BEE International Brings Homogenization to Graphene Production

US-based BEE International (BEEI) has been one of the leading providers of high-pressure homogenization equipment for industries ranging from pharmaceuticals to food and beverage for the last three decades.

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BEEI has recently become a corporate member of The Graphene Council and we took their recent membership as an opportunity to learn more about how its homogenization equipment operates and how it can benefit the field of graphene and its production.

Here is our interview.

Q: Can you please explain how your technology works and how it has traditionally been used?

A: BEE International manufactures top of the line high-pressure homogenization equipment that has widespread applications across multiple industries including Pharmaceuticals, Biotech, Cannabis, Chemical, Industrial, as well as Food & Beverage.  BEEI’s machines use electro-hydraulic pressure to generate force. This force pushes product through a fixed orifice (nozzle) which creates a liquid jet that is shot into a processing cell (emulsifying cell/ “EC”) at pressures up to 45,000psi. Machines can reach up to 45,000 psi in R&D, pilot or production scale with flow capacities ranging from 6 L/hr. all the way up to nearly L/hr. 

The force generated by the intensifier pump(s) and the nozzle is then absorbed by a series of tubular bead like components within the Emulsifying Cell.  These “reactors” are aligned in parallel inside the EC and receive the product jet stream, exposing it to a customizable blend of shear, impact, and cavitation forces. Each of these forces can be “dialed in or out” depending on your processing needs, giving you a highly customizable process to maximize your efficiencies.

Thirty years ago, when BEEI was founded at Technion-Israel Institute of Technology by our founder Tal Shechter, machines like ours were primarily used in the Pharma and Bio spaces.  Over the years these markets have expanded into other fields such as food processing, chemical and industrial applications, and even cannabinoid products. 

Our ultimate goal was, and remains, to manufacture the highest quality equipment that can be customized and tailored to fit nearly any application.  BEEI does not choose to generalize our clients’ applications and provide standard yet inefficient processing solutions; instead, we empower our uses to create ‘their best process’ fitting their needs. 

Simply put, BEEI creates the most versatile high-pressure homogenizer on the market today.  We have yet to find another company who produces a machine that provides end users with a comparably high level of control over their processing parameters in such a precise, easy to use, and scalable fashion.  These variable controls are why we see success in such a multitude of industries. These very same controls help our end users, researchers, developers, and production managers maximize processing efficiencies like never before.  

Q: How is this technology applicable to the production and processing of graphene?

The strongest graphene production technologies available today are chemical vapor deposition and liquid-phase exfoliation of graphene, although there are many more. Typically, companies seek to capitalize on one method over the other and BEEI specializes in the liquid phase exfoliation of graphite to graphene.

Exfoliation of graphite can occur from the following mechanisms:

• Compressible Flow Exfoliation: Graphite is forced through a small orifice at a high pressure. The pressure and orifice size are variable.
• High Shear: The narrow interior elements of a vessel impart shear forces on a product and this interaction between the two can delicately reduce layer counts.
• Cavitation: The configuration of the reactors can influence the environment seen by the graphite. This configuration may include alternating orifice size which can induce micro cavitation of bubbles or microjets, in addition to stress waves.
• Collision Exfoliation: The user may wish to engage the reverse flow mode in which graphite is returned into the initial flux stream, inducing particle-particle collisions. The amplitude of the aforementioned forces can again be tuned based on range of orifice sizes used, solvent choice, and pressure.
• Chemical Exfoliation: The control over the high-stress environment within the reaction cell as well as ability to incorporate multiple materials throughout the process has the potential to functionalize graphene.

The emulsifier technology can produce graphene, which can then be subsequently used for integration. The phrase ‘add graphene to a product and make it better’ aligns perfectly with that of a homogenizer.

A few examples include the use of a dual injection stream:

• Incorporation of a solid material (e.g., cementitious) into the flow of the liquid-phase reaction chamber to effectively mix the material.
• Addition of nanoparticles (e.g., ZnO) to integrate with graphene thereby creating new products. For example: new catalysts or a modified electronic structure.
• Colloidal assemblies through apolar and polar solvent droplet formation.

This versatility is a shining and disruptive area where BEEI excels. A small study1 looked at temperature, number of passes, and pressure on the exfoliation expanding to other 2D materials. This excludes other variable reactor configurations, which has more than a million possibilities.

This number may seem daunting, but they all follow similar trends in-terms of targeting the exfoliation mechanisms mentioned previously. The configuration can then be used to hone in on a specific product and allows multiple businesses to have a patent protected procedure that is extremely unlikely to be the same.  There are also more nuanced variables to adjust that can fine-tune the product, which can be multi- or single layer.

Solvent and additive choice is an incredibly important parameter for the stability of graphene dispersions; therefore, inertness comes into question. Much of the instrument is resistant to most chemicals and where there are vulnerabilities, additionally parts may be exchanged or substituted for a chemically resistant part based on the intended chemical use.

Particle size control in the vertical or horizontal plane can be finely tuned. The range can span from a client needing large 3-layered graphene particles, reducing the grain boundaries for their electronic applications, or creating single-layer graphene particles for their nano-graphene applications. This is made possible through the control of the forces being dialed back enough to target the intermolecular van-der-Waals forces or strong enough to disrupt strong covalent intramolecular interactions.

1) M. J. Large et al, Adv. Mater. Technol., 5, ()

The processing of Graphene requires a specific, tailored, and repeatable approach that most equipment on the market today is unable to provide. BEEI equipment enables users to delicately exfoliate Graphite and reduce layer counts while still maintaining a high aspect ratio and cell morphology. This process is then made more efficient by the ability to customize and select the forces they wish to be involved.

Q: What are some of the beneficial properties to graphene that are imparted by your technology?

Homogenization and the incorporation of graphene into a plethora of products.

Scalability of liquid-phase graphene products.

Stability of graphene dispersions not possible through conventional means.

Q: What kind of graphene-related companies would benefit from the use of your technology?

Companies involved in the following fields would benefit --- (but BEEI is always open to exploring all emerging applications): 

• The conductive ink industry. The standard is silver paste, however with proper processing, a graphene paste can be produced that reaches conductivity levels required for electronic applications (e.g., 28 kS m-1). Additionally, conductive graphene inks can be used for photovoltaics, biomedical sensors, flexible displays, automotive applications, RFID, and PCB technologies.
• Coating companies wishing to integrate graphene into their polymeric matrix.
• Cement and concrete. The ability to exfoliate and stabilize graphene in a water-based solvent at a high through-put is made viable through BEEI technology.
• Companies with a small-scale invention looking to advance the technological readiness level and begin scale up.
• Specialty surface-engineered companies looking to improve or upscale their catalyst.
• Graphene-enhanced sensors.
• Wearable graphite e-textiles.
• Environmentally friendly graphene producers.
• Battery industries.

BEE International provides processing solutions for companies at any stage from small batch R&D to large scale manufacturing. Whether you are looking to begin processing Graphene and need to establish a viable process, working on creating new products or applications, or wish to scale an existing product in a more efficient way, BEEI will be able to provide the necessary equipment to achieve these goals as well as accommodate future growth potential.

Q: What, if any, restrictions might there be on applying your technology to many varied forms of graphene?

The choice of graphite may present a restriction on through-put as a preliminary particle size reduction may be required before a quick configuration change is required to produce single-layer graphene.

This technology is solution based, graphene technologies that require high temperatures in solution to become active are also restricted.

Applications requiring a solid must go through a subsequent isolation step.

*** We encourage anyone encountering these restrictions to reach out to BEEI for a consult as we love to share our processing knowledge and discuss possible work arounds. 

Q: How do you ultimately see your company’s role in the graphene supply chain?

BEE International recognizes the widespread application of Graphene as well as other 2D materials and the potential impact they will have on society. As companies look to innovative and produce products that pave the way for technological advancement, there becomes a need for proven and dependable equipment that can achieve efficient and scalable results. BEE International is uniquely capable of providing these solutions and welcomes the opportunity to assist in developing new technologies.  

BEEI can offer versatility like no other and truly cornerstones the liquid exfoliation of graphite. This includes patent protected processes. The creation of standards to regulate graphene require a reliable large-scale production method which is offered. The liquid-phase exfoliation of graphene and other 2D-related materials and the applications therein can be created, scaled and commercialized through the incorporation of BEEI’s emulsifying cell.

When people start looking into the commercialization of graphene and graphene-enabled products, one of the first companies they likely come across is the UK-based Haydale Graphene Industries PLC. 

This is due—at least in part—to the fact that Haydale has been around for a relatively long time in the graphene business and was one of the first publically traded graphene suppliers, not to mention it being one of the leading companies in the production of graphene from facilities in the UK, USA and the Far East.

Over the years, Haydale has established itself as one of the go-to companies if you wanted graphene to have just the right properties for the device you wanted to develop. The task of functionalizing and dispersing graphene so that it bonds with the resin or polymer matrix in which it is being used has proven trickier than many companies had initially thought, leaving the uninitiated mixing in batches of graphene to their product only to have it make the product worse rather than better. By providing the expertise on how to extract the attractive properties from graphene, Haydale has created the backbone of its business.

In recent years, Haydale has continued to move up the value chain offering its own devices based on its functionalized graphene.

Now Haydale has become one of The Graphene Council’s Corporate Members,  and we took that opportunity to talk to the company’s CEO, Ray Gibbs, to ask about the company’s most recent commercial developments as well as see how he sees the market evolving over time. Here is our interview:

Q: Your purchase of Advanced Composite Materials, what did that give you that you didn’t have before and how has it changed your business?

The simple answer us it gave us a presence in the USA, which is a massive market—and gave us a base in the USA with meaningful sales. Also, we have a new nanomaterial that broadened our offering and is now part of our advanced materials Strategic Business Unit. The business itself had 15 plus blue-chip companies as clients. The aim is to cross sell some of our other nanomaterials, such as Graphene and Carbon Nano Tubes, into them. So that is really good news and even more so as we've grown that business with a new $2.6 million contract in April of this year.

Q: You have divided your business into two business units. Resins, Polymers, and Composites, which will concentrate on marketing and selling the newly developed graphene infused carbon fibre pre-impregnated materials (‘pre-preg’). The second unit, Advanced Materials, principally hosts the Group’s silicon carbide (‘SiC’) products and the newly developed graphene inks and pastes for the self-monitoring blood glucose device market. Why was this done and what do you anticipate it will allow you to do?

The key element to making these two strategic business units is focus. These business units are profit and loss driven.  Each has a dedicated managing director. One is based in the USA and that is Trevor Rudderham. He’s been on board from the time we bought the company, Advanced Composite Materials, in South Carolina. We also have a new person who has recently started named Keith Broadbent. Keith has come from Ultra Electronics, a large UK defense company. Before that he was running the production for prestigious Princess Yachts and Sunseeker International. So, he knows an awful lot about the composites industry.  This really is all about focusing on products and profits by driving sales in this fiscal year.

Q: Huntsman Corporation (‘Huntsman’) for graphene infused Araldite® epoxy resin. What’s happening there at this point? And what is Huntsman expecting to do with the epoxy resin? If it goes through, do you expect this to open up possibilities with similar big chemical companies?

We started our collaboration with Huntsman, a world leader in high end epoxy resins and adhesives, with an exclusivity arrangement about 18 months ago and it's been quite a journey. There are no sales yet but it’s been good for us though because we've learnt an awful lot of know-how about how to mix, choosing appropriate dispersions methods, what cure protocol to adopt and how the surface activations of materials affect our materials. One fundamental thing that it proved to us is that Huntsman did not want any change to the resin once we added in nanomaterials. Generally adding nano materials at low levels will alter the viscosity and downstream processing methods.  The minute you do that is when capital expenditure happens and that alerts the finance teams to cash outflows (often not in any budget). The key then is to avoid processing changes and the need for capital spend. The work has produced some fundamental know how on mixing, dispersion and processing. The overall effect produces a result which we call “functional intensity”.

Yes we've got an exclusive with Huntsman and they've been very prescriptive in telling other people that have approached them that they are working with Haydale and no one else, which is great news and very reassuring But in terms of that, they're honed their focus unashamedly on thermal conductivity. Why? Because thermal conductivity can improve thermoset output by up to 100%. In thick section moldings, such as wind turbine blades, for example, if you can reduce the exotherm reaction (heat) resulting from the “setting process” by 50% and the resin cure time by 50% then you have about a 100-percent increase in output. Not only that but the heat management produces a better-quality product, with less rejection and homogeneous cure. Now that is a pretty fundamental improvement if you look at the way that the composite industry is today and the production constraints that exist.

So Huntsman is all about better quality, and speed of output and being able to work on thicker structures. Of course, there is not only one aspect of the composites industry; you've got electrical conductivity some mechanical issues to address as well.  We have seen a 20% increase in mechanical performance of a carbon fibre composite, independently verified. That offers a potential weight saving of one fifth if you keep the same mechanical performance. Some of the other things that came out of that work has meant that we have been very successful improving aircraft composites. For example, in conjunction with Airbus and GKN we have produced an aileron that is 600 percent higher in its electrical conductivity, capable of defeating certain levels of lightning strike. Potentially our work could reduce the parasitic copper in an aircraft which can weigh up to 3 tonnes. Now that is a big thing for the aviation industry wishing to find ways of reducing weight.

Q: Haydale has become known as one of the most established expert companies on how to functionalize graphene in the precise way to make any given product possess the properties that your clients are attempting to achieve. Can you detail how that expertise evolved? Did each new customer provide new challenges and discoveries that led you to understanding how graphene can best be functionalized? Or was it just a matter of applying the same fundamental principles and practices to different clients? Or was it a combination of both?

The key thing is everyone's material—when they provide it—is different. Different shapes, sizes, flakes, thicknesses and it all comes with different levels of activated chemicals on the surface. So, if you've got a material that's come with a lot of oxygen on the surface, you're not going to get electrically conductive material because oxygen is an insulator and that may be inappropriate for certain applications. Hence, knowing and understanding the raw untreated materials is critical. That is something we have done for years now—we call it material fingerprinting—knowing what is on the surface of the material that we receive from a range of customers or suppliers is crucial. It may be that it's used with the functional groups already on the surface and it is compatible with the host material. On the other hand, it may not be suitable “chemically” for the application. And if it's not then we will use our own patented process to change the surface activation using our low temperature patented plasma technology. It's all about knowing and understanding what you've got and applying your own technique and processes to get the desired product improvement.

Q: We’ve seen some of your reported work with graphene inks to create film pressure sensors. Can you give us an update on that work and where it now stands commercially?

Several of these projects remain under non-disclosure agreements so that might be difficult to do. But we have got a number of things in the works with our patented pressure sensor. This derived from using our own proprietary inks by the Welsh Center for Printing and Coating at Swansea University. We have a five-year agreement with them that anything produced using our material we get right of first refusal on the intellectual property (IP). With the graphene loaded piezo resistive ink used to make the pressure sensor we filed a patent on this product. There is a range of things that we're looking at the moment, some in the sporting arena, some in protective elements and others in diagnostic mode—I can't really say much more! Suffice to say, we are in the process of getting applications moving from a commercial aspect and there’s a lot of potential activities to go at from adding pressure sensors on flooring to predict foot fall in the retail industry, to measuring impact on athletes engaged in contact sport for example. There are many industrial applications too offering massive opportunities. Its an exciting area, and all derived from Graphene.

Q: Is the aim of your company to move further up the value chain to producing devices that use your functionalized graphene? If so, what kind of devices are you looking to make and in what application areas? And how do you eventually seeing your company being arranged, i.e. 50 percent production of functionalized graphene for clients and 50 percent of your own production of devices based on your graphene?

I think if you look at the market place what you see is many producers trying to go up the value chain by providing some form of added value material. That material forms what I would call a master batch and it comes in many forms. For example, our conductive ink is form of a master batch because it’s using a resin—as a binder-based system—it’s adding graphene and other materials up to 40% to it to create a conductive screen printable ink. And we've been successful in the Far East in our new operation over there in producing some biomedical sensor inks. That's a part of the production line of a self-diagnostic biomedical device, which is blood glucose monitor.

By applying that same principle to what we just talked about with the Huntsman epoxy in terms of supplying a master batch into a customer so they can use as a concentrated form, a bit like a paste like the Coca-Cola syrup, for example: Customers receives the epoxy concentrate, dilutes it down with the neat base resin to what loading they want to use and you have a controlled process. That's really what I see. I don't envisage Haydale as a business selling anyone graphene flakes or powders because that frankly is a “me-too” commodity in my view. It also means we don't have the same element of control because the customer can take the graphene that you supplied—functionalized as appropriate—and it may or may not work because effectively they may have the wrong mixing and processing tools and protocols. And so we've got no control over that. Working with the customer in partnership is key.

What we have fundamentally is a supply chain set up through our collaboration partners, such as AMG in Germany who have some of our plasma reactors and they're ready to produce industrial quantities of masterbatch.

Q: What remains one of the biggest challenges in the commercialization of graphene-enabled products, i.e. price, quality of product, buyer awareness, etc.?

There is definitely a need for customer awareness of what can be done with nanomaterials. Everyone talks about standardization. A lot of the materials in the graphene space derive from effectively mined organic material, such as graphite. Graphite has been mined and sold for over 150 years but does not have any standards. But then you're dealing with things in the microscale as opposed to the nanoscale, which is one magnitude smaller than micro.

So effectively what you end up with graphite is small changes in supply impurities and the like make little or no impact if you put it into the industrial product like carbon brakes shoes or refactory linings.  Once you get to the nano-stage, knowing what you've got is very important as little impurities make a difference and therefore, yes, that is one important aspect of the whole process. 

For me, inconsistencies need to be the key message. Standardization is important and it will become very relevant particularly for large organizations seeking consistent volume supply; and I think what we've learned, particularly with the likes of Huntsman, for example, is that the two key questions they want to know is what is your disaster recovery plan for anything you supply us and do you have a more than one production site. Plus, secondly how robust is your supply chain. Those aspects will impact on people going forward.

I do think that the marketplace is getting itself ready.  Price is an issue where values for what appears similar products can be markedly different. The trained buyer will always look for the cheaper price but that may be a mistake especially if a material that is twice the price of another only needs a quarter of the loading of the cheaper material. Production is probably in advance of supply.  I’ve met many customers who tried nano materials before and said it doesn't work because I think probably they really didn’t understand what the material they had in terms of its functional group, its size, its morphology and the loading levels required. Agglomeration is an often-used complaint. Knowledge is beginning to permeate through the industry, which is good news. There’s lots of companies out there that are willing to take this on because when you change fundamentally products with very small doses of nanomaterials—we’re talking about under half of 1 percent here and sometime less—those massive changes can deliver real value.

Q: What do you think is the most important role for industry groups to play in helping to address those issues?

I think a lot of that is due to understanding of the marketplace. There is still a bit of hype that is still in the industry. Hype is not necessarily always bad as long as it is controlled. Hype helps generate ongoing research and development for all the processes and products. Hype goes astray when it makes exaggerated or wild claims that produce a distrust or misuse of materials in the marketplace. I think that's beginning to be understood. This is where the likes of the Graphene Council and others have a role to play in educating industry generally. We can use any help we can get to do that as we grow the market. There are too many providers chasing a market that is growing but is not large enough to satisfy production capacity today. If that isn’t rectified soon I would expect there to be casualties, and that is already happening.

We meet a number of companies that say, “I’ve tried carbon nanotubes, I’ve tried graphene and it doesn't work.” But in the past the engineer would actually say, “Oh well, I'll put more into this mix because it's bound to improve it.” In our nano world adding less is more. It’s an education process that for me is crucial in the industry we're in today.

I think the Graphene Council has got a role where it's important to inform and in to try to get industry to think about the benefit derived from a consistent, quality supply of material. We spend a lot of time going around the world doing a lot of presentations just trying to grow belief by providing verified data, which is crucial in getting the customer to say, “OK, it's not just been verified by the suppliers it’s been verified by an independent third party.” For me, that’s another area of credibility that needs to be driven by the industry.

A word of caution from someone who spends his life in this area: there are no magic products yet which will revolutionize the way we live. There is great hype surrounding the potential of graphene, but our experience tells us that we should be talking about evolution, not revolution. Our aspirations are great, but we will see transformation over time.

 We are already creating transformation, some things at a quicker pace than others. We have combined scientific knowledge, technological innovation and engineering know-how to create products that are significantly better than their predecessors. But we need opinion formers and august bodies to align with the producers and users of nano materials. This is where the likes of the Graphene Council, The National Graphene Institute in Manchester and the EU based Graphene Flagship have major parts to play.

 We absolutely believe there is so much more we can do and so much further than we can go, but to do so, we need to work in partnership with other major organizations who are the ‘early adopters’ those prepared to take calculated risks for that is where true economic returns arise – together we must go out into the new territories and explore what is possible. Eyes wide open!

 By doing so, we can work together to forge a better future for us all and ultimately, create material change in the world around us. That is the Haydale vision.

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Australia-based Imagine Intelligent Materials (Imagine IM) was launched back in by a divergent group of scientists, engineers and business leaders that recognized that the time was right for launching a business that made devices from graphene.

A couple of the keys to Imagine IM’s business strategy have been to control their own supply chain and to produce devices that really depended on graphene rather than just lending a marketing tag to a product that was not improved by graphene. To do this, they opened their graphene pilot plant in Geelong, Victoria, Australia in August with a capacity of up to 10 metric tonnes of graphene per year.

This plant will provide the material that the company will use to create smart materials for detecting stress, temperature and moisture. These smart materials can be offered as “drop-in” solutions for large-scale manufacturing processes.

As an example of this, Imagine IM has partnered with Geofabrics Australasia to develop a leak location system that employs “a conductive non-woven geotextile in between two non-conductive membranes to allow the detection of defects in the membrane.” 

In a the Q&A provided below, we speak to Imagine IM’s CEO, Chris Gilbey, to find out more about the relationship between their graphene production and device manufacturing and learn about how he sees the nascent graphene industry shaping up over both the short- and long-term.

Q: You are involved in both the manufacturing of graphene—with a production capacity of 10 metric tonnes per year—and using graphene to make smart materials for sensing temperature, stress and moisture. I was wondering if you could breakdown your business with a bit more detail. Are you actually manufacturing devices for sensing, or are you producing master batches for other device manufacturers to make the devices?

Our view is that that graphene is not a product. It’s a means to make products. And you can't make the appropriate graphene unless and until you understand what the end product application is going to be, what the functionalization requirements are, what the plant and product requirements are, etc.  We want to deliver solutions...and it happens that graphene turns out to be a highly efficient way to achieve some things as long as you understand what the rules of the supply chain are that you want to work in.

Q: Could you describe the graphene that your plant produces? What is the quality of the graphene and what applications is it suited for?

We make multilayered graphene in the plant we have built. But frankly it’s not about the graphene. It’s about the process of developing a masterbatch material. The quality is the wrong question to ask frankly. Quality with respect to what criteria? If you measure quality in terms of size of nanoplatelets and you make platelets that are 75 microns in size hypothetically and the application requires you to make graphene that that will fit into a 50-micron fiber then you have a mismatch. Quality at this point in the evolution of graphene applications is a largely misunderstood proposition in my view.

I believe that in any industry you always start with the customer need. Quality is less important than functionality and price. Rolls Royce might be a bench mark of quality in the automotive sector or perhaps they may be more correctly a benchmark of luxury. What then is quality? Back in the early days of GM the board of the company would have argued that they made quality autos. But Alfred Sloane and also Peter Drucker would perhaps have argued that they had incomplete information from the field and, as a result, made determinations that were entirely out of sync with reality!

What we focus on is developing fit-for-purpose graphene at the lowest possible price, and at a location that meets the supply chain objectives of customers. At this point in time, our focus is on developing appropriate levels of conductivity in materials—in particular industrial fibers and fabrics. Conductivity is a pre-requisite of delivering sensing.

Q: Is the idea that your 10 metric tonne production capacity will fulfill your own internal needs for master batches or device manufacturing? Or do you intend to sell some of that production to other companies?

No point in selling graphene to anyone. Not enough sustainable margin plus volume to make it into a business. Graphene as a feedstock material is in the early stages of being commoditized. More people will bring production on line, at lower prices, and many of the players will get into a race to the bottom on price. After all, there are already Taiwanese and Chinese companies boasting of >100 tonnes per year capacity. That is not the business we are in.

Q: Do you have a five-year plan on that production capacity? In other words, do you foresee that will be meeting your market needs in five years or will you have to increase capacity? What are your current operating rates?

Short answer is that if our vision was to only need to produce 10 tonnes per year in five years, we would have already died and gone to heaven. 10 tonnes will satisfy one product sku in Australia. We are in discussions currently to set up a plant in the US that will get us started in that market - just started!

The answer is in any event that you have to have distributed manufacturing that is close to your end use application in order to be part of mass manufacturing supply chains. I would anticipate market needs in tonnages greater than 100 tonnes for that one sku in a global scenario. At the end of the day, we want volume, volume, volume.

Q: How did you come to focus on the smart materials market? Was it something inherent in the graphene that you produced that lent itself to this application area? Or did you see an unmet need in the marketplace and then tailored your graphene for this use?

Actually the strategy is to reframe the concept of unmet needs and look at it through an economic lens. The intention is to become a disruptive player in mass manufacturing in the first instance and to be able to make smarter products at lower prices where we can positively impact the economics of products; i.e. there may be a need that is currently met, but if we can make a solution that radically changes the economics we get to win.

Q: As one of the early graphene manufacturers, what do you see lacking in today's graphene supply chain, i.e. lack of industry standards, poor understanding among users of graphene’s capabilities, etc.?

Simple answer: Certification. Industry standards are going be like legal structures for copyright. They will always trail the reality of disruptive technology. Why is Netflix such a powerhouse now? Because they figured that most people would prefer to purchase content legally than steal it, and the studios couldn't get their heads out of their backsides.

However, most manufacturers don't just want for there to be a QA process. They have to have it in order to be able to de-risk their businesses. At the center of our business is the concept and the reality of certification. It’s proprietary, just as the Dolby Labs certification process is, and the WL Gore certification process is. We have just started, funded in part by a federal government grant in Australia, a Graphene Supply Chain Certification and Research Facility at Swinburne University in Melbourne. This is the first of its kind worldwide and will enable us to look at the impact of the almost infinite permutations of changes to materials that take place in the nano-domain.

Q: What sort of movements and developments do you expect to see in the graphene marketplace over the next 5-10 years? Will applications become more narrow and defined or broader and dispersed? Will digital electronics become a reality or an afterthought? Any thoughts on the future?

All I can say to that is that I firmly believe that applications that utilize nanomaterials will be ubiquitous in 10 years. Equally, I think there will be a massive shake out in the marketplace. One company in the UK is rolling up a bunch of the early-stage graphene start-ups that couldn't get product to market. I think that the Gartner hype curve is playing itself out as one would anticipate and there will be a tremendous amount of consolidation over the next few years.

Companies like Samsung will be dominant in electronics applications as they pertain to consumer electronics (along with several Chinese companies). The bottom line for me is that the people who focus on selling graphene will be marginalized over the next ten years. Mass manufacturing is where the money will be. 3D printing will be a small business for quite a while yet. The big chemicals companies and the PE companies that have a focus on chemicals and advanced materials will remain the smartest guys in they room—meaning that BASF, DuPont, and similar will stand on the side lines and will pick off the little guys as they run into trouble. And somewhere in there a Google will emerge that redefines the whole sector...and a bunch of shareholders will make a lot on the way through and a bunch will lose out... And the Chinese may come through as the dominant country in the space... And hopefully we will find ourselves on the positive side of the ledger...

The bottom line is that anyone who thinks that they are going to make money out of graphene from applications that use only small amounts will find that their business models are unsustainable. Mainly because it is in no one's interest (who is a supplier) to sell small quantities of a material except with a giant margin and that doesn't incentivize you to develop scale....

I find this area of human enterprise to be utterly fascinating! And if you read for instance, what Danny Kahneman did, when he was asked to advise the Israeli army and air forces on how to identify future leaders and how his advice ran absolutely 180 degrees contrary to what was in place at the time, and the success of his research and approach, to me that is what is going to be needed conceptually to build an industry!

When we think of graphene, we conjure up cutting-edge and emerging technologies that have a place in a sci-fi movie, and rightly so. But to make those dreams into reality it is coming down to a nearly two-century-old specialty chemical company to produce the building blocks. William Blythe, a 170-year-old inorganic specialty chemical and advanced materials company based in the UK, has established itself as one of the premier graphene oxide producers, enabling other companies to fabricate next-generation devices.

In May of this year, William Blythe added graphene oxide to its portfolio of products and ramped up production of the material to large lab-scale manufacturing, reaching kilogram capacity production. At this point, the company can manufacture up to 20 kg of powdered graphene oxide per annum with the aim of increasing to tonnage scale in the next 6 – 12 months.

To accompany the launch of this new product line, William Blythe has created its GOgraphene website at which you can order the company’s graphene oxide product, as well as find a blog that discusses the experience of launching a graphene-based business.

The Graphene Council took the opportunity of this recent business launch to talk to William Blythe’s Global Marketing & Sales Director, Marc C.G. de Pater, and in the interview below you can read how this company evolved and found itself at the forefront of  one of the most cutting-edge materials, graphene.

Q: Can you explain how a 170-year-old specialty chemical company like William Blythe found itself transitioning into the production of graphene oxide?

A: William Blythe was originally founded to support the textile industry, however over the last 170 years, William Blythe has transformed into an inorganic chemicals manufacturer, who is now on its way to becoming an advanced materials supplier. The expertise William Blythe has developed over the years, as well as its focus on innovation and product development, means the chemistry of graphene oxide fits very well with William Blythe core capabilities.

Q: Can you explain a little bit about the graphene oxide dispersions you produce and how these dispersions fit into the value chain that ultimately lead to products that may find their way into our store shelves?

A: William Blythe currently manufactures a high concentration graphene oxide dispersion at 10 mg/mL, or 1%. The manufacture of a high concentration is designed to maximize the options for graphene oxide users – the optimal concentration of graphene oxide is still being researched but is likely to be highly dependent on the application in question. Higher graphene oxide concentrations can lead to difficulty when diluting the dispersion, however William Blythe has developed a dispersion which can be very easily diluted, as demonstrated in this video: https://www.youtube.com/watch?v=xLixtvZRq0w.

In terms of the value chain, the nature of graphene oxide means William Blythe is positioned at the start. The graphene oxide dispersions offered allow William Blythe’s customers an opportunity to revolutionize the products they sell. Any graphene oxide, or graphene oxide derivative, that ends up on the store shelves is likely to be present in small concentrations, with consumers only aware of its presence through the enhanced properties they observe in the products they purchase.

Q: Why has your company struck upon graphene oxide production rather than single-crystal monolayer graphene? Was that because of what your customers were looking for or did it fit your business plans better in terms of both current production and how you see the market developing?

A: A combination of both – while the chemistry of graphene oxide synthesis fits very well with William Blythe expertise, there is also a strong argument for graphene oxide use over graphene in many situations. Graphene is a hydrophobic material, which means it can be very difficult to obtain good dispersions in various media. Graphene oxide, however, is highly hydrophilic and is reported to disperse very well in many polar solvents. By obtaining the required dispersion with graphene oxide and then reducing to graphene, graphene oxide may also allow users to gain the desired properties of graphene while achieving the dispersion characteristics needed.  William Blythe therefore believes graphene oxide has the ability to exist in the graphene market, employed in systems and applications where graphene would not be suitable.

Q: There seems to be an issue of wide disparity in the quality of graphene products. Is this something that will just be sorted out in the marketplace, or do you think standards will need to be instituted before this problem is fully addressed?

A: Graphene products are so new to the market it is understandable that there is so much variation in product quality. As more users investigate and adopt graphene or graphene oxide products into their applications, a consensus is likely to evolve naturally over what constitutes appropriate material for use. Formal standards may come into place at some point, however if graphene derivatives are already well established by this time it would be reasonable to expect these to take the approximate form of the informal standards already adopted. William Blythe will of course support the establishment of both informal and formal standards for graphene oxide where possible.

Q: What is the range of applications that your customers are using for the graphene oxide that you produce? And what is it about your product that makes them choose yours rather than others, i.e. price, quality, etc.?

A: William Blythe’s graphene oxide is of interest to a wide variety of applications. While it is not possible to disclose specific applications or customers, we can indicate that the range is broad enough to cover applications from membrane technology to advanced coating technology. The biggest attractions to William Blythe’s graphene oxide are its quality (dispersibility and number of layers) and the scale at which the material can be supplied. As a long established chemical manufacturer William Blythe is already planning to scale up manufacture to tonnage quantities. This, combined with a long history of manufacturing and supplying high quality chemicals gives customers confidence in William Blythe’s ability to support the launch of their technologies.

To support those still in research phases of graphene oxide application development, William Blythe recently launched a webshop, www.go-graphene.com , which sells research quantities of graphene oxide powder and aqueous dispersions. The feedback from this indicates the biggest draws are the competitive pricing and excellent dispersion characteristics.

Q: You are located near the University of Manchester where graphene was first discovered and a major research facility has been created. Has this proximity had an impact on your business? If so, in what way?

A: To an extent, the proximity of William Blythe’s headquarters to the University of Manchester has been of benefit. Members of both the commercial and technical teams at William Blythe have been able to attend meetings and conferences which may have been more difficult if the locations had been less convenient. These events have helped William Blythe to establish some of the understanding and network which are invaluable to the business today. Having said that, William Blythe is sufficiently committed to the development, manufacture and commercialization of graphene oxide that the same activities would have been pursued irrelevant of geography.

Q: Do you foresee William Blythe moving further up stream in the value chain by manufacturing products that employ your graphene oxide? Or will you remain producing dispersions of graphene oxides?

A: William Blythe intends to continue selling both graphene oxide dispersions and powders as well as any other relevant graphene derivatives which make sense in the future. Alongside these it is possible that William Blythe will offer products which fit in further down the supply chain. The volume and caliber of global graphene oxide research is so high at the moment it seems very likely there are other opportunities for William Blythe in the graphene derivative marketplace.

Q: Can you paint a picture of both William Blythe’s graphene business in the next 5 to 10 years and how the market will look more generally in those time periods?

A: Based on William Blythe’s market intelligence, it is anticipated that graphene products will be well established in the supply chain of several industries within the next 5 – 10 years. Naturally this means graphene oxide volume requirements will have risen and potentially the market price will be lowered. William Blythe expects to still be offering highly competitive pricing for high quality graphene oxide, with manufacture moving to a new dedicated graphene oxide plant. Early estimations predict William Blythe’s graphene oxide plant will have an annual production capacity of 10 tonnes.

For decades, industries have evolved their products to meet consumer demands. From the evolution of 3D printers and the electrification of motor vehicles, to the development of new materials like graphene, the world continues to look different than the decade before. For the industrial market, this is no different.

In these photos, you will see a transformation from New York City in the early ’s (left) using horse and carriages as the most common means of transportation to a picture of New York City in the , where automobiles had become the number one source of transportation with the invention of the Model T in . These images quickly, but accurately, depict how new technologies can result in completely different products, consumer expectations and behaviors.

(Sources: National Archives; The Bowery Boys)

The Transition To Lithium

The continued changes in the automotive market directly impact the industrial grease market. As the world shifts from the standard combustion engine to electric vehicles, there will be a greater demand for lithium. According to NLGI, lithium greases account for more than 75% of global lithium consumption. To put this into perspective, the country of Brazil has only 5% of the global lithium reserve. To produce lithium greases in Brazil, it requires 500 tons of lithium metal per year.

As the production of electric vehicles increases, so will the lithium demand. Lithium consumption is expected to significantly increase on a global scale, with an anticipated 20,000 tons per year to 50,000 tons per year by —ultimately, impacting the cost of lithium greases.

Table 1 represents the most common applications and their corresponding lithium demands within the global marketplace.

Table 1 (Source: Dakota Minerals)

The Search For A Lithium Alternative

In the process of discovering an alternative to lithium and complex lithium, there are several thickeners suited for high-quality greases. The advantages and disadvantages can be found in Table 2.

Table 2 (Source: Lubrizol internal training)

Calcium Sulfonate greases are multipurpose and require minimal additives to deliver desired performance benefits within different applications. Table 3 illustrates the results of four-ball and Timken tests. Using basic, calcium sulfonate grease—without additional additives—it indicates the exceptional performance that can be achieved within high-temperature environments.

Table 3 (Source: Lubrizol internal data)

The Search for Lithium Grease Alternatives

Although there is not a “perfect grease” within the marketplace, calcium sulfonate greases have proven to be a sustainable alternative to complex lithium greases. If grease manufacturers decide to select this as an alternative solution, it is recommended they seek additives that ensure superior performance. When selecting a calcium sulfonate grease, there are a couple items to consider:

• Pumpability: Due to differing characteristics found in thickeners and soap fibers, three calcium sulfonate greases could present different pumping results. The DIN allows us to evaluate this property and draw comparisons between similar products as illustrated in Table 4.
• Water washing: Due to differences in methodology, calcium sulfonate greases may present good water wash results by ASTM d (Wash-out) and bad by ASTM D (Spray-off). Table 4 illustrates significant variations between base greases (without additives). If performance additives are used, spray-off can be reduced by up to 10%.

Table 4 illustrates an example of complete formulation of Calcium Sulfonate grease and performance additives developed for the steel industry. These additives allow for excellent water washing results to be obtained in both ASTM d (wash-out) and ASTM D (Spray-off) method. Additionally, grease presents high performance EP and stability to shear. (Source: Lubrizol internal benchmarking)

Table 5 illustrates how a calcium sulfonate grease can be used with specific additives to achieve desired performance in automotive or industrial applications. (Source: Lubrizol internal benchmarking)

The GC-LB norm is one of the most recognized for the automotive segment. Table 6 illustrates an example of complete formulation of Calcium Sulfonate grease and performance additives developed for the automotive industry that serves GC-LB. We highlight in blue some very relevant results obtained during evaluation of this formulation.

Table 6 (Source: Internal Lubrizol data)

Table 7

The versatility of Calcium Sulfonate greases compared to Lithium Greases can be compared according to Table 7. With the use of appropriate formulations and additives it can be used with good or optimal performance in virtually all segments of the industry, including food where lithium is inadequate.

Our View

As the industrial and automotive markets continue to evolve, discovering lithium grease alternatives is essential. Calcium sulfonate greases serve as an excellent alternative as it features exceptional versatility within various industries, as well as high anti-wear and anti-corrosion properties. While there is currently no mandate to implement the switch from lithium greases to calcium sulfonate greases, this new alternative can serve as an effective and economical choice for manufacturers.

To learn how the shift to calcium sulfonate greases could benefit your business, contact a Lubrizol representative today.

If you want to learn more, please visit our website Graphene Grease.