CN115322749A - Hexagonal boron nitride-vanadium dioxide composite material and preparation method and application thereof - Google Patents
Hexagonal boron nitride-vanadium dioxide composite material and preparation method and application thereof Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 89
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 title claims abstract description 80
- 229910052796 boron Inorganic materials 0.000 title claims abstract description 80
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- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
- C09K5/02—Materials undergoing a change of physical state when used
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/0066—Use of inorganic compounding ingredients
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/28—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof by elimination of a liquid phase from a macromolecular composition or article, e.g. drying of coagulum
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2201/00—Foams characterised by the foaming process
- C08J2201/04—Foams characterised by the foaming process characterised by the elimination of a liquid or solid component, e.g. precipitation, leaching out, evaporation
- C08J2201/048—Elimination of a frozen liquid phase
- C08J2201/0484—Elimination of a frozen liquid phase the liquid phase being aqueous
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2301/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
- C08J2301/08—Cellulose derivatives
- C08J2301/26—Cellulose ethers
- C08J2301/28—Alkyl ethers
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
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Abstract
The application relates to the technical field of heat-conducting composite materials, in particular to a hexagonal boron nitride-vanadium dioxide composite material and a preparation method and application thereof. The preparation method of the hexagonal boron nitride-vanadium dioxide composite material comprises the following steps: dispersing hexagonal boron nitride, vanadium dioxide, a silane coupling agent and a dispersing agent in water to obtain a precursor solution; and preparing the precursor solution into the hexagonal boron nitride-vanadium dioxide composite material with an oriented arrangement structure by adopting an ice template method. The hexagonal boron nitride-vanadium dioxide composite material prepared by the ice template method is an aerogel material which directionally grows along with the growth direction of ice crystals and has an ordered arrangement mode, and the hexagonal boron nitride-vanadium dioxide composite material improves the heat conduction performance through a porous structure which is arranged in an oriented mode, so that the hexagonal boron nitride-vanadium dioxide composite material can be used as a filler template and silicon rubber to be compounded as a phase-change heat conduction interface material, and has a good application prospect.
Description
Technical Field
The application belongs to the technical field of heat-conducting composite materials, and particularly relates to a hexagonal boron nitride-vanadium dioxide composite material and a preparation method and application thereof.
Background
Hexagonal boron nitride (hBN) is an excellent insulating and heat conducting material with excellent electrical insulation, thermal conductivity, chemical and thermal stability as a heat conducting material. Vanadium dioxide as an inorganic reversible phase change material can generate metal-insulation phase change at the phase change temperature, and has the advantages of stable performance and difficult deformation. Vanadium dioxide is adsorbed on the hexagonal boron nitride nanosheet to form the phase-change heat-conducting composite filler of hexagonal boron nitride-vanadium dioxide, and meanwhile, the phase-change heat-storage composite filler has high-efficiency heat dissipation and phase-change heat storage capacities, and meanwhile, due to the metal-insulation phase change of the vanadium dioxide, an electron-phonon coupling high-efficiency heat dissipation channel is added, so that the heat conduction capacity of the composite filler is further improved.
Thermal interface materials are widely used in the field of electronic packaging and play an indispensable role. The thermal interface material is used as an electronic heat dissipation material and is mainly filled between the chip and the soaking piece, so that the thermal interface material is used for reducing the interface thermal resistance and improving the heat dissipation performance of the chip. The technical scheme for preparing the thermal interface material at present mainly comprises the following steps: 1) The high heat conduction filler is added into the resin matrix in disorder to form a thermal interface material; the thermal interface material obtained in the mode has the advantages of high interface thermal resistance, poor heat dissipation capability and high required filler volume ratio; 2) The high heat conduction filler is orderly added into the resin matrix to form a thermal interface material; the thermal interface material obtained in the mode has the advantages of small interface thermal resistance, good heat dissipation capacity and small volume ratio of required fillers, but the capacity of eliminating the hot spot of the chip is still limited; 3) The high-heat-conductivity filler is added into the phase-change organic matrix, and the high-heat-conductivity filler is softened during heating to improve the contact area and reduce the interface thermal resistance; the thermal interface material obtained in such a way can reduce the interface thermal resistance, but has the risk of oil spilling, and the capacity of eliminating the hot spot of the chip is still limited. When the hexagonal boron nitride-vanadium dioxide composite material is used as a thermal interface material, the corresponding heat conducting property of the material is still to be mentioned.
Disclosure of Invention
The application aims to provide a hexagonal boron nitride-vanadium dioxide composite material, and a preparation method and application thereof, and aims to solve the technical problem of how to improve the thermal conductivity of the hexagonal boron nitride-vanadium dioxide composite material.
In order to achieve the purpose of the application, the technical scheme adopted by the application is as follows:
in a first aspect, the present application provides a method for preparing a hexagonal boron nitride-vanadium dioxide composite material, comprising:
dispersing hexagonal boron nitride, vanadium dioxide, a silane coupling agent and a dispersing agent in water to obtain a precursor solution;
and preparing the precursor solution into the hexagonal boron nitride-vanadium dioxide composite material with an oriented arrangement structure by adopting an ice template method.
In one embodiment, the mass ratio of the hexagonal boron nitride to the vanadium dioxide to the silane coupling agent to the dispersing agent is (4-12) to (1-3) to (0.1-0.3) to (0.01-0.03); and/or the presence of a gas in the atmosphere,
the mass volume ratio of the hexagonal boron nitride to the water is (4-12) g, (20-60) mL.
In one embodiment, the method for preparing the aerogel material with an orientation arrangement structure from the precursor solution by using an ice template method comprises the following steps: and (3) defoaming the precursor solution, and then performing liquid nitrogen freeze drying treatment.
In one embodiment, the liquid nitrogen freeze drying process comprises: freezing in liquid nitrogen at-190 deg.c to-200 deg.c for 30-45 min, and drying in a freeze drier under 0.5-1.5 Pa vacuum degree for 10-14 hr.
In one embodiment, the silane coupling agent is selected from at least one of a vinyl silane coupling agent, an aminosilane coupling agent, and a methacryloxy silane coupling agent; and/or the presence of a gas in the gas,
the dispersant is at least one selected from cellulose, carboxymethyl cellulose, hydroxyethyl cellulose, hydroxypropyl methyl cellulose and sodium hydroxymethyl cellulose.
In one embodiment, the method of making further comprises: and (3) placing the hexagonal boron nitride-vanadium dioxide composite material with the orientation arrangement structure in polysiloxane for dipping treatment, and then curing treatment.
In one embodiment, the polysiloxane is selected from at least one of polydimethylsiloxane, polymethylvinylsiloxane, and polymethylphenylvinylsiloxane.
In one embodiment, the curing process comprises: precuring for 0.5 to 1 hour at the temperature of between 50 and 70 ℃, and then curing for 1.5 to 2.5 hours at the temperature of between 110 and 130 ℃.
In a second aspect, the application provides a hexagonal boron nitride-vanadium dioxide composite material, which is prepared by the preparation method of the application.
In a third aspect, the application provides an application of the hexagonal boron nitride-vanadium dioxide composite material prepared by the preparation method of the application as a thermal interface material.
According to the preparation method of the hexagonal boron nitride-vanadium dioxide composite material provided by the first aspect of the application, the ice template method is adopted to prepare the precursor solution containing the hexagonal boron nitride, the vanadium dioxide, the silane coupling agent and the dispersing agent into the hexagonal boron nitride-vanadium dioxide composite material with the oriented arrangement structure, the hexagonal boron nitride-vanadium dioxide composite material prepared by the ice template method is an aerogel material which directionally grows along with the growth direction of ice crystals and has an ordered arrangement mode, and the hexagonal boron nitride-vanadium dioxide composite material improves the heat conduction performance through the oriented arrangement porous structure, so that the hexagonal boron nitride-vanadium dioxide composite material can be used as a filler template and silicon rubber to be compounded as a phase-change heat conduction interface material, and has a good application prospect.
The hexagonal boron nitride-vanadium dioxide composite material provided by the second aspect of the application is prepared by the preparation method, and based on the characteristics of the preparation method, the hexagonal boron nitride-vanadium dioxide composite material provided by the application is an aerogel material which directionally grows along with the growth direction of ice crystals and has an ordered arrangement mode, and the hexagonal boron nitride-vanadium dioxide composite material improves the heat conduction performance through a porous structure in oriented arrangement, so that the hexagonal boron nitride-vanadium dioxide composite material can be used as a phase-change heat conduction interface material to be compounded with silicon rubber as a filler template, and has a good application prospect.
According to the third aspect of the application, the hexagonal boron nitride-vanadium dioxide composite material prepared by the ice template method has a highly ordered arrangement mode, and the porous structures arranged in an oriented mode can form high heat dissipation channels, so that the heat conduction performance is improved, and therefore, a thermal interface material with better heat conduction performance can be prepared, and the material can be well applied between a chip and a soaking plate.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present application, the drawings required for the embodiments or the prior art descriptions will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present application, and it is obvious for those skilled in the art to obtain other drawings without creative efforts.
FIG. 1 is a diagram of the appearance of a hexagonal boron nitride-vanadium dioxide composite material provided by an embodiment of the present application;
fig. 2 is an appearance diagram of the hexagonal boron nitride-vanadium dioxide composite material and silicone rubber provided in the embodiment of the present application after being compounded.
Detailed Description
In order to make the technical problems, technical solutions and advantageous effects to be solved by the present application more clearly apparent, the present application is further described in detail below with reference to the embodiments. It should be understood that the specific embodiments described herein are merely illustrative of and not restrictive on the broad application.
In this application, the term "and/or" describes an association relationship of associated objects, meaning that there may be three relationships, e.g., a and/or B, which may mean: a alone, A and B together, and B alone. Wherein A and B can be singular or plural. The character "/" generally indicates that the former and latter associated objects are in an "or" relationship.
In the present application, "at least one" means one or more, "plural" means two or more. "at least one of the following" or similar expressions refer to any combination of these items, including any combination of the singular or plural items.
It should be understood that, in various embodiments of the present application, the sequence numbers of the above-mentioned processes do not mean the execution sequence, some or all of the steps may be executed in parallel or executed sequentially, and the execution sequence of each process should be determined by its function and inherent logic, and should not constitute any limitation to the implementation process of the embodiments of the present application.
The terminology used in the embodiments of the present application is for the purpose of describing particular embodiments only and is not intended to be limiting of the application. As used in the examples of this application and the appended claims, the singular forms "a", "an", and "the" are intended to include the plural forms as well, unless the context clearly indicates otherwise.
The weight of the related components mentioned in the description of the embodiments of the present application may not only refer to the specific content of each component, but also represent the proportional relationship of the weight among the components, and therefore, the content of the related components is scaled up or down within the scope disclosed in the description of the embodiments of the present application as long as it is scaled up or down according to the description of the embodiments of the present application. Specifically, the mass described in the specification of the examples of the present application may be a mass unit known in the chemical field such as μ g, mg, g, kg, etc.
The terms "first" and "second" are used for descriptive purposes only and are used for distinguishing purposes such as substances from one another and are not to be construed as indicating or implying relative importance or to implicitly indicate the number of technical features indicated. For example, a first XX may also be referred to as a second XX, and similarly, a second XX may also be referred to as a first XX, without departing from the scope of embodiments of the present application. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature.
The first aspect of the embodiments of the present application provides a method for preparing a hexagonal boron nitride-vanadium dioxide composite material, including the following steps:
s01: dispersing hexagonal boron nitride, vanadium dioxide, a silane coupling agent and a dispersing agent in water to obtain a precursor solution;
s02: and preparing the precursor solution into the hexagonal boron nitride-vanadium dioxide composite material with an oriented arrangement structure by adopting an ice template method.
According to the preparation method of the hexagonal boron nitride-vanadium dioxide composite material provided by the embodiment of the application, the precursor solution containing the hexagonal boron nitride, the vanadium dioxide, the silane coupling agent and the dispersing agent is prepared into the hexagonal boron nitride-vanadium dioxide composite material with an oriented arrangement structure by adopting an ice template method, specifically, the silane coupling agent can modify the hexagonal boron nitride, so that the vanadium dioxide is better compounded on the hexagonal boron nitride, the hexagonal boron nitride-vanadium dioxide composite material has high-efficiency heat dissipation and phase change heat storage capacities simultaneously, the vanadium dioxide phase change material is provided with an electron-phonon coupling high-efficiency heat dissipation channel, so that the heat conduction capacity of the composite material is further improved, the dispersing agent can enable the precursor solution to be uniformly dispersed, and the uniformly dispersed precursor solution can directionally grow along with the ice crystal growth direction by using the ice template method to generate the aerogel material with an ordered arrangement mode.
In the step S01, the hexagonal boron nitride with the heat conduction function is a hexagonal boron nitride nanosheet, and the vanadium dioxide with the reversible phase change function is granular, so that the vanadium dioxide can be well compounded on the surface of the hexagonal boron nitride nanosheet. And the silane coupling agent can modify the surface of the hexagonal boron nitride nanosheet, so that the granular vanadium dioxide can be better adsorbed.
In one embodiment, the silane coupling agent is selected from at least one of a vinyl silane coupling agent, an aminosilane coupling agent, and a methacryloxy silane coupling agent; the silane coupling agent can well modify hexagonal boron nitride nanosheets. Further, the dispersant is at least one selected from the group consisting of cellulose, carboxymethyl cellulose, hydroxyethyl cellulose, hydroxypropyl methyl cellulose, and sodium hydroxymethyl cellulose. The dispersing agent can uniformly disperse the precursor solution.
In one embodiment, the mass ratio of the hexagonal boron nitride to the vanadium dioxide to the silane coupling agent to the dispersant is (4-12) to (1-3) to (0.1-0.3) to (0.01-0.03); specifically, the amount of hexagonal boron nitride can be 4-12 g, the amount of vanadium dioxide can be 1-3 g, the amount of silane coupling agent can be 0.1-0.3 g, and the amount of dispersant can be 0.01-0.03 g; furthermore, the mass volume ratio of the hexagonal boron nitride to the water is (4-12) g (20-60) mL. Under the condition of the proportion, the hexagonal boron nitride-vanadium dioxide composite material with the oriented arrangement structure can be generated through full reaction.
In the step S02, the step of preparing the aerogel material with the oriented arrangement structure from the precursor solution by adopting an ice template method comprises the following steps: and (3) defoaming the precursor solution, and then carrying out liquid nitrogen freeze drying treatment.
The ice template method is to utilize the orientation of ice crystal growth under temperature gradient and to form the oriented porous template of the heat conducting stuffing through fast pre-freezing and freeze drying of the precursor solution so as to produce oriented thermal interface material. Specifically, treating the precursor solution for 5-10 minutes by using a cell crushing instrument to obtain a uniform precursor solution, then placing the precursor solution into a high-speed mixer for defoaming treatment, and pouring the precursor solution into a cylindrical mold; freezing the dispersion liquid filled into the mold by using liquid nitrogen, and drying the precursor solution in a freeze dryer after the precursor solution is completely frozen to obtain hBN-VO of the aerogel material 2 A composite material.
In one embodiment, the liquid nitrogen freeze drying process comprises: freezing in liquid nitrogen at-190 deg.c to-200 deg.c for 30-45 min, and drying in a freeze drier under 0.5-1.5 Pa vacuum degree for 10-14 hr. For example, it is first frozen in liquid nitrogen at-196 ℃ for 45min and then dried in a freeze-dryer under a vacuum of 1.0Pa for 12h. The aerogel material with the ordered arrangement mode can be better generated under the conditions.
In one embodiment, the method of making further comprises: and (3) placing the hexagonal boron nitride-vanadium dioxide composite material with the orientation arrangement structure in polysiloxane for dipping treatment, and then curing treatment. Therefore, the hexagonal boron nitride-vanadium dioxide composite material can be filled in the silicon rubber and used for preparing a thermal interface material.
Further, the polysiloxane is selected from at least one of polydimethylsiloxane, polymethylvinylsiloxane and polymethylphenylvinylsiloxane. When the polysiloxane is selected from polydimethylsiloxane, the hexagonal boron nitride-vanadium dioxide-dimethyl silicone rubber composite thermal interface material can be generated, when the polysiloxane is selected from polymethylvinylsiloxane, the hexagonal boron nitride-vanadium dioxide-methyl vinyl silicone rubber composite thermal interface material can be generated, and when the polysiloxane is selected from polymethylphenylvinylsiloxane, the hexagonal boron nitride-vanadium dioxide-methyl phenyl vinyl silicone rubber composite thermal interface material can be generated.
Furthermore, the hexagonal boron nitride-vanadium dioxide composite material with the orientation arrangement structure is placed in polysiloxane for dipping treatment for 6-12 h, so that the liquid polysiloxane can be fully dipped in the hexagonal boron nitride-vanadium dioxide composite material in the form of aerogel. The subsequent curing treatment comprises: pre-curing for 0.5-1 h at 50-70 ℃, and then curing for 1.5-2.5 h at 110-130 ℃. This is sufficient to cure the polysiloxane to form a silicone rubber.
Further, a curing agent (for example, platinum catalyst) may be added to the polysiloxane in an amount of 8 to 12% by mass.
In a second aspect of the embodiments of the present application, a hexagonal boron nitride-vanadium dioxide composite material is provided, and is prepared by the preparation method of the present application.
The hexagonal boron nitride-vanadium dioxide composite material provided by the embodiment of the application is prepared by the preparation method provided by the embodiment of the application, and based on the characteristics of the preparation method provided by the embodiment of the application, the hexagonal boron nitride-vanadium dioxide composite material provided by the application is an aerogel material which directionally grows along with the growth direction of ice crystals and has an ordered arrangement mode, and the hexagonal boron nitride-vanadium dioxide composite material has improved heat conduction performance through a porous structure which is arranged in an oriented way, so that the hexagonal boron nitride-vanadium dioxide composite material can be used as a phase-change heat-conduction interface material by being compounded with a filler template and silicon rubber, and has a good application prospect.
A third aspect of the embodiments of the present application provides an application of the hexagonal boron nitride-vanadium dioxide composite material prepared by the preparation method of the present application as a thermal interface material.
The embodiment of the application provides a hexagonal boron nitride-vanadium dioxide composite material prepared by an ice template method, which has a highly ordered arrangement mode, and a porous structure in orientation arrangement can form a high heat dissipation channel, so that the heat conduction performance is improved, and therefore, a thermal interface material with better heat conduction performance can be prepared, and the material can be well applied between a chip and a soaking plate.
In a specific embodiment, the preparation method of the hexagonal boron nitride-vanadium dioxide composite material comprises the following steps:
1) Mixing and stirring 4-12 g of hexagonal boron nitride, 1-3 g of vanadium dioxide, 0.1-0.3 g of silane coupling agent, 0.01-0.03 mg of dispersing agent and 20-60mL of deionized water in a glass beaker for several minutes to obtain a precursor solution;
2) Treating the precursor solution for 5-10 minutes by using a cell crusher, then placing the treated precursor solution into a high-speed mixer for defoaming, and pouring the defoamed precursor solution into a cylindrical mold;
3) Freezing the precursor solution filled into the mold by using liquid nitrogen, and drying the precursor solution in a freeze dryer after the precursor solution is completely frozen to obtain the hBN-VO with the oriented porous structure 2 Composite (aerogel-like).
4) hBN-VO after drying 2 Adding polysiloxane (containing 8-12% of platinum catalyst) into the composite material, placing the composite material in a vacuum drying oven for overnight impregnation, precuring for 0.5-1 h at the temperature of 50-70 ℃, and then curing for 1.5-2.5 h at the temperature of 110-130 ℃ to obtain the sample block hexagonal boron nitride-vanadium dioxide composite material, wherein the hexagonal boron nitride-vanadium dioxide composite material is used as a thermal interface material, and the thermal conductivity is tested on a thermal conductivity meter measured by a transient plane heat source method.
The hexagonal boron nitride-vanadium dioxide composite material is prepared by an ice template method, specifically, a precursor solution processed by a cell crushing instrument is frozen by using liquid nitrogen, a freeze-dried sample, namely the aerogel hexagonal boron nitride-vanadium dioxide composite material, is obtained by drying by using a freeze dryer, and then liquid silicone rubber is added into the freeze-dried sample to be soaked to obtain the hexagonal boron nitride-vanadium dioxide-rubber composite thermal interface material. The hexagonal boron nitride-vanadium dioxide composite material prepared by the ice template method has longitudinal orientation, forms a porous structure with oriented arrangement of heat-conducting fillers, improves the heat-conducting property, fills the hexagonal boron nitride-vanadium dioxide composite fillers with oriented structures, forms a phase-change heat-conducting composite interface material, and enables the thermal interface material to have the capabilities of quick heat dissipation and phase-change heat storage, thereby efficiently reducing chip hot spots.
The following description will be given with reference to specific examples.
Example 1
The preparation method of the hexagonal boron nitride-vanadium dioxide composite material comprises the following steps:
step S11: mixing and stirring 8.48g of hexagonal boron nitride, 2.12g of vanadium dioxide, 0.212g of silane coupling agent (gamma-methacryloxypropyltrimethoxysilane), 0.53mg of dispersing agent (sodium hydroxymethyl cellulose) and 30mL of deionized water in a glass beaker for several minutes to obtain a precursor solution;
step S12: treating the precursor solution for 10 minutes by using a cell crusher to obtain uniform dispersion liquid, placing the dispersion liquid into a high-speed mixer for defoaming treatment, and pouring the dispersion liquid into a cylindrical mold;
step S13: freezing the dispersion liquid filled into the mould by using liquid nitrogen, and putting the dispersion liquid into a freeze dryer for drying treatment after the dispersion liquid is completely frozen to obtain the aerogel-like hexagonal boron nitride-vanadium dioxide composite material;
step S14: adding polydimethylsiloxane (containing 10% of platinum catalyst) into a sample of the hexagonal boron nitride-vanadium dioxide composite material, placing the sample in a vacuum drying oven for overnight immersion for 12 hours, precuring at 60 ℃ for 0.5 hour, and curing at 120 ℃ for 2 hours to obtain a sample block; the thermal conductivity of the sample block is tested on a thermal conductivity meter measured by a transient plane heat source method.
Example 2
The preparation method of the hexagonal boron nitride-vanadium dioxide composite material comprises the following steps:
step S21: mixing and stirring 6.35g of hexagonal boron nitride, 1.59g of vanadium dioxide, 0.159g of silane coupling agent (3-aminopropyltriethoxysilane), 0.40mg of dispersing agent (sodium hydroxymethyl cellulose) and 30mL of deionized water in a glass beaker for several minutes to obtain a precursor solution;
step S22: treating the precursor solution for 10 minutes by using a cell crusher to obtain uniform dispersion liquid, placing the dispersion liquid into a high-speed mixer for defoaming treatment, and pouring the dispersion liquid into a cylindrical mold;
step S23: freezing the dispersion liquid filled into the mould by using liquid nitrogen, and drying the dispersion liquid in a freeze dryer after the dispersion liquid is completely frozen to obtain an aerogel-like hexagonal boron nitride-vanadium dioxide composite material;
step S24: adding polydimethylsiloxane (containing 10% of platinum catalyst) into a sample of the hexagonal boron nitride-vanadium dioxide composite material, placing the sample in a vacuum drying oven for overnight impregnation, precuring at 60 ℃ for 0.5h, and curing at 120 ℃ for 2h to obtain a sample block; the thermal conductivity of the sample block is measured on a thermal conductivity meter by a transient plane heat source method.
Example 3
The preparation method of the hexagonal boron nitride-vanadium dioxide composite material comprises the following steps:
step S31: mixing and stirring 4.24g of hexagonal boron nitride, 1.06g of vanadium dioxide, 0.106g of silane coupling agent (3-aminopropyltriethoxysilane), 0.26mg of dispersing agent (sodium hydroxymethyl cellulose) and 30mL of deionized water in a glass beaker for several minutes to obtain a precursor solution;
step S32: treating the precursor solution for 10 minutes by using a cell crusher to obtain uniform dispersion liquid, placing the dispersion liquid into a high-speed mixer for defoaming treatment, and pouring the dispersion liquid into a cylindrical mold;
step S33: freezing the dispersion liquid filled into the mould by using liquid nitrogen, and putting the dispersion liquid into a freeze dryer for drying treatment after the dispersion liquid is completely frozen to obtain the aerogel-like hexagonal boron nitride-vanadium dioxide composite material;
step S34: adding polydimethylsiloxane (containing 10% of platinum catalyst) into a sample of the hexagonal boron nitride-vanadium dioxide composite material, placing the sample in a vacuum drying oven for overnight impregnation, precuring at 60 ℃ for 0.5h, and curing at 120 ℃ for 2h to obtain a sample block; the thermal conductivity of the sample block is tested on a thermal conductivity meter measured by a transient plane heat source method.
Comparative example 1
Directly adding polydimethylsiloxane (containing 10% of platinum catalyst) into an empty mould, placing the mould in a vacuum drying oven for overnight dipping, pre-curing for 0.5h at 60 ℃, curing for 2h at 120 ℃ to obtain a sample block, and testing the thermal conductivity of the sample block on a thermal conductivity meter measured by a transient plane heat source method.
Comparative example 2
The method comprises the steps of providing a hexagonal boron nitride-vanadium dioxide composite material prepared in the prior art (mixing the hexagonal boron nitride-vanadium dioxide composite material prepared by hydrothermal method and a high polymer uniformly by using a high-speed mixer, placing the mixture in a mold, and curing to obtain the hexagonal boron nitride-vanadium dioxide-high polymer composite material in random arrangement), wherein the mass of the hexagonal boron nitride and the vanadium dioxide is the same as that of the hexagonal boron nitride and the vanadium dioxide in example 1.
Adding polydimethylsiloxane (containing 10% of platinum catalyst) into a sample of the hexagonal boron nitride-vanadium dioxide composite material, putting the sample into a vacuum drying oven for overnight impregnation, precuring at 60 ℃ for 0.5h, and curing at 120 ℃ for 2h to obtain a sample block; the thermal conductivity of the sample block is tested on a thermal conductivity meter measured by a transient plane heat source method.
Formation test
(1) Appearance of the product
FIG. 1 is a diagram of hexagonal boron nitride-vanadium dioxide composites in aerogel form prepared in examples, two samples per example; FIG. 2 is an external view of the hexagonal boron nitride-vanadium dioxide composite material and the silicone rubber provided in the examples after the materials are compounded.
(2) Thermal conductivity
The thermal conductivities of the above examples and comparative examples are shown in table 1 below.
TABLE 1
The above data in table 1 illustrates: the hexagonal boron nitride-vanadium dioxide composite material prepared by the embodiment of the application has better heat-conducting property after being compounded with the silicon rubber, so that the hexagonal boron nitride-vanadium dioxide composite material can be used as a thermal interface material to efficiently reduce the hot spots of a chip.
The above description is only exemplary of the present application and should not be taken as limiting the present application, as any modification, equivalent replacement, or improvement made within the spirit and principle of the present application should be included in the protection scope of the present application.
Claims (10)
1. A preparation method of a hexagonal boron nitride-vanadium dioxide composite material is characterized by comprising the following steps:
dispersing hexagonal boron nitride, vanadium dioxide, a silane coupling agent and a dispersing agent in water to obtain a precursor solution;
and preparing the precursor solution into the hexagonal boron nitride-vanadium dioxide composite material with an oriented arrangement structure by adopting an ice template method.
2. The method according to claim 1, wherein the mass ratio of the hexagonal boron nitride, the vanadium dioxide, the silane coupling agent and the dispersant is (4-12): 1-3): 0.1-0.3: (0.01-0.03); and/or the presence of a gas in the gas,
the mass volume ratio of the hexagonal boron nitride to the water is (4-12) g, (20-60) mL.
3. The method of claim 1, wherein the forming the precursor solution into the aerogel material having an oriented arrangement structure by using an ice template method comprises: and (3) defoaming the precursor solution, and then carrying out liquid nitrogen freeze drying treatment.
4. The method of claim 3, wherein the liquid nitrogen freeze-drying process comprises: freezing in liquid nitrogen at-190 deg.c to-200 deg.c for 30-45 min, and drying in a freeze drier under 0.5-1.5 Pa vacuum degree for 10-14 hr.
5. The production method according to any one of claims 1 to 4, wherein the silane coupling agent is selected from at least one of a vinyl silane coupling agent, an aminosilane coupling agent, and a methacryloxy silane coupling agent; and/or the presence of a gas in the atmosphere,
the dispersing agent is at least one selected from cellulose, carboxymethyl cellulose, hydroxyethyl cellulose, hydroxypropyl methyl cellulose and sodium hydroxymethyl cellulose.
6. The method of any one of claims 1-4, further comprising: and (3) placing the hexagonal boron nitride-vanadium dioxide composite material with the orientation arrangement structure in polysiloxane for dipping treatment, and then curing treatment.
7. The method of claim 6, wherein the polysiloxane is at least one selected from the group consisting of polydimethylsiloxane, polymethylvinylsiloxane and polymethylphenylvinylsiloxane.
8. The method of claim 6, wherein the curing process comprises: precuring for 0.5 to 1 hour at the temperature of between 50 and 70 ℃, and then curing for 1.5 to 2.5 hours at the temperature of between 110 and 130 ℃.
9. A hexagonal boron nitride-vanadium dioxide composite material, characterized in that it is prepared by the preparation method of any one of claims 1 to 8.
10. The use of the hexagonal boron nitride-vanadium dioxide composite material prepared by the preparation method according to any one of claims 1 to 8 in the preparation of thermal interface materials.
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