CN114410113B - Flowing type fine heat-conducting silicone grease and preparation method thereof - Google Patents
Flowing type fine heat-conducting silicone grease and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a flowing type fine heat-conducting silicone grease and a preparation method thereof, wherein the heat-conducting silicone grease comprises the following components in parts by weight: 100 parts of silicone oil, 800-2800 parts of heat conducting filler, 2-20 parts of silane coupling agent, 2-20 parts of dialkyl hypophosphorous acid and 0.1-5 parts of antioxidant. The preparation method comprises the following steps: uniformly mixing the heat conducting filler and the silane coupling agent in a high-speed mixer, and then adding dialkyl hypophosphorous acid for continuous mixing to obtain heat conducting powder with double-layer coating on the surface; and mixing the modified heat conducting powder with silicone oil and an antioxidant at a high speed to obtain the flowing type fine heat conducting silicone grease. The invention adopts different kinds of modifiers to carry out surface modification on the powder by a two-step method, not only improves the compatibility of the filler and the silicone oil, but also improves the wetting effect of the powder surface and solves the silicone grease thixotropic phenomenon caused by high filling of fine particle size powder. The prepared heat-conducting silicone grease has good knife coating property, low viscosity, good flowing property and good aging resistance.
Description
Technical Field
The invention relates to the technical field of heat-conducting silicone grease, in particular to flowing type fine heat-conducting silicone grease with good blade coating property and low viscosity and a preparation method thereof.
Background
With the development of integration and densification of electronic components, heat generated during operation of the electronic components is higher and higher, and particularly in the field of 5G communication electronics, the use of high-power chips has raised higher requirements on heat dissipation performance. The traditional solution is to install a radiator or a radiating fin above the components to achieve the purpose of reducing the temperature, but because the radiating component cannot realize good and tight interface contact with the components, the contact thermal resistance between the radiating component and the components is increased, so that the radiating effect is affected. Therefore, the surface of the component needs to be coated with a layer of heat-conducting silicone grease or a heat-conducting gasket or a heat-conducting phase-change material and other thermal interface materials are added between the component and the radiator, so that heat can be promoted to be transferred to the outside more, and the stable operation of the component is ensured. Compared with the heat-conducting gasket and the heat-conducting phase-change material, the heat-conducting silicone grease has good wettability, convenient construction and easy cleaning in later period, can be used for a long time at the working temperature of-50 ℃ to 250 ℃ and keeps the grease state, has good adaptability to different thermal interfaces, and becomes an ideal choice of the interface heat-conducting material.
Because the heat conductivity of traditional heat conduction silicone grease is not high, the heat dissipation performance is insufficient to meet the heat dissipation requirements of higher power and more complex environments, and therefore, the heat conduction performance of the silicone grease is often improved by adding heat conduction filler. For example, chinese patent CN109438987 a discloses a high thermal conductivity silicone grease and a method for preparing the same. By adopting the surface modifier to carry out surface modification on more than two kinds of powder with different particle diameters, the bulk density of the heat conducting filler is improved, the compatibility between the powder and the silicone oil is also improved, and the prepared heat conducting silicone grease has heat conductivity coefficient as high as more than 5 w/m.k and good insulativity. Chinese patent CN111777995a discloses an insulating high thermal conductivity silicone grease, which is capable of effectively reducing thermal contact resistance between fillers by compounding liquid metal thermal conductive paste and ceramic fillers, and maintaining good insulating property of the thermal conductivity silicone grease while obtaining high-efficiency thermal conductivity (thermal conductivity coefficient exceeding 10w/m·k).
Although the heat conductivity of the silicone grease can be remarkably improved by the method, most of the obtained silicone grease is a touch-type paste, has high viscosity and poor leveling property, and cannot meet the construction requirements in certain occasions including screen printing. Chinese patent 107603224A discloses a heat-conducting silicone grease composition with high heat conductivity and low viscosity, wherein a multi-dimensional filler and a multi-dimensional filler are compounded and then filled into silicone oil, and the prepared heat-conducting silicone grease has good flowing property, but metal aluminum powder or silver powder can influence the ageing resistance of the silicone grease and reduce the insulating property of the silicone grease. The Chinese patent 109486192A is compounded by using heat conducting fillers with different types and different particle sizes, the heat conductivity coefficient of the silicone grease can be improved to 3.75 w/m.k, the viscosity is as low as 68000 mPa.s, but the median diameter of the used filler reaches 50 mu m, and the maximum particle diameter exceeds 200 mu m, which is not beneficial to the blade coating performance and the anti-sedimentation stability performance of the silicone grease in the storage process. In order to meet the requirement that the heat conduction silicone grease can fully contact the interface surface under the condition of lower pressure, the fine silicone grease prepared from the fine particle size powder is more favorable for filling the gap of the contact interface, but the fine particle size powder is easy to cause silicone grease thixotropic during high filling, so that the preparation of the flowing fine heat conduction silicone grease with good fluidity and scratch coating property has very important significance.
Disclosure of Invention
The invention aims to solve the problems in the prior art and provides a silicone grease with high heat conductivity and both flowing property and blade coating property and a preparation method thereof. The silane coupling agent and the dialkyl hypophosphorous acid are adopted to carry out surface organic treatment on the fine-particle-size heat-conducting filler by a two-step method, so that the compatibility between powder and a silicone oil system can be effectively improved, the maximum filling amount of the powder in matrix resin is increased, the problems of thixotropic and high viscosity caused by high filling of the fine-particle-size powder are avoided, the storage stability period of the modified powder is long, and the silicone grease has good flowing property, high heat conductivity and good scratch coating property.
The invention provides a flowing type fine heat-conducting silicone grease which is characterized by comprising the following components in parts by weight: 100 parts of silicone oil, 800-2800 parts of heat conducting powder, 2-20 parts of silane coupling agent, 2-20 parts of dialkyl hypophosphorous acid and 0.1-5 parts of antioxidant.
The preparation method of the flowing type fine heat-conducting silicone grease comprises the following steps: adding a heat conducting filler and a silane coupling agent into a high-speed mixer, mixing at a high speed for 2-30min at a rotating speed of 500-5000 rpm/min to uniformly mix the heat conducting filler and the silane coupling agent, then adding dialkyl hypophosphorous acid, and continuing to mix at a high speed to obtain heat conducting powder with double-layer cladding on the surface; and then adding the obtained heat conducting filler, silicone oil and antioxidant into a planetary stirrer, and mixing for 1-3 hours at the temperature of 50-150 ℃ and the rotating speed of 100-2000rpm/min to obtain the flowing type fine heat conducting silicone grease.
It should be noted that the modification process of the two-step method, that is, the surface modification of the filler by using the long-chain alkyl silane coupling agent and then the secondary coating by using the dialkylhypophosphorous acid, is a necessary condition for achieving the above purpose, and the modification of the modification step will affect the final effect. Firstly, adopting a silane coupling agent to coat the surface of the filler to ensure that the surface of the powder adsorbs grafted long-chain silane molecules, thereby improving the compatibility of the powder and silicone oil resin and enabling the filler to realize the maximum filling amount in the silicone oil resin as far as possible; if the filler is coated with the dialkyl hypophosphorous acid, too many small molecular substances are soaked or adsorbed on the surface of the powder, so that grafting of a long-chain silane coupling agent is not facilitated, the compatibility of the powder and silicone resin is reduced, and the viscosity of the silicone resin is improved.
The silane coupling agent is a long-chain alkyl polyfunctional silane coupling agent and comprises one of dodecyl trimethoxy silane, dodecyl triethoxy silane, dodecyl methyl dimethoxy silane, hexadecyl trimethoxy silane and octadecyl trimethoxy silane. The macromolecular chain of the long-chain alkyl silane coupling agent can form tight molecular chain winding with silicone oil molecules, and after the macromolecular chain is adsorbed on the surface of the powder, the oil absorption value of the modified powder can be effectively reduced, the compatibility between the powder and matrix resin is improved, and the maximum filling part of the powder in the silicone oil resin is increased.
The dialkyl hypophosphorous acid is short-chain alkyl substituted hypophosphorous acid, and comprises one of diethyl hypophosphorous acid, dipropyl hypophosphorous acid, diisobutyl hypophosphorous acid, 1-ethyl-2-propyl hypophosphorous acid and dibutyl hypophosphorous acid. The dialkyl hypophosphorous acid has excellent infiltration effect on the surface of the powder due to the lower molecular weight and the shorter molecular chain length, and overcomes the defect of poor infiltration of the long-chain silane coupling agent, so that a denser coating layer is formed on the surface of the powder, the interaction force among the powder, especially among the fine-particle-size powder, is reduced, the bulk density of the powder in the resin is effectively improved, the problems of poor additivity and the like of the modified powder in the long-term placing process are avoided, and the obtained heat-conducting silicone grease is lower in viscosity and better in fluidity.
The heat conducting powder is one or more than two of aluminum oxide, zinc oxide, magnesium oxide, boron nitride, silicon nitride, aluminum nitride, silicon micro powder, aluminum hydroxide, magnesium hydroxide, aluminum powder and copper powder, and is preferably one or more than two of aluminum oxide, zinc oxide and aluminum powder.
Preferably, the alumina is spherical alumina with a compound particle size, the median diameter is 1-20 mu m, and the maximum particle size is less than 40 mu m; the zinc oxide is irregularly shaped, the median diameter is 0.5-1.5 mu m, and the maximum particle diameter is less than 20 mu m; the aluminum powder is irregularly shaped, the median diameter is 1-20 mu m, and the maximum particle diameter is less than 40 mu m; the maximum particle size of the powder can be achieved by particle size classification techniques.
The silicone oil is one or more than two of methyl-terminated polydimethylsiloxane, methyl-terminated polymethylphenylsiloxane, vinyl-terminated polydimethylsiloxane and vinyl-terminated polymethylphenylsiloxane, and the viscosity of the silicone oil is 30-5000 mPas, preferably 50-1000 mPas. When the viscosity is lower than 50 mPas, the molecular weight of the silicone oil is too low, the prepared heat conduction silicone grease is easy to cause the problem of oil bleeding on the surface after being placed for a long time, when the viscosity is higher than 1000 mPas, the viscosity of the heat conduction silicone grease is higher, the heat conduction silicone grease is difficult to disperse well in the processing process, and meanwhile, the blade coating property of the silicone grease is also poor, so that the operation convenience of the construction process is affected.
The antioxidant is one of antioxidant 1010, antioxidant 1076, antioxidant 168 and antioxidant 1135.
Compared with the prior art, the invention has the beneficial effects that:
the method comprises the steps of adopting a long-chain silane coupling agent and dialkyl hypophosphorous acid as surface modifiers to carry out surface modification on a heat-conducting filler by a two-step method, wherein the long-chain alkyl silane coupling agent can improve the compatibility between powder and resin, the maximum filling amount of the powder in the resin is increased, the dialkyl hypophosphorous acid improves the coating effect of the surface of the powder, and the high viscosity and thixotropy caused by high filling of the powder and large proportion of fine particle size are avoided.
The heat-conducting filler compounded by the powder with the plurality of fine particle sizes can improve the blade coating property of the silicone grease and improve the operation convenience of construction.
Detailed Description
For the purpose of better illustrating the invention, technical solutions and advantages, the invention will be further described with reference to specific examples. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
The sources of the raw materials used in the examples and comparative examples are described below:
methyl phenyl silicone oil: wake chemistry (China); alumina powder: shanghai hundred graphic high New Material stock Co., ltd; zinc oxide powder: shijia Baisheng chemical industry Limited liability company; dodecyl trimethoxy silane: nanjing full-chemical industry Co., ltd; hexadecyltrimethoxysilane: nanjing full-chemical industry Co., ltd; octadecyltrimethoxysilane: nanjing full-chemical industry Co., ltd; diethyl phosphinic acid: self-making; dipropyl hypophosphorous acid: self-making; antioxidant 1010: changzhou friendly chemical Co., ltd;
the test methods used in the examples and comparative examples are described below:
viscosity: the viscosity of the heat conductive silicone grease was measured using a Bowler-Nordheim viscometer with a T91 spindle at 12rpm.
Blade coatability: the maximum thickness of the silicone grease is tested by adopting a scraper fineness gauge, 3 g of silicone grease is weighed at the maximum scale position of the scraper fineness gauge, the scraper is rapidly pulled to the minimum scale position from the maximum scale position by the double hand-held scraper, and the position where particles gather or scratches appear is immediately observed, namely the maximum granularity of the silicone grease. The maximum particle size of the silicone grease can reflect the difficulty of the silicone grease in the blade coating process, and the larger the particle size is, the larger the resistance of the silicone grease in the blade coating process is, and the worse the blade coating property is.
Thermal conductivity coefficient: the sample is tested by adopting a DRL-III heat conductivity coefficient tester of Xiangtan instrument limited company, and the diameter of the sample is 3cm and the thickness is 2mm.
Example 1
The flowing type fine heat-conducting silicone grease comprises the following components in parts by weight: 100 parts of methylphenyl silicone oil with the viscosity of 350 mPas, 400 parts of spherical alumina with the median diameter of 5 mu m, 300 parts of zinc oxide with the median diameter of 0.9 mu m, 2 parts of dodecyl trimethoxy silane, 2 parts of diethyl hypophosphorous acid and 1 part of antioxidant.
The preparation method of the fine and smooth flowing type heat conduction silicone grease comprises the following two steps:
adding spherical aluminum oxide, zinc oxide and dodecyl trimethoxy silane into a high-speed mixer according to the proportion, mixing at a high speed for 3 minutes at a rotating speed of 3000rpm, then adding diethyl hypophosphorous acid according to the proportion, and continuing mixing at a high speed for 3 minutes to obtain heat conduction powder with double layers coated on the surface;
and (3) adding the prepared heat-conducting powder, methyl phenyl silicone oil and an antioxidant into a planetary disperser according to the proportion, wherein the rotating speed is 500rpm, starting vacuumizing, heating to 80 ℃, and mixing for 2 hours to obtain the flowing type fine heat-conducting silicone grease.
Comparative example 1
The heat-conducting silicone grease of the comparative example comprises the following components in parts by weight: 100 parts of methylphenyl silicone oil with the viscosity of 350 mPas, 400 parts of spherical alumina with the median diameter of 5 mu m, 300 parts of zinc oxide with the median diameter of 0.9 mu m, 4 parts of dodecyl trimethoxy silane and 1 part of antioxidant.
The preparation method of the comparative example comprises the following two steps:
adding spherical aluminum oxide, zinc oxide and dodecyl trimethoxy silane into a high-speed mixer according to the proportion, and mixing at a high speed for 6 minutes at a rotating speed of 3000rpm to obtain surface-coated heat conducting powder;
and (3) adding the prepared heat conducting powder, methyl phenyl silicone oil and an antioxidant into a planetary dispersing machine according to the proportion, wherein the rotating speed is 500rpm, starting vacuumizing, heating to 80 ℃, and mixing for 2 hours to obtain the heat conducting silicone grease.
Example 2
The flowing type fine heat-conducting silicone grease comprises the following components in parts by weight: 100 parts of methylphenyl silicone oil with the viscosity of 350 mPas, 700 parts of spherical alumina with the median diameter of 5 mu m, 400 parts of zinc oxide with the median diameter of 0.9 mu m, 3 parts of dodecyl trimethoxy silane, 3 parts of dipropyl hypophosphorous acid and 1 part of antioxidant.
The preparation method of the fine and smooth flowing type heat conduction silicone grease comprises the following two steps:
adding spherical aluminum oxide, zinc oxide and dodecyl trimethoxy silane into a high-speed mixer according to the proportion, mixing at a high speed for 3 minutes at a rotating speed of 3000rpm, then adding dipropyl hypophosphorous acid according to the proportion, and continuing mixing at a high speed for 3 minutes to obtain heat conduction powder with double layers coated on the surface;
and (3) adding the prepared heat-conducting powder, methyl phenyl silicone oil and an antioxidant into a planetary disperser according to the proportion, wherein the rotating speed is 500rpm, starting vacuumizing, heating to 80 ℃, and mixing for 2 hours to obtain the flowing type fine heat-conducting silicone grease.
Comparative example 2
The heat-conducting silicone grease of the comparative example comprises the following components in parts by weight: 100 parts of methylphenyl silicone oil with the viscosity of 350 mPas, 700 parts of spherical alumina with the median diameter of 5 mu m, 400 parts of zinc oxide with the median diameter of 0.9 mu m, 6 parts of dipropyl hypophosphorous acid and 1 part of antioxidant.
The preparation method of the comparative example comprises the following two steps:
adding spherical aluminum oxide, zinc oxide and dipropyl hypophosphorous acid into a high-speed mixer according to the proportion, and mixing at a high speed for 6 minutes at a rotating speed of 3000rpm to obtain surface-coated heat conducting powder;
and (3) adding the prepared heat conducting powder, methyl phenyl silicone oil and an antioxidant into a planetary dispersing machine according to the proportion, wherein the rotating speed is 500rpm, starting vacuumizing, heating to 80 ℃, and mixing for 2 hours to obtain the heat conducting silicone grease.
Example 3
The fine and smooth flowing type heat conduction silicone grease comprises the following components in parts by weight: 100 parts of methylphenyl silicone oil with the viscosity of 200 mPas, 700 parts of spherical alumina with the median diameter of 10 mu m, 270 parts of spherical alumina with the median diameter of 5 mu m, 500 parts of zinc oxide with the median diameter of 0.9 mu m, 4 parts of hexadecyl trimethoxy silane, 4 parts of diethyl hypophosphorous acid and 1 part of antioxidant.
The preparation method of the fine and smooth flowing type heat conduction silicone grease comprises the following two steps:
adding spherical aluminum oxide, zinc oxide and hexadecyl trimethoxy silane into a high-speed mixer according to the proportion, mixing at a high speed for 5 minutes at a rotating speed of 4000rpm, then adding diethyl hypophosphorous acid according to the proportion, and continuing mixing at a high speed for 2 minutes to obtain heat conduction powder with double layers coated on the surface;
and (3) adding the prepared heat-conducting powder, the methylphenyl silicone oil and the antioxidant into the planetary dispersing machine according to the proportion, wherein the rotating speed is 300rpm, starting vacuumizing, heating to 100 ℃, and mixing for 2 hours to obtain the flowing type fine heat-conducting silicone grease.
Comparative example 3
The heat-conducting silicone grease of the comparative example comprises the following components in parts by weight: 100 parts of methylphenyl silicone oil with the viscosity of 200 mPas, 700 parts of spherical alumina with the median diameter of 10 mu m, 270 parts of spherical alumina with the median diameter of 5 mu m, 500 parts of zinc oxide with the median diameter of 0.9 mu m, 4 parts of hexadecyl trimethoxy silane, 4 parts of diethyl hypophosphorous acid and 1 part of antioxidant.
The preparation method of the heat-conducting silicone grease comprises the following two steps:
adding spherical aluminum oxide, zinc oxide and diethyl hypophosphorous acid into a high-speed mixer according to the proportion, and mixing at a high speed for 7 minutes at a rotating speed of 4000rpm to obtain heat conduction powder contained on the surface;
and (3) adding the prepared heat-conducting powder, methyl phenyl silicone oil, hexadecyl trimethoxy silane and an antioxidant into a planetary disperser according to the proportion, wherein the rotating speed is 300rpm, starting vacuumizing, heating to 100 ℃, and mixing for 2 hours to obtain the heat-conducting silicone grease.
Example 4
The fine and smooth flowing type heat conduction silicone grease comprises the following components in parts by weight: 100 parts of methylphenyl silicone oil with the viscosity of 100 mPas, 1000 parts of spherical alumina with the median diameter of 20 mu m, 250 parts of spherical alumina with the median diameter of 10 mu m, 250 parts of spherical alumina with the median diameter of 5 mu m, 500 parts of zinc oxide with the median diameter of 0.9 mu m, 6 parts of octadecyltrimethoxysilane, 6 parts of dipropyl hypophosphorous acid and 1 part of antioxidant. The preparation method of the fine and smooth flowing type heat conduction silicone grease comprises the following two steps:
adding spherical aluminum oxide, zinc oxide and octadecyl trimethoxy silane into a high-speed mixer according to the proportion, mixing at a high speed for 10 minutes at a rotating speed of 5000rpm, then adding dipropyl hypophosphorous acid according to the proportion, and continuing mixing at a high speed for 5 minutes to obtain heat conduction powder with double-layer cladding on the surface;
and (3) adding the prepared heat-conducting powder, the methylphenyl silicone oil and the antioxidant into the planetary dispersing machine according to the proportion, wherein the rotating speed is 200rpm, starting vacuumizing, heating to 100 ℃, and mixing for 3 hours to obtain the flowing type fine heat-conducting silicone grease.
Comparative example 4
The heat-conducting silicone grease of the comparative example comprises the following components in parts by weight: 100 parts of methylphenyl silicone oil with the viscosity of 100 mPas, 1000 parts of spherical alumina with the median diameter of 50 mu m, 250 parts of spherical alumina with the median diameter of 25 mu m, 250 parts of spherical alumina with the median diameter of 5 mu m, 500 parts of zinc oxide with the median diameter of 0.9 mu m, 6 parts of octadecyltrimethoxysilane, 6 parts of dipropyl hypophosphorous acid and 1 part of antioxidant.
The preparation method of the heat-conducting silicone grease comprises the following two steps:
adding spherical aluminum oxide, zinc oxide and octadecyl trimethoxysilane into a high-speed mixer according to the proportion, mixing at a high speed for 10 minutes at a rotation speed of 5000rpm, then adding dipropyl hypophosphorous acid according to the proportion, and continuing mixing at a high speed for 5 minutes to obtain heat conduction powder with double-layer cladding on the surface;
and (3) adding the prepared heat conducting powder, methyl phenyl silicone oil and an antioxidant into a planetary dispersing machine according to the proportion, wherein the rotating speed is 200rpm, starting vacuumizing, heating to 100 ℃, and mixing for 3 hours to obtain the heat conducting silicone grease.
The heat conductive silicone greases prepared in examples 1 to 4 and comparative examples 1 to 4 were subjected to performance tests including blade coatability, heat conductivity, viscosity, etc., and the results are shown in table 1, wherein NA indicates that the test was impossible.
TABLE 1
From the test results in table 1, it can be seen that:
when the filling part of filler is low (embodiment 1 and embodiment 2), the heat conduction silicone grease has excellent comprehensive performance, the heat conduction coefficient can reach 2.4w/m.k, and the heat conduction silicone grease has very low viscosity and excellent blade coating property; continuing to increase the filler addition (examples 3 and 4), the thermal conductivity of the silicone grease was further increased to 4.0w/m.k, but still lower viscosity and blade coatability could be maintained;
the modification of the filler (comparative examples 1 and 2) with a single modifier or the modification sequence of the modifiers (comparative example 3) affects the final coating effect of the coupling agent on the filler surface, which results in the occurrence of thixotropic (comparative example 1) or poorly stirrable, high viscosity (comparative examples 2 and 3) conditions of silicone grease.
According to the method, silicone grease with low viscosity and high heat conductivity coefficient can be prepared by using coarse-grain-diameter spherical alumina (comparative example 4) as a filler, but the silicone grease has poor knife coating property and is easy to settle and agglomerate in the placing process.
Finally, it should be noted that the above embodiments are only for illustrating the technical solution of the present invention and not for limiting the scope of the present invention, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that the technical solution of the present invention may be modified or some or all of the technical features thereof may be equally substituted; such modifications and substitutions do not depart from the spirit of the invention.
Claims (4)
1. A flowing type fine heat-conducting silicone grease is characterized in that: the components and parts by weight are as follows:
silicone oil: 100 parts of
And (3) a heat conducting filler: 800-2800 parts
Silane coupling agent: 2-10 parts
Dialkylphosphinic acids: 2-10 parts
An antioxidant: 0.1-5 parts
The silane coupling agent is a long-chain alkyl silane coupling agent and is selected from one of dodecyl trimethoxy silane, dodecyl triethoxy silane, dodecyl methyl dimethoxy silane, hexadecyl trimethoxy silane and octadecyl trimethoxy silane;
the dialkyl hypophosphorous acid is short-chain alkyl substituted hypophosphorous acid, and is selected from one of diethyl hypophosphorous acid, dipropyl hypophosphorous acid, diisobutyl hypophosphorous acid, 1-ethyl-2-propyl hypophosphorous acid and dibutyl hypophosphorous acid;
the heat conducting filler is selected from one or more than two of aluminum oxide, zinc oxide, magnesium oxide, boron nitride, silicon nitride, aluminum nitride, silicon micro powder, aluminum hydroxide, magnesium hydroxide, aluminum powder and copper powder, wherein the bit diameter D50 is 0.2-30 mu m;
the preparation method of the flowing type fine heat-conducting silicone grease comprises the following steps: adding a heat conducting filler and a silane coupling agent into a high-speed mixer, mixing at a high speed of 500rpm-5000rpm for 2-30min to uniformly mix the heat conducting filler and the silane coupling agent, then adding dialkyl hypophosphorous acid, and continuing to mix at a high speed to obtain heat conducting powder with double-layer coating on the surface; then adding the obtained heat conducting powder, silicone oil and antioxidant into a planetary mixer, and mixing for 1-3 hours at the temperature of 50-150 ℃ and the rotating speed of 100-2000rpm to obtain the flowing type fine heat conducting silicone grease.
2. The drool type fine and smooth heat-conducting silicone grease according to claim 1, wherein: the silicone oil is at least one of methyl silicone oil and phenyl silicone grease, and the viscosity is 20 mPas-5000 mPas.
3. The drool type fine and smooth heat-conducting silicone grease according to claim 1, wherein: the heat conducting filler is one or more of irregular, spherical, spheroidal and lamellar.
4. The drool type fine and smooth heat-conducting silicone grease according to claim 1, wherein: the antioxidant is one of antioxidant 1010, antioxidant 1076, antioxidant 168 and antioxidant 1135.
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| CN202111313321.3A CN114410113B (en) | 2021-11-08 | 2021-11-08 | Flowing type fine heat-conducting silicone grease and preparation method thereof |
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| CN202111313321.3A CN114410113B (en) | 2021-11-08 | 2021-11-08 | Flowing type fine heat-conducting silicone grease and preparation method thereof |
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| CN114410113A CN114410113A (en) | 2022-04-29 |
| CN114410113B true CN114410113B (en) | 2023-06-09 |
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| CN115433461B (en) * | 2022-09-15 | 2023-11-24 | 矽时代材料科技股份有限公司 | Heat-conducting silicone grease with low oil separation rate and long storage life and preparation method thereof |
| CN115558293B (en) * | 2022-10-12 | 2023-06-16 | 杭州之江有机硅化工有限公司 | Heat-conducting silicone grease composition and application thereof |
| CN115710461B (en) * | 2022-11-18 | 2023-09-26 | 广州集泰化工股份有限公司 | High-performance heat-conducting silicone grease and preparation method and application thereof |
| CN115960466B (en) * | 2022-12-28 | 2024-04-26 | 广东金戈新材料股份有限公司 | Thixotropic silicone grease with low thermal resistance and high thermal conductivity and preparation method thereof |
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| CN107793763B (en) * | 2017-10-20 | 2020-08-11 | 佛山市三水铠潮材料科技有限公司 | High-temperature-resistant heat-conducting silicone grease and preparation method thereof |
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