CN110591660A - Preparation method of efficient heat-conducting composite graphene oxide film - Google Patents
Preparation method of efficient heat-conducting composite graphene oxide film Download PDFInfo
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- CN110591660A CN110591660A CN201910895845.4A CN201910895845A CN110591660A CN 110591660 A CN110591660 A CN 110591660A CN 201910895845 A CN201910895845 A CN 201910895845A CN 110591660 A CN110591660 A CN 110591660A
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- 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
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- 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
- C01B32/198—Graphene oxide
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- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
- C09K5/08—Materials not undergoing a change of physical state when used
- C09K5/14—Solid materials, e.g. powdery or granular
Abstract
The invention provides a preparation method of a composite graphene oxide film with high-efficiency heat conduction, which comprises the steps of coating a mixed dispersion liquid of graphene oxide water/nano-scale metal powder/carbon nano tubes on a substrate, immersing the substrate of the mixed dispersion liquid into a solidification liquid, taking out the substrate for drying, repeatedly coating the mixed dispersion liquid of the graphene oxide water/nano-scale metal powder/carbon nano tubes on the substrate, immersing the substrate into the solidification liquid, taking out the substrate for drying, repeating the process, and obtaining films with corresponding layers as required; the process enables the groups on the graphene oxide and the groups in the solidification liquid to spontaneously form covalent bonds or ionic bonds, the graphene oxide film is quickly cross-linked and self-assembled, original naturally-accumulated graphene sheets are connected together by utilizing bond energy, and due to the addition of the nano-scale metal powder and the carbon nano tubes, the heat conductivity coefficient of the graphene film in the Z direction is greatly improved, so that the composite graphene oxide film with high heat conduction efficiency is obtained, and the performance and the thickness of the film can be controlled through the repeated process. The preparation method of the invention has simple operation and low cost, and the obtained composite film has high mechanical property and can realize mass production.
Description
Technical Field
The invention belongs to the technical field of graphene composite materials, and particularly relates to a preparation method of a composite graphene oxide film with high heat conduction efficiency.
Background
Graphene is a substance composed of carbon atoms which are arranged in a hexagonal mode in a two-dimensional plane monoatomic layer thickness, has excellent performances such as high charge mobility, high mechanical strength and high surface area, and is widely applied to thin-film solar cells, flat display electrodes, capacitors, photovoltaic devices and coating mechanical strength enhancement.
The preparation method of the graphene film is most common in a vapor deposition method and a redox method, and the obtained graphene film has good electrical conductivity, thermal conductivity and mechanical strength; at present, graphene films are relatively widely applied to composite films, such as films formed by compounding high polymer such as graphene oxide and polyvinyl alcohol (PVA) and compounding with ionic liquid, which are main research directions of graphene oxide composite films, but are prepared by blending with the help of good performance of high polymer materials, and the fact that the acting force between graphene layers and interlamination is strengthened by covalent bonds formed by a small amount of small molecules is not considered, and the graphene films are all single-layer graphene composite films formed by compounding, so that the good mechanical properties of the graphene films are not fully utilized.
The addition of the carbon nano tubes can form a Z-direction heat conduction network structure in the multilayer graphene oxide, and the metal powder helps the carbon nano tubes to be connected in a better heat conduction mode to form a more integral heat conduction path, so that the heat conduction coefficient is further improved.
Disclosure of Invention
The technical problem to be solved is as follows: the invention aims to overcome the defects of the prior art and provide a preparation method of a composite graphene oxide film with high heat conduction efficiency, so that groups on graphene oxide and groups in a solidification liquid spontaneously form covalent bonds or ionic bonds and a heat conduction network is formed inside the graphene oxide film, the graphene oxide film is further rapidly crosslinked and self-assembled, and original naturally-accumulated graphene sheets are connected together by utilizing bond energy: the obtained efficient heat-conducting composite graphene oxide film has high mechanical property, and is simple to operate and low in cost.
Technical scheme
A preparation method of a composite graphene oxide film with high heat conduction efficiency comprises the steps of firstly coating a mixed dispersion liquid of graphene oxide water/nanoscale metal powder/carbon nano tubes on a substrate, immersing the substrate with the mixed dispersion liquid into a solidification liquid, then taking out the substrate and drying to obtain a single-layer self-assembled composite graphene oxide film: coating the mixed dispersion liquid on the substrate attached with the composite film, and repeatedly immersing, drying and coating to obtain the multilayer self-assembled efficient heat-conducting composite graphene oxide composite film;
the mixed dispersion liquid of the graphene oxide water/the nano-scale metal powder/the carbon nano tube is obtained by mixing components in steam water through ultrasonic dispersion, and the solute of the solidification liquid is one of ionic liquid, amine or inorganic salt.
Further, the concentration of the graphene oxide water mixed dispersion liquid is 1-15 mg/mL.
Further, the substrate is one of glass, polyethylene terephthalate vinegar, or silicon.
Further, the concentration of the solidification solution is 0.1-20 mg/mL.
Further, the solvent of the coagulating liquid is one of water, alkane, alcohol or halogenated hydrocarbon.
Further, the ionic liquid is one of butyl p-3-methylimidazole (L) lactate, 1, 2-ethylenediamine trifluoromethanesulfonate or 1, 2-ethylenediamine nitrate.
Further, the amine is two of ammonia water, p-phenylenediamine, diphenyldiamine, 1, 2-ethylenediamine, 1, 4-butanediamine, 1, 6-hexanediamine or 1, 8-octanediamine.
Further, the inorganic salt is one of calcium oxide or iron oxide.
Further, the drying temperature is 25 ℃.
Further, the nano-scale metal powder is one of tin powder, copper powder, silver powder and nickel powder.
Has the advantages that:
1. according to the preparation method, the composite graphene oxide mixed dispersion liquid is coated to form a film, the substrate with the composite graphene oxide is immersed in the solidification liquid, a covalent bond or an ionic bond is formed between a group on the graphene oxide and a group in the solidification liquid spontaneously in the process, the graphene oxide mixed dispersion liquid is quickly cross-linked and self-assembled, original naturally-accumulated graphene sheet layers are connected together by utilizing bond energy to obtain a high-performance film, and the performance and the thickness of the film are controllable in the repeated process;
2. the preparation method adopts the mixed dispersion liquid of the ultrasonic dispersion graphene oxide water/nano-scale metal powder/carbon nano-tubes to uniformly disperse the mixed solution, and the high-efficiency heat-conducting composite graphene oxide film product with excellent performance is prepared by further determining the concentration of the composite graphene oxide mixed solution and the concentration of the solidification solution;
3. the efficient heat-conducting composite graphene oxide film disclosed by the invention has high mechanical properties, and is remarkably improved in tensile strength and elastic modulus compared with the existing graphene oxide film.
4. Compared with the existing graphene oxide film, the efficient heat-conducting composite graphene oxide film provided by the invention has the advantage that the heat-conducting effect in the heat-conducting coefficient, particularly in the Z direction, is obviously improved.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, embodiments of the present invention will be described in further detail below.
Example 1
In this example, 1, 8-octanediamine is used as a solute of a coagulating liquid to prepare a composite film, and the preparation process is as follows:
preparing a composite graphene oxide mixed solution: the graphene oxide is prepared by taking graphite as a raw material by adopting a traditional hummers method or an improved hummers method: mixing and dissolving 200mg of freeze-dried GO powder, 15mg of nano tin powder and 30mg of carbon nano tubes into 40mL of steamed pomegranate water, and performing ultrasonic dispersion for 1 hour to fully disperse the mixture to form 6.125mg/mL of composite graphene oxide mixed aqueous solution;
preparing a solidification liquid: dissolving 5mg of 1, 8-octanediamine into 50mL of distilled durum water, and performing ultrasonic dispersion for 10min to fully disperse the mixture to form 0.1mg/mL of solidification solution;
coating the graphene oxide aqueous solution on a substrate, wherein the substrate material is a glass substrate with the thickness of 60mm x 30mm x 2mm, immersing the glass substrate with the composite graphene oxide mixed aqueous solution into a solidification solution, reacting for 10min, taking out the substrate, drying for 10h at room temperature, coating a layer of composite graphene oxide mixed aqueous solution on the substrate, and repeating the processes of immersion, drying and coating to obtain the high-efficiency heat-conducting composite graphene oxide film.
Example 2
In the embodiment, ethanol is used as a solute of a solidification solution to prepare the composite film, and the preparation process is as follows:
preparing a composite graphene oxide mixed solution: the graphene oxide is prepared by taking graphite as a raw material by adopting a traditional hummers method or an improved hummers method: mixing and dissolving 200mg of freeze-dried GO powder, 15mg of nano silver powder and 30mg of carbon nano tubes into 40mL of steamed pomegranate water, and performing ultrasonic dispersion for 1 hour to fully disperse the mixture to form 6.125mg/mL of composite graphene oxide mixed water solution;
preparing a solidification liquid: dissolving 5mg of ethanol in 50mL of distilled water, and performing ultrasonic dispersion for 10min to fully disperse the ethanol to form 0.1mg/mL of coagulating liquid;
coating the graphene oxide aqueous solution on a substrate, wherein the substrate material is a glass substrate with the thickness of 60mm x 30mm x 2mm, immersing the glass substrate with the composite graphene oxide mixed aqueous solution into a solidification solution, reacting for 10min, taking out the substrate, drying for 10h at room temperature, coating a layer of composite graphene oxide mixed aqueous solution on the substrate, and repeating the processes of immersion, drying and coating to obtain the high-efficiency heat-conducting composite graphene oxide film.
Example 3
In this embodiment, the compound film is prepared by using biphenyldiamine as a solidifying solution solute, and the preparation process is as follows:
preparing a composite graphene oxide mixed solution: the graphene oxide is prepared by taking graphite as a raw material by adopting a traditional hummers method or an improved hummers method: mixing and dissolving 200mg of freeze-dried GO powder, 15mg of nano copper powder and 30mg of carbon nano tubes into 40mL of steamed pomegranate water, and performing ultrasonic dispersion for 1 hour to fully disperse the mixture to form 6.125mg/mL of composite graphene oxide mixed aqueous solution;
preparing a solidification liquid: dissolving 5mg of biphenyldiamine in 50mL of distilled durum water, and performing ultrasonic dispersion for 10min to fully disperse the biphenyldiamine to form 0.1mg/mL solidification liquid;
coating the graphene oxide aqueous solution on a substrate, wherein the substrate material is a glass substrate with the thickness of 60mm x 30mm x 2mm, immersing the glass substrate with the composite graphene oxide mixed aqueous solution into a solidification solution, reacting for 10min, taking out the substrate, drying for 10h at room temperature, coating a layer of composite graphene oxide mixed aqueous solution on the substrate, and repeating the processes of immersion, drying and coating to obtain the high-efficiency heat-conducting composite graphene oxide film.
Claims (10)
1. A preparation method of a composite graphene oxide film with high heat conduction efficiency is characterized by comprising the following steps: firstly, coating the mixed dispersion liquid of graphene oxide water/nano-scale metal powder/carbon nano tubes on a substrate, immersing the substrate with the mixed dispersion liquid into a solidification liquid, then taking out the substrate and drying to obtain a single-layer self-assembled composite graphene oxide film: coating the mixed dispersion liquid on the substrate attached with the composite film, and repeatedly immersing, drying and coating to obtain the multilayer self-assembled efficient heat-conducting composite graphene oxide composite film; the mixed dispersion liquid of the graphene oxide water/the nano-scale metal powder/the carbon nano tube is obtained by mixing components in steam water through ultrasonic dispersion, and the solute of the solidification liquid is one of ionic liquid, amine or inorganic salt.
2. The preparation method of the efficient heat-conducting composite graphene oxide film according to claim 1, characterized by comprising the following steps: the concentration of the graphene oxide water mixed dispersion liquid is 1-15 mg/mL.
3. The preparation method of the efficient heat-conducting composite graphene oxide film according to claim 1, characterized by comprising the following steps: the substrate is one of glass, polyethylene terephthalate vinegar or silicon.
4. The preparation method of the efficient heat-conducting composite graphene oxide film according to claim 1, characterized by comprising the following steps: the concentration of the solidification solution is 0.1-20 mg/mL.
5. The preparation method of the efficient heat-conducting composite graphene oxide film according to claim 1, characterized by comprising the following steps: the solvent of the coagulating liquid is one of water, alkane, alcohol or halogenated hydrocarbon.
6. The preparation method of the efficient heat-conducting composite graphene oxide film according to claim 1, characterized by comprising the following steps: the ionic liquid is one of butyl BUTYL 3-methylimidazole (L) lactate, 1, 2-ethanediamine triflate or 1, 2-ethanediamine nitrate.
7. The preparation method of the efficient heat-conducting composite graphene oxide film according to claim 1, characterized by comprising the following steps: the amine is two of ammonia water, p-phenylenediamine, diphenyldiamine, 1, 2-ethylenediamine, 1, 4-butanediamine, 1, 6-hexanediamine or 1, 8-octanediamine.
8. The preparation method of the efficient heat-conducting composite graphene oxide film according to claim 1, characterized by comprising the following steps: the inorganic salt is one of calcium oxide or ferric oxide.
9. The preparation method of the efficient heat-conducting composite graphene oxide film according to claim 1, characterized by comprising the following steps: the drying temperature is 25 ℃.
10. The preparation method of the efficient heat-conducting composite graphene oxide film according to claim 1, characterized by comprising the following steps: the nano-scale metal powder is one of tin powder, copper powder, silver powder and nickel powder.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111962070A (en) * | 2020-09-08 | 2020-11-20 | 中国科学院上海应用物理研究所 | Preparation method of inorganic salt nano-film and inorganic salt nano-film obtained by preparation method |
| CN112376027A (en) * | 2020-11-13 | 2021-02-19 | 无锡华鑫检测技术有限公司 | Preparation method of graphene oxide metal nanosheet composite material |
| CN112938944A (en) * | 2021-04-09 | 2021-06-11 | 常州富烯科技股份有限公司 | Preparation method of graphene film |
-
2019
- 2019-09-21 CN CN201910895845.4A patent/CN110591660A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111962070A (en) * | 2020-09-08 | 2020-11-20 | 中国科学院上海应用物理研究所 | Preparation method of inorganic salt nano-film and inorganic salt nano-film obtained by preparation method |
| CN112376027A (en) * | 2020-11-13 | 2021-02-19 | 无锡华鑫检测技术有限公司 | Preparation method of graphene oxide metal nanosheet composite material |
| CN112938944A (en) * | 2021-04-09 | 2021-06-11 | 常州富烯科技股份有限公司 | Preparation method of graphene film |
| CN112938944B (en) * | 2021-04-09 | 2023-09-12 | 常州富烯科技股份有限公司 | Preparation method of graphene film |
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