CN113184840B - Thermal interface material with isotropic thermal conductivity and preparation method thereof - Google Patents
Thermal interface material with isotropic thermal conductivity and preparation method thereof Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title abstract description 6
- 239000002135 nanosheet Substances 0.000 claims abstract description 22
- 239000006185 dispersion Substances 0.000 claims abstract description 11
- 239000007788 liquid Substances 0.000 claims abstract description 9
- 239000000758 substrate Substances 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 7
- 239000011248 coating agent Substances 0.000 claims abstract description 3
- 238000000576 coating method Methods 0.000 claims abstract description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 54
- 229910002804 graphite Inorganic materials 0.000 claims description 43
- 239000010439 graphite Substances 0.000 claims description 43
- 238000010438 heat treatment Methods 0.000 claims description 39
- 239000004642 Polyimide Substances 0.000 claims description 14
- 229920001721 polyimide Polymers 0.000 claims description 14
- 239000002131 composite material Substances 0.000 claims description 11
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 10
- 229910021389 graphene Inorganic materials 0.000 claims description 10
- 229910052786 argon Inorganic materials 0.000 claims description 5
- 229910052582 BN Inorganic materials 0.000 claims description 4
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 4
- MHABMANUFPZXEB-UHFFFAOYSA-N O-demethyl-aloesaponarin I Natural products O=C1C2=CC=CC(O)=C2C(=O)C2=C1C=C(O)C(C(O)=O)=C2C MHABMANUFPZXEB-UHFFFAOYSA-N 0.000 claims description 2
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 claims description 2
- 239000011521 glass Substances 0.000 claims description 2
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 2
- 239000000395 magnesium oxide Substances 0.000 claims description 2
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 2
- 229920003229 poly(methyl methacrylate) Polymers 0.000 claims description 2
- 239000005020 polyethylene terephthalate Substances 0.000 claims description 2
- 239000004926 polymethyl methacrylate Substances 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 2
- 239000002064 nanoplatelet Substances 0.000 description 13
- 239000000084 colloidal system Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- DKGAVHZHDRPRBM-UHFFFAOYSA-N Tert-Butanol Chemical compound CC(C)(C)O DKGAVHZHDRPRBM-UHFFFAOYSA-N 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 239000003575 carbonaceous material Substances 0.000 description 3
- 238000003892 spreading Methods 0.000 description 3
- 230000000712 assembly Effects 0.000 description 2
- 238000000429 assembly Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000004108 freeze drying Methods 0.000 description 2
- 238000007710 freezing Methods 0.000 description 2
- 230000008014 freezing Effects 0.000 description 2
- 230000017525 heat dissipation Effects 0.000 description 2
- 230000003321 amplification Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000001246 colloidal dispersion Methods 0.000 description 1
- 239000011231 conductive filler Substances 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- -1 etc. Chemical compound 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000005087 graphitization Methods 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 239000002060 nanoflake Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
- C01B32/19—Preparation by exfoliation
- C01B32/192—Preparation by exfoliation starting from graphitic oxides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/064—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with boron
- C01B21/0648—After-treatment, e.g. grinding, purification
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/20—Graphite
- C01B32/205—Preparation
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/20—Graphite
- C01B32/21—After-treatment
- C01B32/23—Oxidation
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
- C01B2204/24—Thermal properties
Abstract
The invention provides a thermal interface material with isotropic heat conductivity, which comprises two-dimensional nano sheets, wherein the nano sheets are vertically oriented and radially distributed in the plane direction; the preparation method comprises the steps of uniformly coating the two-dimensional nano sheet dispersion liquid on a substrate, and using a microneedle to slide outwards by taking a certain point of a plane as a circle center to form a plurality of radial scratches, wherein the scratches are distributed at equal angles. Transferring into a freeze dryer, and drying to obtain three-dimensional assembly. The thermal interface material has a thermal conductivity of 50-200W/mK in the vertical direction and a thermal conductivity of 20-200W/mK in the horizontal direction. The method is simple and controllable, has high efficiency and good effect, and is a novel method for preparing the thermal interface material.
Description
Technical Field
The invention relates to the field of materials, in particular to a thermal interface material with isotropic heat conductivity and a preparation method thereof.
Background
As electronic packages are moving toward miniaturization, integration, and intelligence, the power density per unit area within electronic devices is also rapidly increasing. If the heat generated by the electronic product during operation cannot be discharged in time, the working performance and the service life of the chip can be greatly influenced, and the efficient heat management design is a key for solving the problem. Currently, commercial thermal interface materials have a thermally conductive filler content of 50-90wt%, typically less than 10W/mK, and such conventional thermal interface materials have difficulty meeting heat dissipation requirements. Accordingly, there is a need to develop new thermal interface materials to address the ever-increasing thermal management issues associated with the rapid development of semiconductor devices.
Two-dimensional sheet materials such as graphene, which have excellent thermal conductivity (1000-5000W/mK), are considered to be a thermal interface material with great plasticity and development potential. However, as a typical two-dimensional sheet material, the ultra-high thermal conductivity of graphene is only represented in the in-plane direction, and its thermal conductivity in the out-of-plane direction is less than 3W/mK. How to change the high heat conduction performance in the horizontal direction into the performance in the vertical direction of the macroscopic assembly is the key for solving the longitudinal heat transfer requirement of the thermal interface material. Research shows that the thermal interface material has high longitudinal heat conductivity and high horizontal heat dissipation performance, so that the interface thermal resistance between the thermal interface material and the contact surface is reduced, and the thermal interface material is favorable for fully playing the rapid heat conduction function as the thermal interface material.
The disclosure of this background section is only intended to increase the understanding of the general background of the invention and should not be taken as an admission or any form of suggestion that this information forms the prior art that is already known to a person of ordinary skill in the art.
Disclosure of Invention
The invention aims to provide a thermal interface material with isotropic heat conductivity, which mainly comprises two-dimensional nano sheets, wherein the nano sheets are vertically oriented and radially distributed in the plane direction. The thermal interface material has a thermal conductivity of 50-200W/mK in the vertical direction and a thermal conductivity of 20-200W/mK in the horizontal direction.
Nanoplatelets suitable for use in the present invention include, but are not limited to: one or more of graphene oxide, graphite oxide, expanded graphite, expandable graphite, crystalline flake graphite, boron nitride, etc., aluminum oxide, magnesium oxide, aluminum nitride.
The invention also provides a preparation method of the isotropic thermal interface material, which mainly utilizes microneedle shearing to realize high-precision arrangement and orientation regulation of the nano-sheet colloid dispersion liquid. The method comprises the following specific steps:
(1) Preparing two-dimensional nano-sheet dispersion liquid, wherein the concentration of the dispersion liquid is 10-300mg/g.
(2) Uniformly coating the two-dimensional nano sheet dispersion liquid on a substrate, and using a microneedle to outwards slide by taking a certain point of a plane as a circle center to form a plurality of radial scratches, wherein the scratches are distributed at equal angles.
(3) Transferring into a freeze dryer, and drying to obtain three-dimensional assembly.
Further, the substrate includes, but is not limited to, PET, PMMA, glass.
Further, in step 2, the angle of the adjacent scratches is 0.01 to 1 .
Further, the diameter of the microneedle is 10um-500um.
Further, the two-dimensional nano-sheet is a graphite oxide nano-sheet, the thickness is 0.01-10um, and the sheet diameter is 10-300 um.
In order to improve the thermal properties of the graphite oxide, the method may further comprise the steps of:
a) Immersing the three-dimensional assembly in a polyimide solution (solvent DMAC) to allow the solution to substantially fill the assembly voids (typically vacuum impregnation means can be employed); taking out and drying to obtain the composite three-dimensional assembly.
b) And (3) placing the composite three-dimensional assembly in a tube furnace, heating under the protection of high-purity argon (99.999%), heating from room temperature to 300 at a heating rate of 5 /min, preserving heat for 1h, heating to 1200 at a heating rate of 2 /min, and preserving heat for 1h to obtain the preliminary carbonized assembly.
c) And then heating from room temperature to 1500 at a heating rate of 10 /min, continuously heating to 3000 at a heating rate of 2 /min, preserving heat for 1h, and graphitizing to finally obtain the three-dimensional cross-linked vertically oriented graphene thermal interface material.
Further, the concentration in the polyimide solution is 3wt% to 20wt%.
The invention has the beneficial effects that: 1. the graphene thermal interface material prepared by the graphite oxide nano-sheets has low price and simple process, is suitable for large-scale continuous production, and is suitable for industrial amplification application.
2. The invention is a universal method for controlling microstructure of low-dimensional nano material, which has remarkable effect on macro assembly of other two-dimensional materials, such as boron nitride and the like, besides preparation of carbon-based thermal interface materials.
3. The radial structure designed by the invention fully exerts excellent heat conduction performance in the plane of the two-dimensional lamellar material in the horizontal direction, not only has high heat conduction in the longitudinal direction but also can be quickly soaked in the horizontal direction, and has great application prospect in the field of thermal interface materials.
Drawings
FIG. 1 is a schematic view of a three-dimensional radial structure of the present invention: the two-dimensional nano-sheets are vertically oriented and radially distributed in the plane direction.
Fig. 2 is a Scanning Electron Microscope (SEM) of the surface and cross section of the graphite oxide nanoplatelets of example 1: FIG. 2a is an upper surface of a graphite oxide nanoplatelet; figure 2b is a longitudinal section of a graphite oxide nanoplatelet. The dashed lines indicate the two-dimensional ply orientation direction.
Fig. 3 is a Scanning Electron Microscope (SEM) of the surface and cross section of the graphite oxide nanoplatelets of example 2: FIG. 3a is an upper surface of a graphite oxide nanoplatelet; figure 3b is a longitudinal section of a graphite oxide nanoplatelet.
Fig. 4 is a Scanning Electron Microscope (SEM) of the surface and cross section of the graphite oxide nanoplatelets of example 3: FIG. 4a is an upper surface of a graphite oxide nanoplatelet; figure 4b is a longitudinal section of a graphite oxide nanoplatelet.
Fig. 5 is a Scanning Electron Microscope (SEM) of the surface and cross section of the graphite oxide nanoplatelets of example 4: FIG. 5a is an upper surface of a graphite oxide nanoplatelet; figure 5b is a longitudinal section of a graphite oxide nanoplatelet.
Fig. 6 is a schematic view of sliding outward from a center of a circle in a radial pattern.
Detailed Description
Examples of the invention are given below, which are further illustrative of the invention. And not to limit the scope of the invention.
Example 1
Spreading 100mg/g graphite oxide nano sheet (sheet diameter 50-100um, thickness 0.5 um) colloid dispersion on PET substrate, sliding outwards from a circle center according to radial pattern by using microneedle, setting sliding radius 2cm, and setting adjacent scratch angle to 0.5 degree until scratch is distributed over the whole circular region. And (3) rapidly freezing the sample, and then freeze-drying in a freeze dryer to obtain the radial graphene oxide nano-sheet assembly.
And (3) immersing the graphite oxide three-dimensional assembly in a polyimide acid solution (12 wt%) in vacuum for 2h, taking out, placing in a tertiary butanol solution for replacement for 72h, taking out and drying to obtain the graphite oxide/polyimide composite three-dimensional assembly.
And (3) placing the prepared graphite oxide/polyimide composite three-dimensional assembly in a tubular furnace, heating under the protection of high-purity argon (99.999%), heating from room temperature to 300 at a heating rate of 5 /min, preserving heat for 1h, heating to 1200 at a heating rate of 2 /min, and preserving heat for 1h to obtain the preliminary carbonized assembly. The carbonized assembly is placed in a high temperature furnace, heated from room temperature to 1500 at a heating rate of 10 /min, then graphitized at 3000 at a heating rate of 2 /min, and finally the graphitized three-dimensionally crosslinked pure carbon material sample has isotropic thermal conductivity. The LFA476 laser flash instrument was used to test a thermal conductivity of 75W/mK in the machine direction and 46W/mK in the transverse direction.
Example 2
150mg/g of a colloidal dispersion of graphite oxide (graphite oxide: graphene oxide=8:2, mass ratio), wherein graphite oxide nano-sheets (sheet diameter 50-100um, thickness 0.5 um) and graphene oxide (sheet diameter 10-50um, thickness 0.9 nm), were tiled on a PET substrate, sliding was performed according to a radial pattern from a circle center outwards with a microneedle, sliding radius was set to 1cm, and adjacent scratch angles were 0.2 degrees until scratches were distributed over the entire circular region. And (3) rapidly freezing the sample, and then freeze-drying in a freeze dryer to obtain the radial graphene oxide nano-sheet assembly.
Immersing the graphite oxide three-dimensional assembly in a polyimide acid solution (12 wt%) for 2h, taking out, placing in a tertiary butanol solution for replacement for 72h, taking out and drying to obtain the graphite oxide/polyimide composite three-dimensional assembly.
And (3) placing the prepared graphite oxide/polyimide composite three-dimensional assembly in a tubular furnace, heating under the protection of high-purity argon (99.999%), heating from room temperature to 300 at a heating rate of 5 /min, preserving heat for 1h, heating to 1200 at a heating rate of 2 /min, and preserving heat for 1h to obtain the preliminary carbonized assembly. The carbonized assembly is placed in a high temperature furnace, the temperature is raised to 1500 from room temperature at a heating rate of 10 /min, then the temperature is raised to 3000 at a heating rate of 2 /min for graphitization, and finally the graphitized three-dimensional crosslinked pure carbon material sample has isotropic heat conductivity. The LFA476 laser flash instrument was used to test that the longitudinal thermal conductivity was 114W/mK and the transverse thermal conductivity was 73W/mK.
Example 3
Spreading 80mg/g Boron Nitride (BNs) colloid dispersion liquid on a PET substrate, sliding outwards from a circle center according to a radial pattern by using a microneedle, setting the sliding radius to be 1cm, and setting the adjacent scratch angle to be 0.2 degree until the scratch is distributed in the whole circular area. The samples were flash frozen and then lyophilized in a freeze dryer to give radial BNNs assemblies. The LFA476 laser flash instrument was used to test that the longitudinal thermal conductivity was 59W/mK and the transverse thermal conductivity was 21W/mK.
Example 4
Spreading 80mg/g crystalline flake graphite/graphite oxide (mass fraction crystalline flake graphite: graphite oxide=5:5) colloid dispersion on a PET substrate, wherein crystalline flake graphite (average flake diameter 80um, thickness 1-10 um) and graphite oxide nano-flakes (flake diameter 50-100um, thickness 0.1 um) slide outwards from a circle center according to radial patterns by using a microneedle, setting a sliding radius of 3cm, and setting an adjacent scratch angle to be 0.4 degree until scratches are distributed over the whole circular area. The sample was rapidly frozen and then lyophilized in a freeze dryer to obtain radial crystalline flake graphite/graphite oxide assemblies.
Immersing the composite three-dimensional assembly in a polyimide acid solution (12 wt%) for 2h, taking out, placing in a tertiary butanol solution for replacement for 72h, taking out and drying to obtain the graphite oxide/polyimide composite three-dimensional assembly.
And (3) placing the prepared graphite oxide/polyimide composite three-dimensional assembly in a tubular furnace, heating under the protection of high-purity argon (99.999%), heating from room temperature to 300 at a heating rate of 5 /min, preserving heat for 1h, heating to 1200 at a heating rate of 2 /min, and preserving heat for 1h to obtain the preliminary carbonized assembly. The carbonized assembly is placed in a high temperature furnace, heated from room temperature to 1500 at a heating rate of 10 /min, then graphitized at 3000 at a heating rate of 2 /min, and finally the graphitized three-dimensionally crosslinked pure carbon material sample has isotropic thermal conductivity. The LFA476 laser flash instrument was used to test that the longitudinal thermal conductivity was 59W/mK and the transverse thermal conductivity was 21W/mK.
Claims (4)
1. The thermal interface material with isotropic thermal conductivity is characterized by comprising two-dimensional nano sheets, wherein the nano sheets are vertically oriented and radially distributed in the plane direction; the thickness of the two-dimensional nano sheet is 0.01-10 mu m, and the sheet diameter is 10-300 mu m; the thermal interface material has a thermal conductivity of 50-200W/mK in the vertical direction and a thermal conductivity of 20-200W/mK in the horizontal direction, and is prepared by the following method:
(1) Preparing a two-dimensional nano-sheet dispersion liquid, wherein the concentration of the dispersion liquid is 10-300mg/g; the two-dimensional nano sheet is graphite oxide, expanded graphite, expandable graphite, crystalline flake graphite, boron nitride, aluminum oxide, magnesium oxide and aluminum nitride;
(2) Uniformly coating the two-dimensional nano sheet dispersion liquid on a substrate, and using a microneedle to slide outwards by taking a certain point of a plane as a circle center to form a plurality of radial scratches, wherein the scratches are distributed at equal angles; the angle of the adjacent scratches is 0.01-1 degrees; the diameter of the micro needle is 10 m-500 m;
(3) Transferring into a freeze dryer, and drying to obtain three-dimensional assembly.
2. The thermal interface material of claim 1 wherein the substrate is PET, PMMA, glass.
3. The thermal interface material of claim 1, further comprising the steps of:
a) Immersing the three-dimensional assembly obtained in the step 3 in polyimide solution to enable the solution to fully fill the gaps of the assembly; taking out and drying to obtain a composite three-dimensional assembly; the solvent of the polyimide solution is DMAC;
b) Placing the composite three-dimensional assembly in a tube furnace, heating under the protection of high-purity argon with the concentration of 99.999%, heating from room temperature to 300 at the heating rate of 5 /min, preserving heat for 1h, heating to 1200 at the heating rate of 2 /min, and preserving heat for 1h to obtain a preliminary carbonized assembly;
c) And then heating from room temperature to 1500 at a heating rate of 10 /min, continuously heating to 3000 at a heating rate of 2 /min, preserving heat for 1h, and graphitizing to finally obtain the three-dimensional cross-linked vertically oriented graphene thermal interface material.
4. A thermal interface material as defined in claim 3, wherein the polyimide solution has a concentration of 3wt% to 20wt%.
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