CN110791104A - High-temperature-resistant low-modulus silicon material and preparation method thereof - Google Patents
High-temperature-resistant low-modulus silicon material and preparation method thereof Download PDFInfo
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- CN110791104A CN110791104A CN201910883821.7A CN201910883821A CN110791104A CN 110791104 A CN110791104 A CN 110791104A CN 201910883821 A CN201910883821 A CN 201910883821A CN 110791104 A CN110791104 A CN 110791104A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- 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
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- C—CHEMISTRY; METALLURGY
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
Abstract
The invention discloses a high-temperature-resistant low-modulus silicon material and a preparation method thereof in the technical field of silicon materials, and the preparation method comprises the following steps: s1: selecting materials, S2, S3, carrying out primary stirring, S3, carrying out secondary stirring, S4, carrying out reaction, S5, carrying out primary cooling, S6, carrying out vacuum stirring, and S7, carrying out vacuum stirring, wherein ceramic micro powder, tourmaline, butyl titanate and absolute ethyl alcohol are adopted to obtain a solution, the tourmaline and the ceramic micro powder are mutually lapped to form a heat conduction network, so that the prepared heat conduction organosilicon material has a heat conduction path, the heat conductivity is further improved, the heat conduction performance and the heat dissipation performance of the prepared heat conduction organosilicon material are better, and meanwhile, the ceramic micro powder also enables the prepared heat conduction organosilicon material to have excellent performances such as corrosion resistance, high temperature resistance, weather resistance, insulation, reflective heat insulation, scratch resistance of the surface, scrub resistance and the like.
Description
Technical Field
The invention relates to the technical field of silicon materials, in particular to a high-temperature-resistant low-modulus silicon material and a preparation method thereof.
Background
With the increasing development of the electronic and electrical industry, electronic products are continuously updated to high integration, high power and small miniaturization to meet the requirements of emerging markets. However, high integration, high power and miniaturization can increase the heat generated by electronic components in unit area rapidly, if the heat is not conducted out in time, the service performance and service life of electronic and electric products are affected seriously, the current common technical method is to adopt interface heat conduction materials to fill the gap part, reduce the thermal resistance between the heating components and the radiator, and radiate the heat in time, thereby ensuring the stable and normal operation of equipment, the existing silicon material has poor heat conduction and radiation capability, and the service life of the electronic and electric products is affected seriously, therefore, the high temperature resistant low modulus silicon material and the preparation method thereof are provided.
Disclosure of Invention
The invention aims to provide a high-temperature-resistant low-modulus silicon material and a preparation method thereof, so as to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme: a high-temperature resistant low-modulus silicon material and a preparation method thereof comprise the following steps:
s1: selecting materials: the heat-conducting powder coating comprises, by weight, 10-20 parts of silicone oil, 20-40 parts of heat-conducting powder filler, 3-6 parts of low-modulus additive, 1-3 parts of high-temperature-resistant additive, 2-4 parts of crosslinking agent, 2-4 parts of platinum catalyst, 1-3 parts of ceramic micropowder, 2-5 parts of tourmaline, 2-5 parts of butyl titanate and 2-4 parts of absolute ethyl alcohol;
s2, preparation: uniformly stirring and reacting the ceramic micro powder, the tourmaline, the butyl titanate and the absolute ethyl alcohol in the S1 to obtain a solution;
s3, primary stirring: putting the silicone oil in the S1 into a dispersion machine, adding the heat-conducting powder filler and the low-modulus auxiliary agent in batches, and stirring and reacting for 40-80 min at room temperature;
s3, secondary stirring: adding the solution obtained in the step S2 into a dispersion machine in the stirring reaction process in the step S3, stirring for 10-20 min, then adding a high-temperature-resistant auxiliary agent and a crosslinking agent, and continuing stirring;
s4, reaction: heating to 100-115 ℃ under the vacuum protection condition, vacuumizing, stirring and dispersing for 40-80 min;
s5, primary cooling: after the S4 reaction is finished, standing to cool the obtained material to 68-72 ℃;
s6, vacuum stirring: after cooling, adding a platinum catalyst into the dispersion machine, vacuumizing and stirring for reacting for 25-40 min;
s7, secondary cooling: after the S6 reaction is finished, standing until the material is cooled to room temperature, and then taking out the prepared high-temperature-resistant low-modulus silicon material.
Further, the low-modulus auxiliary agent in S1 is hydroxy vinyl silicone oil or alkoxy vinyl silicone oil, and the viscosity is 1-30 cp.
Further, the refractory aid in S1 is selected from one or more of an organosilicon copper complex, an organosilicon aluminum complex, an organosilicon iron complex and an organosilicon zirconium complex.
Further, the silicone oil in S1 is methyl vinyl silicone oil or phenyl vinyl silicone oil, and the heat conductive powder filler in S1 is one or more selected from aluminum oxide, zinc oxide, boron nitride, silicon carbide, aluminum nitride, graphene, aluminum powder, and carbon nanotube powder.
Further, the cross-linking agent in S1 is composed of terminal hydrogen-containing silicone oil and side hydrogen-containing silicone oil in a mass ratio of 1: 1.5-2, the viscosity is 1-16 cp, and the platinum catalyst in S1 is a Kanstet platinum catalyst, and the viscosity is 300-1000 cp.
Further, in the step S2, the butyl titanate, the tourmaline, the ceramic micro powder and the absolute ethyl alcohol are mixed, and the mixture is stirred for 5-10 min at the stirring speed of 400-500 r/min.
Furthermore, the particle size of the heat-conducting powder filler in the S1 is 0.5-20 μm, and the shape is spherical.
Compared with the prior art, the invention has the beneficial effects that:
1) according to the invention, ceramic micro powder, tourmaline, butyl titanate and absolute ethyl alcohol are adopted to obtain a solution, and the tourmaline and the ceramic micro powder are mutually lapped to form a heat conduction network, so that the prepared heat conduction organosilicon material has a heat conduction path, the heat conductivity of the heat conduction organosilicon material is further improved, the heat conduction performance and the heat dissipation performance of the prepared heat conduction organosilicon material are better, and meanwhile, the ceramic micro powder also enables the prepared heat conduction organosilicon material to have excellent performances of corrosion resistance, high temperature resistance, weather resistance, insulation, reflective heat insulation, scratch resistance, scrubbing resistance and the like of the surface;
2) the low-modulus auxiliary agent is adopted, so that the dispersion effect and the filling rate of the heat-conducting filler powder are improved, the formation of a heat-conducting network chain of the heat-conducting filler is facilitated, the performances of low hardness and low modulus of the heat-conducting organosilicon material after curing are facilitated, the prepared heat-conducting organosilicon material has the advantages of low modulus, stable heat-conducting performance, no oil seepage, no volatilization and the like, the high-temperature-resistant auxiliary agent is added, the high-temperature-resistant performance is improved, the long-term heat dissipation stability under the high-temperature condition is ensured, and the service life is longer.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A high-temperature resistant low-modulus silicon material and a preparation method thereof comprise the following steps:
s1: selecting materials: the heat-conducting powder comprises silicon oil, heat-conducting powder filler, low-modulus additive, high-temperature-resistant additive, cross-linking agent, platinum catalyst, ceramic micro-powder, tourmaline, butyl titanate and absolute ethyl alcohol, wherein 10 parts of silicon oil, 20 parts of heat-conducting powder filler, 3 parts of low-modulus additive, 1 part of high-temperature-resistant additive, 2 parts of cross-linking agent, 2 parts of platinum catalyst, 1 part of ceramic micro-powder, 2 parts of tourmaline, 2 parts of butyl titanate and 2 parts of absolute ethyl alcohol are respectively weighed according to parts by weight;
s2, preparation: uniformly stirring and reacting the ceramic micro powder, the tourmaline, the butyl titanate and the absolute ethyl alcohol in the S1 to obtain a solution;
s3, primary stirring: putting the silicone oil in the S1 into a dispersion machine, adding the heat-conducting powder filler and the low-modulus auxiliary agent in batches, and stirring and reacting for 40min at room temperature;
s3, secondary stirring: adding the solution obtained in the step S2 into a dispersion machine in the stirring reaction process in the step S3, stirring for 10min, then adding a high-temperature resistant auxiliary agent and a crosslinking agent, and continuing stirring;
s4, reaction: heating to 100 ℃ under the vacuum protection condition, vacuumizing, stirring, and performing dispersion reaction for 40 min;
s5, primary cooling: after the S4 reaction is finished, standing to cool the obtained material to 68 ℃;
s6, vacuum stirring: after cooling, adding a platinum catalyst into the dispersion machine, vacuumizing and stirring for reaction for 25 min;
s7, secondary cooling: after the S6 reaction is finished, standing until the material is cooled to room temperature, and then taking out the prepared high-temperature-resistant low-modulus silicon material.
The low-modulus auxiliary agent in S1 is hydroxy vinyl silicone oil or alkoxy vinyl silicone oil, and the viscosity is 1 cp;
the high-temperature resistant auxiliary agent in S1 is selected from one or more of organic silicon copper complex, organic silicon aluminum complex, organic silicon iron complex and organic silicon zirconium complex;
the silicone oil in S1 is methyl vinyl silicone oil or phenyl vinyl silicone oil, and the heat-conducting powder filler in S1 is one or more selected from aluminum oxide, zinc oxide, boron nitride, silicon carbide, aluminum nitride, graphene, aluminum powder and carbon nano tube powder;
the cross-linking agent in S1 is composed of end hydrogen-containing silicone oil and side hydrogen-containing silicone oil in a mass ratio of 1:1.5, the viscosity is 1cp, the platinum catalyst in S1 is a Kanst platinum catalyst, and the viscosity is 300 cp;
s2, mixing the butyl titanate, the tourmaline, the ceramic micro powder and the absolute ethyl alcohol, and stirring for 5min at the stirring speed of 400 r/min;
the heat-conducting powder filler in S1 has a spherical shape and a particle size of 0.5 μm.
Example 2
A high-temperature resistant low-modulus silicon material and a preparation method thereof comprise the following steps:
s1: selecting materials: 15 parts of silicone oil, 30 parts of heat-conducting powder filler, 5 parts of low-modulus additive, 2 parts of high-temperature-resistant additive, 3 parts of crosslinking agent, 3 parts of platinum catalyst, 2 parts of ceramic micropowder, 4 parts of tourmaline, 4 parts of butyl titanate and 3 parts of absolute ethyl alcohol are respectively weighed according to parts by weight;
s2, preparation: uniformly stirring and reacting the ceramic micro powder, the tourmaline, the butyl titanate and the absolute ethyl alcohol in the S1 to obtain a solution;
s3, primary stirring: putting the silicone oil in the S1 into a dispersion machine, adding the heat-conducting powder filler and the low-modulus auxiliary agent in batches, and stirring and reacting for 60min at room temperature;
s3, secondary stirring: adding the solution obtained in the step S2 into a dispersion machine in the stirring reaction process in the step S3, stirring for 15min, then adding a high-temperature resistant auxiliary agent and a crosslinking agent, and continuing stirring;
s4, reaction: heating to 105 ℃ under the vacuum protection condition, vacuumizing, stirring, and dispersing for reaction for 60 min;
s5, primary cooling: after the S4 reaction is finished, standing to cool the obtained material to 70 ℃;
s6, vacuum stirring: after cooling, adding a platinum catalyst into the dispersion machine, vacuumizing and stirring for reacting for 35 min;
s7, secondary cooling: after the S6 reaction is finished, standing until the material is cooled to room temperature, and then taking out the prepared high-temperature-resistant low-modulus silicon material.
The low-modulus auxiliary agent in S1 is hydroxy vinyl silicone oil or alkoxy vinyl silicone oil, and the viscosity is 20 cp;
the high-temperature resistant auxiliary agent in S1 is selected from one or more of organic silicon copper complex, organic silicon aluminum complex, organic silicon iron complex and organic silicon zirconium complex;
the silicone oil in S1 is methyl vinyl silicone oil or phenyl vinyl silicone oil, and the heat-conducting powder filler in S1 is one or more selected from aluminum oxide, zinc oxide, boron nitride, silicon carbide, aluminum nitride, graphene, aluminum powder and carbon nano tube powder;
the cross-linking agent in S1 is composed of end hydrogen-containing silicone oil and side hydrogen-containing silicone oil in a mass ratio of 1:1.7, the viscosity is 10cp, the platinum catalyst in S1 is a Kanst platinum catalyst, and the viscosity is 700 cp;
s2, mixing the butyl titanate, the tourmaline, the ceramic micro powder and the absolute ethyl alcohol, and stirring for 7min at the stirring speed of 450 r/min;
the heat-conducting powder filler in S1 has a particle size of 10 μm and a spherical shape.
Example 3
A high-temperature resistant low-modulus silicon material and a preparation method thereof comprise the following steps:
s1: selecting materials: the preparation method comprises the following steps of (1) weighing 20 parts of silicone oil, 40 parts of heat-conducting powder filler, 6 parts of low-modulus auxiliary agent, 3 parts of high-temperature-resistant auxiliary agent, 4 parts of crosslinking agent, 4 parts of platinum catalyst, 3 parts of ceramic micro powder, 5 parts of tourmaline, 5 parts of butyl titanate and 4 parts of absolute ethyl alcohol respectively according to the parts by weight;
s2, preparation: uniformly stirring and reacting the ceramic micro powder, the tourmaline, the butyl titanate and the absolute ethyl alcohol in the S1 to obtain a solution;
s3, primary stirring: putting the silicone oil in the S1 into a dispersion machine, adding the heat-conducting powder filler and the low-modulus auxiliary agent in batches, and stirring and reacting for 80min at room temperature;
s3, secondary stirring: adding the solution obtained in the step S2 into a dispersion machine in the stirring reaction process in the step S3, stirring for 20min, then adding a high-temperature resistant auxiliary agent and a crosslinking agent, and continuing stirring;
s4, reaction: heating to 115 ℃ under the vacuum protection condition, vacuumizing, stirring, and performing dispersion reaction for 80 min;
s5, primary cooling: after the S4 reaction is finished, standing to cool the obtained material to 72 ℃;
s6, vacuum stirring: after cooling, adding a platinum catalyst into the dispersion machine, vacuumizing and stirring for reacting for 40 min;
s7, secondary cooling: after the S6 reaction is finished, standing until the material is cooled to room temperature, and then taking out the prepared high-temperature-resistant low-modulus silicon material.
The low-modulus auxiliary agent in S1 is hydroxy vinyl silicone oil or alkoxy vinyl silicone oil, and the viscosity is 30 cp;
the high-temperature resistant auxiliary agent in S1 is selected from one or more of organic silicon copper complex, organic silicon aluminum complex, organic silicon iron complex and organic silicon zirconium complex;
the silicone oil in S1 is methyl vinyl silicone oil or phenyl vinyl silicone oil, and the heat-conducting powder filler in S1 is one or more selected from aluminum oxide, zinc oxide, boron nitride, silicon carbide, aluminum nitride, graphene, aluminum powder and carbon nano tube powder;
the cross-linking agent in S1 is composed of terminal hydrogen-containing silicone oil and side hydrogen-containing silicone oil in a mass ratio of 1:2, the viscosity is 16cp, the platinum catalyst in S1 is a Kanst platinum catalyst, and the viscosity is 1000 cp;
s2, mixing the butyl titanate, the tourmaline, the ceramic micro powder and the absolute ethyl alcohol, and stirring for 10min at the stirring speed of 500 r/min;
the heat-conducting powder filler in S1 has a particle size of 20 μm and a spherical shape.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (7)
1. A high-temperature resistant low-modulus silicon material and a preparation method thereof are characterized in that: the method comprises the following steps:
s1: selecting materials: the heat-conducting powder coating comprises, by weight, 10-20 parts of silicone oil, 20-40 parts of heat-conducting powder filler, 3-6 parts of low-modulus additive, 1-3 parts of high-temperature-resistant additive, 2-4 parts of crosslinking agent, 2-4 parts of platinum catalyst, 1-3 parts of ceramic micropowder, 2-5 parts of tourmaline, 2-5 parts of butyl titanate and 2-4 parts of absolute ethyl alcohol;
s2, preparation: uniformly stirring and reacting the ceramic micro powder, the tourmaline, the butyl titanate and the absolute ethyl alcohol in the S1 to obtain a solution;
s3, primary stirring: putting the silicone oil in the S1 into a dispersion machine, adding the heat-conducting powder filler and the low-modulus auxiliary agent in batches, and stirring and reacting for 40-80 min at room temperature;
s3, secondary stirring: adding the solution obtained in the step S2 into a dispersion machine in the stirring reaction process in the step S3, stirring for 10-20 min, then adding a high-temperature-resistant auxiliary agent and a crosslinking agent, and continuing stirring;
s4, reaction: heating to 100-115 ℃ under the vacuum protection condition, vacuumizing, stirring and dispersing for 40-80 min;
s5, primary cooling: after the S4 reaction is finished, standing to cool the obtained material to 68-72 ℃;
s6, vacuum stirring: after cooling, adding a platinum catalyst into the dispersion machine, vacuumizing and stirring for reacting for 25-40 min;
s7, secondary cooling: after the S6 reaction is finished, standing until the material is cooled to room temperature, and then taking out the prepared high-temperature-resistant low-modulus silicon material.
2. The high-temperature-resistant low-modulus silicon material and the preparation method thereof according to claim 1 are characterized in that: the low-modulus auxiliary agent in the S1 is hydroxyl vinyl silicone oil or alkoxy vinyl silicone oil, and the viscosity is 1-30 cp.
3. The high-temperature-resistant low-modulus silicon material and the preparation method thereof according to claim 1 are characterized in that: the high-temperature resistant auxiliary agent in S1 is selected from one or more of organic silicon copper complex, organic silicon aluminum complex, organic silicon iron complex and organic silicon zirconium complex.
4. The high-temperature-resistant low-modulus silicon material and the preparation method thereof according to claim 1 are characterized in that: the silicone oil in S1 is methyl vinyl silicone oil or phenyl vinyl silicone oil, and the heat-conducting powder filler in S1 is one or more selected from aluminum oxide, zinc oxide, boron nitride, silicon carbide, aluminum nitride, graphene, aluminum powder and carbon nano tube powder.
5. The high-temperature-resistant low-modulus silicon material and the preparation method thereof according to claim 1 are characterized in that: the cross-linking agent in the S1 is composed of terminal hydrogen-containing silicone oil and side hydrogen-containing silicone oil in a mass ratio of 1: 1.5-2, the viscosity is 1-16 cp, the platinum catalyst in the S1 is a Kanst platinum catalyst, and the viscosity is 300-1000 cp.
6. The high-temperature-resistant low-modulus silicon material and the preparation method thereof according to claim 1 are characterized in that: and in the step S2, the butyl titanate, the tourmaline, the ceramic micro powder and the absolute ethyl alcohol are mixed, and the mixture is stirred for 5-10 min at the stirring speed of 400-500 r/min.
7. The high-temperature-resistant low-modulus silicon material and the preparation method thereof according to claim 1 are characterized in that: the particle size of the heat-conducting powder filler in the S1 is 0.5-20 mu m, and the shape is spherical.
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Application publication date: 20200214 |