CN113185762A - Expanded graphite thermal interface material and preparation method thereof - Google Patents
Expanded graphite thermal interface material and preparation method thereof Download PDFInfo
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- CN113185762A CN113185762A CN202110495381.5A CN202110495381A CN113185762A CN 113185762 A CN113185762 A CN 113185762A CN 202110495381 A CN202110495381 A CN 202110495381A CN 113185762 A CN113185762 A CN 113185762A
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- expanded graphite
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
- C09K5/08—Materials not undergoing a change of physical state when used
- C09K5/14—Solid materials, e.g. powdery or granular
Abstract
The invention discloses an expanded graphite thermal interface material and a preparation method thereof, wherein the preparation method comprises the following steps: 1) preparing expanded graphite by using a graphite film as a raw material by adopting an oxidation intercalation method; 2) carrying out surface treatment on the expanded graphite by using a silane coupling agent to obtain modified expanded graphite; 3) and fully infiltrating the modified expanded graphite with polyolefin in a vacuum infiltration manner to obtain the expanded graphite thermal interface material. Firstly, the expanded graphite is prepared by expanding a graphite film, the internal network of the expanded graphite is well communicated, the heat conduction is facilitated, and the problem of poor dispersion performance does not exist due to the polyolefin integrally infiltrated in the process of preparing the composite material. And in addition, the expansion times of the expanded graphite can be adjusted in the preparation process, so that the experiment is convenient to carry out. And thirdly, the polyolefin is distributed on the surface of the expanded graphite more uniformly by integrally modifying the blocky expanded graphite, so that the purpose of controllable polyolefin infiltration amount is achieved.
Description
Technical Field
The invention belongs to the technical field of inorganic non-metallic materials, and particularly relates to an expanded graphite thermal interface material and a preparation method thereof.
Background
The rapid development of electronic devices places higher demands on heat dissipation. High thermal conductivity polymer composites are key materials to address heat dissipation issues in electronic applications. To improve the thermal properties of the polymer, various fillers are used. Generally, highly thermally conductive polymers are prepared by increasing the filler loading, but the high filler loading deteriorates the mechanical properties and processability of the polymer matrix, limiting its applications. Preparing low loadings of thermally conductive polymers remains a significant challenge. At present, a great deal of work has been done in adjusting the orientation of fillers, constructing a continuous thermal conduction pathway to improve the thermal conductivity enhancement efficiency and synthesizing polymer composites with low filler loading. Two-dimensional fillers, such as graphene, tend to be horizontally oriented by simple handling, so the final composite typically exhibits high in-plane thermal conductivity (K)∥) But limited thermal conductivity through the plane (K)⊥). However, the preparation of polymeric composites is more difficult due to the horizontal orientation of the two-dimensional filler material during processing. Typically, the orientation of the filler is adjusted by building a three-dimensional (3D) filler network, adding external/electric fields or complex machining processes, and through-plane heat conduction pathways are built in the polymer matrix. However, these methods also have time/energy consumption problems, and are highly challenging to apply in practice. To synthesize anisotropic heat-conducting polymers with lower loadingsCompound composite materials, there is a strong need for an efficient and simple method to adjust the orientation of the filler and to increase the thermal conductivity.
In addition, the heat conducting filler of the common thermal interface material has the problem of dispersibility regardless of metal powder or ceramic particles, and the filling amount is large, and most of the heat conducting filler is more than 60% (mass fraction). The poor dispersibility has the problem that filler particles cannot effectively contact with each other and cannot establish a heat conduction path, so that the result of poor heat conduction performance is obtained.
Disclosure of Invention
In order to solve the technical problems in the background art, the present invention provides an expanded graphite thermal interface material and a method for preparing the same.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows: in one aspect, the invention provides a preparation method of an expanded graphite thermal interface material, which comprises the following steps:
1) preparing expanded graphite by an oxidation intercalation method;
2) carrying out surface treatment on the expanded graphite by using a silane coupling agent to obtain modified expanded graphite;
3) and fully infiltrating the modified expanded graphite with polyolefin in a vacuum infiltration manner to obtain the expanded graphite thermal interface material.
Further, the raw material for preparing the expanded graphite in the step 1) is a graphite film.
Further, the step 1) is specifically as follows: placing a graphite film in a mold with a cover plate above, adding concentrated sulfuric acid and hydrogen peroxide in any proportion, oxidizing and intercalating the graphite film into expandable graphite by two oxidants, and controlling expansion times by adjusting the position of the cover plate above the mold to obtain expandable graphite with different densities; and then repeatedly cleaning the expandable graphite until the cleaning solution is neutral, and drying the cleaned expandable graphite to obtain the expanded graphite.
Further, the step 2) is specifically as follows: adding a silane coupling agent into a mixed solution of deionized water and absolute ethyl alcohol, and hydrolyzing for a period of time at a certain temperature to obtain a silane coupling agent hydrolysate; and soaking the expanded graphite in silane coupling agent hydrolysate, and reacting for a period of time at a certain temperature to obtain the modified expanded graphite.
Further, the volume ratio of the deionized water to the absolute ethyl alcohol in the mixed solution of the deionized water and the absolute ethyl alcohol is 0.2-0.33.
Further, the hydrolysis temperature is 70-90 ℃, and the hydrolysis time is 15-20 h.
Further, the temperature of the expanded graphite soaked in the silane coupling agent hydrolysate is 70-90 ℃, and the reaction time is 2-6 h.
Further, the method also comprises a step of cleaning and drying after the reaction is finished.
Further, the step 3) is specifically as follows: placing the modified expanded graphite in a container, adding a mixed solution of polyolefin and acetone, vacuumizing to enable the polyolefin to fully infiltrate the expanded graphite, and then curing at high temperature to obtain the expanded graphite thermal interface material.
Further, the mass filling amount of the expanded graphite in the expanded graphite thermal interface material is 10-50%.
Further, the temperature of the high-temperature curing is 120-150 ℃, and the time of the high-temperature curing is 6-8 h.
In another aspect, the present invention provides an expanded graphite thermal interface material, which is prepared by any one of the above methods for preparing an expanded graphite thermal interface material.
The invention has the beneficial effects that: 1) the invention adopts a new, simple and convenient constrained expansion method to prepare the high-orientation constrained expanded graphite. The expanded graphite can spontaneously orient in one direction during expansion by virtue of the boundary constraints of the vessel and establish a continuous heat conduction path within, which is of great benefit for the preparation of anisotropic composites and low filler loadings.
2) The invention adopts the blocky expanded graphite as the filler, so that the problem of dispersibility is not considered, and the blocky expanded graphite is communicated internally, has simple preparation process and is convenient to control the internally communicated density.
3) Firstly, the expanded graphite is prepared by expanding a graphite film, the internal network of the expanded graphite is well communicated, the heat conduction is facilitated, and the problem of poor dispersion performance does not exist due to the polyolefin integrally infiltrated in the process of preparing the composite material. And in addition, the expansion times of the expanded graphite can be adjusted in the preparation process, so that the experiment is convenient to carry out. And thirdly, the polyolefin is distributed on the surface of the expanded graphite more uniformly by integrally modifying the blocky expanded graphite, so that the purpose of controllable polyolefin infiltration amount is achieved.
Detailed Description
For a better understanding of the present invention, the following examples are given to illustrate the present invention, but the present invention is not limited to the following examples.
Example 1
Selecting 10 pieces of graphite film with thickness of 25 μm and thickness of 10 × 10cm, 3.76 g; flatly paving the graphite film at the bottom of the mold, adding hydrogen peroxide and then adding concentrated sulfuric acid, wherein the volume ratio of the hydrogen peroxide to the concentrated sulfuric acid is 1: 5; the graphite film is rapidly expanded into expandable graphite, and the expansion multiple of the graphite film is adjusted to be 400 times by adjusting the position of the glass cover plate; washing the expandable graphite to be neutral by deionized water, and drying the neutral expandable graphite at high temperature to obtain expanded graphite; hydrolyzing 0.5g of silane coupling agent in a mixed solution of deionized water and absolute ethyl alcohol with the volume ratio of 0.2, and carrying out reaction at 80 ℃ for 20 hours; cutting 400 times of expanded graphite into 4 × 4 × 4cm expanded graphite blocks, soaking in silane coupling agent hydrolysate, washing with anhydrous ethanol for 4-7 times at 80 deg.C for 4 hr; drying the expanded graphite with the surface treated at a low temperature, soaking the dried expanded graphite in 30g of mixed solution of polyolefin and acetone in vacuum, and curing the dried expanded graphite at a high temperature to obtain a composite material; and cutting the composite material into a standard size to obtain the heat-conducting gasket with the mass filling amount of the expanded graphite of 11.13%.
Example 2
Selecting 20 pieces of graphite film with thickness of 25 μm and thickness of 10 × 10cm, and weighing 7.52 g; flatly paving the graphite film at the bottom of the mold, adding hydrogen peroxide and then adding concentrated sulfuric acid, wherein the volume ratio of the hydrogen peroxide to the concentrated sulfuric acid is 1: 4; the graphite film is rapidly expanded into expandable graphite, and the expansion multiple of the graphite film is adjusted to be 400 times by adjusting the position of the glass cover plate; washing the expandable graphite to be neutral by deionized water, and drying the neutral expandable graphite at high temperature to obtain expanded graphite; hydrolyzing 0.5g of silane coupling agent in a mixed solution of deionized water and absolute ethyl alcohol with the volume ratio of 0.25, and carrying out reaction at 80 ℃ for 20 hours; cutting 400 times of expanded graphite into 4 × 4 × 4cm expanded graphite blocks, soaking in silane coupling agent hydrolysate, washing with anhydrous ethanol for 4-7 times at 80 deg.C for 4 hr; drying the expanded graphite with the surface treated at a low temperature, soaking the dried expanded graphite in 24g of mixed solution of polyolefin and acetone in vacuum, and curing the mixture at a high temperature to obtain a composite material; and cutting the composite material into a standard size to obtain the heat-conducting gasket with the mass filling amount of the expanded graphite of 23.84%.
Example 3
Selecting 20 pieces of graphite film with the thickness of 40 μm and the thickness of 10 × 10cm, and weighing 9.14 g; flatly paving the graphite film at the bottom of the mold, adding hydrogen peroxide and then adding concentrated sulfuric acid, wherein the volume ratio of the hydrogen peroxide to the concentrated sulfuric acid is 1: 4; the graphite film is rapidly expanded into expandable graphite, and the expansion multiple of the graphite film is adjusted to be 500 times by adjusting the position of the glass cover plate; washing the expandable graphite to be neutral by deionized water, and drying the neutral expandable graphite at high temperature to obtain expanded graphite; hydrolyzing 0.5g of silane coupling agent in a mixed solution of deionized water and absolute ethyl alcohol with the volume ratio of 0.28, and carrying out reaction at 80 ℃ for 20 hours; cutting 500 times of expanded graphite into 4 × 4 × 4cm expanded graphite blocks, soaking in silane coupling agent hydrolysate, washing with anhydrous ethanol for 4-7 times at 80 deg.C for 4 hr; drying the expanded graphite with the surface treated at a low temperature, soaking the dried expanded graphite in 30g of mixed solution of polyolefin and acetone in vacuum, and curing the dried expanded graphite at a high temperature to obtain a composite material; and cutting the composite material into a standard size to obtain the heat-conducting gasket with the mass filling amount of the expanded graphite of 23.32%.
Example 4
Selecting 14.61g of 30 single graphite films with the thickness of 60 mu m and the thickness of 10 multiplied by 10 cm; flatly paving the graphite film at the bottom of the mold, adding hydrogen peroxide and then adding concentrated sulfuric acid, wherein the volume ratio of the hydrogen peroxide to the concentrated sulfuric acid is 1: 5; the graphite film is rapidly expanded into expandable graphite, and the expansion multiple of the graphite film is adjusted to be 400 times by adjusting the position of the glass cover plate; washing the expandable graphite to be neutral by deionized water, and drying the neutral expandable graphite at high temperature to obtain expanded graphite; hydrolyzing 0.5g of silane coupling agent in a mixed solution of deionized water and absolute ethyl alcohol with the volume ratio of 0.2, and carrying out reaction at 80 ℃ for 20 hours; cutting 400 times of expanded graphite into 4 × 4 × 4cm expanded graphite blocks, soaking in silane coupling agent hydrolysate, washing with anhydrous ethanol for 4-7 times at 80 deg.C for 4 hr; drying the expanded graphite with the surface treated at a low temperature, soaking the dried expanded graphite in 25g of mixed solution of polyolefin and acetone in vacuum, and curing the dried expanded graphite at a high temperature to obtain a composite material; and cutting the composite material into a standard size to obtain the heat-conducting gasket with the mass filling amount of the expanded graphite of 49.34%.
Example 5
Selecting 14.61g of 30 single graphite films with the thickness of 60 mu m and the thickness of 10 multiplied by 10 cm; flatly paving the graphite film at the bottom of the mold, adding hydrogen peroxide and then adding concentrated sulfuric acid, wherein the volume ratio of the hydrogen peroxide to the concentrated sulfuric acid is 1: 4.5; the graphite film is rapidly expanded into expandable graphite, and the expansion multiple of the graphite film is adjusted to be 500 times by adjusting the position of the glass cover plate; washing the expandable graphite to be neutral by deionized water, and drying the neutral expandable graphite at high temperature to obtain expanded graphite; hydrolyzing 0.5g of silane coupling agent in a mixed solution of deionized water and absolute ethyl alcohol with the volume ratio of 0.2, and carrying out reaction at 80 ℃ for 20 hours; cutting 500 times of expanded graphite into 4 × 4 × 4cm expanded graphite blocks, soaking in silane coupling agent hydrolysate, washing with anhydrous ethanol for 4-7 times at 80 deg.C for 4 hr; drying the expanded graphite with the surface treated at a low temperature, soaking the dried expanded graphite in 25g of mixed solution of polyolefin and acetone in vacuum, and curing the dried expanded graphite at a high temperature to obtain a composite material; and cutting the composite material into a standard size to obtain the heat-conducting gasket with the mass filling amount of the expanded graphite of 49.34%.
The above description is only a specific embodiment of the present invention, and not all embodiments, and any equivalent modifications of the technical solutions of the present invention, which are made by those skilled in the art through reading the present specification, are covered by the claims of the present invention.
Claims (12)
1. A preparation method of an expanded graphite thermal interface material is characterized by comprising the following steps:
1) preparing expanded graphite by an oxidation intercalation method;
2) carrying out surface treatment on the expanded graphite by using a silane coupling agent to obtain modified expanded graphite;
3) and fully infiltrating the modified expanded graphite with polyolefin in a vacuum infiltration manner to obtain the expanded graphite thermal interface material.
2. The method for producing an expanded graphite thermal interface material according to claim 1, wherein the raw material for producing the expanded graphite in the step 1) is a graphite film.
3. The method for preparing an expanded graphite thermal interface material according to claim 2, wherein the step 1) is specifically: placing a graphite film in a mold with a cover plate above, adding concentrated sulfuric acid and hydrogen peroxide in any proportion, oxidizing and intercalating the graphite film into expandable graphite by two oxidants, and controlling expansion times by adjusting the position of the cover plate above the mold to obtain expandable graphite with different densities; and then repeatedly cleaning the expandable graphite until the cleaning solution is neutral, and drying the cleaned expandable graphite to obtain the expanded graphite.
4. The method for preparing an expanded graphite thermal interface material according to claim 1, wherein the step 2) is specifically: adding a silane coupling agent into a mixed solution of deionized water and absolute ethyl alcohol, and hydrolyzing for a period of time at a certain temperature to obtain a silane coupling agent hydrolysate; and soaking the expanded graphite in silane coupling agent hydrolysate, and reacting for a period of time at a certain temperature to obtain the modified expanded graphite.
5. The method of claim 4, wherein the volume ratio of the deionized water to the absolute ethyl alcohol in the mixed solution of the deionized water and the absolute ethyl alcohol is 0.2 to 0.33.
6. The method of claim 4, wherein the hydrolysis reaction temperature is 70-90 ℃ and the hydrolysis time is 15-20 h.
7. The method for preparing the expanded graphite thermal interface material according to claim 4, wherein the temperature of the reaction of soaking the expanded graphite in the silane coupling agent hydrolysate is 70-90 ℃, and the reaction time is 2-6 h.
8. The method of claim 4, further comprising the step of cleaning and drying after the reaction is completed.
9. The method for preparing an expanded graphite thermal interface material according to claim 1, wherein the step 3) is specifically: placing the modified expanded graphite in a container, adding a mixed solution of polyolefin and acetone, vacuumizing to enable the polyolefin to fully infiltrate the expanded graphite, and then curing at high temperature to obtain the expanded graphite thermal interface material.
10. The method of claim 9, wherein the expanded graphite thermal interface material has an expanded graphite mass loading of 10-50%.
11. The method as claimed in claim 9, wherein the temperature of the high temperature curing is 120-150 ℃ and the time of the high temperature curing is 6-8 h.
12. An expanded graphite thermal interface material produced by the process for producing an expanded graphite thermal interface material according to any one of claims 1 to 11.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113788986A (en) * | 2021-09-07 | 2021-12-14 | 天津大学 | Modified graphite-based functional filler, thermal interface material and preparation method thereof |
| CN114621734A (en) * | 2022-04-24 | 2022-06-14 | 桂林电子科技大学 | Expanded graphite-carbon fiber thermal interface material and preparation method thereof |
| CN116534854A (en) * | 2023-04-25 | 2023-08-04 | 广东思泉新材料股份有限公司 | Expanded foaming graphite film, preparation method thereof and application thereof in semiconductor heat dissipation device |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113788986A (en) * | 2021-09-07 | 2021-12-14 | 天津大学 | Modified graphite-based functional filler, thermal interface material and preparation method thereof |
| CN114621734A (en) * | 2022-04-24 | 2022-06-14 | 桂林电子科技大学 | Expanded graphite-carbon fiber thermal interface material and preparation method thereof |
| CN116534854A (en) * | 2023-04-25 | 2023-08-04 | 广东思泉新材料股份有限公司 | Expanded foaming graphite film, preparation method thereof and application thereof in semiconductor heat dissipation device |
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Application publication date: 20210730 |