CN112853432A - Preparation method of graphene/aluminum composite material heat dissipation film - Google Patents
Preparation method of graphene/aluminum composite material heat dissipation film Download PDFInfo
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- CN112853432A CN112853432A CN202110156748.0A CN202110156748A CN112853432A CN 112853432 A CN112853432 A CN 112853432A CN 202110156748 A CN202110156748 A CN 202110156748A CN 112853432 A CN112853432 A CN 112853432A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 64
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 58
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 47
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 47
- 239000002131 composite material Substances 0.000 title claims abstract description 36
- 230000017525 heat dissipation Effects 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 238000010438 heat treatment Methods 0.000 claims abstract description 26
- 238000000137 annealing Methods 0.000 claims abstract description 16
- 239000011259 mixed solution Substances 0.000 claims abstract description 16
- 238000001652 electrophoretic deposition Methods 0.000 claims abstract description 13
- 239000011888 foil Substances 0.000 claims abstract description 12
- 238000007865 diluting Methods 0.000 claims abstract description 6
- 238000005406 washing Methods 0.000 claims abstract description 6
- 239000000243 solution Substances 0.000 claims description 16
- 238000001291 vacuum drying Methods 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 10
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 10
- 239000012286 potassium permanganate Substances 0.000 claims description 10
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 5
- 238000005119 centrifugation Methods 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 238000010790 dilution Methods 0.000 claims description 5
- 239000012895 dilution Substances 0.000 claims description 5
- 238000004070 electrodeposition Methods 0.000 claims description 5
- 238000009713 electroplating Methods 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 5
- 238000011010 flushing procedure Methods 0.000 claims description 5
- 238000007731 hot pressing Methods 0.000 claims description 5
- 239000001257 hydrogen Substances 0.000 claims description 5
- 229910052739 hydrogen Inorganic materials 0.000 claims description 5
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 230000007935 neutral effect Effects 0.000 claims description 5
- 238000006386 neutralization reaction Methods 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 230000003647 oxidation Effects 0.000 claims description 5
- 238000007254 oxidation reaction Methods 0.000 claims description 5
- 238000003825 pressing Methods 0.000 claims description 5
- 235000010344 sodium nitrate Nutrition 0.000 claims description 5
- 239000004317 sodium nitrate Substances 0.000 claims description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 5
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 5
- 238000000034 method Methods 0.000 abstract description 5
- 239000007864 aqueous solution Substances 0.000 abstract description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 2
- 230000005540 biological transmission Effects 0.000 abstract description 2
- 125000000524 functional group Chemical group 0.000 abstract description 2
- 239000002105 nanoparticle Substances 0.000 abstract description 2
- 239000002077 nanosphere Substances 0.000 abstract description 2
- 239000001301 oxygen Substances 0.000 abstract description 2
- 229910052760 oxygen Inorganic materials 0.000 abstract description 2
- 239000002245 particle Substances 0.000 abstract description 2
- 238000005245 sintering Methods 0.000 abstract description 2
- 238000000465 moulding Methods 0.000 abstract 1
- 230000003472 neutralizing effect Effects 0.000 abstract 1
- 230000001590 oxidative effect Effects 0.000 abstract 1
- 239000000463 material Substances 0.000 description 6
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 230000037303 wrinkles Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D13/00—Electrophoretic coating characterised by the process
- C25D13/02—Electrophoretic coating characterised by the process with inorganic material
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21D—WORKING OR PROCESSING OF SHEET METAL OR METAL TUBES, RODS OR PROFILES WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21D22/00—Shaping without cutting, by stamping, spinning, or deep-drawing
- B21D22/02—Stamping using rigid devices or tools
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21D—WORKING OR PROCESSING OF SHEET METAL OR METAL TUBES, RODS OR PROFILES WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21D37/00—Tools as parts of machines covered by this subclass
- B21D37/16—Heating or cooling
-
- 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
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D13/00—Electrophoretic coating characterised by the process
- C25D13/22—Servicing or operating apparatus or multistep processes
Abstract
The application discloses a preparation method of a graphene/aluminum composite material heat dissipation film, which sequentially comprises the following steps: preparing a mixed solution, oxidizing and neutralizing, diluting and centrifuging, washing, electrophoretic deposition, annealing and heat treatment, and hot-press molding. According to the method, an aluminum foil is used as an electrode to carry out electrophoretic deposition in an aqueous solution of graphene oxide to prepare the graphene/aluminum composite film, then the distance between the composite film layers is shortened through a high-temperature high-pressure sintering process, oxygen-containing functional groups are thoroughly removed, aluminum elements shrink to form nanosphere particles, and finally the graphene/aluminum composite material heat dissipation film is obtained; the invention fully utilizes the two-dimensional plane of the graphene to carry out phonon transmission, and inserts nano particles between graphene layers to improve longitudinal thermal conductivity; the composite material film prepared by the invention has good uniformity and thickness controllability, and has the advantages of large structural strength, high heat conductivity coefficient, uniform heat conduction in all directions, small density, stable performance and the like.
Description
Technical Field
The invention relates to the field of new energy technology development, in particular to a preparation method of a graphene/aluminum composite material heat dissipation film.
Background
With the continuous progress of science and technology, the development of industries such as electronics and electricity tends to be more intensive and miniaturized. The electronic device can release a large amount of heat during working, and if the heat cannot be conducted out in time, local high temperature is easily caused, so that the service life of the device is shortened, and even the effect is lost; therefore, higher requirements are put on heat dissipation of electronic devices, and the heat conduction material is required to have more excellent heat conduction performance and electrical insulation performance.
The heat dissipation material plays a very important role in the heat management technology, and the traditional heat dissipation materials such as silver, copper, aluminum and the like cannot meet the heat dissipation requirement of the existing electronic equipment due to the reasons of high thermal expansion coefficient, high density, serious influence of the material heat conductivity on the purity and the like; meanwhile, the graphite heat dissipation material applied to various electronic devices at the present stage has limited the improvement of the heat conduction performance due to the facts that the lamellar structure is not obvious, the internal pores and the wrinkles are difficult to eliminate and the like. Therefore, the development of new high-performance heat-dissipating film materials is imperative.
Disclosure of Invention
The technical problem to be solved by the invention is to overcome the defects and shortcomings in the background art and provide a preparation method of a graphene/aluminum composite material heat dissipation film.
In order to solve the technical problems, the technical scheme provided by the invention is as follows:
the embodiment of the application discloses a preparation method of a graphene/aluminum composite material heat dissipation film, which sequentially comprises the following steps:
s1 preparation of mixed solution: uniformly mixing 10-20 parts of concentrated sodium nitrate and 1600-1800 parts of concentrated sulfuric acid in parts by mass, adding 20-40 parts of natural flaky graphite powder, and stirring for full reaction to obtain a mixed solution;
s2 oxidation neutralization: slowly adding 80-100 parts of potassium permanganate into the mixed solution prepared in the step S1, uniformly stirring, and gradually dropwise adding 40% hydrogen peroxide solution to remove residual potassium permanganate until the solution becomes bright yellow;
s3 dilution centrifugation: diluting the mixture prepared in the step S2 with water, and centrifuging the mixture by using a high-speed centrifuge to obtain graphene oxide;
s4 flushing: washing the graphene oxide prepared in the step S3 with a 10% hydrochloric acid solution and deionized water until the solution is neutral, and filtering and dehydrating in a vacuum drying oven to obtain graphene oxide;
s5 electrophoretic deposition: adding the graphene oxide washed in the step S4 into deionized water for ultrasonic dispersion, performing electrophoretic deposition in an electroplating bath, performing electrodeposition for 5-6 min under the condition of constant voltage of 30-50V by using aluminum foils as positive and negative electrodes, forming a gel-like dark film on the surface of an aluminum foil anode, and putting the gel-like dark film into a vacuum drying oven for vacuum drying to obtain a graphene/aluminum composite film;
s6 annealing heat treatment: placing the graphene/aluminum composite film prepared in the step S5 into an atmosphere furnace, introducing nitrogen, heating to 300 ℃, keeping the temperature for 10-20 min, introducing hydrogen, heating to 500-700 ℃, carrying out annealing heat treatment, keeping the temperature for 30-600 min, and naturally cooling;
s7 hot press forming: and (4) forming the graphene/aluminum composite film subjected to annealing heat treatment in the step S6 by adopting a hot pressing technology, wherein the oil cylinder pressure is 40MPa, the pressing temperature is 600 ℃, and naturally cooling to obtain the graphene/aluminum composite material heat dissipation film.
Compared with the prior art, the invention has the advantages that: according to the method, an aluminum foil is used as an electrode to carry out electrophoretic deposition in a graphene oxide aqueous solution to prepare the graphene/aluminum composite film, the interlayer spacing of the composite film is shortened by means of a high-temperature and high-pressure sintering process, oxygen-containing functional groups are completely removed, aluminum elements shrink to form nanosphere particles, and finally the graphene/aluminum composite material heat dissipation film is obtained; the invention fully utilizes the two-dimensional plane of the graphene to carry out phonon transmission, and inserts nano particles between graphene layers to improve longitudinal thermal conductivity; the composite material film prepared by the invention has good uniformity and thickness controllability, and has the characteristics of large structural strength, high heat conductivity coefficient, uniform heat conduction in all directions, small density, stable performance and the like.
Detailed Description
Technical solutions in the embodiments of the present invention will be described in detail below, and it is apparent that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
Example 1
S1 preparation of mixed solution: uniformly mixing 15 parts of concentrated sodium nitrate and 1680 part of concentrated sulfuric acid in parts by mass, adding 30 parts of natural flaky graphite powder, and stirring for full reaction to obtain a mixed solution;
s2 oxidation neutralization: slowly adding 90 parts of potassium permanganate into the mixed solution prepared in the step S1, stirring uniformly, and gradually dropwise adding 40% hydrogen peroxide solution to remove residual potassium permanganate until the solution becomes bright yellow;
s3 dilution centrifugation: diluting the mixture prepared in the step S2 with water, and centrifuging the mixture by using a high-speed centrifuge to obtain graphene oxide;
s4 flushing: washing the graphene oxide prepared in the step S3 with a 10% hydrochloric acid solution and deionized water until the solution is neutral, and filtering and dehydrating in a vacuum drying oven to obtain graphene oxide;
s5 electrophoretic deposition: adding the graphene oxide washed in the step S4 into deionized water for ultrasonic dispersion, performing electrophoretic deposition in an electroplating bath, performing electrodeposition for 5.2min under the condition of 36V constant voltage by using aluminum foils as positive and negative electrodes, forming a gel-like dark film on the surface of an aluminum foil anode, and putting the gel-like dark film into a vacuum drying oven for vacuum drying to obtain a graphene/aluminum composite film;
s6 annealing heat treatment: placing the graphene/aluminum composite film prepared in the step S5 into an atmosphere furnace, introducing nitrogen, heating to 300 ℃, keeping the temperature for 15min, introducing hydrogen, heating to 600 ℃ for annealing heat treatment, keeping the temperature for 40min, and naturally cooling;
s7 hot press forming: and (4) forming the graphene/aluminum composite film subjected to annealing heat treatment in the step S6 by adopting a hot pressing technology, wherein the oil cylinder pressure is 40MPa, the pressing temperature is 620 ℃, and naturally cooling to obtain the graphene/aluminum composite material heat dissipation film.
Example 2
S1 preparation of mixed solution: uniformly mixing 13 parts of concentrated sodium nitrate and 1620 parts of concentrated sulfuric acid in parts by weight, adding 26 parts of natural flaky graphite powder, and stirring for full reaction to obtain a mixed solution;
s2 oxidation neutralization: slowly adding 82 parts of potassium permanganate into the mixed solution prepared in the step S1, uniformly stirring, and gradually dropwise adding 40% hydrogen peroxide solution to remove residual potassium permanganate until the solution becomes bright yellow;
s3 dilution centrifugation: diluting the mixture prepared in the step S2 with water, and centrifuging the mixture by using a high-speed centrifuge to obtain graphene oxide;
s4 flushing: washing the graphene oxide prepared in the step S3 with a 10% hydrochloric acid solution and deionized water until the solution is neutral, and filtering and dehydrating in a vacuum drying oven to obtain graphene oxide;
s5 electrophoretic deposition: adding the graphene oxide washed in the step S4 into deionized water for ultrasonic dispersion, performing electrophoretic deposition in an electroplating bath, performing electrodeposition for 5.5min under the condition of 40V constant voltage by using aluminum foils as positive and negative electrodes, forming a gel-like dark film on the surface of an aluminum foil anode, and putting the gel-like dark film into a vacuum drying oven for vacuum drying to obtain a graphene/aluminum composite film;
s6 annealing heat treatment: placing the graphene/aluminum composite film prepared in the step S5 into an atmosphere furnace, introducing nitrogen, heating to 300 ℃, keeping the temperature for 18min, introducing hydrogen, heating to 660 ℃, carrying out annealing heat treatment, keeping the temperature for 50min, and naturally cooling;
s7 hot press forming: and (4) forming the graphene/aluminum composite film subjected to annealing heat treatment in the step S6 by adopting a hot pressing technology, wherein the oil cylinder pressure is 40MPa, the pressing temperature is 600 ℃, and naturally cooling to obtain the graphene/aluminum composite material heat dissipation film.
Example 3
S1 preparation of mixed solution: uniformly mixing 18 parts of concentrated sodium nitrate and 1740 parts of concentrated sulfuric acid in parts by weight, adding 36 parts of natural flaky graphite powder, and stirring for full reaction to obtain a mixed solution;
s2 oxidation neutralization: slowly adding 96 parts of potassium permanganate into the mixed solution prepared in the step S1, uniformly stirring, and gradually dropwise adding 40% hydrogen peroxide solution to remove residual potassium permanganate until the solution becomes bright yellow;
s3 dilution centrifugation: diluting the mixture prepared in the step S2 with water, and centrifuging the mixture by using a high-speed centrifuge to obtain graphene oxide;
s4 flushing: washing the graphene oxide prepared in the step S3 with a 10% hydrochloric acid solution and deionized water until the solution is neutral, and filtering and dehydrating in a vacuum drying oven to obtain graphene oxide;
s5 electrophoretic deposition: adding the graphene oxide washed in the step S4 into deionized water for ultrasonic dispersion, performing electrophoretic deposition in an electroplating bath, performing electrodeposition for 5.8min under the condition of 42V constant voltage by using aluminum foils as positive and negative electrodes, forming a gel-like dark film on the surface of an aluminum foil anode, and putting the gel-like dark film into a vacuum drying oven for vacuum drying to obtain a graphene/aluminum composite film;
s6 annealing heat treatment: placing the graphene/aluminum composite film prepared in the step S5 into an atmosphere furnace, introducing nitrogen, heating to 300 ℃, keeping the temperature for 13min, introducing hydrogen, heating to 680 ℃ for annealing heat treatment, keeping the temperature for 55min, and naturally cooling;
s7 hot press forming: and (4) forming the graphene/aluminum composite film subjected to annealing heat treatment in the step S6 by adopting a hot pressing technology, wherein the oil cylinder pressure is 40MPa, the pressing temperature is 600 ℃, and naturally cooling to obtain the graphene/aluminum composite material heat dissipation film.
The thermal conductivity of the graphene/aluminum composite material heat dissipation film prepared in each of the above embodiments is measured by a laser flash method, and the obtained measurement results are shown in the following table.
The above embodiments are merely illustrative of the technical concepts and features of the present invention, and the purpose of the embodiments is to enable those skilled in the art to understand the contents of the present invention and implement the present invention, and not to limit the protection scope of the present invention. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.
Claims (1)
1. A preparation method of a graphene/aluminum composite material heat dissipation film is characterized by sequentially comprising the following steps:
s1 preparation of mixed solution: uniformly mixing 10-20 parts of concentrated sodium nitrate and 1600-1800 parts of concentrated sulfuric acid in parts by mass, adding 20-40 parts of natural flaky graphite powder, and stirring for full reaction to obtain a mixed solution;
s2 oxidation neutralization: slowly adding 80-100 parts of potassium permanganate into the mixed solution prepared in the step S1, uniformly stirring, and gradually dropwise adding 40% hydrogen peroxide solution to remove residual potassium permanganate until the solution becomes bright yellow;
s3 dilution centrifugation: diluting the mixture prepared in the step S2 with water, and centrifuging the mixture by using a high-speed centrifuge to obtain graphene oxide;
s4 flushing: washing the graphene oxide prepared in the step S3 with a 10% hydrochloric acid solution and deionized water until the solution is neutral, and filtering and dehydrating in a vacuum drying oven to obtain graphene oxide;
s5 electrophoretic deposition: adding the graphene oxide washed in the step S4 into deionized water for ultrasonic dispersion, performing electrophoretic deposition in an electroplating bath, performing electrodeposition for 5-6 min under the condition of constant voltage of 30-50V by using aluminum foils as positive and negative electrodes, forming a gel-like dark film on the surface of an aluminum foil anode, and putting the gel-like dark film into a vacuum drying oven for vacuum drying to obtain a graphene/aluminum composite film;
s6 annealing heat treatment: placing the graphene/aluminum composite film prepared in the step S5 into an atmosphere furnace, introducing nitrogen, heating to 300 ℃, keeping the temperature for 10-20 min, introducing hydrogen, heating to 500-700 ℃, carrying out annealing heat treatment, keeping the temperature for 30-600 min, and naturally cooling;
s7 hot press forming: and (4) forming the graphene/aluminum composite film subjected to annealing heat treatment in the step S6 by adopting a hot pressing technology, wherein the oil cylinder pressure is 40MPa, the pressing temperature is 600 ℃, and naturally cooling to obtain the graphene/aluminum composite material heat dissipation film.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN202110156748.0A CN112853432A (en) | 2021-02-05 | 2021-02-05 | Preparation method of graphene/aluminum composite material heat dissipation film |
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| CN202110156748.0A CN112853432A (en) | 2021-02-05 | 2021-02-05 | Preparation method of graphene/aluminum composite material heat dissipation film |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113796945A (en) * | 2021-10-29 | 2021-12-17 | 苏州海宇新辰医疗科技有限公司 | Cryoablation tube |
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