CN112188812A - Preparation method of graphene composite nano-diamond heat dissipation film - Google Patents
Preparation method of graphene composite nano-diamond heat dissipation film Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 82
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- 230000017525 heat dissipation Effects 0.000 title claims abstract description 55
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- USIUVYZYUHIAEV-UHFFFAOYSA-N diphenyl ether Chemical compound C=1C=CC=CC=1OC1=CC=CC=C1 USIUVYZYUHIAEV-UHFFFAOYSA-N 0.000 claims description 4
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- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 2
- 125000000217 alkyl group Chemical group 0.000 claims description 2
- 239000011668 ascorbic acid Substances 0.000 claims description 2
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- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 2
- XQSBLCWFZRTIEO-UHFFFAOYSA-N hexadecan-1-amine;hydrobromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[NH3+] XQSBLCWFZRTIEO-UHFFFAOYSA-N 0.000 claims description 2
- -1 hydrazine hydrate sodium bisulfite Chemical compound 0.000 claims description 2
- 229920002401 polyacrylamide Polymers 0.000 claims description 2
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- 229910052708 sodium Inorganic materials 0.000 claims description 2
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- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 2
- DAJSVUQLFFJUSX-UHFFFAOYSA-M sodium;dodecane-1-sulfonate Chemical compound [Na+].CCCCCCCCCCCCS([O-])(=O)=O DAJSVUQLFFJUSX-UHFFFAOYSA-M 0.000 claims description 2
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K7/00—Constructional details common to different types of electric apparatus
- H05K7/20—Modifications to facilitate cooling, ventilating, or heating
- H05K7/2039—Modifications to facilitate cooling, ventilating, or heating characterised by the heat transfer by conduction from the heat generating element to a dissipating body
Abstract
The invention belongs to the technical field of materials, and particularly relates to a preparation method of a graphene composite nano-diamond heat dissipation film, which comprises the following steps: s1, preparing graphene composite nano-diamond slurry; s2, coating the graphene composite nano-diamond slurry obtained in the step S1 on a release film; s3, drying the release film coated in the step S2, and stripping to obtain a stripping film; and S4, carrying out carbonization and deoxidation treatment and graphitization treatment on the stripping film obtained in the step S3 to obtain the graphene composite nano diamond heat dissipation film. On one hand, the thickness of the graphene composite nano diamond heat dissipation film is adjustable, and the longitudinal heat conductivity of the graphene composite nano diamond heat dissipation film is improved. On the other hand, the preparation method is simple and feasible, can not generate a large amount of tar, has simple and stable treatment process and higher repeatability, and has great significance for environmental protection.
Description
Technical Field
The invention belongs to the technical field of materials, and particularly relates to a preparation method of a graphene composite nano-diamond heat dissipation film.
Technical Field
With the increasing development of consumer electronics such as mobile phones, tablets, computers and the like, the requirements for equipment operation experience are improved, electronic devices are developing in the directions of being light, thin and small, and the requirements for hardware configuration of electronic products are high, so that the power density of the devices is gradually increased, the power consumption and the heat productivity are increased rapidly, heat accumulation cannot be dissipated in a short time, the temperature of a chip is increased rapidly, and the stability, the service life and the safety of electronic components are seriously affected. The heat dissipation material has become an important way to solve the overheating problem, and is an important guarantee for the reliable and high-speed operation of electronic components. The mainstream heat dissipation material in electronic equipment in the market at present is a high-heat-conductivity graphite film which is mainly formed by sintering polyimide, coal tar is generated in the preparation process, the environment is polluted, the polyimide film is mainly imported from abroad, the preparation cost is high, the process is complex, and the localization of the high-quality polyimide film still needs a long time.
Graphene is a novel two-dimensional material, is the thinnest and high-strength nano material in the world at present, has the thermal conductivity coefficient of 5300W/m.K, is an ideal heat conduction material, and provides an opportunity for the development of a new generation of heat dissipation materials. At present, a large number of manufacturers exist in China, and the quality of the graphene oxide is continuously improved, so that a foundation is laid for the graphene oxide. Graphene oxide is mainly used as a main raw material for preparing the graphene heat dissipation film, the reduced graphene oxide heat dissipation film is obtained by spin coating, spray coating, coating film forming and reduction at high temperature, but the production energy consumption is high, the cost is high, and the graphene film prepared by the methods has low thickness and low heat flux, and cannot meet the requirement of the current electronic equipment on increasing rapid heat dissipation.
Disclosure of Invention
The invention aims to overcome the technical problems that a graphene film obtained by a method in the prior art is low in thickness and heat flux, cannot meet the requirement of current electronic equipment for increasing rapid heat dissipation, and the like, and provides a preparation method of a graphene composite nano diamond heat dissipation film.
The purpose of the invention is realized by the following technical scheme:
a preparation method of a graphene composite nano-diamond heat dissipation film comprises the following steps:
s1, preparing graphene composite nano-diamond slurry;
s2, coating the graphene composite nano-diamond slurry obtained in the step S1 on a release film;
s3, drying the release film coated in the step S2, and stripping to obtain a stripping film;
s4, carrying out carbonization and deoxidation treatment and graphitization treatment on the stripping film obtained in the step S3 to obtain a graphene composite nano diamond heat dissipation film;
in the step S1, the graphene composite nanodiamond slurry is composed of the following components in percentage by weight: 0.05-5% of graphene oxide, 0.05-1% of nano diamond, 0.05-1% of dispersing agent, 0.05-1% of reducing agent and the balance of water.
In the preparation method of the graphene composite nano-diamond heat dissipation film, in step S1, the components of the slurry are mixed, stirred and ultrasonically processed to prepare the slurry with the viscosity of 5000-200000 mPa · S, and then vacuumized and defoamed for 5-60 min until bubbles completely disappear. And then coating the composite slurry obtained in the step S1 on a release film by a blade coating mode, a gravure coating mode, a dip coating mode, a slot coating mode or a transfer coating mode. And S3, placing the release film coated with the slurry in a forced air drying oven for drying, peeling the graphene composite nano-diamond from the release film, and then performing deoxidation treatment and graphitization treatment on the peeled release film in the step S4. And a deoxidation treatment process, namely putting the obtained stripping film into a carbonization furnace for deoxidation treatment. And (4) graphitization treatment, namely putting the deoxidized stripping film into a high-temperature graphite furnace, and performing graphitization treatment under the atmosphere of vacuum, argon or nitrogen.
Preferably, the size of the graphene oxide is 1-30 μm.
And (3) pre-selecting, wherein the size of the nano diamond is 1-500 nm.
Preferably, the reducing agent is one or a mixture of more than two of ascorbic acid, hydrazine hydrate sodium bisulfite and sodium borohydride reducing agent.
Preferably, the dispersant is one or a mixture of two or more of polyvinylpyrrolidone, sodium carboxymethylcellulose, polyethylene glycol, polyvinyl alcohol, hexadecyl ammonium bromide, sodium dodecyl benzene sulfonate, sodium dodecyl sulfonate, sodium alkyl diphenyl ether disulfonate, polyacrylamide, acrylic resin and modified acrylic resin.
Preferably, in the step S2, the coating thickness of the slurry on the release film is 10 to 500 μm, and then the slurry is dried in a forced air drying oven at 60 to 100 ℃ for 10 to 120 min.
Preferably, the hydrodeoxygenation treatment in the step S3 includes: heating to 300-1800 ℃ at a heating rate of 2-5 ℃/min, and keeping the temperature for 2-8 h.
Preferably, the graphitizing in the step S4 includes heating the stripped film after the deoxidation treatment to 2000-3000 ℃ at a heating rate of 2-5 ℃/min, and maintaining the temperature for 0.5-2 h.
Preferably, the graphene composite nano-diamond heat dissipation film obtained in the step S4 is rolled to a density of 1-2 g/cm3The calendering pressure is 1-50 MPa.
Preferably, the thickness of the graphene composite nano-diamond heat dissipation film after rolling is 100-500 μm. The rolling processing is carried out by adopting a roller press, and the thickness of the heat dissipation film can be adjusted by controlling the pressure in the rolling process.
Compared with the prior art, the invention has the following technical effects:
according to the preparation method of the graphene composite nano-diamond heat dissipation film, provided by the invention, graphene and nano-diamond are used as raw materials of the heat dissipation film, so that on one hand, the thickness of the obtained graphene composite nano-diamond heat dissipation film is adjustable, and the longitudinal heat conductivity of the graphene composite nano-diamond heat dissipation film is improved. On the other hand, the preparation method is simple and feasible, can not generate a large amount of tar, has simple and stable treatment process and higher repeatability, and has great significance for environmental protection.
Drawings
Fig. 1 is a flow chart of the preparation of graphene composite nanodiamond slurry according to the preparation method of the present invention;
FIG. 2 is a thermal imaging diagram of the graphene composite nanodiamond heat dissipation film obtained by the method of example 1;
fig. 3 is a thermal imaging diagram of the graphene composite nanodiamond heat dissipation film obtained by the method of example 2.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be described in detail below with reference to specific examples and comparative examples. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the examples given herein without any inventive step, are within the scope of the present invention.
Unless otherwise specified, the devices used in this example are all conventional experimental devices, the materials and reagents used are commercially available, and the experimental methods without specific descriptions are also conventional experimental methods.
Example 1
A preparation method of a graphene composite nano-diamond heat dissipation film comprises the following steps:
(1) preparing graphene slurry: mixing 5% of oxidized thin-layer graphene powder and 90% of deionized water according to the weight percentage, stirring and ultrasonically preparing composite slurry with the viscosity of 20000 mPa.s, and then carrying out vacuumizing and defoaming treatment for 5 minutes;
(2) coating: coating the composite slurry obtained in the step (1) on PET by adopting a scraper coating mode to form a graphene heat dissipation film with the thickness of 100 microns, and drying the graphene heat dissipation film in a forced air drying oven to strip the graphene heat dissipation film from the PET;
(3) pre-reduction treatment: putting the graphene oxide film obtained in the step (2) into a carbonization furnace for carbonization and deoxidation treatment;
(4) graphitization treatment: placing the graphene oxide film subjected to the pre-reduction treatment in the step (3) into a high-temperature graphite furnace, performing graphitization treatment in a vacuum, argon or nitrogen atmosphere, and performing full graphitization to obtain a graphene heat dissipation film;
(5) rolling treatment: rolling the graphitized graphene film obtained in the step (4) by using a roller press until the density is 1-2 g/cm3The graphene heat dissipation film with high heat conductivity, high performance and controllable thickness can be obtained, wherein the heat conductivity is 1200 +/-100W/m.K, the longitudinal heat conductivity is 10 +/-3W/m.K, and the range is wide.
Example 2
A preparation method of a graphene composite nano-diamond heat dissipation film comprises the following steps:
(1) preparing graphene/nano-diamond composite slurry: mixing 5% of graphene oxide thin layer powder, 0.05% of nano diamond powder and 89.95% of deionized water according to the weight percentage, stirring and ultrasonically preparing composite slurry with the viscosity of 20000 mPa.s, and then carrying out vacuum pumping and defoaming treatment for 10 minutes;
(2) coating: coating the composite slurry obtained in the step (1) on PET by adopting a scraper coating mode to form a graphene heat dissipation film with the thickness of 100 microns, and drying the graphene heat dissipation film in a forced air drying oven to strip the graphene heat dissipation film from the PET;
(3) pre-reduction treatment: putting the graphene oxide film obtained in the step (2) into a carbonization furnace for carbonization and deoxidation treatment;
(4) graphitization treatment: placing the graphene oxide film subjected to the pre-reduction treatment in the step (3) into a high-temperature graphite furnace, performing graphitization treatment in a vacuum, argon or nitrogen atmosphere, and performing full graphitization to obtain a graphene heat dissipation film;
(5) rolling treatment: rolling the graphitized graphene film obtained in the step (4) to a density of 1-2 g/cm by using a roller machine3The graphene heat dissipation film with high heat conductivity, high performance and controllable thickness can be obtained, wherein the heat conductivity is 1300 +/-50W/m.K, the longitudinal heat conductivity is 15 +/-3W/m.K, and the range is wide.
Examples of the experiments
The graphene composite nano-diamond heat dissipation films obtained by the methods of example 1 and example 2 were subjected to a thermal imaging experiment to obtain thermal imaging diagrams, as shown in fig. 1 and fig. 2. From fig. 1 and 2, it can be shown that the graphene composite nano-diamond heat dissipation film with diamond added into the composite slurry has lower surface temperature and faster heat dissipation under the same temperature.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention, and not for limiting the protection scope of the present invention, although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (10)
1. A preparation method of a graphene composite nano-diamond heat dissipation film is characterized by comprising the following steps:
s1, preparing graphene composite nano-diamond slurry;
s2, coating the graphene composite nano-diamond slurry obtained in the step S1 on a release film;
s3, drying the release film coated in the step S2, and stripping to obtain a stripping film;
s4, carrying out carbonization and deoxidation treatment and graphitization treatment on the stripping film obtained in the step S3 to obtain a graphene composite nano diamond heat dissipation film;
in the step S1, the graphene composite nanodiamond slurry is composed of the following components in percentage by weight: 0.05-5% of graphene oxide, 0.05-1% of nano diamond, 0.05-1% of dispersing agent, 0.05-1% of reducing agent and the balance of water.
2. The method for preparing the graphene composite nano-diamond heat dissipation film according to claim 1, wherein the size of the graphene oxide is 1-30 μm.
3. The method for preparing the graphene composite nano-diamond heat dissipation film according to claim 1, wherein the size of the nano-diamond is 1-500 nm.
4. The method for preparing the graphene composite nano-diamond heat dissipation film according to claim 1, wherein the reducing agent is one or a mixture of more than two of ascorbic acid, hydrazine hydrate sodium bisulfite and sodium borohydride reducing agent.
5. The method for preparing the graphene composite nano-diamond heat dissipation film according to claim 1, wherein the dispersant is one or a mixture of two or more of polyvinylpyrrolidone, sodium carboxymethylcellulose, polyethylene glycol, polyvinyl alcohol, cetyl ammonium bromide, sodium dodecylbenzenesulfonate, sodium dodecylsulfonate, sodium alkyl diphenylether disulfonate, polyacrylamide, acrylic resin, and modified acrylic resin.
6. The method for preparing the graphene composite nano-diamond heat dissipation film according to claim 1, wherein in the step S2, the coating thickness of the slurry on the release film is 10-500 μm, and then the release film is dried in a forced air drying oven at 60-100 ℃ for 10-120 min.
7. The method for preparing the graphene composite nano-diamond heat dissipation film according to claim 1, wherein the deoxidation treatment in step S3 includes: heating to 300-1800 ℃ at a heating rate of 2-5 ℃/min, and keeping the temperature for 2-8 h.
8. The method for preparing the graphene composite nano-diamond heat dissipation film according to claim 1, wherein the graphitization in the step S4 includes raising the temperature of the stripped film after the deoxidation treatment to 2000-3000 ℃ at a temperature raising rate of 2-5 ℃/min, and maintaining the temperature for 0.5-2 h.
9. The method for preparing the graphene composite nano-diamond heat dissipation film according to claim 1, wherein the graphene composite nano-diamond heat dissipation film obtained in the step S4 is rolled until the density is 1-2 g/cm3The calendering pressure is 1-50 MPa.
10. The method for preparing the graphene composite nano-diamond heat dissipation film according to claim 9, wherein the thickness of the graphene composite nano-diamond heat dissipation film after rolling is 100 to 500 μm.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113387702A (en) * | 2021-06-23 | 2021-09-14 | 浙江原邦材料科技有限公司 | High-thermal-conductivity graphene composite heat dissipation film and preparation method thereof |
| CN114864938A (en) * | 2021-11-22 | 2022-08-05 | 广东一纳科技有限公司 | Conductive paste containing carbon material and secondary battery |
| CN114958239A (en) * | 2022-06-27 | 2022-08-30 | 汤超 | Composite forming method and formula of radiating fin |
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Application publication date: 20210105 |