3

10.2

2.05

0.1

Table 1 Chemical composition of gas atomised 316L powders, as provided by the suppler [1]

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Fig. 1 Particle size distribution of the gas atomised 316L powder [1]

“Feedstocks containing PP reach 100% soluble content removal after 24 h, while materials with HDPE reach only 90%. This mass loss indicates that HDPE hinders the dissolution of the wax mixture and the use of PP could be more beneficial in speeding up the debinding process..." adjust the viscosity of the binder system and as components soluble in n-heptane. The insoluble fraction was the backbone. Feedstocks with maleic anhydride-grafted and non-grafted polypropylene and high-density polyethylene backbones were evaluated.

Stearic acid was added to the nongrafted backbones as a dispersant agent, at a similar weight fraction to that used for grafting.

The powder used was gas atomised 316L stainless steel, with the chemical composition shown in Table 1 and a particle size distribution shown in Fig. 1.

Feedstock materials were prepared in a laboratory-scale kneader with counter-rotating rollers. The set temperature of the kneader was 185°C, the rotational speed of the rollers 60 rpm and

kneading time 30 min. All of the binder components were introduced together to the kneading chamber and, after they were completely melted, the stainless steel powder was added. After compounding, the material was ground using a cutting mill with integral sieve. The feedstock formulations are shown in Table 2.

Cylinders with 8 mm diameter and 5 mm height were compression moulded in a vacuum press. The compression cycle comprised (i) preheating the material for 40 min at 1 bar, at the maximum temperature, (ii) compression at 50 bar for 5 min at the maximum temperature and (iii) cooling to 30°C and compressing at 50 bar for 15 min. The maximum temperature was adjusted for each feedstock on the basis of preliminary trials at temperatures between 150 and 190°C. The selected temperatures were 175°C, 185°C, 160°C and 150°C for the PP+SA, PPgMA, HDPE + SA and HDPEgMA feedstocks, respectively.

With regard to solvent debinding behaviour, Fig. 2 shows the leached soluble binder for the four feedstocks investigated. Feedstocks containing polypropylene lose mass faster than those containing HDPE, regardless of whether grafting or SA was used.

Feedstocks containing PP reach 100% soluble content removal after 24 h, while materials with HDPE reach only 90%. This mass loss indicates that HDPE hinders the dissolution of the wax mixture and the use of PP could be more beneficial in speeding up the debinding process in n-heptane.

In terms of morphology, it appears that all of the green feedstocks showed excellent dispersions of the particles in the matrix, on the basis

316L (vol.%)

Mixture of waxes (vol.%)

PP (vol.%)

HDPE (vol.%)

PPgMA (vol.%)

HDPEgMA (vol.%)

SA (vol.%)

PP+SA

55.00

24.75

20.05

-

-

-

0.20

PPgMA

55.00

24.75

-

-

20.25

-

-

HDPE+SA

55.00

24.75

-

20.05

-

-

0.20

HDPEgMA

55.00

24.75

-

-

-

20.25

-

Short notation

Table 2 Compositions of the evaluated feedstocks [1]

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110

Leached soluble binder (%)

of scanning electron microscopy (SEM) assessments. However, PP forms a network of thicker connections between particles, whereas the connections made by HDPE are much thinner and weaker. The debound specimens of PP + SA show large elongated pores in comparison to debound HDPE + SA specimens.

This morphology can be explained by the better compatibility of the waxes with HDPE than PP, and could be the reason for the differences in the solvent debinding rate (Fig. 2).

The use of grafted backbones has a significant effect on the adhesion to the powder. As observed in previous studies by this group, grafting helps to create a better connection between the polar surface powder and the backbone, especially when comparing the morphology of the MAgHDPE with that of HDPE + SA. Nevertheless, the size and distribution of pores of the solvent debound specimens are not affected by grafting of the backbone.

Thermogravimetric analysis (TGA) shows the recorded mass loss over temperature for the binder components and feedstocks (Fig. 3).

Stearic acid and one of the waxes decompose at low temperatures, whereas the second wax decomposes at higher temperatures.

Due to a similar structure, the PP backbones decompose at similar temperatures to the second wax, but the HDPE-based backbones

100 90 80 70 60 50 40

40 20 0

10

15

20

25

Fig. 2 Leached soluble binder at different immersion times for four feedstocks [1]

decompose at higher temperatures.

These differences in the backbone decomposition affect the decomposition of the feedstocks. All feedstocks show a first decomposition ramp corresponding to the low molecular weight compounds. However, the second ramp of mass loss starts at a lower temperature for the PP + SA and MAgPP feedstocks than for MAgHDPE and HDPE + SA. Based on these results, the nature of the main backbone chain plays a more critical role in the thermal debinding behaviour than the backbone grafting.

The authors concluded that grafting the backbone improves the adhesion to the powder, especially for HDPE. In general, an improved adhesion to the powder could be used to reduce the amount of backbone in the binder and to optimise the debinding rate. These issues are the subject of ongoing research by the group. However, the effects of backbone grafting on the carbon content and composition of the sintered parts must also be investigated in the follow-up projects.

(b) 100 (b) 100

HDPEHDPE MAgHDPE 40 MAgHDPE PP PP MAgPP MAgPP 20 Wax1 Wax1 Wax2 Wax2 SA SA 0 100 100 200 200 300 300 400

99

99

98

98

97

97

96

96

95

95

94

94

Mass loss (Wt.%)

60

5

Mass loss (Wt.%)

60

Mass loss (Wt.%)

Mass loss (Wt.%)

80

0

Time (h)

(a) 100 (a) 100 80

HDPE+SA MAgHDPE PP+SA MAgPP

93 92

400 500

500 600

600

91

Temperature Temperature (°C) (°C)

MAgPP MAgPP 93 HDPE+SA HDPE+SA PP+SA 92 PP+SA MAgHDPE MAgHDPE 91 100 100 200 200 300 300 400

400 500

500 600

600

Temperature Temperature (°C) (°C)

Fig. 3 TGA curves of (a) binder components and (b) feedstocks [1]

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Fig. 4 TGA thermogram (a) and DSC thermogram (b) of oxalic acid 2-hydrate; the insert graph was obtained after a 30 min isotherm performed at 120°C by DSC [2]

Accelerated PIM processing by chemical modifications in the binder during the debinding stage The second paper reviewed was presented by Cristina Berges, Juan Alfonso Naranjo, Macarena Jimenez, Manuel Carmona, Ignacio Garrido and Gemma Herranz (Universidad de Castilla-La Mancha, Spain) and addressed the acceleration of MIM processing by chemical modifications in the binder during the debinding stage [2].

Currently, the most commonly used feedstock in Europe by MIM manufacturers is based on polyacetal (POM) and polyolefin and comprises a catalytic removal of the binder system. The catalytic debinding time is usually in the range 3–10 h, depending on the feedstock material and the component size.

Nevertheless, this methodology is not free from experimental issues in the industrial process, and this debinding time might be insufficient with certain geometries.

From both research and industrial points of view, it has been reported that, in order for MIM technology to continue market growth, there is a need to focus on new powder materials (high-temperature intermetallics, particulate composites or controlled porosity) and processing

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sophistication, so that dimensional control and the process yield can be improved. Also, for environmental reasons, it is highly desirable to develop a faster, cleaner and cheaper debinding process. Efforts to achieve complex shapes at high precision and quality have been focused on optimising sintering time and atmosphere, mould design and feedstock modification for the injection process, moving towards lowering the viscosity and water-soluble binders.

The catalytic debinding process has proven processing and handling advantages, since it allows the manufacture of thicker components than those in thermal debinding. In catalytic debinding, PIM manufacturers typically control the catalyst level within the furnace at up to 4 vol.% of the gas flow, achieving a debinding rate of 1-6 mm/h. Enhancements of this catalytic reaction have been investigated in terms of the optimisation of the experimental set-up conditions. Therefore, by varying the flow rate of the carrier gas, the catalyst and the catalyst level within the furnace debinding zone, the debinding rate can be optimised.

Nevertheless, it is important to note that a high purge gas flow rate is needed to increase the debinding rate. Also, no studies have been found in the literature dealing with binder modification of the catalytic feedstock to speed up the PIM process.

December 2021

In the reported work, chemical additives to the binder have been proposed, with the purpose of reacting with the generated formaldehyde gas and leading to a forced acid-catalysed degradation reaction of the POM component.

The addition of these so-called ‘accelerator’ compounds for formaldehyde capture in the feedstock mixture was expected to mainly cause two effects. On the one hand, favouring the debinding process and increasing the process yield will bring the possibility of manufacturing components with bigger sizes and higher cross-sectional thicknesses or, in the case of thin geometries, becoming a more efficient process reducing the catalyst consumption and energy costs. On the other hand, this process allows the capture of formaldehyde residue, forming a valued product and avoiding its further burning, which is beneficial from an environmental point of view.

Chemicals that can act as the trapping molecules of formaldehyde residue are those with a nucleophilic character, such as N-based molecules (polyamines) forming methylol compounds. These materials strongly participate in further polymerisation reactions by means of polycondensation at high temperature.

The most typical accelerator resins are based on melamine or urea compounds. N-based compounds

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have been selected over O-based compounds, such as phenol, bisphenol A, bisphenol F or derivatives, due to OH functional groups showing less nucleophilic character than nitrogen-based ones. However, it is important to consider the gas atmosphere composition generated after the thermal degradation of the binder, since it can affect the green and sintered components.

In this reported work, initially, with the aim of enhancing the debinding rate, the accelerator concentration and the acid concentration with respect to the POM and inert gas flow, respectively, were to be determined.

Also, the acid type to be employed in this study was to be selected.

Although nitric acid is typically used in industrial catalytic debinding, the acid gas atmosphere for this preliminary study was required to show thermal stability and to allow working in batches. In this context, the most suitable experimental conditions to produce the catalysed POM degradation followed by the polymerisation reaction of Melamine-Formaldehyde (MF) resins were to be investigated.

Once the isolated system was characterised, the process would be applied to the real MIM feedstocks widely used in industry (316L, 17-4PH stainless steels or FeNi alloys) using chemical reactors based on industrial conditions, in a future second phase of the study.

The POM employed in the reported study was a commercial grade powder without any additives, typically used as the polyacetal component of catalytic MIM feedstocks. This was a homopolymer type with a melt flow index of 15 g/10 min. Melamine was selected as the N-based molecule to produce the Melamine-Formaldehyde (MF) resin by a polycondensation reaction. Oxalic acid 2-hydrate was employed to ensure the acidic conditions that catalyse the chemical reactions, involving simultaneous POM degradation and MF resin production.

To establish the experimental conditions at the laboratory scale, oxalic acid 2-hydrate was thermally characterised by TGA and

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Melamine (mol)

Formaldehyde (mol)

Product aspect

Reaction 1

1

50

White cloudy

Reaction 2

1

12

Clear colourless viscous

Reaction 3

1

5

White cloudy

Table 3 Reactions 1-3 performed in DSC with different M/F molar ratios and product aspect [2] DSC analysis, as shown in Fig. 4.

The TGA thermogram, performed under nitrogen atmosphere with a heating ramp at 5°C/min to 700°C and cooling ramp at 25°C/min to room temperature, showed a weight loss up to 100°C, corresponding to water molecule vapourisation, and a second weight loss below 200°C, corresponding to acid vapourisation.

Additionally, the DSC thermogram, performed with a heating ramp at 5°C/min to 250°C, showing several endothermal peaks, which corresponded to water vapourisation at 100°C, acid sublimation below 150°C and a degradation peak in a higher temperature range. Also, the insert graph in Fig. 4b showed the heat flow change during the 30 min isotherm at 120°C (from time = 20 min).

In contrast to industrial catalytic debinding, which uses the catalyst in vapour form, being transported to the sintering furnace by means of an inert carrier gas, the in-situ generation of the catalyst required a temperature that favoured catalyst vapourisation from its solid form. In this case, a vapourisation temperature of 120°C was considered for comparison with that used in the industrial process, where nitric acid is traditionally employed. In a first approach, POM degradation was analysed by considering a closed furnace without carrier gas and no catalyst losses, for favouring the formaldehyde trapping. For this purpose, the vapourisation flux of the oxalic acid occurring at 120°C for 30 min was also calculated by DSC in the range 20-26 min (Fig. 4b, inset), estimating the power required for vapour formation at 120°C and the vapourisation enthalpy. Evidently, by observing the vapourisation of the

oxalic acid, the amount of catalyst evaporated can be increased with increasing temperature, increasing the debinding rate but reducing the economic feasibility of the process.

By this assessment, the optimum temperature can be defined.

The mixtures of POM, melamine and oxalic acid firstly underwent the reactions defined by DSC using hermetic high-volume pans, so that the gas atmosphere (catalyst and released formaldehyde) produced during the reaction time could be maintained and the MF resin formation could take place. The following thermal cycle was employed: ramp at 5°C/min to 120°C (hold 240 min), followed by a cooling ramp at 25°C/ min. The reaction time, established as 240 min, was high enough to ensure the occurrence of the polymerisation reaction. The products obtained from the previous reactions were characterised by TGA analysis under nitrogen atmosphere at the following conditions: heating from 25 to 700°C at a ramp of 5°C/min, followed by a cooling ramp of 25°C/min from 700 to 25°C. The structures of the MF resins vary significantly with the reaction conditions (molar ratios of the reactants, pH, time, catalyst and temperature). Therefore, in this study, different mixtures of POM and melamine were prepared, corresponding to a varied concentration of melamine/formaldehyde (M/F) molar ratios, as indicated in Table 3.

The stoichiometric molar ratio in MF resins is 1:6, so the concentrations employed were selected to study different situations, trying to force the capture of the released formaldehyde: (i) a high excess of formaldehyde (M/ F=1/50) - Reaction

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Fig. 5 TGA thermogram of reference products: POM, POM+oxalic acid; melamine and M/F=1/6 [2]

“The mixture of POM with oxalic acid showed a fast degradation rate below 200°C, compared with the POM degradation, demonstrating that this acid is able to decompose the polymer even at low temperature; the melamine reactant is thermally decomposed at higher temperature (300°C).”

1, (ii) a moderate excess of formaldehyde (M/F=1/12) - Reaction 2 and (iii) a moderate excess of melamine (M/ F=1/5) Reaction 3 in Table 3.

Regarding the in-situ generation of the catalyst using oxalic acid in the reactions, the vapourisation flux of the acid at 120°C was used to determine that only 7.58% of the oxalic acid underwent the vapourisation process.

Despite this low amount of vapourisation, results have suggested that several reactions occur, on employing this acid at 120°C during the DSC experiments.

Before describing the TGA results for reactions 1–3 (Fig. 6), the

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TGA analysis of the four reference products (POM, POM + oxalic acid, melamine and M/F=1/6 under basic pH conditions) can be seen in Fig. 5.

The mixture of POM with oxalic acid showed a fast degradation rate below 200°C, compared with the POM degradation, demonstrating that this acid is able to decompose the polymer even at low temperature; the melamine reactant is thermally decomposed at higher temperature (300°C); and the conventional MF resin from a M/F molar ratio 1/6 shows a significant weight loss around 400°C. In Fig. 6a, the TGA curve evolution gives evidence of

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MF resin formation in all cases and the residual weights of the samples corresponding to reactions 1–3 are approximately 0.0, 3.7 and 1.2%, respectively. Also, the lowest M/F molar ratio gave the highest degradation rate compared with the other two MF resins, indicating a lower MF resin formation yield. Furthermore, the TGA derived curves of the samples, in which the maximum value of the different peaks could be determined, are reported in Fig. 6b. These results provide information regarding the curing mechanism and the MF resin structure obtained in each case.

The major weight losses in Reaction 1 were observed in the temperature range from 25 to 210°C (Fig. 6a), corresponding to 90.5% of the total mass and associated with water vapourisation, the released formaldehyde and oxalic acid residue.

The water vapourisation is related to the thermal curing process, by means of two processes: selfcondensation of methylol compounds, leading to ether bridge formation, and condensation between melamine and methylol groups, leading to methylene bridges. In the second temperature range, from 210 to 390°C, the weight loss (only 4.2%) was associated with the elimination of formaldehyde from ether bridges, forming methylene bridges followed by the breakdown of methylene groups of the MF resin, in accordance with the small peak determined in Fig. 6b at 380°C. The final temperature range above 390°C can be related to the thermal degradation of triazine ring and the formation of HCN, CO2 and CO. In this range, only 4.8 wt.% is decomposed and the final residual weight is nearly 0.0%, meaning that very little MF resin was obtained using a high excess of formaldehyde.

In Reaction 2, weight losses were observed in temperature ranges from 25 to 200°C, 200 to 385°C and at temperatures higher than 385°C. In the first temperature range, several weight losses were detected, attributed to water vapourisation, non-reacted formaldehyde thermal degradation and oxalic acid residue,

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Euro PM2021: Advances in MIM feedstocks

Fig. 6 TGA thermogram (a) and derivatives curves (b) of reactions 1, 2 and 3 after DSC experiments [2]

but these were lower than in the case of Reaction 1, 62.3% and 90.5%, respectively. Compared with Reaction 1, the peak at 380°C, corresponding to the main structural decomposition of methylene-MF resins, was more relevant, when the formaldehyde excess is moderate, as can be seen in Fig. 6b. Also, an intense peak at 520°C and a related 17.8% weight loss can be noted, that can be attributed to a branched structure, in which methylene bridges dominate.

This result may correspond to a high molecular weight and narrow distribution product but with low crosslinking, since the moderate excess of formaldehyde favours the chain growth of the resin.

Finally, Reaction 3 showed the lowest weight loss of the TGA signal from 25 to 200°C (29.5% in contrast to 90.5% and 62.3% for Reactions 1 and 2, respectively). Also, only one peak was determined in this range, at 170°C (Fig. 6b), which may be attributed to oxalic acid residue. The second temperature range of weight losses was determined as 200–400°C, composed of two degradation regions with a total mass degradation of 43.3%. The first peak, determined at 275°C in Fig. 6b, corresponded to 21% weight loss and may be related to non-reacted melamine, due to the molar ratio employed in this case (total concentration of melamine

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corresponds to 35.8 wt.% in Reaction 3). Also, the further weight losses around 400°C showed a main peak at 380°C, together with a small peak at 400°C (Fig. 6b). These were related to the methylene bridge breakdown of the varied MF structures formed.

The highest temperature range above 400°C corresponded to the highest weight loss (25.8%). However, no peak was noticeable in this range, in contrast to Reaction 2. This means that high thermostable products were present with a broad molecular weight distribution, when a moderate excess of melamine is used, due to a high degree of crosslinking.

In summary, the lower presence of formaldehyde in the reaction enhances the crosslinking process in the resins and the formation of more thermostable products.

On the basis of these results, it could be concluded that a M/F molar ratio between 1/5 and 1/12 could be defined as the most suitable to increase the MF resin formation.

Overall, the authors have concluded that it is possible to affirm that, by changing the debinding temperature, it is possible to modify POM degradation and, therefore, the MF formation. All of this information will be subsequently applied to the study of the POM debinding rate in ongoing research. This project will also be enriching, from a scientific

point of view, in investigating the influence of accelerator chemical structure on the decomposition sub-products obtained and analysing possible changes in the composition of emitted gases. What is clear is that such chemical modifications of the POM-based binder are suggested in order to further increase the debinding rate and, thus, the efficiency of MIM technology.

Unraveling the homogeneity of MIM The final paper reviewed was based on the recognition that defects in MIM parts are often not detectable until after sintering and that, therefore, much could be gained from the availability of analytical methods able to enhance understanding of the homogeneity of MIM feedstocks and green parts at an earlier stage in the process chain. This paper was presented by Sherif Madkour, Ingolf Hennig, Wieland Koban and Marie-Claire Hermant (BASF SE, Germany) [3].

The method presented by these authors considered the system under investigation as a binary system with metal/conductive fillers and binder/ polymer. Also, it assumed that the homogeneity of a binary (polymer/ filler) highly filled suspension is

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Screw configuration Sample

Original

Rework

Defects remarks

A

Kneader

-

No defect

B

Screw A

-

Cracks

C

Screw A

Screw A

No defect

D

Screw B

-

No defect

Table 4 A summary of the samples used and their description [3]

a function of two types of mixing: dispersive mixing and distributive mixing. On the one hand, good dispersive mixing means a smaller agglomerate size. Consequently, measuring the surface area of the metal agglomerates within the polymer matrix would be an accurate estimate of the quality of dispersive mixing. This could be achieved in a semi-quantitative manner utilising dielectric spectroscopy and/or quantitatively using BET N2-sorption. On the other hand, the quality of distributive mixing could be estimated by determining the interparticle distance; the better the former, the lower the latter; where interparticle distance > 0. Volume Intrusion Mercury (Hg) porosimetry was the characterisation method selected for this task.

BASF’s Catamold® 8620 was used as the system under investigation for this reported work. All samples used had the same recipes and identical metal powder loading. The presented measurements were focused on studying the homogeneity of the feedstock. It is well known

that the compounding process is a major player in the feedstock’s homogeneity quality. Therefore, only the compounding process was changed and all other post-processes (injection moulding, debinding and sintering) and their processing parameters were kept constant.

To produce a sample with different homogeneities, four different sets of feedstock samples were produced and tested.

1. Sample A: Feedstock produced on kneader 2. Feedstock from the twin-screw extruder (TSE) utilising screw configuration A 3. Reworked feedstock on the TSE with screw configuration A 4. Feedstock from TSE utilising screw configuration B, which had tailored dispersive and distributive mixing through precise shear application with guidance from the analytical results Despite the identical recipe and post-processing conditions, kneaded feedstock showed no defects,

whereas the extruded feedstock with screw A showed cracks in the sintered part. This led to the conclusion that different homogeneities could result in such defects.

A summary of all samples used is given in Table 4.

In dielectric spectroscopy, an AC electric field is applied to the dielectric material under investigation. The material is polarised due to the fact that the permanent dipoles and the induced dipoles try to orient themselves along the applied E field.

This yields a dielectric relaxation behaviour that is described by the so-called complex dielectric function ε*(f) = ε′(f) − iε″(f), where ε′ and ε″ are the real and imaginary (loss) parts of the complex dielectric function.

Here, f denotes the frequency and i is the imaginary unit.

Dipolar relaxation processes are characterised by their relaxation time, where the corresponding relaxation process shows a step in ε′(f) and a maximum in ε″(f). For polymers, the relevant relaxation processes are named α-, β- and ɣ- relaxations. Below the relaxation frequency, the dipoles can follow the applied E field, whereas, at higher frequencies, they cannot. However, in the range 60-90 GHz, there should no longer be any dipolar relaxation process, only electronic polarisation processes can still contribute to ε′ and yield an ε′ (electronic polarisation) in the range of 2–2.5. There is no dielectric loss contribution coming from electronic polarisation, meaning that ε’’ (electronic polarisation) = 0.

Fig. 7 Left; Schematic visualisation of interfacial polarisation in the case of agglomerated versus non-agglomerated conducting particles in a binder matrix, Right; Set-up of DS in microwave range 60–90 GHz [3]

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48

A

14

75 GHz

TSE Sample C

12 11

e¢¢

e¢

44 42 40 38 36

B

13

46

10 9

Kneader Sample A

8 7

6E+10

7E+10

8E+10

Frequency [Hz]

6

9E+10

6E+1

C 14

B

75 GHz

14

13

12

TSE Sample C

e¢¢ @ 75 GHz

12

e¢¢

11 10 9 8

6

6E+10

7E+10

8E+10

12 10

e¢¢IP @75 GHz (measured)

TSE Sample C

Kneader Sample A

8 6 4 2 0 0.00

0.02

0.04

Conductivity [S/cm]

0.06

Fig. 8 Example of measurements of (A) dielectric permittivity (B) dielectric loss as a function of frequency for a TSE - sample C and a Kneader – sample A. The blue and brown lines are reproducibility measurements for the TSE and the orange and black lines are for the kneader samples. (C) Contribution of ε″cond – black (measured by 4-point-contact resistivity) vs. that of ε″ IP, at 75 GHz, as a function of specific conductivity for samples A and C [3]

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0 0.00

9E+10

C e¢¢cond calculated from DC conducivity

8

2

Frequency [Hz]

14

10

4

Kneader Sample A

7

e¢¢ @ 75 GHz

e¢

There is another interesting polarisation phenomenon arising in this range, namely MaxwellWagner-Sillars polarisation (also called interfacial polarisation). In a heterogeneous system (e.g., polymeric system filled with metal particles), such interfacial polarisation takes place due to the huge difference in electrical conductivity between polymer (insulating) and metal particle (metallic conductivity). The electrons of the metal fillers are blocked at the interface to the polymer. The countercharge at the interface is created due to the electronic polarisation of the polymer. Thus, the induced interface dipoles result in the interfacial polarisation of the system, see Fig. 7. Since 48 A this polarisation75takes GHz place only at the polymer/filler interface and in a 46 frequency range where the interfacial TSE polarisation is the dominant process, 44 Sample C analysing the corresponding complex permittivity function; ε′ and ε″, should 42 give deep insights into the state of the available conductive surface area in 40 contact with the polymer.

Kneader The dielectric measurements in Sample A 38 the microwave range (60–90 GHz) were carried out with a corrugated 36 waveguide, as a sample holder. The S 6E+10 parameters 7E+10 (which 8E+10 9E+10 refer to the scatFrequency [Hz] tering matrix of a microwave network): S11 (reflection) and S21 (transmission) were measured via the network analyser with wave extenders for each 75 GHz 14 B frequency. From these parameters, the dielectric parameters ε′ and ε″ can 13 TSE be calculated. All measurements were 12 Sample C done at room temperature.

11 From the measured S-parameters, the dielectric parameters ε′ and ε″ of 10 the sample material were calculated 9 at each frequency point, using the swissto12 materials measurement 8 Kneader software, which uses well-known Sample A 7 equations for the reflection and transmission coefficient for a plane wave 6 onto a flat sample 6E+10 impinging 7E+10 vertically 8E+10 9E+10 with thickness d, to calculate S 11 calc (ε′, Frequency [Hz] ε″,d) and S21 calc (ε′, ε″,d). In addition, it uses a least squares optimisation to find the values of ε′ and ε″ until the difference between measured and calculated S11 (S21) is minimal. Fig. 8 shows an example of a dataset for different materials.

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B 105

C

95 90

-K ne ad er

85 80 SE

A

75

65

-T

70

R2 = 0.94

0.18

0.19

0.20

0.21

0.22

C

95 90 85 80 75

B-TSE

70 0.23

2.5

Sorption BET Area [m2/g]

Goal

D ign

100

Re wo rki ng eff ec t Im pr ov ed sc re w de s

-R ew or k

100

D -Im pr ov

TS E

.T SE

105

µ Agglomerates surface Area

110

B

µ Agglomerates Surface Area- Aip [µ m2]

A

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2.4

A-Kneader Reference

2.3 2.2 2.1 2.0 1.9 Average pore diameter [µm]

1.8

1.7

Fig. 9 (a) Correlation between the surface area of the agglomerates calculated from dielectric spectroscopy versus the BET area measured from N2-sorption. The red line is a linear fit with R2 of 0.94. (b) Homogeneity map for all samples measured. A detailed description of the samples is given in Table 4 [3]

To confirm that the calculated surface area of the agglomerates does indeed reflect the measured value, the BET area is plotted against the calculated number proportional to the surface area (Aip) measured from dielectric spectroscopy (given in Fig. 9a). Fig. 9 reflects a strong linear proportionality with R2 =0.94, confirming this assumption.

Hg- Porosimetry is a method of structure analysis, where pore diameters in the 0.001 µm - 430 µm range can be measured. With mercury porosimetry, pore information is obtained by forcing liquid mercury into these pores by increasing the external pressure. As the pressure is incrementally increased, the amount of mercury required to fill the pores is recorded. This information, as well as information concerning the contact

angle, is used to calculate the pore structures using the Washburn equation. Pore area, pore volume, bulk density and porosity values could all be measured or calculated.

Measuring the pore size distribution of debound granulates and brown parts serves as a good tool to quantify the quality of the binder distribution and thus the quality of the distributive mixing. By measuring both debound granulates and brown parts, conclusive insights into the effect of TSE, kneader, and injection moulding on distributive mixing could be made. Fig. 10a depicts a typical set of data presented as log differential intrusion as a function of pore size diameter.

The porosimetry results for Catamold have shown that the pore size distribution of Catamold has

“Measuring the pore size distribution of debound granulates and brown parts serves as a good tool to quantify the quality of the binder distribution and thus the quality of the distributive mixing.”

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three main regions, each revealing new insights into its structure. The three different regions, as illustrated in Fig. 10a, are: • Region I. Pores mainly due to air bubbles formed during compounding, see Fig. 10b and its inset. These bubbles are normally completely degassed during injection moulding • Region II. Polymer domains imprint, which gives the most important insights into the distributive mixing • Region III. Shrinkage gaps due to POM’s strong crystallinity/ shrinkage behaviour, which only appears in the green part and feedstock and not in the brown state Region II is the most relevant and important range in the porosity measurements. It normally extends between around 10 µm – 0.5 µm and dominates over 95% of the total intrusion volume, in debound feedstocks and brown parts. However, for feedstock and green parts (non-porous sample geometry with the binder, thus measuring only the surface porosity), no peaks are observed in this region. Therefore, region II is assigned to the binder imprint. Consequently, the average pore size diameter in region II is

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Euro PM2021: Advances in MIM feedstocks

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0.5

Region II

0.4 0.3

Region III

Region I

0.2 0.1 0.0 100

1

0.1

B

Feedsto debinde Green p Brown p

0.012

0.008

0.004

0.000

0.01

500 400

B

0.016

Log Differential Intrusion [mL/g]

10

Pore size Diameter [µm]

Log Differential Intrusion [mL/g]

0.016

Feedstock debinded feedstock Green part Brown part

C

Feedstock debinded feedstock Green part Brown part

0.7

0.012

0.008

Feedstock

0.004

Log Differential Intrusion [mL/g]

Log Differential Intrusion [mL/g]

A

0.6 0.5 0.4 0.3 0.2 0.1 0.0

0.000 500 400

300

200

100

5

Pore size Diameter [µm]

C

sample A -1 sample A -2 sample B -1 sample B -2 sample C -1 sample C -2 sample D-1 sample D-2

0.7

Log Differential Intrusion [mL/g]

Log Differential Intrusion [mL/g]

the interparticle distance in the 3D network and defines the quality of the distributive mixing in the feedstocks (TSE or kneader effect) and parts (injection moulding effect). Fig. 10c shows the results of all samples measured as well as the reproducibility measurement for each sample.

Having now shown that the surface area of the agglomerates (Fig. 9a), as well as the interparticle distance (Fig. 10c), could be quantitatively measured, the next step was to assemble all the measured information, in order to assess the homogeneity quality of the samples of Catamold 8620.

Fig. 9b shows the proposed A Feedstockrepresentation to assess the overall debinded feedstock Green parthomogeneity quality in the so-called 0.5 Brown part homogeneity map. The X-axis Region II presents information on average 0.4 interparticle distance (average pore size diameter) and the Y-axis 0.3 III of Region I presents information onRegion the size the agglomerates (interfacial polari0.2 sation surface area). To achieve optimum homogeneity requires 0.1 the lowest possible interparticle distance, with the highest possible 0.0 surface area.

100 10 9b shows 1 that 0.1 Fig. sample 0.01 B (TSE) Pore size Diameter has worse distributive[µm] and dispersive mixing, compared with the kneaded sample. However, by reworking the B 0.016 Feedstock feedstock in the TSE, sample C, both debinded feedstock Green part dispersive and distributive mixing Brown part were significantly improved. Though 0.012 the reworked sample has better dispersive mixing, even compared to the kneaded materials, it still Feedstock 0.008 slightly lags in terms of distributive mixing. In the light of the new insight delivered by this study, screw B was 0.004 designed to improve distributive mixing quality, by carefully adding mixing elements to the screw 0.000 configuration.

Sample D (TSE-with 500 400 300 200 100 improved design) depicts Porescrew size Diameter [µm] the superior homogeneity quality, as compared with samples A and C. This indicates the potential for using a TSE for compounding MIM feedstocks.

These results were in good agreement with defect observations on sintered parts, where sample A, C and D, were found to be defect-free.

0.6 0.5 0.4 0.3 0.2 0.1 0.0 5

4

3

2

Pore size Diameter [µm]

1

Fig. 10 (A) Log differential intrusion as a function of pore size diameter over the whole measured range, for feedstock – green, debound feedstock -yellow, green part -dark green, and brown part -brown, illustrating the 3 different regions discussed. (B) A zoom onto Region I (Inset) Microscope picture of feedstock cross-section showing the pore due to air bubbles (C) Log differential volume intrusion as a function of pore size diameter for samples A- red, B-blue, C-green, and D-gray. The dashed curves are reproducibility measurements [3]

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Consequently, distributive mixing could probably be one crucial parameter in avoiding cracks in the final parts.

Overall, the authors concluded that the developed method could prove to be a powerful tool, sensitive enough to detect small differences in overall homogeneity and giving new insights into feedstocks and green part quality. More importantly, this could be used as guidance for compounding process design to ensure high-quality feedstocks for reliable MIM part production.

Author and contacts Dr David Whittaker Tel: +44 1902 338498 whittakerd4@gmail.com [1] Christian Kukla, Montanuniversitaet Leoben christian.kukla@unileoben.ac.at [2] Cristina Berges, Universidad de Castilla-La Mancha cristina.berges@uclm.es [3] Sherif Madkour, BASF SE sherif.madkour@basf.com

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References [1] Effect of backbone selection on the solvent debinding of metal injection moulding feedstocks, Kukla C., Cano S., Schuschnigg S., Holzer C., Gonzalez-Gutierrez J. As presented at the Euro PM2021 Virtual Congress, October 18–22 2021, and published in the proceedings by the European Powder Metallurgy Association (EPMA) [2] Accelerated PIM processing by chemical modifications in the binder during the debinding stage, Cristina Berges, Juan Alfonso Naranjo, Macarena Jimenez, Manuel Carmona, Ignacio Garrido, Gemma Herranz.

As presented at the Euro PM2021 Virtual Congress, October 18–22 2021, and published in the proceedings by the European Powder Metallurgy Association (EPMA) [3] Unraveling the Homogeneity of MIM, Sherif Madkour, Ingolf Hennig, Wieland Koban, Marie-Claire Hermant. As presented at the Euro PM2021 Virtual Congress, October 18–22 2021, and published in the proceedings by the European Powder Metallurgy Association (EPMA)

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CATAMOLD® MOTION 8620: BASF’S NEW LOW ALLOY FEEDSTOCK BASED ON PREALLOYED METAL POWDERS BASF SE, the market leader in feedstocks for Metal Injection Moulding, has expanded its feedstock range with the release of Catamold® motion 8620, a low alloy steel feedstock suited to high performance automotive applications.

In this paper, the company’s Marie-Claire Hermant, Rudolf Seiler, and Thorsten Staudt introduce the new feedstock and the strategy behind the move to pre-alloyed, water atomised powders. The properties and performance of the new system are compared with those of the company’s existing Catamold 8620 that uses the master alloy approach.

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The growth of MIM in China: an analysis

What drives the success of an industry: chance or strategy?

Lessons from the growth of MIM in China In March 2007, the very first issue of PIM International featured a review of MIM in Asia. China’s MIM industry was estimated as having around twenty MIM firms, many modest in size and of limited capability, with Taiwan accounting for another fifteen. Fast forward less than fifteen years, and Greater China now accounts for half of global MIM production, is a leader in MIM-grade powder production, and is home to a host of production equipment manufacturers.

Industry consultant Dr Chiou Yau Hung (Dr Q) assesses just what happened to drive this success: good fortune, good strategy, or a slice of both?

When Apple launched its new iPhone 13, we were very happy to see that parts produced by Metal Injection Moulding still featured heavily. While the company’s requirements for MIM parts are very demanding across the board, this is especially the case in terms of part complexity, tolerances and appearance. It is in the latter – in a part’s aesthetic features – where the capabilities of MIM products can often be best demonstrated.

Their excellent metallic appearance and surface finish, in addition to a variety of special capabilities unique to certain alloys, all available at a relatively quick production speed, are some of the key factors in MIM’s rise in popularity. And the technology’s progress shows little sign of slowing, with the new generation of folding smartphones relying on metal injection moulded hinges to deliver stable, long term performance.

I believe that we are all curious as to the reasons driving the rapid growth of the MIM industry in Greater China – including mainland China, Taiwan, Hong Kong, and Macau – in

Vol. 15 No. 4 © 2021 Inovar Communications Ltd

the last decade. Is success down to being in the right place at the right time, to a series of coincidences, or can individuals and governments, through strategic goals or individual efforts, drive the success of an industry? Here is my analysis.

MIM plants in a major economic zone In mainland China, there are two major triangular economic zones – the Pearl River and the Yangtze River deltas. Together, these are home to

Number of MIM plants in the Great Bay Area

Zhaoqing

Guangzhou

Huizhou

Dongguan

Foshan

Zhongshan

Shenzhen

Jiangmen Zhuhai

Macau

Hong Kong

Fig. 1 Number of MIM plants in the Great Bay Area (Drawing by Dr Q and graphic by http://pharmaboardroom.com)

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Fig. 2 A view of Shenzhen's Civic Center and Lianhuashan Park (Courtesy Sparktour / Wikimedia)

almost the entire capacity of Chinese manufacturing. Within the Pearl River Delta, the Greater Bay Area (GBA) represents nine cities from the Guangdong province, as well as the entirety of the Macau and Hong Kong regions (Fig. 1). This is the world’s most populous bay area – greater than San Francisco, New York, and Tokyo – and alone represents one of the largest economies in the world.

The GBA hosts the greatest number of MIM plants in Greater China.

The GBA is also home to a leading manufacturing innovation city: Shenzhen. While the region faces increasing competition for low-cost manufacturing from Southeast Asian countries such as India and Vietnam, as well as in rapid research and development for innovative electronics from Europe, the United States, and Japan, the industry here naturally aims to keep its name relevant through its MIM technology capabilities. With the ability to meet

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the needs of a large number of orders in a short amount of time, it slots into place with the product development and mass-production methods already established in the GBA.

Without knowledge, there is no power: outstanding teachers as the catalyst for success The dissemination of knowledge is crucial when considering whether a new technology can be adopted by a region. I joined the MIM industry in 1991, one afternoon during the first week of my master’s degree, and, after thirty years in the field, I have come up with a list of the three most respected educators from Greater China who have played a key role in nurturing and developing the talent that enabled the industry’s success.

December 2021

Prof Kuen-Shyang Hwang Prof Kuen-Shyang Hwang (Fig. 3) teaches in the Department of Materials Science and Engineering, Taiwan University. He returned to Taiwan in 1988 from the United States, where he began his MIM research. All of Prof Hwang's teachings and research are related to PM and MIM, an area in which he has mentored many students, many of whom are now in the MIM industry.

Among these is Dr Y C Lu, Professor Hwang’s first PhD graduate, of Taiwan Powder Technology Co., Ltd. (TPT). TPT was the first company in Asia to produce MIM 3C products on a large-scale production order.

In terms of technical contribution, Prof Hwang was the one who advocated ASTM F75 alloys for smartphones; this alloy has since been used in the camera frames of over 500 million smartphones since 2016. He has published two textbooks, Powder Metallurgy

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The growth of MIM in China: an analysis

(3rd ed.) and Metal Injection Molding (2nd ed.), both of which are widely used in industry and academia.

However, he has often said that, while we can record our knowledge in such books, we should better appreciate the real-world skills, know-how and experiences which are key to making things happen and keeping the MIM industry strong and vibrant.

Prof Shun-Tian (Paul) Lin Prof Shun-Tian Lin (Fig. 4) teaches in the Department of Mechanical Engineering, Taiwan University of Science and Technology. He returned to Taiwan from the United States in 1991 to promote the MIM of iron, stainless steel, copper and carbides, as well as ceramics. My master’s and PhD courses were guided by Prof Lin. His highest achievement is bridging the gap between PIM research and industry. Using his in-depth knowledge of a wide range of materials, he has guided many companies in Greater China to successfully integrate MIM and CIM technology into their products.

Prof Xuanhui Qu Prof Xuanhui Qu (Fig. 5) teaches Powder Metallurgy at the School of Materials Science and Engineering, within the University of Science and Technology Beijing.

He is a Chinese-educated scholar who, since the beginning of his professorship in 1992, has trained over one hundred postgraduate students, many of whom are active in the MIM industry, including engineers, CTOs and CEOs. He allows students to guide their own work – something very admirable amid potentially rigid academic life. Today, he is the president of the MIM Association of the China Powder Metallurgy Alliance (CPMA), as well as the president of Powder Metallurgy Committee of the Chinese Society of Metals.

He has served as Editor in Chief of the journal Powder Metallurgy Technology, the longest-running Chinese PM journal, since 2010.

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Fig. 3 Prof Kuen-Shyang Hwang

Fig. 4 Prof Shun-Tian (Paul) Lin

Fig. 5 Prof Xuanhui Qu

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Government initiatives as a driver of R&D

Fig. 6 The launch of Apple's Lightning Connector in 2012 was a major turning point in the growth of MIM in the 3C sector, with at least a billion of these leads now estimated to have been produced

As early as 1996, MIM was identified as one of the key technologies for the future of China’s manufacturing industry. MIM research and development programmes have been continuously supported by government programmes such as the National Natural Science Foundation of China (NSFC), the National High-Tech R&D Program of China (863 Program), the National Basic Research Program of China (973 Program), and the National Key Research and Development Program of China, to name just a few.

With the support of these R&D programmes, great progress has been made in basic research, from alloy selection, to binder design, fundamental process research and so on. The success of this basic research has established a substantial foundation for the rapid development of China's MIM industry.

Coincidental timing

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Fig. 7 MIM micro-gear reduction modules, with small motor drives, are used as a lifting mechanism on smartphones with a retractable camera

In life, some things develop naturally, and some are helped along by luck. The successful development of industrial technology also needs coincidence. These are some of the 'coincidences' that I believe had an impact on the development of MIM in China.

Fig. 8 The camera lens protector used in the latest Apple iPhones is made by MIM using CoCrMo alloy (ASTM F75) (Courtesy Apple)

The winter crisis that catalysed massive infrastructure development In early 2008 in China, a severe winter blizzard paralysed transportation and affected hundreds of millions of people preparing to return home for the Chinese New Year. The weather also worsened the ongoing economic depression at that time, as workers were left unable to return to their workplaces. Following this crisis, the Chinese government began to focus on the improvement and construction of the country's transportation infrastructure – power networks, communications, roads, railways, and water supply. After ten years of construction, the foundations of the

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The growth of MIM in China: an analysis

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Liquidmetal Liquidmetal Liquidmetal Liquidmetal Liquidmetal Liquidmetal

Liquidmetal Liquidmetal Liquidmetal Investment Investment casting Investment Investmentcasting casting casting Liquidmetal Liquidmetal Investment Investmentcasting casting

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Fig. 9 Comparison of advantages between MIM and competitive processes

relevant transportation systems had been transformed.

Connected with this, the MIM industry found the opportunity to benefit not only from increased government funding, leading to rapid adoption by a variety of sectors, but it also directly benefited from the new, faster, more efficient transportation networks.

Smartphones drive business opportunities The rise of MIM technology can be viewed in parallel to the rise of smartphones. With perhaps the same global impact as the adoption of fire, smartphones have changed human civilisation. They allow unprecedented information transmission and clearer, more widespread communication than ever before. Of course, this universal electronic device needs to be strong, functional and aesthetically appealing. MIM products provided the necessary structural strength for this whilst having the desired aesthetically appealing appearance (Figs. 6–8).

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The COVID-19 pandemic, the US/ China semiconductor trade war, and the wider semiconductor crisis led to reduced smartphone production, resulting in a reduction in the demand for MIM parts for this application.

This resulting spare capacity led to an immediate production shift in Greater China. Small smartphone parts were replaced by components for domestic products, often larger in size. This shift was in part possible thanks to the low cost of Chinese MIM powders. This, combined with low domestic transport costs, has allowed raw materials and products to be produced nearer the point of demand, without the need for international shipping. The MIM industry in Greater China has, in this instance, proven itself resilient.

Energy conservation and carbon reduction: an opportunity to challenge other processes By the end of 2021, countries around the world will begin a new wave of energy regulation. This gives the MIM industry a powerful business opportunity as a relatively energy-efficient

manufacturing process. MIM is highly flexible and offers many advantages for small parts manufacturing, especially in comparison to processes with high energy consumption and a negative environmental impact, such as die casting, lost-wax casting (investment casting), traditional casting, forging, etc (Fig. 9).

The rise and rise of domestic equipment suppliers The localisation of MIM equipment production began in about 2011 and hasn’t stopped since. More than five generations of batch vacuum sintering and debinding furnaces were developed in only a decade. The invention of oxalic acid catalytic debinding by Shenzhen SinterZone technology Co., Ltd. in 2014 was a big step towards reducing the environmental impact of the MIM debinding process. Ningbo HIPER Vacuum Technology Co., Ltd. advanced its batch vacuum sintering furnace technology to six-zone temperature control. Continuous sintering furnaces have also been manufactured for five years by Hiper and SinterZone.

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The growth of MIM in China: an analysis

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“At least ten powder manufacturers in China produce more than 2,500 tons of MIM powder a year – there is even one small factory with a single atomiser, yet it can also produce 250 tons of MIM powder a year. This easy sourcing of raw materials has therefore also been a major boost for MIM's development.”

All these equipment innovations have been based on a desire for greater environmental protection, CO2 reduction, energy conservation, and safety. In addition to furnace technology, innovations have also been introduced that automate feedstock kneading and granulation, saving on labour costs.

The high-volume production of MIM powders One could be mistaken for thinking that the materials used by MIM today are based on quite long-established specifications such MPIF Standard 35.

Don't overlook the fact that, historically, industrial powder production had never been able to atomise high percentages of d50 < 15 µm fine powder. The production of MIM grade powders is as high as ever.

At least ten powder manufacturers in China produce more than 2,500 tons of MIM powder a year – there is even one small factory with a single atomiser, yet it can also produce 250 tons of MIM powder a year. This easy sourcing of raw materials has therefore also been a major boost for MIM's development.

Rapid, efficient tooling removes the barriers to MIM Greater China has a lot of plastic injection moulding companies, meaning there are also quite a few corresponding injection moulding tooling factories. Although the tooling used for MIM and plastic injection moulding are different, a ‘general’ injection moulding tooling factory may still have experience manufacturing

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some sets of MIM tools. Moreover, these factories can quickly learn the specific manufacturing expertise needed for MIM tools, and expand production.

Today, a record number of rapid tooling producers exist with the ability to complete a set of four-cavity moulds within seven days, in order to provide prototypes to customers.

Perhaps this is the main reason why the MIM industry does not use additively manufactured rapid prototypes.

Many tooling factories in Greater China already operate highly efficient and automated ‘lights out’ production – this is a real enabler of the fast delivery times offered by the MIM industry.

multi-step combination of traditional industrial technologies. Each step requires careful learning, observation, recording and operation. Due to its unique human resources and the nature of business in Greater China, the MIM industry has been able to adapt itself into just what its customers need.

Of course, it is not always ‘plain sailing’: equipment manufacturers are working day and night, both to fulfil equipment orders and develop new equipment, and many MIM factories use the current intermittent power supply situation to complete customer orders – including the author himself, as I write this manuscript. Welcome to Greater China and its MIM family!

Author Dr Q (Y H Chiou) You neeD Technical Office chiou_yh@yahoo.com.tw

Outlook and expectations Although MIM technology has only existed for around half a century, it has been promoted in Greater China since 1985. The fortuitous combination of the many events and circumstances presented here has resulted in the Chinese MIM industry accounting for half of the world’s production. What is clear is that wellfunded R&D centres, connected to industry by high-profile ‘technology champions’, all operating within a defined strategic national framework, can result in what, by any standards, is a major success story.

While many people still don't know MIM by name, its products have followed people into their smartphones, cars and domestic appliances. MIM technology is a

December 2021

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FROM OUR

ARCHIVE

INSIDE CHINA’S LARGEST MIM COMPANY: INNOVATION, RESEARCH AND THE MIM SMART FACTORY AT JIANGSU GIAN TECHNOLOGY CO., LTD. The ability to innovate is the cornerstone of the successful evolution of technology companies.

Jiangsu Gian Technology Co., Ltd., China’s largest Metal Injection Moulding company, has always followed such a philosophy.

Dr Chiou Yau Hung (Dr Q) visited the company on behalf of PIM International and spoke with Junwen Wu, the company’s vice president, about how innovation, from materials development to the use of Artificial Intelligence for advanced quality management, has become the driving force behind the company’s success.

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MIM 420 martensitic stainless steel

A microstructural investigation of 420 martensitic stainless steel processed by MIM Type 420 martensitic stainless steel covers a wide carbon range of 0.15% to 0.45%.

Demand for this material from the 3C, automotive, biomedical and aerospace industries has been increasing thanks to its combination of moderate corrosion resistance, high hardness, and good tensile properties. In this study, Shu-Hsu Hsieh, Dr Chung-Huei Chueh, and I-Shiuan Chen, from Chenming Electronic Technology Corp. (UNEEC), Taiwan, investigated Nb-alloyed 420 produced using BASF SE's Catamold 420 W feedstock. Decarburisation was examined in samples processed in both a graphite furnace and a molybdenum lined furnace. Microstructure, phase and hardness variations from the sintered state to each specific stage in heat treatment were also explored. Additionally, the influence of niobium on the formation of intergranular compounds, carbides, and carbonitrides was also assessed in each heat treatment stage for comparison.

Among the most exciting emerging developments in the modern 3C (computer, communication and consumer-electronics) industry are applications based on advanced metallic materials. These new applications take advantage of materials with excellent mechanical strength combined with reasonably high corrosion resistance, wear resistance and specific magnetic properties, such as ferromagnetism or paramagnetism, depending on the product design and function. These materials include stainless steels and cobalt alloys, as well as other cutting-edge alloys.

Some well-known examples for these advanced alloys are camera components (switches and buttons), laptop and smartphone hinges, cases for wearable devices, soft magnetic applications, electronic packaging, heat sinks/heat spreaders for cooling electronics, and USB connectors.

A high degree of skill and precision engineering is needed to create the components that go into such devices and there are many hurdles to overcome. It is, however, important that

Vol. 15 No. 4 © 2021 Inovar Communications Ltd

product designers in this field are able to find and select the proper materials quickly and easily in order to keep on top of the fast-paced development.

Stainless steels, a group of advanced ferrous alloys, were invented at the beginning of the 20th century in Germany (Eduard

Maurer and Benno Strauss in 1912) and in England (Harry Brearley in 1913). In accordance with the European standard EN 10088, steel is classed as stainless when its chemical composition has a minimum chromium content of 10.5%, which enables the formation of a thin, tenacious, and protective chromium oxide

Fig. 1 Sintering furnaces at Chenming Electronic Technology Corp. (UNEEC), a Taiwan-based global OEM/ODM and a major MIM component producer with operations in Dongguan, China, since 2002

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MIM 420 martensitic stainless steel

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“The typical heat treatment process for martensitic stainless steels such as 420 includes heating to the soft-annealed condition, where islands of spherical carbides exist in a ferritic matrix, resulting in a soft steel which allows subsequent cold work or machining.” passive film. Stainless steels can be ferritic, austenitic, martensitic or a combination of all phases, according to their chemical composition.

Martensitic stainless steels (MSSs), formed via diffusionless transformation, are a class of stainless steels with hardenability, meaning that the mechanical properties of the steels can be significantly altered by a hardening heat treatment to achieve the desired mechanical properties, such as superior strength, high hardness and high toughness, etc. This type of steel is characterised by a limited chromium content (normally between 11.5% and 18%) and carbon contents among the highest of the stainless steels most commonly used (generally between 0.1% and 1%, C<0.015% for the supermartensitic grades), as can be observed in a conventional Schaeffler diagram. MSS type 410 is a grade that is regarded as a general purpose martensitic steel and contains about 12 wt.% Cr and 0.1 wt.% C to provide strength.

Applications for type 410 include fasteners, springs, pins, cutlery, hardware, gun clips, microparts, turbine blades, coal screens, pump rods, nuts, bolts, fittings, ball bearings, shafts, impellers, pistons, and valves. The carbon level – and consequently, strength – increase in the 420, 440A, 440B, and 440C alloy series. MSS type 420 covers a wide carbon range of 0.15% to 0.5%, the selected carbon content depending on the desired hardness, and therefore has a relatively wide range of hardness levels in both the hardened and tempered conditions.

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Higher carbon leads to increased hardness at the expense of ductility and corrosion performance. Versatile hardness can be obtained via heat treatment cycles, and this makes type 420 desirable where tempered products are necessary for specific applications, such as laptop/smartphone hinges, steam generators, mixer blades, fasteners, cutlery, machine parts, bushings, surgical tools, firearms, needle valves and ball valves. 440A, 440B, and 440C, in particular, have an increased Cr level in order to maintain corrosion resistance.

In general, 440A has excellent hardening performance and high hardness, and its toughness is higher than that of 440B and 440C. 440C stainless steel is a member of the 400 series of stainless steels. It has the highest carbon content among them. The standout properties of this type of steel are its hardness, mechanical strength and fatigue resistance, making it useful in the production of cutting tools. Due to 440C’s high carbon content, it does not have outstanding corrosion resistance, but it can still be used for applications that require moderate corrosion resistance such as surgical instruments, cutting tools, nozzles and bearings. 440C steel is sometimes called ‘surgical stainless’.

Alloying elements, like Mo, Ni, V, Nb, Al and Cu, are added for the enhancement of specific properties. Molybdenum can be added to enhance mechanical properties or corrosion resistance, as it is in type 422 stainless steel. Nickel can be added for the same reason in type

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414 and 431. When higher Cr levels are designed to improve corrosion resistance, nickel also serves to stabilise the desired microstructure and to prevent excessive free ferrite.

The limitations on the alloy content required to maintain the desired fully martensitic structure restrict the obtainable corrosion resistance to moderate levels. Chromium, a high ferrite stabilising element, and carbon, an austenite stabilising element, are balanced so that the steel has an austenitic structure at high temperature and a martensitic structure at ambient temperatures.

One of the benefits of martensitic steel is that it becomes stronger and harder after heat treatment. Heat treatment is the controlled heating and cooling operation performed on the material. When the material is subjected to heat treatment, the atomic structure or microstructure may change due to movement of dislocations, increase or decrease in solubility of atoms, increase in grain size, formation of new grains, creation of new different phase and change in crystal structure [1-12].

The typical heat treatment process for martensitic stainless steels such as 420 includes heating to the soft-annealed condition, where islands of spherical carbides exist in a ferritic matrix, resulting in a soft steel which allows subsequent cold work or machining. Moreover, a subsequent austenitising treatment forms an austenitic structure and fully or partially dissolved carbides, cooling or quenching to transform the austenite to martensite, followed by tempering of the martensitic structure to improve toughness and ductility.

During the transformation of FCC γ- phase (austenite) into a BCC lattice structure, after reaching the critical cooling rate that is high enough to suppress the solid-state diffusion of dissolved carbon atoms, the lattice structure is deformed and the nucleation of a martensite grain grows rapidly through the material until it approaches another grain boundary. When the cooling rate is fast enough, the dissolved carbon in

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MIM 420 martensitic stainless steel

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the austenite cannot diffuse out of the FCC lattice structure, leading to a tetragonal lattice distortion (i.e., BCT, or body-centered tetragonal, crystal structure). As for cryogenic treatments [13-25], normally carryied out after a conventional quench process but before tempering, these are usually carried out at -80°C and -196°C, corresponding to dry ice sublimation temperature and liquid nitrogen boiling temperature, respectively.

When heat-treated steels are cooled to extremely cold temperatures, retained austenite is transformed to martensite. Retained austenite is brittle and, if not transformed to martensite, can cause chipping or cracking. As a worst case, retained austenite can act as nucleation sites for metal fatigue. In order to increase ductility and toughness, martensite is heat treated in a process called tempering. Strength typically decreases with increasing tempering temperature and time and a corresponding increase in toughness is expected.

Heat treating martensitic stainless steels is essential to achieve improved strength, fracture toughness and hardness, depending on carbon content. The final microstructure of AISI 420 is very dependent on the prior heat treatment that the steel receives and typically consists of martensite, undissolved and/ or re-precipitated carbides and retained austenite. The volume fraction and size of the carbide particles present in the steel and the amount of retained austenite play a major role in determining the hardness, strength, toughness, corrosion resistance, and wear resistance of the steel.

Powder metallurgical processes are increasingly deployed for the manufacture of mechanical parts for numerous industrial and consumer applications. When suitably compounded with polymeric binder materials, these inorganic powders can be moulded in the same manner as thermoplastics.

The most common example of this approach is Metal Injection Moulding

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Fe

C

Cr

Mo

Nb

Ni

Si

Mn

Bal

0.57

13.03

0.07

1.48

0.18

0.74

0.72

Table 1 BASF Catamold 420 W chemical composition (wt.%)

Annealing

910°C for 2 hours in Ar atmosphere

Austenisation and quenching

Ar, 1020°C, 15 min / oil quench

Cryogenic treatment

2 hours, -80°C,

Tempering

200°C for 2 hours in Ar atmosphere

Table 2 Heat treatment conditions for BASF Catamold 420 W

for small parts with high shape complexity, tight tolerances, and high production volumes. For parts with simple shapes, extrusion or simple compression moulding may be used.

The products obtained via this process can avoid the density gradient that occurs in the conventional ‘press & sinter’ Powder Metallurgy process. MIM uses the shaping advantage of plastic injection moulding, but expands the applications to numerous high performance metals and alloys. This advanced technology has grown in popularity in the past three decades as an effective approach to producing geometrically complicated near-net shape parts, with high dimensional accuracy and excellent surface finish, and it can make thin-walled parts to tight tolerances for a variety of industries using a process that is extremely cost-competitive for large scale production. Major markets for MIM include medical, automotive and aerospace, as well as the 3C sector previously mentioned [26-44].

The high level of freedom when designing geometrically, sophisticated, high-strength, high-volume production parts, with a fine surface finish, accurate tolerance, and flexible material choice has enabled MIM to thrive in the 3C area. The electronics industry is a major user of MIM parts, accounting for robust sales growth globally, but especially in Asia. Connectors with complex geometries are now major MIM products and the continuing

miniaturisation of electronic devices demands ever smaller components in order to achieve better performance at lower cost. This is where MIM has a unique competitive advantage.

In this article, Nb-modified 420 was prepared via the MIM process and its microstructures, phases, and precipitates were investigated.

Decarburisation was investigated in a graphite furnace and a molybdenum lined furnace, respectively. Hardness and microstructure in each specific stage of heat treatment were also examined and assessed.

Experimental procedure The feedstock used in this study, Catamold 420 W, was manufactured by BASF using its proprietary polyoxyethylene-based (POM) binder system. This is based on Nb-modified type 420 martensitic stainless steel powder and the composition is shown in Table 1.

Green parts were prepared by injection moulding under various conditions using a NISSEI NEX 50T machine. Moulded parts were then subject to a debinding process in a WINTEAM HT-220LTZL furnace in fuming nitric acid. Sintering trials were first performed in a SHIMADZU VHSgr 40/40/150-M graphite batch furnace using argon atmosphere at 60 kPa pressure. For comparison, sintering was also conducted in a Nabertherm VHT 40/16-MO H2

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MIM 420 martensitic stainless steel

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(110)

martensite/ferrite

Intensity (a.u.)

NbN/NbC

(200)

(111) (200) (b) 420 (sintered in N2)

(a) 420 (sintered in Ar) 20

30

40

50

60

70

80

2θ (°)

Fig. 2 X-ray diffraction (XRD) patterns of sintered 420 W specimen (a) 420 W sintered state, based on 1355°C sintering, graphite furnace, Ar atmosphere (b) 420 W sintered state, based on 1340°C sintering, molybdenum line furnace, N2 atmosphere

molybdenum lined furnace in flowing nitrogen at 100 kPa pressure, at 1340°C for 3 hours with 5 K/min heating rate. The conditions chosen for heat treatment are given in Table 2.

X-ray diffraction, XRD, (D2, Bruker, Karlsruhe, Germany) was applied for crystal structure identification.

Element distribution was assessed via EPMA (JXA-8200SX, JEOL, Japan) with EDS (X-MAX 50, Oxford Instruments, UK). For morphological, microscopic and phase investigations, Optical Microscope (HM-3006, Jia Yu Apparatus Co., Ltd., Taiwan) and FESEM (JSM-7800F Prime,

JEOL, Japan) with electron backscatter diffraction (EBSD) detector (NordlysNano, Oxford Instruments, UK) were applied. Transmission Electron Microscope, TEM (JEM-2100F, JEOL, Japan), with EDS (INCA X-sight, OXFORD, UK) was also applied.

Results The XRD patterns of Ar-sintered 420 W are shown in Fig. 2 (a). The major crystal structure is BCT martensite or BCC ferrite, since these two crystal structures are indistinguishable in

“The surface region has lower hardness than the central region, implying that the presence of ferrite white layer led to the hardness reduction, while the central region structure is still based on a high hardness martensite matrix.”

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XRD due to having quite similar lattice constants. The optical microscopy (OM) images of Ar-sintered 420 W surface and central regions are shown in Fig. 3 (a) and (b), respectively. From the OM results, martensite is the major structure and thus the presence of BCC ferrite can be excluded in the XRD results in Fig. 2 (a). From OM images, it can be clearly observed that a roughly 100 μm to 150 μm thickness of decarburisation white-layer appeared near the upper side of the surface region.

Utilising EPMA mapping in Fig. 3 (e) also revealed the presence of low-carbon and high-chromium concentration areas, confirming the decarburisation phenomenon aforementioned. For the central region, the microstructure is identified as martensite, as shown in Fig. 3 (c), (f), and (g), and there is a significant amount of precipitated particles, both on grain boundaries (intergranular compound, highlighted by the red arrow) as well as inside the grains, shown in Fig. 3 (c). The precipitated particles are abundant in Nb and C, as demonstrated in EDS elemental mapping in Fig. 3 (d). Table 3 also points out the hardness deviation between the surface and central regions of sintered specimens. The surface region has lower hardness than the central region, implying that the presence of ferrite white layer led to the hardness reduction, while the central region structure is still based on a high hardness martensite matrix.

Commercial martensitic stainless steels are often supplied in the annealed state, allowing the material to be easily formed and machined by the fabricator or user. Annealing is recognised as the procedure whereby a material is heated to and held at a suitable temperature and then cooled at a well-defined rate to reduce hardness, improve machinability, facilitate cold workability, produce a specific microstructure, or obtain desired mechanical, physical or other properties.

In this work, the annealing process was conducted at 910°C for 2 hours in Ar atmosphere. The OM images of the annealed 420 W surface and central

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(a)

(b)

(c)

(d)

(e)

(f)

(g)

Fig. 3 Analysis of 420 W sintered state, based on 1355°C sintering, graphite furnace, Ar atmosphere (a) OM image of surface region (b) OM image of central region (c) FESEM image of central region (d) EDS elemental mapping of central region (e) EPMA elemental mapping of surface region (f) TEM image of central region (g) Electron diffraction patterns of TEM image above

regions are shown in Fig. 4 (a) and (b), respectively. Decarburisation white layers of 100 μm to 150 μm thickness near the surface region are still observed, implying that the annealing treatment cannot effectively eliminate this white layer.

EPMA mapping was also applied to confirm this phenomenon, in Fig. 4 (e), indicating lower carbon concentration in this decarburisation white layer.

As for the FESEM microstructure, the whole specimen is transformed

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Sintered

Annealed

Quenched

Cryogenic Treatment

Tempered

Central region

516

204

578

592

538

Surface region

351

158

647

663

622

Table 3 Hardness (Hv) of heat treated 420 W specimen

from a martensitic matrix to a α-ferrite matrix in this heat treatment condition, as shown in Fig. 4 (c) and (d), which also corresponds with the hardness result in Table 3,

since ferrite structure is soft and substantially low in hardness.

Intergranular compounds are still visible, and some small particles (less than 0.5 μm in size) are formed

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(a)

(b)

(c)

(d)

(e)

Fig. 4 Analysis of 420 W annealed state, based on annealing at 910°C for 2 hours at Ar atmosphere (a) OM image of surface region (b) OM image of central region (c) ESEM image of surface region (d) FESEM image of central region (e) EPMA elemental mapping of surface region

inside the grains, as shown in Fig. 4 (c) and (d).

After annealing, a subsequent austenisation and quenching heat treatment was applied. This hardening treatment, specified for martensitic stainless steels, typically consists of heating to a temperature high enough to ensure an FCC austenitic structure with carbon in solid solution, followed by rapid cooling (air cooling or oil quenching) to form martensite at room temperature. Air cooling of a fully austenitic structure usually produces full hardening in type 420, but oil quenching

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is utilised for larger sections to ensure complete transformation to martensite. An undesirable complication of type 420 is the tendency to retain austenite (RA) after quenching.

The presence of significant amounts of retained austenite reduces the as-quenched hardness of the alloy and may promote embrittlement, if fresh, untempered martensite forms during tempering.

Multiple tempering steps can be used to temper the fresh martensite, or cryogenic (sub-zero) treatment can be used to reduce the retained austenite content prior to tempering. For the

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quenched specimen prepared, the surface and central regions both have a martensite matrix structure with some particles, shown in Fig. 5 (a)-(c).

The surface cooling rate is higher than that of the central region during the quenching step; thus, this caused a relatively higher hardness at the surface, as indicated in Table 3.

Intergranular compounds seem to be dissolved in this state, due to the rapid cooling rate via oil quenching to suppress the formation of this compound. Moreover, small particles are still abundantly dispersed, due to the austenisation temperature of 1020°C possibly not being high enough to completely dissolve the particles in the austenite phase. Increasing the austenisation temperature typically enhances carbide dissolution and increases the solubility of alloying elements in the austenite, but also leads to grain coarsening and reduces the martensitic transformation, thereby increasing the volume fraction of retained austenite. The decarburisation white layer seems to be eliminated in this stage and the carbon concentration profile is uniform in EPMA mapping, shown in Fig. 5 (d). This is due to the heating to high temperature in austenisation step being able to provide sufficient energy and time for carbon to diffuse from the inner region (with higher concentration) to the carbon-deficient decarburisation white layer and, thus, in turn it makes the carbon concentration uniformly distributed across the whole specimen.

The precipitated particles are abundant in Nb and C, as shown in EDS mapping in Fig. 5 (e). In EBSD phase identification in Fig. 5 (f), BCT martensite matrix and NbC particles are the major microstructural features in the quenched state. BCT and BCC lattice structures are indistinguishable in EBSD due to their similar lattice constants, but BCC structure can be excluded on the basis of OM morphologies. A TEM image of martensite and its electron diffraction patterns are shown in Fig.5 (g) and (h), respectively and are consistent with EBSD results. The selected area ‘D’ in Fig. 5 (g) and (h)

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(a)

(b)

(c)

(d)

(e)

(f)

(g)

(h)

(i)

(j)

(k)

(l)

Fig. 5 Analysis of 420 W quenched state, based on oil quenching at 1020°C for 1 hour at Ar atmosphere (a) OM image of surface region (b) OM image of central region (c) FESEM image of surface region (d) EPMA elemental mapping of surface region (e) EDS elemental mapping of surface region (f) EBSD phase mapping of surface region (g) TEM image of central region (h) Electron diffraction patterns of TEM image selected area “D” (i) Electron diffraction patterns of TEM image selected area “DE circle” (j) TEM image (dark field image) of retained austenite in selected area “DE circle” (k) TEM image of small particles in selected area “M” (l) Electron diffraction patterns of TEM image selected area “M”

is a single martensite lath. Some retained austenite could be detected in Fig. 5 (i), as electron diffraction patterns of austenite, and Fig. 5 (j)

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TEM dark field image, respectively.

The DE circle indicates that the D and E two laths were simultaneously selected and analysed using selected

area diffraction. Retained austenite is normally observed within martensite laths. Particles with NbC structure were also verified, as shown in Fig. 5

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(a)

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(b)

(c)

(d)

(e)

(f)

(i)

(g)

(h)

(j)

Fig. 6 Analysis of 420 W cryogenic (sub-zero) treatment state, based on 1355°C sintering, graphite furnace, Ar atmosphere (a) OM image of surface region (b) OM image of central region (c) FESEM image of central region (d) EDS elemental mapping of central region (e) EBSD phase mapping of central region (f) EBSD image quality (IQ) maps of central region (g) BCC/BCT crystal orientation mapping of Fig. 6 (f) IQ maps (h) Boundaries with misorientation from 2° to 62° of Fig. 6 (f) IQ maps (i) TEM image of central region (j) Electron diffraction patterns of TEM image above

(k) and (l), also being consistent with EBSD results Fig. 5 (f).

The presence of retained austenite is problematic for many applications because, among other effects, it reduces the dimensional stability

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of steel components. The fraction of retained austenite should consequently be reduced as much as possible. Cryogenic treatment is the supplement for the conventional heat treatment process, in which materials

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are subjected to very low temperatures, to enhance the mechanical properties of the material being treated. This treatment is done after quenching and before the tempering of steel [45-46]. Various advantages,

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(a)

(b)

(c)

(d)

(e)

(f)

Fig. 7 Analysis of 420 W tempered state, based on 1355°C sintering, graphite furnace, Ar atmosphere (a) OM image of surface region (b) OM image of central region (c) FESEM image of central region (d) EDS elemental mapping of central region (e) TEM image of central region (f) Electron diffraction patterns of TEM image above

such as improved wear resistance, reduced residual stress, increase in hardness, dimensional stability, fatigue resistance, toughness by transformation of retained austenite into martensite and precipitation of ultrafine carbides [47-50] were noted. In this study, cryogenic treatment was conducted at -80°C for 2 hours to assist some retained austenite being further transformed to martensite. The morphologies from Fig. 6 (a)-(c) are almost similar to the images obtained from the quenched state, martensite as the major matrix with disperse NbC precipitates. Phase identification from EBSD phase mapping is shown in Fig. 6 (e) and reveals that a BCT martensite matrix and NbC precipitates are the major microstructural features in this condition. EBSD

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image quality (IQ) maps were shown in Fig. 6 (f) and these can clearly identify each martensites lath’s boundary.

Boundaries with misorientations from 2° to 62° are demonstrated in Fig. 6 (h) and, from this, the prior austenite grain (PAG) boundary could be clearly depicted by the red line. From TEM morphologies in Fig. 6 (i) and selected area ‘J1’ diffraction patterns in Fig. 6 (j), the structure was identified as martensite. The diffraction spots marked by the yellow and blue circles belonged to two martensite grains.

The last process in heat treatment is tempering. In the ‘as-quenched’ or ‘sub-zero treatment’ martensitic condition, the steel is hard and brittle and may contain pockets of retained austenite. Quenching is therefore followed by tempering to reduce brittleness, increase ductility/toughness

and reduce residual stresses.

The presence of residual stress could obviously be deleterious to the mechanical and corrosion properties. A good combination of toughness and strength is then achieved. In the case of type 420, tempering is performed at a low temperature (below 400°C).

Great care is taken to prevent the tempering process from taking place within the temperature range of 450°C to 600°C: this interval is considered critical as it reduces resistance to brittle fracture and significantly reduces corrosion resistance. The 200°C tempering treatment results from Fig. 7 are quite similar to the quenched and cryogenic treatment states in microstructure, a major phase of martensite and dispersed particles,

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(a)

(b)

(c)

(d)

(e)

C

N

Fe

Cr

Nb

Mo

Ni

Central region

12.40

26.99

1.82

2.19

56.60

0

0

Surface region

12.15

26.56

2.53

2.37

56.40

0

0

Table 4 EPMA quantitative analysis of the precipitated particles (at%)

since tempering at 200°C may not induce microstructural change, such as carbide coarsening or carbide precipitation. Only the stresses induced due to the hardening operation will be relieved via this low temperature 200°C tempering treatment.

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In general, graphite insulation is more likely to absorb moisture than metal insulation in furnace systems and this might be the potential root cause for the decarburisation occurring in previous discussion. Based on this, a molybdenum lined furnace was also used in this research for

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comparison. As shown in Fig. 8 (a) to (d), from surface to central regions are martensite matrice without the presence of a decarburisation layer. EBSD results in Fig. 8 (e) and (f) also confirmed the martensite BCT structure and the dispersed particles as being NbN. EBSD image quality (IQ) maps were shown in Fig. 8 (g), which can clearly identify each martensite lath’s boundary. Boundaries with misorientations from 2° to 62°are demonstrated in Fig. 8 (i) and, from this, the prior austenite grain (PAG) boundary could be clearly depicted

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MIM 420 martensitic stainless steel

(f)

(g)

(j)

(h)

(k)

(i)

(l)

Fig. 8 Analysis of 420 W sintered state, based on molybdenum line furnace in flowing nitrogen at 100kPa pressure, 1340°C for 3 hours (a) OM image of surface region (b) OM image of central region (c) FESEM image of surface region (d) FESEM image of central region (e) EBSD phase mapping of surface region (f) EBSD phase mapping of central region (g) EBSD image quality (IQ) maps of central region (h) BCC/BCT crystal orientation mapping of Fig. 8 (g) IQ maps (i) Boundaries with misorientation from 2° to 62° of Fig. 8 (g) IQ maps (j) TEM image of surface region (k) Electron diffraction patterns of TEM image above, selected area “R” (l) Electron diffraction patterns of TEM image above, selected area “Q”

by the red line. TEM images and diffraction patterns also verified the BCT martensite and NbN structure from Fig. 8 (j) to (l). The XRD analysis in Fig. 2 (b) implies martensite matrix as the major microstructure, which is consistent with OM, EBSD and TEM results aforementioned.

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EDS mapping results from Fig. 9 (a) and (b) revealed that the spherical particles are abundant in Nb, Cr and N. The carbon distribution in Fig. 9 (a) is uniform and none of the deficient (decarburisation) area is observed. EPMA mapping results from Fig. 10 (a) and (b) are

consistent with the EDS analysis results.

From Table 4, the EPMA quantitative analysis results also verified the precipitated particles as containing the major C, N, and Nb elements. Combining the results from XRD, EBSD and EPMA,

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the structures of the precipitated particles are ‘carbo-nitride’ based compound and the exact structure is Nb (C,N).

Table 5 shows that almost no N or Nb are detected in the martensitic matrix from the top to the bottom area of the sintered specimen, due to the low solubility of nitrogen in martensitic matrix.

Based on the results from Table 4 and Table 5, nitrogen atoms are effectively diffusing into the 420 W sintered sample, but most of nitrogen atoms are forming carbonitride Nb (C,N) particles, rather than dissolving in the martensitic matrix, owing to the limited solubility of nitrogen in martensite aforementioned. Also, Nb is a strong carbide and nitride former (with affinity towards nitrogen being higher than for Cr) [51]. Consequently, type 420 is able to keep an effective content of chromium in the matrix, which will be beneficial for corrosion resistance.

(a)

(b)

Discussion

Fig. 9 Analysis of 420 W in the sintered state, based on molybdenum line furnace in flowing nitrogen at 100kPa pressure, 1340°C for 3 hours (a) EDS elemental mapping of surface region (b) EDS elemental mapping of central region

C

N

Fe

Cr

Nb

Mo

Ni

Top

1.13

0

83.62

14.76

0.05

0.05

0.39

Bottom

1.13

0

84.36

14.23

0.03

0.06

0.19

Table 5 EPMA quantitative analysis of the martensitic matrix (at%)

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Decarburisation is recognised as the loss of carbon atoms from the surface of ferrous materials producing a carbon concentration gradient across a short distance below the surface. This is a serious problem as the weaker surface layer reduces wear resistance, enabling fatigue failures to occur more easily.

This occurs when carbon atoms at the ferrous material’s surface interact with the oxygen, metal oxide or moisture in the atmosphere when it is heated at 600°C or above, where the driving force is the carbon chemical potential across the material and the atmosphere [52–70].

Carbon from the interior diffuses towards the surface, moving from high to low concentration and continues until the maximum depth of decarburisation is established.

Concerning the loss of carbon in sintering, a continuous layer of soft ferrite is being produced together with ferrite formation around austenite grains and this ferrite

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(a)

(b)

Fig. 10 Analysis of 420 W in the sintered state, based on molybdenum line furnace in flowing nitrogen at 100 kPa pressure, 1340°C for 3 hours (a) EPMA elemental mapping of surface region (b) EPMA elemental mapping of central region

structure is maintained on cooling to room temperature due to insufficient hardenability (carbon is a key element inenhancing hardenability).

Apart from these areas, austenite will subsequently transform to a martensitic structure in the cooling stage. Hence, the final structure in the decarburisation layer is based on a ferrite and martensite mixed structure. In this work, decarburisation is obvious at the upper surface region in sintered specimen based on the graphite furnace system and this lead the hardness variance between the surface and central regions. In general, graphite insulation is more likely to absorb moisture than metal insulation and this could explain the presence of the decarburisation white layer in

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the graphite furnace system, but it’s not being observed in the metal furnace system.

The surface hardness in the as-sintered state is lower than the standard type 420 value, but can be improved via high temperature austenitisation diffusion in the heat treatment procedures, as shown in Table 3. Carbon atoms are thus distributed homogeneously from the central region to the upper surface.

During the austenitisation stage, an excess amount of carbon is dissolved and then cooled rapidly to form ‘supersaturation’ martensite.

This supersaturation martensite has a higher extent of lattice distortion, compared with the as-sintered state, and is revealed from the hardness variance in Table 3.

However, 420 W has quite a high carbon content and seems not to be easy to dissolve totally in the supersaturation state; hence, remaining undissolved carbon is precipitated in the form of NbC particles. In the subsequent cryogenic treatment, some remaining retained austenite (RA) is further transformed to martensite to enhance overall hardness, but the increment is limited due to the low RA volume fraction.

In the final step, tempering caused some degree of hardness reduction as expected, for improving ductility and toughness. For the morphologies from the quenched to the tempered state, the matrices are all martensite, differing only in hardness.

Upon furnace cooling after sintering, there will be sufficient time

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Composition (wt%): Fe-xC-13Cr-1.5Nb

L

1500

Temperature_Celsius

BCC+FCC+NbC 1250 FCC+NbC FCC+NbC+M7C3 1000 FCC_A1+NbC+M23C6

750

0.35

BCC+NbC+M23C6

0.40

0.45

0.50

Mass_Percent C

Fig. 11 Pseudo-binary phase diagram: Fe-Cr-Nb-C for the Nb-modified 420 alloy. See Table 6 for composition analysis

for diffusion to form compounds, especially near the grain boundary region, due to the lowest activation energy for forming compounds in this boundary. Hence, for slow cooling rates, having sufficient time during sintering, intergranular compounds are observed. The subsequent annealing state’s morphology revealed a similar

intergranular compound distribution to sintered state due to a similar slow cooling. However, in the subsequent quenched and cryogenic treatment state, those intergranular compounds are dissolved, due to the high cooling rate. From a mechanical point of view, intergranular compounds are deleterious to strength [71-80]

“From a mechanical point of view, intergranular compounds are injurious to strength [71-80] and, therefore, the dissolving of intergranular compounds via heat treatment in this study is beneficial to a specimen’s overall mechanical strength.”

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and, therefore, the dissolving of intergranular compounds via heat treatment in this study is beneficial to a specimen’s overall mechanical strength.

In this research, the MIM 420 powder composition is modified by adding niobium, to stabilise carbon via the forming of niobium carbide (graphite furnace system) and niobium carbo-nitride Nb(C,N) in the molybdenum lined furnace, which results in inhibiting the formation of chromium carbides, such as Cr23C6 and Cr7C3. These chromium carbides are well known to lead to the sensitization phenomenon. Consequently, type 420 is able to keep an effective content of chromium in the matrix, which will be beneficial for corrosion resistance.

Fig. 11 shows a pseudo-binary Fe-Cr-Nb-C phase diagram calculated by Thermo-Calc software for the Nb-modified 420 stainless steel.

From this diagram, it is predicted that the only stable carbide existing above 1000°C will be NbC and this prediction is entirely consistent with the XRD, EBSD and TEM results.

According to the simulated phase diagram, it can be inferred that NbC is a relatively stable carbide in the Nb-modified 420 stainless steel. Therefore, NbC particles can be clearly observed even after annealing at 910°C or oil quenching from 1020°C. Since thermodynamic simulation software is normally used to calculate various properties in an equilibrium state, the experimental results obtained for a non-equilibrium state did not coincide with those simulated with Thermo-Calc software [81].

Conclusions Martensitic stainless steel 420 samples were prepared using the MIM process. A graphite furnace and a molybdenum lined furnace were used for surface microstructure comparison and this study confirms that decarburisation occurred only in the graphite furnace system because of its relatively higher moisture

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content than the molybdenum lined furnace. Lower hardness and decarburisation of the ferrite layer near the surface region can be improved by subsequent heat treatment procedures via carbon diffusion.

In each stage of heat treatment, martensitic stainless steel 420 samples were also characterised by their SEM microstructure, EBSD phase mapping, and TEM electron diffraction to investigate the variation. The starting powder was based on niobium-modified type 420 and easily formed niobium carbide (NbC) in the graphite furnace and niobium carbonitride Nb(C,N) in the molybdenum lined furnace), which results in inhibiting the formation of chromium carbides, such as Cr23C6 and Cr7C3. These chromium carbides are well known to lead to the sensitisation phenomenon.

Consequently, type 420 is able to keep an effective content of chromium in the matrix, which is beneficial for corrosion resistance.

On the basis of the results obtained, this study achieved its proposed objectives, successfully investigating carburisation issues and indicating solutions to the decarburisation problems addressed, which are frequently encountered in the MIM industry. The heat treatment parameters in this study may not be fully applicable for all MIM cases due to feedstock chemistry, solid loading, tooling mould geometry, and dimension differences, but this absolutely provides a direction to refer.

NbC Composition Mole fraction

Mass fraction

Nb

0.51257

0.88581

C

0.48066

0.10739

Fe

0.00346

0.00359

Cr

0.00332

0.00321

Mo

6.67717E-13

1.19162E-12

Ni

5.19339E-13

5.66972E-13

Mn

5.19339E-13

5.30726E-13

Si

5.19339E-13

2.71324E-13

Mole fraction

Mass fraction

Cr

0.55641

0.71341

Fe

0.14359

0.19774

C

0.03000

0.08885

Nb

4.04503E-7

9.26697E-7

Mo

8.07344E-13

1.90999E-12

Ni

7.00000E-13

1.01306E-12

Mn

7.00000E-13

9.48294E-13

Si

7.00000E-13

4.84797E-13

Mole fraction

Mass fraction

Cr

0.62767

0.73571

Fe

0.16543

0.20827

C

0.20690

0.05602

Mo

2.11174E-11

4.56716E-11

Acknowledgements

Mn

1.47974E-12

1.83258E-12

Ni

7.93103E-13

1.04930E-12

The authors gratefully acknowledge Chenming Electronic Technology Corp. (UNEEC), and R&D centre colleagues, for sharing their pearls of wisdom during this research, assisting us at every point and without whom this task would not have been possible to accomplish.

The authors wish to express herein their gratitude to Zhang-Yi Huang, as well as to Run-Ming Mai (UNEEC Dongguan plant) for their valuable assistance in this research. The

Nb

0.00000E0

0.00000E0

Si

0.00000E0

0.00000E0

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Component

M7C3 Composition Component

M23C6 Composition Component

Table 6 Compositions of the Nb modified 420 alloy referenced in Fig. 11

authors would like to appreciate contributions from Martin Blömacher (BASF SE) and Allen Huang (BASF China), by supporting the molybdenum lined furnace sintering and sample preparation given to this

research. The authors would also like to express their appreciations to Professor Ming-Wei Wu, National Taipei University of Technology, for the Thermo-Calc software simulation in this research.

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Authors

J. Mater. Sci. Lett., 2003, vol. 22, pp.

1151–1153.

Shu-Hsu Hsieh; Dr. Chung-Huei Chueh; I-Shiuan Chen Chenming Electronic Technology Corp. (UNEEC), Taiwan DH_Hsieh@tw.uneec.com

[12] J.C. Ezechidelu, S.O. Enibe, D.O. Obikwelu, P.S. Nnamchi, C.S. Obayi: Int. J. Adv. Res. Sci. Eng. Technol.

(IJARSET)., 2016, vol. 3, no. 4, pp. 6–12.

Advanced Application R&D Dept., R&D Center Chenming Electronic Technology Corp. (UNEEC), 2F, No. 27, Sec. 6, Minquan E. Rd., Neihu Dist., Taipei City 114, Taiwan

[14] D.N. Collins, J. Dormer: Heat Treatment of Metals., 1997, no. 3

www.uneec.com

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For more information contact Jon Craxford, Advertising Sales Director Tel: +44 207 1939 749 jon@inovar-communications.com

MIM, CIM & AM parts producers

Metal powders

Ecrimesa Group

Advanced Technology & Materials Co., Ltd. 36

Indo-US MIM Tec Pvt Ltd

www.atmcn.com/english

Epson Atmix Corporation

13

Hunan Hualiu New Materials Co.,Ltd.

51

Jiangxi Yuean Superfine Metal Co Ltd

49

47

www.parmatech.com

Shanghai Future Group

www.hlpowder.com

45

www.indo-mim.com

Parmatech Corporation

www.atmix.co.jp

21

www.ecrimesa.es

43

www.future-sh.com

www.yueanmetal.com

KBM Advanced Materials, LLC

39

www.kbmadvanced.com/en

LD Metal Powders

53

www.ldpowder.com

Phoenix Scientific Industries Ltd

Powder atomisers Phoenix Scientific Industries Ltd

37

www.psiltd.co.uk

37

www.psiltd.co.uk

Sandvik Osprey Ltd

10

Binders & feedstocks

08

Advanced Metalworking Practices, LLC

www.materials.sandvik

Tekna Ultra Fine Powder Technology

17

www.ampmim.com

www.tekna.com

26

BASF SE

29

www.catamold.com

www.ultrafinepowder.com

KRAHN Ceramics GmbH

27

www.krahn-ceramics.com/en

Polymim GmbH

Tooling Erowa AG www.erowa.com

Vol. 15 No. 4 © 2021 Inovar Communications Ltd

54

www.polymim.com

24

Ryer Inc.

IFC

www.ryerinc.com

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123

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Furnaces & furnace supplies Centorr Vacuum Industries, Inc

Injection moulding machines 20

Arburg GmbH & Co. KG

OBC

www.arburg.com

www.vacuum-furnaces.com

CM Furnaces Inc.

25

www.cmfurnaces.com

Cremer Thermoprozessanlagen GmbH

15

www.cremer-polyfour.de

Elnik Systems

19

www.elnik.com

Kerafol GmbH & Co. KG

31

www.kerafol.com

Mut Advanced Heating GmbH

30

www.mut-jena.de

Ningbo Hiper Vacuum Technology Co Ltd

33

www.hiper.cn

Signature Vacuum Systems, Inc.

34

www.signaturevacuum.com

TAV Vacuum Furnaces SpA

Debinding systems Elnik Systems

19

www.elnik.com

LÖMI GmbH

35

www.loemi.com

Atmospheres & gas generation Nel ASA

14

www.nelhydrogen.com

55

www.tav-vacuumfurnaces.com

Tisoma GmbH

42

www.tisoma.de

AM technology 3D Systems Inc.

06

www.3dsystems.com

Digital Metal® 22

HIP systems & services Cremer Thermoprozessanlagen GmbH

www.digitalmetal.tech

15

www.cremer-polyfour.de

The ExOne Company

04

www.exone.com

Alphabetical index

124

20th Plansee Seminar.............................................. 74

Ecrimesa Group ...................................................... 21

3D Systems, Inc....................................................... 06

Elnik Systems ......................................................... 19

Advanced Metalworking Practices, LLC................. 17

Epson Atmix Corporation ...................................... 13

Advanced Technology & Materials Co., Ltd. ......... 36

Erowa AG ................................................................. 24

Arburg GmbH & Co. KG........................................OBC

Foshan Genyilong Technology Co., Ltd. ................. 57

BASF SE .................................................................. 29

Hunan Hualiu New Materials Co.,Ltd. ................... 51

Centorr Vacuum Industries, Inc ............................ 20

Indo-US MIM Tec Pvt Ltd ....................................... 45

CM Furnaces Inc. ................................................... 25

Jiangxi Yuean Superfine Metal Co Ltd .................. 49

Cremer Thermoprozessanlagen GmbH ................ 15

KBM Advanced Materials, LLC............................... 39

Digital Metal® ......................................................... 22

Kerafol GmbH & Co. KG.......................................... 31

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Feedstock mixers Foshan Genyilong Technology Co., Ltd.

57

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Winkworth Machinery Ltd

The Barnes Global Advisors

41

60

www.barnesglobaladvisors.com

Wohlers Associates

59

www.wohlersassociates.com

For more information contact Jon Craxford, Advertising Sales Director Tel: +44 207 1939 749 jon@inovar-communications.com

Events 20th Plansee Seminar

Available in both digital and print formats, PIM International is the perfect platform to promote your company to a global audience.

74

www.plansee-seminar.com

MIM2022

82

www.mim2022.org

PM China 2022

96

www.pmexchina.com

PowderMet2022 / AMPM2022

104

www.powdermet2022.org / www.ampm2022.org

RAPID + TCT

62

www.rapid3devent.com

World PM2022

IBC

www.worldpm2022.com

KRAHN Ceramics GmbH......................................... 27

Ryer Inc. .................................................................IFC

LD Metal Powders................................................... 53

Sandvik Osprey Ltd ................................................ 10

LÖMI GmbH ............................................................ 35

Shanghai Future Group ......................................... 43

MIM2022 .................................................................. 82

Signature Vacuum Systems, Inc. .......................... 34

Mut Advanced Heating GmbH ................................ 30

TAV Vacuum Furnaces SpA .................................... 55

Nel ASA ................................................................... 14

Tekna ....................................................................... 08

Ningbo Hiper Vacuum Technology Co Ltd ............. 33

The Barnes Global Advisors.................................... 60

Parmatech Corporation ......................................... 47

The ExOne Company............................................... 04

Phoenix Scientific Industries Ltd ........................... 37

Tisoma GmbH ......................................................... 42

PM China 2022 ........................................................ 96

Ultra Fine Powder Technology ............................... 26

PolyMIM GmbH ....................................................... 54

Winkworth Machinery Ltd ...................................... 41

PowderMet2022 / AMPM2022 .............................. 104

Wohlers Associates................................................. 59

RAPID + TCT. ........................................................... 62

World PM2022 ....................................................... IBC

Vol. 15 No. 4 © 2021 Inovar Communications Ltd

December 2021 PIM International

125

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Industry events PIM International is dedicated to driving awareness and development of MIM, CIM and sinter-based AM industries and its related technologies. Key to this aim is our support of a range of international partner conferences. View our complete events listing on www.pim-international.com

2022 MIM2022 February 21–23, 2022 West Palm Beach, FL, USA www.mim2022.org

20th Plansee Seminar May 30–June 3, 2022 Plansee Group, Reutte, Austria www.plansee-seminar.com

Asiamold March 3–5, 2022 Guangzhou, China www.asiamold-china.cn.messefrankfurt.com

PowderMet2022 / AMPM2022 June 12–15, 2022 Portland, OR, USA www.powdermet2022.org / www.ampm2022.org

6th Additive Manufacturing Forum Berlin 2022 March 14–15, 2022 Berlin, Germany www.am-forum.eu

EPHJ Trade Show June 14–17, 2022 Geneva, Switzerland www.ephj.ch/en

Hannover Messe 2022 April 25–29, 2022 Hannover, Germany www.hannovermesse.de

Ceramitec 2022 June 21–24, 2022 Munich, Germany www.ceramitec.com

RAPID + TCT 2022 May 17–19, 2022 Detroit, MI, USA www.rapid3devent.com

EPMA Powder Metallurgy Summer School June 20–24, 2022 Ciudad Real, Spain www.summerschool.epma.com

PM China 2022 May 23–25, 2022 Shanghai, China www.pmexchina.com

Ceramics Expo 2022 August 29–31, 2022 Cleveland, OH, USA www.ceramicsexpousa.com PMTi2022 August 29–31, 2022 Montréal, Canada www.pmti2022.org

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13th International Conference on Hot Isostatic Pressing September 11–14, 2022 Columbus, OH, USA www.hip2022.com World PM2022 October 9–13, 2022 Lyon, France www.worldpm2022.com

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9- 13 OCTOBER 2022 LYON - FRANCE

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