IEC TS 62607-6-1:2020
(Main)Nanomanufacturing - Key control characteristics - Part 6-1: Graphene-based material - Volume resistivity: four probe method
Nanomanufacturing - Key control characteristics - Part 6-1: Graphene-based material - Volume resistivity: four probe method
IEC TS 62607-6-1:2020 establishes a standardized method to determine the electrical key control characteristic
– volume resistivity
for powder consisting of graphene-based material like flakes of graphene, few layer graphene and/or reduced graphene oxide after preparation of a sample in pellet form by
– four probe method
using powder resistivity measurement system.
The volume resistivity is a measure of the quality of powder-type graphene products in terms of electrical property and reflects the density-dependency shown in a pellet of powder-type graphene.
The volume conductivity can directly be derived from the volume resistivity.
Typical application areas are industries that use powder-type graphene products for graphene manufacture, potential developers, and users who produce graphene-based products. As the volume resistivity measured according to this document requires the preparation of a sample in the form of a pellet, this document describes in detail
– an apparatus to prepare consistently a test sample, the pellet,
– the preparation of the pellet starting from powder-type graphene,
– the measurement procedure to measure the volume resistivity (or volume conductivity) of the pellet, and
– the data analysis, the interpretation and reporting of the results.
General Information
Standards Content (Sample)
IEC TS 62607-6-1 ®
Edition 1.0 2020-07
TECHNICAL
SPECIFICATION
colour
inside
Nanomanufacturing – Key control characteristics –
Part 6-1: Graphene-based material – Volume resistivity: four probe method
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IEC TS 62607-6-1 ®
Edition 1.0 2020-07
TECHNICAL
SPECIFICATION
colour
inside
Nanomanufacturing – Key control characteristics –
Part 6-1: Graphene-based material – Volume resistivity: four probe method
INTERNATIONAL
ELECTROTECHNICAL
COMMISSION
ICS 07.120 ISBN 978-2-8322-8561-9
– 2 – IEC TS 62607-6-1:2020 © IEC 2020
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 . 8
3.3 Terms related to measurements . 8
4 Sample preparation . 10
5 Measurement of volume resistivity of graphene pellet . 10
5.1 Description of the measurement apparatus . 10
5.2 Determination of sample amount . 12
5.3 The measurement procedures . 12
6 Data analysis and interpretation of results . 12
6.1 General . 12
6.2 Analysis of volume resistivity as a function of the applied pressures . 13
6.3 Calculation of volume conductivity of a pellet . 13
6.4 Analysis of volume resistivity (or volume conductivity) as a function of the
volume density of graphene pellet . 13
7 Report . 14
Annex A (informative) Case studies . 15
A.1 Graphene (reduced graphene oxide (rGO) and graphene nanopowder
(GNP)) . 15
A.2 Morphology change of rGO flakes before and after pressurization. 15
A.3 Raman spectroscopy measurement of graphene powder before and after
pressurization up to 52 MPa. 16
A.4 Results on powder resistivity measurements . 17
A.4.1 Powder resistivity measurement of rGO-A (company 1) with various
amounts . 17
A.4.2 Powder resistivity measurement of 1,0 g of rGO-B (company 2). 19
A.4.3 Powder resistivity measurement of GNP . 22
A.4.4 Powder resistivity measurement of graphene oxides with different
amounts of oxygen . 26
Bibliography . 32
Figure 1 – Measurement system . 11
Figure A.1 – FE-SEM images of rGO flakes of (A) Company 1 (rGO-A), (B) Company 2
(rGO-B) and (C) graphene nanopowder (GNP) before (left) and after (right)
pressurization . 15
Figure A.2 – Raman spectra of (A) rGO-A, (B) rGO-B and (C) GNP before (black line)
and after (red line) pressurization . 16
Figure A.3 – Comparison data for I /I of rGO-A (short-dash line), rGO-B (solid line)
D G
and GNP (long-dash line) before and after pressurization . 16
Figure A.4 – Correlation plots of (A) thickness, (B) volume resistivity (ρ ), and (C)
v
volume conductivity (σ ) as a function of the applied pressure: (1) 0,1 g and (2) 0,2 g
v
of rGO-A . 18
Figure A.5 – Correlation plots of (A) volume resistivity (ρ ) and (B) volume conductivity
v
(σ ) as a function of the volume density (d ) of a graphene pellet: 0,1 g (filled symbol)
v v
and 0,2 g (unfilled symbol) of rGO-A . 19
Figure A.6 – Correlation plots of (A) thickness (t), (B) volume resistivity (ρ ), and
v
(C) volume conductivity (σ ) of rGO-B (1,0 g) as a function of the applied pressure . 19
v
Figure A.7 – Correlation plots of (A) volume resistivity (ρ ) and (B) volume conductivity
v
(σ ) of rGO-B (1,0 g) as a function of the volume density (d ) of the graphene pellet . 20
v v
Figure A.8 – Correlation plots of (A) volume resistivity (ρ ) and (B) volume conductivity
v
(σ ) as a function of the volume density (d )of graphene pellets: 0,1 g (filled symbol),
v v
0,2 g (unfilled symbol) of rGO-A and 1,0 g (lined symbol) of rGO-B . 20
Figure A.9 – Correlation plots of (A) thickness (t), (B) volume resistivity (ρ ), and (C)
v
volume conductivity (σ ) as a function of the applied pressure: (1) 0,1 g and (2) 0,2 g
v
of GNP . 22
Figure A.10 – Correlation plots of (A) volume resistivity (ρ ) and (B) volume
v
conductivity (σ ) as a function of the volume density (d ) of a graphene pellet: 0,1 g
v v
(filled symbol) and 0,2 g (unfilled symbol) of GNP . 23
Figure A.11 – Comparison plots of (A) volume resistivity (ρ ) and (B) volume
v
conductivity (σ ) as a function of the volume density (d ) of graphene pellets: rGO-A
v v
(filled symbol) and GNP (unfilled symbol). 23
Figure A.12 – XPS survey spectra of as-received (A) rGO-A, (B) rGO-B and (C) GNP . 24
Figure A.13 – Correlation plots of thickness (t) as a function of the applied pressure:
0,3 g samples of four types of graphene oxide (G-a, G-b, G-c, and G-d) . 26
Figure A.14 – Correlation plots of volume resistivity (ρ ) as a function of the applied
v
pressure: 0,3 g samples of four types of graphene oxide (G-a, G-b, G-c, and G-d) . 27
Figure A.15 – Correlation plots of volume conductivity (σ ) as a function of the applied
v
pressure: 0,3 g samples of four types of graphene oxide (G-a, G-b, G-c, and G-d) . 28
Figure A.16 – Correlation plots of volume resistivity (ρ ) as a function of the volume
v
density (d ) of graphene oxide pellet (G-a, G-b, G-c, and G-d) . 29
v
Figure A.17 – Correlation plots of volume conductivity (σ ) as a function of the volume
v
density (d ) of graphene oxide pellet (G-a, G-b, G-c, and G-d) . 30
v
Figure A.18 – Comparison plots of (A) volume resistivity (σ ) and (B) volume
v
conductivity (σ ) as a function of the volume density (d ) of graphene oxide pellet
v v
(G‑a, G-b, G-c, and G-d) . 30
Table 1 – Minimum thickness of the pellet vs amount of the used sample at the
maximum applied pressure . 12
Table A.1 – An example of the measurement parameters for rGO-A (0,2 g) . 17
Table A.2 – Volume resistivity and volume conductivity of rGO pellets . 21
Table A.3 – Volume resistivity and volume conductivity of GNP pellets . 23
Table A.4 – Summary of XPS data of three graphene samples in a powder form . 24
Table A.5 – Volume resistivity (ρ ) and volume conductivity (σ ) of graphene pellets . 25
v v
Table A.6 – Volume resistivity (σ ) and volume conductivity (σ ) of four graphene oxide
v v
pellets . 31
– 4 – IEC TS 62607-6-1:2020 © IEC 2020
INTERNATIONAL ELECTROTECHNICAL COMMISSION
____________
NANOMANUFACTURING –
KEY CONTROL CHARACTERISTICS –
Part 6-1: Graphene-based material –
Volume resistivity: four probe method
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