IEC TS 62607-2-5:2022

Nanomanufacturing - Key control characteristics - Part 2-5: Carbon nanotube materials - Mass density of vertically-aligned carbon nanotubes: X-ray absorption method

IEC TS 62607-2-5:2022 specifies the protocols for determining the mass density of vertically-aligned carbon nanotubes (VACNTs) by X-ray absorption method. This document outlines experimental procedures, data formats, and some case studies. These protocols are applicable to VACNT films with thickness larger than several tens of micrometres. There are no limitations in materials for substrate.

General Information

• Status: Published
• Publication Date: 07-Nov-2022
• ICS: 07.030 - Physics. Chemistry
• 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: 16-Dec-2022
• Completion Date: 08-Nov-2022

Standards Content (Sample)

IEC TS 62607-2-5
®

Edition 1.0 2022-11
TECHNICAL
SPECIFICATION

colour
inside


Nanomanufacturing – Key control characteristics –
Part 2-5: Carbon nanotube materials – Mass density of vertically-aligned carbon
nanotubes: X-ray absorption method
IEC TS 62607-2-5:2022-11(en)

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IEC TS 62607-2-5

®


Edition 1.0 2022-11




TECHNICAL



SPECIFICATION








colour

inside










Nanomanufacturing – Key control characteristics –

Part 2-5: Carbon nanotube materials – Mass density of vertically-aligned carbon

nanotubes: X-ray absorption method

























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ELECTROTECHNICAL


COMMISSION





ICS 07.030; 07.120 ISBN 978-2-8322-6030-2




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– 2 – IEC TS 62607-2-5:2022 © IEC 2022
CONTENTS
FOREWORD . 4
INTRODUCTION . 6
1 Scope . 7
2 Normative references . 7
3 Terms, definitions, and abbreviated terms . 7
3.1 Terms and definitions . 7
3.2 Abbreviated terms . 8
4 Measurement of mass density of vertically-aligned carbon nanotubes with X-ray
absorption method . 8
4.1 General . 8
4.2 Measurement principle . 8
4.3 Description of measurement equipment and apparatus . 9
4.4 Sample preparation . 9
4.5 Thickness measurement with X-ray absorption method . 9
4.6 Density measurement with X-ray absorption method . 10
5 Appropriate data formats . 11
Annex A (informative) Case study of mass density measurements for vertically-aligned
carbon nanotubes . 13
A.1 Overview. 13
A.2 Sample preparation for VACNTs . 13
A.3 Confirmation of X-ray incidence parallel to the substrate surface . 13
A.4 Thickness and mass density measurements with transmitted X-ray intensity
profiles . 14
A.5 Measurement results for a VACNT film with a thickness of several hundred
micrometres . 16
A.6 Measurement results for a VACNT film with a thickness of several
millimetres . 18
Bibliography . 20

Figure 1 – Measurement principle of X-ray absorption method . 8
Figure 2 – Parameters determining the spatial resolution of X-ray absorption method . 9
Figure 3 – Example of X-ray projection image of VACNTs grown on Si substrate . 10
Figure 4 – Example of transmitted X-ray intensity profile for VACNT sample . 10
Figure 5 – Example of calibration result for non-monochromatic incident X-ray . 11
Figure A.1 – Schematic drawings of beam alignment procedures for X-ray absorption
measurement . 14
Figure A.2 – X-ray projection images and transmitted X-ray intensity profiles observed
for two VACNT samples . 15
Figure A.3 – Cross-sectional scanning electron microscope images of two VACNT
samples . 16
Figure A.4 – X-ray projection image and transmitted X-ray intensity profile observed for
a thicker VACNT film. 17
Figure A.5 – Cross-sectional scanning electron microscope image of a thicker VACNT
film . 17
Figure A.6 – X-ray projection image and transmitted X-ray intensity profile observed for
a millimetre-thick VACNT film . 19

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IEC TS 62607-2-5:2022 © IEC 2022 – 3 –
Figure A.7 – X-ray projection image and mass density profile observed for a millimetre-
thick VACNT film . 19

Table 1 – Possible data format to be given together with density of VACNTs obtained
with X-ray absorption method. 12
Table A.1 – Parameters obtained from the transmitted X-ray intensity profiles for two
VACNT samples . 16
Table A.2 – Parameters obtained from the transmitted X-ray intensity profile for a
thicker VACNT film . 17

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INTERNATIONAL ELECTROTECHNICAL COMMISSION
____________

NANOMANUFACTURING – KEY CONTROL CHARACTERISTICS –

Part 2-5: Carbon nanotube materials – Mass density of vertically-aligned
carbon nanotubes: X-ray absorption method

FOREWORD
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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 62607-2-5 has been prepared by IEC technical committee 113: Nanotechnology
standardization 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
113/674/DTS 113/696/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.

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IEC TS 62607-2-5:2022 © IEC 2022 – 5 –
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,
• replaced by a revised edition, or
• amended.

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– 6 – IEC TS 62607-2-5:2022 © IEC 2022
INTRODUCTION
Vertically-aligned carbon nanotubes (VACNTs) are array structures, in which nanotubes are
oriented in the perpendicular direction to a substrate surface. VACNTs are useful in many
electronic device applications such as field-emission devices, gas and biological sensors,
thermal interface materials, supercapacitors, and so on. Chemical vapour deposition (CVD) is
one of the common methods for the synthesis of VACNTs, where CNTs can be grown in the
presence of metal catalysts, via thermal decomposition of hydrocarbon sources such as
methane, ethylene, acetylene, ethanol, and so on.
Physical (electrical, thermal, etc.) properties of VACNT films really depend on their density,
which is reflected by distribution and alignment behaviours of individual CNTs. The mass
density of nanotubes in VACNT samples was evaluated in various ways. The first choice is
measuring the sample mass gain, which is successively divided by the height and the area of
the VACNT samples for obtaining density values. However, this mass gain method is a
destructive method, and is effective only if the mass of CNTs can be measured with a
microbalance, so that the mass density can be estimated from the mass gain during the CVD
growth. The second method is counting the number of CNTs in scanning electron microscope
(SEM) or transmission electron microscope (TEM) images. However, this counting method is
less reliable when the nanotubes are not grown straight on the substrate and the density is low.
Liquid-induced compaction can compact the VACNT samples to a maximum density with wetting
or drying process of alcohols. However, these methods are destructive analyses (except for
SEM) and are not designed for incorporating the wide distribution in size and alignment of
nanotubes observed in realistic VACNT samples. Hence, there is strong demand for the
development of new reliable methods for evaluating density in VACNTs.
In this context, an X-ray absorption method is proposed as a standard protocol for evaluating
density of VACNTs. X-rays can transmit through the film parallel to the substrate surface, and
the transmitted X-rays are detected by a high-resolution X-ray imaging apparatus. The observed
X-ray projection images can enable the substrate, VACNT film, and air regions to be identified
easily. The film density can be calculated from the measured X-ray transmittance of the film.
This method is an effective and versatile technique of nondestructive analysis for VACNT film
density.

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IEC TS 62607-2-5:2022 © IEC 2022 – 7 –
NANOMANUFACTURING – KEY CONTROL CHARACTERISTICS –

Part 2-5: Carbon nanotube materials – Mass density of vertically-aligned
carbon nanotubes: X-ray absorption method



1 Scope
This part of IEC 62607 specifies the protocols for determining the mass density of vertically-
aligned carbon nanotubes (VACNTs) by X-ray absorption method. This document outlines
experimental procedures, data formats, and some case studies. These protocols are applicable
to VACNT films with thickness larger than several tens of micrometres. There are no limitations
in materials for substrate.
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.
There are no normative references in this document.
3 Terms, definitions, and abbreviated terms
3.1 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
3.1.1
carbon nanotube
CNT
nanotube composed of carbon
[SOURCE: ISO/TS 80004-3:2020 [1], 3.3.3, modified – Note 1 to entry has been deleted.]
3.1.2
single-walled carbon nanotube
SWCNT
carbon nanotube consisting of a single cylindrical graphene layer
[SOURCE: ISO/TS 80004-3:2020, 3.3.4, modified – The term "single-wall carbon nanotube" and
Note 1 to entry have been deleted.]

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3.1.3
multi-walled carbon nanotube
MWCNT
carbon nanotube composed of nested, concentric or near-concentric graphene layers with
interlayer distances similar to those of graphite
[SOURCE: ISO/TS 80004-3:2020, 3.3.6, modified – The term "multiwall carbon nanotube" and
Note 1 to entry have been deleted.]
3.1.4
vertically-aligned carbon nanotubes
VACNTs
carbon nanotube bundle grown in the perpendicular direction to a substrate surface
3.2 Abbreviated terms
CVD chemical vapour deposition
SEM scanning electron microscope
4 Measurement of mass density of vertically-aligned carbon nanotubes with
X-ray absorption method
4.1 General
X-ray is well known for its high penetrating power and has been widely used for n
...