CN107325783A - A kind of LED packaging silicon rubbers of high index of refraction high-transmittance high rigidity and preparation method thereof - Google Patents

A kind of LED packaging silicon rubbers of high index of refraction high-transmittance high rigidity and preparation method thereof Download PDF

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Publication number
CN107325783A
CN107325783A CN201710356261.0A CN201710356261A CN107325783A CN 107325783 A CN107325783 A CN 107325783A CN 201710356261 A CN201710356261 A CN 201710356261A CN 107325783 A CN107325783 A CN 107325783A
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parts
component
led packaging
refraction
transmittance
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董俊祥
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Yongcheng Polymer Material (changzhou) Co Ltd
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Yongcheng Polymer Material (changzhou) Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J183/00Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
    • C09J183/04Polysiloxanes
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02Non-macromolecular additives
    • C09J11/06Non-macromolecular additives organic
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/08Macromolecular additives
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L33/00Semiconductor 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
    • H01L33/48Semiconductor 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
    • H01L33/52Encapsulations
    • H01L33/56Materials, e.g. epoxy or silicone resin
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2203/00Applications
    • C08L2203/20Applications use in electrical or conductive gadgets
    • C08L2203/204Applications use in electrical or conductive gadgets use in solar cells
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/02Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
    • C08L2205/025Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/03Polymer mixtures characterised by other features containing three or more polymers in a blend
    • C08L2205/035Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Manufacturing & Machinery (AREA)
  • Computer Hardware Design (AREA)
  • Power Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)

Abstract

LED packaging silicon rubbers of a kind of high index of refraction high-transmittance high rigidity of the present invention and preparation method thereof include two kinds of components of AB, and the weight ratio of both components is A:B=1:2, wherein component A is included:Methyl phenyl vinyl polysiloxane, vinyl benzene based polyalcohol, the catalyst containing platinum, tackifier, inhibitor;B component is included:The hydrogeneous silicones of methyl phenyl vinyl polysiloxane, Vinylphenyl silicon resin, aminomethyl phenyl.A kind of LED packaging silicon rubbers of high index of refraction high rigidity prepared by the present invention have that refractive index is high, hardness is big, viscosity is easily adjusted, excellent heat resistance and the features such as to base material excellent caking property.

Description

A kind of LED packaging silicon rubbers of high index of refraction high-transmittance high rigidity and preparation method thereof
Technical field
The present invention relates to a kind of preparation method of the LED packaging silicon rubbers of high index of refraction high-transmittance high rigidity, specifically It is related to a kind of high index of refraction, high rigidity, high-adhesion, the LED packaging silicon rubbers of color inhibition, belongs to adhesive technical field.
Background technology
LED light emitting diodes are as new high-performance solid light-emitting component, with power consumption is small, operating voltage is low, luminous The advantages of efficiency high, small radiation, green non-pollution, the application field in illumination market is more and more wider, is increasingly becoming future The main flow lamp source of in the market, with boundless market prospects.
During LED component is produced, chip fabrication techniques, fluorescent material manufacturing technology, heat dissipation technology and package material The performance of material can all make a significant impact on its luminous efficiency, brightness and service life.Traditional packaging plastic uses epoxy Resin, the packaging plastic of this material have the shortcomings that it is obvious, such as be heated or ultraviolet irradiation after easily xanthochromia, internal stress it is big So that the fragility of material is big, shock resistance difference etc., therefore with the development of LED especially high-powered LED lamp, epoxy resin envelope It is difficult to meet the market demand to fill glue.The organic siliconresin packaging plastic resistance to purple stronger because the particularity of its molecular structure makes it have Outer aging, light transmittance is high, refractive index is high, be difficult the advantages of xanthochromia, shock resistance are good, in recent years gradually substituted epoxy resin into For the main product in LED packaging plastics market.
Organic siliconresin packaging plastic is due to resistance to ag(e)ing is good, light transmittance is high, refractive index is high, be difficult xanthochromia, using the longevity The advantages of ordering long, in recent years by numerous scholars and business research.Refractive index and transparency are higher, and interface light loss is fewer, so that LED luminous flux and light utilization efficiency can be improved, in addition, hardness is higher, heat endurance is higher, while hydroscopicity, raising can be reduced Sulfur resistance.Hardness is high, and internal stress easily ftractures greatly, cause in the market most of organic siliconresin packaging plastic hardness exist Below 55D.
There is provided a kind of packaging plastic preparation method of high refraction high intensity, Wen Zhong for Publication No. 103013431A patent Do not describe to improve hardness and the method for light transmittance.
The content of the invention
To solve problem above, the invention provides a kind of system of the LED packaging plastics of high index of refraction high grade of transparency high rigidity Preparation Method.
The technical solution adopted for the present invention to solve the technical problems is:
A kind of LED packaging silicon rubbers of high index of refraction high-transmittance high rigidity, include two kinds of components of A and B, the component A and B component Weight ratio be 1:2;
Wherein, the component A includes the raw material of following parts by weight:50 ~ 80 parts of methyl phenyl vinyl polysiloxane, ethenylphenyl 20 ~ 50 parts of silicones, 0.02 ~ 0.2 part of platinum catalyst, 1-4 parts of tackifier;0.01 ~ 0.05 part of inhibitor;The B component bag Include the raw material of following parts by weight:10 ~ 30 parts of methyl phenyl vinyl polysiloxane, 20 ~ 50 parts of Vinylphenyl silicon resin, methylbenzene 35 ~ 55 parts of the hydrogeneous silicones of base.
As a further improvement on the present invention, described methyl phenyl vinyl polysiloxane is the silicon tree containing MDT structures Fat, its molecular formula is:(ViMe2SiO1/2) x (PhSiO3/2) y (PhSiO) z, wherein, x values be 10 ~ 30, y values be 30 ~ 70, z values are that 20 ~ 50, Me is methyl, and Vi is vinyl, and Ph is phenyl.
As a further improvement on the present invention, described Vinylphenyl silicon resin molecular formula is to be divided into (ViMe2SiO1/ 2) x (PhSiO3/2) y, wherein x values are that 10 ~ 70, y values are 10-50;According to the difference of X and y values, it is arranged to two kinds of physics shapes State, one kind is solvent-laden mixture, and one kind is not solvent-laden polymer, wherein the solvent used in solvent-laden mixture is Toluene or dimethylbenzene, solid content is 30% ~ 70%.
As a further improvement on the present invention, described catalyst is platinum-methyl phenyl silicone complex, and platinum contains Amount is in 4000ppm ~ 7500ppm.
As a further improvement on the present invention, described tackifier are to contain phenyl, epoxy and acryloyl-oxy functional group Siloxanes ring body hydrating polymer.
As a further improvement on the present invention, described inhibitor is ethynylcyclohexanol or 1, the propine -1- of 1,3- triphenyl -2 One or both of alcohol.
As a further improvement on the present invention, described hydrogeneous silicones is the hydrogeneous polymer containing methyl and phenyl, Hydrogen content is 0.2% ~ 0.8%.
A kind of preparation method of the LED packaging silicon rubbers of high index of refraction high-transmittance high rigidity, the preparation process of the component A For:By weight fraction for 50 ~ 80 parts methyl phenyl vinyl polysiloxane, 20 ~ 50 parts of Vinylphenyl silicon resin, 0.02 ~ 0.2 part of platinum catalyst, 1 ~ 4 part of tackifier, 0.01 ~ 0.05 part of inhibitor, are sequentially added in stirring container, and stirring is equal 80 ~ 120 DEG C of decompressions are warming up to after even de- low 1 ~ 3 hour, produce the component A;The preparation process of the B component is:By weight Fraction is 10 ~ 30 parts of methyl phenyl vinyl polysiloxane, 20 ~ 50 parts of Vinylphenyl silicon resin, 35 ~ 55 parts of methylbenzene The hydrogeneous silicones of base, is sequentially added in stirring container, 80 ~ 120 DEG C of decompressions is warming up to after being stirred after stirring de- low by 1 ~ 3 Hour, produce the B component;Component A and B component are both needed to again enter after 80 DEG C ~ 120 DEG C decompressions remove solvent in de- low 1 ~ 3 hour Row married operation.
The beneficial effects of the invention are as follows:
Favourable using above-mentioned technical proposal shows as:LED packaging plastics prepared by the present invention are by A, B component according to 1:2 weight ratios Resin, vinyl, catalyst, inhibitor, the tackifier of example mixing, during the course of the reaction component A offer high intensity, B component are carried For the resin, vinyl, crosslinking agent of high intensity.The formula designed by the present invention, can improve the crosslink density that colloid reacts, So as to improve intensity and hardness after solidification.
Embodiment
In order that objects and advantages of the present invention are more clearly understood, traveling one is entered to the present invention below in conjunction with the present embodiment Step is described in detail, it will be appreciated that the specific embodiments described herein are merely illustrative of the present invention, is not used to limit this hair It is bright.
Embodiment 1
The preparation of component A:Weigh 70 parts of methyl phenyl vinyl polysiloxane, 26.9 parts of Vinylphenyl silicon resin, platinum catalysis 0.1 part of agent, 3 parts of tackifier, 0.02 part of inhibitor, are sequentially added in stirring container, and 80 ~ 120 DEG C are warming up to after stirring and is subtracted Pressure-off is low 1 ~ 3 hour, produces the component A;
The preparation of B component:Weigh 10 parts of methyl phenyl vinyl polysiloxane, 45 parts of Vinylphenyl silicon resin, 45 parts of first The hydrogeneous silicones of base phenyl, is sequentially added in stirring container, 80 ~ 120 DEG C of decompressions is warming up to after being stirred after stirring de- It is low 1 ~ 3 hour, produce the B component;
In use, by the component A and B component of above-mentioned preparation according to weight ratio 1:2 proportioning is well mixed, vacuum row bubble 30 ~ 60 Minute, it can also be warming up to 30 ~ 50 DEG C and stand nature row's bubble, when in colloid leaving no air bubbles inside post package to required component, first existing Heat 0.5 ~ 1 hour, then heated 2 ~ 3 hours at 150 DEG C at a temperature of 80 DEG C, be down to after room temperature and produce required product, product glues 4000mpa.s is spent, refractive index is 1.54, and transparency is 99.5%, and hardness is 72D, solidification is not ftractureed.
Embodiment 2
The preparation of component A:Weigh 80 parts of methyl phenyl vinyl polysiloxane, 18 parts of Vinylphenyl silicon resin, platinum catalyst 0.05 part, 2 parts of tackifier, 0.01 part of inhibitor, sequentially add in stirring container, 80 ~ 120 DEG C of decompressions be warming up to after stirring It is de- low 1 ~ 3 hour, produce the component A;
The preparation of B component:Weigh 10 parts of methyl phenyl vinyl polysiloxane, 46 parts of Vinylphenyl silicon resin, 44 parts of first The hydrogeneous silicones of base phenyl, is sequentially added in stirring container, 80 ~ 120 DEG C of decompressions is warming up to after being stirred after stirring de- It is low 1 ~ 3 hour, produce the B component;
In use, by the component A and B component of above-mentioned preparation according to weight ratio 1:2 proportioning is well mixed, vacuum row bubble 30 ~ 60 Minute, it can also be warming up to 30 ~ 50 DEG C and stand nature row's bubble, when in colloid leaving no air bubbles inside post package to required component, first existing Heat 0.5 ~ 1 hour, then heated 2 ~ 3 hours at 130 DEG C at a temperature of 70 DEG C, be down to after room temperature and produce required product, product glues 3500mpa.s is spent, refractive index is 1.545, and transparency is 99.5%, and hardness is 70D, solidification is not ftractureed.
Embodiment 3
The preparation of component A:Weigh 65 parts of methyl phenyl vinyl polysiloxane, 31.9 parts of Vinylphenyl silicon resin, platinum catalysis 0.1 part of agent, 3 parts of tackifier, 0.01 part of inhibitor, are sequentially added in stirring container, and 80 ~ 120 DEG C are warming up to after stirring and is subtracted Pressure-off is low 1 ~ 3 hour, produces the component A;
The preparation of B component:Weigh 20 parts of methyl phenyl vinyl polysiloxane, 40 parts of Vinylphenyl silicon resin, 40 parts of first The hydrogeneous silicones of base phenyl, is sequentially added in stirring container, 80 ~ 120 DEG C of decompressions is warming up to after being stirred after stirring de- It is low 1 ~ 3 hour, produce the B component;
In use, by the component A and B component of above-mentioned preparation according to weight ratio 1:2 proportioning is well mixed, vacuum row bubble 30 ~ 60 Minute, it can also be warming up to 30 ~ 50 DEG C and stand nature row's bubble, when in colloid leaving no air bubbles inside post package to required component, first existing Heat 0.5 ~ 1 hour, then heated 2 ~ 3 hours at 150 DEG C at a temperature of 70 DEG C, be down to after room temperature and produce required product, product glues It is 1.54 to spend 4600mpa.s refractive indexes, and transparency is 99.5%, and hardness is 68D, and solidification is not ftractureed.
Described above is only some embodiments of the present invention, every formula range described in the claims in the present invention Inside belong to protection category of the present invention.
Using the above-mentioned desirable embodiment according to the present invention as enlightenment, by above-mentioned description, relevant staff is complete Various changes and amendments can be carried out without departing from the scope of the technological thought of the present invention' entirely.The technology of this invention Property scope is not limited to the content on specification, it is necessary to its technical scope is determined according to right.

Claims (8)

1. a kind of LED packaging silicon rubbers of high index of refraction high-transmittance high rigidity, it is characterised in that:Include two kinds of components of A and B, institute The weight ratio for stating component A and B component is 1:2;
Wherein, the component A includes the raw material of following parts by weight:50 ~ 80 parts of methyl phenyl vinyl polysiloxane, ethenylphenyl 20 ~ 50 parts of silicones, 0.02 ~ 0.2 part of platinum catalyst, 1-4 parts of tackifier;0.01 ~ 0.05 part of inhibitor;The B component bag Include the raw material of following parts by weight:10 ~ 30 parts of methyl phenyl vinyl polysiloxane, 20 ~ 50 parts of Vinylphenyl silicon resin, methylbenzene 35 ~ 55 parts of the hydrogeneous silicones of base.
2. the LED packaging silicon rubbers of high index of refraction high-transmittance high rigidity according to claim 1, it is characterised in that described Methyl phenyl vinyl polysiloxane be the silicones containing MDT structures, its molecular formula is:(ViMe2SiO1/2)x (PhSiO3/2) y (PhSiO) z, wherein, x values are that 10 ~ 30, y values are that 30 ~ 70, z values are that 20 ~ 50, Me is methyl, and Vi is ethene Base, Ph is phenyl.
3. the LED packaging silicon rubbers of high index of refraction high-transmittance high rigidity according to claim 1, it is characterised in that described Vinylphenyl silicon resin molecular formula to be divided into (ViMe2SiO1/2) x (PhSiO3/2) y, wherein x values are 10 ~ 70, y values For 10-50;According to the difference of X and y values, it is arranged to two kinds of physical states, one kind is solvent-laden mixture, and one kind is without molten The polymer of agent, wherein the solvent used in solvent-laden mixture is toluene or dimethylbenzene, solid content is 30% ~ 70%.
4. the LED packaging silicon rubbers of high index of refraction high-transmittance high rigidity according to claim 1, it is characterised in that institute The catalyst stated is platinum-methyl phenyl silicone complex, and platinum content is in 4000ppm ~ 7500ppm.
5. the LED packaging silicon rubbers of high index of refraction high-transmittance high rigidity according to claim 1, it is characterised in that described Tackifier be the siloxanes ring body hydrating polymer containing phenyl, epoxy and acryloyl-oxy functional group.
6. the LED packaging silicon rubbers of high index of refraction high-transmittance high rigidity according to claim 1, it is characterised in that described Inhibitor be one or both of ethynylcyclohexanol or the propine -1- alcohol of 1,1,3- triphenyls -2.
7. the LED packaging silicon rubbers of high index of refraction high-transmittance high rigidity according to claim 1, it is characterised in that described Hydrogeneous silicones be the hydrogeneous polymer containing methyl and phenyl, hydrogen content is 0.2% ~ 0.8%.
8. a kind of preparation method of the LED packaging silicon rubbers of high index of refraction high-transmittance high rigidity as described in claim 1 ~ 6, its It is characterised by, the preparation process of the component A is:By weight fraction for 50 ~ 80 parts methyl phenyl vinyl polysiloxane, 20 ~ 50 parts of Vinylphenyl silicon resin, 0.02 ~ 0.2 part of platinum catalyst, 1 ~ 4 part of tackifier, 0.01 ~ 0.05 part of suppression Agent, is sequentially added in stirring container, and 80 ~ 120 DEG C of decompressions are warming up to after stirring and take off low 1 ~ 3 hour, the component A is produced; The preparation process of the B component is:Methyl phenyl vinyl polysiloxane, 20 ~ 50 parts of ethene by weight fraction for 10 ~ 30 parts Base phenyl polysiloxane, the hydrogeneous silicones of 35 ~ 55 parts of aminomethyl phenyl, are sequentially added in stirring container, stir equal after stirring 80 ~ 120 DEG C of decompressions are warming up to after even de- low 1 ~ 3 hour, produce the B component;Component A and B component are both needed at 80 DEG C ~ 120 DEG C Decompression carries out married operation again after removing solvent within de- low 1 ~ 3 hour.
CN201710356261.0A 2017-05-19 2017-05-19 A kind of LED packaging silicon rubbers of high index of refraction high-transmittance high rigidity and preparation method thereof Pending CN107325783A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110330946A (en) * 2019-03-29 2019-10-15 天永诚高分子材料(常州)有限公司 A kind of low viscosity high heat conduction organosilicon gel and preparation method thereof
CN110964327A (en) * 2019-12-16 2020-04-07 杭州之江新材料有限公司 High-refractive-index transparent silica gel and preparation method and application thereof
CN113025054A (en) * 2019-12-25 2021-06-25 新特能源股份有限公司 Silicon rubber composition, preparation method thereof and packaging adhesive
CN113105863A (en) * 2021-03-01 2021-07-13 华南理工大学 Ultrahigh-hardness silicone resin film and preparation method and application thereof

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Publication number Priority date Publication date Assignee Title
CN101213257A (en) * 2005-06-28 2008-07-02 陶氏康宁东丽株式会社 Curable organopolysiloxane resin composition and optical part molded therefrom
CN103013431A (en) * 2012-12-03 2013-04-03 烟台德邦先进硅材料有限公司 High-refractivity LED (Light-Emitting Diode) package silica gel
CN105969301A (en) * 2016-06-29 2016-09-28 上海康达化工新材料股份有限公司 Organic silicone for high-power LED packaging and methods of preparing and using same

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101213257A (en) * 2005-06-28 2008-07-02 陶氏康宁东丽株式会社 Curable organopolysiloxane resin composition and optical part molded therefrom
CN103013431A (en) * 2012-12-03 2013-04-03 烟台德邦先进硅材料有限公司 High-refractivity LED (Light-Emitting Diode) package silica gel
CN105969301A (en) * 2016-06-29 2016-09-28 上海康达化工新材料股份有限公司 Organic silicone for high-power LED packaging and methods of preparing and using same

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110330946A (en) * 2019-03-29 2019-10-15 天永诚高分子材料(常州)有限公司 A kind of low viscosity high heat conduction organosilicon gel and preparation method thereof
CN110964327A (en) * 2019-12-16 2020-04-07 杭州之江新材料有限公司 High-refractive-index transparent silica gel and preparation method and application thereof
CN110964327B (en) * 2019-12-16 2021-09-17 杭州之江新材料有限公司 High-refractive-index transparent silica gel and preparation method and application thereof
CN113025054A (en) * 2019-12-25 2021-06-25 新特能源股份有限公司 Silicon rubber composition, preparation method thereof and packaging adhesive
CN113105863A (en) * 2021-03-01 2021-07-13 华南理工大学 Ultrahigh-hardness silicone resin film and preparation method and application thereof
CN113105863B (en) * 2021-03-01 2022-06-14 华南理工大学 Ultrahigh-hardness silicone resin film and preparation method and application thereof

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