Search Result of Chinese Standard: 'GB/T 33818-2017'
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Carbon nanotube conductive paste
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Detail Information of GB/T 33818-2017; GB/T33818-2017
Description (Translated English): Carbon nanotube conductive paste
Sector / Industry: National Standard (Recommended)
Classification of Chinese Standard: G13
Classification of International Standard: 59.100.20
Word Count Estimation: 13,169
Date of Issue: 2017-05-31
Date of Implementation: 2017-12-01
Quoted Standard: GB/T 606; GB/T 1725; GB/T 6753.1; GB/T 22235-2008; GB/T 24490; GB/T 24491; GB/T 2303.10
Proposing organization: Chinese Academy of Sciences
Issuing agency(ies): General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China, China National Standardization Administration Committee
Summary: This standard specifies the terms, requirements and test methods, inspection rules, and marking, packaging, shipping, storage and order contents of carbon nanotube conductive pastes. This standard is applicable to the quality inspection and acceptance of liquid phase products using multi-walled carbon nanotubes as conductive medium in Keng ion batteries, conductive coatings and conductive adhesives. Single-walled carbon nanotube slurry products can be implemented with reference to this standard.
GB/T 33818-2017
Carbon nanotube conductive paste
ICS 59.100.20
G13
National Standards of People's Republic of China
Carbon nanotube conductive paste
2017-05-31 released
2017-12-01 Implementation
General Administration of Quality Supervision, Inspection and Quarantine of People's Republic of China
China National Standardization Administration released
Foreword
This standard was drafted in accordance with the rules given in GB/T 1.1-2009.
This standard proposed by the Chinese Academy of Sciences.
This standard by the National Standardization Technical Committee of nano-materials sub-technical committee (TC279/SC1) centralized.
This standard was drafted. Beijing Tian Nai Technology Co., Ltd., Shenzhen Bei Te Rui Nami Technology Co., Ltd., Hefei Guoxuan Transtech Services
Source Co., Ltd., Chennai (Zhenjiang) Materials Technology Co., Ltd., Shenzhen City, the era of New Energy Technology Co., Ltd., Metallurgical Industry Information Standard
Institute and so on.
The main drafters of this standard. Mao guan, Yan Yan, Meijia, Xu Xiaoming, Feng Guanghui, Li Xiaojun, check Xiufang, He Chia slow, Lu Xue, Li Weidong,
Dai Shi Feng.
Carbon nanotube conductive paste
1 Scope
This standard specifies the terms carbon nanotube conductive paste, requirements and testing methods, inspection rules and signs, packaging, transportation, storage and
Order Contents.
This standard applies to lithium-ion batteries, conductive coatings and conductive adhesives and other fields using multi-walled carbon nanotubes as the conductive medium of the liquid phase
Department of product quality inspection and acceptance. Single-walled carbon nanotube slurry products can refer to the implementation of this standard.
2 Normative references
The following documents for the application of this document is essential. For dated references, only the dated version applies to this article
Pieces. For undated references, the latest edition (including all amendments) applies to this document.
GB/T 606 chemical reagent moisture determination Karl Fischer method
GB/T 1725 Paints, varnishes and plastics Determination of non-volatile matter content
GB/T 6753.1 Paints, varnishes and printing inks - Determination of fineness of grinding
Determination of liquid viscosity GB/T 22235-2008
GB/T 24490 multi-walled carbon nanotubes purity measurement methods
GB/T 24491 multi-walled carbon nanotubes
QB/T 2303.10 Slurry paper for batteries - Part 10. Determination of pH
3 Terms and definitions
The following terms and definitions apply to this document.
3.1
Carbon nanotube carbon nanotube
Nanotubes made of carbon atoms.
Note. Usually consists of curly carbon layer, including single-walled carbon nanotubes, double-walled carbon nanotubes and multi-walled carbon nanotubes.
[GB/T 30544.3-2015, Definition 4.3]
3.2
Multi-walled carbon nanotubes multi-waledcarbonnanotubes; MWCNTs
Three or more layers of graphite sheets are crimped into a coaxial nested hollow quasi-one-dimensional tubular nanocarbon material.
[GB/T 24491-2009, Definition 3.1]
3.3
Multiphase mixture composed of carbon nanotubes as a main solid component and as a conductive medium with a certain liquid.
Note. According to the type of liquid, generally divided into aqueous slurry and non-aqueous slurry.
3.4
Aggregate agglomerate
Stacks, aggregates, or a mixture of both formed by stacking or winding a plurality of carbon nanotubes have an outer surface area of
The sum of the surface areas of single carbon nanotubes is similar.
Note 1. Aggregates are weak forces, such as van der Waals forces or simple physical entanglement.
Note 2. Aggregates are also referred to as secondary particles, whereas source particles are referred to as primary particles.
3.5
Solid content solidcontent
Carbon nanotubes conductive paste after drying in the specified conditions accounted for the percentage of the weight of the slurry before drying.
Note. The solid content of slurry after drying carbon nanotubes and may be dispersed aids, stabilizers and so on.
3.6
Slurry fineness hegmanfinenessofpaste
The size of carbon nanotube aggregates in the slurry.
3.7
Slurry light transmittance transmittanceofpaste
The luminous flux of a liquid passing through it is the percentage of its incoming luminous flux.
3.8
Volume resistivity volumeresistivity
Resistivity per unit volume of the membrane prepared in the prescribed procedure.
4 requirements
4.1 Principles
Technical requirements for carbon nanotube slurry include general technical requirements and additional technical requirements for specific application areas. Carbon nanotube slurry at
Meet the general technical requirements, based on the use of this product, the supply and demand sides negotiate to select the appropriate additional technical requirements.
4.2 General technical requirements
4.2.1 Appearance. The appearance of the product should be black liquid slurry, uniform state, no obvious particles, have a certain mobility.
4.2.2 Slurry carbon nanotubes should be consistent with GB/T 24491 in the technical requirements.
4.2.3 Slurry solids content and carbon nanotube content data should be provided by the supplier to the demand side.
4.2.4 auxiliary components in the slurry mass fraction of more than 0.5%, the need to provide component categories (for example, macromolecules).
4.2.5 slurry fineness should not exceed 10μm.
4.2.6 carbon tube concentration diluted to 0.005% (mass fraction) of the light transmittance should not exceed 20%.
4.2.7 slurry coating volume resistivity should not exceed 1.0Ω · cm.
4.3 Additional technical requirements (for lithium-ion battery field)
4.3.1 The value of the viscosity of the slurry After standard sample calibration, the value provided by the supplier.
4.3.2 The total content of magnetic foreign matter (Fe, Cr, Ni, Zn, Co) in the slurry should not exceed 0.002% (mass fraction) of the carbon content.
4.3.3 The content of soluble metallic element impurities (Fe, Cr, Ni, Cu, Zn, Co) in the slurry should not exceed 0.2% of the carbon content
number). If users have special requirements, they can be negotiated by both parties.
4.3.4 Anhydrous water content system should not exceed.2000 × 10-6 (mass fraction). If users have special requirements, can be both parties by supply and demand
Business OK.
4.3.5 Aqueous slurry product pH value should generally be within the range of 5.0 to 9.0.
5 test methods
5.1 appearance
Visual inspection.
5.2 Solid content
According to GB/T 1725 determination and calculation results.
5.3 carbon nanotubes content
5.3.1 Follow the procedure in 5.2 to prepare a sample of the dried pulp.
5.3.2 According to the procedure specified in GB/T 24490, determine and calculate the content of carbon nanotubes.
5.4 slurry fineness
According to GB/T 6753.1 determination.
5.5 Light transmittance
5.5.1 Instruments and materials
Ultrasonic cleaner, UV-visible spectrophotometer, high-speed mixer (maximum speed of at least 3000rpm), cuvettes and other auxiliary
Aids
5.5.2 Preparation before testing
5.5.2.1 Wash the 1 cm cuvette and glassware with an ultrasonic cleaner and dry.
5.5.2.2 Open the UV - visible spectrophotometer, after the start stable 30min before measuring, the wavelength is set to 546nm.
5.5.3 Test procedure
5.5.3.1 The sample slurry to be tested sealed with self-sealing bags, and then stirred with a glass rod 5min, the slurry in a uniform state.
5.5.3.2 Weigh 0.5g ± 0.01g slurry samples with an analytical balance and place in a beaker.
5.5.3.3 Add a suitable amount of solvent miscible with the slurry The sample to be diluted to a concentration of carbon nanotubes of 0.001%.
Note. The amount of solvent can generally press (50000 × carbon nanotubes in the slurry content -0.5) g to.
5.5.3.4 The diluted solution was sealed, the solution was stirred at 3000r/min stirring speed 30min ± 0.1min, after standing still
10min.
5.5.3.5 Pipette the supernatant, clean the cuvette reservoir, and wipe clean the cuvette reservoir with its outer side wall.
5.5.3.6 Then pipette the supernatant, into the liquid pool, the liquid level height of the cell cuvette 2/3, into the UV - visible light
Meter, until the value is stable read the transmittance value.
5.5.4 Calculation Results
5.5.4.1 Parallel measurement three times, if the deviation between the three test results does not exceed 10%, the measured value is valid; the arithmetic mean is measured
result.
5.5.4.2 If the deviation between the measured values exceeds 10%, then re-test 3 times; if necessary, according to 5.5.3 re-sample, test.
5.6 Volume resistivity
5.6.1 Instruments and materials
Four-probe resistivity meter, blast oven, tablet press, glass plate, standard blade applicator, high temperature polyester film (PET film) and others
Auxiliary tools.
5.6.2 Sample Preparation
5.6.2.1 The slurry sample to be tested sealed with ziplock bag, and then stirred with a glass rod 5min, the slurry in a uniform state.
5.6.2.2 drip ethanol on a clean glass plate, the PET film on the flat glass, wipe the PET film with paper, and glass tight
Close fit. A suitable amount of slurry sample was placed on the PET film and the slurry was scraped using a standard knife coater (slit.200 μm).
5.6.2.3 into the blast oven drying 80 ℃ ~ 120 ℃ 1h ~ 2h.
5.6.2.4 After drying the sample film cut into thin discs 15mm in diameter, making two or more. Placed in the tablet press to 10t pressure
Durance 3min ~ 5min.
5.6.2.5 Measure the thickness of the dressing on the membrane after compaction using a screw micrometer and test 3 different positions and average.
5.6.2.6 Volume resistivity of the test sample using a four-probe resistivity instrument, select the appropriate range, the dressing thickness, wafer diameter (15mm)
Other data input to the tester parameter settings, other parameters automatically selected by the tester.
5.6.3 Calculation Results
5.6.3.1 For the same sample, test 2 samples, each of which needs to measure the volume resistivity data of 3 different positions. in case
The test data is valid if the deviation between each set of test data does not exceed 10%.
5.6.3.2 With four probe resistivity instrument comes with software processing data, giving the results; or take its arithmetic average.
5.6.3.3 If the deviation between each set of test data exceeds 10%, the test data is invalid. Need to re-test, if necessary, re-sample
test.
5.7 viscosity
According to GB/T 22235-2008 rotary viscometer method to determine the requirements.
5.8 magnetic foreign body content
The test needs to be determined by the supply and demand sides negotiated. By consensus, the method in Appendix A can also be implemented.
5.9 soluble metal elements impurity content
The test needs to be determined by the supply and demand sides negotiated. By consensus, the method in Appendix B may also be implemented.
5.10 water-free system
According to GB/T 606 in the determination.
5.11 pH value
Measure according to QB/T 2303.10.
6 inspection rules
6.1 Batch
6.1.1 products should be batch inspection.
6.1.2 inspection lot from the same delivery date, the same use of slurry composition.
6.2 The number of samples
Each batch of at least 3 samples.
6.3 inspection items
6.3.1 Test classification
The product inspection specified in this standard is divided into batch inspection and type inspection.
6.3.2 batch inspection
6.3.2.1 Each batch of product appearance, solid content batch test.
6.3.2.2 For lithium-ion battery applications, but also deal with the magnetic foreign body content, the content of soluble metal impurities and water-free system of water
The amount of batch inspection.
6.3.3 type test
Type inspection In one of the following conditions, the technical requirements of the standard specified in all tests.
a) Raw material batch number, model, supplier, etc. have changed;
b) When the production process has changed;
c) normal production of 3 months;
d) the production equipment is discontinued for more than three months and the first production is started again;
e) customer use for special requirements.
6.3.4 batch inspection and type inspection items
See Table 1 (lithium-ion battery applications as an example).
Table 1
Test item requirements Article number Test method Article number Test category
Appearance 4.2.1 5.1 batch inspection
Solid content 4.2.3 5.2 batch test
Conductive agent content 4.2.3 5.3 Type test
Slurry fineness 4.2.5 5.4 type test
Slurry light transmittance 4.2.6 5.5 type test
Volume resistivity 4.2.7 5.6 type test
Viscosity 4.3.1 5.7 type test
Magnetic foreign body content 4.3.2 5.8 batch test
Soluble metal impurity content 4.3.3 5.9 batch test
Water content of anhydrous systems 4.3.4 5.10 batch inspection
pH 4.3.5 5.11 type test
6.4 inspection and acceptance
6.4.1 The product shall be inspected by the supplier's quality supervision department to ensure that the quality of the product meets the requirements of this standard or the contract of the contract and the quality
Amount of certificate.
6.4.2 When the appearance of the pulp product is unqualified, the quality of the product shall be judged as unqualified.
6.4.3 slurry product composition, fineness, relative absorbance, conductivity and other tests in one failed, sentenced to the batch of products failed.
6.4.4 The demand side should receive the product according to the standard test, if the test results inconsistent with the provisions of this standard or contract, should be in
Within 15 days from the date of receipt of the product, it shall be submitted to the supplier for negotiation between the supplier and the buyer. For arbitration, arbitration at the demand side, and by the supply and demand
Side to participate.
7 logo, packaging, transportation, storage
7.1 Packaging and marking
7.1.1 The products tested by the general 20L ~ 50L for a packing unit. Packed tightly, the outer wall of the barrel should be affixed with a library label,
It states.
a) Supply Number (supply list number for the shipment);
b) the company's trademark and name;
c) product specifications;
d) date of production;
e) company contact information, address.
7.1.2 If the customer has specific requirements, can be the appropriate packaging and logo design.
7.1.3 When supplied, each batch of product shall be accompanied by the "Report on the Conductive Paste Test of Carbon Nanotubes", which shall include the relevant technical parameters of the batch of products.
7.1.4 Each batch of products with "invoices," including but not limited to the following.
a) Customer's name and address;
c) product code
d) product name
e) product lot number;
f) packaging specifications;
g) delivery quantity and total weight;
h) others.
7.2 Transportation and storage
7.2.1 The product is suitable for storage under normal normal ambient temperature. The warehouse should be ventilated and dry. Products from the date of production, upon request
Packaging, storage conditions, shelf life of not more than 12 months.
7.2.2 Product stacking should be neat, clean, registered trademarks, production lot number and other signs should be clearly identified, non-stressful.
7.2.3 Avoid mixing and mixing with items that can spoil or damage the package.
7.2.4 During storage and transportation, the packaging of the product shall be clean and undamaged. Any product that leaks out of the package shall not be returned to the package.
8 Order Contents
The contents of the purchase order should include but not limited to the following.
a) product name
b) Specification or related technical requirements;
c) the quantity;
d) price;
e) delivery date;
f) Other relevant information.
Appendix A.
(Informative)
Determination of magnetic foreign matter content
A.1 Test equipment and materials
ICP-OES, analytical balance (range 1000g, accurate to 0.01g), electric hot plate, electric
Blender, super magnet (coated with Teflon, magnetic force ≥ 5000Gs), beaker, volumetric flask, graduated cylinder, glass rod, watch glass, filter paper, funnel and its
He assisted tools.
A.2 Reagents
A.2.1 nitric acid (superior pure, 65%).
A.2.2 hydrochloric acid (superior pure, 37%).
A.2.3 Deionized water.
A.2.4 standard stock solution (containing iron, copper, zinc, nickel, chromium, cobalt, concentration 100 × 10-6).
A.3 Analysis steps
A.3.1 Preparation of standard solution
With 5% nitric acid iron, zinc, nickel, chromium, cobalt standard stock solution diluted in 50mL volumetric flask, the standard stock solution sampling
The amount and concentration after dilution are shown in Table A.1.
Table A.1
Take the volume of stock solution/mL 0 1 2 4
After the preparation of the standard solution concentration/× 10-6 0 2 4 8
A.3.2 pre-treatment
A.3.2.1 Weigh slurry 350g placed in 1000mL plastic, add 350mL deionized water, with a super-coated Teflon bar magnet (magnetic
Force ≥ 5000Gs) for 1h on the roller.
A.3.2.2 Remove the magnetic bar into a 250mL beaker, add deionized water ultrasonic cleaning 30s, washed 3 to 5 times until the clear liquid clarification (clear
Direct visual inspection after cleaning bar magnet, carefully observe the surface of the bar magnet obvious metal particles, if more obvious in the test data to focus on
Note this sample).
A.3.2.3 Take two 100mL beaker, one without any sample, as a blank sample, the cleaned magnetic rod into another beaker, two
Beaker were added 60mL dilute aqua regia (1. 1) (the bar can be immersed), boiled until the liquid near dry, add a small amount of deionized water.
A.3.2.4 to be boiled solution was cooled to room temperature, filtered with a funnel to 100mL volumetric flask, and rinsed with deionized water beaker and magnetic rod
2 to 3 times, the lotion into the volumetric flask, shake the volume to be measured.
A.3.3 Test
ICP-OES test which Fe, Zn, Ni, Cr, Co content.
A.4 results that method
A.4.1 Magnetic foreign body content of Fe, Zn, Ni, Cr, Co and 5 kinds of metal content.
A.4.2 Parallel test 3 times, if the deviation between each test data does not exceed 10%, the test data is valid, the result is its arithmetic
Mean.
A.4.3 If the deviation between each set of test data exceeds 10%, the test data is invalid. Need to re-test, if necessary, re-sample test.
Appendix B
(Informative)
Soluble metallic elements - Determination of impurity content
B.1 Test equipment and materials
Inductively coupled plasma atomic emission spectrometer (ICP-OES), analytical balance (range 100g, accurate to 0.0001g), hot plate, burn
Cup......
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