CN102703008A - Silane coupling agent modified resin cycloaliphatic epoxy resin high-power LED (light emitting diode) packaging adhesive - Google Patents
Silane coupling agent modified resin cycloaliphatic epoxy resin high-power LED (light emitting diode) packaging adhesive Download PDFInfo
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- CN102703008A CN102703008A CN2012102198268A CN201210219826A CN102703008A CN 102703008 A CN102703008 A CN 102703008A CN 2012102198268 A CN2012102198268 A CN 2012102198268A CN 201210219826 A CN201210219826 A CN 201210219826A CN 102703008 A CN102703008 A CN 102703008A
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- epoxy resin
- cycloaliphatic epoxy
- power led
- led encapsulation
- silane coupler
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Abstract
The invention relates to silane coupling agent modified resin cycloaliphatic epoxy resin high-power LED (light emitting diode) packaging adhesive which is characterized by consisting of a component A and a component B, wherein the component A and the component B are mixed according to ratio of 1:(0.9-1.0) for construction, the component A comprises organosilicone modified cycloaliphatic epoxy resin, a silane coupling agent, a reactive diluent, transparent royal purple dye colour paste, an antifoaming agent and a softening agent, and the component B comprises a curing agent, an accelerating agent, an ultraviolet absorber, polyatomic alcohol and an antioxidant. The invention provides the silane coupling agent modified resin cycloaliphatic epoxy resin high-power LED packaging adhesive which has the advantages of transparency, strong bonding force, difficult cracking, ultraviolet resistance, high-temperature corrosion resistance and low temperature resistance, and high-cost organosilicone is avoided being adopted; and meanwhile, the defects of brittleness, high hygroscopicity, low light transmission, poor ultraviolet resistance and the like of epoxy resin packaging adhesive are overcome, so that the silane coupling agent modified resin cycloaliphatic epoxy resin high-power LED packaging adhesive is more suitable for being used as high-power LED packaging adhesive, has the advantages of good property, low cost and simple preparation process, and leading technology in country, and is suitable for industrial production.
Description
Technical field
The present invention relates to a kind of LED packaging plastic, be specifically related to silane coupler modified cycloaliphatic epoxy resin high-power LED encapsulation glue.
Background technology
Light emitting diode (LED) is compared each side because of it with incandescent light, luminescent lamp and is all had more advantage as third generation semiconductor illuminating light source, is widely used in fields such as illumination, radiating light source and indicating meter.In the great power LED use, the photon that radiative recombination produces can produce loss when outwards launching, and a lot of light can't be mapped to the outside from chip.Through applying the higher relatively substratum transparent of one deck specific refractory power at chip surface is packaging plastic, owing to this glue-line is between chip and the air, thereby effectively reduces the loss of photon at the interface, improves and gets optical efficiency.In addition, the effect of packaging plastic also comprises carries out mechanical protection to chip, stress relief, and as a kind of guide structure.Therefore, require that its transmittance is high, specific refractory power is high, Heat stability is good, good fluidity and be easy to spraying.Be to improve the safety of great power LED encapsulation, require also that packaging plastic has that cementability is strong, agent of low hygroscopicity, low-stress, characteristic such as ageing-resistant.
High-power LED encapsulation glue mainly adopts organosilicon at present, but its cost height and cementability are poor, have reduced the safety of novel large-power LED, are difficult to satisfy the encapsulation requirement of great power LED.Bisphenol A type epoxy resin has shortcomings such as adding behind the solidifying agent easy xanthochromia under short, short-wave radiation of storage time or the high temperature, cementability are poor, easy to crack, high-hygroscopicity, more is not suitable for high-power LED encapsulation.But cycloaliphatic epoxy resin directly is connected on the alicyclic ring because of epoxy group(ing); Can form stiff molecule structure closely, solidify the back cross-linking density and increase, make that the material after solidifying has higher heat-drawn wire; Because of not containing phenyl ring, show good ultra-violet resistance ability and agent of low hygroscopicity in the molecular structure.
Existing commercially available high-power LED encapsulation glue, most of by external import, like Dow corning company, Japan XINYUE etc., its price is all higher.Silane coupler modified cycloaliphatic epoxy resin high-power LED encapsulation glue among the present invention; Select for use silane coupling agent to participate in the cycloaliphatic epoxy resin copolymerization on the one hand; Improve polymer architecture stability; Improve its bonding strength and water tolerance, avoid at high temperature occurring that the packaging plastic gasification expands and cause peeling off or ftractureing; Cycloaliphatic epoxy resin is earlier through organic-silicon-modified on the other hand; In structure, introduce the Si-O key; Have more advantages such as transmittance height, heat-resistant stability is good, ultraviolet resistance is strong, water absorbability is low after the curing, be more suitable for being used for high-power LED encapsulation, and cost is low, performance is good, production technique is simple; Be fit to suitability for industrialized production, the instead external product.
Summary of the invention
The purpose of this invention is to provide a kind of transparent, bonding force by force, not easy to crack, UV resistant, high temperature resistant high erosion and low temperature resistant silane coupler modified cycloaliphatic epoxy resin high-power LED encapsulation glue; Avoid the organic silicon packaging glue that adopts cost high; Overcome simultaneously the existing gluing relay of epoxy encapsulation poor, be shortcomings such as fragility, high-hygroscopicity, low-transmittance, ultra-violet resistance difference; Be more suitable for being used as high-power LED encapsulation glue, good performance, less cost make the external import high-power LED encapsulation of its instead glue.
Content of the present invention is silane coupler modified cycloaliphatic epoxy resin high-power LED encapsulation glue, it is characterized in that, this packaging plastic is made up of A, B two components, through A, B component by 1: (0.9-1.0) be used for construction after mixing, wherein each method for preparing ingredients thereof is following:
The preparation of component A: with mass percent be 95%～97% organic-silicon-modified cycloaliphatic epoxy resin, 0.5%-1% silane coupling agent, 1.6%～3.6% reactive thinner, 0.02%～0.10% transparent royal purple dye paste, 0.08%～0.18% skimmer and 0.5%～1% flexibilizing agent weighing is good in proportion, under 70-90 ℃ of condition, stir 3-4h to mixing;
The preparation of B component: with mass percent is that weighing is good in proportion for 98%～99% mixed acid anhydride solidifying agent, 0.2%～1% promotor, 0.5% uv-absorbing agent, 0.5% polyvalent alcohol and 0.01%～0.09% inhibitor; Under 70-90 ℃ of condition, stir 3-4h, mix.
Press the silane coupler modified cycloaliphatic epoxy resin high-power LED encapsulation glue of such scheme; It is characterized in that described organic-silicon-modified cycloaliphatic epoxy resin preparation method is following: in reaction unit, add cycloaliphatic epoxy resin; Behind the heating and melting; Add 0.5%～1% catalyzer triphenyl phosphorus and 20%～30% silicone resin midbody, be warming up to 120 ℃ of reaction 4h after, underpressure distillation removes the water of dereaction generation.
Press the silane coupler modified cycloaliphatic epoxy resin high-power LED encapsulation glue of such scheme; It is characterized in that described cycloaliphatic epoxy resin is a 4 vinyl epoxy cyclohexane, 3; 4-epoxycyclohexyl methyl methacrylic acid ester, 3; 4-epoxy cyclohexylmethyl-3; In 4-epoxy cyclohexyl carbonic ether, 3-epoxy ethyl-7-oxabicyclo [4,1,0] heptane, two (7-oxabicyclo [4.1.0] 3-methyl in heptan adipic acid esters), NSC 7352 diepoxide, the hexahydrophthalic acid bisglycidyl ester one or more.
Press the silane coupler modified cycloaliphatic epoxy resin high-power LED encapsulation glue of such scheme, it is characterized in that described silicone resin midbody is methyl phenyl silicone resin, methyl silicon resin, low phenyl methyl silicone resin, phenmethyl silicone resin, epoxy modified silicone resin, organosilicon polyester modified resin, gathers in methyl silicon resin, the amino silicone one or more.
Press the silane coupler modified cycloaliphatic epoxy resin high-power LED encapsulation glue of such scheme; It is characterized in that described silane coupling agent is a dialkoxy fundamental mode coupling agent; Participate in the cycloaliphatic epoxy resin copolymerization, improved polymer architecture stability, improved packaging plastic bonding strength and water tolerance.
Press the silane coupler modified cycloaliphatic epoxy resin high-power LED encapsulation glue of such scheme; It is characterized in that described reactive thinner is epoxy propane butyl ether, propylene oxide phenyl ether, benzyl glycidyl ether, tertiary carbonic acid glycidyl ether, 1, one or more in the 4-butyleneglycol glycidyl ether.
Press the silane coupler modified cycloaliphatic epoxy resin high-power LED encapsulation glue of such scheme, it is characterized in that described solidifying agent is the mixture that 60%-70% methylhexahydrophthalic anhydride or hexahydrophthalic anhydride and 30%-40% gather the nonane diacid acid anhydride.
Press the silane coupler modified cycloaliphatic epoxy resin high-power LED encapsulation glue of such scheme, it is characterized in that described promotor is one or more in tetramethyl-amine bromide, tetraethylammonium bromide, tetramethyl-iodate amine, tetraethyl-iodate amine, tetrabutyl iodate amine, tetramethylphosphonium iodide and the chlorinated tetraphenenyl phosphorus.
Press the silane coupler modified cycloaliphatic epoxy resin high-power LED encapsulation glue of such scheme, it is characterized in that described uv-absorbing agent is the uv-absorbing agent of maximum absorption wavelength more than 360nm.
Press the silane coupler modified cycloaliphatic epoxy resin high-power LED encapsulation glue of such scheme; It is characterized in that described inhibitor is 2; The 6-ditertbutylparacresol; In four [β-(3, the 5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester, β-(3, the 5-di-tert-butyl-hydroxy phenyl) propionic acid octadecanol ester one or more.
Silane coupler modified cycloaliphatic epoxy resin high-power LED encapsulation glue, this packaging plastic has following characteristics: (1) outward appearance is a transparent liquid, no segregation, particle and gel, each component color distortion is obvious; (2) being 1.5～2h at 120 ℃ of following gel times, is 0.8～1h at 150 ℃ of following gel times; (3) shock strength is greater than 12.8 KJ/m
2(4) bending strength is greater than 14J; (5) shrinking percentage is less than 0.5%; (6) second-order transition temperature is greater than 423K; (7) resistivity is greater than 6 * 10
13Ω m; (8) thermal shock :-70 ℃ of (30min) → 100 ℃ (30min) circulations 200-300 time, no change; (9) cross twice Reflow Soldering (peak temperature: 260-265 ℃, time 10-30s), packaging plastic does not have and comes off and the xanthochromia phenomenon; (10) 85 ℃, 85% relative humidity, 100 ℃ of digestion 1h of red ink or soak at room temperature 30 days all do not have infiltration.This kind transparency height, bonding force by force, not easy to crack, UV resistant, high temperature resistant high erosion and low temperature resistant packaging plastic, be more suitable for being used for high-power LED encapsulation.
Embodiment
Further introduce the present invention through embodiment below, but embodiment can not be construed as limiting the invention.
Embodiment 1
⑴ prepare organic-silicon-modified cycloaliphatic epoxy resin: in reaction unit, add the 74%4-vinyl epoxy cyclohexane; Behind the heating and melting; Add 1% catalyzer triphenyl phosphorus and 25% methyl phenyl silicone resin, be warming up to 120 ℃ of reaction 4h after, underpressure distillation removes the water that dereaction generates;
⑵ the preparation of component A: with mass percent be 96% organic-silicon-modified cycloaliphatic epoxy resin, 0.6% dialkoxy fundamental mode coupling agent, 2.6% epoxy propane butyl ether, 0.6% flexibilizing agent, 0.14% skimmer and 0.06% transparent royal purple dye paste weighing is good in proportion, under 70-90 ℃ of condition, stir 3-4h to mixing;
⑶ the preparation of B component: with mass percent is 98% methylhexahydrophthalic anhydride and the mixture, 0.92% tetramethyl-amine bromide, 0.5% uv-absorbing agent, 0.5% glycerine and the 0.08% 4 [β-(3 that gather the nonane diacid acid anhydride; The 5-di-tert-butyl-hydroxy phenyl) propionic acid] weighing is good in proportion for pentaerythritol ester, under 70-90 ℃ of condition, stirs 3-4h to mixing;
⑷ A, B two components are used for construction after mixing by 1:0.95.
Embodiment 2
⑴ prepare organic-silicon-modified cycloaliphatic epoxy resin: in reaction unit, add 70%3; 4-epoxycyclohexyl methyl methacrylic acid ester; Behind the heating and melting; Add 1% catalyzer triphenyl phosphorus and 29% phenmethyl silicone resin, be warming up to 120 ℃ of reaction 4h after, underpressure distillation removes the water of dereaction generation;
⑵ the preparation of component A: with mass percent be 96% organic-silicon-modified cycloaliphatic epoxy resin, 0.8% dialkoxy fundamental mode coupling agent, 2.5% propylene oxide phenyl ether, 0.5% flexibilizing agent, 0.14% skimmer and 0.06% transparent royal purple dye paste weighing is good in proportion, under 70-90 ℃ of condition, stir 3-4h to mixing;
⑶ the preparation of B component: with mass percent is 98% methylhexahydrophthalic anhydride and the mixture, 0.95% tetramethyl-iodate amine, 0.5% uv-absorbing agent, 0.5% glycerine and 0.05%2 that gather the nonane diacid acid anhydride; 6-ditertbutylparacresol weighing in proportion is good, under 70-90 ℃ of condition, stirs 3-4h to mixing;
⑷ A, B two components are used for construction after mixing by 1:0.95.
Claims (10)
1. silane coupler modified cycloaliphatic epoxy resin high-power LED encapsulation glue; It is characterized in that: this packaging plastic is made up of A, B two components; Through A, B component by 1: (0.9-1.0) be used for construction after mixing; Wherein the preparation method of A component is for being that weighing is good in proportion for 95%～97% organic-silicon-modified cycloaliphatic epoxy resin, 0.5%-1% silane coupling agent, 1.6%～2.6% reactive thinner, 0.5%～1% flexibilizing agent, 0.08%～0.18% skimmer and 0.02%～0.10% transparent royal purple dye paste with mass percent; Under 70-90 ℃ of condition, stir 3-4h, mix; The preparation method of B component is for being that weighing is good in proportion for 97%～99% mixed acid anhydride solidifying agent, 0.2%～0.8% promotor, 0.5% uv-absorbing agent, 0.5% polyvalent alcohol and 0.01%～0.09% inhibitor with mass percent; Under 70-90 ℃ of condition, stir 3-4h, mix.
2. silane coupler modified cycloaliphatic epoxy resin high-power LED encapsulation glue as claimed in claim 1; It is characterized in that described organic-silicon-modified cycloaliphatic epoxy resin preparation method is following: in reaction unit, add cycloaliphatic epoxy resin; Behind the heating and melting; Add 0.5%～1% catalyzer triphenyl phosphorus and 20%～30% silicone resin midbody, be warming up to 120 ℃ of reaction 4h after, underpressure distillation removes the water of dereaction generation.
3. silane coupler modified cycloaliphatic epoxy resin high-power LED encapsulation glue as claimed in claim 1; It is characterized in that described cycloaliphatic epoxy resin is a 4 vinyl epoxy cyclohexane, 3; 4-epoxycyclohexyl methyl methacrylic acid ester, 3; 4-epoxy cyclohexylmethyl-3; In 4-epoxy cyclohexyl carbonic ether, 3-epoxy ethyl-7-oxabicyclo [4,1,0] heptane, two (7-oxabicyclo [4.1.0] 3-methyl in heptan adipic acid esters), NSC 7352 diepoxide, the hexahydrophthalic acid bisglycidyl ester one or more.
4. silane coupler modified cycloaliphatic epoxy resin high-power LED encapsulation glue as claimed in claim 1 is characterized in that described silicone resin midbody is methyl phenyl silicone resin, methyl silicon resin, low phenyl methyl silicone resin, phenmethyl silicone resin, epoxy modified silicone resin, organosilicon polyester modified resin, gathers in methyl silicon resin, the amino silicone one or more.
5. silane coupler modified cycloaliphatic epoxy resin high-power LED encapsulation glue as claimed in claim 1 is characterized in that described silane coupling agent is a dialkoxy fundamental mode coupling agent.
6. silane coupler modified cycloaliphatic epoxy resin high-power LED encapsulation glue as claimed in claim 1; It is characterized in that described reactive thinner is epoxy propane butyl ether, propylene oxide phenyl ether, benzyl glycidyl ether, tertiary carbonic acid glycidyl ether, 1, one or more in the 4-butyleneglycol glycidyl ether.
7. silane coupler modified cycloaliphatic epoxy resin high-power LED encapsulation glue as claimed in claim 1 is characterized in that described solidifying agent is the mixture that 60%-70% methylhexahydrophthalic anhydride or hexahydrophthalic anhydride and 30%-40% gather the nonane diacid acid anhydride.
8. silane coupler modified cycloaliphatic epoxy resin high-power LED encapsulation glue as claimed in claim 1 is characterized in that described promotor is one or more in tetramethyl-amine bromide, tetraethylammonium bromide, tetramethyl-iodate amine, tetraethyl-iodate amine, tetrabutyl iodate amine, tetramethylphosphonium iodide and the chlorinated tetraphenenyl phosphorus.
9. silane coupler modified cycloaliphatic epoxy resin high-power LED encapsulation glue as claimed in claim 1 is characterized in that described uv-absorbing agent is the uv-absorbing agent of maximum absorption wavelength more than 360nm.
10. silane coupler modified cycloaliphatic epoxy resin high-power LED encapsulation glue as claimed in claim 1; It is characterized in that described inhibitor is 2; The 6-ditertbutylparacresol; In four [β-(3, the 5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester, β-(3, the 5-di-tert-butyl-hydroxy phenyl) propionic acid octadecanol ester one or more.
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| CN2012102198268A CN102703008A (en) | 2012-06-29 | 2012-06-29 | Silane coupling agent modified resin cycloaliphatic epoxy resin high-power LED (light emitting diode) packaging adhesive |
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| CN2012102198268A CN102703008A (en) | 2012-06-29 | 2012-06-29 | Silane coupling agent modified resin cycloaliphatic epoxy resin high-power LED (light emitting diode) packaging adhesive |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105331120A (en) * | 2015-12-14 | 2016-02-17 | 苏州鑫德杰电子有限公司 | Encapsulating material for metalized film capacitor |
| CN108659469A (en) * | 2018-05-18 | 2018-10-16 | 北京市射线应用研究中心 | The epoxy resin-matrix neutron shielding material and preparation and application that organic siliconresin is modified |
| CN108676168A (en) * | 2018-06-08 | 2018-10-19 | 北京化工大学 | A kind of preparation method of heat resist modification organosilicon material |
| CN109021774A (en) * | 2018-06-21 | 2018-12-18 | 福州开发区兴清供销公司 | A kind of anticorrosive paint |
| CN110256898A (en) * | 2019-04-16 | 2019-09-20 | 北京氦舶科技有限责任公司 | A kind of optical ink and its preparation and transparent conductive film |
| CN114316869A (en) * | 2021-12-31 | 2022-04-12 | 江苏科化新材料科技有限公司 | Two-component thermosetting epoxy resin composition and application thereof, two-component thermosetting epoxy resin and preparation method and application thereof |
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| CN101831143A (en) * | 2010-05-06 | 2010-09-15 | 宁波德洲精密电子有限公司 | High-performance liquid epoxy resin composition for packaging LEDs |
| CN102174306A (en) * | 2011-01-26 | 2011-09-07 | 烟台德邦电子材料有限公司 | Conductive adhesive for LED (light emitting diode) packaging and preparation method of conductive adhesive |
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| CN101531874A (en) * | 2008-03-10 | 2009-09-16 | 成都市双流新达实业有限责任公司 | Fast-drying, low-temperature type environmental-protection epoxy resin bicomponent dry coating and preparation method thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105331120A (en) * | 2015-12-14 | 2016-02-17 | 苏州鑫德杰电子有限公司 | Encapsulating material for metalized film capacitor |
| CN108659469A (en) * | 2018-05-18 | 2018-10-16 | 北京市射线应用研究中心 | The epoxy resin-matrix neutron shielding material and preparation and application that organic siliconresin is modified |
| CN108676168A (en) * | 2018-06-08 | 2018-10-19 | 北京化工大学 | A kind of preparation method of heat resist modification organosilicon material |
| CN109021774A (en) * | 2018-06-21 | 2018-12-18 | 福州开发区兴清供销公司 | A kind of anticorrosive paint |
| CN110256898A (en) * | 2019-04-16 | 2019-09-20 | 北京氦舶科技有限责任公司 | A kind of optical ink and its preparation and transparent conductive film |
| CN114316869A (en) * | 2021-12-31 | 2022-04-12 | 江苏科化新材料科技有限公司 | Two-component thermosetting epoxy resin composition and application thereof, two-component thermosetting epoxy resin and preparation method and application thereof |
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Application publication date: 20121003 |