CN103409041A - Application of flexible thermal conductive insulation adhesive on LED (Light Emitting Diode) heat dissipation substrate - Google Patents
Application of flexible thermal conductive insulation adhesive on LED (Light Emitting Diode) heat dissipation substrate Download PDFInfo
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- 238000009413 insulation Methods 0.000 title claims abstract description 58
- 239000000853 adhesive Substances 0.000 title claims abstract description 50
- 230000001070 adhesive effect Effects 0.000 title claims abstract description 50
- 230000017525 heat dissipation Effects 0.000 title abstract description 8
- 239000000758 substrate Substances 0.000 title abstract 5
- 239000003822 epoxy resin Substances 0.000 claims abstract description 40
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 40
- 239000000463 material Substances 0.000 claims abstract description 39
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 26
- 238000002360 preparation method Methods 0.000 claims abstract description 18
- 239000007822 coupling agent Substances 0.000 claims abstract description 14
- 238000005096 rolling process Methods 0.000 claims abstract description 14
- 239000003960 organic solvent Substances 0.000 claims abstract description 13
- 238000001035 drying Methods 0.000 claims abstract description 12
- 239000011248 coating agent Substances 0.000 claims abstract description 9
- 238000000576 coating method Methods 0.000 claims abstract description 9
- 239000007787 solid Substances 0.000 claims abstract description 8
- 239000004850 liquid epoxy resins (LERs) Substances 0.000 claims abstract description 4
- 239000011256 inorganic filler Substances 0.000 claims description 23
- 229910003475 inorganic filler Inorganic materials 0.000 claims description 23
- 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 claims description 22
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 20
- 239000012528 membrane Substances 0.000 claims description 18
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 15
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 12
- 239000000203 mixture Substances 0.000 claims description 12
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 239000003292 glue Substances 0.000 claims description 10
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 10
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 9
- 229910052582 BN Inorganic materials 0.000 claims description 8
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 8
- 150000001875 compounds Chemical class 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
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 8
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 8
- 229920000459 Nitrile rubber Polymers 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 7
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 claims description 6
- MQJKPEGWNLWLTK-UHFFFAOYSA-N Dapsone Chemical compound C1=CC(N)=CC=C1S(=O)(=O)C1=CC=C(N)C=C1 MQJKPEGWNLWLTK-UHFFFAOYSA-N 0.000 claims description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- 229960000860 dapsone Drugs 0.000 claims description 6
- 238000000465 moulding Methods 0.000 claims description 6
- -1 trimethylammonium hexanediamine Chemical compound 0.000 claims description 6
- YBRVSVVVWCFQMG-UHFFFAOYSA-N 4,4'-diaminodiphenylmethane Chemical compound C1=CC(N)=CC=C1CC1=CC=C(N)C=C1 YBRVSVVVWCFQMG-UHFFFAOYSA-N 0.000 claims description 4
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 4
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 4
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 claims description 4
- 239000005062 Polybutadiene Substances 0.000 claims description 3
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims description 3
- VOOLKNUJNPZAHE-UHFFFAOYSA-N formaldehyde;2-methylphenol Chemical compound O=C.CC1=CC=CC=C1O VOOLKNUJNPZAHE-UHFFFAOYSA-N 0.000 claims description 3
- 229920002857 polybutadiene Polymers 0.000 claims description 3
- 229910017083 AlN Inorganic materials 0.000 claims description 2
- PIGFYZPCRLYGLF-UHFFFAOYSA-N Aluminum nitride Chemical compound [Al]#N PIGFYZPCRLYGLF-UHFFFAOYSA-N 0.000 claims description 2
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 2
- XGULBQUJRQPLOG-OOOULUNWSA-N O([C@@H]1[C@@H](C)[C@H](O)CC(=O)O[C@@H]([C@H](/C=C(\C)/C=C/C(=O)[C@H](C)C[C@@H]1CC=O)COCC=1C=CC=CC=1)CC)[C@@H]1O[C@H](C)[C@@H](O)[C@H](N(C)C)[C@H]1O Chemical compound O([C@@H]1[C@@H](C)[C@H](O)CC(=O)O[C@@H]([C@H](/C=C(\C)/C=C/C(=O)[C@H](C)C[C@@H]1CC=O)COCC=1C=CC=CC=1)CC)[C@@H]1O[C@H](C)[C@@H](O)[C@H](N(C)C)[C@H]1O XGULBQUJRQPLOG-OOOULUNWSA-N 0.000 claims description 2
- 229920013649 Paracril Polymers 0.000 claims description 2
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 2
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims description 2
- 229910021502 aluminium hydroxide Inorganic materials 0.000 claims description 2
- 229910003460 diamond Inorganic materials 0.000 claims description 2
- 239000010432 diamond Substances 0.000 claims description 2
- 150000002460 imidazoles Chemical class 0.000 claims description 2
- 239000000395 magnesium oxide Substances 0.000 claims description 2
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 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
- 239000003921 oil Substances 0.000 claims description 2
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 2
- 229920002554 vinyl polymer Polymers 0.000 claims description 2
- 239000011787 zinc oxide Substances 0.000 claims description 2
- 239000002313 adhesive film Substances 0.000 abstract description 6
- 239000012790 adhesive layer Substances 0.000 abstract 1
- 238000013329 compounding Methods 0.000 abstract 1
- 239000002270 dispersing agent Substances 0.000 abstract 1
- 210000004379 membrane Anatomy 0.000 description 15
- 239000004593 Epoxy Substances 0.000 description 9
- 238000000034 method Methods 0.000 description 8
- 238000011056 performance test Methods 0.000 description 7
- 239000000243 solution Substances 0.000 description 6
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 5
- 229910052782 aluminium Inorganic materials 0.000 description 5
- STBLNCCBQMHSRC-BATDWUPUSA-N (2s)-n-[(3s,4s)-5-acetyl-7-cyano-4-methyl-1-[(2-methylnaphthalen-1-yl)methyl]-2-oxo-3,4-dihydro-1,5-benzodiazepin-3-yl]-2-(methylamino)propanamide Chemical compound O=C1[C@@H](NC(=O)[C@H](C)NC)[C@H](C)N(C(C)=O)C2=CC(C#N)=CC=C2N1CC1=C(C)C=CC2=CC=CC=C12 STBLNCCBQMHSRC-BATDWUPUSA-N 0.000 description 4
- 229940125878 compound 36 Drugs 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 238000001291 vacuum drying Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 238000004381 surface treatment Methods 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 239000002362 mulch Substances 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 239000006087 Silane Coupling Agent Substances 0.000 description 1
- 239000004902 Softening Agent Substances 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 150000004645 aluminates Chemical class 0.000 description 1
- 239000005030 aluminium foil Substances 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 210000002469 basement membrane Anatomy 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 239000011889 copper foil Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000010030 laminating Methods 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000003245 working effect Effects 0.000 description 1
Landscapes
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention relates to application of a flexible thermal conductive insulation adhesive on an LED (Light Emitting Diode) heat dissipation substrate, which comprises preparation of a flexible thermal conductive insulation adhesive and a flexible thermal conductive insulation adhesive film. The flexible thermal conductive insulation adhesive contains liquid epoxy resin, solid epoxy resin, a flexibilizer, a curing agent, a high thermal conductive inorganic filling material, an organic solvent, a coupling agent, a dispersing agent and a flatting agent. A preparation method of the flexible thermal conductive insulation adhesive film comprises the following steps of coating the flexible thermal conductive insulation adhesive on a release film through a coating machine, and roasting through a temperature control drying tunnel to prepare a flexible thermal conductive insulation adhesive layer for the LED heat dissipation substrate; and compounding the release film for covering on the adhesive surface, and rolling and forming to prepare the flexible thermal conductive insulation adhesive film for the LED heat dissipation substrate. The adhesive film disclosed by the invention is used for the LED heat dissipation substrate and has the characteristics of high heat dissipation, insulation, heat resistance, release intensity, flexible and the like.
Description
Technical field
The present invention is patent CN102676109A, and patent name is the division of " a kind of LED heat radiating material with the preparation method of flexible heat conductive insulating glued membrane ".Belong to macromolecule material preparation area.Relate to the application of a kind of flexible Heat Conductive Insulation Adhesive on the LED heat radiating material.
Background technology
Photodiode (LED) is as a kind of emerging product got most of the attention, and high brightness arranged, the advantages such as volume is little, the life-span is long, environmental protection and energy saving, has been widely used in the industries such as indoor and outdoor lighting, indicating meter light source, lamps for vehicle, backlight.Along with popularizing of LED application, the principal element and the technical bottleneck that restrict its development are heat dissipation problems.Improve LED luminous efficiency and work-ing life, solving LED product heat dissipation problem becomes one of most important problem of present stage.Exploitation for the flexible heat conductive insulating glued membrane of LED heat radiating material become in the urgent need to.
Flexibility coat copper plate (FCCL) with flexible thermal conductive insulation glue film preparation has the not available good characteristic of rigidity copper-clad plate, and it has also possessed advantage light, thin, deflection on the basis that has good electrical insulating property, high-cooling property, high heat resistance.Because the most of product of FCCL is to offer the user with continuous rolling form, therefore, adopt FCCL to produce flexible printed-circuit board (FPC) and be beneficial to the automatic continuous production that realizes FPC and the continuity surface mounting of carrying out components and parts on FPC.
At present, in domestic disclosed patent, CN101798439A has introduced a kind of conductive adhesive film, and this conductive adhesive film has no to describe possesses electrical insulating property.Though and mean to can be used for flexible sheet, in performance test, there is no the test data about flexibility.Patent CN201830544U has introduced a kind of heat-conducting covering film, and this mulch film is three-decker, one deck heat conductive insulating basement membrane, one deck heat conductive insulating glue-line and one deck release layer.This mulch film has certain insulativity and thermal conductivity, but complicated process of preparation.
Summary of the invention
The object of the invention is to the radiating requirements for LED, provide a kind of LED heat radiating material with flexible heat conductive insulating glued membrane.This LED heat radiating material is strong by flexible heat conductive insulating glued membrane snappiness, electrical insulating property is high, cohesiveness is strong, for the making of LED heat radiating material, can realize that high heat radiation, high-insulativity, deflection are high, the characteristics such as high heat resistance, high-peeling strength.
For achieving the above object, the invention provides a kind of flexible Heat Conductive Insulation Adhesive, comprise that component and mass fraction thereof are as follows:
Liquid epoxy resin, consumption 5.0-35 part, preferably 10-30 part;
Solid-state epoxy resin, consumption 15-65 part, preferably 20-60 part;
Toughner, consumption 5.0-55 part, preferably 10-50 part;
Solidifying agent, consumption 0.5-15 part, preferably 1.0-10 part;
High heat conduction inorganic filler, consumption 30-330 part, preferably 50-300 part;
Organic solvent, consumption 30-220 part, preferably 50-200 part;
Coupling agent, consumption 0.5-6.0 part, preferably 1.0-5.0 part;
Flow agent, consumption 0.05-2.5 part, preferably 0.1-2.0 part;
Wherein, described liquid-state epoxy resin is that the trade mark that Yueyang Ba Ling petrochemical industry epoxy resin division department produces is CYD-128: epoxy equivalent (weight) 184-194, E-44: epoxy equivalent (weight) 210-240, E-42: the bisphenol A type epoxy resin of epoxy equivalent (weight) 230-280, E-51 bisphenol A type epoxy resin, or the trade mark of Zhongyuan Science & Technology Chemical Industry Co., Ltd., Gaomi City is Oxiron2000: a kind of in the polybutadiene epoxy resin of epoxy equivalent (weight) 222-238.
Described solid epoxy resin is that the trade mark that Yueyang Ba Ling petrochemical industry epoxy resin division department produces is CYD-011: epoxy equivalent (weight) 450-500, CYD-014: epoxy equivalent (weight) 900-1000, CYD-017: the bisphenol A type epoxy resin of epoxy equivalent (weight) 1750-2100, or the trade mark that Yueyang Ba Ling petrochemical industry epoxy resin division department produces is A001-09: epoxy equivalent (weight) 195-210, CYDCN-100: a kind of in the o-cresol formaldehyde epoxy resin of epoxy equivalent (weight) 195-210.
Described toughner is carboxyl end of the liquid acrylonitrile-butadiene rubber CTBN1300 * 8, CTBN1300 * 13, CTBN1300 * 31, amino terminated liquid nitrile rubber ATBN1300 * 35, ATBN1300 * 16, one or more in end-vinyl paracril VTBN1300 * 33, VTBN1300 * 43, optional producer is U.S. Noveon company limited.
Described solidifying agent is a kind of in mphenylenediamine, dapsone, trimethylammonium hexanediamine, methylene dianiline (MDA) maleic anhydride phthalate anhydride, imidazoles.
In above-mentioned flexible Heat Conductive Insulation Adhesive, described high heat conduction inorganic filler is any one or more mixtures in aluminium nitride, boron nitride, silicon nitride, silicon carbide, norbide, aluminum oxide, magnesium oxide, zinc oxide, aluminium hydroxide, diamond, and its median size is 0.1 μ m-20 μ m.
Any one or more mixtures in the preferred boron nitride of described high heat conduction inorganic filler, silicon carbide, aluminum oxide, its median size are 1 μ m-15 μ m preferably.
Described coupling agent is silane coupling agent, the optional trade mark is KH550, KH560, KH570, optional producer is military organosilicon novel material company limited greatly, titanate coupling agent, the optional trade mark is TMC-101, TMC-201, TMC-102, and optional producer is that Guangzhou is polymerized to million industry organosilicon raw material company limiteds, aluminate coupling agent, the optional trade mark is HY-133, HY-1108, HY-988, and optional producer is that the Hangzhou Jesse blocks any one or more mixtures in chemical industry company limited.
The described flow agent trade mark is any one or more mixtures in H-142, H-140, H-1331, H-1330, H-1231, H-123.But being the Guangzhou Hensel, producer digests company limited.
Described organic solvent is one or more in dimethyl formamide, N,N-DIMETHYLACETAMIDE, ethyl acetate, butanone, acetone, toluene, dimethylbenzene, methyl alcohol, ethanol, tetrahydrofuran (THF), sherwood oil.
The preparation method of flexible Heat Conductive Insulation Adhesive of the present invention, its preparation process is as follows:
(1) high heat conduction inorganic filler is placed under 140 ℃-160 ℃ of vacuum drying ovens and vacuumizes and dry except moisture 2-4h, be cooled to room temperature; By proportional quantity, take high heat conduction inorganic filler in the aqueous ethanolic solution of the volumetric concentration 95% that is dissolved with coupling agent, heating in water bath to 40 ℃-80 ℃, after stirring 2-4h, filter, after absolute ethanol washing 2-6 time, in 60 ℃ of-100 ℃ of lower vacuum-drying 12-24h, grind, obtain surface treated high heat conduction inorganic filler, stand-by;
(2) press proportional quantity, epoxy resin, toughner, surface treated high heat conduction inorganic filler, solidifying agent, flow agent and organic solvent are mixed, ball grinding stirring 12h-24h at room temperature, fully be uniformly dispersed, the gained mixed solution removes by filter impurity by 300 mesh filter screens, namely obtains flexible Heat Conductive Insulation Adhesive.
A kind of LED heat radiating material of the present invention is with flexible heat conductive insulating glued membrane, adopt above-mentioned flexible Heat Conductive Insulation Adhesive to make: described LED heat radiating material comprises with flexible heat conductive insulating glued membrane: covering with release film, be coated on LED heat radiating material on separate-type paper or release film with flexible heat conductive insulating glue-line, and be covered in the LED heat radiating material with the release film on flexible heat conductive insulating glue-line.
Described LED heat radiating material with flexible heat conductive insulating glue film manufacturing process is: described flexible Heat Conductive Insulation Adhesive is coated on release film through coating machine, walking speed be under 8-10m/min after the baking of multi-control temperature section drying tunnel, obtain the LED heat radiating material made by described flexible Heat Conductive Insulation Adhesive with flexible heat conductive insulating glue-line, the temperature of described multi-control temperature section drying tunnel is respectively 55 ℃-60 ℃-70 ℃-75 ℃; Finally, in the compound covering release film of surface with glue, the moulding of compound release film continuous rolling, the continuous rolling mold temperature is 30 ℃-50 ℃, and linear pressure is 2-5MPa, and rolling-line speed is 8-10m/min; By above-mentioned steps, make the LED heat radiating material with flexible heat conductive insulating glued membrane.
Above-mentioned coating machine is coated on the thickness on release film and covers and is 10-60 μ m with release film thickness, and described flexible heat conductive insulating bondline thickness is 30-120 μ m.
The invention has the beneficial effects as follows: LED heat radiating material provided by the invention is with flexible heat conductive insulating glued membrane, snappiness is strong, electrical insulating property is high, cohesiveness is strong, making for the LED heat radiating material, can realize the characteristics such as high heat radiation, high-insulativity, deflection, high heat resistance, high-peeling strength.
Embodiment
Further illustrate by the following examples flexible Heat Conductive Insulation Adhesive of the present invention, and the LED heat radiating material prepared with flexible Heat Conductive Insulation Adhesive is with flexible heat conductive insulating glued membrane.But the present invention is not limited to these embodiment.
In following embodiment, each amounts of components related in flexible Heat Conductive Insulation Adhesive process for preparation is with reference to subordinate list 1, with the LED heat radiating material by the performance test results of the copper-clad plate of flexible thermal conductive insulation glue film preparation in Table 2.
Embodiment 1
High heat conduction inorganic filler is placed in to 140 ℃ of lower vacuumizing and drying of vacuum drying oven except moisture 4h, is cooled to room temperature; By proportional quantity, take high heat conduction inorganic filler in the aqueous ethanolic solution that is dissolved with coupling agent KH560 (ethanol concentration of volume percent 95%), heating in water bath to 40 ℃, after stirring 4h, filter, after absolute ethanol washing 2 times, in 60 ℃ of lower vacuum-drying 12h, pulverize to such an extent that surface treated high heat conduction inorganic filler is stand-by;
Select bisphenol A type epoxy resin E-44 as liquid-state epoxy resin, select bisphenol A type epoxy resin CYD-014 as solid epoxy resin, select CTBN1300 * 31 as toughner, select dapsone as solidifying agent, select the mixture (arbitrarily than) of aluminum oxide, boron nitride and silicon carbide as high heat conduction inorganic filler, select H-1331 as flow agent, select the mixing solutions of ethyl acetate, butanone and toluene (arbitrarily than) as organic solvent; Press proportional quantity epoxy resin, toughner, surface treated high heat conduction inorganic filler, solidifying agent, flow agent and organic solvent are mixed, stir 12h at room-temperature ball-milling, fully be uniformly dispersed; The gained mixed solution removes by filter impurity by 300 mesh filter screens, obtains flexible Heat Conductive Insulation Adhesive.
The flexible Heat Conductive Insulation Adhesive of gained is coated on 50 μ m release films through coating machine, walking speed be under 8m/min after the baking of multi-control temperature section drying tunnel, obtain by described flexible Heat Conductive Insulation Adhesive and make the LED heat radiating material with flexible heat conductive insulating glue-line, thickness is 50 μ m, and its multi-control temperature section drying tunnel temperature is respectively 55 ℃-60 ℃-70 ℃-75 ℃.Finally, cover and use release film in the compound 36 μ m of surface with glue, compound covering release film continuous rolling moulding, the continuous rolling mold temperature is 30 ℃, and linear pressure is 2MPa, and rolling-line speed is 8m/min.By above-mentioned steps, make the LED heat radiating material with flexible heat conductive insulating glued membrane.
The release film on flexible heat conductive insulating glued membrane surface is removed, with Procuring glue-line laminating 50 μ m aluminium foils and 35 μ m Copper Foils, pressed down 2min at 5MPa/175 ℃, in baking oven, solidify 1h under 170 ℃, make LED heat radiating material heat-conduction flexible aluminum base copper-clad plate.Its performance test results is in Table 2.
Embodiment 2
The surface treatment process of high heat conduction inorganic filler as described in example 1 above, replaces coupling agent with KH550.
Select bisphenol A type epoxy resin E-42 as liquid-state epoxy resin, select bisphenol A type epoxy resin CYD-011 as solid epoxy resin, select carboxyl end of the liquid acrylonitrile-butadiene rubber CTBN1300 * 8 as toughner, select dapsone as solidifying agent, select (arbitrarily than) mixture of aluminum oxide, boron nitride and silicon carbide as high heat conduction inorganic filler, select H-140 as flow agent, select the mixing solutions of ethyl acetate, tetrahydrofuran (THF) and dimethyl formamide (arbitrarily than) as organic solvent.The process for preparation of Heat Conductive Insulation Adhesive as described in example 1 above, flexible Heat Conductive Insulation Adhesive respectively fill a prescription consumption as shown in embodiment in table 12.
The flexible Heat Conductive Insulation Adhesive of gained is coated on 50 μ m release films through coating machine, walking speed be under 9m/min after the baking of multi-control temperature section drying tunnel, namely by described flexible Heat Conductive Insulation Adhesive, make the LED heat radiating material with flexible heat conductive insulating glue-line, thickness is 50 μ m, and its multi-control temperature section drying tunnel temperature is respectively 55 ℃-60 ℃-70 ℃-75 ℃; Finally, cover and use release film in the compound 36 μ m of surface with glue, compound covering release film continuous rolling moulding, the continuous rolling mold temperature is 30 ℃, and linear pressure is 3MPa, and rolling-line speed is 9m/min.By above-mentioned steps, make the LED heat radiating material with flexible heat conductive insulating glued membrane.
As described in example 1 above, its performance test results is in Table 2 for the preparation process of LED heat radiating material use heat-conduction flexible aluminum base copper-clad plate.
Embodiment 3
The surface treatment process of high heat conduction inorganic filler as described in example 1 above, replaces coupling agent with TMC-201.
Select polybutadiene epoxy resin Oxiron2000 as liquid-state epoxy resin, select o-cresol formaldehyde epoxy resin CYDCN-100 as solid epoxy resin, select amino terminated liquid nitrile rubber ATBN1300 * 35 as toughner, select dapsone as solidifying agent, select the mixture of aluminum oxide, boron nitride and silicon carbide (arbitrarily than) as high heat conduction inorganic filler, select H-1231 as flow agent, select the mixing solutions of acetone, tetrahydrofuran (THF) and dimethyl formamide (arbitrarily than) as organic solvent.The process for preparation of flexible Heat Conductive Insulation Adhesive as described in example 1 above, flexible Heat Conductive Insulation Adhesive respectively fill a prescription consumption as shown in embodiment in table 13.
The flexible Heat Conductive Insulation Adhesive of gained is coated on 50 μ m release films through coating machine, after walking speed is that under 10m/min, multi-control temperature section drying tunnel toasts through 55 ℃-60 ℃-70 ℃-75 ℃, namely by described flexible Heat Conductive Insulation Adhesive, make the LED heat radiating material with flexible heat conductive insulating glue-line, thickness is 50 μ m.Finally, cover and use release film in the compound 36 μ m of surface with glue, compound covering release film continuous rolling moulding, the continuous rolling mold temperature is 50 ℃, and linear pressure is 4MPa, and rolling-line speed is 10m/min.By above-mentioned steps, make the LED heat radiating material with flexible heat conductive insulating glued membrane.
As described in example 1 above, its performance test results is in Table 2 for the preparation process of LED heat radiating material use heat-conduction flexible aluminum base copper-clad plate.
Embodiment 4
The surface treatment process of high heat conduction inorganic filler as described in example 1 above, replaces coupling agent with HY-133.
Select bisphenol A type epoxy resin E-51 as liquid-state epoxy resin, select bisphenol A type epoxy resin CYD-017 as solid epoxy resin, select amino terminated liquid nitrile rubber ATBN1300 * 35 as toughner, select dapsone as solidifying agent, select the mixture of aluminum oxide, boron nitride and silicon carbide (arbitrarily than) as high heat conduction inorganic filler, select H-1231 as flow agent, select the mixing solutions of acetone, tetrahydrofuran (THF) and dimethyl formamide (arbitrarily than) as organic solvent.The process for preparation of flexible Heat Conductive Insulation Adhesive as described in example 1 above, flexible Heat Conductive Insulation Adhesive respectively fill a prescription consumption as shown in embodiment in table 14.
The flexible Heat Conductive Insulation Adhesive of gained is coated on 50 μ m release films through coating machine, after walking speed is that under 10m/min, multi-control temperature section drying tunnel toasts through 55 ℃-60 ℃-70 ℃-75 ℃, namely by described flexible Heat Conductive Insulation Adhesive, make the LED heat radiating material with flexible heat conductive insulating glue-line, thickness is 50 μ m.Finally, cover and use release film in the compound 36 μ m of surface with glue, compound covering release film continuous rolling moulding, the continuous rolling mold temperature is 50 ℃, and linear pressure is 4MPa, and rolling-line speed is 10m/min.By above-mentioned steps, make the LED heat radiating material with flexible heat conductive insulating glued membrane.
As described in example 1 above, its performance test results is in Table 2 for the preparation process of LED heat radiating material use heat-conduction flexible aluminum base copper-clad plate.
LED heat radiating material of the present invention, with flexible heat conductive insulating glued membrane, has high thermal conductivity coefficient, and prepared LED heat radiating material has the good characteristics such as high withstand voltage value, high-peeling strength, deflection, high insulation with flexible thermal conductivity aluminum matrix copper-clad plate.
The above, still can make various do not break away from distortion of the present invention and replacements based on technology contents of the present invention and technical characterstic for those skilled in the art.Therefore, protection scope of the present invention should be not limited to embodiment act person, and should comprise various do not break away from distortion of the present invention and replacements, and is contained by appended claims.Each amounts of components table (mass fraction) of the flexible Heat Conductive Insulation Adhesive of subordinate list table 1
Component | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 |
Liquid-state epoxy resin | 5 (parts) | 15 (parts) | 20 (parts) | 35 (parts) |
Solid epoxy resin | 65 (parts) | 45 (parts) | 30 (parts) | 15 (parts) |
Softening agent | 55 (parts) | 35 (parts) | 10 (parts) | 5 (parts) |
Solidifying agent | 15 (parts) | 10 (parts) | 5 (parts) | 5 (parts) |
High heat conduction inorganic filler | 30 (parts) | 100 (parts) | 250 (parts) | 330 (parts) |
Coupling agent | (0.5 part) | (1.5 part) | (4.0 part) | (6.0 part) |
Flow agent | (0.05 part) | (0.1 part) | (1.5 part) | (2.5 part) |
Organic solvent | 30 (parts) | 90 (parts) | 160 (parts) | 220 (parts) |
Subordinate list table 2 is with the performance test table of LED heat radiating material with the copper-clad plate of flexible thermal conductive insulation glue film preparation
Claims (11)
1. the application of a flexible Heat Conductive Insulation Adhesive, is characterized in that, described flexible Heat Conductive Insulation Adhesive comprise component and mass fraction as follows:
(1) liquid epoxy resin, consumption 5.0-35 part;
(2) solid-state epoxy resin, consumption 15-65 part;
(3) toughner, consumption 5.0-55 part;
(4) solidifying agent, consumption 0.5-15 part;
(5) high heat conduction inorganic filler, consumption 30-330 part;
(6) organic solvent, consumption 30-220 part;
(7) coupling agent, consumption 0.5-6.0 part;
(8) flow agent, consumption 0.05-2.5 part;
This flexible Heat Conductive Insulation Adhesive is used as the LED heat radiating material with flexible heat conductive insulating glued membrane, its membrane preparation method is: described flexible Heat Conductive Insulation Adhesive is coated on release film through coating machine, walking speed be under 8-10m/min after the baking of multi-control temperature section drying tunnel, obtain the LED heat radiating material made by described flexible Heat Conductive Insulation Adhesive with flexible heat conductive insulating glue-line, the temperature of described multi-control temperature section drying tunnel is respectively 55 ℃-60 ℃-70 ℃-75 ℃; Finally, in the compound covering release film of surface with glue, compound covering release film continuous rolling moulding, the continuous rolling mold temperature is 30 ℃-50 ℃, and linear pressure is 2-5MPa, and rolling-line speed is 8-10m/min; By above-mentioned steps, make the LED heat radiating material with flexible heat conductive insulating glued membrane.
2. the application of a kind of flexible Heat Conductive Insulation Adhesive as claimed in claim 1, is characterized in that, described flexible Heat Conductive Insulation Adhesive comprise component and mass fraction as follows:
(1) liquid epoxy resin, consumption 10-30 part;
(2) solid-state epoxy resin, consumption 20-60 part;
(3) toughner, consumption 10-50 part;
(4) solidifying agent, consumption 1.0-10 part;
(5) high heat conduction inorganic filler, consumption 50-300 part;
(6) organic solvent, consumption 50-200 part;
(7) coupling agent, consumption 1.0-5.0 part;
(8) flow agent, consumption 0.1-2.0 part.
3. the application of a kind of flexible Heat Conductive Insulation Adhesive as claimed in claim 1 is characterized in that: described liquid-state epoxy resin is that the trade mark is that CYD-128, E-44, E-42 or E-51 bisphenol A type epoxy resin or the trade mark are a kind of in the Oxiron2000 polybutadiene epoxy resin.
4. the application of a kind of flexible Heat Conductive Insulation Adhesive as claimed in claim 1 is characterized in that: described solid epoxy resin is that the trade mark is that CYD-011, CYD-014 or CYD-017 bisphenol A type epoxy resin or the trade mark are a kind of in the o-cresol formaldehyde epoxy resin of A001-09, CYDCN-100.
5. the application of a kind of flexible Heat Conductive Insulation Adhesive as claimed in claim 1, it is characterized in that: described toughner is carboxyl end of the liquid acrylonitrile-butadiene rubber CTBN1300 * 8, CTBN1300 * 13, CTBN1300 * 31, amino terminated liquid nitrile rubber ATBN1300 * 35, ATBN1300 * 16, one or more in end-vinyl paracril VTBN1300 * 33, VTBN1300 * 43.
6. the application of a kind of flexible Heat Conductive Insulation Adhesive as claimed in claim 1 is characterized in that: described solidifying agent is a kind of in mphenylenediamine, dapsone, trimethylammonium hexanediamine, methylene dianiline (MDA) maleic anhydride phthalate anhydride, imidazoles.
7. the application of a kind of flexible Heat Conductive Insulation Adhesive as claimed in claim 1, it is characterized in that: described high heat conduction inorganic filler is any one or more mixtures in aluminium nitride, boron nitride, silicon nitride, silicon carbide, norbide, aluminum oxide, magnesium oxide, zinc oxide, aluminium hydroxide, diamond, and its median size is 0.1 μ m-20 μ m.
8. the application of a kind of flexible Heat Conductive Insulation Adhesive as claimed in claim 1 is characterized in that: described high heat conduction inorganic filler is selected any one or more mixtures in boron nitride, silicon carbide, aluminum oxide, its median size 1 μ m-15 μ m.
9. the application of a kind of flexible Heat Conductive Insulation Adhesive as claimed in claim 1 is characterized in that: described coupling agent is that the trade mark is any one or more mixtures in KH550, KH560, KH570, TMC-101, TMC-201, TMC-102, HY-133, HY-1108, HY-988.
10. the application of a kind of flexible Heat Conductive Insulation Adhesive as claimed in claim 1 is characterized in that: described flow agent is that the trade mark is any one or more mixtures in H-142, H-140, H-1331, H-1330, H-1231, H-123.
11. the application of a kind of flexible Heat Conductive Insulation Adhesive as claimed in claim 1 is characterized in that: described organic solvent is one or more in dimethyl formamide, N,N-DIMETHYLACETAMIDE, ethyl acetate, butanone, acetone, toluene, dimethylbenzene, methyl alcohol, ethanol, tetrahydrofuran (THF), sherwood oil.
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