CN116751559A - High-temperature-resistant high-reliability organic silicon heat-conducting pouring sealant for inverter and preparation method thereof - Google Patents

High-temperature-resistant high-reliability organic silicon heat-conducting pouring sealant for inverter and preparation method thereof Download PDF

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CN116751559A
CN116751559A CN202310650423.7A CN202310650423A CN116751559A CN 116751559 A CN116751559 A CN 116751559A CN 202310650423 A CN202310650423 A CN 202310650423A CN 116751559 A CN116751559 A CN 116751559A
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carbon fiber
heat
parts
conducting
silicone oil
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谢荣
郑柚田
陈如琴
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Shenzhen Shengkangtai Organosilicon Material Co ltd
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Shenzhen Shengkangtai Organosilicon Material Co ltd
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J183/00Adhesives based on 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; Adhesives based on derivatives of such polymers
    • C09J183/04Polysiloxanes
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02Non-macromolecular additives
    • C09J11/04Non-macromolecular additives inorganic
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00Properties
    • C08L2201/08Stabilised against heat, light or radiation or oxydation
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2203/00Applications
    • C08L2203/20Applications use in electrical or conductive gadgets
    • C08L2203/206Applications use in electrical or conductive gadgets use in coating or encapsulating of electronic parts

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  • Organic Chemistry (AREA)
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Abstract

The application relates to the technical field of electronic potting materials, and particularly discloses a high-temperature-resistant high-reliability organic silicon heat-conducting potting adhesive for an inverter and a preparation method thereof, wherein the potting adhesive consists of a component A and a component B in a mass ratio of (0.8-1.2): 1; the component A comprises the following raw materials in parts by weight: 30-50 parts of a heat conducting filler; 15-25 parts of modified heat-conducting carbon fiber; 10-40 parts of vinyl silicone oil; 0.2-2 parts of methyl silicone oil; 0.1-0.5 part of platinum catalyst; the component B comprises the following raw materials in parts by weight: 30-50 parts of a heat conducting filler; 15-25 parts of modified heat-conducting carbon fiber; 10-40 parts of vinyl silicone oil; 6-10 parts of hydrogen-containing silicone oil; 0.2-2 parts of methyl silicone oil; 0.1-0.5 part of crosslinking inhibitor. The application has the advantages of improving the mechanical property, heat resistance and heat conductivity of the pouring sealant.

Description

High-temperature-resistant high-reliability organic silicon heat-conducting pouring sealant for inverter and preparation method thereof
Technical Field
The application relates to the technical field of electronic potting materials, in particular to a high-temperature-resistant high-reliability organic silicon heat-conducting potting adhesive for an inverter and a preparation method thereof.
Background
With the rapid development of microelectronic integration technology, electronic components and instruments are increasingly used in the electronics industry. In order to ensure stability and reliability of electronic devices, the electronic devices have the performances of shock resistance, vibration resistance, severe environment resistance, electric insulation, heat conduction and the like, and often need to be encapsulated and protected. The pouring sealant is widely applied to various electronic components and plays roles of bonding, sealing, pouring and coating protection. The pouring sealant is liquid before reaction, has good fluidity, can be used for pouring various products and is easy to fill gaps, and a protective layer is formed on the surface of an electronic component after reaction and solidification, so that the pouring sealant has the functions of water resistance, moisture resistance, dust resistance, insulation, heat conduction, confidentiality, corrosion resistance, temperature resistance and vibration resistance. The organic silicon pouring sealant has the characteristics of good high and low temperature resistance, good insulativity and small viscosity, and is favored in the fields of LED encapsulation, motor encapsulation, sealing protection and the like at present.
According to the material types, pouring sealants are divided into three main categories: epoxy resin pouring sealant, organic silicon resin pouring sealant and polyurethane pouring sealant, and different types of pouring sealants have respective advantages and disadvantages. The organic silicon pouring sealant has the advantages of good high and low temperature resistance, good insulativity and small viscosity, but has poor thermal conductivity, and in the related art, the thermal conductivity of the material is generally improved by adding thermal conductive fillers such as aluminum oxide, aluminum nitride and the like.
Aiming at the related technology, the addition amount of the heat-conducting filler in the organic silicon pouring sealant is too small, and the heat conduction of the material is not obviously improved; the addition amount of the heat-conducting filler in the organic silicon pouring sealant is too much, so that the organic silicon pouring sealant is increased in adhesiveness and is unfavorable for pouring, and the filler is easy to agglomerate, so that the mechanical property of the material is poor.
Disclosure of Invention
In order to improve the heat conductivity and mechanical property of the organic silicon pouring sealant at the same time, the application provides the high-temperature-resistant high-reliability inverter organic silicon heat conduction pouring sealant and the preparation method thereof.
In a first aspect, the application provides a high-temperature-resistant high-reliability organic silicon heat-conducting pouring sealant for an inverter, which adopts the following technical scheme:
the high-temperature-resistant high-reliability inverter organosilicon heat-conducting pouring sealant consists of a component A and a component B in a mass ratio of (0.8-1.2) to 1;
the component A comprises the following raw materials in parts by weight:
30-50 parts of a heat conducting filler;
15-25 parts of modified heat-conducting carbon fiber;
10-40 parts of vinyl silicone oil;
0.2-2 parts of methyl silicone oil;
0.1-0.5 part of platinum catalyst;
the component B comprises the following raw materials in parts by weight:
30-50 parts of a heat conducting filler;
15-25 parts of modified heat-conducting carbon fiber;
10-40 parts of vinyl silicone oil;
6-10 parts of hydrogen-containing silicone oil;
0.2-2 parts of methyl silicone oil;
0.1-0.5 part of crosslinking inhibitor;
the preparation method of the modified heat-conducting carbon fiber comprises the following steps:
pretreating, namely soaking the carbon fiber in a sodium persulfate aqueous solution, performing ultrasonic treatment, performing solid-liquid separation, washing with water, and drying to obtain pretreated carbon fiber;
coating, namely preparing silicon dioxide sol, soaking the pretreated carbon fiber in the silicon dioxide sol, uniformly mixing, filtering and drying to obtain coated carbon fiber;
and (3) carrying out plasma treatment, namely adding the coated carbon fiber into a silane coupling agent solution, uniformly mixing, removing the solvent, drying, and carrying out plasma treatment to obtain the modified heat-conducting carbon fiber.
By adopting the technical scheme, the carbon fiber has the characteristics of high temperature resistance, friction resistance, corrosion resistance and the like, the carbon fiber has higher axial heat conductivity coefficient along the carbon fiber, but has lower radial heat conductivity coefficient along the carbon fiber, and the carbon fiber is directly added into the organic silicon pouring sealant to improve the mechanical property, but reduce the heat conductivity coefficient of the pouring sealant; according to the application, the carbon fiber is soaked in the sodium persulfate aqueous solution, the ultrasonic treatment can promote the chemical oxidation of ammonium persulfate, so that the surface of the carbon fiber is etched and peeled, the oxygen-containing functional groups such as hydroxyl groups and the like on the surface of the carbon fiber are increased, the specific surface area is increased, and the surface of the carbon fiber is changed from hydrophobicity to hydrophilicity; the silica sol forms a silica layer after being solidified on the surface of the carbon fiber, the bonding strength of the silica sol and the carbon fiber is high, the heat conductivity coefficient of the silica is far higher than that of the carbon fiber, the defect of low heat conductivity coefficient of the carbon fiber can be improved, and the defect that the silica filler is easy to agglomerate when directly added is overcome; because a large number of hydrophilic hydroxyl groups exist on the surface of the silicon dioxide layer, the silane coupling agent is adsorbed on the surface of the silicon dioxide layer, and a layer of thinner polymer film is formed on the surface of the silicon dioxide layer by the silane coupling agent during plasma treatment, the aggregation between fillers can be prevented, the compatibility with organic polymers can be increased, impurities adsorbed on the surface of the silicon dioxide layer can be effectively removed, active groups are introduced, interaction between the active groups and the polymers can occur, even chemical bonds can be generated, so that modified heat-conducting carbon fibers are uniformly dispersed in the material, a three-dimensional network structure is formed in the material by the modified heat-conducting carbon fibers, and a heat-conducting passage can be formed when the modified heat-conducting carbon fibers are contacted with each other, so that the mechanical property of the material can be improved, and the heat-conducting property of the material can be improved. Because the carbon fiber and the silicon dioxide layer have high temperature resistance, the high temperature resistance of the material can be improved.
Optionally, the mass concentration of the sodium persulfate aqueous solution is 15-25g/L.
By adopting the technical scheme, the mass concentration of the sodium persulfate aqueous solution is too low, and the oxidation speed is too slow; the mass concentration of the sodium persulfate aqueous solution is too high, which may cause excessive etching and reduce the mechanical properties of the carbon fiber.
Alternatively, the mass of carbon fiber added per 1L of the ammonium persulfate aqueous solution is 20 to 25g.
By adopting the technical scheme, the addition amount of the carbon fiber is too small, so that the waste of ammonium persulfate can be caused; the addition of the carbon fiber is too large, which results in small contact area between the carbon fiber and the ammonium persulfate aqueous solution and insufficient oxidation.
Optionally, the power of the ultrasonic treatment is 350-400W, and the ultrasonic time is 10-15min.
By adopting the technical scheme, excessive etching can be caused by too high ultrasonic power; the ultrasonic power is too small and the etching speed is too slow.
Optionally, the silane coupling agent is selected from any one of gamma-aminopropyl triethoxysilane, gamma- (2, 3-epoxypropoxy) propyl trimethoxysilane, vinyl trimethoxysilane and hexadecyl trimethoxysilane.
By adopting the technical scheme, the silane coupling agent can form a polymer film on the surface of the silicon dioxide layer, reduce the probability of agglomeration and enhance the binding force between the silicon dioxide layer and the polymer.
Optionally, the mass ratio of the coated carbon fiber to the silane coupling agent is 100: (2-4).
By adopting the technical scheme, the silane coupling agent is too little to form a polymer film; too much silane coupling agent can cause waste.
Optionally, the discharge power density during the plasma treatment is 0.2-0.4W/cm, and the treatment time is 4-10min.
By adopting the technical scheme, under the conditions of the discharge power density and the discharge time, the silane coupling agent can be promoted to polymerize into a film, impurities on the surface of the silicon dioxide layer are removed, and active groups are introduced on the surface of the silicon dioxide layer.
In a second aspect, the application provides a preparation method of a high-temperature-resistant high-reliability organic silicon heat-conducting pouring sealant for an inverter, which adopts the following technical scheme:
a preparation method of high-temperature-resistant high-reliability inverter organosilicon heat-conducting pouring sealant comprises the following steps:
step one, mixing, heating and stirring a heat conduction filler, vinyl silicone oil and methyl silicone oil, cooling to below 50 ℃, adding modified heat conduction carbon fiber and a platinum catalyst, and uniformly stirring to obtain a component A;
mixing, heating and stirring the heat-conducting filler, vinyl silicone oil and methyl silicone oil, cooling to below 50 ℃, adding modified heat-conducting carbon fiber and a crosslinking inhibitor for first stirring, and then adding hydrogen-containing silicone oil for second stirring to obtain a component B;
and thirdly, uniformly mixing the component A and the component B, and carrying out vacuum defoaming to obtain the organic silicon heat-conducting pouring sealant.
By adopting the technical scheme, the modified heat-conducting carbon fibers are uniformly dispersed in the material, a three-dimensional net structure is formed in the material, and a heat-conducting passage can be formed when the modified heat-conducting carbon fibers are contacted with each other, so that the mechanical property of the material can be improved, and the heat-conducting property of the material can be improved.
In summary, the application has the following beneficial effects:
1. because the modified heat-conducting carbon fibers are added, the modified heat-conducting carbon fibers are uniformly dispersed in the material, a three-dimensional net structure is formed in the material, and heat-conducting passages can be formed when the modified heat-conducting carbon fibers are contacted with each other, so that the mechanical property of the material and the heat-conducting property of the material can be improved.
2. Because the carbon fiber and the silicon dioxide layer have high temperature resistance, the high temperature resistance of the material can be improved.
Detailed Description
The present application will be described in further detail with reference to examples.
Preparation example of modified heat-conducting carbon fiber
Preparation example 1
The preparation method of the modified heat-conducting carbon fiber comprises the following steps:
pretreating, namely immersing carbon fibers with the length of 1-2mm in a sodium persulfate aqueous solution with the mass concentration of 15g/L, wherein the mass of the carbon fibers added into each 1L of ammonium persulfate aqueous solution is 20g, performing ultrasonic treatment, the power of the ultrasonic treatment is 350W, the ultrasonic time is 15min, the ultrasonic frequency is 40KHz, filtering, flushing with distilled water to pH of 7, and drying to obtain pretreated carbon fibers;
coating treatment, namely preparing silica sol: according to the mol ratio of ethyl orthosilicate to ethanol to water, namely hydrochloric acid=1:6.4:3.8:0.085, fully mixing the ethyl orthosilicate with absolute ethanol, dropwise adding a mixture of deionized water and nitric acid under strong stirring of a magnetic stirrer, stirring and refluxing the reaction mixture at 70 ℃ for 3 hours after the dropwise adding is finished, adding 30% V/V of N, N-dimethylformamide as a drying control chemical additive after the sol is cooled, and continuously stirring for 15 minutes to obtain silica sol; soaking the pretreated carbon fiber in silicon dioxide sol, uniformly stirring, filtering and drying to obtain coated carbon fiber;
the preparation method comprises the steps of performing plasma treatment, namely adding coated carbon fibers into an ethanol water solution of a silane coupling agent, wherein the ethanol volume fraction in the ethanol water solution is 85%, the silane coupling agent is gamma-aminopropyl triethoxysilane, and the mass ratio of the coated carbon fibers to the silane coupling agent is 100:2, removing the solvent after uniformly mixing, drying, performing plasma treatment, wherein the discharge power density during the plasma treatment is 0.2W/cm, and the treatment time is 10min, so as to obtain the modified heat-conducting carbon fiber.
Preparation example 2
The preparation method of the modified heat-conducting carbon fiber comprises the following steps:
pretreating, namely immersing carbon fibers with the length of 1-2mm in a sodium persulfate aqueous solution with the mass concentration of 15g/L, wherein the mass of the carbon fibers added into each 1L of ammonium persulfate aqueous solution is 22g, carrying out ultrasonic treatment, the power of ultrasonic treatment is 380W, the ultrasonic time is 12min, the ultrasonic frequency is 40KHz, filtering, flushing with distilled water to pH of 7, and drying to obtain pretreated carbon fibers;
coating treatment, namely preparing silica sol: according to the mol ratio of ethyl orthosilicate to ethanol to water, namely hydrochloric acid=1:6.4:3.8:0.085, fully mixing the ethyl orthosilicate with absolute ethanol, dropwise adding a mixture of deionized water and nitric acid under strong stirring of a magnetic stirrer, stirring and refluxing the reaction mixture at 70 ℃ for 3 hours after the dropwise adding is finished, adding 30% V/V of N, N-dimethylformamide as a drying control chemical additive after the sol is cooled, and continuously stirring for 15 minutes to obtain silica sol; soaking the pretreated carbon fiber in silicon dioxide sol, uniformly stirring, filtering and drying to obtain coated carbon fiber;
the preparation method comprises the steps of performing plasma treatment, adding coated carbon fibers into an ethanol water solution of a silane coupling agent, wherein the ethanol volume fraction in the ethanol water solution is 85%, the silane coupling agent is gamma- (2, 3-glycidoxy) propyl trimethoxy silane, and the mass ratio of the coated carbon fibers to the silane coupling agent is 100: and 3, removing the solvent after uniformly mixing, drying, performing plasma treatment, wherein the discharge power density during the plasma treatment is 0.2W/cm, and the treatment time is 10min, so as to obtain the modified heat-conducting carbon fiber.
Preparation example 3
The preparation method of the modified heat-conducting carbon fiber comprises the following steps:
pretreating, namely immersing carbon fibers with the length of 1-2mm in a sodium persulfate aqueous solution with the mass concentration of 15g/L, wherein the mass of the carbon fibers added into each 1L of ammonium persulfate aqueous solution is 25g, performing ultrasonic treatment with the power of 400W, the ultrasonic time of 10min and the ultrasonic frequency of 40KHz, filtering, flushing with distilled water to pH of 7, and drying to obtain pretreated carbon fibers;
coating treatment, namely preparing silica sol: according to the mol ratio of ethyl orthosilicate to ethanol to water, namely hydrochloric acid=1:6.4:3.8:0.085, fully mixing the ethyl orthosilicate with absolute ethanol, dropwise adding a mixture of deionized water and nitric acid under strong stirring of a magnetic stirrer, stirring and refluxing the reaction mixture at 70 ℃ for 3 hours after the dropwise adding is finished, adding 30% V/V of N, N-dimethylformamide as a drying control chemical additive after the sol is cooled, and continuously stirring for 15 minutes to obtain silica sol; soaking the pretreated carbon fiber in silicon dioxide sol, uniformly stirring, filtering and drying to obtain coated carbon fiber;
the preparation method comprises the steps of performing plasma treatment, namely adding coated carbon fibers into an ethanol water solution of a silane coupling agent, wherein the ethanol volume fraction in the ethanol water solution is 85%, the silane coupling agent is hexadecyl trimethoxy silane, and the mass ratio of the coated carbon fibers to the silane coupling agent is 100: and 4, removing the solvent after uniformly mixing, drying, performing plasma treatment, wherein the discharge power density during the plasma treatment is 0.2W/cm, and the treatment time is 10min, so as to obtain the modified heat-conducting carbon fiber.
Preparation example 4
The difference from preparation example 2 was that the mass concentration of the sodium persulfate aqueous solution was 10g/L.
Preparation example 5
The difference from preparation example 2 was that the mass concentration of the sodium persulfate aqueous solution was 20g/L.
Preparation example 6
The difference from preparation example 2 was that the mass concentration of the sodium persulfate aqueous solution was 25g/L.
Preparation example 7
The difference from preparation example 2 was that the mass concentration of the sodium persulfate aqueous solution was 35g/L.
Preparation example 8
The difference from preparation example 5 is that the discharge power density at the time of plasma treatment was 0.1W/cm.
Preparation example 9
The difference from preparation example 5 is that the discharge power density at the time of plasma treatment was 0.3W/cm.
Preparation example 10
The difference from preparation example 5 is that the discharge power density at the time of plasma treatment was 0.4W/cm.
PREPARATION EXAMPLE 11
The difference from preparation example 5 is that the discharge power density at the time of plasma treatment was 0.6W/cm.
Comparative preparation example 1
The preparation method of the modified heat-conducting carbon fiber comprises the following steps:
pretreating, namely immersing carbon fibers with the length of 1-2mm in a sodium persulfate aqueous solution with the mass concentration of 15g/L, wherein the mass of the carbon fibers added into each 1L of ammonium persulfate aqueous solution is 22g, carrying out ultrasonic treatment, the power of ultrasonic treatment is 380W, the ultrasonic time is 12min, the ultrasonic frequency is 40KHz, filtering, flushing with distilled water to pH of 7, and drying to obtain pretreated carbon fibers;
coating treatment, namely preparing silica sol: according to the mol ratio of ethyl orthosilicate to ethanol to water, namely hydrochloric acid=1:6.4:3.8:0.085, fully mixing the ethyl orthosilicate with absolute ethanol, dropwise adding a mixture of deionized water and nitric acid under strong stirring of a magnetic stirrer, stirring and refluxing the reaction mixture at 70 ℃ for 3 hours after the dropwise adding is finished, adding 30% V/V of N, N-dimethylformamide as a drying control chemical additive after the sol is cooled, and continuously stirring for 15 minutes to obtain silica sol; soaking the pretreated carbon fiber in silicon dioxide sol, uniformly stirring, filtering and drying to obtain coated carbon fiber;
and (3) carrying out plasma treatment on the coated carbon fiber, wherein the discharge power density during the plasma treatment is 0.2W/cm, and the treatment time is 10min, so as to obtain the modified heat-conducting carbon fiber.
Comparative preparation example 2
The preparation method of the modified heat-conducting carbon fiber comprises the following steps:
coating treatment, namely preparing silica sol: according to the mol ratio of ethyl orthosilicate to ethanol to water, namely hydrochloric acid=1:6.4:3.8:0.085, fully mixing the ethyl orthosilicate with absolute ethanol, dropwise adding a mixture of deionized water and nitric acid under strong stirring of a magnetic stirrer, stirring and refluxing the reaction mixture at 70 ℃ for 3 hours after the dropwise adding is finished, adding 30% V/V of N, N-dimethylformamide as a drying control chemical additive after the sol is cooled, and continuously stirring for 15 minutes to obtain silica sol; soaking carbon fibers with the length of 1-2mm in silicon dioxide sol, uniformly mixing, filtering and drying to obtain coated carbon fibers;
the preparation method comprises the steps of performing plasma treatment, adding coated carbon fibers into an ethanol water solution of a silane coupling agent, wherein the ethanol volume fraction in the ethanol water solution is 85%, the silane coupling agent is gamma- (2, 3-glycidoxy) propyl trimethoxy silane, and the mass ratio of the coated carbon fibers to the silane coupling agent is 100: and 3, removing the solvent after uniformly mixing, drying, performing plasma treatment, wherein the discharge power density during the plasma treatment is 0.2W/cm, and the treatment time is 10min, so as to obtain the modified heat-conducting carbon fiber.
Comparative preparation example 3
The preparation method of the modified heat-conducting carbon fiber comprises the following steps:
pretreating, namely immersing carbon fibers with the length of 1-2mm in a sodium persulfate aqueous solution with the mass concentration of 15g/L, wherein the mass of the carbon fibers added into each 1L of ammonium persulfate aqueous solution is 22g, carrying out ultrasonic treatment, the power of ultrasonic treatment is 380W, the ultrasonic time is 12min, the ultrasonic frequency is 40KHz, filtering, flushing with distilled water to pH of 7, and drying to obtain pretreated carbon fibers;
coating treatment, namely preparing silica sol: according to the mol ratio of ethyl orthosilicate to ethanol to water, namely hydrochloric acid=1:6.4:3.8:0.085, fully mixing the ethyl orthosilicate with absolute ethanol, dropwise adding a mixture of deionized water and nitric acid under strong stirring of a magnetic stirrer, stirring and refluxing the reaction mixture at 70 ℃ for 3 hours after the dropwise adding is finished, adding 30% V/V of N, N-dimethylformamide as a drying control chemical additive after the sol is cooled, and continuously stirring for 15 minutes to obtain silica sol; and soaking the pretreated carbon fiber in the silicon dioxide sol, uniformly stirring, filtering and drying to obtain the modified heat-conducting carbon fiber.
Comparative preparation example 4
The preparation method of the modified heat-conducting carbon fiber comprises the following steps:
coating treatment, namely preparing silica sol: according to the mol ratio of ethyl orthosilicate to ethanol to water, namely hydrochloric acid=1:6.4:3.8:0.085, fully mixing the ethyl orthosilicate with absolute ethanol, dropwise adding a mixture of deionized water and nitric acid under strong stirring of a magnetic stirrer, stirring and refluxing the reaction mixture at 70 ℃ for 3 hours after the dropwise adding is finished, adding 30% V/V of N, N-dimethylformamide as a drying control chemical additive after the sol is cooled, and continuously stirring for 15 minutes to obtain silica sol; and (3) soaking the carbon fiber with the length of 1-2mm in the silicon dioxide sol, uniformly stirring, filtering and drying to obtain the modified heat-conducting carbon fiber.
Examples
Example 1
The high-temperature-resistant high-reliability inverter organosilicon heat-conducting pouring sealant consists of a component A and a component B in a mass ratio of 0.8:1; the component A comprises the following raw materials in parts by weight:
30kg of a heat conducting filler;
25kg of modified heat-conducting carbon fiber;
10kg of vinyl silicone oil;
0.2kg of methyl silicone oil;
0.1kg of a platinum catalyst, which is chloroplatinic acid;
the component B comprises the following raw materials in parts by weight:
30kg of a heat conducting filler;
25kg of modified heat-conducting carbon fiber;
10kg of vinyl silicone oil;
6kg of hydrogen-containing silicone oil;
0.2kg of methyl silicone oil;
0.1kg of a crosslinking inhibitor, wherein the crosslinking inhibitor is acetylene cyclohexanol;
the heat conducting filler in the component A and the heat conducting filler in the component B are spherical alumina, and the mesh number is 2000-3000 mesh; the modified heat-conducting carbon fibers in the component A and the component B are prepared from a preparation example 1; the mass percentage of vinyl in the vinyl silicone oil in the component A and the component B is 1.5 percent, and the viscosity is 100 mPa.S; the hydrogen content of the hydrogen-containing silicone oil is 1.6 percent by mass;
the preparation method of the high-temperature-resistant high-reliability inverter organic silicon heat-conducting pouring sealant comprises the following steps:
step one, mixing and heating a heat conduction filler, vinyl silicone oil and methyl silicone oil to 80 ℃, stirring at 200rpm for 30min, cooling to below 50 ℃, adding a modified heat conduction carbon fiber and a platinum catalyst, and stirring at 200rpm for 30min to obtain a component A;
mixing and heating the heat-conducting filler, the vinyl silicone oil and the methyl silicone oil to 80 ℃, stirring at 200rpm for 30min, cooling to below 50 ℃, adding the modified heat-conducting carbon fiber and the crosslinking inhibitor, stirring for the first time at 200rpm for 30min, adding the hydrogen-containing silicone oil, stirring for the second time at 200rpm for 30min, and obtaining a component B;
and step three, mixing the component A and the component B, stirring for 20min at a rotating speed of 200rpm, and vacuum defoaming to obtain the organic silicon heat-conducting pouring sealant.
Examples 2 to 11
The difference from example 1 is that the modified heat conductive carbon fibers in the A component and the B component were sequentially produced from production examples 2 to 11.
Example 12
The difference with the embodiment 9 is that the high temperature resistant high reliability inverter organosilicon heat conduction pouring sealant consists of a component A and a component B in a mass ratio of 1:1;
the component A comprises the following raw materials in parts by weight:
40kg of a heat conducting filler;
20kg of modified heat-conducting carbon fiber;
25kg of vinyl silicone oil;
1kg of methyl silicone oil;
0.3kg of platinum catalyst;
the component B comprises the following raw materials in parts by weight:
40kg of a heat conducting filler;
20kg of modified heat-conducting carbon fiber;
25kg of vinyl silicone oil;
8kg of hydrogen-containing silicone oil;
1kg of methyl silicone oil;
0.3kg of crosslinking inhibitor.
Example 13
The difference with the embodiment 9 is that the high temperature resistant high reliability inverter organosilicon heat conduction pouring sealant consists of a component A and a component B with the mass ratio of 1.2:1;
the component A comprises the following raw materials in parts by weight:
50kg of a heat conducting filler;
15kg of modified heat-conducting carbon fiber;
40kg of vinyl silicone oil;
2kg of methyl silicone oil;
0.5kg of platinum catalyst;
the component B comprises the following raw materials in parts by weight:
50kg of a heat conducting filler;
15kg of modified heat-conducting carbon fiber;
40kg of vinyl silicone oil;
10kg of hydrogen-containing silicone oil;
2kg of methyl silicone oil;
0.5kg of crosslinking inhibitor.
Comparative example
Comparative examples 1 to 4
The difference from example 2 is that the modified heat conductive carbon fibers in the A and B components were prepared from comparative preparation examples 1 to 4 in this order.
Comparative example 5
The difference from example 2 is that the modified heat conductive carbon fibers in the a and B components are replaced with common carbon fibers of equal weight.
Comparative example 6
The difference from example 2 is that the modified heat conductive carbon fiber in the a-component and the B-component is replaced with spherical alumina of equal weight with a mesh number of 2000-3000 mesh.
Performance test
Detection method
(1) Tensile strength test: the tensile strengths of examples 1 to 13 and comparative examples 1 to 6 were tested in accordance with GB/T528-2009 (measurement of tensile stress strain properties of vulcanized rubber or thermoplastic rubber) using a tensile tester at a tensile speed of 200mm/min;
(2) Thermal deformation temperature test: the heat distortion temperatures of examples 1-13 and comparative examples 1-6 were tested according to the GB1634-79 plastic flexural load heat distortion temperature (referred to as heat distortion temperature) test method;
(3) And (3) heat conduction coefficient test: examples 1-13 and comparative examples 1-6 were tested for thermal conductivity according to ASTM D5470-2017, standard test method for thermal transmission properties of thermally conductive and electrically insulating materials, respectively.
Table 1 test results
As can be seen from the combination of examples 1 to 13 and comparative examples 1 to 6 and the combination of table 1, comparative example 6 only added with the heat conductive filler, and the tensile strength, heat distortion temperature and heat conductivity coefficient were the lowest, and comparative example 5 added with the common carbon fiber based on comparative example 6, the tensile strength, heat distortion temperature and heat conductivity coefficient were all improved, which indicates that the carbon fiber can improve the mechanical properties, heat resistance and heat conductivity of the potting adhesive; the carbon fiber coated with the silicon dioxide layer is added in comparative example 4, so that the tensile strength, the thermal deformation temperature and the heat conductivity coefficient are all improved, probably because the silicon dioxide layer is high-temperature resistant and good in heat conductivity, the thermal deformation temperature and the heat conductivity coefficient of the pouring sealant are improved, and the silicon dioxide layer is coated on the surface of the carbon fiber, so that the mechanical property of the carbon fiber is improved, and the tensile strength of the pouring sealant is improved; comparative example 3 the pretreatment step is added on the basis of comparative example 4, and the tensile strength, the heat distortion temperature and the heat conductivity coefficient are all improved, probably because the specific surface area of the carbon fiber is improved by the pretreatment step, so that the silicon dioxide layer is firmly combined with the carbon fiber; the comparative example 2 is added with a plasma treatment step on the basis of the comparative example 4, and the tensile strength, the thermal deformation temperature and the heat conductivity coefficient are all improved, probably because the silane coupling agent forms a layer of thinner polymer film on the surface of the silicon dioxide layer, the agglomeration between fillers can be prevented, the compatibility with organic polymers can be increased, impurities adsorbed on the surface of the silicon dioxide layer can be effectively removed, active groups are introduced, and the binding force between the modified heat-conducting carbon fiber and the organic polymers is improved; the carbon fiber is subjected to pretreatment, coating treatment and plasma treatment in the embodiment 1-3, and the tensile strength, the thermal deformation temperature and the thermal conductivity are greatly improved, wherein the embodiment 2 has better effect, the silane coupling agent is not added in the plasma treatment in the embodiment 1, the tensile strength, the thermal deformation temperature and the thermal conductivity are reduced, the pretreatment, the coating treatment and the plasma treatment are matched together, the mechanical property, the heat resistance and the thermal conductivity of the pouring sealant can be improved, the silane coupling agent is added in the plasma treatment, the mechanical property and the heat resistance of the pouring sealant can be improved, and the improvement range of the thermal conductivity is smaller; examples 4-7 respectively changed the mass concentration of the sodium persulfate aqueous solution, and as the mass concentration of the sodium persulfate aqueous solution increases, the tensile strength, the heat distortion temperature and the heat conductivity were increased and then decreased, probably because the mass concentration of the sodium persulfate aqueous solution was too low and the oxidation rate was too slow; the mass concentration of the sodium persulfate aqueous solution is too high, which may cause excessive etching, and therefore, the mass concentration of the sodium persulfate aqueous solution is preferably 15 to 25g/L; examples 8 to 11 respectively changed the discharge power density at the time of plasma treatment, and as the discharge power density increased, the tensile strength, the heat distortion temperature and the heat conductivity increased greatly and then increased slowly, so that the discharge power density at the time of plasma treatment was preferably 0.2 to 0.4W/cm; examples 12 and 13 changed the raw material ratios of the potting adhesive, respectively, and the tensile strength, the heat distortion temperature and the heat conductivity were all greatly increased, which indicates that the raw material ratios have a larger influence on the tensile strength, the heat distortion temperature and the heat conductivity of the potting adhesive.
The present embodiment is only for explanation of the present application and is not to be construed as limiting the present application, and modifications to the present embodiment, which may not creatively contribute to the present application as required by those skilled in the art after reading the present specification, are all protected by patent laws within the scope of claims of the present application.

Claims (8)

1. The utility model provides a high temperature resistant high reliability dc-to-ac converter organosilicon heat conduction pouring sealant which characterized in that: consists of a component A and a component B in a mass ratio of (0.8-1.2) 1;
the component A comprises the following raw materials in parts by weight:
30-50 parts of a heat conducting filler;
15-25 parts of modified heat-conducting carbon fiber;
10-40 parts of vinyl silicone oil;
0.2-2 parts of methyl silicone oil;
0.1-0.5 part of platinum catalyst;
the component B comprises the following raw materials in parts by weight:
30-50 parts of a heat conducting filler;
15-25 parts of modified heat-conducting carbon fiber;
10-40 parts of vinyl silicone oil;
6-10 parts of hydrogen-containing silicone oil;
0.2-2 parts of methyl silicone oil;
0.1-0.5 part of crosslinking inhibitor;
the preparation method of the modified heat-conducting carbon fiber comprises the following steps:
pretreating, namely soaking the carbon fiber in a sodium persulfate aqueous solution, performing ultrasonic treatment, performing solid-liquid separation, washing with water, and drying to obtain pretreated carbon fiber;
coating, namely preparing silicon dioxide sol, soaking the pretreated carbon fiber in the silicon dioxide sol, uniformly mixing, filtering and drying to obtain coated carbon fiber;
and (3) carrying out plasma treatment, namely adding the coated carbon fiber into a silane coupling agent solution, uniformly mixing, removing the solvent, drying, and carrying out plasma treatment to obtain the modified heat-conducting carbon fiber.
2. The high-temperature-resistant high-reliability organic silicon heat conduction pouring sealant for an inverter, which is disclosed in claim 1, is characterized in that: the mass concentration of the sodium persulfate aqueous solution is 15-25g/L.
3. The high-temperature-resistant high-reliability inverter organosilicon heat-conducting pouring sealant according to claim 1, wherein the mass of carbon fiber added into each 1L of ammonium persulfate aqueous solution is 20-25g.
4. The high-temperature-resistant high-reliability organic silicon heat conduction pouring sealant for an inverter, which is disclosed in claim 1, is characterized in that: the power of the ultrasonic treatment is 350-400W, and the ultrasonic time is 10-15min.
5. The high-temperature-resistant high-reliability organic silicon heat conduction pouring sealant for an inverter, which is disclosed in claim 1, is characterized in that: the silane coupling agent is selected from any one of gamma-aminopropyl triethoxysilane, gamma- (2, 3-epoxypropoxy) propyl trimethoxysilane, vinyl trimethoxysilane and hexadecyl trimethoxysilane.
6. The high-temperature-resistant high-reliability organic silicon heat conduction pouring sealant for an inverter, which is disclosed in claim 5, is characterized in that: the mass ratio of the coated carbon fiber to the silane coupling agent is 100: (2-4).
7. The high-temperature-resistant high-reliability organic silicon heat conduction pouring sealant for an inverter, which is disclosed in claim 1, is characterized in that: the discharge power density is 0.2-0.4W/cm during the plasma treatment, and the treatment time is 4-10min.
8. The method for preparing the high-temperature-resistant high-reliability inverter organosilicon heat-conducting pouring sealant according to any one of claims 1 to 7, which is characterized in that: the method comprises the following steps:
step one, mixing, heating and stirring a heat conduction filler, vinyl silicone oil and methyl silicone oil, cooling to below 50 ℃, adding modified heat conduction carbon fiber and a platinum catalyst, and uniformly stirring to obtain a component A;
mixing, heating and stirring the heat-conducting filler, vinyl silicone oil and methyl silicone oil, cooling to below 50 ℃, adding modified heat-conducting carbon fiber and a crosslinking inhibitor for first stirring, and then adding hydrogen-containing silicone oil for second stirring to obtain a component B;
and thirdly, uniformly mixing the component A and the component B, and carrying out vacuum defoaming to obtain the organic silicon heat-conducting pouring sealant.
CN202310650423.7A 2023-06-03 2023-06-03 High-temperature-resistant high-reliability organic silicon heat-conducting pouring sealant for inverter and preparation method thereof Pending CN116751559A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN117384584A (en) * 2023-10-13 2024-01-12 广东思泉新材料股份有限公司 Double-component heat-conducting pouring sealant for OBC charging module and preparation method thereof

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN117384584A (en) * 2023-10-13 2024-01-12 广东思泉新材料股份有限公司 Double-component heat-conducting pouring sealant for OBC charging module and preparation method thereof

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