WO2017028008A1 - 一种高折射率高韧性的耐硫化led封装硅胶 - Google Patents

一种高折射率高韧性的耐硫化led封装硅胶 Download PDF

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WO2017028008A1
WO2017028008A1 PCT/CN2015/086958 CN2015086958W WO2017028008A1 WO 2017028008 A1 WO2017028008 A1 WO 2017028008A1 CN 2015086958 W CN2015086958 W CN 2015086958W WO 2017028008 A1 WO2017028008 A1 WO 2017028008A1
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component
parts
refractive index
silica gel
sio
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PCT/CN2015/086958
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English (en)
French (fr)
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陈维
庄恒冬
陈田安
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烟台德邦先进硅材料有限公司
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Priority to PCT/CN2015/086958 priority Critical patent/WO2017028008A1/zh
Publication of WO2017028008A1 publication Critical patent/WO2017028008A1/zh

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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
    • 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
    • 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
    • C09J11/08—Macromolecular additives

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  • the invention relates to a high refractive index LED package silica gel, in particular to a high refractive index, sulfurization resistant, cold and thermal shock resistant LED package silica gel, belonging to the technical field of adhesives.
  • the current packaging materials used in LEDs mainly include epoxy resin and silicone materials.
  • the internal stress of epoxy resin is too large, yellowing, poor resistance to high and low temperature, poor aging resistance, and silicone materials, low internal stress, high and low temperature resistance. Good, not yellow, the overall performance is significantly better than epoxy resin, so it quickly replaces epoxy resin and is widely used in the field of LED packaging.
  • the high refractive index organic silica gel having a refractive index higher than 1.50 has an increasing use rate with higher light extraction efficiency.
  • the refractive index of high-refractive-index LED packaged silica gel in China can reach between 1.50 and 1.55.
  • silicone resin vinyl silicone oil and hydrogen-containing silicone oil
  • the relative content of silicone resin is low and the crosslinking density is low.
  • the bonding effect is not ideal, so the resistance to vulcanization is poor, the bonding interface is easily broken, and the high-silicone resin content and high cross-linking density of the LED package silica gel have improved resistance to vulcanization, but due to its excessive internal stress. It will lead to a decrease in the toughness of the material, and the reaction may occur in the use of high and low temperature thermal shock lamps, cracking of the encapsulating material, and failure of the bonding interface.
  • the present invention provides a high refractive index LED packaged silica gel with the advantages of the prior art, and has the advantages of high hardness, excellent resistance to vulcanization, excellent adhesion, and excellent cold and thermal shock resistance.
  • a high refractive index LED package silica gel comprising A component and B component, the weight ratio of the A component to the B component is 10:1;
  • composition and composition of the raw materials of the component A are as follows:
  • composition and composition of the raw materials of the B component are as follows:
  • the inhibitor is 0.1 to 0.3 parts by weight.
  • the present invention can also be improved as follows.
  • the advantageous effect of the above further embodiment is that, as the matrix resin, it is a silicone resin containing vinyl, which improves the strength and hardness of the product and improves the vulcanization resistance.
  • the adhesive of the present invention contains an epoxy group and an alkoxy group, and its structural formula is as shown above.
  • the addition of the adhesive improves the adhesion of the encapsulating material to the plastic and the metal substrate, and the presence of the ring further improves the vulcanization resistance of the polymer.
  • the platinum-based catalyst is a platinum-methylphenylpolysiloxane complex or a platinum-olefin complex.
  • the platinum-based catalyst is a platinum-methylphenylpolysiloxane complex and has a platinum content of from 3,000 to 10,000 ppm.
  • the molecular formula of the methylphenyl hydrogen-containing silicone resin is: (HMe 2 SiO 1/2 ) 3 (MePhSiO 1/2 ) n (PhSiO 3/2 ) 4 , wherein the Me is a methyl group, Ph It is a phenyl group, 4 ⁇ n ⁇ 6.
  • the beneficial effect of using the above further embodiment is that the methylphenyl hydrogen-containing silicone resin of the present invention as a crosslinking agent is also a hydrogen-containing silicone resin, which not only provides active hydrogen to participate in the crosslinking reaction, but also increases the crosslinking density.
  • the presence of the D chain link (MePhSiO 1/2 ) improves the toughness of the entire system, improves the thermal shock resistance, and has a low viscosity, which reduces the viscosity, strength and toughness of the entire system.
  • the terminal hydrogen-containing diphenylpolysiloxane has the formula: (HMe 2 SiO 1/2 ) 1 (Ph 2 SiO 1/2 ) m , wherein the Me is a methyl group and the Ph is a phenyl group. , 4 ⁇ m ⁇ 6.
  • the beneficial effect of using the above further embodiment is that the hydrogen-containing diphenyl polysiloxane of the present invention acts as a chain extender, which not only provides active hydrogen to participate in the chain extension reaction, but also increases the crosslinking density and improves the toughness of the polymer.
  • the cold and thermal shock resistance is improved, and the viscosity is low, which lowers the viscosity, improves the strength and toughness of the entire system.
  • the inhibitor is selected from the group consisting of ethynylcyclohexanol or 1,1,3-triphenyl-2-propyn-1-ol.
  • the inhibitor is 1,1,3-triphenyl-2-propyn-1-ol, and the structural formula is:
  • the second aspect of the present invention discloses a method for preparing the foregoing high refractive index LED packaged silica gel, comprising the steps of preparing the component A and the step of preparing the component B;
  • the preparation step of the component A is as follows: 80 to 90 parts of methylphenylvinyl silicone resin, 8 to 18 parts of vinyl dimethyl diphenyl polysiloxane, and 0.1 to 0.3 parts of platinum catalyst. 1 to 5 parts of the binder are sequentially added to the mixer, stirred for 3 to 5 hours, and uniformly mixed to obtain the A component;
  • the preparation step of the B component is as follows: 40 to 60 parts of the methylphenyl hydrogen-containing silicone resin, 40 to 60 parts of the hydrogen diphenyl polysiloxane, and 0.1 to 0.3 parts of the inhibitor are sequentially added to the mixer. The mixture was stirred for 3 to 5 hours, and uniformly mixed to obtain a component B.
  • a third aspect of the present invention discloses a method for using the high-refractive-index LED packaged silicon, in which the A component and the B component are uniformly mixed in a weight ratio of 10:1, and vacuum defoamed for 20 to 40 minutes. Dispensing or potting on the package to be packaged, first heating at 100 ⁇ 120 ° C for 0.5 ⁇ 1.5 hours, then heating at 100 ⁇ 200 ° C for 3 ⁇ 5 hours, curing.
  • the high refractive index LED packaged silica gel of the invention is composed of components A and B, and the component A provides high strength resin, vinyl, catalyst and binder in the reaction, and the B component provides high.
  • Strength resin, crosslinking agent, chain extender and inhibitor, high refractive index LED of the present invention Encapsulated silica gel, in addition to vinyl silicone resin, the curing agent is methyl phenyl hydrosilane resin combined with hydrogen diphenyl polysiloxane, the content of silicone resin increases, and at the same time, the silicone resin is added.
  • the combination of silicone resin and suitable silicone, the combination of crosslinking agent and chain extender reduces the internal stress of the cured material, good interfacial adhesion, and improves the thermal shock resistance and resistance of the product. High temperature performance.
  • Methylphenyl vinyl silicone resin (ViMe 2 SiO 1/2 ) (PhSiO 3/2 ) 5 ;
  • Vinyl dimethyl diphenyl polysiloxane (ViMe 2 SiO 1/2 ) 10 ( ViMePh 2 SiO 1/2 ) 10 ;
  • the platinum-based catalyst is a platinum-methylphenyl polysiloxane complex
  • Methylphenyl hydrogen-containing silicone resin (HMe 2 SiO 1/2 ) 3 (MePhSiO 1/2 ) 5 (PhSiO 3/2 ) 4 ;
  • Hydrogenated diphenyl polysiloxane (HMe 2 SiO 1/2 ) 1 (Ph 2 SiO 1/2 ) 4 ;
  • the inhibitor is ethynylcyclohexanol.
  • component A 80 parts of methyl phenyl vinyl silicone resin, 18 parts of vinyl dimethyl diphenyl polysiloxane, 0.1 part of platinum catalyst, and 2.9 parts of binder were added to the mixer for mixing. Stir well for 3h to obtain the A component;
  • component B Weigh 40 parts of dimethyldiphenyl hydrogen-containing silicone resin, 59.8 parts of hydrogen diphenylpolysiloxane, and inhibitor 1,1,3-triphenyl-2-propyne 1-propanol 0.2 parts. Adding to the mixer in turn, mixing for 3 hours and stirring uniformly, that is, the B component is obtained;
  • the A component and the B component are uniformly mixed in a weight ratio of 10:1, vacuum defoamed for 20 minutes, dispensed or potted on the package to be packaged, and first heated at 120 ° C for 1 hour. Then, heat at 150 ° C for 4 hours.
  • Methylphenyl vinyl silicone resin (ViMe 2 SiO 1/2 ) (PhSiO 3/2 ) 3.5 ;
  • Vinyl dimethyl diphenyl polysiloxane (ViMe 2 SiO 1/2 ) 70 ( ViMePh 2 SiO 1/2 ) 70 ;
  • the platinum-based catalyst is a platinum-olefin complex
  • Methylphenyl hydrogen silicone resin (HMe 2 SiO 1/2 ) 3 (MePhSiO 1/2 ) 4 (PhSiO 3/2 ) 4 ;
  • Hydrogenated diphenyl polysiloxane (HMe 2 SiO 1/2 ) 1 (Ph 2 SiO 1/2 ) 5 ;
  • the inhibitor is 1,1,3-triphenyl-2-propyn-1-ol.
  • component A Preparation of component A: Weigh 90 parts of methyl phenyl vinyl silicone resin, 8 parts of vinyl dimethyl diphenyl polysiloxane, 0.3 parts of platinum catalyst, and 1.0 part of binder are sequentially added to the mixer for mixing. Stir well for 5h to obtain the A component;
  • component B 60 parts of dimethyldiphenyl hydrogen-containing silicone resin was weighed, and 39.7 parts of hydrogen diphenylpolysiloxane was contained, and 0.3 parts of inhibitor. Adding to the mixer in turn, mixing for 5 hours and stirring uniformly, that is, the B component is obtained;
  • the A component and the B component are uniformly mixed in a weight ratio of 10:1, vacuum defoamed for 40 minutes, dispensed or potted on the package to be packaged, and first heated at 100 ° C for 1.5 hours. Then, heat at 100 ° C for 5 hours.
  • Methylphenyl vinyl silicone resin (ViMe 2 SiO 1/2 ) 2 (PhSiO 3/2 ) 8 ;
  • Vinyl dimethyl diphenyl polysiloxane (ViMe 2 SiO 1/2 ) 40 ( ViMePh 2 SiO 1/2 ) 40 ;
  • the platinum-based catalyst is a platinum-methylphenyl polysiloxane complex
  • Methylphenyl hydrogen-containing silicone resin (HMe 2 SiO 1/2 ) 3 (MePhSiO 1/2 ) 6 (PhSiO 3/2 ) 4 ;
  • Hydrogenated diphenyl polysiloxane (HMe 2 SiO 1/2 ) 1 (Ph 2 SiO 1/2 ) 6 ;
  • the inhibitor is 1,1,3-triphenyl-2-propyn-1-ol.
  • component A 85 parts of methyl phenyl vinyl silicone resin, 9.8 parts of vinyl dimethyl diphenyl polysiloxane, 0.2 parts of platinum catalyst, and 5 parts of binder were sequentially added to a mixer. Mixing for 4 hours and stirring to obtain the A component;
  • component B 50 parts of dimethyldiphenyl hydrogen-containing silicone resin was weighed, 49.9 parts of hydrogen diphenylpolysiloxane was contained, and 0.1 part of inhibitor was weighed. Adding to the mixer in turn, mixing for 4 hours and stirring evenly, that is, the B component is obtained;
  • the A component and the B component are uniformly mixed in a weight ratio of 10:1, vacuum defoamed for 20 minutes, dispensed or potted on the package to be packaged, and first heated at 120 ° C for 0.5 hour. Then, heat at 200 ° C for 3 hours.
  • Methylphenyl vinyl silicone resin (ViMe 2 SiO 1/2 ) (PhSiO 3/2 ) 5 ;
  • the platinum-based catalyst is a platinum-methylphenyl polysiloxane complex
  • Adhesive (adhesive of the present invention)
  • Methylphenyl hydrogen-containing silicone resin (HMe 2 SiO 1/2 ) 3 (MePhSiO 1/2 ) 5 (PhSiO 3/2 ) 4 ;
  • the inhibitor is ethynylcyclohexanol.
  • component A Weigh 97 parts of methyl phenyl vinyl silicone resin, 0.2 parts of platinum-based catalyst, and 2.8 parts of binder are sequentially added to the mixer, and mixed and stirred to obtain the A component;
  • component B 98.8 parts of dimethyldiphenylhydrogensilicone resin and 0.2 parts of inhibitor were weighed. Adding to the mixer in turn, mixing and stirring evenly, that is, the B component;
  • the A component and the B component are uniformly mixed in a weight ratio of 10:1, vacuum defoamed for 20 minutes, dispensed or potted on the package to be packaged, and first heated at 120 ° C for 1 hour. Then, heat at 150 ° C for 4 hours.
  • Vinyl dimethyl diphenyl polysiloxane (ViMe 2 SiO 1/2 ) 70 ( ViMePh 2 SiO 1/2 ) 70 ;
  • the platinum-based catalyst is a platinum-olefin complex
  • Adhesive (adhesive of the present invention)
  • Hydrogenated diphenyl polysiloxane (HMe 2 SiO 1/2 ) 1 (Ph 2 SiO 1/2 ) 5 ;
  • the inhibitor is 1,1,3-triphenyl-2-propyn-1-ol.
  • component A Preparation of component A: Weigh 97 parts of vinyl dimethyl diphenyl polysiloxane, 0.2 parts of platinum-based catalyst, and 2.8 parts of binder are sequentially added to the mixer, and the mixture is uniformly stirred to obtain the component A;
  • component B 98.8 parts of hydrogen diphenylpolysiloxane and 0.2 parts of inhibitor were weighed. Adding to the mixer in turn, mixing and stirring evenly, that is, the B component;
  • the A component and the B component are uniformly mixed in a weight ratio of 10:1, vacuum defoamed for 20 minutes, dispensed or potted on the package to be packaged, and first heated at 120 ° C for 1 hour. Then, heat at 150 ° C for 4 hours.
  • Methylphenyl vinyl silicone resin (ViMe 2 SiO 1/2 ) 2 (PhSiO 3/2 ) 8 ;
  • Vinyl dimethyl diphenyl polysiloxane (ViMe 2 SiO 1/2 ) 40 ( ViMePh 2 SiO 1/2 ) 10 ;
  • the platinum-based catalyst is a platinum-methylphenyl polysiloxane complex
  • Methylphenyl hydrogen-containing silicone resin (HMe 2 SiO 1/2 ) 3 (MePhSiO 1/2 ) 6 (PhSiO 3/2 ) 4 ;
  • Hydrogenated diphenyl polysiloxane (HMe 2 SiO 1/2 ) 1 (Ph 2 SiO 1/2 ) 6 ;
  • the inhibitor is 1,1,3-triphenyl-2-propyn-1-ol.
  • component A 85 parts of methyl phenyl vinyl silicone resin, 14.8 parts of vinyl dimethyl diphenyl polysiloxane, 0.2 parts of platinum catalyst were added to the mixer in sequence, and the mixture was stirred and evenly obtained.
  • component B 50 parts of dimethyldiphenyl hydrogen-containing silicone resin was weighed, 49.8 parts of hydrogen diphenylpolysiloxane was contained, and 0.2 part of inhibitor was weighed. Adding to the mixer in turn, mixing and stirring evenly, that is, the B component;
  • the A component and the B component are uniformly mixed in a weight ratio of 10:1, vacuum defoamed for 20 minutes, dispensed or potted on the package to be packaged, and first heated at 120 ° C for 1 hour. Then, heat at 150 ° C for 4 hours.
  • Test method First, according to GB2411-1980 (1989) plastic Shore hardness test method to make test pieces; Second, package 2835 bracket, keep the color temperature range between 5500 ⁇ 6000K. Curing conditions: heating at 120 ° C for 1 hour and then heating at 150 ° C for 4 hours.
  • Test 1 According to GB2411-1980 (1989) plastic Shore hardness test method to test the hardness of the test piece; Test 2: use 50% ethanol solution red ink, put into the packaged 2835 stent, placed at 80 ° C for 2 hours, Observe the red ink penetration phenomenon; Test 3: 2g sulfur powder at the bottom of the closed glass bottle, place the 2835 stent in the center of the bottle, test the luminous flux before and after 8 hours at 80 °C, calculate the luminous flux retention rate; Test 4: Pack the cured 2835 stent Into the cold and hot shock box, temperature -40 ⁇ 125 ° C, 3min / 30min, 1 cycle per hour, test 200 cycles after the dead light rate.

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Abstract

本发明涉及一种LED封装硅胶，具体涉及一种高折射率的LED封装硅胶，属于胶粘剂技术领域。本发明的高折射率的LED封装硅胶，包括A组分和B组分，所述A组分与B组分的重量比为10:1；其中，所述A组分包括以下重量份的原料组分：甲基苯基乙烯基硅树脂80～90份，乙烯基二甲基二苯基聚硅氧烷8～18份，铂系催化剂0.1～0.3份，粘接剂1～5份；所述B组分包括以下重量份的原料组分：甲基苯基含氢硅树脂40～60份，端含氢二苯基聚硅氧烷40～60份，抑制剂0.1～0.3份。本发明的高折射率的LED封装硅胶具有硬度高、耐硫化、粘接性优异，且耐冷热冲击性能优异等有益效果。

Description

一种高折射率高韧性的耐硫化LED封装硅胶 技术领域
本发明涉及一种高折射率的LED封装硅胶，特别是涉及一种高折射率、耐硫化、耐冷热冲击的LED封装硅胶，属于胶粘剂技术领域。
背景技术
随着LED应用越来越广泛，对LED封装材料的要求也越来越高。LED目前所用封装材料主要有环氧树脂与有机硅材料，环氧树脂内应力过大，黄变，耐高低温性能差，耐老化性能差，而有机硅材料，内应力小，耐高低温性能好，不黄变，综合性能明显优于环氧树脂，因此迅速取代环氧树脂，被广泛用于LED封装领域。而折射率高于1.50的高折射率的有机硅胶，以其更高的取光效率，用量日益增长。
随着工业的发展，空气中的含硫量日益增加，如果封装材料选用不当，空气中的硫会穿过封装材料或其粘接界面，对支架的银层进行腐蚀，形成黑色硫化银，导致光衰急剧增加。因此这就给封装材料带来了新的挑战，必须提高耐硫化性能。
目前国内高折射率的LED封装硅胶虽然折射率可以达到1.50～1.55之间，但是由于配方设计上普遍采用含有硅树脂，乙烯基硅油、含氢硅油等配合，硅树脂相对含量低，交联密度低，而且粘接效果不理想，所以导致耐硫化差，粘接界面易破坏等，而高硅树脂含量，高交联密度的LED封装硅胶虽然耐硫化性能提高，但因其过高的内应力，会导致材料的韧性降低，反应在使用中高低温冷热冲击死灯、封装材料开裂、粘接界面失效等现象发生。
发明内容
本发明针对现有技术的不足，提供一种高折射率的LED封装硅胶，具有硬度高、耐硫化、粘接性优异，且耐冷热冲击性能优异等有益效果。
本发明解决上述技术问题的技术方案如下：一种高折射率LED封装硅胶，包括A组分和B组分，所述A组分与B组分的重量比为10:1；
其中，所述A组分的原料组成及配比如下：
Figure PCTCN2015086958-appb-000001
所述B组分的原料组成及配比如下：
甲基苯基含氢硅树脂      40～60重量份；
端含氢二苯基聚硅氧烷    40～60重量份；
抑制剂                  0.1～0.3重量份。
在上述技术方案的基础上，本发明还可以做如下改进。
进一步，所述甲基苯基乙烯基硅树脂的分子式为(ViMe2SiO1/2)x(PhSiO3/2)y，其中，所述Me为甲基，Vi为乙烯基，Ph为苯基，x：y＝1:3.5～5。
采用上述进一步方案的有益效果是，作为基体树脂，是一种硅树脂，含有乙烯基,提高产品强度与硬度,提高耐硫化性能。
进一步，所述乙烯基二甲基二苯基聚硅氧烷的分子式为：(ViMe2SiO1/2)a(ViMePh2SiO1/2)b，其中，所述Me为甲基，Vi为乙烯基，Ph为苯基，10≤a≤70，10≤b≤70，并且a：b＝1:1。
采用上述进一步方案的有益效果是，乙烯基二甲基二苯基聚硅氧烷的加入提供了可以参与反应的乙烯基，降低体系固化后的应力，提高了耐冷热冲击的性能。
进一步，所述的粘接剂的结构式为：
Figure PCTCN2015086958-appb-000002
本发明的粘接剂含有环氧基与烷氧基官能团，其结构式如上所示。粘接剂的加入，提高了封装材料对塑料及金属基材的粘接性，并且环体的存在，进一步提高了聚合物耐硫化性能。
进一步，所述铂系催化剂为铂-甲基苯基聚硅氧烷配合物或铂-烯烃配合物。
优选的，所述铂系催化剂为铂-甲基苯基聚硅氧烷配合物，并且铂含量为3000～10000ppm。
进一步，所述甲基苯基含氢硅树脂的分子式为：(HMe2SiO1/2)3(MePhSiO1/2)n(PhSiO3/2)4，其中，所述Me为甲基，Ph为苯基，4≤n≤6。
采用上述进一步方案的有益效果是，本发明的甲基苯基含氢硅树脂作为交联剂，也是一种含氢的硅树脂，不仅提供了活泼氢参与交联反应，提高了交联密度，D链节(MePhSiO1/2)的存在，提高了整个体系的韧性，提高了耐冷热冲击性能，并且粘度低，对于整个体系起到粘度降低，强度、韧性提高的作用。
进一步，所述端含氢二苯基聚硅氧烷的分子式为： (HMe2SiO1/2)1(Ph2SiO1/2)m，其中，所述Me为甲基，Ph为苯基，4≤m≤6。
采用上述进一步方案的有益效果是，本发明的端含氢二苯基聚硅氧烷作为扩链剂，不仅提供了活泼氢参与扩链反应，提高了交联密度，提高了聚合物的韧性，提高了耐冷热冲击性能，并且粘度低，对于整个体系起到粘度降低，强度、韧性提高的作用。
进一步，所述抑制剂选自乙炔基环己醇或1,1,3-三苯基-2-丙炔-1-醇。
优选的，所述抑制剂为1,1,3-三苯基-2-丙炔-1-醇，其结构式为：
Figure PCTCN2015086958-appb-000003
本发明第二方面公开了制备前述高折射率LED封装硅胶的方法，包括A组分的制备步骤及B组分的制备步骤；其中，
1)所述A组分的制备步骤如下：将甲基苯基乙烯基硅树脂80～90份，乙烯基二甲基二苯基聚硅氧烷8～18份，铂系催化剂0.1～0.3份，粘接剂1～5份依次加入搅拌机内，搅拌3～5h，混合均匀获得A组分；
2)所述B组分的制备步骤如下：将甲基苯基含氢硅树脂40～60份，端含氢二苯基聚硅氧烷40～60份，抑制剂0.1～0.3份依次加入搅拌机内，搅拌3～5h，混合均匀获得B组分。
本发明第三方面公开了前述高折射率LED封装硅的使用方法，为将所述A组分和B组分按重量比为10:1的配比混合均匀，真空脱泡20～40分钟，点胶或灌胶于待封装件上，先在100～120℃加热0.5～1.5小时，再在100～200℃加热3～5小时，固化即可。
本发明的有益效果是：本发明高折射率的LED封装硅胶由A、B组分组成，A组分在反应中提供高强度的树脂、乙烯基、催化剂与粘接剂，B组分提供高强度的树脂、交联剂、扩链剂及抑制剂，本发明的高折射率的LED 封装硅胶，除了乙烯基硅树脂以外，其固化剂为甲基苯基含氢硅树脂与端含氢二苯基聚硅氧烷相配合，硅树脂的含量增加，同时，增加了硅树脂中的苯基含量；另外，进一步增加了交联密度，提高了产品的硬度，提高了耐硫化性能，并且添加了特殊结构的粘接剂，从而固化后对基材附着力优异。采用硅树脂与适合聚硅氧烷相结合，交联剂与扩链剂相结合，降低固化后的材料的内应力，良好的界面粘接性，提高了产品的耐冷热冲击的性能及耐高温性能。
具体实施方式
以下对本发明的原理和特征进行描述，所举实例只用于解释本发明，并非用于限定本发明的范围。
实施例1
1.原料
甲基苯基乙烯基硅树脂：(ViMe2SiO1/2)(PhSiO3/2)5；
乙烯基二甲基二苯基聚硅氧烷：(ViMe2SiO1/2)10(ViMePh2SiO1/2)10；
铂系催化剂为铂-甲基苯基聚硅氧烷配合物；
甲基苯基含氢硅树脂：(HMe2SiO1/2)3(MePhSiO1/2)5(PhSiO3/2)4；
端含氢二苯基聚硅氧烷：(HMe2SiO1/2)1(Ph2SiO1/2)4；
抑制剂为乙炔基环己醇。
2.制备方法
A组分的制备：称取甲基苯基乙烯基硅树脂80份，乙烯基二甲基二苯基聚硅氧烷18份，铂系催化剂0.1份，粘接剂2.9份依次加入搅拌机内混合3h搅拌均匀，即得所述A组分；
B组分的制备：称取二甲基二苯基含氢硅树脂40份，端含氢二苯基聚硅氧烷59.8份，抑制剂1,1,3-三苯基-2-丙炔-1-醇0.2份。依次加入搅拌机内，混合3h搅拌均匀，即得所述B组分；
使用时，将所述A组分、B组分按重量比为10:1的配比混合均匀，真空脱泡20分钟，点胶或灌胶于待封装件上，先在120℃加热1小时，再在150℃加热4小时，即可。
实施例2
1.原料
甲基苯基乙烯基硅树脂：(ViMe2SiO1/2)(PhSiO3/2)3.5；
乙烯基二甲基二苯基聚硅氧烷：(ViMe2SiO1/2)70(ViMePh2SiO1/2)70；
铂系催化剂为铂-烯烃配合物；
甲基苯基含氢硅树脂：(HMe2SiO1/2)3(MePhSiO1/2)4(PhSiO3/2)4；
端含氢二苯基聚硅氧烷：(HMe2SiO1/2)1(Ph2SiO1/2)5；
抑制剂为1,1,3-三苯基-2-丙炔-1-醇。
2.制备方法
A组分的制备：称取甲基苯基乙烯基硅树脂90份，乙烯基二甲基二苯基聚硅氧烷8份，铂系催化剂0.3份，粘接剂1.0份依次加入搅拌机内混合5h搅拌均匀，即得所述A组分；
B组分的制备：称取二甲基二苯基含氢硅树脂60份，端含氢二苯基聚硅氧烷39.7份，抑制剂0.3份。依次加入搅拌机内，混合5h搅拌均匀，即得所述B组分；
使用时，将所述A组分、B组分按重量比为10:1的配比混合均匀，真空脱泡40分钟，点胶或灌胶于待封装件上，先在100℃加热1.5小时，再在100℃加热5小时，即可。
实施例3
1.原料
甲基苯基乙烯基硅树脂：(ViMe2SiO1/2)2(PhSiO3/2)8；
乙烯基二甲基二苯基聚硅氧烷：(ViMe2SiO1/2)40(ViMePh2SiO1/2)40；
铂系催化剂为铂-甲基苯基聚硅氧烷配合物；
甲基苯基含氢硅树脂：(HMe2SiO1/2)3(MePhSiO1/2)6(PhSiO3/2)4；
端含氢二苯基聚硅氧烷：(HMe2SiO1/2)1(Ph2SiO1/2)6；
抑制剂为1,1,3-三苯基-2-丙炔-1-醇。
2.制备方法
A组分的制备：称取甲基苯基乙烯基硅树脂85份，乙烯基二甲基二苯基聚硅氧烷9.8份，铂系催化剂0.2份，粘接剂5份依次加入搅拌机内，混合4h搅拌均匀即得所述A组分；
B组分的制备：称取二甲基二苯基含氢硅树脂50份，端含氢二苯基聚硅氧烷49.9份，抑制剂0.1份。依次加入搅拌机内，混合4h搅拌均匀，即得所述B组分；
使用时，将所述A组分、B组分按重量比为10:1的配比混合均匀，真空脱泡20分钟，点胶或灌胶于待封装件上，先在120℃加热0.5小时，再在200℃加热3小时，即可。
对比例1
1.原料组成
甲基苯基乙烯基硅树脂：(ViMe2SiO1/2)(PhSiO3/2)5；
铂系催化剂为铂-甲基苯基聚硅氧烷配合物；
粘接剂(本发明粘接剂)
甲基苯基含氢硅树脂：(HMe2SiO1/2)3(MePhSiO1/2)5(PhSiO3/2)4；
抑制剂为乙炔基环己醇。
2.制备方法
A组分的制备：称取甲基苯基乙烯基硅树脂97份，铂系催化剂0.2份，粘接剂2.8份依次加入搅拌机内，混合搅拌均匀即得所述A组分；
B组分的制备：称取二甲基二苯基含氢硅树脂98.8份，抑制剂0.2份。依次加入搅拌机内，混合搅拌均匀，即得所述B组分；
使用时，将所述A组分、B组分按重量比为10:1的配比混合均匀，真空脱泡20分钟，点胶或灌胶于待封装件上，先在120℃加热1小时，再在150℃加热4小时，即可。
对比例2
1.原料组成
乙烯基二甲基二苯基聚硅氧烷：(ViMe2SiO1/2)70(ViMePh2SiO1/2)70；
铂系催化剂为铂-烯烃配合物；
粘接剂(本发明粘接剂)
端含氢二苯基聚硅氧烷：(HMe2SiO1/2)1(Ph2SiO1/2)5；
抑制剂为1,1,3-三苯基-2-丙炔-1-醇。
2.制备方法
A组分的制备：称取乙烯基二甲基二苯基聚硅氧烷97份，铂系催化剂0.2份，粘接剂2.8份依次加入搅拌机内，混合搅拌均匀即得所述A组分；
B组分的制备：称取端含氢二苯基聚硅氧烷98.8份，抑制剂0.2份。依次加入搅拌机内，混合搅拌均匀，即得所述B组分；
使用时，将所述A组分、B组分按重量比为10:1的配比混合均匀，真空脱泡20分钟，点胶或灌胶于待封装件上，先在120℃加热1小时，再在150℃加热4小时，即可。
对比例3
1.原料组成
甲基苯基乙烯基硅树脂：(ViMe2SiO1/2)2(PhSiO3/2)8；
乙烯基二甲基二苯基聚硅氧烷：(ViMe2SiO1/2)40(ViMePh2SiO1/2)10；
铂系催化剂为铂-甲基苯基聚硅氧烷配合物；
甲基苯基含氢硅树脂：(HMe2SiO1/2)3(MePhSiO1/2)6(PhSiO3/2)4；
端含氢二苯基聚硅氧烷：(HMe2SiO1/2)1(Ph2SiO1/2)6；
抑制剂为1,1,3-三苯基-2-丙炔-1-醇。
2.制备方法
A组分的制备：称取甲基苯基乙烯基硅树脂85份，乙烯基二甲基二苯基聚硅氧烷14.8份，铂系催化剂0.2份依次加入搅拌机内，混合搅拌均匀即得所述A组分；
B组分的制备：称取二甲基二苯基含氢硅树脂50份，端含氢二苯基聚硅氧烷49.8份，抑制剂0.2份。依次加入搅拌机内，混合搅拌均匀，即得所述B组分；
使用时，将所述A组分、B组分按重量比为10:1的配比混合均匀，真空脱泡20分钟，点胶或灌胶于待封装件上，先在120℃加热1小时，再在150℃加热4小时，即可。
试验方法：一、根据GB2411-1980(1989)塑料邵氏硬度试验方法制作试片；二、封装2835支架，保持色温范围在5500～6000K之间。固化条件：先在120℃加热1小时，再在150℃加热4小时。测试一：根据GB2411-1980(1989)塑料邵氏硬度试验方法测试试件硬度；测试二：用50％乙醇溶液红墨水，放入封装固化完毕的2835支架，在80℃放置2小时后， 观察红墨水渗透现象；测试三：密闭玻璃瓶底部2g硫粉，瓶中央放置封装固化完毕的2835支架，测试80℃8小时前后光通量，计算光通量保持率；测试四：封装固化完毕的2835支架放入冷热冲击箱，温度-40～125℃，3min/30min，每小时1个循环，测试200个循环后死灯率。
表1性能指标表
Figure PCTCN2015086958-appb-000004
通过表1可以看出，实施例1、2、3与对比实施例1比较可以看出，树脂含量高虽然提高了硬度，提高了耐硫化，但是耐冷热冲击性能下降；实施例1、2、3与对比实施例2比较可以看出，纯聚硅氧烷体系虽然耐冷热冲击性能优异，但是耐硫化性能很差；实施例1、2、3与对比实施例3比较可以看出，不加粘接剂，封装材料对基材粘接性差，会导致红墨水渗漏，耐硫化下降。
以上所述仅为本发明的较佳实施例，并不用以限制本发明，凡在本发明的精神和原则之内，所作的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。

Claims (10)

  1. 一种高折射率LED封装硅胶，包括A组分和B组分，所述A组分与B组分的重量比为10:1；其中，
    所述A组分的原料组成及配比如下：
    Figure PCTCN2015086958-appb-100001
    所述B组分的原料组成及配比如下：
    甲基苯基含氢硅树脂      40～60重量份；
    端含氢二苯基聚硅氧烷    40～60重量份；
    抑制剂                  0.1～0.3重量份。
  2. 根据权利要求1所述的高折射率LED封装硅胶，其特征在于，所述甲基苯基乙烯基硅树脂的分子式为(ViMe2SiO1/2)x(PhSiO3/2)y，其中，所述Me为甲基，Vi为乙烯基，Ph为苯基，x：y＝1:3.5～5。
  3. 根据权利要求1所述的高折射率LED封装硅胶，其特征在于，所述乙烯基二甲基二苯基聚硅氧烷的分子式为：(ViMe2SiO1/2)a(ViMePh2SiO1/2)b，其中，所述Me为甲基，Vi为乙烯基，Ph为苯基，10≤a≤70，10≤b≤70，并且a：b＝1:1。
  4. 根据权利要求1所述的高折射率LED封装硅胶，其特征在于，所述铂系催化剂为铂-甲基苯基聚硅氧烷配合物或铂-烯烃配合物。
  5. 根据权利要求4所述的高折射率LED封装硅胶，其特征在于，所述铂-甲基苯基聚硅氧烷配合物中铂含量为3000～10000ppm。
  6. 根据权利要求1所述的高折射率LED封装硅胶，其特征在于，所述的粘接剂的结构式为：
    Figure PCTCN2015086958-appb-100002
  7. 根据权利要求1所述的高折射率LED封装硅胶，其特征在于，所述甲基苯基含氢硅树脂的分子式为：(HMe2SiO1/2)3(MePhSiO1/2)n(PhSiO3/2)4，其中，所述Me为甲基，Ph为苯基，4≤n≤6。
  8. 根据权利要求1所述的高折射率LED封装硅胶，其特征在于，所述端含氢二苯基聚硅氧烷的分子式为：(HMe2SiO1/2)1(Ph2SiO1/2)m，其中，所述Me为甲基，Ph为苯基，4≤m≤6。
  9. 根据权利要求1所述的高折射率LED封装硅胶，其特征在于，所述抑制剂选自乙炔基环己醇或1,1,3-三苯基-2-丙炔-1-醇。
  10. 权利要求1-9任一权利要求所述高折射率LED封装硅胶的方法，包括A组分的制备步骤及B组分的制备步骤；其中，
    1)A组分的制备：将甲基苯基乙烯基硅树脂80～90份，乙烯基二甲基二苯基聚硅氧烷8～18份，铂系催化剂0.1～0.3份，粘接剂1～5份依次加入搅拌机内，搅拌3～5h，混合均匀获得A组分；
    2)B组分的制备：将甲基苯基含氢硅树脂40～60份，端含氢二苯基聚硅氧烷40～60份，抑制剂0.1～0.3份依次加入搅拌机内，搅拌3～5h，混合均匀获得B组分。
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CN114686160A (zh) * 2022-04-28 2022-07-01 成都硅宝科技股份有限公司 一种光伏叠瓦组件用无溶剂高韧性有机硅导电胶及其制备方法
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