CN109971415B - High-thermal-conductivity organic silicon adhesive and preparation method thereof - Google Patents

High-thermal-conductivity organic silicon adhesive and preparation method thereof Download PDF

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CN109971415B
CN109971415B CN201910285779.9A CN201910285779A CN109971415B CN 109971415 B CN109971415 B CN 109971415B CN 201910285779 A CN201910285779 A CN 201910285779A CN 109971415 B CN109971415 B CN 109971415B
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陈立
王波
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Jiangmen gunaite Technology 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
    • 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
    • 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
    • C09J11/06Non-macromolecular additives organic
    • 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
    • C09J11/08Macromolecular additives
    • 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
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/38Boron-containing compounds
    • C08K2003/382Boron-containing compounds and nitrogen
    • C08K2003/385Binary compounds of nitrogen with boron
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/002Physical properties
    • C08K2201/003Additives being defined by their diameter
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/02Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
    • C08L2205/025Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Adhesives Or Adhesive Processes (AREA)

Abstract

The invention relates to a high-thermal-conductivity organic silicon sealant, which is characterized in that an effective bridging structure is formed between granular silicon carbide and boron nitride sheets through accurately regulating and controlling the size and the shape of a thermal conductive material, a compact thermal conductive path is formed by lapping, and then graphene is used for modifying the thermal conductive path, so that a graphene thermal conductive layer is formed on the surface of the thermal conductive path, and the thermal conductive effect of the high-thermal-conductivity organic silicon sealant is further improved. The specific formula comprises hydroxyl-terminated polydimethylsiloxane, dimethyl silicone oil, heat-conducting filler, toughening agent, coupling agent, antioxidant and catalyst. The sealant can be widely used for sealing or bonding various electronic components.

Description

High-thermal-conductivity organic silicon adhesive and preparation method thereof
Technical Field
The invention belongs to the technical field of sealants, and particularly relates to the technical field of high-thermal-conductivity organosilicon electronic sealants.
Background
With the rapid development of integration technology and assembly technology, higher requirements are put on the heat dissipation performance of materials used for electronic components and logic circuits. At present, the heat dissipation of electronic components mainly adopts a contact conduction mode to realize effective heat dissipation, and the common contact mode has two modes of mechanical fastening and heat-conducting glue bonding. The heat-conducting glue bonding means that the heat-radiating fins and the electronic components are bonded through the heat-conducting adhesive, no gap exists, and the heat-conducting glue bonding is insulating and cannot loosen or move after being cured. The base material of the heat-conducting adhesive generally comprises acrylic acid, polyurethane, organic silicon and epoxy resin, wherein the organic silicon has the advantages of good heat resistance, electrical insulation, corrosion resistance and the like, and is a better material for manufacturing the heat-conducting adhesive.
The organic silicon heat-conducting glue is generally prepared by taking organic silicon as a matrix and adding additives such as filling materials, heat-conducting materials and the like to mix, the heat conductivity coefficient of the organic silicon is not high, and the heat conductivity coefficient of the whole heat-conducting glue is required to be improved through the heat-conducting materials. For example, CN2015108153207 discloses a single-component heat-conducting silica gel, which is composed of polysiloxane, cross-linking agent, coupling agent, catalyst, inhibitor, toughening agent, stabilizer, magnesium oxide, and chromium carbide; CN201210476392X discloses a bi-component low-hardness high-thermal-conductivity room-temperature curing organic silicon heat-conducting adhesive, which consists of a component A and a component B, wherein the component A comprises a base material and a platinum catalyst, the component B consists of the base material, terminal hydrogen-containing silicone oil, side chain hydrogen-containing silicone oil and an inhibitor, and the base material is prepared from divinyl silicone oil, aluminum oxide and hexamethyldisilazane.
The filler added in the existing organic silicon heat-conducting adhesive is usually coated by organic silicon to form an independent particle system, and the organic silicon among particle interfaces limits the heat-conducting efficiency of the organic silicon heat-conducting adhesive, so that the heat-conducting efficiency of the existing organic silicon heat-conducting adhesive is lower.
Disclosure of Invention
In order to solve the defects of the prior art, the invention provides a high-heat-conductivity organic silicon adhesive, which has the following specific scheme:
the high heat conductivity organic silicon adhesive comprises 100 parts of hydroxyl-terminated polydimethylsiloxane, 20-45 parts of dimethyl silicone oil, 60-90 parts of heat conductive filler, 1-15 parts of toughening agent, 0.1-5 parts of coupling agent, 0.1-1 part of antioxidant and 0.5-1 part of catalyst;
the heat-conducting filler comprises a mixture of silicon carbide, boron nitride and graphene, the mass ratio of the silicon carbide to the boron nitride to the graphene is 1-5:15-20:0.5-1, the silicon carbide is zero-dimensional granular silicon carbide with the granularity of 1.5 microns, the boron nitride is two-dimensional flaky boron nitride with the thickness of less than 20nm, and the graphene layer is less than 1 nanometer;
the toughening agent comprises one or a mixture of more of glycerol, monoethylene glycol, 1, 3-butanediol and 1, 4-butanediol;
the coupling agent is a silane coupling agent and comprises one or a mixture of more of methyltrimethoxysilane, dimethyldimethoxysilane, vinyl trimethoxysilane, vinyl triethoxysilane and tetraethoxysilane;
the antioxidant brand comprises a mixture of one or more of 1010, 9701, 264, 168, 1076, DNP, CA;
the catalyst is a compound of organic tin and methylimidazole, and the mass ratio of the organic tin to the methylimidazole is 0.1-0.5: 1; the organic tin comprises one or more of dibutyltin dilaurate, dipentylene dilaurate, dihexylene dilaurate, dimethoxydibutylene, diethoxydehexyltin, diethoxydioctyltin, dibutoxydehexyltin and dipropoxydibutylene;
according to the high-thermal-conductivity organic silicon adhesive, the size and the shape of a thermal conductive material are accurately regulated and controlled, an effective bridging structure is formed between granular silicon carbide and boron nitride sheets, a compact thermal conductive passage is formed by lapping, then graphene is used for modifying the thermal conductive passage, a graphene thermal conductive layer is formed on the surface of the thermal conductive passage, and the thermal conductive effect is further improved.
In addition, the catalyst used is a complex of organotin and methylimidazole, the tin atom of which can have a weak interaction with the nitrogen atom of methylimidazole at room temperature, which renders it catalytically inactive at room temperature. When the temperature is raised to a certain temperature, the weak interaction disappears, so that the active electrons of the tin atoms are released to catalyze polymerization to realize the solidification of the binder. Thereby realizing long-term preservation of the adhesive at room temperature.
The invention also provides a preparation method of the heat-conducting organic silicon adhesive, which comprises the following specific preparation steps:
(1) adding a dispersing agent of a Fule coating DS-172 type into deionized water to prepare a 1-5% aqueous solution, then sequentially adding granular silicon carbide and two-dimensional flaky boron nitride into the aqueous solution, fully stirring and dispersing for 20-60min, then adding graphene, and continuing stirring for 20-60 min. Then filtering and washing to obtain a heat-conducting filler composite;
(2) and adding the heat-conducting filler composite and the silane coupling agent into a grinding machine to grind for 20-30min to obtain the modified heat-conducting filler composite. The mass ratio of the filler composite to the silane coupling agent is 100: 0.1-5;
(3) and sequentially adding the hydroxyl-terminated polydimethylsiloxane, the dimethyl silicone oil, the modified filler complex, the toughening agent, the coupling agent, the antioxidant and the catalyst into a kneader, and kneading in vacuum for 10-50min at room temperature to obtain the single-component heat-conducting organic silicon adhesive.
The preparation method adopts a gradual dispersion deposition method to ensure that the heat-conducting filler composite has uniform structure, clear layers and high heat-conducting efficiency. And then, a bonding group is introduced into the surface of the heat-conducting filler composite by a grinding modification method, and the heat-conducting filler composite is further crosslinked with a binder system, so that the bonding force is stronger.
The invention also provides a using method of the heat-conducting organic silica gel, which comprises the steps of preheating the heat-conducting organic silica gel to 40-50 ℃ to enable the heat-conducting organic silica gel to fully flow when in use, then casting the heat-conducting organic silica gel onto a related device, and heating and curing at the curing temperature of 100-110 ℃.
Detailed Description
The principles and features of this invention are described below in conjunction with examples which are set forth to illustrate, but are not to be construed to limit the scope of the invention. Meanwhile, in order to characterize the heat conduction efficiency of the prepared organic silicon adhesive, the adhesive prepared by the embodiment of the invention is tested for the heat conduction coefficient after being cured and formed, and is specifically completed by adopting a heat flow method heat conduction instrument. The following formulas are all calculated by weight fraction:
example 1.
The high-thermal-conductivity organic silicon adhesive comprises 100 parts of hydroxyl-terminated polydimethylsiloxane, 25 parts of dimethyl silicone oil, 60 parts of thermal-conductivity filler, 10 parts of glycerol, 5 parts of methyltrimethoxysilane, 0.2 part of 1010-type antioxidant and 0.8 part of catalyst. The heat-conducting filler comprises a mixture of silicon carbide, boron nitride and graphene, the mass ratio of the silicon carbide to the boron nitride to the graphene is 3:15:0.8, the particle size of the silicon carbide is 1.5 micrometers, the thickness of the boron nitride is less than 20nm, and the thickness of a graphene layer is less than 1 nm; the catalyst is a compound of dibutyltin dilaurate and methylimidazole, and the mass ratio of the organotin to the methylimidazole is 0.1: 1.
The preparation method comprises the following specific steps:
(1) adding a Yile-coated DS-172 type dispersing agent into deionized water to prepare a 2% aqueous solution, then sequentially adding granular silicon carbide and two-dimensional flaky boron nitride into the aqueous solution, wherein the total mass ratio of the granular silicon carbide to the two-dimensional flaky boron nitride to the aqueous solution is 10:100, fully stirring and dispersing for 30min, then adding graphene, and continuing stirring for 30 min. Then filtering and washing to obtain the heat-conducting filler composite.
(2) Adding the heat-conducting filler composite and 10% methyltrimethoxysilane (0.5 part) in the formula into a grinding machine to grind for 20min to obtain the modified heat-conducting filler composite.
(3) And sequentially adding hydroxyl-terminated polydimethylsiloxane, dimethyl silicone oil, a modified filler composite, glycerol, methyltrimethoxysilane (4.5 parts), a 1010 type antioxidant and a catalyst into a kneader, and kneading in vacuum at room temperature, wherein the vacuum degree is-0.06-0.1 MPa, and the kneading time is 30min, so as to obtain the single-component heat-conducting organic silicon adhesive.
The curing temperature of the obtained heat-conducting organic silicon adhesive is 105 ℃, and the heat conductivity coefficient after curing is measured to be 5.28W/m.K.
Example 2.
The high-thermal-conductivity organic silicon adhesive comprises 100 parts of hydroxyl-terminated polydimethylsiloxane, 30 parts of dimethyl silicone oil, 60 parts of thermal-conductivity filler, 10 parts of glycerol, 5 parts of methyltrimethoxysilane, 0.2 part of 1010-type antioxidant and 0.5 part of catalyst. The heat-conducting filler comprises a mixture of silicon carbide, boron nitride and graphene, the mass ratio of the silicon carbide to the boron nitride to the graphene is 2:18:0.8, the particle size of the silicon carbide is 1.5 micrometers, the thickness of the boron nitride is less than 20nm, and the thickness of a graphene layer is less than 1 nm; the catalyst is a compound of dibutyltin dilaurate and methylimidazole, and the mass ratio of the organotin to the methylimidazole is 0.1: 1.
The preparation method is the same as that of example 1, the curing temperature of the obtained heat-conducting organic silicon adhesive is 107 ℃, and the heat conductivity coefficient after curing is 5.43W/m.K.
Example 3.
The high-thermal-conductivity organic silicon adhesive comprises 100 parts of hydroxyl-terminated polydimethylsiloxane, 25 parts of dimethyl silicone oil, 60 parts of thermal-conductivity filler, 10 parts of glycerol, 5 parts of methyltrimethoxysilane, 0.2 part of 1010-type antioxidant and 0.8 part of catalyst. The heat-conducting filler comprises a mixture of silicon carbide, boron nitride and graphene, the mass ratio of the silicon carbide to the boron nitride to the graphene is 3:15:0.8, the particle size of the silicon carbide is 1.5 micrometers, the thickness of the boron nitride is less than 20nm, and the thickness of a graphene layer is less than 1 nm; the catalyst is a compound of diethoxydehexyltin and methylimidazole, and the mass ratio of the organic tin to the methylimidazole is 0.3: 1.
The preparation method is the same as example 1. The curing temperature of the obtained heat-conducting organic silicon adhesive is 102 ℃, and the heat conductivity coefficient after curing is measured to be 5.36W/m.K.
Example 4.
The high-thermal-conductivity organic silicon adhesive comprises 100 parts of hydroxyl-terminated polydimethylsiloxane, 25 parts of dimethyl silicone oil, 80 parts of thermal-conductivity filler, 10 parts of glycerol, 5 parts of methyltrimethoxysilane, 0.2 part of 1010-type antioxidant and 0.8 part of catalyst. The heat-conducting filler comprises a mixture of silicon carbide, boron nitride and graphene, the mass ratio of the silicon carbide to the boron nitride to the graphene is 4:15:0.9, the particle size of the silicon carbide is 1.5 micrometers, the thickness of the boron nitride is less than 20nm, and the thickness of a graphene layer is less than 1 nm; the catalyst is a compound of diethoxydehexyltin and methylimidazole, and the mass ratio of the organic tin to the methylimidazole is 0.3: 1.
The preparation method is the same as example 1. The curing temperature of the obtained heat-conducting organic silicon adhesive is 102 ℃, and the heat conductivity coefficient after curing is measured to be 5.88W/m.K.
Example 5.
The high-thermal-conductivity organic silicon adhesive comprises 100 parts of hydroxyl-terminated polydimethylsiloxane, 25 parts of dimethyl silicone oil, 60 parts of thermal-conductive filler, 8 parts of monoethylene glycol, 3 parts of vinyl triethoxysilane, 0.2 part of 1010-type antioxidant and 0.8 part of catalyst. The heat-conducting filler comprises a mixture of silicon carbide, boron nitride and graphene, the mass ratio of the silicon carbide to the boron nitride to the graphene is 3:15:0.8, the particle size of the silicon carbide is 1.5 micrometers, the thickness of the boron nitride is less than 20nm, and the thickness of a graphene layer is less than 1 nm; the catalyst is a compound of dibutyltin dilaurate and methylimidazole, and the mass ratio of the organotin to the methylimidazole is 0.1: 1.
The preparation method comprises the following specific steps:
(1) adding a Yile-coated DS-172 type dispersing agent into deionized water to prepare a 2% aqueous solution, then sequentially adding granular silicon carbide and two-dimensional flaky boron nitride into the aqueous solution, wherein the total mass ratio of the granular silicon carbide to the two-dimensional flaky boron nitride to the aqueous solution is 10:100, fully stirring and dispersing for 30min, then adding graphene, and continuing stirring for 30 min. Then filtering and washing to obtain the heat-conducting filler composite.
(2) Adding the heat-conducting filler composite and 20% of vinyltriethoxysilane (0.6 part) in the formula into a grinding machine to grind for 20min to obtain the modified heat-conducting filler composite.
(3) And sequentially adding hydroxyl-terminated polydimethylsiloxane, dimethyl silicone oil, a modified filler complex, diethylene glycol, vinyl triethoxysilane (2.4 parts), 1010 type antioxidant and a catalyst into a kneader, and kneading at room temperature in vacuum at a vacuum degree of-0.06-0.1 MPa for 20min to obtain the single-component heat-conducting organic silicon adhesive.
The curing temperature of the obtained heat-conducting organic silicon adhesive is 105 ℃, and the heat conductivity coefficient after curing is measured to be 5.17W/m.K.
Example 6.
The high-thermal-conductivity organic silicon adhesive comprises 100 parts of hydroxyl-terminated polydimethylsiloxane, 25 parts of dimethyl silicone oil, 65 parts of thermal-conductivity filler, 8 parts of 1, 4-butanediol, 4 parts of ethyl orthosilicate, 0.2 part of DNP type antioxidant and 0.8 part of catalyst. The heat-conducting filler comprises a mixture of silicon carbide, boron nitride and graphene, the mass ratio of the silicon carbide to the boron nitride to the graphene is 3:15:0.8, the particle size of the silicon carbide is 1.5 micrometers, the thickness of the boron nitride is less than 20nm, and the thickness of a graphene layer is less than 1 nm; the catalyst is a compound of dibutyltin dilaurate and methylimidazole, and the mass ratio of the organotin to the methylimidazole is 0.1: 1.
The preparation method comprises the following specific steps:
(1) adding a Yile-coated DS-172 type dispersing agent into deionized water to prepare a 2% aqueous solution, then sequentially adding granular silicon carbide and two-dimensional flaky boron nitride into the aqueous solution, wherein the total mass ratio of the granular silicon carbide to the two-dimensional flaky boron nitride to the aqueous solution is 10:100, fully stirring and dispersing for 30min, then adding graphene, and continuing stirring for 30 min. Then filtering and washing to obtain the heat-conducting filler composite.
(2) Adding the heat-conducting filler composite and 15% of tetraethoxysilane (0.6 part) in the formula into a grinding machine to grind for 25min to obtain the modified heat-conducting filler composite.
(3) And sequentially adding hydroxyl-terminated polydimethylsiloxane, dimethyl silicone oil, a modified filler complex, 1, 4-butanediol, ethyl orthosilicate (3.4 parts), a DNP type antioxidant and a catalyst into a kneader, and kneading at room temperature in vacuum at a vacuum degree of-0.06-0.1 MPa for 30min to obtain the single-component heat-conducting organic silicon adhesive.
The curing temperature of the obtained heat-conducting organic silicon adhesive is 105 ℃, and the heat conductivity coefficient after curing is measured to be 5.64W/m.K.
Comparative example.
The comparative example refers to a formula system with the patent number of CN2015108153207, and the specific formula comprises, by weight, 40 parts of alkoxy-terminated polysiloxane, 1 part of methyl hydrogenpolysiloxane, 0.8 part of rare earth coupling agent, 0.6 part of platinum catalyst, 0.2 part of alkynol, NBR9 part, 0.4 part of zinc stearate, 2641 parts of anti-aging agent, 20 parts of magnesium oxide and 39 parts of chromium carbide. The thermal conductivity coefficient of the prepared single-component organic silicon thermal conductive adhesive is 3.36W/m.K.
Through the analysis of the above examples and comparative examples, it can be found that the heat-conducting silicone adhesive prepared by the invention can significantly improve the heat-conducting efficiency.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.

Claims (6)

1. The high heat conductivity organic silicon adhesive comprises 100 parts of hydroxyl-terminated polydimethylsiloxane, 20-45 parts of dimethyl silicone oil, 60-90 parts of heat conductive filler, 1-15 parts of toughening agent, 0.1-5 parts of coupling agent, 0.1-1 part of antioxidant and 0.5-1 part of catalyst; the heat-conducting filler is characterized by comprising a mixture of silicon carbide, boron nitride and graphene, wherein the mass ratio of the silicon carbide to the boron nitride to the graphene is =1-5:15-20:0.5-1, the silicon carbide is zero-dimensional granular silicon carbide with the granularity of 1.5 micrometers, the boron nitride is two-dimensional flaky boron nitride with the thickness of less than 20nm, and the graphene layer is less than 1 nm;
the catalyst is a composite of organic tin and methylimidazole, and the mass ratio of the organic tin to the methylimidazole is 0.1-0.5: 1.
2. The high thermal conductivity silicone adhesive according to claim 1, wherein the organic tin comprises one or more of dibutyltin dilaurate, dipentylene dilaurate, dihexylene dilaurate, dimethoxydibutylene, diethoxydehexyltin, diethoxydioctyltin, dibutoxydehexyltin, and dipropoxydibutylene.
3. The silicone adhesive according to claim 1, wherein the toughening agent comprises one or more of glycerol, monoethylene glycol, 1, 3-butanediol, and 1, 4-butanediol.
4. The high thermal conductivity silicone adhesive according to claim 1, wherein the coupling agent is a silane coupling agent, and comprises one or a mixture of several of methyltrimethoxysilane, dimethyldimethoxysilane, vinyltrimethoxysilane, vinyltriethoxysilane, and ethyl orthosilicate.
5. The silicone adhesive of claim 1, wherein the antioxidant brand comprises a mixture of one or more of 1010, 9701, 264, 168, 1076, DNP, CA.
6. The preparation method of the heat-conducting silicone adhesive according to any one of claims 1 to 5, comprising the following specific steps:
(1) adding a Yile-coated DS-172 type dispersing agent into deionized water to prepare 1-5% aqueous solution, then sequentially adding granular silicon carbide and two-dimensional flaky boron nitride into the aqueous solution, fully stirring and dispersing for 20-60min, then adding graphene, continuously stirring for 20-60min, filtering and washing to obtain a heat-conducting filler composite;
(2) adding the heat-conducting filler complex and a silane coupling agent into a grinding machine to grind for 20-30min to obtain a modified heat-conducting filler complex; the mass ratio of the filler composite to the silane coupling agent is 100: 0.1-5;
(3) and sequentially adding the hydroxyl-terminated polydimethylsiloxane, the dimethyl silicone oil, the modified filler complex, the toughening agent, the coupling agent, the antioxidant and the catalyst into a kneader, and kneading in vacuum for 10-50min at room temperature to obtain the single-component heat-conducting organic silicon adhesive.
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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107760256A (en) * 2017-09-26 2018-03-06 广州机械科学研究院有限公司 A kind of lower shrinkage heat conductive flame-retarding double-component condensed type organic silicon potting adhesive and its preparation method and application
KR101927641B1 (en) * 2017-09-29 2018-12-10 영남대학교 산학협력단 Flexible printed circuit board apparatus with enhanced heat-radiating property
CN109439236A (en) * 2018-11-30 2019-03-08 中国科学院金属研究所 A kind of thermoconductive glue of containing graphene and its preparation method and application

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107760256A (en) * 2017-09-26 2018-03-06 广州机械科学研究院有限公司 A kind of lower shrinkage heat conductive flame-retarding double-component condensed type organic silicon potting adhesive and its preparation method and application
KR101927641B1 (en) * 2017-09-29 2018-12-10 영남대학교 산학협력단 Flexible printed circuit board apparatus with enhanced heat-radiating property
CN109439236A (en) * 2018-11-30 2019-03-08 中国科学院金属研究所 A kind of thermoconductive glue of containing graphene and its preparation method and application

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
SiC-BN填料杂化柔性电绝缘高导热材料;徐昉等;《高分子材料科学与工程》;20180930;第34卷(第9期);第156页 *

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