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ACCORDs contribution to standards in Graphene

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The Versailles Project on Advanced Materials and Standards (VAMAS) was established following an economic summit in 1982 held at Versailles by the Heads of State of the G7 group of nations and representatives from the Commission of the European Communities.

The main objective of VAMAS is to promote world trade by innovation and adoption of advanced materials through international collaborations that provide the technical basis for harmonisation of measurement methods, leading to best practices and standards.

The benefits of VAMAS includes, among others, support to the development of national and international standards through the development of test methods and procedures, provision of reliable material properties or the contribution to standard bodies leading directly to international standards.

Relevant connections, through Memorandum of Understanding between VAMAS and key bodies such as ISO and IEC have been established to ensure the rapid take-up of the work carried out, and in particular to accelerate the development of standards for advanced materials.

The Technical Work Areas (TWA) are responsible for planning and carrying out the VAMAS projects. 42 TWAs have been established, of which 17 are currently active. New/evolving advanced materials topics are under discussion for a possible creation of corresponding new TWAs.

TWA 41, a relatively young TWA, is “Graphene and Related 2D Materials”. Its objective is to validate different methodologies of measurement for graphene and related 2D materials (GR2M), including determining the uncertainties associated in measurement, sample preparation, and data analysis. Interlaboratory studies are being conducted and the results form the basis for future standardisation. 14 Project Areas have been defined, with last of them being still in progress.

Dr. Dan Hodoroaba (BAM), WP2 Leader in ACCORDs, is leading the project 13 within TWA 41 on “Lateral size of graphene oxide flakes by Scanning Electron Microscopy (SEM)” and participated in the project 12 “Lateral size and thickness measurement of few-layer graphene flakes using scanning electron microscopy (SEM) and atomic force microscopy (AFM)”. The result of these international interlaboratory comparison projects will be used directly for further development of ISO TS 23879 “Structural characterization of graphene oxide flakes: thickness and lateral size measurement using AFM and SEM” under ISO/TC 229 “Nanotechnologies”, with validated measurement procedures for the reliable and accurate evaluation of the morphology of the GR2Ms. Several standards related to the characterisation of the GR2M are under development within ISO/TC 229 “Nanotechnologies”, e. g. ISO/TS 21356-1:2021 Nanotechnologies — Structural characterization of graphene — Part 1: Graphene from powders and dispersions. Further, under TWA 2 “Surface Chemical Analysis”, the “Chemical composition of functionalized graphene with X-ray photoelectron spectroscopy (XPS)” is tested within the project A33 led by Dr. Jörg Radnik (BAM). The results of the corresponding completed ILC are just being published and the developed measurement procedures and knowledge will serve as input to ISO TS 23359 “Chemical characterisation of graphene related 2D materials in powders and suspensions” also under development under ISO/TC 229 “Nanotechnologies”.

SEM, AFM and XPS are the key techniques in ISO/AWI TS 23879 and ISO CD TS 2359, and are also part of the portfolio of analytical capabilities available in ACCORDs, where beyond the knowledge acquired in each technique, the correlation with further material characteristic properties, including biological reactivity or chemistry, will allow progressing in the development of standards and reliable methodologies for advanced materials. Analytical techniques like Energy-Dispersive X-ray Spectroscopy (EDX) coupled with an electron microscope, or Time-of-Flight Secondary Ion Mass Spectrometry (ToF-SIMS) have been proved in ACCORDs to show their potential in the reliable elemental characterisation of GR2Ms, including the imaging option. They are under discussion to be further adapted and added into the physico-chemical analysis workflow of GR2Ms along the production chain as standard measurement procedures.

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