CN113829406B - Preparation method of heat conducting fin - Google Patents
Preparation method of heat conducting fin Download PDFInfo
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- CN113829406B CN113829406B CN202111318327.XA CN202111318327A CN113829406B CN 113829406 B CN113829406 B CN 113829406B CN 202111318327 A CN202111318327 A CN 202111318327A CN 113829406 B CN113829406 B CN 113829406B
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- 238000002360 preparation method Methods 0.000 title abstract description 11
- 239000000463 material Substances 0.000 claims abstract description 59
- 239000000945 filler Substances 0.000 claims abstract description 24
- 238000003825 pressing Methods 0.000 claims abstract description 23
- 239000000203 mixture Substances 0.000 claims abstract description 17
- 239000011230 binding agent Substances 0.000 claims abstract description 11
- 238000005520 cutting process Methods 0.000 claims abstract description 10
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 239000002994 raw material Substances 0.000 claims abstract description 5
- 238000000034 method Methods 0.000 claims description 77
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 75
- 239000011231 conductive filler Substances 0.000 claims description 50
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 40
- 239000004917 carbon fiber Substances 0.000 claims description 40
- 239000002041 carbon nanotube Substances 0.000 claims description 27
- 229910021393 carbon nanotube Inorganic materials 0.000 claims description 27
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 27
- 229910002804 graphite Inorganic materials 0.000 claims description 23
- 239000010439 graphite Substances 0.000 claims description 23
- 229910021389 graphene Inorganic materials 0.000 claims description 22
- 229910052582 BN Inorganic materials 0.000 claims description 21
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 21
- -1 polymethylsiloxane Polymers 0.000 claims description 16
- 230000003746 surface roughness Effects 0.000 claims description 16
- 238000004519 manufacturing process Methods 0.000 claims description 15
- 239000002245 particle Substances 0.000 claims description 15
- 238000001125 extrusion Methods 0.000 claims description 13
- 238000004073 vulcanization Methods 0.000 claims description 13
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 12
- 229920005989 resin Polymers 0.000 claims description 10
- 239000011347 resin Substances 0.000 claims description 10
- 238000005229 chemical vapour deposition Methods 0.000 claims description 9
- 239000007788 liquid Substances 0.000 claims description 9
- 229920001296 polysiloxane Polymers 0.000 claims description 9
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 8
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 8
- 229920001187 thermosetting polymer Polymers 0.000 claims description 7
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 6
- 229910021382 natural graphite Inorganic materials 0.000 claims description 6
- 239000000377 silicon dioxide Substances 0.000 claims description 6
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 claims description 5
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 5
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 5
- OTKXURHKRLMLIY-UHFFFAOYSA-N [SiH3]O[SiH2]C#N Chemical compound [SiH3]O[SiH2]C#N OTKXURHKRLMLIY-UHFFFAOYSA-N 0.000 claims description 4
- 229920000297 Rayon Polymers 0.000 claims description 3
- 229920001807 Urea-formaldehyde Polymers 0.000 claims description 3
- 238000001241 arc-discharge method Methods 0.000 claims description 3
- 229910021383 artificial graphite Inorganic materials 0.000 claims description 3
- 239000003822 epoxy resin Substances 0.000 claims description 3
- 238000000608 laser ablation Methods 0.000 claims description 3
- 239000002048 multi walled nanotube Substances 0.000 claims description 3
- 239000005011 phenolic resin Substances 0.000 claims description 3
- 229920000647 polyepoxide Polymers 0.000 claims description 3
- 229920001721 polyimide Polymers 0.000 claims description 3
- 239000009719 polyimide resin Substances 0.000 claims description 3
- 229920002635 polyurethane Polymers 0.000 claims description 3
- 239000004814 polyurethane Substances 0.000 claims description 3
- 229920002050 silicone resin Polymers 0.000 claims description 3
- 239000002109 single walled nanotube Substances 0.000 claims description 3
- 239000002904 solvent Substances 0.000 claims description 3
- 229920006305 unsaturated polyester Polymers 0.000 claims description 3
- 235000012239 silicon dioxide Nutrition 0.000 claims description 2
- 238000004299 exfoliation Methods 0.000 claims 2
- 238000004381 surface treatment Methods 0.000 abstract description 3
- 239000000853 adhesive Substances 0.000 description 13
- 230000001070 adhesive effect Effects 0.000 description 13
- 238000012360 testing method Methods 0.000 description 12
- 230000000052 comparative effect Effects 0.000 description 4
- 238000007731 hot pressing Methods 0.000 description 4
- 238000007711 solidification Methods 0.000 description 4
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000011031 large-scale manufacturing process Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 229920001568 phenolic resin Polymers 0.000 description 2
- 230000008023 solidification Effects 0.000 description 2
- 238000003490 calendering Methods 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B26—HAND CUTTING TOOLS; CUTTING; SEVERING
- B26D—CUTTING; DETAILS COMMON TO MACHINES FOR PERFORATING, PUNCHING, CUTTING-OUT, STAMPING-OUT OR SEVERING
- B26D1/00—Cutting through work characterised by the nature or movement of the cutting member or particular materials not otherwise provided for; Apparatus or machines therefor; Cutting members therefor
- B26D1/01—Cutting through work characterised by the nature or movement of the cutting member or particular materials not otherwise provided for; Apparatus or machines therefor; Cutting members therefor involving a cutting member which does not travel with the work
- B26D1/04—Cutting through work characterised by the nature or movement of the cutting member or particular materials not otherwise provided for; Apparatus or machines therefor; Cutting members therefor involving a cutting member which does not travel with the work having a linearly-movable cutting member
- B26D1/06—Cutting through work characterised by the nature or movement of the cutting member or particular materials not otherwise provided for; Apparatus or machines therefor; Cutting members therefor involving a cutting member which does not travel with the work having a linearly-movable cutting member wherein the cutting member reciprocates
- B26D1/08—Cutting through work characterised by the nature or movement of the cutting member or particular materials not otherwise provided for; Apparatus or machines therefor; Cutting members therefor involving a cutting member which does not travel with the work having a linearly-movable cutting member wherein the cutting member reciprocates of the guillotine type
- B26D1/09—Cutting through work characterised by the nature or movement of the cutting member or particular materials not otherwise provided for; Apparatus or machines therefor; Cutting members therefor involving a cutting member which does not travel with the work having a linearly-movable cutting member wherein the cutting member reciprocates of the guillotine type with a plurality of cutting members
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C35/00—Heating, cooling or curing, e.g. crosslinking or vulcanising; Apparatus therefor
- B29C35/02—Heating or curing, e.g. crosslinking or vulcanizing during moulding, e.g. in a mould
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/001—Combinations of extrusion moulding with other shaping operations
- B29C48/0022—Combinations of extrusion moulding with other shaping operations combined with cutting
-
- 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
Abstract
The invention provides a preparation method of a heat conducting fin, which comprises the following steps: mixing the raw materials of all components of the heat conducting sheet to obtain a mixed material, wherein the mixed material comprises a binder and an anisotropic filler; extruding the mixed material into a sheet; placing a plurality of sheets into a mold frame, wherein the mold frame is provided with an inner cavity with one end being open; inserting an upward pressing structure with a plurality of inserting sheets into the mixed material of the mold frame by pressing to form a mold for preparing the heat conducting sheet, so that the anisotropic heat conducting filler in the material is perpendicular to the inserting sheets; vulcanizing the mixed material; demolding the vulcanized mixture to obtain the heat conducting sheets with anisotropic heat conducting fillers arranged along the direction perpendicular to the inserting sheets. The invention solves the problem of surface treatment while cutting through the die with the inserting sheet.
Description
Technical Field
The invention belongs to the technical field of heat conduction and dissipation, and particularly relates to a preparation method of a heat conduction sheet.
Background
Currently, the principle of extrusion method is that anisotropic heat conductive filler (such as carbon fiber) is directionally arranged along the flowing direction of fluid in the process of extruding materials by an extruder; and stacking, hot-pressing, solidifying and slicing the extruded materials to obtain the longitudinal high-heat-conductivity gasket.
However, this method has the following problems:
1. the surface of the cured and cut sample is rough (roughness is 10-30um and even higher), and the consequence is that when the gasket is applied, the contact effect is poor, so that the interface thermal resistance is obviously increased;
2. for the problem of rough surface of a sample cut after solidification, the solution 1 is to polish the surface, but the gaskets are very soft products, so that polishing is very difficult, and the effect of reducing the roughness is difficult to achieve;
3. for the problem of rough surface of a sample cut after solidification, in the solution 2, after semi-solidification cutting, pressing is carried out to enable the upper surface and the lower surface to be smoother, but the semi-solidification degree is not well controlled, and meanwhile, the directionality of anisotropic heat conduction filler in the material is reduced, so that the heat conduction performance is reduced;
4. either scheme 1 or scheme 2 makes the preparation process more complicated and does not solve the problem well.
Disclosure of Invention
In view of one or more of the problems in the prior art, the present invention provides a method for preparing a thermally conductive sheet, comprising:
mixing the raw materials of all components of the heat conducting sheet to obtain a mixed material, wherein the mixed material comprises a binder and an anisotropic filler;
extruding the mixed material into a sheet;
placing a plurality of sheets into a mold frame, wherein the mold frame is provided with an inner cavity with one end being open;
inserting an upward pressing structure with a plurality of inserting sheets into the mixed material of the mold frame by pressing to form a mold for preparing the heat conducting sheet, so that the anisotropic heat conducting filler in the material is perpendicular to the inserting sheets;
vulcanizing the mixed material;
demolding the vulcanized mixture to obtain the heat conducting sheets with anisotropic heat conducting fillers arranged along the direction perpendicular to the inserting sheets.
Optionally, the step of placing a plurality of sheets into the mold frame, wherein the plurality of sheets has a height not less than a height of an inner cavity of the mold.
Optionally, before the step of extruding the mixture into a sheet, the method further comprises:
and removing bubbles from the mixed material in vacuum.
Optionally, in the step of extruding the mixed material into a sheet, the mixed material is extruded into a sheet by an extruder, wherein the extruder is at least one of a single screw extruder, a twin screw extruder and a non-screw extruder, preferably, the extrusion thickness is 0.5-3mm, preferably 1-2mm, and the extrusion rate is 1-10mm/s, preferably 3-7mm/s.
Optionally, in the step of vulcanizing the mixed material, vulcanization is performed at normal temperature or below 150 ℃.
Optionally, the anisotropic thermally conductive filler comprises a one-dimensional thermally conductive filler or/and a two-dimensional thermally conductive filler.
Optionally, the one-dimensional heat conducting filler comprises carbon nanotubes or/and carbon fibers;
preferably, the carbon nanotube thermally conductive sheet preparation method is at least one selected from the group consisting of a laser ablation method, an arc discharge method, and a Chemical Vapor Deposition (CVD) method;
preferably, the carbon nanotubes are selected from at least one of single-walled carbon nanotubes and multi-walled carbon nanotubes;
preferably, the diameter of the carbon nanotubes is 2-200nm, more preferably 10-100nm;
preferably, the length of the carbon nanotubes is 10-300 μm, more preferably 20-150 μm;
preferably, the thermal conductivity of the carbon nanotubes is 500W/(m·k) or more, more preferably 1000W/(m·k) or more;
preferably, the carbon nanotubes are contained in the thermally conductive sheet in an amount of 20wt.% to 80wt.%; more preferably 40wt.% to 65wt.%.
Optionally, the carbon fiber is selected from at least one of a viscose-based carbon fiber, a pitch-based carbon fiber, and a PAN-based carbon fiber; preferably pitch-based carbon fibers;
preferably, the carbon fibers have a length of 10-600 μm, more preferably 100-400 μm;
preferably, the carbon fibers have a diameter of 10-30 μm, more preferably 8-15 μm;
preferably, the carbon fiber has a thermal conductivity of 600W/(mK) or more, more preferably 1000W/(mK) or more;
preferably, the carbon fiber is contained in the thermally conductive sheet in an amount of 20wt.% to 80wt.%, more preferably 40wt.% to 65wt.%.
Optionally, the two-dimensional heat conductive filler is selected from at least one of boron nitride, graphene, graphite and boron nitride;
preferably, the boron nitride is specifically hexagonal boron nitride;
preferably, the boron nitride has a sheet diameter of 0.05-400 μm, more preferably 50-300 μm;
preferably, the content of the boron nitride in the thermally conductive sheet is 20wt.% to 80wt.%, more preferably 40wt.% to 65wt.%;
preferably, the preparation method of the graphene heat-conducting sheet is at least one of a chemical vapor deposition method, a self-mechanical stripping method, a redox method and a solvent stripping method;
preferably, the graphene has a sheet diameter of 1-400 μm, more preferably 10-200 μm;
preferably, the graphene has a thermal conductivity of 700W/(m·k) or more, more preferably 1200W/(m·k) or more;
preferably, the graphene is present in the thermally conductive sheet in an amount of 20wt.% to 80wt.%, more preferably 40wt.% to 65wt.%;
preferably, the graphite sheet is selected from at least one of graphitized natural graphite, graphitized expanded graphite, natural graphite, expanded graphite, and artificial graphite.
Preferably, the graphite has a sheet diameter of 1-400 μm, more preferably 20-200 μm;
preferably, the graphite has a thickness of 0.01-10 μm, more preferably 1-5 μm;
preferably, the graphite is present in the thermally conductive sheet in an amount of 20wt.% to 80wt.%, more preferably 40wt.% to 65wt.%.
Optionally, the mixture further comprises an isotropic heat conductive filler, wherein the isotropic heat conductive filler comprises at least one of aluminum oxide, aluminum nitride, silicon carbide and silicon dioxide;
preferably, the particle size of the isotropic heat conductive filler is 0.1-120 μm, preferably 5-50 μm; the isotropic heat conductive filler is present in an amount of 10wt.% to 60wt.%.
Optionally, the binder accounts for 10wt.% to 50wt.% of the thermally conductive sheet;
preferably, the binder is a thermosetting resin;
further preferably, the thermosetting resin is at least one selected from the group consisting of epoxy resin, unsaturated polyester, phenolic resin, polymethylsiloxane, silicone resin, liquid silicone gum, phthaldiallyl resin, polyimide resin, urea resin and polyurethane, preferably liquid silicone gum;
further preferably, the liquid silicone gum comprises one or more of polydimethylsiloxane, dimethylcyclosiloxane, alpha, omega-dihydroxypolydimethylsiloxane, alpha, omega-dihydroxypolymethyl3, 3-trifluoropropyl siloxane, polydiphenylsiloxane, cyanosiloxysilane, and alpha, omega-diethylpolydimethylsiloxane.
The preparation method of the heat conducting fin solves the problem of surface treatment while cutting through the die with the inserting sheet, namely realizes cutting and surface treatment in one step, realizes stable product, keeps the internal structure of the product and can realize the purpose of large-scale production.
According to the invention, the smooth inserting sheets are inserted into the mixed material in a certain direction and at a certain interval, so that the anisotropic heat conduction filler in the mixed material is perpendicular to the inserting sheets, the anisotropic heat conduction filler is directly solidified and molded in a mold, and after demolding, the inserting sheets are removed, so that the heat conduction sheets with the anisotropic heat conduction filler arranged along the longitudinal direction are directly obtained, the process steps are simplified, and the product stability is realized.
Drawings
The accompanying drawings are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate the invention and together with the embodiments of the invention, serve to explain the invention. In the drawings:
fig. 1 is a schematic view of a flowchart of a method for manufacturing a thermally conductive sheet according to the present invention;
FIG. 2 is a schematic view showing an example of using a mold and a release frame in the method for producing a thermally conductive sheet according to the present invention;
FIG. 3 is a schematic view of another embodiment of the method for producing a thermally conductive sheet according to the present invention using a mold and a release frame;
fig. 4 is a photograph of a thermally conductive sheet obtained by the production method of example 1;
fig. 5 is a photograph of the thermally conductive sheet obtained by the production method of comparative example 1.
Detailed Description
Hereinafter, only certain exemplary embodiments are briefly described. As will be recognized by those of skill in the pertinent art, the described embodiments may be modified in various different ways without departing from the spirit or scope of the present invention. Accordingly, the drawings and description are to be regarded as illustrative in nature and not as restrictive.
The following disclosure provides many different embodiments, or examples, for implementing different features of the invention. They are, of course, merely examples and are not intended to limit the invention. In addition, the present invention provides examples of various specific processes and materials, but one of ordinary skill in the art will recognize the application of other processes and/or the use of other materials.
The preferred embodiments of the present invention will be described below with reference to the accompanying drawings, it being understood that the preferred embodiments described herein are for illustration and explanation of the present invention only, and are not intended to limit the present invention.
Fig. 1 is a schematic view of a flowchart of a method for preparing a thermally conductive sheet according to the present invention, as shown in fig. 1, the method comprising:
step S1, mixing the raw materials of the components of the heat conducting fin to obtain a mixed material, wherein the mixed material comprises a binder and an anisotropic filler;
step S2, extruding the mixed material into a sheet-shaped sheet;
step S3, placing a plurality of sheets into a mold frame 12 (shown in fig. 2 and 3) having an inner cavity with one end open;
step S4, inserting an upward pressing structure 11 with a plurality of inserting sheets 111 into the mixed material of the mold frame by pressing to form a mold for preparing the heat conducting sheet, so that the anisotropic heat conducting filler in the material is perpendicular to the inserting sheets;
s5, vulcanizing the mixed material;
and S6, demolding the vulcanized mixture to obtain the heat conducting sheets with anisotropic heat conducting fillers arranged along the direction perpendicular to the inserting sheets.
Preferably, the surface roughness of the insert sheet is 0.01-0.50 μm, preferably 0.01-0.10 μm.
According to the preparation method of the heat conducting fin, the mixed materials can be directionally controlled, so that the stability of the product is realized; the heat conducting fin has good formability and does not need cutting; controlling some fluidity components in the mixed material so as not to influence the distribution of the filler in the heat conducting sheet, especially the orientation of the anisotropic heat conducting filler; the process is simple, and the large-scale production difficulty is small.
In one embodiment, step S2 is preceded by:
and removing bubbles from the mixed material in vacuum.
In one embodiment, in step S1, the anisotropic heat conductive filler includes a one-dimensional heat conductive filler or/and a two-dimensional heat conductive filler, wherein:
the one-dimensional heat conduction filler comprises carbon nano tubes or/and carbon fibers;
in one embodiment, the carbon nanotube thermally conductive sheet manufacturing method is selected from at least one of a laser ablation method, an arc discharge method, and a Chemical Vapor Deposition (CVD) method.
Preferably, the carbon nanotubes are selected from single-walled carbon nanotubes or/and multi-walled carbon nanotubes.
Preferably, the diameter of the carbon nanotubes is 2-200nm, more preferably 10-100nm.
Preferably, the carbon nanotubes have a length of 10-300 μm, more preferably 20-150 μm.
Preferably, the carbon nanotubes have a thermal conductivity of 500W/(mK) or more, more preferably 1000W/(mK) or more.
Preferably, the carbon nanotubes are contained in the thermally conductive sheet in an amount of 20wt.% to 80wt.%; more preferably 40wt.% to 65wt.%.
In one embodiment, the carbon fibers are selected from at least one of viscose-based carbon fibers, pitch-based carbon fibers, and PAN-based carbon fibers; pitch-based carbon fibers are preferred.
Preferably, the carbon fibers have a length of 10-600 μm, more preferably 100-400 μm.
Preferably, the carbon fibers have a diameter of 10-30 μm, more preferably 8-15 μm.
Preferably, the carbon fiber has a thermal conductivity of 600W/(mK) or more, more preferably 1000W/(mK) or more.
Preferably, the carbon fiber is contained in the thermally conductive sheet in an amount of 20wt.% to 80wt.%, more preferably 40wt.% to 65wt.%.
In one embodiment, the two-dimensional thermally conductive filler is selected from at least one of boron nitride, graphene, graphite, and boron nitride.
Preferably, the boron nitride is specifically hexagonal boron nitride.
Preferably, the boron nitride has a sheet diameter of 0.05 to 400. Mu.m, more preferably 50 to 300. Mu.m.
Preferably, the boron nitride is contained in the thermally conductive sheet in an amount of 20wt.% to 80wt.%, more preferably 40wt.% to 65wt.%.
Preferably, the graphene heat-conducting sheet preparation method is at least one selected from a chemical vapor deposition method, a self-mechanical stripping method, a redox method and a solvent stripping method.
Preferably, the graphene has a sheet diameter of 1-400 μm, more preferably 10-200 μm.
Preferably, the graphene has a thermal conductivity of 700W/(m·k) or more, more preferably 1200W/(m·k) or more.
Preferably, the graphene is contained in the thermally conductive sheet in an amount of 20wt.% to 80wt.%, more preferably 40wt.% to 65wt.%.
Preferably, the graphite sheet is selected from at least one of graphitized natural graphite, graphitized expanded graphite, natural graphite, expanded graphite, and artificial graphite.
Preferably, the graphite has a sheet diameter of 1 to 400. Mu.m, more preferably 20 to 200. Mu.m.
Preferably, the graphite has a thickness of 0.01 to 10. Mu.m, more preferably 1 to 5. Mu.m.
Preferably, the graphite is present in the thermally conductive sheet in an amount of 20wt.% to 80wt.%, more preferably 40wt.% to 65wt.%.
In one embodiment, the mixture further comprises an isotropic thermally conductive filler comprising at least one of alumina, aluminum nitride, silicon carbide, silica.
Preferably, the particle size of the isotropic heat conductive filler is 0.1-120 μm, preferably 5-50 μm; the isotropic heat conductive filler is present in an amount of 10wt.% to 60wt.%.
In one embodiment, the binder is present in an amount of 10wt.% to 50wt.% of the thermally conductive sheet.
Preferably, the binder is a thermosetting resin.
Further preferably, the thermosetting resin is at least one selected from the group consisting of epoxy resin, unsaturated polyester, phenolic resin, polymethylsiloxane, silicone resin, liquid silicone gum, phthaldiallyl resin, polyimide resin, urea resin and polyurethane, preferably liquid silicone gum.
Further preferably, the liquid silicone gum comprises one or more of polydimethylsiloxane, dimethylcyclosiloxane, alpha, omega-dihydroxypolydimethylsiloxane, alpha, omega-dihydroxypolymethyl3, 3-trifluoropropyl siloxane, polydiphenylsiloxane, cyanosiloxysilane, and alpha, omega-diethylpolydimethylsiloxane.
In one embodiment, in step S2, the mixture is extruded into a sheet by an extruder which is at least one of a single screw extruder, a twin screw extruder and a screw-less extruder, preferably with an extrusion thickness of 0.5-3mm, preferably 1-2mm, and an extrusion rate of 1-10mm/S, preferably 3-7mm/S.
In one embodiment, in step S3, the plurality of sheets has a height not less than a height of the cavity of the mold.
In one embodiment, in step S4, the pressing structure is combined with the mold frame by calendaring, and the plurality of inserting pieces on the pressing structure divide the mixed material placed in the mold frame into a plurality of mixed materials, and two inserting pieces are sandwiched between two sides of the mixed material, and the surface of the mixed material contacts the surface of the inserting pieces.
In one embodiment, as shown in fig. 2, a recess (not shown) corresponding to the insert plate 111 is provided in the mold frame 12, and the plurality of insert plates 111 of the upper press structure 11 are inserted into the plurality of recesses corresponding to the inner surface of the mold frame, so that the mixed material put into the mold frame is divided into a plurality of pieces of mixed material.
In one embodiment, as shown in fig. 3, a slot plate 14 is provided in the mold frame, the slot plate is provided with a groove corresponding to the side surface of the insert sheet, and a plurality of insert sheets of the upper pressing structure are inserted into the mold frame, and the insert sheets are inserted into the grooves of the slot plate, so that the mixed materials put into the mold frame are separated into a plurality of mixed materials.
In one embodiment, in step S5, vulcanization is performed at ambient temperature or below 150 ℃.
In one embodiment, as shown in fig. 2 and 3, in step S6, the mixture pieces spaced apart in multiple pieces are ejected from the mold by the ejector frame 22, and the cutting is completed while reducing the roughness of the multiple pieces of mixture.
Preferably, the bottom plate 13 of the mold frame 12 is detachable, and the mixture material in pieces spaced apart is pressed into the mold frame by the mold release upper pressing plate 21 from the mold frame from which the bottom plate is removed.
In a preferred embodiment, the method for preparing the heat conductive sheet comprises:
mixing the raw materials of all the components to obtain a mixed material, wherein the mixed material at least comprises a binder, an anisotropic heat conduction filler or an isotropic heat conduction filler;
after removing bubbles in vacuum, extruding the mixture into a sheet shape through extrusion equipment, wherein the extrusion thickness is 0.5-3mm, preferably 1-2mm, the extrusion speed is 1-10mm/s, preferably 3-7mm/s, the extrusion length and width are not particularly limited, and the mixture can be placed in a die frame and is generally 1-2mm smaller than the length and width of the die frame;
the extruded sheets are placed into a die frame for stacking layer by layer, and the stacking height is higher than the height of the die frame and is consistent with the height of the inner cavity;
placing the upper pressing structure at a corresponding position on the die frame, wherein the corresponding position is that the longitudinally arranged smooth inserting sheets on the upper pressing structure correspond to the inner groove of the die frame, and pressing the upper pressing structure into the die frame by pressing; the small sheets which are smooth are longitudinally arranged on the upper pressing structure and are inserted into the material, so that the anisotropic heat conduction filler in the material is perpendicular to the sheets;
and (3) taking out the die after heating and vulcanizing, demolding, and removing the sheet to directly obtain the heat conducting sheets with anisotropic heat conducting fillers arranged along the longitudinal direction.
The following examples prepared the thermally conductive sheet by the above-described preparation method, and the thermally conductive sheet was subjected to test characterization by the following test method:
thermal resistance: the thermal resistance of a 1mm thermally conductive sheet was tested at 50% compression using ASTM D5470 standard;
thermal conductivity coefficient: adopting ASTM D5470 standard, respectively taking 1mm, 2mm and 3mm each sample for testing, and fitting and calculating to obtain;
surface roughness: the roughness of the surface of the heat conducting strip was tested using the GB/T3505-2009 standard.
Example 1
In this example, the following components were used:
anisotropic heat conductive filler: carbon nanotubes with a diameter of 2nm and a length of 10 μm, a thermal conductivity of 550W/(mK) and a content of 80wt.%;
an adhesive: polydimethyl cyclosiloxane, content 20wt.%;
vulcanization temperature: normal temperature;
through testing, the heat conducting strip made of the die insert sheet is shown in fig. 4, and the performance parameters are as follows:
surface roughness: 0.394 μm
Thermal resistance: 0.76K cm 2 /W
Thermal conductivity coefficient: 15.37W/(mK).
Example 2
Anisotropic heat conductive filler: pitch-based carbon fiber having a diameter of 10 μm and a length of 100 μm, a thermal conductivity of 650W/(mK) and a content of 20wt.%;
isotropic thermally conductive filler: alumina, particle size 0.1 μm, content 60wt.%;
an adhesive: polydimethylsiloxane, content 20wt.%;
vulcanization temperature: 145 ℃;
through the test, the performance parameters of the heat conducting strip made by the die insert sheet are as follows:
surface roughness: 0.342 μm
Thermal resistance: 0.67K cm 2 /W
Thermal conductivity coefficient: 17.25W/(mK).
Example 3
Anisotropic heat conductive filler: pitch-based carbon fiber having a diameter of 15 μm and a length of 250 μm, a thermal conductivity of 1200W/(mK), and a content of 60wt.%;
isotropic thermally conductive filler: silicon carbide, particle size 30 μm, content 15wt.%;
an adhesive: alpha, omega-diethyl polydimethylsiloxane content 25wt.%;
vulcanization temperature: 120 ℃;
through the test, the performance parameters of the heat conducting strip made by the die insert sheet are as follows:
surface roughness: 0.214 μm
Thermal resistance: 0.41K cm 2 /W
Thermal conductivity coefficient: 32.41W/(mK).
Example 4
Anisotropic heat conductive filler: pitch-based carbon fiber having a diameter of 25 μm and a length of 350 μm, a thermal conductivity of 1000W/(mK), and a content of 50wt.%;
isotropic thermally conductive filler: silica having a particle size of 15 μm and a content of 25wt.%;
an adhesive: polydimethyl cyclosiloxane, content 25wt.%;
vulcanization temperature: 80 ℃;
through the test, the performance parameters of the heat conducting strip made by the die insert sheet are as follows:
surface roughness: 0.275 μm
Thermal resistance: 0.50K cm 2 /W
Thermal conductivity coefficient: 25.47W/(mK).
Example 5
Anisotropic heat conductive filler: graphene, diameter 5 μm, thermal conductivity 750W/(m·k), content 40wt.%;
isotropic thermally conductive filler: aluminum nitride, particle size 10 μm, content 30wt.%;
an adhesive: alpha, omega-dihydroxy polydimethylsiloxane in an amount of 30wt.%;
vulcanization temperature: 60 ℃;
through the test, the performance parameters of the heat conducting strip made by the die insert sheet are as follows:
surface roughness: 0.364 μm
Thermal resistance: 0.91K cm 2 /W
Thermal conductivity coefficient: 12.41W/(mK).
Example 6
Anisotropic heat conductive filler: graphene with a diameter of 200 μm and a thermal conductivity of 1500W/(mK) and a content of 80wt.%;
isotropic thermally conductive filler: alumina, particle size 30 μm, content 10wt.%;
an adhesive: polydimethyl cyclosiloxane, content 10wt.%;
vulcanization temperature: 120 ℃;
through the test, the performance parameters of the heat conducting strip made by the die insert sheet are as follows:
surface roughness: 0.297 μm
Thermal resistance: 0.63K cm 2 /W
Thermal conductivity coefficient: 18.84W/(mK).
Example 7
Anisotropic heat conductive filler: graphene with a diameter of 100 μm and a thermal conductivity of 1100W/(mK) and a content of 60wt.%;
isotropic thermally conductive filler: silica having a particle size of 1 μm and a content of 20wt.%;
an adhesive: polydimethyl cyclosiloxane, content 30wt.%;
vulcanization temperature: 120 ℃;
through the test, the performance parameters of the heat conducting strip made by the die insert sheet are as follows:
surface roughness: 0.254 μm
Thermal resistance: 0.70K cm 2 /W
Thermal conductivity coefficient: 16.75W/(mK).
Example 8
Anisotropic heat conductive filler: graphite, sheet diameter 200 μm, diameter 5 μm, content 65wt.%; isotropic thermally conductive filler: silicon carbide with a particle size of 120 μm and a content of 10wt.%
An adhesive: polydiphenylsiloxane, content 25wt.%;
vulcanization temperature: 120 ℃;
through the test, the performance parameters of the heat conducting strip made by the die insert sheet are as follows:
surface roughness: 0.374 μm
Thermal resistance: 0.84K cm 2 /W
Thermal conductivity coefficient: 13.67W/(mK).
Example 9
Anisotropic heat conductive filler: graphite, sheet diameter 60 μm, diameter 2 μm, content 45wt.%; isotropic thermally conductive filler: alumina with a particle size of 5 μm and a content of 35wt.%
An adhesive: polydiphenylsiloxane, content 20wt.%;
vulcanization temperature: 120 ℃;
through the test, the performance parameters of the heat conducting strip made by the die insert sheet are as follows:
surface roughness: 0.246 μm
Thermal resistance: 0.73K cm 2 /W
Thermal conductivity coefficient: 15.94W/(mK).
Example 10
Example 10
Anisotropic heat conductive filler: boron nitride, sheet diameter 60 μm, content 25wt.%;
isotropic thermally conductive filler: silica having a particle diameter of 40 μm and a content of 25wt.%
An adhesive: cyanosiloxysilane, content 50wt.%;
vulcanization temperature: 90 ℃;
through the test, the performance parameters of the heat conducting strip made by the die insert sheet are as follows:
surface roughness: 0.263 μm
Thermal resistance: 0.89K cm 2 /W
Thermal conductivity coefficient: 12.64W/(mK).
Comparative example 1
Anisotropic heat conductive filler: carbon nanotubes with a diameter of 2nm and a length of 10 μm, a thermal conductivity of 550W/(mK) and a content of 80wt.%;
isotropic thermally conductive filler;
an adhesive: polydimethyl cyclosiloxane, content 20wt.%;
the heat conducting sheet obtained by stacking, hot pressing, semi-curing cutting and pressing the materials extruded by the extruder is shown in fig. 5, and the performance parameters are as follows:
surface roughness: 2.174 μm
Thermal resistance: 1.20K cm 2 /W
Thermal conductivity coefficient: 9.14W/(mK).
Comparative example 2
Anisotropic heat conductive filler: pitch-based carbon fiber having a diameter of 10 μm and a length of 100 μm, a thermal conductivity of 650W/(mK) and a content of 20wt.%;
isotropic thermally conductive filler: alumina, particle size 0.1 μm, content 60wt.%;
an adhesive: polydimethylsiloxane, content 20wt.%;
the performance parameters of the heat conducting sheet obtained after stacking, hot pressing, semi-curing cutting and pressing of the materials extruded by the extruder are as follows:
surface roughness: 1.875 μm
Thermal resistance: 1.37K cm 2 /W
Thermal conductivity coefficient: 7.89W/(mK).
Comparative example 3
Anisotropic heat conductive filler: graphene, diameter 10 μm, thermal conductivity 750W/(m·k), content 40wt.%;
isotropic thermally conductive filler: aluminum nitride, particle size 10 μm, content 30wt.%;
an adhesive: alpha, omega-dihydroxy polydimethylsiloxane in an amount of 30wt.%;
the performance parameters of the heat conducting sheet obtained after stacking, hot pressing, semi-curing cutting and pressing of the materials extruded by the extruder are as follows:
surface roughness: 2.341 μm
Thermal resistance: 1.24K cm 2 /W
Thermal conductivity coefficient: 8.75W/(mK).
Finally, it should be noted that: the foregoing description is only a preferred embodiment of the present invention, and the present invention is not limited thereto, but it is to be understood that modifications and equivalents of some of the technical features described in the foregoing embodiments may be made by those skilled in the art, although the present invention has been described in detail with reference to the foregoing embodiments. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (57)
1. A method for producing a heat conductive sheet, comprising:
mixing the raw materials of all components of the heat conducting sheet to obtain a mixed material, wherein the mixed material comprises a binder and an anisotropic filler;
extruding the mixed material into a sheet;
placing a plurality of sheets into a mold frame, wherein the mold frame is provided with an inner cavity with one end being open;
inserting an upward pressing structure with a plurality of inserting sheets into the mixed material of the mold frame by pressing to form a mold for preparing the heat conducting sheet, so that the anisotropic heat conducting filler in the material is perpendicular to the inserting sheets, and the surface roughness of the inserting sheets is 0.01-0.50 mu m;
vulcanizing the mixed material;
demolding the vulcanized mixed material, and reducing the roughness of a plurality of mixed materials while finishing cutting to obtain heat conducting sheets with anisotropic heat conducting fillers arranged along the direction perpendicular to the inserting sheets;
wherein, the step of putting a plurality of sheets into a mould frame, the height of the plurality of sheets is not less than the height of an inner cavity of the mould;
wherein, in the step of demoulding the vulcanized mixture,
the bottom plate of the die frame is detachable, and the mixed materials with multiple pieces at intervals are pressed into the die frame from the die frame with the bottom plate removed through the die-stripping upper pressing plate.
2. The method of producing a thermally conductive sheet according to claim 1, wherein the step of extruding the mixture into a sheet further comprises:
and removing bubbles from the mixed material in vacuum.
3. The method according to claim 1, wherein in the step of extruding the mixture into a sheet, the mixture is extruded into a sheet by an extruder, and the extruder is at least one of a single screw extruder, a twin screw extruder, and a non-screw extruder.
4. The method of producing a heat conductive sheet according to claim 3, wherein the extrusion thickness is 0.5 to 3mm and the extrusion rate is 1 to 10mm/s.
5. The method of producing a thermally conductive sheet according to claim 4, wherein the extrusion thickness is 1 to 2mm and the extrusion rate is 3 to 7mm/s.
6. The method of producing a heat conductive sheet according to claim 1, wherein in the step of vulcanizing the mixture, vulcanization is performed at a room temperature or at a temperature lower than 150 ℃.
7. The method of producing a thermally conductive sheet according to claim 1, wherein the anisotropic thermally conductive filler comprises a one-dimensional thermally conductive filler or/and a two-dimensional thermally conductive filler.
8. The method of producing a thermally conductive sheet according to claim 7, wherein the one-dimensional thermally conductive filler comprises carbon nanotubes or/and carbon fibers.
9. The method of producing a thermally conductive sheet according to claim 8, wherein the method of producing carbon nanotubes is at least one selected from the group consisting of a laser ablation method, an arc discharge method, and a Chemical Vapor Deposition (CVD) method.
10. The method of producing a thermally conductive sheet according to claim 8, wherein the carbon nanotubes are at least one selected from the group consisting of single-walled carbon nanotubes and multi-walled carbon nanotubes.
11. The method of producing a thermally conductive sheet as claimed in claim 8, wherein the carbon nanotubes have a diameter of 2 to 200nm.
12. The method of claim 11, wherein the carbon nanotubes have a diameter of 10 to 100 a nm a.
13. The method of manufacturing a thermally conductive sheet according to claim 8, wherein the carbon nanotubes have a length of 10 to 300 μm.
14. The method of claim 13, wherein the carbon nanotubes have a length of 20 to 150 μm.
15. The method of producing a thermally conductive sheet according to claim 8, wherein the carbon nanotubes have a thermal conductivity of 500W/(m-K) or more.
16. The method of producing a thermally conductive sheet according to claim 15, wherein the carbon nanotubes have a thermal conductivity of 1000W/(m-K) or more.
17. The method of producing a thermally conductive sheet according to claim 8, wherein the carbon nanotubes are contained in the thermally conductive sheet in an amount of 20 to 80wt.%.
18. The method of producing a thermally conductive sheet according to claim 17, wherein the carbon nanotubes are contained in the thermally conductive sheet in an amount of 40wt.% to 65wt wt.%.
19. The method of producing a thermally conductive sheet according to claim 8, wherein the carbon fiber is at least one selected from the group consisting of a viscose-based carbon fiber, a pitch-based carbon fiber and a PAN-based carbon fiber.
20. The method of claim 19, wherein the carbon fiber is a pitch-based carbon fiber.
21. The method of producing a thermally conductive sheet according to claim 8, wherein the carbon fiber has a length of 10 to 600 μm.
22. The method of producing a thermally conductive sheet according to claim 8, wherein the carbon fiber has a length of 100 to 400 μm.
23. The method of producing a thermally conductive sheet according to claim 8, wherein the carbon fiber has a diameter of 10 to 30 μm.
24. The method of producing a thermally conductive sheet according to claim 23, wherein the carbon fiber has a diameter of 8 to 15 μm.
25. The method of producing a thermally conductive sheet according to claim 8, wherein the carbon fiber has a thermal conductivity of 600W/(mK) or more.
26. The method of producing a thermally conductive sheet according to claim 25, wherein the carbon fiber has a thermal conductivity of 1000W/(m-K) or more.
27. The method of producing a thermally conductive sheet according to claim 8, wherein the carbon fiber is contained in the thermally conductive sheet in an amount of 20 to 80wt.%.
28. The method of producing a heat conductive sheet according to claim 27, wherein the carbon fiber is contained in the heat conductive sheet in an amount of 40 to 65 wt% by weight.
29. The method of producing a thermally conductive sheet according to claim 7, wherein the two-dimensional thermally conductive filler is at least one selected from the group consisting of boron nitride, graphene, graphite and boron nitride.
30. The method of manufacturing a thermally conductive sheet as claimed in claim 29, wherein the boron nitride is hexagonal boron nitride.
31. The method of producing a thermally conductive sheet according to claim 29, wherein the sheet diameter of the boron nitride is 0.05 to 400 μm.
32. The method of manufacturing a thermally conductive sheet according to claim 31, wherein the sheet diameter of the boron nitride is 50 to 300 μm.
33. The method of producing a thermally conductive sheet according to claim 29, wherein the content of the boron nitride in the thermally conductive sheet is 20 to 80wt.%.
34. The method of producing a thermally conductive sheet according to claim 33, wherein the content of the boron nitride in the thermally conductive sheet is 40wt.% to 65wt.%.
35. The method for producing a thermally conductive sheet according to claim 29, wherein the method for producing graphene is at least one selected from the group consisting of a chemical vapor deposition method, a self-mechanical exfoliation method, a redox method and a solvent exfoliation method.
36. The method of claim 29, wherein the graphene has a sheet diameter of 1-400 μm.
37. The method of claim 36, wherein the graphene has a sheet diameter of 10-200 μm.
38. The method of producing a thermally conductive sheet according to claim 29, wherein the graphene has a thermal conductivity of 700W/(m-K) or more.
39. The method of producing a thermally conductive sheet according to claim 38, wherein the graphene has a thermal conductivity of 1200W/(m-K) or more.
40. The method of producing a thermally conductive sheet according to claim 29, wherein the graphene is contained in the thermally conductive sheet in an amount of 20 to 80wt.%.
41. The method of producing a thermally conductive sheet as claimed in claim 40, wherein the graphene is contained in the thermally conductive sheet in an amount of 40wt.% to 65 wt%.
42. The method of producing a thermally conductive sheet according to claim 29, wherein the graphite is at least one selected from the group consisting of graphitized natural graphite, graphitized expanded graphite, natural graphite, expanded graphite and artificial graphite.
43. The method of claim 29, wherein the graphite has a sheet diameter of 1-400 μm.
44. The method of manufacturing a thermally conductive sheet as claimed in claim 43, wherein the graphite has a sheet diameter of 20 to 200. Mu.m.
45. The method of manufacturing a thermally conductive sheet according to claim 29, wherein the graphite has a thickness of 0.01 to 10 μm.
46. The method of claim 45, wherein the graphite has a thickness of 1-5 μm.
47. The method of producing a thermally conductive sheet according to claim 29, wherein the graphite is contained in the thermally conductive sheet in an amount of 20 to 80wt.%.
48. The method of producing a heat conductive sheet according to claim 47, wherein the content of graphite in the heat conductive sheet is 40wt.% to 65wt wt.%.
49. The method of producing a thermally conductive sheet according to claim 1, wherein the mixed material further comprises an isotropic thermally conductive filler comprising at least one of alumina, aluminum nitride, silicon carbide, and silicon dioxide.
50. The method of producing a heat conductive sheet according to claim 49, wherein the particle diameter of the isotropic heat conductive filler is 0.1 to 120. Mu.m.
51. The method of producing a heat conductive sheet according to claim 50, wherein the isotropic heat conductive filler has a particle diameter of 5 to 50. Mu.m.
52. The method of producing a heat conductive sheet according to claim 49, wherein the content of the isotropic heat conductive filler is 10wt.% to 60wt.%.
53. The method of producing a thermally conductive sheet according to claim 1, wherein the binder is contained in an amount of 10 to 50wt.% of the thermally conductive sheet.
54. The method of producing a thermally conductive sheet according to claim 1, wherein the binder is a thermosetting resin.
55. The method for producing a heat conductive sheet according to claim 54 wherein said thermosetting resin is at least one selected from the group consisting of epoxy resin, unsaturated polyester, phenol resin, polymethylsiloxane, silicone resin, liquid silicone gel, phthalallyl resin, polyimide resin, urea resin and polyurethane.
56. The method of claim 55, wherein the thermosetting resin is a liquid silicone gel.
57. The method for preparing a thermally conductive sheet as claimed in claim 56, wherein said liquid silicone gel comprises one or more of polydimethylsiloxane, dimethylcyclosiloxane, α, ω -dihydroxypolydimethylsiloxane, α, ω -dihydroxypolymethyl3, 3, 3-trifluoropropyl siloxane, polydiphenylsiloxane, cyanosiloxysilane, and α, ω -diethylpolydimethylsiloxane.
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