A two-component thermal conductive gel with high thermal conductivity, low viscosity, and high thixotropy

Abstract

The present invention discloses a two-component thermal conductive gel with high thermal conductivity, low viscosity and high thixotropy. The modifier and the treating agent are respectively suitable for forming an intermolecular force network structure of polar molecules in the system of the thermal conductive component A and the gel component B, which is beneficial to the improvement of the thixotropy of the thermal conductive component A and the gel component B and the improvement of the room temperature storage stability. By compounding the linear isopropenyl-terminated silicone oil and the cyano-terminated silicone oil, and through the interaction with the modifier and the treating agent of the present invention respectively, the thixotropy and the room temperature stability of the A and B components are further improved. The two-component thermal conductive gel of the present invention has the properties of high thermal conductivity, low viscosity and high thixotropy, can resist sedimentation and phase separation at room temperature during storage, is high temperature resistant, and can be used at 200 °C.

Description

Technical Field

[0001] The present invention belongs to the technical field of thermal conductive gels, and particularly relates to a two-component thermal conductive gel with high thermal conductivity, low viscosity and high thixotropy. Background Art

[0002] A thermal conductive gel is a gel-like thermal conductive material made by compounding silica gel with thermal conductive fillers through kneading, stirring and encapsulation. It includes thermal conductive silicone grease made with various silicone resins as the matrix and adding metals with relatively high thermal conductivity such as silver, copper and aluminum, and also includes thermal conductive gel materials made with various silicone oils as the matrix and adding thermal conductive fillers such as zinc oxide, magnesium oxide, aluminum nitride and boron nitride, which are widely used in the heat dissipation of electronic components.

[0003] The thermal conductive gel has the advantages of good affinity, good weather resistance, high and low temperature resistance and insulation, and at the same time has strong plasticity and can be filled at uneven interfaces, which can meet the heat transfer requirements under various applications.

[0004] When the existing two-component gel is stored at room temperature, sedimentation and stratification will occur, and the use temperature cannot be too high, and it often cannot be used at 200 °C. Summary of the Invention

[0005] Object of the Invention: The technical problem to be solved by the present invention is to provide a two-component thermal conductive gel with high thermal conductivity, low viscosity and high thixotropy to avoid sedimentation and phase separation during storage at room temperature in view of the deficiencies of the prior art.

[0006] In order to achieve the above object of the invention, the technical solution adopted by the present invention is as follows:

[0007] A two-component thermal conductive gel with high thermal conductivity, low viscosity and high thixotropy, comprising a thermal conductive component A and a gel component B;

[0008] Among them, the thermal conductive component A includes the following components in parts by mass:

[0009] 3-5 parts of silicone oil capped with methacrylate group;

[0010] 2-5 parts of linear silicone oil capped with isopropenyl;

[0011] 1-3 parts of modifier;

[0012] 0.01-0.05 parts of crosslinking promoter;

[0013] Li7La3Zr2O 12 35-55 parts of fine powder;

[0014] 35-50 parts of La2Ce2O7 fine powder;

[0015] The gel component B includes the following components in parts by mass:

[0016] 5 - 8 parts of cyano - terminated silicone oil;

[0017] 5 - 8 parts of hydrogen - containing silicone oil;

[0018] 5 - 8 parts of treating agent;

[0019] 0.001 - 0.005 parts of complexing agent;

[0020] 40 - 50 parts of titanium monoxide fine powder;

[0021] 35 - 40 parts of MgFe2O4 fine powder.

[0022] Specifically, the heat - conducting component A and the gel component B are mixed according to a mass ratio of 1~1.2:1.

[0023] Specifically, in the heat - conducting component A, the dynamic viscosity of the methacrylate - terminated silicone oil is 200~300 cst, and the branching factor is 0.2~0.3; the dynamic viscosity of the linear isopropenyl - terminated silicone oil is 150~250 cst.

[0024] Specifically, in the heat - conducting component A, the modifier is a mixture of isooctyl stearate and isononyl gluconate according to a mass ratio of 1~1.2:1; the cross - linking promoter is any one or two of manganese oleate, nickel isostearate, and cobalt isodecanoate according to a mass ratio of 1~1.2:1.

[0025] Specifically, in the heat - conducting component A, the particle size of the Li7La3Zr2O 12 fine powder is 30~70 microns; the particle size of the La2Ce2O7 fine powder is 5~10 microns.

[0026] Specifically, in the heat - conducting component B, the dynamic viscosity of the cyano - terminated silicone oil is 200~300 cst, and the branching factor is 0.5~0.7; the dynamic viscosity of the hydrogen - containing silicone oil is 150~250 cst, and the branching factor is 0.3~0.5.

[0027] Specifically, in the heat - conducting component B, the treating agent is any one or two of phenyltriethoxysilane, hydrogenated castor oil, and palmitic acid according to a mass ratio of 1~1.2:1; the complexing agent is any one or two of oleylamine, dimethyl maleate, and tin benzoate according to a mass ratio of 1~1.2:1.

[0028] Specifically, in the heat - conducting component B, the particle size of the titanium monoxide fine powder is 20~50 microns; the particle size of the MgFe2O4 fine powder is 1~3 microns.

[0029] Furthermore, the present invention also provides a method for preparing the above-mentioned two-component thermal conductive gel with high thermal conductivity, low viscosity, and high thixotropy, which includes the following steps:

[0030] (1) Prepare thermal conductive component A:

[0031] Step A1: Add a part of linear isopropenyl-terminated silicone oil to the silicone oil terminated with methacrylate group, heat up to 40 - 60 °C, stir and mix, control the stirring rate at 300 - 500 revolutions per minute, stir for 10 - 30 minutes, and after stirring and cooling to room temperature, obtain the first mixed solution of component A;

[0032] Step A2: Perform ice-water bath stirring on the first mixed solution of component A obtained in step (A1), control the stirring rate at 300 - 500 revolutions per minute, slowly add the modifier, control the dropping time at 1 - 3 hours, and after the dropping is completed, stir for another 20 - 40 minutes to obtain the second mixed solution of component A;

[0033] Step A3: Keep ice-water bath stirring, control the stirring rate at 300 - 500 revolutions per minute, add the remaining formulated amount of linear isopropenyl-terminated silicone oil to the second mixed solution of component A obtained in step (A3), and stir for 1 - 3 hours to obtain the third mixed solution of component A;

[0034] Step A4: Keep ice-water bath stirring, control the stirring rate at 200 - 400 revolutions per minute, slowly add the crosslinking accelerator to the third mixed solution of component A obtained in step (A3), control the dropping time at 6 - 12 minutes, and after the dropping is completed, continue to stir for 3 - 5 minutes, and stir and heat up to room temperature under sealed conditions to obtain the fourth mixed solution of component A;

[0035] Step A5: Add Li7La3Zr2O 12 micropowder and La2Ce2O7 micropowder together to the fourth mixed solution of component A obtained in step (A4), stir at a speed of 1200 - 1600 revolutions per minute for 3 - 5 minutes, and then transfer to a three-roll grinder for grinding 10 - 20 times to obtain the first mixture of component A;

[0036] Step A6: Put the first mixture of component A obtained in step (A5) into a planetary vacuum degassing machine, evacuate to below 1 kPa, set the rotation speed at 800 - 1000 revolutions per minute, and degas for 3 - 5 minutes to obtain thermal conductive component A;

[0037] (2) Prepare gel component B:

[0038] Step B1: Add a part of cyano-terminated silicone oil to the hydrogen-containing silicone oil, heat up to 50 - 70 °C, stir and mix, control the stirring rate at 300 - 500 revolutions per minute, stir for 20 - 40 minutes, and after stirring and cooling to room temperature, obtain the first mixed solution of component B;

[0039] Step B2: Subject the first B-component mixture obtained in step (B2) to ice-water bath stirring, control the stirring rate at 300 - 500 revolutions per minute, add the treatment agent to the first B-component mixture, and stir for 10 - 30 minutes to obtain the second B-component mixture;

[0040] Step B3: Maintain ice-water bath stirring, control the stirring rate at 300 - 500 revolutions per minute, add the remaining amount of cyano-terminated silicone oil to the second B-component mixture obtained in step (B3), and stir for 1 - 3 hours to obtain the third B-component mixture;

[0041] Step B4: Maintain ice-water bath stirring, control the stirring rate at 200 - 400 revolutions per minute, slowly add the complexing agent dropwise to the third B-component mixture obtained in step (B3), control the dropping time at 6 - 12 minutes, after the dropping is completed, continue to stir for 3 - 5 minutes, and stir and heat up to room temperature under sealed conditions to obtain the fourth B-component mixture;

[0042] Step B5: Add titanium monoxide micropowder and MgFe2O4 micropowder together to the fourth B-component mixture obtained in step (B4) at a high speed of 1200 - 1600 revolutions per minute to obtain the first B-component mixture;

[0043] Step B6: Put the first B-component mixture obtained in step (B5) into a planetary vacuum defoaming machine, evacuate to below 1 kPa, set the rotation speed at 800 - 1000 revolutions per minute, and defoam for 3 - 5 minutes to obtain the gel component B;

[0044] (3) Preparation of the two-component thermal conductive gel:

[0045] Uniformly mix the obtained thermal conductive component A and gel component B in a weight ratio of 1:1, and then cure to obtain.

[0046] Specifically, in step A1, 25 - 35% of the linear isopropenyl-terminated silicone oil in the formula amount is added to the methacrylate-based silicone oil; in step B1, 40 - 60% of the cyano-terminated silicone oil in the formula amount is added to the hydrogen-containing silicone oil.

[0047] Beneficial effects:

[0048] (1) The modifiers and treatment agents used in the present invention are respectively suitable for forming an intermolecular force network structure of polar molecules in the systems of the thermal conductive component A and the gel component B, which is beneficial to the improvement of the thixotropy and room temperature storage stability of the thermal conductive component A and the gel component B.

[0049] (2) In the present invention, a linear isopropenyl-capped silicone oil is compounded with a cyano-capped silicone oil. By interacting with the modifier and the treatment agent described in the present invention respectively, the thixotropy and room-temperature stability of components A and B are further improved.

[0050] (3) In the formula of the present invention, the cyano-capped silicone oil is rich in capped cyano groups, which is beneficial to improving the high-temperature stability after the reaction of components A and B, so that the product cured from components A and B can be used at a temperature of 200 °C for a long time.

[0051] (4) The two-component thermal conductive gel of the present invention has the properties of high thermal conductivity, low viscosity, and high thixotropy. It can resist sedimentation and phase separation at room temperature during storage, is high-temperature resistant, and can be used at 200 °C. Specific Embodiments

[0052] The present invention can be better understood according to the following embodiments. Example 1

[0053] The two-component thermal conductive gel material of this example includes a thermal conductive component A and a gel component B, and the mass ratio of the thermal conductive component A to the gel component B is 1:1.

[0054] Among them, component A includes the following raw materials in parts by mass: 3 parts of modified silicone oil I, 2 parts of modified silicone oil II, 1 part of modifier, 0.01 part of crosslinking promoter, 35 parts of filler I, and 35 parts of filler II.

[0055] Component B includes the following raw materials in parts by mass: 5 parts of modified silicone oil III, 5 parts of modified silicone oil IV, 5 parts of treatment agent, 0.001 part of complexing agent, 40 parts of filler III, and 35 parts of filler IV.

[0056] In this example, the modified silicone oil I is a silicone oil capped with a branched factor of 0.2 methacrylate group and a kinematic viscosity of 200 cst, and the modified silicone oil II is a linear isopropenyl-capped silicone oil with a kinematic viscosity of 150 cst.

[0057] In this example, the modified silicone oil III is a silicone oil capped with a branched factor of 0.5 cyano group and a kinematic viscosity of 200 cst, and the modified silicone oil IV is a hydrogen-containing silicone oil with a branched factor of 0.3 and a kinematic viscosity of 150 cst.

[0058] In this example, the modifier is a mixture of isooctyl stearate and isononyl gluconate with a mass ratio of 1:1.

[0059] In this example, the crosslinking promoter is manganese oleate.

[0060] In this example, the filler I is Li7La3Zr2O with a particle size of 30 - 50 microns 12, filler two is La2Ce2O7 with a particle size of 5 - 7 microns, filler three is titanium monoxide with a particle size of 20 - 35 microns, and filler four is MgFe2O4 with a particle size of 1 - 2 microns.

[0061] In this embodiment, the treating agent is phenyltriethoxysilane.

[0062] In this embodiment, the complexing agent is oleylamine.

[0063] The preparation method of the two-component thermal conductive gel material in this embodiment includes the following steps:

[0064] Component A:

[0065] Step A1: Add 30% of the required amount of modified silicone oil two to all of the modified silicone oil one, heat up to 40 - 60 °C, stir and mix, control the stirring rate at 300 revolutions per minute, stir for 10 minutes, and after stirring and cooling to room temperature, obtain mixture one (A);

[0066] Step A2: Carry out ice-water bath stirring on the mixture one (A) obtained in step (A2), control the stirring rate at 300 revolutions per minute, slowly dropwise add the modifier, control the dropping time at 1 hour, and after the dropping is completed, stir for another 20 minutes to obtain mixture two (A);

[0067] Step A3: Keep the ice-water bath stirring, control the stirring rate at 300 revolutions per minute, add the remaining 50% of the modified silicone oil two to the mixture two (A) obtained in step (A3), and stir for 1 hour to obtain mixture three (A);

[0068] Step A4: Keep the ice-water bath stirring, control the stirring rate at 200 revolutions per minute, slowly dropwise add the crosslinking accelerator to the mixture three (A) obtained in step (A3), control the dropping time at 6 minutes, after the dropping is completed, continue to stir for 3 minutes, and stir and heat up to room temperature under sealed conditions to obtain mixture four (A);

[0069] Step A5: Add filler one and filler two together to the mixture four (A) obtained in step (A4), stir at a high speed of 1200 - 1600 revolutions per minute, stir for 3 minutes, and then transfer to a three-roll mill for grinding 10 times to obtain mixture one (A);

[0070] Step A6: Put the mixture one (A) obtained in step (A5) into a planetary vacuum degassing machine, evacuate to 1 kPa, set the rotation speed to 800 revolutions per minute, and degas for 3 minutes to obtain the component A mixture.

[0071] Component B:

[0072] Step B1: Add 50% of the required amount of Modified Silicone Oil III to all of Modified Silicone Oil IV, heat up to 50°C, stir and mix, control the stirring rate at 300 revolutions per minute, stir for 20 minutes, and after stirring and cooling to room temperature, obtain Mixture 1 (B);

[0073] Step B2: Carry out ice-water bath stirring on the obtained Mixture 1 (B) in Step (B2), control the stirring rate at 300 revolutions per minute, add the treating agent to Mixture 1 (B) at one time, and stir for 10 - 30 minutes to obtain Mixture 2 (B);

[0074] Step B3: Keep the ice-water bath stirring, control the stirring rate at 300 revolutions per minute, add the remaining 50% of Modified Silicone Oil III to the obtained Mixture 2 (A) in Step (B3), and stir for 1 hour to obtain Mixture 3 (B);

[0075] Step B4: Keep the ice-water bath stirring, control the stirring rate at 200 revolutions per minute, slowly add the crosslinking accelerator to the obtained Mixture 3 (B) in Step (B3), control the dropping time at 6 minutes, after the dropping is completed, continue to stir for 3 - 5 minutes, and stir and heat up to room temperature under sealed conditions to obtain Mixture 4 (B);

[0076] Step B5: Add Filler III and Filler IV together to the obtained Mixture 4 (B) in Step (B4) at a high speed of 1200 revolutions per minute to obtain Mixture 1 (B);

[0077] Step B6: Put the obtained Mixture 1 (B) in Step (B5) into a planetary vacuum defoaming machine, evacuate to 1 kPa, set the rotation speed at 800 revolutions per minute, and defoam for 3 minutes to obtain the B-component mixture;

[0078] The A-component and the B-component are uniformly mixed at a weight ratio of 1:1 and cured.

[0079] After testing, the viscosities of the obtained A-component and B-component are 460000 cp and 470000 cp respectively (7# rotor, 10 rpm), the thixotropy indices (7# rotor, η 10rpm / η 1rpm ) are 14.6 and 14.4 respectively, and the thermal conductivities are 5.9 W / (m・K) and 6.0 W / (m・K) respectively.

[0080] The thermal conductivity of the A-component and the B-component after reaction is 5.9 W / (m・K). After being treated at 200°C for 1000 hours, the change rate of the thermal conductivity is 2.5%. After being treated at 200°C for 5000 hours, the change rate of the thermal conductivity is 3.7%. Example 2

[0081] The two-component thermal conductive gel material of this embodiment includes a thermal conductive component A and a gel component B, and the mass ratio of the thermal conductive component A to the gel component B is 1.2:1.

[0082] Among them, component A includes the following raw materials in parts by mass: 5 parts of modified silicone oil I, 5 parts of modified silicone oil II, 3 parts of modifier, 0.05 part of crosslinking promoter, 55 parts of filler I, and 50 parts of filler II.

[0083] Component B includes the following raw materials in parts by mass: 8 parts of modified silicone oil III, 8 parts of modified silicone oil IV, 8 parts of treating agent, 0.005 part of complexing agent, 50 parts of filler III, and 40 parts of filler IV.

[0084] In this embodiment, the modified silicone oil I is a silicone oil capped with a branching factor of 0.3 methacrylate group and a kinematic viscosity of 300 cst, and the modified silicone oil II is a linear isopropenyl-capped silicone oil with a kinematic viscosity of 150 cst.

[0085] In this embodiment, the modified silicone oil III is a silicone oil capped with a branching factor of 0.7 cyano group and a kinematic viscosity of 300 cst, and the modified silicone oil IV is a hydrogen-containing silicone oil with a branching factor of 0.5 and a kinematic viscosity of 250 cst.

[0086] In this embodiment, the modifier is a mixture of isooctyl stearate and isononyl gluconate with a mass ratio of 1.2:1.

[0087] In this embodiment, the crosslinking promoter is a mixture of nickel isostearate and cobalt isodecanoate with a mass ratio of 1.2:1.

[0088] In this embodiment, the filler I is Li7La3Zr2O with a particle size of 50-70 microns 12 , the filler II is La2Ce2O7 with a particle size of 7-10 microns, the filler III is titanium monoxide with a particle size of 35-50 microns, and the filler IV is MgFe2O4 with a particle size of 2-3 microns.

[0089] In this embodiment, the treating agent is a mixture of hydrogenated castor oil and palmitic acid with a mass ratio of 1.2:1.

[0090] In this embodiment, the complexing agent is a mixture of dimethyl maleate and tin benzoate with a mass ratio of 1.2:1.

[0091] The preparation method of the two-component thermal conductive gel material of this embodiment includes the following steps:

[0092] Component A:

[0093] Step A1: Add 30% of the required addition amount of modified silicone oil II to all of the modified silicone oil I, heat up to 40-60 °C, stir and mix, control the stirring rate at 500 revolutions per minute, and stir for 30 minutes. After stirring and cooling to room temperature, a mixed liquid I (A) is obtained;

[0094] Step A2: Perform ice - water bath stirring on the first mixture (A) obtained in step (A2), control the stirring rate at 500 revolutions per minute, slowly add the modifier, control the addition time at 3 hours. After the addition is completed, stir for another 40 minutes to obtain the second mixture (A).

[0095] Step A3: Maintain ice - water bath stirring, control the stirring rate at 500 revolutions per minute, add the remaining 50% of the second modified silicone oil to the second mixture (A) obtained in step (A3), and stir for 3 hours to obtain the third mixture (A).

[0096] Step A4: Maintain ice - water bath stirring, control the stirring rate at 400 revolutions per minute. Slowly add the cross - linking promoter to the third mixture (A) obtained in step (A3), control the addition time at 12 minutes. After the addition is completed, continue to stir for 5 minutes and then stir and heat up to room temperature under sealed conditions to obtain the fourth mixture (A).

[0097] Step A5: Add the first filler and the second filler together to the fourth mixture (A) obtained in step (A4), stir at a high speed of 1600 revolutions per minute for 5 minutes, and then transfer it to a three - roll mill for grinding 20 times to obtain the first mixture (A).

[0098] Step A6: Put the first mixture (A) obtained in step (A5) into a planetary vacuum degassing machine, evacuate to 1 kPa, set the rotation speed at 1000 revolutions per minute, and degas for 5 minutes to obtain the A - component mixture.

[0099] Component B:

[0100] Step B1: Add 50% of the required amount of the third modified silicone oil to all of the fourth modified silicone oil, heat up to 70 °C, stir and mix, control the stirring rate at 500 revolutions per minute, and stir for 40 minutes. After stirring and cooling to room temperature, obtain the first mixture (B).

[0101] Step B2: Perform ice - water bath stirring on the first mixture (B) obtained in step (B2), control the stirring rate at 500 revolutions per minute, add the treating agent to the first mixture (B) at one time, and stir for 30 minutes to obtain the second mixture (B).

[0102] Step B3: Maintain ice - water bath stirring, control the stirring rate at 500 revolutions per minute, add the remaining 50% of the third modified silicone oil to the second mixture (A) obtained in step (B3), and stir for 3 hours to obtain the third mixture (B).

[0103] Step B4: Maintain stirring in an ice-water bath with a stirring rate controlled at 400 revolutions per minute. Slowly add a crosslinking promoter to the mixture (B) obtained in step (B3) over a period of 12 minutes. After the addition is complete, continue stirring for 5 minutes and then stir and heat up to room temperature under sealed conditions to obtain mixture (B) four.

[0104] Step B5: Add filler three and filler four together to mixture (B) four obtained in step (B4) and stir at a high speed of 1600 revolutions per minute to obtain mixture (B) one.

[0105] Step B6: Place mixture (B) one obtained in step (B5) into a planetary vacuum degassing machine, evacuate to 1 kPa, set the rotation speed to 1000 revolutions per minute, and degas for 5 minutes to obtain the B-component mixture.

[0106] Component A and component B are uniformly mixed at a weight ratio of 1:1 for curing.

[0107] After testing, the viscosities of the obtained component A and component B are 410000 cp and 430000 cp respectively (7# rotor, 10 rpm), the thixotropic indices (7# rotor, η 10rpm / η 1rpm ) are 17.8 and 17.5 respectively, and the thermal conductivities are 6.3 W / (m・K) and 6.4 W / (m・K) respectively.

[0108] The thermal conductivity of the reaction product of component A and component B is 6.1 W / (m・K). After being treated at 200 °C for 1000 hours, the change rate of the thermal conductivity is 2.1%. After being treated at 200 °C for 5000 hours, the change rate of the thermal conductivity is 3.3%. Example 3

[0109] The two-component thermally conductive gel material of this example includes a thermally conductive component A and a gel component B, and the mass ratio of the thermally conductive component A to the gel component B is 1:1.

[0110] Among them, component A includes the following raw materials in parts by mass: 4 parts of modified silicone oil one, 3 parts of modified silicone oil two, 2 parts of modifier, 0.03 parts of crosslinking promoter, 45 parts of filler one, and 42 parts of filler two.

[0111] Component B includes the following raw materials in parts by mass: 6 parts of modified silicone oil three, 7 parts of modified silicone oil four, 6 parts of treatment agent, 0.003 parts of complexing agent, 45 parts of filler three, and 37 parts of filler four.

[0112] In this example, modified silicone oil one is a silicone oil with a kinetic viscosity of 250 cst and a branching factor of 0.25 capped with a methacrylate group, and modified silicone oil two is a linear isopropenyl-capped silicone oil with a kinetic viscosity of 200 cst.

[0113] In this embodiment, the modified silicone oil III is a cyanide-terminated silicone oil with a branching factor of 0.6 and a kinematic viscosity of 250 cst, and the modified silicone oil IV is a hydrogen-containing silicone oil with a branching factor of 0.4 and a kinematic viscosity of 200 cst.

[0114] In this embodiment, the modifier is a mixture of isooctyl stearate and isononyl gluconate with a mass ratio of 1.1:1.

[0115] In this embodiment, the crosslinking promoter is a mixture of manganese oleate and cobalt isodecanoate with a mass ratio of 1.1:1.

[0116] In this embodiment, the first filler is Li7La3Zr2O with a particle size of 45 - 55 microns 12 , the second filler is La2Ce2O7 with a particle size of 7 - 9 microns, the third filler is titanium monoxide with a particle size of 30 - 40 microns, and the fourth filler is MgFe2O4 with a particle size of 1.5 - 2.5 microns.

[0117] In this embodiment, the treating agent is a mixture of phenyltriethoxysilane and palmitic acid with a mass ratio of 1.1:1.

[0118] In this embodiment, the complexing agent is a mixture of oleylamine and dimethyl maleate with a mass ratio of 1.1:1.

[0119] The preparation method of the two-component thermal conductive gel in this embodiment includes the following steps:

[0120] Component A:

[0121] Step A1: Add 30% of the required amount of modified silicone oil II to all of the modified silicone oil I, heat up to 40 - 60 °C, stir and mix, control the stirring rate at 400 revolutions per minute, and stir for 20 minutes. After stirring and cooling to room temperature, obtain the first mixture (A);

[0122] Step A2: Stir the first mixture (A) obtained in step (A2) in an ice-water bath, control the stirring rate at 400 revolutions per minute, slowly dropwise add the modifier, control the dropping time at 2 hours. After the dropping is completed, stir for another 30 minutes to obtain the second mixture (A);

[0123] Step A3: Keep stirring in the ice-water bath, control the stirring rate at 400 revolutions per minute, add the remaining 50% of the modified silicone oil II to the second mixture (A) obtained in step (A3), and stir for 2 hours to obtain the third mixture (A);

[0124] Step A4: Keep stirring in the ice-water bath, control the stirring rate at 300 revolutions per minute, slowly dropwise add the crosslinking promoter to the third mixture (A) obtained in step (A3), control the dropping time at 9 minutes. After the dropping is completed, continue to stir for 4 minutes, and stir and heat up to room temperature under sealed conditions to obtain the fourth mixture (A);

[0125] Step A5: Add filler 1 and filler 2 together into the mixed solution 4 (A) obtained in step (A4), stir at a high speed of 1400 revolutions per minute for 4 minutes, and then transfer it to a three-roll grinder for grinding 15 times to obtain mixture 1 (A);

[0126] Step A6: Put the mixture 1 (A) obtained in step (A5) into a planetary vacuum degassing machine, evacuate to 1 kPa, set the rotation speed to 900 revolutions per minute, and degas for 4 minutes to obtain the A-component mixture;

[0127] Component B:

[0128] Step B1: Add 50% of the required addition amount of modified silicone oil 3 to all of the modified silicone oil 4, heat up to 50 - 70 °C, stir and mix, control the stirring rate at 4 revolutions per minute, stir for 30 minutes, and then cool to room temperature after stirring to obtain the mixed solution 1 (B);

[0129] Step B2: Stir the mixed solution 1 (B) obtained in step (B2) in an ice-water bath, control the stirring rate at 400 revolutions per minute, add the treatment agent to the mixed solution 1 (B) at one time, and stir for 20 minutes to obtain the mixed solution 2 (B);

[0130] Step B3: Keep stirring in the ice-water bath, control the stirring rate at 400 revolutions per minute, add the remaining 50% of the modified silicone oil 3 to the mixed solution 2 (A) obtained in step (B3), and stir for 2 hours to obtain the mixed solution 3 (B);

[0131] Step B4: Keep stirring in the ice-water bath, control the stirring rate at 300 revolutions per minute, slowly dropwise add the crosslinking promoter to the mixed solution 3 (B) obtained in step (B3), control the dropping time at 9 minutes, after the dropping is completed, continue to stir for 4 minutes, and stir and heat up to room temperature under sealed conditions to obtain the mixed solution 4 (B);

[0132] Step B5: Add filler 3 and filler 4 together into the mixed solution 4 (B) obtained in step (B4), stir at a high speed of 1400 revolutions per minute to obtain mixture 1 (B);

[0133] Step B6: Put the mixture 1 (B) obtained in step (B5) into a planetary vacuum degassing machine, evacuate to 1 kPa, set the rotation speed to 900 revolutions per minute, and degas for 4 minutes to obtain the B-component mixture;

[0134] The A component and the B component are uniformly mixed at a weight ratio of 1:1 and cured.

[0135] After testing, the viscosities of the obtained A component and B component are 420000 cp and 420000 cp respectively (7# rotor, 10 rpm), thixotropic index (7# rotor, η 10rpm / η 1rpm ) were 15.8 and 16.1 respectively, and the thermal conductivities were 6.1 W / (m·K) and 6.1 W / (m·K) respectively.

[0136] The thermal conductivity of the reaction product of component A and component B was 6.0 W / (m·K). After being treated at 200 °C for 1000 hours, the change rate of the thermal conductivity was 2.2%. After being treated at 200 °C for 5000 hours, the change rate of the thermal conductivity was 3.5%. Comparative Example 1

[0137] Commercially available AOK TF600 two-component gel was selected.

[0138] After testing, the viscosities of component A and component B were 3800000 cp and 3900000 cp respectively (7# rotor, 10 rpm), thixotropic index (7# rotor, η 10rpm / η 1rpm ) were 9.1 and 9.2 respectively, and the thermal conductivities were 5.7 W / (m·K) and 5.8 W / (m·K)

[0139] The thermal conductivity of the reaction product of component A and component B was 5.7 W / (m·K). After being treated at 200 °C for 1000 hours, the change rate of the thermal conductivity was 30.2%. After being treated at 200 °C for 5000 hours, the change rate of the thermal conductivity was 58.1%.

[0140] The present invention provides an idea and method for a two-component thermal conductive gel with high thermal conductivity, low viscosity and high thixotropy. There are many methods and ways to specifically implement this technical solution. The above description is only the preferred embodiment of the present invention. It should be noted that for those of ordinary skill in the art, without departing from the principle of the present invention, several improvements and retouches can be made, and these improvements and retouches should also be regarded as the protection scope of the present invention. Each component not clearly defined in this embodiment can be realized by the prior art.

Claims

1. A two-component thermal conductive gel with high thermal conductivity, low viscosity, and high thixotropy, characterized in that, It includes a heat-conducting component A and a gel component B; Among them, the heat-conducting component A includes the following components in parts by mass: 3-5 parts of silicone oil capped with methacrylate groups; 2-5 parts of linear silicone oil capped with isopropenyl groups; 1-3 parts of modifier; 0.01-0.05 parts of crosslinking promoter; Li7La3Zr2O 12 35 - 55 parts of fine powder; 35-50 parts of La2Ce2O7 fine powder; The gel component B includes the following components in parts by mass: 5-8 parts of silicone oil capped with cyano groups; 5-8 parts of hydrogen-containing silicone oil; 5-8 parts of treating agent; 0.001-0.005 parts of complexing agent; 40-50 parts of titanium monoxide fine powder; 35-40 parts of MgFe2O4 fine powder; In the heat-conducting component A, the modifier is a mixture of isooctyl stearate and isononyl gluconate in a mass ratio of 1-1.2:1; In the heat-conducting component B, the treating agent is any one or a mixture of two of phenyltriethoxysilane, hydrogenated castor oil, and palmitic acid in a mass ratio of 1-1.2:

1.

2. The two-component thermal conductive gel with high thermal conductivity, low viscosity and high thixotropy according to claim 1, characterized in that The said heat-conducting component A and the said gel component B are mixed in a mass ratio of 1-1.2:

1.

3. The two-component thermal conductive gel with high thermal conductivity, low viscosity and high thixotropy according to claim 1, characterized in that, In the heat-conducting component A, the dynamic viscosity of the silicone oil capped with methacrylate groups is 200-300 cst, and the branching factor is 0.2-0.3; the dynamic viscosity of the linear silicone oil capped with isopropenyl groups is 150-250 cst.

4. The two-component thermal conductive gel with high thermal conductivity, low viscosity, and high thixotropy according to claim 1, characterized in that, In the heat-conducting component A, the crosslinking promoter is any one or a mixture of two of manganese oleate, nickel isostearate, and cobalt isodecanoate in a mass ratio of 1-1.2:

1.

5. The two-component thermal conductive gel with high thermal conductivity, low viscosity and high thixotropy according to claim 1, wherein In the heat-conducting component A, the 12 particle size of the fine powder is 30 to 70 microns; the particle size of the La2Ce2O7 fine powder is 5 to 10 microns.

6. The two-component thermal conductive gel with high thermal conductivity, low viscosity and high thixotropy according to claim 1, characterized in that In the heat-conducting component B, the dynamic viscosity of the silicone oil capped with cyano groups is 200-300 cst, and the branching factor is 0.5-0.7; the dynamic viscosity of the hydrogen-containing silicone oil is 150-250 cst, and the branching factor is 0.3-0.

5.

7. The two-component thermal conductive gel with high thermal conductivity, low viscosity and high thixotropy according to claim 1, characterized in that, In the heat-conducting component B, the complexing agent is any one or a mixture of two of oleylamine, dimethyl maleate, and tin benzoate in a mass ratio of 1-1.2:

1.

8. The two-component thermal conductive gel with high thermal conductivity, low viscosity and high thixotropy according to claim 1, characterized in that, In the heat-conducting component B, the particle size of the titanium monoxide fine powder is 20-50 microns; the particle size of the MgFe2O4 fine powder is 1-3 microns.

9. The preparation method of the two-component thermal conductive gel with high thermal conductivity, low viscosity and high thixotropy according to claim 1, characterized in that, It includes the following steps: (1) Prepare the heat-conducting component A: Step A1: Add a part of the linear silicone oil capped with isopropenyl groups to the silicone oil capped with methacrylate groups, heat up to 40-60 °C, stir and mix, control the stirring rate at 300-500 revolutions per minute, and the stirring time is 10-30 minutes. After stirring and cooling to room temperature, obtain the first mixed solution of component A; Step A2: Carry out ice-water bath stirring on the first mixed solution of component A obtained in step (A1), control the stirring rate at 300-500 revolutions per minute, slowly dropwise add the modifier, control the dropping time at 1-3 hours, and after the dropping is completed, stir for another 20-40 minutes to obtain the second mixed solution of component A; Step A3: Keep ice-water bath stirring, control the stirring rate at 300-500 revolutions per minute, add the remaining formulated amount of the linear silicone oil capped with isopropenyl groups to the second mixed solution of component A obtained in step (A3), and stir for 1-3 hours to obtain the third mixed solution of component A; Step A4: Maintain stirring in an ice-water bath with the stirring rate controlled at 200 - 400 revolutions per minute. Slowly add a crosslinking promoter to the third mixed solution of Component A obtained in step (A3) over a dropping time of 6 - 12 minutes. After the addition is complete, continue stirring for 3 - 5 minutes and then stir and heat up to room temperature under sealed conditions to obtain the fourth mixed solution of Component A; Step A5: Add Li7La3Zr2O 12 fine powder and La2Ce2O7 fine powder together into the fourth mixed solution of component A obtained in step (A4), stir for 3 - 5 minutes at a rotation speed of 1200 - 1600 revolutions per minute, and then transfer it to a three-roll grinder for grinding 10 - 20 times to obtain the first mixture of component A; Step A6: Place the first mixture of Component A obtained in step (A5) into a planetary vacuum degassing machine, evacuate to below 1 kPa, set the rotation speed to 800 - 1000 revolutions per minute, and degas for 3 - 5 minutes to obtain the heat-conducting component A; (2) Prepare the gel component B: Step B1: Add a portion of cyano-terminated silicone oil to the hydrogen-containing silicone oil, heat up to 50 - 70 °C, stir and mix with the stirring rate controlled at 300 - 500 revolutions per minute for 20 - 40 minutes. After stirring and cooling to room temperature, obtain the first mixed solution of Component B; Step B2: Carry out stirring in an ice-water bath on the first mixed solution of Component B obtained in step (B2) with the stirring rate controlled at 300 - 500 revolutions per minute. Add the treatment agent to the first mixed solution of Component B and stir for 10 - 30 minutes to obtain the second mixed solution of Component B; Step B3: Maintain stirring in an ice-water bath with the stirring rate controlled at 300 - 500 revolutions per minute. Add the remaining amount of cyano-terminated silicone oil to the second mixed solution of Component B obtained in step (B3) and stir for 1 - 3 hours to obtain the third mixed solution of Component B; Step B4: Maintain stirring in an ice-water bath with the stirring rate controlled at 200 - 400 revolutions per minute. Slowly add a complexing agent to the third mixed solution of Component B obtained in step (B3) over a dropping time of 6 - 12 minutes. After the addition is complete, continue stirring for 3 - 5 minutes and then stir and heat up to room temperature under sealed conditions to obtain the fourth mixed solution of Component B; Step B5: Add titanium monoxide fine powder and MgFe2O4 fine powder together to the fourth mixed solution of Component B obtained in step (B4) at a high speed of 1200 - 1600 revolutions per minute to obtain the first mixture of Component B; Step B6: Place the first mixture of Component B obtained in step (B5) into a planetary vacuum degassing machine, evacuate to below 1 kPa, set the rotation speed to 800 - 1000 revolutions per minute, and degas for 3 - 5 minutes to obtain the gel component B; (3) Prepare the two-component heat-conducting gel: Uniformly mix the obtained heat-conducting component A and gel component B in a weight ratio of 1:1, and then cure to obtain the product.

10. The preparation method of the two-component thermal conductive gel with high thermal conductivity, low viscosity and high thixotropy according to claim 9, characterized in that, In step A1, add 25 - 35% of the linear isopropenyl-terminated silicone oil in terms of the formula amount to the methacrylate-based silicone oil; in step B1, add 40 - 60% of the cyano-terminated silicone oil in terms of the formula amount to the hydrogen-containing silicone oil.