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CN115627075A - Low-hardness heat-conducting gasket with low surface viscosity and preparation method thereof - Google Patents

Low-hardness heat-conducting gasket with low surface viscosity and preparation method thereof Download PDF

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Publication number
CN115627075A
CN115627075A CN202211267888.6A CN202211267888A CN115627075A CN 115627075 A CN115627075 A CN 115627075A CN 202211267888 A CN202211267888 A CN 202211267888A CN 115627075 A CN115627075 A CN 115627075A
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silicone oil
low
heat
stirring
gasket
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王信端
徐维富
任俊
唐新开
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Shenzhen Dem Technology Co ltd
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Shenzhen Dem Technology Co ltd
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
    • C08J7/04—Coating
    • C08J7/0427—Coating with only one layer of a composition containing a polymer binder
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D183/00—Coating compositions based on 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; Coating compositions based on derivatives of such polymers
    • C09D183/04—Polysiloxanes
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/20—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes for coatings strippable as coherent films, e.g. temporary coatings strippable as coherent films
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
    • C09K5/08—Materials not undergoing a change of physical state when used
    • C09K5/14—Solid materials, e.g. powdery or granular
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2383/00—Characterised by the use 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; Derivatives of such polymers
    • C08J2383/04—Polysiloxanes
    • C08J2383/07—Polysiloxanes containing silicon bound to unsaturated aliphatic groups
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2483/00—Characterised by the use 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; Derivatives of such polymers
    • C08J2483/04—Polysiloxanes
    • C08J2483/05—Polysiloxanes containing silicon bound to hydrogen
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2483/00—Characterised by the use 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; Derivatives of such polymers
    • C08J2483/04—Polysiloxanes
    • C08J2483/07—Polysiloxanes containing silicon bound to unsaturated aliphatic groups
    • 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
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C08K2003/2227—Oxides; Hydroxides of metals of aluminium
    • 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
    • C08K5/00—Use of organic ingredients
    • C08K5/54—Silicon-containing compounds
    • C08K5/541—Silicon-containing compounds containing oxygen
    • C08K5/5415—Silicon-containing compounds containing oxygen containing at least one Si—O bond
    • C08K5/5419—Silicon-containing compounds containing oxygen containing at least one Si—O bond containing at least one Si—C bond
    • 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
    • C08K7/00—Use of ingredients characterised by shape
    • 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
    • C08K7/00—Use of ingredients characterised by shape
    • C08K7/16—Solid spheres
    • C08K7/18—Solid spheres inorganic

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  • Combustion & Propulsion (AREA)
  • Thermal Sciences (AREA)
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Abstract

The invention discloses a heat-conducting gasket with low hardness, low surface viscosity and a preparation method thereof, and the heat-conducting gasket comprises a sheet body of a sizing material component and a heat-conducting gasket formed by surface treatment oil, and comprises a formula of the sizing material component and a formula of the surface treatment oil, wherein inorganic heat-conducting powder is one or a combination of more of spherical alumina, angular alumina, aluminum hydroxide and zinc oxide. Therefore, the heat conducting gasket prepared by the method has higher heat conductivity coefficient, lower hardness and volatility as well as high resilience rate, the operability of the heat conducting gasket is greatly improved by carrying out surface treatment on the heat conducting gasket, and the actual use requirements of users are effectively met.

Description

Low-hardness heat-conducting gasket with low surface viscosity and preparation method thereof
Technical Field
The invention relates to the technical field of thermal interface materials, in particular to a heat-conducting gasket with low hardness, a low surface and a low viscosity and a preparation method thereof.
Background
As is known, with the advent of the 5G era, electronic components are becoming smaller and smaller, and electronic components are also being integrated together, and their power is also becoming larger and larger, which results in the exposure of their heat generation problems, and air exists between the heat source and the heat sink, and is a poor conductor of heat, resulting in poor heat dissipation. According to reliable analysis, the service life of the component is reduced by half when the temperature of the component is increased by 10 ℃, and the service life of the electronic component is greatly reduced, so that the heat management discipline is developed. The existing thermal interface management materials comprise heat-conducting silicone grease, heat-conducting gaskets, heat-conducting mud and the like, the heat-conducting silicone grease can be in close contact with electronic components, so that the heat dissipation of the heat-conducting silicone grease is good, but the heat-conducting silicone grease is short in service life, and can be pulverized and failed due to drying for a long time, so that the heat dissipation effect is greatly reduced.
The heat-conducting gasket is named because the heat-conducting gasket has the characteristics of low stress and never drying in the using state, can be used for uneven PCB boards and components, but has more complex process and higher requirement on the viscosity of glue stock, and needs to be kept in a vacuum state in the whole manufacturing process. The heat-conducting gasket can be used under the condition of larger gap, has good effect on heat dissipation of electronic components, and has multiple functions of sealing, shock absorption, insulation and the like. The hardness and the surface viscosity of the currently used heat-conducting silica gel gaskets are in a trade-off relationship, generally speaking, low hardness corresponds to high viscosity, the heat-conducting gaskets with low hardness and low thickness basically cannot be manufactured, great challenges are brought to the operation of workers, and the working efficiency is seriously influenced. Therefore, a heat conducting gasket with low hardness, low surface viscosity and a preparation method thereof are provided for solving the problems.
Disclosure of Invention
In view of the above-mentioned shortcomings in the prior art, the present invention is directed to a heat conductive gasket with low hardness, low surface viscosity and a method for manufacturing the same.
In order to achieve the purpose, the invention adopts the following technical scheme:
a heat-conducting pad with low hardness, surface and low viscosity comprises a heat-conducting pad composed of a sizing component and a surface treatment oil;
the rubber material comprises the following components in percentage by mass:
85% -90% of inorganic heat conducting powder;
5 to 15 percent of first vinyl silicone oil;
0.5 to 1.5 percent of hydrogen-containing silicone oil;
0.05 to 0.1 percent of coupling agent;
0.15 to 0.3 percent of inhibitor;
0.2 to 0.4 percent of catalyst;
the surface treatment oil comprises the following components in percentage by mass:
80-85% of second vinyl silicone oil;
10-15% of vinyl silicone resin;
2 to 5 percent of hydrogen-containing silicone oil;
0.5 to 2 percent of inhibitor;
1% -2% of a catalyst;
wherein, the inorganic heat conducting powder is one or a combination of more of spherical alumina, angular alumina, aluminum hydroxide and zinc oxide.
Preferably, the inorganic heat-conducting powder comprises the following components in percentage by mass:
40% -90% of spherical alumina;
0 to 30 percent of angular alumina;
0 to 35 percent of aluminum hydroxide.
Preferably, the spherical alumina has a particle size of 1 to 50 μm, the angular alumina has a particle size of 45 to 70 μm, and the aluminum hydroxide has a particle size of 30 to 80 μm.
Preferably, the dynamic viscosity of the first vinyl silicone oil and the second vinyl silicone oil is 50 to 5000mPa · s.
Preferably, the first vinyl silicone oil is prepared by mixing and compounding vinyl silicone oil with dynamic viscosity of 50-100 mPa & s and vinyl silicone oil with dynamic viscosity of 3000-5000 mPa & s, and the compounding ratio is 1.5-3.1; the second vinyl silicone oil is prepared by mixing vinyl silicone oil with the dynamic viscosity of 100-1000 mPa.s and vinyl silicone oil with the dynamic viscosity of 3000-5000 mPa.s in a compounding ratio of 3-6.1.
Preferably, the vinyl silicon resin has a dynamic viscosity of 100 to 2000 mPas.
Preferably, the hydrogen-containing silicone oil is one or a combination of lateral hydrogen-containing silicone oil and terminal hydrogen-containing silicone oil, and the optimal hydrogen content is 0.05-0.18 wt%.
Preferably, the coupling agent is one or more of octyl trimethoxysilane, decyl trimethoxysilane, dodecyl trimethoxysilane and hexadecyl trimethoxysilane, and the inhibitor is one or more of benzotriazole, cyclohexylynol and methylbutynol.
Preferably, the catalyst is a platinum catalyst, and the optimal platinum content is 100-5000 ppm.
Preferably, the preparation method of the heat conduction gasket with the low hardness, the low surface viscosity is characterized in that: the manufacturing process comprises the following steps:
s1, respectively weighing raw materials with corresponding percentage mass according to each component of the sizing material component, putting the first vinyl silicone oil into a reaction kettle, starting stirring, putting the inorganic heat conduction powder into the reaction kettle for 3-6 times at a rotating speed of 10-30 r/min, stirring for 5-10 min, putting a coupling agent into the reaction kettle at a stirring rotating speed of 10-30 r/min, stirring for 10-30 min, heating to 120-150 ℃, continuing to stir for 20-40 min, cooling to room temperature, sequentially putting hydrogen-containing silicone oil, an inhibitor and a catalyst into the reaction kettle at a stirring rotating speed of 20-50 r/min, stirring for 10-60 min, and starting vacuumizing for 2-12 h to obtain the sizing material component;
s2, respectively weighing raw materials according to the mass percentage of each component of the surface treatment oil, respectively putting divinyl silicon oil, silicone resin, lateral hydrogen and an inhibitor into a reaction kettle, starting stirring at the rotating speed of 10-30 r/min, adding a catalyst after stirring for 30-60 min at the rotating speed of 20-50 r/min, and starting vacuumizing for 1-2 h after stirring for 10-30 min to obtain the surface treatment oil;
s3, coating the surface treatment oil on the surface of the release film by using a coating machine, wherein the coating thickness is 20-100 mu m, rolling the rubber material component into a sheet shape by using the release film coated with the surface treatment oil as a base film, and vulcanizing and molding at 120-150 ℃ for 30-60 min to obtain the heat conduction gasket.
Due to the adoption of the scheme, a large amount of spherical alumina is used for realizing large amount of filling, the cost of the heat conduction gasket is effectively reduced while the heat conductivity is increased, the heat conductivity coefficient can reach 1.8-3.5W/m.K, the manufacture of the low-hardness heat conduction gasket is realized by reducing the crosslinking density of vinyl and hydrogen-containing silicone oil, the Shore (Shore hardness) 00 of the gasket is in the range of 15-25 hardness, the gasket has softer hardness and is easy to deform and fill gaps, so that the gasket can be tightly filled between a heating source and a radiator; meanwhile, the surface treatment oil is smeared on the surface of the heat conduction gasket through the release film, and the surface of the heat conduction gasket is subjected to viscosity removal treatment, so that the prepared heat conduction gasket is low in viscosity, good in operability and convenient to prepare; therefore, the heat conducting gasket prepared by the method has higher heat conductivity coefficient, lower hardness and volatility as well as high resilience rate, the operability of the heat conducting gasket is greatly improved by carrying out surface treatment on the heat conducting gasket, and the actual use requirements of users are effectively met.
Drawings
FIG. 1 is a table showing the performance of the product according to the embodiment of the present invention.
Detailed Description
The embodiments of the invention will be described in detail below with reference to the drawings, but the invention can be implemented in many different ways as defined and covered by the claims.
In the description of the present invention, it is to be understood that the terms "center", "longitudinal", "lateral", "length", "width", "thickness", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", "clockwise", "counterclockwise", and the like, indicate orientations and positional relationships based on those shown in the drawings, and are used only for convenience of description and simplicity of description, and do not indicate or imply that the device or element being referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus, are not to be construed as limiting the present invention. Furthermore, the terms "first", "second" and "first" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, features defined as "first", "second", may explicitly or implicitly include one or more of the described features. In the description of the present invention, "a plurality" means two or more unless specifically defined otherwise.
In the description of the present invention, it should be noted that the terms "mounted," "connected," and "connected" are to be construed broadly and may be, for example, fixedly connected, detachably connected, or integrally connected unless otherwise explicitly stated or limited. Either mechanically or electrically. They may be directly connected or indirectly connected through intervening media, or may be connected through the use of two elements or the interaction of two elements. The specific meanings of the above terms in the present invention can be understood by those skilled in the art according to specific situations.
Before working the present embodiment, the following detailed description of the present embodiment is given in connection with the present embodiment for the sake of convenience in understanding the present embodiment, but the present invention can be embodied in many different ways as defined and covered by the claims.
The invention is illustrated by 3 examples:
example 1:
s1, weighing 7.34g of vinyl silicone oil with the dynamic viscosity of 100 mPas and 3.72g of vinyl silicone oil with the dynamic viscosity of 3500 mPas to prepare first vinyl silicone oil, weighing 91g of inorganic heat-conducting powder (wherein the inorganic heat-conducting powder comprises 35g of 5-micron spherical alumina, 16g of 45-micron spherical alumina, 20g of 50-micron angular alumina and 20g of 75-micron aluminum hydroxide), putting the first vinyl silicone oil into a reaction kettle, starting stirring, dividing the inorganic heat-conducting powder into 3 times, putting the mixture into the reaction kettle at the stirring mixing speed of 20r/min, stirring for 10min, adding 0.15g of decyl trimethoxy silane, stirring for 10min at 20r/min, then heating to 120 ℃, continuing to stir for 20min, after the mixture is cooled to room temperature, continuing to sequentially adding 0.8g of side hydrogen-containing silicone oil, the hydrogen content of 0.1 wt, 0.3g of cyclohexyl alkynol inhibitor and 0.25g of platinum catalyst (the platinum content of 300 ppm), stirring for 2h at the stirring speed of 30r/min, and obtaining a vacuum stirring component.
S2, weighing 11.6g of vinyl silicone oil with the dynamic viscosity of 5000 mPas and 69.8g of vinyl silicone oil with the dynamic viscosity of 1000 mPas to prepare second vinyl silicone oil, weighing 11.6g of vinyl silicone resin with the dynamic viscosity of 1000 mPas, 4.1g of side hydrogen-containing silicone oil, 0.18-wt% of hydrogen content and 1.2g of cyclohexynyl alcohol inhibitor, putting the raw materials into a reaction kettle, stirring and mixing at the rotating speed of 20r/min for 40min, continuously adding 1.7g of platinum catalyst (with the platinum content of 300 ppm), stirring and mixing at the rotating speed of 20r/min for 30min, and then vacuumizing for 1h to obtain the surface treatment oil.
S3, coating the surface treatment oil on a release film on one surface by using a coating machine, wherein the coating thickness is 20 microns, rolling the rubber material component into a sheet shape by using the release film coated with the surface treatment oil as a bottom film, and vulcanizing and molding at 120 ℃ for 40min to obtain the heat-conducting gasket.
Example 2:
s1, weighing 8.14g of vinyl silicone oil with the dynamic viscosity of 350 mPas and 3.05g of vinyl silicone oil with the dynamic viscosity of 3500 mPas to prepare first vinyl silicone oil, weighing 93g of inorganic heat-conducting powder (wherein the inorganic heat-conducting powder comprises 35g of 5-mu m spherical alumina, 10g of 45-mu m spherical alumina, 30g of 90-mu m spherical alumina, 13g of 50-mu m angular alumina and 5g of 75-mu m aluminum hydroxide), putting the first vinyl silicone oil into a reaction kettle, starting stirring, dividing the inorganic heat-conducting powder into 5 times, putting the mixture into the reaction kettle at a stirring and mixing speed of 20r/min, stirring for 30min, adding 0.2g of dodecyl trimethoxy silane after mixing, stirring at a stirring speed of 20r/min, stirring for 15min, then heating to 120 ℃, continuing stirring for 40min, after the mixture is cooled to room temperature, continuing to add 0.63g of side silicone oil containing hydrogen, 0.1 wt of hydrogen, 0.22g of cyclohexylynol inhibitor, 0.28g of platinum catalyst (platinum catalyst content of 300 ppm), stirring at a stirring speed of 25 ppm, and vacuumizing to obtain a platinum component.
S2, weighing 18g of vinyl silicone oil with the dynamic viscosity of 5000 mPas and 63.1g of vinyl silicone oil with the dynamic viscosity of 1000 mPas to prepare second vinyl silicone oil, weighing 11.7g of vinyl silicone resin with the dynamic viscosity of 1000 mPas, 5.0g of side hydrogen-containing silicone oil, 0.18 percent of hydrogen content and 0.9g of cyclohexynol inhibitor, putting the raw materials into a reaction kettle, stirring and mixing at the rotating speed of 20r/min for 30min, continuously adding 1.4g of platinum catalyst (with the platinum content of 3000 ppm), stirring and mixing at the rotating speed of 20r/min for 20min, stirring for 20min, and vacuumizing for 1.5h to obtain the surface treatment oil.
S3, coating the surface treatment oil on a release film on one surface by using a coating machine, wherein the coating thickness is 50 microns, rolling the rubber material component into a sheet shape by using the release film coated with the surface treatment oil as a bottom film, and vulcanizing and molding at 150 ℃ for 20min to obtain the heat-conducting gasket.
Example 3:
s1, weighing 8.13g of vinyl silicone oil with the dynamic viscosity of 300 mPas as first vinyl silicone oil, weighing 95g of inorganic heat-conducting powder (wherein the inorganic heat-conducting powder comprises 30g of 5-micron spherical alumina, 20g of 45-micron spherical alumina, 35g of 90-micron spherical alumina and 10g of 75-micron aluminum hydroxide), putting the first vinyl silicone oil into a reaction kettle, starting stirring, putting the inorganic heat-conducting powder into the reaction kettle for 3 times at the stirring and mixing speed of 30r/min, stirring for 25min, adding 0.14g of hexadecyl trimethoxy silane after mixing, stirring and mixing at the stirring speed of 20r/min, stirring for 20min, then heating to 130 ℃, continuing stirring for 25min, after the mixture is cooled to room temperature, continuing to add 0.46g of lateral hydrogen-containing silicone oil, 0.1 wt of hydrogen content, 0.16g of methyl butinol inhibitor and 0.20g of platinum catalyst (the platinum content is 1000 ppm), stirring and mixing at the stirring speed of 50r/min, stirring for 25min, and vacuumizing for 2h to obtain a sizing material.
S2, weighing 11.6g of vinyl silicone oil with the dynamic viscosity of 5000 mPas and 69.8g of vinyl silicone oil with the dynamic viscosity of 1000 mPas, mixing to obtain second vinyl silicone oil, weighing 11.6g of vinyl silicone resin with the dynamic viscosity of 1000 mPas, 4.1g of side hydrogen-containing silicone oil, 0.18-wt% of hydrogen content and 1.2g of methylbutinol inhibitor, putting the raw materials into a reaction kettle, stirring and mixing at the rotating speed of 30r/min for 30min, continuously adding 1.7g of platinum catalyst (with the platinum content of 1000 ppm), stirring for 20min at the rotating speed of 30r/min, and vacuumizing for 1h to obtain the surface treatment oil.
S3, coating the surface treatment oil on a release film on one surface by using a coating machine, wherein the coating thickness is 20 microns, rolling the rubber material component into a sheet shape by using the release film coated with the surface treatment oil as a bottom film, and vulcanizing and molding at 130 ℃ for 30min to obtain the heat-conducting gasket.
Thus, the product performance test table of examples 1 to 3 in FIG. 1 was obtained through the test.
Therefore, the invention can realize a large amount of filling by using a large amount of spherical alumina, effectively reduces the cost of the heat conduction gasket while increasing the heat conductivity, the heat conductivity coefficient can reach 1.8-3.5W/m.K, realizes the manufacture of the low-hardness heat conduction gasket by reducing the cross-linking density of vinyl and hydrogen-containing silicone oil, the shore (Shore hardness) 00 of the gasket is in the range of 15-25 hardness, the gasket has softer hardness, is easy to deform and fill gaps, and can be tightly filled between a heating source and a radiator; meanwhile, the surface treatment oil is smeared on the surface of the heat conduction gasket through the release film, and the surface of the heat conduction gasket is subjected to viscosity removal treatment, so that the prepared heat conduction gasket is low in viscosity and good in operability, is convenient to prepare, and greatly meets the actual use requirements of users.
The embodiment provides a heat-conducting gasket with low hardness, low surface viscosity, comprising a heat-conducting gasket consisting of a sizing component and surface treatment oil;
the rubber material comprises the following components in percentage by mass:
85% -90% of inorganic heat conducting powder;
5 to 15 percent of first vinyl silicone oil;
0.5 to 1.5 percent of hydrogen-containing silicone oil;
0.05 to 0.1 percent of coupling agent;
0.15 to 0.3 percent of inhibitor;
0.2 to 0.4 percent of catalyst;
the surface treatment oil comprises the following components in percentage by mass:
80-85% of second vinyl silicone oil;
10-15% of vinyl silicone resin;
2 to 5 percent of hydrogen-containing silicone oil;
0.5 to 2 percent of inhibitor;
1% -2% of a catalyst;
wherein, the inorganic heat conducting powder is one or a combination of more of spherical alumina, angular alumina, aluminum hydroxide and zinc oxide.
Preferably, the inorganic heat-conducting powder comprises the following components in percentage by mass:
40% -90% of spherical alumina;
0 to 30 percent of angular alumina;
0 to 35 percent of aluminum hydroxide.
Further, the spherical alumina of the present example has a particle size of 1 to 50 μm, the angular alumina has a particle size of 45 to 70 μm, and the aluminum hydroxide has a particle size of 30 to 80 μm.
Further, the dynamic viscosity of the first vinyl silicone oil and the second vinyl silicone oil of the present example was 50 to 5000mPa · s.
Further, the first vinyl silicone oil of the embodiment is prepared by mixing and compounding vinyl silicone oil with dynamic viscosity of 50-100 mPa.s and vinyl silicone oil with dynamic viscosity of 3000-5000 mPa.s, wherein the compounding ratio is 1.5-3.1; the second vinyl silicone oil is prepared by mixing vinyl silicone oil with the dynamic viscosity of 100mPa & s-1000 mPa & s and vinyl silicone oil with the dynamic viscosity of 3000mPa & s-5000 mPa & s in a compounding ratio of 3-6.1.
Further, the dynamic viscosity of the vinyl-based silicone resin of the present example is 100 mPas to 2000 mPas.
Further, the hydrogen-containing silicone oil of the embodiment is one or a combination of lateral hydrogen-containing silicone oil and terminal hydrogen-containing silicone oil, and the optimal hydrogen content is 0.05-0.18 wt%.
Further, the coupling agent of the present embodiment is one or more combinations of octyl trimethoxysilane, decyl trimethoxysilane, dodecyl trimethoxysilane and hexadecyl trimethoxysilane, and the inhibitor is one or more combinations of benzotriazole, cyclohexylynol and methylbutynol.
Further, the catalyst of the embodiment is a platinum catalyst, and the optimal platinum content is 100 to 5000ppm.
The preparation method of the heat conduction gasket with the low hardness, the low surface viscosity, provided by the embodiment is characterized by comprising the following steps of: the manufacturing process comprises the following steps:
s1, respectively weighing raw materials with corresponding percentage mass according to each component of the sizing material component, putting the first vinyl silicone oil into a reaction kettle, starting stirring, putting the inorganic heat conduction powder into the reaction kettle for 3-6 times at a rotating speed of 10-30 r/min, stirring for 5-10 min, putting a coupling agent into the reaction kettle at a stirring rotating speed of 10-30 r/min, stirring for 10-30 min, heating to 120-150 ℃, continuing to stir for 20-40 min, cooling to room temperature, sequentially putting hydrogen-containing silicone oil, an inhibitor and a catalyst into the reaction kettle at a stirring rotating speed of 20-50 r/min, stirring for 10-60 min, and starting vacuumizing for 2-12 h to obtain the sizing material component;
s2, respectively weighing raw materials with corresponding mass percentages according to the components of the surface treatment oil, respectively putting divinyl silicon oil, silicon resin, lateral hydrogen and an inhibitor into a reaction kettle, starting stirring at the stirring speed of 10-30 r/min, adding a catalyst after stirring for 30-60 min at the stirring speed of 20-50 r/min, and starting vacuumizing for 1-2 h after stirring for 10-30 min to obtain the surface treatment oil;
s3, coating the surface treatment oil on the surface of the release film by using a coating machine, wherein the coating thickness is 20-100 mu m, rolling the rubber material component into a sheet shape by using the release film coated with the surface treatment oil as a base film, and vulcanizing and molding at 120-150 ℃ for 30-60 min to obtain the heat conduction gasket.
The above description is only a preferred embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications of equivalent structures and equivalent processes, which are made by using the contents of the present specification and the accompanying drawings, or directly or indirectly applied to other related technical fields, are included in the scope of the present invention.

Claims (10)

1. A low-hardness, low-surface-viscosity heat-conducting gasket is characterized in that: comprises a heat-conducting pad consisting of a sizing component and surface treatment oil;
the rubber material comprises the following components in percentage by mass:
85% -90% of inorganic heat-conducting powder;
5% -15% of first vinyl silicone oil;
0.5 to 1.5 percent of hydrogen-containing silicone oil;
0.05 to 0.1 percent of coupling agent;
0.15 to 0.3 percent of inhibitor;
0.2 to 0.4 percent of catalyst;
the surface treatment oil comprises the following components in percentage by mass:
80-85% of second vinyl silicone oil;
10-15% of vinyl silicone resin;
2 to 5 percent of hydrogen-containing silicone oil;
0.5 to 2 percent of inhibitor;
1% -2% of a catalyst;
wherein, the inorganic heat conducting powder is one or a combination of more of spherical alumina, angular alumina, aluminum hydroxide and zinc oxide.
2. A low-hardness, surface-area, low-adhesion thermal gasket as set forth in claim 1 wherein: the inorganic heat-conducting powder comprises the following components in percentage by mass:
40% -90% of spherical alumina;
0 to 30 percent of angular alumina;
0 to 35 percent of aluminum hydroxide.
3. The low-hardness, surface-adhesion, and heat-conducting gasket as claimed in claim 1, wherein: the grain size of the spherical alumina is 1-50 mu m, the grain size of the angular alumina is 45-70 mu m, and the grain size of the aluminum hydroxide is 30-80 mu m.
4. The low-hardness, surface-adhesion, and heat-conducting gasket as claimed in claim 1, wherein: the dynamic viscosity of the first vinyl silicone oil and the second vinyl silicone oil is 50-5000 mPa.
5. The low-hardness, surface-adhesion, and heat-conducting gasket as claimed in claim 1, wherein: the first vinyl silicone oil is prepared by mixing and compounding vinyl silicone oil with dynamic viscosity of 50-100 mPa.s and vinyl silicone oil with dynamic viscosity of 3000-5000 mPa.s, and the compounding ratio is 1.5-3.1; the second vinyl silicone oil is prepared by mixing vinyl silicone oil with the dynamic viscosity of 100-1000 mPa.s and vinyl silicone oil with the dynamic viscosity of 3000-5000 mPa.s in a compounding ratio of 3-6.1.
6. A low-hardness, surface-area, low-adhesion thermal gasket as set forth in claim 1 wherein: the dynamic viscosity of the vinyl silicone resin is 100mPa & s-2000 mPa & s.
7. The low-hardness, surface-adhesion, and heat-conducting gasket as claimed in claim 1, wherein: the hydrogen-containing silicone oil is one or a combination of lateral hydrogen-containing silicone oil and terminal hydrogen-containing silicone oil, and the optimal hydrogen content is 0.05-0.18 wt%.
8. The low-hardness, surface-adhesion, and heat-conducting gasket as claimed in claim 1, wherein: the coupling agent is one or more of octyl trimethoxysilane, decyl trimethoxysilane, dodecyl trimethoxysilane and hexadecyl trimethoxysilane, and the inhibitor is one or more of benzotriazole, cyclohexylynol and methylbutynol.
9. A low-hardness, surface-area, low-adhesion thermal gasket as set forth in claim 1 wherein: the catalyst is a platinum catalyst, and the optimal platinum content is 100-5000 ppm.
10. A method for preparing a low-hardness, surface-adhesion, and low-tack thermal gasket as claimed in claims 1 to 9, wherein: a preparation method of a heat conduction gasket with low hardness, low surface viscosity is characterized in that: the manufacturing process comprises the following steps:
s1, respectively weighing raw materials with corresponding percentage mass according to the components of the sizing material, putting the first vinyl silicone oil into a reaction kettle, starting stirring, putting the inorganic heat conduction powder into the reaction kettle for 3-6 times at a rotating speed of 10-30 r/min, after stirring for 5-10 min, putting a coupling agent into the reaction kettle at a stirring rotating speed of 10-30 r/min, after stirring for 10-30 min, heating to 120-150 ℃, continuing stirring for 20-40 min, cooling to room temperature, sequentially putting hydrogen-containing silicone oil, an inhibitor and a catalyst into the reaction kettle at a stirring rotating speed of 20-50 r/min, after stirring for 10-60 min, starting vacuumizing for 2-12 h to obtain the sizing material component;
s2, respectively weighing raw materials with corresponding mass percentages according to the components of the surface treatment oil, respectively putting divinyl silicon oil, silicon resin, lateral hydrogen and an inhibitor into a reaction kettle, starting stirring at the stirring speed of 10-30 r/min, adding a catalyst after stirring for 30-60 min at the stirring speed of 20-50 r/min, and starting vacuumizing for 1-2 h after stirring for 10-30 min to obtain the surface treatment oil;
s3, coating the surface treatment oil on the surface of the release film by using a coating machine, wherein the coating thickness is 20-100 mu m, rolling the rubber material component into a sheet shape by using the release film coated with the surface treatment oil as a base film, and vulcanizing and molding at 120-150 ℃ for 30-60 min to obtain the heat conduction gasket.
CN202211267888.6A 2022-10-17 2022-10-17 Low-hardness heat-conducting gasket with low surface viscosity and preparation method thereof Pending CN115627075A (en)

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CN103408937A (en) * 2013-07-30 2013-11-27 深圳德邦界面材料有限公司 Sticky or non-sticky heat conduction interface material and preparation method thereof
CN107459938A (en) * 2017-08-14 2017-12-12 东莞市哲华电子有限公司 A kind of preparation method of composite type heat radiation silica gel pad
CN108949056A (en) * 2018-07-17 2018-12-07 德阳中碳新材料科技有限公司 A kind of preparation method of heat-conducting interface material and products thereof
CN210820979U (en) * 2019-09-23 2020-06-23 苏州泰吉诺新材料科技有限公司 Online coating equipment for heat-conducting gasket glue film layer
CN113396055A (en) * 2019-02-07 2021-09-14 信越化学工业株式会社 Thermally conductive silicone rubber sheet having thermally conductive adhesive layer

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6344104B1 (en) * 1998-01-09 2002-02-05 Shin-Etsu Chemical Co., Ltd. Method of reducing surface tackiness of low-hardness thermally conductive silicone rubber sheet
CN1827720A (en) * 2004-12-27 2006-09-06 信越化学工业株式会社 Preparation of heat transfer member and heat-dissipating structure
CN102533152A (en) * 2012-01-18 2012-07-04 苏州领胜电子科技有限公司 Heat-conducting siliconfilm and manufacturing method thereof
CN102555331A (en) * 2012-01-18 2012-07-11 苏州领胜电子科技有限公司 Thermal-conductive silicon sheet and manufacturing method thereof
CN103408937A (en) * 2013-07-30 2013-11-27 深圳德邦界面材料有限公司 Sticky or non-sticky heat conduction interface material and preparation method thereof
CN107459938A (en) * 2017-08-14 2017-12-12 东莞市哲华电子有限公司 A kind of preparation method of composite type heat radiation silica gel pad
CN108949056A (en) * 2018-07-17 2018-12-07 德阳中碳新材料科技有限公司 A kind of preparation method of heat-conducting interface material and products thereof
CN113396055A (en) * 2019-02-07 2021-09-14 信越化学工业株式会社 Thermally conductive silicone rubber sheet having thermally conductive adhesive layer
CN210820979U (en) * 2019-09-23 2020-06-23 苏州泰吉诺新材料科技有限公司 Online coating equipment for heat-conducting gasket glue film layer

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