CN113980468A - Preparation method of vertically-oriented three-dimensional expanded graphite heat conductor and reinforced heat-conducting polymer matrix composite material thereof - Google Patents
Preparation method of vertically-oriented three-dimensional expanded graphite heat conductor and reinforced heat-conducting polymer matrix composite material thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
- C08K3/042—Graphene or derivatives, e.g. graphene oxides
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- 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
- C09K5/08—Materials not undergoing a change of physical state when used
- C09K5/14—Solid materials, e.g. powdery or granular
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/005—Additives being defined by their particle size in general
Abstract
The invention discloses a preparation method of a vertically-oriented three-dimensional expanded graphite heat conductor and a reinforced heat-conducting polymer matrix composite material thereof, and relates to the vertically-oriented three-dimensional expanded graphite heat conductor, the preparation method thereof and the application of the heat-conducting polymer matrix composite material in improving the heat-conducting property. In addition, the invention provides a polymer matrix composite material reinforced by the vertically-oriented three-dimensional expanded graphite heat conductor, wherein the vertically-oriented three-dimensional expanded graphite heat conductor is used as a continuous phonon transmission framework for efficiently improving the heat conduction performance of the polymer matrix composite material, and the longitudinal heat conduction performance of the heat conduction polymer matrix composite material can reach 10-40W/(m.K).
Description
Technical Field
The invention belongs to the technical field of preparation of heat-conducting polymer-based composite materials, and relates to a vertically-oriented three-dimensional expanded graphite heat conductor, a preparation method thereof and application of the heat conductor as a filler to enhance the heat-conducting property of a heat-conducting polymer-based composite material, in particular to a vertically-oriented three-dimensional expanded graphite heat conductor, a preparation method thereof, a polymer-based heat-conducting polymer-based composite material adopting the heat conductor as a high-heat-conducting filler, and a preparation method of the heat-conducting polymer-based composite material.
Background
With the rapid development of highly integrated, lightweight, multifunctional devices in the electronics industry, the packaging density of electronic components or units has increased significantly. The heat accumulation during the use of electronic products can cause overheating and failure of the electronic products, and has become an important determinant for hindering the development of next-generation electronic components. It is therefore highly desirable to design and fabricate high performance thermally conductive polymer matrix composites that facilitate the transfer of heat from a heat source to a heat sink by reducing the thermal contact resistance.
To date, various thermally conductive inorganic fillers have been used in polymer matrices to increase the thermal conductivity of polymeric materials. However, it is noted that very high loadings (> 40 vol%) of micron filler loading in the polymer matrix are required to produce thermally conductive polymer matrix composites with higher thermal conductivity. However, this deteriorates the processability of the thermally conductive polymer-based composite material. On the other hand, although nanofillers show superior performance at low filler loading fractions. But the agglomeration phenomenon caused by strong self-interaction limits the further utilization of the nano-materials. Therefore, the development of a preparation method of a novel high thermal conductive polymer matrix composite material is extremely important.
Disclosure of Invention
In view of the above problems in the prior art, an object of the present invention is to provide a vertically oriented three-dimensional expanded graphite thermal conductor, a method for preparing the same, and a use of the vertically oriented three-dimensional expanded graphite thermal conductor as a filler in a thermally conductive polymer matrix composite material.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the present invention provides a vertically-oriented three-dimensional expanded graphite heat conductor composed of exfoliated expanded graphite and graphene oxide uniformly distributed on the exfoliated expanded graphite. The transverse dimension of the flake expanded graphite is 10-500 mu m, and the thickness is 0.1-2 mu m. The lateral size of the graphene oxide is 0.5-10 mu m, and the thickness of the graphene oxide is 0.74-5 nm. The mass percentage of the graphene oxide in the three-dimensional expanded graphite heat conductor is 2.5-25%.
In the technical scheme of the invention, the density of the vertically-oriented three-dimensional expanded graphite heat conductor is 150-950 mg/cm3。
In the technical scheme of the invention, the vertically-oriented three-dimensional expanded graphite heat conductor is a macroscopic three-dimensional continuous structure.
Preferably, in the thermally conductive polymer-based composite material, the expanded graphite flakes in the vertically oriented three-dimensional expanded graphite thermal conductor are connected to each other by graphene oxide.
In the technical scheme of the invention, the vertically-oriented three-dimensional expanded graphite heat conductor is prepared by the following method:
(1) adding flaky expanded graphite into a graphene oxide aqueous solution under the condition of mechanical stirring to obtain flaky expanded graphite-graphene oxide mixed aqueous slurry;
(2) and (3) carrying out freeze drying treatment on the flake expanded graphite-graphene oxide mixed aqueous slurry to obtain the vertically oriented three-dimensional expanded graphite heat conductor.
In the technical scheme of the invention, the flake expanded graphite-graphene oxide mixed aqueous slurry in the step (1) does not contain a surfactant.
The invention also provides a filler, which is a vertically-oriented three-dimensional expanded graphite heat conductor. Can be used as a heat-conducting reinforcing filler in a heat-conducting polymer matrix composite material.
The invention also provides a heat-conducting polymer composite material, which comprises the vertically-oriented three-dimensional expanded graphite heat conductor as a filler and a polymer matrix.
Further, the polymer matrix comprises polydimethylsiloxane, a silicon rubber curing agent, a catalyst and the like.
Further, the curing agent is silicone oil containing active hydrogen.
Further, the volume percentage of the three-dimensional structure flake expanded graphite-graphene oxide hybrid heat conductor is 6.7-42% based on 100% of the total volume of the heat-conducting composite polymer matrix composite material.
Further, the volume percentage of the polydimethylsiloxane is 29-46% based on 100% of the total volume of the heat-conducting polymer matrix composite.
Further, the volume percentage of the curing agent is 29-46% based on 100% of the total volume of the heat-conducting polymer matrix composite.
Further, the preparation method of the heat-conducting polymer matrix composite material comprises the following steps:
(1) mixing a curing agent and polydimethylsiloxane in a mechanical blending mode to prepare a polydimethylsiloxane mixture;
(2) and (2) injecting the polydimethylsiloxane mixture obtained in the step (1) into the three-dimensional structure flaky expanded graphite-graphene oxide hybrid material under reduced pressure, and heating and curing to obtain the heat-conducting polymer matrix composite material formed by taking the three-dimensional structure flaky expanded graphite-graphene oxide hybrid heat conductor as a heat-conducting filler and taking the polydimethylsiloxane mixture as a polymer matrix.
The pressure of the decompression injection process in the step (2) is-15 Pa to-30 Pa.
The time of the decompression injection process in the step (2) is 2-6 h.
And (2) heating and curing in three temperature sections of 110-130 ℃, 130-150 ℃ and 180-210 ℃ in sequence.
The heating curing time of each temperature section in the step (2) is 2-4 h.
In the technical scheme of the invention, the graphene oxide, the flaky expanded graphite and the water in the step (1) are mixed according to the mass ratio of 1: 5-50: 50-100.
Preferably, the sheet-like expanded graphite sheet has a transverse dimension of from 10 μm to 500. mu.m, such as 10 μm, 20 μm, 25 μm, 50 μm, 80 μm, 100 μm, 150 μm, 200 μm, 220 μm, 300 μm, 400 μm, or 500 μm, and the like.
Preferably, the lateral dimension of the graphene oxide is 0.5 μm to 10 μm, such as 500nm, 550nm, 800nm, 1 μm, 2 μm, 3 μm, 4 μm, 6 μm, 8 μm, or 10 μm, and the like.
Preferably, the thickness of the exfoliated expanded graphite is from 100nm to 2 μm, for example, 100nm, 210nm, 300nm, 500nm, 1 μm or 2 μm.
Preferably, the mass percentage of the graphene oxide is 2.5% to 25%, for example, 2.5%, 3%, 4%, 5%, 8%, 10%, 12%, 15%, 18%, 20%, 22%, 24% or 25% based on 100% of the total mass of the hybrid material.
In a second aspect, the present invention provides a method for producing a vertically oriented three-dimensional expanded graphite heat conductor as described in the first aspect, the method comprising the steps of:
(1) adding flaky expanded graphite flakes into a graphene oxide aqueous solution under the condition of ball milling and blending to obtain flaky expanded graphite-graphite oxide aqueous mixed solution;
(2) freezing the flake expanded graphite-graphite oxide mixed solution to form a frozen mixed solution, and freezing and drying the frozen mixed solution to obtain the flake expanded graphite-graphene oxide hybrid heat conductor with a three-dimensional continuous structure.
In the technical scheme of the invention, the mixed liquid of the flake expanded graphite and the graphite oxide in the step (1) does not contain a surfactant.
In the present invention, the flake-shaped expanded graphite-graphite oxide mixed solution is prepared by using mechanical stirring because the mechanical stirring can prevent the crushing of the expanded graphite.
The addition of the graphene oxide in the invention has two main functions: (1) the graphene oxide can be connected with adjacent flaky expanded graphite sheets to serve as a heat-conducting bridge to enhance heat transfer between the adjacent flaky expanded graphite sheets, reduce interface thermal resistance between the flaky expanded graphite sheets and the graphene, and improve the heat-conducting property of the integral vertically-oriented three-dimensional expanded graphite heat conductor; (2) the graphene oxide can also play a role in supporting the vertically-oriented three-dimensional expanded graphite heat conductor, so that the mechanical property of the three-dimensional heat conductor is improved, and the collapse of the vertically-oriented three-dimensional expanded graphite heat conductor in the subsequent decompression operation is avoided.
Preferably, the graphene oxide, the flaky expanded graphite and the water in the step (1) are mixed according to a mass ratio of 1: 5-50: 50-100.
Preferably, the rotation speed of the mechanical stirring in the step (1) is 30rpm to 60rpm, such as 30rpm, 33rpm, 34rpm, 40rpm, 42rpm, 45rpm, 50rpm, 55rpm, 56rpm or 60rpm, etc. In the preferred technical scheme, the ball milling rotating speed is limited to 40 rpm-50 rpm, and the uniform flaky expanded graphite-graphite oxide mixed liquid is more favorably formed in the rotating speed range, and the expanded graphite can be prevented from being crushed.
Preferably, the ball milling time in the step (1) is 20-30 min, such as 20min, 22min, 24min, 26min, 28min or 30 min.
Preferably, the freezing temperature of the freezing treatment of the flake expanded graphite-graphite oxide mixed solution in the step (2) is-35 to-50 ℃, for example, -35 ℃, -38 ℃, -40 ℃, -45 ℃ or-50 ℃.
Preferably, the freezing time in step (2) is 12h to 24h, such as 12h, 13h, 16h, 17h, 18h, 19h, 20h, 21h, 22h, 23h or 24 h.
Preferably, the vacuum degree of the freeze drying treatment in the step (2) is-25 to-80 Pa, such as-20 Pa, -25Pa, -30Pa, -35Pa, -40Pa, -45Pa, -50Pa, -55Pa, -60Pa, -65Pa, -70Pa, -75Pa or-80 Pa.
Preferably, the freezing temperature of the freeze-drying treatment in the step (2) is-50 to-35 ℃, such as-50 ℃, -47 ℃, -45 ℃, -43 ℃, -40 ℃, -37 ℃ or-35 ℃.
Preferably, the freeze-drying time in the step (2) is 36-48 h, such as 36h, 37h, 38h, 39h, 40h, 41h, 42h, 43h, 44h, 45h, 46h, 47h or 48 h.
As a preferable technical scheme of the preparation method of the three-dimensional structure flaky expanded graphite-graphene oxide hybrid material, the method comprises the following steps:
(1) adding flaky expanded graphite flakes, graphene oxide, flaky expanded graphite and water into a graphene oxide aqueous solution under the condition of mechanical stirring to obtain a flaky expanded graphite-graphite oxide mixed solution;
(2) freezing the flake expanded graphite-graphite oxide mixed solution to form a frozen mixed solution, and freezing and drying the frozen mixed solution to obtain the vertically-oriented three-dimensional expanded graphite heat conductor.
In a third aspect, the present invention provides a filler, which is the vertically-oriented three-dimensional expanded graphite heat conductor of the first aspect.
In a fourth aspect, the present invention provides the use of the vertically oriented three-dimensional expanded graphite heat conductor of the first aspect as a heat conductive filler for a heat conductive polymer matrix composite.
In a fifth aspect, the present invention provides a polymer-based thermally conductive polymer-based composite material, which comprises the vertically oriented three-dimensional expanded graphite thermal conductor of the first aspect as a thermally conductive filler and a polymer matrix. Preferably, the polymer matrix is a mixture of polydimethylsiloxane, a curing agent and a catalyst, polydimethylsiloxane, polycarbonate and phenolic resin.
In an embodiment of the present invention, the thermal conductivity of the thermally conductive polymer-based composite material is 10W/(m · K) to 30W/(m · K), for example, 10W/(m · K), 15W/(m · K), 20W/(m · K), 25W/(m · K), or 30W/(m · K).
As a preferred technical solution of the heat-conducting polymer-based composite material of the present invention, the preferred technical solution provides a heat-conducting polymer-based composite material in which a vertically-oriented three-dimensional expanded graphite heat conductor is used as a heat-conducting filler and a mixture of polydimethylsiloxane, a curing agent and a catalyst is used as a polymer matrix. In the preferred technical scheme, the flake expanded graphite-graphene oxide hybrid materials with the preferred three-dimensional structures are connected with each other.
Preferably, the polymer matrix is polydimethylsiloxane.
Preferably, the curing agent is hydroxyl-terminated silicone oil.
Preferably, the catalyst is selected from platinum catalysts.
Preferably, the volume percentage of the three-dimensional structure sheet-like expanded graphite-graphene oxide hybrid material is 2.5% to 39%, for example, 2.5%, 5%, 7%, 9%, 11%, 14%, 17%, 21%, 25%, 29%, 31%, 35%, 39%, or the like, based on 100% of the total volume of the thermally conductive polymer-based composite material.
Preferably, the polydimethylsiloxane is 61% to 97.5% by volume, such as 61%, 65%, 68%, 73%, 83.2%, 93.5% or 97.5% by volume, based on 100% of the total volume of the thermally conductive polymer matrix composite.
Preferably, the volume percentage of the curing agent is 2% to 10%, such as 2%, 3%, 5%, 8%, or 10%, etc., based on 100% of the total volume of the thermally conductive polymer matrix composite.
Preferably, the volume percentage of the catalyst is 0.1% to 1%, such as 0.1%, 0.2%, 0.3%, 0.4%, 0.5%, 0.7%, or 1%, etc., based on 100% of the total volume of the thermally conductive polymer-based composite.
In the technical scheme of the invention, the total volume of all the components of the heat-conducting polymer matrix composite material is 100%.
In a sixth aspect, the present invention provides a method for preparing a thermally conductive polymer matrix composite according to the preferred embodiment of the fourth aspect, the method comprising the steps of:
(1) adding a curing agent and a catalyst into polydimethylsiloxane, and mixing to obtain a high-molecular matrix;
(2) and (2) injecting the high molecular matrix obtained in the step (1) into the three-dimensional structure flaky expanded graphite-graphene oxide hybrid material under reduced pressure, and heating and curing to obtain the heat-conducting polymer matrix composite material formed by taking the three-dimensional structure flaky expanded graphite-graphene oxide hybrid material as a filler and taking polydimethylsiloxane as the high molecular matrix.
Preferably, the pressure of the reduced pressure injection process in the step (2) is-10 Pa to-20 Pa, such as-10 Pa, -12Pa, -14Pa, -16Pa, -18Pa, or-20 Pa.
Preferably, the time of the reduced pressure injection process in the step (2) is 1h to 5h, such as 1h, 1.2h, 1.4h, 1.5h, 1.7h, 2h, 2.2h, 3.4h, 3.8h, 3.9h, 4.2h, 4.4h, 4.8h, 4.9h or 5h, and the like.
Preferably, the heating and curing in the step (2) are sequentially performed in three temperature sections of 120-140 ℃, 150-180 ℃ and 190-220 ℃;
wherein the temperature of the first temperature section can be 120 ℃, 124 ℃, 127 ℃, 130 ℃, 131 ℃, 135 ℃ or 140 ℃ and the like; the second temperature stage can be 150 deg.C, 155 deg.C, 159 deg.C, 162 deg.C, 167 deg.C, 174 deg.C or 180 deg.C; the temperature of the third temperature section may be 190 ℃, 195 ℃, 200 ℃, 205 ℃, 210 ℃, 215 ℃ or 220 ℃, etc.
Preferably, the heating curing time of each temperature section is 1h to 3h, such as 1h, 1.3h, 1.5h, 1.9h, 2.1h, 2.4h, 2.7h or 3 h.
Preferably, the heating curing time is 1 to 3 hours at the three temperatures of 130 ℃, 160 ℃ and 200 ℃ in sequence.
As a further preferable technical solution of the preparation method of the thermally conductive polymer-based composite material of the present invention, the method comprises the steps of:
(1) adding a curing agent and a catalyst into polydimethylsiloxane, and mixing to obtain a polydimethylsiloxane mixture;
(2) and (2) injecting the polydimethylsiloxane mixture obtained in the step (1) into the three-dimensional structure flaky expanded graphite-graphene oxide hybrid material under reduced pressure, and heating and curing to obtain the heat-conducting polymer matrix composite material formed by taking the three-dimensional structure flaky expanded graphite-graphene oxide hybrid material as a heat-conducting filler and taking the polydimethylsiloxane mixture as a polymer matrix.
Drawings
Fig. 1 is an SEM picture of a vertically oriented three-dimensional expanded graphite-graphene oxide thermal conductor.
Detailed Description
Examples
(1) Preparing a vertical-orientation three-dimensional expanded graphite-graphene oxide heat conductor:
expanded graphite with the diameter of 100 mu m and the thickness of 1 mu m, graphene oxide with the diameter of 5 mu m and water are mixed according to the mass ratio of 50: 1: 100, the ball milling speed is 50rpm, and the ball milling time is 1 h.
And (3) performing directional freezing treatment on the expanded graphite-graphene oxide mixed aqueous slurry, and freezing for 12 hours at the temperature of-30 ℃. Putting the frozen aqueous slurry into a freeze dryer for freeze drying treatment, wherein the vacuum degree of the freeze drying treatment is-30 Pa, the freezing temperature of the freeze drying treatment is-52 ℃, and the time of the freeze drying treatment is 24 hours; the density of the obtained vertical-orientation three-dimensional expanded graphite-graphene oxide heat conductor is 416mg/cm3. As shown in fig. 1, the vertically-oriented three-dimensional expanded graphite-graphene oxide heat conductor has a good vertically-arranged filler structure.
(2) Preparing a heat-conducting polymer matrix composite material by taking a vertically-oriented three-dimensional expanded graphite-graphene oxide heat conductor as a heat-conducting filler:
and mixing polydimethylsiloxane and hydroxyl-terminated silicone oil according to the volume ratio of 8: 1, injecting the mixture into a vertical orientation three-dimensional expanded graphite-graphene oxide heat conductor with the volume percentage of 22% under reduced pressure, wherein the pressure in the reduced pressure injection process is-25 Pa, the time of the reduced pressure injection process is 3h, and sequentially heating and curing the mixture at 135 ℃, 162 ℃ and 203 ℃ for 2h to obtain the heat-conducting polymer matrix composite material formed by taking the vertical orientation three-dimensional expanded graphite-graphene oxide heat conductor as a heat-conducting filler and taking a polydimethylsiloxane mixture as a polymer matrix.
The heat conduction composite material has high heat conductivity, the heat conductivity in the vertical direction can reach 21.5W/(m.K), and the heat conductivity in the horizontal direction can reach 8.5W/(m.K), and the heat conductivity is derived from expanded graphite and graphene oxide channels which are vertically arranged in the composite material.
Comparative example 1
In the comparative example, a polydimethylsiloxane/expanded graphite blend was obtained by directly blending polydimethylsiloxane with the same filler loading as in example 1. Subsequently, a thermally conductive polymer-based composite was prepared in the same manner as in example 1
The thermal conductivity of the thermal conductive composite material obtained by the comparative example is 2.5W/(m.K) in the vertical direction, and the thermal conductivity in the horizontal direction is 5.5W/(m.K). It is apparent that since the comparative example is a thermally conductive composite prepared by the blending method, the discontinuous expanded graphite thermal conduction path results in a lower thermal conductivity of the comparative example. The higher horizontal thermal conductivity in the comparative example is due to the fact that the expanded graphite can be oriented in the horizontal direction during the curing of the polydimethylsiloxane blend due to the effect of gravity.
The applicant states that the present invention is illustrated in detail by the above examples, but the present invention is not limited to the above detailed methods, i.e. it is not meant that the present invention must rely on the above detailed methods for its implementation. It should be understood by those skilled in the art that any modification of the present invention, equivalent substitutions of the raw materials of the product of the present invention, addition of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.
Claims (10)
1. A vertically-oriented three-dimensional expanded graphite heat conductor is characterized in that the heat conductor is composed of flaky expanded graphite and reduced graphene oxide, and the flaky expanded graphite and the reduced graphene oxide are vertically arranged in the vertically-oriented three-dimensional expanded graphite heat conductor; the vertical orientation three-dimensional expanded graphite heat conductor is of a three-dimensional structure.
2. The vertically oriented three-dimensional expanded graphite heat conductor according to claim 1, wherein the expanded graphite sheet has a lateral dimension of 10 to 500 μm and a thickness of 0.1 to 2 μm; the lateral size of the graphene oxide is 0.5-10 mu m, and the thickness of the graphene oxide is 0.74-5 nm.
3. The vertically oriented three-dimensional expanded graphite heat conductor according to claim 1, wherein the graphene oxide is present in the three-dimensional expanded graphite heat conductor at 2.5 to 25% by mass; the density of the three-dimensional expanded graphite heat conductor is 150-950 mg/cm3。
4. The preparation method of the three-dimensional structure flake expanded graphite-graphene oxide hybrid material according to any one of claims 1 to 3, wherein the method comprises the following steps:
(1) adding flaky expanded graphite into the graphene oxide aqueous slurry under the mechanical stirring state to obtain expanded graphite-graphene oxide mixed slurry;
(2) performing directional freezing treatment on the expanded graphite-graphene oxide mixed aqueous slurry, and then performing freeze drying to obtain a vertical oriented expanded graphite-graphene oxide hybrid material;
(3) carrying out high-temperature reduction treatment on the expanded graphite-graphene oxide hybrid material in a nitrogen atmosphere to obtain a vertically-oriented three-dimensional expanded graphite heat conductor;
wherein the expanded graphite-graphene oxide mixed slurry in the step (1) does not contain a surfactant component; the expanded graphite and the graphene oxide are connected through polar groups such as hydroxyl and carboxyl on the surface of the graphene oxide.
5. The method according to claim 4, wherein in the step (1), the graphene oxide, the flaky expanded graphite and the water are mixed according to a mass ratio of 1: 5-50: 50-100; the rotation speed of the mechanical stirring is 30-60 rpm, and the time is 20-30 min.
6. The method according to claim 4, wherein the step (2) is to perform vertical orientation freezing treatment on the expanded graphite-graphene oxide mixed aqueous slurry to form a frozen mixed solution, and perform freeze drying treatment on the frozen mixed solution to obtain a vertical orientation expanded graphite-graphene oxide hybrid material; the freezing temperature of the freezing treatment of the expanded graphite-graphene oxide mixed solution is-35 ℃ to 50 ℃; the freezing time of the freezing treatment is 12-24 h; the vacuum degree of the freeze drying treatment is-25 Pa to 80 Pa; the freezing temperature of the freeze drying treatment is-50 ℃ to 35 ℃.
7. A filler, wherein the filler is the vertically oriented three-dimensional expanded graphite heat conductor according to any one of claims 1 to 3.
8. Use of the vertically oriented three-dimensional expanded graphite heat conductor as claimed in any one of claims 1 to 3 as a heat conductive reinforcing filler in a heat conductive polymer matrix composite.
9. A thermally conductive polymer composite comprising the vertically oriented three-dimensional expanded graphite thermally conductive body according to any one of claims 1 to 3 as a filler and a polymer matrix.
10. A method of making a thermally conductive polymer composite as claimed in claim 9, comprising the steps of:
(1) mixing a curing agent and polydimethylsiloxane in a mechanical blending mode to prepare a polydimethylsiloxane mixture;
(2) and (2) injecting the polydimethylsiloxane mixture obtained in the step (1) into the three-dimensional structure flaky expanded graphite-graphene oxide hybrid material under reduced pressure, and heating and curing to obtain the heat-conducting polymer matrix composite material formed by taking the three-dimensional structure flaky expanded graphite-graphene oxide hybrid heat conductor as a heat-conducting filler and taking the polydimethylsiloxane mixture as a polymer matrix.
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| CN115448297A (en) * | 2022-08-26 | 2022-12-09 | 广东墨睿科技有限公司 | Method for enhancing longitudinal heat-conducting property of graphene heat-conducting film, graphene heat-conducting film and application of graphene heat-conducting film |
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