CN102690620A - Ultraviolet-resistant nano titanium dioxide doped cycloaliphatic epoxy resin LED (light emitting diode) packaging glue - Google Patents
Ultraviolet-resistant nano titanium dioxide doped cycloaliphatic epoxy resin LED (light emitting diode) packaging glue Download PDFInfo
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- CN102690620A CN102690620A CN2012101971333A CN201210197133A CN102690620A CN 102690620 A CN102690620 A CN 102690620A CN 2012101971333 A CN2012101971333 A CN 2012101971333A CN 201210197133 A CN201210197133 A CN 201210197133A CN 102690620 A CN102690620 A CN 102690620A
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- cycloaliphatic epoxy
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Abstract
The invention relates to an ultraviolet-resistant nano titanium dioxide doped cycloaliphatic epoxy resin LED (light emitting diode) packaging glue which is characterized by comprising a component A and a component B, wherein the components A and B are mixed according to the proportion of 1: (0.9-1.0) and then used for construction; the component A comprises cycloaliphatic epoxy resin, a reactive diluent, a transparent bluish violet dye color paste, a defoaming agent and a flexibility agent; and the component B comprises a curing agent, an accelerating agent, a nano ultraviolet absorbing agent, polylol and an antioxidant. The ultraviolet-resistant nano titanium dioxide doped cycloaliphatic epoxy resin LED packaging glue has the characteristics of high transparency, good ultraviolet ageing resistance, strong binding power and low moisture absorption, avoids adopting organic silicon with high cost, overcomes the defects of high moisture absorption, poor ultraviolet resistance, low short wave transmissivity and the like of the traditional bisphenol A epoxy resin, and is more suitable for being used as an ultraviolet-based white light and blue light LED packaging glue. The ultraviolet-resistant nano titanium dioxide doped cycloaliphatic epoxy resin LED packaging glue has the advantages of good performance, low cost and simple process, and is suitable for industrial massive production.
Description
Technical field
The present invention relates to a kind of LED packaging plastic, be specifically related to the good titanium doped cycloaliphatic epoxy resin LED of the nanometer titanium dioxide packaging plastic of a kind of anti-ultraviolet ageing performance.
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 that its transmittance is high, specific refractory power is high, Heat stability is good, good fluidity 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, the anti-ultraviolet ageing ability of improving the LED packaging plastic is to improve the prerequisite in LED life-span.
The anti-ultraviolet aging ability of LED packaged material can be through the epoxy molecule structure design, add means such as uv-absorbing agent and improve.Cycloaliphatic epoxy resin is not owing to contain phenyl ring in the molecular structure; Its UVA amount is low; Compare with bisphenol A type epoxy resin, show good ultraviolet aging resistance performance and agent of low hygroscopicity, and the material after solidifying has higher heat-drawn wire and cohesiveness preferably.Nano titanium dioxide has bigger specific surface area and nanoscale effect; Its optical property is compared with conventional material all to have largely and is improved; It has advantages such as nontoxic, high photo and thermal stability as a kind of inorganic uv-absorbing agent, and extremely low consumption just can improve the optical property of epoxy resin.
Summary of the invention
The purpose of this invention is to provide the titanium doped cycloaliphatic epoxy resin LED of the nanometer titanium dioxide packaging plastic that a kind of transparency is high, the ultraviolet aging resistance performance is good, cohesive force is strong, water absorbability is low; 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 white light and blue-ray LED packaging plastic based on UV-light.
Content of the present invention is the titanium doped cycloaliphatic epoxy resin LED of an a kind of uvioresistant nanometer titanium dioxide 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: the 1. preparation of component A: with mass percent be 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 weighing is good in proportion, under 70-90 ℃ of condition, stir 3-4h, mix; 2. 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% polyvalent alcohol, 0.05% nanometer uv-absorbing agent and 0.01%～0.09% inhibitor; Under 70-90 ℃ of condition, stir 3-4h, mix.
Press the titanium doped cycloaliphatic epoxy resin LED of a kind of uvioresistant nanometer titanium dioxide 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 the titanium doped cycloaliphatic epoxy resin LED of a kind of uvioresistant nanometer titanium dioxide 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 the titanium doped cycloaliphatic epoxy resin LED of a kind of uvioresistant nanometer titanium dioxide 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 the titanium doped cycloaliphatic epoxy resin LED of a kind of uvioresistant nanometer titanium dioxide 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 the titanium doped cycloaliphatic epoxy resin LED of a kind of uvioresistant nanometer titanium dioxide packaging plastic of such scheme, it is characterized in that described nanometer uv-absorbing agent is that particle diameter is the titanium oxide of 20nm.
Press the titanium doped cycloaliphatic epoxy resin LED of a kind of uvioresistant nanometer titanium dioxide 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.
The titanium doped cycloaliphatic epoxy resin LED of a kind of uvioresistant nanometer titanium dioxide packaging plastic, this packaging plastic has following characteristics: 1. outward appearance is a transparent liquid, no segregation, particle and gel; 2. mix behind 0.05% the nano titanium oxide, can reach the effect of complete shielding ultraviolet rays, make it have good anti-ultraviolet ageing performance; 3. being 1.5～2h at 120 ℃ of following gel times, is 0.8～1h at 150 ℃ of following gel times; 4. shock strength is greater than 12.8 KJ/m
2, 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. Reflow Soldering: cross twice Reflow Soldering (peak temperature: 260-265 ℃, time 10-30s), packaging plastic does not have and comes off and the xanthochromia phenomenon; 10. high temperature resistance high humidity: 85 ℃, 85% relative humidity, 100 ℃ of digestion 1h of red ink or soak at room temperature 30 days, all do not have infiltration.
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 be 96.6%4-vinyl epoxy cyclohexane, 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;
⑵ the preparation of B component: with mass percent is 98.4% methylhexahydrophthalic anhydride and the mixture, 0.97% tetramethyl-amine bromide, 0.5% glycerine, 0.05%20nm titanium 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;
⑶ 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 is 96.8%3-epoxy ethyl-7-oxabicyclo [4; 1; 0] weighing is good in proportion for heptane, 2.5% propylene oxide phenyl ether, 0.5% 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 B component: with mass percent is 98.4% methylhexahydrophthalic anhydride and the mixture, 1% tetramethyl-iodate amine, 0.5% glycerine, the 0.05%20nm titanium 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;
⑶ A, B two components are used for construction after mixing by 1:0.95.
Claims (8)
1. the titanium doped cycloaliphatic epoxy resin LED of uvioresistant nanometer titanium dioxide 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, nanometer uv-absorbing agent, polyvalent alcohol and inhibitor.
2. the titanium doped cycloaliphatic epoxy resin LED of a kind of uvioresistant nanometer titanium dioxide as claimed in claim 1 packaging plastic; It is characterized in that each method for preparing ingredients thereof is following: the 1. 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; 2. 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, 0.05% uv-absorbing agent and 0.01%～0.09% inhibitor; Under 70-90 ℃ of condition, stir 3-4h, mix.
3. like claim 1 and the titanium doped cycloaliphatic epoxy resin LED of 2 described a kind of uvioresistant nanometer titanium dioxides packaging plastic; 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 the titanium doped cycloaliphatic epoxy resin LED of 2 described a kind of uvioresistant nanometer titanium dioxides packaging plastic; 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 the titanium doped cycloaliphatic epoxy resin LED of 2 described a kind of uvioresistant nanometer titanium dioxides packaging plastic, 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 the titanium doped cycloaliphatic epoxy resin LED of 2 described a kind of uvioresistant nanometer titanium dioxides packaging plastic, 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 the titanium doped cycloaliphatic epoxy resin LED of 2 described a kind of uvioresistant nanometer titanium dioxides packaging plastic, it is characterized in that described nanometer uv-absorbing agent is that particle diameter is the titanium oxide of 20nm.
8. like claim 1 and the titanium doped cycloaliphatic epoxy resin LED of 2 described a kind of uvioresistant nanometer titanium dioxides packaging plastic; 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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| CN2012101971333A CN102690620A (en) | 2012-06-15 | 2012-06-15 | Ultraviolet-resistant nano titanium dioxide doped cycloaliphatic epoxy resin LED (light emitting diode) packaging glue |
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| CN2012101971333A CN102690620A (en) | 2012-06-15 | 2012-06-15 | Ultraviolet-resistant nano titanium dioxide doped cycloaliphatic epoxy resin LED (light emitting diode) packaging glue |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103560201A (en) * | 2013-11-20 | 2014-02-05 | 电子科技大学 | Ultraviolet light-emitting diode promoting growth of plants |
| CN103897344A (en) * | 2012-12-26 | 2014-07-02 | 第一毛织株式会社 | Epoxy resin composition for encapsulating semiconductor device and semiconductor device encapsulated using the same |
| CN107502279A (en) * | 2017-08-11 | 2017-12-22 | 汕头市骏码凯撒有限公司 | A kind of high temperature resistant thixotropy LED packaging plastics and preparation method thereof |
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| JP2009099784A (en) * | 2007-10-17 | 2009-05-07 | Nitto Denko Corp | Method of manufacturing optical semiconductor device |
| CN101752490A (en) * | 2009-12-25 | 2010-06-23 | 彩虹集团公司 | A kind of LED packaging slurry and preparation method thereof |
| 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 |
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2012
- 2012-06-15 CN CN2012101971333A patent/CN102690620A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2009099784A (en) * | 2007-10-17 | 2009-05-07 | Nitto Denko Corp | Method of manufacturing optical semiconductor device |
| CN101752490A (en) * | 2009-12-25 | 2010-06-23 | 彩虹集团公司 | A kind of LED packaging slurry and preparation method thereof |
| 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 |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103897344A (en) * | 2012-12-26 | 2014-07-02 | 第一毛织株式会社 | Epoxy resin composition for encapsulating semiconductor device and semiconductor device encapsulated using the same |
| US9695294B2 (en) | 2012-12-26 | 2017-07-04 | Cheil Industries, Inc. | Epoxy resin composition for encapsulating semiconductor device and semiconductor device encapsulated using the same |
| CN103560201A (en) * | 2013-11-20 | 2014-02-05 | 电子科技大学 | Ultraviolet light-emitting diode promoting growth of plants |
| CN103560201B (en) * | 2013-11-20 | 2016-07-06 | 电子科技大学 | A kind of UV LED promoting plant growing |
| CN107502279A (en) * | 2017-08-11 | 2017-12-22 | 汕头市骏码凯撒有限公司 | A kind of high temperature resistant thixotropy LED packaging plastics and preparation method thereof |
| CN107502279B (en) * | 2017-08-11 | 2020-11-06 | 汕头市骏码凯撒有限公司 | High-temperature-resistant thixotropic LED packaging adhesive and preparation method thereof |
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Application publication date: 20120926 |