CN107974232B - LED chip insulating heat-conducting die bond adhesive and preparation method thereof - Google Patents
LED chip insulating heat-conducting die bond adhesive and preparation method thereof Download PDFInfo
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- CN107974232B CN107974232B CN201711442544.3A CN201711442544A CN107974232B CN 107974232 B CN107974232 B CN 107974232B CN 201711442544 A CN201711442544 A CN 201711442544A CN 107974232 B CN107974232 B CN 107974232B
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- 239000000853 adhesive Substances 0.000 title claims abstract description 46
- 230000001070 adhesive effect Effects 0.000 title claims abstract description 46
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 238000002156 mixing Methods 0.000 claims abstract description 41
- 239000013078 crystal Substances 0.000 claims abstract description 37
- 239000000463 material Substances 0.000 claims abstract description 37
- 239000007787 solid Substances 0.000 claims abstract description 37
- 229920005989 resin Polymers 0.000 claims abstract description 30
- 239000011347 resin Substances 0.000 claims abstract description 30
- 238000011049 filling Methods 0.000 claims abstract description 26
- 239000003054 catalyst Substances 0.000 claims abstract description 23
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 19
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 19
- 239000000945 filler Substances 0.000 claims description 36
- 239000003292 glue Substances 0.000 claims description 31
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical group [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 20
- 239000006185 dispersion Substances 0.000 claims description 18
- 239000003822 epoxy resin Substances 0.000 claims description 18
- 229920000647 polyepoxide Polymers 0.000 claims description 18
- RAXXELZNTBOGNW-UHFFFAOYSA-N imidazole Natural products C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 claims description 17
- -1 imidazole compound Chemical class 0.000 claims description 16
- 229920002545 silicone oil Polymers 0.000 claims description 14
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical group [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 claims description 13
- 238000003756 stirring Methods 0.000 claims description 13
- 229910052582 BN Inorganic materials 0.000 claims description 11
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 11
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 11
- 229920001296 polysiloxane Polymers 0.000 claims description 11
- 229910052710 silicon Inorganic materials 0.000 claims description 11
- 239000010703 silicon Substances 0.000 claims description 11
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 11
- 229920002554 vinyl polymer Polymers 0.000 claims description 11
- 229910052739 hydrogen Inorganic materials 0.000 claims description 10
- 239000001257 hydrogen Substances 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 10
- 229910052697 platinum Inorganic materials 0.000 claims description 10
- 239000007822 coupling agent Substances 0.000 claims description 9
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 8
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 8
- 125000002723 alicyclic group Chemical group 0.000 claims description 7
- PXKLMJQFEQBVLD-UHFFFAOYSA-N bisphenol F Chemical compound C1=CC(O)=CC=C1CC1=CC=C(O)C=C1 PXKLMJQFEQBVLD-UHFFFAOYSA-N 0.000 claims description 6
- LXBGSDVWAMZHDD-UHFFFAOYSA-N 2-methyl-1h-imidazole Chemical compound CC1=NC=CN1 LXBGSDVWAMZHDD-UHFFFAOYSA-N 0.000 claims description 5
- MWSKJDNQKGCKPA-UHFFFAOYSA-N 6-methyl-3a,4,5,7a-tetrahydro-2-benzofuran-1,3-dione Chemical compound C1CC(C)=CC2C(=O)OC(=O)C12 MWSKJDNQKGCKPA-UHFFFAOYSA-N 0.000 claims description 5
- ZCUJYXPAKHMBAZ-UHFFFAOYSA-N 2-phenyl-1h-imidazole Chemical compound C1=CNC(C=2C=CC=CC=2)=N1 ZCUJYXPAKHMBAZ-UHFFFAOYSA-N 0.000 claims description 4
- 239000004841 bisphenol A epoxy resin Substances 0.000 claims description 4
- 150000008064 anhydrides Chemical group 0.000 claims description 3
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 claims description 3
- LTVUCOSIZFEASK-MPXCPUAZSA-N (3ar,4s,7r,7as)-3a-methyl-3a,4,7,7a-tetrahydro-4,7-methano-2-benzofuran-1,3-dione Chemical compound C([C@H]1C=C2)[C@H]2[C@H]2[C@]1(C)C(=O)OC2=O LTVUCOSIZFEASK-MPXCPUAZSA-N 0.000 claims description 2
- FBHPRUXJQNWTEW-UHFFFAOYSA-N 1-benzyl-2-methylimidazole Chemical compound CC1=NC=CN1CC1=CC=CC=C1 FBHPRUXJQNWTEW-UHFFFAOYSA-N 0.000 claims description 2
- ULKLGIFJWFIQFF-UHFFFAOYSA-N 5K8XI641G3 Chemical compound CCC1=NC=C(C)N1 ULKLGIFJWFIQFF-UHFFFAOYSA-N 0.000 claims description 2
- JLTDJTHDQAWBAV-UHFFFAOYSA-N N,N-dimethylaniline Chemical compound CN(C)C1=CC=CC=C1 JLTDJTHDQAWBAV-UHFFFAOYSA-N 0.000 claims description 2
- BBKXDHBLPBKCFR-FDGPNNRMSA-L beryllium;(z)-4-oxopent-2-en-2-olate Chemical compound [Be+2].C\C([O-])=C\C(C)=O.C\C([O-])=C\C(C)=O BBKXDHBLPBKCFR-FDGPNNRMSA-L 0.000 claims description 2
- FJDJVBXSSLDNJB-LNTINUHCSA-N cobalt;(z)-4-hydroxypent-3-en-2-one Chemical compound [Co].C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O FJDJVBXSSLDNJB-LNTINUHCSA-N 0.000 claims description 2
- 239000000835 fiber Substances 0.000 claims description 2
- ANSXAPJVJOKRDJ-UHFFFAOYSA-N furo[3,4-f][2]benzofuran-1,3,5,7-tetrone Chemical compound C1=C2C(=O)OC(=O)C2=CC2=C1C(=O)OC2=O ANSXAPJVJOKRDJ-UHFFFAOYSA-N 0.000 claims description 2
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims description 2
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 2
- 239000000395 magnesium oxide Substances 0.000 claims description 2
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 2
- VYKXQOYUCMREIS-UHFFFAOYSA-N methylhexahydrophthalic anhydride Chemical compound C1CCCC2C(=O)OC(=O)C21C VYKXQOYUCMREIS-UHFFFAOYSA-N 0.000 claims description 2
- 229920002050 silicone resin Polymers 0.000 claims 2
- 239000004842 bisphenol F epoxy resin Substances 0.000 claims 1
- 238000000034 method Methods 0.000 description 12
- 230000000052 comparative effect Effects 0.000 description 9
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 8
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 8
- 230000008569 process Effects 0.000 description 8
- 238000012360 testing method Methods 0.000 description 7
- 239000011231 conductive filler Substances 0.000 description 5
- 238000009413 insulation Methods 0.000 description 4
- 239000004408 titanium dioxide Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 2
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- 239000004332 silver Substances 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical group [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 239000003365 glass fiber Substances 0.000 description 1
- 239000004519 grease Substances 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000009775 high-speed stirring Methods 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 238000007781 pre-processing Methods 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 230000008646 thermal stress Effects 0.000 description 1
Classifications
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- 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
- 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
- C09J163/00—Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
-
- 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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
-
- 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
- C08K2201/011—Nanostructured additives
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/20—Applications use in electrical or conductive gadgets
-
- 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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention belongs to the technical field of adhesives, and particularly relates to an LED chip insulating heat-conducting solid crystal adhesive and a preparation method thereof. The specially-made heat-conducting filling material is formed by mixing heat-conducting filling materials with different shapes, such as a needle shape, a sheet shape or a spherical shape, the needle-shaped heat-conducting filling material and the spherical heat-conducting filling material are pre-mixed with a certain amount of connecting agent, so that the needle-shaped heat-conducting filling material and the spherical heat-conducting filling material are connected with each other to form a certain three-dimensional structure, and then the needle-shaped heat-conducting filling material and the spherical heat-conducting filling material are mixed with resin, a cross-linking agent, a catalyst, an adhesive and the like, so that the distance between the heat-conducting filling materials does not exist within a certain range, the heat-conducting coefficient is high, the using.
Description
Technical Field
The invention belongs to the technical field of adhesives, and particularly relates to an LED chip insulating heat-conducting solid crystal adhesive and a preparation method thereof.
Background
Compared with incandescent lamps and fluorescent lamps, the LED lamp has lower energy consumption and longer service life, and can realize intelligent control, so the LED lamp has very wide application market. According to incomplete statistics, the LED capacity of China in 2010 is more than 700 billion yuan, and the LED capacity is increased by 7 times in 2013, so that the LED power generation method is widely applied to various places such as industry, families, offices and the like.
In the application process of the prior LED lamp, as partial light energy of a chip of the LED lamp is converted into heat energy in the light emitting process, the use temperature of the chip is overhigh, a junction temperature phenomenon is formed, and the luminous flux and the service life of the LED lamp are seriously influenced; meanwhile, in the working process, due to the repeated heating junction temperature of the chip, each module of the LED lamp can continuously experience thermal circulation, and due to different materials of different modules, the thermal expansion coefficients of the different modules can also be different, so that interlayer thermal stress is generated, the materials of the modules are warped, cracked and stripped, and the like, and then the LED lamp fails, so that the phenomenon of lamp death is generated. LED lamps therefore require a better heat dissipation system to avoid chip junction temperatures.
At present, a heat conduction path of an LED lamp mainly comprises a chip, a solid crystal adhesive, a bracket and heat conduction silicone grease, and heat generated by the chip can be dissipated into the air through the path in a heat conduction mode, so that the LED chip keeps a stable working environment in the use process, the junction temperature of the chip is avoided, and a better application effect is achieved. The importance of the solid crystal glue is self-evident because the solid crystal glue is the first gateway of the heat conducting system and directly determines the success or failure of the heat conducting performance.
At present, the heat-conducting solid crystal glue is generally formed by mixing heat-conducting filling materials, resin, dispersing agents and adhesives, and mainly comprises two main directions: the insulating solid crystal glue and the conductive silver glue have certain difference in the application direction. The conductive silver adhesive is mainly used for heat conduction and electric conduction as the name suggests, is usually applied to a vertical structure and can also be applied to a horizontal structure, but has the hidden danger of electric leakage when being applied in a large range; the insulating die bond adhesive can be used for heat conduction and is mainly applied to horizontal structures. At present, the heat conduction filler of the insulating solid crystal glue is mainly alumina, aluminum nitride, boron nitride and the like, the heat conductivity coefficient of the heat conduction filler is concentrated on 50-200W/(M.K), the heat conductivity coefficient of the insulating solid crystal glue added with a certain amount of heat conduction filler is concentrated on 0.3-0.5W/(M.K), and the heat conductivity coefficient is low, but if the heat conduction filler is added too much, although the heat conductivity of the insulating solid crystal glue can be improved, the viscosity of the insulating solid crystal glue is higher, the bonding force is reduced, and the application effect of the insulating solid crystal glue is limited.
The general using method of the heat-conducting filler is to directly mix the heat-conducting filler with resin, a cross-linking agent, a catalyst, an adhesive and the like, and the mixture is uniformly dispersed under a high-speed stirring process, so that the prepared insulating solid crystal glue is uniformly dispersed in the internal heat-conducting filler, but in a microscopic state, the distance between the heat-conducting fillers still exists and is full of a resin matrix, the heat conduction efficiency is poor, although the distance between the fillers can be shortened by adding the using amount of the heat-conducting filler, the purpose of increasing the conduction efficiency is achieved, the heat-conducting filler is limited by the overall viscosity of the glue, so that the heat conduction addition amount of the heat-conducting filler is limited, and the difference between the heat conduction coefficient of the general insulating solid crystal glue.
In summary, the conventional insulating die attach adhesive has a low thermal conductivity, and when too much heat conductive filler is added to the insulating die attach adhesive, the heat conductive system of the insulating die attach adhesive can be improved due to the absence of a proper heat conductive filler, but the viscosity of the insulating die attach adhesive is high, the bonding force is reduced, and the application effect of the insulating die attach adhesive is limited. Therefore, it is very necessary to develop a new LED chip insulating die attach adhesive and a preparation method thereof.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a preparation method of a glass fiber reinforced heat conducting gasket.
The technical scheme for solving the technical problems is as follows: an LED chip insulation heat conduction solid crystal glue comprises the following components in parts by weight: 40-80 parts of resin, 25-85 parts of cross-linking agent, 0.1-0.3 part of catalyst, 1-10 parts of adhesive and 50-200 parts of specially-made heat-conducting filler.
Further, the resin is epoxy resin or organic silicon resin.
Furthermore, the epoxy resin is one or more of bisphenol A type epoxy resin E54, E51, E44, bisphenol F type epoxy resin or alicyclic epoxy resin.
Wherein the molecular formula of the bisphenol F type epoxy resin is as follows:
the molecular formula of the alicyclic epoxy resin is as follows:
furthermore, the organic silicon resin is polysiloxane and is prepared by mixing the component a and the component b according to a molar ratio of 1: 1, mixing;
the molecular formula of the component a is as follows:
wherein
Is composed of
The molecular formula of the component b is as follows:
further, the kind of the crosslinking agent corresponds to the kind of the resin.
Furthermore, when the resin is epoxy resin, the cross-linking agent is anhydride curing agent, imidazole curing agent or BF3A quasi-complex.
Preferably, the crosslinking agent is methyltetrahydrophthalic anhydride, methylhexahydrophthalic anhydride, methylnadic anhydride, pyromellitic anhydride, 2-methylimidazole, 2-ethyl-4-methylimidazole, 2-phenylimidazole, BF3-monoethylamine, BF3-benzylamine or BF3One or more than two of dimethylaniline.
Furthermore, when the resin is organic silicon resin, the cross-linking agent is hydrogen-containing silicone oil or vinyl silicone oil; wherein,
the molecular formula of the hydrogen-containing silicone oil is as follows:
the molecular formula of the vinyl silicone oil is as follows:
further, the kind of the catalyst corresponds to the kind of the resin.
Furthermore, when the resin is epoxy resin, the catalyst is imidazole compound or tertiary amine carboxylate.
Preferably, the imidazole compound is 2-phenylimidazole or 1-benzyl-2-methylimidazole; the tertiary amine carboxylate is hydrated cobalt acetylacetonate or beryllium acetylacetonate.
Furthermore, when the resin is organic silicon resin, the catalyst is a platinum catalyst Karstedt, and the platinum content is 5000 ppm.
Further, the adhesive is nano titanium dioxide modified by a coupling agent; the method specifically comprises the following steps: mixing the nano titanium dioxide and the coupling agent by a dry method, and drying and storing; wherein the coupling agent is siloxane polymer (such as KH550, KH570, etc.) containing amino and vinyl at side chain or terminal chain, and the titanium dioxide is nano-scale titanium dioxide; the weight ratio of the coupling agent to the titanium dioxide is 0.1-2, and the coupling agent and the titanium dioxide are required to be uniformly mixed before use.
Further, the preparation method of the specially-made heat-conducting filler comprises the following steps: mixing the heat-conducting fillers with different shapes with 0.1-1 wt% of a connecting agent respectively to prepare different mixed materials; and adding the different mixed materials into a high-speed dispersion machine respectively, and stirring and mixing uniformly to prepare the special heat-conducting filler.
Wherein the heat-conducting filler is spherical alumina, spherical magnesium oxide, spherical aluminum nitride, acicular alumina, flaky boron nitride or boron nitride fiber.
The molecular formula of the connecting agent is as follows:
the preparation method of the LED chip insulating heat-conducting solid crystal glue comprises the following steps: adding 40-80 parts of resin, 25-85 parts of cross-linking agent, 0.1-0.3 part of catalyst and 1-10 parts of adhesive into a stirrer in sequence, uniformly mixing and stirring, then adding 50-200 parts of special heat-conducting filling mixture, uniformly mixing and stirring, and further uniformly mixing by using a centrifugal dispersion machine to obtain the insulating heat-conducting solid crystal glue.
The invention has the characteristics and beneficial effects that:
the specially-made heat-conducting filling material is formed by mixing heat-conducting filling materials with different shapes, such as a needle shape, a sheet shape or a spherical shape, the needle-shaped heat-conducting filling material and the spherical heat-conducting filling material are pre-mixed with a certain amount of connecting agent, so that the needle-shaped heat-conducting filling material and the spherical heat-conducting filling material are connected with each other to form a certain three-dimensional structure, and then the needle-shaped heat-conducting filling material and the spherical heat-conducting filling material are mixed with resin, a cross-linking agent, a catalyst, an adhesive and the like, so that the distance between the heat-conducting filling materials does not exist within a certain range, the heat-conducting coefficient is high, the using.
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.
Example 1
An LED chip insulation heat conduction solid crystal glue comprises the following components in parts by weight: 60 parts of vinyl-containing organic silicon polysiloxane resin, 35 parts of hydrogen-containing silicone oil cross-linking agent, 0.3 part of platinum catalyst Karstedt, 9 parts of nano titanium dioxide adhesive and 150 parts of special heat-conducting filler.
The preparation method of the LED chip insulating heat-conducting solid crystal glue comprises the following steps:
(1) preparation of specially-made heat-conducting filling material
a. Adding 100 parts of heat-conducting filler aluminum oxide (needle-shaped) into a high-speed dispersion machine, adding 1 part of a connecting agent, uniformly mixing, and hermetically storing;
b. adding 100 parts of heat-conducting filler hexagonal boron nitride (spherical) into a high-speed dispersion machine, adding 0.2 part of a connecting agent, uniformly mixing, and hermetically storing;
c. b, adding the alumina (needle-shaped) mixed material obtained in the step a into a high-speed dispersion machine, slowly adding the hexagonal boron nitride (spherical) mixed material obtained in the step b in the mixing process, and uniformly stirring and mixing at a high speed to obtain the specially-made heat-conducting filler;
(2) 60 parts of vinyl-containing organic silicon polysiloxane resin, 35 parts of hydrogen-containing silicone oil cross-linking agent, 0.3 part of platinum catalyst Karstedt and 9 parts of nano titanium dioxide adhesive are sequentially added into a stirrer to be uniformly mixed, then 150 parts of specially-made heat-conducting filler is added to be slowly stirred and mixed, and the mixture is further uniformly mixed by a centrifugal dispersion machine after being uniformly mixed to prepare the insulating solid crystal glue.
Example 2
An LED chip insulation heat conduction solid crystal glue comprises the following components in parts by weight: 80 parts of vinyl-containing organic silicon polysiloxane resin, 45 parts of hydrogen-containing silicone oil cross-linking agent, 0.2 part of platinum catalyst Karstedt, 8 parts of nano titanium dioxide adhesive and 120 parts of special heat-conducting filler.
The preparation method of the LED chip insulating heat-conducting solid crystal glue comprises the following steps:
(1) preparation of specially-made heat-conducting filling material
a. Adding 50 parts of heat-conducting filler aluminum oxide (flake), adding 0.5 part of connecting agent, uniformly mixing, and hermetically storing;
b. adding 100 parts of heat-conducting filler hexagonal boron nitride (spherical) into a high-speed dispersion machine, adding 0.2 part of a connecting agent, uniformly mixing, and hermetically storing;
c. b, adding the aluminum oxide (flaky) mixed material obtained in the step a into a high-speed dispersion machine, slowly adding the hexagonal boron nitride (spherical) mixed material obtained in the step b in the mixing process, and uniformly stirring and mixing at a high speed to obtain the specially-made heat-conducting filler;
(2) adding 80 parts of vinyl organic silicone polysiloxane resin, 45 parts of hydrogen-containing silicone oil cross-linking agent, 0.2 part of platinum catalyst Karstedt and 8 parts of nano titanium dioxide adhesive into a stirrer in sequence, uniformly mixing and stirring, then adding 120 parts of specially-made heat-conducting filler, slowly stirring and mixing, further uniformly mixing by a centrifugal dispersion machine after uniformly mixing, and preparing the insulating solid crystal glue.
Example 3
An LED chip insulation heat conduction solid crystal glue comprises the following components in parts by weight: 40 parts of E51 bisphenol A epoxy resin, 40 parts of alicyclic epoxy resin, 85 parts of methyl tetrahydrophthalic anhydride, 0.2 part of 2-methylimidazole catalyst, 5 parts of nano titanium dioxide adhesive and 180 parts of special heat-conducting filler.
The preparation method of the LED chip insulating heat-conducting solid crystal glue comprises the following steps:
(1) preparation of specially-made heat-conducting filling material
a. Adding 100 parts of heat-conducting filler aluminum oxide (needle-shaped) into a high-speed dispersion machine, adding 1 part of a connecting agent, uniformly mixing, and hermetically storing;
b. adding 100 parts of heat-conducting filler alumina (spherical) into a high-speed dispersion machine, adding 1 part of a connecting agent, uniformly mixing, and hermetically storing;
c. adding the alumina (needle-shaped) mixed material obtained in the step a into a high-speed dispersion machine, slowly adding the alumina (spherical) mixed material obtained in the step b in the mixing process, and uniformly stirring and mixing at a high speed to obtain the specially-made heat-conducting filler;
(2) adding 40 parts of E51 bisphenol A epoxy resin, 40 parts of alicyclic epoxy resin, 85 parts of methyl tetrahydrophthalic anhydride, 0.2 part of 2-methylimidazole catalyst and 5 parts of nano titanium dioxide adhesive into a stirrer in sequence, uniformly mixing and stirring, then adding 180 parts of special heat-conducting filler, slowly stirring and mixing, uniformly mixing, and further uniformly mixing by using a centrifugal dispersion machine to prepare the insulating solid crystal glue.
Comparative example 1
60 parts of vinyl-containing organic silicon polysiloxane resin, 35 parts of hydrogen-containing silicone oil cross-linking agent, 0.3 part of platinum catalyst Karstedt and 9 parts of nano titanium dioxide adhesive are sequentially added into a stirrer to be uniformly mixed, 75 parts of aluminum oxide (needle) and 75 parts of hexagonal boron nitride (spherical) are added to be slowly stirred and mixed, and the materials are further uniformly mixed by a centrifugal dispersion machine after being uniformly mixed to prepare the insulating solid crystal glue.
Comparative example 2
Adding 80 parts of vinyl-containing organic silicone polysiloxane resin, 45 parts of hydrogen-containing silicone oil cross-linking agent, 0.2 part of platinum catalyst Karstedt and 8 parts of nano titanium dioxide adhesive into a stirrer in sequence, uniformly mixing, adding 40 parts of aluminum oxide (flake) and 80 parts of hexagonal boron nitride (sphere), slowly stirring and mixing, further uniformly mixing by a centrifugal dispersion machine after uniformly mixing, and preparing the insulating solid crystal glue.
Comparative example 3
Adding 40 parts of E51 bisphenol A epoxy resin, 40 parts of alicyclic epoxy resin, 85 parts of methyl tetrahydrophthalic anhydride, 0.2 part of 2-methylimidazole catalyst and 5 parts of coupling agent modified nano titanium dioxide adhesive into a stirrer in sequence, uniformly mixing, adding 180 parts of alumina (spherical), slowly stirring and mixing, and further uniformly mixing by a centrifugal dispersion machine to obtain the insulating solid crystal glue.
The insulating die bond adhesives of examples 1-3 and comparative examples 1-3 were tested, test one: testing viscosity by adopting AR-G2 equipment and a conical plate rotor at the rotating speed of 10rpm and the temperature of 25 ℃; and (2) testing: a thrust test, namely adhering a 2 x 2mm silicon wafer to an aluminum substrate by adopting insulating die attach adhesive, and testing the thrust value when the silicon wafer is pushed away; and (3) testing: and placing the insulating die-bonding adhesive on a specific mould, preparing a sample plate with the same thickness, and testing the heat conductivity coefficient of the sample plate.
TABLE 1 Performance index Table
| Performance index ﹨ sample | Example 1 | Example 2 | Example 3 | Comparative example 1 | Comparative example 2 | Comparative example 3 |
| Viscosity (Pa. s) | 13 | 10 | 8 | 28 | 24 | 11 |
| Thrust (Kg) | 5.4 | 6.1 | 6.5 | 2.3 | 2.8 | 5.6 |
| Thermal conductivity W/(M. K) | 0.80 | 0.73 | 0.85 | 0.35 | 0.30 | 0.38 |
As can be seen from table 1, in example 3, compared with comparative example 3, it can be seen that, after the heat conductive fillers with different shapes are mixed into the insulating solid crystal glue, the change in viscosity and thrust performance is not large under the same usage amount, but the heat conductivity coefficients of the heat conductive fillers with different shapes are far larger than that of a single heat conductive filler; the comparison between examples 1 and 2 and comparative examples 1 and 2 shows that the same type and amount of heat-conducting material is adopted, however, after the special heat-conducting filling material is prepared by pre-processing the heat-conducting mixture, the influence on the viscosity and the thrust performance is found to be large, and the heat conductivity coefficient can be obviously increased.
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 (10)
1. The LED chip insulating heat-conducting solid crystal adhesive is characterized by comprising the following components in parts by weight: 40-80 parts of resin, 25-85 parts of cross-linking agent, 0.1-0.3 part of catalyst, 1-10 parts of adhesive and 50-200 parts of specially-made heat-conducting filler;
the resin is epoxy resin or organic silicon resin;
the preparation method of the special heat-conducting filling material comprises the following steps: mixing the heat-conducting fillers with different shapes with 0.1-1 wt% of a connecting agent respectively to prepare different mixed materials; adding the different mixed materials into a high-speed dispersion machine respectively, and stirring and mixing uniformly to prepare the special heat-conducting filler;
the molecular formula of the connecting agent is as follows:
2. the LED chip insulating and heat conducting solid crystal adhesive according to claim 1, wherein when the resin is epoxy resin, the cross-linking agent is anhydride curing agent, imidazole curing agent or BF (BF) curing agent3A quasi-complex; the catalyst is imidazole compound or tertiary amine carboxylate.
3. The LED chip insulating and heat conducting die attach adhesive according to claim 2, wherein the epoxy resin is one or a mixture of two or more of bisphenol A epoxy resin E54, E51, E44, bisphenol F epoxy resin and alicyclic epoxy resin;
the anhydride curing agent is one or the mixture of more than two of methyl tetrahydrophthalic anhydride, methyl hexahydrophthalic anhydride, methyl nadic anhydride or pyromellitic anhydride;
the imidazole curing agent is one or a mixture of more than two of 2-methylimidazole, 2-ethyl-4-methylimidazole or 2-phenylimidazole;
the BF described3The complex is BF3-monoethylamine, BF3-benzylamine or BF3-one or a mixture of two or more of dimethylaniline;
the imidazole compound is 2-phenylimidazole or 1-benzyl-2-methylimidazole; the tertiary amine carboxylate is hydrated cobalt acetylacetonate or beryllium acetylacetonate.
4. The LED chip insulating and heat conducting die attach adhesive according to claim 3, wherein the bisphenol F type epoxy resin has a molecular formula:
the molecular formula of the alicyclic epoxy resin is as follows:
5. the LED chip insulating and heat conducting solid crystal adhesive according to claim 1, wherein when the resin is a silicone resin, the cross-linking agent is hydrogen-containing silicone oil or vinyl silicone oil;
the catalyst is a platinum catalyst Karstedt, and the platinum content is 5000 ppm.
6. The LED chip insulating and heat conducting solid crystal glue according to claim 5, wherein the silicone resin is polysiloxane, and the component a and the component b are mixed according to a molar ratio of 1: 1, mixing;
the molecular formula of the component a is as follows:
wherein
Is composed of
The molecular formula of the component b is as follows:
the molecular formula of the hydrogen-containing silicone oil is as follows:
the molecular formula of the vinyl silicone oil is as follows:
7. the LED chip insulating and heat conducting die attach adhesive according to claim 1, wherein the adhesive is nano titanium dioxide modified by a coupling agent; the weight ratio of the coupling agent to the nano titanium dioxide is 0.1-2.
8. The LED chip insulating and heat conducting die attach adhesive according to claim 7, wherein the coupling agent is KH550 or KH 570.
9. The LED chip insulating and heat conducting solid crystal glue according to claim 7, wherein the heat conducting filler is spherical aluminum oxide, spherical magnesium oxide, spherical aluminum nitride, needle-shaped aluminum oxide, flaky boron nitride or boron nitride fiber.
10. The preparation method of the LED chip insulating heat-conducting solid crystal adhesive according to claim 1, wherein 40-80 parts of resin, 25-85 parts of cross-linking agent, 0.1-0.3 part of catalyst and 1-10 parts of adhesive are sequentially added into a stirrer, mixed and stirred uniformly, then 50-200 parts of special heat-conducting filling mixture is added, stirred and mixed uniformly, and further mixed uniformly by a centrifugal dispersion machine to prepare the insulating heat-conducting solid crystal adhesive.
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| CN109294514A (en) * | 2018-09-29 | 2019-02-01 | 烟台德邦先进硅材料有限公司 | A kind of LED chip organosilicon crystal-bonding adhesive |
| CN109735235A (en) * | 2019-01-07 | 2019-05-10 | 冯欢心 | A kind of thermally conductive high refractive index LED transparent epoxy resin casting glue and preparation method thereof |
| CN109837058A (en) * | 2019-02-23 | 2019-06-04 | 冯欢心 | A kind of high refractive index thermally conductive LED transparent organic silicon casting glue and preparation method thereof |
| CN109852337A (en) * | 2019-02-23 | 2019-06-07 | 冯欢心 | A kind of LED transparent organic silicon casting glue of high refractive index high viscosity and preparation method thereof |
| KR102164171B1 (en) * | 2019-04-26 | 2020-10-13 | (주)엘프스 | self-assembled conductive bonding paste for mini LED chip bonding, mini LED chip-circuit board bondig module comprising the same and manufacturing method thereof |
| CN110922937B (en) * | 2019-11-19 | 2021-12-07 | 烟台德邦科技股份有限公司 | Organosilicon heat-conducting encapsulating silica gel with excellent performance |
| CN110903793A (en) * | 2019-11-22 | 2020-03-24 | Tcl华星光电技术有限公司 | Frame sealing adhesive material and liquid crystal display panel |
| CN114806077B (en) * | 2021-01-18 | 2023-05-26 | 万华化学集团股份有限公司 | Epoxy resin composition and preparation method and application thereof |
| CN114213979B (en) * | 2021-11-10 | 2023-09-05 | 中科检测技术服务(重庆)有限公司 | Electronic material glue solution and preparation method thereof |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104263299A (en) * | 2014-09-01 | 2015-01-07 | 上海三思电子工程有限公司 | Single-component epoxy thermal conductive adhesive and preparation method thereof |
| CN104479623A (en) * | 2014-12-03 | 2015-04-01 | 湖南皓志科技股份有限公司 | Normal-temperature solidified organic silicon pouring sealant having high thermal conductivity |
| CN106634809A (en) * | 2016-12-06 | 2017-05-10 | 烟台德邦先进硅材料有限公司 | Anti-poisoning anti-sedimentation high-cohesiveness thermal conductive silica gel for LED (Light-Emitting Diode) power supply packaging |
| CN106753210A (en) * | 2016-12-09 | 2017-05-31 | 烟台德邦先进硅材料有限公司 | A kind of heat conduction is bonded silica gel |
| CN106753207A (en) * | 2015-11-20 | 2017-05-31 | 烟台史密得机电设备制造有限公司 | A kind of preparation of high thermal conductivity casting glue |
| KR20170114184A (en) * | 2016-04-05 | 2017-10-13 | 주식회사 에이치알에스 | Liquid silicone addition type adhesive composition |
-
2017
- 2017-12-27 CN CN201711442544.3A patent/CN107974232B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104263299A (en) * | 2014-09-01 | 2015-01-07 | 上海三思电子工程有限公司 | Single-component epoxy thermal conductive adhesive and preparation method thereof |
| CN104479623A (en) * | 2014-12-03 | 2015-04-01 | 湖南皓志科技股份有限公司 | Normal-temperature solidified organic silicon pouring sealant having high thermal conductivity |
| CN106753207A (en) * | 2015-11-20 | 2017-05-31 | 烟台史密得机电设备制造有限公司 | A kind of preparation of high thermal conductivity casting glue |
| KR20170114184A (en) * | 2016-04-05 | 2017-10-13 | 주식회사 에이치알에스 | Liquid silicone addition type adhesive composition |
| CN106634809A (en) * | 2016-12-06 | 2017-05-10 | 烟台德邦先进硅材料有限公司 | Anti-poisoning anti-sedimentation high-cohesiveness thermal conductive silica gel for LED (Light-Emitting Diode) power supply packaging |
| CN106753210A (en) * | 2016-12-09 | 2017-05-31 | 烟台德邦先进硅材料有限公司 | A kind of heat conduction is bonded silica gel |
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