WO2022057083A1 - High-thermal-conductivity self-leveling modified ceramic liquid potting material and preparation method therefor - Google Patents

High-thermal-conductivity self-leveling modified ceramic liquid potting material and preparation method therefor Download PDF

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WO2022057083A1
WO2022057083A1 PCT/CN2020/131364 CN2020131364W WO2022057083A1 WO 2022057083 A1 WO2022057083 A1 WO 2022057083A1 CN 2020131364 W CN2020131364 W CN 2020131364W WO 2022057083 A1 WO2022057083 A1 WO 2022057083A1
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parts
powder
ceramic
silicone oil
treatment agent
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PCT/CN2020/131364
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Chinese (zh)
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唐正华
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平湖阿莱德实业有限公司
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J183/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
    • C09J183/04—Polysiloxanes
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02—Non-macromolecular additives
    • C09J11/04—Non-macromolecular additives inorganic
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
    • C09K5/08—Materials not undergoing a change of physical state when used
    • C09K5/14—Solid materials, e.g. powdery or granular
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C08K2003/2227—Oxides; Hydroxides of metals of aluminium
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00—Specific properties of additives
    • C08K2201/002—Physical properties
    • C08K2201/003—Additives being defined by their diameter
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2203/00—Applications
    • C08L2203/20—Applications use in electrical or conductive gadgets
    • C08L2203/206—Applications use in electrical or conductive gadgets use in coating or encapsulating of electronic parts
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00—Polymer mixtures characterised by other features
    • C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
    • C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure

Definitions

  • the invention belongs to the technical field of materials, and in particular relates to a self-leveling modified ceramic liquid potting material with high thermal conductivity and a preparation method thereof.
  • Thermally conductive electronic potting glue is a protective glue used for potting electronic components, power supplies and electronic products.
  • the potting glue is liquid before curing and has fluidity. The viscosity of the glue depends on the material, performance, The production process is different; the potting glue can realize its use value after it is completely cured.
  • the thermal conductivity of high thermal conductivity potting products on the market is generally concentrated below 3W/(mk), and the technical requirements are more than 4W/(mk), which means that the thermal conductivity powder: the oil needs to be greater than 12, and it is required to have good drainage. Foaming, the viscosity needs to be controlled below 30,000 mPa.S, which has reached the technical bottleneck of traditional potting glue products.
  • the purpose of the present invention is to provide a self-leveling modified ceramic liquid potting material with high thermal conductivity and a preparation method thereof.
  • this potting material is made up of A component and B component, it is characterized in that,
  • the A component is composed of the following components by weight: vinyl silicone oil, 1000-2500 parts of modified ceramic filler powder, 0.01-10 parts of ceramic powder treatment agent, and 0.01-5 parts of platinum catalyst, wherein the vinyl The total amount of silicone oil, ceramic powder treatment agent and platinum catalyst is 100 parts;
  • the B component is composed of the following components in parts by weight: vinyl silicone oil, 1-50 parts of hydrogen-containing silicone oil, 1,000-2,500 parts of modified ceramic filler powder, 0.01-10 parts of ceramic powder treatment agent, and 0.001 part of inhibitor It is composed of 5 parts, wherein the total amount of vinyl silicone oil, hydrogen-containing silicone oil, ceramic powder treatment agent and inhibitor is 100 parts.
  • the high thermal conductivity self-leveling modified ceramic liquid filling material is characterized in that the preparation method of the modified ceramic filler powder is as follows: atomizing and spraying the ceramic powder treatment agent solution on the ceramic filler in a high-speed disperser , fully mixed at 100° C. for 20 minutes to obtain modified ceramic filler powder, wherein the weight ratio of ceramic filler to ceramic powder treatment agent is 1000:0.01-10.
  • the self-leveling modified ceramic liquid filling material with high thermal conductivity is characterized in that the ceramic filler comprises spherical thermally conductive powder with a particle size of 0.2-2 ⁇ m, spherical thermally conductive powder with a particle size of 5-20 ⁇ m, and a particle size of 40-20 ⁇ m. Any two or three mixtures of 120 ⁇ m spherical thermally conductive powders.
  • the high thermal conductivity self-leveling modified ceramic liquid filling material is characterized in that the ceramic filler is specifically alumina powder, aluminum nitride powder, silicon nitride powder, boron nitride powder, silicon carbide powder One or any mixture of materials.
  • the high thermal conductivity self-leveling modified ceramic liquid filling material is characterized in that the ceramic powder treatment agent is alkoxysilane monomer, alkoxysilane oligomer, monoalkoxytitanate, aluminum One or any mixture of acid esters and zirconates.
  • the high thermal conductivity self-leveling modified ceramic liquid filling material is characterized in that the oil viscosity of the vinyl silicone is in the range of 30-200 mPa ⁇ S, preferably 30-100 mPa ⁇ S, more preferably 50 mPa ⁇ S.
  • the high thermal conductivity self-leveling modified ceramic liquid filling material is characterized in that the hydrogen-containing silicone oil is one or any of several of: terminal methyl hydrogen-containing silicone oil, terminal hydrogen-containing silicone oil, and end-side hydrogen-containing silicone oil
  • the mixture contains 0.01-0.8% wt of hydrogen.
  • the self-leveling modified ceramic liquid filling material with high thermal conductivity is characterized in that the platinum catalyst is a Castel platinum catalyst, and the inhibitor is an alkynol compound, vinyl polysiloxane, amide compound, maleic acid One of the acid ester compounds.
  • Modification of ceramic filler powder Add 1000 parts of ceramic filler with different particle size ratios into a high-speed disperser, the dispersion speed is 1500-4000rmp, and the ceramic powder treatment agent solution is sprayed by atomization under high shear. 0.01-10 parts are dispersed on the ceramic filler, fully mixed for 5 to 10 minutes, and then treated at 100°C to 130°C for 20 minutes to obtain modified ceramic filler powder for use;
  • Component A Add 0.01-10 parts of vinyl silicone oil with a viscosity of 50mPa ⁇ S and 0.01-10 parts of ceramic powder treatment agent into the planetary machine, and then add 1,000-2,500 parts of modified ceramic filler powder, and mix the materials at room temperature 30min, heat up to the material temperature of 140°C, heat and mix for 2h, lower the temperature for 1h under a vacuum degree greater than 0.095Mpa, cool down to room temperature and add 0.01 to 5 parts of platinum catalyst, of which vinyl silicone oil, ceramic powder treatment agent and platinum catalyst are combined. The amount is 100 servings;
  • Component B Add 0.01-10 parts of vinyl silicone oil with a viscosity of 50mPa ⁇ S and 0.01-10 parts of ceramic powder treatment agent to the planetary machine, and then add 1,000-2,500 parts of modified ceramic filler powder, and mix the materials at room temperature for 30 minutes. The temperature was raised to the material temperature of 140°C, heated and kneaded for 2 hours, and then lowered for 1 hour at a vacuum degree greater than 0.095Mpa. After cooling to room temperature, 1-50 parts of hydrogen-containing silicone oil and 0.001-5 parts of inhibitors were added, among which vinyl silicone oil and hydrogen-containing silicone oil were added. , The total amount of ceramic powder treatment agent and inhibitor is 100 parts;
  • component A and component B are mixed in a 1:1 dispensing ratio and rapidly vulcanized at room temperature to form a highly flexible rubber elastomer.
  • the present invention has reasonable formula and simple and easy preparation process.
  • secondary wet coating modified thermal conductive powder on the basis of traditional dry modified ceramic powder, the self-leveling modification with good fluidity and high thermal conductivity can be prepared.
  • Ceramic liquid potting material By adding secondary wet coating modified thermal conductive powder on the basis of traditional dry modified ceramic powder, the self-leveling modification with good fluidity and high thermal conductivity can be prepared. Ceramic liquid potting material.
  • Modification of ceramic filler powder Add 2000 parts of spherical alumina powder with different particle size ratios into a high-speed disperser, the dispersion speed is 2000rmp, and 5 parts of the ceramic powder treatment agent solution are dispersed by atomization and spraying under high shear. On the alumina powder, fully mixed for 10min, and then treated at 110°C for 20min to obtain modified ceramic filler powder.
  • Component A Add 97 parts of vinyl silicone oil with a viscosity of 50mPa ⁇ S and 2 parts of ceramic powder treatment agent into the planetary machine and mix them evenly, then add 1,300 parts of modified ceramic filler powder, mix the materials at room temperature for 30 minutes, and heat up to The material temperature was 140°C after heating and kneading for 2 hours, and then it was lowered for 1 hour under a vacuum degree greater than 0.095Mpa. After cooling to room temperature, 1 part of platinum catalyst was added.
  • Component B Add 67.5 parts of vinyl silicone oil with a viscosity of 50mPa ⁇ S and 2 parts of ceramic powder treatment agent into the planetary machine, and mix them evenly, then add 1,300 parts of modified ceramic filler powder, mix the materials at room temperature for 30 minutes, and heat up to The temperature of the material is 140°C after heating and kneading for 2 hours, and then the vacuum degree is greater than 0.095Mpa, and it is lowered for 1 hour. After cooling to room temperature, 30 parts of hydrogen-containing silicone oil and 0.5 part of inhibitor are added.
  • Component A Add 99 parts of vinyl silicone oil with a viscosity of 50mPa ⁇ S to the planetary machine, add 1,300 parts of modified ceramic filler powder, mix the materials at room temperature for 30 minutes, heat up to the material temperature of 140 °C, heat and mix for 2 hours, and then vacuum The temperature was lower than 0.095Mpa for 1 hour, and then 1 part of platinum catalyst was added after cooling to room temperature.
  • Component B add 69.5 parts of vinyl silicone oil with a viscosity of 50mPa ⁇ S to the planetary machine, add 1300 parts of modified ceramic filler powder, mix the materials at room temperature for 30 minutes, heat up to the material temperature of 140 °C, heat and mix for 2 hours, and then vacuum The temperature is higher than 0.095Mpa, and it is lowered for 1 hour. After cooling to room temperature, 30 parts of hydrogen-containing silicone oil and 0.5 parts of inhibitor are added.
  • Modification of ceramic filler powder Add 3000 parts of spherical alumina powder with different particle size ratios into a high-speed disperser, the dispersion speed is 2000rmp, and 5 parts of ceramic powder treatment agent solution are sprayed by atomization under high shear. Disperse on alumina powder, thoroughly mix for 10min, and then treat at 110°C for 20min to obtain modified ceramic filler powder.
  • Component A Add 99 parts of vinyl silicone oil with a viscosity of 50mPa ⁇ S to the planetary machine, add 2,000 parts of modified ceramic filler powder, mix the materials at room temperature for 30 minutes, heat up to the material temperature of 140 °C, heat and mix for 2 hours, and then vacuum The temperature was lower than 0.095Mpa for 1 hour, and then 1 part of platinum catalyst was added after cooling to room temperature.
  • Component B Add 69.5 parts of vinyl silicone oil with a viscosity of 50mPa ⁇ S to the planetary machine, add 2,000 parts of modified ceramic filler powder, mix the materials at room temperature for 30 minutes, heat up to the material temperature of 140 °C, heat and mix for 2 hours, and then vacuum The temperature is higher than 0.095Mpa, and it is lowered for 1 hour. After cooling to room temperature, 30 parts of hydrogen-containing silicone oil and 0.5 parts of inhibitor are added.
  • Modification of ceramic filler powder Add 3000 parts of spherical alumina powder with different particle size ratios into a high-speed disperser, the dispersion speed is 2000rmp, and 5 parts of ceramic powder treatment agent solution are sprayed by atomization under high shear. Disperse on alumina powder, thoroughly mix for 10min, and then treat at 110°C for 20min to obtain modified ceramic filler powder.
  • Component A Add 97 parts of vinyl silicone oil with a viscosity of 50mPa ⁇ S and 2 parts of ceramic powder treatment agent into the planetary machine, and mix them evenly, then add 2,000 parts of modified ceramic filler powder, mix the materials at room temperature for 30 minutes, and heat up to The material temperature was 140°C after heating and kneading for 2 hours, and then it was lowered for 1 hour under a vacuum degree greater than 0.095Mpa. After cooling to room temperature, 1 part of platinum catalyst was added.
  • Component B Add 67.5 parts of vinyl silicone oil with a viscosity of 50mPa ⁇ S and 2 parts of ceramic powder treatment agent into the planetary machine, and mix them evenly, then add 2,000 parts of modified ceramic filler powder, mix the materials at room temperature for 30 minutes, and heat up to The temperature of the material is 140°C after heating and kneading for 2 hours, and then the vacuum degree is greater than 0.095Mpa, and it is lowered for 1 hour. After cooling to room temperature, 30 parts of hydrogen-containing silicone oil and 0.5 part of inhibitor are added.
  • Test method Test the thermal conductivity of the potting material after curing according to ASTM D 5470-2012. The higher the thermal conductivity, the better the thermal conductivity of the gasket; the viscosity of the potting material is tested according to ASTM D2196-2015. The hardness of the potting material is tested according to ASTM D2240-2015. The test results are shown in Table 1.

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Abstract

A high-thermal-conductivity self-leveling modified ceramic liquid potting material and a preparation method therefor. The potting material consists of a component A and a component B. The component A consists of the following components in parts by weight: vinyl silicone oil, 1000-2500 parts of modified ceramic filler powder, 0.01-10 parts of a ceramic powder treatment agent, and 0.01-5 parts of a platinum catalyst. The component B consists of the following components in parts by weight: vinyl silicone oil, 1-50 parts of hydrogen-containing silicone oil, 1000-2500 parts of modified ceramic filler powder, 0.01-10 parts of a ceramic powder treatment agent, and 0.001-5 parts of an inhibitor. Secondary wet coated modified thermally conductive powder is added on the basis of conventional dry-process modified ceramic powder, thereby preparing the self-leveling modified ceramic liquid potting material having good fluidity and high thermal conductivity.

Description

高导热自流平改性陶瓷液体灌封材料及其制备方法High thermal conductivity self-leveling modified ceramic liquid potting material and preparation method thereof 技术领域technical field
本发明属于材料技术领域，具体涉及一种高导热自流平改性陶瓷液体灌封材料及其制备方法。The invention belongs to the technical field of materials, and in particular relates to a self-leveling modified ceramic liquid potting material with high thermal conductivity and a preparation method thereof.
背景技术Background technique
随着现代电子通讯业的迅猛发展，尤其是进入5G时代人们越来越重视产品的稳定性和使用体验，对电子产品的耐候性和可靠性有了有更高的审核标准，所以越来越多的电子产品需要使用灌封。导热电子灌封胶是一种用于灌封电子元件、电源、电子产品上的防护性胶水，灌封胶在未固化前属于液体状，具有流动性，胶液黏度根据产品的材质、性能、生产工艺的不同而有所区别；灌封胶完全固化后才能实现它的使用价值，固化后使用能为电子器件提供最佳的内应力需求，保证元器件间不会相互影响，避免元器件直接暴露在空气中，防止元器件受到环境侵蚀，提高元器件的使用寿命，达到防水、防尘、导热的作用。With the rapid development of the modern electronic communication industry, especially in the 5G era, people pay more and more attention to the stability and use experience of products, and have higher audit standards for the weather resistance and reliability of electronic products, so more and more Many electronic products require potting. Thermally conductive electronic potting glue is a protective glue used for potting electronic components, power supplies and electronic products. The potting glue is liquid before curing and has fluidity. The viscosity of the glue depends on the material, performance, The production process is different; the potting glue can realize its use value after it is completely cured. After curing, it can provide the best internal stress requirements for electronic devices, ensure that the components will not affect each other, and avoid direct Exposure to the air can prevent the components from being corroded by the environment, improve the service life of the components, and achieve the functions of waterproof, dustproof and thermal conductivity.
目前市面上高导热灌封类产品导热系数普遍集中在3W/(m.k)以下，对于技术要求达到4W/(m.k)以上，这意味着导热粉：油需大于12，同时要求具有很好的排泡性，需要控制粘度在3万mPa.S以下，已经到了传统灌封胶类产品技术瓶颈。At present, the thermal conductivity of high thermal conductivity potting products on the market is generally concentrated below 3W/(mk), and the technical requirements are more than 4W/(mk), which means that the thermal conductivity powder: the oil needs to be greater than 12, and it is required to have good drainage. Foaming, the viscosity needs to be controlled below 30,000 mPa.S, which has reached the technical bottleneck of traditional potting glue products.
发明内容SUMMARY OF THE INVENTION
针对现有技术中存在的问题，本发明设计的目的在于提供一种高导热自流平改性陶瓷液体灌封材料及其制备方法。In view of the problems existing in the prior art, the purpose of the present invention is to provide a self-leveling modified ceramic liquid potting material with high thermal conductivity and a preparation method thereof.
本发明通过以下技术方案加以实现：The present invention is achieved through the following technical solutions:
所述的高导热自流平改性陶瓷液体灌封材料，该灌封材料由A组分和B组 分构成，其特征在于，Described high thermal conductivity self-leveling modified ceramic liquid potting material, this potting material is made up of A component and B component, it is characterized in that,
所述A组分由以下重量份的组分组成：乙烯基硅油、改性陶瓷填料粉1000～2500份、陶瓷粉料处理剂0.01～10份、铂金催化剂0.01～5份组成，其中，乙烯基硅油、陶瓷粉料处理剂和铂金催化剂总量为100份；The A component is composed of the following components by weight: vinyl silicone oil, 1000-2500 parts of modified ceramic filler powder, 0.01-10 parts of ceramic powder treatment agent, and 0.01-5 parts of platinum catalyst, wherein the vinyl The total amount of silicone oil, ceramic powder treatment agent and platinum catalyst is 100 parts;
所述B组分由以下重量份的组分组成：乙烯基硅油、含氢硅油1～50份、改性陶瓷填料粉1000～2500份、陶瓷粉料处理剂0.01～10份、以及抑制剂0.001～5份组成，其中乙烯基硅油、含氢硅油、陶瓷粉料处理剂和抑制剂总量为100份。The B component is composed of the following components in parts by weight: vinyl silicone oil, 1-50 parts of hydrogen-containing silicone oil, 1,000-2,500 parts of modified ceramic filler powder, 0.01-10 parts of ceramic powder treatment agent, and 0.001 part of inhibitor It is composed of 5 parts, wherein the total amount of vinyl silicone oil, hydrogen-containing silicone oil, ceramic powder treatment agent and inhibitor is 100 parts.
所述的高导热自流平改性陶瓷液体灌装材料，其特征在于所述改性陶瓷填料粉的制备方法为，在高速分散机中将陶瓷粉料处理剂溶液雾化喷撒在陶瓷填料上，充分混合100℃处理20min，得到改性陶瓷填料粉，其中陶瓷填料与陶瓷粉料处理剂的重量比为1000:0.01-10。The high thermal conductivity self-leveling modified ceramic liquid filling material is characterized in that the preparation method of the modified ceramic filler powder is as follows: atomizing and spraying the ceramic powder treatment agent solution on the ceramic filler in a high-speed disperser , fully mixed at 100° C. for 20 minutes to obtain modified ceramic filler powder, wherein the weight ratio of ceramic filler to ceramic powder treatment agent is 1000:0.01-10.
所述的高导热自流平改性陶瓷液体灌装材料，其特征在于所述陶瓷填料包括粒径为0.2～2μm的球形导热粉、粒径为5～20μm的球形导热粉、粒径为40～120μm的球形导热粉中的任意两种或三种混合物。The self-leveling modified ceramic liquid filling material with high thermal conductivity is characterized in that the ceramic filler comprises spherical thermally conductive powder with a particle size of 0.2-2 μm, spherical thermally conductive powder with a particle size of 5-20 μm, and a particle size of 40-20 μm. Any two or three mixtures of 120μm spherical thermally conductive powders.
所述的高导热自流平改性陶瓷液体灌装材料，其特征在于所述陶瓷填料具体为氧化铝粉料、氮化铝粉料、氮化硅粉料、氮化硼粉料，碳化硅粉料中的一种或任意几种混合物。The high thermal conductivity self-leveling modified ceramic liquid filling material is characterized in that the ceramic filler is specifically alumina powder, aluminum nitride powder, silicon nitride powder, boron nitride powder, silicon carbide powder One or any mixture of materials.
所述的高导热自流平改性陶瓷液体灌装材料，其特征在于所述陶瓷粉料处理剂为烷氧基硅烷单体、烷氧基硅烷低聚物、单烷氧基钛酸酯、铝酸酯类、锆酸酯类中的一种或任意几种混合物。The high thermal conductivity self-leveling modified ceramic liquid filling material is characterized in that the ceramic powder treatment agent is alkoxysilane monomer, alkoxysilane oligomer, monoalkoxytitanate, aluminum One or any mixture of acid esters and zirconates.
所述的高导热自流平改性陶瓷液体灌装材料，其特征在于所述乙烯基硅的油粘度范围在30～200mPa·S之间，优选30～100mPa·S，更优选50mPa·S。The high thermal conductivity self-leveling modified ceramic liquid filling material is characterized in that the oil viscosity of the vinyl silicone is in the range of 30-200 mPa·S, preferably 30-100 mPa·S, more preferably 50 mPa·S.
所述的高导热自流平改性陶瓷液体灌装材料，其特征在于所述含氢硅油为： 端甲基含氢硅油、端含氢硅油、端侧含氢硅油中的一种或任意几种混合物，含氢量为0.01～0.8％wt。The high thermal conductivity self-leveling modified ceramic liquid filling material is characterized in that the hydrogen-containing silicone oil is one or any of several of: terminal methyl hydrogen-containing silicone oil, terminal hydrogen-containing silicone oil, and end-side hydrogen-containing silicone oil The mixture contains 0.01-0.8% wt of hydrogen.
所述的高导热自流平改性陶瓷液体灌装材料，其特征在于所述铂金催化剂为卡斯特铂金催化剂，抑制剂为炔醇类化合物，乙烯基类聚硅氧烷，酰胺化合物，马来酸酯类化合物中的一种。The self-leveling modified ceramic liquid filling material with high thermal conductivity is characterized in that the platinum catalyst is a Castel platinum catalyst, and the inhibitor is an alkynol compound, vinyl polysiloxane, amide compound, maleic acid One of the acid ester compounds.
所述的高导热自流平改性陶瓷液体灌装材料的制备方法，其特征在于包括以下步骤：The method for preparing a self-leveling modified ceramic liquid filling material with high thermal conductivity is characterized by comprising the following steps:
1)陶瓷填料粉体改性：将不同粒径配比的陶瓷填料1000份加入高速分散机中，分散速度为1500～4000rmp，高剪切下通过雾化喷撒方式将陶瓷粉料处理剂溶液0.01-10份分散在陶瓷填料上，充分混合处理5～10min，然后100℃～130℃处理20min，得到改性陶瓷填料粉，备用；1) Modification of ceramic filler powder: Add 1000 parts of ceramic filler with different particle size ratios into a high-speed disperser, the dispersion speed is 1500-4000rmp, and the ceramic powder treatment agent solution is sprayed by atomization under high shear. 0.01-10 parts are dispersed on the ceramic filler, fully mixed for 5 to 10 minutes, and then treated at 100°C to 130°C for 20 minutes to obtain modified ceramic filler powder for use;
2)A组分：在行星机中加入粘度为50mPa·S的乙烯基硅油和陶瓷粉料处理剂0.01～10份混合均匀后，加入改性陶瓷填料粉1000～2500份，物料在室温下混合30min，升温至物料温度140℃加热混炼2h后于真空度大于0.095Mpa下脱低1h，降温至室温后加入铂金催化剂0.01～5份，其中乙烯基硅油、陶瓷粉料处理剂和铂金催化剂总量为100份；2) Component A: Add 0.01-10 parts of vinyl silicone oil with a viscosity of 50mPa·S and 0.01-10 parts of ceramic powder treatment agent into the planetary machine, and then add 1,000-2,500 parts of modified ceramic filler powder, and mix the materials at room temperature 30min, heat up to the material temperature of 140°C, heat and mix for 2h, lower the temperature for 1h under a vacuum degree greater than 0.095Mpa, cool down to room temperature and add 0.01 to 5 parts of platinum catalyst, of which vinyl silicone oil, ceramic powder treatment agent and platinum catalyst are combined. The amount is 100 servings;
B组分：在行星机中加入粘度为50mPa·S的乙烯基硅油和陶瓷粉料处理剂0.01～10份混合均匀后，加入改性陶瓷填料粉1000～2500份，物料在室温下混合30min，升温至物料温度140℃加热混炼2h后于真空度大于0.095Mpa下脱低1h，降温至室温后加入1～50份含氢硅油，0.001～5份抑制剂，其中乙烯基硅油、含氢硅油、陶瓷粉料处理剂和抑制剂总量为100份；Component B: Add 0.01-10 parts of vinyl silicone oil with a viscosity of 50mPa·S and 0.01-10 parts of ceramic powder treatment agent to the planetary machine, and then add 1,000-2,500 parts of modified ceramic filler powder, and mix the materials at room temperature for 30 minutes. The temperature was raised to the material temperature of 140°C, heated and kneaded for 2 hours, and then lowered for 1 hour at a vacuum degree greater than 0.095Mpa. After cooling to room temperature, 1-50 parts of hydrogen-containing silicone oil and 0.001-5 parts of inhibitors were added, among which vinyl silicone oil and hydrogen-containing silicone oil were added. , The total amount of ceramic powder treatment agent and inhibitor is 100 parts;
使用时，将A组分和B组分按1:1点胶混合室温快速硫化成高柔性橡胶弹性体。When in use, component A and component B are mixed in a 1:1 dispensing ratio and rapidly vulcanized at room temperature to form a highly flexible rubber elastomer.
本发明配方合理，制备工艺简单易行，通过在传统干法改性陶瓷粉体基础 上增加了二次湿法包覆改性导热粉，从而制备出流动性好，导热性能高自流平改性陶瓷液体灌封材料。The present invention has reasonable formula and simple and easy preparation process. By adding secondary wet coating modified thermal conductive powder on the basis of traditional dry modified ceramic powder, the self-leveling modification with good fluidity and high thermal conductivity can be prepared. Ceramic liquid potting material.
具体实施方式detailed description
以下结合具体实施例对本发明做进一步详细描述，以便更好的理解本发明。The present invention will be further described in detail below with reference to specific embodiments for better understanding of the present invention.
实施例1Example 1
陶瓷填料粉体改性：将2000份不同粒径配比球形氧化铝粉加入高速分散机中，分散速度为2000rmp，高剪切下通过雾化喷撒方式将5份陶瓷粉体处理剂溶液分散在氧化铝粉上，充分混合处理10min，然后110℃处理20min，得到改性陶瓷填料粉。Modification of ceramic filler powder: Add 2000 parts of spherical alumina powder with different particle size ratios into a high-speed disperser, the dispersion speed is 2000rmp, and 5 parts of the ceramic powder treatment agent solution are dispersed by atomization and spraying under high shear. On the alumina powder, fully mixed for 10min, and then treated at 110°C for 20min to obtain modified ceramic filler powder.
A组份：在行星机中加入97份粘度为50mPa·S的乙烯基硅油和陶瓷粉料处理剂2份混合均匀后，加入改性陶瓷填料粉1300份，物料在室温下混合30min，升温至物料温度140℃加热混炼2h后于真空度大于0.095Mpa下脱低1h，降温至室温后加入铂金催化剂1份。Component A: Add 97 parts of vinyl silicone oil with a viscosity of 50mPa·S and 2 parts of ceramic powder treatment agent into the planetary machine and mix them evenly, then add 1,300 parts of modified ceramic filler powder, mix the materials at room temperature for 30 minutes, and heat up to The material temperature was 140°C after heating and kneading for 2 hours, and then it was lowered for 1 hour under a vacuum degree greater than 0.095Mpa. After cooling to room temperature, 1 part of platinum catalyst was added.
B组份：在行星机中加入67.5份粘度为50mPa·S的乙烯基硅油和陶瓷粉料处理剂2份混合均匀后，加入改性陶瓷填料粉1300份，物料在室温下混合30min，升温至物料温度140℃加热混炼2h后于真空度大于0.095Mpa下脱低1h，降温至室温后加入30份含氢硅油，0.5份抑制剂。Component B: Add 67.5 parts of vinyl silicone oil with a viscosity of 50mPa·S and 2 parts of ceramic powder treatment agent into the planetary machine, and mix them evenly, then add 1,300 parts of modified ceramic filler powder, mix the materials at room temperature for 30 minutes, and heat up to The temperature of the material is 140°C after heating and kneading for 2 hours, and then the vacuum degree is greater than 0.095Mpa, and it is lowered for 1 hour. After cooling to room temperature, 30 parts of hydrogen-containing silicone oil and 0.5 part of inhibitor are added.
对比例1Comparative Example 1
陶瓷填料粉体改性同实施例1。The modification of ceramic filler powder is the same as that in Example 1.
A组份：在行星机中加入99份粘度为50mPa·S的乙烯基硅油，加入改性陶瓷填料粉1300份，物料在室温下混合30min，升温至物料温度140℃加热混炼2h后于真空度大于0.095Mpa下脱低1h，降温至室温后加入铂金催化剂1份。Component A: Add 99 parts of vinyl silicone oil with a viscosity of 50mPa·S to the planetary machine, add 1,300 parts of modified ceramic filler powder, mix the materials at room temperature for 30 minutes, heat up to the material temperature of 140 ℃, heat and mix for 2 hours, and then vacuum The temperature was lower than 0.095Mpa for 1 hour, and then 1 part of platinum catalyst was added after cooling to room temperature.
B组份：在行星机中加入69.5份粘度为50mPa·S的乙烯基硅油，加入改性陶瓷填料粉1300份，物料在室温下混合30min，升温至物料温度140℃加热混 炼2h后于真空度大于0.095Mpa下脱低1h，降温至室温后加入30份含氢硅油，0.5份抑制剂。Component B: add 69.5 parts of vinyl silicone oil with a viscosity of 50mPa·S to the planetary machine, add 1300 parts of modified ceramic filler powder, mix the materials at room temperature for 30 minutes, heat up to the material temperature of 140 ℃, heat and mix for 2 hours, and then vacuum The temperature is higher than 0.095Mpa, and it is lowered for 1 hour. After cooling to room temperature, 30 parts of hydrogen-containing silicone oil and 0.5 parts of inhibitor are added.
对比例2Comparative Example 2
陶瓷填料粉体改性：将3000份不同粒径配比的球形氧化铝粉加入高速分散机中，分散速度为2000rmp，高剪切下通过雾化喷撒方式将5份陶瓷粉体处理剂溶液分散在氧化铝粉上，充分混合处理10min，然后110℃处理20min，得到改性陶瓷填料粉。Modification of ceramic filler powder: Add 3000 parts of spherical alumina powder with different particle size ratios into a high-speed disperser, the dispersion speed is 2000rmp, and 5 parts of ceramic powder treatment agent solution are sprayed by atomization under high shear. Disperse on alumina powder, thoroughly mix for 10min, and then treat at 110°C for 20min to obtain modified ceramic filler powder.
A组份：在行星机中加入99份粘度为50mPa·S的乙烯基硅油，加入改性陶瓷填料粉2000份，物料在室温下混合30min，升温至物料温度140℃加热混炼2h后于真空度大于0.095Mpa下脱低1h，降温至室温后加入铂金催化剂1份。Component A: Add 99 parts of vinyl silicone oil with a viscosity of 50mPa·S to the planetary machine, add 2,000 parts of modified ceramic filler powder, mix the materials at room temperature for 30 minutes, heat up to the material temperature of 140 ℃, heat and mix for 2 hours, and then vacuum The temperature was lower than 0.095Mpa for 1 hour, and then 1 part of platinum catalyst was added after cooling to room temperature.
B组份：在行星机中加入69.5份粘度为50mPa·S的乙烯基硅油，加入改性陶瓷填料粉2000份，物料在室温下混合30min，升温至物料温度140℃加热混炼2h后于真空度大于0.095Mpa下脱低1h，降温至室温后加入30份含氢硅油，0.5份抑制剂。Component B: Add 69.5 parts of vinyl silicone oil with a viscosity of 50mPa·S to the planetary machine, add 2,000 parts of modified ceramic filler powder, mix the materials at room temperature for 30 minutes, heat up to the material temperature of 140 ℃, heat and mix for 2 hours, and then vacuum The temperature is higher than 0.095Mpa, and it is lowered for 1 hour. After cooling to room temperature, 30 parts of hydrogen-containing silicone oil and 0.5 parts of inhibitor are added.
对比例3Comparative Example 3
陶瓷填料粉体改性：将3000份不同粒径配比的球形氧化铝粉加入高速分散机中，分散速度为2000rmp，高剪切下通过雾化喷撒方式将5份陶瓷粉体处理剂溶液分散在氧化铝粉上，充分混合处理10min，然后110℃处理20min，得到改性陶瓷填料粉。Modification of ceramic filler powder: Add 3000 parts of spherical alumina powder with different particle size ratios into a high-speed disperser, the dispersion speed is 2000rmp, and 5 parts of ceramic powder treatment agent solution are sprayed by atomization under high shear. Disperse on alumina powder, thoroughly mix for 10min, and then treat at 110°C for 20min to obtain modified ceramic filler powder.
A组份：在行星机中加入97份粘度为50mPa·S的乙烯基硅油和陶瓷粉料处理剂2份混合均匀后，加入改性陶瓷填料粉2000份，物料在室温下混合30min，升温至物料温度140℃加热混炼2h后于真空度大于0.095Mpa下脱低1h，降温至室温后加入铂金催化剂1份。Component A: Add 97 parts of vinyl silicone oil with a viscosity of 50mPa·S and 2 parts of ceramic powder treatment agent into the planetary machine, and mix them evenly, then add 2,000 parts of modified ceramic filler powder, mix the materials at room temperature for 30 minutes, and heat up to The material temperature was 140°C after heating and kneading for 2 hours, and then it was lowered for 1 hour under a vacuum degree greater than 0.095Mpa. After cooling to room temperature, 1 part of platinum catalyst was added.
B组份：在行星机中加入67.5份粘度为50mPa·S的乙烯基硅油和陶瓷粉料 处理剂2份混合均匀后，加入改性陶瓷填料粉2000份，物料在室温下混合30min，升温至物料温度140℃加热混炼2h后于真空度大于0.095Mpa下脱低1h，降温至室温后加入30份含氢硅油，0.5份抑制剂。Component B: Add 67.5 parts of vinyl silicone oil with a viscosity of 50mPa·S and 2 parts of ceramic powder treatment agent into the planetary machine, and mix them evenly, then add 2,000 parts of modified ceramic filler powder, mix the materials at room temperature for 30 minutes, and heat up to The temperature of the material is 140°C after heating and kneading for 2 hours, and then the vacuum degree is greater than 0.095Mpa, and it is lowered for 1 hour. After cooling to room temperature, 30 parts of hydrogen-containing silicone oil and 0.5 part of inhibitor are added.
测试方法：按照ASTM D 5470-2012测试固化后灌封材料的导热系数，导热系数越高垫片的热传导性能越好；按ASTM D2196-2015测试灌封材料粘度。按ASTM D2240-2015测试灌封材料硬度。测试结果见表1。Test method: Test the thermal conductivity of the potting material after curing according to ASTM D 5470-2012. The higher the thermal conductivity, the better the thermal conductivity of the gasket; the viscosity of the potting material is tested according to ASTM D2196-2015. The hardness of the potting material is tested according to ASTM D2240-2015. The test results are shown in Table 1.
表1Table 1
Figure PCTCN2020131364-appb-000001
Figure PCTCN2020131364-appb-000001
以上所述仅为本发明的较佳实施方式，凡在本发明的申请范围之内所作的任何构造，修改以及原理的等效变化，等同替换和改进等，均包含在本发明的保护范围之内。The above are only the preferred embodiments of the present invention, and any structures, modifications and equivalent changes in principles, equivalent replacements and improvements made within the scope of the present invention are all included in the protection scope of the present invention. Inside.

Claims (9)

  1. 高导热自流平改性陶瓷液体灌封材料，该灌封材料由A组分和B组分构成，其特征在于，High thermal conductivity self-leveling modified ceramic liquid potting material, the potting material is composed of A component and B component, and is characterized in that:
    所述A组分由以下重量份的组分组成：乙烯基硅油、改性陶瓷填料粉1000～2500份、陶瓷粉料处理剂0.01～10份、铂金催化剂0.01～5份组成，其中，乙烯基硅油、陶瓷粉料处理剂和铂金催化剂总量为100份；The A component is composed of the following components by weight: vinyl silicone oil, 1000-2500 parts of modified ceramic filler powder, 0.01-10 parts of ceramic powder treatment agent, and 0.01-5 parts of platinum catalyst, wherein the vinyl The total amount of silicone oil, ceramic powder treatment agent and platinum catalyst is 100 parts;
    所述B组分由以下重量份的组分组成：乙烯基硅油、含氢硅油1～50份、改性陶瓷填料粉1000～2500份、陶瓷粉料处理剂0.01～10份、以及抑制剂0.001～5份组成，其中乙烯基硅油、含氢硅油、陶瓷粉料处理剂和抑制剂总量为100份。The B component is composed of the following components in parts by weight: vinyl silicone oil, 1-50 parts of hydrogen-containing silicone oil, 1,000-2,500 parts of modified ceramic filler powder, 0.01-10 parts of ceramic powder treatment agent, and 0.001 part of inhibitor It is composed of 5 parts, wherein the total amount of vinyl silicone oil, hydrogen-containing silicone oil, ceramic powder treatment agent and inhibitor is 100 parts.
  2. 如权利要求1所述的高导热自流平改性陶瓷液体灌装材料，其特征在于所述改性陶瓷填料粉的制备方法为，在高速分散机中将陶瓷粉料处理剂溶液雾化喷撒在陶瓷填料上，充分混合100℃处理20min，得到改性陶瓷填料粉，其中陶瓷填料与陶瓷粉料处理剂的重量比为1000:0.01-10。The self-leveling modified ceramic liquid filling material with high thermal conductivity according to claim 1, wherein the preparation method of the modified ceramic filler powder is as follows: atomizing and spraying the ceramic powder treatment agent solution in a high-speed disperser On the ceramic filler, fully mix at 100 DEG C for 20min to obtain modified ceramic filler powder, wherein the weight ratio of ceramic filler to ceramic powder treatment agent is 1000:0.01-10.
  3. 如权利要求2所述的高导热自流平改性陶瓷液体灌装材料，其特征在于所述陶瓷填料包括粒径为0.2～2μm的球形导热粉、粒径为5～20μm的球形导热粉、粒径为40～120μm的球形导热粉中的任意两种或三种混合物。The self-leveling modified ceramic liquid filling material with high thermal conductivity according to claim 2, wherein the ceramic filler comprises spherical thermally conductive powder with a particle size of 0.2-2 μm, spherical Any two or three mixtures of spherical thermally conductive powders with a diameter of 40-120 μm.
  4. 如权利要求2所述的高导热自流平改性陶瓷液体灌装材料，其特征在于所述陶瓷填料具体为氧化铝粉料、氮化铝粉料、氮化硅粉料、氮化硼粉料，碳化硅粉料中的一种或任意几种混合物。The self-leveling modified ceramic liquid filling material with high thermal conductivity according to claim 2, wherein the ceramic filler is specifically alumina powder, aluminum nitride powder, silicon nitride powder, boron nitride powder , one or any mixture of silicon carbide powder.
  5. 如权利要求1所述的高导热自流平改性陶瓷液体灌装材料，其特征在于所述陶瓷粉料处理剂为烷氧基硅烷单体、烷氧基硅烷低聚物、单烷氧基钛酸酯、铝酸酯类、锆酸酯类中的一种或任意几种混合物。The self-leveling modified ceramic liquid filling material with high thermal conductivity according to claim 1, wherein the ceramic powder treatment agent is alkoxysilane monomer, alkoxysilane oligomer, monoalkoxytitanium One or any mixture of acid esters, aluminates and zirconates.
  6. 如权利要求1所述的高导热自流平改性陶瓷液体灌装材料，其特征在于所述乙烯基硅的油粘度范围在30～200mPa·S之间，优选30～100mPa·S，更优选50mPa·S。The self-leveling modified ceramic liquid filling material with high thermal conductivity according to claim 1, wherein the oil viscosity of the vinyl silicone is in the range of 30-200 mPa·S, preferably 30-100 mPa·S, more preferably 50 mPa ·S.
  7. 如权利要求1所述的高导热自流平改性陶瓷液体灌装材料，其特征在于所述含氢硅油为：端甲基含氢硅油、端含氢硅油、端侧含氢硅油中的一种或任意几种混合物，含氢量为0.01～0.8％wt。The self-leveling modified ceramic liquid filling material with high thermal conductivity as claimed in claim 1, wherein the hydrogen-containing silicone oil is one of: terminal methyl hydrogen-containing silicone oil, end-side hydrogen-containing silicone oil, and end-side hydrogen-containing silicone oil Or any mixture, the hydrogen content is 0.01-0.8%wt.
  8. 如权利要求1所述的高导热自流平改性陶瓷液体灌装材料，其特征在于所述铂金催化剂为卡斯特铂金催化剂，抑制剂为炔醇类化合物，乙烯基类聚硅氧烷，酰胺化合物，马来酸酯类化合物中的一种。The self-leveling modified ceramic liquid filling material with high thermal conductivity according to claim 1, wherein the platinum catalyst is a Castel platinum catalyst, and the inhibitor is an alkynol compound, a vinyl polysiloxane, an amide compound, one of the maleate compounds.
  9. 权利要求1所述的高导热自流平改性陶瓷液体灌装材料的制备方法，其特征在于包括以下步骤：The preparation method of the self-leveling modified ceramic liquid filling material with high thermal conductivity according to claim 1, is characterized in that comprising the following steps:
    1)陶瓷填料粉体改性：将不同粒径配比的陶瓷填料1000份加入高速分散机中，分散速度为1500～4000rmp，高剪切下通过雾化喷撒方式将陶瓷粉料处理剂溶液0.01-10份分散在陶瓷填料上，充分混合处理5～10min，然后100℃～130℃处理20min，得到改性陶瓷填料粉，备用；1) Modification of ceramic filler powder: Add 1000 parts of ceramic filler with different particle size ratios into a high-speed disperser, the dispersion speed is 1500-4000rmp, and the ceramic powder treatment agent solution is sprayed by atomization under high shear. 0.01-10 parts are dispersed on the ceramic filler, fully mixed for 5 to 10 minutes, and then treated at 100°C to 130°C for 20 minutes to obtain modified ceramic filler powder for use;
    2)A组分：在行星机中加入粘度为50mPa·S的乙烯基硅油和陶瓷粉料处理剂0.01～10份混合均匀后，加入改性陶瓷填料粉1000～2500份，物料在室温下混合30min，升温至物料温度140℃加热混炼2h后于真空度大于0.095Mpa下脱低1h，降温至室温后加入铂金催化剂0.01～5份，其中乙烯基硅油、陶瓷粉料处理剂和铂金催化剂总量为100份；2) Component A: Add 0.01-10 parts of vinyl silicone oil with a viscosity of 50mPa·S and 0.01-10 parts of ceramic powder treatment agent to the planetary machine, and then add 1,000-2,500 parts of modified ceramic filler powder, and mix the materials at room temperature 30min, heat up to the material temperature of 140°C, heat and mix for 2h, lower the temperature for 1h under a vacuum degree greater than 0.095Mpa, cool down to room temperature and add 0.01 to 5 parts of platinum catalyst, of which vinyl silicone oil, ceramic powder treatment agent and platinum catalyst are combined. The amount is 100 servings;
    B组分：在行星机中加入粘度为50mPa·S的乙烯基硅油和陶瓷粉料处理剂0.01～10份混合均匀后，加入改性陶瓷填料粉1000～2500份，物料在室温下混合30min，升温至物料温度140℃加热混炼2h后于真空度大于0.095Mpa下脱低1h，降温至室温后加入1～50份含氢硅油，0.001～5份抑制剂，其中乙烯基硅 油、含氢硅油、陶瓷粉料处理剂和抑制剂总量为100份；Component B: Add 0.01-10 parts of vinyl silicone oil with a viscosity of 50mPa·S and 0.01-10 parts of ceramic powder treatment agent to the planetary machine, and then add 1,000-2,500 parts of modified ceramic filler powder, and mix the materials at room temperature for 30 minutes. The temperature was raised to the material temperature of 140°C, heated and kneaded for 2 hours, and then lowered for 1 hour at a vacuum degree greater than 0.095Mpa. After cooling to room temperature, 1-50 parts of hydrogen-containing silicone oil and 0.001-5 parts of inhibitors were added, among which vinyl silicone oil and hydrogen-containing silicone oil were added. , The total amount of ceramic powder treatment agent and inhibitor is 100 parts;
    使用时，将A组分和B组分按1:1点胶混合室温快速硫化成高柔性橡胶弹性体。When in use, component A and component B are mixed in a 1:1 dispensing ratio and rapidly vulcanized at room temperature to form a highly flexible rubber elastomer.
PCT/CN2020/131364 2020-09-21 2020-11-25 High-thermal-conductivity self-leveling modified ceramic liquid potting material and preparation method therefor WO2022057083A1 (en)

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