CN112969355A - Graphene heat dissipation film and preparation method thereof - Google Patents
Graphene heat dissipation film and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a graphene heat dissipation film and a preparation method thereof, and the preparation method comprises the following steps: firstly, the method comprises the following steps: carrying out heat treatment on the polyimide film to obtain a heat-conducting graphite film semi-finished product, and carrying out needling treatment on the surface to form pores; II, secondly: carrying out strong acid oxidation, intercalation stripping, water washing and acid-base neutralization on graphite micro-sheets or graphite film waste by a Hummers method to obtain graphene oxide slurry; thirdly, the method comprises the following steps: adding a dispersing agent, an adhesive and a defoaming agent into the graphene oxide slurry, and stirring to obtain a graphene oxide slurry mixed solution; fourthly, the method comprises the following steps: coating the graphene oxide slurry mixed solution on the surface of the heat-conducting graphite film semi-finished product to obtain a graphene composite film; fifthly: dehydrating and drying the graphene composite membrane to obtain a dried graphene composite membrane; sixthly, the method comprises the following steps: rewinding the dried graphene composite film to obtain a graphene oxide composite film coiled material; seventhly, the method comprises the following steps: vertically placing a graphene oxide composite film coiled material, placing a graphite pipe, and carrying out decoking, graphene oxide reduction and graphite crystallization to obtain a high-thickness graphene composite film coiled material; eighthly: and rolling the high-thickness graphene composite film coiled material.
Description
Technical Field
The invention relates to the technical field of heat dissipation materials, in particular to a graphene heat dissipation film and a preparation method thereof.
Background
With the rapid development of electronic information technology, electronic devices are increasingly developed to high power, light weight and integration, but the power density of the devices is gradually increased, heat is accumulated and cannot be dissipated in a short time, and the temperature of a chip is rapidly increased. According to the 10 degree rule, the lifetime of the device is reduced by half for every 10 degrees rise in temperature, and therefore, the heat dissipation temperature seriously affects the performance and safety of the electronic device.
At present, the mainstream heat dissipation solution in intelligent electronic devices such as mobile phones and tablet computers is to use a high thermal conductivity graphite film as a main heat dissipation component, and the commercially available high thermal conductivity graphite film is prepared by using a polyimide film (abbreviated as PI film) as a raw material, sintering at a high temperature and rolling. The thicker the heat-conducting graphite film is, the higher the heat flux is, which is required by the heat dissipation application trend of electronic devices, but because the high heat-conducting graphite film is limited by the limitation of the raw material thickness of the PI film, the thicker the PI film is, the expansion and pulverization phenomenon is easy to occur in the high-temperature firing process, and the high-thickness graphite film with a complete structure cannot be obtained. Under the condition that the existing high-thickness PI film firing technology cannot be broken through at present, the high-thickness PI film is generally prepared by attaching double faced adhesive tapes between multiple layers of graphite films, for example, a 70-micron thick graphite film is prepared by attaching 5-micron double faced adhesive tapes between two layers of 32-micron graphite films, but the scheme has extremely low self thermal conductivity of a high-molecular adhesive, so that the transmission of upper and lower heat of the graphite film is influenced, and the thermal conductivity is greatly reduced.
The emerging graphene is a two-dimensional carbon nano-structure material formed by single-layer graphite sheets, the theoretical thermal conductivity can reach 5300W/m.K, and the graphene is an ideal heat dissipation material. At present, graphene oxide is mainly used as a main raw material for preparing a graphene heat dissipation film, and the preparation method comprises the following steps: the graphene oxide is dispersed in water to form graphene oxide dispersion liquid, then the graphene heat dissipation film is obtained through coating, drying, carbonization, graphitization and calendaring processes, however, in the coating process, graphene oxide slurry needs to be used as a flexible substrate base material of a release PET (polyethylene terephthalate) film or release paper, then the flexible substrate is removed after moisture drying treatment, but after the substrate is removed, the dried graphene oxide can only be cut into sheets to be fired because the flexibility of the film is insufficient, and the production efficiency is greatly reduced.
Therefore, how to prepare a graphene heat dissipation film which has high thickness, complete structure and high thermal conductivity and is suitable for large-scale coil firing is urgent.
Disclosure of Invention
The invention aims to provide a graphene heat dissipation film which is high in thickness, complete in structure, high in heat conductivity and suitable for large-scale coil firing and a preparation method thereof.
The technical scheme adopted by the invention for solving the technical problems is as follows: a preparation method of a graphene heat dissipation film comprises the following steps:
the method comprises the following steps: the heat-conducting graphite film semi-finished product is obtained by high-temperature firing heat treatment of the PI film with the conventional thickness, then needling treatment is carried out on the surface of the PI film to form fine pores, the PI film is a polyimide film, and the thickness of the PI film with the conventional thickness is generally 17-40 um.
Step two: carrying out strong acid oxidation and intercalation stripping on natural graphite micro-sheets or artificial graphite film waste by a Hummers method, washing with water, and carrying out acid-base neutralization treatment to obtain graphene oxide slurry;
step three: adding a dispersing agent, an adhesive and a defoaming agent into the graphene oxide slurry obtained in the step two, and uniformly stirring to obtain a graphene oxide slurry mixed solution;
step four: uniformly coating the graphene oxide slurry mixed solution obtained in the third step on the surface of the heat-conducting graphite film semi-finished product to obtain a graphene oxide composite film;
step five: dehydrating and drying the graphene oxide composite membrane obtained in the fourth step to obtain a dry graphene oxide composite membrane;
step six: rewinding the dried graphene oxide composite film obtained in the fifth step to obtain a graphene oxide composite film coiled material;
step seven: vertically placing the graphene oxide composite film coiled material obtained in the sixth step, respectively placing high-strength graphite pipes at the center and the outer ring of the graphene oxide composite film coiled material to support the graphene oxide composite film coiled material not to collapse, simultaneously ensuring that the graphene oxide coiled material is fully foamed in high-temperature graphitization, then performing decoking and graphene oxide reduction, and then performing high-temperature graphite crystallization treatment to obtain an expanded high-thickness graphene composite film coiled material;
step eight: and C, rolling the high-thickness graphene film coiled material obtained in the step seven to obtain a high-density high-thickness high-flexibility graphene heat dissipation film coiled material finished product.
Further, the method comprises the following steps: the temperature range in the first step is 2600-.
Further, the method comprises the following steps: the volume ratio of the graphene oxide slurry to the dispersant to the adhesive to the defoaming agent in the third step is (10-50) to (50-90): 0-1: 0-1, and the stirring speed in the third step is 100-3000 rpm.
Further, the method comprises the following steps: in the third step, the solid content of graphene oxide in the graphene oxide slurry mixed solution is 1-10 wt%, and the viscosity is 5000-.
Further, the method comprises the following steps: the temperature of the dehydration drying in the step five is 100-150 ℃.
Further, the method comprises the following steps: the temperature range of the decoking treatment and the graphene oxide reduction in the seventh step is 150-1200 ℃.
Further, the method comprises the following steps: the temperature range of the high-temperature graphite crystallization treatment in the seventh step is 1200-2800 ℃.
A graphene heat dissipation film prepared by the method of any one of claims 1-7.
Further, the method comprises the following steps: the graphene and heat conduction graphite film are arranged alternately.
Further, the method comprises the following steps: the graphene and the heat conduction graphite film are provided with a plurality of groups, and the adjacent groups of graphene and the heat conduction graphite film or graphene and graphene are jointed and connected.
The invention has the beneficial effects that: the invention overcomes the technical difficulty of the firing, expansion and pulverization of the existing high-thickness PI film; 2. the thickness of the graphene heat-dissipation film can be controlled by controlling the coating amount of the graphene oxide slurry mixed solution; 3. the step of removing the flexible substrate after coating the graphene oxide is realized, and the coiled material of the graphene heat dissipation film is fired by virtue of the flexibility of the heat-conducting graphite film.
Drawings
Fig. 1 is a schematic structural diagram of a graphene heat dissipation film in the first embodiment;
fig. 2 is a schematic structural diagram of a graphene heat dissipation film in the second embodiment;
fig. 3 is a schematic structural diagram of a graphene heat dissipation film in the third embodiment;
fig. 4 is a schematic structural diagram of a graphene heat dissipation film in the fourth embodiment;
fig. 5 is a schematic structural view of a graphene heat dissipation film in the fifth embodiment;
fig. 6 is a schematic structural view of a graphene heat dissipation film in the sixth embodiment;
labeled as: 1. graphene; 2. a thermally conductive graphite film;
Detailed Description
The invention is further described with reference to the following figures and detailed description.
A preparation method of a graphene heat dissipation film comprises the following steps:
the method comprises the following steps: carrying out high-temperature firing heat treatment on a PI film with a conventional thickness to obtain a semi-finished product of a heat-conducting graphite film, and carrying out needling treatment on the surface of the PI film to form fine pores, wherein the PI film is a polyimide film;
step two: carrying out strong acid oxidation and intercalation stripping on natural graphite micro-sheets or artificial graphite film waste by a Hummers method, washing with water, and carrying out acid-base neutralization treatment to obtain graphene oxide slurry;
step three: adding a dispersing agent, an adhesive and a defoaming agent into the graphene oxide slurry obtained in the second step, and uniformly stirring to obtain a graphene oxide slurry mixed solution, wherein the dispersing agent can be one or more of water, N-methyl pyrrolidone, N-dimethylformamide, polyvinyl alcohol, polyethylene glycol, ethylene glycol, xylene and acetone; the adhesive can be water-based acrylic resin, water-based epoxy resin or water-based bi-component polyurethane; the defoaming agent can be one or more of emulsified silicone oil, a higher alcohol fatty acid ester compound, polyoxyethylene polyoxypropylene pentaerythritol ether, polyoxyethylene polyoxypropylene amine ether, polyoxypropylene glycerol ether, polyoxypropylene polyoxyethylene glycerol ether and polydimethylsiloxane;
step four: uniformly coating the graphene oxide slurry mixed solution obtained in the third step on the surface of the heat-conducting graphite film semi-finished product to obtain a graphene oxide composite film, wherein the coating can adopt the processes of spraying, suspension coating, dip coating and the like, the graphene oxide slurry mixed solution can be coated on one side or two sides of the heat-conducting graphite film semi-finished product, and the coating thickness is adjusted by controlling the coating amount of the graphene oxide slurry mixed solution, so that graphene films with different thicknesses are prepared; in order to obtain the graphene heat dissipation film with high thickness to the maximum extent, the graphene film with the good coating can be laminated in multiple layers through a laminating machine;
step five: dehydrating and drying the graphene oxide composite membrane obtained in the fourth step to obtain a dry graphene oxide composite membrane;
step six: rewinding the dried graphene oxide composite film obtained in the fifth step to obtain a graphene oxide composite film coiled material, wherein a certain interlayer gap is reserved between layers of the graphene oxide composite film coiled material when rewinding is carried out, so that the graphene oxide composite film coiled material is prevented from being cracked due to expansion during heat treatment;
step seven: vertically placing the graphene oxide composite film coiled material obtained in the sixth step, respectively placing high-strength graphite pipes at the center and the outer ring of the graphene oxide composite film coiled material to support the graphene oxide composite film coiled material not to collapse, simultaneously ensuring that the graphene oxide coiled material is fully foamed in high-temperature graphitization, then performing decoking and graphene oxide reduction, and then performing high-temperature graphite crystallization treatment to obtain an expanded high-thickness graphene composite film coiled material;
step eight: and rolling the high-thickness graphene film coiled material obtained in the step seven to obtain a high-density high-thickness high-flexibility graphene heat dissipation film coiled material finished product, wherein the rolling mode can be high-pressure flat needling rolling or vacuum rolling.
On the basis of the above, the temperature range in the first step is 2600-.
On the basis, the volume ratio of the graphene oxide slurry, the dispersing agent, the adhesive and the defoaming agent in the third step is (10-50) to (50-90): 0-1: 0-1, the volumes of the adhesive and the defoaming agent are not zero, and the stirring speed in the third step is 100-3000 rpm.
On the basis, the solid content of the graphene oxide in the graphene oxide slurry mixed solution in the third step is 1-10 wt%, and the viscosity is 5000-.
On the basis, the temperature of the dehydration drying in the step five is 100-150 ℃.
On the basis, the temperature range of the decoking treatment and the graphene oxide reduction in the seventh step is 150-1200 ℃.
On the basis, the temperature range of the high-temperature graphite crystallization treatment in the seventh step is 1200-2800 ℃.
A graphene heat dissipation film prepared by the method of any one of claims 1-7.
On the basis, the graphene film comprises graphene 1 and heat conduction graphite films 2, wherein the graphene 1 and the heat conduction graphite films 2 are alternately arranged.
On the basis, the graphene 1 and the heat conduction graphite film 2 are provided with multiple groups, the adjacent groups of graphene 1 and the heat conduction graphite film 2 or the layers of the graphene 1 and the heat conduction graphite film 2 are jointed and connected, and the number of the layers of the graphene 1 and the heat conduction graphite film 2 can be set according to actual conditions.
The first embodiment is as follows: (as shown in FIG. 1)
The graphene heat dissipation film comprises a group of graphene 1 and a heat conduction graphite film 2.
Example two: (as shown in FIG. 2)
The graphene heat dissipation film comprises a heat conduction graphite film 2 and two graphene 1, wherein the heat conduction graphite film 2 is respectively attached to the two graphene 1.
Example three: (as shown in FIG. 3)
The graphene heat dissipation film comprises three groups of graphene 1 and a heat conduction graphite film 2, wherein the graphene 1 and the heat conduction graphite film 2 are arranged in a staggered mode.
Example four: (as shown in FIG. 4)
Graphene heat dissipation membrane includes four graphite alkene 1 and two heat conduction graphite membrane 2, and wherein two graphite alkene 1 set up in the outside, and two other graphite alkene 1 set up in the inboard and the laminating is connected, two heat conduction graphite membrane 2 sets up respectively between inboard graphite alkene 1 and outside graphite alkene 1.
Example five: (as shown in FIG. 5)
The graphene heat dissipation film comprises six groups of graphene 1 and heat conduction graphite films 2, wherein the graphene 1 and the heat conduction graphite films 2 are arranged in a staggered mode.
Example six: (as shown in FIG. 6)
The graphene heat dissipation film comprises six groups of graphene 1 and a heat conduction graphite film 2, wherein the three groups of graphene 1 and the heat conduction graphite film 2 are symmetrically arranged with the other three groups of graphene 1 and the other three groups of heat conduction graphite film 2, and the two graphene 1 in the middle are attached and connected.
Example seven:
a preparation method of a graphene heat dissipation film comprises the following steps:
the method comprises the following steps: carrying out high-temperature firing heat treatment at 2600 ℃ on the PI film with the conventional thickness to obtain a semi-finished product of the heat-conducting graphite film, and then carrying out needling treatment on the surface of the semi-finished product to form fine pores;
step two: carrying out strong acid oxidation and intercalation stripping on natural graphite micro-sheets or artificial graphite film waste by a Hummers method, washing with water, and carrying out acid-base neutralization treatment to obtain graphene oxide slurry;
step three: adding 50 parts of water, 0.1 part of water-based acrylic resin and 0.1 part of emulsified silicone oil into 10 parts of graphene oxide slurry, and uniformly stirring at the rotating speed of 100rpm to obtain a graphene oxide slurry mixed solution;
step four: uniformly spraying the graphene oxide slurry mixed solution obtained in the third step on the surface of the heat-conducting graphite film semi-finished product to obtain a graphene oxide composite film;
step five: slowly dehydrating and drying the graphene oxide composite membrane obtained in the fourth step at 100 ℃ to obtain a dried graphene oxide composite membrane;
step six: rewinding the dried graphene oxide composite film obtained in the fifth step to obtain a graphene oxide composite film coiled material, wherein a certain interlayer gap is reserved between layers when rewinding;
step seven: vertically placing the graphene oxide composite film coiled material obtained in the sixth step, respectively placing high-strength graphite pipes at the center and the outer ring of the graphene oxide composite film coiled material to support the graphene oxide composite film coiled material not to collapse, then performing decoking and graphene oxide reduction at a high temperature of 150 ℃, and then performing high-temperature graphite crystallization treatment at a high temperature of 1200 ℃ to obtain an expanded high-thickness graphene composite film coiled material;
step eight: and G, performing vacuum calendering on the high-thickness graphene film coiled material obtained in the step seven to obtain a high-density high-thickness high-flexibility graphene heat dissipation film coiled material finished product.
Example eight:
a preparation method of a graphene heat dissipation film comprises the following steps:
the method comprises the following steps: carrying out high-temperature firing heat treatment at 2750 ℃ on the PI film with the conventional thickness to obtain a semi-finished product of the heat-conducting graphite film, and then carrying out needling treatment on the surface of the semi-finished product to form fine pores;
step two: carrying out strong acid oxidation and intercalation stripping on natural graphite micro-sheets or artificial graphite film waste by a Hummers method, washing with water, and carrying out acid-base neutralization treatment to obtain graphene oxide slurry;
step three: adding 70 parts of N-methyl pyrrolidone, 0.5 part of water-based epoxy resin and 0.5 part of higher alcohol fatty acid ester compound into 30 parts of graphene oxide slurry, and uniformly stirring at the rotating speed of 1500rpm to obtain a graphene oxide slurry mixed solution;
step four: uniformly coating the graphene oxide slurry mixed solution obtained in the third step on the surface of the heat-conducting graphite film semi-finished product in a suspension manner to obtain a graphene oxide composite film;
step five: slowly dehydrating and drying the graphene oxide composite membrane obtained in the fourth step at 125 ℃ to obtain a dried graphene oxide composite membrane;
step six: rewinding the dried graphene oxide composite film obtained in the fifth step to obtain a graphene oxide composite film coiled material, wherein a certain interlayer gap is reserved between layers when rewinding;
step seven: vertically placing the graphene oxide composite film coiled material obtained in the sixth step, respectively placing high-strength graphite pipes at the center and the outer ring of the graphene oxide composite film coiled material to support the graphene oxide composite film coiled material not to collapse, then performing decoking and graphene oxide reduction at the high temperature of 800 ℃, and then performing high-temperature graphite crystallization treatment at the high temperature of 2000 ℃ to obtain an expanded high-thickness graphene composite film coiled material;
step eight: and F, performing high-pressure flat needling rolling on the high-thickness graphene film coiled material obtained in the step seven to obtain a high-density high-thickness high-flexibility graphene heat dissipation film coiled material finished product.
Example nine:
a preparation method of a graphene heat dissipation film comprises the following steps:
the method comprises the following steps: carrying out high-temperature firing heat treatment at 2900 ℃ on the PI film with the conventional thickness to obtain a semi-finished product of the heat-conducting graphite film, and then carrying out needling treatment on the surface of the semi-finished product of the heat-conducting graphite film to form fine pores;
step two: carrying out strong acid oxidation and intercalation stripping on natural graphite micro-sheets or artificial graphite film waste by a Hummers method, washing with water, and carrying out acid-base neutralization treatment to obtain graphene oxide slurry;
step three: adding 90 parts of polyethylene glycol, 1 part of waterborne epoxy resin and 1 part of polyoxyethylene polyoxypropylene pentaerythritol ether into 50 parts of graphene oxide slurry, and uniformly stirring at the rotating speed of 3000rpm to obtain graphene oxide slurry mixed liquor;
step four: uniformly dip-coating the graphene oxide slurry mixed solution obtained in the third step on the surface of the heat-conducting graphite film semi-finished product to obtain a graphene oxide composite film;
step five: slowly dehydrating and drying the graphene oxide composite membrane obtained in the fourth step at 150 ℃ to obtain a dried graphene oxide composite membrane;
step six: rewinding the dried graphene oxide composite film obtained in the fifth step to obtain a graphene oxide composite film coiled material, wherein a certain interlayer gap is reserved between layers when rewinding;
step seven: vertically placing the graphene oxide composite film coiled material obtained in the sixth step, respectively placing high-strength graphite pipes at the center and the outer ring of the graphene oxide composite film coiled material to support the graphene oxide composite film coiled material not to collapse, then performing decoking and graphene oxide reduction at a high temperature of 1200 ℃, and then performing high-temperature graphite crystallization treatment at a high temperature of 2800 ℃ to obtain an expanded high-thickness graphene composite film coiled material;
step eight: and G, performing vacuum calendering on the high-thickness graphene film coiled material obtained in the step seven to obtain a high-density high-thickness high-flexibility graphene heat dissipation film coiled material finished product.
The above-mentioned embodiments are intended to illustrate the objects, technical solutions and advantages of the present invention in further detail, and it should be understood that the above-mentioned embodiments are only exemplary embodiments of the present invention, and are not intended to limit the present invention, and any modifications, equivalents, improvements and the like made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A preparation method of a graphene heat dissipation film is characterized by comprising the following steps: the method comprises the following steps:
the method comprises the following steps: carrying out high-temperature firing heat treatment on the PI film with the conventional thickness to obtain a semi-finished product of the heat-conducting graphite film, and carrying out needling treatment on the surface of the semi-finished product to form fine pores;
step two: carrying out strong acid oxidation and intercalation stripping on natural graphite micro-sheets or artificial graphite film waste by a Hummers method, washing with water, and carrying out acid-base neutralization treatment to obtain graphene oxide slurry;
step three: adding a dispersing agent, an adhesive and a defoaming agent into the graphene oxide slurry obtained in the step two, and uniformly stirring to obtain a graphene oxide slurry mixed solution;
step four: uniformly coating the graphene oxide slurry mixed solution obtained in the third step on the surface of the heat-conducting graphite film semi-finished product to obtain a graphene oxide composite film;
step five: dehydrating and drying the graphene oxide composite membrane obtained in the fourth step to obtain a dry graphene oxide composite membrane;
step six: rewinding the dried graphene oxide composite film obtained in the fifth step to obtain a graphene oxide composite film coiled material;
step seven: vertically placing the graphene oxide composite film coiled material obtained in the sixth step, respectively placing high-strength graphite pipes at the center and the outer ring of the graphene oxide composite film coiled material to support the graphene oxide composite film coiled material not to collapse, then performing decoking and graphene oxide reduction, and then performing high-temperature graphite crystallization treatment to obtain an expanded high-thickness graphene composite film coiled material;
step eight: and C, rolling the high-thickness graphene film coiled material obtained in the step seven to obtain a high-density high-thickness high-flexibility graphene heat dissipation film coiled material finished product.
2. The method for preparing a graphene heat dissipation film according to claim 1, wherein the method comprises the following steps: the temperature range in the first step is 2600-.
3. The method for preparing a graphene heat dissipation film according to claim 1, wherein the method comprises the following steps: the volume ratio of the graphene oxide slurry to the dispersant to the adhesive to the defoaming agent in the third step is (10-50) to (50-90): (0-1): (0-1), the stirring speed in the third step is 100-3000 rpm.
4. The method for preparing a graphene heat dissipation film according to claim 1, wherein the method comprises the following steps: in the third step, the solid content of graphene oxide in the graphene oxide slurry mixed solution is 1-10 wt%, and the viscosity is 5000-.
5. The method for preparing a graphene heat dissipation film according to claim 1, wherein the method comprises the following steps: the temperature for dehydration and drying in the fifth step is 100-150 ℃.
6. The method for preparing a graphene heat dissipation film according to claim 1, wherein the method comprises the following steps: the temperature range of the decoking treatment and the graphene oxide reduction in the seventh step is 150-1200 ℃.
7. The method for preparing a graphene heat dissipation film according to claim 1, wherein the method comprises the following steps: the temperature range of the high-temperature graphite crystallization treatment in the seventh step is 1200-2800 ℃.
8. A graphite alkene heat dissipation membrane which characterized in that: prepared by the method of any one of claims 1 to 7.
9. The graphene heat spreading film according to claim 8, wherein: the graphene-based heat-conducting graphite film comprises graphene (1) and a heat-conducting graphite film (2), wherein the graphene (1) and the heat-conducting graphite film (2) are arranged alternately.
10. The graphene heat spreading film according to claim 9, wherein: the graphene (1) and the heat-conducting graphite film (2) are provided with multiple groups, and the adjacent groups of graphene (1) and the heat-conducting graphite film (2) or graphene (1) and graphene (1) are jointed and connected.
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