CN112409791A - Heat-conducting composite material and preparation method thereof - Google Patents
Heat-conducting composite material and preparation method thereof Download PDFInfo
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Abstract
The invention provides a heat-conducting composite material which comprises a polymer matrix and a heat-conducting filler filled in the polymer matrix, wherein the heat-conducting filler is a boron nitride nanosheet grafted with an amino functional group at the edge. The preparation method of the heat-conducting composite material comprises the following steps: preparing a heat-conducting filler dispersion liquid: grafting amino functional groups on the edges of the boron nitride nanosheets through surface modification to obtain the heat-conducting filler; dispersing the heat-conducting filler in a dispersing agent to form a heat-conducting filler dispersion liquid; preparation of polymer matrix solution: carrying out polymerization reaction on monomers corresponding to the polymer matrix under the action of heating and a catalyst to obtain a polymer matrix solution; adding the heat-conducting filler dispersion liquid into the polymer matrix solution according to a preset proportion, and stirring and mixing to obtain mixed slurry; and curing the mixed slurry to form a film, thereby obtaining the heat-conducting composite material. The heat-conducting composite material provided by the invention has good heat-conducting property and mechanical property.
Description
Technical Field
The invention belongs to the technical field of heat conduction materials, and particularly relates to a heat conduction composite material and a preparation method thereof.
Background
With the advent of the 5G era, electronic equipment is becoming thinner and smaller, and the high integration and structural complexity of internal electronic components of the electronic equipment greatly increases the heating power per unit area of the electronic equipment, and the heat generated by the electronic equipment seriously affects the service performance and service life of the electronic equipment. There are data showing that the failure problem of 55% of electronic products is caused by excessive temperature. Therefore, heat dissipation of electronic devices is a problem to be solved.
Compared with the traditional metal and ceramic materials, the polymer has wide application due to the advantages of light weight, low cost, good insulating property, good processing property and the like. For example, in the field of microelectronic packaging, a substrate of a printed circuit board is mostly made of materials such as polyimide, polyester and the like, so that the printed circuit board has good electrical insulation performance and can meet the requirements of different application scenes on the mechanical strength of the substrate; for example, the matrix of the thermal interface material for assisting the heat dissipation of the chip is mostly polyolefin or silica gel, so that the good flexibility can greatly fill up the gap of the contact surface and reduce the air thermal resistance. In heat exchange and heating engineering, polymers such as polyurethane can be used for replacing metal materials to be applied to environments with high corrosion, strength and toughness, and manufacturing cost and product weight are reduced. However, interface scattering frequently occurs in the transmission process of phonons due to a large number of defects and chain entanglement in the polymer, the phonon free path is greatly reduced, and the thermal conductivity of the polymer is low (-0.2W/m.K), so that the further application of the polymer in the field of thermal management is limited.
At present, the main method for improving the thermal conductivity of the polymer is to fill high thermal conductive filler into a polymer matrix, and form a thermal conductive path inside the polymer matrix through the filler so as to improve the overall thermal conductivity. Among many heat conductive fillers, boron nitride has a graphene-like crystal structure, is composed of six-membered ring layers composed of alternating, covalently bonded boron atoms and nitrogen atoms, has high thermal conductivity, wide band gap, and good stability, and is widely used in electronic packaging and high-voltage devices. At present, the heat conductivity of the polymer composite material using unmodified boron nitride as the heat conductive filler needs to be improved.
Disclosure of Invention
In view of the defects in the prior art, the invention provides a heat-conducting composite material and a preparation method thereof, and aims to solve the problem that the heat-conducting performance of the existing polymer composite material is poor.
In order to achieve the above object, an aspect of the present invention provides a thermally conductive composite material, including a polymer matrix and a thermally conductive filler filled in the polymer matrix, wherein the thermally conductive filler is boron nitride nanosheets grafted with amino functional groups at edges.
Preferably, in the heat-conducting composite material, the mass percentage of the heat-conducting filler is 10% -50%.
Preferably, the transverse size of the boron nitride nanosheet is 200 nm-300 nm, and the thickness is 3 nm-4 nm.
Preferably, the polymer matrix is further added with epoxy resin, and the mass percentage of the epoxy resin in the polymer matrix is 25-30%.
Preferably, the polymer matrix is selected from one or more of cyanate ester resin, polyethylene, polyvinyl alcohol, polyimide, polymethyl methacrylate, polydimethylsiloxane, polycarbonate, polyurethane and silicon rubber.
Another aspect of the present invention is to provide a method for preparing the thermally conductive composite material as described above, which comprises:
preparing a heat-conducting filler dispersion liquid: grafting amino functional groups on the edges of the boron nitride nanosheets through surface modification to obtain the heat-conducting filler; dispersing the heat-conducting filler in a dispersing agent to form a heat-conducting filler dispersion liquid;
preparation of polymer matrix solution: carrying out polymerization reaction on monomers corresponding to the polymer matrix under the action of heating and a catalyst to obtain a polymer matrix solution;
adding the heat-conducting filler dispersion liquid into the polymer matrix solution according to a preset proportion, and stirring and mixing to obtain mixed slurry;
and curing the mixed slurry to form a film, thereby obtaining the heat-conducting composite material.
Preferably, the preparation of the thermally conductive filler dispersion comprises:
taking hexagonal boron nitride as a raw material, adopting urea as a modifier, mixing the hexagonal boron nitride with the urea, adding a ball-milling auxiliary agent, and then placing the mixture in ball-milling equipment to perform a ball-milling process to obtain boron nitride nanosheet powder with amino functional groups grafted on the edges;
and washing and drying the boron nitride nanosheet powder, and then adding the boron nitride nanosheet powder into a dispersion liquid for dispersion to obtain the heat-conducting filler dispersion liquid.
Preferably, the ball milling auxiliary agent is sodium chloride or potassium chloride, and the ball milling process is performed in N2Or Ar protective atmosphere, and the dispersing agent is deionized water, ethanol, acetone or 1, 4-dioxane.
Preferably, the preparation method further comprises: and adding epoxy resin into the polymer matrix solution to toughen and modify the polymer matrix.
Preferably, the polymer matrix is cyanate ester resin, and the preparation of the polymer matrix solution comprises:
adding a cyanate monomer and a catalyst into a reaction container, and carrying out oil bath heating on the reaction container to enable the cyanate monomer to carry out polymerization reaction so as to obtain the polymer matrix solution; wherein the catalyst is dibutyltin dilaurate or bis-n-butyltin oxide.
Preferably, the curing the mixed slurry into a film comprises: and performing vacuum defoaming treatment on the mixed slurry, pouring the mixed slurry into a mold, heating and curing, cooling, and demolding to obtain the heat-conducting composite material.
Preferably, the curing the mixed slurry into a film comprises: and carrying out vacuum filtration on the mixed slurry to form a film, heating and solidifying the film-forming material, and cooling to obtain the heat-conducting composite material.
In the heat-conducting composite material provided by the embodiment of the invention, the heat-conducting filler is grafted with amino (-NH) on the edge2) The boron nitride nanosheet with the functional group increases the wettability of the boron nitride nanosheet filler, so that the boron nitride nanosheet filler can be better mixed with a polymer matrix, and the thermal conductivity of the heat-conducting composite material can be effectively improved.
The preparation method of the heat-conducting composite material provided by the embodiment of the invention has the advantages of simple process flow and easy realization of process conditions, and is beneficial to large-scale industrial application.
Drawings
FIG. 1 is a process flow diagram of a method of making a thermally conductive composite in an embodiment of the invention;
FIG. 2 is a graph illustrating a test of thermal conductivity of a thermally conductive composite in an embodiment of the present invention;
fig. 3 is a graph showing the mechanical properties of the thermally conductive composite in the example of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, embodiments of the present invention are described in detail below with reference to the accompanying drawings. Examples of these preferred embodiments are illustrated in the accompanying drawings. The embodiments of the invention shown in the drawings and described in accordance with the drawings are exemplary only, and the invention is not limited to these embodiments.
It should be noted that, in order to avoid obscuring the present invention with unnecessary details, only the structures and/or processing steps closely related to the scheme according to the present invention are shown in the drawings, and other details not so relevant to the present invention are omitted.
The embodiment of the invention firstly provides a heat-conducting composite material, which comprises a polymer matrix and a heat-conducting filler filled in the polymer matrix, wherein the heat-conducting filler is a boron nitride nanosheet grafted with an amino functional group at the edge.
In a preferred scheme, in the heat-conducting composite material, the mass percentage of the heat-conducting filler is 10% -50%. The transverse size of the boron nitride nanosheet is 200 nm-300 nm, and the thickness of the boron nitride nanosheet is 3 nm-4 nm.
The heat-conducting filler in the heat-conducting composite material is grafted with amino (-NH) at the edge2) The boron nitride nanosheet with the functional group increases the wettability of the boron nitride nanosheet filler, so that the boron nitride nanosheet filler can be better mixed with a polymer matrix, and the thermal conductivity of the heat-conducting composite material can be effectively improved.
In a preferable scheme, the polymer matrix is further added with epoxy resin, and the mass percentage of the epoxy resin in the polymer matrix is 25-30%. The polymer matrix is modified by adding the epoxy resin, so that the mechanical property of the heat-conducting composite material can be improved, and the toughness of the heat-conducting composite material can be enhanced. More preferably, the epoxy resin is selected from the group consisting of epoxy resins of type E51, which have the advantages of high epoxy value and low viscosity.
In a preferred embodiment, the polymer matrix is cyanate ester resin, and polyethylene, polyvinyl alcohol, polyimide, polymethyl methacrylate, polydimethylsiloxane, polycarbonate, polyurethane, and silicone rubber can also be used. The above resins may be used alone or in combination of two or more. Most preferably, the bisphenol A cyanate ester resin is selected, and the cyanate ester resin is used as a polymer matrix, so that the polymer matrix has good dielectric properties (low dielectric loss and dielectric constant), good wet heat resistance (low water absorption rate) and excellent adhesive property.
The embodiment of the present invention also provides a preparation method of the above thermal conductive composite material, referring to fig. 1, the preparation method includes:
s10, preparing a heat-conducting filler dispersion liquid: grafting amino functional groups on the edges of the boron nitride nanosheets through surface modification to obtain the heat-conducting filler; and dispersing the heat-conducting filler in a dispersing agent to form a heat-conducting filler dispersion liquid.
In a preferred scheme, hexagonal boron nitride is used as a raw material, urea is used as a modifier, the hexagonal boron nitride and the urea are mixed, a ball-milling auxiliary agent is added, and then the mixture is placed in ball-milling equipment to be subjected to a ball-milling process, so that boron nitride nanosheet powder with amino functional groups grafted on the edges is obtained. And then washing and drying the boron nitride nanosheet powder, and then adding the boron nitride nanosheet powder into a dispersion liquid for dispersion to obtain the heat-conducting filler dispersion liquid.
Specifically, the lateral dimension of the hexagonal boron nitride is 5-10 μm, and the thickness is about 200 nm. The ball milling auxiliary agent can be selected from sodium chloride or potassium chloride, and the ball milling process is performed in N2Or under the protection of Ar atmosphere, and the dispersing agent can be selected from water, ethanol, acetone or 1, 4-dioxane. Urea is used as a modifier, and stripping and modification of hexagonal boron nitride are realized by mechanical ball milling with the aid of a ball milling assistant, so that boron nitride nanosheet powder with amino functional groups grafted on the edges is obtained, wherein the transverse size of the boron nitride nanosheet is 200-300 nm, and the thickness of the boron nitride nanosheet is 3-4 nm.
The addition of the sodium chloride or potassium chloride ball-milling auxiliary agent is helpful for providing stronger shearing force in the ball-milling process and promoting the stripping of the hexagonal boron nitride. In addition, sodium chloride or potassium chloride is easily dissolved in water, can be removed after being washed and dried for several times, and has no pollution to samples and is convenient and quick.
And washing and drying the boron nitride nanosheet powder, wherein the excess urea and the ball-milling auxiliary agent are mainly removed, and pure boron nitride nanopowder is obtained. The specific process can be as follows: dissolving the boron nitride nanosheet powder in deionized water, filtering, and drying, preferably repeatedly washing and drying for 2-3 times.
More specifically, in the ballIn the grinding process, the mass ratio of the hexagonal boron nitride to the urea to the ball-milling auxiliary agent can be set within the range of 1-2: 20-25: 5-10, the rotating speed of the ball mill can be set within the range of 350 r/min-500 r/min, and Al can be used2O3Or ZrO2Or agate grinding balls with the diameter of 10mm and/or 1mm and the ball-to-material ratio of 1-5 are subjected to ball milling treatment at normal temperature for 6-10 hours to obtain the modified boron nitride nanosheet powder. And dispersing the prepared boron nitride sheet powder in deionized water, repeatedly washing and drying to remove redundant urea and ball-milling auxiliary agents, dispersing the purified boron nitride nano powder in dispersion liquid, and finally obtaining stable heat-conducting filler dispersion liquid.
S20, preparation of polymer matrix solution: and carrying out polymerization reaction on monomers corresponding to the polymer matrix under the action of heating and a catalyst to obtain the polymer matrix solution.
The polymer matrix is selected from one or more of cyanate ester resin, polyethylene, polyvinyl alcohol, polyimide, polymethyl methacrylate, polydimethylsiloxane, polycarbonate, polyurethane and silicon rubber.
In a preferred embodiment, the heating may be selected as an oil bath heating, and the heating temperature and time are set according to the polymerization reaction of the monomers for forming the polymer matrix.
In a preferred scheme, the epoxy resin is added into the polymer matrix solution, the mixture is formed by continuous heating and stirring, and the polymer matrix is modified by adding the epoxy resin, so that the mechanical property of the finally obtained heat-conducting composite material can be improved, and the toughness of the finally obtained heat-conducting composite material can be enhanced. More preferably, the epoxy resin is selected from the group consisting of epoxy resins of type E51, which have the advantages of high epoxy value and low viscosity.
In a preferred embodiment, the polymer matrix is cyanate ester resin, and the preparation of the polymer matrix solution includes: adding a cyanate monomer and a catalyst into a reaction container, and carrying out oil bath heating on the reaction container to enable the cyanate monomer to carry out polymerization reaction so as to obtain the polymer matrix solution; wherein the catalyst is dibutyltin dilaurate or bis-n-butyltin oxide. The cyanate resin is used as a polymer matrix, has good dielectric properties (low dielectric loss and dielectric constant), good wet heat resistance (low water absorption) and excellent adhesive properties.
And S30, adding the heat-conducting filler dispersion liquid into the polymer matrix solution according to a preset proportion, and stirring and mixing to obtain mixed slurry.
Wherein the predetermined proportion is determined according to the mass percentage of the heat-conducting filler in the finally prepared heat-conducting composite material. In a preferred scheme, the mass percent of the heat-conducting filler in the heat-conducting composite material to be prepared is 10-50%.
S40, curing the mixed slurry to form a film, and obtaining the heat-conducting composite material.
Among them, it is preferable to form a film by curing in one of the following two ways:
the first method is as follows: and performing vacuum defoaming treatment on the mixed slurry, pouring the mixed slurry into a mold, heating and curing, cooling, and demolding to obtain the heat-conducting composite material.
The second method comprises the following steps: and carrying out vacuum filtration on the mixed slurry to form a film, heating and solidifying the film-forming material, and cooling to obtain the heat-conducting composite material.
And in the second preferred use mode, the mixed slurry is subjected to vacuum filtration, so that the boron nitride nanosheet heat-conducting filler in the polymer matrix can form regular orientation arrangement under the action of the vacuum filtration, a good heat-conducting passage is formed, and the heat-conducting performance of the finally obtained heat-conducting composite material is further improved.
Among them, in the heat curing process of the first and second modes, a mode of heating with a gradual temperature rise is preferably used, for example: firstly heating at 120 ℃ for 2h, then heating to 150 ℃ for 2h, then heating to 180 ℃ for 2h, and then heating to 200 ℃ for 2 h.
The above-described thermally conductive composite material and the method for preparing the same will be described below with reference to specific examples, and it will be understood by those skilled in the art that the following examples are only specific examples of the above-described thermally conductive composite material and the method for preparing the same of the present invention, and are not intended to limit the entirety thereof.
Example 1: preparation of heat conductive filler dispersion
The mass ratio of the hexagonal boron nitride to the urea to the sodium chloride is 1: 20: 5 mixing in a planetary ball mill under N2Under the protection of atmosphere, ZrO with 10mm and 1mm sphere diameters respectively is used at a rotating speed of 500r/min2Grinding the balls, and performing ball milling treatment for 10 hours. Washing and drying the obtained powder in deionized water to remove redundant urea and sodium chloride to obtain pure boron nitride nano powder, and then selecting deionized water as a dispersing agent to disperse the pure boron nitride nano powder in the deionized water to finally obtain the pure and stable heat-conducting filler. Urea added in the ball milling process realizes the modification of the boron nitride nanosheets, and-NH is grafted on the edge of the boron nitride nanosheets2A functional group.
Example 2: preparation of Polymer matrix solutions
In this embodiment, the polymer matrix is cyanate ester resin, and the preparation process thereof is as follows:
7g of bisphenol A type cyanate ester monomer and 0.05g of catalyst (dibutyltin dilaurate) are sequentially put into a reaction vessel, heated by adopting an oil bath at 90 ℃ for 30min, and a light yellow transparent cyanate ester polymer liquid is obtained after the polymerization reaction is finished, namely the polymer matrix solution is obtained.
Adding 3g E51 type epoxy resin into the prepared cyanate ester polymer solution, and continuously stirring and heating for 15min to obtain a mixture of cyanate ester resin and epoxy resin.
Example 3: preparation of heat-conducting composite material
The heat conductive filler dispersion liquid obtained in example 1 was added to the polymer matrix solution (a mixture of a cyanate ester resin and an epoxy resin) obtained in example 2 in a predetermined ratio and stirred and mixed to obtain a mixed slurry. Wherein, the heat-conducting filler dispersion liquid is added according to the mass percentages of 10%, 20%, 30%, 40% and 50% of the heat-conducting filler in the finally prepared heat-conducting composite material.
Curing the mixed slurry to form a film, so as to obtain the heat-conducting composite material: and (2) carrying out vacuum defoaming treatment on the mixed slurry for 30min, pouring the mixed slurry into a preheated mold, heating for 2h at the temperature of 120 ℃, then heating for 2h at the temperature of 150 ℃, then heating for 2h at the temperature of 180 ℃, heating for 2h at the temperature of 200 ℃ and heating for 2h for curing by heating, naturally cooling to room temperature after the curing process is finished, and demolding to obtain the heat-conducting composite material.
This example prepares thermally conductive composite samples a1, a2, A3, a4, and a5 that yield thermally conductive fillers in the mass percentages of 10%, 20%, 30%, 40%, and 50%, respectively.
Thermal conductivity and mechanical properties were tested on the thermally conductive composite samples a 1-a 5, and the results of the thermal conductivity and tensile strength were shown in fig. 2 and 3 and in table 1 below.
Table 1: test data of thermal conductivity and mechanical Properties of the thermally conductive composite of example 3
| Sample (I) | A1 | A2 | A3 | A4 | A5 |
| Thermal conductivity (W/m. K) | 1.06 | 1.13 | 1.42 | 2.11 | 1.83 |
| Tensile Strength (MPa) | 80.0 | 87.5 | 94.1 | 89.3 | 86.8 |
Example 4: preparation of heat-conducting composite material
A mixed slurry was prepared in the manner as described in example 3, and this example is different from example 3 in that the process of curing the mixed slurry into a film was different.
Specifically, the curing film-forming process of the present embodiment specifically includes: adding acetone (other diluents can be selected in other embodiments) into the mixed slurry for dilution, carrying out vacuum filtration on the diluted mixed slurry for 20h to form a film, heating and curing the film-formed material, wherein the heating process is the same as that of embodiment 3, and naturally cooling to room temperature after the curing process is finished to obtain the heat-conducting composite material.
This example prepares thermally conductive composite samples B1, B2, B3, B4, and B5 that obtained 10%, 20%, 30%, 40%, and 50% by mass of the thermally conductive filler, respectively.
Thermal conductivity and mechanical properties were tested on the thermally conductive composite samples B1-B5, and the results of the thermal conductivity and tensile strength were shown in fig. 2 and 3 and in table 2 below.
Table 2: test data of thermal conductivity and mechanical properties of the thermally conductive composite of example 4
| Sample (I) | B1 | B2 | B3 | B4 | B5 |
| Thermal conductivity (W/m. K) | 1.40 | 1.65 | 1.84 | 2.32 | 2.02 |
| Tensile Strength (MPa) | 83.0 | 84.6 | 92.2 | 90.2 | 88.3 |
Comparing example 3 with example 4, it can be seen that, under the same other process conditions, the heat conductive composite material prepared in example 4 by using a vacuum filtration film formation method has better heat conductive performance. The mixed slurry is subjected to vacuum filtration, so that the boron nitride nanosheet heat-conducting filler in the polymer matrix can form regular orientation arrangement under the action of filtration, a good heat-conducting passage is formed, and the heat-conducting performance of the finally obtained heat-conducting composite material is further improved.
Comparative example
Compared with the embodiment 3, the thermal conductive filler in the embodiment adopts the unmodified boron nitride nanosheet, the unmodified boron nitride nanosheet is dissolved in the deionized water, and the thermal conductive filler dispersion liquid is obtained by stirring and dispersing.
Except for the difference in the dispersion liquid of the thermal conductive filler, the other processes of this example are performed completely with reference to example 3, and this example prepares thermal conductive composite samples C1, C2, C3, C4 and C5, which have thermal conductive fillers (unmodified boron nitride nanosheets) in the mass percentages of 10%, 20%, 30%, 40% and 50%, respectively.
Thermal conductivity and mechanical properties were tested on the thermally conductive composite samples C1-C5, and the results of the thermal conductivity and tensile strength were shown in fig. 2 and 3 and in table 3 below.
Table 3: test data of thermal conductivity and mechanical properties of the thermally conductive composite of comparative example
| Sample (I) | C1 | C2 | C3 | C4 | C5 |
| Thermal conductivity (W/m. K) | 0.89 | 1.02 | 1.25 | 2.48 | 1.63 |
| Tensile Strength (MPa) | 78.6 | 83.2 | 88.1 | 85.4 | 84.5 |
Comparing the example 3 with the comparative example, it can be seen that, under the same other process conditions, the boron nitride nanosheet with the amino functional group grafted on the edge is adopted as the heat-conducting filler in the technical scheme of the present invention, and compared with the unmodified boron nitride nanosheet adopted as the heat-conducting filler, the boron nitride nanosheet has a better heat-conducting property. This is due to the grafting of the edges with amino groups (-NH)2) The functional group increases the wettability of the boron nitride nanosheet filler, so that the boron nitride nanosheet filler can be better mixed with a polymer matrix, and the thermal conductivity of the heat-conducting composite material can be effectively improved.
The foregoing is directed to embodiments of the present application and it is noted that numerous modifications and adaptations may be made by those skilled in the art without departing from the principles of the present application and are intended to be within the scope of the present application.
Claims (12)
1. A heat-conducting composite material comprises a polymer matrix and a heat-conducting filler filled in the polymer matrix, and is characterized in that the heat-conducting filler is boron nitride nanosheets grafted with amino functional groups at the edges.
2. The heat conductive composite material according to claim 1, wherein the mass percentage of the heat conductive filler in the heat conductive composite material is 10% to 50%.
3. The thermally conductive composite of claim 1, wherein the boron nitride nanoplates have a lateral dimension of 200nm to 300nm and a thickness of 3nm to 4 nm.
4. The heat conductive composite material as claimed in claim 1, wherein an epoxy resin is further added to the polymer matrix, and the mass percentage of the epoxy resin in the polymer matrix is 25-30%.
5. The thermally conductive composite material as claimed in any one of claims 1 to 4, wherein the polymer matrix is one or more selected from cyanate ester resin, polyethylene, polyvinyl alcohol, polyimide, polymethyl methacrylate, polydimethylsiloxane, polycarbonate, polyurethane and silicone rubber.
6. A method of making a thermally conductive composite material as claimed in any one of claims 1 to 5, comprising:
preparing a heat-conducting filler dispersion liquid: grafting amino functional groups on the edges of the boron nitride nanosheets through surface modification to obtain the heat-conducting filler; dispersing the heat-conducting filler in a dispersing agent to form a heat-conducting filler dispersion liquid;
preparation of polymer matrix solution: carrying out polymerization reaction on monomers corresponding to the polymer matrix under the action of heating and a catalyst to obtain a polymer matrix solution;
adding the heat-conducting filler dispersion liquid into the polymer matrix solution according to a preset proportion, and stirring and mixing to obtain mixed slurry;
and curing the mixed slurry to form a film, thereby obtaining the heat-conducting composite material.
7. The method of preparing a thermally conductive composite material as claimed in claim 6, wherein the preparation of the thermally conductive filler dispersion comprises:
taking hexagonal boron nitride as a raw material, adopting urea as a modifier, mixing the hexagonal boron nitride with the urea, adding a ball-milling auxiliary agent, and then placing the mixture in ball-milling equipment to perform a ball-milling process to obtain boron nitride nanosheet powder with amino functional groups grafted on the edges;
and washing and drying the boron nitride nanosheet powder, and then adding the boron nitride nanosheet powder into a dispersion liquid for dispersion to obtain the heat-conducting filler dispersion liquid.
8. The method for preparing the heat-conducting composite material as claimed in claim 7, wherein the ball-milling assistant is sodium chloride or potassium chloride, and the ball-milling process is carried out under N2Or Ar protective atmosphere, and the dispersing agent is deionized water, ethanol, acetone or 1, 4-dioxane.
9. The method of preparing a thermally conductive composite material as claimed in claim 6, further comprising: and adding epoxy resin into the polymer matrix solution to toughen and modify the polymer matrix.
10. The method of claim 6, wherein the polymer matrix is cyanate ester resin, and the preparing of the polymer matrix solution comprises:
adding a cyanate monomer and a catalyst into a reaction container, and carrying out oil bath heating on the reaction container to enable the cyanate monomer to carry out polymerization reaction so as to obtain the polymer matrix solution; wherein the catalyst is dibutyltin dilaurate or bis-n-butyltin oxide.
11. The method of any one of claims 6-10, wherein curing the mixed slurry into a film comprises: and performing vacuum defoaming treatment on the mixed slurry, pouring the mixed slurry into a mold, heating and curing, cooling, and demolding to obtain the heat-conducting composite material.
12. The method of any one of claims 6-10, wherein curing the mixed slurry into a film comprises: and carrying out vacuum filtration on the mixed slurry to form a film, heating and solidifying the film-forming material, and cooling to obtain the heat-conducting composite material.
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| CN202011323211.0A CN112409791A (en) | 2020-11-23 | 2020-11-23 | Heat-conducting composite material and preparation method thereof |
| PCT/CN2020/135164 WO2022104949A1 (en) | 2020-11-23 | 2020-12-10 | Thermally conductive composite material and preparation method therefor |
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