Industry news

Perpetuus Advanced Materials Reactor

Perpetuus secures independent verification for the quality of its functionalised graphene materials

Quality test follows independent verification of Perpetuus’ high volume production capacity

Perpetuus Advanced Materials (“Perpetuus”), a British company at the forefront of advanced materials development, announces the successful results of a quality study on its functionalised graphenes by Cardiff University.

Graphenes, specifically functionalised by Perpetuus for use as nano enhancing fillers and enablers within polymers, were produced by Perpetuus under independently observed conditions and used in this test.

A full analysis and characterisation of the materials produced was undertaken by scientists at the Cardiff Catalysis Institute, School of Chemistry, Cardiff University, led by Dr. David Morgan. The analysis included Raman, XPS, XRD and Microscopy. Dr. Thierry Mathis of Swansea University supervised the SEM Microscopy for the quality study. The results of the study demonstrated that Perpetuus’ proprietary plasma production process delivered industrial scale quantities of highly crystalline, friable functionalised graphenes.

Many applications for graphene are limited by graphene typically being unable to exist unsupported over extended lengths and widths, instead stability is achieved through several – typically less than ten – layers. The study concluded the Perpetuus Plasma method of graphene production could generate stacks of typically under ten layer thicknesses, with high quality domains.

Perpetuus was pleased with the results and accordingly asked Dr. David Morgan to then test the same materials used in the study for applicability to a commercial environment by coordinating and supervising the production of conductive ink. The Directors were delighted that the resulting ink, with a resistivity of 5 ohm per square, was concluded in the test to be suitable for mass-market commercialisation. The study concluded: “This form of ink production offers a great improvement over existing methods.”

The graphene materials used in the Cardiff study were produced by Perpetuus as part of an independent quantity verification process. That procedure was undertaken by industrial process experts Scott Grant (attended by accountants Grant Thornton UK LLP as independent observers). The study concluded that Perpetuus had a theoretical production capacity of 140 tonnes per annum from a single reactor.

The Board of Perpetuus believes that the results from the independent quantity and quality studies of Perpetuus’ functionalised graphene materials show that:

  • Perpetuus has a production capacity of 140,000 kilos per annum; and importantly that
  • Perpetuus’ plasma production process can produce friable highly crystalline functionalised materials that are suitable for commercial use.

Perpetuus believes these two studies represent the first verifiable, comprehensive ‘full suite’ analysis of commercial quantity production of graphenes.

John Buckland, CEO of Perpetuus Advanced Materials, said:

“One of the greatest challenges the graphene industry faces today is how to produce high quality functionalised materials, on a large scale, at low cost, using reliable and robust technology.

By undertaking this independent study and making our graphenes available at £50 per kilogram, we hope to build confidence amongst potential producers of graphene enabled applications and products. I sincerely hope other graphene material producers invest in similar testing protocols, using the ‘full-suite’ characterisation and analysis developed by Cardiff and Swansea Universities.

“We are delighted that we have been able to independently verify the functionality of our conductive inks and pastes, which we believe begins to demonstrate the potential of 2D materials and allows potential customers real visibility of and the opportunity to gain confidence in our work.”

The full Cardiff Catalysis Institute report is available here.

Notes to Editors:

Copies of the volume output verification study and the quality characterisation study, along with pictures from the exercise and a detailed event timeline can be viewed here.

Perpetuus functionalised graphene GNP’s, Stacks and Inks samples are available for pre-qualified student and researchers to aid their studies.

For further information contact:

Perpetuus Advanced Materials Ltd

Public Relations – perpetuus@mhpc.com

Technical Information – www.perpetuusam.com

Perpetuus Graphene Stacks

Perpetuus Carbon Group announces commercial relationship with G24 Power

Press Release: 12th November 2014

UK based Perpetuus Carbon Group and G24 Power Ltd have entered into a Memorandum of Understanding, a precursor to a full commercial partnership and manufacturing agreement.

Perpetuus are the world’s largest producer and supplier of high quality, functionalised graphenes. G24 are a world-renowned authority in the dye sensitized solar cell (DSSC) market, with expertise in the production of conductive, multifunctional, multilayer coated webs.

Using Perpetuus functionalised graphenes, G24 will produce to order a range of advanced graphene enabled components, in sheet or roll form. G24’s advanced manufacturing equipment enables production capacity of 1000’s of metres of components per month for areas such as:

  • Resistance heating
  • Bio-sensor platforms
  • Barrier packaging
  • Composite physical reinforcements
  • Water treatment
  • Proton Exchange Membrane (PEM) Fuel Cell
  • Thermal management and heat dissipation
  • EMI shielding
  • Electrodes for batteries and super capacitors
  • LI-AIR battery cathodes

Thermal conductivity of greater than 500 W/M°K along with surface resistivity of substantially less than 1 Ω/sq, can been achieved on rolls of material, produced at a specific thicknesses, on specified substrates, for components used in aerospace, marine, automotive, energy generation and energy storage industries.

graphene enabled coating equipment

Source: G24 Power – Roll to Roll Coating Equipment

 

Graphene Enabled Coating on 300mm Sheet

Source: G24 Power – Graphene Enabled Coating on 300mm Sheet

On 19-20th November 2014, Perpetuus and G24 will be exhibiting samples of some of these new graphene-enabled components at IDtechEx Graphene Live! and Printed Electronics USA 2014 in Santa Clara, California. Perpetuus and G24 technology experts will be available to discuss customer specifications and requirements.

http://www.idtechex.com/graphene-live-usa/conference.asp

John Buckland, CEO of Perpetuus Carbon Group said,

“We were impressed how quickly the technical team at G24 took our graphene enabled compounds and started producing components that can be used in so many exciting areas of industry. Their manufacturing equipment and scientists are first class and I have no doubt our partnership will quickly make us the world’s first manufacturer of graphene enabled components in many market sectors. This new relationship, together with other collaborations sets Perpetuus Carbon Group apart from our competitors as the only business truly able to commercially produce graphene enabled products. Our existing and soon to be expanded facility in South Wales, UK, has the capability to grow into the world’s first centre for manufacturing graphene enabled products. Taken together with exciting advances in R&D at the Institute of Graphene at Manchester University, we believe that George Osborne’s vision of the UK being the powerhouse of graphene technology will soon become a reality”.

Richard Costello, CEO of G24 Power said,

“G24 are known the world over for excellence in the field of DSSC PV technology. Our expertise in this regard has delivered a capability to produce high-speed, roll-to-roll, precision thickness coatings. Working with Perpetuus we have configured our production equipment to manufacture graphene-enabled coatings and films to precise specifications. We can therefore produce to order a range of components and applications for the automotive, aerospace, marine, electronics, as well as other market sectors. With Perpetuus producing commercial quantities of functionalised graphenes we are perfectly placed to supply the global market with these exciting new products.”

Notes for editors

Until recently graphene production has been limited to outputs of grams per week and as a consequence graphene remains one of the most expensive materials by weight known to man. When it comes to utilising graphene on a large scale, industry and researchers all over the world have been frustrated and often held back by the same problems – no large volume sources, no reliable suppliers of inexpensive, high quality materials and graphene’s tendency to agglomerate, which causes significant reduction in potential surface area, often meaning their graphenes cannot be processed.

The Perpetuus dielectric barrier discharge plasma method of production, overcomes the historical problems and now produces friable sub stacks of single, bi and tri-layer graphenes, with nano engineered surfaces, enhanced with the functionalities that provide both ease of dispersion and covalent bonding within any chosen matrix. The Perpetuus plant in South Wales, UK can provide more than 100 tonnes of graphenes per annum and is the only graphene production unit anywhere in the world, where its production capacity has been independently verified – a task that was undertaken by work-study experts Scott-Grant and Auditors Grant Thornton in August of this year.

 

About Perpetuus Carbon Group Ltd

For any company to be successful in the commercialisation of graphene materials they need to offer ALL the following features to a customer:

  • Functionalisation by implanting a variety of chemical groups onto and within graphenes to nano surface modify graphene to customer specifications.
  • Reliable and consistent supply of high quality graphenes for R&D.
  • Immediate availability of materials in grams and kilos.
  • Rapid delivery of tonnes rather than grams.
  • Production in Commercial quantities.
  • Competitive pricing.
  • An environmentally friendly production process (this will become more relevant as the industry expands).
  • Environmental impact studies and life cycle analysis on all outputs and by-products.
  • Comprehensive and reliable characterisation data.
  • Manageable, transportable, user-friendly graphene presented in ‘stacks’. (Graphenes as single layers are invisible to the naked eye and cannot be packaged or handled).

Perpetuus offer all the above to its customers. Perpetuus are not aware of any other business in the world who can offer the full range of these goods and services to its customers and therefore we believe, we, a British Company, are the world’s leading producer and supplier of high quality nano surfaced engineered graphenes.

For further information contact:

Public Relations – andrew.leach@mhpc.com

Technical Information – info@perpetuusenergy.com

Perpetuus Dielectric Barrier Discharge Reactor

Independent Verification of Production Capacity for Graphenes of 140 Tonnes per Annum

Press Release: 3rd October 2014

Perpetuus Carbon Group Announce the Independent Verification of their Production Capacity for Graphenes of 140 Tonnes per Annum

UK based Perpetuus Carbon Group, the world’s largest producer of purified and functionalised graphene, are pleased to announce the results of an independent verification of their graphene material production.

Industrial process experts Scott Grant, with Grant Thornton Accountants in attendance, conducted an independent work-study in September 2014. The aim of this study was to ascertain the annual production capacity of the Perpetuus Dielectric Barrier Discharge Reactor.

Using a measurement study that complied with BS 3138:1992, the conclusion of the study was that the annual theoretical capacity, running 30kg batches of raw graphite, is 140 tonnes per annum from a single reactor.

During the quantity audit, two 30kg batches of graphene stacks, surface-engineered with 3% oxygen functionalities, were produced and randomly sealed samples were taken for independent quality testing. Both Swansea University and the National Graphene Institute in Manchester have been independently commissioned to formally characterize the material from Scott Grant’s quantity work-study. This was also audited by Grant Thornton Accountants. The material characterization results will be published on the Perpetuus web site within the next six weeks.

Input Material – Graphite. Output Material – Graphene Nanoplatelet ‘Stacks’ (10µm scale) Image credit – Swansea University

Input Material – Graphite. Output Material – Graphene Nanoplatelet ‘Stacks’ (10µm scale)
Image credit – Swansea University

Perpetuus are the first business to submit themselves for independent material testing by the Graphene Characterization and Standardization Services (GCSS) run by Graphene Enterprise Award 2014 winner, Antonios Oikonomou, based at the National Graphene Institute, Manchester.

The consistently high quality of materials, together with immediate availability of commercial quantities, has in the last year resulted in over 200 R&D customer orders of Perpetuus graphenes. The ability to specify exact surface engineering requirements has enabled customers from Japan, Korea, the EU and USA to rapidly move towards the commercialization of their ‘graphene enabled’ products.

Perpetuus Chief Executive, John Buckland said, “Hype and misinformation is one of the biggest problems facing the graphene industry. It is our hope that by being the first business to allow third parties to independently audit and verify the quantity of our production and the quality characteristics of our graphene materials, it will encourage others in our industry to follow suit. The market for graphenes has reached a tipping point and genuine enquiries from industry are at an all-time high and rapidly increasing. However, we know from our customers, they will only commit to R&D if they have confidence that they can obtain commercial quantities of high quality functionalised materials when they are ready to shift to commercial scale production”.

Perpetuus Director, Ian Walters said, “We hope our open and transparent approach to current graphene industry capabilities will enhance our reputation as an authority in the commercialisation of graphenes. The rise of customer confidence in Perpetuus requires us to commission three new reactors with enhanced technical and production capacity and move into new premises early in 2015”.

About Perpetuus Carbon Group Ltd

For any company to be successful in the commercialisation of graphene-based materials they need to offer ALL the following features to customers:

  • Functionalization by implanting a variety of chemical groups onto and within graphenes, in order to surface-modify graphenes to suit customer specifications.
  • Reliable and consistent supply of high quality graphenes for R&D.
  • Immediate availability of materials in grams and kilos.
  • Rapid delivery of tonnes rather than grams.
  • Commercial quantities.
  • Competitive pricing.
  • An environmentally friendly production process (this will become more relevant as the industry expands).
  • Environmental impact studies and life cycle analysis on all outputs and by-products.
  • Comprehensive and reliable characterization data.
  • Manageable, transportable, user-friendly graphene presented in ‘stacks’. (Graphenes as single layers are invisible to the naked eye and cannot be packaged or handled).

Perpetuus offer all the above to their customers.

Perpetuus are not aware of any other business in the world that can offer the full range of these goods and services to their customers and therefore we believe that we are the world’s leading producer and supplier of high quality nano surface-engineered graphenes.

For further information contact:

Public Relations – andrew.leach@mhpc.com

Technical Information – info@perpetuusenergy.com

Perpetuus Carbon Technologies logo

Perpetuus featured on ‘The Engineer’

The Engineer

Carbon Crusade

10 March 2014 | By Stuart Nathan
Click here to view this article on www.theengineer.co.uk

UK firms are pioneering the production techniques that could bring graphene to the masses.

It’s been proclaimed a ‘wonder material’ that will be the springboard for a new technological revolution. It has earned its discoverers Nobel prizes, formed the foundation for dedicated institutes and, if publicity is to be believed, is set to inveigle itself into every aspect of our lives. Name a superlative property and someone will claim it has it. Graphene has received more hype than a whole series of blockbuster superhero movies.

But graphene is real; and huge research budgets are focusing on it worldwide. For the uninitiated, graphene is a pure form of carbon consisting of a single flat sheet of carbon atoms arranged in hexagons: in effect, a single layer of graphite. It’s often referred to as a two-dimensional material, although, strictly speaking, it isn’t; it’s one atom thick and atoms are not dimensionless.

perfect graphene structure

Perfect graphene structure such as this is, in practice, almost impossible to achieve.

First isolated at Manchester University in 2003 by Russian-born materials scientists Andre Geim and Konstantin Novoselov, graphene had previously been studied theoretically but was thought to be thermodynamically unstable. Geim proved this was wrong when he took a thin piece of graphite that had been prepared by a student and ‘peeled’ off a sheet of graphene using a piece of adhesive tape.

‘We believe that the first commercial applications are likely to be conductive inks in the next five years”.

Paul Mason, Technology Strategy Board

Intensive investigation of the properties of small samples of this new material triggered excitement in the scientific community and the technology industry: although infinitesimally thin, it seemed to be immensely strong, with a breaking strain 100 times greater than a film of steel of the same thickness. It conducts heat as well as diamond and appears to enable ‘ballistic transport’ of electrons — zero-resistance electrical conductivity. It’s transparent, can convert visible light into electric current, and is flexible and biocompatible.

The deluge of encouraging results triggered a rush to commercialise graphene — a rush that shows no signs of slowing down. Electronics companies, with South Korea’s Samsung in the lead, have thrown resources at the problem, hoping that graphene will be the key for anything from new forms of touchscreen display to innovative batteries. This has led to concerns that, with its relatively smaller budget available for research, the UK will once again see a discovery made on these shores exploited for profit elsewhere.

Andre Geim

Andre Geim: The first scientist to isolate graphene, and incidentally the
only person ever to win a Nobel Prize and an IgNobel Prize (for
levitating frogs)

Despite this, there is a small but growing band of UK companies — alongside the National Graphene Institute, based at Manchester — exploring ways to manufacture graphene in bulk. There are still no products containing the material on the market — these companies sell graphene to companies developing applications. While for university materials science departments, isolated flakes of graphene are fine for experimentation, to a company developing products, a reliable supply of graphene in amounts large enough to make prototypes, with robust and repeatable properties, is vital. Once commercial applications are developed, dependable manufacturing techniques will be indispensable.

There are two ways to make graphene. Geim and Novoselov’s method, flaking sheets of graphene off a chunk of graphite, is known as ‘top-down’. In a manufacturing context, this isn’t done using sticky tape, no matter how appealing the image might be: the graphite can be vibrated with soundwaves (sonication); treated with acid and thermally shocked; or bombarded with ions in a plasma to break the weak bonds between the graphene layers that make up graphite and exfoliate sheets of the material from the bulk. The other method doesn’t use graphite: rather, it seeks to force individual carbon atoms from some other source, generally a hydrocarbon, to combine into graphene’s hexagonal grid; this is known as a ‘bottom-up’ approach. This is what electronics companies such as Samsung are favouring, as they require larger areas of graphene. A process called chemical vapour deposition (CVD) is commonly used, where a carbon containing vapour is deposited onto a flat substrate — often copper — guided by a catalyst that can be a solid or in the vapour phase.

 

powdered graphene

Powdered graphene made using a bottom-up process by Applied Graphene Materials.

The UK graphene community contains proponents of both top-down and bottom-up processes. But there is a complicating factor: the properties of the materials produced are very strongly influenced by the manufacturing process and this, in turn, influences the applications for which they can be developed.

‘We believe that the first commercial applications are likely to be conductive inks in the next five years, and for that you need very small fragments of graphene, a few layers thick: what’s known as nanoplatelets,’ says Paul Mason, head of innovation at the Technology Strategy Board, which is funding development of graphene applications via a £2.5m competition for feasibility studies, alongside the Engineering and Physical Sciences Research Council (EPSRC). ‘And conductive inks, used alongside a jet printer and a 3D printing mindset, could be a powerful technology. Think of them in conjunction with the plastic electronics sector, in which the UK has a strong foothold. Following on from that, we’re expecting to see commercial applications in composites, using graphene’s physical properties and, again, the UK is very strong there. The electronics applications, such as displays and touchscreens, will come in after that and we think we’re looking at 10 to 15 years for those to hit the markets. It’s a long game.’

Ultimately, Mason says, the goal for the competition is for graphene to contribute to the UK economy. ‘But we aren’t sticklers for the exploitation itself to be in the UK,’ he adds. ‘If someone came to us with an idea for a technology that Samsung would license from them for £10m, we’d consider that a UK gain. And we aren’t concerned about what sector it’s in. Electronics using graphene are often seen as a South Korean strength, but we aren’t about to tell ARM not to work on a graphene transistor.’

The thought of perfect sheets of graphene forming a flexible, transparent touch-screen fall down because of the realities of manufacturing, says Ian Walters, who founded one of the UK’s first graphene makers, top-down producer Heydale, in Cardiff, and has since founded another, Perpetuus Carbon Technologies, near Swansea. ‘You can’t make a perfect graphene sheet over a wide area,’ he said. ‘You get islands of crystallinity — and it’s the crystallinity you’re after because otherwise you just have amorphous carbon, which is useless — and those islands grow together. But then you have grain boundaries, and those disrupt the conductivity of the sheet.’

That’s not the only problem, he adds. ‘You’ve got to get the sheet off the substrate and the material isn’t robust. If you manage to isolate it from the metal, then all that happens is that it rolls up and forms a nanotube.’

Perpetuus, which like so many high-tech startups in the UK is based on a nondescript industrial estate next to a pet-food warehouse, uses a top-down method to make graphene nanoplatelets. Its anonymous buildings house a reactor that can hold some 30kg of powdered graphite, which is subjected to treatment with a plasma of high-energy ions generated by UV light and a high voltage from a specific arrangement of electrodes. This, Walters says, gives it the ability to produce 100 tonnes of graphene products per year; plans are afoot to install a more advanced analysis lab at its HQ and to build a new production facility in nearby Port Talbot with two larger reactors.

dispersions of graphene

Dispersions of graphene in a liquid are important for making conductive inks and anti-fouling coatings.

‘One of the problems with processing graphene is that it’s very inert stuff; it doesn’t like to mix with anything,’ he says. ‘So we can functionalise it; by changing the process gas in the reactor, we can make surface-functionalised graphene with oxygen groups, carbonyl groups; amine groups; or fluorine. Oxygen-functionalised with disperse in water, and can also form covalent bonds with epoxy, as can amine groups. There’s a fair bit of trial and error in making the desired product,’ he adds, ‘because on an atomic level, we don’t understand what’s happening in the reactor; we can tweak things such as the level of vacuum, the electrode voltages, the vapour composition and so on.’

The result is a graphene nanoplatelet powder that visually appears little different from the graphite that went in, but can be characterised using analytical techniques such as scanning electron microscopy (which reveals images of the wrinkled sheets of graphene) and X-ray diffraction (which shows the level of crystallinity); an increase in volume also indicates the transformation, as the layers of graphite are forced apart. ‘It’s important to remember that graphene is graphitic carbon, and as soon as you have stacked layers you essentially have graphite,’ Walters says. The fewer layers in a nanoplatelet and the more space between them, the more the graphene-like properties predominate over the graphitic ones.

Perpetuus can also produce graphene that is studded — or as Walters puts it, decorated — with micrometre-scale nuggets of other minerals. Decorating the edge of the graphene sheet with silver, for example, enhances the conductivity of the material in ink, and decorating with zinc oxide imparts piezoelectric properties. This raises possibilities such as using a graphene-ink printed stretchy membrane as a wound healing dressing, which could be used internally or externally, with movement generating an electric current and field to stimulate blood flow to damaged tissue; it could also be used for stress-strain actuators. Other techniques include intercalation, where other elements can be placed between graphene layers with some freedom of movement.

‘We can make a film of dispersed nanoplatelets that is more than 85 per cent transparent and approaches the properties of indium tin oxide for display screens,’ Walters says.

Walters, like others in the UK sector, isn’t overly concerned with the Asian electronics firms amassing patents in the field. ‘At the moment, it works much like the pharmaceutical industry,’ he says. ‘The larger companies are waiting for smaller, more agile research-oriented companies to make breakthroughs, then they dive in with support.’

Another graphene maker, Claudio Marinelli, business development director of Applied Graphene Materials, agrees. ‘South Korean IP isn’t as much of a problem as some people think it is; in the first place, many of those patents are somewhat speculative and in all probability won’t be defensible,’ he tells The Engineer. ‘You can’t equate patents to commercialisation in this kind of field. And the UK has the largest number of experts per capita working in this field than anywhere apart from South Korea; anyone is just as likely to come through with commercial applications, and it’s a fact that the cost of development of technology is only a tenth of the cost of going to market: that’s the main parallel with pharmaceuticals and why large companies are keen to support innovation from smaller ones.’

Claudio Marinelli

“Graphene will come into its own where you need a combination of two or more of its properties, and even then you’ll have to prove that it’s better than what’s available.”
Claudio Marinelli, Applied Graphene Materials.

Unlike Perpetuus, AGM makes graphene using a bottom-up process, developed by Karl Coleman of Durham University, . But the process isn’t CVD, Marinelli insists, because although it starts with carbon in the form of a vapour of simple alcohols, it isn’t deposited on anything. ‘We prefer to call it a continuous gas-phase synthesis,’ he says. The carbon-containing vapour is brought into contact with a catalyst that isn’t incorporated into the graphene, making free nanoplatelets 2–10 graphene layers thick, and about 2–3µm in size. ‘We think this is a superior product of high purity, because with exfoliation you always have some non-exfoliated graphite in the sample,’ adds Marinelli. ‘These platelets are dispersible with surfactants, and can be used in paints, inks, coatings and composites.’ Like Mason, Marinelli expects inks to lead the commercial market by some years.

UK manufacturers tend to shun the acid-heat top-down method. ‘It produces an extremely large amount of contaminated water,’ says Liam Britnell, technical director of Bluestone UK, affiliated to the National Graphene Institute and one of the few UK producers to use CVD to make graphene sheets, depositing it onto a variety of substrates. ‘That has to be treated, which pushes the cost up and adds a lot of complexity to your processing.’

 

konstantin novoselov

Konstantin (Kostya) Novoselov in his lab at Manchester University. Novoselov shared the Nobel Prize with Andre Geim.

The challenge for graphene, as Claudio Marinelli sees it, is to transfer the properties that are predicted by theory or have been found in very small amounts of material to bulk materials or dispersions. ‘If you’re looking at exploiting any one particular property the chances are that there will be other materials available that can do it. Graphene will come into its own where you need a combination of two or more of its properties, and even then you’ll have to prove that it’s better than what’s available.’

Ian Walters puts it slightly differently. ‘Graphene is an inspiration’, he says. ‘In developing applications, you move towards the properties you want. Sometimes, it turns out you can use something else to give the same effect, but you wouldn’t have been looking at all if it weren’t for graphene.’