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GB/T 37152-2018

Chinese Standard: 'GB/T 37152-2018'
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Detail Information of GB/T 37152-2018; GB/T37152-2018
Description (Translated English): Nanotechnology--Carbon nanotube materials--Sheet resistance
Sector / Industry: National Standard (Recommended)
Classification of Chinese Standard: G13
Classification of International Standard: 59.100.20
Word Count Estimation: 14,141
Date of Issue: 2018-12-28
Date of Implementation: 2018-12-28
Drafting Organization: Shenzhen Standard Technology Research Institute, Shenzhen Defang Nano Technology Co., Ltd., National Nano Science Center, Shenzhen Institute of Metrology and Quality Inspection
Administrative Organization: National Nanotechnology Standardization Technical Committee
Proposing organization: Chinese Academy of Sciences


GB/T 37152-2018
Nanotechnology--Carbon nanotube materials--Sheet resistance
ICS 59.100.20
G13
National Standards of People's Republic of China
Nanotechnology carbon nanotube material sheet resistance
(IEC /T S62607-2-1.2012, Nanomanufacturing-Keycontrolcharacteristics-
Part 2-1.Carbonnanotubematerial-Filmresistance, IDT)
Published on.2018-12-28
2018-12-28 implementation
State market supervision and administration
China National Standardization Administration issued
Content
Foreword III
Introduction IV
1 range 1
2 Terms and definitions, abbreviations 1
3 sample preparation method 2
4 Determination of thin layer resistance of carbon nanotubes 3
5 Data Analysis/Results Description 5
Appendix A (informative) Example Analysis 6
Reference 9
Foreword
This standard was drafted in accordance with the rules given in GB/T 1.1-2009.
This standard uses the translation method equivalent to IEC /T S62607-2-1.2012 "Nano Manufacturing Key Control Characteristics Part 2-1. Carbon
Nanotube material film resistance.
This standard has made the following editorial changes.
--- Change the standard name to "Nanotechnology carbon nanotube material sheet resistance".
This standard was proposed by the Chinese Academy of Sciences.
This standard is under the jurisdiction of the National Nanotechnology Standardization Technical Committee (SAC/TC279).
This standard was drafted by Shenzhen Standard Technology Research Institute, Shenzhen Defang Nano Technology Co., Ltd., National Nano Science Center,
Shenzhen Institute of Metrology and Quality Inspection.
The main drafters of this standard. Wang Yiqun, Jin Song, Kong Lingyong, Ge Guanglu, Wang Xiaoping, Gao Jie, Shang Weili, Li Zhongyuan.
introduction
New materials containing carbon nanotubes (CNTs) have two major trends in the next generation of industrial applications.
a) Conductive composites for field-emission displays (FEDs), flexible displays and printed electronics
material;
b) Nanocomposites for mechanical applications, making full use of their outstanding mechanical properties such as high Young's modulus, high elasticity and high tensile strength
And so on.
This standard mainly relates to the conductive composite material in the above a). At present, conductive composite materials are widely used in the electronics industry, so it is necessary
Establish test method standards to evaluate their electrical performance.
The electrical properties of CNTs used in conductive composites are very important to both manufacturers and users. This standard specifies the guide
A simple method for detecting the electrical properties of CNTs of electrical composites.
Nanotechnology carbon nanotube material sheet resistance
1 Scope
This standard specifies the standard method for the detection of thin-layer resistance of carbon nanotubes, so that users can choose the right combination of their own applications.
Choose. The purpose of this standard is to evaluate the consistent control of the conductivity of the final product of different batches of products manufactured by the same production procedure.
For each application, the relationship between the parameters measured according to the specified method and the performance parameters of the relevant product should be established. This standard includes the following
content.
a) the definition of the terms used in this document;
b) recommendations for the preparation of samples;
c) summary of experimental procedures for measuring the sheet resistance of carbon nanotubes;
d) results analysis and data discussion;
e) case analysis;
f) References.
2 Terms and definitions, abbreviations
Note. The more comprehensive series of nanotechnology terminology standards IEC /ISO /T S80004 is being prepared by the first joint working group of IEC TC113/ISO TC229.
Medium and will be included in different parts of IEC /ISO /T S80004. This standard will be used in conjunction with the terminology in the latest version of IEC /ISO /T S80004.
The definition is consistent. Unspecified terms are taken from the scientific literature.
2.1 Terms and definitions
The following terms and definitions apply to this document.
2.1.1
Single-walled carbon nanotubes single-walcarbonnanotube; SWCNT
A carbon nanotube formed by crimping a single layer of graphene sheets.
Note. Seamless nanoscale cylindrical honeycomb structure formed by crimping a single layer of graphene sheets.
[ISO /T S80004-3.2010, definition 4.4]
2.1.2
Multiwall carbon nanotubes multiwalcarbonnanotube; MWCNT
A carbon nanotube having a seamless casing structure obtained by crimping a coaxial or nearly coaxial multilayer graphene sheet.
Note. The structure is formed by nesting a plurality of single-walled carbon nanotubes. The smaller diameter is cylindrical, and the cross section tends to have a polygonal structure as the diameter increases.
[ISO /T S80004-3.2010, definition 4.6]
2.1.3
Carbon nanotube film CNTfilm
A single-walled or multi-walled carbon nanotube film formed by a substrate filtration method or the like.
See Figure 1 (c).
2.1.4
Sheet resistance sheetresistance
Rs
The sheet resistance of a semiconductor or thin metal film, the resistance of a film having substantially the same thickness as the current.
Note 1. Two-dimensional (xy) sheet resistance (Rs) can be used to determine the electrical resistance of a film with consistent electrical properties. In a geometric rectangle, Rs=R/(L/w), where R is
The resistance to be tested, R = V/I, L is the spacing of the parallel electrodes, the voltage difference across the electrodes is represented by V, and w is the length of the electrode. Current I must follow the membrane
The plane flows, not perpendicular to it (see Figure 4). The aspect ratio L/w is the number of squares of the film sample. The unit of the sheet resistance can be expressed in ohms (Ω), this
For ease of expression, in ohms per square (Ω/sq).
Note 2. See references [1~4].
2.1.5
Current-voltage characteristics I-Vcharacteristic
IV characteristics
There is a relationship between the current and the corresponding voltage (or potential difference).
2.1.6
Four probe measurement method 4-probemeasurement
A method of measuring the resistance of a material, and the measured resistance value is not affected by the probe resistance and contact resistance.
Note. In the method, the four probes in contact with the sample to be tested are arranged in a straight line, the voltage is measured by two probes located inside, and the current is passed through two external probes.
Come on. The sample resistance can be calculated from Ohm's law, and its resistivity can be obtained by introducing the geometric parameters of the sample. See reference [3, 4].
2.1.7
4-wire measurement
A four-probe measurement using the wire as a probe.
2.1.8
Four point measurement method 4-pointmeasurement
A four-probe measurement using a point tip as a probe.
Note. This method is commonly used to measure the sheet resistance of a film sample that is much wider than the probe spacing.
2.2 Abbreviations
The following abbreviations apply to this document.
DCE. Dichloroethane;
DMF.N, N-Dimethylformamide;
PVDF. Polyvinylidenefluoride;
THF. Tetrahydrofuran.
3 sample preparation method
3.1 Overview
In the four-probe measurement method, the powdered carbon nanotubes are preferably processed into a sheet or film sample [5, 6]. Due to the preparation of the sheet sample
It is possible to cause deformation and change the intrinsic properties of carbon nanotubes due to high pressure, so film samples are preferred for testing. To avoid any
The external force may have a significant impact on the measurement, and it is important to prepare a large area of uniform carbon nanotube film. In the preparation process of the film, test
Consider two important factors.
a) selecting a suitable dispersant;
b) Determine the amount of carbon nanotubes needed to prepare the film.
If it is difficult to prepare a uniform carbon nanotube film having a suitable geometrical parameter, the film can be cut into a strip shape.
3.2 Reagents
3.2.1 Carbon nanotubes
Untreated carbon nanotubes should be used for experimental testing.
3.2.2 Dispersant
THF is recommended as a standard dispersant for commonly used carbon nanotubes [7, 8]. With other organic dispersants (such as DMF, ethanol, 1,2-
Compared with DCE), THF can uniformly disperse carbon nanotubes, reduce the surface damage of carbon nanotubes during ultrasonic dispersion, and can be in the shape of a film.
After being separated, it is effectively separated. It is recommended to use THF with a purity of >99.8% to reduce the contamination of carbon nanotubes. This standard compares and summarizes no
The experimental results of the same dispersant are included in Table A.1 of Appendix A.
3.3 Preparation of carbon nanotube film
First, disperse 2mg of carbon nanotubes in 20mL THF solution, set the initial temperature to 25 ° C, sonication (bath, 40
kHz) 30min. The suspension was vacuum filtered using a 220 nm pore size PVDF filter (25 mm diameter) to form a thin film.
(see picture 1). The film was dried in an environment of 80 ° C for 12 h and above to constant weight. The film thickness after treatment is (50 ± 1) μm, the film diameter
It is 18mm (see A.2 and A.3).
Description.
(a)---dispersion process of carbon nanotubes in tetrahydrofuran solution;
(b)---filtering equipment;
(c) --- A carbon nanotube film formed by filtering through a 220 nm pore size, 25 mm diameter PVDF filter.
Figure 1 Preparation of carbon nanotube film
3.4 Preparation of ribbon carbon nanotube film
The carbon nanotube film was cut into a strip sample suitable for four-wire measurement by an antistatic cutter. Sample recommended size. Width is
1mm~2mm, length is about 10mm.
4 Determination of thin layer resistance of carbon nanotubes
4.1 Four point measurement method
4.1.1 Method application range
The method is suitable for the sheet resistance of carbon nanotube film samples whose shape and flatness remain unchanged during film preparation and testing.
Determination.
4.1.2 Experimental procedures and measurement conditions
The structural principle of the probe and the schematic diagram of the probe card in the four-point measurement method are shown in Fig. 2.
The four-point measuring device consists of four platinum needles arranged equidistantly with a uniform tip radius, usually with a needle spacing of 1 mm. Current source (A) passed
Two external probes provide current and a voltmeter (V) measures the voltage between the two internal probes (see Figure 2a) to determine the sample resistance. volt
It must have a high input impedance, otherwise the equations (1) and (2) listed in Chapter 5 cannot be used.
a) Four-point probe schematic b) Typical four-point probe board
Description.
S---probe spacing.
Figure 2 Principle of four-point measurement
Testing can be performed using a commercial probe platform (see Figure 3). The carbon nanotube film is placed on a height adjustable sample stage. Adjusting the sample stage
The height is such that the probe is in contact with the carbon nanotube film. Observe the physical contact of the probe with the surface of the sample by means of an optical microscope. Adjacent exploration
The needle spacing is 1mm. During the test, a small current (up to 1 μA) was used to avoid sample damage.
Figure 3 Four-point measuring device
4.2 Four-wire measurement method
4.2.1 Application scope of the method
The method is suitable for the sheet resistance measurement of a strip carbon nanotube film sample.
A simple device for measuring the resistance is shown in Fig. 4. Four platinum wires with a diameter of 0.1mm are vertically fixed to an insulating substrate and protected.
The distance between the platinum wires is L=3mm. Place the platinum wire electrode on the sample without damage. Use small current (up to 1μA)
The assay is performed to avoid sample damage.
Description.
L --- proximity probe spacing;
t --- ribbon carbon nanotube film thickness;
w---band carbon nanotube film width.
Figure 4 Schematic diagram of the four-wire measurement method
5 Data Analysis/Results Description
5.1 Four-point measurement method for measuring SWCNT or MWCNT sheet resistance
The calculation formula for measuring the sheet resistance by four-point measurement method is shown in formula (1).
Rs=F×
(1)
In the formula.
Rs --- sheet resistance;
V --- measured voltage;
I --- test current;
The slope of the V/I ---V/I curve;
F --- geometric correction factor [9,10].
When the sample size is much larger than the probe spacing S (see Figure 2), F = (π/ln2) = 4.53236. Other special cases can be found in the references.
Figure 1 and Table 1 in [9]. For example, when the center of the circle is measured and the diameter of the circle is greater than 40S, a measurement with an accuracy of more than 99% can be obtained.
As a result; when the diameter of the circle is measured and the diameter of the circle is larger than 100 S, a measurement error of not more than 1% can be obtained.
5.2 Four-wire measurement method for measuring SWCNT or MWCNT sheet resistance
The calculation formula for measuring the sheet resistance by the four-wire measurement method is shown in equation (2).
Rs=
÷ (2)
In the formula.
Rs --- sheet resistance;
V --- measured voltage;
I --- test current;
V/I --- the slope of the voltage relative current;
w --- the width of the sample measured by a calibrated optical microscope;
L --- line spacing.
Appendix A
(informative appendix)
Case Analysis
A.1 Sample preparation
A.1.1 SWCNT and MWCNT
SWCNT comes from two producers and MWCNT comes from three producers. The above untreated CNTs were used throughout the experiment.
A.1.2 Selection of dispersant
The organic dispersants used to disperse CNTs are mainly DMF, THF and 1,2-DCE. Among them, in terms of facilitating operation and dispersion,
THF works best. A fully dispersed CNT suspension can be obtained by the treatment thereof, and the surface damage of the CNT during ultrasonic vibration is reduced.
Finally, it can be quickly dried to form a film.
Table A.1 lists the properties considered for the dispersion of carbon nanotubes and the preparation of the film.
Table A.1 Dispersant properties for film preparation
THF DMF 1,2-DCE
CNT dispersion effect is good depending on the type of CNTs
Ultrasonic treatment
Degree of influence on the electronic structure of CNT
No effect [7] Influential (nanotube π bond rupture) [11]
influential
(Cl2 or HCl doping) [12]
Evaporation is very fast and fast
A.2 Determination of the amount of SWCNTs and/or MWCNTs
In order to determine the amount of CNT required to form a uniform thickness of carbon nanotube film, a certain amount of CNT is dispersed in a volume-determined dispersion.
Tested in the agent. When 1 mg of SWCNT or MWCNT is used, the film thickness is in the range of 10 μm to 50 μm. When using 5mg
When SWCNT or MWCNT, the film thickness is easily controlled within the range of (90 ± 5) μm, but the film is brittle, especially when it is mechanically
When the force is cut into strips. When 2mgSWCNT or MWCNT is used, the film with the most uniform thickness (50±1)μm can be obtained.
The CNTs were uniformly bundled, and the ribbon samples in the four-wire measurement method exhibited strong toughness. The above results show that 2mg CNT is prepared uniformly
A suitable amount of film of thickness. The thickness of the strip SWCNT or MWCNT can be obtained by field emission scanning electron microscopy (fieldemission-
Scanning electron microscopy, FE-SEM), as shown in Figure A.1.
Description.
The ribbon-shaped carbon nanotube film shown in the figure is prepared by using (A) 1 mg, (B) and (D) 2 mg, and (C) 5 mg of CNT, respectively, dispersed in 20 mL.
In THF. (D) is a side view of a self-supporting uniform thickness ribbon carbon nanotube film.
Figure A.1 FE-SEM image of a ribbon carbon nanotube film
A.3 Preparation of carbon nanotube film
First, 2mg SWCNT or MWCNT is dispersed in 20mL THF for sonication (bath, 40kHz, 25 °C)
30min. The suspension obtained by sonication was vacuum filtered with a 220 nm pore size PVDF membrane (25 mm diameter) and shaped.
Film formation. Finally, it was dried at 80 ° C for 12 h to obtain a carbon nanotube film having a diameter of 18 mm.
The main purpose of dispersion and filtration is to prepare a carbon nanotube film with uniform thickness and large area (as shown in Figure A.2(A)).
Point measurement method. Sometimes, a carbon nanotube film having a uniform thickness and having a suitable geometric factor is difficult to produce. When the film sample produces edge curl
At the time (Fig. A.2(B)), the film was cut into a strip sample (Fig. A.2(C)), and the sheet resistance was measured by a four-wire measurement method.
Description.
(A)---thickness uniform CNT film, suitable for four-point measurement method;
(B) --- edge curled CNT film, not suitable for four-point measurement;
(C) --- Cut into a strip of CNT film, suitable for four-wire measurement.
Figure A.2 Preparation of the obtained carbon nanotube film
A.4 Measurement results of thin layer resistance (Rs) of carbon nanotubes
Table A.2 is a thin sample measured by four-wire measurement method for SWCNTs and MWCNTs prepared by five different manufacturers.
Layer resistance Rs value. The CNTs supplied by each manufacturer were filmed 5 times, and each time the film was formed, it was cut into strip samples for measurement. In Table A.2
The sheet resistance values of the respective CNT samples were quite close. The results show that the strips with uniform properties can be prepared by the method provided in this standard.
Carbon nanotube film.
Table A.2 Resistance and Sheet Resistance of Banded MWCNTs and SWCNTs
CNT unit 1 2 3 4 5
Relative comprehensive uncertainty
Value ±n(%)a
MWCNT
(A)
R(Ω) 19.03 27.27 27.04 20.83 20.38
Rs(Ω/sq) 5.45 5.45 5.41 5.42 5.43 5.43±0.37%
MWCNT
(B)
R(Ω) 2080 1920 1860 1680 1310
Rs(Ω/sq) 693.3 672.0 620,0 616.0 679.5 656.17±5.44%
MWCNT
(C)
R(Ω) 226.8 185.6 210.3 225.4 202.6
Rs(Ω/sq) 83.92 89.09 92.53 78.89 83.07 85.50±6.26%
SWCNT
(D)
R(Ω) 9.55 7.0 7.4 7.6 6.4
Rs(Ω/sq) 1.43 1.40 1.53 1.52 1.79 1.53±9.80%
SWCNT
(E)
R(Ω) 38.9 36.0 52.1 38.2 36.1
Rs (Ω/sq) 14.00 12.60 18.24 16.43 14.44 15.10±14.64%
An (%) includes all relative uncertainties, and n is the standard deviation/average value x 100.
Table A.3 compares the measurement results of the four-point measurement method and the four-line measurement method, where the raw materials of the film-forming samples used in the two methods are from
The same supplier. Both the center and the edge of the film were tested using the four-point measurement. By comparison, the measurement results of the two methods are basically
Consistent. This indicates that the measurement of the sheet resistance is not affected by the measurement method when the sample preparation conditions are the same.
Table A.3 Comparison of four-point measurement method and four-line measurement method under the same sample preparation conditions
Method Thin layer resistance Rs/(Ω/sq)
Four-point measurement 5.45 (center) and 5.45 (edge)
Four-wire measurement method 5.43±0.02 (average)
The sample parameters are as follows.
--- Four-point measurement method. The sample diameter is 18 mm and the probe spacing (s) is 1.0 mm.
--- Four-wire measurement method. The proximity probe spacing (L) is 3 mm, and the CNT sample width (w) is in the range of 0.6 mm to 0.8 mm.
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Related standard:   GB/T 22379-2017  GB/T 33818-2017
   
 
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