CN110560342A - preparation method of efficient heat-conducting surface-modified graphene film - Google Patents
preparation method of efficient heat-conducting surface-modified graphene film Download PDFInfo
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- CN110560342A CN110560342A CN201910895844.XA CN201910895844A CN110560342A CN 110560342 A CN110560342 A CN 110560342A CN 201910895844 A CN201910895844 A CN 201910895844A CN 110560342 A CN110560342 A CN 110560342A
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- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D1/00—Processes for applying liquids or other fluent materials
- B05D1/18—Processes for applying liquids or other fluent materials performed by dipping
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- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
- B05D3/007—After-treatment
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
- B05D7/24—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials for applying particular liquids or other fluent materials
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
- B05D7/50—Multilayers
- B05D7/52—Two layers
- B05D7/54—No clear coat specified
- B05D7/544—No clear coat specified the first layer is let to dry at least partially before applying the second layer
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
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- B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
- B05D7/50—Multilayers
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- B05D7/54—No clear coat specified
- B05D7/546—No clear coat specified each layer being cured, at least partially, separately
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2217/00—Coatings on glass
- C03C2217/20—Materials for coating a single layer on glass
- C03C2217/29—Mixtures
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2218/00—Methods for coating glass
- C03C2218/10—Deposition methods
- C03C2218/11—Deposition methods from solutions or suspensions
- C03C2218/111—Deposition methods from solutions or suspensions by dipping, immersion
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2218/00—Methods for coating glass
- C03C2218/30—Aspects of methods for coating glass not covered above
- C03C2218/32—After-treatment
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Abstract
the invention provides a preparation method of a high-efficiency heat-conducting surface-modified graphene film, which comprises the steps of coating graphene oxide aqueous dispersion on a substrate, immersing the substrate of the dispersion into a solidification solution, taking out the substrate for drying, repeatedly coating the graphene oxide aqueous dispersion on the substrate, immersing the substrate into the solidification solution, taking out the substrate for drying, repeating the process, finally doping nano metal powder and carbon nano tube powder dispersion on the surface, and obtaining a film 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 rapidly cross-linked and self-assembled, original naturally-accumulated graphene sheets are connected together by utilizing bond energy, and due to the addition of the nanoscale metal powder and the carbon nano tubes on the surface of the graphene oxide film, the upper surface and the lower surface of the graphene film are in heat conduction connection, so that the heat conductivity coefficient in the Z direction is greatly improved, the surface modified graphene oxide film with high-efficiency heat conduction is obtained, and the performance and the thickness of the film can be controlled by 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 high-efficiency heat-conducting surface-modified graphene film.
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.
and the surface of the carbon nano tube is added with a heat conduction network structure which can form a Z direction in two sides of the graphene oxide film, and the metal powder helps the carbon nano tubes to be connected in a better heat conduction manner, so that a more integral heat conduction path is formed, and further 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 high-efficiency heat-conducting surface modified graphene film, so that a group on graphene oxide and a group in a solidification liquid spontaneously form a covalent bond or an ionic bond and a heat-conducting network is formed inside the graphene oxide and the group in the solidification liquid, and then the graphene oxide and the graphene oxide are quickly cross-linked 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 high-efficiency heat-conducting surface-modified graphene film comprises the steps of coating a graphene oxide aqueous dispersion solution on a substrate, immersing the substrate with the dispersion solution into a solidification solution, taking out the substrate and drying to obtain a single-layer self-assembled composite graphene oxide film, coating the dispersion solution on the substrate attached with the composite film, repeatedly immersing, drying and coating, and finally adding nano metal powder and a carbon nano tube dispersion solution on the surface to obtain the multilayer self-assembled high-efficiency heat-conducting surface-modified graphene oxide composite film;
the graphene oxide water or nano-scale metal powder/carbon nano tube dispersion liquid is obtained by mixing all components in distilled 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 dispersion liquid is coated to form a film, the substrate with the 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 dispersion liquid is rapidly cross-linked and self-assembled, graphene sheets which are naturally stacked originally are connected together by using 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 ultrasonic dispersion of graphene oxide water or a mixed dispersion liquid of nano metal powder/carbon nano tubes to uniformly disperse the mixed solution, and prepares a high-efficiency heat-conducting surface-modified graphene oxide film product with excellent performance by further determining the concentration of a surface-modified graphene oxide mixed solution and the concentration of a solidification solution;
3. The efficient heat-conducting surface-modified 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 surface-modified 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: dissolving 200mg of freeze-dried GO powder into 40mL of steamed pomegranate water, and performing ultrasonic dispersion for 1 hour to fully disperse the powder to form 5mg/mL of composite graphene oxide mixed aqueous solution;
Preparing a nano metal powder/carbon nano tube mixed solution: mixing and dissolving 15mg of copper powder and 30mg of carbon nano tubes into 20mL of pomegranate water, and performing ultrasonic dispersion for 1 hour to fully disperse the copper powder and the carbon nano tubes to form 2.25mg/mL of nano metal powder/carbon nano tube mixed water 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 60mm x 30mm x 2mm glass substrate, immersing the glass substrate with the graphene oxide mixed aqueous solution into a coagulating liquid, reacting for 10min, taking out the substrate, drying for 10h at room temperature, coating a layer of surface modified graphene oxide mixed aqueous solution on the substrate, repeating the processes of immersing, drying and coating, and finally coating a nano metal powder/carbon nano tube mixed solution and drying to obtain the high-efficiency heat-conducting surface modified 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: dissolving 200mg of freeze-dried GO powder into 40mL of steamed pomegranate water, and performing ultrasonic dispersion for 1 hour to fully disperse the powder to form 5mg/mL of composite graphene oxide mixed aqueous solution;
preparing a nano metal powder/carbon nano tube mixed solution: mixing and dissolving 15mg of silver powder and 30mg of carbon nano tubes into 20mL of steamed pomegranate water, and performing ultrasonic dispersion for 1 hour to fully disperse the silver powder and the carbon nano tubes to form 2.25mg/mL of nano metal powder/carbon nano tube 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 60mm x 30mm x 2mm glass substrate, immersing the glass substrate with the graphene oxide mixed aqueous solution into a coagulating liquid, reacting for 10min, taking out the substrate, drying for 10h at room temperature, coating a layer of surface modified graphene oxide mixed aqueous solution on the substrate, repeating the processes of immersing, drying and coating, and finally coating a nano metal powder/carbon nano tube mixed solution and drying to obtain the high-efficiency heat-conducting surface modified 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: dissolving 200mg of freeze-dried GO powder into 40mL of steamed pomegranate water, and performing ultrasonic dispersion for 1 hour to fully disperse the powder to form 5mg/mL of composite graphene oxide mixed aqueous solution;
Preparing a nano metal powder/carbon nano tube mixed solution: mixing and dissolving 15mg of tin powder and 30mg of carbon nano tubes into 20mL of steam pomegranate water, and performing ultrasonic dispersion for 1 hour to fully disperse the tin powder and the carbon nano tubes to form 2.25mg/mL of nano metal powder/carbon nano tube mixed water 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 60mm x 30mm x 2mm glass substrate, immersing the glass substrate with the graphene oxide mixed aqueous solution into a coagulating liquid, reacting for 10min, taking out the substrate, drying for 10h at room temperature, coating a layer of surface modified graphene oxide mixed aqueous solution on the substrate, repeating the processes of immersing, drying and coating, and finally coating a nano metal powder/carbon nano tube mixed solution and drying to obtain the high-efficiency heat-conducting surface modified graphene oxide film.
by adopting the formula and the method, the obtained graphene oxide film has excellent heat-conducting property and can be widely applied to actual production.
Claims (10)
1. A preparation method of a high-efficiency heat-conducting surface-modified graphene film is characterized by comprising the following steps: firstly, coating the graphene oxide aqueous dispersion liquid on a substrate, immersing the substrate with the 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 dispersion liquid on the substrate attached with the composite film, repeatedly immersing, drying and coating to obtain a multilayer self-assembled efficient heat-conducting composite graphene oxide composite film, and finally coating the surface with the nano metal powder dispersion liquid; the graphene oxide water or the nano metal powder and the carbon nano tube dispersion liquid are obtained by mixing all components in the pomegranate 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 high-efficiency heat-conducting surface-modified graphene 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 high-efficiency heat-conducting surface-modified graphene 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 high-efficiency heat-conducting surface-modified graphene 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 high-efficiency heat-conducting surface-modified graphene 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 high-efficiency heat-conducting surface-modified graphene 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 high-efficiency heat-conducting surface-modified graphene 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 high-efficiency heat-conducting surface-modified graphene 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 high-efficiency heat-conducting surface-modified graphene film according to claim 1, characterized by comprising the following steps: the drying temperature is 25 ℃.
10. The preparation method of the high-efficiency heat-conducting surface-modified graphene 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 (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113629350A (en) * | 2021-08-06 | 2021-11-09 | 东莞塔菲尔新能源科技有限公司 | Power battery heat-conducting coating diaphragm and preparation method thereof |
| CN117567949A (en) * | 2023-11-16 | 2024-02-20 | 东莞市福顺胶垫制品有限公司 | Double-sided adhesive tape and production process thereof |
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- 2019-09-21 CN CN201910895844.XA patent/CN110560342A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113629350A (en) * | 2021-08-06 | 2021-11-09 | 东莞塔菲尔新能源科技有限公司 | Power battery heat-conducting coating diaphragm and preparation method thereof |
| CN117567949A (en) * | 2023-11-16 | 2024-02-20 | 东莞市福顺胶垫制品有限公司 | Double-sided adhesive tape and production process thereof |
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Application publication date: 20191213 |