IEC TS 62607-6-21:2022

Nanomanufacturing - Key control characteristics - Part 6-21: Graphene-based material - Elemental composition, C/O ratio: X-ray photoelectron spectroscopy

IEC TS 62607-6-21:2022 establishes a standardized method to determine the chemical key control characteristics
- elemental composition, and
- C/O ratio
for powders of graphene-based materials by
- X-ray photoelectron spectroscopy (XPS).
The elemental composition (species and relative abundance) is derived by the elemental binding energy and integral peak area at corresponding portion of XPS spectrum.
- The elemental composition refers to main elements in graphene powders, typically including carbon (C), oxygen (O), nitrogen (N), sulfur (S) , chloride (Cl) and silicon (Si).
- This document is applicable to graphene powders consisting of graphene, bilayer graphene (2LG), trilayer graphene (3LG), few-layer graphene (FLG), graphene nanoplate (GNP), reduced graphene oxide (rGO), graphene oxide (GO), and functionalized graphene powders.
- Typical application areas are the microelectronics and thermal management industries, e.g. batteries, integrated circuits, high-frequency electronics. This document can be used by manufacturers in research and development and by downstream users for product selection.

General Information

• Status: Published
• Publication Date: 21-Sep-2022
• ICS: 07.030 - Physics. Chemistry
• ICS: 07.120 - Nanotechnologies
• Technical Committee: TC 113 - Nanotechnology for electrotechnical products and systems
• Drafting Committee: WG 8 - TC 113/WG 8
• Current Stage: PPUB - Publication issued
• Start Date: 17-Oct-2022
• Completion Date: 22-Sep-2022

Standards Content (Sample)

IEC TS 62607-6-21 ®
Edition 1.0 2022-09
TECHNICAL
SPECIFICATION
colour
inside
Nanomanufacturing – Key control characteristics –
Part 6-21: Graphene-based material – Elemental composition, C/O ratio: X-ray
photoelectron spectroscopy
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IEC TS 62607-6-21 ®
Edition 1.0 2022-09
TECHNICAL
SPECIFICATION
colour
inside
Nanomanufacturing – Key control characteristics –

Part 6-21: Graphene-based material – Elemental composition, C/O ratio: X-ray

photoelectron spectroscopy
INTERNATIONAL
ELECTROTECHNICAL
COMMISSION
ICS 07.120; 07.030 ISBN 978-2-8322-5700-5

– 2 – IEC TS 62607-6-21:2022  IEC 2022
CONTENTS
FOREWORD . 4
INTRODUCTION . 6
1 Scope . 7
2 Normative references . 7
3 Terms and definitions . 7
3.1 General terms . 7
3.2 Key control characteristics measured in accordance with this document . 9
4 General . 10
4.1 Measurement instrument . 10
4.2 Calibration of measurement instrument . 10
4.3 Charge control . 10
4.4 Quantitative analysis . 11
5 Measurement procedure . 12
5.1 Sample preparation . 12
5.2 Measurement conditions . 12
5.3 Measurement procedure . 12
6 Data analysis . 13
7 Uncertainty estimation . 13
8 Measurement report . 13
8.1 General . 13
8.2 Test sample identification . 13
8.3 Ambient conditions. 13
8.4 Instrumental information . 14
8.5 Measurement specific information . 14
8.6 Measurement results . 14
Annex A (informative) Relative sensitivity factors . 15
A.1 Overview. 15
A.2 Elemental relative sensitivity factors . 16
A.2.1 General . 16
A.2.2 Pure-element relative sensitivity factors . 16
A.2.3 Elemental relative sensitivity factors from measurements with
compounds . 16
A.2.4 Set of elemental relative sensitivity factors . 16
Annex B (informative) Discussion about the influence of surface contamination . 17
B.1 Sampling depth . 17
B.2 Test study of surface contamination . 18
Annex C (informative) Case study for GNP . 20
C.1 Test sample . 20
C.2 Measurement results using XPS . 20
Annex D (informative) Case study for GO . 24
D.1 Test sample . 24
D.2 Measurement results . 24
Bibliography . 26

Figure 1 – Illustration of XPS peak measured . 11

Figure 2 – Digital photos of test samples as pressed pellet of graphene powder on
different substrates . 12
Figure B.1 – Schematic diagram of sampling depth and XPS spectra . 17
Figure B.2 – Data distribution of relative abundance of C 1s at five test positions
through long-time vacuum desorption treatment . 18
Figure B.3 – XPS spectra of C 1s through thermal desorption of different temperatures
for 1 h . 19
Figure C.1 – Morphologies of GNP sample . 20
Figure C.2 – Survey spectrum of GNP test sample . 21
Figure C.3 – XPS spectra of the main elements of C 1s, O 1s, N 1s, Cl 2p and S 2p
peaks in GNP test sample . 22
Figure C.4 – Data distribution of relative abundance of C, O, and N elements and C/O
ratio of eleven test positions in GNP test sample . 23
Figure D.1 – Data distribution of relative abundance of C, O, S and N elements and
C/O ratio of twelve test positions in GO test sample . 25

Table 1 – Reference values for the peak positions on the binding-energy scale, E . 10
ref n
Table B.1 – Relative abundance of C 1s at different times of vacuum desorption . 19
Table B.2 – Relative abundance of C 1s through vacuum desorption under different
temperatures for 1 h . 19
Table C.1 – Relative abundance of main elements and C/O ratio in GNP test sample . 23
Table D.1 – Relative abundance of main elements and C/O ratio in GO test sample . 24

– 4 – IEC TS 62607-6-21:2022  IEC 2022
INTERNATIONAL ELECTROTECHNICAL COMMISSION
____________
NANOMANUFACTURING – KEY CONTROL CHARACTERISTICS –

Part 6-21: Graphene-based material – Elemental composition,
C/O ratio: X-ray photoelectron spectroscopy

FOREWORD
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IEC TS 62607-6-21 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
...