Heat-conducting gel as well as application and use method thereof

Abstract

The invention discloses heat-conducting gel and application and a using method thereof, the heat-conducting gel comprises a component A and a component B in a mass ratio of 1: 1, the component A comprises the following components in parts by weight: 30-55 parts of vinyl fluorosilicone oil, 1-2.5 parts of terminal hydrogen-containing fluorosilicone oil, 5-10 parts of side hydrogen-containing fluorosilicone oil, 0.1-0.25 part of a catalyst, 0.05-0.2 part of an inhibitor, 1725-2600 parts of composite heat-conducting filler and 15-25 parts of silicon carbide nanowires; the component B is prepared from the following components in parts by weight: 30 to 55 parts of vinyl fluorosilicone oil, 1 to 2.5 parts of terminal hydrogen-containing fluorosilicone oil, 2.5 to 5 parts of catalyst, 1725 to 2600 parts of composite heat-conducting filler and 15 to 25 parts of silicon carbide nanowire. The heat-conducting gel provided by the invention has excellent heat-conducting property, anti-swelling property and anti-settling property.

Description

Technical Field

[0001] This invention belongs to the field of thermal conductive materials technology, specifically relating to a thermal conductive gel and its application and usage method. Background Technology

[0002] With the development of high-power-density electronic devices such as data centers, high-performance computing chips, and 5G base stations, traditional air cooling and indirect liquid cooling are no longer sufficient to meet heat dissipation requirements. Immersion liquid cooling technology has become the mainstream development direction due to its advantages such as high efficiency, low noise, and energy saving. However, this technology places stringent requirements on thermal interface materials (TIMs): the materials must be immersed in fluorinated or hydrocarbon coolants for extended periods while maintaining structural stability, not swelling, not precipitating, and possessing high thermal conductivity to achieve efficient heat transfer between the chip and the coolant.

[0003] In existing technologies, conventional organosilicon thermal conductive gels, while possessing good flexibility and interfacial wettability, are prone to swelling, softening, or even dissolution in fluorinated liquids or hydrocarbon coolants, leading to increased thermal resistance and decreased mechanical strength, severely impacting system reliability. For example, CN119371828A discloses a two-component addition-type thermal conductive gel using a crosslinking system of vinyl silicone oil and hydrogen-containing silicone oil, filled with thermally conductive fillers such as alumina and aluminum hydroxide, but it does not consider its application stability in immersion cooling scenarios; another example is CN119931357A, which reports a method for preparing a two-component fluorosilicone gel, providing good elasticity, no oil seepage, and good solvent resistance, but with relatively low thermal conductivity.

[0004] In addition, although high-filling thermally conductive fillers (such as diamond, aluminum nitride, and boron nitride) can improve thermal conductivity, they can also lead to a sharp increase in the viscosity of the gel system, making it difficult to process and causing severe sedimentation during storage or use, resulting in uneven local thermal performance.

[0005] Therefore, there is an urgent need to develop a novel thermal interface gel material that combines high thermal conductivity and anti-settling properties and can be applied to immersion liquid cooling scenarios. Summary of the Invention

[0006] In view of the shortcomings of the prior art, the purpose of this invention is to provide a thermally conductive gel and its application and usage method.

[0007] To achieve this objective, the present invention adopts the following technical solution: In a first aspect, the present invention provides a thermally conductive gel comprising component A and component B in a mass ratio of 1:1, wherein: Component A, by weight, comprises: Vinyl fluorosilicone oil 30-55 parts, end-containing hydrofluorosilicone oil 1-2.5 parts, side-containing hydrofluorosilicone oil 5-10 parts, catalyst 0.1-0.25 parts, inhibitor 0.05-0.2 parts, composite thermally conductive filler 1725-2600 parts, silicon carbide nanowires 15-25 parts; Component B, by weight, comprises: Vinyl fluorosilicone oil 30-55 parts, end-hydrogen fluorosilicone oil 1-2.5 parts, catalyst 2.5-5 parts, composite thermally conductive filler 1725-2600 parts, silicon carbide nanowires 15-25 parts.

[0008] This invention constructs a three-dimensional network with a dual hydrophobic framework of "fluorine-silicone" by using vinyl fluorosilicone oil and hydrofluorosilicone oil (end-containing hydrofluorosilicone oil and side-containing hydrofluorosilicone oil) as base polymers and carrying out an addition curing reaction of the base polymers. The fluorine groups can endow the thermally conductive gel with low surface energy and chemical inertness to fluorinated liquids / hydrocarbon liquids, giving the thermally conductive gel excellent anti-swelling properties, which can meet the application requirements of immersion liquid cooling.

[0009] Meanwhile, by introducing silicon carbide nanowires, this invention not only has a thermal conductivity but also forms a spatial steric hindrance network through "entanglement." Through the interaction of van der Waals forces with the composite thermally conductive filler, it increases the dispersibility of the composite thermally conductive filler and inhibits its sedimentation.

[0010] Therefore, the thermally conductive gel provided by the present invention has excellent thermal conductivity, anti-swelling properties, and anti-settling properties.

[0011] In component A of this invention, the 30-55 parts of vinyl fluorosilicone oil can be 30 parts, 35 parts, 40 parts, 45 parts, 50 parts, 55 parts, etc.; the 1-2.5 parts of end-containing hydrofluorosilicone oil can be 1 part, 1.2 parts, 1.5 parts, 1.8 parts, 2 parts, 2.2 parts, 2.5 parts, etc., but are not limited to the listed values. Other unlisted point values ​​or range values ​​within the numerical range are also applicable; the 5-10 parts of side-containing hydrofluorosilicone oil can be 5 parts, 6 parts, 7 parts, etc. The amounts can be 8 parts, 9 parts, 10 parts, etc., but are not limited to the listed values. Other unlisted values ​​or ranges within the same range are also applicable. The catalyst (0.1-0.25 parts) can be 0.1 parts, 0.12 parts, 0.15 parts, 0.18 parts, 0.2 parts, 0.22 parts, 0.25 parts, etc., but are not limited to the listed values. Other unlisted values ​​or ranges within the same range are also applicable. The inhibitor (0.05-0.2 parts) can be 0.05 parts... The amounts are specified as 0.08 parts, 0.1 parts, 0.12 parts, 0.15 parts, 0.18 parts, 0.2 parts, etc., but are not limited to the listed values. Other unlisted point values ​​or range values ​​within the same range are also applicable. The 1725-2600 parts of the composite thermally conductive filler can be 1725 parts, 1750 parts, 1800 parts, 1850 parts, 1900 parts, 1950 parts, 2000 parts, 2050 parts, 2100 parts, 2150 parts, 2200 parts, etc. 2250 parts, 2300 parts, 2350 parts, 2400 parts, 2450 parts, 2500 parts, 2550 parts, 2600 parts, etc., but not limited to the listed values. Other unlisted point values ​​or range values ​​within the value range are also applicable. The 15-25 parts of silicon carbide nanowires can be 15 parts, 16 parts, 18 parts, 20 parts, 22 parts, 25 parts, etc., but not limited to the listed values. Other unlisted point values ​​or range values ​​within the value range are also applicable.

[0012] In component B of this invention, the 30-55 parts of vinyl fluorosilicone oil can be 30 parts, 35 parts, 40 parts, 45 parts, 50 parts, 55 parts, etc., but are not limited to the listed values. Other unlisted values ​​or ranges within the numerical range are also applicable. The 1-2.5 parts of end-containing hydrofluorosilicone oil can be 1 part, 1.2 parts, 1.5 parts, 1.8 parts, 2 parts, 2.2 parts, 2.5 parts, etc., but are not limited to the listed values. Other unlisted values ​​or ranges within the numerical range are also applicable. The 2.5-5 parts of catalyst can be 2.5 parts, 2.8 parts, 3 parts, 3.2 parts, 3.5 parts, 4 parts, 4.5 parts, 5 parts, etc., but are not limited to the listed values. Other unlisted values ​​or ranges within the numerical range are also applicable. The 1725-2600 parts of the composite thermally conductive filler can be 1725 parts, 1750 parts, 1800 parts, 1850 parts, 1900 parts, 1950 parts, 2000 parts, 2050 parts, 2100 parts, 2150 parts, 2200 parts, 2250 parts, 2300 parts, 2350 parts, 2400 parts, 2450 parts, 2500 parts, 2550 parts, 2600 parts, etc., but are not limited to the listed values. Other unlisted point values ​​or range values ​​within the value range are also applicable. The 15-25 parts of the silicon carbide nanowire can be 15 parts, 16 parts, 18 parts, 20 parts, 22 parts, 25 parts, etc., but are not limited to the listed values. Other unlisted point values ​​or range values ​​within the value range are also applicable.

[0013] It should be noted that in this invention, components with the same name in components A and B, such as vinyl fluorosilicone oil, end-hydrogen fluorosilicone oil, catalyst, composite thermally conductive filler, and silicon carbide nanowires, can be completely identical or be similar materials with different parameters. In order to facilitate the preparation and application of thermally conductive gel, this invention preferably uses the same components, which will not be elaborated further here.

[0014] Preferably, the vinyl fluorosilicone oil comprises 25-40 parts of double-ended vinyl fluorosilicone oil, such as 25 parts, 26 parts, 28 parts, 30 parts, 32 parts, 35 parts, 38 parts, 40 parts, etc., but not limited to the listed values. Other unlisted point values ​​or range values ​​within the value range are also applicable. The single-ended vinyl fluorosilicone oil comprises 5-15 parts, such as 5 parts, 6 parts, 8 parts, 10 parts, 12 parts, 14 parts, 15 parts, etc., but not limited to the listed values. Other unlisted point values ​​or range values ​​within the value range are also applicable.

[0015] In this invention, the vinyl fluorosilicone oil in components A and B is the same component, each including 25-40 parts of double-ended vinyl fluorosilicone oil, such as 25 parts, 26 parts, 28 parts, 30 parts, 32 parts, 35 parts, 38 parts, 40 parts, etc., but not limited to the listed values. Other unlisted point values ​​or range values ​​within the value range are also applicable. The single-ended vinyl fluorosilicone oil is 5-15 parts, such as 5 parts, 6 parts, 8 parts, 10 parts, 12 parts, 14 parts, 15 parts, etc., but not limited to the listed values. Other unlisted point values ​​or range values ​​within the value range are also applicable.

[0016] Preferably, the viscosity of the dual-terminated vinyl fluorosilicone oil is 500-20000 mPa·s, such as 500 mPa·s, 1000 mPa·s, 2000 mPa·s, 5000 mPa·s, 8000 mPa·s, 10000 mPa·s, 12000 mPa·s, 15000 mPa·s, 18000 mPa·s, 20000 mPa·s, etc., but is not limited to the listed values. Other unlisted point values ​​or range values ​​within the numerical range are also applicable.

[0017] Preferably, the viscosity of the single-ended vinyl fluorosilicone oil is 100-1000 mPa·s, such as 100 mPa·s, 200 mPa·s, 300 mPa·s, 400 mPa·s, 500 mPa·s, 600 mPa·s, 700 mPa·s, 800 mPa·s, 900 mPa·s, 1000 mPa·s, etc., but is not limited to the listed values. Other unlisted point values ​​or range values ​​within the numerical range are also applicable.

[0018] Preferably, the vinyl content of the double-ended vinyl fluorosilicone oil and the single-ended vinyl fluorosilicone oil is independently selected from 0.05-0.5%, such as 0.05%, 0.1%, 0.15%, 0.2%, 0.25%, 0.3%, 0.35%, 0.4%, 0.45%, 0.5%, etc., but is not limited to the listed values. Other unlisted point values ​​or range values ​​within the value range are also applicable.

[0019] Preferably, the fluorine content in the double-ended vinyl fluorosilicone oil and the single-ended vinyl fluorosilicone oil is independently selected from 5-12%, such as 5%, 6%, 7%, 8%, 9%, 10%, 11%, 12%, etc., but is not limited to the listed values. Other unlisted point values ​​or range values ​​within the value range are also applicable.

[0020] Preferably, the hydrogen content of the end-containing hydrofluoric silicone oil is 0.05-0.1%, such as 0.05%, 0.06%, 0.07%, 0.08%, 0.09%, 0.1%, etc., but is not limited to the listed values. Other unlisted point values ​​or range values ​​within the value range are also applicable.

[0021] Preferably, the hydrogen content of the hydrofluoric silicone oil is 0.05-0.5%, for example, 0.05%, 0.1%, 0.15%, 0.2%, 0.25%, 0.3%, 0.35%, 0.4%, 0.45%, 0.5%, but is not limited to the listed values. Other unlisted point values ​​or range values ​​within the numerical range are also applicable.

[0022] Preferably, the fluorine content in the end-containing hydrofluoric silicone oil and the side-containing hydrofluoric silicone oil is independently selected from 0.05-0.5%, for example 0.05%, 0.1%, 0.15%, 0.2%, 0.25%, 0.3%, 0.35%, 0.4%, 0.45%, 0.5%, but is not limited to the listed values. Other unlisted point values ​​or range values ​​within the numerical range are also applicable.

[0023] Preferably, the composite thermally conductive filler includes at least two of diamond, aluminum nitride, and aluminum oxide, and more preferably includes a combination of diamond, aluminum nitride, and aluminum oxide.

[0024] Preferably, the diamond includes modified diamond A and modified diamond B.

[0025] Preferably, the particle size D50 of the modified diamond A is 120-180 μm, such as 120 μm, 130 μm, 140 μm, 150 μm, 160 μm, 170 μm, 180 μm, etc., but is not limited to the listed values. Other unlisted point values ​​or range values ​​within the numerical range are also applicable.

[0026] Preferably, the particle size D50 of the modified diamond B is 40-45 μm, such as 40 μm, 41 μm, 42 μm, 43 μm, 44 μm, 45 μm, etc., but is not limited to the listed values. Other unlisted point values ​​or range values ​​within the numerical range are also applicable.

[0027] Preferably, the aluminum nitride includes modified aluminum nitride, and the particle size D50 of the modified aluminum nitride is preferably 2-5 μm, such as 2 μm, 2.5 μm, 3 μm, 3.5 μm, 4 μm, 4.5 μm, 5 μm, etc., but not limited to the listed values. Other unlisted point values ​​or range values ​​within the numerical range are also applicable.

[0028] Preferably, the alumina comprises modified single-crystal ultrafine alumina, and the particle size D50 of the modified single-crystal ultrafine alumina is preferably 0.4-1 μm, such as 0.4 μm, 0.5 μm, 0.6 μm, 0.7 μm, 0.8 μm, 0.9 μm, 1 μm, etc., but is not limited to the listed values. Other unlisted point values ​​or range values ​​within the numerical range are also applicable.

[0029] Preferably, the composite thermally conductive filler in components A and B of the present invention is the same. By weight, the composite thermally conductive filler includes 1250-1750 parts of modified diamond A, for example, 1250 parts, 1300 parts, 1350 parts, 1400 parts, 1450 parts, 1500 parts, 1550 parts, 1600 parts, 1650 parts, 1700 parts, 1750 parts, etc., but is not limited to the listed values. Other unlisted point values ​​or range values ​​within the numerical range are also applicable. Modified diamond B... 150-250 parts, such as 150 parts, 160 parts, 170 parts, 180 parts, 190 parts, 200 parts, 210 parts, 220 parts, 230 parts, 240 parts, 250 parts, etc., but not limited to the listed values. Other unlisted point values ​​or range values ​​within the value range are also applicable. 300-500 parts of modified aluminum nitride, such as 300 parts, 320 parts, 350 parts, 380 parts, 400 parts, 420 parts, 450 parts, 480 parts, 500 parts, etc., but not limited to the listed values. Other unlisted point values ​​or range values ​​within the value range are also applicable. 25-100 parts of modified single-crystal ultrafine alumina, such as 25 parts, 30 parts, 40 parts, 50 parts, 60 parts, 70 parts, 80 parts, 90 parts, 100 parts, etc., but not limited to the listed values. Other unlisted point values ​​or range values ​​within the value range are also applicable.

[0030] This invention introduces a multi-scale composite thermally conductive filler system, in which diamond mainly serves to construct thermally conductive pathways, while small-particle-size aluminum nitride and / or aluminum oxide can fill voids and improve compactness; at the same time, the multi-scale composite thermally conductive filler system can also reduce the viscosity of the slurry during the preparation process through particle size energy level matching, which is beneficial to the preparation process.

[0031] Preferably, the average diameter of the silicon carbide nanowire is 50-100 nm, such as 50 nm, 60 nm, 70 nm, 80 nm, 90 nm, 100 nm, etc., but is not limited to the listed values. Other unlisted point values ​​or range values ​​within the numerical range are also applicable.

[0032] Preferably, the average length of the silicon carbide nanowire is 10-30 μm, such as 10 μm, 12 μm, 15 μm, 18 μm, 20 μm, 22 μm, 25 μm, 28 μm, 30 μm, etc., but is not limited to the listed values. Other unlisted point values ​​or range values ​​within the numerical range are also applicable.

[0033] Preferably, the catalyst is a platinum catalyst, and the platinum content is preferably 1000-10000 ppm, such as 1000 ppm, 2000 ppm, 3000 ppm, 4000 ppm, 5000 ppm, 6000 ppm, 7000 ppm, 8000 ppm, 9000 ppm, 10000 ppm, etc., but not limited to the listed values. Other unlisted point values ​​or range values ​​within the numerical range are also applicable.

[0034] The present invention preferably uses platinum catalysis for multi-stage temperature crosslinking, and more preferably uses Karstedt catalyst (platinum content of 2000-10000 ppm), which can achieve rapid curing at room temperature without byproducts.

[0035] In one specific embodiment of the present invention, the thermally conductive gel comprises component A and component B in a mass ratio of 1:1, wherein: Component A, by weight, comprises: 25-40 parts of double-ended vinyl fluorosilicone oil; 5-15 parts of single-ended vinyl fluorosilicone oil; Contains 1-2.5 parts of hydrofluoric silicone oil; Contains 5-10 parts of hydrofluoric silicone oil; Platinum catalyst 0.1-0.25 parts; Inhibitor 0.05-0.2 parts; Modified diamond A1250-1750 parts; Modified diamond B 150-250 parts; 300-500 parts of modified aluminum nitride; 25-100 parts of modified single-crystal ultrafine alumina; 15-25 parts of silicon carbide nanowires; Component B, by weight, comprises: 25-40 parts of double-ended vinyl fluorosilicone oil; 5-15 parts of single-ended vinyl fluorosilicone oil; Contains 1-2.5 parts of hydrofluoric silicone oil; Platinum catalyst 2.5-5 parts; Modified diamond A1250-1750 parts; Modified diamond B 150-250 parts; 300-500 parts of modified aluminum nitride; 25-100 parts of modified single-crystal ultrafine alumina; 15-25 parts of silicon carbide nanowires.

[0036] The thermally conductive gel provided by this invention has the following advantages: i. Excellent resistance to swelling: The thermally conductive gel provided by this invention still has excellent chemical stability when immersed in fluorinated liquid / hydrocarbon coolant, which can inhibit swelling and maintain stable thermal conductivity. ii. Combining high thermal conductivity and good interfacial wettability, the thermally conductive gel provided by the present invention has a high thermal conductivity coefficient and excellent thermal conductivity performance, while maintaining good interfacial wettability, which is beneficial to heat transfer; iii. The thermally conductive gel provided by this invention can adapt to filling thermally conductive gaps in large-tolerance scenarios by relying on its own rheological properties in the gel state; iv. The thermally conductive gel provided by the present invention has excellent storage stability, which can suppress the sedimentation and stratification of composite thermally conductive fillers, and ensure that the thermally conductive gel still has excellent and uniform performance during long-term storage and use.

[0037] The present invention also provides a method for preparing the thermally conductive gel as described in the first aspect, the method comprising: (1) Mix the components in the prescribed amounts in component A to obtain component A; (2) Mix the components in the formula amount of component B to obtain component B.

[0038] As a preferred embodiment of the present invention, the preparation method includes: (1) Preparation of component A: The formulation amounts of double-ended vinyl fluorosilicone oil, single-ended vinyl fluorosilicone oil and platinum catalyst were mixed under vacuum stirring, heated to 120°C and stirred, and then hydrogen-containing fluorosilicone oil was added and mixed to obtain matrix A. Modified diamond A, modified diamond B, modified aluminum nitride, modified single-crystal ultrafine alumina, and silicon carbide nanowires are mixed to obtain powder A; Matrix A and powder A are mixed, and hydrofluoric silicone oil and inhibitor are added. Vacuum mixing and degassing are carried out at 90-100℃ and cooled to room temperature to obtain component A. (2) Preparation of component B: The formulation amounts of double-ended vinyl fluorosilicone oil, single-ended vinyl fluorosilicone oil and part of platinum catalyst were mixed under vacuum stirring, heated to 120°C and stirred, and then hydrogen-containing fluorosilicone oil was added and mixed to obtain matrix B. Modified diamond A, modified diamond B, modified aluminum nitride, modified single-crystal ultrafine alumina, and silicon carbide nanowires are mixed to obtain powder B; After mixing matrix B and powder B, the remaining platinum catalyst is added, and the mixture is vacuum degassed and mixed at a temperature of 90-100℃. After cooling to room temperature, component B is obtained.

[0039] In a second aspect, the present invention provides the application of the thermally conductive gel as described in the first aspect in a thermal interface material for immersion liquid cooling.

[0040] Thirdly, the present invention provides a method of using the thermally conductive gel as described in the first aspect, the method comprising: After mixing components A and B, apply the mixture to the surface to be used and allow it to cure.

[0041] Preferably, the curing temperature is 100-120℃, such as 100℃, 105℃, 110℃, 115℃, 120℃, etc., but not limited to the listed values. Other unlisted point values ​​or range values ​​within the value range are also applicable. The time is 20-30 min, such as 20 min, 21 min, 22 min, 23 min, 24 min, 25 min, 26 min, 27 min, 28 min, 29 min, 30 min, etc., but not limited to the listed values. Other unlisted point values ​​or range values ​​within the value range are also applicable.

[0042] As a specific embodiment of the present invention, the method of use includes: Components A and B are filled, mixed, extruded and applied to the interface to be used, and heated to 100-120℃ for 20-30 minutes to cure, in order to match the thermal conductivity requirements of uneven gaps and fully meet the application requirements of immersion liquid cooling.

[0043] Compared with the prior art, the present invention has the following beneficial effects: (1) Through molecular structure design and multi-scale filler synergy, this invention obtains a high thermal conductivity organosilicon gel that can be used in immersion liquid cooling environment, which solves the problems of filler sedimentation, easy swelling and thermal conductivity decay in existing gels in fluorinated liquids or hydrocarbon coolants. (2) The filler sedimentation rate of the thermally conductive gel provided by the present invention is <2%, the thermal conductivity of the cured material is ≥11.5 W / (m·K), and BLT=0.2 mm, which can perfectly fit the chip and the heat sink. At the same time, after soaking in 3M fluorinated liquid for 1000 hours, the volume swelling rate is ≤3%, and the thermal resistance attenuation rate of the sandwich module is ≤10%. (3) The thermally conductive gel provided by the present invention is compatible with existing dispensing processes and is suitable for large-scale production. Detailed Implementation

[0044] The technical solution of the present invention will be further illustrated below through specific embodiments. Those skilled in the art should understand that the embodiments described are merely illustrative of the present invention and should not be construed as limiting the invention in any way.

[0045] Unless otherwise specified, the raw materials involved in the following specific embodiments of the present invention are all conventional materials in the art, and can be purchased from commercially available products. Some raw material information is as follows: Double-ended vinyl fluorosilicone oil-1: viscosity 500 mPa·s, purchased from Anhui Handie Electronic Materials Co., Ltd., model 923; Double-ended vinyl fluorosilicone oil-2: viscosity 1000 mPa·s, purchased from Anhui Handie Electronic Materials Co., Ltd., model 925; Single-ended vinyl fluorosilicone oil-1; viscosity 100 mPa·s, purchased from Shandong Dongyue Polymer Materials Co., Ltd., model DY-FS10; Single-ended vinyl fluorosilicone oil-2; viscosity 500 mPa·s, purchased from Shandong Dongyue Polymer Materials Co., Ltd., model DY-FS50; Hydrofluoric silicone oil-1 with hydrogen content of 0.05%, purchased from Guangdong Chenxi New Material Technology Co., Ltd., model number 357; Hydrofluoric silicone oil-2 with hydrogen content of 0.15%, purchased from Guangdong Chenxi New Material Technology Co., Ltd., model number 359; Side-containing hydrofluoric silicone oil-1; H content is 0.5%, purchased from Guangdong Chenxi New Material Technology Co., Ltd., model number 560; Side-containing hydrofluoric silicone oil-2; H content is 1.0%, purchased from Guangdong Chenxi New Material Technology Co., Ltd., model number 580; Platinum catalyst: Karstedt catalyst, purchased from Zijun Chemical (Zhongshan) Co., Ltd., model PT2000; Inhibitor: Ethynyl alcohol, purchased from Zijun Chemical (Zhongshan) Co., Ltd., model PH; Modified diamond A-1: ​​with a particle size D50 of 150 μm, purchased from Changsha Moben New Materials Co., Ltd., model A150-1; Modified diamond A-2: with a particle size D50 of 120 μm, purchased from Changsha Moben New Materials Co., Ltd., model A120-1; Modified diamond B-1: particle size D50 is 45 μm, purchased from Changsha Moben New Materials Co., Ltd., model A45-1; Modified diamond B-2: particle size D50 is 45 μm, purchased from Changsha Moben New Materials Co., Ltd., model A45; Modified aluminum nitride-1: with a particle size D50 of 5 μm, purchased from Suzhou Jinyi New Material Technology Co., Ltd., model AN2-A; Modified aluminum nitride-2: particle size D50 is 2 μm, purchased from Suzhou Jinyi New Material Technology Co., Ltd., model AN5-A; Modified single-crystal ultrafine alumina-1: particle size D50 is 0.6 μm, purchased from Sumitomo Corporation, model AA-04; Modified single-crystal ultrafine alumina-2: with a particle size D50 of 1 μm, purchased from Ya'an Baitu High-tech Materials Co., Ltd., model NSM-1S; Silicon carbide nanowires-1: 30 μm in length, purchased from Xi'an Ruixi Biotechnology Co., Ltd., model SiC30; Silicon carbide nanowires-2: 10 μm in length, purchased from Xi'an Ruixi Biotechnology Co., Ltd., model SiC10; Example 1 This embodiment provides a thermally conductive gel and its preparation method, comprising component A and component B in a mass ratio of 1:1, wherein: Component A, by weight, comprises: Double-ended vinyl fluorosilicone oil - 135 parts; Single-ended vinyl fluorosilicone oil - 112.5 parts; End-containing hydrofluoric silicone oil - 12.5 parts; Side-containing hydrofluoric silicone oil - 15 parts; 0.25 parts platinum catalyst; Inhibitor 0.1 part; Modified diamond A-11400 parts; Modified diamond B-1177.5 parts; Modified aluminum nitride - 1350 parts; Modified single-crystal ultrafine alumina - 150 parts; Silicon carbide nanowires - 122.5 parts; Component B, by weight, comprises: Double-ended vinyl fluorosilicone oil - 135 parts; Single-ended vinyl fluorosilicone oil - 112.5 parts; End-containing hydrofluoric silicone oil - 12.5 parts; 5 parts platinum catalyst; Modified diamond A-11400 parts; Modified diamond B-1177.5 parts; Modified aluminum nitride - 1350 parts; Modified single-crystal ultrafine alumina - 150 parts; Silicon carbide nanowires - 122.5 parts.

[0046] The preparation method is as follows: (1) Preparation of component A: The formulated amounts of double-ended vinyl fluorosilicone oil, single-ended vinyl fluorosilicone oil and platinum catalyst were mixed under vacuum stirring, heated to 120°C and stirred, and then hydrogen-containing fluorosilicone oil was added and mixed for 2 h to obtain matrix A. Modified diamond A, modified diamond B, modified aluminum nitride, modified single-crystal ultrafine alumina and silicon carbide nanowires are mixed in a high-speed mixer to obtain powder A; Matrix A and powder A are mixed, and hydrofluoric silicone oil and inhibitor are added. Vacuum mixing and degassing are carried out for 4 h at 100℃. After cooling to room temperature, component A is obtained. (2) Preparation of component B: The formulation amounts of double-ended vinyl fluorosilicone oil, single-ended vinyl fluorosilicone oil and part of platinum catalyst were mixed under vacuum stirring, heated to 120°C and stirred, and then hydrogen-containing fluorosilicone oil was added and mixed for 2 h to obtain matrix B. Modified diamond A, modified diamond B, modified aluminum nitride, modified single-crystal ultrafine alumina, and silicon carbide nanowires are mixed to obtain powder B; After mixing matrix B and powder B, the remaining platinum catalyst was added, and the mixture was vacuum degassed and mixed for 4 h at 100°C. After cooling to room temperature, component B was obtained.

[0047] Example 2 This embodiment provides a thermally conductive gel and its preparation method.

[0048] The difference from Example 1 is that, in this example, single-ended vinyl fluorosilicone oil-1 is not added, and the weight parts of double-ended vinyl fluorosilicone oil-1 in components A and B are both 47.5 parts.

[0049] Example 3 This embodiment provides a thermally conductive gel and its preparation method.

[0050] The difference from Example 1 is that in this example, the modified diamond A-1 in components A and B is replaced with unmodified diamond (particle size D50 of 150 μm, purchased from Jiangxi Hengzuan, model UTC-90 / 100).

[0051] Example 4 This embodiment provides a thermally conductive gel and its preparation method.

[0052] The difference from Example 1 is that, in this example, no modified single-crystal ultrafine alumina-1 is added, and the weight parts of modified aluminum nitride-1 in components A and B are both 400 parts.

[0053] Example 5 This embodiment provides a thermally conductive gel and its preparation method, comprising component A and component B in a mass ratio of 1:1, wherein: Component A, by weight, comprises: Double-ended vinyl fluorosilicone oil - 225 parts; Single-ended vinyl fluorosilicone oil - 25 parts; End-containing hydrofluoric silicone oil - 21 parts; Side-containing hydrofluoric silicone oil - 25 parts; 0.1 parts platinum catalyst; Inhibitor 0.05 parts; Modified diamond A-21250 parts; Modified diamond B-2150 parts; Modified aluminum nitride - 2300 parts; Modified single-crystal ultrafine alumina - 225 parts; Silicon carbide nanowires - 215 parts; Component B, by weight, comprises: Double-ended vinyl fluorosilicone oil - 225 parts; Single-ended vinyl fluorosilicone oil - 25 parts; End-containing hydrofluoric silicone oil - 21 parts; Two parts of platinum catalyst; Modified diamond A-21250 parts; Modified diamond B-2150 parts; Modified aluminum nitride - 2300 parts; Modified single-crystal ultrafine alumina - 225 parts; Silicon carbide nanowires - 215 parts.

[0054] The preparation method is the same as in Example 1.

[0055] Example 6 This embodiment provides a thermally conductive gel and its preparation method, comprising component A and component B in a mass ratio of 1:1, wherein: Component A, by weight, comprises: Double-ended vinyl fluorosilicone oil - 140 parts; Single-ended vinyl fluorosilicone oil - 115 parts; End-containing hydrofluoric silicone oil - 12.5 parts; Side-containing hydrofluoric silicone oil - 110 parts; 0.25 parts platinum catalyst; Inhibitor 0.2 parts; Modified diamond A-11750 parts; Modified diamond B-1250 parts; Modified aluminum nitride - 1500 parts; Modified single-crystal ultrafine alumina - 1100 parts; Silicon carbide nanowires - 125 parts; Component B, by weight, comprises: Double-ended vinyl fluorosilicone oil - 140 parts; Single-ended vinyl fluorosilicone oil - 115 parts; End-containing hydrofluoric silicone oil - 12.5 parts; 5 parts platinum catalyst; Modified diamond A-11750 parts; Modified diamond B-1250 parts; Modified aluminum nitride - 1500 parts; Modified single-crystal ultrafine alumina - 1100 parts; Silicon carbide nanowires - 125 parts.

[0056] The preparation method is the same as in Example 1.

[0057] Comparative Example 1 This comparative example provides a thermally conductive gel and its preparation method.

[0058] The difference from Example 1 is that, in this comparative example, the double-ended vinyl fluorosilicone oil-1 in components A and B is replaced with vinyl silicone oil (viscosity 500 mPa·s, purchased from Guangdong Chenxi, model 1107A-500), and the single-ended vinyl fluorosilicone oil-1 is replaced with vinyl silicone oil (viscosity 100 mPa·s, purchased from Guangdong Chenxi, model 1107M-100).

[0059] Comparative Example 2 This comparative example provides a thermally conductive gel and its preparation method.

[0060] The difference from Example 1 is that, in this comparative example, the terminal hydrogen-containing fluorosilicone oil-1 in components A and B is replaced with terminal hydrogen-containing silicone oil (H content of 0.15%, purchased from Guangdong Chenxi, model 355), and the side-containing hydrogen-containing fluorosilicone oil-1 is replaced with side-containing silicone oil (H content of 0.5%, purchased from Guangdong Chenxi, model 386).

[0061] Comparative Example 3 This comparative example provides a thermally conductive gel and its preparation method.

[0062] The difference from Example 1 is that, in this comparative example, silicon carbide nanowires-1 in components A and B are omitted.

[0063] Comparative Example 4 This comparative example provides a thermally conductive gel and its preparation method.

[0064] The difference from Example 1 is that, in this comparative example, the double-ended vinyl fluorosilicone oil-1 in components A and B was replaced with vinyl silicone oil (viscosity 500 mPa·s, purchased from Guangdong Chenxi, model 1107A-500), the single-ended vinyl fluorosilicone oil-1 was replaced with vinyl silicone oil (viscosity 100 mPa·s, purchased from Guangdong Chenxi, model 1107M-100), the end-containing hydrogen fluorosilicone oil-1 was replaced with end-containing hydrogen silicone oil (H content 0.15%, purchased from Guangdong Chenxi, model 355), and the side-containing hydrogen fluorosilicone oil-1 was replaced with side-containing hydrogen silicone oil (H content 0.5%, purchased from Guangdong Chenxi, model 386).

[0065] Application Example 1 This application example provides a method of using the aforementioned thermally conductive gel, as follows: Components A and B are filled into 400cc EFD tubes and mixed evenly through 28 static mixing tubes using a pneumatic dispensing machine. The mixture is then extruded and rapidly cured by heating at 100℃ for 30 minutes.

[0066] Performance testing The performance of the thermally conductive gels provided in the examples and comparative examples, as well as the products after gel curing, was tested using the following methods: (1) Sedimentation rate: The sedimentation rates of thermally conductive gel components A and B were tested according to ASTM D 869 standard, and the larger value of the two was recorded. (2) Extrusion rate: Using 90 psi air pressure, 400CC tube, connected to 28 static mixing nozzles with an inner diameter of 10 mm, weigh the material extruded in 1 min; (3) Thermal conductivity: The product was cured according to Application Example 1, and the thermal conductivity of the cured product was tested according to ASTM D 5470 standard. (4) Electrical insulation performance: Dielectric strength was tested according to ASTM D 149 standard; (5) Hardness (SHORE C): The hardness of the product after curing is tested according to ASTM D 2240 standard; (6) Swelling rate: A 20×2×20 mm sample was immersed in fluorinated liquid (FC-3283) at a temperature of 110℃ for 1000 h. The volume change rate before and after immersion was tested and calculated as the swelling rate. (7) Thermal resistance change rate of sandwich module: The thermal resistance was tested according to ASTM D 5470 standard, and then soaked according to (6) to test the thermal resistance after soaking for 1000 h and calculate the thermal resistance change rate.

[0067] The test results are shown in Table 1: Table 1 As can be seen from the examples and performance tests, the thermally conductive gel provided by the present invention has excellent thermal conductivity, anti-swelling properties and anti-settling properties, and can meet the application requirements of immersion liquid cooling.

[0068] As can be seen from the comparison of Example 1 and Comparative Examples 1-2 and 4, both vinyl fluorosilicone oil and hydrogen fluorosilicone oil are indispensable in this invention. The absence of either one will prevent the thermally conductive gel from having excellent anti-swelling properties.

[0069] As can be seen from the comparison between Example 1 and Comparative Example 3, the silicon carbide nanowires in the thermally conductive gel provided by the present invention can increase the dispersibility of the composite thermally conductive filler, inhibit the sedimentation of the composite thermally conductive filler, and give the thermally conductive gel excellent anti-settling performance.

[0070] The present invention has been illustrated through the above embodiments, but the present invention is not limited to the above process steps, that is, it does not mean that the present invention must rely on the above process steps to be implemented. Those skilled in the art should understand that any improvements to the present invention, equivalent substitutions of the raw materials used in the present invention, additions of auxiliary components, and selection of specific methods, etc., all fall within the protection scope and disclosure scope of the present invention.

Claims

1. A thermally conductive gel, characterized in that, It includes component A and component B in a mass ratio of 1:1, wherein: Component A, by weight, comprises: Vinyl fluorosilicone oil 30-55 parts, end-containing hydrofluorosilicone oil 1-2.5 parts, side-containing hydrofluorosilicone oil 5-10 parts, catalyst 0.1-0.25 parts, inhibitor 0.05-0.2 parts, composite thermally conductive filler 1725-2600 parts, silicon carbide nanowires 15-25 parts; Component B, by weight, comprises: Vinyl fluorosilicone oil 30-55 parts, end-hydrogen fluorosilicone oil 1-2.5 parts, catalyst 2.5-5 parts, composite thermally conductive filler 1725-2600 parts, silicon carbide nanowires 15-25 parts.

2. The thermally conductive gel according to claim 1, characterized in that, The vinyl fluorosilicone oil comprises 25-40 parts of double-ended vinyl fluorosilicone oil and 5-15 parts of single-ended vinyl fluorosilicone oil. Preferably, the viscosity of the double-ended vinyl fluorosilicone oil is 500-20000 mPa·s; Preferably, the viscosity of the single-ended vinyl fluorosilicone oil is 100-1000 mPa·s.

3. The thermally conductive gel according to claim 1 or 2, characterized in that, The hydrogen content of the end-capped hydrogen-fluorinated silicone oil is 0.05-0.1%; Preferably, the hydrogen content of the hydrofluoric silicone oil is 0.05-0.5%.

4. The thermally conductive gel according to any one of claims 1-3, characterized in that, The composite thermally conductive filler includes at least two of diamond, aluminum nitride, and aluminum oxide, preferably a combination of diamond, aluminum nitride, and aluminum oxide.

5. The thermally conductive gel according to claim 4, characterized in that, The diamonds include modified diamond A and modified diamond B; Preferably, the particle size D50 of the modified diamond A is 120-180 μm; Preferably, the particle size D50 of the modified diamond B is 40-45 μm; Preferably, the aluminum nitride comprises modified aluminum nitride, and more preferably, the particle size D50 of the modified aluminum nitride is 2-5 μm; Preferably, the alumina comprises modified single-crystal ultrafine alumina, and more preferably, the particle size D50 of the modified single-crystal ultrafine alumina is 0.4-1 μm.

6. The thermally conductive gel according to claim 4 or 5, characterized in that, By weight, the composite thermally conductive filler comprises 1250-1750 parts of modified diamond A, 150-250 parts of modified diamond B, 300-500 parts of modified aluminum nitride, and 25-100 parts of modified single-crystal ultrafine alumina.

7. The thermally conductive gel according to any one of claims 1-6, characterized in that, The average diameter of the silicon carbide nanowires is 50-100 nm. Preferably, the average length of the silicon carbide nanowires is 10-30 μm.

8. The application of a thermally conductive gel as described in any one of claims 1-7 in a thermal interface material for immersion liquid cooling.

9. A method of using the thermally conductive gel as described in any one of claims 1-7, characterized in that, The method of use includes: After mixing components A and B, apply the mixture to the surface to be used and allow it to cure.

10. The method of use according to claim 9, characterized in that, The curing temperature is 100-120℃ and the time is 20-30 min.

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