CN108305789B - Preparation method of polyacrylonitrile/molybdenum disulfide composite material for supercapacitor - Google Patents
Preparation method of polyacrylonitrile/molybdenum disulfide composite material for supercapacitor Download PDFInfo
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- 229920002239 polyacrylonitrile Polymers 0.000 title claims abstract description 45
- 229910052982 molybdenum disulfide Inorganic materials 0.000 title claims abstract description 23
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 title claims abstract description 18
- 239000002131 composite material Substances 0.000 title claims abstract description 14
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000004926 polymethyl methacrylate Substances 0.000 claims abstract description 30
- 229920003229 poly(methyl methacrylate) Polymers 0.000 claims abstract description 29
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910052961 molybdenite Inorganic materials 0.000 claims abstract description 11
- 238000002156 mixing Methods 0.000 claims abstract description 9
- RWVGQQGBQSJDQV-UHFFFAOYSA-M sodium;3-[[4-[(e)-[4-(4-ethoxyanilino)phenyl]-[4-[ethyl-[(3-sulfonatophenyl)methyl]azaniumylidene]-2-methylcyclohexa-2,5-dien-1-ylidene]methyl]-n-ethyl-3-methylanilino]methyl]benzenesulfonate Chemical compound [Na+].C1=CC(OCC)=CC=C1NC1=CC=C(C(=C2C(=CC(C=C2)=[N+](CC)CC=2C=C(C=CC=2)S([O-])(=O)=O)C)C=2C(=CC(=CC=2)N(CC)CC=2C=C(C=CC=2)S([O-])(=O)=O)C)C=C1 RWVGQQGBQSJDQV-UHFFFAOYSA-M 0.000 claims abstract description 8
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 7
- 239000000203 mixture Substances 0.000 claims abstract description 7
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000008367 deionised water Substances 0.000 claims description 27
- 229910021641 deionized water Inorganic materials 0.000 claims description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 27
- 239000000843 powder Substances 0.000 claims description 18
- 239000000243 solution Substances 0.000 claims description 16
- 238000003756 stirring Methods 0.000 claims description 13
- 238000005406 washing Methods 0.000 claims description 11
- 238000001035 drying Methods 0.000 claims description 9
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 9
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 8
- 238000005303 weighing Methods 0.000 claims description 8
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 claims description 6
- 238000009210 therapy by ultrasound Methods 0.000 claims description 6
- 238000003828 vacuum filtration Methods 0.000 claims description 6
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 239000011259 mixed solution Substances 0.000 claims description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 3
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 239000012298 atmosphere Substances 0.000 claims description 3
- 239000007789 gas Substances 0.000 claims description 3
- 239000001257 hydrogen Substances 0.000 claims description 3
- 229910052739 hydrogen Inorganic materials 0.000 claims description 3
- 239000003990 capacitor Substances 0.000 abstract description 10
- 239000003792 electrolyte Substances 0.000 abstract description 8
- 150000002500 ions Chemical class 0.000 abstract description 7
- 239000011148 porous material Substances 0.000 abstract description 7
- 239000011258 core-shell material Substances 0.000 abstract description 4
- 230000009286 beneficial effect Effects 0.000 abstract description 3
- 229910015667 MoO4 Inorganic materials 0.000 abstract description 2
- 238000003763 carbonization Methods 0.000 abstract description 2
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 abstract description 2
- 239000002057 nanoflower Substances 0.000 abstract description 2
- 239000011734 sodium Substances 0.000 abstract description 2
- 238000000034 method Methods 0.000 description 8
- 239000007772 electrode material Substances 0.000 description 5
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000007773 negative electrode material Substances 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 239000007774 positive electrode material Substances 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 229910052723 transition metal Inorganic materials 0.000 description 2
- -1 transition metal sulfide Chemical class 0.000 description 2
- 229910016002 MoS2a Inorganic materials 0.000 description 1
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 1
- 239000002033 PVDF binder Substances 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000006258 conductive agent Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 1
- 238000004080 punching Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/24—Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/48—Conductive polymers
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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
- Y02E60/13—Energy storage using capacitors
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- Microelectronics & Electronic Packaging (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
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Abstract
The invention discloses a preparation method of a polyacrylonitrile/molybdenum disulfide composite material for a super capacitor. Mixing sodium molybdate dihydrate (Na)2MoO4·2H2O), thiourea (CH)4N2S) and a polymethyl methacrylate/polyacrylonitrile (PMMA/PAN) core-shell structure are uniformly mixed, and the mixture is subjected to hydrothermal reaction and high-temperature carbonization to obtain MoS2A/PAN composite. The preparation method disclosed by the invention adopts PMMA as a template to form a PAN hollow spherical structure with uniform large pores, and MoS grows on the surface of PAN2The nanoflower not only facilitates the transport of electrolyte ions, but also has higher specific surface area, and is beneficial to forming a double electric layer. And the whole preparation process is simple and environment-friendly.
Description
Technical Field
The invention relates to the technical field of electrochemistry, in particular to the field of super capacitors, and particularly relates to a preparation method of a polyacrylonitrile/molybdenum disulfide composite material for a super capacitor.
Background
The electrochemical performance of the electrode material of the supercapacitor is generally limited by a plurality of factors, such as specific surface area, pore size distribution, conductivity and the like. First, the larger the specific surface area, the more electrolyte ions are adsorbed, and more energy can be stored. Second, pore size and structure also affect the formation of the electric double layer. Only if the pore size is proper and electrolyte ions are allowed to enter, the surface of the electrode material can be infiltrated to form an electric double layer. And the complex pore channel structure also influences the smoothness of electrolyte ions in the pore channels. The electrochemical performance of the electrode material of the supercapacitor is improved by combining the characteristics of polyacrylonitrile and molybdenum disulfide from the two angles.
Molybdenum disulfide (MoS)2) As a transition metal sulfide, the transition metal sulfide has a graphite-like layered structure and is stable in physicochemical properties. Through long-term scientific research, nano-scale MoS with different shapes is successfully prepared by various methods2And (3) granules.
Disclosure of Invention
The invention provides a preparation method of a polyacrylonitrile/molybdenum disulfide electrode composite material for a super capacitor, aiming at improving the electrochemical performance of a super capacitor electrode material.
The invention provides a preparation method of polyacrylonitrile/molybdenum disulfide composite material for a super capacitor, which comprises the following steps:
A. the preparation method of the core-shell structure of polymethyl methacrylate PMMA/polyacrylonitrile PAN comprises the following steps:
a-1, adding methyl methacrylate MMA and potassium persulfate KPS into deionized water, and stirring for a period of time under the nitrogen atmosphere;
a-2, adding the solution obtained in the step A-1, acrylonitrile AN and potassium persulfate KPS into deionized water, and stirring for a period of time in a nitrogen atmosphere;
a-3, centrifuging the PMMA/PAN solution obtained in the step A-2, washing the PMMA/PAN solution for a plurality of times by using deionized water, and drying the washed PMMA/PAN solution to obtain a PMMA/PAN core-shell structure;
B. mixing the above PMMA/PAN core-shell structure with sodium molybdate dihydrate (Na)2MoO4·2H2O), thiourea (CH)4N2S) mixing, and carrying out hydrothermal reaction to obtain MoS2/PMMA/PAN；
C. High temperature carbonization of MoS from step B2PMMA/PAN, PMMA is removed to obtain MoS2A/PAN composite.
In the technical scheme of the invention, the steps A-1 and A-2 are stirred for 2-4 hours at the temperature of 60-80 ℃ under the nitrogen atmosphere.
In the technical scheme of the invention, the specific method of the step B is as follows:
b-1, weighing sodium molybdate dihydrate and thiourea (the mass ratio is 1:2) powder, adding into deionized water, and uniformly stirring;
b-2, weighing the PMMA/PAN powder in the step A-3, adding deionized water, and ultrasonically stirring; and the mass ratio of the PMMA/PAN powder to the sodium molybdate dihydrate is 1:10-1: 50.
B-3, mixing the solutions in the step B-1 and the step B-2 by ultrasonic wave, and carrying out hydrothermal reaction at the temperature of 120-;
b-4, vacuum filtering, washing with deionized water for several times and drying to obtain MoS2/PMMA/PAN。
In the technical scheme of the invention, the specific method of the step C is as follows: mixing MoS2Heating PMMA/PAN powder at the temperature of 600-2/PAN。
In the technical scheme of the invention, the specific method of the step A is as follows:
a-1, adding 5-10ml of methyl methacrylate MMA and 5-10mg of potassium persulfate KPS into 300ml of 100-one deionized water, and stirring for 3-5 hours at 60-80 ℃ in a nitrogen atmosphere by using a magnetic stirrer;
a-2, taking 100-200ml of the solution obtained in the step A-1, 4-15ml of acrylonitrile AN and 1-10mg of potassium persulfate KPS, adding into 50-200ml of deionized water, and stirring for 2-4 hours at 60-80 ℃ in a nitrogen atmosphere by using a magnetic stirrer;
and A-3, centrifuging the PMMA/PAN solution obtained in the step A-2, washing the solution with deionized water for a plurality of times and drying the washed solution.
In the technical scheme of the invention, the specific method of the step B is as follows:
b-1, weighing sodium molybdate dihydrate and thiourea (the mass ratio is 1:2) powder, adding the powder into deionized water, and stirring for 30 minutes to 1 hour;
b-2, weighing the PMMA/PAN powder in the step A-3, adding deionized water, and carrying out ultrasonic treatment for 1-2 hours; and the mass ratio of the PMMA/PAN powder to the sodium molybdate dihydrate is 1:10-1: 50.
B-3, mixing the solutions in the step B-1 and the step B-2, performing ultrasonic treatment for 1-2 hours, pouring the mixture into a reaction kettle, and performing hydrothermal reaction for 8-24 hours at the temperature of 120-;
b-4, carrying out vacuum filtration on the mixed solution in the step B-3, washing the mixed solution for a plurality of times by using deionized water, and drying to obtain MoS2/PMMA/PAN。
In the technical scheme of the invention, the specific method of the step C is as follows:
c-1. MoS2Heating PMMA/PAN powder at 600-800 ℃ for 30 minutes-2 hours in the atmosphere of hydrogen (5%) and argon (95%) mixed gas;
c-2, respectively washing the powder obtained in the step C-1 with ethanol and deionized water, and performing vacuum filtration to obtain MoS2/PAN。
The second aspect of the invention provides a polyacrylonitrile/molybdenum disulfide composite material for a super capacitor prepared by the method.
A third aspect of the present invention provides a supercapacitor, which structurally comprises: the carbon-based porous electrode comprises a capacitor positive and negative electrode shell, a diaphragm, electrolyte, an elastic sheet, a steel sheet, positive and negative electrode current collectors and positive and negative electrode materials, wherein the positive and negative electrode materials are the carbon-based porous electrode materials.
The polyacrylonitrile/molybdenum disulfide composite material prepared by the invention adopts PMMA as a template to form a PAN hollow spherical structure with uniform large pores, and MoS grows on the surface of the PAN2The nanoflower not only facilitates the transport of electrolyte ions, but also has higher specific surface area, and is beneficial to forming a double electric layer. And the whole preparation process is simple and environment-friendly.
Wherein, the spherical MoS is grown by a hydrothermal method2The preparation method has the advantages of easy control of the preparation process, uniform product particles, environmental friendliness and the like. The PAN hollow pellet prepared by taking the polymethyl methacrylate PMMA as the template has controllable structure and uniform aperture, and is convenient for electrolyte ion transportation. And MoS2The combination is beneficial to improving the transfer efficiency of ions, increasing the effective specific surface area and further improving the overall electrochemical performance of the double electric layer capacitor
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the principles of the invention and not to limit the invention. In the drawings, there is shown in the drawings,
FIG. 1 is one of the flow charts of the preparation of the polyacrylonitrile/molybdenum disulfide composite material of the present invention. In the figure, 1 is PAN, 2 is PMMA, and 3 is MoS2。
Detailed Description
The following describes embodiments of the present invention with reference to the drawings.
Example 1
(1) Adding 5ml of Methyl Methacrylate (MMA) and 5mg of potassium persulfate KPS into 150ml of deionized water, and stirring for 4 hours at 75 ℃ in a nitrogen atmosphere by using a magnetic stirrer;
(2) adding 50ml of the solution obtained in the step (1), 4ml of acrylonitrile AN and 4mg of potassium persulfate KPS into 100ml of deionized water, and stirring for 2 hours at 70 ℃ in a nitrogen atmosphere by using a magnetic stirrer;
(3) and (3) centrifuging the PMMA/PAN solution obtained in the step (2), washing with deionized water for several times and drying.
(4) Weighing 0.3g of sodium molybdate dihydrate and 0.6g of thiourea powder, adding the mixture into 40ml of deionized water, and stirring for 30 minutes;
(5) weighing 30mg of PMMA/PAN powder in the step (3), adding 20ml of deionized water, and carrying out ultrasonic treatment for 1 hour;
(6) mixing the solutions in the step (4) and the step (5) for ultrasonic treatment for 1 hour, pouring the mixture into a reaction kettle, and carrying out hydrothermal reaction for 12 hours at 180 ℃;
(7) carrying out vacuum filtration on the mixed solution in the step (6), washing with deionized water for several times, and drying;
(8) heating the powder in the step (7) at 700 ℃ for 30 minutes under the atmosphere of mixed gas of hydrogen (5%) and argon (95%);
(9) washing the powder obtained in the step (8) with ethanol and deionized water respectively, and performing vacuum filtration to obtain MoS2a/PAN composite;
(10) and (3) mixing the substance obtained in the step (9), polyvinylidene fluoride and carbon black, and dissolving the mixture in N-methyl pyrrolidone to prepare slurry, wherein the mass ratio of the active substance to the adhesive to the conductive agent is 8:1: 1.
(11) And (3) coating the slurry prepared in the step (10) on foamed nickel, and drying for 24 hours in vacuum at the temperature of 80 ℃.
(12) And (3) punching the foamed nickel in the step (11) into a pole piece by using a punch with the diameter of 13 um.
(13) The button type super capacitor is assembled by the sequence of the positive electrode shell, the pole piece, the diaphragm, the pole piece, the elastic piece and the negative electrode shell, and a plurality of drops of electrolyte are added in the assembling process.
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited by the foregoing examples, which are provided to illustrate the principles of the invention, and that various changes and modifications may be made without departing from the spirit and scope of the invention, which is also intended to be covered by the appended claims. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (1)
1. A preparation method of polyacrylonitrile/molybdenum disulfide composite material for a supercapacitor comprises the following steps:
(1) adding 5ml of Methyl Methacrylate (MMA) and 5mg of potassium persulfate KPS into 150ml of deionized water, and stirring for 4 hours at 75 ℃ in a nitrogen atmosphere by using a magnetic stirrer;
(2) adding 50ml of the solution obtained in the step (1), 4ml of acrylonitrile AN and 4mg of potassium persulfate KPS into 100ml of deionized water, and stirring for 2 hours at 70 ℃ in a nitrogen atmosphere by using a magnetic stirrer;
(3) centrifuging the PMMA/PAN solution obtained in the step (2), washing with deionized water for several times and drying;
(4) weighing 0.3g of sodium molybdate dihydrate and 0.6g of thiourea powder, adding the mixture into 40ml of deionized water, and stirring for 30 minutes;
(5) weighing 30mg of PMMA/PAN powder in the step (3), adding 20ml of deionized water, and carrying out ultrasonic treatment for 1 hour;
(6) mixing the solutions in the step (4) and the step (5) for ultrasonic treatment for 1 hour, pouring the mixture into a reaction kettle, and carrying out hydrothermal reaction for 12 hours at 180 ℃;
(7) carrying out vacuum filtration on the mixed solution in the step (6), washing with deionized water for several times, and drying;
(8) heating the powder in the step (7) at 700 ℃ for 30 minutes in a mixed gas atmosphere containing 5% of hydrogen and 95% of argon;
(9) washing the powder obtained in the step (8) with ethanol and deionized water respectively, and performing vacuum filtration to obtain MoS2A/PAN composite.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101219785A (en) * | 2008-01-23 | 2008-07-16 | 上海应用技术学院 | Method for manufacturing carbon nano-hollow sphere with polymethyl methacrylate/polyacrylonitrile nucleocapsid polymer as forerunner body |
| CN106128784A (en) * | 2016-08-26 | 2016-11-16 | 重庆文理学院 | A kind of molybdenum bisuphide/Graphene hollow compound microsphere and preparation method thereof |
| CN106669435A (en) * | 2016-12-31 | 2017-05-17 | 青岛翰兴知识产权运营管理有限公司 | Graphene modified sodium alginate-polyacrylonitrile heterogeneous enhanced type hollow fiber membrane |
| CN107492655A (en) * | 2017-07-07 | 2017-12-19 | 东华大学 | A kind of molybdenum disulfide/carbon composite and its preparation method and application |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101633499B (en) * | 2009-06-25 | 2011-08-17 | 上海理工大学 | PAN-base carbon hollow nanospheres preparation method |
| CN102502582A (en) * | 2011-10-31 | 2012-06-20 | 上海理工大学 | Preparation method of three dimensional ordered macroporous charcoal material |
| CN102992405B (en) * | 2012-12-10 | 2014-08-20 | 江苏大学 | Preparation method for molybdenum disulfide nanometer nuclear shell nano-structure |
| CN104971744B (en) * | 2015-06-02 | 2017-07-11 | 浙江理工大学 | A kind of electrolysis water catalysis material of cobalt sulfide and molybdenum disulfide nano core shell structure |
| CN106571240B (en) * | 2016-11-15 | 2018-06-01 | 江苏大学 | A kind of preparation method and its usage of hollow silica/titanium dioxide microballoon sphere of original position carbon doped layer time structure |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101219785A (en) * | 2008-01-23 | 2008-07-16 | 上海应用技术学院 | Method for manufacturing carbon nano-hollow sphere with polymethyl methacrylate/polyacrylonitrile nucleocapsid polymer as forerunner body |
| CN106128784A (en) * | 2016-08-26 | 2016-11-16 | 重庆文理学院 | A kind of molybdenum bisuphide/Graphene hollow compound microsphere and preparation method thereof |
| CN106669435A (en) * | 2016-12-31 | 2017-05-17 | 青岛翰兴知识产权运营管理有限公司 | Graphene modified sodium alginate-polyacrylonitrile heterogeneous enhanced type hollow fiber membrane |
| CN107492655A (en) * | 2017-07-07 | 2017-12-19 | 东华大学 | A kind of molybdenum disulfide/carbon composite and its preparation method and application |
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