CN110713721A - Preparation method of high-thermal-conductivity silicone rubber - Google Patents
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Abstract
The invention discloses a preparation method of high-thermal-conductivity silicone rubber, which comprises the steps of mixing graphite with spherical thermal-conductivity filler, stripping natural graphite into graphene with a thinner nano lamellar structure by adopting a planetary ball milling method, promoting the dispersion of the spherical thermal-conductivity filler to obtain the graphene-coated thermal-conductivity filler, forming silicone rubber compound by proportioning, fully dispersing the modified thermal-conductivity filler in a silicone rubber matrix under the ultrasonic action to form a thermal-conductivity network, and preparing the silicone rubber nanocomposite with high thermal-conductivity coefficient by high-temperature high-pressure die pressing. The preparation method of the high-thermal-conductivity silicone rubber provided by the invention can easily enable graphene and a thermal-conductivity filler to form a communicated thermal-conductivity network in the silicone rubber, and particularly can greatly improve the heat dissipation performance of the silicone rubber thermal interface material by using a very small amount of graphene, and is particularly suitable for the heat dissipation field of electronic products.
Description
Technical Field
The invention relates to a preparation method of high-thermal-conductivity silicone rubber, belonging to the technical field of preparation methods of high-thermal-conductivity silicone rubber nano composite materials.
Background
With the advent of the 5G era, rapid development of electronic devices in the direction of miniaturization and integration has led to the inevitable generation of a large amount of heat during operation of electronic devices, resulting in a rapid rise in the internal temperature of electronic equipment. If the heat dissipation problem of these heating elements is not solved effectively, their service life is seriously affected. Therefore, the efficient heat dissipation capability has become a key factor that limits the service life of electronic devices. In order to enable the electronic device to operate efficiently and stably for a long time, effective heat management measures must be taken to take away heat generated during the operation of the electronic device in time, so that the devices are ensured to be in a good working environment. The thermal interface material is a material with good heat dissipation performance, and is mainly used for filling up micro-gaps and holes with uneven surfaces generated when two materials are jointed or contacted, and expelling air in the contact gaps, so that a good heat conduction path is formed between the heater and the radiator, and the heat dissipation efficiency of the radiator is improved. The common thermal interface materials mainly include heat-conducting silicone grease, heat-conducting silicone rubber and heat-conducting gaskets.
The heat conductive silicone rubber has excellent properties such as high heat conductivity, insulation property and low hardness, and is therefore the most commonly used heat conductive gasket in microelectronic heat dissipation. At present, many researchers at home and abroad have carried out corresponding research on heat-conducting silicone rubber, but the following problems still exist: firstly, the thermal conductivity of the silicone rubber is not high; second, the requirement for electrical insulation cannot be met. Therefore, the development of the silicone rubber thermal interface material with high thermal conductivity and electrical insulation is a problem to be solved in the field of heat dissipation of electronics and electrical appliances.
In order to improve the thermal conductivity of the heat-conducting silicone rubber composite material, a heat-conducting filler is usually added to improve the thermal conductivity, and the currently commonly used heat-conducting filler is alumina, aluminum nitride, metal powder, boron nitride, silicon carbide and the like, but the heat-conducting filler has a low thermal conductivity, and a high thermal conductivity can be obtained only under the condition of a high filling amount, so that the processing performance of the heat-conducting silicone rubber composite material is reduced, and the hardness of the vulcanized rubber is improved (functional materials, 2014,45(20): 20001-20006; Journal of Applied Polymer Science 2010,32(7):5705-5712), which greatly limits the application. Graphene as a novel carbon material has the characteristic of high thermal conductivity, and theoretically, the thermal conductivity of single-layer graphene is as high as 5150W/m.k, so that graphene is the material with the highest thermal conductivity at present. Meanwhile, graphene has high diameter-thickness ratio (more than 5000) and specific surface area (2600m2/g), and is very favorable for interaction and compatibility with matrix resin. However, graphene has a high thermal conductivity and a high electrical conductivity, so that the insulating property thereof is greatly impaired. In addition, graphene is mainly stripped in an ultrasonic mode at present, but the stripping effect is not very outstanding, and meanwhile, the dispersion in a resin matrix is not good, so that the improvement of the thermal conductivity of the graphene to the silicone rubber is greatly influenced. Therefore, how to balance the thermal conductivity and the insulation of the heat-conducting silicone rubber breaks through the key technology of filler preparation is one of the technical problems to be solved urgently in the heat-conducting industry. For example, chinese patent 201310629967.1 discloses a graphene-containing high thermal conductivity silicone rubber composite material and a preparation method thereof, in which graphene is directly added to a substrate to obtain a thermal conductivity silicone rubber composite material, and the thermal conductivity coefficient of graphene is only 0.3 to 1.5W/m · k due to poor compatibility between graphene and silicone rubber. Chinese patent 201310406773.5 discloses a heat-conducting electrically-insulating silicon rubber thermal interface material and a preparation method thereof, wherein graphene is dispersed into a thinner and more uniform nano-sheet structure under ultrasonic waves, and then the graphene is compounded with spherical aluminum oxide, mixed with silicon rubber, and subjected to compression molding to obtain the electrically-insulating silicon rubber thermal interface material with the thermal conductivity coefficient of 3.3W/m.k. The Chinese invention patent CN102827480A discloses a method for preparing a high-thermal-conductivity silicone rubber composite material, wherein the thermal conductivity coefficient is improved by adding expanded graphite into a silicone rubber matrix, but the treatment process of graphite is more complicated and is not beneficial to industrial large-scale production. The Chinese invention patent 201811584072.X discloses a high-thermal-conductivity and high-strength silicone rubber/graphene composite material and a preparation method thereof, the compatibility between graphene and silicone rubber is improved by adding the graphene into the silicone rubber after ball milling, and the thermal conductivity coefficient of the composite material can reach 3.49W/m.k at most. Chinese patent 201310372003.3 discloses a high thermal conductivity insulating and heat conducting silica gel pad and a preparation method thereof, which is to fully grind a base material such as silica gel to realize the fusion between a silica gel base and inorganic heat conducting particles, so that the thermal conductivity coefficient can be improved to more than 5.0W/m.k.
Although the method for preparing the heat-conducting silicone rubber can enable the heat conductivity coefficient to reach more than 5.0W/m.k, the method cannot embody the advantage that the graphene with ultrahigh heat-conducting property is applied to the silicone rubber, and cannot meet the requirement of high-power electronic equipment on the heat-conducting property of the heat-conducting material. Therefore, the preparation method of the high-heat-conductivity insulating silicone rubber has the advantages that the toughness of the silicone rubber is effectively improved, the silicone rubber can be conveniently produced in a large scale, and the preparation method is very important for developing the high-heat-conductivity insulating silicone rubber with excellent performance and promoting the wide application of the silicone rubber in the electronic and electrical industry.
Disclosure of Invention
The invention aims to solve the defects of the prior art and solve the problems, and provides a preparation method of high-thermal-conductivity silicone rubber.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
the preparation method of the high-thermal-conductivity silicone rubber comprises the following steps:
the material of S1 is selected,
selecting graphite, heat-conducting filler, a silicon rubber substrate, silicon oil, a catalyst, an inhibitor and a cross-linking agent;
the planetary ball milling of S2 is carried out,
mixing graphite and a heat-conducting filler in a solid phase, and carrying out planetary ball milling to obtain a graphene-coated filler;
the ultrasonic wave treatment is carried out at S3,
carrying out ultrasonic treatment on the graphene coated filler to obtain a treated heat conducting filler;
the mixture is subjected to the S4 mixing,
putting the graphene coated filler, the heat conducting filler, the silicon rubber base material, the silicon oil, the catalyst, the inhibitor and the cross-linking agent into a double-roll open mill, and fully mixing to obtain a silicon rubber compound;
s5 removing the bubbles in the vacuum,
placing the silicon rubber compound in a vacuum oven for removing internal bubbles;
s6, die pressing and forming are carried out,
and (3) putting the defoamed silicon rubber compound into a flat vulcanizing press to perform high-temperature high-pressure compression molding to obtain the high-heat-conductivity silicon rubber.
Preferably, in step S1, the following components are taken in parts by mass: 0.1-2 parts of graphite, 20-80 parts of silicone rubber base material, 5-85 parts of heat-conducting filler, 0.1-5 parts of silicone oil, 0.01-2 parts of catalyst and inhibitor: 0.01 to 1 part, and 0.1 to 2 parts of a crosslinking agent.
Preferably, the crystal grain size of the graphite is 0.5 mm-1 μm, the carbon content is 80-99.99%, and the density is 0.7-1.40%;
the silicon rubber base material is one or a combination of more of dimethyl silicon rubber, methyl vinyl silicon rubber and methyl phenyl silicon rubber;
the heat-conducting filler is one or a combination of more of aluminum oxide, zinc oxide, silicon carbide, boron nitride, silicon nitride and aluminum nitride, and the particle size is 0.3-500 mu m;
the cross-linking agent is one or more of 2, 5-dimethyl-2, 5-bis (tert-butylperoxy) hexane, dicumyl peroxide, benzoyl peroxide and 2, 4-dichlorobenzoyl peroxide;
the inhibitor is one or more of methyl phenyl diethoxy silane, diphenyl silanediol and hexamethylcyclotrisilazane;
the silicone oil is one or the combination of two of hydrogen-containing silicone oil and dimethyl silicone oil, wherein the hydrogen content of the hydrogen-containing silicone oil accounts for 0.05-0.2% of the total weight of the hydrogen-containing silicone oil;
the catalyst is a platinum catalyst.
Preferably, in the step S2, the planetary ball milling time is 30 to 240min, and the ball milling rotation speed is 100 to 600 r/min.
Preferably, in the step S3, the ultrasonic power is 300W, and the ultrasonic treatment time is 30-120 min.
Preferably, in the step S4, the rotation speed of the two-roll mill is 30 to 100rpm, and the mixing time is 10 to 30 min.
Preferably, in the step S5, the vacuum oven has a vacuum degree of 0.095, and the treatment is performed at a temperature of 30 to 70 ℃ for 30 to 100 min.
Preferably, in the step S6, the mold pressing temperature is 100-165 ℃, the mold pressing pressure is 1-15 MPa, and the mold pressing time is 5-30 min.
The invention has the following beneficial effects:
the preparation method of the high-thermal-conductivity silicone rubber can easily enable the graphene and the thermal-conductivity filler to form a communicated thermal-conductivity network in the silicone rubber, particularly, the method can greatly improve the heat dissipation performance of the silicone rubber thermal interface material by using a very small amount of graphene, and is particularly suitable for the heat dissipation field of electronic products.
Detailed Description
The invention provides a preparation method of high-thermal-conductivity silicone rubber. The technical solutions of the present invention are described in detail below to make them easier to understand and master.
The preparation method of the high-thermal-conductivity silicone rubber comprises the following steps:
selecting materials, namely selecting graphite, heat-conducting filler, silicon rubber base material, silicone oil, catalyst, inhibitor and cross-linking agent.
And (3) planetary ball milling, namely mixing graphite and a heat-conducting filler in a solid phase, and performing planetary ball milling to obtain the graphene coated filler. The planetary ball milling time is 30-240 min, and the ball milling speed is 100-600 r/min.
And (3) performing ultrasonic treatment, namely performing ultrasonic treatment on the graphene coated filler to obtain the treated heat conducting filler. The ultrasonic power is 300W, and the ultrasonic treatment time is 30-120 min.
And mixing, namely putting the graphene coated filler, the heat-conducting filler, the silicon rubber base material, the silicon oil, the catalyst, the inhibitor and the cross-linking agent into a double-roll mill for fully mixing to obtain the silicon rubber compound. The rotating speed of the double-roller open mill is 30-100 rpm, and the mixing time is 10-30 min.
And (4) removing bubbles in vacuum, namely placing the silicon rubber compound in a vacuum oven to remove internal bubbles. The vacuum degree of the vacuum oven is 0.095, and the treatment is carried out for 30-100 min at the maintenance temperature of 30-70 ℃.
And (3) compression molding, namely putting the defoamed silicon rubber compound into a flat vulcanizing press to perform high-temperature high-pressure compression molding to obtain the high-thermal-conductivity silicon rubber. The mould pressing temperature is 100-165 ℃, the mould pressing pressure is 1-15 MPa, and the mould pressing time is 5-30 min.
When the materials are selected, the materials are taken according to the following parts by mass: 0.1-2 parts of graphite, 20-80 parts of silicone rubber base material, 5-85 parts of heat-conducting filler, 0.1-5 parts of silicone oil, 0.01-2 parts of catalyst and inhibitor: 0.01 to 1 part, and 0.1 to 2 parts of a crosslinking agent.
The components are explained in detail:
the graphite has a crystal grain size of 0.5 mm-1 μm, a carbon content of 80-99.99%, and a density of 0.7-1.40%.
The silicon rubber base material is one or a combination of more of dimethyl silicon rubber, methyl vinyl silicon rubber and methyl phenyl silicon rubber.
The heat-conducting filler is one or a combination of more of aluminum oxide, zinc oxide, silicon carbide, boron nitride, silicon nitride and aluminum nitride, and the particle size is 0.3-500 mu m.
The cross-linking agent is one or a combination of 2, 5-dimethyl-2, 5-bis (tert-butylperoxy) hexane, dicumyl peroxide, benzoyl peroxide and 2, 4-dichlorobenzoyl peroxide.
The inhibitor is one or more of methyl phenyl diethoxy silane, diphenyl silanediol and hexamethylcyclotrisilazane.
The silicone oil is one or the combination of two of hydrogen-containing silicone oil and dimethyl silicone oil, wherein the hydrogen content of the hydrogen-containing silicone oil accounts for 0.05-0.2% of the total weight of the hydrogen-containing silicone oil.
The catalyst is a platinum catalyst.
The heat-conducting filler in the present invention may be subjected to a surface treatment before being subjected to planetary ball milling, and the surface treatment agent is one or a combination of a151, WD-10, KH550, KH560 and KH 570.
Example 1
Selecting the following components in parts by mass, wherein the natural graphene (with the particle size of 1 mu m) is prepared from the following raw materials: 0.5 part; methyl vinyl silicone rubber: 80 parts of a mixture; spherical alumina (particle size 75 μm): 70 parts of (B); hydrogen-containing silicone oil (hydrogen content is 0.06 percent of the total weight of the hydrogen-containing silicone oil): 1.0 part; platinum catalyst: 0.05 part; diphenyl silanediol: 0.01 part; 2, 5-dimethyl-2, 5-bis (t-butylperoxy) hexane: 0.1 part.
Firstly, spherical alumina powder with the particle size of 75 microns and natural graphene (with the particle size of 1 micron) are subjected to solid-phase mixing by adopting planetary ball milling to obtain the graphene-coated heat-conducting filler, wherein the ball milling speed is 100r/min, and the ball milling time is 200 min. And secondly, adding the graphene-coated heat-conducting filler into the methyl vinyl silicone rubber, and treating for 80min under ultrasonic waves with the ultrasonic power of 300W. Then, the silicone rubber premix containing the heat-conducting filler, hydrogen-containing silicone oil, platinum catalyst, diphenylsilanediol and 2, 5-dimethyl-2, 5-bis (t-butylperoxy) hexane were kneaded in a two-roll mill at room temperature for 30min to obtain a silicone rubber compound. Wherein the rotation speed of the two-roll open mill is 70 rpm. The rubber compound was placed in a vacuum oven (degree of vacuum 0.095) and treated at 30 ℃ for 80min to remove internal air bubbles. And finally, putting the heat-conducting silicone rubber compound into a mold, and molding the nano carbon material and the silicone rubber resin filled with the heat-conducting filler through high-temperature and high-pressure mold. Wherein the mould pressing temperature is 130 ℃, the mould pressing pressure is 5MPa, and the mould pressing time is 30 min. And taking out the sample after the grinding tool is naturally cooled to room temperature, thus obtaining the high-heat-conductivity silicon rubber nano composite material. The heat conduction coefficient of the heat conduction silicon rubber composite material is 5.5W/m.K, and the thickness is 1.0 mm.
Example 2
Selecting the following components in parts by mass, namely natural graphite (with the thickness of 70 mm): 0.64 part, methylphenyl silicone rubber: 75 parts, boron nitride and zinc oxide: 75 parts of hydrogen-containing silicone oil (the hydrogen content accounts for 0.1 percent of the total weight of the hydrogen-containing silicone oil): 1.0 part, platinum catalyst: 1.0 part, methylphenyldiethoxysilane: 0.02 part; 2, 4-dichlorobenzoyl peroxide: 0.2 part.
Firstly, a mixture of boron nitride and zinc oxide and natural graphite (with the thickness of 70mm) are mixed in a solid phase manner by adopting planetary ball milling to obtain the graphene-coated heat-conducting filler, wherein the ball milling speed is 250r/min, and the ball milling time is 100 min. And secondly, adding the graphene-coated heat-conducting filler into methyl phenyl silicone rubber, and treating for 60min under ultrasonic waves with the ultrasonic power of 300W. Then, the silicone rubber premix containing the heat-conducting filler, hydrogen-containing silicone oil, platinum catalyst, methyl phenyl diethoxy silane and 2, 4-dichlorobenzoyl peroxide are mixed in a two-roll mill for 20min at room temperature to obtain silicone rubber compound. Wherein the rotation speed of the two-roll open mill is 70 rpm. The rubber compound was placed in a vacuum oven (degree of vacuum 0.095) and treated at 40 ℃ for 50min to remove internal air bubbles. And finally, putting the heat-conducting silicone rubber compound into a mold, and molding the nano carbon material and the silicone rubber resin filled with the heat-conducting filler through high-temperature and high-pressure mold. Wherein the mould pressing temperature is 140 ℃, the mould pressing pressure is 3.5MPa, and the mould pressing time is 20 min. And taking out the sample after the grinding tool is naturally cooled to room temperature, thus obtaining the high-heat-conductivity silicon rubber nano composite material. The heat conduction coefficient of the heat conduction silicon rubber composite material is 8.3W/m.K, and the thickness is 2.5 mm.
Example 3
Selecting the following components in parts by mass, namely natural graphite (with the particle size of 55 mm): 0.15 part, dimethyl silicone rubber: 70 parts, aluminum oxide and silicon nitride: 65 parts of hydrogen-containing silicone oil (the hydrogen content accounts for 0.1 percent of the total weight of the hydrogen-containing silicone oil): 2.0 parts, platinum catalyst: 1.0 part, hexamethylcyclotrisilazane: 0.02 part; benzoyl peroxide: 0.2 part.
Firstly, a mixture of aluminum oxide and silicon nitride and natural graphite (with the particle size of 55mm) are mixed in a solid phase by adopting planetary ball milling to obtain the graphene-coated heat-conducting filler, wherein the ball milling speed is 250r/min, and the ball milling time is 100 min. And secondly, adding the graphene-coated heat-conducting filler into the dimethyl silicone rubber, and treating for 60min under ultrasonic waves with the ultrasonic power of 300W. Then, the silicone rubber premix containing the heat-conducting filler, hydrogen-containing silicone oil, platinum catalyst, hexamethylcyclotrisilazane and benzoyl peroxide are mixed in a two-roll mill for 30min at room temperature to obtain the silicone rubber compound. Wherein the rotation speed of the two-roll open mill is 90 rpm. The rubber compound was placed in a vacuum oven (degree of vacuum 0.095) and treated at 50 ℃ for 20min to remove internal air bubbles. And finally, putting the heat-conducting silicon rubber compound into a mould, and filling the nano-carbon material and the heat-conducting filler into the silicon rubber resin through high-temperature high-pressure mould pressing. Wherein the mould pressing temperature is 120 ℃, the mould pressing pressure is 6.0MPa, and the mould pressing time is 25 min. And taking out the sample after the grinding tool is naturally cooled to room temperature, thus obtaining the high-heat-conductivity silicon rubber nano composite material. The heat conduction coefficient of the heat conduction silicon rubber composite material is 9.2W/m.K, and the thickness is 3.5 mm.
Example 4
Selecting the following components in parts by mass, namely natural graphite (the grain diameter of a crystal is 10 mm): 0.15 part, methyl vinyl silicone rubber: 75 parts, hexagonal boron nitride: 80 parts of hydrogen-containing silicone oil (the hydrogen content accounts for 0.15 percent of the total weight of the hydrogen-containing silicone oil): 3.0 parts, platinum catalyst: 1.0 part, methylphenyldiethoxysilane: 0.02 part; 2, 4-dichlorobenzoyl peroxide: 0.2 part.
Firstly, mixing hexagonal boron nitride and natural graphite (with the crystal grain diameter of 10mm) in a solid phase by adopting planetary ball milling to obtain the graphene-coated heat-conducting filler, wherein the ball milling speed is 500r/min, and the ball milling time is 60 min. And secondly, adding the graphene-coated heat-conducting filler into the methyl vinyl silicone rubber, and treating for 60min under ultrasonic waves with the ultrasonic power of 300W. Then, the silicone rubber premix containing the heat-conducting filler, hydrogen-containing silicone oil, platinum catalyst, methyl phenyl diethoxy silane and 2, 4-dichlorobenzoyl peroxide are mixed in a two-roll mill for 30min at room temperature to obtain silicone rubber compound. Wherein the rotation speed of the two-roll open mill is 90 rpm. The rubber compound was placed in a vacuum oven (degree of vacuum 0.095) and treated at 40 ℃ for 50min to remove internal air bubbles. And finally, putting the heat-conducting silicon rubber compound into a mould, and filling the nano-carbon material and the heat-conducting filler into the silicon rubber matrix through high-temperature high-pressure mould pressing. Wherein the mould pressing temperature is 120 ℃, the mould pressing pressure is 10MPa, and the mould pressing time is 30 min. And taking out the sample after the grinding tool is naturally cooled to room temperature, thus obtaining the high-heat-conductivity silicon rubber nano composite material. The heat-conducting silicon rubber composite material has the heat conductivity coefficient of 12W/m.K and the thickness of 3.0 mm.
Example 5
Selecting the following components in parts by mass, namely natural graphite (with the particle size of 100 mm): 0.64 part, methylphenyl silicone rubber: 75 parts, boron nitride: 75 parts of hydrogen-containing silicone oil (the hydrogen content accounts for 0.1 percent of the total weight of the hydrogen-containing silicone oil): 2.5 parts, platinum catalyst: 1.5 parts, methylphenyldiethoxysilane: 0.05 part; 2, 5-dimethyl-2, 5-bis (t-butylperoxy) hexane: 1.0 part.
Firstly, mixing boron nitride and natural graphite (with the particle size of 100mm) in a solid phase by adopting planetary ball milling to obtain the graphene-coated heat-conducting filler, wherein the ball milling speed is 250r/min, and the ball milling time is 100 min. And secondly, adding the graphene-coated heat-conducting filler into methyl phenyl silicone rubber, and treating for 60min under ultrasonic waves with the ultrasonic power of 300W. Then, the silicone rubber premix containing the heat conductive filler, hydrogen-containing silicone oil, platinum catalyst, methyl phenyl diethoxysilane and 2, 5-dimethyl-2, 5-bis (t-butylperoxy) hexane were kneaded in a two-roll mill at room temperature for 30min to obtain a silicone rubber compound. Wherein the rotation speed of the two-roll open mill is 95 rpm. The rubber compound was placed in a vacuum oven (degree of vacuum 0.095) and treated at 60 ℃ for 10min to remove internal air bubbles. And finally, putting the heat-conducting silicon rubber compound into a mould, and filling the nano-carbon material and the heat-conducting filler into the silicon rubber resin through high-temperature high-pressure mould pressing. Wherein the mould pressing temperature is 120 ℃, the mould pressing pressure is 15MPa, and the mould pressing time is 30 min. And taking out the sample after the grinding tool is naturally cooled to room temperature, thus obtaining the high-heat-conductivity silicon rubber nano composite material. The heat conduction coefficient of the heat conduction silicon rubber composite material is 15W/m.K, and the thickness is 2.0 mm.
The following table 1 shows performance indexes of the examples.
Through the above description, it can be found that the preparation method of the high thermal conductivity silicone rubber of the present invention easily forms a communicated thermal conductive network between the graphene and the thermal conductive filler in the silicone rubber, and particularly, the method can achieve the purpose of greatly improving the heat dissipation performance of the silicone rubber thermal interface material by using a very small amount of graphene, and is particularly suitable for the heat dissipation field of electronic products.
The technical solutions of the present invention are fully described above, it should be noted that the specific embodiments of the present invention are not limited by the above description, and all technical solutions formed by equivalent or equivalent changes in structure, method, or function according to the spirit of the present invention by those skilled in the art are within the scope of the present invention.
Claims (8)
1. The preparation method of the high-thermal-conductivity silicone rubber is characterized by comprising the following steps:
the material of S1 is selected,
selecting graphite, heat-conducting filler, a silicon rubber substrate, silicon oil, a catalyst, an inhibitor and a cross-linking agent;
the planetary ball milling of S2 is carried out,
mixing graphite and a heat-conducting filler in a solid phase, and carrying out planetary ball milling to obtain a graphene-coated filler;
the ultrasonic wave treatment is carried out at S3,
carrying out ultrasonic treatment on the graphene coated filler to obtain a treated heat conducting filler;
the mixture is subjected to the S4 mixing,
putting the graphene coated filler, the heat conducting filler, the silicon rubber base material, the silicon oil, the catalyst, the inhibitor and the cross-linking agent into a double-roll open mill, and fully mixing to obtain a silicon rubber compound;
s5 removing the bubbles in the vacuum,
placing the silicon rubber compound in a vacuum oven for removing internal bubbles;
s6, die pressing and forming are carried out,
and (3) putting the defoamed silicon rubber compound into a flat vulcanizing press to perform high-temperature high-pressure compression molding to obtain the high-heat-conductivity silicon rubber.
2. The method for preparing the high thermal conductive silicone rubber according to claim 1, wherein:
in the step S1, the following components are taken in parts by mass: 0.1-2 parts of graphite, 20-80 parts of silicone rubber base material, 5-85 parts of heat-conducting filler, 0.1-5 parts of silicone oil, 0.01-2 parts of catalyst and inhibitor: 0.01 to 1 part, and 0.1 to 2 parts of a crosslinking agent.
3. The method for preparing the high thermal conductive silicone rubber according to claim 2, wherein:
the particle size of the graphite crystal is 0.5 mm-1 mu m, the carbon content is 80-99.99%, and the density is 0.7-1.40%;
the silicon rubber base material is one or a combination of more of dimethyl silicon rubber, methyl vinyl silicon rubber and methyl phenyl silicon rubber;
the heat-conducting filler is one or a combination of more of aluminum oxide, zinc oxide, silicon carbide, boron nitride, silicon nitride and aluminum nitride, and the particle size is 0.3-500 mu m;
the cross-linking agent is one or more of 2, 5-dimethyl-2, 5-bis (tert-butylperoxy) hexane, dicumyl peroxide, benzoyl peroxide and 2, 4-dichlorobenzoyl peroxide;
the inhibitor is one or more of methyl phenyl diethoxy silane, diphenyl silanediol and hexamethylcyclotrisilazane;
the silicone oil is one or the combination of two of hydrogen-containing silicone oil and dimethyl silicone oil, wherein the hydrogen content of the hydrogen-containing silicone oil accounts for 0.05-0.2% of the total weight of the hydrogen-containing silicone oil;
the catalyst is a platinum catalyst.
4. The method for preparing the high thermal conductive silicone rubber according to claim 1, wherein:
in the step S2, the planetary ball milling time is 30-240 min, and the ball milling speed is 100-600 r/min.
5. The method for preparing the high thermal conductive silicone rubber according to claim 1, wherein:
in the step S3, the ultrasonic power is 300W, and the ultrasonic treatment time is 30-120 min.
6. The method for preparing the high thermal conductive silicone rubber according to claim 1, wherein:
in the step S4, the rotation speed of the double-roll open mill is 30-100 rpm, and the mixing time is 10-30 min.
7. The method for preparing the high thermal conductive silicone rubber according to claim 1, wherein:
in the step S5, the vacuum degree of the vacuum oven is 0.095, and the treatment is carried out for 30-100 min at the maintenance temperature of 30-70 ℃.
8. The method for preparing the high thermal conductive silicone rubber according to claim 1, wherein:
in the step S6, the mould pressing temperature is 100-165 ℃, the mould pressing pressure is 1-15 MPa, and the mould pressing time is 5-30 min.
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| CN111334049A (en) * | 2020-04-14 | 2020-06-26 | 广东思泉新材料股份有限公司 | Method for preparing heat-conducting silicone rubber gasket from waste artificially-synthesized graphite film |
| CN112080149A (en) * | 2020-09-28 | 2020-12-15 | 苏州欧纳克纳米科技有限公司 | Silicone rubber high-heat-conduction material |
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