CN113567293B - Method for testing carbon nano tube content in carbon nano tube conductive paste - Google Patents
Method for testing carbon nano tube content in carbon nano tube conductive paste Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 156
- 239000002041 carbon nanotube Substances 0.000 title claims abstract description 151
- 229910021393 carbon nanotube Inorganic materials 0.000 title claims abstract description 151
- 238000012360 testing method Methods 0.000 title claims abstract description 78
- 238000000034 method Methods 0.000 title claims abstract description 47
- 239000002270 dispersing agent Substances 0.000 claims abstract description 41
- 230000004580 weight loss Effects 0.000 claims abstract description 36
- 238000002411 thermogravimetry Methods 0.000 claims abstract description 35
- 239000007787 solid Substances 0.000 claims abstract description 32
- 238000001035 drying Methods 0.000 claims abstract description 14
- 238000010438 heat treatment Methods 0.000 claims description 21
- 239000012298 atmosphere Substances 0.000 claims description 15
- 230000001681 protective effect Effects 0.000 claims description 12
- 239000012300 argon atmosphere Substances 0.000 claims description 4
- 239000001307 helium Substances 0.000 claims description 4
- 229910052734 helium Inorganic materials 0.000 claims description 4
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 4
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 12
- 229910052782 aluminium Inorganic materials 0.000 description 12
- 239000011888 foil Substances 0.000 description 12
- 238000005303 weighing Methods 0.000 description 9
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 6
- 239000006258 conductive agent Substances 0.000 description 6
- 239000010439 graphite Substances 0.000 description 5
- 229910002804 graphite Inorganic materials 0.000 description 5
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 4
- 229910001416 lithium ion Inorganic materials 0.000 description 4
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 4
- 239000002002 slurry Substances 0.000 description 4
- 229910052786 argon Inorganic materials 0.000 description 3
- 239000007772 electrode material Substances 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 229920000049 Carbon (fiber) Polymers 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000004917 carbon fiber Substances 0.000 description 2
- 229910052744 lithium Inorganic materials 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000002035 prolonged effect Effects 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- KFDQGLPGKXUTMZ-UHFFFAOYSA-N [Mn].[Co].[Ni] Chemical compound [Mn].[Co].[Ni] KFDQGLPGKXUTMZ-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000011149 active material Substances 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- QHGJSLXSVXVKHZ-UHFFFAOYSA-N dilithium;dioxido(dioxo)manganese Chemical compound [Li+].[Li+].[O-][Mn]([O-])(=O)=O QHGJSLXSVXVKHZ-UHFFFAOYSA-N 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- GELKBWJHTRAYNV-UHFFFAOYSA-K lithium iron phosphate Chemical compound [Li+].[Fe+2].[O-]P([O-])([O-])=O GELKBWJHTRAYNV-UHFFFAOYSA-K 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000001757 thermogravimetry curve Methods 0.000 description 1
- 229920001169 thermoplastic Polymers 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
- 239000004416 thermosoftening plastic Substances 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
- G01N5/04—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by removing a component, e.g. by evaporation, and weighing the remainder
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y35/00—Methods or apparatus for measurement or analysis of nanostructures
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Nanotechnology (AREA)
- Engineering & Computer Science (AREA)
- General Health & Medical Sciences (AREA)
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- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
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- Carbon And Carbon Compounds (AREA)
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Abstract
The invention provides a method for testing the content of carbon nanotubes in carbon nanotube conductive paste. The method comprises the following steps:(1) Testing the solid content of the conductive paste of the carbon nano tube to be tested to obtain the solid content of the conductive paste of the carbon nano tube to be tested and a drying product of the carbon nano tube to be tested; (2) Taking a dispersant with the same type as the dispersant in the carbon nanotube conductive paste to be tested, and performing thermogravimetric analysis and test to obtain the weight loss rate A of the dispersant 1 The method comprises the steps of carrying out a first treatment on the surface of the (3) Performing thermogravimetric analysis test on the dried product of the carbon nanotube to be detected to obtain the weight loss rate A of the dried product of the carbon nanotube to be detected 2 The method comprises the steps of carrying out a first treatment on the surface of the (4) By adjusting the solid content and the weight loss rate A 1 And weight loss ratio A 2 And calculating to obtain the carbon nanotube content in the carbon nanotube conductive paste to be measured. According to the invention, the interference of the sample contacting with air moisture can be eliminated by a thermogravimetric analysis method, and the dispersing agent weight loss rate is obtained more accurately and intuitively by using a thermogravimetric curve, so that the accuracy of a test result is improved.
Description
Technical Field
The invention belongs to the technical field of material content analysis in lithium ion batteries, and relates to a method for testing the content of carbon nanotubes in carbon nanotube conductive paste.
Background
Conductive pastes are thick objects formed by uniformly distributing conductive materials in thermoplastic or thermosetting materials. The carbon nano tube is a one-dimensional tubular nano material formed by curling single-layer or multi-layer graphite, has a plurality of excellent characteristics, and has higher electronic conductivity and lower required dosage when being applied to conductive slurry compared with the traditional conductive agents such as the traditional conductive carbon black, conductive graphite, conductive carbon fiber and the like. The carbon nanotube conductive paste has attractive application prospect in the aspect of lithium ion power battery conductive agents, is used as a novel efficient conductive agent of a lithium ion power battery, and is constructed into a cross-connected network through mutual cross superposition in practical application so as to transfer electrons, thereby realizing conduction, and the carbon nanotubes are contacted with each other in the network or are compounded with substances with other conductive characteristics so as to be contacted with each other, so that the high-current discharge capacity of the battery is effectively improved, and the battery capacity is remarkably improved. Meanwhile, the excellent heat conduction performance of the carbon nano tube is also beneficial to heat dissipation of the battery during charge and discharge, so that polarization of the battery is reduced, high-low temperature performance of the battery is improved, and the cycle life of the battery is prolonged. And the carbon nanotube conductive paste can be applied to various electrode materials, such as lithium iron phosphate, lithium cobaltate, lithium manganate, ternary nickel cobalt manganese, graphite and other electrode materials.
The carbon nano tube conductive paste is a novel efficient conductive agent for lithium batteries, can replace traditional conductive agents such as traditional conductive carbon black, conductive graphite, conductive carbon fiber and the like, has the superior characteristics of ultra-high length-diameter ratio, ultra-large specific surface area, ultra-low volume resistivity and the like, can be applied to various electrode materials such as LFP, LCO, LMN, NCM or graphite and the like, and has the addition amount of only 0.5-1%, so that the following performances of the battery core can be remarkably improved: the internal resistance of the battery is obviously reduced; the gram capacity of the active material is improved; the consumption of the conductive agent and the consumption of the binder are obviously reduced; the high-current discharge power density is improved; enhancing electrolyte absorption; the service life is prolonged. The carbon nano tube has excellent conductivity, and can improve the conductivity of the pole piece and the battery performance when being applied to a lithium ion battery.
At present, a common method for testing the content of the carbon nano tube in the carbon nano tube conductive paste comprises the steps of directly heating a CNT conductive paste solid residue and a dispersing agent with a tube furnace through nitrogen protection, taking out, cooling and weighing, calculating the weight loss rate of the sample mass reduction before and after heating as the percentage of the original mass, and calculating the content of the carbon nano tube in the CNT conductive paste through a formula, wherein the method is complicated and time-consuming due to the fact that an external balance is used for weighing for multiple times, the precision of the external balance is 0.0001g, and the calculation result of the weight loss rate is interfered due to the fact that the external balance is contacted with air for multiple times, so that the calculation result of the content of the carbon nano tube in the final carbon nano tube conductive paste is influenced.
Therefore, how to improve the accuracy of the carbon nanotube content test in the carbon nanotube conductive paste is a technical problem to be solved.
Disclosure of Invention
The invention aims to provide a method for testing the content of carbon nanotubes in carbon nanotube conductive paste. According to the invention, the interference of the sample contacting with air moisture can be eliminated by a thermogravimetric analysis method, and the dispersing agent weight loss rate is obtained more accurately and intuitively by using a thermogravimetric curve, so that the accuracy of a test result is improved.
In order to achieve the aim of the invention, the invention adopts the following technical scheme:
the invention provides a method for testing the content of carbon nanotubes in carbon nanotube conductive paste, which comprises the following steps:
(1) Testing the solid content of the conductive paste of the carbon nano tube to be tested to obtain the solid content of the conductive paste of the carbon nano tube to be tested and a drying product of the carbon nano tube to be tested;
(2) Taking a dispersant with the same type as the dispersant in the carbon nanotube conductive paste to be tested, and performing thermogravimetric analysis and test to obtain the weight loss rate A of the dispersant 1 ；
(3) Performing thermogravimetric analysis test on the dried product of the carbon nanotube to be detected in the step (1) to obtain the weight loss rate A of the dried product of the carbon nanotube to be detected 2 ；
(4) The weight loss rate A of the dispersant is obtained by the solid content of the carbon nano tube conductive paste to be measured 1 And the weight loss rate A of the carbon nano tube drying product to be measured 2 And calculating to obtain the carbon nanotube content in the carbon nanotube conductive paste to be measured.
In the thermal weight test and analysis process of the carbon nanotube conductive paste, the carbon nanotubes are not weightless, and the dispersing agent is remarkably weightless.
According to the invention, the thermogravimetric analysis test method is adopted, the interference of the sample contacting with air moisture can be eliminated, the calculation of the dispersing agent weight loss rate can be directly obtained through an instrument, the possible error of manual calculation is avoided, the dispersing agent weight loss rate is more accurately and intuitively obtained, the accuracy of a test result is further improved, and the operation is simple.
Preferably, the method for testing the solid content of the carbon nanotube conductive paste to be tested in the step (1) includes:
(I) Before placing the carbon nanotube conductive paste to be tested on the current collector, obtaining the weight m of the current collector 1 ；
(II) placing the carbon nanotube conductive paste to be tested on the surface of a current collector to obtain the weight m of the current collector with the carbon nanotube conductive paste to be tested 2 ；
(III) drying the current collector with the carbon nanotube conductive paste to be tested to obtain the weight m of the dried current collector 3 ；
(IV) by weight of current collector m 1 Weight m of current collector with carbon nanotube conductive paste to be tested 2 And weight m of dried current collector 3 And (3) calculating to obtain the solid content of the carbon nanotube conductive paste to be detected in the step (1).
Preferably, the calculation formula of the calculation in the step (IV) is solid content= (m) 3 -m 1 )/(m 2 -m 1 )*100％。
Preferably, the temperature of the drying in step (III) is 100 to 150 ℃, such as 100 ℃, 110 ℃, 120 ℃,130 ℃, 140 ℃, or 150 ℃, etc., and the time is 2 to 6 hours, such as 2 hours, 3 hours, 4 hours, 5 hours, or 6 hours, etc.
Preferably, the method of thermogravimetric analysis test of step (2) comprises:
placing a dispersing agent with the same type as the dispersing agent in the carbon nanotube conductive paste to be detected on a thermogravimetric analyzer, heating up under a protective atmosphere, testing a thermogravimetric curve, and obtaining the weight loss rate A of the dispersing agent according to the thermogravimetric curve 1 。
Preferably, in the thermogravimetric analysis test according to the step (2), the temperature after the temperature increase is 600 to 800 ℃, for example 600 ℃, 650 ℃, 700 ℃, 750 ℃, 800 ℃, or the like.
In the invention, when the temperature is raised to 600-800 ℃, the thermogravimetric curve of the dispersing agent tends to be gentle, namely the reaction is finished, and the residual components of the dispersing agent reach constant weight.
Preferably, in the thermogravimetric analysis test according to the step (2), the temperature before the temperature rise is 25 to 30 ℃, for example, 25 ℃, 26 ℃, 27 ℃, 28 ℃, 29 ℃, 30 ℃ or the like.
Preferably, the thermogravimetric analysis test of step (2) has a temperature rise rate of 5-15 ℃/min, such as 5 ℃/min, 6 ℃/min, 7 ℃/min, 8 ℃/min, 9 ℃/min, 10 ℃/min, 11 ℃/min, 12 ℃/min, 13 ℃/min, 14 ℃/min or 15 ℃/min, etc.
In the thermal gravimetric analysis testing process, the temperature rising speed is too high, so that the weight loss curve is offset towards the high temperature direction, and the weight loss rate calculation result is affected.
Preferably, the thermogravimetric analysis test of step (2) the protective atmosphere comprises any one or a combination of at least two of a nitrogen atmosphere, an argon atmosphere or a helium atmosphere.
Preferably, the method of thermogravimetric analysis test of step (3) comprises:
placing the dried product of the carbon nano tube to be tested in the step (1) on a thermogravimetric analyzer, heating up under protective atmosphere, testing a thermogravimetric curve, and obtaining the weight loss rate A of the dispersing agent according to the thermogravimetric curve 1 。
Preferably, in the thermogravimetric analysis test in the step (3), the temperature after the temperature increase is 600 to 800 ℃, for example 600 ℃, 650 ℃, 700 ℃, 750 ℃, 800 ℃, or the like.
Preferably, in the thermogravimetric analysis test according to the step (3), the temperature before the temperature rise is 25 to 30 ℃, for example, 25 ℃, 26 ℃, 27 ℃, 28 ℃, 29 ℃, 30 ℃ or the like.
Preferably, the thermogravimetric analysis test of step (3) has a temperature rise rate of 5-15 ℃/min, such as 5 ℃/min, 6 ℃/min, 7 ℃/min, 8 ℃/min, 9 ℃/min, 10 ℃/min, 11 ℃/min, 12 ℃/min, 13 ℃/min, 14 ℃/min or 15 ℃/min, etc.
Preferably, the thermogravimetric analysis test of step (3) the protective atmosphere comprises any one or a combination of at least two of a nitrogen atmosphere, an argon atmosphere or a helium atmosphere.
Preferably, the calculation formula of the calculation in the step (4) is that
As a preferred technical scheme, the method for testing the carbon nanotube content in the carbon nanotube conductive paste comprises the following steps:
(1) Testing the solid content of the conductive paste of the carbon nano tube to be tested to obtain the solid content of the conductive paste of the carbon nano tube to be tested and a drying product of the carbon nano tube to be tested;
(I) Before placing the carbon nanotube conductive paste to be tested on the current collector, obtaining the weight m of the current collector 1 ；
(II) placing the carbon nanotube conductive paste to be tested on the surface of a current collector to obtain the weight m of the current collector with the carbon nanotube conductive paste to be tested 2 ；
(III) drying the current collector with the carbon nanotube conductive paste to be tested at 100-150 ℃ for 2-6 h to obtain the weight m of the dried current collector 3 ；
(IV) as a solid content= (m 3 -m 1 )/(m 2 -m 1 ) Calculating by using a calculation formula of 100% to obtain the solid content of the carbon nanotube conductive paste to be measured in the step (1);
(2) Placing a dispersant with the same type as the dispersant in the carbon nanotube conductive paste to be tested on a thermogravimetric analyzer, heating from 25-30 ℃ to 600-800 ℃ at a heating rate of 5-15 ℃/min under a protective atmosphere, testing a thermogravimetric curve, and obtaining a weight loss rate A of the dispersant according to the thermogravimetric curve 1 ；
(3) Placing the dried product of the carbon nano tube to be detected in the step (1) on a thermogravimetric analyzer, heating from 25-30 ℃ to 600-800 ℃ at a heating rate of 5-15 ℃/min under a protective atmosphere, testing a thermogravimetric curve, and obtaining the weight loss rate A of the dried product of the carbon nano tube to be detected according to the thermogravimetric curve 2 ；
(4) To be used forAnd (3) calculating the calculation formula to obtain the carbon nanotube content in the carbon nanotube conductive paste to be measured.
Compared with the prior art, the invention has the following beneficial effects:
according to the invention, the interference of the sample contacting with air moisture can be eliminated by a thermogravimetric analysis method, the dispersing agent weight loss rate is obtained more accurately and intuitively by using a thermogravimetric curve, the accuracy of a test result is further improved, and the operation is simple.
Drawings
FIG. 1 is a thermogram of the dispersant of example 1.
FIG. 2 is a graph showing the thermogravimetric profile of the dried product of carbon nanotubes to be tested in example 1.
Detailed Description
The technical scheme of the invention is further described by the following specific embodiments. It will be apparent to those skilled in the art that the examples are merely to aid in understanding the invention and are not to be construed as a specific limitation thereof.
Example 1
The embodiment provides a method for testing the content of carbon nanotubes in carbon nanotube conductive paste, which comprises the following steps:
(1) And testing the solid content of the carbon nanotube conductive paste to be tested:
(I) A piece of 10cm x 10cm aluminum foil is taken, and an analytical balance is used for weighing the aluminum foil with the weight of m 1 ；
(II) after uniformly stirring the carbon nanotube conductive paste to be measured, 4g of the paste is placed on an aluminum foil, and the paste is weighed on an analytical balance and recorded to have a mass of m 2 ；
(III) placing the aluminum foil with the slurry in an oven, baking at 130 ℃ for 4 hours, and rapidly weighing and recording the mass m 3 ；
(IV) as a solid content= (m 3 -m 1 )/(m 2 -m 1 ) Calculating 100% of calculation formula to obtain the solid content of the carbon nanotube conductive paste to be tested, testing 3 groups in parallel, and taking an average value;
(2) Placing 10mg of dispersing agent in 70 mu L of alumina crucible, placing the alumina crucible in a thermogravimetric analyzer, introducing 50ml/min of argon, heating the temperature from 30 ℃ to 800 ℃ at a heating rate of 10 ℃/min, testing to obtain a thermogravimetric curve shown in figure 1, and calculating the weight loss rate of the dispersing agent A by taking the second step of the curve after the completion 1 ；
(3) Grinding the dried product of the carbon nano tube to be detected in the step (1) into powder, taking 10mg, and obtaining a thermogravimetric graph shown in the figure 2 in the same thermogravimetric analysis process as the step (2) to obtain the weight loss rate A of the dried product of the carbon nano tube to be detected 2 ；
(4) To be used forAnd (3) calculating the calculation formula to obtain the carbon nanotube content in the carbon nanotube conductive paste to be measured.
Example 2
The embodiment provides a method for testing the content of carbon nanotubes in carbon nanotube conductive paste, which comprises the following steps:
(1) And testing the solid content of the carbon nanotube conductive paste to be tested:
(I) A piece of 10cm x 10cm aluminum foil is taken, and an analytical balance is used for weighing the aluminum foil with the weight of m 1 ；
(II) after uniformly stirring the carbon nanotube conductive paste to be measured, 5g of the paste is placed on an aluminum foil, and the paste is weighed on an analytical balance and recorded to have a mass of m 2 ；
(III) placing the aluminum foil with the slurry in an oven, baking at 100 ℃ for 6 hours, quickly weighing and recording the mass m 3 ；
(IV) as a solid content= (m 3 -m 1 )/(m 2 -m 1) *100% of the calculation formula is used for calculating to obtain the solid content of the carbon nanotube conductive paste to be measured, 3 groups are tested in parallel, and an average value is obtained;
(2) Placing 10mg of dispersing agent in a 70 mu L alumina crucible, placing the alumina crucible in a thermogravimetric analyzer, introducing 50ml/min argon, heating the temperature from 30 ℃ to 600 ℃ at a heating rate of 5 ℃/min, testing to obtain a thermogravimetric curve, and taking a second step of the curve after the completion to calculate the weight loss rate of the dispersing agent to be A 1 ；
(3) Grinding the dried product of the carbon nano tube to be detected in the step (1) into powder, taking 10mg, and obtaining the weight loss rate A of the dried product of the carbon nano tube to be detected in the same thermogravimetric analysis process as in the step (2) 2 ；
(4) To be used forAnd (3) calculating the calculation formula to obtain the carbon nanotube content in the carbon nanotube conductive paste to be measured.
Example 3
The embodiment provides a method for testing the content of carbon nanotubes in carbon nanotube conductive paste, which comprises the following steps:
(1) And testing the solid content of the carbon nanotube conductive paste to be tested:
(I) A piece of 10cm x 10cm aluminum foil is taken, and an analytical balance is used for weighing the aluminum foil with the weight of m 1 ；
(II) after uniformly stirring the carbon nanotube conductive paste to be measured, taking 3g of the paste, placing the paste on an aluminum foil, weighing the paste on an analytical balance, and recording the mass of the paste as m 2 ；
(III) placing the aluminum foil with the slurry in an oven, baking at 150 ℃ for 2 hours, quickly weighing and recording the mass m 3 ；
(IV) as a solid content= (m 3 -m 1 )/(m 2 -m 1) *100% of the calculation formula is used for calculating to obtain the solid content of the carbon nanotube conductive paste to be measured, 3 groups are tested in parallel, and an average value is obtained;
(2) Placing 10mg of dispersing agent in a 70 mu L alumina crucible, placing the alumina crucible in a thermogravimetric analyzer, introducing 50ml/min argon, heating the temperature from 30 ℃ to 700 ℃ at a heating rate of 15 ℃/min, testing to obtain a thermogravimetric curve, and taking a second step of the curve after the completion to calculate the weight loss rate of the dispersing agent to be A 1 ；
(3) Grinding the dried product of the carbon nano tube to be detected in the step (1) into powder, taking 10mg, and obtaining the weight loss rate A of the dried product of the carbon nano tube to be detected in the same thermogravimetric analysis process as in the step (2) 2 ；
(4) To be used forAnd (3) calculating the calculation formula to obtain the carbon nanotube content in the carbon nanotube conductive paste to be measured.
Example 4
The difference between this embodiment and embodiment 1 is that the same conductive paste of carbon nanotubes to be measured is selected, and in step (2), the heating rate is 20 ℃/min.
The remaining test methods and parameters were consistent with example 1.
Specific values and calculation results of the respective parameters in examples 1 to 4 are shown in Table 1.
TABLE 1
As can be seen from the data in examples 1 and 4, the temperature rise rate is too high during the thermogravimetric test, which results in a smaller measured weightlessness and a deviation in the carbon nanotube content test results.
In summary, the method of the invention can eliminate the interference of the sample contacting with the air moisture by the thermogravimetric analysis, and can obtain the weight loss rate of the dispersing agent more accurately and intuitively by using the thermogravimetric curve, thereby improving the accuracy of the test result and having simple operation.
The applicant declares that the above is only a specific embodiment of the present invention, but the scope of the present invention is not limited thereto, and it should be apparent to those skilled in the art that any changes or substitutions that are easily conceivable within the technical scope of the present invention disclosed by the present invention fall within the scope of the present invention and the disclosure.
Claims (15)
1. A method for testing the content of carbon nanotubes in a carbon nanotube conductive paste, the method comprising the steps of:
(1) Testing the solid content of the conductive paste of the carbon nano tube to be tested to obtain the solid content of the conductive paste of the carbon nano tube to be tested and a drying product of the carbon nano tube to be tested;
(2) Taking a dispersant with the same type as the dispersant in the carbon nanotube conductive paste to be tested, and performing thermogravimetric analysis and test to obtain the weight loss rate A of the dispersant 1 ；
(3) Performing thermogravimetric analysis test on the dried product of the carbon nanotube to be detected in the step (1) to obtain the weight loss rate A of the dried product of the carbon nanotube to be detected 2 ；
(4) By treating the testSolid content of carbon nanotube conductive paste and weight loss ratio A of dispersant 1 And the weight loss rate A of the carbon nano tube drying product to be measured 2 Calculating to obtain the content of the carbon nano tube in the carbon nano tube conductive paste to be measured; the calculation formula of the calculation in the step (4) is
2. The method for testing the carbon nanotube content in the carbon nanotube conductive paste according to claim 1, wherein the method for testing the solid content of the carbon nanotube conductive paste to be tested in step (1) comprises:
(I) Before placing the carbon nanotube conductive paste to be tested on the current collector, obtaining the weight m of the current collector 1 ；
(II) placing the carbon nanotube conductive paste to be tested on the surface of a current collector to obtain the weight m of the current collector with the carbon nanotube conductive paste to be tested 2 ；
(III) drying the current collector with the carbon nanotube conductive paste to be tested to obtain the weight m of the dried current collector 3 ；
(IV) by weight of current collector m 1 Weight m of current collector with carbon nanotube conductive paste to be tested 2 And weight m of dried current collector 3 And (3) calculating to obtain the solid content of the carbon nanotube conductive paste to be detected in the step (1).
3. The method for testing the carbon nanotube content in the carbon nanotube conductive paste according to claim 2, wherein the calculated calculation formula in the step (IV) is solid content= (m) 3 -m 1 )/(m 2 -m 1 )*100％。
4. The method for testing the carbon nanotube content in the carbon nanotube conductive paste according to claim 2, wherein the temperature of the drying in the step (III) is 100 to 150 ℃ for 2 to 6 hours.
5. The method for testing the carbon nanotube content in the carbon nanotube conductive paste according to claim 1, wherein the method for thermogravimetric analysis testing in step (2) comprises:
placing a dispersing agent with the same type as the dispersing agent in the carbon nanotube conductive paste to be detected on a thermogravimetric analyzer, heating up under a protective atmosphere, testing a thermogravimetric curve, and obtaining the weight loss rate A of the dispersing agent according to the thermogravimetric curve 1 。
6. The method according to claim 5, wherein in the thermogravimetric analysis test in step (2), the temperature after the temperature rise is 600 to 800 ℃.
7. The method according to claim 5, wherein in the thermogravimetric analysis test in step (2), the temperature before the temperature rise is 25 to 30 ℃.
8. The method for testing the carbon nanotube content in a carbon nanotube conductive paste according to claim 5, wherein the thermogravimetric analysis test in step (2) is performed at a temperature rise rate of 5-15 ℃/min.
9. The method of claim 5, wherein the thermogravimetric analysis test in step (2) is performed in a protective atmosphere comprising any one or a combination of at least two of a nitrogen atmosphere, an argon atmosphere, and a helium atmosphere.
10. The method for testing the carbon nanotube content in the carbon nanotube conductive paste according to claim 1, wherein the method for thermogravimetric analysis testing in step (3) comprises:
placing the dried product of the carbon nano tube to be detected in the step (1) on a thermogravimetric analyzer, and heating in a protective atmosphereTesting a thermal weight curve, and obtaining the weight loss rate A of the carbon nanotube drying product to be tested according to the thermal weight curve 2 。
11. The method according to claim 10, wherein in the thermogravimetric analysis test in step (3), the temperature after the temperature rise is 600 to 800 ℃.
12. The method according to claim 10, wherein in the thermogravimetric analysis test in step (3), the temperature before the temperature rise is 25 to 30 ℃.
13. The method for testing the carbon nanotube content in the carbon nanotube conductive paste according to claim 10, wherein the thermogravimetric analysis test in the step (3) is performed at a temperature rise rate of 5-15 ℃/min.
14. The method of claim 10, wherein the thermogravimetric analysis test in step (3) is performed in a protective atmosphere comprising any one or a combination of at least two of a nitrogen atmosphere, an argon atmosphere, and a helium atmosphere.
15. The method for testing the carbon nanotube content in the carbon nanotube conductive paste according to claim 1, wherein the method for testing comprises the steps of:
(1) Testing the solid content of the conductive paste of the carbon nano tube to be tested to obtain the solid content of the conductive paste of the carbon nano tube to be tested and a drying product of the carbon nano tube to be tested;
(I) Before placing the carbon nanotube conductive paste to be tested on the current collector, obtaining the weight m of the current collector 1 ；
(II) placing the carbon nanotube conductive paste to be tested on the surface of a current collector to obtain the weight m of the current collector with the carbon nanotube conductive paste to be tested 2 ；
(III) drying the current collector with the carbon nanotube conductive paste to be tested at 100-150 ℃ for 2-6 h to obtain the weight m of the dried current collector 3 ；
(IV) as a solid content= (m 3 -m 1 )/(m 2 -m 1 ) Calculating by using a calculation formula of 100% to obtain the solid content of the carbon nanotube conductive paste to be measured in the step (1);
(2) Placing a dispersant with the same type as the dispersant in the carbon nanotube conductive paste to be tested on a thermogravimetric analyzer, heating from 25-30 ℃ to 600-800 ℃ at a heating rate of 5-15 ℃/min under a protective atmosphere, testing a thermogravimetric curve, and obtaining a weight loss rate A of the dispersant according to the thermogravimetric curve 1 ；
(3) Placing the dried product of the carbon nano tube to be detected in the step (1) on a thermogravimetric analyzer, heating from 25-30 ℃ to 600-800 ℃ at a heating rate of 5-15 ℃/min under a protective atmosphere, testing a thermogravimetric curve, and obtaining the weight loss rate A of the dried product of the carbon nano tube to be detected according to the thermogravimetric curve 2 ；
And (3) calculating the calculation formula to obtain the carbon nanotube content in the carbon nanotube conductive paste to be measured.
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