CN110950321A - High-specific-surface-area and high-conductivity carbon nanotube material and preparation method thereof - Google Patents
High-specific-surface-area and high-conductivity carbon nanotube material and preparation method thereof Download PDFInfo
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- CN110950321A CN110950321A CN201911302049.1A CN201911302049A CN110950321A CN 110950321 A CN110950321 A CN 110950321A CN 201911302049 A CN201911302049 A CN 201911302049A CN 110950321 A CN110950321 A CN 110950321A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 111
- 239000002041 carbon nanotube Substances 0.000 title claims abstract description 98
- 229910021393 carbon nanotube Inorganic materials 0.000 title claims abstract description 98
- 239000000463 material Substances 0.000 title claims abstract description 57
- 238000002360 preparation method Methods 0.000 title abstract description 17
- 239000011248 coating agent Substances 0.000 claims abstract description 44
- 238000000576 coating method Methods 0.000 claims abstract description 44
- 238000004544 sputter deposition Methods 0.000 claims abstract description 23
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 19
- 239000007789 gas Substances 0.000 claims abstract description 17
- 239000006185 dispersion Substances 0.000 claims abstract description 14
- 239000007788 liquid Substances 0.000 claims abstract description 13
- 239000000758 substrate Substances 0.000 claims abstract description 13
- 239000011261 inert gas Substances 0.000 claims abstract description 10
- 150000001721 carbon Chemical group 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 27
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 claims description 16
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 15
- 239000011889 copper foil Substances 0.000 claims description 15
- 229910052757 nitrogen Inorganic materials 0.000 claims description 14
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 12
- 239000001294 propane Substances 0.000 claims description 8
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 6
- 229910052742 iron Inorganic materials 0.000 claims description 6
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- 229910017052 cobalt Inorganic materials 0.000 claims description 4
- 239000010941 cobalt Substances 0.000 claims description 4
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 4
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 4
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 claims description 4
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 claims description 4
- 229910052759 nickel Inorganic materials 0.000 claims description 3
- 239000000843 powder Substances 0.000 claims description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 2
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 claims description 2
- 229910052786 argon Inorganic materials 0.000 claims description 2
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 claims description 2
- 229910052710 silicon Inorganic materials 0.000 claims description 2
- 239000010703 silicon Substances 0.000 claims description 2
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims 1
- 239000002086 nanomaterial Substances 0.000 abstract description 2
- 239000002002 slurry Substances 0.000 description 11
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 10
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 229920002799 BoPET Polymers 0.000 description 5
- 229910000019 calcium carbonate Inorganic materials 0.000 description 5
- 239000003054 catalyst Substances 0.000 description 5
- 239000003822 epoxy resin Substances 0.000 description 5
- 229920000647 polyepoxide Polymers 0.000 description 5
- 239000000523 sample Substances 0.000 description 5
- 238000001514 detection method Methods 0.000 description 4
- 239000013077 target material Substances 0.000 description 4
- 239000002131 composite material Substances 0.000 description 3
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 238000005234 chemical deposition Methods 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 229910052744 lithium Inorganic materials 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 239000012808 vapor phase Substances 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- -1 doping Chemical compound 0.000 description 1
- 238000010891 electric arc Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000004108 freeze drying Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 239000011232 storage material Substances 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 238000001132 ultrasonic dispersion Methods 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/158—Carbon nanotubes
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/158—Carbon nanotubes
- C01B32/16—Preparation
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2202/00—Structure or properties of carbon nanotubes
- C01B2202/20—Nanotubes characterized by their properties
- C01B2202/22—Electronic properties
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2202/00—Structure or properties of carbon nanotubes
- C01B2202/20—Nanotubes characterized by their properties
- C01B2202/30—Purity
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2202/00—Structure or properties of carbon nanotubes
- C01B2202/20—Nanotubes characterized by their properties
- C01B2202/32—Specific surface area
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2202/00—Structure or properties of carbon nanotubes
- C01B2202/20—Nanotubes characterized by their properties
- C01B2202/36—Diameter
Abstract
A carbon nanotube material with high specific surface area and high conductivity and a preparation method thereof. The invention belongs to the technical field of carbon nano-material preparation. The invention solves the technical problems of low conductivity and small specific surface area of the existing carbon nanotube material. The carbon nanotube material of the present invention is a carbon nanotube material grown with a carbon nanotube as a substrate. The method comprises the following steps: firstly, coating dispersion liquid containing carbon nano tubes on a substrate, and then drying; secondly, carrying out vacuum sputtering coating on the substrate obtained in the first step; and thirdly, introducing inert gas, preserving heat at the temperature of 400-1000 ℃, then introducing mixed gas of carbon atom gas and inert gas at the temperature of 550-1000 ℃, and preserving heat to obtain the high-specific surface area and high-conductivity carbon nanotube material. The carbon nano tube has the purity of more than 98 percent and the specific surface area of up to 100m2/g～500m2G, and there is no need to feed into the prepared carbon nano tubeFurther processing is carried out, the good conductivity is kept, and the resistivity is as low as 32 omega/□.
Description
Technical Field
The invention belongs to the technical field of carbon nano-material preparation, and particularly relates to a high-specific surface area and high-conductivity carbon nano-tube material and a preparation method thereof.
Background
The carbon nanotube is a one-dimensional cylindrical hollow structure, and can also be understood as being formed by curling a graphite sheet structure. The diameter of the carbon nanotube is about several to hundreds of nanometers, the length of the carbon nanotube is generally in the micron order and is several times of the diameter, and therefore the carbon nanotube has a larger length-diameter ratio. From the aspect of preparation, methods for preparing carbon nanotubes include arc discharge, laser evaporation, vapor phase chemical deposition and the like. At present, carbon nanotube manufacturers mainly adopt a vapor phase chemical deposition (CVD) method, that is, a catalyst containing transition metal elements such as iron, cobalt or nickel as active substances is prepared, then the catalyst is placed in a tube furnace, and carbon atom-containing gas is introduced at high temperature, so that carbon nanotube powder can grow on the surface of the catalyst. From the performance, the carbon nano tube has good heat conduction, electric conduction and mechanical strength, and can be used for composite materials, additives and the like, and the strength, the electric conductivity and the like of the materials are enhanced.
The carbon nano tube with high specific surface area and high conductivity has obvious advantages in the using process, for example, the carbon nano tube is used for a lithium battery, can improve the multiplying power, the circulation and other performances of the battery, and can also be used in the fields of composite conductive materials, hydrogen storage materials and the like.
At present, there are two main approaches for preparing carbon nanotubes with high specific surface area and high conductivity by a CVD method, and firstly, the carbon nanotubes with the smallest tube diameter are grown by regulating and controlling the preparation of a catalyst, so that the carbon nanotubes have high specific surface area and good conductivity. Application No. 201910051905.4 discloses a method for preparing carbon nanotubes with high specific surface area, but the carbon nanotubes prepared by the method generally have high impurity content, and the carbon content is generally about 90-95%.
Another method is to treat the prepared carbon nanotubes, including doping, activating, etc. The patent application No. 201710036962.6 discloses a method for preparing porous carbon nanotubes, which further increases the specific surface area of the carbon nanotubes. The patent takes a carbon nano tube as a raw material, and prepares the porous carbon nano tube by solution preparation, ultrasonic dispersion treatment, acid oxidation, freeze drying, vacuum sintering, acid soaking, washing and suction filtration and vacuum drying. But such methods may compromise the good electrical conductivity of the carbon nanotubes.
Disclosure of Invention
The invention solves the technical problems of low conductivity and small specific surface area of the existing carbon nanotube material, and provides a carbon nanotube material with high specific surface area and high conductivity and a preparation method thereof.
The carbon nanotube material with high specific surface area and high conductivity of the invention is a carbon nanotube material grown by taking a carbon nanotube as a substrate, the tube diameter of the carbon nanotube material is 5 nm-200 nm, the specific surface area is 100m2/g～500m2The carbon content is more than 98 percent; the appearance is black powder.
The preparation method of the carbon nanotube material with high specific surface area and high conductivity of the invention is carried out according to the following steps:
firstly, coating the dispersion liquid containing the carbon nano tube on a substrate, wherein the coating thickness is 0.05-0.5 mm, and then drying at the temperature of 100-200 ℃;
secondly, carrying out vacuum sputtering coating on the substrate obtained in the first step, wherein the sputtering coating parameters are as follows: the current is 0.2A-20A, the vacuum degree is 10-4Pa to 10Pa, and vacuum sputtering coating for 10 to 300 seconds after glow starting;
and thirdly, putting the substrate obtained in the second step into a tubular furnace, introducing inert gas, preserving the heat for 5-60 min at the temperature of 400-1000 ℃, then introducing mixed gas of carbon atom gas and inert gas at the temperature of 550-1000 ℃, and preserving the heat for 20-120 min under the condition to obtain the high-specific surface area and high-conductivity carbon nanotube material.
Further limiting, the mass fraction of the carbon nanotubes in the dispersion liquid in the step one is 5-20%.
Further limiting, in the step one, the substrate is a silicon wafer or a copper foil.
Further limited, the coating thickness in the step one is 0.125 mm-0.25 mm.
Further limiting, the film type of the vacuum sputtering coating in the second step is one or a combination of several of iron, cobalt and nickel according to any ratio.
And further limiting, after glow starting, carrying out vacuum sputtering coating for 30-150 s in the step two.
Further limiting, in the third step, the volume ratio of the carbon atom gas to the inert gas in the mixed gas is 1: (0.2-10).
Further, in the third step, the inert gas is nitrogen or argon.
Further defined, the carbon atom gas in step three comprises methane, propane, propylene or acetylene.
The carbon nano tube with high specific surface area and high conductivity is prepared by a special catalyst preparation process, the purity and the specific surface area are both high, the purity can reach more than 98 percent, and the specific surface area can reach 100m2/g～500m2The prepared carbon nano-tube does not need to be further processed, retains good conductivity and has the resistivity as low as 32 omega/□.
In addition, the material can be used as an additive to prepare a composite material, so that the strength, the heat conduction and the electric conductivity of the material are improved, and the material can also be used as an electric conduction agent to be added into a lithium battery, so that the performances of the battery, such as cycle, rate and the like, are improved.
Meanwhile, the preparation method is simple to operate and easy to produce.
Detailed Description
The first embodiment is as follows: in the embodiment, the preparation method of the high-specific-surface-area and high-conductivity carbon nanotube material comprises the following steps:
firstly, coating aqueous dispersion liquid containing carbon nano tubes on a copper foil, wherein the coating thickness is 0.125mm, and then drying at the temperature of 100 ℃; wherein the mass fraction of the carbon nano-tubes in the aqueous dispersion liquid is 5 percent;
secondly, carrying out vacuum sputtering coating on the copper foil obtained in the first step, wherein the sputtering coating parameters are as follows: the current was 0.5A and the vacuum degree was 10-2Pa, the target material is an iron target, and after glow starting, vacuum sputtering coating is carried out for 10 s;
putting the copper foil obtained in the step two into a tube furnace, introducing nitrogen, preserving the heat for 30min at the temperature of 500 ℃, and then introducing a mixed gas of propane and nitrogen at the temperature of 700 ℃, wherein the volume ratio of propane to nitrogen is 1: 0.2, and preserving the heat for 20min under the condition to obtain the carbon nanotube material with high specific surface area and high conductivity.
As a result of examination, the specific surface area of the carbon nanotube material obtained in the present embodiment was 390m2The carbon content is 99.2 percent.
And (3) detection test: 1.5 parts by mass of the carbon nanotube material prepared in the embodiment, 11 parts by mass of calcium carbonate, 37.5 parts by mass of epoxy resin and 5 parts by mass of water are stirred at a rotation speed of 1000rpm for 10 minutes, the viscosity is 3500mPa · S, and then the slurry is ground by a three-roll grinder for 10 minutes, so that slurry containing the carbon nanotube material in the embodiment is obtained.
The resulting slurry containing the carbon nanotube material of the present embodiment was coated on a PET film using a coater to a coating thickness of 200 μm, and then dried, and the film resistivity was measured to be 32 Ω/□ using a four-probe tester.
The second embodiment is as follows: in the embodiment, the preparation method of the high-specific-surface-area and high-conductivity carbon nanotube material comprises the following steps:
firstly, coating aqueous dispersion liquid containing carbon nano tubes on a copper foil, wherein the coating thickness is 0.25mm, and then drying at the temperature of 100 ℃; wherein the mass fraction of the carbon nano-tubes in the aqueous dispersion liquid is 5 percent;
secondly, carrying out vacuum sputtering coating on the copper foil obtained in the first step, wherein the sputtering coating parameters are as follows: current was, vacuum degree was 10- 2Pa, the target material is an iron target, and vacuum sputtering coating is carried out for 150s after glow starting;
putting the copper foil obtained in the step two into a tube furnace, introducing nitrogen, preserving the heat for 30min at the temperature of 500 ℃, and then introducing a mixed gas of propane and nitrogen at the temperature of 700 ℃, wherein the volume ratio of propane to nitrogen is 1: and 5, preserving the heat for 50min under the condition to obtain the carbon nanotube material with high specific surface area and high conductivity.
As a result of the examination, the specific surface area of the carbon nanotube material obtained in the present embodiment was 353m2(ii)/g, carbon content 99.1%。
And (3) detection test: 1.5 parts by mass of the carbon nanotube material prepared in the embodiment, 11 parts by mass of calcium carbonate, 37.5 parts by mass of epoxy resin and 5 parts by mass of water are stirred at a rotation speed of 1000rpm for 10 minutes, and the mixture is ground by a three-roll grinder for 10 minutes to obtain slurry containing the carbon nanotube material in the embodiment.
The resulting slurry containing the carbon nanotube material of the present embodiment was coated on a PET film using a coater to a coating thickness of 200 μm, and then dried, and the film resistivity was measured to be 42 Ω/□ using a four-probe tester.
The third concrete implementation mode: in the embodiment, the preparation method of the high-specific-surface-area and high-conductivity carbon nanotube material comprises the following steps:
firstly, coating N-methylpyrrolidone (NMP) dispersion liquid containing carbon nano tubes on a copper foil, wherein the coating thickness is 0.05mm, and then drying at the temperature of 100 ℃; wherein the mass fraction of the carbon nano-tubes in the N-methylpyrrolidone (NMP) dispersion liquid is 5 percent;
secondly, carrying out vacuum sputtering coating on the copper foil obtained in the first step, wherein the sputtering coating parameters are as follows: current was 10A and vacuum degree was 10-2Pa, the target material is an iron target, and after glow starting, vacuum sputtering coating is carried out for 300 s;
putting the copper foil obtained in the step two into a tube furnace, introducing nitrogen, preserving the heat for 30min at the temperature of 500 ℃, and then introducing a mixed gas of propane and nitrogen at the temperature of 600 ℃, wherein the volume ratio of propylene to nitrogen is 1: 1, and preserving the heat for 20min under the condition to obtain the carbon nanotube material with high specific surface area and high conductivity.
As a result, the specific surface area of the carbon nanotube material obtained in the present embodiment was 270m2The carbon content is 99.4 percent.
And (3) detection test: taking 1.5 parts by mass of the carbon nanotube material prepared in the embodiment, 11 parts by mass of calcium carbonate, 37.5 parts by mass of epoxy resin and 5 parts by mass of water, stirring for 10min at the rotation speed of 1000rpm, wherein the viscosity is 4600mPa & S, and then grinding for 10min by using a three-roll grinder to obtain slurry containing the carbon nanotube material in the embodiment.
The resulting slurry containing the carbon nanotube material of the present embodiment was coated on a PET film using a coater to a coating thickness of 200 μm, and then dried, and the film resistivity was measured to be 37 Ω/□ using a four-probe tester.
The fourth concrete implementation mode: in the embodiment, the preparation method of the high-specific-surface-area and high-conductivity carbon nanotube material comprises the following steps:
firstly, coating N-methylpyrrolidone (NMP) dispersion liquid containing carbon nano tubes on a copper foil, wherein the coating thickness is 0.25mm, and then drying at the temperature of 100 ℃; wherein the mass fraction of the carbon nano-tubes in the N-methylpyrrolidone (NMP) dispersion liquid is 10 percent;
secondly, carrying out vacuum sputtering coating on the copper foil obtained in the first step, wherein the sputtering coating parameters are as follows: current was 5A and vacuum degree was 10-1Pa, the target material is a cobalt target, and after glow starting, vacuum sputtering coating is carried out for 30 s;
putting the copper foil obtained in the step two into a tube furnace, introducing nitrogen, preserving the heat for 30min at the temperature of 500 ℃, and then introducing a mixed gas of propane and nitrogen at the temperature of 600 ℃, wherein the volume ratio of propylene to nitrogen is 1: and 5, preserving the heat for 20min under the condition to obtain the carbon nanotube material with high specific surface area and high conductivity.
It was found that the specific surface area of the carbon nanotube material obtained in the present embodiment was 249m2The carbon content is 99.2 percent.
And (3) detection test: 1.5 parts by mass of the carbon nanotube material prepared in the embodiment, 11 parts by mass of calcium carbonate, 37.5 parts by mass of epoxy resin and 5 parts by mass of water are stirred at a rotation speed of 1000rpm for 10 minutes, and the mixture is ground by a three-roll grinder for 10 minutes to obtain slurry containing the carbon nanotube material in the embodiment.
The resulting slurry containing the carbon nanotube material according to the present embodiment was coated on a PET film using a coater to a coating thickness of 200 μm, and then dried, and the film resistivity was measured to be 39 Ω/□ using a four-probe tester.
And (3) comparison test: mixing water solution containing 5% of carbon nanotubesThe dispersion was coated on a copper foil to a coating thickness of 0.125mm using an automatic coating machine, and then dried at 100 ℃. The specific surface area is 149m2The carbon content is 98.7 percent. The carbon nano tube is a carbon nano tube with the model number of CN19 produced by Harbin gold technology company Limited.
Taking 1.5 parts by mass of carbon nanotubes in a comparative test, 11 parts by mass of calcium carbonate, 37.5 parts by mass of epoxy resin and 5 parts by mass of water, stirring for 10min at the rotation speed of 1000rpm, wherein the viscosity is 2680mPa & S, and then grinding for 10min by using a three-roll grinder to obtain slurry containing the carbon nanotubes in the embodiment.
The obtained slurry containing the carbon nanotubes of the present embodiment was coated on a PET film using a coater to a coating thickness of 200 μm, and then dried, and the film resistivity was measured to be 328 Ω/□ using a four-probe tester.
Claims (10)
1. The carbon nanotube material with high specific surface area and high conductivity is characterized in that the carbon nanotube material with high specific surface area and high conductivity is grown by taking a carbon nanotube as a substrate, the tube diameter of the carbon nanotube material is 5 nm-200 nm, and the specific surface area of the carbon nanotube material is 100m2/g～500m2The carbon content is more than 98 percent; the appearance is black powder.
2. The method for preparing a high specific surface area and high conductivity carbon nanotube material according to claim 1, wherein the method comprises the following steps:
firstly, coating the dispersion liquid containing the carbon nano tube on a substrate, wherein the coating thickness is 0.05-0.5 mm, and then drying at the temperature of 100-200 ℃;
secondly, carrying out vacuum sputtering coating on the substrate obtained in the first step, wherein the sputtering coating parameters are as follows: the current is 0.2A-20A, the vacuum degree is 10-4Pa to 10Pa, and vacuum sputtering coating for 10 to 300 seconds after glow starting;
and thirdly, putting the substrate obtained in the second step into a tubular furnace, introducing inert gas, preserving the heat for 5-60 min at the temperature of 400-1000 ℃, then introducing mixed gas of carbon atom gas and inert gas at the temperature of 550-1000 ℃, and preserving the heat for 20-120 min under the condition to obtain the high-specific surface area and high-conductivity carbon nanotube material.
3. The method for preparing a high specific surface area and high conductivity carbon nanotube material according to claim 2, wherein the mass fraction of carbon nanotubes in the dispersion liquid in the step one is 5% to 20%.
4. The method for preparing a high specific surface area and high conductivity carbon nanotube material of claim 2, wherein in the first step, the substrate is a silicon wafer or a copper foil.
5. The method for preparing a high specific surface area and high conductivity carbon nanotube material of claim 2, wherein the coating thickness in the first step is 0.125mm to 0.25 mm.
6. The method for preparing the carbon nanotube material with high specific surface area and high conductivity according to claim 2, wherein the kind of the film of the vacuum sputtering coating in the second step is one or a combination of iron, cobalt and nickel.
7. The method for preparing the carbon nanotube material with high specific surface area and high conductivity according to claim 2, wherein the sputtering is performed for 30-150 s after the glow is started in the second step.
8. The method for preparing the high-specific-surface-area and high-conductivity carbon nanotube material according to claim 2, wherein the volume ratio of the carbon atom gas to the inert gas in the mixed gas in step three is 1: (0.2-10).
9. The method for preparing a high specific surface area and high conductivity carbon nanotube material of claim 2, wherein the inert gas in step three is nitrogen or argon.
10. The method for preparing a high specific surface area and high conductivity carbon nanotube material of claim 2, wherein the carbon atom gas comprises methane, propane, propylene or acetylene in step three.
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| CN201911302049.1A CN110950321A (en) | 2019-12-17 | 2019-12-17 | High-specific-surface-area and high-conductivity carbon nanotube material and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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