High-performance heat-conducting silicone potting adhesive and preparation method thereof

By combining spherical and non-spherical alumina powders and treating with vinyl silicone oil, a low-viscosity, high-thermal-conductivity potting compound was prepared. This solved the problem of insufficient adhesion and thermal conductivity of addition-cure silicone rubber in small gaps and large-size devices, and improved the flowability and stability of the potting compound.

CN119799275BActive Publication Date: 2026-02-06YANTAI DARBOND TECH
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Patent Information

Application Number
CN202411972994.3
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2024-12-30
Publication Date
2026-02-06
Estimated Expiration
2044-12-30

AI Technical Summary

Technical Problem

Existing addition-cure silicone rubbers have weak adhesion when cured at room temperature or low temperature, making it difficult to ensure thermal conductivity and adhesion when potting in small gaps, and they are not adaptable to the deformation of large-sized devices.

Method used

By combining spherical and non-spherical alumina powders with vinyl silicone oil and hydrogen-containing silicone oil, and using DB06 filler surface treatment agent and platinum catalyst, the catalyst concentration and binder type are adjusted to prepare a low-viscosity, high-thermal-conductivity, and low-modulus potting compound. The thermally conductive filler is treated by vacuum dispersion and mixing to ensure uniform dispersion.

Benefits of technology

It achieves good filling in small gaps while improving thermal conductivity and adhesion, enhancing the stability and lifespan of electronic components, and reducing the risk of settling.

✦ Generated by Eureka AI based on patent content.

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Abstract

The application provides a high-performance heat-conducting silicone pouring sealant, which is composed of component A and component B in a weight ratio of 1:1, wherein the component A is composed of the following raw materials: 5-15 parts of vinyl silicone oil, 80-95 parts of heat-conductive filler, 1-5 parts of DB06 filler surface treatment agent and 0.1-1 part of platinum gold catalyst; and the component B is composed of the following raw materials: 2-10 parts of vinyl silicone oil, 2-7 parts of hydrogen-containing silicone oil, 80-95 parts of heat-conductive filler, 1-5 parts of DB06 filler surface treatment agent, 0.01-0.2 parts of inhibitor, 0.1-1 part of adhesive and 0.1-1 part of toning agent. The pouring sealant has low viscosity, which is beneficial to good filling and sealing of small gaps of devices; high heat conductivity, which is beneficial to heat dissipation of electronic components; good adhesion and high elongation at break, which ensure the working stability and reliability of electronic components and prolong the service life of electronic components.
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Description

[0001] The present application relates to a kind of organic silicon heat-conducting pouring sealant, especially a kind of low viscosity, high thermal conductivity, low modulus, high elongation two-component addition type organic silicon pouring sealant and its preparation method, can be applied to the pouring application of various electric components, especially suitable for less than 100 μm small gap pouring occasion. BACKGROUND

[0002] Silicone glue has excellent high and low temperature performance and electrical insulation performance, and is widely used in the pouring and bonding of electronic components. Especially addition type silicone rubber, because of the characteristics of no by-product produced in the curing process and low shrinkage, it is favored by the majority of users. At present, there are many manufacturers of addition type heat-conducting pouring silicone, and the thermal conductivity is 0.6-4 W / m·K, and the application scenarios are different, which can basically meet the use requirements of different customers. However, the adhesion of addition type silicone rubber is very low, especially at room temperature or low temperature curing, which basically has no adhesion to the base material; in addition, the pouring gap is very small in some application occasions, and the particle size of the heat-conducting filler and the viscosity of the pouring sealant need to be controlled under the premise of ensuring the heat-conducting requirement; some large size samples also have certain requirements on the elongation of the pouring sealant to cope with the influence of deformation. SUMMARY

[0003] The present application provides a preparation method of a low viscosity, high thermal conductivity, high elongation, small particle size and good adhesion organic silicon pouring silicone to achieve good flow performance during pouring, good heat-conducting performance and adhesion performance after curing, and high elongation at break, thereby improving the reliability and stability of electronic components and increasing the service life.

[0004] The technical scheme for solving the above technical problems is as follows: a high-performance heat-conducting organic silicon pouring sealant is composed of A component and B component in a weight ratio of 1:1, the A component is composed of the following raw materials: 5-15 parts of vinyl silicone oil, 80-95 parts of heat-conducting filler, 1-5 parts of DB06 filler surface treatment agent and 0.1-1 part of platinum catalyst; the B component is composed of the following raw materials: 2-10 parts of vinyl silicone oil, 2-7 parts of hydrogen-containing silicone oil, 80-95 parts of heat-conducting filler, 1-5 parts of DB06 filler surface treatment agent, 0.01-0.2 parts of inhibitor, 0.1-1 parts of adhesive and 0.1-1 parts of toning agent.

[0005] On the basis of the above technical scheme, the present application can also be improved as follows.

[0006] Further, the heat-conducting filler is alumina powder, which can be divided into spherical alumina and non-spherical alumina according to different particle shapes, and spherical alumina and non-spherical alumina are used in the present application, and the particle size of the alumina powder used is D99 ≤ 50 μm.

[0007] The beneficial effect of the above scheme is that the combination of spherical alumina and non-spherical alumina can effectively connect the heat conduction channels and improve the thermal conductivity of the potting adhesive, while reducing the risk of sedimentation during storage of the potting adhesive.

[0008] In addition, the method of using coarse and fine alumina is also adopted. Since there is a large space between the large particle size powders, especially between the large particle size spherical powders, the use of smaller particle size powders can effectively fill the space and has less effect on the viscosity, thereby improving the thermal conductivity of the potting adhesive while ensuring good flow performance.

[0009] Further, the viscosity of the vinyl silicone oil is in the range of 50-2000 mPa.s.

[0010] Further, the vinyl silicone oil is end vinyl silicone oil (linear type) and branched vinyl silicone oil, the structural formula of the end vinyl silicone oil is represented by the following general formula (I), and the structural formula of the branched vinyl silicone oil is represented by the following general formula (II):

[0011] CH2=CH-Si(CH3)2O[(CH3)2SiO] n (CH3)2Si-CH=CH2 (I); (CH3)3SiO[(CH3)2SiO] m [(CH2=CH)(CH3)SiO] p Si(CH3)3 (II); wherein, n=50-200, m+p=50-260.

[0012] Further, the hydrogen-containing silicone oil has a structural formula represented by the following general formula (III): R-Si(CH3)2-O-[SiHCH3-O] a -[Si-(CH3)2-O] b -Si(CH3)2-R (III), wherein R represents CH3 or H, and a+b=8-98.

[0013] Further, the DB06 filler surface treatment agent is a self-made long-chain siloxane, and the preparation method is as follows:

[0014] 405g of end hydrogen-containing silicone oil with a hydrogen content of 0.1% is added to a flask, 15g of vinyl trimethoxysilane and 0.1g of platinum gold catalyst (5000ppm) are fully mixed and uniformly mixed, the mixed liquid is added to the flask while stirring, and after the addition is completed, the reaction is carried out for 3h, and the temperature in the bottle is controlled at 90℃. 30g of 1-nonene is added and the reaction is continued for 2.5h, and then the low boiling point material is removed.

[0015] Further, the catalyst is a platinum gold catalyst, and the concentration of the platinum gold catalyst is 1000-5000ppm.

[0016] The beneficial effect of the above further scheme is that the curing speed of the pouring sealant can be effectively adjusted by adjusting the amount and concentration of the catalyst.

[0017] Further, the toner is carbon black.

[0018] The beneficial effect of the above further scheme is that the A and B components are mixed into different colors, and the uniformity of the mixture of the A and B components can be judged by color during the mixing of the sealant, which is convenient and simple to operate.

[0019] Further, the inhibitor is methyl butynol, ethynylcyclohexanol, maleate, etc., and the present application preferably uses ethynylcyclohexanol.

[0020] Further, the adhesion agent is γ-glycidoxypropyltrimethoxysilane, γ-glycidoxypropyltriethoxysilane, 2-(3,4-epoxycyclohexyl)ethyltrimethoxysilane, γ-methacryloyloxypropyltrimethoxysilane, γ-methacryloyloxypropyltriethoxysilane, vinyltrimethoxysilane, vinyltriisopropenoxysilane, etc., and the present application preferably uses γ-glycidoxypropyltrimethoxysilane and vinyltriisopropenoxysilane.

[0021] Another technical solution of the present application to solve the above technical problems is as follows: the preparation method comprises the following steps:

[0022] 1) 5-15 parts of vinyl silicone oil, 1-5 parts of DB06 filler surface treatment agent, and 80-95 parts of heat-conducting filler are sequentially added into a double-planetary dynamic mixing stirrer, and stirred under the conditions of a vacuum degree of -0.1 MPa, a dispersion speed of 600 rpm, and a revolution speed of 20 rpm, the temperature in the kettle is kept at 130°C, and after 2 hours of stirring and dispersion, the temperature is lowered to 40°C, 0.1-1 parts of platinum gold catalyst is added, and stirring is continued for 20 minutes to obtain a product ready for use.

[0023] 2) 2-10 parts of vinyl silicone oil, 2-7 parts of hydrogen-containing silicone oil, 1-5 parts of DB06 filler surface treatment agent, 80-95 parts of heat-conducting filler, and 0.1-1 parts of toner are sequentially added into a double-planetary dynamic mixing stirrer, and stirred under the conditions of a vacuum degree of -0.1 MPa, a dispersion speed of 600 rpm, and a revolution speed of 20 rpm, the temperature in the kettle is kept at 130°C, and after 2 hours of stirring and dispersion, the temperature is lowered to 40°C, 0.01-0.2 parts of inhibitor and 0.1-1 parts of adhesion agent are added, and stirring is continued for 20 minutes to obtain a product ready for use.

[0024] 3) When used, the A and B components are mixed uniformly at a weight ratio of 1:1, and cured at 100°C for 1 hour to obtain the product.

[0025] The application has the beneficial effects that the heat-conducting filler is dispersed more uniformly, the viscosity and thixotropy of the pouring and sealing glue are effectively reduced, and the anti-settling property of the filler is increased.

[0026] The application has the beneficial effects that the lower viscosity is beneficial to the flow of the pouring and sealing glue, the small gaps of the device can be well filled and sealed, the high thermal conductivity is beneficial to the heat dissipation of the electronic components, the good adhesion and high elongation at break ensure the working stability and reliability of the electronic components, and the service life of the electronic components is prolonged, and the two components with similar mass ratio are beneficial to the blending operation and the mixing is more uniform. DETAILED DESCRIPTION

[0027] The principles and features of the application are described below, and the examples are only used to explain the application and not to limit the scope of the application.

[0028] Example 1

[0029] 4 parts of vinyl silicone oil with a viscosity of 50 mPa.s, 1 part of vinyl silicone oil with a viscosity of 2000 mPa.s, 1 part of DB06 filler surface treatment agent, 40 parts of D50 20 μm spherical alumina powder, 30 parts of D50 10 μm spherical alumina powder, and 10 parts of D50 2 μm non-spherical alumina powder were sequentially added into a double planetary dynamic mixing stirrer, and stirred under the conditions of a vacuum degree of-0.1 MPa, a dispersion speed of 600 rpm, a revolution speed of 20 rpm, a kettle temperature of 130 DEG C, and a stirring and dispersion time of 2 hours, and then cooled to 40 DEG C, 0.1 parts of platinum gold catalyst was added, and stirred for 20 minutes to obtain a product.

[0030] 2 parts of vinyl silicone oil with a viscosity of 1000 mPa.s, 2 parts of hydrogen-containing silicone oil, 1 part of DB06 filler surface treatment agent, 40 parts of D50 20 μm spherical alumina powder, 30 parts of D50 10 μm spherical alumina powder, 10 parts of D50 2 μm non-spherical alumina powder, and 0.1 parts of carbon black were sequentially added into a double planetary dynamic mixing stirrer, and stirred under the conditions of a vacuum of-0.1 MPa, a dispersion speed of 600 rpm, a revolution speed of 20 rpm, a kettle temperature of 130 DEG C, and a stirring and dispersion time of 2 hours, and then cooled to 40 DEG C, 0.01 parts of acetylene cyclohexanol, 0.05 parts of gamma-glycidyl ether oxypropyl trimethoxysilane, and 0.05 parts of vinyl triisopropylene oxide silane were added, and stirred for 20 minutes to obtain a product.

[0031] The viscosity of 50 mPa.s vinyl silicone oil is a straight-chain vinyl silicone oil, and its structural formula is CH2=CH-Si(CH3)2O[(CH3)2SiO]4(CH3)2Si-CH=CH 2;

[0032] The viscosity of 2000 mPa.s vinyl silicone oil is a straight-chain vinyl silicone oil, and its structural formula is CH2=CH-Si(CH3)2O[(CH3)2SiO] 135 (CH3)2Si-CH=CH 2;

[0033] The viscosity of 1000 mPa.s vinyl silicone oil is a branched-chain vinyl silicone oil, and its structural formula is (CH3)3SiO[(CH3)2SiO] 70 [(CH2=CH)(CH3)SiO]3Si(CH3) 3;

[0034] The structural formula of the hydrogen-containing silicone oil is CH3-Si(CH3)2-O-[SiHCH3-O]7-[Si-(CH3)2-O] 60 -Si(CH3)2- CH 3。

[0035] Example 2

[0036] The viscosity of 100 mPa.s vinyl silicone oil 12 parts, viscosity of 1000 mPa.s vinyl silicone oil 3 parts, DB06 filler surface treatment agent 5 parts, D50 is 20 μm spherical alumina powder 55 parts, D50 is 10 μm spherical alumina powder 35 parts, D50 is 2 μm non-spherical alumina powder 5 parts are added into the double planetary power mixer in turn, under the condition of vacuum degree-0.1 MPa, dispersion speed is 600 rpm, the revolution speed is 20 rpm, the kettle temperature is kept at 130℃, after stirring and dispersing for 2 hours, the temperature is reduced to 40℃, platinum gold catalyst 1 part is added, and the stirring is continued for 20 minutes, then the material is discharged for standby.

[0037] The viscosity of 100 mPa.s vinyl silicone oil 8 parts, the viscosity of 500 mPa.s vinyl silicone oil 2 parts, 5 parts of end containing hydrogen silicone oil, 2 parts of side containing hydrogen silicone oil, DB06 filler surface treatment agent 5 parts, D50 is 20 μm spherical alumina powder 55 parts, D50 is 10 μm spherical alumina powder 35 parts, D50 is 2 μm non-spherical alumina powder 5 parts, carbon black 1 part, in turn into double planetary power mixer, under the condition of vacuum-0.1 MPa, dispersion speed is 600 r / min, the public speed is 20 r / min, stirring, kettle temperature is kept at 130℃, after stirring dispersion 2 hours, cooling to 40℃, add acetylene group cyclohexanol 0.2 parts, γ-glycidyl ether oxygen propyl trimethoxysilane 0.8 parts, vinyl triisopropylene oxygen silane 0.2 parts, continue to stir 20 minutes can be discharged for standby.

[0038] The viscosity of 100 mPa.s vinyl silicone oil is linear vinyl silicone oil, and its structural formula is: CH2=CH-Si(CH3)2O[(CH3)2SiO] 12 (CH3)2Si-CH=CH2; the viscosity of 500 mPa.s vinyl silicone oil is linear vinyl silicone oil, and its structural formula is: CH2=CH-Si(CH3)2O[(CH3)2SiO] 70 (CH3)2Si-CH=CH2; the viscosity of 1000 mPa.s vinyl silicone oil is branched vinyl silicone oil, and its structural formula is: (CH3)3SiO[(CH3)2SiO] 70 [(CH2=CH)(CH3)SiO]3Si(CH3)3; the structural formula of the end containing hydrogen silicone oil is: H-Si(CH3)2-O-[Si-(CH3)2-O] 66 -Si(CH3)2- H; the structural formula of the side containing hydrogen silicone oil is: CH3-Si(CH3)2-O-[SiHCH3-O]7-[Si-(CH3)2-O] 60 -Si(CH3)2- CH 3。

[0039] Example 3

[0040] The viscosity of 100 mPa.s vinyl silicone oil 6 parts, the viscosity of 500 mPa.s vinyl silicone oil 4 parts, DB06 filler surface treatment agent 3 parts, D50 20 μm spherical alumina powder 45 parts, D50 10 μm spherical alumina powder 37 parts, D50 2 μm non-spherical alumina powder 3 parts were added into the double planetary dynamic mixing stirrer in turn, under the condition of vacuum-0.1 MPa, dispersion speed 600 rpm, revolution speed 20 rpm, the temperature in the kettle was kept at 130℃, after stirring and dispersing for 2 hours, the temperature was decreased to 40℃, platinum gold catalyst 0.5 parts was added, and stirring was continued for 20 minutes, then the product was discharged for standby.

[0041] The viscosity of 100 mPa.s vinyl silicone oil 4.5 parts, the viscosity of 500 mPa.s vinyl silicone oil 1.5 parts, hydrogen-containing silicone oil 3 parts, side hydrogen-containing silicone oil 2 parts, DB06 filler surface treatment agent 3 parts, D50 20 μm spherical alumina powder 45 parts, D50 10 μm spherical alumina powder 37 parts, D50 2 μm non-spherical alumina powder 3 parts, carbon black 0.5 parts were added into the double planetary dynamic mixing stirrer in turn, under the condition of vacuum-0.1 MPa, dispersion speed 600 rpm, revolution speed 20 rpm, the temperature in the kettle was kept at 130℃, after stirring and dispersing for 2 hours, the temperature was decreased to 40℃, ethynylcyclohexanol 0.06 parts, γ-glycidoxypropyltrimethoxysilane 0.3 parts, vinyltriisopropenoxysilane 0.2 parts were added, and stirring was continued for 20 minutes, then the product was discharged for standby.

[0042] The viscosity of 100 mPa.s vinyl silicone oil is linear vinyl silicone oil, and its structural formula is: CH2=CH-Si(CH3)2O[(CH3)2SiO] 12 (CH3)2Si-CH=CH2; the viscosity of 500 mPa.s vinyl silicone oil is linear vinyl silicone oil, and its structural formula is: CH2=CH-Si(CH3)2O[(CH3)2SiO] 70 (CH3)2Si-CH=CH2;

[0043] The structural formula of the hydrogen-containing silicone oil is: H-Si(CH3)2-O-[Si-(CH3)2-O] 66 -Si(CH3)2-H; the structural formula of the side hydrogen-containing silicone oil is: CH3-Si(CH3)2-O-[SiHCH3-O]7-[Si-(CH3)2-O] 60 -Si(CH3)2-CH 3。

[0044] Comparative Example 1

[0045] The viscosity of 100 mPa.s vinyl silicone oil 6 parts, the viscosity of 500 mPa.s vinyl silicone oil 4 parts, DB06 filler surface treatment agent 3 parts, D50 20 μm spherical alumina powder 45 parts, D50 10 μm spherical alumina powder 37 parts, D50 2 μm non-spherical alumina powder 3 parts are sequentially added into a double planetary dynamic mixing stirrer, under normal temperature conditions, under the condition of vacuum degree -0.1 MPa, stirring at a dispersion speed of 600 rpm and a revolution speed of 20 rpm, after stirring and dispersing for 2 hours, platinum gold catalyst 0.5 parts is added, and stirring is continued for 20 minutes to obtain a product.

[0046] The viscosity of 100 mPa.s vinyl silicone oil 4.5 parts, the viscosity of 500 mPa.s vinyl silicone oil 1.5 parts, end hydrogen-containing silicone oil 3 parts, side hydrogen-containing silicone oil 2 parts, DB06 filler surface treatment agent 3 parts, D50 20 μm spherical alumina powder 45 parts, D50 10 μm spherical alumina powder 37 parts, D50 2 μm non-spherical alumina powder 3 parts, carbon black 0.5 parts are sequentially added into a double planetary dynamic mixing stirrer, under normal temperature conditions, under the condition of vacuum -0.1 MPa, stirring at a dispersion speed of 600 rpm and a revolution speed of 20 rpm, after stirring and dispersing for 2 hours, ethynylcyclohexanol 0.06 parts, γ-glycidoxypropyltrimethoxysilane 0.3 parts, and vinyltriisopropenoxysilane 0.2 parts are added, and stirring is continued for 20 minutes to obtain a product.

[0047] The viscosity of 100 mPa.s vinyl silicone oil is a linear vinyl silicone oil, and its structural formula is: CH2=CH-Si(CH3)2O[(CH3)2SiO] 12 (CH3)2Si-CH=CH2; the viscosity of 500 mPa.s vinyl silicone oil is a linear vinyl silicone oil, and its structural formula is: CH2=CH-Si(CH3)2O[(CH3)2SiO] 70 (CH3)2Si-CH=CH2; the structural formula of the end hydrogen-containing silicone oil is: H-Si(CH3)2-O-[Si-(CH3)2-O] 66 -Si(CH3)2- H; the structural formula of the side hydrogen-containing silicone oil is: CH3-Si(CH3)2-O-[SiHCH3-O]7-[Si-(CH3)2-O] 60 -Si(CH3)2- CH 3。

[0048] Comparative Example 2

[0049] Six parts of vinyl silicone oil with a viscosity of 100 mPa·s, four parts of vinyl silicone oil with a viscosity of 500 mPa·s, 45 parts of spherical alumina powder with a D50 of 20 μm, 37 parts of spherical alumina powder with a D50 of 10 μm, and three parts of non-spherical alumina powder with a D50 of 2 μm were sequentially added to a dual planetary mixer. The mixture was stirred at room temperature under a vacuum of -0.1 MPa, a dispersion speed of 600 rpm, and a revolution speed of 20 rpm. After stirring and dispersing for 2 hours, 0.5 parts of platinum catalyst were added, and stirring was continued for another 20 minutes before the mixture was discharged for use.

[0050] Add 4.5 parts of vinyl silicone oil with a viscosity of 100 mPa·s, 1.5 parts of vinyl silicone oil with a viscosity of 500 mPa·s, 3 parts of end-hydrogen silicone oil, 2 parts of side-hydrogen silicone oil, 45 parts of spherical alumina powder with a D50 of 20 μm, 37 parts of spherical alumina powder with a D50 of 10 μm, 3 parts of non-spherical alumina powder with a D50 of 2 μm, and 0.5 parts of carbon black sequentially into a double planetary mixer. Under normal temperature conditions, stir at a vacuum of -0.1 MPa, a dispersion speed of 600 rpm, and a revolution speed of 20 rpm. After stirring and dispersing for 2 hours, add 0.06 parts of ethynylcyclohexanol, 0.3 parts of γ-glycidyl etheroxypropyltrimethoxysilane, and 0.2 parts of vinyltriisopropoxysilane. Continue stirring for 20 minutes before discharging for later use.

[0051] The vinyl silicone oil with a viscosity of 100 mPa·s is a linear vinyl silicone oil with the structural formula: CH2=CH-Si(CH3)2O[(CH3)2SiO] 12 (CH3)2Si-CH=CH2; the vinyl silicone oil with a viscosity of 500 mPa·s is a linear vinyl silicone oil, and its structural formula is: CH2=CH-Si(CH3)2O[(CH3)2SiO] 70 (CH3)2Si-CH=CH2;

[0052] The structural formula of the hydrogen-containing silicone oil is: H-Si(CH3)2-O-[Si-(CH3)2-O] 66 -Si(CH3)2- H; the structural formula of the side-containing hydrogen silicone oil is: CH3-Si(CH3)2-O-[SiHCH3-O]7-[Si-(CH3)2-O] 60 -Si(CH3)2- CH 3。

[0053] Specific experimental examples

[0054] The performance of the two-component potting silicone of the present invention was tested through the following experiments.

[0055] Experimental Example 1: Viscosity Test

[0056] The A component and B component obtained in the above Examples 1-3 and Comparative Examples 1-2 were tested according to the standard GB / T 2794-2013.

[0057] Test Example 2: Thermal conductivity test

[0058] The thermal conductivity of the samples prepared in Examples 1-3 and Comparative Examples 1-2 was tested according to ASTM D5470 using a Hot Disk TPS 2500S thermal conductivity meter.

[0059] Test Example 3: Modulus test

[0060] The test was performed using DMA tensile mode, and the sample thickness was 1 mm

[0061] Test Example 4: Adhesion strength test

[0062] The test was performed according to the national standard GB / T 7124-2008, and the substrate was glass / aluminum.

[0063] Test Example 5: Pressing test

[0064] After mixing the glue, the glue was dropped onto the glass sheet, and the glass sheet was pasted at 25°C for 4 h, and then pressed with a 2 kg weight for 30 min, and the glue layer thickness was measured.

[0065] Test Example 6: Elongation at break test

[0066] The test was performed according to the national standard GB / T 528-2009.

[0067] Test Example 7: Settling test

[0068] The test results are shown in the following table:

[0069]

[0070] As can be seen from the table, first, the heat-conducting filler is treated under heating condition using the DB06 filler surface treatment agent, and the prepared pouring sealant has lower viscosity and thixotropy under the premise of ensuring the required heat conductivity of 2 W / m*K, and the anti-settling property is also good, and it is easy to stir uniformly after being placed for 6 months, while the heat-conducting filler in the comparative example 2 is not treated in any way, and the prepared heat-conducting pouring sealant is difficult to stir uniformly after being placed for 6 months due to serious filler settling. Secondly, the alumina filler D99 used in the application is ≤ 50 μm, and the pressing thickness is lower, which is more conducive to the filling of small gaps. As is known, the adhesion of domestic addition type silicone is very weak when being cured at medium and low temperatures, while the adhesion strength of the prepared pouring sealant is better, which is incomparable to the pouring sealants with the same heat conductivity prepared by other manufacturers. The elongation of the prepared pouring sealant is higher, and it is more suitable for the pouring of large-size devices. In summary, the heat-conducting filler of the prepared pouring sealant has small particle size, low viscosity, good filling property, strong adhesion and high elongation, and finally the reliability and service life of the product can be effectively ensured.

[0071] The above description is only the preferred embodiment of the application, and is not intended to limit the application, and any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the application shall be included in the protection scope of the application.

Claims

1. A high-performance heat-conducting silicone potting adhesive, characterized in that, A component and B component are composed according to 1:1 weight ratio, the A component is composed of the following raw materials: vinyl silicone oil 5-15 parts, heat-conducting filler 80-95 parts, DB06 filler surface treatment agent 1-5 parts, platinum gold catalyst 0.1-1 part; the B component is composed of the following raw materials: vinyl silicone oil 2-10 parts, hydrogen-containing silicone oil 2-7 parts, heat-conducting filler 80-95 parts, DB06 filler surface treatment agent 1-5 parts, inhibitor 0.01-0.2 parts, adhesive 0.1-1 parts, toning agent 0.1-1 parts; The DB06 filler surface treatment agent is a self-made long-chain siloxane; its preparation method is as follows: 405g of end hydrogen-containing silicone oil with a hydrogen content of 0.1% is added into a flask, 15g of vinyl trimethoxysilane and 0.1g of 5000ppm platinum gold catalyst are fully mixed and uniformly mixed, the mixed solution is added dropwise into the flask while stirring, after the dropwise addition is completed, the reaction is carried out for 3h, the temperature in the bottle is controlled at 90℃, 30g of 1-nonene is added, the reaction is continued for 2.5h, and then low-boiling substances are removed to obtain the product; The preparation method of the high-performance heat-conducting silicone pouring sealant comprises the following steps: 1) vinyl silicone oil 5-15 parts, DB06 filler surface treatment agent 1-5 parts, heat-conducting filler 80-95 parts are sequentially added into a double-planetary dynamic mixing stirrer, stirring is carried out under the conditions of a vacuum degree of-0.1MPa, a dispersion speed of 600r / min, a revolution speed of 20r / min, the temperature in the kettle is kept at 130℃, after stirring and dispersing for 2h, the temperature is lowered to 40℃, platinum gold catalyst 0.1-1 part is added, and stirring is continued for 20min to obtain a product ready for use; 2) vinyl silicone oil 2-10 parts, hydrogen-containing silicone oil 2-7 parts, DB06 filler surface treatment agent 1-5 parts, heat-conducting filler 80-95 parts, toning agent 0.1-1 parts are sequentially added into a double-planetary dynamic mixing stirrer, stirring is carried out under the conditions of a vacuum degree of-0.1MPa, a dispersion speed of 600r / min, a revolution speed of 20r / min, the temperature in the kettle is kept at 130℃, after stirring and dispersing for 2h, the temperature is lowered to 40℃, inhibitor 0.01-0.2 parts and adhesive 0.1-1 parts are added, and stirring is continued for 20min to obtain a product ready for use; 3) when used, the A and B components are mixed uniformly according to a weight ratio of 1:1, curing is carried out at 100℃ for 1h to obtain the product.

2. The high-performance thermal conductive silicone potting sealant according to claim 1, characterized in that, The heat-conducting filler is spherical alumina and non-spherical alumina powder, and the particle size D99 is ≤50μm. 3.The high-performance thermal conductive silicone potting adhesive according to claim 1, characterized in that, The viscosity of the vinyl silicone oil ranges from 50mPa.s to 2000mPa.s; the vinyl silicone oil is linear end vinyl silicone oil and branched vinyl silicone oil, the structural formula of the linear end vinyl silicone oil is represented by (I): CH2=CH-Si(CH3)2O[(CH3)2SiO] n (CH3)2Si-CH=CH2(I); The structural formula of the branched vinyl silicone oil is represented by (II): (CH3)3SiO[(CH3)2SiO] m [(CH2=CH)(CH3)SiO] p Si(CH3)3 (II); wherein, n=50-200; m+p=50-260.

4. The high-performance thermal conductive silicone potting sealant according to claim 1, characterized in that, The hydrogen-containing silicone oil is represented by (III): R-Si(CH3)2-O-[SiHCH3-O] a -[Si-(CH3)2-O] b -Si(CH3)2-R (III); wherein, R represents CH3 or H, and a+b=8-98.

5. The high-performance thermal conductive silicone potting sealant according to claim 1, characterized in that, The concentration of the platinum catalyst is 1000-5000 ppm; the toner is carbon black; the inhibitor is one of methyl butynol, ethynyl cyclohexanol, maleate; the bonding agent is one or two of γ-glycidoxypropyltrimethoxysilane, γ-glycidoxypropyltriethoxysilane, 2-(3,4-epoxycyclohexyl)ethyltrimethoxysilane, γ-methacryloyloxypropyltrimethoxysilane, γ-methacryloyloxypropyltriethoxysilane, vinyltrimethoxysilane, vinyltriisopropenoxysilane. The concentration of the platinum catalyst is 1000-5000 ppm; the toner is carbon black; the inhibitor is one of methyl butynol, ethynyl cyclohexanol, maleate; the bonding agent is one or two of γ-glycidoxypropyltrimethoxysilane, γ-glycidoxypropyltriethoxysilane, 2-(3,4-epoxycyclohexyl)ethyltrimethoxysilane, γ-methacryloyloxypropyltrimethoxysilane, γ-methacryloyloxypropyltriethoxysilane, vinyltrimethoxysilane, vinyltriisopropenoxysilane.

Citation Information

Patent Citations

  • Heat-conduction electronic potting adhesive and preparation method thereof

    CN102942895A

  • Low-viscosity and high-thermal-conductivity two-component potting silica gel

    CN113845875A