IEC TS 62607-6-18:2022

Nanomanufacturing - Key control characteristics - Part 6-18: Graphene-based material - Functional groups: TGA-FTIR

IEC TS 62607-6-18:2022(E) establishes a standardized method to determine the chemical key control characteristic
functional groups  for functionalized graphene-based material and graphene oxide by
thermogravimetry analysis (TGA) coupled with Fourier transform infrared spectroscopy (FTIR), referred to as TGA-FTIR.  The content of functional groups is derived by changes in mass of the sample as a function of temperature using TGA. Materials evolved during these mass changes are then analysed using coupled FTIR to identify functional groups.
The functional groups determined according to 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 functionalized graphene powder and graphene oxide that can be pyrolysed and gasified with elevated temperature during TGA.
Typical application areas are quality control for graphene manufacturers, and product selection for downstream users.

General Information

• Status: Published
• Publication Date: 13-Dec-2022
• 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: 13-Jan-2023
• Completion Date: 14-Dec-2022

Standards Content (Sample)

IEC TS 62607-6-18
®

Edition 1.0 2022-12
TECHNICAL
SPECIFICATION

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Nanomanufacturing – Key control characteristics –
Part 6-18: Graphene-based material – Functional groups: TGA-FTIR
IEC TS 62607-6-18:2022-12(en)

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IEC TS 62607-6-18

®


Edition 1.0 2022-12




TECHNICAL



SPECIFICATION








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Nanomanufacturing – Key control characteristics –

Part 6-18: Graphene-based material – Functional groups: TGA-FTIR


























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– 2 – IEC TS 62607-6-18:2022  IEC 2022
CONTENTS
FOREWORD . 3
INTRODUCTION . 5
1 Scope . 6
2 Normative references . 6
3 Terms and definitions . 6
4 General . 9
4.1 Measurement principle . 9
4.2 Sample preparation method . 9
4.3 Measurement system . 9
4.4 Description of measurement equipment . 9
4.5 Supporting materials . 9
4.6 Ambient conditions during measurement . 10
5 Measurement procedure . 10
5.1 Calibration of measurement equipment . 10
5.2 Detailed protocol of the measurement procedure . 10
6 Data analysis . 11
7 Results to be reported . 12
7.1 General . 12
7.2 Product or sample identification . 12
7.3 Test conditions . 12
7.4 Measurement specific information . 12
7.5 Test results . 12
Annex A (informative) Format of the test report . 13
Annex B (informative) Case study: Data analysis . 15
B.1 Confirmation of characteristic temperature points from TGA curve . 15
B.2 Analysis of FTIR spectra obtained at different ashing temperatures . 15
B.3 Analysis of FTIR spectra obtained by TGA-FTIR measurements . 16
B.4 Confirmation and quantification of the functional groups . 17
Bibliography . 19

Figure 1 – Flow chart of data analysis . 11
Figure B.1 – Weight loss curve (left) obtained from TGA-FTIR measurement and
corresponding differential weight loss curve (right) . 15
Figure B.2 – FTIR spectra corresponding to different ashing temperature points . 15
Figure B.3 – A 3D FTIR spectrum obtained by one FTIR-TGA measurement . 16
Figure B.4 – Absorption dynamics of each gas component . 17
Figure B.5 – Absorption dynamics of each gas component . 17
Figure B.6 – Weight loss dynamics of each gas component . 18

Table A.1 – Product identification (in accordance with IEC 62565-3-1) . 13
Table A.2 – General material description (in accordance with IEC 62565-3-1). 13
Table A.3 – Test information . 14
Table A.4 – Measurement results . 14

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IEC TS 62607-6-18:2022  IEC 2022 – 3 –
INTERNATIONAL ELECTROTECHNICAL COMMISSION
____________

NANOMANUFACTURING – KEY CONTROL CHARACTERISTICS –

Part 6-18: Graphene-based material – Functional groups: TGA-FTIR

FOREWORD
1) The International Electrotechnical Commission (IEC) is a worldwide organization for standardization comprising
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9) Attention is drawn to the possibility that some of the elements of this IEC Publication may be the subject of patent
rights. IEC shall not be held responsible for identifying any or all such patent rights.
IEC TS 62607-6-18 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
113/680/DTS 113/706/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.

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– 4 – IEC TS 62607-6-18:2022  IEC 2022
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 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 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.

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IEC TS 62607-6-18:2022  IEC 2022 – 5 –
INTRODUCTION
One of the most well-studied routes for the preparation of graphene is the oxidation and
reduction process. The most cost-effective process to obtain graphene is the exfoliation of
natural graphite layers after oxidation to get individual oxidized layers and then de-oxygenation
1
(reduction) of these individual layers [1], [2] . During the oxidation process, various
functionalized groups (-OH, -O-, -COOH, C=O, etc.) go into the graphene skeleton, breaking
the π bond of graphene structure [3]. Oxygen attachment to graphene in any chemical form
(epoxide, hydroxyl, carboxyl and ketonic-type functional groups) both on the basal plane and at
the edges reduces electronic states at the Fermi level [4], [5], [6]. The type and content of
functional groups affect the physiochemical properties of graphene. Therefore, the identification
and quantification of functional groups on graphene powder is believed to be a key control
characteristic for its production and application.
Coupling thermal gravimetric analysis (TGA) and Fourier transform infrared spectroscopy (FTIR)
is an excellent solution to identify and quantify functional groups on graphene powder. In TGA-
FTIR, while mass changes such as sample pyrolysis and vaporization that accompany changes
in temperature are measured quantitatively by the TGA, qualitative analysis of the gaseous
components can be conducted simultaneously by FTIR measurement of the obtained spectra.
This document focuses on determining the type and content of functional groups (e.g. hydroxyl,
amino, carboxyl, alkyl, carbonyl, sulfonic acid group) on graphene powder by coupling TGA and
FTIR.
___________
1
Numbers in square brackets refer to the Bibliography.

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NANOMANUFACTURING – KEY CONTROL CHARACTERISTICS –

Part 6-18: Graphene-based material – Functional groups: TGA-FTIR



1 Scope
This part of IEC TS 62607 establishes a standardized method to determine the chemical key
control characteristic
• functional groups
for functionalized graphene-based material and graphene oxide by
• thermogravimetry analysis (TGA) coupled with Fourier transform infrared spectroscopy
(FTIR), referred to as TGA-FTIR.
The content of functional groups is derived by changes in mass of the sample as a function of
temperature using TGA. Materials evolved during these mass changes are then analysed using
coupled FTIR to identify functional groups.
• The functional groups determined according to 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 functionalized graphene powder and graphene oxide that can
be pyrolysed and gasified with elevated temperature during TGA.
• Typical application areas are quality control for graphene manufacturers, and product
selection for downstream users.
2 Normative references
There are no normative references in this document.
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
3.1 General terms
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.

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IEC TS 62607-6-18:2022  IEC 2022 – 7 –
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
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]
3.1.3
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.
3.1.4
blank detail specification
BDS
structured generic specification of the set of key control characteristics which are needed to
describe a specific nano-enabled product without assigning specific values and/or attributes
Note 1 to entry: The templates defined in a blank detail specification list the key control characteristics for the nano-
enabled material or product without assigning specific values to it.
Note 2 to entry: Examples of nano-enabled products are: nanomaterials, nanocomposites and nano-subassemblies.
Note 3 to entry: Blank detail specifications are intended to be used by industrial users to prepare their detail
specifications used in bilateral procurement contracts. A blank detail specification facilitates the comparison and
benchmarking of different materials. Furthermore, a standardized format makes procurement more efficient and more
error robust.
3.1.5
sectional blank detail specification
SBDS
specification based on a blank detail specification adapted for a subgroup of the nano-enabled
product
Note 1 to entry: In general the sectional blank detail specification contains a subset of those KCCs listed in the
blank detail specification. In addition, sectional specific key control characteristics may be added if they are not listed
in the blank detail specification.
Note 2 to entry: The templates defined in the sectional blank detail specification may contain key control
characteristics with and without assigned values and attributes.
Note 3 to entry: The section can be defined by application, manufacturing method or general material properties.
3.1.6
detail specification
DS
specification based on a blank detail specification with assigned values and attributes

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Note 1 to entry: The properties listed in the detail specification are usually a subset of the key control characteristics
listed in the relevant blank detail specification. The industrial partners define only those properties which are required
for the intended application.
Note 2 to entry: Detail specifications are defined by the industrial partners. SDOs will be involved only if there is a
general need for a detail specification in an industrial sector.
Note 3 to entry: The industrial partners may define additional key control characteristics if they are not listed in the
blank detail specification.
3.1.7
key cont
...