CN109971415A - A kind of high heat conduction organosilicon adhesive and preparation method thereof - Google Patents
A kind of high heat conduction organosilicon adhesive and preparation method thereof Download PDFInfo
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- CN109971415A CN109971415A CN201910285779.9A CN201910285779A CN109971415A CN 109971415 A CN109971415 A CN 109971415A CN 201910285779 A CN201910285779 A CN 201910285779A CN 109971415 A CN109971415 A CN 109971415A
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- Prior art keywords
- heat conduction
- parts
- organosilicon adhesive
- graphene
- high heat
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- 239000000853 adhesive Substances 0.000 title claims abstract description 34
- 230000001070 adhesive effect Effects 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims description 13
- 229910010271 silicon carbide Inorganic materials 0.000 claims abstract description 37
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 34
- 229910052582 BN Inorganic materials 0.000 claims abstract description 33
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims abstract description 33
- 238000011049 filling Methods 0.000 claims abstract description 33
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 31
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims abstract description 29
- 239000004205 dimethyl polysiloxane Substances 0.000 claims abstract description 28
- 235000013870 dimethyl polysiloxane Nutrition 0.000 claims abstract description 28
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims abstract description 28
- 239000003054 catalyst Substances 0.000 claims abstract description 25
- -1 polydimethylsiloxane Polymers 0.000 claims abstract description 23
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 16
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 14
- 229940008099 dimethicone Drugs 0.000 claims abstract description 14
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims abstract description 14
- 239000007822 coupling agent Substances 0.000 claims abstract description 9
- 239000012745 toughening agent Substances 0.000 claims abstract description 8
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 claims description 20
- LXBGSDVWAMZHDD-UHFFFAOYSA-N 2-methyl-1h-imidazole Chemical compound CC1=NC=CN1 LXBGSDVWAMZHDD-UHFFFAOYSA-N 0.000 claims description 18
- XLSZMDLNRCVEIJ-UHFFFAOYSA-N methylimidazole Natural products CC1=CNC=N1 XLSZMDLNRCVEIJ-UHFFFAOYSA-N 0.000 claims description 18
- 239000000203 mixture Substances 0.000 claims description 18
- 239000007864 aqueous solution Substances 0.000 claims description 13
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 9
- 229910052796 boron Inorganic materials 0.000 claims description 9
- 239000000945 filler Substances 0.000 claims description 9
- WERYXYBDKMZEQL-UHFFFAOYSA-N butane-1,4-diol Chemical compound OCCCCO WERYXYBDKMZEQL-UHFFFAOYSA-N 0.000 claims description 8
- 150000001875 compounds Chemical class 0.000 claims description 8
- 238000004898 kneading Methods 0.000 claims description 8
- 150000001336 alkenes Chemical class 0.000 claims description 7
- 239000003795 chemical substances by application Substances 0.000 claims description 7
- BFXIKLCIZHOAAZ-UHFFFAOYSA-N methyltrimethoxysilane Chemical compound CO[Si](C)(OC)OC BFXIKLCIZHOAAZ-UHFFFAOYSA-N 0.000 claims description 7
- 229910052710 silicon Inorganic materials 0.000 claims description 6
- 239000010703 silicon Substances 0.000 claims description 6
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 239000002270 dispersing agent Substances 0.000 claims description 5
- 239000006185 dispersion Substances 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 4
- 239000008139 complexing agent Substances 0.000 claims description 4
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 3
- 229920002554 vinyl polymer Polymers 0.000 claims description 3
- AXPZIVKEZRHGAS-UHFFFAOYSA-N 3-benzyl-5-[(2-nitrophenoxy)methyl]oxolan-2-one Chemical compound [O-][N+](=O)C1=CC=CC=C1OCC1OC(=O)C(CC=2C=CC=CC=2)C1 AXPZIVKEZRHGAS-UHFFFAOYSA-N 0.000 claims description 2
- XEGFIBDEWQCOQN-UHFFFAOYSA-N C(CCC)O[Sn](CCCCCC)(CCCCCC)OCCCC Chemical compound C(CCC)O[Sn](CCCCCC)(CCCCCC)OCCCC XEGFIBDEWQCOQN-UHFFFAOYSA-N 0.000 claims description 2
- QLCGFUKTPZHCND-UHFFFAOYSA-N diethoxy(dioctyl)stannane Chemical compound CCCCCCCC[Sn](OCC)(OCC)CCCCCCCC QLCGFUKTPZHCND-UHFFFAOYSA-N 0.000 claims description 2
- 125000001891 dimethoxy group Chemical group [H]C([H])([H])O* 0.000 claims description 2
- PYBNTRWJKQJDRE-UHFFFAOYSA-L dodecanoate;tin(2+) Chemical compound [Sn+2].CCCCCCCCCCCC([O-])=O.CCCCCCCCCCCC([O-])=O PYBNTRWJKQJDRE-UHFFFAOYSA-L 0.000 claims description 2
- 238000010422 painting Methods 0.000 claims description 2
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 2
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical group [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims 2
- 238000003763 carbonization Methods 0.000 claims 2
- 229910000077 silane Inorganic materials 0.000 claims 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims 1
- 241000218195 Lauraceae Species 0.000 claims 1
- 235000017858 Laurus nobilis Nutrition 0.000 claims 1
- 235000005212 Terminalia tomentosa Nutrition 0.000 claims 1
- 239000011231 conductive filler Substances 0.000 claims 1
- AYOHIQLKSOJJQH-UHFFFAOYSA-N dibutyltin Chemical compound CCCC[Sn]CCCC AYOHIQLKSOJJQH-UHFFFAOYSA-N 0.000 claims 1
- SNRUBQQJIBEYMU-UHFFFAOYSA-N dodecane Chemical group CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 claims 1
- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 11
- 239000010410 layer Substances 0.000 abstract description 5
- 230000000694 effects Effects 0.000 abstract description 4
- 239000000565 sealant Substances 0.000 abstract description 3
- 239000011229 interlayer Substances 0.000 abstract description 2
- 238000007789 sealing Methods 0.000 abstract 1
- 238000007711 solidification Methods 0.000 description 15
- 230000008023 solidification Effects 0.000 description 15
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 12
- 239000003292 glue Substances 0.000 description 9
- 235000011187 glycerol Nutrition 0.000 description 6
- 238000000034 method Methods 0.000 description 6
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 description 5
- 239000012975 dibutyltin dilaurate Substances 0.000 description 5
- 229920001296 polysiloxane Polymers 0.000 description 5
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 4
- 230000008859 change Effects 0.000 description 4
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 4
- 238000012546 transfer Methods 0.000 description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- 229910003978 SiClx Inorganic materials 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- WVTJRFGZMGLFAS-UHFFFAOYSA-N diethoxy(dihexyl)stannane Chemical compound C(CCCCC)[Sn](OCC)(OCC)CCCCCC WVTJRFGZMGLFAS-UHFFFAOYSA-N 0.000 description 3
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 239000000741 silica gel Substances 0.000 description 3
- 229910002027 silica gel Inorganic materials 0.000 description 3
- 229920002545 silicone oil Polymers 0.000 description 3
- 238000004026 adhesive bonding Methods 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- UFGZSIPAQKLCGR-UHFFFAOYSA-N chromium carbide Chemical compound [Cr]#C[Cr]C#[Cr] UFGZSIPAQKLCGR-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 230000017525 heat dissipation Effects 0.000 description 2
- 150000002431 hydrogen Chemical class 0.000 description 2
- 239000000395 magnesium oxide Substances 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 229910052697 platinum Inorganic materials 0.000 description 2
- 229910052718 tin Inorganic materials 0.000 description 2
- 229910003470 tongbaite Inorganic materials 0.000 description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-N Acrylic acid Chemical class OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- USEBIPUIVPERGC-UHFFFAOYSA-N Dibutylone Chemical compound CCC(N(C)C)C(=O)C1=CC=C2OCOC2=C1 USEBIPUIVPERGC-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 239000003431 cross linking reagent Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000004585 electronic sealant Substances 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- XYIBRDXRRQCHLP-UHFFFAOYSA-N ethyl acetoacetate Chemical compound CCOC(=O)CC(C)=O XYIBRDXRRQCHLP-UHFFFAOYSA-N 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- XCMFHUYZTPVWAY-UHFFFAOYSA-N methyl-tris(methylperoxy)silane Chemical compound C[Si](OOC)(OOC)OOC XCMFHUYZTPVWAY-UHFFFAOYSA-N 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 125000004433 nitrogen atom Chemical group N* 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 230000035935 pregnancy Effects 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- YUYCVXFAYWRXLS-UHFFFAOYSA-N trimethoxysilane Chemical compound CO[SiH](OC)OC YUYCVXFAYWRXLS-UHFFFAOYSA-N 0.000 description 1
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J183/00—Adhesives 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
- C09J183/04—Polysiloxanes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/38—Boron-containing compounds
- C08K2003/382—Boron-containing compounds and nitrogen
- C08K2003/385—Binary compounds of nitrogen with boron
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The present invention relates to a kind of high heat conduction organosilicon sealants, the high heat conduction organosilicon adhesive, pass through the accuracy controlling to Heat Conduction Material size and shape, granular silicon carbide and boron nitride piece interlayer is set to be formed with effect bridging structure, it is overlapped to form closely knit thermal conducting path, then it is modified using graphene, so that thermal conducting path surface is formed one layer of graphene heat-conducting layer, further improves its heat-conducting effect.Specific formula includes hydroxyl endblocked polydimethylsiloxane, dimethicone, heat filling, toughener, coupling agent, antioxidant, catalyst.The sealant can be widely used in the sealing or bonding of all kinds of electronic components.
Description
Technical field
The invention belongs to sealant technical fields, and in particular to a kind of organic silicon electronic sealant technology neck of high thermal conductivity
Domain.
Background technique
With the rapid development of integrated technology and package technique, to the thermal diffusivity of electronic component, logic circuit material therefor
More stringent requirements are proposed for energy.Currently, the heat dissipation of electronic component is main to realize effective heat dissipation by the way of contact conduction, often
The way of contact has mechanical fasteners and thermally conductive glue sticking two ways.Wherein, thermally conductive gluing knot refers to through thermally conductive gluing
Agent is bonded cooling fin and electronic component, and there is no gaps, and insulate, and will not loosen, move after solidification.The matrix of heat-conducting glue
Material generally comprises several major class of acrylic acid, polyurethane, organosilicon, epoxy resin, and wherein organosilicon has good heat resistance, electricity
The advantages that gas insulating properties, corrosion resistance is the preferred materials for making heat-conducting glue.
Generally using organosilicon as matrix, the auxiliary agents such as addition filler material, Heat Conduction Material mix organosilicon heat-conducting glue, organic
The thermal coefficient of silicon itself is not high, needs to improve the thermal coefficient of entire heat-conducting glue by Heat Conduction Material.Such as
CN2015108153207 discloses a kind of one pack system heat conductive silica gel, by polysiloxanes, crosslinking agent, coupling agent, catalyst, inhibition
Agent, toughener, stabilizer, magnesia, chromium carbide composition；CN201210476392X discloses a kind of bi-component soft height and leads
Hot cell temperature cured silicone heat-conducting glue, is made of component A and B component, and wherein component A includes base-material and platinum catalyst, B component by
Base-material, end containing hydrogen silicone oil, side chain containing hydrogen silicone oil and inhibitor composition, the base-material is by bi-vinyl silicone oil, aluminium oxide and pregnancy
Base disilazane is prepared.
Filler added by existing organosilicon heat-conducting glue is usually by silicone covering at independent granular system, granular boundary
Between organosilicon limit its heat transfer efficiency, cause the heat transfer efficiency of existing organosilicon heat-conducting glue lower.
Summary of the invention
To solve the deficiencies in the prior art, the present invention provides a kind of high heat conduction organosilicon adhesive, and concrete scheme is as follows:
A kind of high heat conduction organosilicon adhesive, including 100 parts of hydroxyl endblocked polydimethylsiloxane, dimethicone 20-
45 parts, 60-90 parts of heat filling, 1-15 parts of toughener, 0.1-5 parts of coupling agent, 0.1-1 parts of antioxidant, catalyst 0.5-1
Part；
The heat filling includes the mixture of silicon carbide, boron nitride and graphene, and the mass ratio of three is silicon carbide: nitrogen
Change boron: graphene=1-5:15-20:0.5-1, the silicon carbide are 1.5 microns of the granular carborundum granularity of zero dimension, boron nitride two
It ties up platelet boron nitride thickness and is less than 20nm, graphene thickness less than 1 nanometer；
The toughener includes one of glycerine, diethylene glycol, 1,3-BDO, 1,4-butanediol or a variety of
Mixture；
The coupling agent is silane coupling agent, including methyltrimethoxysilane, dimethyldimethoxysil,ne, vinyl
The mixture of one or more of trimethoxy silane, vinyltriethoxysilane, ethyl orthosilicate；
The antioxidant trade mark includes 1010,9701,264,168,1076, one of DNP, CA or a variety of mixing
Object；
The catalyst is the compound of organotin and methylimidazole, and the mass ratio of organotin and methylimidazole is 0.1-
0.5:1；The organotin includes dibutyl tin dilaurate, tin dilaurate diamyl alkene, tin dilaurate dihexyl alkene, dimethoxy
Base dibutyl alkene, diethoxy dihexyl tin, diethoxy dioctyl tin, dibutoxy dihexyl tin, dipropoxy dibutyl
One of alkene or a variety of mixtures；
The high heat conduction organosilicon adhesive makes granular silicon carbide by the accuracy controlling to Heat Conduction Material size and shape
It is formed with effect bridging structure with boron nitride piece interlayer, is overlapped to form closely knit thermal conducting path, then it is modified using graphene, is made
Thermal conducting path surface forms one layer of graphene heat-conducting layer, further improves its heat-conducting effect.
In addition, used catalyst is the compound of organotin and methylimidazole, the tin atom of organotin can at room temperature
There are weak interaction force between the nitrogen-atoms of methylimidazole, which makes it not have catalytic activity at room temperature.Work as temperature
After degree is increased to a certain temperature, which, which disappears, makes the active electrons of tin atom discharge catalytic polymerization realization bonding in turn
The solidification of agent.The adhesive is set to realize the preservation of long period at room temperature in turn.
The present invention also provides a kind of preparation methods of heat conduction organosilicon adhesive, and specific preparation process is as follows:
(1) painting easily happy DS-172 type dispersing agent is add to deionized water to the aqueous solution for being made into 1-5%, it then will be granular
Silicon carbide and two-dimensional sheet boron nitride sequentially add in above-mentioned aqueous solution, and dispersion 20-60min is sufficiently stirred, then adds stone
Black alkene continues to stir 20-60min.Then it is filtered, washed to obtain heat filling complex；
(2) above-mentioned heat filling complex and silane coupling agent are added in grinder and grind 20-30min, obtain modification
Heat filling complex.The mass ratio of the filler complex and silane coupling agent is 100:0.1-5；
(3) by hydroxyl endblocked polydimethylsiloxane, dimethicone, modified filler complex, toughener, coupling agent,
Antioxidant, catalyst are added sequentially in kneader, and vacuum kneading 10-50min obtains one pack system heat-conducting organic silica gel at room temperature
Stick.
The preparation method keeps heat filling complex structure uniform using the method for gradually dispersed deposition, and clear layer is led
The thermal efficiency is high.Then so that heat filling complex surfaces is introduced binding affinity group by the modified method of grinding, further with it is viscous
The crosslinking of agent system is tied, keeps bonding force stronger.
The present invention also provides the application method of the heat-conducting organic silica gel, when use, is first preheating to 40-50 DEG C, is made
It is sufficiently flowed, and is then cast on related device, is heating and curing, and 100-110 DEG C of solidification temperature.
Specific embodiment
The principles and features of the present invention are described below, and illustrated embodiment is served only for explaining the present invention, is not intended to
It limits the scope of the invention.Meanwhile to characterize the heat transfer efficiency of made organic silicon adhesive, the present invention is narrated made from embodiment
Adhesive is specifically completed using heat flow method conductometer by testing thermal coefficient after curing molding.Formula as below is equal
In terms of weight fraction:
Embodiment 1.
A kind of high heat conduction organosilicon adhesive, including 100 parts of hydroxyl endblocked polydimethylsiloxane, dimethicone 25
Part, 60 parts of heat filling, 10 parts of glycerine, 5 parts of methyltrimethoxysilane, 0.2 part of 1010 type antioxidant, catalyst 0.8
Part.Wherein, heat filling includes the mixture of silicon carbide, boron nitride and graphene, and the mass ratio of three is silicon carbide: nitridation
Boron: graphene=3:15:0.8, the silicon carbide be the granular carborundum granularity of zero dimension be 1.5 microns, boron nitride is two-dimensional sheet
Boron nitride thickness is less than 20nm, graphene thickness is less than 1nm；Catalyst is the compound of dibutyl tin dilaurate and methylimidazole
The mass ratio of object, organotin and methylimidazole is 0.1:1.
Specific preparation process is as follows:
(1) by apply easily happy DS-172 type dispersing agent be add to deionized water be made into 2% aqueous solution, then by granulated carbon
SiClx and two-dimensional sheet boron nitride sequentially add in above-mentioned aqueous solution, granular silicon carbide and two-dimensional sheet boron nitride and aqueous solution
Total mass ratio is 10:100, and dispersion 30min is sufficiently stirred, and then adds graphene and continues to stir 30min.Then it filters, wash
Wash to obtain heat filling complex.
(2) in above-mentioned heat filling complex and formula 10% methyltrimethoxysilane (0.5 part) is added to and is ground
20min is ground in grinding machine, obtains modified heat filling complex.
(3) by hydroxyl endblocked polydimethylsiloxane, dimethicone, modified filler complex, glycerine, methyl trimethoxy
Oxysilane (4.5 parts), 1010 type antioxidants, catalyst are added sequentially in kneader, at room temperature vacuum kneading, vacuum
Degree -0.06-0.1MPa, kneading time 30min obtain one pack system heat conduction organosilicon adhesive.
The solidification temperature of gained heat conduction organosilicon adhesive is 105 DEG C, and it is 5.28W/mK that thermal coefficient is measured after solidification.
Embodiment 2.
A kind of high heat conduction organosilicon adhesive, including 100 parts of hydroxyl endblocked polydimethylsiloxane, dimethicone 30
Part, 60 parts of heat filling, 10 parts of glycerine, 5 parts of methyltrimethoxysilane, 0.2 part of 1010 type antioxidant, catalyst 0.5
Part.Wherein, heat filling includes the mixture of silicon carbide, boron nitride and graphene, and the mass ratio of three is silicon carbide: nitridation
Boron: graphene=2:18:0.8, the silicon carbide is 1.5 microns of the granular carborundum granularity of zero dimension, boron nitride is two-dimensional sheet nitrogen
Change boron thickness and is less than 20nm, graphene thickness less than 1nm；Catalyst is the compound of dibutyl tin dilaurate and methylimidazole
The mass ratio of object, organotin and methylimidazole is 0.1:1.
The preparation method is the same as that of Example 1, and the solidification temperature of gained heat conduction organosilicon adhesive is 107 DEG C, measures and leads after solidification
Hot coefficient is 5.43W/mK.
Embodiment 3.
A kind of high heat conduction organosilicon adhesive, including 100 parts of hydroxyl endblocked polydimethylsiloxane, dimethicone 25
Part, 60 parts of heat filling, 10 parts of glycerine, 5 parts of methyltrimethoxysilane, 0.2 part of 1010 type antioxidant, catalyst 0.8
Part.Wherein, heat filling includes the mixture of silicon carbide, boron nitride and graphene, and the mass ratio of three is silicon carbide: nitridation
Boron: graphene=3:15:0.8, the silicon carbide is 1.5 microns of the granular carborundum granularity of zero dimension, boron nitride is two-dimensional sheet nitrogen
Change boron thickness and is less than 20nm, graphene thickness less than 1nm；Catalyst is the compound of diethoxy dihexyl tin and methylimidazole
The mass ratio of object, organotin and methylimidazole is 0.3:1.
The preparation method is the same as that of Example 1.The solidification temperature of gained heat conduction organosilicon adhesive is 102 DEG C, measures and leads after solidification
Hot coefficient is 5.36W/mK.
Embodiment 4.
A kind of high heat conduction organosilicon adhesive, including 100 parts of hydroxyl endblocked polydimethylsiloxane, dimethicone 25
Part, 80 parts of heat filling, 10 parts of glycerine, 5 parts of methyltrimethoxysilane, 0.2 part of 1010 type antioxidant, catalyst 0.8
Part.Wherein, heat filling includes the mixture of silicon carbide, boron nitride and graphene, and the mass ratio of three is silicon carbide: nitridation
Boron: graphene=4:15:0.9, the silicon carbide is 1.5 microns of the granular carborundum granularity of zero dimension, boron nitride is two-dimensional sheet nitrogen
Change boron thickness and is less than 20nm, graphene thickness less than 1nm；Catalyst is the compound of diethoxy dihexyl tin and methylimidazole
The mass ratio of object, organotin and methylimidazole is 0.3:1.
The preparation method is the same as that of Example 1.The solidification temperature of gained heat conduction organosilicon adhesive is 102 DEG C, measures and leads after solidification
Hot coefficient is 5.88W/mK.
Embodiment 5.
A kind of high heat conduction organosilicon adhesive, including 100 parts of hydroxyl endblocked polydimethylsiloxane, dimethicone 25
Part, 60 parts of heat filling, 8 parts of diethylene glycol, 3 parts of vinyltriethoxysilane, 0.2 part of 1010 type antioxidant, catalysis
0.8 part of agent.Wherein, heat filling includes the mixture of silicon carbide, boron nitride and graphene, and the mass ratio of three is silicon carbide:
Boron nitride: graphene=3:15:0.8, the silicon carbide is 1.5 microns of the granular carborundum granularity of zero dimension, boron nitride is two-dimensional slice
Shape boron nitride thickness is less than 20nm, graphene thickness is less than 1nm；Catalyst is answering for dibutyl tin dilaurate and methylimidazole
The mass ratio of conjunction object, organotin and methylimidazole is 0.1:1.
Specific preparation process is as follows:
(1) by apply easily happy DS-172 type dispersing agent be add to deionized water be made into 2% aqueous solution, then by granulated carbon
SiClx and two-dimensional sheet boron nitride sequentially add in above-mentioned aqueous solution, granular silicon carbide and two-dimensional sheet boron nitride and aqueous solution
Total mass ratio is 10:100, and dispersion 30min is sufficiently stirred, and then adds graphene and continues to stir 30min.Then it filters, wash
Wash to obtain heat filling complex.
(2) in above-mentioned heat filling complex and formula 20% vinyltriethoxysilane (0.6 part) is added to
20min is ground in grinder, obtains modified heat filling complex.
(3) by hydroxyl endblocked polydimethylsiloxane, dimethicone, modified filler complex, diethylene glycol, ethylene
Ethyl triethoxy silicane alkane (2.4 parts), 1010 type antioxidants, catalyst are added sequentially in kneader, at room temperature vacuum kneading,
Vacuum degree -0.06-0.1MPa, kneading time 20min obtain one pack system heat conduction organosilicon adhesive.
The solidification temperature of gained heat conduction organosilicon adhesive is 105 DEG C, and it is 5.17W/mK that thermal coefficient is measured after solidification.
Embodiment 6.
A kind of high heat conduction organosilicon adhesive, including 100 parts of hydroxyl endblocked polydimethylsiloxane, dimethicone 25
Part, 65 parts of heat filling, 8 parts of 1,4-butanediol, 4 parts of ethyl orthosilicate, 0.2 part of DNP type antioxidant, 0.8 part of catalyst.Its
In, heat filling includes the mixture of silicon carbide, boron nitride and graphene, and the mass ratio of three is silicon carbide: boron nitride: graphite
Alkene=3:15:0.8, the silicon carbide is 1.5 microns of the granular carborundum granularity of zero dimension, boron nitride is two-dimensional sheet boron nitride thickness
It is less than 1nm less than 20nm, graphene thickness；Catalyst is the compound of dibutyl tin dilaurate and methylimidazole, organotin
Mass ratio with methylimidazole is 0.1:1.
Specific preparation process is as follows:
(1) by apply easily happy DS-172 type dispersing agent be add to deionized water be made into 2% aqueous solution, then by granulated carbon
SiClx and two-dimensional sheet boron nitride sequentially add in above-mentioned aqueous solution, granular silicon carbide and two-dimensional sheet boron nitride and aqueous solution
Total mass ratio is 10:100, and dispersion 30min is sufficiently stirred, and then adds graphene and continues to stir 30min.Then it filters, wash
Wash to obtain heat filling complex.
(2) in above-mentioned heat filling complex and formula 15% ethyl orthosilicate (0.6 part) is added in grinder
25min is ground, modified heat filling complex is obtained.
(3) by hydroxyl endblocked polydimethylsiloxane, dimethicone, modified filler complex, 1,4-butanediol, positive silicon
Acetoacetic ester (3.4 parts), DNP type antioxidant, catalyst are added sequentially in kneader, at room temperature vacuum kneading, vacuum degree-
0.06-0.1MPa, kneading time 30min obtain one pack system heat conduction organosilicon adhesive.
The solidification temperature of gained heat conduction organosilicon adhesive is 105 DEG C, and it is 5.64W/mK that thermal coefficient is measured after solidification.
Comparative example
For comparative example referring to the formula system of Patent No. CN2015108153207, specific formula is alcoxyl by weight
40 parts of base terminated polysiloxane, 1 part of methyl hydrogen polysiloxanes, 0.8 part of rare-earth coupling agent, 0.6 part of platinum catalyst, alkynol class
0.2 part, NBR9 parts, 0.4 part of zinc stearate, 1 part of antioxidant 264,20 parts of magnesia, 39 parts of chromium carbide.Obtained one pack system
The thermal coefficient of organosilicon heat-conducting glue is 3.36W/mK.
It is analyzed through the foregoing embodiment with comparative example, it can be found that heat conduction organosilicon adhesive prepared by the present invention can be shown
It writes and improves its heat transfer efficiency.
The foregoing is merely presently preferred embodiments of the present invention, is not intended to limit the invention, it is all in spirit of the invention and
Within principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (7)
1. a kind of high heat conduction organosilicon adhesive, including 100 parts of hydroxyl endblocked polydimethylsiloxane, dimethicone 20-45
Part, 60-90 parts of heat filling, 1-15 parts of toughener, 0.1-5 parts of coupling agent, 0.1-1 parts of antioxidant, 0.5-1 parts of catalyst；
It is characterized in that, the heat filling includes the mixture of silicon carbide, boron nitride and graphene, the mass ratio of three is carbonization
Silicon: boron nitride: graphene=1-5:15-20:0.5-1, the silicon carbide are that the granular carborundum granularity of zero dimension is 1.5 microns, nitrogen
Changing boron is that two-dimensional sheet boron nitride thickness is less than 20nm, graphene thickness less than 1 nanometer.
2. according to right want 1 described in a kind of high heat conduction organosilicon adhesive, which is characterized in that the catalyst be organotin with
The mass ratio of the compound of methylimidazole, organotin and methylimidazole is 0.1-0.5:1.
3. according to right want 2 described in a kind of high heat conduction organosilicon adhesive, which is characterized in that the organotin include two laurels
Sour dibutyl tin, tin dilaurate diamyl alkene, tin dilaurate dihexyl alkene, dimethoxy dibutyl alkene, diethoxy dihexyl
One of tin, diethoxy dioctyl tin, dibutoxy dihexyl tin, dipropoxy dibutyl alkene or a variety of mixtures.
4. according to right want 1 described in a kind of high heat conduction organosilicon adhesive, which is characterized in that the toughener includes the third three
One of alcohol, diethylene glycol, 1,3-BDO, 1,4-butanediol or a variety of mixtures.
5. according to right want 1 described in a kind of high heat conduction organosilicon adhesive, which is characterized in that the coupling agent be it is silane coupled
Agent, including methyltrimethoxysilane, dimethyldimethoxysil,ne, vinyltrimethoxysilane, vinyl triethoxyl
The mixture of one or more of silane, ethyl orthosilicate.
6. according to right want 1 described in a kind of high heat conduction organosilicon adhesive, which is characterized in that the antioxidant trade mark includes
1010,9701,264,168,1076, one of DNP, CA or a variety of mixtures.
7. the preparation method of heat conduction organosilicon adhesive described in any one of claims 1-6, specific preparation process is as follows:
(1) painting easily happy DS-172 type dispersing agent is add to deionized water to the aqueous solution for being made into 1-5%, then by granular carbonization
Silicon and two-dimensional sheet boron nitride sequentially add in above-mentioned aqueous solution, and dispersion 20-60min is sufficiently stirred, then adds graphene
Continue to stir 20-60min, is then filtered, washed to obtain heat filling complex；
(2) above-mentioned heat filling complex and silane coupling agent are added in grinder and grind 20-30min, must be modified thermally conductive
Filler complex.The mass ratio of the filler complex and silane coupling agent is 100:0.1-5；
(3) by hydroxyl endblocked polydimethylsiloxane, dimethicone, modified filler complex, toughener, coupling agent, antioxygen
Agent, catalyst are added sequentially in kneader, and vacuum kneading 10-50min obtains one pack system heat conduction organosilicon adhesive at room temperature.
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| CN115216267B (en) * | 2022-08-16 | 2023-08-22 | 西卡(江苏)工业材料有限公司 | Environment-friendly high-adhesion high-thermal-conductivity organic silicon pouring sealant and preparation method and application thereof |
| CN115433380A (en) * | 2022-09-03 | 2022-12-06 | 东莞市零度导热材料有限公司 | Manufacturing process of low-volatility heat conducting fin |
| CN115873500A (en) * | 2022-12-28 | 2023-03-31 | 中国海洋石油集团有限公司 | Graphene heat-conducting adhesive and preparation method and application thereof |
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