CN103820065A - Conductive adhesive for packaging outdoor LED - Google Patents
Conductive adhesive for packaging outdoor LED Download PDFInfo
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- CN103820065A CN103820065A CN201410061093.9A CN201410061093A CN103820065A CN 103820065 A CN103820065 A CN 103820065A CN 201410061093 A CN201410061093 A CN 201410061093A CN 103820065 A CN103820065 A CN 103820065A
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Abstract
The invention discloses a conductive adhesive for packaging outdoor LED, and relates to the technical field of new energy. The conductive adhesive is prepared by using the following raw materials, by weight, 60-90 parts of a conductive filler, 0.5-15 parts of an epoxy diluent, 0.3-3 parts of a silicone resin inert agent, 5-25 parts of an epoxy resin, 0.5-5 parts of an epoxy curing agent, 0-0.5 parts of an curing accelerator, 0.1-0.3 parts of an antioxidant and 0.1-0.3 parts of an ultraviolet light stabilizer. The conductive adhesive is prepared through the steps of material preparation, primary mixing, semi-final mixing and final mixing. The conductive adhesive has the characteristics of superior electricity and heat conductivity, high bonding strength, good ultraviolet and ageing resistances and the like, can be used for packaging outdoor LED, and can also be used for packaging large-power LED.
Description
Technical field
The present invention relates to technical field of new energies, particularly a kind of outdoor LED encapsulation conductive resin.
Background technology
In recent years, LED, as a kind of novel green energy conservation technology, is widely used in display screen gradually, illumination at home, car lighting, the aspects such as Landscape Lighting.In future, LED illumination will become the focus lighting engineering of tool market outlook.In the making of LED illuminating device, LED packaged material is an of paramount importance technology.LED packaged material must possess higher transmittance, higher specific refractory power, good resistance to xanthochromia, thermotolerance.Particularly the packaged material of great power LED and outdoor LED, very high in the requirement of the aspects such as ultraviolet aging resistance, wet fastness, cementability, thermal diffusivity, and traditional LED encapsulates conductive resin aspect ultraviolet aging resistance, mostly Shortcomings.
Chinese patent (application number is 201110028116.2) " a kind of conductive resin for LED encapsulation and preparation method thereof ", a kind of conductive resin for packaged LED is disclosed, it is made up of each raw material of following weight percent: conductive powder 75%～95%, epoxy resin 2%～12%, epoxide diluent 1%～10%, solidifying agent 1%～3%, curing catalyst 0%～1%, coupling agent 0.5%～2%; The superior performance of this invention LED conductive resin, heat-conductivity conducting is effective, fully meets the service requirements of high light large power LED chip.Another Chinese patent (application number is 200910021736.6) " conductive silver glue of a kind of packaged LED and preparation method thereof ", comprises following component: super fine silver powder; Glue matrix; Solvent; Solidifying agent accounts for; Curing catalyst; Auxiliary agent; The preparation method of conductive silver glue, comprises following steps: 1) take by weight percentage glue matrix and solvent, super fine silver powder, solidifying agent, curing catalyst, auxiliary agent; 2) by taken resin and solvent, high-speed stirring, by resin dispersion in solvent; 3) take by weight percentage solidifying agent and add in mixed system, carry out supersound process, obtain mixed system; 4) super fine silver powder is added in mixed system, dispersed with stirring, obtains preliminary conductive silver glue; 5) weigh curing catalyst; 6) weigh auxiliary agent, 7) load weighted promotor and auxiliary agent are joined in the conductive silver glue preparing, carry out rolling with three rod milling trains, obtain conductive silver glue product.
Summary of the invention
Technical problem to be solved by this invention is to provide that a kind of electrical and thermal conductivity performance is superior, bonding strength is high, uvioresistant and ageing-resistant effective conductive resin.
For achieving the above object, the technical solution used in the present invention is a kind of outdoor LED encapsulation of invention conductive resin, is to be formed by following preparation of raw material by weight:
Conductive filler material 60-90 epoxide diluent 0.5-15 silicone resin inert agents 0.3-3
Epoxy resin 5-25 epoxy hardener 0.5-5 curing catalyst 0-0.5
Antioxidant 0.1-0.3 UV light stabilizing agent 0.1-0.3.
Described conductive filler material is the silver powder of particle diameter 1-150 micron.
Described epoxide diluent is neodecanoic acid glycidyl ester.
Described epoxy resin is E51 bisphenol A type epoxy resin, bisphenol-A epoxy resin (its epoxy equivalent (weight) is 190-260), 3,4-epoxycyclohexyl methyl 3, a kind of in 4-epoxycyclohexyl manthanoate or two kinds or three kinds; In the time being two or three, the ratio of each component is equal portions or other ratio.
Also can adopt E44 bisphenol A type epoxy resin to substitute E51 bisphenol A type epoxy resin, or the mixture replacing E51 bisphenol A type epoxy resin (now, the ratio of each component is equal portions or other ratio) of employing E44 bisphenol A type epoxy resin and E51 bisphenol A type epoxy resin.
Also can adopt 3,4-epoxycyclohexyl methyl 3,4-epoxycyclohexyl manthanoate adds a kind of in dicyclopentadiene diepoxide, 4 vinyl epoxy cyclohexane or two kinds again and substitutes 3,4-epoxycyclohexyl methyl 3,4-epoxycyclohexyl manthanoate, now, the ratio of each component is equal portions or other ratio.
Described silicone resin inert agents is one or more in methyl silicon resin, methyl phenyl silicone resin, epoxide modified silicone resin, amino silicone, poly-methyl silicon resin, polyphenylmethyl base silicone resin; In the time being two or more, the ratio of each component is equal portions or other ratio.
Described epoxy hardener is one or more in derivative, the diaminodiphenylmethane of Dyhard RU 100, diaminodiphenylsulfone(DDS), diaminodiphenylsulfone(DDS); In the time being two or more, the ratio of each component is equal portions or other ratio.
Described curing catalyst is one or more in 2-ethyl-4-methylimidazole, 2-phenyl-4-methyl-5-hydroxymethyl imidazoles, N-Methylimidazole, acetylacetone copper, zinc acetylacetonate; In the time being two or more, the ratio of each component is equal portions or other ratio.
Described antioxidant is 4-methyl-2,6 DI-tert-butylphenol compounds, distearyl pentaerythritol diphosphite, three (nonyl phenol) phosphorous acid ester, two (2,4-di-tert-butyl-phenyl) pentaerythritol diphosphites, β-(3,5-di-tert-butyl-hydroxy phenyl) one or more in propionic acid octadecanol ester, four [β-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester; In the time being two or more, the ratio of each component is equal portions or other ratio.
Described UV light stabilizing agent is 1-methyl-8-(1,2,2,6,6-pentamethyl--4-piperidines) sebate, salicylate, two (1,2,2,6,6-pentamethyl--4-piperidyl) sebate, two (3,5-di-tert-butyl-4-hydroxyl benzyl monoethyl phosphate) one or more in nickel, 2-(2 '-hydroxyl-3 ', 5 '-di-tert-butyl-phenyl)-5-chloro benzo triazole; In the time being two or more, the ratio of each component is equal portions or other ratio.
Meanwhile, also provide a kind of method of preparing above-mentioned outdoor LED encapsulation conductive resin, its preparation process is as follows:
(i), get the raw materials ready: take respectively by weight percentage above-mentioned each component raw material, for subsequent use;
(ii), just mixed: epoxide diluent for subsequent use, epoxy resin, silicone resin inert agents are mixed, become just batch mixing, for subsequent use;
(iii), compound: in first batch mixing for subsequent use, add epoxy hardener, curing catalyst, antioxidant, UV light stabilizing agent and coupling agent, mix, become compound material, for subsequent use;
(iv), mixed eventually: in compound material for subsequent use, to add conductive filler material, mix in a vacuum, be outdoor LED encapsulation conductive resin.
Outdoor LED encapsulation conductive resin of the present invention, owing to having adopted the fabulous micron order silver powder of electrical and thermal conductivity, makes its electrical and thermal conductivity performance superior; Add neodecanoic acid glycidyl ester as epoxide diluent, improved greatly weathering resistance; Add silicone resin inert agents, not only improved conductive adhesive characteristic, improved bonding strength, and significantly improved yellowing resistance; Add antioxidant and UV light stabilizing agent, greatly improved ageing-resistant and uvioresistant performance.
Embodiment
Below in conjunction with embodiment, the present invention is further illustrated.Explanation is below to adopt the mode exemplifying, but protection scope of the present invention should not be limited to this.
Embodiment mono-:
(i), get the raw materials ready: by weight (gram or kilogram ton or other weight unit, lower with) take respectively 2 parts of 1 part of 8 parts of 2 parts of 6 parts of 80 parts, silver powder, neodecanoic acid glycidyl esters, bisphenol-A epoxy resins, E51 bisphenol A type epoxy resins, methyl phenyl silicone resin, Dyhard RU 100s, 0.5 part of 2-phenyl-4-methyl-5-hydroxymethyl imidazoles, 4-methyl-2 of particle diameter 50-110 micron, 6 0.2 part of DI-tert-butylphenol compounds, 1-methyl-8-(1,2,2,6,6-pentamethyl--4-piperidines) 0.3 part of sebate, for subsequent use;
(ii), just mixed: at normal temperatures, neodecanoic acid glycidyl ester for subsequent use, bisphenol-A epoxy resin, E51 bisphenol A type epoxy resin, methyl phenyl silicone resin are mixed (mixing time is 20 minutes), become just batch mixing, for subsequent use;
(iii), compound: add Dyhard RU 100 for subsequent use, 2-phenyl-4-methyl-5-hydroxymethyl imidazoles, 4-methyl-2,6 DI-tert-butylphenol compounds, 1-methyl-8-(1,2 in first batch mixing for subsequent use, 2,6,6-pentamethyl--4-piperidines) sebate, mix, become compound material, for subsequent use;
(iv), mixed eventually: in compound material for subsequent use, to add micron order silver powder for subsequent use, mix in a vacuum, be outdoor LED encapsulation conductive resin.
After testing, the outdoor LED encapsulation conductive resin that the present embodiment obtains, its haze value <0.5%, transparence >98%, thermal conductivity 25.5W/mK.
Embodiment bis-:
(i), get the raw materials ready: 9 parts of 70 parts, silver powder, the neodecanoic acid glycidyl esters, 3 that take respectively by weight particle diameter 50-110 micron, 4-epoxycyclohexyl methyl 3,0.2 part of 3 parts of 4-epoxycyclohexyl manthanoate, 12 parts of E51 bisphenol A type epoxy resins, 3 parts of methyl phenyl silicone resins, 2 parts of Dyhard RU 100s, 0.5 part of 2-phenyl-4-methyl-5-hydroxymethyl imidazoles, distearyl pentaerythritol diphosphite, two (1,2,2,6,6-pentamethyl--4-piperidyl) 0.3 part of sebate, for subsequent use;
(ii), just mixed: at normal temperatures, by neodecanoic acid glycidyl ester, 3 for subsequent use, 4-epoxycyclohexyl methyl 3,4-epoxycyclohexyl manthanoate, E51 bisphenol A type epoxy resin, methyl phenyl silicone resin mix (mixing time is 20 minutes), become just batch mixing, for subsequent use;
(iii), compound: add Dyhard RU 100 for subsequent use, 2-phenyl-4-methyl-5-hydroxymethyl imidazoles, distearyl pentaerythritol diphosphite, two (1,2,2 in first batch mixing for subsequent use, 6,6-pentamethyl--4-piperidyl) sebate, mix, become compound material, for subsequent use;
(iv), mixed eventually: in compound material for subsequent use, to add micron order silver powder for subsequent use, mix in a vacuum, be outdoor LED encapsulation conductive resin.
After testing, the outdoor LED encapsulation conductive resin that the present embodiment obtains, its haze value <0.5%, transparence >98%, thermal conductivity 25W/mK.
Embodiment tri-:
(i), get the raw materials ready: 8 parts of 70 parts, silver powder, the neodecanoic acid glycidyl esters, 3 that take respectively by weight particle diameter 50-110 micron, 4-epoxycyclohexyl methyl 3,7 parts of 4-epoxycyclohexyl manthanoate, 10 parts of E51 bisphenol A type epoxy resins, 2 parts of methyl phenyl silicone resins, 2 parts of diaminodiphenylsulfone(DDS)s, 0.5 part of N-Methylimidazole, 4-methyl-2,6 0.2 part of DI-tert-butylphenol compounds, two (1,2,2,6,6-pentamethyl--4-piperidyl) 0.3 part of sebate, for subsequent use;
(ii), just mixed: at normal temperatures, by neodecanoic acid glycidyl ester, 3 for subsequent use, 4-epoxycyclohexyl methyl 3,4-epoxycyclohexyl manthanoate, E51 bisphenol A type epoxy resin, methyl phenyl silicone resin mix (mixing time is 20 minutes), become just batch mixing, for subsequent use;
(iii), compound: add diaminodiphenylsulfone(DDS) for subsequent use, N-Methylimidazole, 4-methyl-2 in first batch mixing for subsequent use, 6 DI-tert-butylphenol compounds, two (1,2,2,6,6-pentamethyl--4-piperidyl) sebate, mix, and becomes compound material, for subsequent use;
(iv), mixed eventually: in compound material for subsequent use, to add micron order silver powder for subsequent use, mix in a vacuum, be outdoor LED encapsulation conductive resin.
After testing, the outdoor LED encapsulation conductive resin that the present embodiment obtains, its haze value <0.5%, transparence >98%, thermal conductivity 26W/mK.
Embodiment tetra-:
(i), get the raw materials ready: 0.5 part of 2 parts of 3 parts of 9 parts of 10 parts of 10 parts of 65 parts, silver powder, neodecanoic acid glycidyl esters, bisphenol-A epoxy resins, E51 bisphenol A type epoxy resins, methyl phenyl silicone resins, Dyhard RU 100s, the zinc acetylacetonate, 4-methyl-2 that take respectively by weight particle diameter 50-110 micron, 6 0.2 part of DI-tert-butylphenol compounds, two (1,2,2,6,6-pentamethyl--4-piperidyl) 0.3 part of sebate, for subsequent use;
(ii), just mixed: at normal temperatures, neodecanoic acid glycidyl ester for subsequent use, bisphenol-A epoxy resin, E51 bisphenol A type epoxy resin, methyl phenyl silicone resin are mixed (mixing time is 20 minutes), become just batch mixing, for subsequent use;
(iii), compound: add Dyhard RU 100 for subsequent use, zinc acetylacetonate, 4-methyl-2 in first batch mixing for subsequent use, 6 DI-tert-butylphenol compounds, two (1,2,2,6,6-pentamethyl--4-piperidyl) sebate, mix, and becomes compound material, for subsequent use;
(iv), mixed eventually: in compound material for subsequent use, to add micron order silver powder for subsequent use, mix in a vacuum, be outdoor LED encapsulation conductive resin.
After testing, the outdoor LED encapsulation conductive resin that the present embodiment obtains, its haze value <0.5%, transparence >97%, thermal conductivity 28W/mK.
Embodiment five:
(i), get the raw materials ready: 6 parts of 80 parts, silver powder, the neodecanoic acid glycidyl esters, 3 that take respectively by weight particle diameter 50-110 micron, 4-epoxycyclohexyl methyl 3,0.2 part of 6 parts of 4-epoxycyclohexyl manthanoate, 4 parts of E51 bisphenol A type epoxy resins, 1 part of methyl phenyl silicone resin, 2 parts of Dyhard RU 100s, 0.5 part of zinc acetylacetonate, distearyl pentaerythritol diphosphite, two (1,2,2,6,6-pentamethyl--4-piperidyl) 0.3 part of sebate, for subsequent use;
(ii), just mixed: at normal temperatures, by neodecanoic acid glycidyl ester, 3 for subsequent use, 4-epoxycyclohexyl methyl 3,4-epoxycyclohexyl manthanoate, E51 bisphenol A type epoxy resin, methyl phenyl silicone resin mix (mixing time is 20 minutes), become just batch mixing, for subsequent use;
(iii), compound: in first batch mixing for subsequent use, add Dyhard RU 100 for subsequent use, zinc acetylacetonate, distearyl pentaerythritol diphosphite, two (1,2,2,6,6-pentamethyl--4-piperidyl) sebate, mix, become compound material, for subsequent use;
(iv), mixed eventually: in compound material for subsequent use, to add micron order silver powder for subsequent use, mix in a vacuum, be outdoor LED encapsulation conductive resin.
After testing, the outdoor LED encapsulation conductive resin that the present embodiment obtains, its haze value <0.5%, transparence >96%, thermal conductivity 27W/mK.
Comparative example 1:
Get the raw materials ready: according to prior art formula, take respectively by weight 75 parts, micron order silver powder, 1,9 parts of 4-butyleneglycol glycidyl ethers, 12 parts of E51 bisphenol A type epoxy resins, 3 parts of Dyhard RU 100s, 1 part of 2-heptadecyl imidazoles, for the conducting resin composition based on 100 parts, for subsequent use.
Compound method: at normal temperatures, by 1,4-butyleneglycol glycidyl ether and E51 bisphenol A type epoxy resin mix 20 minutes to even, then add Dyhard RU 100,2-heptadecyl imidazoles, after mixing, be ground to the mixture of uniform and smooth with three-roll grinder, then add micron order silver powder, keep mixing under vacuum, be LED encapsulation conductive resin.
After testing, the conductive resin that this comparative example obtains, its haze value <0.5%, transparence >95%, thermal conductivity 22W/mK.
Conductive resin after embodiment mono-～embodiment five and comparative example 1 solidified does ultraviolet resistance radiative aging performance, the results are shown in Table 1.
Table 1
Detection data by the various embodiments described above can be found out, outdoor LED encapsulation conductive resin of the present invention possesses higher transmittance and good heat dispersion, particularly the performance aspect ultraviolet aging resistance is very good, meets the use standard of outdoor LED encapsulation conductive resin.
Outdoor LED encapsulation conductive resin of the present invention, both can be used for encapsulating outdoor LED, also can be used for packaged high-power LED.
Claims (10)
1. an outdoor LED encapsulation conductive resin, it is characterized in that being formed by following preparation of raw material by weight:
Conductive filler material 60-90 epoxide diluent 0.5-15 silicone resin inert agents 0.3-3
Epoxy resin 5-25 epoxy hardener 0.5-5 curing catalyst 0-0.5
Antioxidant 0.1-0.3 UV light stabilizing agent 0.1-0.3.
2. outdoor LED encapsulation conductive resin as claimed in claim 1, is characterized in that: described conductive filler material is the silver powder of particle diameter 1-150 micron.
3. outdoor LED encapsulation conductive resin as claimed in claim 1, is characterized in that: described epoxide diluent is neodecanoic acid glycidyl ester.
4. outdoor LED encapsulation conductive resin as claimed in claim 1, it is characterized in that: described epoxy resin is E51 bisphenol A type epoxy resin, bisphenol-A epoxy resin, 3,4-epoxycyclohexyl methyl 3, a kind of in 4-epoxycyclohexyl manthanoate or two kinds or three kinds; In the time being two or three, the ratio of each component is equal portions or other ratio.
5. outdoor LED encapsulation conductive resin as claimed in claim 1, is characterized in that: described silicone resin inert agents is one or more in methyl silicon resin, methyl phenyl silicone resin, epoxide modified silicone resin, amino silicone, poly-methyl silicon resin, polyphenylmethyl base silicone resin; In the time being two or more, the ratio of each component is equal portions or other ratio.
6. outdoor LED as claimed in claim 1 encapsulation conductive resin, is characterized in that: described epoxy hardener is one or more in derivative, the diaminodiphenylmethane of Dyhard RU 100, diaminodiphenylsulfone(DDS), diaminodiphenylsulfone(DDS); In the time being two or more, the ratio of each component is equal portions or other ratio.
7. outdoor LED encapsulation conductive resin as claimed in claim 1, is characterized in that: described curing catalyst is one or more in 2-ethyl-4-methylimidazole, 2-phenyl-4-methyl-5-hydroxymethyl imidazoles, N-Methylimidazole, acetylacetone copper, zinc acetylacetonate; In the time being two or more, the ratio of each component is equal portions or other ratio.
8. outdoor LED encapsulation conductive resin as claimed in claim 1, it is characterized in that: described antioxidant is 4-methyl-2,6 DI-tert-butylphenol compounds, distearyl pentaerythritol diphosphite, three (nonyl phenol) phosphorous acid ester, two (2,4-di-tert-butyl-phenyl) pentaerythritol diphosphites, β-(3,5-di-tert-butyl-hydroxy phenyl) one or more in propionic acid octadecanol ester, four [β-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester; In the time being two or more, the ratio of each component is equal portions or other ratio.
9. outdoor LED encapsulation conductive resin as claimed in claim 1, it is characterized in that: described UV light stabilizing agent is 1-methyl-8-(1 2,2,6,6-pentamethyl--4-piperidines) sebate, salicylate, two (1,2,2,6,6-pentamethyl--4-piperidyl) one or more in sebate, two (3,5-di-tert-butyl-4-hydroxyl benzyl monoethyl phosphate) nickel, 2-(2 '-hydroxyl-3 ', 5 '-di-tert-butyl-phenyl)-5-chloro benzo triazole; In the time being two or more, the ratio of each component is equal portions or other ratio.
10. the preparation method of outdoor LED encapsulation conductive resin as described in any one in claim 1-9, is characterized in that preparation process is as follows:
(i), get the raw materials ready: take respectively by weight percentage above-mentioned each component raw material, for subsequent use;
(ii), just mixed: epoxide diluent for subsequent use, epoxy resin, silicone resin inert agents are mixed, become just batch mixing, for subsequent use;
(iii), compound: in first batch mixing for subsequent use, add epoxy hardener, curing catalyst, antioxidant and UV light stabilizing agent, mix, become compound material, for subsequent use;
(iv), mixed eventually: in compound material for subsequent use, to add conductive filler material, mix in a vacuum, be outdoor LED encapsulation conductive resin.
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| CN201410061093.9A CN103820065A (en) | 2014-02-24 | 2014-02-24 | Conductive adhesive for packaging outdoor LED |
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| CN201410061093.9A CN103820065A (en) | 2014-02-24 | 2014-02-24 | Conductive adhesive for packaging outdoor LED |
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| CN110117404A (en) * | 2018-02-05 | 2019-08-13 | 台燿科技股份有限公司 | Resin combination, and use prepreg, metal foil laminated board and printed circuit board obtained by the composition |
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| CN105111985A (en) * | 2015-08-07 | 2015-12-02 | 苏州晶雷光电照明科技有限公司 | Conductive silver adhesive for assembling LED |
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| CN109563238B (en) * | 2016-08-10 | 2021-08-27 | 三键有限公司 | Epoxy resin composition and conductive adhesive containing same |
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| JP7430892B2 (en) | 2016-08-10 | 2024-02-14 | 株式会社スリーボンド | Epoxy resin composition and conductive adhesive containing the same |
| KR102312045B1 (en) | 2016-08-10 | 2021-10-12 | 가부시끼가이샤 쓰리본드 | Epoxy resin composition and conductive adhesive comprising same |
| CN109563238A (en) * | 2016-08-10 | 2019-04-02 | 三键有限公司 | Composition epoxy resin and electrically conductive adhesive containing it |
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| CN107446520A (en) * | 2017-06-29 | 2017-12-08 | 晶丰电子封装材料（武汉）有限公司 | A kind of normal temperature cure conducting resinl and its process for connecting rechargeable battery pack |
| CN107446520B (en) * | 2017-06-29 | 2019-03-01 | 晶丰电子封装材料（武汉）有限公司 | A kind of normal temperature cure conducting resinl and its process for connecting rechargeable battery pack |
| CN110117404A (en) * | 2018-02-05 | 2019-08-13 | 台燿科技股份有限公司 | Resin combination, and use prepreg, metal foil laminated board and printed circuit board obtained by the composition |
| CN110117404B (en) * | 2018-02-05 | 2021-12-07 | 台燿科技股份有限公司 | Resin composition, and prepreg, metal foil laminate and printed wiring board produced using the same |
| CN108795373A (en) * | 2018-07-11 | 2018-11-13 | 佛山腾鲤新能源科技有限公司 | A kind of LED encapsulation filled-type conductive silver glue |
| CN111978735A (en) * | 2019-05-22 | 2020-11-24 | 天津莱尔德电子材料有限公司 | One-part curable dispensable thermal management and/or EMI mitigation materials |
| CN115011074A (en) * | 2021-08-20 | 2022-09-06 | 广东四会互感器厂有限公司 | Epoxy resin composition, preparation method and application thereof |
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