CN115709987A - Method for dispersing carbon nanotubes by using molten mixed salt - Google Patents
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 123
- 239000002041 carbon nanotube Substances 0.000 title claims abstract description 118
- 229910021393 carbon nanotube Inorganic materials 0.000 title claims abstract description 118
- 238000000034 method Methods 0.000 title claims abstract description 53
- 150000003839 salts Chemical class 0.000 title claims abstract description 37
- 239000006185 dispersion Substances 0.000 claims abstract description 60
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000011833 salt mixture Substances 0.000 claims abstract 2
- 239000011550 stock solution Substances 0.000 claims description 22
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims description 20
- 239000000843 powder Substances 0.000 claims description 15
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 7
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 6
- 238000005303 weighing Methods 0.000 claims description 5
- CECABOMBVQNBEC-UHFFFAOYSA-K aluminium iodide Chemical compound I[Al](I)I CECABOMBVQNBEC-UHFFFAOYSA-K 0.000 claims description 4
- 239000002238 carbon nanotube film Substances 0.000 claims description 4
- 238000002844 melting Methods 0.000 claims description 4
- 230000008018 melting Effects 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 235000011164 potassium chloride Nutrition 0.000 claims description 4
- 239000001103 potassium chloride Substances 0.000 claims description 4
- 239000002109 single walled nanotube Substances 0.000 claims description 3
- 239000002079 double walled nanotube Substances 0.000 claims description 2
- 239000010408 film Substances 0.000 claims description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 2
- 239000002048 multi walled nanotube Substances 0.000 claims description 2
- 239000011780 sodium chloride Substances 0.000 claims description 2
- PUGUQINMNYINPK-UHFFFAOYSA-N tert-butyl 4-(2-chloroacetyl)piperazine-1-carboxylate Chemical compound CC(C)(C)OC(=O)N1CCN(C(=O)CCl)CC1 PUGUQINMNYINPK-UHFFFAOYSA-N 0.000 claims description 2
- 239000002253 acid Substances 0.000 abstract description 6
- 238000005411 Van der Waals force Methods 0.000 abstract description 5
- 230000001590 oxidative effect Effects 0.000 abstract description 3
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 239000007800 oxidant agent Substances 0.000 abstract description 2
- 239000002904 solvent Substances 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- 238000011031 large-scale manufacturing process Methods 0.000 abstract 1
- 238000001914 filtration Methods 0.000 description 15
- 239000007788 liquid Substances 0.000 description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 12
- 239000008367 deionised water Substances 0.000 description 10
- 229910021641 deionized water Inorganic materials 0.000 description 10
- 238000006243 chemical reaction Methods 0.000 description 7
- 238000003756 stirring Methods 0.000 description 6
- 229910052799 carbon Inorganic materials 0.000 description 5
- 238000001816 cooling Methods 0.000 description 5
- 239000012530 fluid Substances 0.000 description 5
- 238000007710 freezing Methods 0.000 description 5
- 230000008014 freezing Effects 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 5
- 239000002244 precipitate Substances 0.000 description 5
- 239000002002 slurry Substances 0.000 description 5
- 239000006228 supernatant Substances 0.000 description 5
- 229910016747 AlCl3—NaCl—KCl Inorganic materials 0.000 description 4
- 238000001237 Raman spectrum Methods 0.000 description 4
- 239000002131 composite material Substances 0.000 description 4
- 230000003993 interaction Effects 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000003930 superacid Substances 0.000 description 3
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- PQLAYKMGZDUDLQ-UHFFFAOYSA-K aluminium bromide Chemical compound Br[Al](Br)Br PQLAYKMGZDUDLQ-UHFFFAOYSA-K 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 229910001416 lithium ion Inorganic materials 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 239000004570 mortar (masonry) Substances 0.000 description 2
- 239000002071 nanotube Substances 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- KEQGZUUPPQEDPF-UHFFFAOYSA-N 1,3-dichloro-5,5-dimethylimidazolidine-2,4-dione Chemical compound CC1(C)N(Cl)C(=O)N(Cl)C1=O KEQGZUUPPQEDPF-UHFFFAOYSA-N 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 150000003841 chloride salts Chemical class 0.000 description 1
- XTHPWXDJESJLNJ-UHFFFAOYSA-N chlorosulfonic acid Substances OS(Cl)(=O)=O XTHPWXDJESJLNJ-UHFFFAOYSA-N 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000002612 dispersion medium Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005338 heat storage Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 230000000877 morphologic effect Effects 0.000 description 1
- 229910021392 nanocarbon Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- HIFJUMGIHIZEPX-UHFFFAOYSA-N sulfuric acid;sulfur trioxide Chemical compound O=S(=O)=O.OS(O)(=O)=O HIFJUMGIHIZEPX-UHFFFAOYSA-N 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
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Abstract
The invention discloses a method for dispersing carbon nanotubes by using molten mixed salt, belonging to the technical field of carbon nanotube dispersion. The invention takes a molten low-melting-point aluminum salt mixture as a dispersing solvent. The aluminum salt adopted by the invention has high charge density, and the empty orbit of the aluminum salt can interact with electrons on the surface of the carbon nano tube, so that strong repulsive force exists between the carbon nano tubes to overcome van der Waals force and further disperse the carbon nano tubes. The carbon nano tube dispersion phase provided by the invention consists of the following substances: the low-melting-point aluminum salt-containing mixed molten salt needs to reach a certain mole fraction. The dispersion method provided by the invention has no obvious damage to the microstructure and the length of the carbon nano tube, and can realize the high length-diameter ratio dispersion of the carbon nano tube. In addition, the dispersion method is different from the traditional strong oxidant and strong acid dispersion methods, has mild dispersion conditions, simple process, environmental friendliness and lower price of molten salt, and is suitable for large-scale production and application.
Description
Technical Field
The invention relates to a method for dispersing carbon nanotubes by using molten mixed salt, belonging to the technical field of nano carbon materials. The method can obtain the dispersion liquid without damaging the microstructure of the carbon nano tube, can also obtain the carbon nano tube film and the carbon nano tube paper with a relatively complete structure, has simple and easy dispersion method, and can be applied to the fields of water system slurry, electric conduction, heat storage, composite materials and the like.
Background
The carbon nano tube has excellent mechanical, electrical, optical and thermal properties due to the special sp2 carbon hybrid structure and certain flexibility, and has important application in the fields of composite materials, lithium ion battery additives and the like. However, in practical application, the high length-diameter ratio of the carbon nanotubes, the action of strong van der waals force between the tubes and the pi-pi stacking interaction cause the nanotubes to be easily aggregated and agglomerated, thereby greatly limiting the full play of the excellent performance of the nanotubes in the application fields of composite materials and lithium ion batteries. Therefore, solving the problem of effectively dispersing the carbon nanotubes with high length-diameter ratio has important significance for large-scale application and market promotion.
The nature of carbon nanotube dispersion is the interaction of the carbon nanotube interface with the solvent. By the action of strong acid or strong oxidant and carbon nanotube, hydroxyl, carboxyl and sulfonic group are introduced to the surface of carbon nanotube, so that carbon nanotube slurry with good dispersion can be obtained under mechanical action, which becomes the mainstream carbon nanotube dispersing method at present. However, in such a dispersion method, the structure of the carbon nanotubes is seriously damaged, which greatly reduces the intrinsic conductive properties and mechanical strength of the carbon nanotubes, and these chemical methods mostly use a large amount of oxidizing acid, which causes serious pollution. Finding a dispersion method of long carbon nanotubes is crucial to fully exerting the excellent properties of carbon nanotubes, and also brings opportunities for developing and preparing new carbon nanotube composite materials.
Based on the abundant pi electrons of carbon nanotubes, researchers have proposed that a superacid such as fuming sulfuric acid or chlorosulfonic acid can form charge transfer at the carbon nanotube interface, thereby forming stable dispersion by repulsion between charged carbon nanotubes. They indicate that the dispersion behavior of single-walled carbon nanotubes in strong acid systems is the result of the competition of van der waals forces with electrostatic forces under the action of strong acids. Although the use of super acids can solve the problem of dispersion of carbon nanotubes well, super acids are expensive in industrial production and also increase the safety of equipment and environmental problems.
The invention selects the high-density charge of low-melting-point aluminum salt with low price in a molten state as a main dispersion medium, and the empty track of the aluminum salt is interacted with the electrons on the surface of the carbon nano tube, so that strong repulsive force exists between the carbon nano tubes, strong van der Waals force is overcome, and high-quality carbon nano tube dispersion liquid, dispersion powder, a carbon nano tube film and carbon nano tube paper with perfect structures are obtained.
Disclosure of Invention
In view of the disadvantages of the current carbon nanotube dispersion process, the present invention is directed to a method for dispersing carbon nanotubes with a low melting point aluminum salt.
The dispersion method of the carbon nano tube is carried out according to the following steps:
(1) Respectively weighing a certain amount of aluminum salt and other salts according to the mass fraction to prepare the low-melting-point mixed molten salt. (2) Adding carbon nano tubes with a certain mass fraction into the mixed molten salt, uniformly mixing, and treating for 1-120 hours under a certain condition to obtain a carbon nano tube dispersion stock solution.
(3) And obtaining the dispersed carbon nano tube powder, film or carbon nano tube paper by washing, drying and the like.
The method for dispersing the carbon nano tube by the low-melting-point aluminum salt is characterized in that the low-melting-point aluminum salt is one of aluminum bromide, aluminum chloride and aluminum iodide with the melting point below 500 ℃.
The method for dispersing the carbon nano tube by the low-melting-point aluminum salt is characterized in that the ternary mixed chloride salt is a mixture of aluminum chloride, sodium chloride and potassium chloride, wherein the mole fraction of the aluminum chloride is more than 50%.
The method for dispersing the carbon nano tube by the low-melting-point aluminum salt is characterized in that the mass fraction of the added carbon nano tube is 0.01-5%.
The method for dispersing the carbon nano tube by the aluminum salt with the low melting point is characterized in that the treatment temperature is 80-150 ℃.
The method for dispersing the carbon nanotubes by the low-melting-point aluminum salt is characterized in that the carbon nanotubes can be divided into single-wall carbon nanotubes, double-wall carbon nanotubes and multi-wall carbon nanotubes from the wall number, and can be divided into clustered carbon nanotubes and arrayed carbon nanotubes from the morphological structure.
The invention has the beneficial effects that: the invention designs a novel carbon nanotube dispersing method by means of high charge density of molten salt in a molten state. The interaction between the electron vacancy provided by the aluminum salt and the pi-rich electron of the carbon nanotube is larger than the van der Waals force of the carbon nanotube, so that the carbon nanotube can be uniformly dispersed in the molten aluminum salt and the mixed molten salt thereof under the condition of keeping the length-diameter ratio of the carbon nanotube unchanged. The dispersion method can not cause damage to the carbon nano tube, can keep the excellent performance of the carbon nano tube, can directly obtain water system carbon nano tube dispersion liquid, carbon nano tube powder, a carbon nano tube film and carbon nano tube paper, and provides good conditions for the application of the carbon nano tube. The method is simple and convenient to operate, does not use super-strong acid strong oxidation reagent and surfactant, and is green and environment-friendly. The molten salt has low cost and is suitable for large-batch industrial production.
Drawings
FIG. 1 is a diagram showing a state of a dispersion liquid obtained by treating a dispersed carbon nanotube with a molten salt according to example 1 of the present invention.
FIG. 2 is a scanning electron microscope image of carbon nanotubes after molten salt dispersion in example 1 of the present invention.
FIG. 3 is a transmission electron microscope image of carbon nanotubes after molten salt dispersion in example 1 of the present invention.
FIG. 4 is a comparative graph of Raman spectra before and after molten salt dispersion of example 1 of the present invention.
Detailed Description
The invention is further illustrated by the following specific examples.
Example 1
The aluminum salt dispersion method of the carbon nanotube, the carbon nanotube dispersion slurry that this method proposes is made up of the following mass ratio of material: 0.01 part of array carbon nano tube and 99.99 parts of AlCl3 molten salt.
The method for dispersing the carbon nanotubes by the aluminum salt is carried out according to the following specific steps:
(1) Weighing 9.999g of AlCl3 with the purity of AR level and 0.001g of array carbon nano tube powder, and uniformly stirring.
(2) And (3) placing the mixture into a reaction kettle, stirring and heating to 220 ℃, and preserving heat for 12 hours to obtain a carbon nano tube dispersion stock solution.
(3) And cooling the dispersion stock solution to room temperature, solidifying the stock solution, dissolving the solidified stock solution by using deionized water, standing, filtering, dispersing in deionized water, repeating the steps of standing, filtering and the like until the pH value of the washing supernatant is 7, filtering, freezing and drying to obtain the carbon nano tube powder.
The optical photograph of the carbon nanotube dispersion obtained by the dispersion method is shown in fig. 1, and it can be seen from the figure that the dispersed phase is a uniform fluid and has no precipitate at the bottom of the bottle.
The dispersion method can effectively disperse the carbon nano tubes, and the scanning electron microscope photo and the transmission electron microscope photo of the dispersed carbon nano tubes are shown in figures 2 and 3, the dispersed carbon nano tubes are not arranged in an array any more, but are loosely staggered and connected, so that the possibility of forming the carbon nano tubes is provided, and the obvious entanglement phenomenon does not exist between the tubes.
The dispersion method has a nondestructive dispersion effect, the Raman spectra of the carbon nanotubes before and after dispersion are shown in FIG. 4, the peak position values of the Raman spectra of the dispersed carbon nanotubes are consistent with those of the Raman spectra of the carbon nanotubes before dispersion, and the D/G ratios are close, which indicates that the microstructure of the carbon nanotubes obtained by the dispersion method is not damaged.
Example 2
The method for dispersing the carbon nano tube by the aluminum salt comprises the following steps of: 0.05 part of arrayed carbon nanotubes and 99.5 parts of AlBr3 molten salt.
The method for dispersing the carbon nano tube by the aluminum salt is carried out according to the following specific steps:
(1) 9.95g of AlBr3 with the purity of AR and 0.05g of array carbon nanotube powder are weighed and stirred uniformly.
(2) And (3) placing the mixture into a reaction kettle, stirring and heating to 150 ℃, and preserving heat for 12 hours to obtain a carbon nano tube dispersion stock solution.
(3) And cooling the dispersion stock solution to room temperature, solidifying the stock solution, dissolving the solidified stock solution by using deionized water, standing, filtering, dispersing in deionized water, repeating the steps of standing, filtering and the like until the pH value of the washing supernatant is 7, filtering, freezing and drying to obtain the carbon nano tube powder.
The carbon nano tube-aluminum bromide fused salt dispersion liquid obtained by the method is a uniform fluid, no precipitate exists at the bottom of a bottle, and the dispersion liquid still has no layering phenomenon after being placed for two weeks.
Example 3
The method for dispersing the carbon nano tube by the aluminum salt comprises the following steps of: 0.1 part of arrayed carbon nanotubes and 99.9 parts of AlI3 molten salt.
The method for dispersing the carbon nanotubes by the aluminum salt is carried out according to the following specific steps:
(1) 9.99g of AlI3 with the purity of AR level and 0.01g of array carbon nanotube powder are weighed and stirred uniformly.
(2) And (3) placing the mixture into a reaction kettle, stirring and heating to 220 ℃, and preserving heat for 24 hours to obtain a carbon nano tube dispersion stock solution.
(3) Cooling the dispersion stock solution to room temperature, solidifying the stock solution, dissolving the solidified stock solution by deionized water, standing, filtering, dispersing in deionized water, repeating the steps of standing, filtering and the like until the pH value of the washing supernatant is 7, filtering, freezing and drying to obtain the carbon nano tube powder.
The carbon nano tube-aluminum iodide fused salt dispersion liquid obtained by the method is uniform fluid, no precipitate exists at the bottom of the bottle, and the dispersion liquid still has no layering phenomenon after being placed for two weeks.
Example 4
The aluminum salt dispersion method of the carbon nanotube, the carbon nanotube dispersion slurry that this method proposes is made up of the following mass ratio of material: 0.3 part of array carbon nano tube and 99.7 parts of AlCl3-NaCl-KCl ternary mixed molten salt.
The method for dispersing the carbon nanotubes by the aluminum salt is carried out according to the following specific steps:
(1) Weighing 9.97g of AlCl3, naCl and KCl ternary mixed salt with the purity of AR grade according to a certain molar ratio, fully mixing, putting into an agate mortar, grinding until the three salts are uniformly mixed, and putting into a reaction kettle for sealing for later use; 0.03g of array carbon nanotube powder is weighed and put into ternary mixed salt to be uniformly stirred.
(2) Stirring and heating the mixture in the reaction kettle to 120 ℃, and preserving the heat for 24 hours to obtain the carbon nano tube dispersion stock solution.
(3) And cooling the dispersion stock solution to room temperature, solidifying the stock solution, dissolving the solidified stock solution by using deionized water, standing, filtering, dispersing in deionized water, repeating the steps of standing, filtering and the like until the pH value of the washing supernatant is 7, filtering, freezing and drying to obtain the carbon nano tube powder.
The carbon nano tube-AlCl 3-NaCl-KCl ternary mixed molten salt dispersion liquid obtained by the method is uniform fluid, no precipitate exists at the bottom of a bottle, and the dispersion liquid still has no layering phenomenon after being placed for two weeks.
Example 5
The aluminum salt dispersion method of the carbon nanotube, the carbon nanotube dispersion slurry that this method proposes is made up of the following mass ratio of material: 0.5 part of array carbon nano tube and 99.5 parts of AlCl3-NaCl-KCl ternary mixed molten salt.
The method for dispersing the carbon nanotubes by the aluminum salt is carried out according to the following specific steps:
(1) Weighing 9.95g of AlCl3, naCl and KCl ternary mixed salt with the purity of AR grade according to a certain molar ratio, fully mixing, putting into an agate mortar, grinding until the three salts are uniformly mixed, and putting into a reaction kettle for sealing for later use; 0.05g of array carbon nanotube powder is weighed and put into ternary mixed salt to be uniformly stirred.
(2) Stirring and heating the mixture in the reaction kettle to 120 ℃, and preserving the heat for 72 hours to obtain the carbon nano tube dispersion stock solution.
(3) And cooling the dispersion stock solution to room temperature, solidifying the stock solution, dissolving the solidified stock solution by using deionized water, standing, filtering, dispersing in deionized water, repeating the steps of standing, filtering and the like until the pH value of the washing supernatant is 7, filtering, freezing and drying to obtain the carbon nano tube powder.
The carbon nano tube-AlCl 3-NaCl-KCl ternary mixed molten salt dispersion liquid obtained by the method is a uniform fluid, no precipitate exists at the bottom of a bottle, and the dispersion liquid still has no layering phenomenon after being placed for two weeks.
Claims (7)
1. A method for dispersing carbon nanotubes by using a melt-mixed salt is characterized by comprising the following steps:
(1) Respectively weighing a certain amount of aluminum salt and other salts according to the mass fraction to prepare low-melting-point mixed molten salt;
(2) Adding carbon nano tubes with a certain mass fraction into the mixed molten salt, uniformly mixing, and treating for 1-120 hours under a certain condition to obtain a carbon nano tube dispersion stock solution;
(3) And obtaining the dispersed carbon nano tube powder, film or carbon nano tube paper by washing, further drying and the like.
2. The method of claim 1, wherein the aluminum salt is one of aluminum bromide, aluminum chloride and aluminum iodide having a melting point of 500 ℃ or lower.
3. The method of claim 1, wherein the molten salt mixture is a mixture of aluminum chloride, sodium chloride and potassium chloride, and the mole fraction of aluminum chloride is greater than 50%.
4. The method of claim 1, wherein the carbon nanotubes are added in an amount of 0.01 to 5% by mass.
5. The method of claim 1, wherein the temperature of the molten salt is 80-150 ℃.
6. The method of claim 1, wherein the carbon nanotubes are divided into a number of walls, and may include any one of single-walled carbon nanotubes, double-walled carbon nanotubes, and multi-walled carbon nanotubes.
7. The method of claim 1, wherein the step of dispersing the carbon nanotubes comprises the steps of: the carbon nano tube can be prepared into dispersed carbon nano tube powder after being dispersed, washed and dried, or the carbon nano tube film and the carbon nano tube paper can be obtained after being dispersed and filtered.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2013048095A1 (en) * | 2011-09-28 | 2013-04-04 | Bioneer Corporation | Nano composite consisting of carbon nanotubes and metal oxide and method for manufacturing the same |
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| CN106517153A (en) * | 2016-11-11 | 2017-03-22 | 燕山大学 | Method for improving dispersity of carbon nano tubes |
| KR20190140275A (en) * | 2018-06-11 | 2019-12-19 | 주식회사 엘지화학 | Carbon nanotube dispersed solution and method for preparing the same |
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- 2022-11-14 CN CN202211417847.0A patent/CN115709987A/en active Pending
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|---|---|---|---|---|
| WO2013048095A1 (en) * | 2011-09-28 | 2013-04-04 | Bioneer Corporation | Nano composite consisting of carbon nanotubes and metal oxide and method for manufacturing the same |
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| CN106517153A (en) * | 2016-11-11 | 2017-03-22 | 燕山大学 | Method for improving dispersity of carbon nano tubes |
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| Title |
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