CN111471292B - Preparation method of graphene heat dissipation film - Google Patents
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Abstract
The invention belongs to the technical field of functional coatings, and particularly relates to a preparation method of a graphene heat dissipation film. The invention provides a preparation method of a graphene heat dissipation film, which comprises the following steps: preparing graphene slurry, scraping a film and performing directional treatment: and drying the graphene film by an oriented treatment method, and removing the flexible substrate after drying to obtain a graphene heat dissipation film product. In the technical scheme provided by the invention, complex steps such as calendering and high-temperature hot-pressing treatment are not required, and the preparation method is simple and convenient; meanwhile, the used raw materials are low in price and easy to obtain, so that the production cost is effectively reduced; further, through detection, compared with the similar products sold in the market, the heat dissipation performance of the prepared graphene heat dissipation film product is remarkably improved. The preparation method of the graphene heat dissipation film provided by the invention solves the technical defects that in the prior art, the heat dissipation film is difficult to give consideration to good heat dissipation effect, the preparation process is simple and convenient, and the cost is low.
Description
Technical Field
The invention belongs to the technical field of functional coatings, and particularly relates to a preparation method of a graphene heat dissipation film.
Background
With the advent of the 5G era, electronic products such as smart phones, tablet computers, telephone watches, and the like have become more and more intelligent and sophisticated, wherein the integration density of core components CPU and GPU has been continuously increased, and although powerful and intelligent use functions are provided, the enormous power consumption brings about a rapid increase in the amount of heat generation. The continuous heating causes the temperature of the devices to rise, which seriously affects the reliability and stability of the product, such as slow operation speed of the equipment, device failure, and even causes safety problems, so that the heat generated by the devices needs to be timely dissipated by adopting a heat dissipation scheme.
At present, products in the heat dissipation film industry mainly comprise natural graphite, artificial graphite heat dissipation films and high-heat-conductivity metal sheets; the traditional high-heat-conductivity metal sheet cannot meet the increasingly improved heat dissipation requirement, and is gradually replaced by natural graphite and artificial graphite heat dissipation films, and the natural graphite has poor heat dissipation effect due to factors such as the microstructure of the natural graphite; in contrast, artificial graphite has a relatively good heat dissipation effect, and the current method with better performance is to use a calendering method, mainly adopt a polyimide film to carbonize and graphitize and then calender, or a graphite paper high-temperature hot-pressing treatment, such as: patent document CN107010618A discloses a preparation method for preparing a highly oriented graphene heat dissipation film, which is a process of sintering and cold pressing graphene oxide at a high temperature, but has the technical problems of complexity, high cost and poor orientation effect.
Therefore, the invention provides a preparation method of a graphene heat dissipation film, which is used for solving the technical defects that in the prior art, the heat dissipation film is difficult to have good heat dissipation effect, the preparation process is simple and convenient, and the cost is low, and becomes a problem to be solved by technical personnel in the field.
Disclosure of Invention
In view of this, the invention provides a preparation method of a graphene heat dissipation film, which is used for solving the technical defects that in the prior art, the heat dissipation film is difficult to have a good heat dissipation effect, the preparation process is simple and convenient, and the cost is low.
The invention provides a preparation method of a graphene heat dissipation film, which comprises the following steps:
step one, preparing graphene slurry: dissolving graphite powder, a dispersing agent and a defoaming agent in water, shearing, homogenizing for the first time to obtain a graphene dispersion liquid, mixing the graphene dispersion liquid with resin and a film forming agent, and homogenizing for the second time to obtain graphene slurry;
step two, scraping the film: coating the graphene slurry on the surface of a flexible substrate by adopting a scraper film coating method to obtain a graphene film;
step three, directional processing: and drying the graphene film by an oriented treatment method, and removing the flexible substrate after drying to obtain a graphene heat dissipation film product.
Preferably, the method of directional treatment is selected from: any one or more of electric field treatment, magnetic field treatment, surface induction treatment and air flow treatment.
Preferably, the electric field treatment method comprises the following steps: and placing the graphene film in an electric field of alternating voltage, and electrifying at intervals until the graphene film is dried.
Preferably, the interval time of the interval electrification is 15 s-60 s, and the single electrification time length of the interval electrification is 15 s-60 s.
Preferably, in the first step, the graphite powder is selected from: any one or more of expanded graphite, flake graphite, and natural graphite flakes;
the dispersant is selected from: any one or more of acrylic block copolymer, polyvinyl alcohol and polymethacrylic acid;
the defoaming agent is selected from: any one or more of polyether defoaming agent, organic silicon defoaming agent and mineral oil defoaming agent;
the resin is selected from: any one or more of polyurethane resin, acrylic resin, epoxy resin, styrene butadiene rubber and ABS resin;
the film-forming agent is selected from: any one or more of an alcohol ether film forming agent, an acrylic film forming agent and a polyurethane film forming agent.
Preferably, in the step one, the feeding ratio of the raw materials is as follows by mass: 2-200 parts of graphite powder, 10-100 parts of dispersing agent, 1-10 parts of defoaming agent, 200-600 parts of resin and 5-100 parts of film forming agent.
Preferably, in the first step, the shearing time is 3 hours, and the shearing rotating speed is 600-3000 r/min;
in the first step, the pressure of the first homogenization is 40-100 MPa, and the time of the first homogenization is 3 hours;
in the first step, the pressure of the second homogenization is 20-120 MPa, and the time of the second homogenization is 0.5-2 h.
Preferably, in step two, the flexible substrate is selected from: any one or more of aluminum foil, copper foil, tin foil, PET film and PVC film;
in the second step, the thickness of the flexible substrate is 0.125-0.275 mm.
Preferably, in the second step, the method for coating the film by the doctor blade is as follows: and vacuum-absorbing one surface of a flexible substrate, keeping the gap between a scraper and the flexible substrate to be 200-1000 microns, and transferring the graphene slurry to the other surface of the flexible substrate by the scraper at the moving speed of 6-10 mm/s.
Preferably, in the second step, the thickness of the graphene film is 200-1000 μm;
in the second step, the coating amount of the graphene slurry is 100-1000 g/m2A flexible substrate.
In summary, the invention provides a preparation method of a graphene heat dissipation film, and the preparation method comprises the following steps: preparing graphene slurry, scraping a film and performing directional treatment: and drying the graphene film by an oriented treatment method, and removing the flexible substrate after drying to obtain a graphene heat dissipation film product. In the technical scheme provided by the invention, complex steps such as calendering and high-temperature hot-pressing treatment are not required, and the preparation method is simple and convenient; meanwhile, the used raw materials are low in price and easy to obtain, so that the production cost is effectively reduced; further, through detection, compared with the similar products sold in the market, the heat dissipation performance of the prepared graphene heat dissipation film product is remarkably improved. The preparation method of the graphene heat dissipation film provided by the invention solves the technical defects that in the prior art, the heat dissipation film is difficult to give consideration to good heat dissipation effect, the preparation process is simple and convenient, and the cost is low.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the provided drawings without creative efforts.
Fig. 1 is a schematic flow chart of a preparation method of a graphene heat dissipation film provided by the invention.
Detailed Description
The embodiment of the invention provides a preparation method of a graphene heat dissipation film, which is used for solving the technical defects that in the prior art, the heat dissipation film is difficult to give consideration to good heat dissipation effect, the preparation process is simple and convenient, and the cost is low.
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious 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 derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In order to illustrate the present invention in more detail, the following describes a method for preparing a graphene heat dissipation film according to the present invention with reference to examples.
Example 1
This example is a specific example of preparing a graphene heat dissipation film product 1.
Preparing graphene slurry: dissolving 2kg of graphite powder, 10kg of dispersing agent and 3kg of defoaming agent in 1000L of water, shearing at the rotating speed of 600-3000 r/min for 1.5-5 h, homogenizing at the pressure of 40-100 MPa for 2-6 h to obtain graphene dispersion liquid 1, mixing the graphene dispersion liquid 1 with 200kg of resin and 5kg of film forming agent, and homogenizing at the pressure of 20-120 MPa for 0.5-2 h to obtain graphene slurry 1; in this embodiment, the graphite powder is expanded graphite, the dispersant is an acrylic block copolymer, the defoamer is a mineral oil defoamer, the resin is polyurethane resin, and the film-forming agent is a polyurethane film-forming agent.
Film scraping: coating the graphene slurry 1 on the surface of a flexible substrate by adopting a scraper film coating method to obtain a graphene film 1; in the embodiment, the flexible substrate is an aluminum foil, the thickness of the flexible substrate is 0.125-0.275 mm, the thickness of the graphene film 1 is 200-1000 μm, and the coating amount of the graphene slurry 1 is 100-1000 g/m2A flexible substrate; the method for coating the film by the scraper comprises the following steps: adsorbing the flexible substrate on the surface of a film coating machine by using a vacuum pump, adsorbing one surface of the flexible substrate in vacuum, keeping the gap between a scraper and the flexible substrate at 200-1000 microns, and transferring the graphene slurry 1 to the other surface of the flexible substrate by the scraper at the moving speed of 6-10 mm/s.
Orientation treatment: and drying the graphene film 1 by an oriented treatment method, and removing the flexible substrate after drying to obtain a graphene heat dissipation film product 1. In this embodiment, the method of the directional treatment is selected from electric field treatment; the specific method comprises the following steps: and in a room temperature or low temperature environment, the graphene film is placed in an electric field of alternating voltage, is powered on for 15-60 s, is powered off for 15-60 s, and is powered on at intervals until the graphene film is dried.
Example 2
This example is a specific example of preparing a graphene heat dissipation film product 2.
Preparing graphene slurry: dissolving 100kg of graphite powder, 90kg of dispersing agent and 5kg of defoaming agent in 1000L of water, shearing at the rotating speed of 600-3000 r/min for 1.5-5 h, homogenizing at the pressure of 40-100 MPa for 2-6 h to obtain graphene dispersion liquid 2, mixing the graphene dispersion liquid 2 with 280kg of resin and 60kg of film forming agent, and homogenizing at the pressure of 20-120 MPa for 0.5-2 h to obtain graphene slurry 2; in this embodiment, the graphite powder is flake graphite, the dispersant is an acrylic acid block copolymer, the defoamer is a mineral oil defoamer, the resin is acrylic resin, and the film-forming agent is a polyurethane film-forming agent.
Film scraping: coating the graphene slurry 2 on the surface of the flexible substrate by adopting a scraper film coating method to obtain a graphene film 2; in the embodiment, the flexible substrate is a copper foil, the thickness of the flexible substrate is 0.125-0.275 mm, and the thickness of the graphene film 2 is200 to 1000 mu m, and the coating amount of the graphene slurry 2 is 100 to 1000g/m2A flexible substrate; the method for coating the film by the scraper comprises the following steps: adsorbing the flexible substrate on the surface of a film coating machine by using a vacuum pump, adsorbing one surface of the flexible substrate in vacuum, keeping a gap between a scraper and the flexible substrate to be 200-1000 microns, and transferring the graphene slurry 2 to the other surface of the flexible substrate by the scraper at a moving speed of 6-10 mm/s.
Orientation treatment: and drying the graphene film 2 by an oriented treatment method, and removing the flexible substrate after drying to obtain a graphene heat dissipation film product 2. In this embodiment, the method of the directional treatment is selected from electric field treatment; the specific method comprises the following steps: and in a room temperature or low temperature environment, the graphene film is placed in an electric field of alternating voltage, is powered on for 15-60 s, is powered off for 15-60 s, and is powered on at intervals until the graphene film is dried.
Example 3
This embodiment is a specific example of preparing a graphene heat dissipation film product 3.
Preparing graphene slurry: dissolving 150kg of graphite powder, 100kg of dispersing agent and 7kg of defoaming agent in 1000L of water, shearing at the rotating speed of 600-3000 r/min for 1.5-5 h, homogenizing at the pressure of 40-100 MPa for 2-6 h to obtain graphene dispersion liquid 3, mixing the graphene dispersion liquid 3 with 500kg of resin and 70kg of film forming agent, and homogenizing at the pressure of 20-120 MPa for 0.5-2 h to obtain graphene slurry 3; in this embodiment, the graphite powder is flake graphite, the dispersant is polyvinyl alcohol, the defoamer is an organic silicon defoamer, the resin is epoxy resin, and the film-forming agent is an alcohol ether film-forming agent.
Film scraping: coating the graphene slurry 3 on the surface of the flexible substrate by adopting a scraper film coating method to obtain a graphene film 3; in the embodiment, the flexible substrate is a tin foil, the thickness of the flexible substrate is 0.125-0.275 mm, the thickness of the graphene film 3 is 200-1000 μm, and the coating amount of the graphene slurry 3 is 100-1000 g/m2A flexible substrate; the method for coating the film by the scraper comprises the following steps: adsorbing the flexible substrate on the surface of a film coating machine by using a vacuum pump, adsorbing one surface of the flexible substrate in vacuum, keeping the gap between a scraper and the flexible substrate to be 200-1000 mu m, and transferring the graphene slurry 3 to the other surface of the flexible substrate by the scraper at the moving speed of 6-10 mm/s.
Orientation treatment: and drying the graphene film 3 by an oriented treatment method, and removing the flexible substrate after drying to obtain a graphene heat dissipation film product 3. In this embodiment, the method of the directional processing is magnetic field processing.
Example 4
This embodiment is a specific example of preparing a graphene heat dissipation film product 4.
Preparing graphene slurry: dissolving 200kg of graphite powder, 100kg of dispersing agent and 10kg of defoaming agent in 1000L of water, shearing at the rotating speed of 600-3000 r/min for 1.5-5 h, homogenizing at the pressure of 40-100 MPa for 2-6 h to obtain graphene dispersion liquid 4, mixing the graphene dispersion liquid 4 with 600kg of resin and 100kg of film forming agent, and homogenizing at the pressure of 20-120 MPa for 0.5-2 h to obtain graphene slurry 4; in this embodiment, the graphite powder is a natural graphite flake, the dispersant is polyvinyl alcohol, the defoamer is an organic silicon defoamer, the resin is styrene butadiene rubber, and the film-forming agent is an acrylic film-forming agent.
Film scraping: coating the graphene slurry 4 on the surface of the flexible substrate by adopting a scraper film coating method to obtain a graphene film 4; in the embodiment, the flexible substrate is a PET film, the thickness of the flexible substrate is 0.125-0.275 mm, the thickness of the graphene film 4 is 200-1000 μm, and the coating amount of the graphene slurry 4 is 100-1000 g/m2A flexible substrate; the method for coating the film by the scraper comprises the following steps: adsorbing the flexible substrate on the surface of a film coating machine by using a vacuum pump, adsorbing one surface of the flexible substrate in vacuum, keeping the gap between a scraper and the flexible substrate to be 200-1000 mu m, and transferring the graphene slurry 4 to the other surface of the flexible substrate by the scraper at the moving speed of 6-10 mm/s.
Orientation treatment: and drying the graphene film 4 by an oriented treatment method, and removing the flexible substrate after drying to obtain a graphene heat dissipation film product 4. In this embodiment, the orientation treatment method is surface induction treatment.
Example 5
This embodiment is a specific example of preparing a graphene heat dissipation film product 5.
Preparing graphene slurry: 70kg of graphite powder, 50kg of dispersing agent and 1kg of defoaming agent are dissolved in 1000L of water, the mixture is sheared for 1.5-5 h at the rotating speed of 600-3000 r/min, and then is homogenized for 2-6 h at the pressure of 40-100 MPa to obtain graphene dispersion liquid 5, and after the graphene dispersion liquid 5 is mixed with 300kg of resin and 30kg of film forming agent, the mixture is homogenized for 0.5-2 h at the pressure of 20-120 MPa to obtain graphene slurry 5; in this embodiment, the graphite powder is expanded graphite, the dispersant is polymethacrylic acid, the defoamer is a polyether defoamer, the resin is ABS resin, and the film-forming agent is an acrylic film-forming agent.
Film scraping: coating the graphene slurry 5 on the surface of the flexible substrate by adopting a scraper film coating method to obtain a graphene film 5; in the embodiment, the flexible substrate is a PVC film, the thickness of the flexible substrate is 0.125-0.275 mm, the thickness of the graphene film 5 is 200-1000 μm, and the coating amount of the graphene slurry 5 is 100-1000 g/m2A flexible substrate; the method for coating the film by the scraper comprises the following steps: adsorbing the flexible substrate on the surface of a film coating machine by using a vacuum pump, adsorbing one surface of the flexible substrate in vacuum, keeping the gap between a scraper and the flexible substrate to be 200-1000 mu m, and transferring the graphene slurry 5 to the other surface of the flexible substrate by the scraper at the moving speed of 6-10 mm/s.
Orientation treatment: and drying the graphene film 5 by an oriented treatment method, and removing the flexible substrate after drying to obtain the graphene heat dissipation film product 5. In this embodiment, the method of directional treatment is gas flow treatment.
Example 6
This example is an example of measuring the heat dissipation effect of the products 1 to 5 obtained in examples 1 to 5.
The heat dissipation results of products 1 to 5 were measured, and the results obtained are shown in table 1. In this embodiment, the selected control is a commercially available graphene coolant.
TABLE 1
As can be seen from Table 1, the product prepared by the technical scheme provided by the invention has the thermal conductivity remarkably higher than that of similar products sold in the market, and has good heat dissipation performance.
Example 7
This example is an example of measuring the flexibility and tensile strength of the products 1-5 prepared in examples 1-5.
The flexibility and tensile strength of products 1 to 5 were measured, and the results are shown in Table 2. In this embodiment, the selected control is a commercially available graphene coolant.
TABLE 2
| Sample (I) | Flex cycle (second) | Tensile Strength (MPa) |
| Product 1 | >15000 | >50 |
| Product 2 | >15000 | >50 |
| Product 3 | >15000 | >50 |
| Product 4 | >15000 | >50 |
| Product 5 | >15000 | >50 |
| Reference substance | >15000 | >50 |
As can be seen from Table 2, the product prepared by the technical scheme provided by the invention has the same flex cycle number and tensile strength as similar products sold in the market, and can meet the use requirement.
As can be seen from the above embodiments, the technical solution provided by the present invention has the following advantages:
1. in the preparation method provided by the invention, high-temperature graphitization treatment is not required, so that the operation cost is greatly reduced;
2. by orientation treatment such as applying an electric field, highly oriented graphene nanoplatelets can be obtained: under the action of an electric field, the graphene is polarized to obtain a torque, the torque is gradually oriented in the resin along the direction of the electric field lines to realize high-orientation arrangement, graphene sheet layers are mutually overlapped, and a good electric and heat conducting network is formed in the resin, so that high heat conductivity along the direction of the graphene sheet layers is obtained;
3. according to the preparation method provided by the invention, the graphene nanosheets are well bonded together by adding the adhesive resin, so that the product has excellent flexibility and tensile resistance;
4. compared with the prior art, the heat dissipation film adopts the graphene oxide to prepare the graphene through reduction, the process and the materials are increased, and the cost is high;
5. in the traditional technology, when the polyimide and graphite paper are used for preparing the heat dissipation film, the cost is extremely high, a large amount of tar can be generated in the polyimide sintering process, the environment is protected, the tensile strength of the artificial graphite is reduced, and the artificial graphite is easy to break or damage when being processed improperly.
6. In the prior art, the process for preparing the highly-oriented graphene sheet layer is complex, and the requirement on an instrument is high through high-temperature calendering.
In summary, the invention provides a preparation method of a graphene heat dissipation film, and the preparation method comprises the following steps: preparing graphene slurry, scraping a film and performing directional treatment: and drying the graphene film by an oriented treatment method, and removing the flexible substrate after drying to obtain a graphene heat dissipation film product. In the technical scheme provided by the invention, complex steps such as calendering and high-temperature hot-pressing treatment are not required, and the preparation method is simple and convenient; meanwhile, the used raw materials are low in price and easy to obtain, so that the production cost is effectively reduced; further, through detection, compared with the similar products sold in the market, the heat dissipation performance of the prepared graphene heat dissipation film product is remarkably improved. The preparation method of the graphene heat dissipation film provided by the invention solves the technical defects that in the prior art, the heat dissipation film is difficult to give consideration to good heat dissipation effect, the preparation process is simple and convenient, and the cost is low.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (6)
1. A preparation method of a graphene heat dissipation film is characterized by comprising the following steps:
step one, preparing graphene slurry: dissolving graphite powder, a dispersing agent and a defoaming agent in water, shearing, homogenizing for the first time to obtain a graphene dispersion liquid, mixing the graphene dispersion liquid with resin and a film forming agent, and homogenizing for the second time to obtain graphene slurry;
step two, scraping the film: coating the graphene slurry on the surface of a flexible substrate by adopting a scraper film coating method to obtain a graphene film;
step three, directional processing: drying the graphene film by an oriented treatment method, and removing the flexible substrate after drying to obtain a graphene heat dissipation film product; the method of the directional treatment is selected from: any one or more of electric field treatment and magnetic field treatment;
in the first step, the graphite powder is selected from: any one or more of expanded graphite, flake graphite, and natural graphite flakes;
the dispersant is selected from: any one or more of acrylic block copolymer, polyvinyl alcohol and polymethacrylic acid;
the defoaming agent is selected from: any one or more of polyether defoaming agent, organic silicon defoaming agent and mineral oil defoaming agent;
the resin is selected from: any one or more of polyurethane resin, acrylic resin, epoxy resin, styrene butadiene rubber and ABS resin;
the film-forming agent is selected from: any one or more of an alcohol ether film forming agent, an acrylic film forming agent and a polyurethane film forming agent;
in the first step, the raw materials are fed in a ratio of: 2-200 parts of graphite powder, 10-100 parts of a dispersing agent, 1-10 parts of a defoaming agent, 200-600 parts of resin and 5-100 parts of a film forming agent;
in the first step, the shearing time is 1.5-5 h, and the shearing rotating speed is 600-3000 r/min;
in the first step, the pressure of the first homogenization is 40-100 MPa, and the time of the first homogenization is 2-6 h;
in the first step, the pressure of the second homogenization is 20-120 MPa, and the time of the second homogenization is 0.5-2 h.
2. The method for preparing the electric field according to claim 1, wherein the electric field treatment method is: and placing the graphene film in an electric field of alternating voltage, and electrifying at intervals until the graphene film is dried.
3. The preparation method according to claim 2, wherein the interval time of the interval energization is 15 s-60 s, and the single energization time period of the interval energization is 15 s-60 s.
4. The method according to claim 1, wherein in step two, the flexible substrate is selected from the group consisting of: any one or more of aluminum foil, copper foil, tin foil, PET film and PVC film;
in the second step, the thickness of the flexible substrate is 0.125-0.275 mm.
5. The method according to claim 1, wherein in the second step, the method for coating the film by the doctor blade is as follows: and vacuum-absorbing one surface of a flexible substrate, keeping the gap between a scraper and the flexible substrate to be 200-1000 microns, and transferring the graphene slurry to the other surface of the flexible substrate by the scraper at the moving speed of 6-10 mm/s.
6. The preparation method according to claim 1 or 5, wherein in the second step, the graphene film has a thickness of 200 to 1000 μm;
in the second step, the coating amount of the graphene slurry is 100-1000 g/m2A flexible substrate.
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| CN112608721A (en) * | 2020-12-14 | 2021-04-06 | 碳元科技股份有限公司 | 3D graphite composite heat conduction material, preparation method, composite slurry and smart phone |
| CN113072726A (en) * | 2021-04-02 | 2021-07-06 | 信骅(上海)器材有限公司 | Graphene radiating fin and preparation process thereof |
| 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 |
| CN115709991A (en) * | 2022-10-12 | 2023-02-24 | 东莞市鹏威能源科技有限公司 | Preparation method of graphene composite heat dissipation film with porous structure |
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