Tag Archives: UK National Physical Laboratory NPL

A standard for determining what it means to be graphene

How do you know if your ‘graphene’ light bulb has any graphene in it? How do you know if your orange juice is 100% orange juice? The answer to those questions is that you don’t. So, you must hope there are standards and regulations governing the answers. You must also hope that there are incentives (fines and/or jail time) for obeying those regulations.

In a March 15, 2021 news item on Nanowerk, you’ll find an announcement from the UK’s National Physical Laboratory about an international standard for graphene (Note: A link has been removed),

The National Physical Laboratory (NPL) in the UK in collaboration with international partners, have developed an ISO/IEC [International Standards Organization/International Electrotechnical Commission] standard, ISO/TS 21356-1:2021, for measuring the structural properties of graphene, typically sold as powders or in a liquid dispersion. The ISO/IEC standard allows the supply chain to answer the question ‘what is my material?’ and is based on methods developed with The University of Manchester in the NPL Good Practice Guide 145.

A March ??, 2021 NPL press release, which originated the news item, provides more details,

Over the last few years, graphene, a 2D material with many exciting properties and just one atom thick, has moved from the laboratory into real-world products such as cars and smartphones. However, there is still a barrier affecting the rate of its commercialisation, namely, understanding the true properties of the material. There is not just one type of material, but many, each with different properties that need matching to the many different applications where graphene can provide an improvement.

With hundreds of companies across the globe selling different materials labelled as ‘graphene’, and manufacturing it in different ways, end users who want to improve their products by incorporating few-layer graphene flakes are unable to compare and subsequently select the right material for their product.

Through standardised methods to enable the reliable and repeatable measurement of properties, such as the lateral flake size, flake thickness, level of disorder and specific surface area, industry will be able to compare the many materials available and instil trust in the supply chain.  In conjunction with the international ISO/IEC terminology standard led by NPL, ISO/TS 80004-13:2017, it will be possible for commercially available material to be correctly measured and labelled as graphene, few-layer graphene or graphite.

As the UK’s National Metrology Institute, NPL has been developing and standardising the required metrologically-robust methods for the measurement of graphene and related 2D materials to enable industry to use these materials and realise novel and improved products across many application areas.

The continuation of the NPL-led standardisation work within ISO TC229 (nanotechnologies) will allow the chemical properties of graphene related 2D materials to be determined, as well as the structural properties for different forms of graphene material, such as CVD-grown graphene. This truly international effort to standardise the framework of measurements for graphene is described in more detail in Nature Reviews Physics, including further technical discussion on the new ISO graphene measurement standard.

Dr Andrew J Pollard, Science Area Leader at NPL said: “It is exciting to see this new measurement standard now available for the growing graphene industry worldwide. Based on rigorous metrological research, this standard will allow companies to confidently compare technical datasheets for the first time and is the first step towards verified quality control methods.”

Dr Charles Clifford, Senior Research Scientist at NPL said: “It is fantastic to see this international standard published after several years of development.  To reach international consensus especially across the 37 member countries of ISO TC229 (nanotechnologies) is a testament both to the global interest in graphene and the importance of international cooperation.”

James Baker, CEO of Graphene@Manchester said: “Standardisation is crucial for the commercialisation of graphene in many different applications such as construction, water filtration, energy storage and aerospace. Through this international measurement standard, companies in the UK and beyond will be able to accelerate the uptake of this 21st Century material, now entering many significant markets.”

Here are links to the new standard ISO/TS 21356-1:2021 (Nanotechnologies — Structural characterization of graphene — Part 1: Graphene from powders and dispersions} and the NPL/University of Manchester’s 2017 edition of the Good Practice Guide.

Here’s a second link to the article along with a citation,

The importance of international standards for the graphene community by Charles A. Clifford, Erlon H. Martins Ferreira, Toshiyuki Fujimoto, Jan Herrmann, Angela R. Hight Walker, Denis Koltsov, Christian Punckt, Lingling Ren, Gregory J. Smallwood & Andrew J. Pollard. Nature Reviews Physics (2021) DOI: https://doi.org/10.1038/s42254-021-00278-6 Published 15 March 2021

This paper is behind a paywall.

Searchable database for hazardous nanomaterials and a Graphene Verification Programme

I have two relatively recent news bits about nanomaterials, the second being entirely focused on graphene.

Searchable database

A July 9, 2019 news item on Nanowerk announces a means of finding out what hazards may be associated with 300 different nanomaterials (Note: A Link has been removed),

A new search tool for nanomaterials has been published on the European Union Observatory for Nanomaterials (EUON) website. It will enable regulators to form a better view of available data and give consumers access to chemicals safety information.

The tool combines data submitted by companies in their REACH registrations [Registration, Evaluation, Authorisation and Restriction of Chemicals (REACH) ], data collected about nanomaterials used as ingredients in cosmetic products under the Cosmetics Regulation and data from the public national nanomaterial inventories of Belgium and France.

A July 3, 2019 EUON press release, which originated the news item, provides a bit more detail,

The EUON’s search brings data from these sources together in one place, allowing users to easily search for nanomaterials that are currently on the EU market. The results are linked to ECHA’s [European Chemicals Agency] database of chemicals registered in the EU and, for the first time, summarised information about the substances, their properties as well as detailed safety and characterisation data can be easily found.

Background

While there are over 300 nanomaterials on the EU market, 37 are currently covered by an existing registration under REACH. The information requirements for REACH were revised last year with explicit obligations for nanomaterials manufactured in or imported to the EU. The new requirements enter into force in January 2020 and will result in more publicly available information.

The EUON aims to increase the transparency of information available to the public on the safety and markets of nanomaterials in the EU. A key aim of the observatory is to create a one-stop shop for information, where EU citizens and stakeholders including NGOs, industry, and regulators can all easily find accessible and relevant safety information on nanomaterials on the EU market.

Here’s the searchable database.

Graphene verification

There was a bit of a scandal about fake graphene in the Fall of 2018 (my May 28, 2019 posting gives details). Dexter Johnson provides additional insight and information about the launch of a new graphene verification programme and news of a slightly older graphene verification programme in his July 9, 2019 article for the Nanoclast blog on the IEEE (Institute of Electrical and Electronics Engineers) website (Note: Links have been removed),

Last year [2018], the graphene community was rocked by a series of critical articles that appeared in some high-profile journals. First there was an Advanced Material’s article with the rather innocuously title: “The Worldwide Graphene Flake Production”. It was perhaps the follow-up article that appeared in the journal Nature that really shook things up with its incendiary title: “The war on fake graphene”.

In these two articles it was revealed that material that had been claimed to be high-quality (and high-priced) graphene was little more than graphite powder. Boosted by their appearance in high-impact journals, these articles threatened the foundations of the graphene marketplace.

But while these articles triggered a lot of hand wringing among the buyers and sellers of graphene, it’s not clear that their impact extended much beyond the supply chain of graphene. Whether or not graphene has aggregated back to being graphite is one question. An even bigger one is whether or not consumers are actually being sold a better product on the basis that it incorporates graphene.

Dexter details some of the issues from the consumer’s perspective (Note: Links have been removed),

Consumer products featuring graphene today include everything from headphones to light bulbs. Consequently, there is already confusion among buyers about the tangible benefits graphene is supposed to provide. And of course the situation becomes even worse if the graphene sold to make products may not even be graphene: how are consumers supposed to determine whether graphene infuses their products with anything other than a buzzword?

Another source of confusion arises because when graphene is incorporated into a product it is effectively a different animal from graphene in isolation. There is ample scientific evidence that graphene when included in a material matrix, like a polymer or even paper, can impart new properties to the materials. “You can transfer some very useful properties of graphene into other materials by adding graphene, but just because the resultant material contains graphene it does not mean it will behave like free-standing graphene, explains Tom Eldridge, of UK-based Fullerex, a consultancy that provides companies with information on how to include graphene in a material matrix

The rest of Dexter’s posting goes on to mention two new graphene verification progammes (producer and product) available through The Graphene Council. As for what the council is, there’s this from council’s About webpage,

The Graphene Council was founded in 2013 with a mission to serve the global community of graphene professionals. Today, The Graphene Council is the largest community in the world for graphene researchers, academics, producers, developers, investors, nanotechnologists, regulatory agencies, research institutes, material science specialists and even the general public. We reach more than 50,000 people with an interest in this amazing material. 

Interestingly the council’s offices are located in the US state of North Carolina. (I would have guessed that its headquarters would be in the UK, given the ‘ownership’ the UK has been attempting to establish over graphene Let me clarify, by ownership I mean the Brits want to be recognized as dominant or preeminent in graphene research and commercialization.)

The council’s first verified graphene producer is a company based in the UK as can be seen in an April 1, 2019 posting by council director Terrance Barkan on the council’s blog,

The Graphene Council is pleased to announce that Versarien plc is the first graphene company in the world to successfully complete the Verified Graphene Producer™ program, an independent, third party verification system that involves a physical inspection of the production facilities, a review of the entire production process, a random sample of product material and rigorous characterization and testing by a first class, international materials laboratory.

The Verified Graphene Producer™ program is an important step to bring transparency and clarity to a rapidly changing and opaque market for graphene materials, providing graphene customers with a level of confidence that has not existed before.

“We are pleased to have worked with the National Physical Laboratory (NPL) in the UK, regarded as one of the absolute top facilities for metrology and graphene characterization in the world.
 
They have provided outstanding analytical expertise for the materials testing portion of the program including Raman Spectroscopy, XPS, AFM and SEM testing services.” stated Terrance Barkan CAE, Executive Director of The Graphene Council.
 
Andrew Pollard, Science Area Leader of the Surface Technology Group, National Physical Laboratory, said: “In order to develop real-world products that can benefit from the ‘wonder material’, graphene, we first need to fully understand its properties, reliably and reproducibly.
 
“Whilst international measurement standards are currently being developed, it is critical that material characterisation is performed to the highest possible level.
 
As the UK’s National Measurement Institute (NMI) with a focus on developing the metrology of graphene and related 2D materials, we aim to be an independent third party in the testing of graphene material for companies and associations around the world, such as The Graphene Council.” 
 
Neill Ricketts, CEO of Versarien said: “We are delighted that Versarien is the first graphene producer in the world to successfully complete the Graphene Council’s Verified Graphene Producer™ programme.”
 
“This is a huge validation of our technology and will enable our partners and potential customers to have confidence that the graphene we produce meets globally accepted standards.”
 
“There are many companies that claim to be graphene producers, but to enjoy the benefits that this material can deliver requires high quality, consistent product to be supplied.  The Verified Producer programme is designed to verify that our production facilities, processes and tested material meet the stringent requirements laid down by The Graphene Council.”

“I am proud that Versarien has been independently acclaimed as a Verified Graphene Producer™ and look forward to making further progress with our collaboration partners and numerous other parties that we are in discussions with.”

James Baker CEng FIET, the CEO of Graphene@Manchester (which includes coordinating the efforts of the National Graphene Institute and the Graphene Engineering and Innovation Centre [GEIC]) stated: “We applaud The Graphene Council for promoting independent third party verification for graphene producers that is supported by world class metrology and characterization services.”

“This is an important contribution to the commercialization of graphene as an industrial material and are proud to have The Graphene Council as an Affiliate Member of the Graphene Engineering and Innovation Centre (GEIC) here in Manchester ”.

Successful commercialization of graphene materials requires not only the ability to produce graphene to a declared specification but to be able to do so at a commercial scale.
It is nearly impossible for a graphene customer to verify the type of material they are receiving without going through an expensive and time consuming process of having sample materials fully characterized by a laboratory that has the equipment and expertise to test graphene.

The Verified Graphene Producer™ program developed by The Graphene Councilprovides a level of independent inspection and verification that is not available anywhere else.

As for the “Verified Graphene Product” programme mentioned in Dexter’s article (it’s not included in the excerpts here), I can’t find any sign of it ion the council’s website.

International centre for testing graphene opens in China

An international graphene measurement centre opened in Oct. 2015 but the official launch seems to have just started. A Nov. 23, 2015 news item on Nanowerk makes the announcement,

The China-UK collaborative effort to support the development an international graphene standards and testing centre was officially launched at Zhongguancun Fengtai Science Park, Beijing, China, in October 2015. As the demand for international standards for testing graphene increases, the Centre in Beijing will lay the foundation for the development of graphene industry and high-end applications in China.

A Nov. 23, 2015 UK National Physical Laboratory (NPL) press release, which originated the news item, describes the October 2015 launch in more detail,

A China-UK graphene conference was held as part of the launch activities on the 24 October 2015 and graphene experts from China and the UK’s National Physical Laboratory (NPL) discussed graphene R&D progress and the development of graphene international standards; the discussions included NPL’s work in this area and the related testing methods.

The graphene conference was part of a programme of activities between NPL, Beijing Zhongguancun Fengtai Science Park and the associated Beijing Fengtai New Materials Inspection Institute (BFM) agreed in a Memorandum of Understanding signed in Spring 2015, to support the development of standards and testing in China. Efforts are being made to promote the implementation of standards in China and to introduce new methods of measurement by establishing non-contact and contact-type testing facilities for electrical and structural properties of graphene and other 2D materials at the centre. During the conference, the Chinese Association for Promoting Cooperation between Universities and Industries agreed a strategic cooperation for the centre, which will enable the integration and utilisation of the resources of universities and research institutes. This will lead to knowledge transfer and dissemination of testing standards for the establishment of China’s graphene characterisation platform and applications platform.

The Vice Mayor of Fengtai District, and Fengtai Park director, Jie Zhang (张婕), said that the Zhongguancun Fengtai Park is now actively building an international graphene centre, and that the cooperation of NPL and other international research teams will be instrumental to the success of the centre. NPL’s Principal Research Scientist, Ling Hao (郝玲), added that the partnership with Fengtai Science Park, BFM and other Chinese organisations will be “a win-win collaboration” for graphene research, development and application for both the UK and China.

Executive Chairman of the China Industry-University-Research Institute Collaboration Association (CIUR) Prof Wang Jianhua (王建华) said that graphene international standards and testing is key to national development of a graphene industry. He continued that the China-UK conference will further promote cooperation in graphene research, strengthening resource integration in graphene certification through testing and standards, all will contribute to these exciting R&D developments.

Stephanie Kitchen, Andrew Pollard, Tim Prior and Ling Hao of NPL also made presentations at the China-UK conference and delegates from China National Institute of Standardization, Beijing Institute of Metrology, Beijing Institute of Technology gave presentations and many other research and development institutions attended this conference.

The Brits have been amazing where graphene is concerned. They have been tireless about promoting it and themselves as leaders in the field and this is one more notch on their belt. Just prior to the Graphene Flagship winning one of two places (in 2013) for 1B Euros in research funding over 10 years, I wrote a series of posts (Feb. 2, 2012 starts the series, followed by Feb. 6, 2012, and then there was Feb. 21, 2012) where I expressed my admiration for the Brits’ stellar efforts.