CN111925654B - Aluminum nitride and aluminum oxide compounded heat-conducting insulating silica gel material and preparation method thereof - Google Patents
Aluminum nitride and aluminum oxide compounded heat-conducting insulating silica gel material and preparation method thereof Download PDFInfo
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Abstract
The invention provides an aluminum nitride and aluminum oxide compounded heat-conducting insulating silica gel material and a preparation method thereof. An insulating and heat-conducting silica gel material comprises an insulating silica gel matrix and a heat-conducting filler, wherein the heat-conducting filler comprises heat-conducting particles and a surfactant, the heat-conducting particles are a combination of aluminum nitride particles and aluminum oxide particles, the particle size of the aluminum nitride particles is 20-100 mu m, the particle size of the aluminum oxide particles is 1-30 mu m, and the aluminum nitride particles account for 40-60% of the total weight of the heat-conducting particles; preferably, the particle size of the aluminum nitride particles is 30-80 μm and the particle size of the aluminum oxide particles is 1-20 μm. The particles are closely packed, the ratio of aluminum nitride to aluminum oxide is reasonably matched, and after the particles are treated by the surfactant, the high filling of the aluminum oxide and the aluminum nitride can be realized, so that the heat conductivity coefficient of the heat-conducting insulating silica gel gasket can reach more than 15.0W/(m.K).
Description
Technical Field
The invention relates to a silica gel gasket and a preparation method thereof, in particular to an aluminum nitride and aluminum oxide compounded high-thermal-conductivity, insulating and heat-conducting silica gel gasket and a preparation method thereof.
Background
Statistics show that the reliability of the electronic components is reduced by 10% when the temperature of the electronic components is increased by 2 ℃ and the service life of the electronic components is doubled when the temperature is reduced by 8 ℃; therefore, the role of thermal interface materials in the field of information technology is becoming more and more important. How to further improve the thermal conductivity of the thermal interface material and reduce the thermal resistance is still a very important issue for the electronic packaging and heat dissipation engineering.
The common insulating heat-conducting silica gel sheet is prepared by compounding alumina and silica gel, the heat conductivity coefficient is generally not more than 10W/mK, aluminum nitride has high heat conductivity and high insulativity, the theoretical value of a single crystal is 320W/(m.K), and the actual value can still reach 100W/(m.K) -280W/(m.K), which is 5-10 times of that of the alumina; in order to increase the heat conductivity, the existing research also tries to adopt aluminum nitride as a filler to improve the heat conductivity coefficient of the heat conducting gasket, but the high heat conducting requirement cannot be met. At present, the heat-conducting insulating silica gel material with high heat conductivity coefficient is prepared by compounding aluminum nitride and aluminum oxide as a filler. However, the heat conductivity coefficient of the prepared heat-conducting insulating silica gel material is still not high because the combined particle size of the alumina particles and the aluminum nitride particles is not optimized.
Disclosure of Invention
Aiming at the defects of the heat conductivity coefficient of the existing insulating heat-conducting gasket, the invention aims to provide the heat-conducting insulating heat-conducting silica gel gasket and the preparation method thereof, and the proportion of aluminum nitride and aluminum oxide is reasonably compounded, so that the heat conductivity coefficient is improved, and the product has high heat-conducting performance and excellent insulating performance.
One aspect of the present invention provides an insulating and heat conducting silica gel material, which comprises an insulating silica gel matrix and a heat conducting filler, wherein the heat conducting filler comprises heat conducting particles and a surfactant, the heat conducting particles are a combination of aluminum nitride particles and aluminum oxide particles,
wherein the particle size of the aluminum nitride particles is 20-100 μm, the particle size of the aluminum oxide particles is 1-30 μm, and the aluminum nitride particles account for 40% -60% of the total weight of the heat-conducting particles.
In the technical scheme of the invention, the particle size of the aluminum nitride particles is larger than that of the aluminum oxide particles.
In the technical scheme of the invention, the aluminum nitride particles have a single particle size or have more than 2 different particle sizes, preferably, the particle size of large-particle aluminum nitride in the 2 aluminum nitride particles with different particle sizes is more than 2 times, more preferably 2-5 times of that of small-particle aluminum nitride.
In the technical scheme of the invention, in 2 kinds of aluminum nitride particles with different particle sizes, the mass of the large-particle aluminum nitride particles is more than 2 times that of the small-particle aluminum nitride particles, and preferably 2-4 times.
In the technical scheme of the invention, the alumina particles have more than 3 different particle sizes, preferably, the particle size of large alumina particles in the alumina particles with the 3 different particle sizes is more than 2 times, preferably 2-5 times of that of medium alumina particles; the particle diameter of the medium-sized alumina particles is 2 times or more, preferably 2 to 5 times, the particle diameter of the small-sized alumina particles.
In the technical scheme of the invention, preferably, the particle size of the aluminum nitride particles is 30-80 μm, and the particle size of the aluminum oxide particles is 1-20 μm.
In the technical scheme of the invention, the aluminum nitride particles account for 45-55% of the total weight of the heat-conducting particles, and preferably account for 46-50%.
In the technical scheme of the invention, the alumina particles with the particle size of 5-20 μm account for 15-40% of the total weight of the heat-conducting particles.
In the technical scheme of the invention, the particle size is not more than 5 μm, and the alumina particles with the particle size of more than 1 μm account for 12-35% of the total weight of the heat-conducting particles.
The invention also provides a heat-conducting insulating silica gel gasket which is made of the heat-conducting insulating silica gel material.
The invention also provides a preparation method of the insulating and heat-conducting silica gel material, which sequentially comprises the following steps:
1) compounding aluminum nitride particles and aluminum oxide particles, adding a surfactant, heating and mixing to obtain a heat-conducting filler;
2) adding a heat-conducting filler into a mixture of polydimethylsiloxane, hydrogen-containing silicone oil, simethicone and an inhibitor, fully and uniformly stirring, adding a catalyst, and uniformly stirring to obtain the insulating heat-conducting silicone rubber material.
Preferably, the aluminum nitride particles and the aluminum oxide particles are mixed and stirred uniformly in the step 1), then mixed liquid of the surfactant and the ethanol is added, the mixture is stirred until the powder is wetted, the mixture is continuously stirred and heated to 60-90 ℃, the stirring is kept, the temperature is raised to 120-180 ℃, and the low molecules are removed by vacuumizing, so that the heat-conducting filler is obtained;
preferably, the vacuumizing time is 30-60 min, and the stirring speed is 30-50 r/min.
The invention also provides a preparation method of the insulating heat-conducting silica gel gasket, which comprises the following steps:
and (3) carrying out cold press molding on the insulating and heat-conducting silica gel material through a calender, and cooling the insulating and heat-conducting silica gel material after hot air vulcanization to obtain the insulating and heat-conducting silica gel gasket.
Preferably, the hot air vulcanization temperature is 80-150 ℃, and the vulcanization time is 10-20 min.
Advantageous effects
The invention obtains high heat-conducting property by adopting a filler compounding mode, not only utilizes the filler aluminum nitride with high heat-conducting property to compound the filler aluminum nitride with aluminum oxide, but also unexpectedly finds that when the ion particle diameters of the aluminum oxide and the aluminum nitride reach a certain proportion, the heat-conducting effect produced by the filler aluminum nitride is far higher than that produced by a heat-conducting silica gel gasket which singly adopts the aluminum oxide or the aluminum nitride as the filler. Although not wishing to be bound by theory, the present invention may be that it is important to form efficient heat conduction paths because fillers with high thermal conductivity are in contact with each other using a specific compounding ratio; therefore, the heat-conducting gasket prepared by compounding aluminum nitride and aluminum oxide in different mass ratios and particle sizes can form a high-efficiency heat-conducting network, so that the overall heat-conducting coefficient is improved, and can reach more than 8W/(m.K) and even exceed 9W/(m.K).
Compared with the prior art, the high-heat-conductivity insulating heat-conducting silica gel gasket disclosed by the invention constructs an efficient heat-conducting network by compounding aluminum nitride and aluminum oxide in different weight parts and different particle sizes, and finally realizes the improvement of the heat-conducting property of the silica gel gasket. The high-thermal-conductivity insulating heat-conducting silica gel gasket has good insulativity, and the thermal conductivity coefficient of the high-thermal-conductivity insulating heat-conducting silica gel gasket is improved to be more than 8.0W/(m.K), which cannot be achieved by the prior art.
Detailed Description
The invention will be further described with reference to specific embodiments:
one aspect of the present invention provides an insulating and heat conducting silica gel material, which comprises an insulating silica gel matrix and a heat conducting filler, wherein the heat conducting filler comprises heat conducting particles and a surfactant, the heat conducting particles are a combination of aluminum nitride particles and aluminum oxide particles,
wherein the particle size of the aluminum nitride particles is 20-100 μm, the particle size of the aluminum oxide particles is 1-30 μm, and the aluminum nitride particles account for 40% -60% of the total weight of the heat-conducting particles.
In some embodiments of the present invention, the aluminum nitride particles each have a particle size greater than the particle size of the aluminum oxide particles.
In some embodiments of the present invention, the aluminum nitride particles have a single particle size or 2 or more different particle sizes, and preferably, the particle size of the large-particle aluminum nitride is 2 or more times, more preferably 2 to 5 times, larger than that of the small-particle aluminum nitride in the 2 different particle sizes.
In some embodiments of the invention, the mass of the large aluminum nitride particles is more than 2 times, preferably 2 to 4 times, the mass of the small aluminum nitride particles, of the 2 aluminum nitride particles of different particle sizes.
In some embodiments of the present invention, the alumina particles have more than 3 different particle sizes, preferably, the large alumina particle size is more than 2 times, preferably 2 to 5 times, larger than the medium alumina particle size among the 3 different alumina particle sizes; the particle diameter of the medium-sized alumina particles is 2 times or more, preferably 2 to 5 times, the particle diameter of the small-sized alumina particles.
In some preferred embodiments of the invention, the aluminum nitride particles have a particle size of 30-80 μm and the aluminum oxide particles have a particle size of 1-20 μm.
In some embodiments of the invention, the aluminum nitride particles comprise 45% to 55%, preferably 46% to 50%, of the total weight of the thermally conductive particles.
In some embodiments of the invention, the alumina particles having a particle size of 5 to 20 μm comprise 15 to 40% by weight of the total weight of the thermally conductive particles.
In some embodiments of the invention, the particle size is no more than 5 μm, and the alumina particles above 1 μm comprise 12-35% of the total weight of the thermally conductive particles.
In some preferred embodiments of the present invention, the alumina is one or more of spherical alumina, spheroidal alumina and alpha-alumina; more preferably, the alumina is spherical alumina, and the particle size is one or more of 1 μm, 2 μm, 5 μm, 10 μm, 20 μm and 40 μm.
In some preferred embodiments of the invention, the aluminum nitride is one or two of spherical aluminum nitride or granular aluminum nitride, and when the aluminum nitride is compounded with alumina, the whole thermal conductivity of the gasket can be improved by selecting large particle size; therefore, the aluminum nitride is preferably one or two of spherical aluminum nitride or granular aluminum nitride, and the grain diameter of the aluminum nitride is 30 μm, 50 μm, 80 μm and 100 μm.
In some embodiments of the invention, the insulating silica gel matrix is made from polydimethylsiloxane, hydrogen-containing silicone oil, dimethicone, a catalyst, and an inhibitor.
In some embodiments of the invention, the insulating silica gel matrix is prepared by mixing polydimethylsiloxane, hydrogen-containing silicone oil, dimethicone and an inhibitor, then adding a catalyst, and the thermally conductive filler is added to the mixture before the catalyst is added and stirred uniformly.
In some embodiments of the invention, the polydimethylsiloxane is a vinyl terminated polydimethylsiloxane having a viscosity of 50cps to 5000 cps; the inventor researches and discovers that the strength and toughness of a cured crosslinking network can be improved by matching the vinyl-terminated polydimethylsiloxane with high and low viscosity; therefore, the vinyl-terminated polydimethylsiloxane is preferably used in a combination of 50cps to 500cps and 1000cps to 5000cps, and more preferably, the vinyl-terminated polydimethylsiloxane has a molecular weight of 80 cps to 150 cps: 1500-2500cps with the mass ratio of 1.8-2.2: 1.
In some specific embodiments of the invention, the hydrogen-containing silicone oil is one or more of side chain hydrogen-containing silicone oil, terminal hydrogen-containing silicone oil and terminal side hydrogen-containing silicone oil, and the hydrogen content of the hydrogen-containing silicone oil is 0.10-0.20% of the weight of the hydrogen-containing silicone oil; preferably, the hydrogen-containing silicone oil is a side chain hydrogen-containing silicone oil and a terminal hydrogen-containing silicone oil which are compounded for use; more preferably, the side chain hydrogen-containing silicone oil and the terminal hydrogen-containing silicone oil are compounded according to the mass ratio of 1.8-2.2: 1.
In some embodiments of the invention, the dimethicone has a viscosity of 50cps to 500 cps.
In some embodiments of the invention, the catalyst is selected from one of chloroplatinic acid isopropanol solution, platinum complex, Karstedt platinum catalyst, and has a concentration of 1000ppm to 5000 ppm. Wherein the Karstedt platinum catalyst has high-efficiency catalytic activity and anti-poisoning property; thus, preferably, the catalyst is Karstedt platinum catalyst at a concentration of 3000 ppm.
In some embodiments of the present invention, the inhibitor is selected from one or more of ethynl cyclohexanol, methyl butynol, phenyl butynol, vinyl ring, diallyl maleate, diallyl fumarate, and silanized alkynol. Selecting according to the inhibition effect and the curing temperature; preferably, the inhibitor is ethynl cyclohexanol.
In some embodiments of the present invention, the thermally conductive filler is pretreated by mixing and heating thermally conductive particles with a surfactant solution and drying.
In some embodiments of the present invention, the mass ratio of the thermally conductive particles to the surfactant is 800-.
In some embodiments of the present invention, the thermally conductive filler is 80% to 99%, preferably 90% to 99%, and more preferably 92% to 98% of the insulating and thermally conductive silicone material.
In some embodiments of the invention, the surfactant is: one or two of hexamethyldisilazane, octyltrimethoxysilane, decyltrimethoxysilane, dodecyltrimethoxysilane, hexadecyltrimethylsilane, gamma-methacryloxypropyltrimethoxysilane and gamma- (2, 3-glycidoxy) propyltrimethoxysilane are compounded, and the dosage of the hexamethyldisilazane is 1-5% of the total mass of the heat-conducting filler.
In some embodiments of the invention, the mass ratio of polydimethylsiloxane, hydrogen-containing silicone oil, simethicone, inhibitor and catalyst is 100: 5-20: 5-20: 0.1-0.2: 1 to 2, preferably 100:6:10:0.1: 1.5.
The invention also provides a heat-conducting insulating silica gel gasket which is made of the heat-conducting insulating silica gel material.
The invention also provides a preparation method of the insulating and heat-conducting silica gel material, which sequentially comprises the following steps:
1) compounding aluminum nitride particles and aluminum oxide particles, adding a surfactant, heating and mixing to obtain a heat-conducting filler;
2) adding a heat-conducting filler into a mixture of polydimethylsiloxane, hydrogen-containing silicone oil, simethicone and an inhibitor, fully and uniformly stirring, adding a catalyst, and uniformly stirring to obtain the insulating heat-conducting silicone rubber material.
Preferably, the aluminum nitride particles and the aluminum oxide particles are mixed and stirred uniformly in the step 1), then mixed liquid of the surfactant and the ethanol is added, the mixture is stirred until the powder is wetted, the mixture is continuously stirred and heated to 60-90 ℃, the stirring is kept, the temperature is raised to 120-180 ℃, and the low molecules are removed by vacuumizing, so that the heat-conducting filler is obtained;
preferably, the vacuumizing time is 30-60 min, and the stirring speed is 30-50 r/min.
The invention also provides a preparation method of the insulating heat-conducting silica gel gasket, which comprises the following steps:
and (3) carrying out cold press molding on the insulating and heat-conducting silica gel material through a calender, and cooling the insulating and heat-conducting silica gel material after hot air vulcanization to obtain the insulating and heat-conducting silica gel gasket.
Preferably, the hot air vulcanization temperature is 80-150 ℃, and the vulcanization time is 10-20 min.
In a preferred embodiment of the invention, the thermally conductive particles are in the following combination:
or is
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The following are specific examples
Example 1: aluminum nitride and aluminum oxide compounded high-thermal-conductivity insulating and heat-conducting silica gel gasket
The preparation method comprises the following steps:
1) selecting aluminum nitride and aluminum oxide in a compounding way:
compounding the aluminum nitride and the aluminum oxide, mixing and stirring uniformly, adding a mixed solution of 24 parts of a surfactant and 72 parts of ethanol, fully stirring until the mixed solution is wetted, continuously stirring, heating to 80 ℃, keeping stirring for 4 hours, heating to 150 ℃, and removing low molecules in vacuum to obtain 2400 parts of treated mixed powder;
2) 100 parts of vinyl-terminated polydimethylsiloxane (100 cps: 2000cps 2:1), 6 parts of hydrogen-containing silicone oil (side hydrogen: putting hydrogen-terminated (2: 1), 10 parts of 100cps dimethyl silicone oil and 0.1 part of inhibitor (acetylene cyclohexanol) into a kneader or a planetary stirrer, adding 2400 parts of the compound powder obtained in the step 1), fully and uniformly stirring in the kneader or the planetary stirrer, adding a catalyst, uniformly stirring, and performing vacuum defoaming to obtain a base material;
3) adjusting the calendering thickness of a calender to be 1.5mm (film thickness reduction), cold-pressing and molding the base material through the calender, vulcanizing the base material through hot air in an oven, and cooling to obtain the 1.5mm high-thermal-conductivity insulating heat-conducting silica gel gasket.
4) The standard ASTM-5470 is applied, the heat conductivity coefficient of the high heat conductivity silica gel is measured by using LW-9389 heat conductivity tester in Taiwan Ruiki, and the heat conductivity coefficient obtained by data fitting calculation is 8.87W/(m.K).
Example 2: aluminum nitride and aluminum oxide compounded high-thermal-conductivity insulating and heat-conducting silica gel gasket
The preparation method comprises the following steps:
1) selecting aluminum nitride and aluminum oxide in a compounding way:
compounding the aluminum nitride and the aluminum oxide, uniformly mixing and stirring, adding a mixed solution of 26 parts of a surfactant and 78 parts of ethanol, fully stirring until the mixed solution is wetted, continuously stirring, heating to 80 ℃, keeping stirring for 4 hours, heating to 150 ℃, and removing ethanol in vacuum to obtain 2600 parts of treated mixed powder;
2) 100 parts of vinyl-terminated polydimethylsiloxane (100 cps: 2000cps 2:1), 6 parts of hydrogen-containing silicone oil (side hydrogen: putting hydrogen-terminated (2: 1), 10 parts of 100cps dimethyl silicone oil and 0.1 part of inhibitor (acetylene cyclohexanol) into a kneader or a planetary stirrer, adding 2600 parts of the compound powder obtained in the step 1), fully and uniformly stirring in the kneader or the planetary stirrer, adding a catalyst, uniformly stirring, and performing vacuum defoaming to obtain a base material;
3) adjusting the calendering thickness of a calender to be 1.5mm (film thickness reduction), cold-pressing and molding the base material through the calender, vulcanizing the base material through hot air in an oven, and cooling to obtain the 1.5mm high-thermal-conductivity insulating heat-conducting silica gel gasket.
4) The standard ASTM-5470 is applied, the heat conductivity coefficient of the high heat conductivity silica gel is measured by using LW-9389 heat conductivity tester in Taiwan Ruiki, and the heat conductivity coefficient is 9.54W/(m.K) through data fitting calculation.
Example 3: aluminum nitride and aluminum oxide compounded high-thermal-conductivity insulating and heat-conducting silica gel gasket
The preparation method comprises the following steps:
1) selecting aluminum nitride and aluminum oxide in a compounding way:
compounding the aluminum nitride and the aluminum oxide, mixing and stirring uniformly, adding a mixed solution of 25 parts of a surfactant and 75 parts of ethanol, fully stirring until the mixed solution is wetted, continuing stirring, heating to 80 ℃, keeping stirring for 4 hours, heating to 150 ℃, and removing ethanol in vacuum to obtain 2600 parts of treated mixed powder;
2) 100 parts of vinyl-terminated polydimethylsiloxane (100 cps: 2000cps 2:1), 6 parts of hydrogen-containing silicone oil (side hydrogen: putting hydrogen-terminated (2: 1), 10 parts of 100cps dimethyl silicone oil and 0.1 part of inhibitor (ethynl cyclohexanol) into a kneader or a planetary stirrer, adding 2500 parts of the compound powder obtained in the step 1), fully and uniformly stirring in the kneader or the planetary stirrer, adding a catalyst, uniformly stirring, and performing vacuum defoaming to obtain a base material;
3) adjusting the calendering thickness of a calender to be 1.5mm (film thickness reduction), cold-pressing and molding the base material through the calender, vulcanizing the base material through hot air in an oven, and cooling to obtain the 1.5mm high-thermal-conductivity insulating heat-conducting silica gel gasket.
4) The standard ASTM-5470 is applied, the heat conductivity coefficient of the high heat conductivity silica gel is measured by using LW-9389 heat conductivity tester in Taiwan Ruiki, and the heat conductivity coefficient is 9.15W/(m.K) through data fitting calculation.
Example 4: aluminum nitride and aluminum oxide compounded high-thermal-conductivity insulating and heat-conducting silica gel gasket
By adopting the theory of particle compact packing and reasonably compounding the proportion of aluminum nitride and aluminum oxide, the preparation method is as follows:
1) selecting aluminum nitride and aluminum oxide in a compounding way:
compounding the aluminum nitride and the aluminum oxide, mixing and stirring uniformly, adding a mixed solution of 25 parts of a surfactant and 75 parts of ethanol, fully stirring until the mixed solution is wetted, continuing stirring, heating to 80 ℃, keeping stirring for 4 hours, heating to 150 ℃, and removing ethanol in vacuum to obtain 2600 parts of treated mixed powder;
2) 100 parts of vinyl-terminated polydimethylsiloxane (100 cps: 2000cps 2:1), 6 parts of hydrogen-containing silicone oil (side hydrogen: putting hydrogen-terminated (2: 1), 10 parts of 100cps dimethyl silicone oil and 0.1 part of inhibitor (ethynl cyclohexanol) into a kneader or a planetary stirrer, adding 2500 parts of the compound powder obtained in the step 1), fully and uniformly stirring in the kneader or the planetary stirrer, adding a catalyst, uniformly stirring, and performing vacuum defoaming to obtain a base material;
3) adjusting the calendering thickness of a calender to be 1.5mm (film thickness reduction), cold-pressing and molding the base material through the calender, vulcanizing the base material through hot air in an oven, and cooling to obtain the 1.5mm high-thermal-conductivity insulating heat-conducting silica gel gasket.
4) The heat conductivity coefficient of the high-heat-conductivity silica gel is measured by using a standard ASTM-5470 and an LW-9389 heat conductivity tester in Taiwan Ruiki, and the measured data are as follows:
| Thickness | Imp | K | Press |
| mm | (℃x cm2/W) | W/(m x℃) | (Psi) |
| 1.516 | 2.094 | 7.24 | 40.11 |
| 3.012 | 3.793 | 7.94 | 40.00 |
| 4.445 | 5.295 | 8.39 | 40.02 |
the coefficient of thermal conductivity is 15.00W/(m.K) through data fitting calculation.
Example 5
1) And (3) selecting the single spherical alumina in a compounding way:
compounding the aluminum nitride and the aluminum oxide, mixing and stirring uniformly, adding a mixed solution of 24 parts of a surfactant and 72 parts of ethanol, fully stirring until the mixed solution is wetted, continuously stirring, heating to 80 ℃, keeping stirring for 4 hours, heating to 150 ℃, and removing ethanol in vacuum to obtain 2400 parts of treated mixed powder;
2) 100 parts of vinyl-terminated polydimethylsiloxane (100 cps: 2000cps 2:1), 6 parts of hydrogen-containing silicone oil (side hydrogen: putting hydrogen-terminated (2: 1), 10 parts of 100cps dimethyl silicone oil and 0.1 part of inhibitor (acetylene cyclohexanol) into a kneader or a planetary stirrer, adding 2400 parts of the compound powder obtained in the step 1), fully and uniformly stirring in the kneader or the planetary stirrer, adding a catalyst, uniformly stirring, and performing vacuum defoaming to obtain a base material;
3) adjusting the calendering thickness of a calender to be 1.5mm (film thickness reduction), cold-pressing and molding the base material through the calender, vulcanizing the base material through hot air in an oven, and cooling to obtain the 1.5mm high-thermal-conductivity insulating heat-conducting silica gel gasket.
The standard ASTM-5470 is applied, the heat conductivity coefficient of the high heat conductivity silica gel is measured by using LW-9389 heat conductivity tester in Taiwan Ruiki, and the heat conductivity coefficient is 5.89W/(m.K) through data fitting calculation.
Example 6: aluminum nitride and aluminum oxide compounded high-thermal-conductivity insulating and heat-conducting silica gel gasket
The preparation method comprises the following steps:
1) selecting aluminum nitride and aluminum oxide in a compounding way:
compounding the aluminum nitride and the aluminum oxide, mixing and stirring uniformly, adding a mixed solution of 25 parts of a surfactant and 75 parts of ethanol, fully stirring until the mixed solution is wetted, continuing stirring, heating to 80 ℃, keeping stirring for 4 hours, heating to 150 ℃, and removing ethanol in vacuum to obtain 2600 parts of treated mixed powder;
2) 100 parts of vinyl-terminated polydimethylsiloxane (100 cps: 2000cps 2:1), 6 parts of hydrogen-containing silicone oil (side hydrogen: putting hydrogen-terminated (2: 1), 10 parts of 100cps dimethyl silicone oil and 0.1 part of inhibitor (ethynl cyclohexanol) into a kneader or a planetary stirrer, adding 2500 parts of the compound powder obtained in the step 1), fully and uniformly stirring in the kneader or the planetary stirrer, adding a catalyst, uniformly stirring, and performing vacuum defoaming to obtain a base material;
3) adjusting the calendering thickness of a calender to be 1.5mm (film thickness reduction), cold-pressing and molding the base material through the calender, vulcanizing the base material through hot air in an oven, and cooling to obtain the 1.5mm high-thermal-conductivity insulating heat-conducting silica gel gasket.
4) The standard ASTM-5470 is applied, the heat conductivity coefficient of the high heat conductivity silica gel is measured by using LW-9389 heat conductivity tester in Taiwan Ruiki, and the heat conductivity coefficient is 5.98W/(m.K) through data fitting calculation.
Example 7: aluminum nitride and aluminum oxide compounded high-thermal-conductivity insulating and heat-conducting silica gel gasket
The preparation method comprises the following steps:
1) selecting aluminum nitride and aluminum oxide in a compounding way:
compounding the aluminum nitride and the aluminum oxide, mixing and stirring uniformly, adding a mixed solution of 25 parts of a surfactant and 75 parts of ethanol, fully stirring until the mixed solution is wetted, continuing stirring, heating to 80 ℃, keeping stirring for 4 hours, heating to 150 ℃, and removing the ethanol in vacuum to obtain 2500 parts of treated mixed powder;
2) 100 parts of vinyl-terminated polydimethylsiloxane (100 cps: 2000cps 2:1), 6 parts of hydrogen-containing silicone oil (side hydrogen: putting hydrogen-terminated (2: 1), 10 parts of 100cps dimethyl silicone oil and 0.1 part of inhibitor (ethynl cyclohexanol) into a kneader or a planetary stirrer, adding 2500 parts of the compound powder obtained in the step 1), fully and uniformly stirring in the kneader or the planetary stirrer, adding a catalyst, uniformly stirring, and performing vacuum defoaming to obtain a base material;
3) adjusting the calendering thickness of a calender to be 1.5mm (film thickness reduction), cold-pressing and molding the base material through the calender, vulcanizing the base material through hot air in an oven, and cooling to obtain the 1.5mm high-thermal-conductivity insulating heat-conducting silica gel gasket.
4) The standard ASTM-5470 is applied, the heat conductivity coefficient of the high heat conductivity silica gel is measured by using LW-9389 heat conductivity tester in Taiwan Ruiki, and the heat conductivity coefficient is 5.20W/(m.K) through data fitting calculation.
Example 8: aluminum nitride and aluminum oxide compounded high-thermal-conductivity insulating and heat-conducting silica gel gasket
The preparation method comprises the following steps:
1) selecting aluminum nitride and aluminum oxide in a compounding way:
compounding the aluminum nitride and the aluminum oxide, mixing and stirring uniformly, adding a mixed solution of 25 parts of a surfactant and 75 parts of ethanol, fully stirring until the powder is wetted, continuously stirring, heating to 80 ℃, keeping stirring for 4 hours, heating to 150 ℃, and removing the ethanol in vacuum to obtain 2700 parts of treated mixed powder;
2) 100 parts of vinyl-terminated polydimethylsiloxane (100 cps: 2000cps 2:1), 6 parts of hydrogen-containing silicone oil (side hydrogen: putting hydrogen-terminated (2: 1), 10 parts of 100cps dimethyl silicone oil and 0.1 part of inhibitor (ethynl cyclohexanol) into a kneader or a planetary stirrer, adding 2500 parts of the compound powder obtained in the step 1), fully and uniformly stirring in the kneader or the planetary stirrer, adding a catalyst, uniformly stirring, and performing vacuum defoaming to obtain a base material;
3) adjusting the calendering thickness of a calender to be 1.5mm (film thickness reduction), cold-pressing and molding the base material through the calender, vulcanizing the base material through hot air in an oven, and cooling to obtain the 1.5mm high-thermal-conductivity insulating heat-conducting silica gel gasket.
4) The heat conductivity coefficient of the high-heat-conductivity silica gel is measured by using a standard ASTM-5470 and an LW-9389 heat conductivity tester in Taiwan Ruiki, and the measured data are as follows: the coefficient of thermal conductivity is 6.00W/(m.K) through data fitting calculation.
Various other changes and modifications of the parameters and the proportions thereof which are obvious to those skilled in the art can be made in the light of the above teachings, and all such changes and modifications are intended to be within the scope of the appended claims.
Claims (6)
1. An insulating and heat-conducting silica gel material comprises an insulating silica gel matrix and heat-conducting filler, wherein the heat-conducting filler comprises heat-conducting particles and a surfactant, the heat-conducting particles are a combination of aluminum nitride particles and aluminum oxide particles,
wherein the heat conducting particles are
The preparation method comprises the following steps:
1) compounding aluminum nitride particles and aluminum oxide particles, adding a surfactant, heating and mixing to obtain a heat-conducting filler;
2) adding a heat-conducting filler into a mixture of polydimethylsiloxane, hydrogen-containing silicone oil, simethicone and an inhibitor, fully and uniformly stirring, adding a catalyst, and uniformly stirring to obtain an insulating heat-conducting silicone rubber material;
the mass ratio of the heat conducting particles to the surfactant is 800-1200: 1.
2. A heat conductive insulating silicone rubber gasket made of the heat conductive insulating silicone rubber material according to claim 1.
3. The method for preparing the insulating and heat-conducting silica gel material according to claim 1, which comprises the following steps:
1) compounding aluminum nitride particles and aluminum oxide particles, adding a surfactant, heating and mixing to obtain a heat-conducting filler;
2) adding a heat-conducting filler into a mixture of polydimethylsiloxane, hydrogen-containing silicone oil, simethicone and an inhibitor, fully and uniformly stirring, adding a catalyst, and uniformly stirring to obtain the insulating heat-conducting silicone rubber material.
4. The preparation method of claim 3, wherein the aluminum nitride particles and the aluminum oxide particles in the step 1) are compounded by mixing and stirring the aluminum nitride particles and the aluminum oxide particles uniformly, adding a mixed solution of a surfactant and an organic solvent, stirring until the powder is wetted, continuing stirring, heating to 60-90 ℃, keeping stirring, heating to 120-180 ℃, and vacuumizing to remove the organic solvent to obtain the heat-conducting filler.
5. A preparation method of an insulating heat-conducting silica gel gasket comprises the following steps:
the insulating and heat-conducting silica gel material described in claim 1 or obtained by the preparation method described in claim 3 or 4 is subjected to cold press molding by a calender, and is cooled after being vulcanized by hot air to obtain the insulating and heat-conducting silica gel gasket.
6. The preparation method according to claim 5, wherein the hot air vulcanization temperature is 80 ℃ to 150 ℃ and the vulcanization time is 10min to 20 min.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103059576A (en) * | 2012-12-30 | 2013-04-24 | 深圳市鸿富诚屏蔽材料有限公司 | High-heat-conductivity flexible silica gel gasket and preparation method thereof |
| CN103436019A (en) * | 2013-08-23 | 2013-12-11 | 深圳市鸿富诚屏蔽材料有限公司 | High-heat-conductivity electric-insulation heat-conducting silica gel gasket and preparation method thereof |
| JP2017210518A (en) * | 2016-05-24 | 2017-11-30 | 信越化学工業株式会社 | Thermally conductive silicone composition and cured product of the same |
| JP2020090584A (en) * | 2018-12-04 | 2020-06-11 | 信越化学工業株式会社 | Cured article of heat conductive silicone composition |
| WO2020137086A1 (en) * | 2018-12-25 | 2020-07-02 | 富士高分子工業株式会社 | Heat-conductive composition and heat-conductive sheet employing same |
| CN111909522A (en) * | 2020-06-29 | 2020-11-10 | 深圳先进技术研究院 | Heat-conducting insulating material and preparation method thereof |
-
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Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103059576A (en) * | 2012-12-30 | 2013-04-24 | 深圳市鸿富诚屏蔽材料有限公司 | High-heat-conductivity flexible silica gel gasket and preparation method thereof |
| CN103436019A (en) * | 2013-08-23 | 2013-12-11 | 深圳市鸿富诚屏蔽材料有限公司 | High-heat-conductivity electric-insulation heat-conducting silica gel gasket and preparation method thereof |
| JP2017210518A (en) * | 2016-05-24 | 2017-11-30 | 信越化学工業株式会社 | Thermally conductive silicone composition and cured product of the same |
| JP2020090584A (en) * | 2018-12-04 | 2020-06-11 | 信越化学工業株式会社 | Cured article of heat conductive silicone composition |
| WO2020137086A1 (en) * | 2018-12-25 | 2020-07-02 | 富士高分子工業株式会社 | Heat-conductive composition and heat-conductive sheet employing same |
| CN111909522A (en) * | 2020-06-29 | 2020-11-10 | 深圳先进技术研究院 | Heat-conducting insulating material and preparation method thereof |
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