CN111087823B - Heat conduction gasket with good reworkability and preparation method thereof - Google Patents

Heat conduction gasket with good reworkability and preparation method thereof Download PDF

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Publication number
CN111087823B
CN111087823B CN201911345921.0A CN201911345921A CN111087823B CN 111087823 B CN111087823 B CN 111087823B CN 201911345921 A CN201911345921 A CN 201911345921A CN 111087823 B CN111087823 B CN 111087823B
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parts
silicone oil
gasket
stirring
glass fiber
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CN111087823A (en
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王红玉
万炜涛
陈田安
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Shenzhen Darbond Interface Materials Co ltd
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Shenzhen Darbond Interface Materials Co ltd
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J5/00Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/18Manufacture of films or sheets
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K5/00Heat-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
    • C09K5/08Materials not undergoing a change of physical state when used
    • C09K5/14Solid materials, e.g. powdery or granular
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2383/00Characterised 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
    • C08J2383/04Polysiloxanes
    • C08J2383/08Polysiloxanes containing silicon bound to organic groups containing atoms other than carbon, hydrogen, and oxygen
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2483/00Characterised 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
    • C08J2483/04Polysiloxanes
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2483/00Characterised 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
    • C08J2483/04Polysiloxanes
    • C08J2483/05Polysiloxanes containing silicon bound to hydrogen
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2483/00Characterised 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
    • C08J2483/04Polysiloxanes
    • C08J2483/07Polysiloxanes containing silicon bound to unsaturated aliphatic groups
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • C08K2003/2227Oxides; Hydroxides of metals of aluminium
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K7/00Use of ingredients characterised by shape
    • C08K7/16Solid spheres
    • C08K7/18Solid spheres inorganic

Abstract

The invention belongs to the technical field of organic silicon heat-conducting gaskets, and particularly relates to a heat-conducting gasket with good reworkability and a preparation method thereof. According to the invention, the heat-conducting gasket is prepared by adding the methyl fluorosilicone oil and controlling the proportion of the reaction groups, and the glass fiber surface is attached to the surface of the electronic element, so that the attaching force of the radiator surface and the heat-conducting gasket is stronger than the attaching force of the electronic element and the surface of the heat-conducting gasket. In the process of disassembly, the heat-conducting gasket is separated from the interface of the electronic element, so that the aim of quick repair is fulfilled.

Description

Heat conduction gasket with good reworkability and preparation method thereof
Technical Field
The invention belongs to the technical field of organic silicon heat-conducting gaskets, and particularly relates to a heat-conducting gasket with good reworkability and a preparation method thereof.
Background
The organic silicon heat conduction gasket is used between the electronic element and the radiator, so that the service life and the stability of the electronic element can be improved. The heat conduction gasket has certain compressive capacity in the assembling process, and under the effect of certain temperature pressure in the use, the heat conduction gasket surface is very easily and tightly pasted together with the binding face for the electronic product is dismantled the difficulty, and the repairability is poor. In some emerging fields, such as mining machines, the energy consumption of products is high, the repair frequency is high, and therefore higher requirements are put on the repair property of heat conducting materials.
The heat conducting gasket is difficult to repair mainly because of the following reasons: firstly, the strength of the heat-conducting gasket is poor, and the irregular damage of a product body is caused during disassembly; secondly, unreacted groups remain in the heat conducting gasket and continuously react under the action of temperature and pressure; third, the surface wettability of the thermal pad is lost and is increasingly difficult to rework. Based on the three aspects, the invention prepares the heat-conducting gasket capable of being repaired through the formula design, and is successfully applied to the fields of mining machines and the like.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides the heat conduction gasket with good reworkability and the preparation method thereof.
The technical scheme for solving the technical problems is as follows: a heat conduction gasket with good reworkability comprises the following components in parts by weight: 100 parts of methyl fluorosilicone oil, 5-10 parts of vinyl silicone oil, 5-15 parts of phenyl silicone oil, 1-5 parts of hydrogen-containing silicone oil, 1-3 parts of catalyst, 2-5 parts of coupling agent, 500-800 parts of spherical alumina and 60-90 parts of aluminum hydroxide.
Further, the viscosity of the methyl fluorosilicone oil is 500-1000mPa & s.
Further, the vinyl silicone oil has a vinyl content of 0.05 to 0.3 wt% and a viscosity of 200mPa · s.
Further, the viscosity of the phenyl silicone oil is 500-800 mPas.
Further, the active hydrogen content in the hydrogen-containing silicone oil is 0.2-0.5 wt%.
Further, the catalyst is a platinum catalyst.
Further, the coupling agent is hexadecyl trimethoxy silane.
Further, the spherical alumina is aluminum hydroxide with the particle size of 5-10 mu m.
Further, the particle size of the aluminum hydroxide is 20-40 μm.
The second objective of the present invention is to provide a method for preparing the heat conducting gasket with good reworkability, comprising the following steps:
(1) adding 100 parts of methyl fluorosilicone oil, 5-10 parts of vinyl silicone oil, 5-15 parts of phenyl silicone oil, 1-5 parts of hydrogen-containing silicone oil, 1-3 parts of catalyst and 2-5 parts of coupling agent into a stirring kettle, and stirring for 0.5h at the rotating speed of 20-30 rpm; continuously adding 800 parts of spherical alumina, stirring for 1h at the rotating speed of 30-50 rpm; finally, adding 60-90 parts of aluminum hydroxide, stirring for 0.5h at the rotating speed of 30-50rpm to obtain a mixture;
(2) spreading glass fiber cloth on a release film, calendering the mixture obtained in the step (1), the glass fiber cloth and the release film into a sheet with the thickness of 0.3mm, and vulcanizing at 125 ℃ for 0.5 h; and (3) attaching the glass fiber cloth surface of the obtained sheet to the surface of the electronic element, and attaching the other surface of the sheet to the surface of the radiator.
The invention has the characteristics and beneficial effects that:
according to the invention, the heat-conducting gasket is prepared by adding the methyl fluorosilicone oil and controlling the proportion of the reaction groups, and the glass fiber surface is attached to the surface of the electronic element, so that the attaching force of the radiator surface and the heat-conducting gasket is stronger than the attaching force of the electronic element and the surface of the heat-conducting gasket. In the process of disassembly, the heat-conducting gasket is separated from the interface of the electronic element, so that the aim of quick repair is fulfilled.
Detailed Description
The principles and features of this invention are described below in conjunction with examples, which are set forth to illustrate, but are not to be construed to limit the scope of the invention.
Example 1
A heat conduction gasket with good reworkability comprises the following components in parts by weight: 100 parts of methyl fluorosilicone oil (with the viscosity of 500 mPas), 5 parts of vinyl silicone oil (with the vinyl content of 0.05 wt%), 5 parts of phenyl silicone oil (with the viscosity of 500 mPas), 1 part of hydrogen-containing silicone oil (with the active hydrogen content of 0.2 wt%), 1 part of platinum catalyst, 2 parts of hexadecyl trimethoxy silane, 500 parts of spherical alumina (with the particle size of 5 microns) and 60 parts of aluminum hydroxide (with the particle size of 20 microns).
The preparation method of the heat conduction gasket comprises the following steps:
(1) 100 parts of methyl fluorosilicone oil (with the viscosity of 500 mPas), 5 parts of vinyl silicone oil (with the vinyl content of 0.05 wt%), 5 parts of phenyl silicone oil (with the viscosity of 500 mPas), 1 part of hydrogen-containing silicone oil (with the active hydrogen content of 0.2 wt%), 1 part of platinum catalyst and 2 parts of hexadecyl trimethoxy silane are added into a stirring kettle and stirred for 0.5h at the rotating speed of 20 rpm; continuously adding 500 parts of spherical alumina (with the particle size of 5 mu m), stirring for 1h at the rotating speed of 30 rpm; finally, 60 parts of aluminum hydroxide (the particle size is 20 mu m) is added, and the mixture is stirred for 0.5h at the rotating speed of 30rpm to obtain a mixture;
(2) spreading glass fiber cloth on a release film, calendering the mixture obtained in the step (1), the glass fiber cloth and the release film into a sheet with the thickness of 0.3mm, and vulcanizing at 125 ℃ for 0.5 h; and (3) attaching the glass fiber cloth surface of the obtained sheet to the surface of the electronic element, and attaching the other surface of the sheet to the surface of the radiator.
Example 2
A heat conduction gasket with good reworkability comprises the following components in parts by weight: 100 parts of methyl fluorosilicone oil (the viscosity is 800 mPas), 10 parts of vinyl silicone oil (the vinyl content is 0.1 wt%), 15 parts of phenyl silicone oil (the viscosity is 600 mPas), 5 parts of hydrogen-containing silicone oil (the active hydrogen content is 0.4 wt%), 3 parts of platinum catalyst, 5 parts of hexadecyl trimethoxy silane, 800 parts of spherical alumina (the particle size is 8 mu m) and 90 parts of aluminum hydroxide (the particle size is 30 mu m).
The preparation method of the heat conduction gasket comprises the following steps:
(1) 100 parts of methyl fluorosilicone oil (with the viscosity of 800 mPas), 10 parts of vinyl silicone oil (with the vinyl content of 0.1 wt%), 15 parts of phenyl silicone oil (with the viscosity of 600 mPas), 5 parts of hydrogen-containing silicone oil (with the active hydrogen content of 0.4 wt%), 3 parts of platinum catalyst and 5 parts of hexadecyl trimethoxy silane are added into a stirring kettle and stirred for 0.5h at the rotating speed of 30 rpm; continuously adding 800 parts of spherical alumina (with the particle size of 8 mu m), stirring for 1h at the rotating speed of 50 rpm; finally, 90 parts of aluminum hydroxide (with the particle size of 30 mu m) is added and stirred for 0.5h at the rotating speed of 50rpm to obtain a mixture;
(2) spreading glass fiber cloth on a release film, calendering the mixture obtained in the step (1), the glass fiber cloth and the release film into a sheet with the thickness of 0.3mm, and vulcanizing at 125 ℃ for 0.5 h; and (3) attaching the glass fiber cloth surface of the obtained sheet to the surface of the electronic element, and attaching the other surface of the sheet to the surface of the radiator.
Example 3
A heat conduction gasket with good reworkability comprises the following components in parts by weight: 100 parts of methyl fluorosilicone oil (the viscosity is 1000 mPas), 8 parts of vinyl silicone oil (the vinyl content is 0.3 wt%), 10 parts of phenyl silicone oil (the viscosity is 800 mPas), 3 parts of hydrogen-containing silicone oil (the active hydrogen content is 0.5 wt%), 2 parts of platinum catalyst, 4 parts of hexadecyl trimethoxy silane, 700 parts of spherical alumina (the particle size is 10 mu m) and 75 parts of aluminum hydroxide (the particle size is 40 mu m).
The preparation method of the heat conduction gasket comprises the following steps:
(1) 100 parts of methyl fluorosilicone oil (with the viscosity of 1000 mPas), 8 parts of vinyl silicone oil (with the vinyl content of 0.3 wt%), 10 parts of phenyl silicone oil (with the viscosity of 800 mPas), 3 parts of hydrogen-containing silicone oil (with the active hydrogen content of 0.5 wt%), 2 parts of platinum catalyst and 4 parts of hexadecyl trimethoxy silane are added into a stirring kettle and stirred for 0.5h at the rotating speed of 20 rpm; continuously adding 700 parts of spherical alumina (with the particle size of 10 mu m), stirring for 1h at the rotating speed of 30 rpm; finally, 75 parts of aluminum hydroxide (the particle size is 40 mu m) is added, and the mixture is stirred for 0.5h at the rotating speed of 30rpm to obtain a mixture;
(2) spreading glass fiber cloth on a release film, calendering the mixture obtained in the step (1), the glass fiber cloth and the release film into a sheet with the thickness of 0.3mm, and vulcanizing at 125 ℃ for 0.5 h; and (3) attaching the glass fiber cloth surface of the obtained sheet to the surface of the electronic element, and attaching the other surface of the sheet to the surface of the radiator.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.

Claims (7)

1. A heat conduction gasket with good reworkability is characterized by comprising the following components in parts by weight: 100 parts of methyl fluorosilicone oil, 5-10 parts of vinyl silicone oil, 5-15 parts of phenyl silicone oil, 1-5 parts of hydrogen-containing silicone oil, 1-3 parts of catalyst, 2-5 parts of coupling agent, 500 parts of spherical alumina and 60-90 parts of aluminum hydroxide;
the viscosity of the methyl fluorosilicone oil is 500-1000mPa & s;
the vinyl silicone oil contains 0.05 to 0.3 weight percent of vinyl;
the active hydrogen content in the hydrogen-containing silicone oil is 0.2-0.5 wt%;
the viscosity of the phenyl silicone oil is 500-800mPa & s;
the preparation method of the heat conduction gasket comprises the following steps:
(1) adding 100 parts of methyl fluorosilicone oil, 5-10 parts of vinyl silicone oil, 5-15 parts of phenyl silicone oil, 1-5 parts of hydrogen-containing silicone oil, 1-3 parts of catalyst and 2-5 parts of coupling agent into a stirring kettle, and stirring for 0.5h at the rotating speed of 20-30 rpm; continuously adding 800 parts of spherical alumina, stirring for 1h at the rotating speed of 30-50 rpm; finally, adding 60-90 parts of aluminum hydroxide, stirring for 0.5h at the rotating speed of 30-50rpm to obtain a mixture;
(2) spreading glass fiber cloth on a release film, calendering the mixture obtained in the step (1), the glass fiber cloth and the release film into a sheet with the thickness of 0.3mm, and vulcanizing at 125 ℃ for 0.5 h; and (3) attaching the glass fiber cloth surface of the obtained sheet to the surface of the electronic element, and attaching the other surface of the sheet to the surface of the radiator.
2. The thermal gasket of claim 1, wherein the vinyl silicone oil has a viscosity of 200 mPa-s.
3. The thermal gasket of claim 1 wherein the catalyst is a platinum catalyst.
4. The thermal gasket of claim 1, wherein the coupling agent is hexadecyltrimethoxysilane.
5. The gasket of claim 1, wherein the spherical alumina is aluminum hydroxide with a particle size of 5-10 μm.
6. The gasket of claim 1, wherein the aluminum hydroxide has a particle size of 20 to 40 μm.
7. A method for preparing a heat conductive gasket with good reworkability according to any one of claims 1 to 6, comprising the steps of:
(1) adding 100 parts of methyl fluorosilicone oil, 5-10 parts of vinyl silicone oil, 5-15 parts of phenyl silicone oil, 1-5 parts of hydrogen-containing silicone oil, 1-3 parts of catalyst and 2-5 parts of coupling agent into a stirring kettle, and stirring for 0.5h at the rotating speed of 20-30 rpm; continuously adding 800 parts of spherical alumina, stirring for 1h at the rotating speed of 30-50 rpm; finally, adding 60-90 parts of aluminum hydroxide, stirring for 0.5h at the rotating speed of 30-50rpm to obtain a mixture;
(2) spreading glass fiber cloth on a release film, calendering the mixture obtained in the step (1), the glass fiber cloth and the release film into a sheet with the thickness of 0.3mm, and vulcanizing at 125 ℃ for 0.5 h; and (3) attaching the glass fiber cloth surface of the obtained sheet to the surface of the electronic element, and attaching the other surface of the sheet to the surface of the radiator.
CN201911345921.0A 2019-12-24 2019-12-24 Heat conduction gasket with good reworkability and preparation method thereof Active CN111087823B (en)

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