Services for Industry by Loughborough University

LOUGHBOROUGH MATERIALS CHARACTERISATION CENTRE SERVICES FOR INDUSTRY

SERVICES FOR INDUSTRY

LOUGHBOROUGH MATERIALS CHARACTERISATION CENTRE SERVICES FOR INDUSTRY

WELCOME Loughborough Materials Characterisation Centre (LMCC) is a facility within the Department of Materials at Loughborough University that contains state-of-the-art characterisation instruments. The centre currently contains over £7.5m of equipment, which can be used to characterise metals, ceramics and polymers. One of the centre’s key aims is to support industry by providing consultancy services and contract research. The facilities are supported by an experienced team of specialists.

LOUGHBOROUGH MATERIALS CHARACTERISATION CENTRE SERVICES FOR INDUSTRY

OUR VISION The centre has been carrying out consultancy for external businesses since the centre was formed in 2001. Over this time, we have increased the amount of external consultancy which we carry out. We continue to work with some of the most prestigious global engineering companies. LMCC has a different ethos to a commercial business which directly benefits all our clients in the long term. All income generated from carrying out external consultancy is re-invested directly back into the centre. This allows the centre to keep equipment operational and invest in new state of the art instrumentation to ensure we continue to have world class facilities.

LOUGHBOROUGH MATERIALS CHARACTERISATION CENTRE SERVICES FOR INDUSTRY

OUR BESPOKE APPROACH We understand that every project is different and clients have different approaches. LMCC is very flexible and our approach can be tailored to your requirements. We have three key approaches of how you can interact with LMCC.

LOUGHBOROUGH MATERIALS CHARACTERISATION CENTRE SERVICES FOR INDUSTRY

— “The flexibility which LMCC have provided us within a large R&D project has been integral to the success of the project.” — Joe Bloggs Company A.

BESPOKE CONSULTANCY LMCC has a wealth of experience in carrying out bespoke consultancy for clients to solve real world engineering challenges. We can provide an initial assessment of the specific problem and give suggestions on what may be the most suitable technique(s) to solve your problem. We can supply a complete package from start to finish, where the start can consist of extracting samples, all the way through to interpreting data with full project management and a final report. Alternatively, a client may have a clear vision of which techniques should be used and request that we simply generate the data and provide that data for them to interpret.

PAY AS YOU GO

E-STORE

We have a number of clients who are very experienced in using the techniques available within LMCC, but would like access to the latest equipment without having to invest in the latest models themselves.

LMCC has an online store to help clients who would like a taster of the services which LMCC can provide.

For these clients the equipment is available on a ‘pay as you go’ basis where we charge for hours used. We provide initial training to the client, but staff will be available at all times to provide guidance or help solve specific problems if required. Once the client is trained they can check instrument availability and book through our central booking system 24 hours a day.

If you have a relatively simple task to carry out you can contact LMCC to discuss which technique would be the most appropriate to use. You can then purchase time on the equipment using a debit or credit card. When making the booking you will be able to request a date and a member of LMCC will then contact you to confirm the session. You can attend the session in person or post samples to us. At the end of the session we will provide you with results on a USB memory stick or we can email them to you as per your preference.

— “I have used the LMCC facilities for many years. The service provided is excellent in terms of equipment, speed of sample turnaround, and the flexibility and expertise of their staff. Data provided has been critical to the success of our projects and I am most grateful for such a rich and highly effective collaboration.” — Phil Jinks Senior Research Specialist, 3M 05

LOUGHBOROUGH MATERIALS CHARACTERISATION CENTRE SERVICES FOR INDUSTRY

THE CENTREâ&#x20AC;&#x2122;S CAPABILITY LMCC contains a diverse range of characterisation equipment which can be used by external businesses. The facilities are supported by an experienced team of specialists who ensure the equipment is producing optimum results. The highly qualified staff in the centre are an integral part of our ability to deliver high quality consultancy.

ELECTRON MICROSCOPY LMCC houses a wide range of electron microscopes from a tabletop SEM through to high resolution STEM analysis. The centre is continually investing in new state-of-the-art equipment. These instruments are operated and maintained by an experienced team who enable students, researchers and external businesses to make the best use of the facilities. A range of analytical methods such as EDS and EBSD are available for use.

LOUGHBOROUGH MATERIALS CHARACTERISATION CENTRE SERVICES FOR INDUSTRY

SURFACE ANALYSIS The centre has a range of surface analysis instrumentation available. LMCC has recently upgraded its XPS to enhance its surface characterisation capability.

OPTICAL MICROSCOPY LMCC has an optical microscopy suite which contains a variety of instruments which are available for the optical examination of materials. These range from low power stereo zoom microscopes to high power reflected and transmitted light instruments. 07

LOUGHBOROUGH MATERIALS CHARACTERISATION CENTRE SERVICES FOR INDUSTRY

THERMAL ANALYSIS LMCC has a wealth of experience in thermal analysis. We have the capability to carry out thermal analysis on a range of instruments from a quenching and deformation dilatometer to DSC.

LOUGHBOROUGH MATERIALS CHARACTERISATION CENTRE SERVICES FOR INDUSTRY

MECHANICAL TESTING LMCC has recently invested in an automated micro hardness testing machine to enhance its materials characterisation capability. The system facilitates new research to be conducted in areas such as weld development for power generation steels. The system provides the capability to conduct hardness testing on large areas.

X-RAY DIFFRACTION LMCC has X-Ray Diffraction which is a complimentary technique to our electron microscopy based techniques. Powder X-ray Diffraction can be used to both confirm compound identity and determine if there are crystalline impurities present. The facilities available in LMCC are also capable of analysing solid samples.

LOUGHBOROUGH MATERIALS CHARACTERISATION CENTRE SERVICES FOR INDUSTRY

FOCUSED ION BEAM The Focused Ion Beam (FIB) allows site specific removal of material providing us with the capability to understand how materials and features within the microstructure are interconnected by producing 3D reconstructions of materials. The systems are extremely versatile.

10µm

The FIB is also an important tool when characterising materials which are difficult to prepare using conventional methods. For example; materials with a loose surface layer or cross sections of fabrics. The FIB can be used to produce cross sections through the sample and then carry out subsequent imaging using either electrons or ions.

The FIB allows site specific removal of material; this capability allows site specific TEM samples which are electron transparent (<150 nm) to be produced.

500µm

5µm

LOUGHBOROUGH MATERIALS CHARACTERISATION CENTRE SERVICES FOR INDUSTRY

LMCC has recently been successful in obtaining a grant of £1.2M from EPSRC for a state-of-the-art plasma FIB. This system has many advantages: • Significantly larger cross sections to be produced more rapidly enabling routine characterisation of delicate oxides. • The ability to produce gallium free TEM samples. • The system provides the capability to heat samples up to 1200°C and observe the microstructural change in real time. • The PFIB has state-of-the-art analytical equipment which enables 3D reconstructions to be carried out by industrial clients to solve real world production challenges.

The FIB allows materials to be viewed in 3D. The advantage of this is that real shapes and sizes of grains or precipitated phases can be observed. In addition to this, the connectivity of features within the microstructure can be observed, which finally allows researchers to fully characterise materials with asymmetrical and inhomogeneous microstructures.

Our FIB’s are equipped with a micro manipulator that allows micro bend, torsion and tensile tests to be undertaken on ion milled or as manufactured bulk materials. This allows us to quantify the mechanical properties of specific features within the microstructure at a nano level. 11

LOUGHBOROUGH MATERIALS CHARACTERISATION CENTRE SERVICES FOR INDUSTRY

TRANSMISSION ELECTRON MICROSCOPY Transmission electron microscopy (TEM) is typically perceived as an academic technique. All our transmission electron microscopes are available to industry. The systems are supported by a team of specialists who are experienced in preparing high quality samples and have a wealth of experience in optimising the TEM to ensure optimum results are supplied. All the systems are equipped with Energy-Dispersive X-ray Spectroscopy (EDS) detectors to enable chemical composition mapping of specific features. Selected area diffraction analysis can be utilised to help identify unknown phases.

Typical Industrial Applications • Coating Thickness Measurements • Oxide Thickness Measurements • Examination of materials at the atomic level • Characterisation and quantification of precipitates

2nm

Atomic resolved image of stacking faults in a CdTe solar cell prepared using a Focused Ion Beam.

2nm

High resolution image of a multi walled carbon nanotube.

LOUGHBOROUGH MATERIALS CHARACTERISATION CENTRE SERVICES FOR INDUSTRY

SCANNING ELECTRON MICROSCOPY LMCC houses a wide range of scanning electron microscopes from a tabletop scanning electron microscope (SEM) through to multiple high resolution Field Emission Gun Scanning Electron Microscopes (FEGSEMs). A SEM is an indispensable tool for solving industrial material challenges.

Our systems offer the capability for large-scale EBSD maps to be acquired. The maps show localised deformation in a bent aluminium alloy used for automotive crash protection.

10Âµm

Our latest FEGSEMs have state-of-the-art backscatter detectors which provides excellent Z contrast and channelling contrast in the images.

LOUGHBOROUGH MATERIALS CHARACTERISATION CENTRE SERVICES FOR INDUSTRY

LMCC has recently invested in two state-of-the-art FEGSEM’s to enhance the Centres capability and capacity. Typical Industrial Applications • High resolution surface topography images • Elemental microanalysis and particle characterisation • Precipitate particle size analysis • Defect Identification • Texture Mapping

A wealth of data can be obtained from EBSD. The map below (A) shows the inverse pole figure and (B) shows the band contrast map in addition to the low angle (blue) and high angle (black) grain boundaries.

B 2.5μm

Automated inclusion analysis can be performed by using a backscatter detector and high speed EDS detector. 15

LOUGHBOROUGH MATERIALS CHARACTERISATION CENTRE SERVICES FOR INDUSTRY

— “I have returned regularly for contract XPS analysis at LMCC. Their XPS capability allows me to collect data from discrete regions, 50µm in diameter, which was unachievable elsewhere. Access to the instrument is quick and I am always welcomed with flexibility, out of the box thinking and good humour! The extra value from Loughborough is the follow-up support, assistance and expert advice.” — Jon Barker Senior Analysis and Development Engineer, Xaar

LOUGHBOROUGH MATERIALS CHARACTERISATION CENTRE SERVICES FOR INDUSTRY

SURFACE ANALYSIS LMCC has an X-ray Photoelectron Spectroscopy (XPS). XPS is a surface sensitive technique which provides compositional and chemical state information on the top 3-10 nm of the material. XPS can be used to analyse both powder and solid samples, including metals, ceramics and polymers. XPS provides the capability to carry out depth profiling using an argon ion beam. This technology is vital for producing a multi layered depth profile. It provides the ability to measure changes in the oxidation state and composition of elements as a function of depth. Angle resolved XPS can be carried out to provide the order of individual layers.

Typical Industrial Applications • Within industry, unknown surface contaminants can be the cause of adhesion failures. XPS can be used to identify the contamination quickly and accurately. • The system can be used to determine the thickness of the oxide layer present on stainless steel. • Identification of the thickness and composition of multi-layered coatings. Modern photovoltaic cells have thin films of CdTe and CdS. These layers can be deposited using a number of different methods, which lead to different structural and chemical properties of the individual layers. The TEM can be used to characterise the structure of the individual layers. XPS can be used as an alternative to producing a site specific TEM sample and carrying out EDS. The advantage of this technique is that a larger area can be sampled.

Atomic Percent Depth Profile 80

Atomic Percent %

500

1. CdTe (750 nm) 2. CdS (200 nm)

1000

1500

2000

3. F:SnO (400 nm) 4. Glass

A depth profile of a CdTe solar cell. The profile was produced using an XPS to show the individual layers.

1µm

A TEM micrograph of the individual layers in a CdTe solar cell, the sample was prepared using a Focused Ion Beam. 17

LOUGHBOROUGH MATERIALS CHARACTERISATION CENTRE SERVICES FOR INDUSTRY

MECHANICAL TESTING LMCC offers the capability to carry out automated hardness testing in-house. Hardness testing is a routine test which is used in industry, usually as part of a quality control system, to ensure a consistent product is being manufactured. We have an extremely strong working partnership with a number of industrial partners who can provide sectioning of large components, mechanical testing and NDE testing.

Historically, hardness testing has always been a manual process. Our automated hardness tester allows maps to be produced from large areas which can have several thousand indents.

LOUGHBOROUGH MATERIALS CHARACTERISATION CENTRE SERVICES FOR INDUSTRY

LMCC also has the capability to quantify the chemical composition of the same area that has been hardness tested. The chemical composition can be quantified using a micro X-ray fluorescence (µXRF). This allows a relationship between the chemical composition and the hardness to be developed.

Ni kα

Mo kα

1mm

LOUGHBOROUGH MATERIALS CHARACTERISATION CENTRE SERVICES FOR INDUSTRY

MICRO X-RAY FLUORESCENCE Energy-dispersive X-ray spectroscopy (EDS) is one of the most common methods for producing chemical composition maps on the micro scale. Micro XRF provides the unique capability of producing chemical maps of large samples. Typical Industrial Applications • Coating Thickness Measurements • Elemental Mapping of Large Samples • Analysis of Wet / Dirty Samples

The chemical map on the right shows the iron map from a HP modified 25Cr steel with a multi pass weld. 20

LOUGHBOROUGH MATERIALS CHARACTERISATION CENTRE SERVICES FOR INDUSTRY

THERMAL ANALYSIS Thermal analysis is widely used to study the effect of changes in temperature on materials. These techniques can be used for compositional analysis, investigation of processing history, softening and melting temperatures, cure characterisation and thermal stability as well as providing basic engineering data.

Facilities • Quenching and deformation dilatometer • Thermogravimetry (TGA) • Thermomechanical analysis (TMA) • Differential Scanning Calorimetry (DSC) • High Temperature DSC to 1400°C • Dynamic mechanical analysis (DMA) • Micro-thermal analysis (µ-TA) • Simultaneous TG-DTA up to 1500°C

LOUGHBOROUGH MATERIALS CHARACTERISATION CENTRE SERVICES FOR INDUSTRY

SHORT COURSE

ELECTRON MICROSCOPY AND ANALYTICAL TECHNIQUES LMCC host an annual course into electron microscopy and its associated analytical techniques.

This is an intensive course taught over a three-day period consisting of lectures, industrial case studies and a significant amount of hands on practical sessions (50%).

This course is designed for people from industry who wish to gain a broad understanding into electron microscopy and understand how it can be applied to solve industrial material challenges.

The course runs annually. To find out more information about the course and how to register please visit www.lboro.ac.uk/lmcc

CONTACT US If you would like a quotation for your project please get in touch with Scott or Ryan who will be more than happy to assist you. General enquires E: lmcc@lboro.ac.uk

External enquiries and quotations Dr Ryan MacLachlan T: +44 (0)1509 228574 E: r.c.maclachlan@lboro.ac.uk

www.lboro.ac.uk/lmcc

@lborouniversity /lborouniversity /lborouniversity /lborouniversity

71380/CPS/Mar18

Director Scott Doak T: +44 (0)1509 223314 E: s.s.doak@lboro.ac.uk