CN104877612A - Heat-conducting insulating adhesive and preparation method thereof - Google Patents

Abstract

The invention discloses a thermally conductive and insulating adhesive and a preparation method thereof. The thermally conductive and insulating adhesive is composed of component A and component B; the raw material composition and mass percentage of component A are: amino silicone oil 5% to 20%, silane Coupling agent 2%~8%, epoxy resin 40%~70%, thermal conductive filler 20%~40%, the total percentage of the above raw materials is 100%; B component is curing agent; A component and B group The mass ratio of points is 1～4:1. The thermally conductive and insulating adhesive of the present invention has a longer pot life, higher thermal conductivity and volume resistivity, and is especially suitable for insulating and thermally conductive packaging and bonding in the fields of electronics and electrics.

Description

A kind of heat-conducting insulating adhesive and preparation method thereof

technical field

The invention relates to an adhesive and a preparation method thereof, in particular to an adhesive with heat conduction and insulation properties and a preparation method thereof.

Background technique

With the continuous update and development of integration technology and assembly technology in the electronics industry, the volume of electronic components and logic circuits tends to be miniaturized, but the operating frequency increases sharply. At this time, the heat generated by electronic equipment accumulates rapidly. In order to ensure the normal operation of electronic components with high reliability for a long time, higher and higher requirements are put forward for the thermal conductivity and insulation performance of the bonding adhesive.

Epoxy resin is a polymer matrix commonly used as heat-conducting and insulating adhesives. It has excellent physical and mechanical properties, electrical insulation properties and bonding properties. product, so the shrinkage rate is low. While epoxy resin has many excellent properties, it still has its shortcomings, such as large internal stress after curing, brittle quality, poor heat resistance, impact resistance and heat and humidity resistance, etc. Its application in the high-tech field.

At the same time, the thermal conductivity of the resin is low. To significantly improve the thermal conductivity of the adhesive, the main way is to fill the polymer with thermally conductive components. For example, the patent CN 102719210 A introduces an ultra-low temperature insulating thermally conductive adhesive. The thermally conductive filler is made of metal powder and non Composed of metal heat-conducting powder, the prepared heat-conducting and insulating adhesive has good electrical insulation, but the heat conductivity does not exceed 1W/m·k. Although the existing methods can prepare materials with high thermal conductivity, the materials are not insulating.

Therefore, how to effectively improve the toughness of the epoxy resin and at the same time improve the thermal conductivity and insulation performance of the adhesive is very important for the research and development of thermal conductivity and insulation adhesives with good performance.

Contents of the invention

The purpose of the present invention is to overcome the deficiencies of the prior art, to provide a thermally conductive and insulating adhesive with high thermal conductivity and excellent electrical insulation performance, the thermally conductive and insulating adhesive is composed of A component and B component, and the A component is composed of The mass percentage is composed of 5% to 20% of amino silicone oil, 2% to 8% of silane coupling agent, 40% to 70% of epoxy resin and 20% to 40% of thermally conductive filler. The sum of the above compositions is 100%; B component is curing agent.

The mass ratio of the A component to the B component is 1-4:1.

The amino silicone oil is polydimethylsiloxane containing amino groups in side chains or end groups, the amino group value is 0.5-0.8g/100g, and its structure conforms to the following general formula:

Wherein R ₁ is methyl or hydroxyl, R ₂ is aminoalkyl or R ₁ is aminoalkyl, R ₂ is methyl.

The silane coupling agent is 3-aminopropyltriethoxysilane, 3-glycidyloxypropyltrimethoxysilane, 3-aminopropyltrimethoxysilane, aminophenyltriethoxysilane One or more mixtures of siloxanes.

The epoxy resin is one or a mixture of bisphenol A type epoxy resin and glycidyl ester type epoxy resin.

The thermally conductive filler is one or a combination of boron nitride, aluminum nitride, silicon carbide, aluminum oxide, and carbon fiber, and the particle size of the thermally conductive filler is 0.05 μm to 200 μm.

The curing agent is one or a mixture of modified amine curing agent and modified alicyclic amine curing agent.

Another object of the present invention is to provide a method for preparing a thermally conductive and insulating adhesive, which is characterized in that it comprises the following steps:

(1) Pour 50ml~60ml of absolute ethanol into a 100ml beaker, add glacial acetic acid to adjust the pH of the system to 4~6, add 20%~40% thermally conductive filler with a particle size of 0.05μm~200μm and 0~1 % coupling agent, and adjust the temperature at 50°C to 60°C, stir for 20min to 30min, put it in an ultrasonic cleaner for ultrasonic dispersion for 40min to 50min, and hydrolyze at a constant temperature for 1h to 1.5h, filter, and wash with deionized water until Neutral, put the surface-modified thermally conductive filler into a vacuum drying oven at 40° C. to 60° C. and dry for 12 hours to obtain the surface-treated thermally conductive filler.

(2) Mix 5%-20% amino silicone oil and 2%-8% silane coupling agent in a beaker, stir and react at a temperature of 60°C-80°C for 4h-6h, then add 40% to the beaker % to 70% epoxy resin, stirred for 2h to 2.5h to obtain a modified epoxy resin, added the above-mentioned surface-treated thermally conductive filler to the modified epoxy resin, and stirred at room temperature for 20min to 30min to obtain component A .

(3) Compounding component A and component B in a mass ratio of 1 to 4:1 to obtain a thermally conductive and insulating adhesive.

The excellent effect of the present invention is:

The use of A and B two-component thermally conductive and insulating adhesives greatly prolongs the pot life, and the use of amino silicone oil modified epoxy resin improves the shortcomings of traditional thermally conductive adhesives such as poor toughness and poor heat resistance, and at the same time adds surface-treated thermally conductive fillers, The prepared thermally conductive and insulating adhesive has excellent electrical insulation and high thermal conductivity. The heat-conducting and insulating adhesive of the invention has simple preparation process, low cost and high application value.

Detailed ways

The present invention will be further described below in conjunction with the examples, but the embodiments of the present invention are not limited thereto.

Example 1

(1) Pour 50ml of absolute ethanol into a 100ml beaker, add glacial acetic acid to adjust the pH of the system to be 4, add 8g of boron nitride and 0.15g of 3-aminopropyltriethoxysilane with a particle diameter of 50nm under stirring, and Adjust the temperature at 50°C, stir for 20 minutes, put it in an ultrasonic cleaner for ultrasonic dispersion for 40 minutes, and hydrolyze it at a constant temperature for 1 hour. After filtering, wash it with deionized water until it is neutral, and put the surface-modified thermally conductive filler in a vacuum drying oven Dry at 40°C for 12 hours to obtain a surface-treated thermally conductive filler.

(2) Weigh 4g of amino silicone oil and 2g of 3-aminopropyltriethoxysilane in a beaker, stir and react at a temperature of 60°C for 4h, then add 24g of bisphenol A epoxy resin, stir for 2h, and obtain the improved Add the above-mentioned surface-treated thermally conductive filler to the modified epoxy resin, and stir at room temperature for 20 minutes to obtain component A.

(3) Mix 35g of component A with 12g of modified amine curing agent (component B) to obtain a thermally conductive and insulating adhesive.

Example 2

(1) Pour 50ml of absolute ethanol into a 100ml beaker, add glacial acetic acid to adjust the pH of the system to 5, add 8g of aluminum nitride with a particle size of 50nm and 0.2g of 3-aminopropyltriethoxysilane under stirring, And adjust the temperature at 50°C, stir for 20 minutes, put it in an ultrasonic cleaner for ultrasonic dispersion for 40 minutes, and hydrolyze it at a constant temperature for 1 hour, filter it, wash it with deionized water until it is neutral, and put the surface-modified thermally conductive filler into a vacuum drying oven Dry at 40° C. for 12 hours to obtain a thermally conductive filler after surface treatment.

(2) Weigh 4g of amino silicone oil and 2g of 3-aminopropyltriethoxysilane in a beaker, stir and react at a temperature of 60°C for 4h, then add 24g of bisphenol A epoxy resin, stir for 2h, and obtain the improved Add the above-mentioned surface-treated thermally conductive filler to the modified epoxy resin, and stir at room temperature for 20 minutes to obtain component A.

(3) Mix 36g of component A with 12g of modified amine curing agent (component B) to obtain a thermally conductive and insulating adhesive.

Example 3

(1) Pour 50ml of absolute ethanol into a 100ml beaker, add glacial acetic acid to adjust the pH of the system to 6, add 8g of silicon carbide with a particle size of 50nm and 0.25g of 3-aminopropyltriethoxysilane under stirring, and adjust After stirring for 20 minutes at a temperature of 50°C, put it in an ultrasonic cleaner for ultrasonic dispersion for 45 minutes, and hydrolyze it at a constant temperature for 1.5 hours. Dry at 40°C for 12 hours to obtain a surface-treated thermally conductive filler.

(2) Weigh 4g of amino silicone oil and 2g of 3-aminopropyltriethoxysilane in a beaker, stir and react at a temperature of 60°C for 4h, then add 24g of bisphenol A epoxy resin, stir for 2h, and obtain the improved Put the thermally conductive filler after the above surface treatment into the modified epoxy resin, and stir at room temperature for 20 minutes to obtain component A.

(3) Mix 36g of component A with 12g of modified amine curing agent (component B) to obtain a thermally conductive and insulating adhesive.

Example 4

(1) Pour 50ml of absolute ethanol into a 100ml beaker, add glacial acetic acid to adjust the pH of the system to 5, add 8g of alumina and 0.25g of 3-aminopropyltriethoxysilane with a particle size of 50nm under stirring, and adjust After stirring for 20 minutes at a temperature of 60°C, put it in an ultrasonic cleaner for ultrasonic dispersion for 40 minutes, and hydrolyze it at a constant temperature for 1 hour. After filtering, wash it with deionized water until it is neutral. °C for 12 hours to obtain a surface-treated thermally conductive filler.

(2) Weigh 4g of amino silicone oil and 2g of 3-aminopropyltriethoxysilane in a beaker, stir and react at a temperature of 60°C for 4h, then add 24g of bisphenol A epoxy resin, stir for 2h, and obtain the improved Add the above-mentioned surface-treated thermally conductive filler to the modified epoxy resin, and stir at room temperature for 20 minutes to obtain component A.

(3) Mix 37g of component A with 12g of modified amine curing agent (component B) to obtain a thermally conductive and insulating adhesive.

Example 5

(1) Pour 60ml of absolute ethanol into a 100ml beaker, add glacial acetic acid to adjust the pH of the system to 5, add 8g of boron nitride with a particle size of 50nm, 2g of carbon fiber and 0.3 of 3-aminopropyltriethoxysilane under stirring. g, and adjust the temperature at 60°C, stir for 30 minutes, put it in an ultrasonic cleaner for ultrasonic dispersion for 40 minutes, and hydrolyze it at a constant temperature for 1.5 hours, after filtering, wash it with deionized water until it is neutral, and put the surface-modified thermally conductive filler into a vacuum Dry in a drying oven at 50° C. for 12 hours to obtain a surface-treated thermally conductive filler.

(2) Weigh 4g of amino silicone oil and 1g of 3-aminopropyltriethoxysilane in a beaker, stir and react at a temperature of 60°C for 4h, then add 20g of bisphenol A epoxy resin, stir for 2h, and obtain the improved Add the above-mentioned surface-treated thermally conductive filler to the modified epoxy resin, and stir at room temperature for 20 minutes to obtain component A.

(3) Mix 33g of component A with 15g of modified amine curing agent (component B) to obtain a thermally conductive and insulating adhesive.

Example 6

(1) Pour 60ml of absolute ethanol into a 100ml beaker, add glacial acetic acid to adjust the pH of the system to 5, and add 6g of boron nitride with a particle size of 50nm, 2g of carbon fiber, 2g of spherical alumina and 3-aminopropyl tris Ethoxysilane 0.3g, and adjust the temperature at 60°C, stir for 30min, put it in an ultrasonic cleaner for ultrasonic dispersion for 50min, and hydrolyze at a constant temperature for 1h, filter, wash with deionized water until neutral, and heat-conduct the surface-modified The filler was put into a vacuum drying oven at 50°C and dried for 12 hours to obtain a thermally conductive filler after surface treatment.

(2) Weigh 3g of amino silicone oil and 1g of 3-aminopropyltriethoxysilane in a beaker, stir and react at a temperature of 60°C for 4h, then add 21g of bisphenol A epoxy resin, stir for 2h, and obtain the improved Add the above-mentioned surface-treated thermally conductive filler to the modified epoxy resin, and stir at room temperature for 20 minutes to obtain component A.

(3) Mix 33g of component A with 15g of modified amine curing agent (component B) to obtain a thermally conductive and insulating adhesive.

Example 7

(1) Pour 60ml of absolute ethanol into a 100ml beaker, add glacial acetic acid to adjust the pH of the system to 6, add 6g of spherical alumina with a particle size of 50μm, 2g of silicon carbide, 2g of carbon fiber and 3-aminopropyltriethyl Oxysilane 0.35g, and adjust the temperature to 50°C, after stirring for 25min, put it in an ultrasonic cleaner for ultrasonic dispersion for 45min, and hydrolyze at a constant temperature for 1.5h, after filtering, wash with deionized water until neutral, the surface modified heat conduction The filler was put into a vacuum drying oven and dried at 50° C. for 12 hours to obtain a thermally conductive filler after surface treatment.

(2) Weigh 4g of amino silicone oil and 1g of 3-aminopropyltriethoxysilane in a beaker, stir and react at a temperature of 60°C for 4h, then add 20g of bisphenol A epoxy resin, stir for 2h, and obtain the improved Add the above-mentioned surface-treated thermally conductive filler to the modified epoxy resin, and stir at room temperature for 20 minutes to obtain component A.

(3) Mix 33g of component A with 15g of modified amine curing agent (component B) to obtain a thermally conductive and insulating adhesive.

Example 8

(1) Pour 60ml of absolute ethanol into a 100ml beaker, add glacial acetic acid to adjust the pH of the system to 6, add 6g of boron nitride with a particle size of 50μm, 2g of carbon fiber and 3-glycidyloxypropyl trimethoxy 0.25g of base silane, and adjust the temperature to 50°C, stir for 25min, put it in an ultrasonic cleaner for ultrasonic dispersion for 40min, and hydrolyze at a constant temperature for 1h, filter, wash with deionized water until neutral, put the surface-modified thermally conductive filler Dry in a vacuum drying oven at 45° C. for 12 hours to obtain a surface-treated thermally conductive filler.

(2) Weigh 5g of amino silicone oil and 1g of 3-glycidyl etheroxypropyl trimethoxysilane in a beaker, stir and react at a temperature of 65°C for 4h, then add 20g of glycidyl ester epoxy resin, and stir for 2h , to obtain a modified epoxy resin, add the above-mentioned surface-treated thermally conductive filler into the modified epoxy resin, and stir at room temperature for 20 minutes to obtain component A.

(3) Mix 32g of component A with 16g of modified amine curing agent (component B) to obtain a thermally conductive and insulating adhesive.

Example 9

(1) Pour 60ml of absolute ethanol into a 100ml beaker, add glacial acetic acid to adjust the pH of the system to 6, add 6g of boron nitride with a particle size of 100μm, 2g of carbon fiber and 3-glycidyl etheroxypropyl trimethoxy 0.25g of base silane, and adjust the temperature to 45°C. After stirring for 25min, put it in an ultrasonic cleaner for ultrasonic dispersion for 40min, and hydrolyze it at a constant temperature for 1h. After filtering, wash it with deionized water until it is neutral. Dry in a vacuum drying oven at 40° C. for 12 hours to obtain a surface-treated thermally conductive filler.

(2) Weigh 5g of amino silicone oil and 2g of 3-glycidyl etheroxypropyl trimethoxysilane in a beaker, stir and react at a temperature of 70°C for 4h, then add 20g of glycidyl ester epoxy resin, and stir for 2h , to obtain a modified epoxy resin, add the above-mentioned surface-treated thermally conductive filler into the modified epoxy resin, and stir at room temperature for 20 minutes to obtain component A.

(3) Mix 32g of component A with 17g of modified amine curing agent (component B) to obtain a thermally conductive and insulating adhesive.

Example 10

(1) Pour 60ml of absolute ethanol into a 100ml beaker, add glacial acetic acid to adjust the pH of the system to 5, add 10g of boron nitride with a particle size of 100μm, 2g of carbon fiber and 3-glycidyloxypropyl trimethoxy Base silane 0.3g, and adjust the temperature to 55°C, stir for 25min, put it in an ultrasonic cleaner for ultrasonic dispersion for 40min, and hydrolyze at a constant temperature for 1.5h, filter, wash with deionized water until neutral, and put the surface-modified thermally conductive filler Put it into a vacuum oven and dry at 40° C. for 12 hours to obtain a surface-treated thermally conductive filler.

(2) Weigh 6 g of amino silicone oil and 1 g of 3-glycidyl etheroxypropyl trimethoxysilane in a beaker, stir and react at a temperature of 65 ° C for 4 h, then add 20 g of glycidyl ester type epoxy resin, and stir for 2.5 h, to obtain a modified epoxy resin, add the above-mentioned surface-treated thermally conductive filler into the modified epoxy resin, and stir at room temperature for 20 minutes to obtain component A.

(3) Mix 38g of component A with 11g of modified amine curing agent (component B) to obtain a thermally conductive and insulating adhesive.

Example 11

(1) Pour 60ml of absolute ethanol into a 100ml beaker, add glacial acetic acid to adjust the pH of the system to 5, add 10g of boron nitride with a particle size of 50nm, 2g of carbon fiber and 0.3g of 3-aminopropyltrimethoxysilane under stirring , and adjust the temperature to 50°C, stir for 20 minutes, put it into an ultrasonic cleaner for ultrasonic dispersion for 40 minutes, and hydrolyze it at a constant temperature for 1 hour, after filtering, wash it with deionized water until neutral, and put the surface-modified thermally conductive filler into a vacuum drying oven Dry at 40°C for 12 hours to obtain a surface-treated thermally conductive filler.

(2) Weigh 4g of amino silicone oil and 1g of 3-aminopropyltrimethoxysilane in a beaker, stir and react at 60°C for 4h, then add 20g of glycidyl ester type epoxy resin, stir for 2h to obtain modified For epoxy resin, add the thermally conductive filler after the above surface treatment into the modified epoxy resin, and stir at room temperature for 30 minutes to obtain component A.

(3) Mix 35g of component A with 13g of modified alicyclic amine curing agent (component B) to obtain a thermally conductive and insulating adhesive.

Example 12

(1) Pour 60ml of absolute ethanol into a 100ml beaker, add glacial acetic acid to adjust the pH of the system to 5, add 10g of boron nitride with a particle size of 50nm, 2g of carbon fiber and 0.2g of 3-aminopropyltrimethoxysilane under stirring , and adjust the temperature to 60°C, stir for 30 minutes, put it in an ultrasonic cleaner for ultrasonic dispersion for 50 minutes, and hydrolyze it at a constant temperature for 1.5 hours, after filtering, wash it with deionized water until it is neutral, and put the surface-modified thermal conductive filler into vacuum drying Dry in a box at 40°C for 12 hours to obtain a surface-treated thermally conductive filler.

(2) Weigh 4g of amino silicone oil and 2g of 3-aminopropyltrimethoxysilane in a beaker, stir and react at a temperature of 60°C for 4h, then add 18g of bisphenol A epoxy resin, stir for 2.5h, and obtain the modified Add the above-mentioned surface-treated thermally conductive filler to the modified epoxy resin, and stir at room temperature for 20 minutes to obtain component A.

(3) Mix 33g of component A with 14g of modified alicyclic amine curing agent (component B) to obtain a thermally conductive and insulating adhesive.

Example 13

(1) Pour 60ml of absolute ethanol into a 100ml beaker, add glacial acetic acid to adjust the pH of the system to 5, add 8g of aluminum nitride with a particle size of 100μm, 2g of carbon fiber and 0.25g of aminophenyltriethoxysiloxane under stirring , and adjust the temperature to 60°C, stir for 30 minutes, put it in an ultrasonic cleaner for ultrasonic dispersion for 40 minutes, and hydrolyze it at a constant temperature for 1 hour, after filtering, wash it with deionized water until it is neutral, and put the surface-modified thermally conductive filler into a vacuum drying oven Dry at 40°C for 12 hours to obtain a surface-treated thermally conductive filler.

(2) Weigh 4g of amino silicone oil and 1g of aminophenyltriethoxysiloxane in a beaker, stir and react at 60°C for 4h, then add 19g of bisphenol A epoxy resin, stir for 2.5h to obtain To modify the epoxy resin, add the thermally conductive filler after the above surface treatment into the modified epoxy resin, and stir at room temperature for 20 minutes to obtain component A.

(3) Mix 32g of component A with 16g of modified alicyclic amine curing agent (component B) to obtain a thermally conductive and insulating adhesive.

Example 14

(1) Pour 60ml of absolute ethanol into a 100ml beaker, add glacial acetic acid to adjust the pH of the system to 5, add 10g of boron nitride with a particle size of 50nm, 2g of carbon fiber and 0.15 of aminophenyltriethoxysiloxane under stirring. g, and adjust the temperature to 55°C, stir for 20 minutes, put it into an ultrasonic cleaner for ultrasonic dispersion for 40 minutes, and hydrolyze it at a constant temperature for 1 hour, after filtering, wash it with deionized water until it is neutral, and put the surface-modified thermal conductive filler into vacuum drying Dry in an oven at 40° C. for 12 hours to obtain a surface-treated thermally conductive filler.

(2) Weigh 5g of amino silicone oil and 2g of aminophenyltriethoxysiloxane in a beaker, stir and react at 60°C for 4h, then add 18g of glycidyl ester type epoxy resin, stir for 2h, and obtain the modified Add the above-mentioned surface-treated thermally conductive filler to the modified epoxy resin, and stir at room temperature for 20 minutes to obtain component A.

(3) Mix 35g of component A with 18g of modified alicyclic amine curing agent (component B) to obtain a thermally conductive and insulating adhesive.

Example 15

(1) Pour 60ml of absolute ethanol into a 100ml beaker, add glacial acetic acid to adjust the pH of the system to 5, add 10g of boron nitride with a particle size of 50nm, 2g of carbon fiber and 3-glycidyl etheroxypropyl trimethoxy 0.1g of 3-aminopropyltrimethoxysilane, 0.1g of 3-aminopropyltrimethoxysilane, and adjust the temperature at 50°C. After stirring for 20 minutes, put it in an ultrasonic cleaner for ultrasonic dispersion for 40 minutes, and hydrolyze it at constant temperature for 1.5 hours. After filtering, use deionized water Wash until neutral, put the surface-modified thermally conductive filler into a vacuum drying oven and dry at 40° C. for 12 hours to obtain a surface-treated thermally conductive filler.

(2) Weigh 4g of amino silicone oil, 1g of 3-glycidyloxypropyltrimethoxysilane, and 1g of 3-aminopropyltrimethoxysilane in a beaker, stir and react at 60°C for 4.5h, then add 20g of bisphenol A epoxy resin was stirred and reacted for 2.5 hours to obtain a modified epoxy resin. The above-mentioned surface-treated thermally conductive filler was added to the modified epoxy resin and stirred at room temperature for 30 minutes to obtain component A.

(3) Mix 35g of component A with 10g of modified amine curing agent and 10g of modified alicyclic amine curing agent (component B) to obtain a thermally conductive and insulating adhesive.

Example 16

(1) Pour 60ml of absolute ethanol into a 100ml beaker, add glacial acetic acid to adjust the pH of the system to 5, add 10g of boron nitride with a particle size of 50nm, 2g of carbon fiber and 3-glycidyl etheroxypropyl trimethoxy 0.1g of 3-aminopropyltriethoxysilane and 0.15g of 3-aminopropyltriethoxysilane, and adjust the temperature at 60°C. After stirring for 20 minutes, put it in an ultrasonic cleaner for ultrasonic dispersion for 40 minutes, and hydrolyze it at constant temperature for 1 hour. After filtering, use deionized water Wash until neutral, put the surface-modified thermally conductive filler into a vacuum drying oven at 50° C. and dry for 12 hours to obtain the surface-treated thermally conductive filler.

(2) Weigh 5g of amino silicone oil, 0.5g of 3-glycidyloxypropyltrimethoxysilane, and 0.5g of 3-aminopropyltriethoxysilane in a beaker, and stir the reaction at a temperature of 60°C for 4.5 Add 10g bisphenol A type epoxy resin and 10g glycidyl ester type epoxy resin after h, stir and react for 2.5h, obtain modified epoxy resin, the thermally conductive filler after the above-mentioned surface treatment is joined in modified epoxy resin, Stir at room temperature for 20 min to obtain component A.

(3) Mix 33g of component A with 11g of modified amine curing agent and 11g of modified alicyclic amine curing agent (component B) to obtain a thermally conductive and insulating adhesive.

Example 17

(1) Pour 60ml of absolute ethanol into a 100ml beaker, add glacial acetic acid to adjust the pH of the system to 5, add 10g of boron nitride with a particle size of 50nm, 2g of carbon fiber and 3-glycidyl etheroxypropyl trimethoxy 0.3g of base silane, and adjust the temperature at 60°C, stir for 20min, put it in an ultrasonic cleaner for ultrasonic dispersion for 40min, and hydrolyze it at a constant temperature for 1h, filter it, wash it with deionized water until neutral, put the surface-modified thermally conductive Dry in a vacuum drying oven at 40° C. for 12 hours to obtain a surface-treated thermally conductive filler.

(2) Weigh 5g of amino silicone oil, 0.5g of 3-glycidyloxypropyltrimethoxysilane, and 0.5g of aminophenyltriethoxysiloxane in a beaker, and stir the reaction at a temperature of 60°C for 4.5 Add 10g bisphenol A type epoxy resin and 8g glycidyl ester type epoxy resin after h, stir and react for 2.5h, obtain modified epoxy resin, the thermally conductive filler after the above-mentioned surface treatment is joined in modified epoxy resin, Stir at room temperature for 20 min to obtain component A.

(3) Mix 30g of component A with 12g of modified amine curing agent and 11g of modified alicyclic amine curing agent (component B) to obtain a thermally conductive and insulating adhesive.

Example 18

(1) Pour 60ml of absolute ethanol into a 100ml beaker, add glacial acetic acid to adjust the pH of the system to 5, add 10g of boron nitride with a particle size of 50nm, 2g of carbon fiber and 0.3g of 3-aminopropyltrimethoxysilane under stirring , and adjust the temperature to 60°C, stir for 30 minutes, put it in an ultrasonic cleaner for ultrasonic dispersion for 40 minutes, and hydrolyze it at a constant temperature for 1 hour, after filtering, wash it with deionized water until it is neutral, and put the surface-modified thermally conductive filler into a vacuum drying oven Dry at 40°C for 12 hours to obtain a surface-treated thermally conductive filler.

(2) Weigh 5g of amino silicone oil, 0.5g of 3-glycidyloxypropyltrimethoxysilane, and 0.5g of 3-aminopropyltrimethoxysilane in a beaker, and stir and react at a temperature of 60°C for 4.5h Finally, add 10g of bisphenol A type epoxy resin and 8g of glycidyl ester type epoxy resin, stir and react for 2.5h to obtain a modified epoxy resin, add the thermally conductive filler after the above surface treatment into the modified epoxy resin, and heat at room temperature Stir for 20min to obtain component A.

(3) Mix 30g of component A with 13g of modified amine curing agent and 13g of modified alicyclic amine curing agent (component B) to obtain a thermally conductive and insulating adhesive.

Fully mix the components A and B in the above specific examples, place them in a vacuum drying oven for 30 minutes of vacuum degassing, and pour them into a preheated mold coated with a release agent (diameter 50mm, thickness 3mm) Inside, bake in a vacuum oven at 90°C for 1 hour to obtain a molded thermally conductive insulating material. The thermal conductivity and insulation properties of the material were tested, and the specific test results are shown in Table 1.

Table 1 Properties of thermally conductive and insulating adhesives

Example Thermal conductivity (W/m·k) Volume resistivity (Ω·cm) Dielectric strength (kV/mm) 1 1.4 1.6×10 ¹⁵ 18 2 1.2 1.7×10 ¹⁵ 19 3 1.1 1.8×10 ¹⁵ 17 4 1.1 2.0×10 ¹⁵ twenty one 5 1.6 1.5×10 ¹⁵ twenty two 6 1.9 1.6×10 ¹⁵ twenty one 7 1.5 1.8×10 ¹⁵ 19 8 1.7 1.7×10 ¹⁵ 16 9 1.5 1.9×10 ¹⁵ 18 10 1.2 2.1×10 ¹⁵ 20 11 1.8 2.2×10 ¹⁵ twenty two 12 1.6 1.9×10 ¹⁵ 19 13 1.7 1.7×10 ¹⁵ 17 14 2.0 2.1×10 ¹⁵ 20 15 1.7 2.3×10 ¹⁵ twenty two 16 2.2 2.0×10 ¹⁵ twenty one 17 1.9 2.4×10 ¹⁵ twenty three 18 1.6 2.2×10 ¹⁵ twenty two

Claims (8)

1. a Heat Conductive Insulation Adhesive, it is characterized in that, be made up of component A and B component, described component A by mass percentage be 5% ~ 20% amido silicon oil, the silane coupling agent of 2% ~ 8%, the epoxy resin of 40% ~ 70% and 20% ~ 40% heat conductive filler form, the summation of above-mentioned composition is 100%; B component is solidifying agent.

2. a kind of Heat Conductive Insulation Adhesive according to claim 1, is characterized in that, described component A and the mass ratio of B component are 1 ~ 4: 1.

3. a kind of Heat Conductive Insulation Adhesive according to claim 1, is characterized in that, described amido silicon oil is containing amino polydimethylsiloxane in side chain or end group, and amino value is 0.5 ~ 0.8g/100g, and its structure meets following general formula:

Wherein R ₁for methyl or hydroxyl, R ₂for ammonia alkyl or R ₁for ammonia alkyl, R ₂for methyl.

4. a kind of Heat Conductive Insulation Adhesive according to claim 1, it is characterized in that, described silane coupling agent is one or more mixing in 3-aminopropyl triethoxysilane, 3-glycydoxy Trimethoxy silane, 3-aminopropyl trimethoxysilane, aminophenyl triethoxy silica alkane.

5. a kind of Heat Conductive Insulation Adhesive according to claim 1, is characterized in that, described epoxy resin is one or both mixing in bisphenol A type epoxy resin, glycidyl ester type epoxy resin.

6. a kind of Heat Conductive Insulation Adhesive according to claim 1, it is characterized in that, described heat conductive filler is one or more mixing in boron nitride, aluminium nitride, silicon carbide, aluminum oxide, carbon fiber, and the particle diameter of described heat conductive filler is 0.05 μm ~ 200 μm.

7. a kind of Heat Conductive Insulation Adhesive according to claim 1, is characterized in that, described solidifying agent is one or both mixing in modified amine curing agent, modification aliphatic cyclic amine solidifying agent.

8. a preparation method for Heat Conductive Insulation Adhesive, is characterized in that, described preparation method carries out according to the following steps:

(1) 50ml ~ 60ml dehydrated alcohol is poured in 100ml beaker, adding Glacial acetic acid regulation system pH is 4 ~ 6, the heat conductive filler of 20% ~ 40% and the silane coupling agent of 0 ~ 1% that particle diameter is 0.05 μm ~ 200 μm is added under stirring, and regulate temperature 50 C ~ 60 DEG C, after stirring 20min ~ 30min, put into ultrasonic cleaner ultrasonic disperse 40min ~ 50min, and constant temperature hydrolysis 1h ~ 1.5h, after filtration, with deionized water wash to neutral, the heat conductive filler of finishing is put into vacuum drying oven in 40 DEG C ~ 60 DEG C dry 12h, obtain the heat conductive filler after surface treatment.

(2) amido silicon oil of 5% ~ 20% is mixed with 1% ~ 8% silane coupling agent be placed in beaker, stirring reaction 4h ~ 6h at temperature is 60 DEG C ~ 80 DEG C, the epoxy resin of 40% ~ 70% is added again in beaker, stirring reaction 2h ~ 2.5h, obtain modified epoxy, join in modified epoxy by the heat conductive filler after above-mentioned surface treatment, stirring at room temperature 20min ~ 30min, obtains component A.

(3) ratio being 1 ~ 4: 1 in mass ratio by component A and B component coordinates, and namely obtains described Heat Conductive Insulation Adhesive.