CN112937065A - Preparation method of organic silicon/graphene thermal interface material - Google Patents
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Abstract
The invention belongs to the technical field of thermal interface materials, and discloses a preparation method of an organic silicon/graphene thermal interface material, which comprises the following steps: (1) coating a layer of adhesive on one side of the surface of the graphite film or the graphene film; (2) attaching the silica gel pad to one side coated with the binder graphite film or the graphene film; (3) coating a layer of adhesive on the surface of one side of the silica gel pad sample obtained in the step (2); (4) then, attaching the new graphite film or the graphene film to the sample obtained in the step (3); (5) and (4) repeating the steps (1) to (3) on the basis of obtaining the sample in the step (4), so as to obtain the organosilicon/graphene thermal interface material with a stacked structure. The graphite film is applied to the thermal interface material of an organic silicon system, and the thermal interface material prepared by the method has the advantages of high heat conduction, good mechanical property and good compatibility.
Description
Technical Field
The invention belongs to the technical field of thermal interface materials, and relates to a preparation method of an organic silicon/graphene thermal interface material.
Background
The thermal interface material is an indispensable thermal management material in the field of electronic packaging, is used for filling a gap between two interface contact areas, reduces heat transfer resistance, and plays an important role in performance, service life and stability of an electronic device. Thermal interface materials are typically compounded with highly thermally conductive fillers and a polymer matrix that is light and soft. Silicone [1], one of the most widely used polymer substrates in the industry at present, is soft and stable in performance, and is continuously accepted in the industry. The traditional heat-conducting filler is mainly ceramics (alumina and boron nitride), metals (aluminum powder and silver powder) and the like. With the increasing heat productivity of chips, the problem of heat dissipation of chips becomes one of the key factors restricting the development of chips, and the traditional thermal interface material cannot meet the requirements. The graphene has ultrahigh thermal conductivity, and the experimental measurement result is as high as 5000+ W/(m.K) [2 ]. Secondly, the domestic degree of the graphene is higher, and the domestic related product performance is ahead of the world. The thermal conductivity of the mature commercial graphite film can also reach 1600W/(m.K). Therefore, graphene is expected to be a new and expensive material in the field of thermal interface materials. However, when graphene is combined with silicone, the silicone often does not cure. One possible explanation is: during the preparation process of graphene, some nitrogen, phosphorus and sulfur elements are introduced, and the elements cause poisoning of a platinum catalyst required by organosilicon curing, so that the curing is difficult.
In the prior art, a metal/organic silicon composite material, a ceramic/organic silicon composite material and a carbon-based filler/organic silicon composite material are adopted as thermal interface materials. Wherein, 1, the metal/organic silicon composite material: inoue M3, etc. to research the heat conducting performance of composite material with silver sheet and silver grain as stuffing. The silver sheet and the silver particles are compounded according to a certain proportion, and when the mass fraction of the silver is 85%, the in-plane thermal conductivity of the thermal interface material can reach 26W/(m.K). If the polymer is filled in the form of randomly distributed silver particles, the thermal conductivity of the thermal interface material can reach 11W/(m.K). In the application process of the thermal interface material, heat is transferred through the vertical direction, so the index of the thermal conductivity in the vertical direction is more important. 2. Ceramic/silicone composite: the ceramic particles include aluminum oxide, boron nitride, aluminum nitride, silicon carbide, zinc oxide, and the like. Generally used in the field with higher requirements on electrical insulation performance. Alumina is most commonly used, with the lowest cost, but the intrinsic thermal conductivity is low, about 30W/(m · K), and aluminum nitride has very high intrinsic thermal conductivity, up to 170W/(m · K), but is costly. And (4) the royal ruby and the like are prepared by compounding aluminum oxide and aluminum nitride according to the mass ratio of 89:11, and when the mass fraction of the filler is 90%, the thermal conductivity reaches 4.0W/(m.K). 3. Carbon-based filler/silicone composite: the carbon fiber is a high-heat-conductivity filler, and the heat conductivity can reach 700W/(m.K). Uetani et al [5] use electrostatic flocking method to prepare carbon fiber based thermal interface material, the vertical direction thermal conductivity can reach 23.3W/(m.K), the filler content is 13.2 wt%.
The thermal interface material in the prior art has the following defects: 1. the existing thermal interface material adopting alumina as filler has insufficient heat conductivity and is difficult to adapt to the heat dissipation requirement of the 5G era. The thermal interface material adopting high-thermal-conductivity fillers such as silver, aluminum nitride and the like is high in preparation cost, and the high thermal conductivity of the thermal interface material is not fully utilized, for example, the intrinsic thermal conductivity of silver can reach 429W/(m.K), and when the mass fraction of silver is 85%, the thermal conductivity of the thermal interface material is only 26W/(m.K). 2. Among carbon-based fillers, carbon fibers are the main materials with good performance and mature technology, but carbon fibers are high in cost and are mainly imported from Japan, and the risk that raw materials are controlled abroad exists. The graphite film has a plurality of domestic manufacturers, the heat conductivity is higher than that of carbon fiber, the heat conductivity of the graphite film is more than 1600W/(m.K), and the carbon fiber is about 900W/(m.K). However, the graphite film is difficult to be popularized and applied in the thermal interface material of the organic silicon system mainly because the graphite film easily causes the poisoning and non-curing of the silica gel catalyst.
Reference documents:
[1] sujunjie, Li Miao, von Yihong, Zenghappy, Cheng Xizhong, Wu Cheng Rong.
[2]Tong X C(2011)Thermal Interface Materials in Electronic Packaging.In:Advanced Materials for Thermal Management of Electronic Packaging.Springer Series in Advanced Microelectronics,vol 30.Springer,New York,NY.
[3]Inoue M,Liu J.Effects of Multi-modal Filler Size Distributions on Thermal Conductivity of Electrically Conductive Adhesives Containing Ag Micro and Nanoparticles[J].Transactions of the Japan Institute of Electronics Packaging,2010,2(1):125-133.
[4] Preparation and research of high-performance organosilicon heat-conducting materials [ J ] organosilicon materials, 2017,31(02):82-85.
[5]Uetani K,Ata S,Tomonoh S,et al.Elastomeric Thermal Interface Materials with High Through-Plane Thermal Conductivity from Carbon Fiber Fillers Vertically Aligned by Electrostatic Flocking[J].Advanced Materials,2015,26(33):5857-5862.
Disclosure of Invention
Aiming at the technical problems mentioned in the background technology, the invention provides a preparation method of an organic silicon/graphene thermal interface material, the prepared thermal interface material has a novel organic silicon/graphite film laminated structure, and the problem of catalyst poisoning is avoided because the graphene is directly contacted with the organic silicon in the structure. The schematic diagram of the laminated structure of the silicone/graphite film is shown in fig. 1, a layer of adhesive is respectively sprayed on two sides of the silica gel pad, and the graphite film is adhered on the adhesive, wherein the silica gel pad is cured silicone, and the graphite film cannot be adhered due to poor adhesiveness of the silica gel pad, so a layer of adhesive is respectively sprayed on two sides of the silica gel pad.
The invention aims to provide a preparation method of an organic silicon/graphene thermal interface material, which comprises the following steps:
(1) coating a layer of adhesive on one side of the surface of the graphite film or the graphene film;
(2) attaching the silica gel pad to one side coated with the binder graphite film or the graphene film;
(3) coating a layer of adhesive on the surface of one side of the silica gel pad sample obtained in the step (2);
(4) then, attaching the new graphite film or the graphene film to the sample obtained in the step (3);
(5) and (4) repeating the steps (1) to (3) on the basis of obtaining the sample in the step (4), so as to obtain the organosilicon/graphene thermal interface material with a stacked structure.
The preparation method of the organic silicon/graphene thermal interface material further comprises a step (6), wherein the organic silicon/graphene thermal interface material sample with the stacked structure obtained in the step (5) is cut into slices along the lamination thickness direction, and the thickness of each slice is 0.3-3 mm.
The preparation method of the organic silicon/graphene thermal interface material further comprises a step (7) of polishing the thin slice sample obtained in the step (6).
In the technical scheme of the invention, the volume fraction of the graphite film or the graphene film in the organosilicon/graphene thermal interface material with the stacked structure is 7.4-40%, and is preferably 17.2%.
In the technical scheme of the invention, the thickness of the silica gel pad is 50-200 μm, and preferably 100 μm.
In the technical scheme of the invention, the thickness of the binder is 5-20 μm, and preferably 10 μm.
In the technical scheme of the invention, the thickness of the graphite film or the graphene film is 17-40 μm, and preferably 25 μm.
In the technical scheme of the invention, the thickness of the organosilicon/graphene thermal interface material with the stacked structure is 30 mm.
In the technical scheme of the invention, the cutting adopts ultrasonic cutting or linear cutting.
In the technical scheme of the invention, the adhesive is polybutadiene and polymethyl methacrylate, preferably polybutadiene, and the polybutadiene adhesive has strong viscosity and good elasticity.
Before the silica gel is contacted with the graphite film or the graphene film, the organic silicon is cured into the silica gel pad, and the silica gel pad is pressed into a thin film through rolling equipment. The silica gel pad has poor viscosity, so that the graphite film cannot be adhered. The polyolefin has strong viscosity and good elasticity, so that the polybutadiene adhesive is sprayed on the two surfaces of the silica gel pad.
Compared with the prior art, the technical scheme of the invention has the following beneficial effects:
1. according to the invention, the graphite film is applied to the thermal interface material of an organic silicon system, the prepared organic silicon/graphene thermal interface composite material has good heat conductivity, and when the graphite volume fraction is 17.2 vol% (the thickness of the graphite film is 25 μm, the thickness of the silica gel pad is 100 μm, and the thickness of the binder is 10 μm), the heat conductivity is as high as 75.8W/(m.K).
2. The organic silicon/graphene thermal interface composite material prepared by the invention has good mechanical properties and certain resilience. The test result shows that when the maximum compression strain is 40%, the elastic deformation can be recovered to 20% strain in a short time, and the elastic recovery rate is 50%.
3. The invention belongs to a silica gel-based thermal interface material, which is one of the most widely applied base materials in the field of electronic packaging at present, so that the organic silicon/graphene thermal interface material provided by the invention has good compatibility with the existing system.
Drawings
Fig. 1 is a schematic view of the novel laminated structure of the present invention.
FIG. 2 is a flow chart of the preparation of the silica gel pad/graphite film thermal interface material of the present invention.
FIG. 3 is a schematic diagram of a system for preparing a silica gel pad/graphite film thermal interface material according to the present invention.
FIG. 4 is a sample object diagram of the silica gel pad/graphite film thermal interface material of the present invention.
FIG. 5 is a detection signal output curve of the silica gel pad/graphite film thermal interface material of the present invention using a laser thermal conductivity meter.
FIG. 6 is a graph showing the compression rebound characteristics of the silica gel pad/graphite film thermal interface material of the present invention.
Detailed Description
The present invention will be described in further detail with reference to examples, but the embodiments of the present invention are not limited thereto.
The experimental methods used in the following examples are all conventional methods unless otherwise specified; reagents, materials and the like used in the following examples are commercially available unless otherwise specified.
For the purpose of better explaining the present invention and to facilitate understanding, the present invention will be described in detail by way of specific embodiments with reference to the accompanying drawings.
Example 1
Fig. 2 is a flow chart showing the preparation of the silica gel pad/graphite film thermal interface material of the present invention, and fig. 3 is a schematic diagram showing the device of the silica gel pad/graphite film thermal interface material preparation system of the present invention.
The preparation method comprises (1) selecting 25 μm graphite film and 100 μm cured silica gel pad as raw materials. The supplied materials are coil materials, and the width of the supplied materials is 12 cm. Spraying adhesive on one side of the graphite film. Polybutadiene was used as the binder in this example, and the thickness of the sprayed binder was 10 μm.
(2) The silica gel pad is tightly attached to the graphite film on one side of the adhesive sprayed on the silica gel pad through the roll-to-roll attaching device, and the adhesive is used for changing the polarity of the surface of the silica gel pad so that the silica gel pad can be tightly attached to the graphite film.
(3) And spraying a layer of adhesive again on the surface of one side of the silica gel pad of the sample of the organic silicon/graphite composite membrane obtained after the attaching, wherein the thickness of the adhesive is 10 microns.
(4) Then, a new layer of graphite film is attached to the side, with the adhesive, of the sample obtained in the step (3);
(5) and (4) repeating the steps (1) to (3) for 206 times on the basis of the sample obtained in the fourth step, wherein the lamination thickness reaches 3cm, and thus the organic silicon/graphene thermal interface material with the stacked structure is obtained. The in-plane dimensions of the stack were 12cm x 12 cm.
In this example, the volume fraction of the graphite film was 17.2%.
(6) Depending on the type of adhesive, it is determined whether curing of the laminate is required. The polybutadiene curing conditions used in this example were 120 ℃ for 4 hours. And (3) cutting the organosilicon/graphene thermal interface material sample with the stacked structure obtained in the step (5) into slices along the thickness direction of the stacked layer by using an ultrasonic cutting process, wherein the slices are the thermal interface material, and the thickness of the slices is 0.3-3 mm. The in-plane dimensions of the flakes were cut 3cm by 3cm for experimental testing.
(7) And (4) grinding and polishing the sample obtained in the step (6). Fig. 4 is a sample object diagram of the silica gel pad/graphite film thermal interface material prepared in this example.
Firstly, testing and characterizing:
the organosilicon/graphene thermal interface material prepared in example 1 is tested and characterized, and the results are as follows:
(1) thermal conductivity test
Sample information for silicone/graphene thermal interface material: the thickness of the graphite film is 25 mu m, the thickness of the silica gel pad is 100 mu m, and the thickness of the adhesive is 10 mu m.
The thermal conductivity test criteria are shown in table 1 below.
TABLE 1
The test method comprises the following steps: the thermal diffusivity is tested by a laser thermal conductivity meter LFA467, and fig. 5 shows a schematic diagram of detection signals of the laser thermal conductivity meter. The change rule of the detection curve shows that the test result is credible. The results of testing samples of silicone/graphene thermal interface materials are shown in table 2 below:
TABLE 2
| Detecting items | Results |
| Density p | 2.25g/cm3 |
| Specific heat capacity c | 0.92J/(g·K) |
| Coefficient of thermal diffusion alpha | 36.6mm2/s |
| Thermal conductivity λ (λ ═ α · c · ρ) | 75.8W/(m·K) |
| Thickness s | 2.75mm |
(2) Mechanical Property test
Rebound resilience is an important performance index requirement for thermal gaskets. Fig. 6 shows the rebound condition of 40% of the maximum compressive strain of the thermal conductive gasket prepared in example 1, and the result shows that the sample rebounds to 20% of the compressive strain in a short time, and the rebound rate is 50%.
The above embodiments are merely illustrative of the technical concept and features of the present invention, and the purpose thereof is to enable those skilled in the art to understand the content of the present invention and implement the invention, and not to limit the scope of the present invention, and all equivalent changes or modifications made according to the spirit of the present invention should be covered in the scope of the present invention.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (10)
1. A preparation method of an organic silicon/graphene thermal interface material is characterized by comprising the following steps:
(1) coating a layer of adhesive on one side of the surface of the graphite film or the graphene film;
(2) attaching the silica gel pad to one side coated with the binder graphite film or the graphene film;
(3) coating a layer of adhesive on the surface of one side of the silica gel pad sample obtained in the step (2);
(4) then, attaching the new graphite film or the graphene film to the sample obtained in the step (3);
(5) and (4) repeating the steps (1) to (3) on the basis of obtaining the sample in the step (4), so as to obtain the organosilicon/graphene thermal interface material with a stacked structure.
2. The preparation method of the silicone/graphene thermal interface material according to claim 1, further comprising a step (6) of cutting the silicone/graphene thermal interface material sample of the stacked structure obtained in the step (5) into thin sheets with a thickness of 0.3-3 mm along the thickness direction of the stacked layer.
3. The method for preparing the silicone/graphene thermal interface material according to claim 1, further comprising a step (7) of subjecting the obtained sheet sample obtained in step (6) to a grinding and polishing treatment.
4. The method for preparing the silicone/graphene thermal interface material according to claim 1, wherein the volume fraction of the graphite film or the graphene film in the silicone/graphene thermal interface material in the stacked structure is 7.4% to 40%, preferably 17.2%.
5. The method for preparing the silicone/graphene thermal interface material according to claim 1, wherein the thickness of the silica gel pad is 50-200 μm, preferably 100 μm.
6. The method for preparing the silicone/graphene thermal interface material according to claim 1, wherein the thickness of the binder is 5-20 μm, preferably 10 μm.
7. The method for preparing the silicone/graphene thermal interface material according to claim 1, wherein the thickness of the graphite film or the graphene film is 17-40 μm, preferably 25 μm.
8. The method of claim 1, wherein the stacked-structure silicone/graphene thermal interface material has a thickness of 30 mm.
9. The method for preparing the silicone/graphene thermal interface material according to claim 1, wherein the cutting is ultrasonic cutting or wire cutting.
10. The method of claim 1, wherein the binder is polybutadiene, polymethyl methacrylate, and preferably polybutadiene.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114213986A (en) * | 2021-11-17 | 2022-03-22 | 深圳市鸿富诚新材料股份有限公司 | Heat-conducting and insulating graphene gasket and preparation method thereof |
| CN115092920A (en) * | 2022-06-27 | 2022-09-23 | 常州富烯科技股份有限公司 | Graphene heat-conducting gasket and preparation method thereof |
| CN115340767A (en) * | 2022-08-26 | 2022-11-15 | 安徽宇航派蒙健康科技股份有限公司 | High-thermal-conductivity insulating silica gel and preparation method thereof |
| WO2024036611A1 (en) * | 2022-08-19 | 2024-02-22 | 中国科学院深圳先进技术研究院 | Gecko-claw-imitating composite thermal interface material and preparation method therefor |
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