CN102690621A - Novel LED (light-emitting diode) package resin made from nanometer zinc oxide doping with alicyclic epoxy resin - Google Patents
Novel LED (light-emitting diode) package resin made from nanometer zinc oxide doping with alicyclic epoxy resin Download PDFInfo
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- CN102690621A CN102690621A CN2012101971761A CN201210197176A CN102690621A CN 102690621 A CN102690621 A CN 102690621A CN 2012101971761 A CN2012101971761 A CN 2012101971761A CN 201210197176 A CN201210197176 A CN 201210197176A CN 102690621 A CN102690621 A CN 102690621A
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Abstract
The invention relates to novel LED (light-emitting diode) package resin made from nanometer zinc oxide doping with alicyclic epoxy resin. The novel LED package resin is characterized by being composed of a component A and a component B which are mixed at a ratio of 1:(0.9-1.0) and then utilized for construction, wherein the component A is composed of alicyclic epoxy resin, a reactive diluent, transparent blue and purple dyes paste, a defoamer and a flexibility agent, and the component B is composed of a curing agent, an accelerator, a nanometer ultraviolet absorbent, polylol and antioxidant. The invention provides the LED package resin made from the nanometer zinc oxide doped with the alicyclic epoxy resin, and the LED package resin has the advantages that the transparency is high, the anti-ultraviolet ageing performance is good, the bond force is strong, and the moisture absorption is low, high-cost organosilicon is avoided, simultaneously the faults of the prior bisphenol A epoxy resin that the moisture absorption is high, the anti-ultraviolet ageing performance is poor and the shortwave transmittance is low are overcome, and the LED package resin is suitable for being utilized as the ultraviolet light based white light and blue light LED package resin. The LED package resin has the advantages that the performance is good, the cost is low, the process is simple, and the LED package resin is suitable for the industrial mass production.
Description
Technical field
The present invention relates to a kind of LED packaging plastic, be specifically related to a kind of novel good nano-zinc oxide doped cycloaliphatic epoxy resin LED packaging plastic of ultraviolet aging resistance 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-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; 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.
Summary of the invention
The purpose of this invention is to provide a kind of novel nano-zinc oxide doped cycloaliphatic epoxy resin LED packaging plastic that 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 a kind of novel nano-zinc oxide doped 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: 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, 0.1% 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 novel nano-zinc oxide doped 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 novel nano-zinc oxide doped 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 novel nano-zinc oxide doped 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 novel nano-zinc oxide doped 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 novel nano-zinc oxide doped 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 25nm.
Press a kind of novel nano-zinc oxide doped 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.
A kind of novel nano-zinc oxide doped 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. mix behind 0.1% the nano titanium oxide, make it good shield effectiveness arranged, have good anti-ultraviolet ageing performance ultraviolet region; 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 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 B component: with mass percent is 98.4% methylhexahydrophthalic anhydride and the mixture, 0.92% tetramethyl-amine bromide, 0.5% glycerine, 0.1%25nm zinc 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 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 B component: with mass percent is 98.4% methylhexahydrophthalic anhydride and the mixture, 0.95% tetramethyl-iodate amine, 0.5% glycerine, the 0.1%25nm zinc 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. novel nano-zinc oxide doped 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, nanometer uv-absorbing agent, polyvalent alcohol and inhibitor.
2. a kind of novel nano-zinc oxide doped 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% 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 novel nano-zinc oxide doped 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 novel nano-zinc oxide doped 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 novel nano-zinc oxide doped 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 novel nano-zinc oxide doped 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 novel nano-zinc oxide doped 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 25nm.
8. like claim 1 and 2 described a kind of novel nano-zinc oxide doped 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.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012101971761A CN102690621A (en) | 2012-06-15 | 2012-06-15 | Novel LED (light-emitting diode) package resin made from nanometer zinc oxide doping with alicyclic epoxy resin |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012101971761A CN102690621A (en) | 2012-06-15 | 2012-06-15 | Novel LED (light-emitting diode) package resin made from nanometer zinc oxide doping with alicyclic epoxy resin |
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| CN102690621A true CN102690621A (en) | 2012-09-26 |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2194085A1 (en) * | 2007-09-27 | 2010-06-09 | Mitsubishi Gas Chemical Company, Inc. | Epoxy resin composition, cured object obtained therefrom, and light-emitting diode |
| 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 |
-
2012
- 2012-06-15 CN CN2012101971761A patent/CN102690621A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2194085A1 (en) * | 2007-09-27 | 2010-06-09 | Mitsubishi Gas Chemical Company, Inc. | Epoxy resin composition, cured object obtained therefrom, and light-emitting diode |
| 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 |
Non-Patent Citations (4)
| Title |
|---|
| 夏晓明等: "《功能助剂 塑料 涂料 胶黏剂》", 31 January 2004, 化学工业出版社 * |
| 曹文达: "《建筑装饰材料》", 31 January 2003, 中国电力出版社 * |
| 贺曼罗: "《环氧树脂胶粘剂》", 30 April 2004, 中国石化出版社 * |
| 黄开金: "《纳米材料的制备及应用》", 30 April 2009, 冶金工业出版社 * |
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Owner name: SHANGHAI LIANLANG NEW MATERIAL TECHNOLOGY CO., LTD Free format text: FORMER OWNER: JIANGSU TETRACHEM CO., LTD. Effective date: 20130711 |
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Effective date of registration: 20130711 Address after: 200233, room 6, building 1088, 510 Fu Gang Road, Shanghai, Fengxian District Applicant after: SHANGHAI LIANLANG NEW MATERIAL TECHNOLOGY CO., LTD. Address before: 225400, No. 6-2, Xingang Road, Taixing Economic Development Zone, Taixing, Jiangsu, Taizhou Applicant before: Jiangsu Tetrachem Co.,Ltd. |
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Application publication date: 20120926 |