IEC TS 62607-6-14:2020

Nanomanufacturing - Key control characteristics - Part 6-14: Graphene-based material - Defect level: Raman spectroscopy

IEC TS 62607-6-14:2020 establishes a standardized method to determine the structural key control characteristic
• defect level
for powders consisting of graphene-based material by
• Raman spectroscopy.
The defect level is derived by the intensity ratio of the D+D′ band and 2D band in Raman spectrum, ID+D′/I2D.
• The defect level determined in accordance with 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 graphene powder or graphene-based material, e.g. reduced graphene oxide (rGO), bilayer graphene, trilayer graphene and few-layer graphene.
• Typical application areas are quality control and classification for graphene manufacturers, and product selection for downstream users.
• The method described in this document is appropriate if the physical form of graphene is powder.

General Information

• Status: Published
• Publication Date: 26-Oct-2020
• ICS: 07.120 - Nanotechnologies
• Technical Committee: TC 113 - Nanotechnology for electrotechnical products and systems
• Drafting Committee: PT 62607-6-14 - TC 113/PT 62607-6-14
• Current Stage: PPUB - Publication issued
• Start Date: 12-Nov-2020
• Completion Date: 27-Oct-2020

Standards Content (Sample)

IEC TS 62607-6-14 ®
Edition 1.0 2020-10
TECHNICAL
SPECIFICATION
colour
inside
Nanomanufacturing – Key control characteristics –
Part 6-14: Graphene-based material – Defect level: Raman spectroscopy

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IEC TS 62607-6-14 ®
Edition 1.0 2020-10
TECHNICAL
SPECIFICATION
colour
inside
Nanomanufacturing – Key control characteristics –

Part 6-14: Graphene-based material – Defect level: Raman spectroscopy

INTERNATIONAL
ELECTROTECHNICAL
COMMISSION
ICS 07.120 ISBN 978-2-8322-8940-2

– 2 – IEC TS 62607-6-14:2020  IEC:2020
CONTENTS
FOREWORD . 4
INTRODUCTION . 6
1 Scope . 8
2 Normative references . 8
3 Terms and definitions . 8
3.1 General terms . 8
3.2 Key control characteristics measured in accordance with this document . 11
4 General . 11
4.1 Measurement principle . 11
4.2 Sample preparation method . 12
4.3 Description of measurement equipment/apparatus . 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 accuracy . 13
5.4 Measurement uncertainty source . 13
6 Sampling plan . 13
7 Data analysis / interpretation of results . 13
8 Results to be reported . 14
8.1 General . 14
8.2 Product/sample identification . 14
8.3 Test conditions . 14
8.4 Measurement specific information . 14
8.5 Test results . 14
Annex A (informative) Recommended format of the test report . 15
Annex B (informative) Sampling plan . 17
Annex C (informative) Case study: measurement and data analysis . 18
C.1 Step 1: sample preparation . 18
C.2 Step 2: Raman test . 18
C.3 Step 3: Raman spectra processing . 18
C.4 Step 4: Data analysis . 19
Annex D (informative) Why use the intensity ratio I /I for defect level
D+D′ 2D
characterization of graphene powder? . 22
D.1 Interpretation of characteristic bands in the Raman spectrum of graphene
and Raman scattering mechanism . 22
D.2 Example – Influence of edges in the Raman spectrum of graphene . 22
D.3 Example – Influence of defect in the Raman spectrum of single layer
graphene . 24
D.4 Example – Raman characteristics of reduced graphene sheet . 26
D.5 Conclusion . 27
Bibliography . 28

Figure 1 – Schematic diagram of Raman scattering processes in realistic graphene
material . 6

Figure 2 – Different packing configurations of graphene flakes in film (left) and powder
(right) . 6
Figure 3 – Schematic drawing of Raman spectra of defective graphene (upper) and

pristine graphene (bottom) . 12
Figure 4 – Schematic drawing of sample preparation method . 12
Figure B.1 – Schematic drawing of five-point-sampling method . 17
Figure B.2 – Location of measurement points . 17
Figure C.1 – The field view of graphene sample beneath Raman microscope . 18
Figure C.2 – The procedure of Raman spectrum processing . 19
Figure C.3 – Typical Raman spectrum after processing . 20
Figure C.4 – The overall defect level of one test sample . 21
Figure C.5 – Measurement results of different testing organizations . 21
Figure D.1 – Characteristic bands in the Raman spectrum of graphene and Raman
processes [6] . 22
Figure D.2 – Raman spectra from the edges of a monolayer graphene sample [9] . 23
Figure D.3 – Raman spectra obtained from monolayer graphene samples with
hexagonal and circular holes [10] . 23
Figure D.4 – Raman spectra for four different ion doses in graphene [1] . 24
Figure D.5 – E [I /I ] as a function of L [2] . 24
L D G D
Figure D.6 – (a) Definition of the activated A-region (green) and structurally-
disordered S-region (red). (b-e) Snapshots of the structural evolution of the graphene
sheet for different defect concentrations [1] . 25
Figure D.7 – Evolution of 2D and other second-order bands with increasing ion doses
[5] . 25
Figure D.8 – Raman characteristics of as-made graphene sheet and different types of
reduced graphene sheet film samples: (a) Raman spectra; (b) D/G intensity ratios; (c)
S3/2D intensity ratios [7] . 26
Figure D.9 – Resistivity of as-made graphene sheet and different types of reduced
graphene sheet [7] . 26

Table A.1 – Product identification (in accordance with IEC 62565-3-1) . 15
Table A.2 – General material description (in accordance with IEC 62565-3-1). 15
Table A.3 – Information related with test . 16
Table A.4 – Measurement results . 16
Table C.1 – Average I ′/I of each test point . 20
D+D 2D
– 4 – IEC TS 62607-6-14:2020  IEC:2020
INTERNATIONAL ELECTROTECHNICAL COMMISSION
____________
NANOMANUFACTURING – KEY CONTROL CHARACTERISTICS –

Part 6-14: Graphene-based material – Defect level: Raman spectroscopy

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