Nanomanufacturing - Key control characteristics - Part 6-17: Graphene-based material - Order parameter: X-ray diffraction and transmission electron microscopy

IEC TS 62607-6-17:2023 establishes a standardized method to determine the key control characteristic order parameter for graphene-based material and layered carbon material by X-ray diffraction (XRD) and transmission electron microscopy.
The order parameter is analysed from two perspectives: z-axis and x-y-axis. In the z-axis the order parameter is derived from the full width at half maximum (FWHM) of peak (002) in the XRD spectrum. In the x-y-axis, it is derived from the FWHM of peak (100) corresponding to diffraction patterns obtained by SAED (selected area electron diffraction) technique, which is routinely performed on most transmission electron microscopes in the world.
The method is applicable for graphene-based material and layered carbon material including graphite, expanded graphite, amorphous carbon, vitreous carbon or glassy carbon, the structures of which are clarified by other characterization techniques.
The method is applicable for differentiating few-layer graphene or reduced graphene oxide from layered carbon material.
Typical application area is quality control in manufacturing to ensure batch-to-batch reproducibility.
NOTE Graphene oxide, one type of graphene-based material, is not within the scope of this document.

General Information

Status
Published
Publication Date
02-May-2023
Current Stage
PPUB - Publication issued
Start Date
06-Jun-2023
Completion Date
03-May-2023
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IEC TS 62607-6-17:2023 - Nanomanufacturing - Key control characteristics - Part 6-17: Graphene-based material - Order parameter: X-ray diffraction and transmission electron microscopy Released:5/3/2023
English language
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IEC TS 62607-6-17 ®
Edition 1.0 2023-05
TECHNICAL
SPECIFICATION
colour
inside
Nanomanufacturing – Key control characteristics –
Part 6-17: Graphene-based material – Order parameter: X-ray diffraction and
transmission electron microscopy

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IEC TS 62607-6-17 ®
Edition 1.0 2023-05
TECHNICAL
SPECIFICATION
colour
inside
Nanomanufacturing – Key control characteristics –

Part 6-17: Graphene-based material – Order parameter: X-ray diffraction and

transmission electron microscopy

INTERNATIONAL
ELECTROTECHNICAL
COMMISSION
ICS  07.120 ISBN 978-2-8322-6941-1

– 2 – IEC TS 62607-6-17:2023  IEC 2023
CONTENTS
FOREWORD . 4
INTRODUCTION . 6
1 Scope . 7
2 Normative references . 7
3 Terms and definitions . 7
3.1 General terms . 8
3.2 Key control characteristics measured in accordance with this document . 9
3.3 Terms related to the measurement method . 10
4 General . 11
4.1 Measurement principle . 11
4.2 Sample preparation method . 11
4.3 Description of measurement equipment and apparatus . 12
4.3.1 XRD equipment . 12
4.3.2 TEM equipment . 12
4.4 Supporting materials . 12
4.5 Ambient conditions during measurement . 12
5 Measurement procedure . 13
5.1 Calibration of measurement equipment . 13
5.2 Detailed protocol of the measurement procedure . 13
5.3 Measurement uncertainty source . 14
6 Data analysis . 14
7 Results to be reported . 15
7.1 General . 15
7.2 Product or sample identification . 15
7.3 Test conditions . 15
7.4 Measurement specific information . 15
7.4.1 Detailed explanation of the XRD measurement . 15
7.4.2 Detailed explanation of the TEM measurement . 16
7.5 Test results . 16
Annex A (informative) Format of the test report . 17
Annex B (informative) Case study: Measurement and data analysis . 20
B.1 Data analysis of XRD measurements . 20
B.2 Data analysis of TEM measurements . 21
B.3 Calculation of order parameter . 22
Bibliography . 24

Figure 1 – Different packing configurations of graphene layers in graphite powder and
graphene powder . 6
Figure 2 – A flow chart illustrating the cases when TEM measurement is needed . 14
Figure B.1 – d-spacing versus intensity of HOPG and the fitting result of peak (002) . 20
Figure B.2 – The fitting results of peak (002) of different samples . 21
Figure B.3 – The fitting results of peak (100) of amorphous carbon sample. 21
Figure B.4 – The fitting results of peak (100) of different samples . 22
Figure B.5 – The diagram of graphene area determined by order parameter . 23

Table A.1 – Product identification (in accordance with the relevant blank detail
specification) . 17
Table A.2 – General material description (in accordance with the relevant blank detail

specification) . 17
Table A.3 – Information related to XRD test . 18
Table A.4 – Information related to TEM test . 18
Table A.5 – Measurement results . 19
Table B.1 – Order parameters of different samples . 22

– 4 – IEC TS 62607-6-17:2023  IEC 2023
INTERNATIONAL ELECTROTECHNICAL COMMISSION
____________
NANOMANUFACTURING –
KEY CONTROL CHARACTERISTICS –
Part 6-17: Graphene-based material –
Order parameter: X-ray diffraction and transmission electron microscopy

FOREWORD
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IEC TS 62607-6-17 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
113/700/DTS 113/746/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.

This document was drafted in accordance with ISO/IEC Directives, Part 2, and developed in
accordance with ISO/IEC Directives, Part 1 and ISO/IEC Directives, IEC Supplement, available
at www.iec.ch/members_experts/refdocs. The main document types developed by IEC are
described in greater detail at www.iec.ch/publications.
A list of all parts in the IEC TS 62607 series, published under the general title
Nanomanufacturing – Key control characteristics, can be found on the IEC website.
The committee has decided that the contents of this document will remain unchanged until the
stability date indicated on the IEC website under webstore.iec.ch in the data related to the
specific document. At this date, the document will be
• reconfirmed,
• withdrawn,
• replaced by a revised edition, or
• amended.
IMPORTANT – The "colour inside" logo on the cover page of this document indicates that it
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– 6 – IEC TS 62607-6-17:2023  IEC 2023
INTRODUCTION
Graphite is composed of layers of carbon atoms just a single atom in
...

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