CN110982277A - Single-component temperature-resistant heat-conducting silicon mud composition and preparation method thereof - Google Patents
Single-component temperature-resistant heat-conducting silicon mud composition and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a single-component temperature-resistant heat-conducting silicon mud composition and a preparation method thereof, wherein the single-component temperature-resistant heat-conducting silicon mud composition is prepared from the following raw materials in parts by weight: 100 parts of vinyl polysiloxane; 0.5-6 parts of a crosslinking agent; 100-1300 parts of heat-conducting filler; 5-100 parts of a flame-retardant material; 0.1-8 parts of a silane coupling agent; 1-12 parts of a temperature-resistant auxiliary agent; 0.01-0.5 part of inhibitor; 0.1-0.9 parts of platinum catalyst. The single-component temperature-resistant heat-conducting silicon mud composition is addition-type heat-conducting clay with low crosslinking degree, has low volatility and long-term temperature resistance of 230 ℃ without drying compared with general heat-conducting silicone grease and heat-conducting gel, and can be used for heat management of ultrahigh-temperature electronic devices; the high-heat-conductivity flame-retardant material has high heat-conductivity flame-retardant performance, and can be used for heat dissipation of high-power devices and stable operation of the devices.
Description
Technical Field
The invention belongs to the field of organic silicon materials, and particularly relates to a single-component temperature-resistant heat-conducting silicon mud composition and a preparation method thereof.
Background
In recent years, with the rapid growth of the electronic information industry, electronic products rapidly tend to be light-weighted, miniaturized, and high-performance demanding development, and a circuit substrate and an electronic component are required to be mounted at high density, wherein the heat productivity of a high-power module is higher, so that a high-thermal-conductivity interface material is required to assist heat dissipation. The heat-conducting interface materials currently applied to electronic products comprise heat-conducting silicone grease, heat-conducting silicone sheets, double-sided adhesive tapes, heat-conducting adhesive glues, heat-conducting gels and the like, fill gaps between heating modules/devices and heat dissipation assemblies which need to be cooled rapidly, and are in close contact with the heating modules/devices and the heat dissipation assemblies, so that the temperature of the heating modules/devices is reduced rapidly and effectively. Fill among electric pile power, dc-to-ac converter, high frequency inductance, base station power etc. with heat conduction silicone grease and heat conduction gasket most commonly used, in recent years, high power module local temperature constantly rises, rises to 150 ~ 220 ℃ operation from 80 ~ 100 ℃. Under long-term high temperature, the heat-conducting silicone grease as the non-solidified paste material becomes dry after being used for a period of time, the high-temperature stability is greatly reduced, and the heat-conducting interface is easy to loose and loose due to contact, so that the heat-radiating efficiency is reduced. The heat-conducting silica gel sheet heat-conducting interface material has certain hardness, so that the hardness of the heat-conducting silica gel sheet heat-conducting interface material is increased after the heat-conducting silica gel sheet heat-conducting interface material is heated for a long time, the problem of poor interface contact is similar to the problem, and the heat-conducting silica gel sheet heat-conducting interface material is inconvenient to use in a heterogeneous heating device.
The heat-conducting silicon mud is a jelly, is in a state between the heat-conducting silicone grease and the heat-conducting silicone sheet, and is suitable for heat dissipation of electronic component modules with high integration level and large heat productivity. The application conditions of the heat-conducting daub in the current market are different, and the heat tracing for the pipeline is mainly carried out. Patent ZL00125756.0 'single-component organic heat-conducting daub' belongs to epoxy resin systems and is mainly used in heat tracing systems of transportation pipelines; patent CN106085252A "A Heat conduction daub and its preparation method and application" discloses a heat conduction daub and its preparation method, the base material contains high temperature resistant inorganic glue, it is a non-addition organosilicon system, the heat conduction daub that the invention provides is high in intensity, high temperature resistant, used in heat tracing pipeline and apparatus, do not involve the heat dissipation used for electronic product; patent CN107043541A "heat-conducting silicone gel composition and preparation method thereof" discloses a heat-conducting silicone gel composition and preparation method thereof, relating to selection of basic polymer, modification of heat-conducting material, low-crosslinking degree gel, and application in heat dissipation filling of electronic and electric appliances, not mentioned about its temperature resistance. With the development of miniaturization of electronic equipment, the heat productivity of a high-power module (5G base station assembly) is obviously increased, higher requirements are put on heat conduction materials, and the high-power module can keep stable performance at a high temperature of 200-230 ℃, so that the requirements of products can be met.
Disclosure of Invention
The invention aims to provide a single-component temperature-resistant heat-conducting silicon mud composition which can maintain good performance in a long-term temperature change environment, particularly a high-temperature environment, so that electronic devices can be effectively protected.
In order to achieve the technical effects, the invention adopts the following technical scheme:
the single-component temperature-resistant heat-conducting silicon mud composition is characterized by being prepared from the following raw materials in parts by weight:
100 parts of vinyl polysiloxane;
0.5-6 parts of a crosslinking agent;
100-1300 parts of heat-conducting filler;
5-100 parts of a flame-retardant material;
0.1-8 parts of a silane coupling agent;
1-12 parts of a temperature-resistant auxiliary agent;
0.01-0.5 parts of an inhibitor;
0.1-0.9 parts of platinum catalyst.
The vinyl polysiloxane adopted by the single-component temperature-resistant heat-conducting silicon mud composition is vinyl-terminated polydimethylsiloxane or vinyl-terminated polymethylphenyl siloxane or a mixture of the vinyl-terminated polydimethylsiloxane and the vinyl-terminated polymethylphenyl siloxane, and the viscosity of the vinyl-terminated polydimethylsiloxane or vinyl-terminated polymethylphenyl siloxane is 100-1000 mPa & s.
The cross-linking agent adopted by the single-component temperature-resistant heat-conducting silicon mud composition is as follows:
Me2HSiO(MeHSiO)m(MeRSiO)nSiHMe2wherein R is CH3Or phenyl, wherein m is 2 to 10, n is 1 to 55, and the hydrogen content is 0.05 to 0.3%.
The heat-conducting filler adopted by the single-component temperature-resistant heat-conducting silicon mud composition is one or more of silicon micropowder, aluminum powder, aluminum oxide, zinc oxide, magnesium oxide, aluminum nitride, boron nitride and silicon nitride, and the particle size of the heat-conducting filler is 20 nm-45 mu m.
The flame retardant material adopted by the single-component temperature-resistant heat-conducting silicon mud composition is at least one or more of aluminum hydroxide, magnesium hydroxide, organic montmorillonite, flaky mica powder, zinc borate and a modified nitrogen-phosphorus flame retardant.
The silane coupling agent adopted by the single-component temperature-resistant heat-conducting silicon mud composition is one or more of dodecyl trimethoxy silane, hexadecyl trimethoxy silane, gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane and vinyl triethoxy silane.
The molecular formula of the temperature-resistant auxiliary agent adopted by the single-component temperature-resistant heat-conducting silicon mud composition is as follows:
The inhibitor adopted by the single-component temperature-resistant heat-conducting silicon mud composition is at least one of tetramethyl tetravinylcyclotetrasiloxane, methyl butynol and ethynyl cyclohexanol.
The platinum catalyst adopted by the single-component temperature-resistant heat-conducting silicon mud composition is a complex of tetramethyl divinyl disiloxane and platinum, and the platinum content is 500-3000 ppm.
The invention also provides a preparation method of the single-component temperature-resistant heat-conducting silicon mud composition, which comprises the following steps:
(1) drying 100-1300 parts by weight of heat-conducting filler and 5-100 parts by weight of flame retardant material at a high temperature of 110-130 ℃ for 1-3 h, transferring into a high-speed mixer for mixing, and spraying 0.1-8 parts by weight of silane coupling agent for modification treatment for 1-2 h to obtain mixed powder;
(2) adding 100 parts by weight of vinyl polysiloxane into the mixed powder, kneading, and dehydrating at 100-130 ℃ for 1-2 hours to obtain a base material;
(3) and sequentially adding 1-12 parts by weight of temperature-resistant auxiliary agent, 0.5-6 parts by weight of cross-linking agent, 0.01-0.5 part by weight of inhibitor and 0.1-0.9 part by weight of catalyst into the base material, and uniformly stirring to obtain the heat-conducting silicon mud composition.
The technical solution of the present invention is further explained below.
In the invention, the vinyl polysiloxane can be selected from vinyl-terminated polydimethylsiloxane, vinyl-terminated polymethylphenylsiloxane or a mixture of the vinyl-terminated polydimethylsiloxane and the vinyl-terminated polymethylphenylsiloxane, and the viscosity of the vinyl polysiloxane is 100-1000 mPa & s. The vinyl polysiloxane is preferably vinyl-terminated polymethylphenylsiloxane or vinyl-terminated polydimethylsiloxane having a viscosity of 100 to 500 mPas. The viscosity of the vinyl polysiloxane has certain influence on the consistency and the extrudability of the heat-conducting silicon mud.
The molecular formula of the crosslinking agent is: me2HSiO(MeHSiO)m(MeRSiO)nSiHMe2Wherein R is CH3Or phenyl, wherein m is 2 to 10, n is 1 to 55, and the hydrogen content is 0.05 to 0.3%. The crosslinking agent is preferably R is CH3Or phenyl, wherein m is 2 to 6, n is 10 to 40, and the hydrogen content is 0.05 to 0.2%. In the present invention, the crosslinking agent is a terminal-side hydrogen-containing silicone oil, and the hydrogen content is preferably not too large, and is preferably less than 0.2%, and if the hydrogen content is more than 0.3%, the crosslinking points are too many, and the silicone oil is cured into an elastomer, and the requirement of the heat-conductive silicone paste having a low crosslinking density cannot be satisfied.
The heat-conducting filler is one or more of silicon micropowder, aluminum powder, aluminum oxide, zinc oxide, magnesium oxide, aluminum nitride, boron nitride and silicon nitride, and the particle size of the heat-conducting filler is 20 nm-45 mu m. Preferably, the heat conducting filler is a composite powder of aluminum oxide, zinc oxide, boron nitride and aluminum nitride, and the particle size of the heat conducting filler is 0.1-30 μm. In the invention, a plurality of heat-conducting fillers are compounded, and fillers with different particle sizes are compounded for use, so that a more effective heat-conducting passage can be formed and the heat-conducting efficiency can be improved.
The flame retardant material is at least one or more of aluminum hydroxide, magnesium hydroxide, organic montmorillonite, flaky mica powder, zinc borate and modified nitrogen-phosphorus flame retardant. Preferably, the flame retardant material is one or two of aluminum hydroxide and a modified nitrogen-phosphorus flame retardant.
The silane coupling agent is one or more of dodecyl trimethoxy silane, hexadecyl trimethoxy silane, gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane and vinyl triethoxy silane. Preferably, the silane coupling agent is a compound of hexadecyl trimethoxy silane and gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane, and the compound mass ratio is 2: 1. According to the invention, the silane coupling agent can improve the extrudability of the heat-conducting silicon mud composition, can improve the compatibility of the heat-conducting filler and the heat-conducting silicon mud composition, and simultaneously reduces the hydroxyl amount on the surface of the heat-conducting powder, thereby being beneficial to improving the temperature resistance.
The molecular formula of the temperature-resistant auxiliary agent is as follows:
The inhibitor is at least one of tetramethyl tetravinylcyclotetrasiloxane, methylbutynol and ethynyl cyclohexanol. Preferably, the inhibitor is one of tetramethyltetravinylcyclotetrasiloxane and methylbutinol. In the present invention, the inhibitor is used to prevent local reaction in the heat conductive silicon mud composition from being too high, so that uniformity and overall stability thereof are maintained.
The platinum catalyst is a complex of tetramethyldivinyldisiloxane and platinum, and the platinum content is 500-3000 ppm. The preferred platinum content is 500 to 2500 ppm.
According to a preferred embodiment of the present invention, the preparation method of the single-component temperature-resistant heat-conductive silicon mud composition can adopt the following steps:
(1) drying 100-1300 parts by weight of heat-conducting filler and 5-100 parts by weight of flame retardant material at a high temperature of 110-120 ℃ for 1-2 h, transferring into a high-speed mixer for mixing, and spraying 0.1-8 parts by weight of silane coupling agent into the mixture for modification treatment for 1-2 h to obtain mixed powder;
(2) adding 100 parts by weight of vinyl polysiloxane into the mixed powder, kneading, and dehydrating at 110-130 ℃ for 1-2 hours to obtain a base material;
(3) adding 1-12 parts by weight of temperature-resistant assistant, 0.5-6 parts by weight of cross-linking agent, 0.01-0.5 part by weight of inhibitor and 0.1-0.9 part by weight of catalyst into the base material in sequence, stirring for 1-2 hours, and carrying out low cross-linking curing at normal temperature or at high temperature of 50-80 ℃ for 30-60 min to obtain the heat-conducting silicon mud composition. And packaging the heat-conducting silicon mud composition in a plastic tube or a dispensing cylinder for later use.
Compared with the prior art, the invention has at least the following beneficial effects:
the single-component temperature-resistant heat-conducting silicon mud composition is addition-type heat-conducting clay with low crosslinking degree, a self-synthesized temperature-resistant auxiliary agent is used for chain extension to a main chain of vinyl polysiloxane, and the temperature resistance of the single-component temperature-resistant heat-conducting silicon mud composition is improved under the synergistic effect of phenyl, fluorine-containing groups, phenylboron groups and the like. Compared with the general heat-conducting silicone grease, the silicone grease has low volatility and can resist the temperature of 230 ℃ for a long time without drying, and can be used for the heat management of ultra-high temperature electronic devices; compared with the general bi-component heat-conducting gel, the gel is a single-component package, is very convenient to use and can be used repeatedly.
The single-component temperature-resistant heat-conducting silicon mud composition has high heat-conducting flame-retardant performance, can be used for heat dissipation of high-power devices, and protects stable operation of the devices.
Detailed Description
The invention will be further elucidated and described with reference to the embodiments of the invention described hereinafter. It should be noted that by adjusting the viscosity of the vinyl polysiloxane (for example, by compounding two different viscosities), the type and amount of the heat-conducting filler, the amount of the flame-retardant material, the temperature-resistant auxiliary agent, and the cross-linking agents with different hydrogen contents, the heat-conducting silicon mud composition with different comprehensive properties of high temperature resistance, heat conductivity coefficient, flame retardance, and extrudability can be obtained.
The specific performance test method is as follows:
consistency: testing according to the method specified in GB-T1749;
extrudability: testing was carried out according to the method specified in GB/T13477.3, using a 6mm tip;
coefficient of thermal conductivity: testing according to the method specified in ISO 22007;
flame retardant rating: testing according to a method specified in GB/T2408;
volatile components: the test was carried out according to the HG/T2502 test at a temperature of 230 ℃ for 500 h.
Synthesis of hydrogen-containing silicone oil (crosslinking agent) on end side
A metered amount of tetramethylcyclotetrasiloxane (D) was added to a three-necked flask equipped with a stirrer, reflux condenser and thermometer4 H) Mixing octamethylcyclotetrasiloxane (D4)/tetramethyltetraphenylcyclotetrasiloxane, tetramethyldihydro-disiloxane and pretreated cation exchange resin, carrying out equilibrium reaction at 70-80 ℃ for several hours, filtering, reducing the pressure to-0.09 Mpa, heating to 150-160 ℃, and removing low-boiling-point substances to obtain the end-side hydrogen-containing silicone oil, wherein the contents are shown in Table 1.
TABLE 1 several hydrogen-containing silicone oils on the end side
Synthesis of temperature-resistant auxiliary agent
Wherein m is 1-15, n is 5-35, preferably m is 3-12, n is 10-30, the heat-resisting auxiliary agent is abbreviated as Me2HSiO(CF3C2H4MeSiO)m(Me2SiO)nOB(Ph)O(CF3C2H4MeSiO)m(Me2SiO)nSiHMe2。
Adding metered phenylboronic acid, fluorine-containing end hydrogen-containing silicone oil and Karstedt catalyst into a three-neck flask provided with a stirrer, a reflux condenser tube and a thermometer, mixing, reacting at 70-80 ℃ for several hours, filtering, reducing the pressure to-0.09 Mpa, heating to 150-160 ℃, and removing low-boiling-point substances to obtain modified fluorine-containing end hydrogen-containing silicone oil containing phenyl boron, wherein the modified fluorine-containing end hydrogen-containing silicone oil containing phenyl boron is shown in Table 2.
TABLE 2 modified fluorine-containing terminal hydrogen-containing silicone oils containing benzene and boron
Built silane coupling agent
The compound silane coupling agent is a compound of hexadecyl trimethoxy silane and gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane, and the compound mass ratio is 2: 1.
Example 1
800 parts by mass of alumina having an average particle size of 10 μm, 80 parts by mass of zinc oxide having an average particle size of 0.2 μm, 40 parts by mass of boron nitride having an average particle size of 25 μm, and 60 parts by mass of aluminum hydroxide were dried at a high temperature of 110 ℃ for 1 hour, and then transferred to a high-speed mixer to be mixed, and 5 parts by mass of dodecyltrimethoxysilane was sprayed thereto to carry out modification treatment for 1 hour, thereby obtaining a mixed powder.
50 parts by mass of vinyl-terminated polydimethylsiloxane having a viscosity of 100 mPas, 50 parts by mass of vinyl-terminated polymethylphenylsiloxane having a viscosity of 500 mPas, and kneading the mixed powder, and dehydrating the kneaded powder at a high temperature of 115 ℃ for 1 hour to obtain a base material.
Adding 3 parts by mass of a temperature-resistant assistant No. 1 in the table 2, 2.5 parts by mass of a cross-linking agent No. 1 in the table 1, 0.2 part by mass of a tetramethyltetravinylcyclotetrasiloxane inhibitor and 0.5 part by mass of a complex of tetramethyldivinyldisiloxane and platinum with the concentration of 2500ppm into a base material in sequence, stirring for 1h, and carrying out low-crosslinking curing at normal temperature for 60min to obtain the heat-conducting silicon mud composition. The results of the performance test are shown in Table 3.
Example 2
750 parts by mass of alumina with the average particle size of 8 microns, 50 parts by mass of zinc oxide with the average particle size of 0.2 microns, 50 parts by mass of aluminum nitride with the average particle size of 15 microns and 20 parts by mass of modified nitrogen-phosphorus flame retardant are dried for 1.5 hours at the high temperature, transferred into a high-speed mixer for mixing, and sprayed with 6 parts by mass of compounded silane coupling agent for modification treatment for 1 hour to obtain mixed powder.
50 parts by mass of terminal vinyl polymethylphenylsiloxane having a viscosity of 100 mPas, 50 parts by mass of terminal vinyl polymethylphenylsiloxane having a viscosity of 500 mPas, and kneading the mixed powder, and dehydrating the kneaded powder at a high temperature of 115 ℃ for 1 hour to obtain the base material.
Adding 4 parts by mass of a temperature-resistant assistant No. 2 in the table 2,3 parts by mass of a cross-linking agent No. 2 in the table 1, 0.15 part by mass of a tetramethyltetravinylcyclotetrasiloxane inhibitor and 0.6 part by mass of a platinum-vinylsiloxane complex with the concentration of 2000ppm into a base material in sequence, stirring for 1h, and carrying out low-crosslinking curing at normal temperature for 60min to obtain the heat-conducting silicon mud composition. The results of the performance test are shown in Table 3.
Example 3
1000 parts by mass of alumina with the average particle size of 6.5 microns, 50 parts by mass of zinc oxide with the average particle size of 0.2 microns and 30 parts by mass of modified nitrogen-phosphorus flame retardant are dried for 1 hour at the high temperature of 110 ℃, then are mixed in a high-speed mixer, and then 6 parts by mass of compounded silane coupling agent is sprayed in for modification treatment for 1.5 hours, thus obtaining mixed powder.
70 parts by mass of terminal vinyl polydimethylsiloxane having a viscosity of 100 mPas, 30 parts by mass of terminal vinyl polydimethylsiloxane having a viscosity of 500 mPas, and kneading the mixed powder, and dehydrating the kneaded powder at a high temperature of 115 ℃ for 1 hour to obtain the base material.
6 parts by mass of a temperature-resistant assistant No. 3 in the table 2, 4 parts by mass of a crosslinking agent No. 3 in the table 1, 0.3 part by mass of a tetramethyltetravinylcyclotetrasiloxane inhibitor and 0.7 part by mass of a complex of tetramethyldivinyldisiloxane and platinum with the concentration of 1500ppm are sequentially added into the base material, stirred for 1 hour, and subjected to low crosslinking and curing at 60 ℃ for 30 minutes to obtain the heat-conducting silicon mud composition. The results of the performance test are shown in Table 3.
Example 4
900 parts by mass of alumina with the average particle size of 8 mu m, 30 parts by mass of zinc oxide with the average particle size of 0.2 mu m, 150 parts by mass of aluminum nitride with the average particle size of 12 mu m and 20 parts by mass of modified nitrogen-phosphorus flame retardant are dried at the high temperature of 110 ℃ for 1.5h, are transferred to a high-speed mixer for mixing, and are sprayed with 8 parts by mass of compounded silane coupling agent for modification treatment for 1.5h, so that mixed powder is obtained.
80 parts by mass of terminal vinyl polymethylphenylsiloxane having a viscosity of 100 mPas, 20 parts by mass of terminal vinyl polymethylphenylsiloxane having a viscosity of 500 mPas, and kneading the mixed powder, and dehydrating the kneaded powder at a high temperature of 115 ℃ for 1.5 hours to obtain the base material.
Adding 7 parts by mass of a temperature-resistant assistant No. 4 in the table 2, 4.5 parts by mass of a cross-linking agent No. 4 in the table 1, 0.2 part by mass of a tetramethyltetravinylcyclotetrasiloxane inhibitor and 0.8 part by mass of a complex of tetramethyldivinyldisiloxane and platinum with the concentration of 1000ppm into the base material in sequence, stirring for 1h, and carrying out low-crosslinking curing at 80 ℃ for 30min to obtain the heat-conducting silicon mud composition. The results of the performance test are shown in Table 3.
Comparative example 1:
750 parts by mass of alumina with the average particle size of 8 microns, 50 parts by mass of zinc oxide with the average particle size of 0.2 microns, 50 parts by mass of aluminum nitride with the average particle size of 15 microns and 20 parts by mass of modified nitrogen-phosphorus flame retardant are dried for 1.5 hours at the high temperature, transferred into a high-speed mixer for mixing, and sprayed with 6 parts by mass of compounded silane coupling agent for modification treatment for 1 hour to obtain mixed powder.
50 parts by mass of a vinyl-terminated polydimethylsiloxane having a viscosity of 100 mPas, 50 parts by mass of a vinyl-terminated polymethylphenylsiloxane having a viscosity of 500 mPas, and kneading the mixed powder, and dehydrating the kneaded powder at a high temperature of 115 ℃ for 1.5 hours to obtain a base material.
3 parts by mass of a crosslinking agent No. 2 with a structural formula shown in Table 1, 0.15 part by mass of a tetramethyltetravinylcyclotetrasiloxane inhibitor and 0.6 part by mass of a complex of tetramethyldivinyldisiloxane and platinum with a concentration of 2000ppm are sequentially added into the base material, stirred for 1 hour, and subjected to low-crosslinking curing at normal temperature for 60 minutes to obtain the heat-conducting silicon mud composition. The results of the performance test are shown in Table 3.
TABLE 3 Properties of the examples and comparative examples
As can be seen from Table 3, the heat-conducting silicon mud compositions of examples 1 to 4 and the comparative example are white jelly, and the heat-conducting silicon mud compositions with different comprehensive properties can be obtained by adjusting the proportion and the dosage of the components, wherein the volatile components are all lower than 0.50%, the consistency is 8.9-9.4 cm, the extrudability is 98-131 mL/min, and the heat conductivity is 2.3-3.3W/(m.K). The consistency of the comparative heat-conducting silicon mud which does not use the temperature-resistant additive is reduced from 8.9cm to 5.1cm after being treated for 500 hours at 230 ℃, and the consistency is dried, which indicates that the comparative heat-conducting silicon mud does not resist high temperature; the heat-conducting silicon muds of the examples 1 to 4 using the temperature-resistant additive have small consistency change after being processed at a high temperature of 230 ℃ for 500 hours, are not dried, and have lower volatile content than the comparative example, so that the heat-conducting silicon muds can provide stable heat-conducting and heat-dissipating performance and ensure the long-term stable operation of electronic devices.
Although the invention has been described herein with reference to illustrative embodiments thereof, it should be understood that numerous other modifications and embodiments can be devised by those skilled in the art that will fall within the spirit and scope of the principles of this disclosure.
Claims (10)
1. The single-component temperature-resistant heat-conducting silicon mud composition is characterized by being prepared from the following raw materials in parts by weight:
100 parts of vinyl polysiloxane;
0.5-6 parts of a crosslinking agent;
100-1300 parts of heat-conducting filler;
5-100 parts of a flame-retardant material;
0.1-8 parts of a silane coupling agent;
1-12 parts of a temperature-resistant auxiliary agent;
0.01-0.5 parts of an inhibitor;
0.1-0.9 parts of platinum catalyst.
2. The single-component temperature-resistant heat-conducting silicon mud composition according to claim 1, wherein the vinyl polysiloxane is vinyl-terminated polydimethylsiloxane or vinyl-terminated polymethylphenylsiloxane or a mixture of the vinyl-terminated polydimethylsiloxane and the vinyl-terminated polymethylphenylsiloxane, and the viscosity of the vinyl-terminated polydimethylsiloxane or the mixture of the vinyl-terminated polymethylphenylsiloxane is 100-1000 mPa-s.
3. The single-component temperature-resistant heat-conductive silicon mud composition according to claim 1, wherein the cross-linking agent is: me2HSiO(MeHSiO)m(MeRSiO)nSiHMe2Wherein R is CH3Or phenyl, wherein m is 2 to 10, n is 1 to 55, and the hydrogen content is 0.05 to 0.3%.
4. The single-component temperature-resistant heat-conducting silicon mud composition according to claim 1, wherein the heat-conducting filler is one or more of silicon micropowder, aluminum powder, aluminum oxide, zinc oxide, magnesium oxide, aluminum nitride, boron nitride and silicon nitride, and the particle size of the heat-conducting filler is 20 nm-45 μm.
5. The single-component temperature-resistant heat-conducting silicon mud composition according to claim 1, wherein the flame retardant material is at least one or more of aluminum hydroxide, magnesium hydroxide, organic montmorillonite, flaky mica powder, zinc borate and a modified nitrogen-phosphorus flame retardant.
6. The one-component temperature-resistant heat-conductive silicon mud composition according to claim 1, wherein the silane coupling agent is one or more of dodecyl trimethoxy silane, hexadecyl trimethoxy silane, gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane and vinyl triethoxy silane.
7. The single-component temperature-resistant heat-conducting silicon mud composition according to claim 1, wherein the temperature-resistant auxiliary agent has a molecular formula:
8. The one-component temperature-resistant thermal conductive silicon paste composition according to claim 1, wherein the inhibitor is at least one of tetramethyltetravinylcyclotetrasiloxane, methylbutynol, and ethynylcyclohexanol.
9. The single-component temperature-resistant heat-conducting silicon mud composition according to claim 1, wherein the platinum catalyst is a complex of tetramethyldivinyldisiloxane and platinum, and the platinum content is 500-3000 ppm.
10. The preparation method of the single-component temperature-resistant heat-conductive silicon mud composition of any one of claims 1 to 9, which is characterized by comprising the following steps: (1) drying 100-1300 parts by weight of heat-conducting filler and 5-100 parts by weight of flame retardant material at a high temperature of 110-130 ℃ for 1-3 h, transferring into a high-speed mixer for mixing, and spraying 0.1-8 parts by weight of silane coupling agent for modification treatment for 1-2 h to obtain mixed powder;
(2) adding 100 parts by weight of vinyl polysiloxane into the mixed powder, kneading, and dehydrating at 100-130 ℃ for 1-2 hours to obtain a base material;
(3) and sequentially adding 1-12 parts by weight of temperature-resistant auxiliary agent, 0.5-6 parts by weight of cross-linking agent, 0.01-0.5 part by weight of inhibitor and 0.1-0.9 part by weight of catalyst into the base material, and uniformly stirring to obtain the heat-conducting silicon mud composition.
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