CN102719213A - Modified nano zinc oxide doped cycloaliphatic epoxy resin light-emitting diode (LED) packaging adhesive - Google Patents
Modified nano zinc oxide doped cycloaliphatic epoxy resin light-emitting diode (LED) packaging adhesive Download PDFInfo
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- CN102719213A CN102719213A CN2012102321614A CN201210232161A CN102719213A CN 102719213 A CN102719213 A CN 102719213A CN 2012102321614 A CN2012102321614 A CN 2012102321614A CN 201210232161 A CN201210232161 A CN 201210232161A CN 102719213 A CN102719213 A CN 102719213A
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Abstract
The invention relates to a modified nano zinc oxide doped cycloaliphatic epoxy resin light-emitting diode (LED) packaging adhesive. The modified nano zinc oxide doped cycloaliphatic epoxy resin LED packaging adhesive is characterized by being composed of a component A and a component B, the component A and the component B are mixed according to the ratio of 1: (0.9-1.0), and then the packaging adhesive is used for construction. The component A is composed of a cycloaliphatic epoxy resin, a reactive diluent, transparent royal purple dye color paste, an antifoaming agent and a softening agent, and the component B is composed of a curing agent, an accelerating agent, a silane coupling agent modified nano ultraviolet absorption agent, polyatomic alcohol and an antioxidant. The modified nano zinc oxide doped cycloaliphatic epoxy resin LED packaging adhesive is high in transparency, good in ultraviolet aging resistance performance, high in adhesive power, rapid in solidification and low in viscosity; and according to the packaging adhesive, high-cost organosilicone isn't used, defects that existing bisphenol A epoxy resins are high in moisture absorption, poor in ultraviolet resistance performance and low in short-wave transmissivity are overcome, and the modified nano zinc oxide doped cycloaliphatic epoxy resin LED packaging adhesive can be used as a high-end LED packaging adhesive, a high-power LED packaging adhesive or an LED packaging adhesive based on white light and blue light of ultraviolet light.
Description
Technical field
The present invention relates to a kind of LED packaging plastic, be specifically related to a kind of nano-zinc oxide doped cycloaliphatic epoxy resin LED packaging plastic after silane coupler modified.
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 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 its transmittance and specific refractory power height, Heat stability is good, cohesiveness strong and be easy to spraying.
The LED packaging plastic mainly adopts bisphenol A type epoxy resin and organosilicon at present, and wherein the organosilicon cost is higher, is main with epoxy resin still at present.Can absorb ultraviolet phenyl ring but bisphenol A type epoxy resin contains, absorbing after the ultraviolet ray can the oxidation flavescence, and add have the storage time weak point behind the solidifying agent, shortcomings such as bad adhesion, easy to crack, high-hygroscopicity.Simultaneously, the epoxy resin preheating also can variable color, and then causes the transmitance in short wavelength field to descend, and this phenomenon influences bigger to the luminous luminosity of white light and blue-ray LED.Therefore, anti-ultraviolet ageing ability and the cohesive strength of improving the LED packaging plastic are to improve the prerequisite in LED life-span.
The anti-ultraviolet aging ability of LED packaged material and adhesive property can be through the epoxy molecule structure design, add means such as uv-absorbing agent, inorganic nanoparticles modification and improve.Cycloaliphatic epoxy resin is not owing to contain phenyl ring in the molecular structure, and its UVA amount is low, compares with bisphenol A type epoxy resin, shows good ultraviolet aging resistance performance and agent of low hygroscopicity, and the material after solidifying has higher heat-drawn wire.Nano-class zinc oxide has bigger specific surface area and nanoscale effect; Its optical property is compared with conventional material all to have largely and is improved; Its thin microvoid structure can efficiently radiates heat, prolongs the work-ing life of LED, and it has advantages such as nontoxic, high photo and thermal stability as a kind of inorganic uv-absorbing agent; Can improve the optical property of epoxy resin, but unmodified nano particle is prone to the deposition of reuniting.Nano zine oxide after silane coupler modified; Because of having reduced the surface energy of nano particle; Effectively prevent the reunion of nano particle; Improve its dispersing property in the packaging plastic system, and introduce the Si-O-Si key in the structure, its cohesiveness strengthens, viscosity reduces, toughness improves, solidification rate is accelerated thereby make.
Summary of the invention
The purpose of this invention is to provide that a kind of novel transparency is high, the ultraviolet aging resistance performance is good, cohesive force is strong, toughness is high, quick solidifying, viscosity is low, water absorbability is low LED packaging plastic; Select the nano-zinc oxide doped cycloaliphatic epoxy resin after silane coupler modified for use; Avoid the organosilicon that adopts cost high; Overcome shortcomings such as existing bisphenol A type epoxy resin packaging plastic high-hygroscopicity, ultra-violet resistance difference and shortwave transmitance are low simultaneously, be more suitable for being used as high-end LED packaging plastic, high-power LED encapsulation glue or based on the white light and the blue-ray LED packaging plastic of UV-light.And its performance is good, cost is low, technology is simple, is fit to large-scale industrialization production.
Content of the present invention is a kind of modified nano zinc oxide doping cycloaliphatic epoxy resin LED packaging plastic, 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:
⑴ the preparation of component A: with mass percent is that weighing is good in proportion for 95%～97% cycloaliphatic epoxy resin, 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; Under 70-90 ℃ of condition, stir 3-4h, mix;
⑵ the preparation of B component: with mass percent be 98%～99% mixed acid anhydride solidifying agent, 0.2%～1% promotor, weighing is good in proportion for 0.1% silane coupler modified nanometer uv-absorbing agent, 0.5% polyvalent alcohol and 0.01%～0.09% inhibitor; Under 70-90 ℃ of condition, stir 3-4h, mix.
Press a kind of modified nano zinc oxide doping cycloaliphatic epoxy resin LED packaging plastic 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 a kind of modified nano zinc oxide doping cycloaliphatic epoxy resin LED packaging plastic 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 a kind of modified nano zinc oxide doping cycloaliphatic epoxy resin LED packaging plastic 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 a kind of modified nano zinc oxide doping cycloaliphatic epoxy resin LED packaging plastic 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 a kind of modified nano zinc oxide doping cycloaliphatic epoxy resin LED packaging plastic of such scheme; The preparation method who it is characterized in that described silane coupler modified nanometer uv-absorbing agent is following: transfer pH value to 3-4 the silane coupling agent aqueous solution; Pour in the constant pressure funnel; Slowly be added drop-wise to again in 75 ℃ the nanoparticulate dispersion, in 30min, drip off and insulation reaction 3h gets final product.
Press a kind of modified nano zinc oxide doping cycloaliphatic epoxy resin LED packaging plastic of such scheme, it is characterized in that described silane coupling agent is the trialkyl polyether type silane coupler.
Press a kind of modified nano zinc oxide doping cycloaliphatic epoxy resin LED packaging plastic of such scheme, it is characterized in that described nanometer uv-absorbing agent is that particle diameter is the zinc oxide of 15nm.
Press a kind of modified nano zinc oxide doping cycloaliphatic epoxy resin LED packaging plastic 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.
Modified nano zinc oxide doping cycloaliphatic epoxy resin LED packaging plastic, this packaging plastic has following characteristics: 1. outward appearance is a transparent liquid, no segregation, particle and gel; 2. select the cycloaliphatic epoxy resin that does not contain phenyl ring in the molecular structure for use, its UVA amount is low, shows good ultraviolet aging resistance performance, agent of low hygroscopicity and higher heat-drawn wire; 3. mix behind 0.1% the nano titanium oxide, make it good shield effectiveness arranged, have better anti-ultraviolet ageing performance, and the thin microvoid structure of nano particle helps heat radiation, can prolong the work-ing life of LED ultraviolet region; 4. the nano zine oxide after silane coupler modified, its dispersiveness is improved, and introduces the Si-O-Si key in the structure, its cohesiveness strengthens, viscosity reduces, toughness improves, solidification rate is accelerated thereby make; 5. being 1～1.5h at 120 ℃ of following gel times, is 0.5～0.8h at 150 ℃ of following gel times; 6. shock strength is greater than 12.8 KJ/m
2, bending strength is greater than 14J; 7. second-order transition temperature is greater than 423K; 8.-70 ℃ (30min) circulation of ℃ (30min) → 100 is 200-300 time, the thermal shock 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. 100 ℃ of digestion 1h of red ink or soak at room temperature did not all have infiltration after 30 days, showed that its high temperature resistance (85 ℃) high humidity (85% relative humidity) property is good.
Embodiment
Further introduce the present invention through embodiment below, but embodiment can not be construed as limiting the invention.
Embodiment 1
⑴ the preparation of component A: with mass percent is 96.6%3; Weighing is good in proportion for 4-epoxycyclohexyl methyl methacrylic acid ester, 2.6% epoxy propane butyl ether, 0.6% flexibilizing agent, 0.14% skimmer and 0.06% transparent royal purple dye paste, under 70-90 ℃ of condition, stirs 3-4h to mixing;
⑵ the preparation of modified nanoparticles: transfer pH value to 3-4 the 15% silane coupling agent aqueous solution, pour in the constant pressure funnel, slowly be added drop-wise to again in 75 ℃ 85% nano zinc oxide fluid dispersion, in 30min, drip off and insulation reaction 3h;
⑶ the preparation of B component: with mass percent is 98.4% methylhexahydrophthalic anhydride and the mixture, 0.92% tetramethyl-amine bromide, 0.5% glycerine, 0.1% silane coupler modified nano zine oxide 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 the preparation of component A: with mass percent be 96.8% pair of (7-oxabicyclo [4.1.0] 3-methyl in heptan adipic acid ester), 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;
⑵ the preparation of modified nanoparticles: transfer pH value to 3-4 the 15% silane coupling agent aqueous solution, pour in the constant pressure funnel, slowly be added drop-wise to again in 75 ℃ 85% nano zinc oxide fluid dispersion, in 30min, drip off and insulation reaction 3h;
⑶ the preparation of B component: with mass percent is 98.4% methylhexahydrophthalic anhydride and the mixture, 0.95% tetramethyl-iodate amine, 0.5% glycerine, the 0.1% silane coupler modified nano zine oxide 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. modified nano zinc oxide doping cycloaliphatic epoxy resin LED packaging plastic; 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 A component is made up of cycloaliphatic epoxy resin, flexibilizing agent, reactive thinner, transparent royal purple dye paste and skimmer, and the B component is made up of solidifying agent, promotor, silane coupler modified nanometer uv-absorbing agent, polyvalent alcohol and inhibitor.
2. a kind of modified nano zinc oxide doping cycloaliphatic epoxy resin LED packaging plastic as claimed in claim 1; It is characterized in that each method for preparing ingredients thereof is following: the preparation of ⑴ component A: with mass percent is that weighing is good in proportion for 95%～97% cycloaliphatic epoxy resin, 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; Under 70-90 ℃ of condition, stir 3-4h, mix; ⑵ 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%～0.8% promotor, 0.5% polyvalent alcohol, 0.1% silane coupler modified nanometer uv-absorbing agent and 0.01%～0.09% inhibitor; Under 70-90 ℃ of condition, stir 3-4h, mix.
3. like claim 1 and 2 described a kind of modified nano zinc oxide doping cycloaliphatic epoxy resin LED packaging plastics; 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. like claim 1 and 2 described a kind of modified nano zinc oxide doping cycloaliphatic epoxy resin LED packaging plastics; 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.
5. like claim 1 and 2 described a kind of modified nano zinc oxide doping cycloaliphatic epoxy resin LED packaging plastics, 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.
6. like claim 1 and 2 described a kind of modified nano zinc oxide doping cycloaliphatic epoxy resin LED packaging plastics, 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.
7. like claim 1 and 2 described a kind of modified nano zinc oxide doping cycloaliphatic epoxy resin LED packaging plastics; The preparation method who it is characterized in that described silane coupler modified nanometer uv-absorbing agent is following: transfer pH value to 3-4 the silane coupling agent aqueous solution; Pour in the constant pressure funnel; Slowly be added drop-wise to again in 75 ℃ the nanoparticulate dispersion, in 30min, drip off and insulation reaction 3h gets final product.
8. like claim 1 and 7 described a kind of modified nano zinc oxide doping cycloaliphatic epoxy resin LED packaging plastics, it is characterized in that described silane coupling agent is the trialkyl polyether type silane coupler.
9. like claim 1 and 7 described a kind of modified nano zinc oxide doping cycloaliphatic epoxy resin LED packaging plastics, it is characterized in that described nanometer uv-absorbing agent is that particle diameter is the zinc oxide of 15nm.
10. like claim 1 and 2 described a kind of modified nano zinc oxide doping cycloaliphatic epoxy resin LED packaging plastics; 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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| CN104031356A (en) * | 2014-06-30 | 2014-09-10 | 江苏华程光电科技有限公司 | LED (light-emitting diode) pouring sealant |
| CN104946037A (en) * | 2015-07-16 | 2015-09-30 | 天津科技大学 | Coating liquid for preparing uvioresistant polyester film and preparation method thereof |
| CN105405489A (en) * | 2015-12-16 | 2016-03-16 | 佛山市顺德区百锐新电子材料有限公司 | Low-temperature cured and weldable high-conductivity slurry and preparation method thereof |
| CN106098915A (en) * | 2016-06-21 | 2016-11-09 | 阜阳市光普照明科技有限公司 | A kind of nano-perovskite modified silica-gel being applied to LED plant growth lamp chip package |
| CN109401668A (en) * | 2018-10-30 | 2019-03-01 | 湖南柯盛新材料有限公司 | A kind of purposes of metal complex, epoxy adhesive and preparation method thereof |
| CN113724947A (en) * | 2021-08-31 | 2021-11-30 | 江苏金安电气有限公司 | Dry-type high-voltage bushing insulation device and use method thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104031356A (en) * | 2014-06-30 | 2014-09-10 | 江苏华程光电科技有限公司 | LED (light-emitting diode) pouring sealant |
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| CN106098915A (en) * | 2016-06-21 | 2016-11-09 | 阜阳市光普照明科技有限公司 | A kind of nano-perovskite modified silica-gel being applied to LED plant growth lamp chip package |
| CN109401668A (en) * | 2018-10-30 | 2019-03-01 | 湖南柯盛新材料有限公司 | A kind of purposes of metal complex, epoxy adhesive and preparation method thereof |
| CN113724947A (en) * | 2021-08-31 | 2021-11-30 | 江苏金安电气有限公司 | Dry-type high-voltage bushing insulation device and use method thereof |
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Application publication date: 20121010 |