CN115505265A - High-thermal-conductivity silicone rubber gasket and preparation method and application thereof - Google Patents
High-thermal-conductivity silicone rubber gasket and preparation method and application thereof Download PDFInfo
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- CN115505265A CN115505265A CN202110695463.4A CN202110695463A CN115505265A CN 115505265 A CN115505265 A CN 115505265A CN 202110695463 A CN202110695463 A CN 202110695463A CN 115505265 A CN115505265 A CN 115505265A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
- C08K2003/0812—Aluminium
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/005—Additives being defined by their particle size in general
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
Abstract
The invention relates to the technical field of silicone rubber gaskets, in particular to a high-thermal-conductivity silicone rubber gasket and a preparation method and application thereof. The invention provides a preparation method of a high-thermal-conductivity silicone rubber gasket, which comprises the following steps: mixing silicon rubber, flaky aluminum powder and heat-conducting filler to obtain a mixture; sequentially pressurizing, vulcanizing and cutting the mixture to obtain the high-heat-conductivity silicone rubber gasket; the flaky plane direction of the flaky aluminum powder is parallel to the thickness direction of the high-thermal-conductivity silicone rubber gasket. The preparation method improves the heat conductivity coefficient of the high-heat-conductivity silicone rubber gasket.
Description
Technical Field
The invention relates to the technical field of silicone rubber gaskets, in particular to a high-thermal-conductivity silicone rubber gasket and a preparation method and application thereof.
Background
The heat-conducting silicone rubber gasket is used for electronic products, and air between a heating component and a radiator of electronic equipment is filled in gaps between the heating component and the radiator, so that heat of the electronic equipment is led out in an accelerating mode, and performance and service life of the electronic products are guaranteed. With the rapid development of high power, high density and high integration of electronic components, the increasingly prominent heat dissipation problem has become the bottleneck in the development of high-power electronic components and ultra-large-scale and ultra-high-speed integrated circuits, and especially the rapid development and popularization of the current 5G application technology are faced to improve the heat conductivity of the heat-conducting silicone rubber gasket, so that the heat-conducting silicone rubber gasket becomes an important development subject to be solved urgently in the current microelectronic industry.
The silicon rubber has good flexibility, high-temperature performance and flame retardance, can be tightly attached between a heating component and a radiator, and is a material with low heat conductivity coefficient. The metallic aluminum has excellent heat-conducting property, the heat-conducting coefficient is as high as 237W/m.K, the metallic aluminum has light weight and is easy to process, and the flake aluminum powder is a high-quality heat-conducting filler. The properties of the aluminum powder and the silicon rubber are combined for optimal design and manufacture, so that the silicon rubber gasket with high heat conductivity coefficient can be prepared. But the metal aluminum powder heat-conducting silicone rubber gasket is used less in the manufacturing process at present and only used as an auxiliary filler with less additive. The metal aluminum powder is used as a main heat-conducting filler of the heat-conducting silicon rubber, and the following research and application are provided. Zhu Yi (Zhu Yi, research on silicone rubber thermal interface material for filling aluminum flakes, 2002,6,7-9) 60-70% by mass of aluminum flakes are added into silicone rubber, and the thermal conductivity reaches 1.2-1.3W/m.K; used as a personal name in ancient times xuezzhen, etc. (Ju xuezzhen, etc., dielectric and heat-conducting properties of aluminum particle/silicone rubber composite material, synthetic rubber process, 2007,1,54-58) uses 75% by mass of flaky aluminum powder in silicone rubber, and the heat-conducting coefficient reaches 1.73W/m.K; in the Chinese patent CN109535733A, 58 mass percent of aluminum powder and 2 mass percent of multi-wall carbon nano tubes are used in silicone rubber, and the heat conductivity coefficient reaches 1.2W/m.K. Obviously, the heat-conducting silicone rubber prepared by the method has low heat conductivity coefficient, and the excellent heat-conducting property of the aluminum powder is not exerted.
Disclosure of Invention
The invention aims to provide a high-thermal-conductivity silicone rubber gasket, and a preparation method and application thereof.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a preparation method of a high-thermal-conductivity silicone rubber gasket, which comprises the following steps:
mixing silicon rubber, flake aluminum powder and heat-conducting filler to obtain a mixture;
sequentially pressurizing, vulcanizing and cutting the mixture to obtain the high-heat-conductivity silicone rubber gasket;
the flaky plane direction of the flaky aluminum powder is parallel to the thickness direction of the high-thermal-conductivity silicone rubber gasket.
Preferably, the mass ratio of the silicone rubber, the aluminum flake powder and the heat-conducting filler is 100: (50-200): (5 to 150).
Preferably, the fineness of the aluminum flake is 300-2000 meshes, and the thickness of the aluminum flake is 0.005-0.02 mm.
Preferably, the fineness of the heat-conducting filler is 0.01-45 μm;
the heat-conducting filler comprises one or more of magnesium oxide, boron nitride, aluminum oxide, silicon carbide, carbon fiber, graphite, carbon black and silicon oxide.
Preferably, the silicone rubber comprises a room temperature vulcanizing type liquid silicone rubber;
the room temperature fluidized liquid silicone rubber comprises condensed liquid silicone rubber or addition liquid silicone rubber.
Preferably, the condensed type liquid silicone rubber comprises the following preparation raw materials in parts by weight:
90-95 parts of alpha, omega-dihydroxy polydimethylsiloxane, 2-5 parts of ethyl orthosilicate, 0.5-2 parts of dibutyltin dilaurate and 0-5 parts of simethicone;
the viscosity of the alpha, omega-dihydroxy polydimethylsiloxane is 3000-5000 mPas.
Preferably, the addition type liquid silicone rubber comprises the following preparation raw materials in parts by weight:
80-95 parts of alpha, omega-divinyl polydimethylsiloxane, 2-6 parts of hydrogen-containing polysiloxane, 0.2-2 parts of ethynylcyclohexanol and 0.02-1 part of chloroplatinic acid-divinyl tetramethyl disiloxane complex;
the viscosity of the alpha, omega-divinyl polydimethylsiloxane is 3000-5000 mPa & s;
the hydrogen content in the hydrogenpolysiloxane is 0.2-1.6 mol%.
Preferably, the mixing temperature is 60-80 ℃, and the mixing time is 1-2 h;
the viscosity of the mixture obtained after mixing is 40000-60000 mPas.
Preferably, the pressure vulcanization mode comprises room-temperature pressure vulcanization or heating pressure vulcanization;
the temperature of the room temperature pressure vulcanization is 10-35 ℃; the temperature of the heating and pressurizing vulcanization is 60-120 ℃.
Preferably, the heating and pressurizing vulcanization mode comprises heating and pressurizing constant-pressure vulcanization or heating and pressurizing constant-volume vulcanization.
Preferably, the pressure of the constant pressure vulcanization by heating and pressurizing is 3 to 25MPa.
Preferably, the heating and pressurizing constant volume vulcanization comprises heating and pressurizing single-stage constant volume vulcanization or heating and pressurizing multi-stage constant volume vulcanization.
Preferably, the heating and pressurizing multi-stage constant volume vulcanization comprises 2-5 stages of constant volume.
Preferably, when the multi-stage constant volume vulcanization by heating and pressurizing is 3 stages of constant volumes, the specific process comprises:
1) A first stage of constant volume: the pressure of the first stage constant volume is 5-10 MPa, the temperature is increased from room temperature to 80-120 ℃, the temperature is kept for 1-2 h, and the time for increasing the temperature is less than or equal to 30min;
2) A second stage of constant volume: the second stage has the constant volume pressure of 10-20 MPa, the temperature of 80-120 ℃ and the time of 1-2 h;
3) And (3) third stage constant volume: the third stage has the constant volume pressure of 10-20 MPa, the temperature of 80-120 ℃ and the time of 2-4 h.
The invention also provides the high-thermal-conductivity silicone rubber gasket prepared by the preparation method in the technical scheme, which comprises silicone rubber, and flaky aluminum powder and a thermal-conductivity filler which are filled in the silicone rubber;
the flaky plane direction of the flaky aluminum powder is parallel to the thickness direction of the high-thermal-conductivity silicone rubber gasket.
The invention also provides application of the high-thermal-conductivity silicone rubber gasket in the technical scheme in the field of heat dissipation of electronic products and power batteries.
The invention provides a preparation method of a high-thermal-conductivity silicone rubber gasket, which comprises the following steps: mixing silicon rubber, flaky aluminum powder and heat-conducting filler to obtain a mixture; sequentially pressurizing, vulcanizing and cutting the mixture to obtain the high-heat-conductivity silicone rubber gasket; the flaky plane direction of the flaky aluminum powder is parallel to the thickness direction of the high-thermal-conductivity silicone rubber gasket. In the process of pressurizing and vulcanizing the flaky aluminum powder, the flaky planes of the flaky aluminum powder can be naturally distributed on the vertical plane in the pressurizing direction, and the internal structure of the formed material is characterized in that: the aluminum flakes lay flat one on top of the other, and the silicone rubber is distributed between such layers. However, the structure greatly reduces the heat conduction channel of the flaky aluminum powder on the thickness of the silicone rubber gasket, and the flaky aluminum powder with excellent performance cannot play a role in the application of the heat conduction silicone rubber gasket; aiming at the problems, the vertical plane of the solid block obtained after pressure vulcanization is mechanically cut to obtain the silicone rubber gasket with the flaky plane of the aluminum powder and the thickness direction of the silicone rubber gasket in parallel. The heat conductivity coefficient of the finally prepared high-heat-conductivity silicone rubber gasket can reach more than 3.5W/m.K.
Detailed Description
The invention provides a preparation method of a high-thermal-conductivity silicone rubber gasket, which comprises the following steps:
mixing silicon rubber, flaky aluminum powder and heat-conducting filler to obtain a mixture;
sequentially pressurizing, vulcanizing and cutting the mixture to obtain the high-heat-conductivity silicone rubber gasket;
the flaky plane direction of the flaky aluminum powder is parallel to the thickness direction of the high-thermal-conductivity silicone rubber gasket.
In the present invention, all the starting materials for the preparation are commercially available products known to those skilled in the art unless otherwise specified.
The silicone rubber, the flaky aluminum powder and the heat-conducting filler are mixed to obtain a mixture.
In the present invention, the silicone rubber preferably includes a room temperature vulcanization type liquid silicone rubber; the room-temperature fluidizing liquid silicone rubber preferably includes a condensed type liquid silicone rubber or an addition type liquid silicone rubber.
In the invention, the condensed type liquid silicone rubber comprises the following preparation raw materials in parts by weight: 90-95 parts of alpha, omega-dihydroxy polydimethylsiloxane, 2-5 parts of ethyl orthosilicate, 0.5-2 parts of dibutyltin dilaurate and 0-5 parts of dimethyl silicone oil.
The condensed liquid silicone rubber of the present invention preferably comprises 90 to 95 parts by mass of alpha, omega-dihydroxy polydimethylsiloxane, more preferably 91 to 94 parts by mass, and most preferably 92 to 93 parts by mass. In the present invention, the viscosity of the α, ω -dihydroxypolydimethylsiloxane is preferably 3000 to 5000mPa · s. In the invention, the alpha, omega-dihydroxy polydimethylsiloxane is a molecular structural unit of the condensed liquid silicone rubber.
The condensed liquid silicone rubber preferably contains 2 to 5 parts by mass of tetraethoxysilane, more preferably 2.5 to 4.5 parts by mass, and most preferably 3 to 4 parts by mass, based on the mass of the alpha, omega-dihydroxy polydimethylsiloxane. In the invention, the tetraethoxysilane is a cross-linking agent and can cause alpha-dihydroxy polydimethylsiloxane and omega-dihydroxy polydimethylsiloxane to generate condensation cross-linking reaction.
The condensed type liquid silicone rubber preferably includes 0.5 to 2 parts, more preferably 1 to 1.5 parts, of dibutyltin dilaurate, based on the parts by mass of the α, ω -dihydroxypolydimethylsiloxane. In the present invention, the dibutyltin dilaurate is used as a catalyst.
The condensed type liquid silicone rubber preferably comprises 0 to 5 parts of dimethyl silicone oil, more preferably 1 to 4 parts, and most preferably 2 to 3 parts by mass of the alpha, omega-dihydroxy polydimethylsiloxane. In the invention, the dimethyl silicone oil is a plasticizer, so that the silicone rubber has better flexibility.
In the invention, the addition type liquid silicone rubber preferably comprises the following preparation raw materials in parts by weight: 80-95 parts of alpha, omega-divinyl polydimethylsiloxane, 2-6 parts of hydrogen-containing polysiloxane, 0.2-2 parts of ethynyl cyclohexanol and 0.02-1 part of chloroplatinic acid-divinyl tetramethyl disiloxane complex.
The addition type liquid silicone rubber preferably comprises 80-95 parts of alpha, omega-divinyl polydimethylsiloxane, more preferably 86-93 parts, and most preferably 88-90 parts by mass. In the present invention, the viscosity of the α, ω -divinylpolydimethylsiloxane is preferably 3000 to 5000mPa · s. In the present invention, the α, ω -divinylpolydimethylsiloxane is a molecular structural unit of the addition type liquid silicone rubber.
The addition type liquid silicone rubber preferably comprises 2 to 6 parts of hydrogenpolysiloxane, more preferably 3 to 5 parts of the hydrogenpolysiloxane, based on the mass parts of the alpha, omega-divinyl polydimethylsiloxane; the hydrogen content in the hydrogenpolysiloxane is preferably 0.2 to 1.6mol%, more preferably 0.4 to 1.2mol%, and most preferably 0.6 to 0.9mol%. In the invention, the hydrogen-containing polysiloxane is a cross-linking agent and can enable alpha, omega-divinyl dimethyl polysiloxane to generate addition cross-linking reaction.
The addition type liquid silicon rubber preferably comprises 0.2 to 2 parts of ethynylcyclohexanol, more preferably 0.6 to 1.4 parts, and most preferably 0.8 to 1.0 part by weight of the alpha, omega-divinyl polydimethylsiloxane. In the present invention, the ethynylcyclohexanol functions to control the rate of addition crosslinking reaction.
The addition type liquid silicone rubber preferably comprises 0.02-1 part of chloroplatinic acid-divinyl tetramethyl disiloxane complex, more preferably 0.04-0.6 part, and most preferably 0.06-0.4 part by mass of the alpha, omega-divinyl dimethyl polysiloxane. In the present invention, the chloroplatinic acid-divinyltetramethyldisiloxane complex is a catalyst.
In the present invention, the fineness of the flake aluminum powder is preferably 300 to 2000 mesh, more preferably 500 to 1500 mesh, and most preferably 600 to 1000 mesh.
In the present invention, the aluminum flakes are preferably aluminum foil powder. In the present invention, the thickness of the aluminum foil is preferably 0.005 to 0.02mm, more preferably 0.006 to 0.015mm, and most preferably 0.008 to 0.012mm; the fineness of the aluminum foil is preferably 300 to 2000 meshes, and more preferably 600 to 1200 meshes.
In the present invention, the fineness of the thermally conductive filler is preferably 0.01 to 45 μm, and more preferably 10 to 20 μm. The heat-conducting filler preferably comprises one or more of magnesium oxide, boron nitride, aluminum oxide, silicon carbide, carbon fiber, graphite, carbon black and silicon oxide; the carbon fibers preferably comprise chopped carbon fibers or carbon fiber powder, and the carbon fibers are preferably acrylonitrile-based carbon fibers; the graphite preferably comprises artificial graphite and/or flake graphite; when the heat-conducting filler is more than two of the specific choices, the proportion of the specific substances is not limited in any way, and the specific substances can be mixed according to any proportion.
In the present invention, the mass ratio of the silicone rubber, the aluminum flakes, and the thermally conductive filler is preferably 100: (50-200): (5 to 150), more preferably 100: (60 to 170): (20 to 130), most preferably 100: (90 to 130): (40-90).
In the invention, the heat-conducting filler has the function of auxiliary heat conduction, and simultaneously, the flaky aluminum powder is conveniently and uniformly dispersed in the silicone rubber, and the manufacturing cost is properly reduced; the stability of the heat conducting performance of the product can be further improved by controlling the mass ratio of the silicone rubber, the aluminum flake powder and the heat conducting filler within the range.
In the present invention, the mixing is preferably performed under stirring; the rotation speed of the stirring is not particularly limited in the present invention, and may be a rotation speed known to those skilled in the art. The mixing temperature is preferably 60-80 ℃, more preferably 65-75 ℃, and most preferably 68-70 ℃; the time is preferably 1 to 2 hours, more preferably 1.2 to 1.8 hours, most preferably 1.4 to 1.6 hours.
In the present invention, the specific process of the mixing preferably includes the steps of:
the components of the silicone rubber are added into a kneader, and after first stirring, the flaky aluminum powder and the heat-conducting filler are added for mixing.
In the present invention, the temperature of the first stirring is preferably room temperature, and the time is preferably 15 to 60min, and more preferably 25 to 40min. The rotation speed of the first stirring is not particularly limited in the present invention, and may be performed by a process known to those skilled in the art.
In the present invention, the viscosity of the mixture obtained after the kneading is preferably 40000 to 60000mPa · s, more preferably 45000 to 55000mPa · s.
After the mixture is obtained, the mixture is sequentially subjected to pressure vulcanization and cutting to obtain the high-thermal-conductivity silicone rubber gasket.
In the present invention, the press vulcanization preferably includes room temperature press vulcanization or warm press vulcanization.
In the present invention, the temperature of the room temperature press vulcanization is preferably 10 to 35 ℃, the pressure of the room temperature press vulcanization is preferably 2 to 10MPa, more preferably 3 to 8MPa, most preferably 4 to 5MPa, and the time of the room temperature press vulcanization is preferably 24 hours. In the invention, the room temperature press vulcanization process is preferably to place the mixture in a mold, and the mold does not need to be heated for press vulcanization. The size of the mold is not limited in any way, and the mold can be made in the size known to those skilled in the art. In the embodiment of the invention, the length, the width and the height of the die are respectively 20cm, 12cm and 16cm.
In the present invention, the temperature for the vulcanization by heating and pressing is preferably 60 to 120 ℃, more preferably 80 to 110 ℃.
In the invention, the heating and pressurizing vulcanization mode preferably comprises heating and pressurizing constant-pressure vulcanization or heating and pressurizing constant-volume vulcanization; the pressure of the constant-pressure vulcanization by heating and pressurizing is preferably 3 to 25MPa, more preferably 5 to 20MPa, and most preferably 10 to 15MPa.
In the invention, the heating and pressurizing constant volume vulcanization preferably comprises heating and pressurizing single-stage constant volume vulcanization or heating and pressurizing multi-stage constant volume vulcanization.
In the invention, the heating and pressurizing single-stage constant volume vulcanization is preferably carried out under the heating and pressurizing conditions, and the volume is not adjusted after the volume requirement is met at one time. In the invention, the pressure of the single-stage constant volume vulcanization by heating and pressurizing is preferably 5-10 MPa, the temperature is raised to 80-120 ℃ from room temperature within the time of less than or equal to 30min, and the temperature is kept for 3-4 h. In the specific embodiment of the invention, the heating and pressurizing single-stage constant volume vulcanization is preferably maintained at the temperature of 80 ℃ for 80min, pressurized to 5MPa and continuously maintained for 3h.
In the invention, the heating and pressurizing multi-stage constant volume vulcanization preferably comprises 2-5 stages of constant volumes, and more preferably 3 stages of constant volumes; when the multi-stage constant volume vulcanization of heating and pressurizing is 3 stages of constant volume, the specific process comprises the following steps: 1) The first stage of constant volume: the pressure of the first stage constant volume is 5-10 MPa, the temperature is increased from room temperature to 80-120 ℃, the temperature is kept for 1-2 h, and the time for increasing the temperature is less than or equal to 30min; 2) And (3) second-stage constant volume: the second stage has the constant volume pressure of 10-20 MPa, the temperature of 80-120 ℃ and the time of 1-2 h; 3) And (3) third stage constant volume: the third stage has the constant volume pressure of 10-20 MPa, the temperature of 80-120 ℃ and the time of 2-4 h. More preferably, it comprises: 1) The first stage of constant volume: the pressure of the first stage constant volume is 6-8 MPa, the temperature is increased from room temperature to 90-110 ℃, the temperature is kept for 1.2-1.6 h, and the time for temperature increase is less than or equal to 30min; 2) And (3) second-stage constant volume: the second stage has the constant volume pressure of 13-15 MPa, the temperature of 90-100 ℃ and the time of 1.3-1.7 h; 3) And (3) third stage constant volume: the third stage has the constant volume pressure of 15-18 MPa, the temperature of 90-100 ℃ and the time of 2.5-3.5 h.
After the pressure vulcanization is completed, the invention also preferably comprises pressure relief, and the pressure relief process is not limited in any way by the invention and can be carried out by adopting a process well known to those skilled in the art.
In the invention, the pressure vulcanization process can be carried out in such a way that the flaky plane of the aluminum powder is parallel to the long and wide plane of the solid block.
In the invention, the silicone rubber solid block obtained after the pressurization process is finished is preferably a rectangular parallelepiped structure, the length is preferably 100-1000 mm, the width is preferably 100-600 mm, and the height is preferably 25-120 mm; in the invention, in the length and width surfaces of the silicon rubber solid block, the flaky plane of the aluminum powder is parallel to the length and width surfaces of the solid block.
In the invention, the cutting equipment used for cutting is preferably a belt saw blade machine, a disc saw blade machine, a guillotine shear or a diamond wire cutting machine.
In the present invention, the cutting is preferably performed on a long high plane of the solid block of silicone rubber. The thickness of the heat-conducting silicon rubber gasket is preferably 0.5-5 mm.
The invention also provides the high-thermal-conductivity silicone rubber gasket prepared by the preparation method in the technical scheme, which comprises silicone rubber, and flaky aluminum powder and a thermal-conductivity filler which are filled in the silicone rubber;
the flaky plane direction of the flaky aluminum powder is parallel to the thickness direction of the high-thermal-conductivity silicone rubber gasket.
In the invention, the mass ratio of the silicone rubber, the flaky aluminum powder and the heat-conducting filler is 100: (50-200): (5 to 150), more preferably 100: (60 to 170): (20 to 130), most preferably 100: (90 to 130): (40 to 90).
The invention also provides application of the high-thermal-conductivity silicone rubber gasket in the technical scheme in the field of heat dissipation of electronic products and power batteries. The method of the present invention is not particularly limited, and the method may be performed by a method known to those skilled in the art. In the invention, the electronic product is preferably a smart phone, a unmanned aerial vehicle or an industrial intelligent device.
The highly thermally conductive silicone rubber gasket of the present invention, the preparation method and the application thereof will be described in detail with reference to the following examples, which should not be construed as limiting the scope of the present invention.
Example 1
940g of alpha, omega-dihydroxy polydimethylsiloxane (with the viscosity of 3000 mPas), 30g of ethyl orthosilicate, 10g of dibutyltin dilaurate and 20g of dimethyl silicone oil are added into a kneader, stirred for 45min at room temperature, added with 1.8Kg of sheet-shaped aluminum powder (with the fineness of 800 meshes and the sheet thickness of 0.01 mm) and 0.16Kg of silicon oxide (with the fineness of 5000 meshes), and stirred for 2h at the temperature of 80 ℃ to obtain a mixture (with the viscosity of 40000-60000 mPas);
adding 3kg of the mixture into a mold of a press, wherein the length, the width and the height of the mold are respectively 20cm, 12cm and 16cm, heating and pressurizing for 3-stage constant volume vulcanization treatment (the first constant volume is that the height of the material in the mold cavity is 62mm, the temperature is room temperature, the pressure is 8MPa, the room temperature is increased to 100 ℃ within 30 minutes, and the temperature is kept for 60min; the second constant volume is that the height of the material in the mold cavity is 61mm, the temperature is 100 ℃, the pressure is 12MPa, and the temperature is kept for 90min; the third constant volume is that the height of the material in the mold cavity is 60mm, the temperature is 100 ℃, the pressure is 15MPa, and the temperature is kept for 120 min), and demolding to obtain a silicon rubber solid block;
and cutting the long high plane of the silicon rubber solid block by using a diamond wire cutting machine to obtain the high-heat-conduction silicon rubber gasket with the thickness of 0.5, 1.0, 3.0, 4.0 and 5.0 mm.
Example 2
940g of alpha, omega-dihydroxy polydimethylsiloxane (with the viscosity of 3000 mPas), 30g of ethyl orthosilicate, 10g of dibutyltin dilaurate and 20g of dimethyl silicone oil are added into a kneader, stirred for 45min at room temperature, added with 1Kg of flaky aluminum powder (with the fineness of 800 meshes and the sheet thickness of 0.01 mm) and 1Kg of acrylonitrile-based carbon fiber powder (with the fiber length of 0.1-0.3 mm), and stirred for 2h at the temperature of 80 ℃ to obtain a mixture (with the viscosity of 40000-60000 mPas);
adding 2.75kg of the mixture into a mold of a press, wherein the length, the width and the height of the mold are respectively 20cm, 12cm and 16cm, heating and pressurizing for 3-stage constant volume vulcanization treatment (the first constant volume is that the height of the material in the mold cavity is 62mm, the temperature is room temperature, the pressure is 8MPa, the room temperature is raised to 100 ℃ within 30 minutes, and the temperature is kept for 60min; the second constant volume is that the height of the material in the mold cavity is 61mm, the temperature is 100 ℃, the pressure is 12MPa, and the temperature is kept for 90min; the third constant volume is that the height of the material in the mold cavity is 60mm, the temperature is 100 ℃, the pressure is 15MPa, and the temperature is kept for 120 min), and demolding to obtain a silicon rubber solid block;
and cutting the long high plane of the silicon rubber solid block by using a diamond wire cutting machine to obtain the high-heat-conductivity silicon rubber gasket with the thickness of 0.5 mm, 1.0 mm, 3.0 mm, 4.0 mm and 5.0 mm.
Example 3
940g of alpha, omega-dihydroxy polydimethylsiloxane (with the viscosity of 3000 mPas), 30g of ethyl orthosilicate, 10g of dibutyltin dilaurate and 20g of dimethyl silicone oil are added into a kneader, stirred for 45min at room temperature, added with 1.2Kg of sheet-shaped aluminum powder (with the fineness of 800 meshes and the sheet thickness of 0.01 mm) and 0.8Kg of crystalline flake graphite (with the fineness of 2000 mm), and stirred for 2h at the temperature of 80 ℃ to obtain a mixture (with the viscosity of 40000-60000 mPas);
adding 2.9kg of the mixture into a mold of a press, wherein the length, the width and the height of the mold are respectively 20cm, 12cm and 16cm, heating and pressurizing for 3-stage constant volume vulcanization treatment (the first constant volume is that the height of the material in the mold cavity is 62mm, the temperature is room temperature, the pressure is 8MPa, the room temperature is raised to 100 ℃ within 30 minutes, and the temperature is kept for 60min; the second constant volume is that the height of the material in the mold cavity is 61mm, the temperature is 100 ℃, the pressure is 12MPa, and the temperature is kept for 90min; the third constant volume is that the height of the material in the mold cavity is 60mm, the temperature is 100 ℃, the pressure is 15MPa, and the temperature is kept for 120 min), decompressing, and demolding to obtain a silicon rubber solid block;
and cutting the long high plane of the silicon rubber solid block by using a diamond wire cutting machine to obtain the high-heat-conduction silicon rubber gasket with the thickness of 0.5, 1.0, 3.0, 4.0 and 5.0 mm.
Example 4
940g of alpha, omega-dihydroxy polydimethylsiloxane (with the viscosity of 3000 mPa.s), 30g of ethyl orthosilicate, 10g of dibutyltin dilaurate and 20g of dimethyl silicone oil are added into a kneader and stirred for 45min at room temperature, 1Kg of flaky aluminum powder (with the fineness of 800 meshes and the sheet thickness of 0.01 mm) and 1Kg of acrylonitrile-based carbon fiber powder (with the fiber length of 0.1-0.3 mm) are added and stirred for 2h at the temperature of 80 ℃, and a mixture (with the viscosity of the silicone rubber of 40000-60000 mPa.s) is obtained;
adding 2.75kg of the mixture into a mold of a press, wherein the length, the width and the height of the mold are respectively 20cm, 12cm and 16cm, heating to 80 ℃, maintaining for 80min, pressurizing to 5MPa, continuously maintaining for 3 hours, relieving pressure and demolding to obtain a silicon rubber solid block;
and cutting the long high plane of the silicon rubber solid block by using a diamond wire cutting machine to obtain the high-heat-conduction silicon rubber gasket with the thickness of 0.5, 1.0, 3.0, 4.0 and 5.0 mm.
Test example
The high thermal conductivity silicone rubber gaskets prepared in examples 1 to 4 were subjected to a thermal conductivity test according to the standard test method for thermal conductivity of ASTM5470 thermal conductive electrical insulation materials, and the test results are shown in table 1:
TABLE 1 thermal conductivity of highly thermally conductive silicone rubber gaskets prepared in examples 1-4
As can be seen from Table 1, the high thermal conductivity silicone rubber gasket prepared by the preparation method of the invention has a high thermal conductivity coefficient.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (16)
1. The preparation method of the high-thermal-conductivity silicone rubber gasket is characterized by comprising the following steps of:
mixing silicon rubber, flaky aluminum powder and heat-conducting filler to obtain a mixture;
sequentially pressurizing, vulcanizing and cutting the mixture to obtain the high-heat-conductivity silicone rubber gasket;
the flaky plane direction of the flaky aluminum powder is parallel to the thickness direction of the high-thermal-conductivity silicone rubber gasket.
2. The preparation method according to claim 1, wherein the mass ratio of the silicone rubber, the aluminum flake powder and the heat conductive filler is 100: (50-200): (5-150).
3. The production method according to claim 1 or 2, wherein the fineness of the flaky aluminum powder is 300 to 2000 mesh, and the thickness of the flaky aluminum powder is 0.005 to 0.02mm.
4. The production method according to claim 1 or 2, wherein the fineness of the heat conductive filler is 0.01 to 45 μm;
the heat-conducting filler comprises one or more of magnesium oxide, boron nitride, aluminum oxide, silicon carbide, carbon fiber, graphite, carbon black and silicon oxide.
5. The production method according to claim 1 or 2, wherein the silicone rubber comprises a room temperature vulcanization type liquid silicone rubber;
the room temperature fluidized liquid silicone rubber comprises condensed liquid silicone rubber or addition liquid silicone rubber.
6. The preparation method according to claim 5, wherein the condensed type liquid silicone rubber comprises the following preparation raw materials in parts by mass:
90-95 parts of alpha, omega-dihydroxy polydimethylsiloxane, 2-5 parts of ethyl orthosilicate, 0.5-2 parts of dibutyltin dilaurate and 0-5 parts of simethicone;
the viscosity of the alpha, omega-dihydroxy polydimethylsiloxane is 3000-5000 mPas.
7. The preparation method of claim 5, wherein the addition type liquid silicone rubber comprises the following preparation raw materials in parts by weight:
80-95 parts of alpha, omega-divinyl dimethyl polysiloxane, 2-6 parts of hydrogen-containing polysiloxane, 0.2-2 parts of ethynylcyclohexanol and 0.02-1 part of chloroplatinic acid-divinyl tetramethyl disiloxane complex;
the viscosity of the alpha, omega-divinyl polydimethylsiloxane is 3000-5000 mPa & s;
the hydrogen content in the hydrogenpolysiloxane is 0.2-1.6 mol%.
8. The preparation method according to claim 1, wherein the mixing temperature is 60 to 80 ℃ and the mixing time is 1 to 2 hours;
the viscosity of the mixture obtained after mixing is 40000-60000 mPas.
9. The method according to claim 1, wherein the press vulcanization is carried out by a method comprising room-temperature press vulcanization or elevated-temperature press vulcanization;
the temperature of the room temperature pressure vulcanization is 10-35 ℃; the temperature of the heating and pressurizing vulcanization is 60-120 ℃.
10. The preparation method according to claim 9, wherein the heating and pressurizing vulcanization mode comprises heating and pressurizing constant pressure vulcanization or heating and pressurizing constant volume vulcanization.
11. The method according to claim 10, wherein the pressure of the constant-pressure vulcanization by heating and pressurizing is 3 to 25MPa.
12. The preparation method according to claim 10, wherein the warming and pressurizing constant volume vulcanization comprises a warming and pressurizing single-stage constant volume vulcanization or a warming and pressurizing multi-stage constant volume vulcanization.
13. The preparation method of claim 12, wherein the warming and pressurizing multi-stage constant volume vulcanization comprises 2-5 stages of constant volume.
14. The preparation method of claim 13, wherein when the multi-stage constant volume vulcanization under heating and pressurizing is carried out to 3 stages of constant volumes, the specific process comprises the following steps:
1) The first stage of constant volume: the pressure of the first stage constant volume is 5-10 MPa, the temperature is increased from room temperature to 80-120 ℃, the temperature is kept for 1-2 h, and the time for increasing the temperature is less than or equal to 30min;
2) And (3) second-stage constant volume: the second stage has the constant volume pressure of 10-20 MPa, the temperature of 80-120 ℃ and the time of 1-2 h;
3) And (3) third stage constant volume: the third stage has the constant volume pressure of 10-20 MPa, the temperature of 80-120 ℃ and the time of 2-4 h.
15. The high thermal conductive silicone rubber gasket prepared by the preparation method of claims 1-14, comprising silicone rubber, and aluminum flakes and thermal conductive filler filled in the silicone rubber;
the flaky plane direction of the flaky aluminum powder is parallel to the thickness direction of the high-thermal-conductivity silicone rubber gasket.
16. The high thermal conductivity silicone rubber gasket of claim 15 is used in the heat dissipation field of electronic products and power batteries.
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