CN108102600A - A kind of high index of refraction LED packaging silicon rubbers of ultraviolet resistance and preparation method thereof - Google Patents
A kind of high index of refraction LED packaging silicon rubbers of ultraviolet resistance and preparation method thereof Download PDFInfo
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- CN108102600A CN108102600A CN201711104732.5A CN201711104732A CN108102600A CN 108102600 A CN108102600 A CN 108102600A CN 201711104732 A CN201711104732 A CN 201711104732A CN 108102600 A CN108102600 A CN 108102600A
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- 238000004806 packaging method and process Methods 0.000 title claims abstract description 28
- 229920002379 silicone rubber Polymers 0.000 title claims abstract description 27
- 230000006750 UV protection Effects 0.000 title claims abstract description 17
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims abstract description 21
- 229920002554 vinyl polymer Polymers 0.000 claims abstract description 21
- 239000003054 catalyst Substances 0.000 claims abstract description 17
- 239000004970 Chain extender Substances 0.000 claims abstract description 16
- 239000007767 bonding agent Substances 0.000 claims abstract description 15
- 239000003112 inhibitor Substances 0.000 claims abstract description 14
- 125000000113 cyclohexyl group Chemical group [H]C1([H])C([H])([H])C([H])([H])C([H])(*)C([H])([H])C1([H])[H] 0.000 claims abstract description 12
- -1 methylcyclohexyl vinyl Chemical group 0.000 claims description 53
- 229920001296 polysiloxane Polymers 0.000 claims description 25
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical group [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 20
- 229920002545 silicone oil Polymers 0.000 claims description 13
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 7
- 229910052697 platinum Inorganic materials 0.000 claims description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 3
- 239000004593 Epoxy Substances 0.000 claims description 2
- 229910020388 SiO1/2 Inorganic materials 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 239000001301 oxygen Substances 0.000 claims description 2
- 229910052760 oxygen Inorganic materials 0.000 claims description 2
- ZSIAUFGUXNUGDI-UHFFFAOYSA-N hexan-1-ol Chemical compound CCCCCCO ZSIAUFGUXNUGDI-UHFFFAOYSA-N 0.000 claims 2
- UAEPNZWRGJTJPN-UHFFFAOYSA-N methylcyclohexane Chemical compound CC1CCCCC1 UAEPNZWRGJTJPN-UHFFFAOYSA-N 0.000 claims 2
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 claims 1
- 239000003795 chemical substances by application Substances 0.000 claims 1
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 claims 1
- 230000005764 inhibitory process Effects 0.000 claims 1
- LAQFLZHBVPULPL-UHFFFAOYSA-N methyl(phenyl)silicon Chemical compound C[Si]C1=CC=CC=C1 LAQFLZHBVPULPL-UHFFFAOYSA-N 0.000 claims 1
- GYNNXHKOJHMOHS-UHFFFAOYSA-N methyl-cycloheptane Natural products CC1CCCCCC1 GYNNXHKOJHMOHS-UHFFFAOYSA-N 0.000 claims 1
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 24
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 abstract description 17
- 230000007774 longterm Effects 0.000 abstract description 8
- 239000011347 resin Substances 0.000 abstract description 6
- 229920005989 resin Polymers 0.000 abstract description 5
- 125000002723 alicyclic group Chemical group 0.000 abstract description 4
- 238000006243 chemical reaction Methods 0.000 abstract description 4
- 238000005336 cracking Methods 0.000 abstract description 4
- 230000001070 adhesive effect Effects 0.000 abstract description 3
- 239000000853 adhesive Substances 0.000 abstract description 2
- 238000006467 substitution reaction Methods 0.000 abstract description 2
- 238000010438 heat treatment Methods 0.000 description 9
- 230000000694 effects Effects 0.000 description 6
- 238000005538 encapsulation Methods 0.000 description 6
- QYLFHLNFIHBCPR-UHFFFAOYSA-N 1-ethynylcyclohexan-1-ol Chemical group C#CC1(O)CCCCC1 QYLFHLNFIHBCPR-UHFFFAOYSA-N 0.000 description 4
- 125000004836 hexamethylene group Chemical group [H]C([H])([*:2])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[*:1] 0.000 description 4
- 230000032683 aging Effects 0.000 description 3
- 239000011324 bead Substances 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 239000003822 epoxy resin Substances 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 229920000647 polyepoxide Polymers 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- GGBJHURWWWLEQH-UHFFFAOYSA-N butylcyclohexane Chemical compound CCCCC1CCCCC1 GGBJHURWWWLEQH-UHFFFAOYSA-N 0.000 description 2
- 239000003292 glue Substances 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000004026 adhesive bonding Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000007334 copolymerization reaction Methods 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 125000003700 epoxy group Chemical group 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000002464 physical blending Methods 0.000 description 1
- 230000004224 protection Effects 0.000 description 1
- 238000009738 saturating Methods 0.000 description 1
- 239000002210 silicon-based material Substances 0.000 description 1
- 150000003384 small molecules Chemical group 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 230000035882 stress Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- YUYCVXFAYWRXLS-UHFFFAOYSA-N trimethoxysilane Chemical compound CO[SiH](OC)OC YUYCVXFAYWRXLS-UHFFFAOYSA-N 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
- C09J11/06—Non-macromolecular additives organic
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/48—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor body packages
- H01L33/52—Encapsulations
- H01L33/56—Materials, e.g. epoxy or silicone resin
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
-
- 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
- C08L2203/206—Applications use in electrical or conductive gadgets use in coating or encapsulating of electronic parts
-
- 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
-
- 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
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Organic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Computer Hardware Design (AREA)
- Power Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Adhesives Or Adhesive Processes (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention belongs to high index of refraction LED packaging silicon rubbers of adhesive technical field more particularly to a kind of ultraviolet resistance and preparation method thereof.The LED packaging silicon rubbers of high index of refraction of the present invention are made of A, B component, component A provides resin, vinyl, catalyst and the bonding agent for improving intensity in the reaction, B component provides resin, chain extender, vinyl and the inhibitor for improving intensity, and the LED packaging silicon rubbers of high index of refraction of the present invention are instead of phenyl ring with alicyclic ring cyclohexyl.Under the long-term irradiation of ultraviolet light, the material containing substantial amounts of phenyl ring can absorb a large amount of ultraviolet lights, and unsaturated double-bond is caused to disconnect, and cause phenyl ring open loop, be in particular in xanthochromia of the material under ultraviolet light the long-term irradiation even cracking of material.And the substitution of alicyclic ring cyclohexyl, improve the UV resistance of product.
Description
Technical field
The invention belongs to adhesive technical field more particularly to a kind of ultraviolet resistance high index of refraction LED packaging silicon rubbers and
Its preparation method.
Background technology
With the development of power-type LED, epoxy resin has been unable to meet requirement, but its have as LED encapsulation material it is good
Good adhesive property, dielectric properties, and cheap, easy to operate, in view of the advantages of in organosilicon material performance and reduce into
The considerations of in sheet, makes modifying epoxy resin by organosilicon become numerous research directions by the method for physical blending and chemical copolymerization.
Its molecule chain flexibility can be improved by organosilicon material Toughening Modification of Epoxy, its internal stress is reduced, and then improve and open
Split problem；It is modified to improve the ageing-resistant of epoxy resin using the good heat resistance and strong ultraviolet resistance characteristic of organosilicon
Property, poor heat resistance, ultraviolet resistance the problems such as.
In recent years, the research hotspot of people be progressively transferred to high index of refraction, high transparency organosilicon encapsulating material on.Mesh
Before, the chip high refractive index of power-type LED, about 2.2, and the refractive index of common organosilicon encapsulating material is relatively low, about
1.4, the difference of refractive index is to taking light rate to have a great impact between them.It, can be at it when chip light emitting passes through encapsulating material
Total reflection effect occurs on interface, causes most light reverse reflected inside, can not effectively export, brightness efficiency directly by
Damage.In order to more effectively reduce the light loss that interfacial refraction is brought, efficiency of light extraction is improved as far as possible.It is required that organosilicon and lens material
The refractive index of material is as high as possible, therefore the LED organosilicon material for packaging of high refractive index transparent is to reducing chip and encapsulating material
Refractive index difference be vital.
Since phenyl ring has higher molar refraction and relatively small molecular volume, high index of refraction package material
Expect to study one of most ripe method based on phenyl type organosilicon material and at present.Some researches show that：Phenyl mass fraction
Bigger, the refractive index of organosilicon encapsulating material is higher, while also reduces the shrinking percentage of material, when phenyl mass fraction is 40%
The refractive index of silicon materials is 1.51, refractive index when phenyl content is 50%>1.54, refractive index is up to 1.57 during full phenyl；However, work as
During phenyl content excessively high (more than 50%), the light transmittance of encapsulating material can decline, and thermoplasticity is too big and product is made to lose using valency
Value, as W phenyl=20%-40%, the comprehensive performance of product is relatively best.
But the presence of a large amount of phenyl ring, a large amount of ultraviolet lights are easily absorbed, unsaturated double-bond is caused to disconnect, phenyl ring is caused to be opened
Ring, therefore high folding LED packaging silicon rubbers be there are can occur xanthochromia even to crack under ultraviolet light long-term irradiation, LED encapsulation material it is saturating
Light rate declines.And the LED lamp bead after encapsulating is present with the even dead lamp phenomenon of cracking under the irradiation of long-term UV, seriously affects
The luminous flux and service life of LED lamp bead.
The content of the invention
The present invention in view of the deficiency of the prior art, provides a kind of LED packaging silicon rubbers of high index of refraction, in purple
Xanthochromia and cracking phenomena does not occur under the long-term irradiation of outer light, suitable for the LED lamp bead of outdoor small-power long-term ultraviolet irradiation
Encapsulation.
The technical solution that the present invention solves above-mentioned technical problem is as follows：A kind of high index of refraction LED encapsulation silicon of ultraviolet resistance
Glue, component are 1 by weight by component A and B component:1 composition；
Wherein, the component A count in parts by weight including：50-60 parts of methylcyclohexyl vinyl polysiloxane, methyl ring
1-5 parts of 34-50 parts of hexyl vinyl silicone oil, 0.1-0.3 parts of platinum group catalyst and bonding agent；
The B component includes by weight percentage：50-60 parts of methylcyclohexyl vinyl polysiloxane, chain extender 39-
50 parts and 0.1-0.3 parts of inhibitor.
Wherein, the molecular formula of the methylcyclohexyl vinyl polysiloxane described in component A and B component is (ViMe2SiO1/2)
(CYMeSiO1/2)a(CYSiO3/2)b；Me is methyl, and Vi is vinyl, and CY is cyclohexyl, and the value range of a is 1-4, and b's takes
Value scope is 3-6.
Advantageous effect using above-mentioned further scheme is, as matrix resin, to be a kind of silicones, both contain vinyl
Cross-linking reaction is participated in, also improves product refractive index containing cyclohexyl, D in resinCYPresence can also improve the toughness of product.
Wherein, the molecular formula of methylcyclohexyl vinyl silicone oil described in component A is ViMe (CYSiO1/2)c；Me is first
Base, Vi are vinyl, and CY is cyclohexyl, and the value range of c is 5-45.
Advantageous effect using above-mentioned further scheme is that the addition of methylcyclohexyl vinyl silicone oil is provided and can joined
With the vinyl of reaction, and the viscosity of system is reduced, improve the toughness of system.
Wherein, the bonding agent described in component A is γ-glycidyl ether oxygen third containing epoxy group and alkoxy-functional
Base trimethoxy silane, structural formula are：
Wherein, the platinum group catalyst described in component A is platinum-methyl phenyl silicone complex or platinum-alkene cooperation
One kind in object.
Preferably, the platinum group catalyst described in component A is platinum-olefin complex, and platinum content is 3000~7000ppm.
Wherein, the chain extender described in B component is hydrogeneous Isosorbide-5-Nitrae-dimethyl-silicon butylcyclohexane, and molecular formula is
HMe2SiCYSiMe2H；Me is methyl, and CY is cyclohexyl.
Advantageous effect using above-mentioned further scheme is, as small molecule chain extender, to provide not only active hydrogen, hexamethylene
Base can improve whole system intensity and refractive index, and viscosity is low, and being played for whole system reduces viscosity, improves intensity
Effect.
Wherein, the inhibitor described in B component is ethynylcyclohexanol.
Second object of the present invention is the preparation side for the high index of refraction LED packaging silicon rubbers for providing above-mentioned ultraviolet resistance
Method, step are as follows：
(1) component A is prepared
Take the methylcyclohexyl vinyl polysiloxane, 34-50 parts of methylcyclohexyl vinyl silicon that parts by weight are 50-60 parts
Oil, 0.1-0.3 parts of platinum group catalysts and 1-5 parts of bonding agents, sequentially add in mixer, are mixed evenly to get component A；
(2) B component is prepared
Take the methylcyclohexyl vinyl polysiloxane, 39-50 parts of chain extenders and 0.1-0.3 parts that parts by weight are 50-60 parts
Inhibitor is sequentially added in mixer, is mixed evenly to get B component；
(3) it is 1 by weight by the component A of step (1), the B component of step (2):1 is uniformly mixed, vacuum defoamation 20-
40min, dispensing or encapsulating at a temperature of 100-120 DEG C on part to be packaged, heating 0.5-1.5h, then in 100-200 DEG C of temperature
Lower heating 3-5h cures.
The features of the present invention and advantageous effect are：
The LED packaging silicon rubbers of high index of refraction of the present invention are made of A, B component, and component A provides in the reaction improves intensity
Resin, vinyl, catalyst and bonding agent, B component provide resin, chain extender, vinyl and the inhibitor for improving intensity, this hair
The LED packaging silicon rubbers of bright high index of refraction are instead of phenyl ring with alicyclic ring cyclohexyl.Under the long-term irradiation of ultraviolet light, containing a large amount of
The material of phenyl ring can absorb a large amount of ultraviolet lights, unsaturated double-bond is caused to disconnect, causes phenyl ring open loop, is in particular in that material exists
The xanthochromia even cracking of material under ultraviolet light long-term irradiation.And the substitution of alicyclic ring cyclohexyl, improve the resistance to ultraviolet of product
Performance.
Specific embodiment
The principle of the present invention and feature are described below in conjunction with example, the given examples are served only to explain the present invention, and
It is non-to be used to limit the scope of the present invention.
Embodiment 1
A kind of high index of refraction LED packaging silicon rubbers of ultraviolet resistance, component are 1 by weight by component A and B component:1 group
Into；
Wherein, the component A count in parts by weight including：Methylcyclohexyl vinyl polysiloxane 50g, methylcyclohexyl
Vinyl silicone oil 48.9g, catalyst platinum-olefin complex 0.1g (platinum content 7000ppm) and bonding agent 1g；
The B component includes by weight percentage：Methylcyclohexyl vinyl polysiloxane 50g, chain extender hydrogeneous 1,
4- dimethyl-silicon butylcyclohexane 49.9g and inhibitor ethynylcyclohexanol 0.1g.
The preparation method of the high index of refraction LED packaging silicon rubbers of above-mentioned ultraviolet resistance, step are as follows：
(1) component A is prepared
Take parts by weight be the methylcyclohexyl vinyl polysiloxane of 50g, 48.9g methylcyclohexyls vinyl silicone oil,
0.1g catalyst platinums-olefin complex and 1g bonding agents, sequentially add in mixer, are mixed evenly to get component A；
(2) B component is prepared
Take the hydrogeneous 1,4- dimethyl silicon substrate of methylcyclohexyl vinyl polysiloxane, 49.9g chain extenders that parts by weight are 50g
Hexamethylene and 0.1g inhibitor ethynylcyclohexanols, sequentially add in mixer, are mixed evenly to get B component；
(3) it is 1 by weight by the component A of step (1), the B component of step (2):1 is uniformly mixed, vacuum defoamation
20min, dispensing or encapsulating at a temperature of 120 DEG C on part to be packaged, heating 1.0h, then heats 4h at a temperature of 150 DEG C, Gu
Change.
Embodiment 2
A kind of high index of refraction LED packaging silicon rubbers of ultraviolet resistance, component are 1 by weight by component A and B component:1 group
Into；
Wherein, the component A count in parts by weight including：Methylcyclohexyl vinyl polysiloxane 60g, methylcyclohexyl
Vinyl silicone oil 34.7g, catalyst platinum-olefin complex 0.3g (platinum content 7000ppm) and bonding agent 5g；
The B component includes by weight percentage：Methylcyclohexyl vinyl polysiloxane 60g, chain extender hydrogeneous 1,
4- dimethyl-silicon butylcyclohexane 39.7g and inhibitor ethynylcyclohexanol 0.3g.
The preparation method of the high index of refraction LED packaging silicon rubbers of above-mentioned ultraviolet resistance, step are as follows：
(1) component A is prepared
Take parts by weight be the methylcyclohexyl vinyl polysiloxane of 60g, 34.7g methylcyclohexyls vinyl silicone oil,
0.3g catalyst platinums-olefin complex and 5g bonding agents, sequentially add in mixer, are mixed evenly to get component A；
(2) B component is prepared
Take the hydrogeneous 1,4- dimethyl silicon substrate of methylcyclohexyl vinyl polysiloxane, 39.7g chain extenders that parts by weight are 60g
Hexamethylene and 0.3g inhibitor ethynylcyclohexanols, sequentially add in mixer, are mixed evenly to get B component；
(3) it is 1 by weight by the component A of step (1), the B component of step (2):1 is uniformly mixed, vacuum defoamation
20min, dispensing or encapsulating at a temperature of 120 DEG C on part to be packaged, heating 1.0h, then heats 4h at a temperature of 150 DEG C, Gu
Change.
Embodiment 3
A kind of high index of refraction LED packaging silicon rubbers of ultraviolet resistance, component are 1 by weight by component A and B component:1 group
Into；
Wherein, the component A count in parts by weight including：Methylcyclohexyl vinyl polysiloxane 55g, methylcyclohexyl
Vinyl silicone oil 41.8g, catalyst platinum-olefin complex 0.2g (platinum content 7000ppm) and bonding agent 3g；
The B component includes by weight percentage：Methylcyclohexyl vinyl polysiloxane 55g, chain extender hydrogeneous 1,
4- dimethyl-silicon butylcyclohexane 44.8g and inhibitor ethynylcyclohexanol 0.2g.
The preparation method of the high index of refraction LED packaging silicon rubbers of above-mentioned ultraviolet resistance, step are as follows：
(1) component A is prepared
Take parts by weight be the methylcyclohexyl vinyl polysiloxane of 55g, 41.8g methylcyclohexyls vinyl silicone oil,
0.2g catalyst platinums-olefin complex and 3g bonding agents, sequentially add in mixer, are mixed evenly to get component A；
(2) B component is prepared
Take the hydrogeneous 1,4- dimethyl silicon substrate of methylcyclohexyl vinyl polysiloxane, 44.8g chain extenders that parts by weight are 55g
Hexamethylene and 0.2g inhibitor ethynylcyclohexanols, sequentially add in mixer, are mixed evenly to get B component；
(3) it is 1 by weight by the component A of step (1), the B component of step (2):1 is uniformly mixed, vacuum defoamation
20min, dispensing or encapsulating at a temperature of 120 DEG C on part to be packaged, heating 1.0h, then heats 4h at a temperature of 150 DEG C, Gu
Change.
Comparative example 1
A kind of preparation method of LED packaging silicon rubbers, step are as follows：
(1) component A is prepared：Weigh methyl phenyl vinyl polysiloxane 55g, methyl phenyl vinyl silicone oil 41.8g, bonding
Agent 3g (structural formula) and catalyst platinum-methyl phenyl silicone complex 0.2g (platinum content 7000ppm), sequentially adds stirring
In machine, it is mixed evenly to get component A；
(2) B component is prepared：Weigh methyl phenyl vinyl polysiloxane 55g, chain extender methyl and phenyl hydrogen-containing silicon oil 44.8g,
Inhibitor 1,1,3- triphenyl -2- propine -1- alcohol 0.2g, sequentially adds in mixer, is mixed evenly to get B component；
(3) in use, being 1 by weight by component A, B component:1 proportioning is uniformly mixed, vacuum defoamation 20 minutes, point
Glue or encapsulating first when 120 DEG C of heating 1 are small, then when 150 DEG C of heating 4 are small, cure on part to be packaged.
By the A of embodiment 1,2,3 and comparative example 1, B component by weight 1:1 ratio weighs, and is then uniformly mixed, and takes off
Bubble 30 minutes, the gluing on glass slide, bondline thickness 1mm.Condition of cure：First when 120 DEG C of heating 1 are small, then in 150 DEG C of heating
4 it is small when.Test is put into ultraviolet ageing case and carries out ultraviolet ageing (10Mw/cm2), it is shown in Table 1.
Table 1
By embodiment in table 11,2,3 as can be seen that high compared to phenyl reflect compared with the test data of comparative example 1
Rate LED encapsulation material, cyclohexyl system high index of refraction LED encapsulation material have been improved on ultraviolet-resistant performance.
The foregoing is merely presently preferred embodiments of the present invention, is not intended to limit the invention, it is all the present invention spirit and
Within principle, any modifications, equivalent replacements and improvements are made should all be included in the protection scope of the present invention.
Claims (9)
1. a kind of high index of refraction LED packaging silicon rubbers of ultraviolet resistance, which is characterized in that its component by component A and B component by weight
Than for 1:1 composition；
Wherein, the component A count in parts by weight including：50-60 parts of methylcyclohexyl vinyl polysiloxane, methylcyclohexyl
1-5 parts of 34-50 parts of vinyl silicone oil, 0.1-0.3 parts of platinum group catalyst and bonding agent；
The B component includes by weight percentage：50-60 parts of methylcyclohexyl vinyl polysiloxane, 39-50 parts of chain extender
With 0.1-0.3 parts of inhibitor.
2. LED packaging silicon rubbers according to claim 1, which is characterized in that the methyl cyclohexane described in component A and B component
The molecular formula of base vinyl polysiloxane is (ViMe2SiO1/2)(CYMeSiO1/2)a(CYSiO3/2)b；
Wherein, Me is methyl, and Vi is vinyl, and CY is cyclohexyl, and the value range of a is 1-4, and the value range of b is 3-6.
3. LED packaging silicon rubbers according to claim 1, which is characterized in that the methylcyclohexyl vinyl described in component A
The molecular formula of silicone oil is ViMe (CYSiO1/2)c；
Wherein, Me is methyl, and Vi is vinyl, and CY is cyclohexyl, and the value range of c is 5-45.
4. LED packaging silicon rubbers according to claim 1, which is characterized in that the bonding agent described in component A is to contain epoxy
γ-glycidyl ether oxygen propyl trimethoxy silicane of base and alkoxy-functional, structural formula are：
5. LED packaging silicon rubbers according to claim 1, which is characterized in that platinum group catalyst described in component A for platinum-
One kind in methyl phenyl silicone complex or platinum-olefin complex.
6. LED packaging silicon rubbers according to claim 5, which is characterized in that platinum group catalyst described in component A for platinum-
Olefin complex, platinum content are 3000~7000ppm.
7. LED packaging silicon rubbers according to claim 1, which is characterized in that chain extender described in B component for hydrogeneous Isosorbide-5-Nitrae-
Dimethyl-silicon butylcyclohexane, molecular formula HMe2SiCYSiMe2H；
Wherein, Me is methyl, and CY is cyclohexyl.
8. LED packaging silicon rubbers according to claim 1, which is characterized in that the inhibitor described in B component is acetylene basic ring
Hexanol.
9. a kind of preparation method of the high index of refraction LED packaging silicon rubbers of any one of the claim 1-8 ultraviolet resistance, feature
It is, step is as follows：
(1) component A is prepared
Take parts by weight be 50-60 parts methylcyclohexyl vinyl polysiloxane, 34-50 parts of methylcyclohexyl vinyl silicone oils,
0.1-0.3 parts of platinum group catalysts and 1-5 parts of bonding agents, sequentially add in mixer, are mixed evenly to get component A；
(2) B component is prepared
Take the methylcyclohexyl vinyl polysiloxane, 39-50 parts of chain extenders and 0.1-0.3 parts of inhibition that parts by weight are 50-60 parts
Agent is sequentially added in mixer, is mixed evenly to get B component；
(3) it is 1 by weight by the component A of step (1), the B component of step (2):1 is uniformly mixed, vacuum defoamation 20-40min,
Dispensing or encapsulating heat 0.5-1.5h at a temperature of 100-120 DEG C, then are heated at a temperature of 100-200 DEG C on part to be packaged
3-5h cures.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110218456A (en) * | 2019-06-20 | 2019-09-10 | 广东信翼科技有限公司 | Cyclohexyl LED encapsulation material and preparation method thereof |
| CN112760079A (en) * | 2020-12-24 | 2021-05-07 | 烟台德邦科技股份有限公司 | High-refraction organic silicon packaging material and preparation method thereof |
| CN117625118A (en) * | 2023-11-28 | 2024-03-01 | 广东鼎立森新材料有限公司 | Preparation method of packaging glue for LED |
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| CN102627859A (en) * | 2011-01-17 | 2012-08-08 | 信越化学工业株式会社 | A silicone resin composition and an optical semiconductor device making use of the composition |
| CN106047278A (en) * | 2016-07-22 | 2016-10-26 | 烟台德邦先进硅材料有限公司 | High-refractive-index yellowing-resistant LED packaging silica gel |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102627859A (en) * | 2011-01-17 | 2012-08-08 | 信越化学工业株式会社 | A silicone resin composition and an optical semiconductor device making use of the composition |
| CN106047278A (en) * | 2016-07-22 | 2016-10-26 | 烟台德邦先进硅材料有限公司 | High-refractive-index yellowing-resistant LED packaging silica gel |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110218456A (en) * | 2019-06-20 | 2019-09-10 | 广东信翼科技有限公司 | Cyclohexyl LED encapsulation material and preparation method thereof |
| CN112760079A (en) * | 2020-12-24 | 2021-05-07 | 烟台德邦科技股份有限公司 | High-refraction organic silicon packaging material and preparation method thereof |
| CN117625118A (en) * | 2023-11-28 | 2024-03-01 | 广东鼎立森新材料有限公司 | Preparation method of packaging glue for LED |
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