CN109536142B - Preparation method of graphene film heat conduction material - Google Patents
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Abstract
The invention discloses a preparation method of a graphene film heat conduction material, which is used for replacing an artificial graphite radiating fin taking PI as a raw material. The preparation method of the graphene film heat conduction material comprises the following steps: 1. preparing a graphene-heat conducting ceramic-polymer composite membrane; 2. carrying out graphitization processing on the graphene-heat conducting ceramic-polymer composite membrane; 3. and (5) rolling treatment. Preparing a graphene-heat conducting ceramic-polymer composite membrane: the preparation method comprises the steps of preparing slurry with the viscosity of 1000-5000cps in a pure water system by using aqueous graphene, a very small amount of non-ionic surfactant, an aqueous polymer film assistant and a heat-conducting ceramic nano powder dispersion liquid, then casting the slurry on a release film, and drying through a drying tunnel to obtain the heat-conducting ceramic nano film, wherein the graphitization process treatment comprises three stages of heating, crystallization and natural cooling. The preparation method has the advantages of simple process, high heat conductivity coefficient of the product, environmental friendliness and no toxic substances generated in the whole process.
Description
Technical Field
The invention relates to a preparation method of a graphene film heat conduction material, and belongs to the technical field of heat conduction and dissipation materials.
Background
Along with the rapid development of electronic technology, the density of electronic components is higher and higher, and power devices have a certain stable working temperature range, however, the high density of the devices means that a large amount of heat is generated. Therefore, how to effectively realize heat dissipation of the device to ensure stable operation of the device is also receiving more attention.
The traditional heat dissipation materials are mainly metal materials, and graphite materials are widely applied to heat dissipation materials of electronic devices due to high thermal conductivity and low density of the graphite materials, wherein the heat-conducting graphite film not only has higher thermal conductivity and lower density than metals such as aluminum, copper and the like, but also can be smoothly attached to any plane and curved surface, so that the heat-conducting graphite film is a popular heat dissipation film for electronic products such as mobile phones, tablet computers, L ED lighting equipment, wearable equipment and the like.
The heat conduction graphite film is prepared by a method 3, a method 2 is low in cost, but the heat conduction coefficient of the graphite film is only 800W/(m.K) which meets the requirement of increasing heat dissipation of electronic products day by day, a method 3 is an improvement on the method 1, other high polymer materials are used for replacing PI, then graphene filling sheets are added, the purpose of increasing the heat conduction coefficient is achieved, however, the main raw material is still a high polymer material, the film still shrinks after being heated in the carbonization process, the heat conduction coefficient of the film is further reduced, and the defect of the heat conduction material is further solved, so that the defect of the heat conduction material in the subsequent high-temperature heat conduction film preparation is further overcome, the defect of the heat conduction material is further overcome, the problem that the heat conduction coefficient of the heat conduction material is reduced, the main heat conduction coefficient of the heat conduction material is reduced, and the heat conduction coefficient of the heat conduction material is reduced by adding an organic graphene filling sheet is further reduced.
Disclosure of Invention
The invention aims to provide a preparation method of a graphene film heat conduction material, which is mainly used for replacing an artificial graphite radiating fin made of a PI raw material and solving some problems in the existing preparation method.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows.
The preparation method of the graphene-heat-conducting ceramic-polymer composite membrane comprises the following steps: the slurry with the viscosity of 1000-plus-5000 cps is prepared by mixing the water-based graphene, a very small amount of non-ionic surfactant, a water-based polymer film assistant and a heat-conducting ceramic nano powder dispersion liquid in a pure water system. And (3) casting the slurry on a release film, and drying the release film through a drying tunnel to obtain the graphene-heat-conducting ceramic-polymer composite film. The width of the composite film is limited only by the coating width of the coating apparatus.
Further, the temperature of the graphene-heat conducting ceramic-polymer composite film during drying in the drying tunnel is 50-90 ℃, and the time is 1-6 min. Because the thickness of the wet film formed by coating is more than 0.1mm, in order to avoid the boiling of water in the wet film caused by overhigh temperature, the temperature of a drying tunnel is not more than 90 ℃, the drying time is not less than 1min, and the water in the wet film is removed under the milder environment as far as possible. A suspension drying tunnel is generally considered to be the best choice.
Further, the thickness of the graphene-heat-conducting ceramic-polymer composite membrane is 0.02-1.5 mm. At present, the most common graphite heat dissipation assembly in intelligent electronic equipment has the thickness of 0.02-1mm, and considering that the thickness of a graphene film is reduced in a high-temperature graphitization process and a calendering process, the thickness of the composite film is controlled to be 0.02-1.5mm, which is most beneficial to subsequent processes.
Further, the preparation ratio of the composite membrane is as follows: the composite material comprises water-based graphene, a non-ionic surfactant, a water-based polymer film aid and a heat-conducting ceramic nano powder dispersion liquid, wherein the mass ratio of the water-based graphene to the non-ionic surfactant to the water-based polymer film aid is (80-95) = (1-6): (3-10): 1-4).
Further, the nonionic surfactant is any one of polyoxyethylene octylphenol ether, polyoxyethylene nonylphenol ether and polyoxyethylene lauryl ether; the water-based polymer film auxiliary agent is any one of polyvinyl alcohol, hydroxypropyl methyl cellulose, sodium hydroxymethyl cellulose and hydroxyethyl cellulose; the heat-conducting ceramic nano powder is any one of aluminum oxide and boron nitride.
Further, in the preparation method of the graphene-thermal conductive ceramic-polymer composite membrane, the method for mixing the aqueous graphene, the nonionic surfactant, the aqueous polymer film assistant and the thermal conductive ceramic nano powder comprises the following steps: one or the combination of any two or more of mechanical stirring, ultrasonic mixing and ball milling mixing. The non-ionic surfactant is used for dispersing the water-based graphene, so that the graphene exists in a sheet form in the slurry, and further exists in a sheet form in the prepared composite membrane, and the sheet form is easy to form a graphite sheet layer with a larger size in the graphitization treatment process, so that the finally formed heat conduction material has better heat conduction performance. The aqueous polymer film assistant is beneficial to forming a composite film with certain toughness after the slurry is coated, and is convenient to peel and rewind. Meanwhile, the surfactant and the film forming auxiliary agent can be cracked at a low temperature section to form coke in the graphitization process, and a high temperature section can also be graphitized, so that defects can not be brought to a final product. The heat-conducting ceramic nano powder has the similar effect as a surfactant, and mainly promotes graphene to be dispersed in slurry in a sheet structure. The surfactant and the heat-conducting ceramic nano powder can play a role in synergistic dispersion, the effect is better than that of a single component, and meanwhile, when the ceramic powder is pyrolyzed in a graphitized high-temperature section, the ceramic powder can play a role similar to a catalyst to promote the reconnection of graphene sheets.
Further, according to the mixing method, the transverse dimension of the aqueous graphene in the mixed slurry is 10-70 μm, the longitudinal dimension of the aqueous graphene is 10-70 μm, and the thickness of the aqueous graphene is 0.4-6 nm.
Further, the graphene-heat-conducting ceramic-polymer composite film is required to be peeled off from the release film, and the bottomless film coiled material is obtained through rewinding treatment.
Further, the non-bottom film coiled material can be used for obtaining the graphene film heat conduction material only by graphitization treatment. The graphitization process is mainly divided into three sections: heating, crystallizing and cooling, wherein the specific procedures are as follows: heating up at a temperature rising rate of 4-8 ℃/min at 0-1000 ℃, heating up at a temperature rising rate of 3-4 ℃/min at 1600-1600 ℃ for 1000-.
The above process parameters are partially adjusted mainly according to my existing technology 201711158854.2, a preparation process of a uniform high-thermal-conductivity graphite film coiled material.
Further, performing cold-pressing steel roll calendering on the graphitized coiled material to obtain the continuous graphene film heat conduction material with uniform thickness.
Furthermore, the graphene film heat conduction material has a thickness of 20-100 μm and a heat conductivity of 1000-1800W/(m.K).
Compared with the prior art, the invention has the following advantages.
1. The raw material is graphene aqueous dispersion, the current China is the world's largest graphene producing country, the raw material supply is reliable and stable, and production stop caused by insufficient raw material supply can not occur. Graphite PI currently has only ten suppliers worldwide, and raw materials are limited by people.
2. The main body of the raw material is graphene, special carbonization treatment is not needed, the preparation process is simpler, graphitization treatment can be directly carried out, meanwhile, the thickness and the width of the final finished product can be customized according to customer requirements, particularly, the thickness and the width are far superior to those of PI graphite flakes, the number of lamination layers can be reduced due to the larger thickness, the negative influence of a double-sided adhesive for lamination on the overall heat conductivity coefficient of the assembly is further reduced, and the large width can be used for manufacturing a large-size heat dissipation assembly and is suitable for heat dissipation of a large-size O L ED screen.
3. The product performance reaches or exceeds that of the PI raw material graphite flake, the horizontal heat conductivity coefficient can reach the same level as that of the PI raw material graphite flake, the heat conductivity coefficient in the vertical direction is far superior to that of the PI raw material graphite flake, and the vertical heat diffusion capability is stronger while the requirement of horizontal heat diffusion is met.
4. The cost is superior to that of the PI raw material graphite flake: the unit price of the current domestic water-based graphene is basically the same as that of graphite PI, the production process of the invention is simpler, the energy consumption is lower, and the yield of one process is superior to that of two processes of PI graphite flake, so the total cost is superior. Meanwhile, the thickness of the graphene film can be more than twice of that of the traditional PI graphite sheet, so that the die cutting and laminating times can be reduced for a die cutting link in the manufacturing process of the heat dissipation assembly, the rejection rate of downstream enterprises can be reduced, the cost can be reduced, the yield can be improved, and more values can be created.
Detailed Description
The present invention will be described in detail with reference to specific embodiments. Of course, the following examples are only some of the examples of the present invention.
Example 1.
The graphene-heat conducting ceramic-polymer composite membrane comprises the following components in percentage by mass: the preparation method comprises the following steps of preparing water-based graphene, a non-ionic surfactant, a water-based polymer film aid and heat-conducting ceramic nano powder =95:1:3:1, wherein the maximum diameter of the water-based graphene is 50 micrometers, the maximum thickness of the water-based graphene is 6 nm, the non-ionic surfactant is octyl phenol polyoxyethylene ether, the water-based polymer film agent is hydroxypropyl methyl cellulose, and the ceramic powder is aluminum oxide (the particle size of D50 is 5 micrometers).
The graphene film heat conduction material is prepared by the following steps.
The method comprises the following steps: the preparation method of the graphene-heat-conducting ceramic-polymer composite membrane comprises the following steps: firstly, adding water-based graphene, a non-ionic surfactant, a water-based polymer film assistant and heat-conducting ceramic nano powder into a stirrer, and stirring for 20 min to form slurry with the viscosity of 2000 cps. And then, casting the slurry on a release film, and drying for 3 min through a drying tunnel at the temperature of 80 ℃ to obtain the graphene-heat-conducting ceramic-polymer composite film with the thickness of 80 microns.
Step two: and stripping the graphene-heat-conducting ceramic-polymer composite film from a release film, and rewinding to obtain the base film-free coiled material. Then graphitizing the coiled material without the bottom film, wherein the specific procedures are as follows: the coiled material is heated from room temperature to 1000 ℃ at the heating rate of 6 ℃/min, then heated to 1600 ℃ at the heating rate of 4 ℃/min, then heated to 2300 ℃ at the heating rate of 2 ℃/min, then heated to 2950 ℃ at the heating rate of 5 ℃/min, and then kept at 2950 ℃ for 8 h and then naturally cooled. And finally, carrying out cold-pressing steel roll calendering on the graphitized coiled material to obtain the continuous large-size coiled graphene film heat conduction material with uniform thickness.
The graphene film heat conduction material obtained by the process has the thickness of 45 mu m and the heat conductivity of 1300W/(m.K).
Example 2.
The graphene-heat conducting ceramic-polymer composite membrane comprises the following components in percentage by mass: the water-based graphene film is prepared from water-based graphene, a non-ionic surfactant, a water-based polymer film aid and heat-conducting ceramic nano powder =90:3:6:1, wherein the maximum diameter of the water-based graphene is 70 mu m, the maximum thickness of the water-based graphene is 3 nm, the non-ionic surfactant is octyl phenol polyoxyethylene ether, the water-based polymer film agent is hydroxypropyl methyl cellulose, and the ceramic powder is aluminum oxide (the particle size of D50 is 15 mu m).
The graphene film heat conduction material is prepared by the following steps.
The method comprises the following steps: the preparation method of the graphene-heat-conducting ceramic-polymer composite membrane comprises the following steps: firstly, adding water-based graphene, a non-ionic surfactant, a water-based polymer film assistant and heat-conducting ceramic nano powder into a stirrer, and stirring for 20 min to form slurry with the viscosity of 5000 cps. And then, casting the slurry on a release film, and drying for 6 min through a drying tunnel at the temperature of 60 ℃ to obtain the graphene-heat-conducting ceramic-polymer composite film with the thickness of 1.5 mm.
Step two: and (3) stripping the graphene-heat-conducting ceramic-polymer composite film from the release film, and rewinding to obtain the base film-free coiled material. Then graphitizing the coiled material without the bottom film, wherein the specific procedures are as follows: the coiled material is heated from room temperature to 1000 ℃ at the heating rate of 6 ℃/min, then heated to 1600 ℃ at the heating rate of 4 ℃/min, then heated to 2300 ℃ at the heating rate of 2 ℃/min, then heated to 2950 ℃ at the heating rate of 5 ℃/min, and then kept at 2950 ℃ for 8 h and then naturally cooled. And finally, carrying out cold-pressing steel roll calendering on the graphitized coiled material to obtain the continuous large-size coiled graphene film heat conduction material with uniform thickness.
The graphene film heat conduction material obtained by the process has the thickness of 1mm and the heat conductivity of 1000W/(m.K).
Example 3.
The graphene-heat conducting ceramic-polymer composite membrane comprises the following components in percentage by mass: the water-based graphene film comprises water-based graphene, a non-ionic surfactant, a water-based polymer film aid and heat-conducting ceramic nano powder =85:5:9:1, wherein the diameter distribution of the water-based graphene is 10-15 mu m, the maximum thickness of the water-based graphene is 0.4 nm, the non-ionic surfactant is octyl phenol polyoxyethylene ether, the water-based polymer film agent is sodium hydroxymethyl cellulose, and the ceramic powder is boron nitride (the particle size of D50 is 1 um).
The graphene film heat conduction material is prepared by the following steps.
The method comprises the following steps: the preparation method of the graphene-heat-conducting ceramic polymer composite membrane comprises the following steps: firstly, adding water-based graphene, a non-ionic surfactant, a water-based polymer film assistant and heat-conducting ceramic nano powder into a stirrer, and stirring for 20 min to form slurry with the viscosity of 1000 cps. And then, casting the slurry on a release film, and drying for 1min through a drying tunnel at the temperature of 90 ℃ to obtain the graphene-heat-conducting ceramic-polymer composite film with the thickness of 20 mu m.
Step two: and stripping the graphene-heat-conducting ceramic-polymer composite film from a release film, and rewinding to obtain the base film-free coiled material. Then graphitizing the coiled material without the bottom film, wherein the specific procedures are as follows: the coiled material is heated from room temperature to 1000 ℃ at the heating rate of 6 ℃/min, then heated to 1600 ℃ at the heating rate of 4 ℃/min, then heated to 2300 ℃ at the heating rate of 2 ℃/min, then heated to 2950 ℃ at the heating rate of 5 ℃/min, and then kept at 2950 ℃ for 8 h and then naturally cooled. And finally, carrying out cold-pressing steel roll calendering on the graphitized coiled material to obtain the continuous large-size coiled graphene film heat conduction material with uniform thickness.
The graphene film heat conduction material obtained by the process has the thickness of 0.02 mm and the heat conductivity of 1800W/(m.K).
Example 4.
The graphene-heat conducting ceramic-polymer composite membrane comprises the following components in percentage by mass: the water-based graphene film is prepared from water-based graphene, a non-ionic surfactant, a water-based polymer film aid and heat-conducting ceramic nano powder =80:6:10:4, wherein the diameter distribution of the water-based graphene is 20-45 mu m, the maximum thickness of the water-based graphene is 5 nm, the non-ionic surfactant is octyl phenol polyoxyethylene ether, the water-based polymer film agent is sodium hydroxymethyl cellulose, and the ceramic powder is boron nitride (the particle size of D50 is 5 mu m).
The graphene film heat conduction material is prepared by the following steps.
The method comprises the following steps: the preparation method of the graphene-heat-conducting ceramic polymer composite membrane comprises the following steps: firstly, adding water-based graphene, a non-ionic surfactant, a water-based polymer film assistant and heat-conducting ceramic nano powder into a stirrer, and stirring for 20 min to form slurry with the viscosity of 5000 cps. And then, casting the slurry on a release film, and drying for 3 min through a drying tunnel at the temperature of 80 ℃ to obtain the graphene-heat-conducting ceramic-polymer composite film with the thickness of 0.25 mm.
Step two: and stripping the graphene-heat-conducting ceramic-polymer composite film from a release film, and rewinding to obtain the base film-free coiled material. Then graphitizing the coiled material without the bottom film, wherein the specific procedures are as follows: the carbonized coiled material is heated from room temperature to 1000 ℃ at the heating rate of 6 ℃/min, then heated to 1600 ℃ at the heating rate of 4 ℃/min, then heated to 2300 ℃ at the heating rate of 2 ℃/min, then heated to 2950 ℃ at the heating rate of 5 ℃/min, and then kept at 2950 ℃ for 8 h and then naturally cooled. And finally, carrying out cold-pressing steel roll calendering on the graphitized coiled material to obtain the continuous large-size coiled graphene film heat conduction material with uniform thickness.
The graphene film heat conduction material obtained by the process has the thickness of 0.11 mm and the heat conductivity of 1100W/(m.K).
While the present invention has been described in detail with reference to the above embodiments, it should be understood that the embodiments are illustrative only, and not restrictive, and that various changes and modifications can be made without departing from the spirit and scope of the invention.
Claims (6)
1. A preparation method of a graphene film heat conduction material is characterized by comprising the following preparation steps:
step 1: preparing a graphene-heat conducting ceramic-polymer composite membrane;
the raw materials and the mass ratio are as follows: the water-based graphene comprises water-based graphene, a non-ionic surfactant, a water-based polymer film assistant, and heat-conducting ceramic nano powder dispersion liquid = (80-95): (1-6): 3-10): 1-4);
mixing the raw materials in a pure water system to prepare slurry with the viscosity of 1000-5000cps, casting the slurry on a release film, and drying through a drying tunnel to obtain the graphene-heat-conducting ceramic-polymer composite film; stripping the graphene-heat-conducting ceramic-polymer composite film from the release film, and rewinding to obtain a base film-free coiled material;
step 2: graphitizing process treatment;
the non-bottom film coiled material is subjected to graphitization processing according to the following procedures: heating at 0-1000 ℃ at a heating rate of 4-8 ℃/min, heating at 1000-1600 ℃ at a heating rate of 3-4 ℃/min, heating at 1600-2300 ℃ at a heating rate of 1-2 ℃/min, heating at 2300-2900 ℃ at a heating rate of 4-6 ℃/min, crystallizing at 2900-3100 ℃ for 1-12 h, and naturally cooling to room temperature;
and step 3: rolling;
rolling the coiled material subjected to the graphitization process by using a cold pressing steel roller to obtain a continuous graphene film heat conduction material with uniform thickness;
the number of graphene sheets of the aqueous graphene is not more than 15, the diameter of a single graphene film sheet is 10-70 μm,
the nonionic surfactant and the aqueous polymer film assistant can be completely pyrolyzed below 800 ℃,
the non-ionic surfactant is any one of octyl phenol polyoxyethylene ether, nonyl phenol polyoxyethylene ether and lauryl alcohol polyoxyethylene ether,
the aqueous polymer film auxiliary agent is any one of polyvinyl alcohol, hydroxypropyl methylcellulose, sodium hydroxymethyl cellulose and hydroxyethyl cellulose,
the heat-conducting ceramic nano powder is any one of aluminum oxide and boron nitride.
2. The preparation method of the graphene film heat-conducting material according to claim 1, wherein the drying temperature of the drying tunnel is 50-90 ℃ and the drying time is 1-6 min.
3. The preparation method of the graphene film heat-conducting material according to claim 1, wherein the thickness of the graphene-heat-conducting ceramic-polymer composite film is 0.02-1.5 mm.
4. The method for preparing the graphene film heat-conducting material according to claim 1, wherein the method comprises the following steps: the mixing method for the aqueous graphene, the nonionic surfactant, the aqueous polymer film assistant and the heat-conducting ceramic nano powder comprises one or the combination of any two or more of mechanical stirring, ultrasonic mixing and ball milling mixing.
5. The preparation method of the graphene film heat-conducting material according to claim 1, wherein the transverse dimension of the aqueous graphene in the mixed slurry is 10-70 μm, the longitudinal dimension of the aqueous graphene in the mixed slurry is 10-70 μm, and the thickness of the aqueous graphene in the mixed slurry is 0.4-6 nm.
6. The method for preparing the graphene film heat-conducting material according to claim 1, wherein the graphene film heat-conducting material has a thickness of 20-100 μm and a heat conductivity of 1000-1800W/(m.K).
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| CN103805144B (en) * | 2014-03-04 | 2016-06-29 | 中国科学院宁波材料技术与工程研究所 | A kind of Graphene heat conducting film and preparation method thereof |
| CN106167693B (en) * | 2016-06-21 | 2020-04-21 | 成都市科愿科技有限公司 | Preparation method of graphene-based film product |
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