CN107768601B - Novel graphene membrane electrode preparation method - Google Patents
Novel graphene membrane electrode preparation method Download PDFInfo
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- CN107768601B CN107768601B CN201710952942.3A CN201710952942A CN107768601B CN 107768601 B CN107768601 B CN 107768601B CN 201710952942 A CN201710952942 A CN 201710952942A CN 107768601 B CN107768601 B CN 107768601B
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 77
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 59
- 239000012528 membrane Substances 0.000 title claims abstract description 58
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 238000000967 suction filtration Methods 0.000 claims abstract description 19
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 18
- 239000010439 graphite Substances 0.000 claims abstract description 18
- 238000003756 stirring Methods 0.000 claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims abstract description 10
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910052748 manganese Inorganic materials 0.000 claims abstract description 10
- 239000011572 manganese Substances 0.000 claims abstract description 10
- 238000002156 mixing Methods 0.000 claims abstract description 10
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 10
- 239000010936 titanium Substances 0.000 claims abstract description 10
- 230000002378 acidificating effect Effects 0.000 claims abstract description 7
- 239000002738 chelating agent Substances 0.000 claims abstract description 7
- 239000006185 dispersion Substances 0.000 claims abstract description 5
- 239000011550 stock solution Substances 0.000 claims description 43
- 238000001035 drying Methods 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 9
- 238000005520 cutting process Methods 0.000 claims description 6
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 6
- 239000002270 dispersing agent Substances 0.000 claims description 6
- 239000000194 fatty acid Substances 0.000 claims description 6
- 229930195729 fatty acid Natural products 0.000 claims description 6
- 150000004665 fatty acids Chemical class 0.000 claims description 6
- 239000000843 powder Substances 0.000 claims description 6
- 238000005086 pumping Methods 0.000 claims description 6
- 229920002545 silicone oil Polymers 0.000 claims description 6
- 239000000243 solution Substances 0.000 claims description 6
- 230000001590 oxidative effect Effects 0.000 claims description 5
- 239000007800 oxidant agent Substances 0.000 claims description 4
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 claims description 3
- LCGVCXIFXLGLHG-UHFFFAOYSA-N cyclopenta-1,3-diene;manganese(2+) Chemical group [Mn+2].C1C=CC=[C-]1.C1C=CC=[C-]1 LCGVCXIFXLGLHG-UHFFFAOYSA-N 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 125000004108 n-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 claims description 3
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 3
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 3
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 3
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 3
- 238000002791 soaking Methods 0.000 claims description 3
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 claims description 3
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 3
- 238000003828 vacuum filtration Methods 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 239000012535 impurity Substances 0.000 abstract description 3
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 239000004519 grease Substances 0.000 abstract description 2
- 239000007788 liquid Substances 0.000 abstract description 2
- 239000010408 film Substances 0.000 description 11
- 238000005516 engineering process Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 230000001413 cellular effect Effects 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 239000007770 graphite material Substances 0.000 description 1
- 238000009396 hybridization Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/04—Processes of manufacture in general
- H01M4/0402—Methods of deposition of the material
-
- 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
- C01B32/182—Graphene
- C01B32/184—Preparation
-
- 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
- C01B32/182—Graphene
- C01B32/194—After-treatment
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
-
- 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
Abstract
The invention discloses a preparation method of a novel graphene membrane electrode, which comprises the following steps of respectively mixing and stirring 8-18 parts by weight of powdered graphite oxide, 1-3 parts by weight of chelating agent, 2-4 parts by weight of titanium source and 2-4 parts by weight of manganese source with 20-30 parts by weight of water with weakly acidic pH value for 10-20 min, and standing for 20-30 min, wherein the preparation method comprises the following beneficial effects: according to the novel graphene membrane electrode preparation method, a large amount of impurities in graphite are oxidized and removed, the graphite oxide dispersion liquid is concentrated, the concentration of the graphite is improved, the attachment degree of graphene on the suction filtration membrane is increased, the loss of the graphene on the suction filtration membrane is reduced, the graphene membrane and the suction filtration membrane are lubricated by high-temperature grease and then separated, and the graphene membrane is not easily damaged.
Description
Technical Field
The invention relates to a preparation method of a graphene membrane electrode, in particular to a preparation method of a novel graphene membrane electrode.
Background
Graphene (a cellular planar thin film formed by carbon atoms in an sp2 hybridization manner, which is a quasi-two-dimensional material with a thickness of only one atomic layer, and is also called monoatomic layer graphite. physicists of manchester university, england, andem, and costing, norwalk, etc., graphene is successfully separated from graphite by using a micro-mechanical stripping method, so that the 2010 norbel prize is obtained together.
In the aspect of energy storage, graphene is also vigorously researched and developed by researchers in recent years. Two-dimensional film materials have also been studied in the industry as one form in which graphene can be functionalized, and nowadays, high conductivity, high strength and excellent toughness exhibited by graphene films that are self-assembled and closely packed layer by layer are also of great interest in the industry.
The graphene film prepared by the existing preparation method of the graphene film has low purity, and when the graphene film is used for manufacturing an electrode in a battery, the power generation efficiency is poor.
Disclosure of Invention
The invention aims to provide a preparation method of a novel graphene membrane electrode and a manufacturing method thereof, so as to solve the problems in the background technology.
The purpose of the invention is realized by the following technical scheme: a preparation method of a novel graphene membrane electrode comprises the following process steps: 1) preparation of stock solution I: respectively taking 8-18 parts by weight of graphite oxide, 1-3 parts by weight of chelating agent, 2-4 parts by weight of titanium source and 2-4 parts by weight of manganese source in powder form, mixing and stirring the powder with 20-30 parts by weight of water with weakly acidic pH value for 10-20 min, standing for 20-30 min, then adding 0.5-1 part by weight of chelating agent, 0.8-1 part by weight of titanium source and 0.8-1 part by weight of manganese source, mixing and stirring the mixture with 10-15 parts by weight of water with weakly acidic pH value for 10-20 min, and standing for 20-30 min to obtain a stock solution I; 2) preparation of stock solution II: mixing the stock solution II with a strong oxidant solution according to a ratio of 4:1, repeatedly stirring for 3 times at 65-70 ℃ to obtain stock solution II, wherein the stirring time is 5-8 min each time, and the interval between the stirring times is 6-10 min; 3) preparation of stock solution III: adding a dispersing agent into the stock solution II obtained in the step 2), stirring for 5-10 min, and then performing ultrasonic dispersion treatment on the stock solution I to obtain a graphite oxide dispersion solution with the mass fraction of 30-50%, namely stock solution III; 4) concentration of stock solution III: drying the stock solution III obtained in the step 3) in a drying chamber at 70-85 ℃ until the mass fraction of water in the stock solution III is below 12%; 5) preparing a graphene film: pouring the concentrated stock solution III obtained in the step 4) onto a pumping membrane of a vacuum filtration device, and carrying out suction filtration on the concentrated stock solution III under the condition of ultrahigh vacuum so as to form a graphene membrane on the pumping membrane; 6) separation of graphene membrane: taking the suction filtration membrane with the graphene membrane in the vacuum device in the step 5), soaking in 70-80 ℃ silicone oil or fatty acid amide for 1-2 h, and then separating the graphene membrane from the suction filtration membrane by a scraper; 7) cleaning and drying of graphene films: washing the graphene film obtained in the step 6) with flowing weak alkaline water with a pH value for 30-40 min, and drying in a drying chamber at 70-85 ℃ for 1-2 h.
The cutting edge of the scraper used in the step 6) is conical, and the width of the cutting edge is 1 mm-1.4 mm.
The dispersing agent in the step 3) is one or two of polyvinylpyrrolidone and polyvinyl alcohol.
The pH value of the weak alkaline water in the step 7) is between 7.35 and 7.45.
The suction filtration membrane with the graphene membrane in the step 6) is completely immersed in the silicone oil or the fatty acid amide.
The titanium source is one or more of titanium tetrachloride or n-butyl titanate.
The manganese source is dicyclopentadienyl manganese.
The invention has the beneficial effects that: according to the novel graphene membrane electrode preparation method, a large amount of impurities in graphite are oxidized and removed, the graphite oxide dispersion liquid is concentrated, the concentration of the graphite is improved, the attachment degree of graphene on the suction filtration membrane is increased, the loss of the graphene on the suction filtration membrane is reduced, the graphene membrane and the suction filtration membrane are lubricated by high-temperature grease and then separated, and the graphene membrane is not easily damaged.
Detailed Description
The following further description is provided in conjunction with the detailed description, but the detailed description below should not be construed as limiting the invention. Various modifications and variations obvious to those skilled in the art, which can be made on the basis of the present invention, should be within the scope of the present invention.
A preparation method of a novel graphene membrane electrode comprises the following process steps: 1) preparation of stock solution I: respectively taking 8-18 parts by weight of graphite oxide, 1-3 parts by weight of chelating agent, 2-4 parts by weight of titanium source and 2-4 parts by weight of manganese source in powder form, mixing and stirring the powder with 20-30 parts by weight of water with weakly acidic pH value for 10-20 min, standing for 20-30 min, then adding 0.5-1 part by weight of chelating agent, 0.8-1 part by weight of titanium source and 0.8-1 part by weight of manganese source, mixing and stirring the mixture with 10-15 parts by weight of water with weakly acidic pH value for 10-20 min, and standing for 20-30 min to obtain a stock solution I; 2) preparation of stock solution II: mixing the stock solution II with a strong oxidant solution according to a ratio of 4:1, repeatedly stirring for 3 times at 65-70 ℃ to obtain stock solution II, stirring for 5-8 min each time with an interval of 6-10 min, and oxidizing a large amount of impurities in the graphite into ions by using the strong oxidant to remove; 3) preparation of stock solution III: adding a dispersing agent into the stock solution II obtained in the step 2), stirring for 5-10 min, and then performing ultrasonic dispersion treatment on the stock solution I to obtain a graphite oxide dispersion solution with the mass fraction of 30-50%, namely stock solution III; 4) concentration of stock solution III: placing the stock solution III obtained in the step 3) in a drying chamber at 70-85 ℃ for drying until the mass fraction of water in the stock solution III is below 12%, concentrating the stock solution III to improve the concentration of graphite in the stock solution III, so that the purity of graphene is improved, the adhesion of graphite on a suction filtration membrane is improved, and the loss of graphite materials is reduced; 5) preparing a graphene film: pouring the concentrated stock solution III obtained in the step 4) onto a pumping membrane of a vacuum filtration device, and carrying out suction filtration on the concentrated stock solution III under the condition of ultrahigh vacuum so as to form a graphene membrane on the pumping membrane; 6) separation of graphene membrane: taking the suction filtration membrane with the graphene membrane in the vacuum device in the step 5), soaking in 70-80 ℃ silicone oil or fatty acid amide for 1-2 h to ensure that the graphene membrane is sufficiently lubricated, and then separating the graphene membrane from the suction filtration membrane by a scraper, so that the integrity of the separated graphene membrane is ensured; 7) cleaning and drying of graphene films: washing the graphene film obtained in the step 6) with flowing weak alkaline water with a pH value for 30-40 min, and drying in a drying chamber at 70-85 ℃ for 1-2 h.
The cutting edge of the scraper used in the step 6) is conical, and the width of the cutting edge is 1 mm-1.4 mm.
The dispersing agent in the step 3) is one or two of polyvinylpyrrolidone and polyvinyl alcohol.
The pH value of the weak alkaline water in the step 7) is between 7.35 and 7.45.
The suction filtration membrane with the graphene membrane in the step 6) is completely immersed in the silicone oil or the fatty acid amide.
The titanium source is one or more of titanium tetrachloride or n-butyl titanate.
The manganese source is dicyclopentadienyl manganese. The above description is only a preferred embodiment of the application and is illustrative of the principles of the technology employed. It will be appreciated by a person skilled in the art that the scope of the invention as referred to in the present application is not limited to the embodiments with a specific combination of the above-mentioned features, but also covers other embodiments with any combination of the above-mentioned features or their equivalents without departing from the inventive concept. For example, the above features may be replaced with (but not limited to) features having similar functions disclosed in the present application.
Claims (6)
1. A preparation method of a graphene membrane electrode is characterized by comprising the following process steps:
1) and preparing a stock solution I: respectively taking 8-18 parts by weight of graphite oxide, 1-3 parts by weight of chelating agent, 2-4 parts by weight of titanium source and 2-4 parts by weight of manganese source in powder form, mixing and stirring the powder with 20-30 parts by weight of water with weakly acidic pH value for 10-20 min, standing for 20-30 min, then adding 0.5-1 part by weight of chelating agent, 0.8-1 part by weight of titanium source and 0.8-1 part by weight of manganese source, mixing and stirring the mixture with 10-15 parts by weight of water with weakly acidic pH value for 10-20 min, and standing for 20-30 min to obtain a stock solution I;
2) and preparing stock solution II: mixing the stock solution I and a strong oxidant solution according to a ratio of 4:1, repeatedly stirring for 3 times at 65-70 ℃ to obtain stock solution II, wherein the stirring time is 5-8 min each time, and the interval between the stirring times is 6-10 min;
3) and preparing stock solution III: adding a dispersing agent into the stock solution II obtained in the step 2), stirring for 5-10 min, and performing ultrasonic dispersion treatment to obtain a graphite oxide dispersion solution with the mass fraction of 30-50%, namely stock solution III;
4) and concentrating the stock solution III: drying the stock solution III obtained in the step 3) in a drying chamber at 70-85 ℃ until the mass fraction of water in the stock solution III is below 12%;
5) and preparing the graphene film: pouring the concentrated stock solution III obtained in the step 4) onto a pumping membrane of a vacuum filtration device, and carrying out suction filtration on the concentrated stock solution III under the condition of ultrahigh vacuum so as to form a graphene membrane on the pumping membrane;
6) and (3) separating the graphene film: taking the suction filtration membrane with the graphene membrane in the vacuum device in the step 5), soaking in 70-80 ℃ silicone oil or fatty acid amide for 1-2 h, and then separating the graphene membrane from the suction filtration membrane by a scraper;
7) cleaning and drying of graphene film: washing the graphene film obtained in the step 6) with flowing weakly alkaline water with a pH value for 30-40 min, and then drying in a drying chamber at 70-85 ℃ for 1-2 h;
the cutting edge of the scraper used in the step 6) is conical, and the width of the cutting edge is 1 mm-1.4 mm.
2. The method for preparing the graphene membrane electrode according to claim 1, wherein: the dispersing agent in the step 3) is one or two of polyvinylpyrrolidone and polyvinyl alcohol.
3. The method for preparing the graphene membrane electrode according to claim 1, wherein: the pH value of the weak alkaline water in the step 7) is between 7.35 and 7.45.
4. The method for preparing the graphene membrane electrode according to claim 1, wherein: the suction filtration membrane with the graphene membrane in the step 6) is completely immersed in the silicone oil or the fatty acid amide.
5. The method for preparing the graphene membrane electrode according to claim 1, wherein: the titanium source is one or more of titanium tetrachloride or n-butyl titanate.
6. The method for preparing the graphene membrane electrode according to claim 1, wherein: the manganese source is dicyclopentadienyl manganese.
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| CN201710952942.3A CN107768601B (en) | 2017-10-13 | 2017-10-13 | Novel graphene membrane electrode preparation method |
| CN202010134666.1A CN111341997B (en) | 2017-10-13 | 2017-10-13 | Preparation method of graphene membrane electrode |
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| CN201710952942.3A CN107768601B (en) | 2017-10-13 | 2017-10-13 | Novel graphene membrane electrode preparation method |
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| CN202010134666.1A Division CN111341997B (en) | 2017-10-13 | 2017-10-13 | Preparation method of graphene membrane electrode |
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| CN107768601A CN107768601A (en) | 2018-03-06 |
| CN107768601B true CN107768601B (en) | 2020-02-21 |
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| CN110911651A (en) * | 2018-09-17 | 2020-03-24 | 湖北虹润高科新材料有限公司 | Silicon/graphene composite negative electrode material for lithium ion battery, self-supporting negative electrode plate and preparation method thereof, and lithium ion battery |
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| CN101591014B (en) * | 2009-06-30 | 2010-12-29 | 湖北大学 | Method for realizing large-scale preparation of monolayer oxidized graphene |
| CN103578771A (en) * | 2012-07-18 | 2014-02-12 | 海洋王照明科技股份有限公司 | Graphene thin film and preparation method and application thereof |
| CN103539108B (en) * | 2013-10-22 | 2016-01-20 | 泰山医学院 | A kind of method preparing graphene oxide |
| CN103708450B (en) * | 2014-01-09 | 2016-04-20 | 重庆大学 | A kind of preparation method of graphene nanobelt paper |
| EP3228592A4 (en) * | 2014-12-02 | 2019-04-03 | Ningbo Zkjh New Material Co. Ltd. | Graphene dispersant and application thereof |
| CN104505491B (en) * | 2014-12-18 | 2016-09-14 | 宁夏共享新能源材料有限公司 | Natural graphite negative electrode material method of modifying and composite |
| CN105293476B (en) * | 2015-11-16 | 2018-07-10 | 复旦大学 | A kind of preparation method of large scale graphene oxide or graphene |
| CN105329884B (en) * | 2015-11-24 | 2017-05-24 | 东南大学 | Method for rapidly peeling and transferring graphene oxide leaching film to substrate |
| CN105752974B (en) * | 2016-04-07 | 2018-06-08 | 张麟德 | The purification process and graphene oxide of graphene oxide |
| CN106395809A (en) * | 2016-11-05 | 2017-02-15 | 上海大学 | Method for preparing oxidized graphene at normal temperature |
| CN107093526B (en) * | 2017-04-14 | 2019-08-02 | 苏州海凌达电子科技有限公司 | With graphite oxide electrode material preparation method and applications as main component |
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| CN107768601A (en) | 2018-03-06 |
| CN111341997A (en) | 2020-06-26 |
| CN111341997B (en) | 2021-05-28 |
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