CN116082047A - Preparation method of heat dissipation in plane and high heat conduction orientation graphite plate outside plane constructed by hot pressing method - Google Patents
Preparation method of heat dissipation in plane and high heat conduction orientation graphite plate outside plane constructed by hot pressing method Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 104
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 88
- 239000010439 graphite Substances 0.000 title claims abstract description 88
- 238000007731 hot pressing Methods 0.000 title claims abstract description 39
- 238000000034 method Methods 0.000 title claims abstract description 24
- 230000017525 heat dissipation Effects 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 238000005087 graphitization Methods 0.000 claims abstract description 12
- 239000011230 binding agent Substances 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 239000000945 filler Substances 0.000 claims abstract description 4
- 238000010438 heat treatment Methods 0.000 claims description 20
- 229910021389 graphene Inorganic materials 0.000 claims description 16
- 239000011302 mesophase pitch Substances 0.000 claims description 16
- 238000001816 cooling Methods 0.000 claims description 15
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 11
- 239000004917 carbon fiber Substances 0.000 claims description 11
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 10
- 239000000843 powder Substances 0.000 claims description 5
- 239000011300 coal pitch Substances 0.000 claims description 3
- 239000011231 conductive filler Substances 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims description 2
- 239000010426 asphalt Substances 0.000 claims 1
- 239000000463 material Substances 0.000 description 4
- 239000003575 carbonaceous material Substances 0.000 description 3
- 239000002131 composite material Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000011295 pitch Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/71—Ceramic products containing macroscopic reinforcing agents
- C04B35/78—Ceramic products containing macroscopic reinforcing agents containing non-metallic materials
- C04B35/80—Fibres, filaments, whiskers, platelets, or the like
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- C01B32/20—Graphite
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/52—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite
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- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/52—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite
- C04B35/528—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite obtained from carbonaceous particles with or without other non-organic components
- C04B35/532—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite obtained from carbonaceous particles with or without other non-organic components containing a carbonisable binder
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- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
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- C04B2235/5208—Fibers
- C04B2235/5216—Inorganic
- C04B2235/524—Non-oxidic, e.g. borides, carbides, silicides or nitrides
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Abstract
The invention relates to a preparation method of an in-plane heat dissipation and out-of-plane high heat conduction oriented graphite plate constructed by a hot pressing method. Firstly, mixing a heat-conducting filler and a binder at a high temperature to obtain a premix, then carrying out primary hot pressing under high pressure to obtain a graphite plate with 10cm multiplied by 1cm in out-of-plane high orientation, then carrying out secondary hot pressing under low pressure to obtain a graphite block with 10cm multiplied by 1cm in-plane with certain orientation, and finally placing the graphite block into a die to carry out high-temperature graphitization to obtain the graphite block with 10cm multiplied by 1 cm. The graphite blocks subjected to the process have anisotropism, and have relatively high heat conductivity in the plane while ensuring high heat conductivity out of the plane, so that the heat transfer efficiency is obviously improved.
Description
Technical Field
The invention relates to a preparation method of an orientation graphite plate with high heat conduction in-plane heat dissipation and out-of-plane heat dissipation constructed by a hot pressing method, belonging to the field of heat conduction composite materials.
Background
With the progress of the age and the development of technology, the aerospace industry is continuously advancing, so that new requirements are put forward on the high integration of various precise components, and new requirements are put forward on the new design in the field of new materials and the ultra-high performance of the materials. One of the problems to be solved is the heat evacuation problem of the spacecraft during launching and flying, so new materials with ultra-high heat conductivity are required to be developed. The carbon material has excellent theoretical thermal conductivity, can resist high temperature and has excellent mechanical property, so the carbon material becomes one of the novel materials developed at present.
However, the heat dissipation balance between the in-plane and out-of-plane heat dissipation of the carbon material cannot be well considered in the heat dissipation process at present, so that the application in the aerospace field needs further development, and how to coordinate the heat dissipation proportion between the two is a key for solving the problem.
Disclosure of Invention
The invention aims to provide an out-of-plane high-heat-conductivity graphite plate, but certain heat dissipation capacity is required to be ensured in the in-plane direction of a graphite plate, so that a graphite block with an in-plane micro-orientation out-of-plane high orientation is prepared by adopting a secondary hot pressing and graphitization process, and the graphite block has excellent performances of in-plane heat dissipation and out-of-plane high heat conduction.
The invention adopts the following technical scheme:
the invention relates to a preparation method of an in-plane heat dissipation and out-of-plane high heat conduction oriented graphite plate constructed by a hot pressing method, which comprises the following steps:
1) Premixing: in a horizontal mixer, respectively mixing the heat-conducting filler with the binder according to a certain mass ratio at 60 ℃ for 1h;
2) Primary hot pressing: filling the premixed expanded graphite/chopped carbon fiber/graphene oxide-mesophase pitch powder into a graphite mold with the volume of 10cm multiplied by 10cm, placing the graphite mold in a vacuum hot press, heating to the softening point of the mesophase pitch with the temperature of 280 ℃ at 3-5 ℃/min, preserving heat for 1-2 hours, heating to the temperature of 1500-2000 ℃ at 5-10 ℃/min, preserving heat for 1-2 hours, applying 30-80Mpa pressure, maintaining the pressure for 1-2 hours, and naturally cooling to room temperature after the hot pressing is finished to obtain a graphite plate with the volume of 10cm multiplied by 1 cm;
3) And (3) secondary hot pressing: filling a graphite plate prepared by primary hot pressing into a graphite mould with the length of 10cm multiplied by 1cm multiplied by 10cm, putting the graphite plate into a vacuum hot press again, heating to 1500-2000 ℃ at the speed of 5-10 ℃/min, preserving heat for 1-2h, applying 5-20Mpa, maintaining the pressure for 1-2h, and naturally cooling to room temperature after the hot pressing is finished to obtain a graphite block with the length of 10cm multiplied by 1 cm;
4) Graphitizing: filling a 10cm multiplied by 1cm graphite block into a 10cm multiplied by 1cm graphene mould to fix the shape, placing the graphite block into a high-temperature graphitization furnace, heating to 2500-3000 ℃ at 5-10 ℃/min, preserving heat for 0.5-1h, and naturally cooling to room temperature after the graphitization process is finished to obtain the 10cm multiplied by 1cm horizontally micro-oriented vertically highly oriented graphite block.
Preferably, the heat conductive filler in step 1) is expanded graphite/chopped carbon fiber/graphene oxide.
Preferably, the binder of step 1) is mesophase pitch/coal pitch.
Preferably, the mass ratio of step 1) is 9:1, 8:2, 7:3.
Preferably, the density of the 10cm X1 cm graphite sheet obtained in step 2) is 1.5-2.5g/cm 3 。
Preferably, the density of the 10 cm. Times.1 cm graphite blocks obtained in step 3) is from 2.1 to 2.8g/cm 3 。
Preferably, the sheet diameter of the expanded graphite is 100-300 μm; the length of the chopped carbon fiber is 3-12mm, and the diameter is 5-8 mu m; the sheet diameter of the graphene oxide is 200-400 mu m.
Preferably, the pitch particle size is 10-50 μm.
The invention has the advantages that: the preparation process is mature and controllable, the preparation time is short, raw materials are easy to obtain, the out-of-plane thermal conductivity of the prepared graphite block can reach 1500-2000W/mK, the in-plane thermal conductivity also has 50-200W/mK, compared with the thermal conductivity of the commercial graphite plate in the vertical and horizontal directions, and in addition, the mechanical property of the graphite block is obviously improved.
Description of the drawings:
FIG. 1 is a schematic diagram of the structure of the present invention;
FIG. 2 is a scanning electron microscope image of the present invention;
Detailed Description
The following 3 examples of the invention are given as further illustration of the invention and are not intended to limit the scope of the invention.
Example 1
1) Premixing: in a horizontal mixer, mixing the expanded graphite with mesophase pitch according to the mass ratio of 9:1 at 60 ℃ for 1h;
2) Primary hot pressing: filling the premixed expanded graphite/chopped carbon fiber/graphene oxide-mesophase pitch powder into a graphite mold with the volume of 10cm multiplied by 10cm, placing the graphite mold in a vacuum hot press, heating to the softening point of mesophase pitch with the temperature of 280 ℃ at 5 ℃/min, preserving heat for 2 hours, heating to 2000 ℃ with the temperature of 10 ℃/min, preserving heat for 2 hours, applying 80Mpa pressure, maintaining the pressure for 1 hour, and naturally cooling to room temperature after hot pressing is finished to obtain a graphite plate with the volume of 10cm multiplied by 1 cm;
3) And (3) secondary hot pressing: filling a graphite plate prepared by primary hot pressing into a graphite mould with the length of 10cm multiplied by 1cm multiplied by 10cm, putting the graphite plate into a vacuum hot press again, heating to 2000 ℃ at the speed of 10 ℃/min, preserving heat for 1h, applying 5Mpa, preserving pressure for 1h, and naturally cooling to room temperature after the hot pressing is finished to obtain a graphite block with the length of 10cm multiplied by 1 cm;
4) Graphitizing: filling a 10cm multiplied by 1cm graphite block into a 10cm multiplied by 1cm graphene mould to fix the shape, placing the graphite block into a high-temperature graphitization furnace, heating to 2800 ℃ at a speed of 10 ℃/min, preserving heat for 0.5h, and naturally cooling to room temperature after the graphitization process is finished to obtain the 10cm multiplied by 1cm horizontally micro-oriented vertically highly oriented graphite block.
Example 2
1) Premixing: in a horizontal mixer, mixing chopped carbon fibers with mesophase pitch according to a mass ratio of 8:2 at 60 ℃ for 1h;
2) Primary hot pressing: filling the premixed expanded graphite/chopped carbon fiber/graphene oxide-mesophase pitch powder into a graphite mold with the volume of 10cm multiplied by 10cm, placing the graphite mold in a vacuum hot press, heating to the softening point of mesophase pitch with the temperature of 280 ℃ at 5 ℃/min, preserving heat for 2 hours, heating to 2000 ℃ with the temperature of 10 ℃/min, preserving heat for 2 hours, applying 50Mpa pressure, maintaining the pressure for 1 hour, and naturally cooling to room temperature after hot pressing is finished to obtain a graphite plate with the volume of 10cm multiplied by 1 cm;
3) And (3) secondary hot pressing: filling a graphite plate prepared by primary hot pressing into a graphite mould with the length of 10cm multiplied by 1cm multiplied by 10cm, putting the graphite plate into a vacuum hot press again, heating to 2000 ℃ at the speed of 10 ℃/min, preserving heat for 1h, applying 10Mpa, preserving pressure for 1h, and naturally cooling to room temperature after the hot pressing is finished to obtain a graphite block with the length of 10cm multiplied by 1 cm;
4) Graphitizing: filling a 10cm multiplied by 1cm graphite block into a 10cm multiplied by 1cm graphene mould to fix the shape, placing the graphite block into a high-temperature graphitization furnace, heating to 2800 ℃ at a speed of 10 ℃/min, preserving heat for 1h, and naturally cooling to room temperature after the graphitization process is finished to obtain the 10cm multiplied by 1cm horizontally micro-oriented vertically highly oriented graphite block.
Example 3
1) Premixing: in a horizontal mixer, mixing graphene oxide with mesophase pitch according to a mass ratio of 9:1 at 60 ℃ for 1h;
2) Primary hot pressing: filling the premixed expanded graphite/chopped carbon fiber/graphene oxide-mesophase pitch powder into a graphite mold with the volume of 10cm multiplied by 10cm, placing the graphite mold in a vacuum hot press, heating to the softening point of mesophase pitch with the temperature of 280 ℃ at 5 ℃/min, preserving heat for 2 hours, heating to 2000 ℃ with the temperature of 10 ℃/min, preserving heat for 2 hours, applying 60Mpa pressure, maintaining the pressure for 1 hour, and naturally cooling to room temperature after hot pressing is finished to obtain a graphite plate with the volume of 10cm multiplied by 1 cm;
3) And (3) secondary hot pressing: filling a graphite plate prepared by primary hot pressing into a graphite mould with the length of 10cm multiplied by 1cm multiplied by 10cm, putting the graphite plate into a vacuum hot press again, heating to 2000 ℃ at the speed of 10 ℃/min, preserving heat for 1h, applying 5Mpa, preserving pressure for 1h, and naturally cooling to room temperature after the hot pressing is finished to obtain a graphite block with the length of 10cm multiplied by 1 cm;
4) Graphitizing: filling a 10cm multiplied by 1cm graphite block into a 10cm multiplied by 1cm graphene mould to fix the shape, placing the graphite block into a high-temperature graphitization furnace, heating to 2800 ℃ at a speed of 10 ℃/min, preserving heat for 0.5h, and naturally cooling to room temperature after the graphitization process is finished to obtain the 10cm multiplied by 1cm horizontally micro-oriented vertically highly oriented graphite block.
The foregoing has described exemplary embodiments of the invention, it being understood that any simple variations, modifications, or other equivalent arrangements which would not unduly obscure the invention may be made by those skilled in the art without departing from the spirit of the invention.
Claims (8)
1. The preparation method of the oriented graphite plate with the functions of in-plane heat dissipation and out-of-plane high heat conduction by using a hot pressing method is characterized by comprising the following steps of:
1) Premixing: in a horizontal mixer, respectively mixing the heat-conducting filler with the binder according to a certain mass ratio at 60 ℃ for 1h;
2) Primary hot pressing: filling the premixed expanded graphite/chopped carbon fiber/graphene oxide-mesophase pitch powder into a graphite mold with the volume of 10cm multiplied by 10cm, placing the graphite mold in a vacuum hot press, heating to the softening point of the mesophase pitch with the temperature of 280 ℃ at 3-5 ℃/min, preserving heat for 1-2 hours, heating to the temperature of 1500-2000 ℃ at 5-10 ℃/min, preserving heat for 1-2 hours, applying 30-80Mpa pressure, maintaining the pressure for 1-2 hours, and naturally cooling to room temperature after the hot pressing is finished to obtain a graphite plate with the volume of 10cm multiplied by 1 cm;
3) And (3) secondary hot pressing: filling a graphite plate prepared by primary hot pressing into a graphite mould with the length of 10cm multiplied by 1cm multiplied by 10cm, putting the graphite plate into a vacuum hot press again, heating to 1500-2000 ℃ at the speed of 5-10 ℃/min, preserving heat for 1-2h, applying 5-20Mpa, maintaining the pressure for 1-2h, and naturally cooling to room temperature after the hot pressing is finished to obtain a graphite block with the length of 10cm multiplied by 1 cm;
4) Graphitizing: filling a 10cm multiplied by 1cm graphite block into a 10cm multiplied by 1cm graphene mould to fix the shape, placing the graphite block into a high-temperature graphitization furnace, heating to 2500-3000 ℃ at 5-10 ℃/min, preserving heat for 0.5-1h, and naturally cooling to room temperature after the graphitization process is finished to obtain the 10cm multiplied by 1cm horizontally micro-oriented vertically highly oriented graphite block.
2. The method for preparing the oriented graphite plate with in-plane heat dissipation and out-of-plane high heat conduction by using the hot pressing method according to claim 1 is characterized in that: the heat conducting filler in the step 1) is expanded graphite/chopped carbon fiber/graphene oxide.
3. The method for preparing the oriented graphite plate with in-plane heat dissipation and out-of-plane high heat conduction by using the hot pressing method according to claim 1 is characterized in that: the binder in the step 1) is mesophase pitch/coal pitch.
4. The method for preparing the oriented graphite plate with in-plane heat dissipation and out-of-plane high heat conduction by using the hot pressing method according to claim 1 is characterized in that: the mass ratio of the step 1) is 9:1, 8:2 and 7:3.
5. The method for preparing the oriented graphite plate with in-plane heat dissipation and out-of-plane high heat conduction by using the hot pressing method according to claim 1 is characterized in that: the density of the 10cm x 1cm graphite sheet obtained in step 2) is 1.5-2.5g/cm 3 。
6. The method for preparing the oriented graphite plate with in-plane heat dissipation and out-of-plane high heat conduction by using the hot pressing method according to claim 1 is characterized in that: the density of the 10cm x 1cm graphite block obtained in the step 3) is 2.1-2.8g/cm 3 。
7. The thermally conductive filler of claim 2 being expanded graphite/chopped carbon fiber/graphene oxide, characterized in that: the sheet diameter of the expanded graphite is 100-300 mu m; the length of the chopped carbon fiber is 3-12mm, and the diameter is 5-8 mu m; the sheet diameter of the graphene oxide is 200-400 mu m.
8. A binder according to claim 3 which is mesophase pitch/coal pitch, characterized in that: the particle size of asphalt is 10-50 μm.
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