CN110540706A - Preparation method of heat-conducting interface material - Google Patents
Preparation method of heat-conducting interface material Download PDFInfo
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Abstract
The invention belongs to the technical field of heat conduction materials, and particularly relates to a preparation method of a heat conduction interface material. The invention discloses a preparation method of a heat-conducting interface material, which comprises the following steps: s1, stirring and mixing; s2, vacuum compaction and S3, banburying to obtain the material.
Description
Technical Field
The invention belongs to the technical field of heat conduction materials, and particularly relates to a preparation method of a heat conduction interface material.
Background
The continuous development of material science enables the application proportion of the heat conduction materials in national defense industry and civil materials to be increased year by year, the heat conduction materials with the characteristics of light weight, good mechanical property, strong electrical insulation, low price and the like become the trend of future development, and the heat conduction materials have wide application prospects in the rapid development of the electronic industry today. Electronic industry products such as LEDs, microelectronic packaging materials and semiconductor devices are continuously developing toward miniaturization, lightness, thinness and intellectualization, and thus people have made higher demands on the thermal conductivity of the materials.
The matrix as a heat-conducting material should have the following properties: the filler has good mechanical property and processing and forming property, and can realize high-quality fractional filling of the filler; good electrical insulation, higher thermal conductivity, low CTE and wide raw material source. The resins used for the heat conductive material are roughly classified into two types, thermosetting and thermoplastic. From the current state of research, the usual substrates are: HDPE, LDPE, PP, PS, PC, PA-6, PA-66, POM, PVC, PVDF; PU and SBS; epoxy, phenolic aldehyde, bismaleimide and modified resins thereof, organic silicon resin, silicon rubber, styrene butadiene rubber, PMR polyimide and other novel modified high-performance resins and the like. However, the heat conductivity of these substrates cannot meet the heat dissipation requirements of the existing electronic products, so that the preparation of high-performance heat-conducting interface materials is an urgent problem to be solved.
disclosure of Invention
in order to solve the above technical problems, a first aspect of the present invention provides a method for preparing a thermal interface material, comprising the following steps: s1, stirring and mixing; s2, vacuum compaction and S3, banburying to obtain the material.
As a preferred technical solution, the step of S1 stirring and mixing includes the following steps: carrying out planetary vacuum pumping stirring on the coupling agent and the rubber substrate at the stirring speed of 800-1300rpm for 1-10 min; adding metal filler, nitride, graphene and a cross-linking agent, performing planetary vacuum pumping stirring at the stirring speed of 800-1300rpm for 1-10 min.
As a preferable technical scheme, the vacuum degree in the step S1 is less than or equal to-0.1 MPa.
as a preferable technical proposal, the vacuum degree in the step S1 is-0.1 MPa.
As a preferred technical solution, the S2 vacuum compaction step includes the following steps: putting the mixture obtained in the step S1 into a vacuum drying oven, vacuumizing to less than or equal to-0.098 MPa, vacuumizing after 1-5 minutes, compacting the material in a vibration compactor, and repeating for at least one time; after the mixture is weighted, the mixture is put into a vacuum drying oven together for vacuumizing less than or equal to-0.098 MPa, and after 1-5 minutes, the mixture is vacuumized and repeated for at least one time.
As a preferred technical solution, the S2 vacuum compaction step includes the following steps: putting the mixture in the step S1 into a vacuum drying oven, vacuumizing to less than or equal to-0.098 MPa, vacuumizing after 1-5 minutes, compacting the material in a vibration compactor, and repeating for 1-5 times; pressing the mixture into a weight, putting the weight into a vacuum drying oven, vacuumizing to-0.098 MPa or below after 1-5 minutes, and repeating for 1-5 times.
As a preferable technical scheme, the force applied to the mixture by the weight is 100-500 kgf.
As a preferred solution, the force applied to the mixture by the weight is 300 kgf.
As a preferred technical solution, the S3 banburying step includes the following steps: banburying the compacted material for 5-15min at the temperature of 180-200 ℃ to obtain the material.
The second aspect of the invention provides a heat conduction material obtained by the preparation method.
Has the advantages that: the preparation method provided by the invention is simple to operate and easy to automate, and the prepared heat-conducting interface material has excellent heat-conducting property and can be well applied to heat dissipation in the field of electronic products.
Detailed Description
For purposes of the following detailed description, it is to be understood that the invention may assume various alternative variations and step sequences, except where expressly specified to the contrary. Moreover, other than in any operating examples, or where otherwise indicated, all numbers expressing, for example, quantities of ingredients used in the specification and claims are to be understood as being modified in all instances by the term "about". Accordingly, unless indicated to the contrary, the numerical parameters set forth in the following specification and attached claims are approximations that may vary depending upon the desired properties to be obtained by the present invention. At the very least, and not as an attempt to limit the application of the doctrine of equivalents to the scope of the claims, each numerical parameter should at least be construed in light of the number of reported significant digits and by applying ordinary rounding techniques.
In order to solve the above problems, the present invention provides a method for preparing a thermal interface material, comprising the following steps: s1, stirring and mixing; s2, vacuum compaction and S3, banburying to obtain the material.
Step S1
As a preferred embodiment, the S1 stirring and mixing step includes the following steps: carrying out planetary vacuum pumping stirring on the coupling agent and the rubber substrate at the stirring speed of 800-1300rpm for 1-10 min; adding metal filler, nitride, graphene and a cross-linking agent, performing planetary vacuum pumping stirring at the stirring speed of 800-1300rpm for 1-10 min;
Preferably, the S1 stirring and mixing step includes the following steps: carrying out planetary vacuum pumping stirring on the coupling agent and the rubber matrix at the stirring speed of 1000rpm for 5 min; adding metal filler, nitride, graphene and a cross-linking agent, and stirring at 1000rpm for 5min in a planetary vacuum pumping manner;
as a preferred embodiment, the degree of vacuum in the step S1 is ≦ 0.1 MPa.
As a preferred embodiment, the vacuum degree in the step S1 is-0.1 MPa.
The raw materials comprise the following specific components in parts by weight: 31-35 parts of rubber matrix, 35-39 parts of metal filler, 16-21 parts of nitride, 15-20 parts of graphene, 0.2-0.5 part of coupling agent and 0.1-1 part of cross-linking agent.
As a preferred embodiment, the raw materials comprise the following specific components in parts by weight: 33.5 parts of rubber matrix, 36.6 parts of metal filler, 20.5 parts of nitride, 17.8 parts of graphene, 0.3 part of coupling agent and 0.6 part of cross-linking agent.
as a preferred embodiment, the rubber matrix comprises at least one of natural rubber, isoprene rubber, styrene-butadiene rubber, fluororubber, silicone rubber, chloroprene rubber, ethylene-propylene-diene rubber, modified ethylene-propylene-diene rubber.
as a preferred embodiment, the rubber matrix comprises ethylene propylene diene monomer.
The ethylene propylene diene monomer is a copolymer of ethylene, propylene and a small amount of non-conjugated diene, the main chain of the ethylene propylene diene monomer consists of chemically stable saturated hydrocarbon, only unsaturated double bonds are contained in side chains, and the ethylene propylene diene monomer has excellent aging resistance such as ozone resistance, heat resistance, weather resistance and the like.
As a preferred embodiment, the Mooney viscosity of the ethylene-propylene-diene rubber is from 35 to 45. The Mooney viscosity is measured according to ASTM D-1646, temperature 125 ℃.
Preferably, the ethylene propylene diene monomer has a mooney viscosity of 40, model 3640, available from dupont dowii.
As a preferred embodiment, the rubber matrix further comprises polypropylene.
In the present application, the polypropylene is formed by propylene addition polymerization, is transparent and light in appearance, and is resistant to corrosion by acids, alkalis, salts and various organic solvents.
As a preferred embodiment, the polypropylene has a melt index of 1 to 3g/10 min.
Preferably, the polypropylene has a melt index of 1.9g/10 min.
in the present application, the melt index is tested with reference to the standard ASTM D1238, 230 degrees celsius/2.16 kg.
In the present application, the polypropylene is of type C133-02, available from DuPont Dow.
As a preferred embodiment, the weight ratio of the ethylene propylene diene monomer to the polypropylene is (0.8-1.1): 1.
preferably, the weight ratio of the ethylene propylene diene monomer to the polypropylene is 0.9: 1.
In the present application, the crosslinking agent is not particularly limited, and is dicumyl peroxide.
In one embodiment, the metal filler includes at least one of copper powder, aluminum powder, silver powder, iron powder, zinc powder, nickel powder, and tin powder.
In one embodiment, the metal filler is aluminum powder.
In a preferred embodiment, the metal filler is a spherical powder.
As a preferred embodiment, the metal filler has an average particle diameter of 1 to 70 μm; preferably, the metal filler has an average particle size of 5 to 40 microns;
As a preferred embodiment, the metal filler is composed of a metal filler having an average particle diameter of 5 to 15 micrometers and a metal filler having an average particle diameter of 30 to 50 micrometers;
Preferably, the weight ratio of the 5-15 micron metal filler to the 30-50 micron metal filler is (1-1.3): 1.
further preferably, the weight ratio of the 10 micron metal filler to the 40 micron metal filler is (1-1.3): 1.
Still more preferably, the weight ratio of the 10 micron metal filler to the 40 micron metal filler is 1.2: 1.
The metal filler forms a heat-conducting network structure on the rubber substrate, and improves the heat-conducting property of the rubber by means of free electrons and phonon vibration.
As a preferred embodiment, the nitride includes at least one of aluminum nitride, silicon nitride, magnesium nitride, titanium nitride, and tantalum nitride.
In a preferred embodiment, the nitride is aluminum nitride.
The aluminum nitride is a covalent bond compound, has a hexagonal wurtzite structure and is white or grey white, and Al atoms and adjacent N atoms form a divergent (AIN4) tetrahedron. AIN has the theoretical density of 3.269, the Mohs hardness of 7-8, the decomposition at 2200-. In addition, the aluminum nitride has the characteristic of being not corroded by aluminum and other molten metals and gallium arsenide, and also has excellent electrical insulation and dielectric properties.
In a preferred embodiment, the aluminum nitride is a spherical powder.
in a preferred embodiment, the aluminum nitride has an average particle size of 1 to 7 μm.
Preferably, the aluminum nitride has an average particle size of 5 microns.
the graphene is an inorganic non-metallic material, and the single-layer graphene is a two-dimensional allotrope of a carbon material, and the structure of the graphene is that single-layer carbon atoms are closely stacked to form a plane, and honeycomb six-membered ring periodic arrangement and stacking are presented. As can be seen from the layer of interatomic force, each carbon atom in the graphene is connected with three adjacent carbon atoms through a sigma bond, and three hybridization orbitals form strong chemical covalent bonds to form an sp2 hybridization structure and three 120-degree bond angles.
The graphene has a geometrical structure different from that of a metal material, so that the heat transfer mechanism is different, and graphene atoms form a lattice network with the atoms, so that heat transfer is performed through lattice vibration, heat conduction is realized by utilizing lattice wave vibration, and the lattice wave vibration is mainly generated through mutual restriction and mutual harmonic vibration of the atoms in the crystal structure.
In a preferred embodiment, the graphene has a sheet diameter of 1 to 10 μm.
Preferably, the sheet diameter of the graphene is 2-3 microns.
The graphene with the sheet diameter of 2-3 microns has a product number of 101457 and is purchased from Nanjing Xiancheng nanotechnology.
As a preferred embodiment, the coupling agent is a titanate coupling agent and/or a silane coupling agent.
as an example of a titanate coupling agent, there is included, but not limited to, isopropyl triisostearoyl titanate.
As a preferred embodiment, the silane coupling agent is selected from at least one of 1-vinyl-1, 1,3,3, 3-pentamethyldisiloxane, 1,3, 5-trivinyl-1, 1,3,5, 5-pentamethyltrisiloxane, vinyltris (dimethylsiloxy) silane, 1, 3-divinyltetraethoxydisiloxane, vinyltris (trimethylsiloxy) silane, vinyltrimethoxysilane, gamma-methacryloxypropyltrimethoxysilane.
As a preferred embodiment, the coupling agent is gamma-methacryloxypropyltrimethoxysilane.
Step S2
As a preferred embodiment, the S2 vacuum compaction step includes the following: putting the mixture obtained in the step S1 into a vacuum drying oven, vacuumizing to less than or equal to-0.098 MPa, vacuumizing after 1-5 minutes, compacting the material in a vibration compactor, and repeating for at least one time; after the mixture is weighted, the mixture is put into a vacuum drying oven together for vacuumizing less than or equal to-0.098 MPa, and after 1-5 minutes, the mixture is vacuumized and repeated for at least one time.
As a preferred embodiment, the S2 vacuum compaction step includes the following: putting the mixture in the step S1 into a vacuum drying oven, vacuumizing to-0.098 MPa, vacuumizing after 2 minutes, compacting the material in a vibration compactor, and repeating for 1-5 times; and (3) pressing the mixture into a heavy object, putting the mixture into a vacuum drying oven, vacuumizing to-0.098 MPa after 2 minutes, and repeating for 1-5 times.
in a preferred embodiment, the force applied to the mixture by the weight is 100 to 500 kgf.
As a preferred embodiment, the force applied to the mixture by the weight is 300 kgf.
Step S3
as a preferred embodiment, the S3 banburying step includes the following steps: banburying the compacted material for 5-15min at the temperature of 180-200 ℃ to obtain the material.
As a preferred embodiment, the S3 banburying step includes the following steps: banburying the compacted material at 190 deg.C for 10 min.
the second aspect of the invention provides a heat conduction material obtained by the preparation method.
As a preferred embodiment, the preparation method of the thermal interface material comprises the following steps:
S1, performing planetary vacuum pumping stirring on the coupling agent and the rubber substrate at the stirring speed of 800-1300rpm for 1-10 min; adding metal filler, nitride, graphene and a cross-linking agent, performing planetary vacuum pumping stirring at the stirring speed of 800-1300rpm for 1-10 min;
S2, placing the mixture obtained in the step S1 into a vacuum drying box, vacuumizing to be less than or equal to-0.098 MPa, vacuumizing after 1-5 minutes, compacting the material in a vibration compactor, and repeating for at least one time; after the mixture is weighted, the mixture is put into a vacuum drying oven together for vacuum pumping until the pressure is less than or equal to-0.098 MPa, and after 1-5 minutes, the mixture is put into vacuum for at least one time.
S3, banburying the compacted material for 5-15min at the temperature of 180-200 ℃ to obtain the material.
The applicant carries out internal mixing after planetary vacuum pumping stirring and applying a force of 100-500kgf in the process of compacting, so that the compatibility of the inorganic filler and the polypropylene/ethylene propylene diene monomer rubber is improved, and the interface adhesive force is improved; meanwhile, a network which is mutually penetrated is formed among the graphene, the metal filler, the nitride and the polypropylene/ethylene propylene diene monomer, and the structure degree of the formed heat-conducting network is increased through continuously optimizing the process, so that the heat-conducting property of the rubber material is improved.
The second aspect of the invention provides a heat-conducting interface material obtained by the preparation method.
The interface material is used for heat dissipation of electronic products.
The electronic products include watches, smart phones, telephones, televisions, video disc players (VCD, SVCD, DVD), video recorders, camcorders, radios, radio cassettes, combination speakers, compact disc players (CD), computers, game machines, and the like.
The present invention will be specifically described below by way of examples. It should be noted that the following examples are only for illustrating the present invention and should not be construed as limiting the scope of the present invention, and that the insubstantial modifications and adaptations of the present invention by those skilled in the art based on the above disclosure are still within the scope of the present invention.
In addition, the starting materials used are all commercially available, unless otherwise specified.
examples
Example 1
A preparation method of a heat-conducting interface material comprises the following steps:
S1, carrying out planetary vacuum pumping stirring on a coupling agent and a rubber matrix at the stirring speed of 1000rpm for 5 min; adding metal filler, nitride, graphene and a cross-linking agent, and performing planetary vacuum pumping stirring at the stirring speed of 1000rpm for 5min under the vacuum degree of-0.1 MPa;
S2, putting the mixture obtained in the step S1 into a vacuum drying box, vacuumizing to-0.098 MPa, vacuumizing after 2 minutes, compacting the material in a vibration compactor, and repeating for 3 times; and (3) pressing the mixture into a weight, putting the weight mixture into a vacuum drying oven, vacuumizing to-0.098 MPa after 2 minutes, and repeating the steps for 3 times.
And S3, banburying the compacted material at 190 ℃ for 10min to obtain the material.
In step S2, the force applied to the mixture by the weight is 300 kgf.
The raw materials comprise the following specific components in parts by weight: 33.5 parts of rubber matrix, 36.6 parts of metal filler, 20.5 parts of nitride, 17.8 parts of graphene, 0.3 part of coupling agent and 0.6 part of cross-linking agent.
The rubber matrix comprises ethylene propylene diene monomer and polypropylene; the melt index of the polypropylene is 1.9g/10min, the model of the polypropylene is C133-02, and the polypropylene is purchased from DuPont Dow. The ethylene propylene diene monomer has a Mooney viscosity of 40 and a model number of 3640, and is purchased from Dupont Dow. The weight ratio of the ethylene propylene diene monomer to the polypropylene is 0.9: 1.
the metal filler is aluminum powder, and the metal filler is composed of aluminum powder with the average particle size of 10 micrometers and aluminum powder with the average particle size of 40 micrometers; the weight ratio of the 10-micron aluminum powder to the 40-micron aluminum powder is 1.2: 1.
The nitride is aluminum nitride, and the average grain diameter of the aluminum nitride is 5 microns.
The graphene is 2-3 microns in sheet diameter, 101457 in product number, and is purchased from Nanjing Xiancheng nanotechnology.
The cross-linking agent is dicumyl peroxide.
Example 2
A preparation method of a heat-conducting interface material comprises the following steps:
S1, carrying out planetary vacuum pumping stirring on a coupling agent and a rubber matrix at the stirring speed of 800rpm for 10 min; adding metal filler, nitride, graphene and a cross-linking agent, and performing planetary vacuum pumping stirring at the stirring speed of 800rpm for 10min under the vacuum degree of-0.1 MPa;
S2, putting the mixture obtained in the step S1 into a vacuum drying box, vacuumizing to-0.098 MPa, vacuumizing after 5 minutes, compacting the material in a vibration compactor, and repeating for 3 times; pressing the mixture into a weight, putting the mixture into a vacuum drying oven, vacuumizing to-0.098 MPa, vacuumizing after 5 minutes, and repeating for 3 times.
and S3, banburying the compacted material for 5min at 200 ℃ to obtain the material.
In step S2, the force applied to the mixture by the weight is 100 kgf.
The raw materials comprise the following specific components in parts by weight: 31 parts of rubber matrix, 35 parts of metal filler, 16 parts of nitride, 15 parts of graphene, 0.2 part of coupling agent and 0.1 part of cross-linking agent.
The specific components of the starting materials are the same as in example 1.
Example 3
a preparation method of a heat-conducting interface material comprises the following steps:
S1, carrying out planetary vacuum pumping stirring on a coupling agent and a rubber matrix at the stirring speed of 1300rpm for 1 min; adding metal filler, nitride, graphene and a cross-linking agent, and performing planetary vacuum pumping stirring at the stirring speed of 1300rpm for 1min under the vacuum degree of-0.1 MPa;
S2, putting the mixture obtained in the step S1 into a vacuum drying box, vacuumizing to-0.098 MPa, vacuumizing after 1 minute, compacting the material in a vibration compactor, and repeating for 5 times; and (3) pressing the mixture into a weight, putting the weight mixture into a vacuum drying oven, vacuumizing to-0.098 MPa after 1 minute, and repeating for 5 times.
And S3, banburying the compacted material for 15min at 180 ℃ to obtain the material.
In step S2, the force applied to the mixture by the weight is 100 kgf.
The raw materials comprise the following specific components in parts by weight: comprises the following components: 35 parts of rubber matrix, 39 parts of metal filler, 21 parts of nitride, 20 parts of graphene, 0.5 part of coupling agent and 1 part of cross-linking agent.
The specific components of the starting materials are the same as in example 1.
Example 4
A preparation method of a heat-conducting interface material comprises the following steps:
S1, carrying out planetary stirring on a coupling agent and a rubber matrix at the stirring speed of 1000rpm for 5 min; adding metal filler, nitride, graphene and a cross-linking agent, stirring at the stirring speed of 1000rpm for 5 min;
S2, putting the mixture obtained in the step S1 into a vacuum drying box, vacuumizing to-0.098 MPa, vacuumizing after 2 minutes, compacting the material in a vibration compactor, and repeating for 3 times; and (3) pressing the mixture into a weight, putting the weight mixture into a vacuum drying oven, vacuumizing to-0.098 MPa after 2 minutes, and repeating the steps for 3 times.
And S3, banburying the compacted material at 190 ℃ for 10min to obtain the material.
In step S2, the force applied to the mixture by the weight is 300 kgf.
The specific components and parts by weight of the raw materials are the same as those in example 1.
Example 5
a preparation method of a heat-conducting interface material comprises the following steps:
S1, carrying out planetary stirring on a coupling agent and a rubber matrix at the stirring speed of 1000rpm for 5 min; adding metal filler, nitride, graphene and a cross-linking agent, stirring at the stirring speed of 1000rpm for 5 min;
S2, putting the mixture obtained in the step S1 into a vacuum drying box, vacuumizing to-0.098 MPa, vacuumizing after 2 minutes, compacting the material in a vibration compactor, and repeating for 10 times; and (3) pressing the mixture into a weight, putting the weight mixture into a vacuum drying oven, vacuumizing to-0.098 MPa after 2 minutes, and repeating for 10 times.
and S3, banburying the compacted material at 190 ℃ for 10min to obtain the material.
In step S2, the force applied to the mixture by the weight is 300 kgf.
The specific components and parts by weight of the raw materials are the same as those in example 1.
Example 6
A preparation method of a heat-conducting interface material comprises the following steps:
S1, carrying out planetary stirring on a coupling agent and a rubber matrix at the stirring speed of 1000rpm for 5 min; adding metal filler, nitride, graphene and a cross-linking agent, stirring at the stirring speed of 1000rpm for 5 min;
S2, putting the mixture obtained in the step S1 into a vacuum drying box, vacuumizing to-0.098 MPa, vacuumizing after 2 minutes, compacting the material in a vibration compactor, and repeating for 3 times; then the mixture is put into a vacuum drying oven to be vacuumized to-0.098 MPa, and the vacuum drying oven is put into the vacuum drying oven to be vacuumized after 2 minutes, and the process is repeated for 3 times.
And S3, banburying the compacted material at 190 ℃ for 10min to obtain the material.
the specific components and parts by weight of the raw materials are the same as those in example 1.
example 7
A preparation method of a heat-conducting interface material comprises the following steps:
S1, carrying out planetary stirring on a coupling agent and a rubber matrix at the stirring speed of 1000rpm for 5 min; adding metal filler, nitride, graphene and a cross-linking agent, stirring at the stirring speed of 1000rpm for 5 min;
s2, putting the mixture obtained in the step S1 into a vacuum drying box, vacuumizing to-0.098 MPa, vacuumizing after 2 minutes, compacting the material in a vibration compactor, and repeating for 3 times; and (3) pressing the mixture into a weight, putting the weight mixture into a vacuum drying oven, vacuumizing to-0.098 MPa after 2 minutes, and repeating the steps for 3 times.
And S3, banburying the compacted material at 190 ℃ for 10min to obtain the material.
In step S2, the weight applies a force of 1000kgf to the mixture.
The specific components and parts by weight of the raw materials are the same as those in example 1.
Performance testing
coefficient of thermal conductivity: test methods refer to standard astm d5470, unit: W/(m.K)
TABLE 1
| Examples | Coefficient of thermal conductivity |
| Example 1 | 26 |
| Example 2 | 23 |
| Example 3 | 24 |
| Example 4 | 14 |
| Example 5 | 19 |
| Example 6 | 13 |
| Example 7 | 15 |
the above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in other forms, and any person skilled in the art may modify or change the technical content of the above disclosure into equivalent embodiments with equivalent changes, but all those simple modifications, equivalent changes and modifications made to the above embodiments according to the technical spirit of the present invention still belong to the protection scope of the present invention.
Claims (10)
1. A preparation method of a heat conduction interface material is characterized by comprising the following steps: s1, stirring and mixing; s2, vacuum compaction and S3, banburying to obtain the material.
2. The method of claim 1, wherein the S1 stirring and mixing step comprises the following steps: carrying out planetary vacuum pumping stirring on the coupling agent and the rubber substrate at the stirring speed of 800-1300rpm for 1-10 min; adding metal filler, nitride, graphene and a cross-linking agent, performing planetary vacuum pumping stirring at the stirring speed of 800-1300rpm for 1-10 min.
3. The method of claim 2, wherein the vacuum in step S1 is ≦ 0.1 MPa.
4. the method according to claim 3, wherein the degree of vacuum in step S1 is-0.1 MPa.
5. The method of claim 1, wherein the S2 vacuum compaction step comprises the following: putting the mixture obtained in the step S1 into a vacuum drying oven, vacuumizing to less than or equal to-0.098 MPa, vacuumizing after 1-5 minutes, compacting the material in a vibration compactor, and repeating for at least one time; after the mixture is weighted, the mixture is put into a vacuum drying oven together for vacuum pumping until the pressure is less than or equal to-0.098 MPa, and after 1-5 minutes, the mixture is put into vacuum for at least one time.
6. The method of claim 5, wherein the S2 vacuum compaction step comprises the following: putting the mixture in the step S1 into a vacuum drying oven, vacuumizing to less than or equal to-0.098 MPa, vacuumizing after 1-5 minutes, compacting the material in a vibration compactor, and repeating for 1-5 times; pressing the mixture into a weight, putting the weight into a vacuum drying oven, vacuumizing to-0.098 MPa or below after 1-5 minutes, and repeating for 1-5 times.
7. The method of claim 5 or 6, wherein the weight applies a force of 100 to 500kgf to the mixture.
8. The method of claim 7, wherein the force applied to the mixture by the weight is 300 kgf.
9. The method of claim 7, wherein the S3 banburying step comprises the following steps: banburying the compacted material for 5-15min at the temperature of 180-200 ℃ to obtain the material.
10. A thermally conductive material obtained by the production method according to any one of claims 1 to 9.
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