CN103044918A - Organosilicone resin/epoxy resin hybrid materials for packaging light emitting diodes - Google Patents

Organosilicone resin/epoxy resin hybrid materials for packaging light emitting diodes Download PDF

Info

Publication number
CN103044918A
CN103044918A CN2011103061821A CN201110306182A CN103044918A CN 103044918 A CN103044918 A CN 103044918A CN 2011103061821 A CN2011103061821 A CN 2011103061821A CN 201110306182 A CN201110306182 A CN 201110306182A CN 103044918 A CN103044918 A CN 103044918A
Authority
CN
China
Prior art keywords
epoxy
silicone resin
resins
resin
light emitting
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN2011103061821A
Other languages
Chinese (zh)
Inventor
张瑛
黄伟
赵晓娟
杨欣
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Institute of Chemistry CAS
Original Assignee
Institute of Chemistry CAS
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Institute of Chemistry CAS filed Critical Institute of Chemistry CAS
Priority to CN2011103061821A priority Critical patent/CN103044918A/en
Publication of CN103044918A publication Critical patent/CN103044918A/en
Pending legal-status Critical Current

Links

Landscapes

  • Structures Or Materials For Encapsulating Or Coating Semiconductor Devices Or Solid State Devices (AREA)
  • Epoxy Resins (AREA)

Abstract

The invention relates to organosilicone resin/epoxy resin hybrid materials suitable for packaging light emitting diodes, and the materials are excellent in heat resistance and UV aging resistance performances. Using weight parts of the organosilicone resin as references, the materials comprise components of: 100 weight parts of the organosilicone resin, 5 to 100 parts of the epoxy resin, an organosilicone resin curing catalyst with an amount of the organosilicone resin being 0.0001 to 0.005 %, and an epoxy resin curing catalyst with an amount of the epoxy resin being 0.001 to 1 %. The organosilicone resin comprises silicon hydrogen, silicon ethylene and silicon-phenyl groups, is liquid at a room temperature, and has a refractive index of 1.51 to 1.54 and a viscosity of 500 to 20000 centipoise; and the epoxy resin does not contain an aromatic structure. The organosilicone resin/epoxy resin hybrid materials can be used for packaging photovoltaic devices or as an optical adhesive, and is especially suitable for being used as packaging materials of the LEDs.

Description

Light emitting diode encapsulation silicone resin/Resins, epoxy hybrid material
Technical field
The invention belongs to the organosilicon macromolecule field, particularly be suitable for the silicone resin of the performances such as good heat-resisting, the ultraviolet aging resistance of having of photodiode (LED) encapsulation usefulness/Resins, epoxy hybrid material.
Background technology
LED-based semiconductor lighting technology has widely Energy-saving Perspective.In recent years, there has been rapid development in the fields such as large power white light LED manufacturing technology, small power white light LEDs integrated lighting technology, LED-backlit source technology, and LED luminous efficiency, brightness and stability have increased significantly.In the process of making white light LED part and backlight device, except chip fabrication techniques, fluorescent material manufacturing technology and heat dissipation technology, the performance of LED packaged material will be on also producing significant impact in its luminous efficiency, brightness and work-ing life.In the past few decades, Resins, epoxy is widely used as the LED packaged material because it has the characteristics such as good mechanical property, adhesive property, high transparent and cost are low.But along with improving constantly of LED power and brightness, traditional Resins, epoxy can not satisfy actual requirement aspect ageing-resistant performance.For example, in use because irradiation and the thermal ageing of UV-light all can make it its colour changed into yellow occur, transmittance descends Resins, epoxy, thereby has greatly shortened the work-ing life of LED.
In recent years, organosilicon material is because it has outstanding ultraviolet resistance and heat aging performance, attracted the concern of increasing LED manufacturers, is considered to promise to be most the packaged material of great power LED of future generation.The main drawback of organosilicon material is that physical strength is lower, and adhesive property is poor; When using as the LED packaged material with this, can cause device reliability lower.
For the advantage of organosilicon material and the advantage of Resins, epoxy are combined, people have been developed the modifying epoxy resin by organosilicon material by the method for physical blending and chemical modification.Chemical modification namely is incorporated into the organosilicon segment in the molecular structure of Resins, epoxy, such as the disclosed technical scheme of USP6632892.In general, the solubility parameter of Resins, epoxy and organosilicon material differs larger, both consistencies are relatively poor, so the way of physical blending need to add the consistency that tensio-active agent improves organosilicon and Resins, epoxy, such as the disclosed technical scheme of USP6800373.
The content of the organosilicon component that chemical modification method is introduced in Resins, epoxy is limited, and is therefore heat-resisting to Resins, epoxy limited with the raising ultraviolet ageing performance; Physically modified need to add tensio-active agent on the one hand, and the heat-resisting and ultraviolet ageing poor-performing of tensio-active agent also is difficult to obtain high transparent material on the other hand.In addition, in above-mentioned physical blending and the chemical modification method, the curing of Resins, epoxy all needs to use anhydride curing agent, and the heat-resisting of material and ultraviolet ageing performance are reduced.
The consistency of Resins, epoxy and organosilicon material is poor, and have its source in both polarity differs greatly.If therefore can improve the polarity of organosilicon material, reduce simultaneously the polarity of Resins, epoxy, will greatly increase both consistencies.In the present invention, by the silicon phenyl being incorporated into the polarity that improves silicone resin in the silicone resin, use simultaneously the Resins, epoxy that does not contain aromatic structure, make silicone resin and Resins, epoxy have good consistency, thereby overcome the shortcoming of aforementioned method of modifying.Simultaneously, in the present invention, a small amount of catalyzer is only used in the curing of Resins, epoxy, does not use acid anhydrides as solidifying agent, has avoided heat-resisting and the ultraviolet ageing reduction of performance.
In addition, the specific refractory power of LED packaged material has remarkably influenced to the luminous efficiency of the device of LED.Because the materials such as GaN as the led chip material have high specific refractory power (being about 2.2), in order effectively to reduce the light loss that interfacial refraction brings, improve as far as possible and get optical efficiency, require the specific refractory power of LED packaged material high as far as possible.Traditional silica gel or the refractive index of silicone material only are 1.41, and the refractive index of desirable packaged material should be as much as possible near the refractive index of GaN.The refractive index of silicone resin of the present invention/Resins, epoxy hybrid material is conducive to improve the luminous efficiency of LED device more than 1.5.
Summary of the invention
It is low to the object of the invention is to overcome the existing anti-ultraviolet of epoxy resin encapsulating material and high temperature ageing performance, and the relatively poor defective of organosilicon material adhesive property, what a kind of anti-ultraviolet and high temperature ageing were provided has good adhesion performance, refractive index more than 1.5, is suitable for the silicone resin of LED encapsulation usefulness/Resins, epoxy hybrid material.
The encapsulation of the light emitting diode of anti-ultraviolet of the present invention and high temperature ageing is with silicone resin/Resins, epoxy hybrid material, and take the weight part of silicone resin as benchmark, its component and content are:
Silicone resin 100 weight parts
Resins, epoxy 5~100 weight parts
The silicone resin curing catalysts of silicone resin consumption 0.0001~0.005%
The epoxy resin cure catalyzer of content of epoxy resin 0.001~1%;
Preferred ingredient and content are:
Silicone resin 100 weight parts
Resins, epoxy 10~50 weight parts
The silicone resin curing catalysts of silicone resin consumption 0.0005~0.001%
The epoxy resin cure catalyzer of content of epoxy resin 0.005~0.5%.
Containing silicon hydrogen, silico ethylene and silicon phenyl group in the described silicone resin, at room temperature is liquid, and refractive index is 1.51~1.54, and viscosity is 500~20000 centipoises.By different officials' energy silica structure cell formations (four sense silica structure unit, trifunctional silica structure unit, difunctionality silica structure unit and simple function silica structure unit), have following structure:
[SiO 4/2] X[R 1SiO 3/2] Y[(R 2)(R 3)SiO 2/2] Z[(CH 3) 2(CH 2=CH)SiO 1/2] U[(CH 3) 2(H)SiO 1/2] V
(1)
Wherein: R 1C 6H 5Or C 6H 5With CH 3Combination; R 2, R 3CH independently 3, C 6H 5In a kind of or its combination; X, Y, Z, U, V are each sense silica structure unit shared molfractions separately in described silicone resin, X+Y+Z+U+V=100%, wherein, X=0~25%, Y=10~80%, Z=0~25%, U=10~20%, V=10~20%, and U/V=0.8~1.2.Silicon phenyl content wherein makes the refractive index of silicone resin between 1.51~1.54, if the silicon phenyl content is too high or too low, the refractive index of silicone resin is in above-mentioned scope, will cause the consistency variation of itself and Resins, epoxy, is difficult to obtain high transparent hybrid material.
Above-mentioned silicone resin can by four sense organosilane monomers, trifunctional organosilane monomer, dual functional organosilane monomer and simple function organosilane monomer are mixed according to above-mentioned X+Y+Z+U+V=100%, obtain through hydrolysis-condensation reaction.Hydrolytic condensation method such as document report (organosilicon synthesis technique and product application, the good fortune the loose people, Wang Yilu writes, Chemical Industry Press, 1999, P730).
Above-mentioned four sense organosilane monomers can be chlorosilane (silicon tetrachlorides); Also can be other organosilane monomer that can be hydrolyzed, such as methoxy silane (tetramethoxy-silicane), oxyethyl group siloxanes (tetraethoxysilane) etc.; Or the mixture of above-mentioned four sense organosilane monomers.
Above-mentioned trifunctional organosilane monomer can be organochlorosilane (trichlorosilane); Also can be other organosilane monomer that can be hydrolyzed, such as methoxy silane (Trimethoxy silane), oxyethyl group siloxanes (triethoxyl silane) etc.; Or the mixture of above-mentioned trifunctional organosilane monomer.
Above-mentioned difunctionality organosilane monomer can be organochlorosilane (dichlorosilane); Also can be other organosilane monomer that can be hydrolyzed, such as methoxy silane (dimethoxy silane), oxyethyl group siloxanes (diethoxy silane) etc.; Or the mixture of above-mentioned difunctionality organosilane monomer.
Above-mentioned simple function organosilane monomer can be organochlorosilane (chlorosilane); Also can be other organosilane monomer that can be hydrolyzed, such as methoxy silane (methoxy silane), oxyethyl group siloxanes (Ethoxysilane) etc.; Or the mixture of above-mentioned simple function organosilane monomer.
Described Resins, epoxy is for not containing the Resins, epoxy of aromatic structure, such as hydrogenated bisphenol A epoxy resin, cycloaliphatic epoxy resin or their mixture.The polarity of Resins, epoxy that does not contain aromatic structure is less, and is better with the consistency of silicone resin.The Resins, epoxy such as the bisphenol A type epoxy resin that contain aromatic structure, relatively poor with the consistency of above-mentioned silicone resin, macroscopical phase-splitting can occur in co-mixing system after curing, even just macroscopical phase-splitting occurs before curing, can not obtain optically transparent silicone resin/Resins, epoxy hybrid material.
It is the common employed catalyzer of silicon hydrogen addition that described silicone resin solidifies employed silicone resin curing catalysts, such as H 2PtCl 6, Rh (PPh 3) 3Cl or Rh (PPh 3) 3Cl 2Deng in a kind of.The consumption of silicone resin curing catalysts is 0.0001~0.001% of silicone resin consumption, if consumption very little, will cause curing reaction incomplete, if consumption is too many, will cause the transmittance of cured silicone resin/Resins, epoxy hybrid material and ageing-resistant performance to reduce.
Described epoxy resin cure catalyzer is the beta diketone metal complex.Its consumption is 0.001~1% of content of epoxy resin.If the consumption of epoxy resin cure catalyzer is too low, will be so that solidification value curing too high or Resins, epoxy be incomplete.If the consumption of epoxy resin cure catalyzer is too high, might cause the initial coloration of cured epoxy resin, and so that the anti-ultraviolet of cured epoxy resin, high temperature ageing degradation.
Described beta diketone metal complex is that structure is X-CO-CH 2The metal complexs such as the copper of the beta diketone of-CO-Y, cobalt, zinc, zirconium, aluminium, manganese, chromium or nickel.X wherein, Y is CH independently 3Perhaps C (CH 3) 3
The epoxy resin cure catalyzer of minute quantity is only used in the curing of Resins, epoxy among the present invention, does not use such as acid anhydride type curing agent.Wherein might cause the beta diketone metal complex of Resins, epoxy initial coloration or anti-ultraviolet and high temperature ageing degradation only need to add seldom amount, therefore initial coloration that solidifying agent and catalyzer bring or the decline of anti-ultraviolet and high temperature ageing performance can be effectively avoided or reduce, also organosilyl content in the cured article can be greatly improved.So the silicone resin of anti-ultraviolet of the present invention and high temperature ageing/Resins, epoxy hybrid material has good ultra-violet resistance energy and high temperature ageing performance.Epoxy resin cure mechanism is: necessarily contain the silicon hydroxyl in the aforesaid silicone resin that obtains by the organosilane monomer hydrolytic condensation, and the material of siliceous hydroxyl and beta diketone metal complex can catalysis Resins, epoxy rapid polymerizations, such as document (Hayase S, Ito T, Suzuki S, Wada M.J Polym Sci Pol Chem.1981; 19 (9): 2185-2194.) and document (Hayase S, Ito T, Suzuki S, Wada M.J Polym Sci Pol Chem.1981; 19 (11): 2977-2985.) report.
The good processing performance that silicone resin of the present invention/Resins, epoxy hybrid material has.For the convenience on using, generally the silicone resin curing catalysts is mixed in advance mutually with Resins, epoxy, be mixed with the A component; And the epoxy resin cure catalyzer is mixed with silicone resin, be mixed with the B component.In use, above-mentioned A component and B component are mixed, then cast, curing molding.In the above-mentioned solidification process, temperature is controlled at 80~160 ℃ of scopes, and preferred temperature is 100~120 ℃.If solidification value is higher than 160 ℃, gained cured silicone resin/Resins, epoxy hybrid material will have the possibility of slight jaundice, and transmittance is reduced, if solidification value is lower than 80 ℃, need significantly to prolong set time, be unfavorable for practical application.
The silicone resin of anti-ultraviolet of the present invention and high temperature ageing/Resins, epoxy hybrid material has good optical transparence and good anti-ultraviolet, heat resistant performance, have good adhesive property and higher refractive index, can be used for the packaged material of luminous or optics or as optical adhesive, as the packaged material of light emitting diode (LED) or as optical adhesive.
Embodiment
Further specify the present invention below by specific embodiment, but the present invention is not limited to following embodiment.
Embodiment 1.
The composition of silicone resin/Resins, epoxy hybrid material is as shown in table 1.The structure of silicone resin is suc as formula (R shown in (1) 1=C 6H 5, X=0, Y=80%, Z=0, U=10%, V=10%), at room temperature be liquid, refractive index is 1.52, viscosity is 2500 centipoises; Resins, epoxy is hydrogenated bisphenol A epoxy resin; The silicone resin curing catalysts is H 2PtCl 6The epoxy resin cure catalyzer is aluminium acetylacetonate.
With H 2PtCl 6Mutually mix in advance with hydrogenated bisphenol A epoxy resin, be mixed with the A component; Aluminium acetylacetonate is mixed with above-mentioned silicone resin, be mixed with the B component.Above-mentioned A component and B component are mixed, and cured article technique is: 80 ℃ of lower curing 1 hour, and then 120 ℃ of lower curing 1 hour.Prepared silicone resin/the transmittance of Resins, epoxy hybrid material, hardness, adhesive property are as shown in table 2, and the transmittance after ultraviolet, the thermal ageing changes as shown in table 3.
Embodiment 2.
The composition of silicone resin/Resins, epoxy hybrid material is as shown in table 1.The structure of silicone resin is suc as formula (R shown in (1) 1=C 6H 5, R 2=CH 3, R 3=C 6H 5, X=25%, Y=10%, Z=25%, U=20%, V=20%), at room temperature be liquid, refractive index is 1.51, viscosity is 500 centipoises; Resins, epoxy is hydrogenated bisphenol A epoxy resin; The silicone resin curing catalysts is H 2PtCl 6The epoxy resin cure catalyzer is zinc acetylacetonate.
With H 2PtCl 6Mutually mix in advance with hydrogenated bisphenol A epoxy resin, be mixed with the A component; Zinc acetylacetonate is mixed with above-mentioned silicone resin, be mixed with the B component.Above-mentioned A component and B component are mixed, and cured article technique is: 150 ℃ of lower curing 1 hour.Prepared silicone resin/the transmittance of Resins, epoxy hybrid material, hardness, adhesive property are as shown in table 2, and the transmittance after ultraviolet, the thermal ageing changes as shown in table 3.
Embodiment 3.
The composition of silicone resin/Resins, epoxy hybrid material is as shown in table 1.The structure of silicone resin is suc as formula (R shown in (1) 1=C 6H 5, R 2=C 6H 5, R 3=C 6H 5, X=0%, Y=50%, Z=20%, U=15%, V=15%), at room temperature be liquid, refractive index is 1.54, viscosity is 2000 centipoises; Resins, epoxy is hydrogenated bisphenol A epoxy resin; The silicone resin curing catalysts is H 2PtCl 6The epoxy resin cure catalyzer is aluminium acetylacetonate.
With H 2PtCl 6Mutually mix in advance with hydrogenated bisphenol A epoxy resin, be mixed with the A component; Aluminium acetylacetonate is mixed with above-mentioned silicone resin, be mixed with the B component.Above-mentioned A component and B component are mixed, and cured article technique is: 90 ℃ of lower curing 0.5 hour, and then 150 ℃ of lower curing 1 hour.Prepared silicone resin/the transmittance of Resins, epoxy hybrid material, hardness, adhesive property are as shown in table 2, and the transmittance after ultraviolet, the thermal ageing changes as shown in table 3.
Embodiment 4.
The composition of silicone resin/Resins, epoxy hybrid material is as shown in table 1.The structure of silicone resin is suc as formula (R shown in (1) 1=C 6H 5, X=0, Y=80%, Z=0, U=10%, V=10%), at room temperature be liquid, refractive index is 1.52, viscosity is 2500 centipoises; Resins, epoxy is hydrogenated bisphenol A epoxy resin; The silicone resin curing catalysts is H 2PtCl 6The epoxy resin cure catalyzer is aluminium acetylacetonate.
With H 2PtCl 6Mutually mix in advance with hydrogenated bisphenol A epoxy resin, be mixed with the A component; Aluminium acetylacetonate is mixed with above-mentioned silicone resin, be mixed with the B component.Above-mentioned A component and B component are mixed, and cured article technique is: 120 ℃ of lower curing 2 hours.Prepared silicone resin/the transmittance of Resins, epoxy hybrid material, hardness, adhesive property are as shown in table 2, and the transmittance after ultraviolet, the thermal ageing changes as shown in table 3.
Embodiment 5.
The composition of silicone resin/Resins, epoxy hybrid material is as shown in table 1.The structure of silicone resin is suc as formula (R shown in (1) 1=C 6H 5, X=0, Y=78%, Z=0, U=12%, V=10%), at room temperature be liquid, refractive index is 1.52, viscosity is 2500 centipoises; Resins, epoxy is hydrogenated bisphenol A epoxy resin; The silicone resin curing catalysts is Rh (PPh 3) 3Cl; The epoxy resin cure catalyzer is aluminium acetylacetonate.
With Rh (PPh 3) 3Cl mixes in advance mutually with hydrogenated bisphenol A epoxy resin, is mixed with the A component; Aluminium acetylacetonate is mixed with above-mentioned silicone resin, be mixed with the B component.Above-mentioned A component and B component are mixed, and cured article technique is: 120 ℃ of lower curing 2 hours.Prepared silicone resin/the transmittance of Resins, epoxy hybrid material, hardness, adhesive property are as shown in table 2, and the transmittance after ultraviolet, the thermal ageing changes as shown in table 3.
Embodiment 6.
The composition of silicone resin/Resins, epoxy hybrid material is as shown in table 1.The structure of silicone resin is suc as formula (R shown in (1) 1=C 6H 5, X=0, Y=80%, Z=0, U=10%, V=10%), at room temperature be liquid, refractive index is 1.52, viscosity is 2500 centipoises; Resins, epoxy is cycloaliphatic epoxy resin 3,4-epoxy group(ing) heptanaphthenic acid-3 ', 4 '-epoxy group(ing) hexamethylene methyl esters; The silicone resin curing catalysts is H 2PtCl 6The epoxy resin cure catalyzer is aluminium acetylacetonate.
With H 2PtCl 6With cycloaliphatic epoxy resin 3,4-epoxy group(ing) heptanaphthenic acid-3 ', 4 '-epoxy group(ing) hexamethylene methyl esters mix in advance mutually, are mixed with the A component; Aluminium acetylacetonate is mixed with above-mentioned silicone resin, be mixed with the B component.Above-mentioned A component and B component are mixed, and cured article technique is: 80 ℃ of lower curing 0.5 hour, and then 150 ℃ of lower curing 1 hour.Prepared silicone resin/the transmittance of Resins, epoxy hybrid material, hardness, adhesive property are as shown in table 2, and the transmittance after ultraviolet, the thermal ageing changes as shown in table 3.
Embodiment 7.
The composition of silicone resin/Resins, epoxy hybrid material is as shown in table 1.The structure of silicone resin is suc as formula (R shown in (1) 1=C 6H 5, R 2=C 6H 5, R 3=C 6H 5, X=0%, Y=60%, Z=18%, U=10%, V=12%), at room temperature be liquid, refractive index is 1.54, viscosity is 20000 centipoises; Resins, epoxy is cycloaliphatic epoxy resin 3,4-epoxy group(ing) heptanaphthenic acid-3 ', the mixture of 4 '-epoxy group(ing) hexamethylene methyl esters and hydrogenated bisphenol A epoxy resin (weight ratio is 1: 1); The silicone resin curing catalysts is Rh (PPh 3) 3Cl; The epoxy resin cure catalyzer is acetylacetonate nickel.
With Rh (PPh 3) 3Cl and above-mentioned cycloaliphatic epoxy resin 3,4-epoxy group(ing) heptanaphthenic acid-3 ', 4 '-epoxy group(ing) hexamethylene methyl esters mixes first mutually with the mixture of hydrogenated bisphenol A epoxy resin, is mixed with the A component; Acetylacetonate nickel is mixed with above-mentioned silicone resin, be mixed with the B component.Above-mentioned A component and B component are mixed, and cured article technique is: 80 ℃ of lower curing 0.5 hour, and then 150 ℃ of lower curing 1 hour.Prepared silicone resin/the transmittance of Resins, epoxy hybrid material, hardness, adhesive property are as shown in table 2, and the transmittance after ultraviolet, the thermal ageing changes as shown in table 3.
Comparative example 1.
The preparation of pure silicone resin.The structure of silicone resin is suc as formula (R shown in (1) 1=C 6H 5, X=0, Y=80%, Z=0, U=10%, V=10%), at room temperature be liquid, viscosity is 2500 centipoises; The silicone resin curing catalysts is H 2PtCl 6Cured article technique is: 80 ℃ of lower curing 0.5 hour, and then 150 ℃ of lower curing 1 hour.Transmittance, hardness, the adhesive property of prepared cured silicone resin are as shown in table 2, and the transmittance after ultraviolet, the thermal ageing changes as shown in table 3.
The composition of table 1. silicone resin/Resins, epoxy hybrid material
Figure BDA0000097758480000081
The performance of table 2. silicone resin/Resins, epoxy hybrid material
The performance of table 3. silicone resin/Resins, epoxy hybrid material
Figure BDA0000097758480000091
In above-described embodiment and the comparative example, the transmittance of material adopts UV-4802 type twin-beam ultraviolet-visible pectrophotometer (UNICO's production) test; Viscosity test adopts DV-II+PRO type viscometer (production of U.S. Brookfield company); LX-D type Shore durometer (production of Yueqing City Hypon Instr Ltd.) is adopted in hardness test; The cohesive strength of material adopts INSTRON 3365 universal testing machines (American I nstron company) to test according to GB7124-86; Refractive index adopts 2WAJ type Abbe refractometer to measure (production of optical instrument factory, Shanghai), and probe temperature is 20 ℃.
Thermal ageing is carried out in baking oven, and aging condition is 150 ℃/72 hours.Ultraviolet ageing carries out in the UV-III type ultraviolet ageing case that the triumphant glad century development in science and technology in Beijing company limited produces, and ultraviolet wavelength is 310nm, and the light intensity that shines material surface is 300mW/cm 2, digestion time is 72 hours.
Can find out that from above-described embodiment silicone resin of the present invention/Resins, epoxy hybrid material has the good transparency and higher refractive index.And compare with pure silicone resin, cohesive strength is improved largely.When the consumption of Resins, epoxy is less than 20 weight part, to compare with pure silicone resin, the anti-ultraviolet of silicone resin/Resins, epoxy hybrid material, heat aging property reduce not obvious.If but consumption surpasses 20 weight parts, compares with pure silicone resin, anti-ultraviolet, the heat aging property of silicone resin/Resins, epoxy hybrid material still have apparent in view reduction, but still greatly are better than pure epoxide resin material.
Silicone resin of the present invention/Resins, epoxy hybrid material, particularly when the silicone resin consumption when 20 weight parts are following owing to have good over-all properties, be suitable for the packaged material as LED or other photoelectric device.

Claims (8)

1. light emitting diode encapsulation is with silicone resin/Resins, epoxy hybrid material, take the weight part of silicone resin as benchmark, it is characterized in that:
Silicone resin 100 weight parts
Resins, epoxy 5~100 weight parts
The silicone resin curing catalysts of silicone resin consumption 0.0001~0.005%
The epoxy resin cure catalyzer of content of epoxy resin 0.001~1%;
Contain silicon hydrogen, silico ethylene and silicon phenyl group in the described silicone resin;
Described Resins, epoxy is not for containing the Resins, epoxy of aromatic structure.
2. light emitting diode according to claim 1 encapsulates with silicone resin/Resins, epoxy hybrid material, it is characterized in that:
Silicone resin 100 weight parts
Resins, epoxy 10~50 weight parts
The silicone resin curing catalysts of silicone resin consumption 0.0005~0.001%
The epoxy resin cure catalyzer of content of epoxy resin 0.005~0.5%.
3. light emitting diode according to claim 1 and 2 encapsulates with silicone resin/Resins, epoxy hybrid material, it is characterized in that: the silicone resin that contains silicon hydrogen, silico ethylene and silicon phenyl group in the described silicone resin, at room temperature be liquid, refractive index is 1.51~1.54, and viscosity is 500~20000 centipoises.
4. light emitting diode according to claim 3 encapsulates with silicone resin/Resins, epoxy hybrid material, and it is characterized in that: the silicone resin that contains silicon hydrogen, silico ethylene and silicon phenyl group in the described silicone resin has following structure:
[SiO 4/2] X[R 1SiO 3/2] Y[(R 2)(R 3)SiO 2/2] Z[(CH 3) 2(CH 2=CH)SiO 1/2] U[(CH 3) 2(H)SiO 1/2] V
(1)
Wherein: R 1C 6H 5Or C 6H 5With CH 3Combination; R 2, R 3CH independently 3, C 6H 5In a kind of or its combination; X, Y, Z, U, V are each sense silica structure unit shared molfractions separately in described silicone resin, X+Y+Z+U+V=100%, wherein, X=0~25%, Y=10~80%, Z=0~25%, U=10~20%, V=10~20%, and U/V=0.8~1.2.
5. light emitting diode according to claim 1 and 2 encapsulates with silicone resin/Resins, epoxy hybrid material, it is characterized in that: described Resins, epoxy is hydrogenated bisphenol A epoxy resin, cycloaliphatic epoxy resin or their mixture for the Resins, epoxy that does not contain aromatic structure.
6. light emitting diode according to claim 1 and 2 encapsulates with silicone resin/Resins, epoxy hybrid material, and it is characterized in that: described silicone resin curing catalysts is H 2PtCl 6, Rh (PPh 3) 3Cl or Rh (PPh 3) 3Cl 2In a kind of.
7. light emitting diode according to claim 1 and 2 encapsulates with silicone resin/Resins, epoxy hybrid material, and it is characterized in that: described epoxy resin cure catalyzer is the beta diketone metal complex.
8. light emitting diode according to claim 7 encapsulates with silicone resin/Resins, epoxy hybrid material, and it is characterized in that: described beta diketone metal complex is that structure is X-CO-CH 2The copper of the beta diketone of-CO-Y, cobalt, zinc, zirconium, aluminium, manganese, chromium or nickel metal complex; X wherein, Y is CH independently 3Perhaps C (CH 3) 3
CN2011103061821A 2011-10-11 2011-10-11 Organosilicone resin/epoxy resin hybrid materials for packaging light emitting diodes Pending CN103044918A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN2011103061821A CN103044918A (en) 2011-10-11 2011-10-11 Organosilicone resin/epoxy resin hybrid materials for packaging light emitting diodes

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN2011103061821A CN103044918A (en) 2011-10-11 2011-10-11 Organosilicone resin/epoxy resin hybrid materials for packaging light emitting diodes

Publications (1)

Publication Number Publication Date
CN103044918A true CN103044918A (en) 2013-04-17

Family

ID=48057790

Family Applications (1)

Application Number Title Priority Date Filing Date
CN2011103061821A Pending CN103044918A (en) 2011-10-11 2011-10-11 Organosilicone resin/epoxy resin hybrid materials for packaging light emitting diodes

Country Status (1)

Country Link
CN (1) CN103044918A (en)

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103602309A (en) * 2013-11-28 2014-02-26 烟台德邦先进硅材料有限公司 High-power packaging silica gel for LED (Light Emitting Diode)
CN103820065A (en) * 2014-02-24 2014-05-28 湖南皓志新材料股份有限公司 Conductive adhesive for packaging outdoor LED
CN105860920A (en) * 2016-05-31 2016-08-17 苏州市奎克力电子科技有限公司 Anti-yellowing pouring sealant for encapsulating LED strip
CN107142072A (en) * 2017-04-10 2017-09-08 复旦大学 A kind of fluorine-containing corrosion-resistant organosilicon adhesive and preparation method thereof
CN107686717A (en) * 2017-09-05 2018-02-13 复旦大学 A kind of preparation method of high-temperature resistant silicone adhesive
CN107980052A (en) * 2017-06-01 2018-05-01 苏州佳亿达电器有限公司 LED encapsulation material with high temperature resistant and ageing-resistant performance
CN108192283A (en) * 2017-11-24 2018-06-22 木林森股份有限公司 Production method of organic silicon modified epoxy resin composition for L ED bracket

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20070142574A1 (en) * 2005-12-19 2007-06-21 Shin-Etsu Chemical Co., Ltd. Epoxy/silicone hybrid resin composition and optical semiconductor device

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20070142574A1 (en) * 2005-12-19 2007-06-21 Shin-Etsu Chemical Co., Ltd. Epoxy/silicone hybrid resin composition and optical semiconductor device

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103602309A (en) * 2013-11-28 2014-02-26 烟台德邦先进硅材料有限公司 High-power packaging silica gel for LED (Light Emitting Diode)
CN103602309B (en) * 2013-11-28 2014-10-22 烟台德邦先进硅材料有限公司 High-power packaging silica gel for LED (Light Emitting Diode)
CN103820065A (en) * 2014-02-24 2014-05-28 湖南皓志新材料股份有限公司 Conductive adhesive for packaging outdoor LED
CN105860920A (en) * 2016-05-31 2016-08-17 苏州市奎克力电子科技有限公司 Anti-yellowing pouring sealant for encapsulating LED strip
CN107142072A (en) * 2017-04-10 2017-09-08 复旦大学 A kind of fluorine-containing corrosion-resistant organosilicon adhesive and preparation method thereof
CN107980052A (en) * 2017-06-01 2018-05-01 苏州佳亿达电器有限公司 LED encapsulation material with high temperature resistant and ageing-resistant performance
CN107686717A (en) * 2017-09-05 2018-02-13 复旦大学 A kind of preparation method of high-temperature resistant silicone adhesive
CN108192283A (en) * 2017-11-24 2018-06-22 木林森股份有限公司 Production method of organic silicon modified epoxy resin composition for L ED bracket

Similar Documents

Publication Publication Date Title
CN101215381B (en) Method for preparing methylphenyl hydrogen-containing silicone oil
CN102504270B (en) High-performance organic silicon electronic pouring sealant and preparation method and application thereof
CN103044918A (en) Organosilicone resin/epoxy resin hybrid materials for packaging light emitting diodes
CN101475689B (en) Preparation of methyl phenyl vinyl silicon resin
CN102702441B (en) Preparation method of organic silicon-polymethyl methacrylate composite materials
CN101880396A (en) Preparation method of organic silicon rubber for encapsulating LED being convenient for vacuum defoamation
CN103122149A (en) Silicon rubber with high refractive index and high transparency for optical encapsulation and preparation method thereof
CN101343365A (en) Preparation method for methyl phenyl vinyl polysiloxane for packaging LED
CN103030752A (en) Polymer microsphere, preparation method and application of polymer microsphere, composition, light diffusion plate or light diffusion film, lamp and backlight module
CN104004491A (en) LED ultraviolet curable organosilicon encapsulation adhesive and preparation method thereof
CN102516500A (en) Organic silicon modified epoxy resin for packaging LED (Light Emitting Diode), and preparation method and application thereof
CN102532900B (en) Organosilicon lens material for power type light-emitting diode (LED) packaging
CN103897644B (en) Preparation method of silicone-modified epoxy resin packaging adhesive
CN102977554A (en) Epoxy/organosilicon co-curing composite material for LED packaging and preparation method
CN102634026B (en) Hydrogen-based silicone resin containing trifunctional group chain element and preparation method thereof
CN101619170A (en) Preparation and application of silica gel for LED packaging
CN104140533A (en) Vinyl-containing phenyl hydro silicone resin and preparation method thereof
CN109762167A (en) A kind of LED small-size chips heat conductive insulating die bond material and preparation method thereof
CN102433005B (en) Liquid phenyl silica gel for LED and preparation method thereof
CN104211965A (en) Preparation method for net-like methyl phenyl vinyl polysiloxane for LED packaging
CN101665572A (en) Organic silicon resin for encapsulating LED and preparation method thereof
CN108300408B (en) Organic silicon material for packaging LED with high luminous flux maintenance rate
CN110229339B (en) Phenyl vinyl siloxane resin, high-refractive-index LED packaging silicon resin composition and preparation method thereof
CN100556954C (en) Light emitting diode encapsulates the organic silicon epoxy resin composition with anti-ultraviolet and high temperature ageing
CN106221237A (en) A kind of LED encapsulation organic silica gel and preparation method thereof

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C02 Deemed withdrawal of patent application after publication (patent law 2001)
WD01 Invention patent application deemed withdrawn after publication

Application publication date: 20130417