Lead Oxide Manufacturing debate - featuring Penox's Mr David Hardy

Issue 119

Spring 2021

A matter of judgement

The great Barton Pot, Ball mill debate: is a better PbO worth the extra cost?

Getting to grips with the latest advances in carbon Why every battery generation reckon they're the smartest

The drive is on to create an international battery passport IAL Potential bonanza for lead as T TEN O global storage rebalances NP

Bringing the industry together

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IUM H LIT

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COVER STORY: LEADY OXIDE MANUFACTURING

The pros and cons of making lead oxide Barton Pot versus Ball mill Which process — the Barton Pot or the Ball mill — is the more efficient way of manufacturing leady oxide? In North America, Barton Pot is preferred, in Europe it’s Ball mill. But it’s more than just a balance between cost and quality.

Lead oxide production is one of the basic building blocks in manufacturing lead acid batteries. A good oxide makes a good battery — it’s as simple as that. But it’s also as complex as what function that battery will be charged to do.

The two main lead oxide production methods are the Ball mill and the Barton Pot processes. Each involves the production of lead oxide (PbO) mixed with unoxidized lead.

56 • Batteries International • Spring 2021

The mix of lead oxide and this unoxidized lead is called leady oxide.

The Barton Pot process involves the oxidation of molten lead, whereas the Ball mill process involves the oxidation of solid lead.

At its simplest, the Barton process, produces leady oxide by feeding molten lead into a pot and vigorously agitating it to break the lead into small droplets. Oxygen from a stream of air oxidizes a certain amount of the

lead into a mixture of yellow lead, red litharge and metallic lead.

Both yellow lead and red litharge are PbO but have different crystalline properties.

In the Ball mill process, leady oxide is produced by placing high-purity lead slugs in a rotating Ball mill, the friction within which generates heat, while a forced flow of air provides oxygen.

This results in particles of litharge and some unoxidized metallic lead.

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COVER STORY: LEADY OXIDE MANUFACTURING LEAD OXIDES • α-PbO known as litharge The crystalline shape is tetragonal. This shape is important in the pasting process in defining the output of the finished battery.

The colour is red, but not to be confused with red lead (below)

At its most basic comparison, the Barton Pot method is more productive, while the leady oxide produced by the Ball Mill method is more reactive.

• β-PbO known as massicot.

The crystalline shape is orthorhombic. The colour is yellow.

• Pb3O4 known as red lead or minium though it can have an orange hue to it.

• Leady oxide, this is when PbO is mixed with a proportion of lead

Comparison of Barton Pot and Ball mill oxides Characteristic

Barton Pot

Ball mill

Particle size

3mm–4mm median diameter

2mm–3mm median diameter

Stability/reactivity in air

Generally more stable

Generally high. Can cause storage and longdistance transport problems

Oxide crystal structures (wt%)

5–30% β−PbO (typ.), remaining balance α-PbO

Essentially 100% α-PbO

Acid absorption (in mg H2SO4 g−1oxide)

160–200 (unmilled, up to 240 with hammer milling)

240

Surface area (m2 g−1)

0.4–1.8

2.0–3.0

Free lead content (wt%)

Approx. 18–28

Approx. 25–35

Paste mixing characteristics

Makes a softer paste that can result in easier pasting

Makes a slightly stiffer paste that can require careful control

Battery performance

Enhances battery life, but can result in lower initial capacity

Batteries have good initial capacity, but possibly shorter life

Process control

Can be more difficult, but recent computer controls are helping

Easier, more consistent oxide

Typical production rate (kg h−1)

300–900

Possibly up to 1000

Investment considerations

Lower initial and operating costs; compact in size; relatively quiet; costs less to maintain; uses less energy to run

Higher initial and operating costs; requires more space; noisy; costlier to maintain

Energy use (kWh t−1)

Up to 100

100–300

Environmental aspects

With well-engineered environmental systems (including baghouse and storage), existing emissions standards can normally be met

Sources: Lead-Acid Batteries (Science and Technology) 2017, Detchko Pavlov and Journal of Power Sources 59, 1996 Michael Mayer, David Rand

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Batteries International • Spring 2021 • 57

COVER STORY: LEADY OXIDE MANUFACTURING

“Barton Pot is most appropriate for cells/ batteries requiring a tetrabasic plate cure, Barton Pot oxide has a significant fraction of orthorhombic lead oxide (β-PbO) which is favoured for tetrabasic cured plates” Roz Batson, chief executive at Clearsci-labs

The Barton Pot and Ball mill lead oxide processes have their own advantages and disadvantages, but for reasons — sometimes still unclear even to those in the market — the Barton Pot is more common in North America while Ball mill is preferred in Europe. Some firms, such as Exide Technologies, use both methods for making lead oxide.

At its most basic comparison, the Barton Pot method is more productive, while the leady oxide produced by the Ball mill method is more reactive.

Although both types are suitable for automotive batteries, many European and Japanese companies favour Ball mill oxide for deep-cycle batteries, whereas in North America Barton Pot is preferred.

“Habit may be a determining factor rather than practicality in some cases,” says one commentator. “Costs are a consideration but, once committed to a system, changing processes would be very expensive as this would entail replacing more than the process itself.”

Differences The differences and relative merits of Barton Pot versus Ball mill leady oxide depend on the user, says Roz Batson, chief executive at Clearsci-

THE POWERFUL USE OF ADDITIVES The basic leady oxide performance can also be enhanced by additives to the positive and negative pastes.

PENOX’s Hardy says: “Such additives focus on improving the crystal structure, paste porosity and finally the electrochemical performance of the active masses — PENOX tetra-basic additives TBLS+ is an example of such an additive. Much work is also taking place on expander formulations for the negative paste to enhance the performance. Again, PENOX has a range of specific expander recipes dependent on the application.

“All this being said, there is still more to be done with the leady oxide itself — a tightening of the current specification ranges is a given but there is also an additional focus on the influence of the PbO crystal modification and the particle size distribution.

“This leads to the concept of modifying the basic oxides — this

58 • Batteries International • Spring 2021

can be via microscopic coating with additives to further enhance the technical performance. An example of this is PENOX Red Lead+, a red lead oxide coated on a particulate level with a tetra-basic sulphate seeding additive. In this way, the tetra-basic seeding crystal distribution within the red lead is very homogenous rather than relying on the (at times) poor macro-mixing in many paste mixers.”

Hardy says that for Barton/P20 processes, the key challenges are to allow for operation and the rapid transition between different final oxide characteristics — varying the particle size, the tamped density, the alpha-beta PbO ratio as required for specific lead battery production.

“All of this has to be achieved while maintaining a highly energy efficient process meeting the latest standards for operator safety and environmental performance.”

labs. Clear Science is a Minneapolis laboratory specializing in the testing, research and development of metals, powders, porous materials, coatings, and advanced materials.

“Barton Pot systems generally require lower initial investment and lower energy to operate. However, ongoing process control is more delicate with Barton Pot,” says Batson.

Ultimately, the relative merits depend on the downstream manufacturing processes (mixing, pasting, curing, formation) and the type of service the cells/batteries will see be they automotive, deep cycling, or float and the like.

Logistics factor in as well, because Ball mill oxide is more reactive and is therefore more difficult to transport long distances.

Barton Pot is most appropriate for cells/batteries requiring a tetrabasic plate cure, says Batson. “Barton Pot oxide has a significant fraction of orthorhombic lead oxide (β-PbO) which is favoured for tetrabasic cured plates.

Ball mill oxide has almost no β-PbO. Its oxide fraction consists of tetragonal lead oxide (α-PbO) which results in a tribasic plate cure.”

Joe McKinley, owner at Eagle Oxide Services, says Ball mill is more costly to set up and more expensive to run in operational terms. There are also oxide characteristic differences. “Ball mill oxide tends to be more reactive than Barton oxide,” he says.

“Many automotive battery manufacturers lean towards using Ball mill oxide in the automobile starting batteries. The high reactivity of the Ball mill oxide tends to give a higher cold cranking amp rating.

“Barton oxide, having a lower reactivity and larger, more dense particles, can be favoured by non-automotive batteries, (forklift, UPS, long-cycle and multiple-cycle batteries, AGM)

“Habit may be a determining factor rather than practicality in some cases. “Costs are a consideration but, once committed to a system, changing processes would be very expensive as this would entail replacing more than the process itself.” www.batteriesinternational.com

COVER STORY: LEADY OXIDE MANUFACTURING IN-HOUSE MANUFACTURING OR SUPPLY DRIVEN?

“Barton oxide, having a lower reactivity and larger, more dense particles, can be favoured by non-automotive batteries, (forklift, UPS, long-cycle and multiple-cycle batteries, AGM) because the life of the batteries tends to last longer with these characteristics of Barton oxide” — Joe McKinley, owner at Eagle Oxide Services because the life of the batteries tends to last longer with these characteristics of Barton oxide.”

Meanwhile some battery manufacturers use both technologies and produce Barton oxide for the negative plates, and Ball mill oxide for the positive plates, or vice versa).

Barton oxide manufacturing can be enhanced by adding a hammer mill after the Barton oxide system that reduces the particle size and increase the acid absorption of Barton oxide, making it similar in action to Ball mill oxide.

This tends to have very small, flake like particles, which gives a high surface area which leads to generally higher acid absorption characteristics for Ball mill oxide compared with Barton oxide. Barton oxide particles tend to be larger and more spherical, which tends to give high apparent density characteristics for Barton oxide.

“Ball mill oxide tends to have all α-PbO crystal structure, being formed at low temperatures. Barton oxide typ-

60 • Batteries International • Spring 2021

Batson says that leady oxide is the most critical starting component for lead acid battery manufacture.

Physical characteristics of leady oxide must be matched correctly to the downstream processes and to the final service application.

“Manufacturers typically have leady oxide characteristics finely tuned to their specific processes.

There is great reluctance to change oxide because it is expensive and time-consuming to confirm good performance after making a change.

“I would assume that battery manufacturers would be incorporating oxide manufacture on-site because they want more control of this critical component.

They may see a cost-benefit in not shipping and in self-certifying their material. Also, there may be a large population of oxide manufacturing systems that are simply aging out of service at the same time and replacements are being installed.”

McKinley says that oxide production, in either form, is a critical process to battery manufacturers.

“They must have lead oxide in some form. In the US and Europe, and a few other countries, a battery manufacturer can purchase lead oxide from lead oxide manufacturers, having it shipped to the battery factory in trucks or bags. Where lead oxide manufacturers are not readily available, the battery factory must have some oxide production equipment in the factory. Most battery factories around the world produce lead oxide in their factory.

“There’s also a difficulty in changing processes. Battery factories that have historically used one oxide or the other, have their downstream processes (pasting, curing, formation) all set up for using that type of oxide and its given characteristics. Changing from one oxide to the other

would require changes to those downstream processes in order to be successful.”

PENOX’s Hardy says that leady oxide production has traditionally been part of the battery manufacturing process — the basic manufacturing process for leady oxide is relatively simple, transport of lead oxide (hazardous material) can be expensive with a lot of administration. Maintaining a leady oxide production capacity to meet the average demand is standard in most lead-acid battery production sites. Where there are peaks in demand or breakdowns then third party suppliers can offer a supply service.

Given that leady oxide accounts for the majority of the active mass (positive and negative plates) for most lead-acid batteries then the control of this material is key to the performance and costs of the battery manufacturer.

Hardy says the performance of lead-acid batteries in each application area become more demanding (reduced weight and costs, greater life-cycle under more varied operational chargedischarge profiles — so the focus on the performance of the active mass (positive and negative) has increased.

“In addition to the leady oxides produced in Barton and Ball mill processes, especially red lead (Pb3O4) and at times litharge, are used to improve the cycling and charge-discharge performance.

“Both red lead and litharge are produced in a two-step oxidation processes that require more specialized production equipment and infrastructure. For the vast majority of lead acid battery manufacturers, such secondary oxidation processes do not make economic sense. Traditionally, such oxides are delivered by specialized oxide producers such as PENOX.”

Given that leady oxide accounts for the majority of the active mass (positive and negative plates) for most lead-acid batteries then the control of this material is key to the performance and costs of the battery manufacturer. www.batteriesinternational.com

COVER STORY: LEADY OXIDE MANUFACTURING ically has a ratio of alpha and β-PbO crystal structures throughout its particles. Barton oxide tends to make a better paste for grid-adhesion,” says McKinley.

David Hardy, chief technology officer of PENOX says that because a mill oxide is produced via an abrasion process, the oxide is much finer than for a Barton oxide: “mill oxide has a

The Barton process offers more flexibility in terms of the oxidation level as well as the product fineness.

Dependent upon the process used for producing the lead cylinders or chips, then a mill oxide in general has a higher specific energy consumption than a Barton oxide.

1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17

Exhaust stack

Pb Ingots Ingot Crane Ingot Dosing Lead Melter Lead Cylinder Casting Machine Elevator For Lead Cylinders Lead Cylinder Storage Bunker Water Injection Oxide Mill Temperature Measurement Sound Proofing Filter Secondary Filter Main ventilator Silencer Transport Equipment Final Product Storage

15

17

12

14 16

13 16 Local Ventilation

1

7

6

2

11 10

3

9

5

4

8

Schematic of a Mill Oxide Process

Schematic of the Ball mill process

1 2 3 4 5 6

Pb Ingot Conveyor Lead Melter Lead Dosing Process Air Inlet Reactor Stirrer Drive System

7 8 9 10 11

Pre-Separator Cyclone Filter Main Ventilator Oxide Product

7 1

4 2

6

3

Schematic representation of the Barton Process For the Oxidation of Liquid Lead

62 • Batteries International • Spring 2021

8

9

11 5

Schematic of the Barton Pot process

10

higher sieve residue, which can be explained by the strong tendency of mill oxide to agglomerate. Scanning electron microscope analysis of Barton and mill oxides shows that mill oxide contains thin flakes of lead from the abrasion process around which fine dust tends to collect and form an agglomerate.”

The Barton process offers more flexibility in terms of the oxidation level as well as the product fineness.

Dependent upon the process used for producing the lead cylinders or chips, then a mill oxide in general has a higher specific energy consumption than a Barton oxide (ca. 100 kWh/t versus 130 kWh/t). Barton systems are available with up to 25-28 tonnes/day oxide capacity. Oxide mills producing more than 30 tonnes/day are commercially available.

The lower reactivity of Barton oxide makes it easier to transport both mechanically and pneumatically. Barton oxide is also less sensitive to further oxidation in the storage silos, especially under warm and humid conditions.

“Serious oxidation in a filter can generate a local fire and in a silo can lead to the need to dig out the product leading to production and product loss. In addition, dependent upon the project scope, a Barton process has a lower capital cost than an equivalent mill oxide process,” says Hardy.

Choosing the oxide McKinley believes that as Ball mill oxide tends to be more reactive than Barton oxide, many automotive battery manufacturers lean towards using Ball mill oxide in the automobile starting batteries. “The high reactivity of the Ball mill oxide tends to give a higher cold cranking amp rating.

“Barton oxide, having lower reactivity and larger, more dense particles, can be favoured by non-automotive batteries, (forklift, UPS, long-cycle and multiple-cycle batteries, AGM) because the life of the batteries tends to last longer with these characteristics of Barton oxide.”

Some battery manufacturers use both technologies and could produce Barton oxide for the negative plates, and Ball mill oxide for the positive plates (or vice-versa).

Barton oxide manufacturing can be enhanced by adding a hammer mill after the Barton oxide system that reduces the particle size and increase the acid absorption of Barton oxide, making it very similar in action to Ball mill oxide.

Hardy believes that from a produc-

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COVER STORY: LEADY OXIDE MANUFACTURING

Inside a Penox plant

INDEPENDENT ANALYSIS OF CAM BALL MILL SHOWS 100% LEVELS OF TETRAGONAL LEADY OXIDE CAM, the Italian industrial automation engineering company, announced on March 16 that leady oxide from its CAM MOP 30 ball mill had been tested by the University of L’Aquila’s department of chemical engineering in Italy. The test results showed: 87.8% tetragonal litharge [red lead], and 12.1% of [the unoxidized] lead, the firm said.

“The results were sensational,” said Francesco Marfisi, electrical manager at CAM: “The thing to note is the high percentage of tetragonal litharge, and the absence of orthorhombic oxide — this is fantastic because it means that batteries produced with this oxide will be more reliable over time, with consistent performance.”

A tetragonal crystal structure allows the leady oxide to better adhere to the grid while orthorhombic crystals are more prone to flaking.

Marfisi says that CAM’s ball mills are the only mills that have an internal cooling system using water spray. “By controlling the temperature inside the mill in a direct manner, you never have peaks of temperature which could cause the formation of orthorhombic crystals.”

The internal cooling system makes the controls of the Ball mill capable of being adjusted precisely very rapidly inside the mill.

The university testing was done under the auspices of professor Giuliana Taglieri and research fellow Valeria Daniele.

ANOTHER WAY TO MAKE LEADY OXIDE One method for making leady oxide without using either the Barton Pot or Ball Process requires a cementation reaction in HCl solution using a pure aluminium or a magnesium rod as the reductant, according to South Korean academics Ho Joon Shin, Ki-Won Kim and Hyo-Jun Ahn. As yet, no commercial production facilities exist.

The particle-size distribution of the leady oxide produced by this new process is similar to that of Ball mill

64 • Batteries International • Spring 2021

oxide. Its acid absorption, however, is much higher because of the different particle shape with respect to Ball mill oxide.

Ball mill oxide is composed of particles of non-uniform plate shape, whereas the new leady oxide is composed of particles of perfect flat (flake) shape. This new method of making oxide has a higher specific surface area and greater acid absorption than Ball mill or Barton Pot oxide.

“Modifying the basic oxides via microscopic coating with additives can further enhance the technical performance.

An example of this is PENOX Red Lead+, a red lead oxide coated on a particulate level with a tetra-basic sulphate seeding additive. In this way, the tetra-basic seeding crystal distribution within the red lead is very homogenous rather than relying on the (at times) poor macro-mixing in many paste mixers” — David Hardy, PENOX tion viewpoint, PENOX’s Barton/P20 leady oxide has some advantages — lower specific energy means reduced energy costs and lower reactivity means lower fire risk in filters and silos and easier storage and handling.

“Mill oxides are often stored for one to two days before using in the paster to avoid excessive reaction and heat generation. One advantage of the mill oxide process is that it tends to run with lower operator intervention (once the lead chips/cylinders are available).”

He says that the major difference between Barton and mill oxide, especially in terms of their electrochemical performance are the particle shape/ form, reactivity (related to the particle size) and the alpha-beta PbO ratio.

“For 4BS (tetra-basic sulphate) curing then Barton oxide (with a given percentage of orthogonal-PbO of around 5%) is preferred. The mill oxide, a pure tetragonal-PbO can only, with high temperature and steam, undergo 4BS curing. 4BS is found more in industrial applications due to the better cycling-life performance and depth of discharge performance.

“With advances in SLI technology trending towards EFB and AGM then 4BS is also preferred. This suggests a Barton leady oxide will be more suitable for such lead battery processes.”

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COVER STORY: LEADY OXIDE MANUFACTURING

The way we were … a brief history of lead oxide production The industrial processing of lead in furnaces dates well before Planté’s invention of the lead battery in 1859. The initial starting point for making lead for batteries was a cumbersome process. Red lead (Pb3O4) was melted in a reverberatory furnace to obtain lead oxide which then had to be run through a hammer mill to reduce the particle size to obtain the powder. The litharge produced was α-PbO. The first big advance in lead oxide manufacture

dates to the late 1890s and a firm with the improbable name of Matthews’ Lancashire, Cheshire and North Wales District White Lead Company. There its manager, George Barton, worked out a system where the melted lead could be stirred mechanically with air and steam and the resultant lead oxide could be skimmed off.

The process was sound but uncommercial as only two thirds of the metal was converted to the oxide. Barton was awarded

66 • Batteries International • Spring 2021

his first patent for this in 1898 but it took him a few years more to perfect the process and further patents were taken out in 1902 and 1908. Around this time the so-called Eckford Pot emerged as a variant on Barton’s invention.

Both Pot processes generated a significant fraction of orthorhombic lead oxide (β-PbO).

Although the Barton Pot only became widespread in North America in the middle of the 20th century, the National Lead Company

in the US in 1913 bought both Eckford’s and Barton’s patents. Both William Eckford and George Barton each made a fortune but to Barton was given the memory of his surname.

Competition for a speedy process to make lead oxide came in the early 1920s from an unusual source a manufacturer of laboratory instruments in Japan.

The man behind the process was Umejiro Shimazu, who changed his name to that of his father, Genzo Shimazu in his honour.

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COVER STORY: LEADY OXIDE MANUFACTURING machine could be built.

The first Shimazu patents describing the ball mill process emerged in the early 1920s but the clincher patent, filed in 1923 and granted in 1925 was called the Process of manufacturing powder of lead suboxide intermingled with power of metallic lead. The cleverness of the idea was in its simplicity. But in practice this required fine ad-

justments to get the right amount of litharge and metallic lead out.

Both the Barton Pot and the Ball mill processes have developed over the years.

Changes in manufacturing have advanced steadily with greater control.

For example, as late as the start of this new century, processes were still being fine-tuned to adapt to the changing secondary lead

feedstock.

The addition of silver, for example, to positive grid alloys is beneficial to the cycle life of SLI batteries.

However, when these grids enter the recycling stream they retard the lead oxidation process. One solution developed by David Prengaman, president of RSR Technologies, was the addition of minute additions of magnesium.

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National Lead Company, Boston photo circa 1900

Shimazu the father was a skilled maker of butsugu (Buddhist altar fittings) with an extraordinary scientific precocity and who set up the Shimadzu Corporation which manufactures specialized equipment to this day.

Genzo Shimazu, the son, realised the potential a ball mill could have in the process. Devices for shaking materials along with hard balls might be old, but it was not until the industrial revolution and the invention of steam power that a

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COVER STORY: LEADY OXIDE MANUFACTURING

Batteries International interviewed Massimiliano Ianniello, general manager at Italy based multinational engineering house, Sovema for his preference for Ball Mill machines.

Which process do you use and why, Barton Pot or Ball mill? How do they differ?

Right from the start Sovema decided to develop only Shimazu Ball mills, as the oxide produced with this process is suitable for all applications. It’s not the case with the oxide produced with the Barton process — especially for applications where cold cranking is required.

What makes the different processes appropriate for use?

The oxide powder produced by these two processes is different by shape, size of the particles, and surface area.

To achieve the best performances, it is necessary to have small-size particles with a wide surface area.

Generally speaking, the Ball mill process produces lead oxide with small particles but wider surface area, compared to the oxide produced with the Barton Pot process. These features

Sovema Ball Mill

affect the reactivity of the oxide, making the oxide produced with Ball mill process suitable for all the applications.

Why are they now being incorporated into battery manufacturers’ factory sites? How important are the processes to successful battery manufacture?

The incorporation of oxide production into battery manufacturing factory sites has been a fact for many decades now. We assume that the critical issues generated by handling and transporting the oxide are not comparable to the benefits of controlling the process in the factory.

Are there rival processes? Other possibilities?

There are other processes to produce lead oxide, however these two are the main ones, with the Ball mill process as the most widespread among battery manufacturers.

What are the challenges and advantages of the process you use?

Lead oxide is at the heart of the battery and its quality is reflected in the quality of the battery itself. Control of the production process is the key to get lead oxide of a high and consistent quality.

Sovema has extensive experience in this more than 350 installations worldwide. Process control is reached

Lead oxide is at the heart of the battery and its quality is reflected in the quality of the battery itself. Control of the production process is the key to get lead oxide of a high and consistent quality. through a design that automatically adjusts the operation of the machine to keep the lead oxide stable.

The main advantages of Sovema system are: • Constant control of the mass in the Ball mill.

• Configuration with external/internal/combined cooling, according to the environmental conditions and the oxide specifications required by the customer • Attention to the energy efficiency, as motors handled by high-efficiency inverters • Predictive maintenance on the main wearing parts • Advanced diagnostic and online troubleshooting • Compliance to Industry 4.0 requirements with remote supervision (from smartphone, tablet, etc.), with direct access to the working parameter, diagnostics, trends etc.

Recently Sovema has introduced a remote control app called ViSo — a mix of the Latin for Visum and Sovema — that works with 30t/day models of Sovema Oxide Ball Mill, to monitor in real-time the status of the machine

The app is able to connect with the machine’s PLC, verify its parameters, and provide visibility for the main trends through any browser by smartphone, computer or tablet. This follows real-time trends and also records the history of the main parameters, such as temperature, depression and weight.

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