CN111363368A - Fluid-like high-thermal-conductivity organic silicon gel and preparation method and application thereof - Google Patents

Fluid-like high-thermal-conductivity organic silicon gel and preparation method and application thereof Download PDF

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CN111363368A
CN111363368A CN202010278850.3A CN202010278850A CN111363368A CN 111363368 A CN111363368 A CN 111363368A CN 202010278850 A CN202010278850 A CN 202010278850A CN 111363368 A CN111363368 A CN 111363368A
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曾亮
齐放
刘洋
柯攀
戴小平
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Hunan Guoxin Semiconductor Technology Co ltd
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    • C08L83/00Compositions 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
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Abstract

The invention discloses a fluid high-thermal-conductivity organic silicon gel and a preparation method and application thereof. The preparation method comprises the steps of respectively preparing the A/B components, and further mixing the A/B components to prepare the fluid high-thermal-conductivity organic silicon gel. The fluid high-thermal-conductivity organic silicon gel has the advantages of high thermal conductivity, low viscosity and the like, can remarkably improve the heat dissipation performance of power electronic devices, can also be suitable for encapsulation of the power electronic devices, and has high use value and good application prospect. The preparation method has the advantages of simple process, convenient operation, easily obtained raw materials, low requirement on equipment and the like, can realize large-scale preparation, is suitable for industrial production, and is favorable for popularization and application of the high-thermal-conductivity organic silicon gel material.

Description

Fluid-like high-thermal-conductivity organic silicon gel and preparation method and application thereof
Technical Field
The invention belongs to the field of electronic packaging materials, particularly relates to a two-component high-thermal-conductivity organic silicon gel for power electronic devices, and particularly relates to a fluid high-thermal-conductivity organic silicon gel as well as a preparation method and application thereof.
Background
The silicone gel is essentially a composition of linear organopolysiloxane, including organohydrogenpolysiloxane containing silicon-bonded hydrogen atoms (Si — H), and organopolysiloxane having double bonds (e.g., bonded vinyl groups). Due to the special structure, the composite material has many excellent properties such as better heat resistance, weather resistance, cold resistance, electric insulation performance and the like, and has lower elastic modulus and ultralow stress; the good elasticity has small stress on chips, bonding wires or wire frames in the power electronic devices, is widely applied to packaging protection of the power electronic devices, and is accepted by most power electronic device manufacturers.
Many common faults of power electronic devices are caused by heat, and if heat generated by the power electronic devices cannot be quickly and effectively transferred out, local temperature rise of the devices is large, which has a great influence on the reliability and stability of the devices. Therefore, the packaging material with higher heat conductivity is used for transferring generated heat as soon as possible, and is the most effective means for reducing the temperature rise of the device. The organic silicon gel is used as a high polymer material, has low heat conductivity coefficient, mainly plays a role in insulation protection, basically cannot play a role in heat conduction, and improves the temperature rise of a device to a certain extent. Therefore, it is a problem to be solved at present to improve the thermal conductivity of the silicone gel as much as possible while ensuring good insulation, high elasticity and low stress.
In order to increase the thermal conductivity of silicone gels, researchers have proposed various strategies, but the increase in thermal conductivity in these strategies not only results in an increase in the cost of the silicone gel, but also results in an increase in the viscosity of the silicone gel; meanwhile, the high viscosity of the organic silicon gel can cause the uneven mixing of the organic silicon gel, the tiny gaps are difficult to fill, and the use efficiency of the organic silicon gel in the application process can not be improved. At present, although researchers pay attention to the importance of low-viscosity and high-thermal-conductivity interface materials, the problem of overlarge viscosity still exists in the existing low-viscosity and high-thermal-conductivity interface materials, and the actual requirements cannot be met, for example, when the organic silicon gel is used for encapsulating power electronic devices, if the viscosity is too high, the organic silicon gel is colloidal or pasty, and the organic silicon gel is very unfavorable for permeating the power electronic devices, so that defects are formed in the devices; meanwhile, the materials have the problems of complex components, high cost and the like, which greatly limits the application of power electronic devices. In fact, the heat conduction of the silicone gel is completely realized by the high heat conduction filler, the heat conductivity coefficient of the resin is very low, so that a large amount of the high heat conduction filler is required to be added for improving the heat conductivity of the silicone gel, but the viscosity is improved by adding the high heat conduction filler in a large amount, so that the high heat conduction and the low viscosity are contradictory. In fact, in order to obtain a silicone gel having both high thermal conductivity and low viscosity, it is necessary to select and treat a filler, and both the average diameter and the surface condition of the filler need to be considered, so that it is necessary to select a good balance point by comprehensively considering the influence of each factor, and it is difficult to achieve the silicone gel having both high thermal conductivity and low viscosity in a technical aspect by blindly pursuing. Therefore, the fluid high-thermal-conductivity organic silicon gel with high thermal conductivity and low viscosity is obtained, and has very important significance for prolonging the service life of power electronic devices and improving the application range of the power electronic devices.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a fluid high-thermal-conductivity organic silicon gel with high thermal conductivity and low viscosity, and a preparation method and application thereof.
In order to solve the technical problems, the invention adopts the technical scheme that:
a fluid high-thermal-conductivity silicone gel comprises a component A and a component B;
the component A comprises the following raw material components in parts by weight:
40-160 parts of vinyl silicone oil;
0.01-1 part of catalyst;
5-35 parts of modified nano filler;
the component B comprises the following raw material components in parts by weight:
Figure BDA0002445791320000021
the modified nano filler is prepared by modifying a nano filler by a coupling agent containing vinyl.
The fluid high-thermal-conductivity organic silicon gel is further improved, and the mass ratio of the component A to the component B is 0.3-0.5: 1.
In the fluid high-thermal-conductivity silicone gel, the structural formula of the vinyl silicone oil is further improved as follows:
Figure BDA0002445791320000022
wherein R is1Is at least one of methyl, phenyl and ethoxy, and a is an integer of 150-1000.
In the fluid silicone gel with high thermal conductivity, the catalyst is platinum (0) -1, 3-divinyl tetramethyl disiloxane complex; the mass percentage of platinum in the platinum (0) -1, 3-divinyl tetramethyl disiloxane complex is 0.3% -2%.
The fluid high-thermal-conductivity organic silicon gel is further improved, and the structural formula of the chain extender is as follows:
Figure BDA0002445791320000023
wherein R is2Is at least one of methyl, phenyl and ethoxy, and b is an integer of 10 to 100.
In the fluid silicone gel with high thermal conductivity, the structural formula of the cross-linking agent is as follows:
Figure BDA0002445791320000031
wherein R is3Is at least one of methyl, phenyl and ethoxy, and c is an integer of 50-100.
In the fluid high-thermal-conductivity silicone gel, the modified nano filler is further improved by the following method: mixing a coupling agent containing vinyl and a mixed solution of isopropanol/toluene to obtain a modified diluent, adding the modified diluent into the nano filler under the stirring condition, heating to 110-130 ℃, continuously stirring for 3-5 h, removing the solvent, and drying to obtain the modified nano filler.
The fluid high-thermal-conductivity organic silicon gel is further improved, wherein the weight ratio of the nano filler to the modified diluent is 4-10: 1; the stirring speed is 500 r/min-1500 r/min;
the coupling agent containing vinyl is a mixture of KH310 and KH 570; the weight ratio of the KH310 to the KH570 is 0.1-1: 1; the weight ratio of the isopropanol to the toluene in the isopropanol/toluene mixed solution is 0.1-0.3: 1; the mass percentage content of the modifier in the modified diluent is 20-50%;
the nano filler is a mixture of nano boron nitride and nano aluminum oxide; the weight ratio of the nano boron nitride to the nano aluminum oxide is 0.1-0.5: 1; the average grain diameter of the nanometer boron nitride is 50 nm-80 nm; the average grain diameter of the nano alumina is 80nm to 150 nm; before use, the nano filler is dried for 3 to 10 hours at the temperature of between 100 and 110 ℃.
As a general technical concept, the present invention also provides a preparation method of the fluid-like high thermal conductive silicone gel, comprising the following steps:
s1, mixing vinyl silicone oil and a catalyst, adding the modified nano filler, ultrasonically dispersing for 15-30 min, grinding and dispersing for 30-60 min, and removing impurities and bubbles to obtain a component A; sequentially adding a chain extender, a cross-linking agent and 1-ethynylcyclohexanol into vinyl silicone oil, adding a modified nano filler, ultrasonically dispersing for 15-30 min, grinding and dispersing for 30-60 min, and removing impurities and bubbles to obtain a component B;
and S2, mixing the component A and the component B obtained in the step S1, removing bubbles, and vulcanizing to obtain the fluid high-thermal-conductivity organic silicon gel.
As a general technical concept, the invention also provides application of the fluid-shaped high thermal conductive silicone gel or the fluid-shaped high thermal conductive silicone gel prepared by the preparation method in power electronic devices.
Compared with the prior art, the invention has the advantages that:
(1) the invention provides a fluid high-thermal-conductivity organic silicon gel which comprises a component A and a component B, wherein the component A is vinyl silicone oil, a catalyst and a modified nano filler, and the component B is vinyl silicone oil, a chain extender, a cross-linking agent, 1-ethynyl cyclohexanol and the modified nano filler. According to the invention, the modified nano filler is prepared by modifying the nano filler by a coupling agent containing vinyl, long-chain-segment alkyl is introduced on the surface of the nano filler through modification, so that more effective organic coating on the surface of the nano filler is realized, and simultaneously, active vinyl is introduced on the surface of the nano filler, so that the nano filler can participate in addition reaction with vinyl silicone oil and a cross-linking agent, the compatibility of the nano filler and organic silicon gel can be greatly improved, and the reduction of the viscosity of the organic silicon gel is facilitated; meanwhile, the modified nano filler can be uniformly distributed in the organic silicon gel as the high-thermal-conductivity nano filler, so that the high-thermal-conductivity nano filler forms an effective thermal-conductivity channel in the organic silicon gel, the thermal conductivity of the organic silicon gel is greatly improved, and the viscosity can be effectively reduced on the premise of ensuring the high thermal conductivity. The fluid high-heat-conductivity organic silicon gel has the advantages of high heat conductivity, low viscosity and the like, can obviously improve the heat dissipation performance of power electronic devices (such as high-power semiconductor modules), has very important significance for improving the service life and the reliability of the power electronic devices, can be suitable for encapsulation of the power electronic devices, further expands the application range on the premise of ensuring better encapsulation efficiency, and has very high use value and very good application prospect.
(2) In the fluid-shaped high-thermal-conductivity organic silicon gel, the vinyl silicone oil containing direct connection, the cross-linking agent and the chain extender are adopted, the original good insulativity, high elasticity and low stress of the organic silicon gel are kept, and meanwhile, side chain groups in the adopted silicone oil such as the vinyl silicone oil, the cross-linking agent and the chain extender contain hydrogen groups (-H), so that a certain proportion of hydrogen bonds can be formed after the organic silicon gel is cured, and the silicone gel is endowed with good rebound resilience and good self-repairability, so that the fluid-shaped high-thermal-conductivity organic silicon gel keeps the advantages of the organic silicon gel such as high elasticity, low stress, high insulativity, self-repairability and the like. In addition, the vinyl silicone oil, the cross-linking agent and the chain extender adopted in the invention have lower viscosity, which ensures that the fluid high-thermal-conductivity organic silicon gel has lower viscosity.
(3) The invention also provides a preparation method of the fluid high-thermal-conductivity organic silicon gel, which comprises the steps of preparing the component A from the vinyl silicone oil, the catalyst and the modified nano filler, preparing the component B from the vinyl silicone oil, the chain extender, the cross-linking agent, the 1-ethynyl cyclohexanol and the modified nano filler, and mixing the component A/B to prepare the fluid high-thermal-conductivity organic silicon gel. In the preparation method, the vulcanization time is reasonably adjusted by utilizing the synergistic effect of the catalyst and the 1-ethynylcyclohexanol, so that a fluid high-thermal-conductivity organic silicon gel with high thermal conductivity, high elasticity, low stress and low viscosity is obtained by balancing the interaction and compounding of all components, the A/B components are respectively prepared, and the two components can be combined and mixed when needed, so that the storage time of the fluid high-thermal-conductivity organic silicon gel can be prolonged; meanwhile, the preparation method has the advantages of simple process, convenient operation, easily obtained raw materials, low requirement on equipment and the like, can realize large-scale preparation, is suitable for industrial production, and is favorable for popularization and application of the high-thermal-conductivity organic silicon gel material.
Detailed Description
The invention is further described below with reference to specific preferred embodiments, without thereby limiting the scope of protection of the invention.
The materials and equipment used in the following examples are commercially available. In the examples of the present invention, unless otherwise specified, the processes used were conventional processes, the equipment used were conventional equipment, and the data obtained were average values of three or more experiments.
Example 1
A fluid high heat conduction organic silicon gel comprises a component A and a component B, wherein the mass ratio of the component A to the component B is 0.3: 1;
the component A comprises the following raw material components in parts by weight:
40 parts of vinyl silicone oil;
0.01 part of catalyst;
5 parts of modified nano filler;
the component B comprises the following raw material components in parts by weight:
Figure BDA0002445791320000051
in this example, the structural formula of the vinyl silicone oil is as follows:
Figure BDA0002445791320000052
wherein the vinyl silicone oil has a purity of 99% and a specific gravity of 0.96g/cm3Of ethyleneThe content of the base was 6.5% by mass, and the viscosity was 2100 mPas.
In this example, the catalyst was a platinum (0) -1, 3-divinyltetramethyldisiloxane complex, and the mass percentage of platinum was 0.3%.
In this example, the structural formula of the chain extender is as follows:
Figure BDA0002445791320000053
wherein the purity of the chain extender is 99 percent, and the specific gravity is 0.96g/cm3The hydrogen content was 0.5% by mass, and the viscosity was 80 mPas.
In this example, the structural formula of the crosslinker is as follows:
Figure BDA0002445791320000054
wherein the purity of the crosslinking agent is 99%, and the specific gravity is 0.96g/cm3The hydrogen content was 0.6% by mass, and the viscosity was 60 mPas.
In this embodiment, the modified nano-filler is prepared by modifying a nano-filler with a coupling agent containing vinyl, and specifically includes: modifying the mixture of nano boron nitride and nano aluminum oxide by using the mixture of KH310 and KH570, comprising the following steps:
(1) drying the nano filler in a drying oven at 100 ℃ for 3h, wherein the nano filler is a mixture of nano boron nitride and nano aluminum oxide; the weight ratio of the nano boron nitride to the nano aluminum oxide is 0.1: 1; the average grain diameter of the nano boron nitride is 50 nm; the average grain diameter of the nano-alumina is 80 nm.
(2) Mixing a coupling agent containing vinyl and a mixed solution of isopropanol/toluene to obtain a modified diluent, wherein the coupling agent containing vinyl is a mixture of KH310 and KH 570; the weight ratio of KH310 to KH570 is 0.1: 1; the weight ratio of the isopropanol to the toluene in the isopropanol/toluene mixed solution is 0.1: 1; the mass percentage of the modifier in the modified diluent is 20 percent.
(3) And (2) pouring the dried nano filler in the step (1) into a high-speed mixer, slowly adding the modified diluent in the step (2) in a stirring state, uniformly mixing, heating to 110 ℃, stirring for 3 hours, evaporating the solvent, and drying in a drying oven at 100 ℃ for 3 hours to obtain the modified nano filler, wherein the weight ratio of the nano filler to the modified diluent is 4: 1, and the rotating speed of the mixer is 500 r/min.
A method for preparing the fluid-like silicone gel with high thermal conductivity in the embodiment includes the following steps:
s1, uniformly mixing 40 parts by mass of vinyl silicone oil and 0.01 part by mass of catalyst, adding 5 parts by mass of modified nano filler, ultrasonically dispersing for 15min, grinding and dispersing for 30min, and removing impurities and bubbles to obtain a component A; and sequentially adding 40 parts by mass of vinyl silicone oil, 10 parts by mass of chain extender, 5 parts by mass of cross-linking agent and 0.01 part by mass of 1-ethynylcyclohexanol, uniformly mixing, adding 10 parts by mass of modified nano-filler, ultrasonically dispersing for 15min, grinding and dispersing for 60min, and removing impurities and bubbles to obtain the component B.
And S2, mixing the component A and the component B obtained in the step S1, removing bubbles, and vulcanizing to obtain the fluid high-thermal-conductivity organic silicon gel.
An application of the fluid-shaped high thermal conductive silicone gel prepared in the embodiment in a power electronic device is specifically to use the fluid-shaped high thermal conductive silicone gel for packaging protection of the power electronic device.
Example 2
A fluid high heat conduction organic silicon gel comprises a component A and a component B, wherein the mass ratio of the component A to the component B is 0.5: 1;
the component A comprises the following raw material components in parts by weight:
160 parts of vinyl silicone oil;
1 part of a catalyst;
35 parts of modified nano filler;
the component B comprises the following raw material components in parts by weight:
Figure BDA0002445791320000061
Figure BDA0002445791320000071
in this example, the structural formula of the vinyl silicone oil is as follows:
Figure BDA0002445791320000072
wherein the vinyl silicone oil has a purity of 99% and a specific gravity of 0.96g/cm3The vinyl content was 4.5% by weight, and the viscosity was 2200 mPas.
In this example, the catalyst was a platinum (0) -1, 3-divinyltetramethyldisiloxane complex, and the mass percentage of platinum was 2%.
In this example, the structural formula of the chain extender is as follows:
Figure BDA0002445791320000073
wherein the purity of the chain extender is 99 percent, and the specific gravity is 0.96g/cm3The hydrogen content was 0.6% by mass, and the viscosity was 80 mPas.
In this example, the structural formula of the crosslinker is as follows:
Figure BDA0002445791320000074
wherein the purity of the crosslinking agent is 99%, and the specific gravity is 0.96g/cm3The hydrogen content was 0.5% by mass, and the viscosity was 65 mPas.
In this embodiment, the modified nano-filler is prepared by modifying a nano-filler with a coupling agent containing vinyl, and specifically includes: modifying the mixture of nano boron nitride and nano aluminum oxide by using the mixture of KH310 and KH570, comprising the following steps:
(1) drying the nano filler in a drying oven at 110 ℃ for 10h, wherein the nano filler is a mixture of nano boron nitride and nano aluminum oxide; the weight ratio of the nano boron nitride to the nano aluminum oxide is 0.5: 1; the average grain diameter of the nano boron nitride is 80 nm; the average grain diameter of the nano alumina is 150 nm.
(2) Mixing a coupling agent containing vinyl and a mixed solution of isopropanol/toluene to obtain a modified diluent, wherein the coupling agent containing vinyl is a mixture of KH310 and KH 570; the weight ratio of KH310 to KH570 is 1: 1; the weight ratio of the isopropanol to the toluene in the isopropanol/toluene mixed solution is 0.3: 1; the mass percentage of the modifier in the modified diluent is 50 percent.
(3) And (2) pouring the dried nano filler in the step (1) into a high-speed mixer, slowly adding the modified diluent in the step (2) in a stirring state, uniformly mixing, heating to 130 ℃, stirring for 5 hours, evaporating the solvent, and drying in a drying oven at 110 ℃ for 10 hours to obtain the modified nano filler, wherein the weight ratio of the nano filler to the modified diluent is 10: 1, and the rotating speed of the mixer is 1500 r/min.
A method for preparing the fluid-like silicone gel with high thermal conductivity in the embodiment includes the following steps:
s1, mixing 160 parts by mass of vinyl silicone oil and 1 part by mass of catalyst uniformly, adding 35 parts by mass of modified nano filler, performing ultrasonic dispersion for 30min, performing grinding dispersion for 60min, and removing impurities and bubbles to obtain a component A; and sequentially adding 180 parts by mass of vinyl silicone oil, 35 parts by mass of chain extender, 15 parts by mass of cross-linking agent and 1 part by mass of 1-ethynylcyclohexanol, uniformly mixing, adding 40 parts by mass of modified nano filler, performing ultrasonic dispersion for 30min, performing grinding dispersion for 60min, and removing impurities and bubbles to obtain a component B.
And S2, mixing the component A and the component B obtained in the step S1, removing bubbles, and vulcanizing to obtain the fluid high-thermal-conductivity organic silicon gel.
An application of the fluid-shaped high thermal conductive silicone gel prepared in the embodiment in a power electronic device is specifically to use the fluid-shaped high thermal conductive silicone gel for packaging protection of the power electronic device.
Example 3
A fluid high heat conduction organic silicon gel comprises a component A and a component B, wherein the mass ratio of the component A to the component B is 2: 5;
the component A comprises the following raw material components in parts by weight:
100 parts of vinyl silicone oil;
0.5 part of a catalyst;
20 parts of modified nano filler;
the component B comprises the following raw material components in parts by weight:
Figure BDA0002445791320000081
in this example, the structural formula of the vinyl silicone oil is as follows:
Figure BDA0002445791320000091
wherein the vinyl silicone oil has a purity of 99% and a specific gravity of 0.96g/cm3The vinyl content was 8.0% by weight, and the viscosity was 2000 mPas.
In this example, the catalyst was a platinum (0) -1, 3-divinyltetramethyldisiloxane complex, and the mass percentage of platinum was 1%.
In this example, the structural formula of the chain extender is as follows:
Figure BDA0002445791320000092
wherein the purity of the chain extender is 99 percent, and the specific gravity is 0.96g/cm3The hydrogen content was 0.6% by mass, and the viscosity was 90 mPas.
In this example, the structural formula of the crosslinker is as follows:
Figure BDA0002445791320000093
wherein the purity of the crosslinking agent is 99%, and the specific gravity is 0.96g/cm3The hydrogen content was 0.7% by mass, and the viscosity was 60 mPas.
In this embodiment, the modified nano-filler is prepared by modifying a nano-filler with a coupling agent containing vinyl, and specifically includes: modifying the mixture of nano boron nitride and nano aluminum oxide by using the mixture of KH310 and KH570, comprising the following steps:
(1) drying the nano filler in a drying box at 105 ℃ for 5 hours, wherein the nano filler is a mixture of nano boron nitride and nano aluminum oxide; the weight ratio of the nano boron nitride to the nano aluminum oxide is 2: 5; the average grain diameter of the nano boron nitride is 60 nm; the average grain diameter of the nano alumina is 120 nm.
(2) Mixing a coupling agent containing vinyl and a mixed solution of isopropanol/toluene to obtain a modified diluent, wherein the coupling agent containing vinyl is a mixture of KH310 and KH 570; the weight ratio of KH310 to KH570 is 1: 2; the weight ratio of the isopropanol to the toluene in the isopropanol/toluene mixed solution is 1: 5; the mass percentage of the modifier in the modified diluent is 35%.
(3) And (2) pouring the dried nano filler in the step (1) into a high-speed mixer, slowly adding the modified diluent in the step (2) in a stirring state, uniformly mixing, heating to 120 ℃, stirring for 4 hours, evaporating the solvent, and drying in a drying oven at 105 ℃ for 6 hours to obtain the modified nano filler, wherein the weight ratio of the nano filler to the modified diluent is 7: 1, and the rotating speed of the mixer is 1000 r/min.
A method for preparing the fluid-like silicone gel with high thermal conductivity in the embodiment includes the following steps:
s1, uniformly mixing 100 parts by mass of vinyl silicone oil and 0.5 part by mass of catalyst, adding 20 parts by mass of modified nano filler, ultrasonically dispersing for 20min, grinding and dispersing for 40min, and removing impurities and bubbles to obtain a component A; sequentially adding 110 parts by mass of vinyl silicone oil, 20 parts by mass of chain extender, 10 parts by mass of cross-linking agent and 0.8 part by mass of 1-ethynylcyclohexanol, uniformly mixing, adding 25 parts by mass of modified nano-filler, ultrasonically dispersing for 25min, grinding and dispersing for 40min, and removing impurities and bubbles to obtain a component B.
And S2, mixing the component A and the component B obtained in the step S1, removing bubbles, and vulcanizing to obtain the fluid high-thermal-conductivity organic silicon gel.
An application of the fluid-shaped high thermal conductive silicone gel prepared in the embodiment in a power electronic device is specifically to use the fluid-shaped high thermal conductive silicone gel for packaging protection of the power electronic device.
Comparative example 1
A silicone gel substantially the same as example 1 except that: the modified nano filler was used in an amount of 3 parts by weight in the component a of comparative example 1.
Comparative example 2
A silicone gel substantially the same as example 2 except that: the modified nano filler was used in an amount of 50 parts by weight in the B component of comparative example 2.
Comparative example 3
A silicone gel substantially the same as example 3 except that: in comparative example 1, the modified nano filler in example 2 is replaced by the unmodified nano filler, wherein the unmodified nano filler adopted in comparative example 1 is a composition of nano boron nitride and nano alumina; the weight ratio of the nano boron nitride to the nano aluminum oxide is 0.5: 1; the average grain diameter of the nano boron nitride is 80 nm; the average grain diameter of the nano alumina is 150 nm.
The performance of the fluid-like highly thermally conductive silicone gels prepared in examples 1 to 3 and the silicone gels prepared in comparative examples 1 to 3 were tested, and the results are shown in table 1 below.
TABLE 1 Performance test results for different Silicone gels
Figure BDA0002445791320000101
Figure BDA0002445791320000111
As shown in table 1, under different treatment conditions, the thermal conductivity of the fluid-like high thermal conductivity silicone gels prepared in examples 1 to 3 of the present invention all reach higher values, substantially reaching 3.0W/(m · K) or more, which indicates that the silicone gels prepared by the present invention have excellent thermal conductivity, and the mechanical properties (penetration and elastic modulus) and the insulating properties (electrical strength) are not much different from those of the non-high thermal conductivity silicone gels, indicating that the silicone gels prepared by the present invention have the advantages of high elasticity, low stress and high insulating property of the silicone gels. More importantly, the viscosity of the organic silicon gel prepared by the invention is lower than 4000mPa & s, and the organic silicon gel is fluid organic silicon gel; the viscosity of the existing high-thermal-conductivity organic silicon gel is as high as more than 120 Pa.s, and the existing high-thermal-conductivity organic silicon gel is pasty organic silicon gel. In addition, compared with the data of the comparative example, it can be found that the more the modified nano heat-conducting filler is added, the better the modified nano heat-conducting filler is, because the cone penetration is reduced and the shape is embodied as a paste after a certain addition amount is reached; after the addition of unmodified nanofillers, the silicone gel is also in the form of a paste, but the thermal conductivity is not high, probably due to the inability of the fillers to form effective thermal conduction channels due to agglomeration. Therefore, the fluid high-thermal-conductivity organic silicon gel has the advantages of high thermal conductivity, high elasticity, low stress, low viscosity and the like, can obviously improve the heat dissipation performance of power electronic devices (such as high-power semiconductor modules), has very important significance for improving the service life and the reliability of the power electronic devices, can be suitable for encapsulation of the power electronic devices, further expands the application range on the premise of ensuring better encapsulation efficiency, and has high use value and good application prospect.
The above examples are merely preferred embodiments of the present invention, and the scope of the present invention is not limited to the above examples. All technical schemes belonging to the idea of the invention belong to the protection scope of the invention. It should be noted that modifications and embellishments within the scope of the invention may be made by those skilled in the art without departing from the principle of the invention, and such modifications and embellishments should also be considered as within the scope of the invention.

Claims (10)

1. A fluid high-thermal-conductivity organic silicon gel is characterized by comprising a component A and a component B;
the component A comprises the following raw material components in parts by weight:
40-160 parts of vinyl silicone oil;
0.01-1 part of catalyst;
5-35 parts of modified nano filler;
the component B comprises the following raw material components in parts by weight:
Figure FDA0002445791310000011
the modified nano filler is prepared by modifying a nano filler by a coupling agent containing vinyl.
2. The fluid-like high thermal conductive silicone gel according to claim 1, wherein the mass ratio of the component A to the component B is 0.3-0.5: 1.
3. The fluid-like highly thermally conductive silicone gel according to claim 1 or 2, characterized in that the structural formula of the vinyl silicone oil is as follows:
Figure FDA0002445791310000012
wherein R is1Is at least one of methyl, phenyl and ethoxy, and a is an integer of 150-1000.
4. The fluid-like highly thermally conductive silicone gel according to claim 1 or 2, characterized in that the catalyst is a platinum (0) -1, 3-divinyltetramethyldisiloxane complex; the mass percentage of platinum in the platinum (0) -1, 3-divinyl tetramethyl disiloxane complex is 0.3% -2%.
5. The fluid-like highly thermally conductive silicone gel according to claim 1 or 2, characterized in that the structural formula of the chain extender is as follows:
Figure FDA0002445791310000013
wherein R is2Is at least one of methyl, phenyl and ethoxy, and b is an integer of 10 to 100.
6. The fluid-like highly thermally conductive silicone gel according to claim 1 or 2, characterized in that the structural general formula of the crosslinking agent is as follows:
Figure FDA0002445791310000021
wherein R is3Is at least one of methyl, phenyl and ethoxy, and c is an integer of 50-100.
7. The fluid-like highly thermally conductive silicone gel according to claim 1 or 2, characterized in that the modified nanofiller is prepared by the following method: mixing a coupling agent containing vinyl and a mixed solution of isopropanol/toluene to obtain a modified diluent, adding the modified diluent into the nano filler under the stirring condition, heating to 110-130 ℃, continuously stirring for 3-5 h, removing the solvent, and drying to obtain the modified nano filler.
8. The fluid-like high thermal conductivity silicone gel according to claim 7, wherein the weight ratio of the nanofiller to the modified diluent is 4-10: 1; the stirring speed is 500 r/min-1500 r/min;
the coupling agent containing vinyl is a mixture of KH310 and KH 570; the weight ratio of the KH310 to the KH570 is 0.1-1: 1; the weight ratio of the isopropanol to the toluene in the isopropanol/toluene mixed solution is 0.1-0.3: 1; the mass percentage content of the modifier in the modified diluent is 20-50%;
the nano filler is a mixture of nano boron nitride and nano aluminum oxide; the weight ratio of the nano boron nitride to the nano aluminum oxide is 0.1-0.5: 1; the average grain diameter of the nanometer boron nitride is 50 nm-80 nm; the average grain diameter of the nano alumina is 80nm to 150 nm; before use, the nano filler is dried for 3 to 10 hours at the temperature of between 100 and 110 ℃.
9. A method for preparing the fluid-like high thermal conductivity silicone gel according to any one of claims 1 to 8, characterized by comprising the following steps:
s1, mixing vinyl silicone oil and a catalyst, adding the modified nano filler, ultrasonically dispersing for 15-30 min, grinding and dispersing for 30-60 min, and removing impurities and bubbles to obtain a component A; sequentially adding a chain extender, a cross-linking agent and 1-ethynylcyclohexanol into vinyl silicone oil, adding a modified nano filler, ultrasonically dispersing for 15-30 min, grinding and dispersing for 30-60 min, and removing impurities and bubbles to obtain a component B;
and S2, mixing the component A and the component B obtained in the step S1, removing bubbles, and vulcanizing to obtain the fluid high-thermal-conductivity organic silicon gel.
10. Use of the fluid-like high thermal conductive silicone gel according to any one of claims 1 to 8 or the fluid-like high thermal conductive silicone gel prepared by the preparation method according to claim 9 in power electronic devices.
CN202010278850.3A 2020-04-10 2020-04-10 Fluid-like high-thermal-conductivity organic silicon gel and preparation method and application thereof Pending CN111363368A (en)

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