CN112712944B - High-thermal-conductivity insulating gasket and preparation method thereof - Google Patents
High-thermal-conductivity insulating gasket and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a high-thermal-conductivity insulating gasket and a preparation method thereof, wherein the high-thermal-conductivity insulating gasket is composed of an insulator and a functional filler, and the functional filler is carbon fiber coated by alumina; according to the high-thermal-conductivity insulating gasket, the alumina-coated carbon fibers are used as the high-thermal-conductivity filler, so that the high thermal conductivity of the carbon fibers is kept, and the electrical conductivity of the carbon fibers is weakened; and then, the prepared high-thermal-conductivity filler is orderly arranged in the insulator by utilizing a mechanical extrusion orientation technology, so that the thermal-conductivity gasket prepared based on the alumina-coated carbon fiber has high thermal conductivity and high insulativity, and meets the requirements of practical application.
Description
Technical Field
The invention relates to the technical field of high-heat-conduction materials, in particular to a high-heat-conduction insulating gasket and a preparation method thereof.
Background
Conventional hard devices and electronic devices have wide application in fields such as wearable equipment, energy storage, implantation medical treatment and the like. Similar to the high thermal conductivity composite nano material, the preparation of the flexible electronic device is also mostly obtained by compounding the conductive material with the flexible polymer matrix. However, during the repeated deformation of the device, a large amount of heat may be accumulated inside the electronic device due to a large contact resistance between the conductive materials, a poor contact between the conductive materials and the polymer substrate, and the like. If not dissipated from the device in a timely manner, this heat will inevitably affect the performance and lifetime of the device and may even compromise the overall system. That is, for electronic devices, stable thermal properties are also important in addition to excellent mechanical and electrical properties.
At present, people mainly improve the heat-conducting property of the high polymer material from the aspects of a matrix, heat-conducting fillers, a forming process, a heat-conducting theoretical model and the like. The traditional heat conduction materials such as metal, electrodeless materials and the like have good heat conduction performance, but have large brittleness, difficult processing, electric conduction and the like, and the application of the heat conduction materials is greatly limited. Among many polymer materials, silicone rubber has excellent properties such as excellent elasticity, low hardness, weather resistance, insulation, processability and the like, so that silicone rubber composite materials are more and more widely applied and are the most commonly used heat-conducting gasket in the aspect of microelectronic heat dissipation. For example, US4574879, US4602678, US4685987 disclose thermally conductive insulating gaskets whose base structure comprises two thermally conductive silicone rubber layers and an insulating layer located between the two thermally conductive silicone rubber layers. In order to enhance the mechanical and voltage breakdown resistance properties, polyimide films and fiberglass cloth are commonly used as an intermediate mechanical reinforcement layer, for example, in US4602678, US4685987, where release fibers are used as an intermediate insulation layer, and in US4574879, US4685987, where polyamide film layers are used as an intermediate insulation layer. However, since the polyimide film and the glass fiber are poor heat-conducting materials, the heat-conducting insulating gasket prepared by the method has poor heat-conducting effect, and the problems of low heat-conducting coefficient and poor insulating property still exist in the current research on the silicon rubber gasket. Therefore, appropriate thermal management materials and structures are searched, and the thermal management materials and structures are applied to the field of electronic devices, and the mechanism of the thermal management materials and structures is deeply researched, so that the thermal management materials and structures are particularly important for the development of new-generation electronic devices.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a high-thermal-conductivity insulating gasket and a preparation method thereof.
The purpose of the invention is realized by the following technical scheme: the high-thermal-conductivity insulating gasket is composed of an insulator and a functional filler, wherein the functional filler is carbon fiber coated by aluminum oxide.
Further, the alumina is alpha-alumina.
Further, the carbon fiber is a short carbon fiber.
Further, the insulator is silica gel.
A preparation method of an insulating gasket with high thermal conductivity comprises the following steps:
s1, preparing a dispersion liquid: mixing carbon fiber, a dispersing agent and an organic solvent, stirring until the carbon fiber and the dispersing agent are uniformly dispersed, and maintaining for 0.5-1.5h at the temperature of 40-60 ℃; wherein the dispersant is a nonionic surfactant;
s2, coating carbon fibers: mixing an aluminum sol aqueous solution with the solid content of 10-30 wt% with the carbon fiber dispersion liquid prepared in the step S1 for reaction, and drying the mixture to constant weight after the reaction is carried out for 1-2 hours to prepare the alumina-coated carbon fiber material;
s3, high-temperature calcination: calcining the alumina-coated carbon fiber material at high temperature under the protection of argon to prepare a crystalline alumina-coated material; wherein the high temperature is 1100-1200 ℃, and the calcination time is 3-5 h;
s4, mechanical extrusion: uniformly mixing the crystalline alumina coating material and silica gel in a scouring machine, and putting the mixture into a press machine to be extruded and molded at the pressure of 5-10MPa and the extrusion speed of 2-10mm/min to obtain the high-heat-conductivity insulating gasket.
Further, the nonionic surfactant in step S1 is a sorbitan fatty acid ester.
Further, in step S1, the organic solvent is any one of n-hexane, petroleum ether, ethanol, and acetone.
Further, the dry weight ratio of the carbon fiber to the aluminum sol is 100: 1-50.
Further, the temperature of the drying in step S2 is controlled at 60-80 ℃.
Wherein, the Carbon Fiber (CF) is a Fiber material of high-strength and high-modulus Fiber with the diameter of 5-10 μm and the Carbon content of more than 90 percent. In the invention, the Carbon Fiber is preferably short Carbon Fiber (Chopped Carbon Fiber), which is prepared by processing Carbon Fiber with high strength and high heat conductivity into a beam by selecting a bundling agent according to requirements and then cutting the beam according to a specified length, and has good heat conductivity.
Among them, the alumina-coated carbon fiber material is preferably alpha-alumina-coated carbon fiber (CF @ Al)2O3) A material; the alpha-alumina is a crystalline inorganic substance, has low interface compatibility with an insulator, is weak in wettability, does not adsorb organic substances, and is favorable for ordered arrangement of the high-thermal-conductivity filler in the insulator;
wherein the volume of the dispersant used for dispersing 10-20g of carbon fiber is 1-3mL, and the volume of the organic solvent is 100-200 mL.
The invention has the following advantages:
(1) according to the high-thermal-conductivity insulating gasket, the crystalline alumina coated carbon fiber is used as the high-thermal-conductivity filler, so that the high thermal conductivity of the carbon fiber is kept, and the electrical conductivity of the carbon fiber is weakened; then, the prepared high-thermal-conductivity filler is orderly arranged in the insulator by utilizing a mechanical extrusion orientation technology, so that the thermal-conductivity gasket prepared based on the alumina-coated carbon fiber obtains high thermal conductivity and high insulativity, and meets the requirements of practical application;
(2) according to the preparation method of the high-thermal-conductivity insulating gasket, the alumina sol is coated on the surface of the carbon fiber through interface adsorption to form the insulating layer, the carbon fiber is converted into the crystalline alumina coated carbon fiber through high-temperature calcination under the protection of inert gas, so that the interface compatibility with an insulator is reduced, the wettability of the alumina coated carbon fiber and the insulator is further reduced, the ordered arrangement of high-thermal-conductivity filler in the insulator is facilitated, and the thermal-conductivity gasket prepared from the alumina coated carbon fiber has high thermal conductivity and insulating property, overcomes the defect of electric conductivity of the high-thermal-conductivity gasket, and meets the requirements of practical application.
Drawings
FIG. 1 shows CF @ Al prepared by the method of the present invention2O3And an X-ray diffraction pattern of CF;
FIG. 2 shows CF @ Al prepared by the method of the present invention2O3Thermogravimetric analysis of (a);
FIG. 3 shows CF @ Al prepared by the method of the present invention2O3And scanning electron microscope images of the cross section of the heat conducting gasket.
Detailed Description
The invention is further described with reference to the following figures and examples, without limiting the scope of the invention to the following:
example 1: the high-thermal-conductivity insulating gasket is composed of an insulator and a functional filler, wherein the functional filler is carbon fiber coated by aluminum oxide, the aluminum oxide is alpha-aluminum oxide, the carbon fiber is short carbon fiber, and the insulator is silica gel.
Example 2: a preparation method of an insulating gasket with high thermal conductivity comprises the following steps:
s1, preparing a dispersion liquid: mixing 10g of short carbon fiber and 1mL of dispersant with 100mL of n-hexane, stirring until the mixture is uniformly dispersed, and maintaining the mixture at the temperature of 40 ℃ for 0.5 h; wherein the dispersant is a sorbitan fatty acid ester;
s2, coating carbon fibers: 5g of an aluminum sol aqueous solution with the solid content of 10 wt% is mixed with the carbon fiber dispersion liquid prepared in the step S1 for reaction, the mixture is dried at 60 ℃ to constant weight after 1 hour of reaction, and the alumina-coated carbon fiber material is prepared, as shown in figure 1, as can be seen in the X-ray diffraction diagram, Al of the coating layer2O3Is alpha-type crystal, after being coated, CF @ Al2O3Still contains the original crystal structure of CF; for CF @ Al2O3A thermogravimetric analysis chart obtained by performing thermogravimetric analysis under a nitrogen atmosphere is shown in fig. 2, and it can be seen from the thermogravimetric analysis chart that the content of the clad layer is 3.97 wt%;
s3, high-temperature calcination: calcining the alumina-coated carbon fiber material at high temperature under the protection of argon to prepare a crystalline alumina-coated material; wherein the high temperature is 1100 ℃, and the calcining time is 3 h;
s4, mechanical extrusion: uniformly mixing the crystalline alumina coating material and silica gel in a scouring machine, placing the mixture in a press machine, extruding and molding at the extrusion speed of 2mm/min and the pressure of 5MPa to obtain the high-heat-conductivity insulating gasket, wherein the microstructure diagram of the section of the high-heat-conductivity insulating gasket is shown in figure 3, and CF @ Al can be seen from the microstructure diagram2O3Vertically aligned in silica gel.
Example 3: a preparation method of an insulating gasket with high thermal conductivity comprises the following steps:
s1, preparing a dispersion liquid: mixing 20g of short carbon fiber and 3mL of dispersant with 200mL of petroleum ether, stirring until the mixture is uniformly dispersed, and maintaining the mixture at the temperature of 60 ℃ for 1.5 hours; wherein the dispersant is a sorbitan fatty acid ester;
s2, coating carbon fibers: mixing 0.2g of an aluminum sol aqueous solution with a solid content of 30 wt% with the carbon fiber dispersion prepared in the step S1 for reaction, drying at 80 ℃ to constant weight after 2 hours of reaction, and obtaining the alumina-coated carbon fiber material, wherein as shown in figure 1, the X-ray diffraction pattern shows that Al of a coating layer2O3Is alpha-type crystal, after being coated, CF @ Al2O3Still contains the original crystal structure of CF; for CF @ Al2O3A thermogravimetric analysis chart obtained by performing thermogravimetric analysis under a nitrogen atmosphere is shown in fig. 2, and it can be seen from the thermogravimetric analysis chart that the content of the clad layer is 3.97 wt%;
s3, high-temperature calcination: calcining the alumina-coated carbon fiber material at high temperature under the protection of argon to prepare a crystalline alumina-coated material; wherein the high temperature is 1200 ℃, and the calcining time is 5 h;
s4, mechanical extrusion: uniformly mixing the crystalline alumina coating material and silica gel in a scouring machine, placing the mixture in a press machine, extruding and molding at the pressure of 10MPa and the extrusion speed of 10mm/min to obtain the high-heat-conductivity insulating gasket, wherein the microstructure diagram of the section of the high-heat-conductivity insulating gasket is shown in figure 3, and CF @ Al can be seen from the microstructure diagram2O3Vertically aligned in silica gel.
Example 4: a preparation method of an insulating gasket with high thermal conductivity comprises the following steps:
s1, preparing a dispersion liquid: mixing 10g of short carbon fiber and 2mL of dispersant with 120mL of ethanol, stirring until the mixture is uniformly dispersed, and maintaining the mixture at the temperature of 50 ℃ for 1 h; wherein the dispersant is a sorbitan fatty acid ester;
s2, coating carbon fibers: mixing 2.5g of an aluminum sol aqueous solution with a solid content of 15 wt% with the carbon fiber dispersion prepared in the step S1 for reaction, drying at 70 ℃ to constant weight after the reaction for 1.5h to obtain the alumina-coated carbon fiber material, wherein as shown in figure 1, the X-ray diffraction pattern shows that the coating layer Al is coated on the alumina-coated carbon fiber material2O3Is alpha-type crystal, after being coated, CF @ Al2O3Still contains the original crystal structure of CF; for CF @ Al2O3A thermogravimetric analysis chart obtained by performing thermogravimetric analysis under a nitrogen atmosphere is shown in fig. 2, and it can be seen from the thermogravimetric analysis chart that the content of the clad layer is 3.97 wt%;
s3, high-temperature calcination: calcining the alumina-coated carbon fiber material at high temperature under the protection of argon to prepare a crystalline alumina-coated material; wherein the high temperature is 1150 ℃, and the calcining time is 4 hours;
s4, mechanical extrusion: uniformly mixing the crystalline alumina coating material and silica gel in a scouring machine, placing the mixture in a press machine, extruding and molding at the pressure of 7MPa and the extrusion speed of 5mm/min to obtain the high-heat-conductivity insulating gasket, wherein the microstructure diagram of the section of the high-heat-conductivity insulating gasket is shown in figure 3, and CF @ Al can be seen from the microstructure diagram2O3Vertically aligned in silica gel.
Example 5: a preparation method of an insulating gasket with high thermal conductivity comprises the following steps:
s1, preparing a dispersion liquid: mixing 10g of short carbon fiber, 2.5mL of dispersing agent and 180mL of acetone, stirring until the mixture is uniformly dispersed, and maintaining the mixture at the temperature of 45 ℃ for 1.5 hours; wherein the dispersant is a sorbitan fatty acid ester;
s2, coating carbon fibers: mixing 4g of an aluminum sol aqueous solution with a solid content of 25 wt% and the carbon fiber dispersion prepared in the step S1 for reaction, drying the mixture at 65 ℃ after the reaction for 1 hour until the weight is constant to prepare the alumina-coated carbon fiber material,as shown in FIG. 1, it can be seen from the X-ray diffraction pattern that the clad layer Al2O3Is alpha-type crystal, after being coated, CF @ Al2O3Still contains the original crystal structure of CF; for CF @ Al2O3A thermogravimetric analysis chart obtained by performing thermogravimetric analysis under a nitrogen atmosphere is shown in fig. 2, and it can be seen from the thermogravimetric analysis chart that the content of the clad layer is 3.97 wt%;
s3, high-temperature calcination: calcining the alumina-coated carbon fiber material at high temperature under the protection of argon to prepare a crystalline alumina-coated material; wherein the high temperature is 1180 ℃, and the calcination time is 4.5 h;
s4, mechanical extrusion: uniformly mixing the crystalline alumina coating material and silica gel in a scouring machine, placing the mixture in a press machine, extruding and molding at the pressure of 8MPa and the extrusion speed of 7mm/min to obtain the high-heat-conductivity insulating gasket, wherein the microstructure diagram of the section of the high-heat-conductivity insulating gasket is shown in figure 3, and CF @ Al can be seen from the microstructure diagram2O3Vertically aligned in silica gel.
For CF @ Al prepared in examples 2-4 above2O3Powder resistance tests and performance tests were performed, and the experimental results are shown in tables 1 and 2.
Table 1: CF @ Al2O3And powder resistance value of CF
| Serial number | Sample name | Al2O3Content (wt.) | Resistance value |
| 1 | CF | Is free of | 0.5Ω |
| 2 | CF@Al2O3 2 | 3.97 | 26.85 |
| 3 | CF@Al2O3 3 | 9.82 | 57.79MΩ |
| 4 | CF@Al2O3 4 | 15.00 | 106.35MΩ |
It can be seen from Table 1 that CF @ Al is increased with the thickness of the clad layer2O3The powder resistance value of (a) increases.
Table 2: CF @ Al2O3And performance of heat-conducting gasket of CF
From table 2, it can be seen that: at the same CF content, CF @ Al2O3The heat conductivity coefficient of the heat-conducting gasket is lower than that of the CF heat-conducting gasket, but the heat conductivity coefficient of the heat-conducting gasket is more than 10W/mK; the volume resistivity and the voltage breakdown resistance are from zero to zero, and high heat conduction and high insulation are realized.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art can substitute or change the technical solution of the present invention and the inventive concept within the technical scope of the present invention.
Claims (7)
1. The high-thermal-conductivity insulating gasket is characterized by comprising an insulator and a functional filler, wherein the functional filler is carbon fiber coated by alumina; then, the prepared high-thermal-conductivity filler is orderly arranged in the insulator by utilizing a mechanical extrusion orientation technology, so that the thermal-conductivity gasket prepared based on the alumina-coated carbon fiber obtains high thermal conductivity and high insulativity;
wherein, the alumina is alpha-alumina; the carbon fiber is short carbon fiber.
2. The gasket of claim 1 wherein said insulation is silicone.
3. The method for preparing an insulating gasket with high thermal conductivity according to claim 1, characterized in that it comprises the following steps:
s1. preparation of dispersion: mixing carbon fiber, a dispersing agent and an organic solvent, stirring until the carbon fiber and the dispersing agent are uniformly dispersed, and maintaining for 0.5-1.5h at the temperature of 40-60 ℃; wherein the dispersant is a nonionic surfactant;
s2, coating carbon fiber: mixing an aluminum sol aqueous solution with the solid content of 10-30 wt% with the carbon fiber dispersion liquid prepared in the step S1 for reaction, and drying the mixture to constant weight after the reaction is carried out for 1-2 hours to prepare the alumina-coated carbon fiber material;
s3, high-temperature calcination: calcining the alumina-coated carbon fiber material at high temperature under the protection of argon to prepare a crystalline alumina-coated material; wherein the high temperature is 1100-1200 ℃, and the calcination time is 3-5 h;
s4, mechanical extrusion: uniformly mixing the crystalline alumina coating material and silica gel in a scouring machine, and putting the mixture into a press machine to be extruded and molded at the pressure of 5-10MPa and the extrusion speed of 2-10mm/min to obtain the high-heat-conductivity insulating gasket.
4. The method as claimed in claim 3, wherein the non-ionic surfactant in step S1 is sorbitan fatty acid ester.
5. The method as claimed in claim 3, wherein the organic solvent in step S1 is any one of n-hexane, petroleum ether, ethanol and acetone.
6. The method for preparing an insulating gasket with high thermal conductivity according to claim 3, wherein the dry weight ratio of the carbon fibers to the aluminum sol is 100: 1-50.
7. The method for preparing an insulating gasket with high thermal conductivity according to claim 3, wherein the drying temperature in step S2 is controlled to be 60-80 ℃.
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| CN116239367B (en) * | 2022-12-28 | 2024-01-09 | 湖南聚能陶瓷材料有限公司 | High-heat-conductivity aluminum oxide ceramic material and ceramic circuit substrate |
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