CN115214202A - High-thermal-conductivity layered thermal interface material and preparation method thereof - Google Patents
High-thermal-conductivity layered thermal interface material and preparation method thereof Download PDFInfo
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Abstract
A preparation method of a high-thermal-conductivity layered thermal interface material belongs to the field of thermal management materials. Relates to a high-thermal-conductivity electrical insulation heat-conduction composite material for high-power electronic equipment. The composite material consists of an upper layer, a middle layer and a lower layer, wherein the upper layer and the lower layer have the same components, the middle layer adopts high filling with four granularities, the upper layer and the lower layer adopt low filling with three granularities, the viscosity of the upper layer and the lower layer is lower, the surfaces of equipment can be more easily attached, the filling amount of the middle layer is high, the viscosity of the middle layer is higher, the particles are tightly connected, more heat conduction paths can be formed, and therefore the high heat conduction performance is realized. The composite material of the middle layer and the upper and lower layers consists of the following components in percentage by mass: 80-98wt% of heat-conducting filler, 0-10wt% of matrix, 1-5wt% of coupling agent (relative to the total mass of the heat-conducting filler) and 1-5wt% of catalyst. The invention modifies fillers with different shapes and particle diameters and is tightly packed in Dinger-FunkThe proportion close to the optimal grain composition is calculated on the basis of the filling model, and the thermal conductivity of the prepared material reaches up to 8 W.m ‑1 ·K ‑1 The viscosity is moderate, and the cost is low, so that the method is suitable for industrial production and manufacturing use.
Description
Technical Field
The invention belongs to the field of heat management materials, and particularly relates to a thermal interface material with high thermal conductivity and a preparation process thereof.
Background
In recent years, with the rapid development of intelligent devices and mechanical devices in China, the loads and power consumption of various electronic devices are continuously increased, and high integration level, small size and high power are the development directions of various electronic devices.
However, the heat dissipation problem is very important when various devices are miniaturized and lightly loaded. The electronic device and the heat sink are in contact with each other at two solid-solid interfacesThe actual contact area of the interface is very small, uneven gaps exist, and the thermal conductivity is low (0.024 W.m) -1 ·K -1 ) The air is filled, and the heat transfer enhancement between the two solid-solid interfaces is just a weak link in the whole heat dissipation system, if the heat cannot be led out in time, waste heat is gathered in a narrow space in the device, so that the problems of overhigh local temperature, uneven heat flow distribution and the like are caused, the normal work of the device is influenced, and the instability of equipment in operation is increased.
If the thermal interface material is filled in a gap between the electronic device and the radiator, the close contact between the electronic device and the radiator can be ensured, and heat generated by the device during working can be effectively led out in time, so that the heat dissipation performance is optimized.
The Chinese patent with patent grant publication number CN109486192B discloses a self-leveling high-heat-conduction high-temperature-resistant thermal interface material and a preparation method thereof, and the technical scheme is characterized in that high-temperature-resistant performance is obtained by adding a high-temperature-resistant matrix and a high-temperature-resistant heat-conduction filler; the filler with different particle diameters and different types is compounded to achieve the maximum filling in the silicone grease so as to obtain the balance of heat conductivity and viscosity, and the finally obtained self-leveling property is good, and the heat conductivity is higher than 3.0 W.m -1 ·K -1 The thermal interface material of (1).
Chinese patent with patent No. CN110204903B discloses a high-thermal-conductivity thermal-conductive silicone grease and a preparation method thereof, wherein the thermal conductivity of the thermal-conductive silicone grease can reach more than 5W/mK, the viscosity is lower than 20 ten thousand MPa.S, and the thermal-conductive silicone grease has the advantages of high thermal-conductive efficiency and good use durability.
However, the above heat-conductive silicone grease has a certain heat-conductive property or a low viscosity, but the technical characteristics of high heat conductivity and high adhesion with equipment are not outstanding, and most devices are developed toward miniaturization, high power and high heat flow at present, and waste heat is concentrated in a narrow space inside the devices, so that it is necessary to develop a thermal interface material which has high heat conductivity and is highly adhered to two solid-solid interfaces of a heating part and a radiating part of the devices.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a layered thermal interface material with high thermal conductivity, wherein the thermal conductivity coefficient of the layered thermal interface material can reach 8 W.m -1 ·K -1 The process is simple, and the market demand can be met.
In order to realize the purpose, the invention provides the following technical scheme:
the high-thermal-conductivity layered thermal interface material is characterized by comprising the following components in percentage by mass:
heat conductive filler: 80-98wt%;
matrix: 0 to 10wt%;
coupling agent: 1-5wt%;
1-5wt% of catalyst.
Further, the heat-conducting filler is divided into an upper layer, a middle layer and a lower layer, wherein the upper layer filler and the lower layer filler consist of the following three types of fillers:
30-60wt% of first heat-conducting filler;
40-60wt% of a second type of heat-conducting filler;
5-20wt% of a third type of heat-conducting filler;
wherein the grain diameter of the first heat conduction filler is 50-100 microns, the second is 3-20 microns, and the third is 0.1-2 microns. The filler is alumina, boron nitride, aluminum nitride, zinc oxide or the mixture thereof, and is spherical or nearly spherical; it has been found that for most appliances, the loading of alumina is preferably 30-50wt% and the loading of aluminum nitride is preferably 40-60wt%.
Further, the intermediate layer heat-conducting filler is composed of the following four types of fillers:
30-50wt% of first heat-conducting filler;
0-20wt% of a second type of heat-conducting filler;
20-40wt% of a third heat-conducting filler;
0-20wt% of a fourth type of heat-conducting filler;
the middle layer and the upper and lower layers have similar fillers, wherein the first type of filler has a particle size of 50-100 microns, the second type of filler has a particle size of 20-40 microns, the third type of filler has a particle size of 1-3 microns, and the fourth type of filler has a particle size of 0.1-0.3 microns. The fillers can be alumina, boron nitride, aluminum nitride, zinc oxide, etc. or mixtures thereof, and can be spherical or nearly spherical in shape, with the total loading of each filler in the intermediate layer being between 40-60wt%.
Further, the upper and lower layer substrates and the intermediate layer substrate are one or more of polyethylene, epoxy resin, acrylic acid, polyurethane or silicone oil, and have a significantly different hardness than the intermediate layer, and it is preferable that the viscosity of the liquid substrate is 90 to 1000cps.
Further, the coupling agent is one or more of 3- (2,3-glycidoxy) propyl trimethoxy silane, vinyl trimethoxy ethoxy silane, gamma-methacryloxypropyl trimethoxy silane and the like; the catalyst is platinum catalyst.
The preparation method of the layered thermal interface material with high thermal conductivity comprises the following two steps:
p1: firstly, respectively carrying out surface modification on heat-conducting fillers, and comprising the following steps:
step 3, adding deionized water according to the minimum water requirement, adding acetic acid to adjust the pH value to acidity, adding coupling agents under continuous oscillation, standing for a period of time until the solution becomes clear to obtain a fully hydrolyzed coupling agent solution, and adding quantitative absolute ethyl alcohol (the mass ratio of alcohol to water is 95: 5);
p2: the thermal interface material is prepared by mixing the filler and the matrix, and the steps are as follows:
adding all the fillers into the matrix in batches according to the particle size, placing the fillers into a planetary stirrer for fully stirring, grinding the fillers for a long time until no macroscopic small particles exist, and finally placing the fillers into a vacuum oven for vacuum defoaming to obtain the thermal interface material.
Through adopting above-mentioned technical scheme, arrange above multiple different kind, different shapes, different particle size filler powder, make to produce synergistic effect between the filler, form abundant heat conduction network in the base member, and calculate suitable coupling agent quantity in order to increase the affinity between base member and filler in view of granule nature itself, promote the dispersion of filler in the base member, then make the filler evenly fill in the base member through stirring and grinding, heat accessible multiple route conducts in thermal interface material body layer, heat conduction efficiency has been promoted. The composite material comprises an upper layer, a middle layer and a lower layer, wherein the upper layer, the lower layer and the middle layer are same in composition, the middle layer is filled with high filler with four granularities, the upper layer and the lower layer are filled with low filler with three granularities, the upper layer and the lower layer are lower in viscosity and are easier to adhere to equipment and the surface of the middle layer, the middle layer is high in filler with high viscosity and is connected tightly among particles, more heat conduction paths can be formed, and the prepared layered composite material has high heat conductivity and good flexibility and has high practical value.
In conclusion, by adopting the technical scheme, the prepared thermal interface material has moderate viscosity, good heat conduction performance and heat conduction coefficient reaching 8 W.m -1 ·K -1 The above.
The invention has at least one of the following beneficial technical effects: firstly, the filler powder with different types and particle sizes is uniformly dispersed in the matrix by mixing and lapping, so that abundant heat conduction network chains are formed, and a better heat dissipation effect is achieved; the upper layer and the lower layer adopt low filling with three granularities, and the viscosity is low under low filling amount, so that the equipment surface can be attached easily and a high filling interface layer can be connected easily.
Secondly, based on the difference of the particle size and the properties of various fillers, the proper amount of the coupling agent is calculated by theory, which is beneficial to the dispersion of the coupling agent in a matrix, and the modified filler powder can be effectively interconnected with the matrix, so that the internal pores and air of the material can be reduced, the compatibility and the affinity of the two are improved, the contact thermal resistance between interfaces is reduced, and the heat conductivity coefficient is improved.
And thirdly, ceramics are used as fillers to prepare the high-thermal-conductivity electrical-insulation thermal interface material, the high-thermal-conductivity electrical-insulation thermal interface material can be applied to occasions with higher requirements on insulation performance, the thickness of the layered thermal interface material prepared by the invention can be large or small, the preparation process is simpler, and the layered thermal interface material can be suitable for different electronic devices.
Drawings
FIG. 1 is a schematic diagram of a heat transfer principle of a thermal interface material and a layered composite material.
Fig. 2 is an SEM image of the thermal interface material.
Note: a. b and c are embodiment 10; d. e, f are embodiment 13
FIG. 3 is a graph showing a close packed model particle size distribution.
Table 1: thermal performance data of the prepared composite.
Detailed Description
The following detailed description of embodiments of the invention
Example 1
A composite thermal interface material with high thermal conductivity is composed of matrix, thermally conductive filler and coupling agent. Wherein, the shapes of the first type, the second type and the third type of fillers are all spherical or nearly spherical, the volume ratio of the third type to the second type to the first type of fillers is 5: 35: 60, the volume filling amount of the fillers is 76vol%, and finally the measured thermal conductivity of the material is 4.40 W.m -1 ·K -1 。
Example 2
A composite thermal interface material with high thermal conductivity is composed of matrix, thermally conductive filler and coupling agent. Wherein the first type, the second type and the third type of fillers are all spherical or nearly spherical, the volume ratio of the third type to the second type to the first type of fillers is 5: 35: 60, the filling amount is 78vol%, and the thermal conductivity of the material is 4.86 W.m -1 ·K -1 。
Embodiment 3
A composite thermal interface material with high thermal conductivity is composed of matrix, thermally conductive filler and coupling agent. Wherein the first type, the second type and the third type of fillers are all spherical or nearly spherical, the volume ratio of the third type to the second type to the first type of fillers is 5: 35: 60, the filling amount is 80vol%, and the thermal conductivity is 5.65 W.m -1 ·K -1 。
Example 4
A composite thermal interface material with high thermal conductivity is composed of matrix, thermally conductive filler and coupling agent. Wherein the first type, the second type and the third type of fillers are all spherical or nearly spherical, the volume ratio of the third type to the second type to the first type of fillers is 5: 35: 60, the filling amount is 82vol%, and the thermal conductivity is 6.60 W.m -1 ·K -1 。
Example 5
A composite thermal interface material with high thermal conductivity is composed of matrix, thermally conductive filler and coupling agent. Wherein the first type, the second type and the third type of fillers are all spherical or nearly spherical, the volume ratio of the third type to the second type to the first type of fillers is 12: 25: 63, the filling amount is 82vol%, and the thermal conductivity is 6.10 W.m -1 ·K -1 。
Example 6
A composite thermal interface material with high thermal conductivity is composed of matrix, thermally conductive filler and coupling agent. Wherein the first type, the second type and the third type of fillers are all spherical or nearly spherical, the volume ratio of the third type to the second type to the first type of fillers is 15: 25: 60, the filling amount is 82vol%, and the thermal conductivity is 6.30 W.m -1 ·K -1 。
Example 7
A composite thermal interface material with high thermal conductivity is composed of matrix, thermally conductive filler and coupling agent. Wherein the first type, the second type and the third type of fillers are all spherical or nearly spherical, the volume ratio of the third type to the second type to the first type of fillers is 15: 25: 60, the filling amount is 84vol%, and the thermal conductivity is 7.21 W.m -1 ·K -1 。
Example 8
A composite thermal interface material with high thermal conductivity is composed of matrix, thermally conductive filler and coupling agent. Wherein the first type, the second type and the third type of fillers are all spherical or nearly spherical, the volume ratio of the third type to the second type to the first type of fillers is 15: 25: 60, the filling amount is 85vol%, and the thermal conductivity is 7.62 W.m -1 ·K -1 。
Example 9
A composite thermal interface material with high thermal conductivity is composed of matrix, thermally conductive filler and coupling agent. Wherein the first type, the second type and the third type of fillers are all spherical or nearly spherical, the volume ratio of the third type to the second type to the first type of fillers is 15: 25: 60, the filling amount is 86vol%, and the thermal conductivity is 7.90 W.m -1 ·K -1 。
Example 10
A composite thermal interface material with high thermal conductivity is composed of matrix, thermally conductive filler and coupling agent. Wherein the first type, the second type and the third type of fillers are all spherical or nearly spherical, the volume ratio of the third type to the second type to the first type of fillers is 10: 35: 55, the filling amount is 84vol%, and the thermal conductivity is 7.27 W.m -1 ·K -1 。
Example 11
A composite thermal interface material with high thermal conductivity is composed of matrix, thermally conductive filler and coupling agent. Wherein the first type, the second type and the third type of fillers are all spherical or nearly spherical, the volume ratio of the third type to the second type to the first type of fillers is 10: 35: 55, the filling amount is 85vol%, and the thermal conductivity is 8.25 W.m -1 ·K -1 。
Example 12
A composite thermal interface material with high thermal conductivity is composed of matrix, thermally conductive filler and coupling agent. Wherein, the first type, the second type, the third type and the fourth type of fillers are all spherical or nearly spherical, the volume ratio of the fourth type to the third type to the second type to the first type of fillers is 13: 17: 37: 33, the filling amount is 85vol%, and the thermal conductivity is 8.10 W.m -1 ·K -1 。
Example 13
A composite thermal interface material with high thermal conductivity is composed of matrix, thermally conductive filler and coupling agent. Wherein, the shapes of the first type, the second type, the third type and the fourth type of fillers are all spherical or nearly spherical, the volume ratio of the fourth type to the third type to the second type to the first type of fillers is 10: 35: 10: 45, the filling amount is 85vol%, and the thermal conductivity of the material is 8.42 W.m -1 ·K -1 。
Example 14
A composite thermal interface material with high thermal conductivity is composed of matrix, thermally conductive filler and coupling agent. Wherein the first type, the second type, the third type and the fourth type of fillers are all spherical or nearly spherical, the volume ratio of the fourth type to the third type to the second type to the first type of fillers is 10: 35: 20: 35, the filling amount is 85vol%, and finally the measured thermal conductivity is 7.92 W.m -1 ·K -1 。
Thermal performance tests were performed on the thermal interface materials prepared in examples 1-14 and the results are shown in table 1.
The layered thermal interface material with the thermal conductivity of 8 W.m is finally prepared by compacting the embodiment 10 as an upper layer and a lower layer and 13 as an intermediate layer -1 ·K -1 The above.
Tight packing model calculation case: selecting three fillers with different particle size distribution ranges, D 50 Carrying out multi-scale mixing and compounding on three fillers with the particle sizes of 60 mu m, 3 mu m and 300nm respectively, and calculating the volume percentage of the three fillers in compounding by adopting a Dinger-Funk equation, wherein the process is as follows: firstly, determining the distribution range of the particle size of the heat-conducting powder filler: the distribution range of 300nm particle size is [0.12,2 ]]The range of the distribution interval of the 3 μm particle diameter is [1.6, 10.0 ]]The distribution range of the particle diameter of 60 μm is [3, 140 ]]. Then, dinger-Funk closest packing equation
Wherein, the values of Dmax =170, dmin =0.15, n =0.37 and U (Dp) in the composite heat-conducting powder filler system are obtained by taking the value of Dp, as shown in the following table2, as shown in the figure:
therefore, the volume of the filler with three different particle sizes of 20 μm, 6 μm and 2 μm in the total composite heat-conducting powder filler is 100-37=63 (%), 37-12=15 (%), 12-0=12 (%). Finally, the volume filling amount of the heat-conducting powder filler with three different particle sizes is obtained, and the formula is as follows: 63vol% of first type filler, 15vol% of second type filler and 12vol% of third type filler.
Table 1 composite thermal performance data
TABLE 2U (Dp) calculated for different Dps
Claims (7)
1. The preparation method of the high-thermal-conductivity layered thermal interface material is characterized in that the thermal interface material consists of the following components in percentage by mass:
heat-conducting filler: 80-98wt%;
matrix: 0 to 10wt%;
coupling agent: 1-5wt%;
1-5wt% of catalyst.
2. The method for preparing the layered thermal interface material with high thermal conductivity as claimed in claim 1, wherein the thermal interface material is composed of the thermal conductive filler and the matrix, and is divided into an upper layer, a middle layer and a lower layer, wherein the thermal conductive filler of the upper layer and the lower layer is composed of the following three types of fillers:
30-60wt% of first heat-conducting filler;
40-60wt% of a second type of heat-conducting filler;
5-20wt% of a third type of heat-conducting filler;
wherein the grain diameter of the first type of heat-conducting filler is 50-100 micrometers, the grain diameter of the second type is 3-20 micrometers, and the grain diameter of the third type is 0.1-2 micrometers; the filler is alumina, boron nitride, aluminum nitride, zinc oxide or a mixture thereof and is spherical or approximately spherical in shape.
3. The method for preparing a layered thermal interface material with high thermal conductivity as claimed in claim 2, wherein the loading amount of the alumina is 30-50wt% and the loading amount of the aluminum nitride is 40-60wt%.
4. The method for preparing a layered thermal interface material with high thermal conductivity as claimed in claim 2, wherein the intermediate layer thermal conductive filler is composed of the following four types of thermal conductive fillers:
30-50wt% of first heat-conducting filler;
0-20wt% of a second type of heat-conducting filler;
20-40wt% of a third type of heat-conducting filler;
0-20wt% of a fourth type of heat-conducting filler;
the middle layer and the upper and lower layers have similar fillers, wherein the particle size of the first filler is 50-100 micrometers, the particle size of the second filler is 20-40 micrometers, the particle size of the third filler is 1-3 micrometers, and the particle size of the fourth filler is 0.1-0.3 micrometer; the filler is alumina, boron nitride, aluminum nitride, zinc oxide or their mixture, and has spherical or nearly spherical shape, and the total filling amount of each filler in the middle layer is 40-60wt%.
5. The layered thermal interface material with high thermal conductivity of claim 2, wherein: the upper and lower layer matrix and the middle layer matrix are one or more of polyethylene, epoxy resin, acrylic acid, polyurethane or silicone oil, and have obviously different hardness compared with the middle layer, if the matrix is liquid, the viscosity is 90-1000cps.
6. A high thermal conductivity thermal interface material as claimed in claim 1, wherein: the coupling agent is one or more of 3- (2,3-glycidoxy) propyl trimethoxy silane, vinyl trimethoxy ethoxy silane and gamma-methacryloxypropyl trimethoxy silane; the catalyst is platinum catalyst.
7. The method of claim 2, wherein the method comprises two steps of:
p1: firstly, the heat conducting filler is respectively subjected to surface modification, and the steps are as follows:
step 1, firstly, respectively putting a certain mass of filler into a vacuum drying oven for drying so as to remove surface moisture and impurities;
step 2, calculating the amount of deionized water and the amount of a modifier required for preparing coupling agent hydrolysate according to the specific surface area of each filler particle and the wettable area of the coupling agent;
step 3, adding deionized water according to the minimum water demand, adding acetic acid to adjust the pH value to acidity, adding coupling agents under continuous oscillation, standing for a period of time until the solution becomes clear to obtain a fully hydrolyzed coupling agent solution, and then adding quantitative absolute ethyl alcohol, wherein the mass ratio of alcohol to water is 95: 5;
step 4, adding the heat-conducting filler respectively, firstly carrying out ultrasonic oscillation for 25-35min, then carrying out water bath heating and magnetic stirring for 25-35min, then placing the mixture into a planetary ball mill for ball milling, and fully bonding inorganic groups of the coupling agent with hydroxyl on the surface of the heat-conducting filler under the high rotating speed and heating state; after the ball milling is finished, the ball milling product is flatly laid on a surface dish and placed in a constant-temperature water bath kettle for drying; finally, placing the mixture in a vacuum drying oven for drying to obtain a mixed filler;
p2: the thermal interface material is prepared by mixing the filler and the matrix, and the steps are as follows:
adding all the fillers into the matrix in batches according to the particle size, placing the fillers into a planetary stirrer for fully stirring, grinding the fillers for a long time until no macroscopic small particles exist, and finally placing the fillers into a vacuum oven for vacuum defoaming to obtain the thermal interface material.
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| 刘永鹤;张岩岩;: "导热氧化铝改性工艺对界面材料导热性能的影响研究", 无机盐工业 * |
| 周文英,寇静利,谷宏智,杜泽强: "导热绝缘聚合物复合材料研究", 上海塑料 * |
| 肖勇;吴孟强;袁颖;庞翔;陈黎;: "无机微/纳米粒子表面包覆改性技术", 电子元件与材料 * |
| 薛茹君;吴玉程;: "硅烷偶联剂表面修饰纳米氧化铝", 应用化学 * |
| 贾春燕;李东红;杨双凤;: "导热填料氧化铝的表面处理研究", 轻金属 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117246027A (en) * | 2023-11-20 | 2023-12-19 | 江苏晶昱宝环境科技有限公司 | High-density composite sound insulation board lamination assembly equipment |
| CN117246027B (en) * | 2023-11-20 | 2024-01-23 | 江苏晶昱宝环境科技有限公司 | High-density composite sound insulation board lamination assembly equipment |
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