CN110982278A - Low-volatilization heat-conducting gasket and preparation method thereof - Google Patents
Low-volatilization heat-conducting gasket and preparation method thereof Download PDFInfo
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- 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
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- 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
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- 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
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- 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
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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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
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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
- C08K7/00—Use of ingredients characterised by shape
- C08K7/16—Solid spheres
- C08K7/18—Solid spheres inorganic
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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
- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
- C08K7/26—Silicon- containing compounds
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Abstract
The invention belongs to the technical field of organic silicon heat-conducting gaskets, and particularly relates to a heat-conducting gasket with low volatilization and a preparation method thereof. In the invention, the raw material resin is selected to control the content of the organic silicon monomer D4-D10 to be below 300ppm, the heat-conducting filler is used after being baked at high temperature, and loose and porous gas-phase silicon and a chain extender are added to react with small molecules, so that the heat-conducting gasket with low volatilization amount is prepared. The obtained gasket is baked for 24 hours at 150 ℃, the weight loss is less than 0.03 percent, and the gasket is successfully applied to the fields of monitoring and the like. The heat conducting gasket is used for monitoring and inside the LED lamp tube, can play a role in heat conducting and radiating, and does not influence the brightness and definition of the lamp.
Description
Technical Field
The invention belongs to the technical field of organic silicon heat-conducting gaskets, and particularly relates to a heat-conducting gasket with low volatilization and a preparation method thereof.
Background
The heat conduction gasket continuously guides out heat generated in the electronic element, and the service life and the use stability of the product are prolonged. The product is in long-term use, and some micromolecules of heat conduction gasket inside can volatilize gradually, and the gasket is because the encapsulation is inside the fluorescent tube, and the surface of transparent material such as glass is gathered to volatile micromolecule, and serious can influence the luminance and the definition of fluorescent tube. Therefore, the volatilization amount of the heat-conducting gasket is controlled, so that the brightness and the definition of the product are not influenced in the using process of the product.
The volatile matter of the heat conducting gasket is mainly water vapor and resin micromolecules. Moisture is mainly introduced by the filler, and small molecules of the resin are difficult to completely remove. For silicone resins, the small molecules are mainly some of the small molecules D4-D10. As long as the content of the small-molecule volatile matters can be greatly reduced, the heat-conducting gasket with low volatilization can be prepared and applied to the fields of monitoring and the like.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a heat conduction gasket with low volatilization and a preparation method thereof.
The technical scheme for solving the technical problems is as follows: a heat conduction gasket with low volatilization comprises the following components in parts by weight: 100 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, 3-5 parts of chain extender, 3-5 parts of gas phase silicon, 1000 parts of spherical alumina and 50-100 parts of zinc oxide.
Further, the vinyl silicone oil has a vinyl content of 0.05-0.3 wt% and a viscosity of 500-1000 mPa.s, wherein the content of the organosilicon monomer D4-D10 is less than or equal to 300 ppm.
Still further, the silicone D4 is monomeric octamethylcyclotetrasiloxane, D5 is decamethylcyclopentasiloxane, D6 is dodecamethylcyclohexasiloxane, D7 is decatetramethylcyclohexasiloxane, D8 is hexadecamethylcyclooctasiloxane, D9 is octadecylcyclononasiloxane, and D10 is eicosylcyclodecasiloxane.
Further, the viscosity of the phenyl silicone oil is 300-600 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 chain extender is polydimethylsiloxane containing active hydrogen groups.
Further, the spherical alumina is aluminum hydroxide with the particle size of 2-5 mu m.
Further, the particle size of the zinc oxide is 0.5-1.0 μm.
The second objective of the present invention is to provide a method for preparing the heat conducting gasket with low volatilization, which comprises the following steps:
(1) baking spherical aluminum oxide and zinc oxide at 105 ℃ for 12h, and cooling to 15-25 ℃ for later use;
(2) adding 100 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 3-5 parts of chain extender into a stirring kettle, and stirring for 0.5h at the rotating speed of 10-30 rpm; continuously adding 1000 parts of the spherical alumina 800-one in the step (1), and stirring for 1h at the rotating speed of 20-30 rpm; adding 50-100 parts of zinc oxide obtained in the step (1), and stirring for 0.5h at the rotating speed of 30-50 rpm; finally, 3-5 parts of gas phase silicon is added, and the mixture is stirred for 0.5h at the rotating speed of 30-50rpm to obtain a mixture;
(3) and (3) pressing the mixture obtained in the step (2) into a sheet with the thickness of 2mm, and vulcanizing at 125 ℃ for 0.5h to obtain the heat-conducting gasket with the volatilization amount of less than 0.03%.
The invention has the characteristics and beneficial effects that:
in the invention, the raw material resin is selected to control the content of the organic silicon monomer D4-D10 to be below 300ppm, the heat-conducting filler is used after being baked at high temperature, and loose and porous gas-phase silicon and a chain extender are added to react with small molecules, so that the heat-conducting gasket with low volatilization amount is prepared. The obtained gasket is baked for 24 hours at 150 ℃, the weight loss is less than 0.03 percent, and the gasket is successfully applied to the fields of monitoring and the like. The heat conducting gasket is used for monitoring and inside the LED lamp tube, can play a role in heat conducting and radiating, and does not influence the brightness and definition of the lamp.
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 low volatilization comprises the following components in parts by weight: 100 parts of vinyl silicone oil (with the vinyl content of 0.05 wt% and the viscosity of 500 mPa.s), 5 parts of phenyl silicone oil (with the viscosity of 300 mPa.s), 1 part of hydrogen-containing silicone oil (with the active hydrogen content of 0.2 wt%), 1 part of platinum catalyst, 3 parts of chain extender, 3 parts of gas phase silicon, 800 parts of spherical alumina and 50 parts of zinc oxide.
The preparation method of the heat conduction gasket with low volatilization comprises the following steps:
(1) baking spherical aluminum oxide and zinc oxide at 105 ℃ for 12h, and cooling to 15-25 ℃ for later use;
(2) adding 100 parts of vinyl silicone oil (with the vinyl content of 0.05 wt% and the viscosity of 500mPa & s), 5 parts of phenyl silicone oil (with the viscosity of 300mPa & s), 1 part of hydrogen-containing silicone oil (with the active hydrogen content of 0.2 wt%), 1 part of platinum catalyst and 3 parts of chain extender into a stirring kettle, and stirring for 0.5h at the rotating speed of 10 rpm; continuously adding 800 parts of the spherical alumina in the step (1), and stirring for 1h at the rotating speed of 20 rpm; adding 50 parts of zinc oxide obtained in the step (1), and stirring for 0.5h at the rotating speed of 30 rpm; finally, 3 parts of gas phase silicon is added, and the mixture is stirred for 0.5h at the rotating speed of 30rpm to obtain a mixture;
(3) pressing the mixture obtained in the step (2) into a sheet with the thickness of 2mm, and vulcanizing at 125 ℃ for 0.5h to obtain a heat-conducting gasket; the obtained heat-conducting gasket is baked for 24 hours at the temperature of 150 ℃, and the weight loss is 0.03 percent.
Example 2
A heat conduction gasket with low volatilization comprises the following components in parts by weight: 100 parts of vinyl silicone oil (with the vinyl content of 0.2wt percent and the viscosity of 800 mPas), 15 parts of phenyl silicone oil (with the viscosity of 500 mPas), 5 parts of hydrogen-containing silicone oil (with the active hydrogen content of 0.3wt percent), 3 parts of platinum catalyst, 5 parts of chain extender, 5 parts of gas phase silicon, 1000 parts of spherical alumina and 100 parts of zinc oxide.
The preparation method of the heat conduction gasket with low volatilization comprises the following steps:
(1) baking spherical aluminum oxide and zinc oxide at 105 ℃ for 12h, and cooling to 15-25 ℃ for later use;
(2) adding 100 parts of vinyl silicone oil (with the vinyl content of 0.2 wt% and the viscosity of 800mPa & s), 15 parts of phenyl silicone oil (with the viscosity of 500mPa & s), 5 parts of hydrogen-containing silicone oil (with the active hydrogen content of 0.3 wt%), 3 parts of platinum catalyst and 5 parts of chain extender into a stirring kettle, and stirring for 0.5h at the rotating speed of 20 rpm; continuously adding 1000 parts of the spherical alumina in the step (1), and stirring for 1h at the rotating speed of 30 rpm; adding 100 parts of zinc oxide obtained in the step (1), and stirring for 0.5h at the rotating speed of 50 rpm; finally, 5 parts of gas phase silicon is added, and the mixture is stirred for 0.5h at the rotating speed of 50rpm to obtain a mixture;
(3) pressing the mixture obtained in the step (2) into a sheet with the thickness of 2mm, and vulcanizing at 125 ℃ for 0.5h to obtain a heat-conducting gasket; the obtained heat-conducting gasket is baked for 24 hours at the temperature of 150 ℃, and the weight loss is 0.028%.
Example 3
A heat conduction gasket with low volatilization comprises the following components in parts by weight: 100 parts of vinyl silicone oil (with the vinyl content of 0.3 wt% and the viscosity of 1000mPa & s), 10 parts of phenyl silicone oil (with the viscosity of 600mPa & s), 3 parts of hydrogen-containing silicone oil (with the active hydrogen content of 0.5 wt%), 2 parts of platinum catalyst, 4 parts of chain extender, 4 parts of gas phase silicon, 900 parts of spherical alumina and 80 parts of zinc oxide.
The preparation method of the heat conduction gasket with low volatilization comprises the following steps:
(1) baking spherical aluminum oxide and zinc oxide at 105 ℃ for 12h, and cooling to 15-25 ℃ for later use;
(2) 100 parts of vinyl silicone oil (with the vinyl content of 0.3 wt% and the viscosity of 1000mPa & s), 10 parts of phenyl silicone oil (with the viscosity of 600mPa & s), 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 chain extender are added into a stirring kettle and stirred for 0.5h, and the rotating speed is 30 rpm; continuously adding 900 parts of the spherical alumina in the step (1), and stirring for 1h at the rotating speed of 30 rpm; adding 80 parts of zinc oxide obtained in the step (1), and stirring for 0.5h at the rotating speed of 40 rpm; finally, 4 parts of gas phase silicon is added and stirred for 0.5h at the rotating speed of 40rpm to obtain a mixture;
(3) pressing the mixture obtained in the step (2) into a sheet with the thickness of 2mm, and vulcanizing at 125 ℃ for 0.5h to obtain a heat-conducting gasket; and baking the obtained heat-conducting gasket for 24 hours at the temperature of 150 ℃, wherein the weight loss is 0.029%.
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 (9)
1. A heat conduction gasket with low volatilization is characterized by comprising the following components in parts by weight: 100 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, 3-5 parts of chain extender, 3-5 parts of gas phase silicon, 1000 parts of spherical alumina and 50-100 parts of zinc oxide.
2. The heat conductive gasket as set forth in claim 1, wherein the vinyl silicone oil has a vinyl content of 0.05 to 0.3 wt% and a viscosity of 500-1000 mPa-s, and the silicone monomers D4-D10 are contained in an amount of 300ppm or less.
3. The thermal gasket of claim 1, wherein the phenyl silicone oil has a viscosity of 300-600 mPa-s.
4. The heat conductive gasket as set forth in claim 1, wherein the active hydrogen content in the hydrogen-containing silicone oil is 0.2-0.5 wt%.
5. The thermal gasket of claim 1 wherein the catalyst is a platinum catalyst.
6. A thermal gasket according to claim 1 wherein the chain extender is an active hydrogen group-containing polydimethylsiloxane.
7. The gasket of claim 1, wherein the spherical alumina is aluminum hydroxide with a particle size of 2-5 μm.
8. The gasket of claim 1, wherein the zinc oxide has a particle size of 0.5 to 1.0 μm.
9. A method for preparing a low-volatility thermal pad of any one of claims 1-8, comprising the steps of:
(1) baking spherical aluminum oxide and zinc oxide at 105 ℃ for 12h, and cooling to 15-25 ℃ for later use;
(2) adding 100 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 3-5 parts of chain extender into a stirring kettle, and stirring for 0.5h at the rotating speed of 10-30 rpm; continuously adding 1000 parts of the spherical alumina 800-one in the step (1), and stirring for 1h at the rotating speed of 20-30 rpm; adding 50-100 parts of zinc oxide obtained in the step (1), and stirring for 0.5h at the rotating speed of 30-50 rpm; finally, 3-5 parts of gas phase silicon is added, and the mixture is stirred for 0.5h at the rotating speed of 30-50rpm to obtain a mixture;
(3) and (3) pressing the mixture obtained in the step (2) into a sheet with the thickness of 2mm, and vulcanizing at 125 ℃ for 0.5h to obtain the heat-conducting gasket with the volatilization amount of less than 0.03%.
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Cited By (2)
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| CN111334050A (en) * | 2020-04-20 | 2020-06-26 | 苏州天脉导热科技股份有限公司 | Heat-conducting silica gel sheet with low content of condensable volatile matters and preparation method thereof |
| CN112852160A (en) * | 2021-01-12 | 2021-05-28 | 深圳德邦界面材料有限公司 | Low-volatility heat-conducting gel and preparation method thereof |
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| CN112852160A (en) * | 2021-01-12 | 2021-05-28 | 深圳德邦界面材料有限公司 | Low-volatility heat-conducting gel and preparation method thereof |
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