CN114276688A - Flame-retardant high-elasticity heat-conducting gasket and preparation method thereof - Google Patents
Flame-retardant high-elasticity heat-conducting gasket and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a flame-retardant high-elasticity heat-conducting gasket and a preparation method thereof, and solves the technical problems that the heat-conducting gasket in the prior art is poor in elasticity, does not rebound after being compressed, is easy to generate air gaps, and accordingly the heat-conducting performance of the gasket is reduced, and the heat-conducting gasket is reduced in elasticity and pollutes a circuit board due to oil leakage during compression. The material comprises the following materials in parts by weight: 100 parts of matrix resin, 3-8 parts of cross-linking agent, 750 parts of heat-conducting powder 800 parts of heat-conducting powder, 200 parts of flame retardant 250 parts of flame retardant, 0.01-0.05 part of inhibitor and 0.1-0.5 part of catalyst, wherein the matrix resin is vinyl-terminated polydimethylsiloxane. The invention selects the proper hydrogen-containing silicone oil and vinyl silicone oil, adjusts the proportion of the hydrogen-containing silicone oil and the vinyl silicone oil to control the elasticity, the hardness and the tensile modulus of the heat-conducting silica gel, and realizes the flame retardant property of the heat-conducting silica gel by adding a certain proportion of aluminum hydroxide and magnesium hydroxide.
Description
Technical Field
The invention relates to a heat-conducting gasket, in particular to a flame-retardant high-elasticity heat-conducting gasket and a preparation method thereof.
Background
In electronic devices, various electronic components are concentrated on one circuit board, resulting in more and more complicated design of the circuit board. And the heating of the electronic component cannot be dissipated in time, so that the possibility of the electronic component being in failure is increased. The heat dissipation of the electronic element is usually realized by adopting a metal heat sink, the metal sheet and the electronic element cannot be in close contact, and if air exists in a gap between the metal sheet and the electronic element, the air is a poor heat conductor, the heat conductivity coefficient of the air is only 0.026W/mK, the air cannot transfer heat to the heat sink, and thus the operating temperature of the electronic element can exceed the expectation.
A heat conduction material is inserted between the electronic element and the radiating fin, so that the occupied air is reduced, and the heat transfer efficiency of the electronic element can be greatly improved. The thermally conductive material may be in the form of wax, paste or oil, and comprises a silicone resin. The heat conducting material is required to be flexible and can adapt to the special-shaped electric appliance element on the circuit board, and the flexibility and the high elasticity of the heat conducting material can ensure that no air gap exists between the electric appliance element and the heat radiating fin.
High strength substrates such as fiberglass mesh are often added to such thermally conductive materials to maintain the cohesive strength of the material, but the addition of these substrates reduces the elasticity of the thermally conductive material, resulting in a material with lower tensile and flexible properties, leaving voids in the electrical components and heat sinks. In order to reduce the influence of flexibility of the base material, oil or a plasticizer may be added, but the heat resistance of the material is reduced. The heating temperature of electrical components such as chips is generally above 100 ℃, at which temperature oil or plasticizer will slowly precipitate and the thermal pad will re-harden until it loses elasticity, and most feasibly the bleeding of such oil or plasticizer will contaminate the electrical components and PCB board traces.
Disclosure of Invention
The invention aims to provide a flame-retardant high-elasticity heat-conducting gasket and a preparation method thereof, and aims to solve the technical problems that the heat-conducting gasket in the prior art is poor in elasticity, does not rebound after being compressed, is easy to generate air gaps, and causes the heat-conducting performance of the gasket to be reduced, and the heat-conducting gasket is reduced in elasticity and pollutes a circuit board due to oil leakage during compression.
In order to achieve the purpose, the invention provides the following technical scheme:
the invention provides a flame-retardant high-elasticity heat-conducting gasket which comprises the following materials in parts by weight:
matrix resin 100
3-8 parts of cross-linking agent
Heat conductive powder 750-
Flame retardant 200-
Inhibitor 0.01-0.05
Catalyst 0.1-0.5
The matrix resin is vinyl-terminated polydimethylsiloxane;
the cross-linking agent is hydrogen-containing silicone oil, the hydrogen content of the hydrogen-containing silicone oil is 0.05-0.3%, the hydrogen-containing silicone oil D3-D1 is less than 1000PPM, the viscosity of the hydrogen-containing silicone oil is 30-60, and the volatile matter is less than 0.5% (at 105 ℃, 1.5 hours).
Further, the vinyl-terminated polydimethylsiloxane has a viscosity of 100-2000mPa & s at 25 ℃.
Further, the heat conducting powder is insulating heat conducting powder, and the insulating heat conducting powder comprises any one or more of alumina mixed powder, magnesia powder, boron nitride powder and aluminum nitride powder.
Further, the particle size of the alumina mixed powder is 5um-100um, and the alumina mixed powder comprises any one or more of spherical alumina particles, spheroidal alumina and non-spheroidal alumina.
Further, the heat conducting powder is a non-insulating heat conducting material, and the non-insulating heat conducting material comprises any one or more of silver, aluminum and carbon.
Further, the flame retardant is any one or two of aluminum hydroxide and magnesium hydroxide.
The invention provides a preparation method of a flame-retardant high-elasticity heat-conducting gasket, which comprises the following steps:
s1, placing the matrix resin, the cross-linking agent and the inhibitor into a double-planet stirring device according to the proportion, wherein the rotating speed of the stirring device is 60-120 r/min, and stirring for 10-50 min;
s2, adding heat-conducting powder with a certain weight into the stirring device, adjusting the rotating speed to be 30-60 r/min, and continuing stirring for 0.5-1 h;
s3, after the materials are cooled to room temperature, adding a catalyst in a ratio by weight, maintaining the rotating speed at 30-60 r/min, stirring for 10-20 min, and vacuumizing at the same time to obtain a heat-conducting silica gel material;
s4, rolling the heat-conducting silica gel rubber material obtained in the step S3 into a sheet with the thickness of 1-5 mm, curing the sheet at the temperature of 100-130 ℃ for 5-20 min, and cutting the sheet into required sizes to obtain the high-elastic flame-retardant heat-conducting silica gel gasket.
Based on the technical scheme, the embodiment of the invention can at least produce the following technical effects:
(1) the flame-retardant high-elasticity heat-conducting gasket and the preparation method thereof provided by the invention have the advantages that the elasticity, the hardness and the tensile modulus of the heat-conducting silica gel are controlled by selecting the proper hydrogen-containing silicone oil and vinyl silicone oil and adjusting the proportion of the hydrogen-containing silicone oil and the vinyl silicone oil. The hydrogen-containing silicone oil is an excellent cross-linking agent of vinyl methyl siloxane, and the vinyl bond of the vinyl silicone oil can be opened by the hydrogen bond of the hydrogen-containing silicone oil to generate addition reaction so that the vinyl silicone oil forms a network structure to finish curing. The addition amount of the heat conducting gasket is too large, so that the heat conducting gasket is too hard, the tensile modulus is increased, and the initial viscosity is poor; if the amount is too small, crosslinking is incomplete, and the film is sticky and the modulus is lowered. Therefore, the high level of elasticity, hardness and tensile modulus must be achieved through a fine formulation test. The flame retardant property of the heat-conducting silica gel is realized by adding aluminum hydroxide and aluminum hydroxide in a certain proportion. The flame retarding mechanism of aluminum hydroxide and magnesium hydroxide is that they are decomposed by a large amount of heat during combustion, and the decomposed substances such as water vapor dilute the combustible gas to achieve the purpose of flame retarding.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be described in detail below. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the examples given herein without any inventive step, are within the scope of the present invention.
The invention provides a flame-retardant high-elasticity heat-conducting gasket which comprises the following materials in parts by weight:
matrix resin 100
3-8 parts of cross-linking agent
Heat conductive powder 750-
Flame retardant 200-
Inhibitor 0.01-0.05
Catalyst 0.1-0.5
The matrix resin is vinyl-terminated polydimethylsiloxane;
the cross-linking agent is hydrogen-containing silicone oil, the hydrogen content of the hydrogen-containing silicone oil is 0.05-0.3%, the hydrogen-containing silicone oil D3-D1 is less than 1000PPM, the viscosity of the hydrogen-containing silicone oil is 30-60, and the volatile matter is less than 0.5% (at 105 ℃, 1.5 hours).
The inhibitor is ethynyl cyclohexanol, and the catalyst is platinum catalyst coordinated with vinyl.
The cross-linking agent is selected from hydrogen-containing silicone oil, and is mainly characterized in that a side chain methyl group or a terminal methyl group of the polymethylsiloxane is replaced by a hydrogen atom, so that the hydrogen-containing silicone oil can spread double bonds on vinyl silicone oil under the action of a metal catalyst to complete addition reaction, and the purposes of chain extension and cross-linking are achieved at the same time. The matrix resin is crosslinked and changes from liquid to solid, and is imparted with a certain cohesive strength and elasticity. The hydrogen content of the hydrogen-containing silicone oil is selected to be 0.05-0.3%, the selection of the hydrogen-containing silicone oil determines the hardness of the heat-conducting gasket, the hardness of the heat-conducting gasket made of the hydrogen-containing silicone oil with high hydrogen content is generally higher, the hardness of the heat-conducting silicone gasket is increased along with the increase of the addition amount of the hydrogen-containing silicone oil, and the surface viscosity is extremely reduced. The total amount of the hydrogen-containing silicone oil D3-D10 is very critical to the oil permeability index of the heat-conducting gasket, and the content is generally required to be less than 1000 PPM. The hydrogen-containing silicone oil has viscosity of 30-60, colorless and transparent appearance, and volatile matter less than 0.5% (105 deg.C, 1.5 hr).
Further, the vinyl-terminated polydimethylsiloxane has a viscosity of 100-2000mPa & s at 25 ℃.
The silicone oil is colorless, tasteless and transparent liquid at normal temperature, and has iodine value lower than 5% and water content lower than 0.1%.
Further, the heat conducting powder is insulating heat conducting powder, and the insulating heat conducting powder comprises any one or more of alumina mixed powder, magnesia powder, boron nitride powder and aluminum nitride powder.
Thermal conductivity 33 for alumina, 36 for magnesia, 300 for aluminum nitride, and 280 for boron nitride.
Further, the particle size of the alumina mixed powder is 5um-100um, and the alumina mixed powder comprises any one or more of spherical alumina particles, spheroidal alumina and non-spheroidal alumina.
The particle size of the alumina is 5um-100u, and the alumina with the particle size, spherical appearance and non-spherical appearance is matched for use, so that ideal material viscosity and thixotropy of the material can be obtained, and the processing performance is improved.
Further, the heat conducting powder is a non-insulating heat conducting material, and the non-insulating heat conducting material comprises any one or more of silver, aluminum and carbon.
Further, the flame retardant is any one or two of aluminum hydroxide and magnesium hydroxide.
The pH value of the aluminum hydroxide is 7.5-9.8, the content of the aluminum hydroxide is more than 99.5%, and the particle size is more than 5000 meshes. The particle size of the magnesium hydroxide is 1-2 microns, and the content is 98-99%.
The invention provides a preparation method of a flame-retardant high-elasticity heat-conducting gasket, which comprises the following steps:
s1, placing the matrix resin, the cross-linking agent and the inhibitor into a double-planet stirring device according to the proportion, wherein the rotating speed of the stirring device is 60-120 r/min, and stirring for 10-50 min;
s2, adding heat-conducting powder with a certain weight into the stirring device, adjusting the rotating speed to be 30-60 r/min, and continuing stirring for 0.5-1 h;
s3, after the materials are cooled to room temperature, adding a catalyst in a ratio by weight, maintaining the rotating speed at 30-60 r/min, stirring for 10-20 min, and vacuumizing at the same time to obtain a heat-conducting silica gel material;
s4, rolling the heat-conducting silica gel rubber material obtained in the step S3 into a sheet with the thickness of 1-5 mm, curing the sheet at the temperature of 100-130 ℃ for 5-20 min, and cutting the sheet into required sizes to obtain the high-elastic flame-retardant heat-conducting silica gel gasket.
Example 1
1.1 materials
1.2 preparation steps
S1, placing the matrix resin, the cross-linking agent and the inhibitor into a double-planet stirring device according to the proportion, wherein the rotating speed of the stirring device is 60r/min, and stirring for 10 min;
s2, adding heat-conducting powder with a certain weight into the stirring device, adjusting the rotating speed to 30r/min, and continuing stirring for 0.5 h;
s3, after the materials are cooled to room temperature, adding a catalyst in a ratio by weight, maintaining the rotating speed at 30r/min, stirring for 10min, and simultaneously vacuumizing to obtain a heat-conducting silica gel material;
s4, rolling the heat-conducting silica gel rubber material obtained in the step S3 into a sheet with the thickness of 2mm, curing the sheet at the temperature of 130 ℃ for 10min, and cutting the sheet into required sizes to obtain the high-elastic flame-retardant heat-conducting silica gel gasket.
Example 2
2.1 materials
2.2 preparation steps
S1, placing the matrix resin, the cross-linking agent and the inhibitor into a double-planet stirring device according to the proportion, wherein the rotating speed of the stirring device is 60r/min, and stirring for 10 min;
s2, adding heat-conducting powder with a certain weight into the stirring device, adjusting the rotating speed to 30r/min, and continuing stirring for 0.5 h;
s3, after the materials are cooled to room temperature, adding a catalyst in a ratio by weight, maintaining the rotating speed at 30r/min, stirring for 20min, and simultaneously vacuumizing to obtain a heat-conducting silica gel material;
s4, rolling the heat-conducting silica gel rubber material obtained in the step S3 into a sheet with the thickness of 2mm, curing the sheet at the temperature of 130 ℃ for 10min, and cutting the sheet into required sizes to obtain the high-elastic flame-retardant heat-conducting silica gel gasket.
Example 3
3.1 materials
3.2 preparation steps
S1, placing the matrix resin, the cross-linking agent and the inhibitor into a double-planet stirring device according to the proportion, wherein the rotating speed of the stirring device is 120r/min, and stirring for 50 min;
s2, adding heat-conducting powder with a certain weight into the stirring device, adjusting the rotating speed to 60r/min, and continuing stirring for 1 h;
s3, after the materials are cooled to room temperature, adding a catalyst in a ratio by weight, maintaining the rotating speed at 60r/min, stirring for 15min, and simultaneously vacuumizing to obtain a heat-conducting silica gel material;
s4, rolling the heat-conducting silica gel rubber material obtained in the step S3 into a sheet with the thickness of 2mm, curing the sheet at the temperature of 100 ℃ for 20min, and cutting the sheet into required sizes to obtain the high-elastic flame-retardant heat-conducting silica gel gasket.
Example 4
4.1 materials
4.2 preparation step
S1, placing the matrix resin, the cross-linking agent and the inhibitor into a double-planet stirring device according to the proportion, wherein the rotating speed of the stirring device is 80r/min, and stirring for 30 min;
s2, adding heat-conducting powder with a certain weight into the stirring device, adjusting the rotating speed to 50r/min, and continuing stirring for 0.6 h;
s3, after the materials are cooled to room temperature, adding a catalyst in a ratio by weight, maintaining the rotating speed at 60r/min, stirring for 16min, and simultaneously vacuumizing to obtain a heat-conducting silica gel sizing material;
s4, rolling the heat-conducting silica gel rubber material obtained in the step S3 into a sheet with the thickness of 2mm, curing the sheet at the temperature of 100 ℃ for 20min, and cutting the sheet into required sizes to obtain the high-elastic flame-retardant heat-conducting silica gel gasket.
Performance detection
The heat conductivity coefficient, the hardness, the compression ratio and the oil permeability of the heat-conducting silica gel gasket tested by the method of ASTM D5470 are shown in the table 1.
TABLE 1
The high elasticity of the thermal conductivity was evaluated by combining hardness and compression ratio.
The flame-retardant high-elasticity heat-conducting gasket and the preparation method thereof provided by the invention have the advantages that the elasticity, the hardness and the tensile modulus of the heat-conducting silica gel are controlled by selecting the proper hydrogen-containing silicone oil and vinyl silicone oil and adjusting the proportion of the hydrogen-containing silicone oil and the vinyl silicone oil. The hydrogen-containing silicone oil is an excellent cross-linking agent of vinyl methyl siloxane, and the vinyl bond of the vinyl silicone oil can be opened by the hydrogen bond of the hydrogen-containing silicone oil to generate addition reaction so that the vinyl silicone oil forms a network structure to finish curing. The addition amount of the heat conducting gasket is too large, so that the heat conducting gasket is too hard, the tensile modulus is increased, and the initial viscosity is poor; if the amount is too small, crosslinking is incomplete, and the film is sticky and the modulus is lowered. Therefore, the high level of elasticity, hardness and tensile modulus must be achieved through a fine formulation test. The flame retardant property of the heat-conducting silica gel is realized by adding aluminum hydroxide and aluminum hydroxide in a certain proportion. The flame retarding mechanism of aluminum hydroxide and magnesium hydroxide is that they are decomposed by a large amount of heat during combustion, and the decomposed substances such as water vapor dilute the combustible gas to achieve the purpose of flame retarding.
Claims (8)
1. The flame-retardant high-elasticity heat-conducting gasket is characterized by comprising the following materials in parts by weight:
matrix resin 100
3-8 parts of cross-linking agent
Heat conductive powder 750-
Flame retardant 200-
Inhibitor 0.01-0.05
Catalyst 0.1-0.5
The matrix resin is vinyl-terminated polydimethylsiloxane;
the cross-linking agent is hydrogen-containing silicone oil, the hydrogen content of the hydrogen-containing silicone oil is 0.05-0.3%, the hydrogen-containing silicone oil D3-D1 is less than 1000PPM, the viscosity of the hydrogen-containing silicone oil is 30-60, and the volatile component is less than 0.5%.
2. The gasket of claim 1, wherein: the viscosity of the vinyl-terminated polydimethylsiloxane is selected to be 100-2000 mPas at 25 ℃.
3. The gasket of claim 2, wherein: the vinyl-terminated polydimethylsiloxane is 500-1000 mPas.
4. The gasket of claim 1, wherein: the heat conducting powder is insulating heat conducting powder, and the insulating heat conducting powder comprises any one or more of aluminum oxide mixed powder, magnesium oxide powder, boron nitride powder and aluminum nitride powder.
5. The gasket of claim 4, wherein: the particle size of the alumina mixed powder is 5-100 um, and the alumina mixed powder comprises any one or more of spherical alumina particles, quasi-spherical alumina and non-spherical alumina.
6. The gasket of claim 1, wherein: the heat conducting powder is a non-insulating heat conducting material which comprises any one or more of silver, aluminum and carbon.
7. The gasket of claim 1, wherein: the flame retardant is any one or two of aluminum hydroxide and magnesium hydroxide.
8. The method for preparing the flame-retardant high-elasticity heat-conducting gasket according to claim 1 is characterized by comprising the following steps of:
s1, placing the matrix resin, the cross-linking agent and the inhibitor into a double-planet stirring device according to the proportion, wherein the rotating speed of the stirring device is 60-120 r/min, and stirring for 10-50 min;
s2, adding heat-conducting powder with a certain weight into the stirring device, adjusting the rotating speed to be 30-60 r/min, and continuing stirring for 0.5-1 h;
s3, after the materials are cooled to room temperature, adding a catalyst in a ratio by weight, maintaining the rotating speed at 30-60 r/min, stirring for 10-20 min, and vacuumizing at the same time to obtain a heat-conducting silica gel material;
s4, rolling the heat-conducting silica gel rubber material obtained in the step S3 into a sheet with the thickness of 1-5 mm, curing the sheet at the temperature of 100-130 ℃ for 5-20 min, and cutting the sheet into required sizes to obtain the high-elastic flame-retardant heat-conducting silica gel gasket.
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| CN115612300A (en) * | 2022-11-03 | 2023-01-17 | 苏州泰吉诺新材料科技有限公司 | Heat-conducting gasket and preparation method thereof |
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