Silicone grease with high thermal conductivity, low oil separation and low thermal resistance

By using homemade silicone oil and powder treatment agent, combined with alumina powder and carbon black with appropriate particle size, the problems of oil extraction, high thermal resistance and excessive viscosity in existing thermal silicone grease are solved, and high thermal conductivity and low oil extraction are achieved The silicon grease with low thermal resistance improves the heat dissipation performance of electronic devices.

CN119410148APending Publication Date: 2025-02-11YANTAI DARBOND TECH
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Patent Information

Application Number
CN202411507333.3
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-10-28
Publication Date
2025-02-11

AI Technical Summary

Technical Problem

The existing thermal grease may experience oil dissipation during use, with high thermal resistance, which cannot meet the heat dissipation needs of high-performance electronic equipment, and excessive viscosity leads to uneven application, affecting the heat dissipation effect.

Method used

Using homemade silicone oil and powder treatment agent, combined with alumina powder and carbon black of appropriate particle size, silicon grease with high thermal conductivity, low oil extraction and low thermal resistance is prepared through specific ratios and processes.

Benefits of technology

It effectively reduces the precipitation rate of oil in silicon grease, reduces the viscosity of silicon grease, improves thermal conductivity, reduces thermal resistance, and improves the uniformity of the coating and heat dissipation effect.

✦ Generated by Eureka AI based on patent content.

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Abstract

The invention relates to silicone grease with high thermal conductivity, low oil separation and low thermal resistance, and belongs to the technical field of organic silicon modification. The high-thermal-conductivity low-oil-separation low-thermal-resistance silicone grease is prepared from the following components in parts by weight: 1 to 10 parts of self-made silicone oil, 1 to 10 parts of powder treating agent, 85 to 97 parts of heat-conducting filler and 0.01 to 0.5 part of carbon black, the self-made silicone oil adopted by the invention reduces the precipitation rate of oil in the silicone grease; the self-made powder treating agent is used, so that the viscosity of the silicone grease is reduced; due to selection of powder with proper particle size and powder proportion, the heat conductivity of the heat-conducting silicone grease is greatly improved, and the heat resistance is reduced.
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Description

Technical Field

[0001] The invention relates to a silicone grease with high thermal conductivity, low oil separation and low thermal resistance, belonging to the technical field of organic silicon modification. Background Art

[0002] In the current era of rapid technological development, the trend of miniaturization and high performance of electronic devices has become an industry consensus. This development trend poses a severe challenge to the thermal management of electronic devices, and efficient heat dissipation solutions have become the key. Thermal grease, as a widely used thermal interface material, is widely used to fill the tiny gaps between electronic components and heat sinks due to its good thermal conductivity to reduce thermal resistance and achieve effective heat transfer. In the future, thermal grease technology will develop in the direction of improving thermal conductivity, enhancing stability and environmental protection, and adapting to a wider range of application scenarios.

[0003] However, there are still some urgent problems to be solved in the existing thermal grease technology on the market. First, some products may have oil separation during use, which not only affects its heat conduction efficiency, but also may cause pollution to the internal components of electronic equipment. Secondly, the high thermal resistance limits the rapid dissipation of heat and cannot meet the heat dissipation requirements of high-performance electronic equipment. Furthermore, the viscosity of existing thermal grease is too high, which may lead to uneven application and affect the heat dissipation effect. Summary of the invention

[0004] In view of the deficiencies in the prior art, the object of the present invention is to provide a silicone grease with high thermal conductivity, low oil separation and low thermal resistance.

[0005] To achieve the above objectives, the technical solutions adopted are:

[0006] The present invention relates to a high thermal conductivity, low oil separation and low thermal resistance silicone grease, which comprises, by weight, 1 to 10 parts of homemade silicone oil, 1 to 10 parts of powder treatment agent, 85 to 97 parts of thermal conductive filler and 0.01 to 0.5 parts of carbon black;

[0007] The structure of the homemade silicone oil is:

[0008]

[0009] Wherein, r=1-50, x=1-50;

[0010] The structure of the powder treatment agent is:

[0011]

[0012] Among them, o=1~50, m=1~50, n=1~50.

[0013] The preparation method of the self-made silicone oil comprises the following steps: adding [2-(3-cyclohexenyl)ethylene]trimethoxysilane and a platinum catalyst into a reaction vessel, stirring at room temperature for 15 to 30 minutes, slowly dropping the side hydrogenated silicone oil therein, and after the dropping is completed, continuing to stir at room temperature for 3 to 5 hours, slowly raising the temperature to 95 to 115° C., and stirring for 2 to 8 hours to obtain the self-made silicone oil. The platinum catalyst is a vinyl complex with a platinum content of 5000 ppm; the side hydrogenated silicone oil is a side hydrogenated silicone oil with a hydrogen content of 0.25 to 5 mmol / g and a viscosity of 15 to 80 mPa.S.

[0014] The reaction formula is:

[0015]

[0016] Wherein r=1~50, x=1~50.

[0017] The preparation method of the powder treatment agent comprises the following steps: adding 3-methacrylate propyl tris(trimethoxysilane), trimethoxy(4-vinylphenyl)silane and platinum catalyst into a reaction container, stirring at room temperature for 15 to 30 minutes, slowly dropping terminal hydrogenated silicone oil thereinto, and after the dropping is completed, continuing to stir at room temperature for 3 to 5 hours, slowly raising the temperature to 95 to 115° C., stirring for 2 to 8 hours, and obtaining the powder treatment agent. The platinum catalyst is a 5000 ppm vinyl complex; the terminal hydrogenated silicone oil is a terminal hydrogenated silicone oil having a hydrogen content of 0.25 to 5 mmol / g and a viscosity of 10 to 50 mPa.S.

[0018] The reaction formula is:

[0019]

[0020] Where o = 1 ~ 50, p = 1 ~ 50, m = 1 ~ 50, n = 1 ~ 50

[0021] The thermal conductive filler is at least one of 0.3um alumina, 1um alumina, 5um alumina, 10um alumina, 15um alumina, 30um alumina, and 40um alumina.

[0022] The thermal conductive filler is a mixture of 0.3um alumina, 5um alumina, 15um alumina and 40um alumina.

[0023] The carbon black is commercially available common carbon black.

[0024] Compared with the prior art, the beneficial effects of the present invention are: the homemade silicone oil prepared by the present invention reduces the oil precipitation rate in the silicone grease; the use of the homemade powder treatment agent reduces the viscosity of the silicone grease; the selection of powder with suitable particle size and the powder ratio greatly improve the thermal conductivity of the thermal conductive silicone grease and reduce the thermal resistance. DETAILED DESCRIPTION

[0025] The present invention is described below in conjunction with examples, which are only used to explain the present invention and are not used to limit the scope of the present invention.

[0026] Add 230g of [2-(3-cyclohexenyl)ethyl]trimethoxysilane and 0.09g of platinum catalyst into a three-necked flask, stir at room temperature for 30min, slowly drop 200g of 5mmol / g side hydrogenated silicone oil thereto, after the addition is complete, continue stirring at room temperature for 4.5h, slowly raise the temperature to 95°C, stir for 4h, and obtain homemade silicone oil; the platinum catalyst is a 5000ppm vinyl complex; the side hydrogenated silicone oil is a side hydrogenated silicone oil with a hydrogen content of 4mmol / g and a viscosity of 20mPa.S.

[0027] Add 422g of 3-methacrylate propyl tris(trimethoxysilane), 224g of trimethoxy(4-vinylphenyl)silane, and 0.5g of platinum catalyst to a three-necked flask and stir at room temperature for 20min. Slowly add terminal hydrogenated silicone oil, and continue stirring at room temperature for 4h after the addition is complete. Slowly raise the temperature to 110°C and stir for 4h. Finally, a powder treatment agent is obtained, wherein the platinum catalyst is a vinyl complex with a platinum content of 5000ppm; the terminal hydrogenated silicone oil is a terminal hydrogenated silicone oil with a hydrogen content of 4mmol / g and a viscosity of 20mPa.S.

[0028] Example 1

[0029] Homemade silicone oil, powder treatment agent, 0.3um alumina, 5um alumina, 15um alumina, 40um alumina and carbon black were mixed in a mass ratio of 3:1:20:15:30:31:0.05.

[0030] Example 2

[0031] Homemade silicone oil, powder treatment agent, 0.3um alumina, 5um alumina, 15um alumina, 40um alumina and carbon black were mixed in a mass ratio of 2:2:20:15:30:31:0.05.

[0032] Comparative Example 1

[0033] Methyl silicone oil (viscosity is 200mPa.S), powder treatment agent, 0.3um alumina, 5um alumina, 15um alumina, 40um alumina, and carbon black are mixed in a mass ratio of 3:1:20:15:30:31:0.05.

[0034] Comparative Example 2

[0035] Homemade silicone oil, hexyltrimethoxysilane, 0.3um alumina, 5um alumina, 15um alumina, 40um alumina, and carbon black were mixed in a mass ratio of 3:1:20:15:30:31:0.05.

[0036] Comparative Example 3

[0037] Homemade silicone oil, powder treatment agent, 1um alumina, 5um alumina, 15um alumina, 40um alumina and carbon black were mixed in a mass ratio of 3:1:20:15:30:31:0.05.

[0038] The properties of the silicone grease samples obtained in various embodiments and comparative examples are shown in Table 1, and the test methods are shown in the description of Table 1.

[0039] Table 1. Performance test results

[0040]

[0041] Compared with Example 2, Example 1 shows that the homemade powder treatment agent reduces the viscosity of silicone grease, but the addition of too much treatment agent will lead to the severity of oil separation; Compared with Comparative Example 1, Example 1 shows that the addition of homemade silicone oil effectively reduces the oil separation of silicone grease; Compared with Comparative Example 2, Example 1 shows that the homemade powder treatment agent can effectively reduce the viscosity of silicone grease and improve the colloid extrusion rate compared with the traditional powder treatment agent; Compared with Comparative Example 3, Example 1 shows that the use of 0.3um alumina powder can more effectively fill the gaps between powders and reduce thermal resistance.

[0042] The above description is only a preferred embodiment of the present invention and is not intended to limit the scope of the present invention. Any modifications, equivalent substitutions, improvements, etc. made within the concept and principle of the present invention should be included in the protection scope of the present invention.

Claims

1. A high thermal conductivity, low oil separation and low thermal resistance silicone grease, characterized in that: According to weight, it contains 1 to 10 parts of homemade silicone oil, 1 to 10 parts of powder treatment agent, 85 to 97 parts of thermal conductive filler, and 0.01 to 0.5 parts of carbon black; The structure of the homemade silicone oil is: Wherein, r=1-50, x=1-50; The structure of the powder treatment agent is: Among them, o=1~50, m=1~50, n=1~50.

2. According to claim 1, the high thermal conductivity, low oil separation and low thermal resistance silicone grease is characterized in that: The method for preparing the homemade silicone oil comprises the following steps: adding [2-(3-cyclohexenyl)ethylene]trimethoxysilane and a platinum catalyst into a reaction container, stirring at room temperature for 15 to 30 minutes, slowly dripping the hydrogenated silicone oil therein, and after the dripping is completed, continuing to stir at room temperature for 3 to 5 hours, slowly raising the temperature to 95 to 115° C., and stirring for 2 to 8 hours to obtain the homemade silicone oil.

3. The high thermal conductivity, low oil separation and low thermal resistance silicone grease according to claim 2, characterized in that: The platinum catalyst is a vinyl complex with a platinum content of 5000 ppm.

4. The high thermal conductivity, low oil separation and low thermal resistance silicone grease according to claim 2, characterized in that: The side hydrogen-containing silicone oil is a side hydrogen-containing silicone oil with a hydrogen content of 0.25 to 5 mmol / g and a viscosity of 10 to 50 mPa.S.

5. The high thermal conductivity, low oil separation and low thermal resistance silicone grease according to claim 1, characterized in that: The preparation method of the powder treatment agent comprises the following steps: adding 3-propyl methacrylate tris(trimethoxysilane), trimethoxy(4-vinylphenyl)silane and a platinum catalyst into a reaction container, stirring at room temperature for 15 to 30 minutes, slowly dripping terminal hydrogenated silicone oil therein, and after the dripping is completed, continuing to stir at room temperature for 3 to 5 hours, slowly raising the temperature to 95 to 115° C., and stirring for 2 to 8 hours to obtain the powder treatment agent.

6. The high thermal conductivity, low oil separation and low thermal resistance silicone grease according to claim 5, characterized in that: The platinum catalyst is a vinyl complex with a platinum content of 5000 ppm; the terminal hydrogen-containing silicone oil is a terminal hydrogen-containing silicone oil with a hydrogen content of 0.25 to 5 mmol / g and a viscosity of 10 to 50 mPa.S.

7. The high thermal conductivity, low oil separation and low thermal resistance silicone grease according to claim 1, characterized in that: The thermal conductive filler is at least one of 0.3um alumina, 1um alumina, 5um alumina, 10um alumina, 15um alumina, 30um alumina, and 40um alumina.

8. The high thermal conductivity, low oil separation and low thermal resistance silicone grease according to claim 7, characterized in that: The thermal conductive filler is a mixture of 0.3um alumina, 5um alumina, 15um alumina and 40um alumina.