IEC TS 62607-6-3:2020

Nanomanufacturing - Key control characteristics - Part 6-3: Graphene-based material - Domain size: substrate oxidation

IEC TS 62607:2020 establishes a standardized method to determine the structural key control characteristic
– domain size
for films consisting of graphene grown by chemical vapour deposition (CVD) on copper by
– substrate oxidation.
It provides a fast, facile and reliable method to evaluate graphene domains formed on copper foil or copper film for understanding the effect of the graphene domain size on properties of graphene and enhancing the performance of high speed, flexible, and transparent devices using CVD graphene.
– The domain size 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. Domain density is an equivalent measure.
– The domain size as derived by this method is defined as the mean value of size of the domains in the observed area specified by supplier in terms of cm2 or µm2.
– The method is applicable for graphene grown on copper by CVD. The characterization is done on the copper foil before transfer to the final substrate.
– As the method is destructive, the samples cannot be re-launched into the fabrication process.

General Information

• Status: Published
• Publication Date: 26-Oct-2020
• ICS: 07.030 - Physics. Chemistry
• ICS: 07.120 - Nanotechnologies
• Technical Committee: TC 113 - Nanotechnology for electrotechnical products and systems
• Drafting Committee: JPT 62607-6-3 - TC 113/JPT 62607-6-3
• Current Stage: PPUB - Publication issued
• Start Date: 27-Oct-2020
• Completion Date: 12-Nov-2020

Overview

IEC TS 62607-6-3:2020 specifies a standardized, reproducible method to determine the graphene domain size for films grown by chemical vapour deposition (CVD) on copper using substrate oxidation. The Technical Specification defines domain size as the mean area of graphene domains in the observed area (reported in cm² or µm²), and notes domain density as an equivalent metric. The measurement is performed on the copper foil/film prior to transfer and is a destructive test - samples cannot be returned to production.

Keywords: IEC TS 62607-6-3:2020, graphene domain size, substrate oxidation, CVD graphene, copper foil, nanomanufacturing, key control characteristic.

Key topics and technical requirements

• Scope and purpose
  • Establishes a fast, facile and reliable method to evaluate graphene domains formed on copper by substrate oxidation.
  • Designed to link domain size to functional properties of graphene for device performance improvement.
• Measurement principle
  • Oxidation of the copper substrate selectively through graphene boundaries reveals domain boundaries for imaging and analysis.
• Sample preparation and measurement
  • Characterization is carried out on CVD-grown graphene on copper before any transfer steps.
  • The method includes calibration requirements (reference to ASTM E1951-14) and defined ambient/measurement conditions.
• Analysis and reporting
  • Domain size reported as mean area over the supplier-specified observed area.
  • Measurement protocol, data to be reported (product/sample ID, test conditions, measurement results) and worked examples (optical/SEM imaging and image analysis tools) are provided.
• Limitations
  • Method applies to graphene grown on copper by CVD only.
  • Destructive nature prevents reuse of tested samples in fabrication.

Applications and practical value

• Quality control and process monitoring for manufacturers of CVD graphene on copper foil or copper films.
• Materials and process engineers evaluating how domain size and domain density affect electrical, thermal and mechanical properties.
• R&D and production teams developing high-speed, flexible, and transparent electronic/optoelectronic devices (e.g., FETs, transparent electrodes, flexible displays).
• Enables suppliers to specify a key control characteristic (KCC) for graphene in the blank detail specification IEC 62565-3-1.

Who should use this standard

• Graphene producers, process engineers, QC labs, materials scientists, device integrators, and certification bodies needing a standardized, reproducible method to quantify graphene domain size for product specifications and performance correlation.

Related standards

• IEC 62565-3-1 (blank detail specification for graphene) - lists the domain size KCC determined by this method.
• ASTM E1951-14 - referenced for microscope magnification calibration.

This Technical Specification supports consistent, comparable reporting of graphene domain metrics across suppliers and users, improving traceability and device performance optimization in nanomanufacturing.

Standards Content (Sample)

IEC TS 62607-6-3 ®
Edition 1.0 2020-10
TECHNICAL
SPECIFICATION
colour
inside
Nanomanufacturing – Key control characteristics –
Part 6-3: Graphene-based material – Domain size: substrate oxidation

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IEC TS 62607-6-3 ®
Edition 1.0 2020-10
TECHNICAL
SPECIFICATION
colour
inside
Nanomanufacturing – Key control characteristics –

Part 6-3: Graphene-based material – Domain size: substrate oxidation

INTERNATIONAL
ELECTROTECHNICAL
COMMISSION
ICS 07.030, ICS 07.120 ISBN 978-2-8322-8939-6 0

– 2 – IEC TS 62607-6-3:2020 © 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 Graphene related terms . 8
3.3 Key control characteristics measured in accordance with this document . 9
4 General . 9
4.1 Measurement principle . 9
4.2 Sample preparation method . 10
4.3 Measurement system . 11
4.4 Description of measurement equipment/apparatus . 12
4.5 Calibration standards . 12
4.6 Ambient conditions during measurement . 12
5 Measurement procedure . 12
5.1 Calibration of measurement equipment . 12
5.2 Detailed protocol of the measurement procedure . 12
5.2.1 General . 12
5.2.2 Example . 13
6 Results to be reported . 13
6.1 General . 13
6.2 Product/sample identification . 13
6.3 Test conditions . 13
6.4 Measurement specific information . 14
6.5 Test results . 14
Annex A (informative) Worked example . 15
A.1 Example. 15
A.2 Sampling plan . 18
A.3 Format of the test report . 19
Annex B (informative) Alternative methods for evaluating graphene domains and
defects . 21
Bibliography . 22

Figure 1 – Applications of graphene . 6
Figure 2 – Schematics for oxidation of copper foil through the graphene boundaries. 10
Figure 3 – Optical image of the graphene domains on Cu foil . 11
Figure 4 – Schematic view of oxidation system . 11
Figure 5 – Optical images of graphene/Cu after oxidation and analysed grain size
distribution . 12
Figure 6 – Example of domain size analysis . 13
Figure A.1 – Photograph of graphene/Cu foil (7cm × 7 cm) for graphene grown at
1 050 °C by CVD with CH . 15
Figure A.2 – SEM image of graphene/Cu after oxidation at the points as specified in
Figure A.6 . 16

Figure A.3 – Measuring graphene domain size of Figure A.2 using Image J . 16
Figure A.4 –Domain size distribution and average domain size of graphene shown in
Figure A.2 . 17
Figure A.5 – Accumulative domain size distribution shown in Figure A.4 and average
domain size of graphene measured at 9 points shown in Figure A.6 . 18
Figure A.6 – Location of the analysed area on the sample . 18
Figure B.1 – Typical methods for observing graphene domain and grain boundaries . 21

Table A.1 – Product identification (in accordance with IEC 62565-3-1) . 19
Table A.2 – General material description (in accordance with IEC 62565-3-1). 19
Table A.3 – Measurement related information . 19
Table A.4 – KCC measurement results . 20

– 4 – IEC TS 62607-6-3:2020 © IEC 2020
INTERNATIONAL ELECTROTECHNICAL COMMISSION
____________
NANOMANUFACTURING –
KEY CONTROL CHARACTERISTICS –
Part 6-3: Graphene-based material –
Domain size: substrate oxidation

FOREWORD
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rights. IEC shall not be held responsible for identifying any or all such patent rights.
The main task of IEC technical committees is to prepare International Standards. In exceptional
circumstances, a technical committee may propose the publication of a Technical Specification
when
• the required support cannot be obtained for the publication of an International Standard,
despite repeated efforts, or
• the subject is still under technical development or where, for any other reason, there is the
future but no immediate possibility of an agreement on an International Standard.
Technical Specifications are subject to review within three years of publication to decide
whether they can be transformed into International Standards.
IEC TS 62607-6-3, which is a Technical Specification, has been prepared by technical
committee 113, Nanotechnology for electrotechnical products and systems.

The text of this Technical Specification is based on the following documents:
Enquiry draft Report on voting
113/496/DTS 113/549/RVDTS
Full information on the voting for the approval of this Technical Specification can be found in
the report on voting indicated in the above table.
This document has been drafted in accordance with the ISO/IEC Directives, Part 2.
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 "http://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 publication indicates
that it contains colours which are considered to be useful for the correct understanding
of its contents. Users should therefore print this document using a colour printer.

– 6 – IEC TS 62607-6-3:2020 © IEC 2020
INTRODUCTION
Graphene with two-dimensional honeycomb structures of carbon atoms is known to have
exceptional electrical, thermal, and mechanical properties. Because of these properties,
graphene is considered for applications in high speed, flexible and transparent devices.
Figure 1 shows the images of graphene field effect transistor, flexible touch screen in display,
and transparent electrode in solar cell. These applications of graphene are promising
candidates for nanoelectronics and optoelectronics. Graphene has been widely investigated by
researchers from academic institutions, research institutes, and industries.

Figure 1 – Applications of graphene
Graphene synthesized on Cu or Ni substrate by chemical vapour deposition (CVD) is composed
of graphene domains formed during the nucleation and initial growth stage. Graphene defects,
such as pinholes, domain boundaries, and cracks, can be formed during the CVD growth or the
transfer process.
Properties of graphene are related to the size and distribution of graphene domains and defects.
As graphene domain size is increased and graphene defects are reduced, electrical and thermal
properties of graphene are improved.
Graphene domains and defects are usually observed by atomic force microscopy (AFM),
scanning electron microscopy (SEM), transmission electron microscopy (TEM), Raman
spectroscopy, and scanning tunnelling microscopy (STM). These analysis methods may cause
inconvenience in preparing a sample for analysis and require very expensive equipment that
provides only local information of several micrometres and below.
Facile, fast, reliable methods of evaluating graphene domains have not yet been established
and urgently need to be developed.

NANOMANUFACTURING –
KEY CONTROL CHARACTERISTICS –
Part 6-3: Graphene-based material –
Domain size: substrate oxidation

1 Scope
This part of IEC TS 62607 establishes a standardized method to determine the structural key
control characteristic
– domain size
for films consisting of graphene grown by chemical vapour deposition (CVD) on copper by
– substrate oxidation.
It provides a fast, facile and reliable method to evaluate graphene domains formed on copper
foil or copper film for understanding the effect of the graphene domain size on properties of
graphene and enhancing the performance of high speed, flexible, and transparent devices using
CVD graphene.
– The domain size 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. Domain density
is an equivalent measure.
– The domain size as derived by this method is defined as the mean value of size of the
2 2
domains in the observed area specified by supplier in terms of cm or µm .
– The method is applicable for graphene grown on copper by CVD. The characterization is
done on the copper foil before transfer to the final substrate.
– As the method is destructive, the samples cannot be re-launched into the fabrication process.
2 Normative references
The following documents are referred to in the text in such a way that some or all of their content
constitutes requirements of this document. For dated references, only the edition cited applies.
For undated references, the latest edition of the referenced document (including any
amendments) applies.
ASTM E1951-14, Standard Guide for Calibrating Reticles and Light Microscope Magnification
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
ISO and IEC maintain terminological databases for use in standardization at the following
addresses:
• IEC Electropedia: available at http://www.electropedia.org/
• ISO Online browsing platform: available at http://www.iso.org/obp

– 8 – IEC TS 62607-6-3:2020 © IEC 2020
3.1
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