CN111777995A - Insulating efficient heat-conducting silicone grease and preparation method thereof - Google Patents
Insulating efficient heat-conducting silicone grease and preparation method thereof Download PDFInfo
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Abstract
The invention discloses an insulating efficient heat-conducting silicone grease and a preparation method thereof, wherein the heat-conducting silicone grease comprises the following components in parts by weight: 80-100 parts of composite spherical heat-conducting filler, 0.5-5 parts of one-dimensional structure heat-conducting material, 0.5-5 parts of two-dimensional structure heat-conducting material, 20-100 parts of liquid metal heat-conducting paste, 4-20 parts of silicone oil, 0.25-2 parts of silane coupling agent and 0.1-1 part of antioxidant. The invention fills the tiny gaps on the surface of the composite spherical heat-conducting filler by the liquid metal heat-conducting paste, effectively reduces the contact thermal resistance among filler particles, can keep the good insulativity of the heat-conducting silicone grease while obtaining high-efficiency heat-conducting performance, and effectively solves the problems of low filling amount, poor heat-conducting effect, easy dry cracking and oil seepage of the traditional heat-conducting silicone grease by adopting the high-efficiency heat-conducting silicone grease.
Description
Technical Field
The invention belongs to the technical field of heat-conducting silicone grease, and particularly relates to insulating efficient heat-conducting silicone grease and a preparation method thereof.
Background
In recent years, along with the rapid development of intelligent and automatic industries, the integration level of electronic components is higher and higher, the heat generated during the work of the electronic components is higher and higher, and particularly in the coming of the 5G communication era, the heat conductivity coefficient of the traditional heat-conducting silicone grease is not high, and the heat dissipation performance is not enough to meet the heat dissipation requirements of higher power and more complex environments. How to further improve the heat-conducting property of the heat-conducting silicone grease becomes a difficult problem in front of researchers; the liquid metal heat conducting paste developed gradually in recent years is a high-end thermal interface material, and has the characteristic of phase change heat absorption, so that the heat conductivity of the liquid metal heat conducting paste is far beyond that of the traditional heat conducting silicone grease, but the liquid metal has high fluidity, and the liquid metal heat conducting paste is easy to flow and lose efficacy in the long-term use process.
Therefore, it is an important subject in the field of liquid metal thermal interface material research to find a material and a method capable of preventing the liquid metal from flowing to cause failure and reducing the electrical conductivity thereof, and simultaneously ensuring the high thermal conductivity thereof.
Disclosure of Invention
In view of the above, the present invention provides an insulating high-efficiency heat-conducting silicone grease, which solves the problems of poor heat-conducting effect, easy dry cracking and oil leakage of the existing heat-conducting silicone grease.
The invention also aims to provide a preparation method of the insulating efficient heat-conducting silicone grease.
In order to achieve the purpose, the technical scheme of the invention is realized as follows: an insulating efficient heat-conducting silicone grease comprises the following components in parts by weight: 80-100 parts of composite spherical heat-conducting filler, 0.5-5 parts of one-dimensional structure heat-conducting material, 0.5-5 parts of two-dimensional structure heat-conducting material, 20-100 parts of liquid metal heat-conducting paste, 4-20 parts of silicone oil, 0.25-2 parts of silane coupling agent and 0.1-1 part of antioxidant.
Preferably, the composite spherical heat-conducting filler comprises a micron-sized spherical heat-conducting filler and a nanometer-sized spherical heat-conducting filler, and the ratio of the weight of the micron-sized spherical heat-conducting filler to the total weight of the composite spherical heat-conducting filler is (0.75-0.95): 1; namely, the composite spherical heat-conducting filler adopted by the heat-conducting silicone grease of the invention must contain micron-sized spherical heat-conducting filler and nanometer-sized heat-conducting filler; and it is illustrated that the ratio of the weight of the micron-sized spherical heat conductive filler to the total weight of the electrically conductive particles may be 0.75: 1; it may also be 0.85: 1; and may be 0.95:1, etc.
Preferably, the average particle size of the micron-sized spherical heat-conducting filler is 3-30 μm; the micron-sized spherical heat-conducting filler is at least one of modified heat-conducting ceramic powder, modified aluminum nitride and modified diamond; that is, in the specific embodiment, the micron-sized spherical heat conductive filler may be any one of the above materials, or may be a combination of any two or more of the above materials.
Preferably, the average particle size of the nanoscale heat-conducting filler is 50-200 nm; the nano-scale heat-conducting filler is at least one of modified alumina and modified heat-conducting ceramic powder; that is, in the specific embodiment, the nanoscale heat-conducting filler may be any one of the two materials, or may be a combination of the two materials.
Preferably, the weight ratio of the liquid metal heat-conducting paste to the composite spherical heat-conducting filler is 1: (1-5); that is, in the specific embodiment, the ratio of the weight of the liquid metal thermal conductive paste to the total weight of the composite spherical thermal conductive filler may be 1: 1; may also be 1: 2.5; may also be 1: 5, etc.; in addition, the liquid metal is added too little, so that the heat conductivity is not obviously improved; the liquid metal is added too much, and the prepared heat-conducting silicone grease is dry and hard and is easy to become conductive.
Preferably, the liquid metal heat conductive paste is at least one of gallium, gallium indium tin zinc, bismuth indium tin, and bismuth indium tin zinc alloy, that is, in a specific embodiment, the liquid metal heat conductive paste may be any one of the above materials, or may be a combination of two or more of the above materials.
Preferably, the average length of the one-dimensional structure heat conduction material is 1-50 μm, and the one-dimensional structure heat conduction material is at least one of modified carbon fiber, carbon nano tube, modified silicon carbide whisker, modified silver nano wire and modified gold nano wire; that is, in the specific embodiment, the one-dimensional structure heat conduction material may be any one of the above-mentioned materials, or may be a combination of two or more of the above-mentioned materials.
Preferably, the average particle size of the two-dimensional structure heat conduction material is 0.5-30 μm, and the two-dimensional structure heat conduction material is at least one of modified sheet graphene, modified sheet boron nitride and modified sheet silicon carbide; that is, in the specific embodiment, the two-dimensional structure heat conduction material may be any one of the above-mentioned materials, or may be a combination of two or more of the above-mentioned materials.
Preferably, the silicone oil is at least one silicone polymer selected from methyl-terminated polydimethylsiloxane, methyl-terminated polymethylphenylsiloxane, vinyl-terminated polymethylsiloxane and vinyl-terminated polymethylphenylsiloxane; that is, in the specific examples, the silicone oil may be any one of the above-described silicone oils, or may be a combination of two or more of the above-described silicone oils.
Preferably, the silane coupling agent is at least one of methyltrimethoxysilane, methyltriethoxysilane, dodecyltrimethoxysilane, phenyltrimethoxysilane and vinyltrimethoxysilane; that is, in the specific examples, the silane coupling agent may be any one of the above-mentioned silane coupling agents, or may be a combination of two or more of the above-mentioned silane coupling agents.
Preferably, the antioxidant is at least one of antioxidant 1010 and antioxidant 1076; specifically, in the specific examples, the antioxidant may be either one of the above two types or a combination of the above two types.
The other technical scheme of the invention is realized as follows: a preparation method of high-efficiency heat-conducting silicone grease comprises the following steps:
step 1, respectively weighing the following components in parts by weight: 80-100 parts of composite spherical heat-conducting filler, 0.5-5 parts of one-dimensional structure heat-conducting material, 0.5-5 parts of two-dimensional structure heat-conducting material, 20-100 parts of liquid metal heat-conducting paste, 4-20 parts of silicone oil, 0.25-2 parts of silane coupling agent and 0.1-1 part of antioxidant;
step 2, sequentially adding the composite spherical heat-conducting filler, the one-dimensional heat-conducting filler and the two-dimensional heat-conducting filler in the step 1 into a high-speed mixer, and mixing and dispersing for 5-30 min under the condition that the online speed is 25-70 m/s;
step 3, adding the liquid metal heat conducting paste in the step 1 into the high-speed mixer in the step 2, and mixing and dispersing for 5-30 min at an online speed of 25-70 m/s to obtain a heat conducting filler after high-speed dispersion;
step 4, placing the heat-conducting filler obtained in the step 3 after high-speed dispersion in a vacuum stirrer, and vacuumizing for 10-30 min at the temperature of 70-120 ℃;
and 5, uniformly mixing the silicone oil, the silane coupling agent and the antioxidant in the step 1, injecting the mixture into the vacuum stirrer in the step 4, vacuumizing and stirring the mixture for 1 to 3 hours at the temperature of 70 to 120 ℃, and vacuumizing and stirring the mixture for 1 to 3 hours at the temperature of 150 to 200 ℃ to obtain the heat-conducting silicone grease.
Preferably, in the step 1, a specific preparation method of the composite spherical heat-conducting filler is as follows:
80-100 parts of micron-sized spherical heat-conducting filler and modified nano-scale heat-conducting filler are mixed according to the weight ratio of 95: 5-75: adding the mixture into a high-speed mixer according to the proportion of 25, and mixing and dispersing for 5-30 min under the condition that the linear speed is 25-70 m/s to obtain the composite spherical heat-conducting filler.
Compared with the prior art, the invention fills the tiny gaps on the surface of the composite spherical heat-conducting filler by the liquid metal heat-conducting paste, effectively reduces the contact thermal resistance among filler particles, obtains high-efficiency heat-conducting performance and simultaneously can still keep good insulativity of the heat-conducting silicone grease, and meanwhile, by adopting the high-efficiency heat-conducting silicone grease disclosed by the invention, the problems of low filling amount, poor heat-conducting effect, easiness in dry cracking and oil leakage existing in the traditional heat-conducting silicone grease are effectively solved; in addition, the method disclosed by the invention coats the micron heat-conducting filler with the nanometer heat-conducting filler in a high-speed dispersion mode, and fills the tiny gaps on the surface of the heat-conducting filler with the liquid metal heat-conducting paste, so that the contact thermal resistance among filler particles is effectively reduced, and the whole process is simple and easy to operate.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The micron-sized spherical heat-conducting filler, the nano-sized heat-conducting filler, the one-dimensional structure heat-conducting material, the two-dimensional structure heat-conducting material, the liquid metal heat-conducting paste, the silicone oil, the silane coupling agent and the antioxidant used in the following embodiments can be purchased.
Example 1
The insulating efficient heat-conducting silicone grease provided by the embodiment 1 comprises the following components in parts by weight:
65 parts of modified heat-conducting ceramic powder with the average particle size of 10 microns, 25 parts of modified heat-conducting ceramic powder with the average particle size of 5 microns, 15 parts of modified heat-conducting ceramic powder with the average particle size of 200nm, 0.5 part of modified sheet graphene with the average particle size of 20 microns, 5 parts of modified carbon fiber with the average particle size of 35 microns, 30 parts of liquid metal heat-conducting paste, 8 parts of methyl silicone oil with the viscosity of 1000CP, 2 parts of vinyl silicone oil with the viscosity of 500CP, 0.5 part of dodecyl trimethoxy silane and 10100.5 parts of antioxidant.
Through calculation, in the components, the weight ratio of the liquid metal heat-conducting paste to the composite spherical heat-conducting filler is 1: 3.5; the ratio of the weight of the micron-sized spherical heat-conducting filler to the total weight of the composite spherical heat-conducting filler is 0.86: 1.
the insulating efficient heat-conducting silicone grease provided in embodiment 1 is prepared by the following method, which includes the following steps:
step 1, adding 65 parts of modified heat-conducting ceramic powder (with an average particle size of 10 μm), 25 parts of modified heat-conducting ceramic powder (with an average particle size of 5 μm) and 15 parts of modified heat-conducting ceramic powder (with an average particle size of 200nm) into a high-speed mixer (FM-3L, Mitsui mine Co., Ltd., Japan) respectively, and mixing and dispersing for 10min at an online speed of 50m/s to obtain a composite spherical heat-conducting filler;
step 2, adding 0.5 part of modified flake graphene (with the average particle size of 20 microns) and 5 parts of modified carbon fiber (with the average particle size of 35 microns) into the high-speed mixer in the step 1, and mixing and dispersing for 10min at the online speed of 50 m/s;
step 3, adding 30 parts of liquid metal heat-conducting paste into the high-speed mixer in the step 2, and then mixing and dispersing for 10min at an online speed of 50m/s to obtain a heat-conducting filler after high-speed dispersion;
step 4, placing the heat-conducting filler obtained in the step 3 after high-speed dispersion in a vacuum stirrer, and vacuumizing for 30min at the temperature of 100 ℃ to remove air in the heat-conducting filler;
and 5, uniformly mixing 8 parts of methyl silicone oil (the viscosity is 1000CP), 2 parts of vinyl silicone oil (the viscosity is 500CP), 0.5 part of dodecyl trimethoxy silane and 0.5 part of antioxidant 1010, adding the mixture into the vacuum stirrer in the step 4, vacuumizing and stirring the mixture for 1 hour at the temperature of 100 ℃, heating the mixture to 150 ℃, and vacuumizing and stirring the mixture for 1 hour at the temperature of 150 ℃ to obtain the heat-conducting silicone grease with the heat conductivity coefficient of 7.5W/m.K.
Example 2
The insulating efficient heat-conducting silicone grease provided by the embodiment 1 comprises the following components in parts by weight:
55 parts of aluminum nitride with the average particle size of 10 microns, 25 parts of aluminum nitride with the average particle size of 5 microns, 20 parts of modified heat-conducting ceramic powder with the average particle size of 200nm, 0.5 part of modified flake graphene with the average particle size of 20 microns, 4 parts of modified carbon fiber with the average particle size of 50 microns, 50 parts of liquid metal heat-conducting paste, 10 parts of methyl silicone oil with the viscosity of 1000CP, 0.5 part of dodecyl trimethoxy silane and 10101 part of antioxidant.
Through calculation, in the components, the weight ratio of the liquid metal heat-conducting paste to the composite spherical heat-conducting filler is 1: 2; the ratio of the weight of the micron-sized spherical heat-conducting filler to the total weight of the composite spherical heat-conducting filler is 0.8: 1.
the insulating efficient heat-conducting silicone grease provided in embodiment 2 is prepared by the following method, which includes the following steps:
step 1, adding 55 parts of aluminum nitride (average particle size of 10 μm), 25 parts of aluminum nitride (average particle size of 5 μm) and 20 parts of modified heat-conducting ceramic powder (average particle size of 200nm) into a high-speed mixer (FM-3L, Nippon Sanjing mine Co., Ltd.) respectively, and mixing and dispersing at an online speed of 55m/s for 10min to obtain a composite spherical heat-conducting filler;
step 2, adding 0.5 part of modified flake graphene (with the average particle size of 20 microns) and 4 parts of modified carbon fiber (with the average particle size of 50 microns) into the high-speed mixer in the step 1, and mixing and dispersing for 10min at the online speed of 50m/s to obtain the high-speed dispersed heat-conducting filler;
and 3, adding 50 parts of liquid metal heat-conducting paste into the high-speed mixer in the step 2, and then mixing and dispersing for 10min at an online speed of 50m/s to obtain the heat-conducting filler after high-speed dispersion.
Step 4, placing the heat-conducting filler obtained in the step 3 after high-speed dispersion in a vacuum stirrer, and vacuumizing for 30min at the temperature of 100 ℃ to remove air in the heat-conducting filler;
and 5, uniformly mixing 10 parts of methyl silicone oil (the viscosity is 1000CP), 0.5 part of dodecyl trimethoxy silane coupling agent and 1 part of antioxidant 1010, adding the mixture into the vacuum stirrer in the step 4, vacuumizing and stirring the mixture for 1 hour at the temperature of 100 ℃, then heating the mixture to 150 ℃, and vacuumizing and stirring the mixture for 1 hour at the temperature of 150 ℃ to obtain the heat-conducting silicone grease with the heat conductivity coefficient of 8.6W/m.K.
Example 3
The insulating efficient heat-conducting silicone grease provided by the embodiment 3 comprises the following components in parts by weight:
75 parts of modified heat-conducting ceramic powder with the average particle size of 10 microns, 15 parts of modified heat-conducting ceramic powder with the average particle size of 5 microns, 10 parts of modified alumina powder with the average particle size of 100nm, 0.5 part of modified flake graphene with the average particle size of 20 microns, 5 parts of modified carbon fiber with the average particle size of 35 microns, 70 parts of liquid metal heat-conducting paste, 8 parts of methyl silicone oil with the viscosity of 1000CP, 3 parts of vinyl silicone oil with the viscosity of 500CP, 0.5 part of dodecyl trimethoxy silane and 10760.5 parts of antioxidant.
Through calculation, in the components, the weight ratio of the liquid metal heat-conducting paste to the composite spherical heat-conducting filler is 1: 1.43; the ratio of the weight of the micron-sized spherical heat-conducting filler to the total weight of the composite spherical heat-conducting filler is 0.9: 1.
the insulating efficient heat-conducting silicone grease provided in embodiment 3 is prepared by the following method, which includes the following steps:
step 1, adding 75 parts of modified heat-conducting ceramic powder (with an average particle size of 10 μm), 15 parts of modified heat-conducting ceramic powder (with an average particle size of 5 μm) and 10 parts of modified alumina powder (with an average particle size of 100nm) into a high-speed mixer (FM-3L, Mitsui mine Co., Ltd., Japan) respectively, and mixing and dispersing for 10min at an online speed of 50m/s to obtain a composite spherical heat-conducting filler;
step 2, adding 0.5 part of modified flake graphene (with the average particle size of 20 microns) and 5 parts of modified carbon fibers (with the average particle size of 35 microns) into the high-speed mixer in the step 1, and mixing and dispersing for 10min at the online speed of 50m/s to obtain the high-speed dispersed heat-conducting filler;
and 3, adding 70 parts of liquid metal heat-conducting paste into the high-speed mixer in the step 2, and mixing and dispersing for 10min at an online speed of 50m/s to obtain the heat-conducting filler after high-speed dispersion.
Step 4, placing the heat-conducting filler obtained in the step 3 after high-speed dispersion in a vacuum stirrer, and vacuumizing for 30min at the temperature of 100 ℃ to remove air in the heat-conducting filler;
and 5, uniformly mixing 8 parts of methyl silicone oil (the viscosity is 1000CP), 3 parts of vinyl silicone oil (the viscosity is 500CP), 0.5 part of dodecyl trimethoxy silane and 0.5 part of antioxidant 1076, adding into the vacuum stirrer in the step 4, vacuumizing and stirring for 1 hour at 100 ℃, then heating to 150 ℃, vacuumizing and stirring for 1 hour at 150 ℃ to obtain the heat-conducting silicone grease with the heat conductivity coefficient of 9.3W/m.K.
Example 4
The insulating efficient heat-conducting silicone grease provided by the embodiment 4 comprises the following components in parts by weight:
60 parts of modified heat-conducting ceramic powder with the average particle size of 10 microns, 20 parts of modified aluminum nitride powder with the average particle size of 5 microns, 10 parts of modified alumina powder with the average particle size of 100nm, 10 parts of modified heat-conducting ceramic powder with the average particle size of 200 microns, 0.5 part of modified sheet graphene with the average particle size of 20 microns, 4 parts of modified carbon fiber with the average particle size of 50 microns, 90 parts of liquid metal heat-conducting paste, 8 parts of methyl silicone oil with the viscosity of 1000CP, 3 parts of vinyl silicone oil with the viscosity of 500CP, 1 part of dodecyl trimethoxy silane, 10100.5 parts of antioxidant and 10760.5 parts of antioxidant.
Through calculation, in the components, the weight ratio of the liquid metal heat-conducting paste to the composite spherical heat-conducting filler is 1: 1.11; the ratio of the weight of the micron-sized spherical heat-conducting filler to the total weight of the composite spherical heat-conducting filler is 0.8: 1.
the insulating efficient heat-conducting silicone grease provided in embodiment 4 is prepared by the following method, which includes the following steps:
step 1, adding 60 parts of modified heat-conducting ceramic powder (with an average particle size of 10 microns), 20 parts of modified aluminum nitride powder (with an average particle size of 5 microns), 10 parts of modified alumina powder (with an average particle size of 100nm) and 10 parts of modified heat-conducting ceramic powder (with an average particle size of 200nm) into a high-speed mixer (FM-3L, Nippon Mitsui mine Co., Ltd.) respectively, and mixing and dispersing for 10min at an online speed of 50m/s to obtain a composite spherical heat-conducting filler;
step 2, adding 0.5 part of modified flake graphene (with the average particle size of 20 microns) and 4 parts of modified carbon fiber (with the average particle size of 50 microns) into the high-speed mixer in the step 1, and mixing and dispersing for 10min at the online speed of 50m/s to obtain the high-speed dispersed heat-conducting filler;
and 3, adding 90 parts of liquid metal heat-conducting paste into the high-speed mixer in the step 2, and mixing and dispersing for 10min at an online speed of 50m/s to obtain the heat-conducting filler after high-speed dispersion.
Step 4, placing the heat-conducting filler obtained in the step 3 after high-speed dispersion in a vacuum stirrer, and vacuumizing for 30min at the temperature of 100 ℃ to remove air in the heat-conducting filler;
and 5, uniformly mixing 8 parts of methyl silicone oil (the viscosity is 1000CP), 3 parts of vinyl silicone oil (the viscosity is 500CP), 1 part of dodecyl trimethoxy silane coupling agent, 0.5 part of antioxidant 1010 and 0.5 part of antioxidant 1076, adding the mixture into a vacuum stirrer in the step 4, vacuumizing and stirring the mixture for 1 hour at the temperature of 100 ℃, then heating the mixture to 150 ℃, and vacuumizing and stirring the mixture for 1 hour at the temperature of 150 ℃ to obtain the heat-conducting silicone grease with the heat conductivity coefficient of 10.1W/m.K.
Comparative example 1
The heat-conducting silicone grease provided by the comparative example 1 comprises the following components in parts by weight:
65 parts of modified heat-conducting ceramic powder with the average particle size of 10 microns, 25 parts of modified heat-conducting ceramic powder with the average particle size of 5 microns, 15 parts of modified heat-conducting ceramic powder with the average particle size of 200nm, 0.5 part of modified sheet graphene with the average particle size of 20 microns, 5 parts of modified carbon fiber with the average particle size of 35 microns, 8 parts of methyl silicone oil with the viscosity of 1000CP, 2 parts of vinyl silicone oil with the viscosity of 500CP and 0.5 part of dodecyl trimethoxy silane.
The heat-conducting silicone grease provided in comparative example 1 is prepared by the following method:
respectively placing 65 parts of modified heat-conducting ceramic powder (with the average particle size of 10 microns), 25 parts of modified heat-conducting ceramic powder (with the average particle size of 5 microns), 15 parts of modified heat-conducting ceramic powder (with the average particle size of 200nm), 0.5 part of modified sheet graphene (with the average particle size of 20 microns) and 5 parts of modified carbon fiber (with the average particle size of 35 microns) in a vacuum stirrer, and vacuumizing for 30min at 100 ℃; then 8 parts of methyl silicone oil (the viscosity is 1000CP), 2 parts of vinyl silicone oil (the viscosity is 500CP) and 0.5 part of dodecyl trimethoxy silane are uniformly mixed and then continuously injected into the vacuum stirrer, and the mixture is vacuumized and stirred for 1 hour at the temperature of 100 ℃; then heating to 150 ℃, and vacuumizing and stirring for 1h at 150 ℃ to obtain the comparative heat-conducting silicone grease with the heat conductivity coefficient of 6.2W/m.K.
Comparative example 2
The heat-conducting silicone grease provided by the comparative example 2 comprises the following components in parts by weight:
65 parts of modified heat-conducting ceramic powder with the average particle size of 10 microns, 25 parts of modified heat-conducting ceramic powder with the average particle size of 5 microns, 15 parts of modified heat-conducting ceramic powder with the average particle size of 200nm, 0.5 part of modified sheet graphene with the average particle size of 20 microns, 5 parts of modified carbon fiber with the average particle size of 35 microns, 200 parts of liquid metal heat-conducting paste, 8 parts of methyl silicone oil with the viscosity of 1000CP, 2 parts of vinyl silicone oil with the viscosity of 500CP and 0.5 part of dodecyl trimethoxy silane.
The heat-conducting silicone grease provided in comparative example 2 is prepared by the following method:
respectively placing 65 parts of modified heat-conducting ceramic powder (with the average particle size of 10 microns), 25 parts of modified heat-conducting ceramic powder (with the average particle size of 5 microns), 15 parts of modified heat-conducting ceramic powder (with the average particle size of 200nm), 0.5 part of modified sheet graphene (with the average particle size of 20 microns) and 5 parts of modified carbon fiber (with the average particle size of 35 microns) in a vacuum stirrer, and vacuumizing for 30min at 100 ℃; adding 150 parts of liquid metal heat-conducting paste, 8 parts of methyl silicone oil with the viscosity of 1000CP, 2 parts of vinyl silicone oil with the viscosity of 500CP and 0.5 part of dodecyl trimethoxy silane coupling agent into the vacuum stirrer, and vacuumizing and stirring for 1 hour at the temperature of 100 ℃; then heating to 150 ℃, and vacuumizing and stirring for 1h at 150 ℃ to obtain the comparative heat-conducting silicone grease with the heat conductivity coefficient of 12W/m.K.
TABLE 1 contents of respective components in examples 1 to 4 and comparative examples 1 to 2
In order to verify the physical properties of the heat-conducting silicone grease obtained in the present invention, the viscosity, the thermal conductivity, the volatility and the volume resistivity of the heat-conducting silicone grease obtained in examples 1 to 4 and comparative examples 1 to 2 were respectively measured, and the measurement results are shown in table 2 below:
TABLE 2 results of measuring physical Properties of thermally conductive Silicone greases obtained in examples 1 to 4 and comparative examples 1 to 2
From the experimental results in table 1 and the test data in table 2, it can be seen that: comparative example 1, in which no liquid metal thermal paste was added, the thermal conductivity was at the level of 6W/m · K, but if the thermal conductivity was increased by increasing the filler filling rate, the viscosity of the thermal grease became large, and a problem of high-temperature dry cracking occurred; the proportion of the liquid metal heat conductive paste added in comparative example 2 is much higher than that of the heat conductive filler, and although the heat conductivity can reach a level of 14W/m · K or more, the heat conductive silicone grease is relatively dry and hard and no longer has insulation.
In embodiments 1 to 4, the micron heat-conducting filler is coated with the nano heat-conducting filler in a high-speed dispersion manner, and the liquid metal heat-conducting paste is used to fill the tiny gaps on the surface of the heat-conducting filler, so that the contact thermal resistance among filler particles is effectively reduced, and the good insulation property of the heat-conducting silicone grease can be maintained while the high-efficiency heat-conducting performance is obtained; therefore, the heat-conducting silicone grease disclosed by the invention has the characteristics of high heat conductivity coefficient, low thermal resistance, insulation and difficulty in drying, and has a good commercial application prospect.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (10)
1. An insulating efficient heat-conducting silicone grease is characterized by comprising the following components in parts by weight: 80-100 parts of composite spherical heat-conducting filler, 0.5-5 parts of one-dimensional structure heat-conducting material, 0.5-5 parts of two-dimensional structure heat-conducting material, 20-100 parts of liquid metal heat-conducting paste, 4-20 parts of silicone oil, 0.25-2 parts of silane coupling agent and 0.1-1 part of antioxidant.
2. The insulating high-efficiency heat-conducting silicone grease as claimed in claim 1, wherein the composite spherical heat-conducting filler comprises micron-sized spherical heat-conducting filler and nanometer-sized spherical heat-conducting filler, and the ratio of the weight of the micron-sized spherical heat-conducting filler to the total weight of the composite spherical heat-conducting filler is (0.75-0.95): 1.
3. the insulating high-efficiency heat-conducting silicone grease as claimed in claim 2, wherein the micron-sized spherical heat-conducting filler has an average particle size of 3-30 μm; the micron-scale spherical heat-conducting filler is at least one of spherical modified heat-conducting ceramic powder, modified aluminum nitride and modified diamond.
4. The insulating high-efficiency heat-conducting silicone grease as claimed in claim 3, wherein the nano-scale heat-conducting filler has an average particle size of 50-200 nm; the nano-scale heat-conducting filler is at least one of modified alumina and modified heat-conducting ceramic powder.
5. The insulating high-efficiency heat-conducting silicone grease as claimed in any one of claims 1 to 4, wherein the weight ratio of the liquid metal heat-conducting paste to the composite spherical heat-conducting filler is 1: (1-5).
6. The insulating high-efficiency heat-conducting silicone grease as claimed in claim 5, wherein the average length of the one-dimensional structure heat-conducting material is 1-50 μm, and the one-dimensional structure heat-conducting material is at least one of modified carbon fiber, carbon nanotube, modified silicon carbide whisker, modified silver nanowire and modified gold nanowire.
7. The insulating efficient heat-conducting silicone grease as claimed in claim 1, wherein the average particle size of the two-dimensional structure heat-conducting material is 0.5-30 μm, and the two-dimensional structure heat-conducting material is at least one of modified sheet graphene, modified sheet boron nitride and modified sheet silicon carbide.
8. The insulating efficient heat-conducting silicone grease as claimed in claim 6 or 7, wherein the liquid metal heat-conducting paste is one of gallium, gallium indium tin zinc, bismuth indium tin zinc alloy; the silicone oil is at least one organic silicon polymer of methyl-terminated polydimethylsiloxane, methyl-terminated polymethylphenylsiloxane, vinyl-terminated polymethylsiloxane and vinyl-terminated polymethylphenylsiloxane; the silane coupling agent is at least one of methyltrimethoxysilane, methyltriethoxysilane, dodecyl trimethoxysilane, phenyl trimethoxysilane and vinyl trimethoxysilane; the antioxidant is at least one of antioxidant 1010 and antioxidant 1076.
9. The preparation method of the high-efficiency heat-conducting silicone grease is characterized by comprising the following steps:
step 1, respectively weighing the following components in parts by weight: 80-100 parts of composite spherical heat-conducting filler, 0.5-5 parts of one-dimensional structure heat-conducting material, 0.5-5 parts of two-dimensional structure heat-conducting material, 20-100 parts of liquid metal heat-conducting paste, 4-20 parts of silicone oil, 0.25-2 parts of silane coupling agent and 0.1-1 part of antioxidant;
step 2, sequentially adding the composite spherical heat-conducting filler, the one-dimensional heat-conducting filler and the two-dimensional heat-conducting filler in the step 1 into a high-speed mixer, and mixing and dispersing for 5-30 min under the condition that the online speed is 25-70 m/s;
step 3, adding the liquid metal heat conducting paste in the step 1 into the high-speed mixer in the step 2, and mixing and dispersing for 5-30 min at an online speed of 25-70 m/s to obtain a heat conducting filler after high-speed dispersion;
step 4, placing the heat-conducting filler obtained in the step 3 after high-speed dispersion in a vacuum stirrer, and vacuumizing for 10-30 min at the temperature of 70-120 ℃;
and 5, uniformly mixing the silicone oil, the silane coupling agent and the antioxidant in the step 1, injecting the mixture into the vacuum stirrer in the step 4, vacuumizing and stirring the mixture for 1 to 3 hours at the temperature of 70 to 120 ℃, and vacuumizing and stirring the mixture for 1 to 3 hours at the temperature of 150 to 200 ℃ to obtain the heat-conducting silicone grease.
10. The method for preparing the high-efficiency heat-conducting silicone grease as claimed in claim 12, wherein in the step 1, the specific preparation method of the composite spherical heat-conducting filler is as follows:
80-100 parts of micron-sized spherical heat-conducting filler and modified nano-scale heat-conducting filler are mixed according to the weight ratio of 95: 5-75: adding the mixture into a high-speed mixer according to the proportion of 25, and mixing and dispersing for 5-30 min under the condition that the linear speed is 25-70 m/s to obtain the composite spherical heat-conducting filler.
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