Nanomanufacturing - Key control characteristics - Part 6-18: Graphene-based material - Functional groups: TGA-FTIR

IEC TS 62607-6-18:2022(E) establishes a standardized method to determine the chemical key control characteristic
functional groups  for functionalized graphene-based material and graphene oxide by
thermogravimetry analysis (TGA) coupled with Fourier transform infrared spectroscopy (FTIR), referred to as TGA-FTIR.  The content of functional groups is derived by changes in mass of the sample as a function of temperature using TGA. Materials evolved during these mass changes are then analysed using coupled FTIR to identify functional groups.
The functional groups determined according to this document will be listed as a key control characteristic in the blank detail specification for graphene IEC 62565-3-1 for graphene powder.
The method is applicable for functionalized graphene powder and graphene oxide that can be pyrolysed and gasified with elevated temperature during TGA.
Typical application areas are quality control for graphene manufacturers, and product selection for downstream users.

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IEC TS 62607-6-18:2022 - Nanomanufacturing - Key control characteristics - Part 6-18: Graphene-based material - Functional groups: TGA-FTIR Released:12/14/2022
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IEC TS 62607-6-18 ®
Edition 1.0 2022-12
Nanomanufacturing – Key control characteristics –
Part 6-18: Graphene-based material – Functional groups: TGA-FTIR
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IEC TS 62607-6-18 ®
Edition 1.0 2022-12
Nanomanufacturing – Key control characteristics –

Part 6-18: Graphene-based material – Functional groups: TGA-FTIR

ICS 07.120 ISBN 978-2-8322-6223-8

– 2 – IEC TS 62607-6-18:2022  IEC 2022
1 Scope . 6
2 Normative references . 6
3 Terms and definitions . 6
4 General . 9
4.1 Measurement principle . 9
4.2 Sample preparation method . 9
4.3 Measurement system . 9
4.4 Description of measurement equipment . 9
4.5 Supporting materials . 9
4.6 Ambient conditions during measurement . 10
5 Measurement procedure . 10
5.1 Calibration of measurement equipment . 10
5.2 Detailed protocol of the measurement procedure . 10
6 Data analysis . 11
7 Results to be reported . 12
7.1 General . 12
7.2 Product or sample identification . 12
7.3 Test conditions . 12
7.4 Measurement specific information . 12
7.5 Test results . 12
Annex A (informative) Format of the test report . 13
Annex B (informative) Case study: Data analysis . 15
B.1 Confirmation of characteristic temperature points from TGA curve . 15
B.2 Analysis of FTIR spectra obtained at different ashing temperatures . 15
B.3 Analysis of FTIR spectra obtained by TGA-FTIR measurements . 16
B.4 Confirmation and quantification of the functional groups . 17
Bibliography . 19

Figure 1 – Flow chart of data analysis . 11
Figure B.1 – Weight loss curve (left) obtained from TGA-FTIR measurement and
corresponding differential weight loss curve (right) . 15
Figure B.2 – FTIR spectra corresponding to different ashing temperature points . 15
Figure B.3 – A 3D FTIR spectrum obtained by one FTIR-TGA measurement . 16
Figure B.4 – Absorption dynamics of each gas component . 17
Figure B.5 – Absorption dynamics of each gas component . 17
Figure B.6 – Weight loss dynamics of each gas component . 18

Table A.1 – Product identification (in accordance with IEC 62565-3-1) . 13
Table A.2 – General material description (in accordance with IEC 62565-3-1). 13
Table A.3 – Test information . 14
Table A.4 – Measurement results . 14


Part 6-18: Graphene-based material – Functional groups: TGA-FTIR

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IEC TS 62607-6-18 has been prepared by IEC technical committee 113: Nanotechnology for
electrotechnical products and systems. It is a Technical Specification.
The text of this Technical Specification is based on the following documents:
Draft Report on voting
113/680/DTS 113/706/RVDTS
Full information on the voting for its approval can be found in the report on voting indicated in
the above table.
The language used for the development of this Technical Specification is English.
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– 4 – IEC TS 62607-6-18:2022  IEC 2022
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Nanomanufacturing – Key control characteristics, can be found on the IEC website.
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One of the most well-studied routes for the preparation of graphene is the oxidation and
reduction process. The most cost-effective process to obtain graphene is the exfoliation of
natural graphite layers after oxidation to get individual oxidized layers and then de-oxygenation
(reduction) of these individual layers [1], [2] . During the oxidation process, various
functionalized groups (-OH, -O-, -COOH, C=O, etc.) go into the graphene skeleton, breaking
the π bond of graphene structure [3]. Oxygen attachment to graphene in any chemical form
(epoxide, hydroxyl, carboxyl and ketonic-type functional groups) both on the basal plane and at
the edges reduces electronic states at the Fermi level [4], [5], [6]. The type and content of
functional groups affect the physiochemical properties of graphene. Therefore, the identification
and quantification of functional groups on graphene powder is believed to be a key control
characteristic for its production and application.
Coupling thermal gravimetric analysis (TGA) and Fourier transform infrared spectroscopy (FTIR)
is an excellent solution to identify and quantify functional groups on graphene powder. In TGA-
FTIR, while mass changes such as sample pyrolysis and vaporization that accompany changes
in temperature are measured quantitatively by the TGA, qualitative analysis of the gaseous
components can be conducted simultaneously by FTIR measurement of the obtained spectra.

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