A two-component thermally conductive gel and its preparation method and application

By optimizing the interface compatibility between filler and silicone in a two-component thermal conductivity gel, problems such as thermal conductivity and viscosity, extrusion and adhesiveness in the prior art are solved, and efficient thermal conductivity and good mechanical properties are achieved, which are suitable for scenarios such as electronic components.

CN116285366BActive Publication Date: 2025-03-25GUANGZHOU JOINTAS CHEM +1

Patent Information

Application Number
CN202310335634.1
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2023-03-31
Publication Date
2025-03-25
Estimated Expiration
2043-03-31

AI Technical Summary

Technical Problem

While improving the thermal conductivity, the existing two-component thermal gel has problems such as excessive viscosity, poor extrusion and poor adhesiveness, which limits its application in electronic components.

Method used

By adding components such as vinyl silicone oil, thermal filler, tackifier and hydrogen-containing organopolysiloxane to components A and B, the interface compatibility between the filler and the silicone is optimized, and the interface friction resistance and heat value are reduced, thereby improving the thermal conductivity, bonding and mechanical properties of the thermal gel.

Benefits of technology

It achieves excellent thermal conductivity, low viscosity, good bonding and mechanical properties of two-component thermal gel, and is suitable for electronic components and power batteries and other scenarios.

✦ Generated by Eureka AI based on patent content.

Smart Images

  • Figure QLYQS_1
    Figure QLYQS_1
  • Figure QLYQS_2
    Figure QLYQS_2
  • Figure QLYQS_3
    Figure QLYQS_3
Patent Text Reader

Abstract

The present invention discloses a two-component thermally conductive gel and a preparation method and application thereof, belonging to the technical field of thermally conductive gels. The two-component thermally conductive gel comprises a component A and a component B: the component A comprises the following components in parts by mass: 100 parts of vinyl silicone oil A, 1500-3000 parts of thermally conductive filler A, and 0.5-10 parts of a tackifier; the component B comprises the following components in parts by mass: 100 parts of vinyl silicone oil B, 2-10 parts of terminal hydrogenated silicone oil, 1-6 parts of hydrogen-containing organic polysiloxane, and 1500-3000 parts of thermally conductive filler B. The present invention obtains a thermally conductive gel having excellent thermal conductivity, low viscosity, bonding performance, and mechanical properties by combining the above-mentioned various raw materials; the hydrogen-containing organic polysiloxane is matched with a tackifier to improve the interface compatibility between the filler and the silicone, reduce the interface friction resistance and calorific value, and effectively improve the bonding force between the thermally conductive gel and the interface.
Need to check novelty before this filing date? Find Prior Art

Description

Technical Field

[0001] The invention relates to the technical field of thermal conductive gels, and in particular to a two-component thermal conductive gel and a preparation method and application thereof. Background Art

[0002] With the development of society and the advancement of science and technology, electronic components are constantly developing towards high power, miniaturization and density, which leads to a large amount of heat accumulation in a limited space when the components are running, seriously affecting the working efficiency and service life of the components. How to quickly guide the excess heat out of electronic components is an urgent problem to be solved. At present, the common thermal conductive products on the market are thermal conductive pads, thermal conductive gels, two-component thermal conductive gels and thermal conductive phase change materials. Among them, thermal conductive gels are further divided into single-component thermal conductive gels and two-component thermal conductive gels. Compared with other thermal conductive products, two-component thermal conductive gels have simple processing technology, low loss, a wide range of applicable working conditions, simple operating equipment, and high thermal conductivity, and are becoming more and more popular with customers.

[0003] However, the current two-component thermally conductive gel also has some problems that need to be solved. High thermal conductivity thermally conductive gels often add a large amount of thermally conductive fillers, which leads to high viscosity of the material, poor extrusion and difficulty in mixing, which in turn affects the curing and mechanical properties of the product; in addition, the two-component thermally conductive gel belongs to an addition system, and its adhesion is poor, which limits its use scenarios.

[0004] CN113736266A discloses a two-component thermally conductive gel and its preparation method and application. The two-component thermally conductive gel includes component A and component B; the component A includes the following components in parts by weight: 10-40 parts of monovinyl-terminated polydimethylsiloxane; 5-10 parts of methyl hydrogen polydimethylsiloxane; 100-200 parts of thermally conductive filler A; the component B includes the following components in parts by weight: 10-40 parts of alkoxy-terminated vinyl polydimethylsiloxane; 100-200 parts of thermally conductive filler B; 0.1-2 parts of catalyst. The two-component thermally conductive gel prepared by using monovinyl-terminated polydimethylsiloxane and alkoxy-terminated vinyl polydimethylsiloxane has good high temperature resistance, low oil yield and high thermal conductivity, and is suitable for the preparation of electronic components; but its viscosity thermal conductivity is only up to 6.0W / mk, which still needs to be improved. Summary of the invention

[0005] The purpose of the present invention is to overcome the shortcomings of the prior art and provide a two-component thermally conductive gel and a preparation method and application thereof. The thermally conductive gel has excellent thermal conductivity, low viscosity, bonding properties and mechanical properties.

[0006] To achieve the above object, in a first aspect of the present invention, the present invention provides a two-component thermally conductive gel, comprising component A and component B:

[0007] The component A comprises the following components in parts by mass: 100 parts of vinyl silicone oil A, 1500-3000 parts of thermal conductive filler A, and 0.5-10 parts of tackifier;

[0008] The B component includes the following components in parts by mass: 100 parts of vinyl silicone oil B, 2 to 10 parts of terminal hydrogen-containing silicone oil, 1 to 6 parts of hydrogen-containing organic polysiloxane, and 1500 to 3000 parts of thermal conductive filler B.

[0009] The present invention combines the above-mentioned various raw materials to obtain a thermally conductive gel with excellent thermal conductivity, low viscosity, bonding performance and mechanical properties.

[0010] The hydrogen-containing organopolysiloxane of the present invention is combined with a tackifier to improve the interfacial compatibility between the filler and the organosilicon, reduce the interfacial friction resistance and calorific value, and effectively improve the bonding force between the thermally conductive gel and the interface.

[0011] The component A comprises the following components in parts by mass: 100 parts of vinyl silicone oil A, 1700-2600 parts of thermal conductive filler A, and 5-8 parts of tackifier;

[0012] The B component includes the following components in parts by mass: 100 parts of vinyl silicone oil B, 3 to 10 parts of terminal hydrogen-containing silicone oil, 2 to 6 parts of hydrogen-containing organic polysiloxane, and 1700 to 2600 parts of thermal conductive filler B.

[0013] As a preferred embodiment of the present invention, the vinyl silicone oil A and the vinyl silicone oil B are independently selected from at least one of side hydroxyl-terminated vinyl silicone oil, single-terminated vinyl silicone oil, double-terminated vinyl silicone oil, T-structured vinyl silicone oil, and phenyl vinyl silicone oil; and the viscosity of the vinyl silicone oil A and the vinyl silicone oil B are both 300cps-2000cps.

[0014] Each component of the two-component thermally conductive filler of the present invention contains a large amount of vinyl silicone oil, which can effectively improve the mechanical properties and hardness of the thermally conductive gel and has a certain wetting effect.

[0015] As a preferred embodiment of the present invention, the component A comprises the following components in parts by mass: 100 parts of divinyl silicone oil-1, 300 parts of zinc oxide with a D50 of 1 μm, 800 parts of aluminum nitride with a D50 of 7 μm, 1500 parts of diamond powder with a D50 of 80 μm, 5 parts of a tackifier, 2.5 parts of dodecyl trimethylsiloxane, and 0.2 parts of a platinum catalyst;

[0016] The B component includes the following components by mass: 100 parts of divinyl silicone oil-1, 6 parts of terminal hydrogen silicone oil, 2 parts of hydrogen-containing organic polysiloxane, 300 parts of zinc oxide with a D50 of 1 μm, 800 parts of aluminum nitride with a D50 of 7 μm, 1500 parts of diamond powder with a D50 of 80 μm, 2.5 parts of dodecyl trimethylsiloxane, and 0.02 parts of 3-methyl-1-butyn-3-ol. By controlling the raw materials of the A component and the B component within this limited range, the performance is further improved.

[0017] By controlling the viscosity between 300cps-2000cps, the viscosity and mechanical properties of the system can be effectively improved. If the viscosity is 300cps, the two-component thermal conductive gel is prone to oil discharge and poor stability. If the viscosity is greater than 2000cps, the extrusion performance is poor, the operability is poor, and the system viscosity is easily too high. Therefore, in the present invention, the viscosity of the vinyl silicone oil needs to be strictly controlled between 300 and 2000cps.

[0018] As a preferred embodiment of the present invention, the hydrogen content of the terminal hydrogen-containing silicone oil is 0.08%-0.3%. If the hydrogen content of the terminal hydrogen-containing silicone oil is lower than 0.08%, the hydrogen content is too little, the reaction activity is low, the reaction rate is low, and the efficiency is poor; if the hydrogen content is higher than 0.3%, the reaction activity is too high, and it is difficult to control the crosslinking density when the crosslinking reaction occurs, which easily causes the hardness of the two-component thermal conductive gel to fluctuate greatly after curing, and the quality is unstable.

[0019] As a preferred embodiment of the present invention, the structural formula of the tackifier is as shown in formula (1):

[0020]

[0021] Wherein, m is a positive integer between 10 and 50, and n is a positive integer between 10 and 50.

[0022] The specific structure of the tackifier contains a large number of epoxy groups, which can play a physical anchoring role on the one hand, and on the other hand can react chemically with certain polar groups (such as amino groups, hydroxyl groups, etc.) on the interface to improve the interfacial compatibility of the thermally conductive filler, so that it has good mechanical properties and bonding properties, reduce interfacial friction resistance and calorific value, and effectively improve the bonding force between the thermally conductive gel and the interface.

[0023] As a preferred embodiment of the present invention, the preparation method of the tackifier comprises the following steps:

[0024] Add terminal hydrogen silicone oil, 4-vinyl-1,2-epoxycyclohexane, solvent and catalyst into a reaction container, react under nitrogen atmosphere, and evacuate to obtain a tackifier;

[0025] The structural formula of the end-side hydrogen silicone oil is shown in formula (2):

[0026]

[0027] Wherein, m is a positive integer between 10 and 50, and n is a positive integer between 10 and 50.

[0028] As a preferred embodiment of the present invention, the mass ratio of the terminal hydrogen silicone oil, 4-vinyl-1,2-epoxycyclohexane, and the solvent is 1:(0.2-0.5):(1-10); and / or

[0029] As a preferred embodiment of the present invention, the solvent includes at least one of toluene, xylene and cyclohexane.

[0030] As a preferred embodiment of the present invention, the catalyst includes at least one of a Custer catalyst, a chloroplatinic acid catalyst, a chloroplatinic acid-isopropanol solution catalyst, and a platinum catalyst.

[0031] As a preferred embodiment of the present invention, the structural formula of the hydrogen-containing organopolysiloxane is shown in formula (3):

[0032]

[0033] Wherein, a is a positive integer between 10 and 50, b is a positive integer between 10 and 50, and c is a positive integer between 10 and 50;

[0034] R is C1~C 20 alkyl.

[0035] Preferably, R is -C6H 13 , -C 10 H 21 , -C 12 H 25 , -C 16 H 33 At least one of .

[0036] Long-chain alkyl groups are added to hydrogen-containing organopolysiloxanes. The polarity of the long-chain alkyl group is relatively close to that of the powder. The addition of long-chain alkyl groups can significantly reduce the polarity difference between the silicone oil system and the powder. According to the principle of similar compatibility, the compatibility is improved, which increases the compatibility with the powder and makes it easier to wet the powder surface, thereby reducing the surface thermal resistance, improving thermal conductivity, and reducing the viscosity of the system.

[0037] The inventors of the present invention have found that, in the specific filler system of the present invention, it is necessary to add hydrogen-containing organopolysiloxane and a tackifier at the same time, wherein the tackifier increases the mechanical and adhesive properties, and the hydrogen-containing organopolysiloxane increases the compatibility with the powder. The tackifier and the hydrogen-containing organopolysiloxane have the same molecular main chain and good compatibility. If there is no hydrogen-containing organopolysiloxane, the compatibility of the tackifier with the silicone oil system will deteriorate, and it will not play a good role in enhancing the mechanical properties and adhesive properties. Under the joint action of the two, the interface compatibility between the filler and the silicone is improved, and the interface friction resistance and calorific value are reduced. That is, the hydrogen-containing organopolysiloxane and the tackifier have a significant synergistic effect in improving the bonding force and thermal conductivity of the thermally conductive filler, and the hydrogen-containing organopolysiloxane and the tackifier need to be added at the same time.

[0038] As a preferred embodiment of the present invention, the thermally conductive filler A and the thermally conductive filler B are independently selected from a combination of a first thermally conductive filler, a second thermally conductive filler and a third thermally conductive filler;

[0039] The mass ratio of the first thermally conductive filler, the second thermally conductive filler, and the third thermally conductive filler is (1-4): (4-10): (5-15);

[0040] The first thermally conductive filler, the second thermally conductive filler, and the third thermally conductive filler are each independently selected from one of aluminum oxide, zinc oxide, magnesium oxide, silicon dioxide, aluminum nitride, boron nitride, aluminum carbide, silicon carbide, aluminum hydroxide, magnesium hydroxide, boehmite, and diamond;

[0041] The D50 of the first thermally conductive filler is 0.3 to 1.5 μm;

[0042] The D50 of the second thermally conductive filler is 3 to 10 μm;

[0043] The D50 of the third thermally conductive filler is 40-100 μm.

[0044] By using the filler with the specific composition, the thermal conductive gel is made denser, the extrusion performance is further improved, and the thermal conductivity is further improved.

[0045] As a preferred embodiment of the present invention, the A component further comprises 0.1 to 5 parts of a catalyst.

[0046] Exemplarily, the catalyst comprises a platinum catalyst.

[0047] As a preferred embodiment of the present invention, the component A further comprises 0.5 to 10 parts of a coupling aid A.

[0048] As a preferred embodiment of the present invention, the B component further comprises 0.01 to 2 parts of an inhibitor.

[0049] Exemplarily, the inhibitor includes at least one of 3-methyl-1-butyn-3-ol, 3-methyl-1-pentyn-3-ol, 3,5-dimethyl-1-hexyn-3-ol, methylvinylcyclotetrasiloxane, and tetramethyldivinyldisiloxane.

[0050] As a preferred embodiment of the present invention, the B component further includes 0.5 to 10 parts of coupling aid B.

[0051] Exemplarily, the coupling aid A and the coupling aid B are each independently selected from at least one of 3-methacryloxypropyltrimethoxysilane, 3-methacryloxypropyltriethoxysilane, 3-methacryloxypropylmethyltriethoxysilane, hexadecyltrimethoxysilane, dodecyltrimethylsiloxane, dodecyltrimethoxysilane, n-decyltrimethylsilane, methyltrimethoxysilane, γ-glycidyloxypropyltrimethoxysilane, stearic acid, oleic acid, lauric acid, and adipic acid.

[0052] In a second aspect of the present invention, the present invention provides a method for preparing a two-component thermally conductive gel, comprising the following steps:

[0053] Add vinyl silicone oil A, thermal conductive filler A, tackifier, and coupling aid A into a reaction kettle, stir evenly, add a catalyst, stir evenly, and obtain component A.

[0054] Vinyl silicone oil B, hydrogen-terminated silicone oil, hydrogen-containing organopolysiloxane, thermal conductive filler B, and coupling aid are mixed evenly, an inhibitor is added, and the mixture is mixed evenly to obtain component B;

[0055] Component A and component B are mixed evenly to obtain a two-component thermal conductive gel.

[0056] In a third aspect of the present invention, the present invention provides the use of a two-component thermally conductive gel in electronic components and power batteries.

[0057] The beneficial effects of the present invention are: (1) the present invention combines the above-mentioned various raw materials to obtain a thermally conductive gel with excellent thermal conductivity, low viscosity, bonding properties and mechanical properties; (2) the hydrogen-containing organic polysiloxane described in the present invention is combined with a thickener to improve the interface compatibility between the filler and the organic silicon, reduce the interface friction resistance and calorific value, and effectively improve the bonding force between the thermally conductive gel and the interface. DETAILED DESCRIPTION

[0058] In order to make the purpose, technical solution and advantages of the embodiments of the present invention clearer, the technical solution in the embodiments of the present invention will be described clearly and completely below. Obviously, the described embodiments are part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0059] There is no particular limitation on the specific dispersion and stirring treatment methods.

[0060] In the present invention, unless otherwise stated, all parts are parts by weight.

[0061] The reagents or instruments used in the present invention without indicating the manufacturer are all conventional products that can be obtained through commercial purchase. The raw material information used in the examples and comparative examples of the present invention is as follows:

[0062] 1. Divinyl silicone oil-1: purchased from Guangzhou Conghua Zhaoshun New Materials Co., Ltd., product model C-1 (300), viscosity 300 cps.

[0063] 2. Vinyl silicone oil-2: purchased from Guangzhou Conghua Zhaoshun New Materials Co., Ltd., product model C-1 (100), viscosity 100 cps.

[0064] 3. Vinyl silicone oil-3: purchased from Guangzhou Conghua Zhaoshun New Materials Co., Ltd., product model C-1 (5000), viscosity 5000cps.

[0065] 4. End hydrogen-containing silicone oil: purchased from Jiangxi Haiduo Chemical Co., Ltd., product model DH-010, hydrogen content mass fraction is 0.1%.

[0066] 5. Side hydrogen-containing silicone oil: purchased from Jiangxi Haiduo Chemical Co., Ltd., product model D-018-120, hydrogen content mass fraction is 0.18%.

[0067] 6. Thickener The structural formula of the thickener is shown in formula (1):

[0068]

[0069] Among them, m=50, n=15.

[0070] The preparation method of the tackifier comprises the following steps:

[0071] 100 parts of end-side hydrogen silicone oil, 600 parts of 4-vinyl-1,2-epoxycyclohexane, 200 parts of toluene, and 3 parts of chloroplatinic acid catalyst were added to a reaction container, and reacted at 75° C. for 3 hours under a nitrogen atmosphere. After the reaction was completed, vacuum was drawn for 1 hour to remove the toluene, thereby obtaining a tackifier;

[0072] The structural formula of the end-side hydrogen silicone oil is shown in formula (2):

[0073]

[0074] Wherein, m is a positive integer between 50 and 15, and n is a positive integer between 15 and 20.

[0075] 6. The structural formula of hydrogen-based organopolysiloxane is shown in formula (3):

[0076]

[0077] Wherein, a=20, b=10, c=20;

[0078] R is -C 12 H 25 .

[0079] Example 1

[0080] A two-component thermal conductive gel, comprising component A and component B:

[0081] The component A comprises the following components in parts by mass: 100 parts of divinyl silicone oil-1, 300 parts of zinc oxide with a D50 of 1 μm, 800 parts of aluminum nitride with a D50 of 7 μm, 1500 parts of diamond powder with a D50 of 80 μm, 5 parts of tackifier, 2.5 parts of dodecyl trimethylsiloxane, and 0.2 parts of platinum catalyst;

[0082] The B component includes the following components in parts by mass: 100 parts of divinyl silicone oil-1, 6 parts of terminal hydrogen silicone oil, 2 parts of hydrogen-containing organic polysiloxane, 300 parts of zinc oxide with a D50 of 1 μm, 800 parts of aluminum nitride with a D50 of 7 μm, 1500 parts of diamond powder with a D50 of 80 μm, 2.5 parts of dodecyltrimethylsiloxane, and 0.02 parts of 3-methyl-1-butyn-3-ol.

[0083] The method for preparing the two-component thermally conductive gel comprises the following steps:

[0084] (1) Add divinyl silicone oil-1, zinc oxide, aluminum nitride, diamond powder, tackifier, and dodecyl trimethylsiloxane in component A to a reaction kettle, stir at 100° C. for 4 hours, cool to room temperature, add platinum catalyst, and stir under vacuum for 30 minutes to obtain component A;

[0085] (2) Add divinyl silicone oil-1, terminal hydrogen silicone oil, hydrogen-containing organopolysiloxane, zinc oxide, aluminum nitride, diamond powder, and dodecyltrimethylsiloxane into a reaction kettle, stir at 100° C. for 4 hours, cool to room temperature, add 3-methyl-1-butyn-3-ol, and stir under vacuum for 30 minutes to obtain component B;

[0086] (3) The component A prepared in step (1) and the component B prepared in step (2) are mixed evenly to obtain a two-component thermally conductive gel.

[0087] Example 2

[0088] A two-component thermal conductive gel, comprising component A and component B:

[0089] The component A comprises the following components in parts by mass: 100 parts of divinyl silicone oil-1, 200 parts of zinc oxide with a D50 of 1 μm, 400 parts of aluminum nitride with a D50 of 7 μm, 900 parts of diamond powder with a D50 of 80 μm, 1 part of a tackifier, 10 parts of dodecyl trimethylsiloxane, and 0.2 parts of a platinum catalyst;

[0090] The B component includes the following components in parts by mass: 100 parts of divinyl silicone oil-1, 2 parts of terminal hydrogen silicone oil, 6 parts of hydrogen-containing organic polysiloxane, 200 parts of zinc oxide with a D50 of 1 μm, 400 parts of aluminum nitride with a D50 of 7 μm, 900 parts of diamond powder with a D50 of 80 μm, 0.5 parts of dodecyl trimethylsiloxane, and 0.02 parts of 3-methyl-1-butyn-3-ol.

[0091] The method for preparing the two-component thermally conductive gel comprises the following steps:

[0092] (1) Add divinyl silicone oil-1, zinc oxide, aluminum nitride, diamond powder, tackifier, and dodecyl trimethylsiloxane in component A to a reaction kettle, stir at 100° C. for 4 hours, cool to room temperature, add platinum catalyst, and stir under vacuum for 30 minutes to obtain component A;

[0093] (2) Add divinyl silicone oil-1, terminal hydrogen silicone oil, hydrogen-containing organopolysiloxane, zinc oxide, aluminum nitride, diamond powder, and dodecyltrimethylsiloxane into a reaction kettle, stir at 100° C. for 4 hours, cool to room temperature, add 3-methyl-1-butyn-3-ol, and stir under vacuum for 30 minutes to obtain component B;

[0094] (3) The component A prepared in step (1) and the component B prepared in step (2) are mixed evenly to obtain a two-component thermally conductive gel.

[0095] Example 3

[0096] A two-component thermal conductive gel, comprising component A and component B:

[0097] The component A comprises the following components in parts by mass: 100 parts of divinyl silicone oil-1, 400 parts of zinc oxide with a D50 of 1 μm, 600 parts of aluminum nitride with a D50 of 7 μm, 1500 parts of diamond powder with a D50 of 80 μm, 8 parts of a tackifier, 10 parts of dodecyl trimethylsiloxane, and 0.2 parts of a platinum catalyst;

[0098] The B component includes the following components in parts by mass: 100 parts of divinyl silicone oil-1, 3 parts of terminal hydrogen silicone oil, 5 parts of hydrogen-containing organic polysiloxane, 400 parts of zinc oxide with a D50 of 1 μm, 600 parts of aluminum nitride with a D50 of 7 μm, 1500 parts of diamond powder with a D50 of 80 μm, 10 parts of dodecyl trimethylsiloxane, and 0.02 parts of 3-methyl-1-butyn-3-ol.

[0099] The method for preparing the two-component thermally conductive gel comprises the following steps:

[0100] (1) Add divinyl silicone oil-1, zinc oxide, aluminum nitride, diamond powder, tackifier, and dodecyl trimethylsiloxane in component A to a reaction kettle, stir at 100° C. for 4 hours, cool to room temperature, add platinum catalyst, and stir under vacuum for 30 minutes to obtain component A;

[0101] (2) Add divinyl silicone oil-1, terminal hydrogen silicone oil, hydrogen-containing organopolysiloxane, zinc oxide, aluminum nitride, diamond powder, and dodecyltrimethylsiloxane into a reaction kettle, stir at 100° C. for 4 hours, cool to room temperature, add 3-methyl-1-butyn-3-ol, and stir under vacuum for 30 minutes to obtain component B;

[0102] (3) The component A prepared in step (1) and the component B prepared in step (2) are mixed evenly to obtain a two-component thermally conductive gel.

[0103] Example 4

[0104] A two-component thermal conductive gel, comprising component A and component B:

[0105] The component A comprises the following components in parts by mass: 100 parts of divinyl silicone oil-1, 200 parts of zinc oxide with a D50 of 1 μm, 500 parts of aluminum nitride with a D50 of 7 μm, 1000 parts of diamond powder with a D50 of 80 μm, 6 parts of tackifier, 5 parts of dodecyl trimethylsiloxane, and 0.2 parts of platinum catalyst;

[0106] The B component includes the following components in parts by mass: 100 parts of divinyl silicone oil-1, 5 parts of terminal hydrogen silicone oil, 3 parts of hydrogen-containing organic polysiloxane, 200 parts of zinc oxide with a D50 of 1 μm, 500 parts of aluminum nitride with a D50 of 7 μm, 1000 parts of diamond powder with a D50 of 80 μm, 5 parts of dodecyl trimethylsiloxane, and 0.02 parts of 3-methyl-1-butyn-3-ol.

[0107] The method for preparing the two-component thermally conductive gel comprises the following steps:

[0108] (1) Add divinyl silicone oil-1, zinc oxide, aluminum nitride, diamond powder, tackifier, and dodecyl trimethylsiloxane in component A to a reaction kettle, stir at 100° C. for 4 hours, cool to room temperature, add platinum catalyst, and stir under vacuum for 30 minutes to obtain component A;

[0109] (2) Add divinyl silicone oil-1, terminal hydrogen silicone oil, hydrogen-containing organopolysiloxane, zinc oxide, aluminum nitride, diamond powder, and dodecyltrimethylsiloxane into a reaction kettle, stir at 100° C. for 4 hours, cool to room temperature, add 3-methyl-1-butyn-3-ol, and stir under vacuum for 30 minutes to obtain component B;

[0110] (3) The component A prepared in step (1) and the component B prepared in step (2) are mixed evenly to obtain a two-component thermally conductive gel.

[0111] Comparative Example 1

[0112] The difference between Comparative Example 1 and Example 1 is that Comparative Example 1 does not contain a tackifier, and the tackifier of component A is replaced by an equal amount of silane coupling agent KH560, and the rest are the same.

[0113] Comparative Example 2

[0114] The difference between Comparative Example 2 and Example 1 is that Comparative Example 2 does not contain hydrogen-containing organopolysiloxane, and is replaced by an equal amount of side hydrogen-containing silicone oil D-018-120, and the rest are the same.

[0115] Comparative Example 3

[0116] The difference between Comparative Example 3 and Example 1 is that Comparative Example 3 does not contain terminal hydrogen-containing silicone oil, and the other parts are the same.

[0117] The two-component thermally conductive gel of this comparative example includes component A and component B:

[0118] The component A comprises the following components in parts by mass: 100 parts of divinyl silicone oil-1, 300 parts of zinc oxide with a D50 of 1 μm, 800 parts of aluminum nitride with a D50 of 7 μm, 1500 parts of diamond powder with a D50 of 80 μm, 5 parts of tackifier, 2.5 parts of dodecyl trimethylsiloxane, and 0.2 parts of platinum catalyst;

[0119] The B component includes the following components in parts by mass: 100 parts of divinyl silicone oil-1, 2 parts of hydrogen-containing organic polysiloxane, 300 parts of zinc oxide with a D50 of 1 μm, 800 parts of aluminum nitride with a D50 of 7 μm, 1500 parts of diamond powder with a D50 of 80 μm, 2.5 parts of dodecyl trimethylsiloxane, and 0.02 parts of 3-methyl-1-butyn-3-ol.

[0120] Comparative Example 4

[0121] The difference between Comparative Example 4 and Example 1 is that Comparative Example 4 uses vinyl silicone oil-2 to replace divinyl silicone oil-1, and the other parts are the same.

[0122] Comparative Example 5

[0123] The difference between Comparative Example 5 and Example 1 is that Comparative Example 5 uses vinyl silicone oil-3 to replace divinyl silicone oil-1, and the other parts are the same.

[0124] Test Case

[0125] The performance of the two-component thermally conductive gel obtained in the above examples and comparative examples was characterized, and the specific test items, test methods and results are as follows:

[0126] 1. Thermal conductivity: For specific test methods, refer to standard ASTM D5470.

[0127] 2. Viscosity: For specific test methods, refer to standard GB / T 10247.

[0128] 3. Hardness: Refer to ASTM D2240 for specific test methods.

[0129] 4. Tensile shear strength: For specific test methods, refer to standard GB / T 7124.

[0130] Table 1 Test results of the two-component thermally conductive gel obtained in the examples and comparative examples

[0131]

[0132] Comparative Examples 1 to 5 show that by controlling the raw materials of component A and component B within the following defined range, the performance is further improved: the component A comprises the following components in parts by mass: 100 parts of divinyl silicone oil-1, 300 parts of zinc oxide with a D50 of 1 μm, 800 parts of aluminum nitride with a D50 of 7 μm, 1500 parts of diamond powder with a D50 of 80 μm, 5 parts of tackifier, 2.5 parts of dodecyl trimethyl siloxane, and 0.2 parts of platinum catalyst; the component B comprises the following components in parts by mass: 100 parts of divinyl silicone oil-1, 6 parts of terminal hydrogenated silicone oil, 2 parts of hydrogen-containing organic polysiloxane, 300 parts of zinc oxide with a D50 of 1 μm, 800 parts of aluminum nitride with a D50 of 7 μm, 1500 parts of diamond powder with a D50 of 80 μm, 2.5 parts of dodecyl trimethyl siloxane, and 0.02 parts of 3-methyl-1-butyn-3-ol. By controlling the raw materials of component A and component B within this limited range, the performance is further improved.

[0133] By comparing Example 1 with Comparative Examples 1 to 2, it can be seen that in the present invention, the tackifier and the hydrogen-containing organopolysiloxane are both indispensable and irreplaceable. If other raw materials are used to replace them, the tackifier and the hydrogen-containing organopolysiloxane cannot play a synergistic role, thereby significantly reducing the performance.

[0134] By comparing Example 1 with Comparative Example 3, it can be seen that in the present invention, terminal hydrogen-containing silicone oil is also indispensable. If terminal hydrogen-containing silicone oil is lacking, the performance will be significantly reduced.

[0135] By comparing Example 1 with Comparative Examples 4 to 5, it can be seen that if the viscosity of the vinyl silicone oil is not within the range of the present invention, the performance will be significantly reduced.

[0136] Finally, it should be noted that the above embodiments are only used to illustrate the technical solution of the present invention rather than to limit the scope of protection of the present invention. Although the present invention has been described in detail with reference to the preferred embodiments, those skilled in the art should understand that the technical solution of the present invention can be modified or replaced by equivalents without departing from the essence and scope of the technical solution of the present invention.

Claims

1. A two-component thermally conductive gel, characterized in that: Including component A and component B: The component A comprises the following components in parts by mass: 100 parts of vinyl silicone oil A, 1500-3000 parts of thermal conductive filler A, and 0.5-10 parts of tackifier; The B component includes the following components in parts by mass: 100 parts of vinyl silicone oil B, 2 to 10 parts of terminal hydrogen-containing silicone oil, 1 to 6 parts of hydrogen-containing organopolysiloxane, and 1500 to 3000 parts of thermal conductive filler B; The viscosity of the vinyl silicone oil A and the vinyl silicone oil B are both 300cps-2000cps; The structural formula of the tackifier is shown in formula (1): Formula (1) Wherein, m is a positive integer between 10 and 50, and n is a positive integer between 10 and 50; The structural formula of the hydrogen-containing organopolysiloxane is shown in formula (3): Formula (3) Wherein, a is a positive integer between 10 and 50, b is a positive integer between 10 and 50, and c is a positive integer between 10 and 50; R is C 12 ~C 20 alkyl.

2. The two-component thermally conductive gel according to claim 1, characterized in that: The vinyl silicone oil A and the vinyl silicone oil B are independently selected from at least one of side hydroxyl-terminated vinyl silicone oil, single-terminated vinyl silicone oil, double-terminated vinyl silicone oil, T-structured vinyl silicone oil, and phenyl vinyl silicone oil; and / or The hydrogen content of the hydrogen-terminated silicone oil is 0.08%-0.3% by mass.

3. The two-component thermally conductive gel according to claim 1, characterized in that: The preparation method of the tackifier comprises the following steps: Add terminal hydrogen silicone oil, 4-vinyl-1,2-epoxycyclohexane, solvent and catalyst into a reaction container, react under nitrogen atmosphere, and evacuate to obtain a tackifier; The structural formula of the end-side hydrogen silicone oil is shown in formula (2): Formula (2) Wherein, m is a positive integer between 10 and 50, and n is a positive integer between 10 and 50.

4. The two-component thermally conductive gel according to claim 3, characterized in that: The mass ratio of the terminal hydrogen silicone oil, 4-vinyl-1,2-epoxycyclohexane and the solvent is 1: (0.2-0.5): (1-10); and / or The solvent comprises at least one of toluene, xylene and cyclohexane; and / or The catalyst comprises at least one of a Custer catalyst, a chloroplatinic acid catalyst, and a chloroplatinic acid-isopropanol solution catalyst.

5. The two-component thermally conductive gel according to claim 1, characterized in that: The thermally conductive filler A and the thermally conductive filler B are each independently selected from a combination of a first thermally conductive filler, a second thermally conductive filler and a third thermally conductive filler; The mass ratio of the first thermally conductive filler, the second thermally conductive filler, and the third thermally conductive filler is (1-4): (4-10): (5-15); The first thermally conductive filler, the second thermally conductive filler, and the third thermally conductive filler are each independently selected from one of aluminum oxide, zinc oxide, magnesium oxide, silicon dioxide, aluminum nitride, boron nitride, aluminum carbide, silicon carbide, aluminum hydroxide, magnesium hydroxide, boehmite, and diamond; The D50 of the first thermally conductive filler is 0.3-1.5 μm; The D50 of the second thermally conductive filler is 3-10 μm; The D50 of the third thermally conductive filler is 40-100 μm.

6. The two-component thermally conductive gel according to claim 1, characterized in that: The A component further comprises 0.1 to 5 parts of a catalyst; and / or The component A further comprises 0.5 to 10 parts of a coupling aid A; and / or The B component further comprises 0.01 to 2 parts of an inhibitor; and / or The B component also includes 0.5 to 10 parts of coupling aid B.

7. The method for preparing the two-component thermally conductive gel according to claim 6, characterized in that: The following steps are involved: Add vinyl silicone oil A, thermal conductive filler A, tackifier, and coupling aid A into a reaction kettle, stir evenly, add a catalyst, stir evenly, and obtain component A; Vinyl silicone oil B, hydrogen-terminated silicone oil, hydrogen-containing organopolysiloxane, thermal conductive filler B, and coupling aid B are mixed evenly, an inhibitor is added, and the mixture is mixed evenly to obtain component B; Component A and component B are mixed evenly to obtain a two-component thermal conductive gel.

8. Use of the two-component thermally conductive gel according to any one of claims 1 to 5 in electronic components and power batteries.

Citation Information

Patent Citations

  • Two-component heat-conducting gel as well as preparation method and application thereof

    CN113736266A

  • Low viscosity and high thermal conductivity organosilicon gel and preparation method thereof

    CN110330946A

  • Epoxy organic silica gel as well as preparation method and application thereof

    CN115637130A

Cited By

  • Preparation and application of gel material based on metformin and oleanolic acid medicine

    CN117159450A