Nanomanufacturing - Key control characteristics - Part 6-4: Graphene-based materials - Surface conductance: non-contact microwave resonant cavity method

IEC TS 62607-6-4:2024 has been prepared by IEC technical committee 113: Nanotechnology for electrotechnical products and systems. It is a Technical Specification.
This second edition cancels and replaces the first edition published in 2016. This edition constitutes a technical revision.
This edition includes the following significant technical changes with respect to the previous edition:
a) changed the document title to better reflect its purpose and application:
old title: Graphene – Surface conductance measurement using resonant cavity
new title: Graphene based materials – Surface conductance: non-contact microwave resonant cavity method.
b) replaced former Figure 1 with new Figure 1 and Figure 2, to better illustrate the method’s fundamentals and its implementation for a non-technical reader.
This part of IEC 62607 establishes a standardized method to determine the key control characteristic
a) surface conductance
for films of graphene and graphene-based materials by the
b) non-contact microwave resonant cavity method
The non-contact microwave resonant cavity method monitors the microwave resonant frequency shifts and changes in the cavity’s quality factor during the insertion of the specimen into the microwave cavity, as a function of the specimen surface area. The empty cavity is an air-filled standard R100 rectangular waveguide operated at one of the resonant frequency modes, typically at 7,5 GHz [4].
1) The method is applicable for graphene materials which are synthesized by chemical vapour deposition (CVD) on metal substrates, epitaxial growth on silicon carbide (SiC), obtained from reduced graphene oxide (rGO), or mechanically exfoliated from graphite [5].
2) This measurement does not explicitly depend on the thickness of the nano-carbon layer. The thickness of the specimen does not need to be known, but it is assumed that the lateral dimensions are uniform over the specimen area.
NOTE In some countries, the R100 standard waveguide is referenced as WR-90.

General Information

Status
Published
Publication Date
27-Feb-2024
Current Stage
PPUB - Publication issued
Start Date
28-Feb-2024
Completion Date
23-Feb-2024
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Technical specification
IEC TS 62607-6-4:2024 - Nanomanufacturing - Key control characteristics - Part 6-4: Graphene-based materials - Surface conductance: non-contact microwave resonant cavity method Released:2/28/2024 Isbn:9782832283172
English language
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IEC TS 62607-6-4 ®
Edition 2.0 2024-02
TECHNICAL
SPECIFICATION
Nanomanufacturing – Key control characteristics –
Part 6-4: Graphene-based materials – Surface conductance: non-contact
microwave resonant cavity method

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IEC TS 62607-6-4 ®
Edition 2.0 2024-02
TECHNICAL
SPECIFICATION
Nanomanufacturing – Key control characteristics –

Part 6-4: Graphene-based materials – Surface conductance: non-contact

microwave resonant cavity method

INTERNATIONAL
ELECTROTECHNICAL
COMMISSION
ICS 07.120  ISBN 978-2-8322-8317-2

– 2 – IEC TS 62607-6-4 © IEC 2024
CONTENTS
FOREWORD . 3
INTRODUCTION . 5
1 Scope . 6
2 Normative references . 6
3 Terms and definitions . 6
3.1 Graphene layers . 7
3.2 Measurement terminology . 8
4 Microwave cavity testing structure . 9
5 Test specimen . 9
6 Measurement procedure . 10
6.1 Apparatus . 10
6.2 Calibration . 10
6.3 Measurements . 11
6.3.1 General . 11
6.3.2 Empty cavity . 11
6.3.3 Specimen . 11
6.3.4 Repeated procedure . 11
6.3.5 Substrate . 12
7 Calculations of surface conductance . 12
8 Report . 12
9 Accuracy consideration . 13
Annex A (informative) Case study of surface conductance measurement of single-
layer and few-layer graphene . 14
A.1 General . 14
A.2 Cavity perturbation procedure . 14
A.3 Experimental procedure . 15
A.4 Results . 15
A.5 Surface conductance of single-layer graphene and few-layer graphene . 16
A.6 Summary . 17
Bibliography . 18

Figure 1 – Microwave cavity test structure . 9
Figure 2 – Microwave cavity testing fixture . 10
Figure A.1 – S magnitude of the resonant peak TE as a function of frequency at
21 103
several specimen insertions (h ) . 16
x
Figure A.2 – Plots of 1/Q − 1/Q as a function of the normalized specimen area (w h ). . 16
x 0 x
IEC TS 62607-6-4 © IEC 2024 – 3 –
INTERNATIONAL ELECTROTECHNICAL COMMISSION
____________
NANOMANUFACTURING –
KEY CONTROL CHARACTERISTICS –
Part 6-4: Graphene-based materials –
Surface conductance: non-contact microwave resonant cavity method

FOREWORD
1) The International Electrotechnical Commission (IEC) is a worldwide organization for standardization comprising
all national electrotechnical committees (IEC National Committees). The object of IEC is to promote international
co-operation on all questions concerning standardization in the electrical and electronic fields. To this end and
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shall not be held responsible for identifying any or all such patent rights.

IEC TS 62607-6-4 has been prepared by IEC technical committee 113: Nanotechnology for
electrotechnical products and systems. It is a Technical Specification.
This second edition cancels and replaces the first edition published in 2016. This edition
constitutes a technical revision.
This edition includes the following significant technical changes with respect to the previous
edition:
a) changed the document title to better reflect its purpose and application:

– 4 – IEC TS 62607-6-4 © IEC 2024
old title: Graphene – Surface conductance measurement using resonant cavity
new title: Graphene based materials – Surface conductance: non-contact microwave
resonant cavity method.
b) replaced former Figure 1 with new Figure 1 and Figure 2, to better illustrate the method’s
fundamentals and its implementation for a non-technical reader.
The text of this Technical Specification is based on the following documents:
Draft Report on voting
113/756/DTS 113/809/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 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, or
• amended.
IMPORTANT – The "colour inside" logo on the cover page of this document 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.

IEC TS 62607-6-4 © IEC 2024 – 5 –
INTRODUCTION
The microwave cavity test method for surface conductance is non-contact, fast, and accurate.
It is well suited for standards development, research and development (R&D), and for quality
control in the manufacturing of two-dimensional (2D) nano-carbon materials. These sheet-like
or flake-like carbon forms can be assembled into atomically thin monolayer or multilayer
graphene materials. They can be stacked, folded, crumpled, or pillared into a variety of nano-
carbon architectures with the vertical dimension limited to a few tenths of a nanometre. Many
of these 2D materials, and their derivatives, are new and exhibit extraordinary physical and
electrical properties such as optical transparency, anisotropic heat diffusivity, and charge
transport that are of significant interest to science, technology, and commercial applications
[1] , [2], [3].
Depending on particular morphologies, density of states, and structural perfection, the surface
−5
S. Conventional direct current
conductance of these materials can vary from1 S to about 10
(DC) surface conductance measurement techniques require a complex test vehicle and
interconnections for making electrical contacts to such materials, which affect and distort the
measurement, thus, making it difficult to resolve the intrinsic properties of the material from the
artifacts associated with the electrical contact formation.
In comparison, the resonant cavity measurement method is non-contact, fast, and avoids the
artifacts associated with the electrical contact formation. Thus, it is well suited for use in R&D
and manufacturing environments where the surface conductance is a critical functional
parameter. Moreover, it can be employed to measure electrical characteristics of other nano-
size structures without the need for establishing electrical contacts or sample thickness.

___________
Numbers in square brackets refer to the Bibliography.

– 6 – IEC TS 62607-6-4 © IEC 2024
NANOMANUFACTURING –
KEY CONTROL CHARACTERISTICS –
Part 6-4: Graphene-based materials –
Surface conductance: non-contact microwave resonant cavity method

1 Scope
This part of IEC 62607 establishes a standardized method to determine the key control
characteristic
• surface conductance
for films of graphene and graphene-based materials by the
• non-contact microwave resonant cavity method
The non-contact microwave resonant cavity method monitors the microwave resonant
frequency shifts and changes in the cavity’s quality factor during the insertion of the specimen
into the microwave cavity, as a function of the specimen surface area. The empty cavity is an
air-filled standard R100 rectangular waveguide operated at one of the resonant frequency
modes, typically at 7,5 GHz [4].
– The method is applicable for graphene materials which are synthesized by chemical vapour
deposition (CVD) on metal substrates, epitaxial growth on silicon carbide (SiC), obtained
from reduced graphene oxide (rGO), or mechanically exfoliated from graphite [5].
– This measurement does not explicitly depend on the thickness of the nano-carbon layer.
The thickness of the specimen does not need to be known, but it is assumed that the lateral
dimensions are uniform over the specimen area.
NOTE In some countries, the R100 standard waveguide is referenced as WR-90.
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.
ISO/TS 80004-13, Nanotechnologies – Vocabulary – Part 13: Graphene and related two-
dimensional (2D) materials
3 Terms and definitions
For the purposes of this document, the terms and definitions given in ISO/TS 80004-13 and the
following apply.
ISO and IEC maintain terminology databases for use in standardization at the following
addresses:
• IEC Electropedia: available at https://www.electropedia.org/
• ISO Online browsing platform: available at https://www.iso.org/obp

IEC TS 62607-6-4 © IEC 2024 – 7 –
3.1 Graphene layers
3.1.1
graphene
graphene layer
single-layer graphene
monolayer graphene
single layer of carbon atoms with each atom bound to three neighbours in a honeycomb
structure
Note 1 to entry: It is an important building block of many carbon nano-objects.
Note 2 to entry: As graphene is a single layer, it is also sometimes called monolayer graphene or single-layer
graphene and abbreviated as 1LG to distinguish it from bilayer graphene (2LG) and few-layer graphene (FLG).
Note 3 to entry: Graphene has edges and can have defects and grain boundaries where the bonding is disrupted.
[SOURCE: ISO/TS 80004-13:2017, 3.1.2.1]
3.1.2
bilayer graphene
2LG
two-dimensional material consisting of two well-defined stacked graphene layers
Note 1 to entry: If the stacking registry is known, it can be specified separately, for example, as "Bernal stacked
bilayer graphene".
[SOURCE: ISO/TS 80004-13:2017, 3.1.2.6]
3.1.3
trilayer graphene
3LG
two-dimensional material consisting of three well-defined stacked graphene layers
Note 1 to entry: If the stacking registry is known, it can be specified separately, for example, as "twisted trilayer
graphene".
[SOURCE: ISO/TS 80004-13:2017, 3.1.2.9]
3.1.4
few-layer graphene
FLG
two-dimensional material consisting of three to ten well-defined stacked graphene layers.
[SOURCE:ISO/TS 80004-13:2017, 3.1.2.10]
3.1.5
graphene oxide
GO
chemically modified graphene prepared by oxidation and exfoliation of graphite, causing
extensive oxidative modification of the basal plane.
Note 1 to entry: Graphene oxide is a single-layer material with a high oxygen content, typically characterized by
C/O atomic ratios of approximately 2,0 depending on the method of synthesis.
[SOURCE: ISO/TS 80004-13:2017, 3.1.2.13]
3.1.6
reduced graphene oxide
rGO
reduced oxygen content form of graphene oxide
Note 1 to entry: This can be produced by chemical, thermal, microwave, photo-chemical, photo-thermal or
microbial/bacterial methods or by exfoliating reduced graphite oxide.
Note 2 to entry: If graphene oxide was fully reduced, then graphene would be the product. However, in practice,
3 2
some oxygen containing functional groups will remain and not all sp bonds will return back to sp configuration.
Different reducing agents will lead to different carbon to oxygen ratios and different chemical compositions in reduced
graphene oxide.
– 8 – IEC TS 62607-6-4 © IEC 2024
Note 3 to entry: It can take the form of several morphological variations such as platelets and worm-like structures.
[SOURCE: ISO/TS 80004-13:2017, 3.1.2.14]
3.1.7
graphene-based material
GBM
graphene material
grouping of carbon-based 2D materials that include one or more of graphene, bilayer graphene,
few-layer graphene, graphene nanoplate, and functionalized variations thereof as well as
graphene oxide and reduced graphene oxide.
Note 1 to entry: "Graphene material" is a short name for graphene-based material.
3.2 Measurement terminology
3.2.1
surface conductance
sheet conductance
characteristic physical property of two-dimensional materials describing the ability to conduct
electric current.
Note 1 to entry: The SI unit of measure of σ is siemens (S). In the trade and industrial literature, however, siemens
s
per square (S/square) is commonly used when referring to surface conductance: G = I/U = σ ·(w/l).
s
Note 2 to entry: The surface conductance (σ ) can be obtained by normalizing conductance G to the specimen width
s
(w) and length (l).
3.2.2
electrical conductivity
σ
v
characteristic physical property of 3D materials describing the ability to conduct electric current.
Note 1 to entry: The electrical conductivity can be obtained from surface conductance dividing it by the conductor
thickness (t), with σ = σ /t. The unit of measure of σ is siemens per metre (S/m).
v s v
3.2.3
surface resistance
sheet resistance
ρ
s
reciprocal of surface conductance, σ
s
Note 1 to entry: Sheet resistance measurements are commonly made to characterize the uniformity of conductive
or semi-conductive coatings for quality assurance. The SI unit of measure of ρ is ohm (Ω). In the trade and industrial
s
literature, however, ohm per square (Ω/square) is commonly used when referring to surface resistance. This is to
avoid confusion between surface resistance and electrical resistance (R), which share the same unit of measure.
3.2.4
microwave cavity
radio frequency cavity
RF cavity
special type of resonator consisting of a closed metal structure that confines electromagnetic
fields in the microwave region of the spectrum.
Note 1 to entry: The structure can be filled with air or other dielectric material. A cavity acts similarly to a resonant
circuit with extremely low loss at its frequency of operation.
Note 2 to entry: Microwave cavities are typically made from closed (or short-circuited) sections of a waveguide.
Every cavity has numerous resonant frequencies (f ) that correspond to electromagnetic field modes satisfying the
r
necessary boundary conditions, i.e. the cavity length is an integer multiple of half-wavelength at resonance.
3.2.5
quality factor
dimension-less parameter describing the ratio of energy stored in the resonant circuit to time-
averaged power loss of the cavity, or equivalently, a resonator's half power bandwidth, (∆f)
relative to the resonant frequency (f )
r
Note 1 to entry: Q = f /∆f
r
IEC TS 62607-6-4 ©
...

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