CN102746487A - LED-packaging epoxy resin composition - Google Patents
LED-packaging epoxy resin composition Download PDFInfo
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- CN102746487A CN102746487A CN2012101586726A CN201210158672A CN102746487A CN 102746487 A CN102746487 A CN 102746487A CN 2012101586726 A CN2012101586726 A CN 2012101586726A CN 201210158672 A CN201210158672 A CN 201210158672A CN 102746487 A CN102746487 A CN 102746487A
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Abstract
The invention discloses a method for improving the performance of a large-power high-light-transmittance LED packaging epoxy resin composition. The composition is composed of a component A and a component B. The composition has excellent UV resistance and yellowing resistance. The composition is advantaged in good manufacturability, good light transmittance, and low light failure. The composition can be used in white-light and blue-light LED packaging. Compared with organosilicon, the composition is advantaged in low price. Innovatively, the component A of the composition is composed of liquid cycloaliphatic epoxy resin, solid cycloaliphatic epoxy resin, and hydrogenated bisphenol A epoxy resin. An anti-forming agent, a color complementary agent, and a dispensing agent are adopted in auxiliary. The system does not contain benzene ring, and yellowing is not easy to occur. The component B is prepared through the steps that: methyl hexahydrophthalic anhydride and hexahydrophthalic anhydride are subjected to a polymerization reaction with promoting agents or cationic initiators such as quaternary phosphonium salt, quaternary ammonium salts, DBU salt, and imidazole; with added phosphate antioxidant, a thermal yellowing capacity is improved. With the applications of an ultraviolet absorber and a light stabilizer, a UV yellowing resisting effect is further improved.
Description
Technical field
The present invention relates to a kind of epoxy resin composite, specifically is a kind of epoxy resin composite that can improve white light LEDs packaged material performance.
Background technology
Because common bisphenol A epoxide resin itself exists thermal conductivity low, phenyl ring is prone to electronics π-π transition takes place and xanthochromia causes some defectives of aspect such as weathering resistance, so under high temperature and the situation than intensive ultraviolet irradiation, be easy to change, influences performance.
Shown in accompanying drawing 6, the light decay of white light is the rapidest, and is therefore when white light LEDs encapsulates, high especially to the performance requriements of resin.
For the epoxy packages of LED, general requirement epoxy resin has higher transparency and stronger anti-xanthochromia ability.Because the part UV-light can leak to the outside in the LED fluorescent material conversion process, so in high printing opacity LED encapsulation field, xanthochromia and thermic xanthochromia that uv irradiation is produced require very high.And epoxy resin is with respect to the congenital price advantage of silicone resin, high hardness intensity and bonding force, so still have stronger magnetism in the high printing opacity LED encapsulation field of white light LEDs and blue-ray LED.
White light LEDs encapsulates the epoxy-resin systems of usefulness, generally will select not to be with the alicyclic resin or the Hydrogenated Bisphenol A 99 resin of phenyl ring.Alicyclic resin commonly used is ERL4221.These several kinds of resins respectively have characteristic.ERL4221 viscosity is low, good manufacturability, and good heat resistance, electrical property is excellent, but cross-linking density is big, and fragility is bigger; Hydrogenated Bisphenol A 99 is in the low good manufacturability of viscosity, and pliability is good, and second-order transition temperature is low, but the poor heat resistance after solidifying.
Add the white light LEDs encapsulation system of fluorescent material for needs; Because the viscosity pole of ERL4221 and hydrogenated bisphenol A epoxy resin is low; So complementary color agent and fluorescent material free settling in storage and solidification process are need be through increasing the sedimentation that viscosity suppresses fluorescent material to system.Increasing method of viscosity has a lot, except out of use bisphenol A epoxide resin, can also add solid or HV alcohols and auxiliary rheological agents etc.For these schemes, though can improve viscosity, other performances have been sacrificed, like thermotolerance, light transmission etc.
How under the situation that guarantees optical property and thermal property, to improve the key that manufacturability just becomes the white light LEDs formulating of recipe.
Summary of the invention
One of purpose of this patent embodiment is to provide a kind of white light of manufacturability and light transmission or epoxy resin composite of blue-ray LED encapsulation usefulness of having improved.A kind of LED encapsulating epoxy resin mixture comprises following A component and B component:
The A component comprises:
The B component comprises:
Scheme further is: said solid cycloaliphatic epoxy resin is EHPE3150.
Scheme further is: said liquid alicyclic epoxy resin is 3,4-epoxycyclohexyl methyl 3, any one among 4-epoxycyclohexyl manthanoate, Celloxide 2000, the Celloxide 2080.
The A component is made up of liquid alicyclic epoxy resin, solid cycloaliphatic epoxy resin and hydrogenated bisphenol A epoxy resin jointly, can come the viscosity and the second-order transition temperature of regulation system through the collocation of three's different ratios.
Scheme further is: said skimmer is any one among BYK-A530, Defom 5400, the BYK-141.The consistency of skimmer and epoxy resin is good, does not influence transmittance.
Scheme further is: blueness that the mixture that said complementary color agent is ultramarine and epoxy resin is mixed with or purple transparent liquid.The requirement colouring power is moderate, excellent heat resistance, and transparency is high.
Scheme further is: said polyvalent alcohol is a glycerine, 1,4-butyleneglycol, 1, any one in 6-pinakon, the NSC 6366.Be used to the viscosity of the system of adjusting, the snappiness of improving technology and increasing system.
Scheme further is: any one in said promotor Wei quaternary alkylphosphonium salt, quaternary ammonium salt, DBU salt, imidazoles or the special-purpose cationic initiator.Have the transmittance height, reaction heat is low, anti-xanthochromia excellent characteristics.
Scheme further is: said oxidation inhibitor is two (3; The 5-di-tert-butyl-phenyl) pentaerythritol diphosphites (oxidation inhibitor 626); And phosphite antioxidant TP-10, TP-10H, 317,517, the polymerizability phosphite antioxidant TP-20 of the two key chemical companies in three (2, the 4-di-tert-butyl-phenyl) phosphorous acid ester, CGA12 or the Taiwan of Ciba, contain be obstructed the multiple functional radical phosphite antioxidant TP-80 of phenolic group and macromole base and their compound system.The anti-xanthochromia ability of these oxidation inhibitor in curing and use strengthens greatly, particularly resistance toheat
Scheme further is: said uv-absorbing agent is 2-hydroxyl-4-methoxy benzophenone (UV-9), 2-hydroxyl-4-octyloxy UVNUL MS-40 (UV-531), 2-(2 '-hydroxyl-5 ' aminomethyl phenyl) benzotriazole (UV-P), 2-(2 ' hydroxyl-5 ' uncle octyl phenyl) benzotriazole (UV-329), 2; 4-dihydroxy benaophenonel (UV-0), 2-Phenylbenzimidazole-5-sulfonic acid (UV-T), 2-(2H-benzotriazole-2-yl)-4; 6-two (1-methyl-phenylethyl) phenol (UV-234), 2-(2H-benzotriazole-2-yl)-6-(dodecyl)-4-methylphenol (UV-571), 2-(2 '-hydroxyl-the 3 '-tertiary butyl-5 '-aminomethyl phenyl)-5-chlorinated benzotriazole (UV-326), 2-(2 '-hydroxyl-3 '; 5 '-di-tert-butyl-phenyl)-5-chlorinated benzotriazole (UV-327), 2 benzotriazole-2-base-4; 6-DI-tert-butylphenol compounds (UV-320), 2-(2H-benzotriazole-2-yl)-4; 6-di-tert-pentyl phenol (UV-328), 2-(2 '-hydroxyl-3 '-isobutyl--the 5 '-tertiary butyl) benzotriazole (UV-325), 2-(2 '-hydroxyl-3 '-[1; The 1-3,5-dimethylphenyl]-5 '-[1; 1; 3; 3 ,-tetramethyl butyl]) benzotriazole (UV-5228), 2,2 ' methylene radical-(6-(2H-benzotriazole)-uncle's 4-octyl group) phenol (UV-5431), 2-(2 '-hydroxyl-3 ' tertiary butyl, 5 '-n-octyl propionate)-benzotriazole (UV5582), 2-cyanic acid-3; 3-diphenyl-ethyl acrylate (UV-335), 2-cyanic acid-3; 3-diphenylacrylate monooctyl ester (UV-336), N-(2-ethoxyl phenenyl)-N '-(4-ethylphenyl) oxalamide (UV-1033), N-(4 benzoic acid ethyl ester) N ', one or more in N '-(methyl, phenyl) carbonamidine (UV-971); Said photostabilizer is Succinic Acid and (4-hydroxyl-2,2,6, the polymkeric substance of 6-tetramethyl--1-piperidines alcohol) (photostabilizer 622), two (2,2,6; 6-tetramethyl--4-piperidyl) sebate (photostabilizer 770), gather-{ [6-[(1,1,3,3 ,-tetramethyl butyl)-amido] 1,3; 5 ,-triazine-2,4-two bases] [(2,2,6, the 6-tetramethyl-piperidyl)-imido grpup]-1; 6-hexane two bases-[(2,2,6, the 6-tetramethyl-piperidyl)-imido grpup] } the two 1-octyloxies-2,2 of (photostabilizer 944), two (3,5-di-t-butyl-4 hydroxybenzyl monoethyl phosphate) nickel (photostabilizer 802), sebacic acid; 6,6-tetramethyl piperidine alcohol ester (photostabilizer 523), sebacic acid two 1,2,2,6; Mixture (3:1) (photostabilizer 292), the methylacrylic acid (1 of 6-pentamethyl-piperidines alcohol ester and (1,2,2,6,6-pentamethyl-piperidines alcohol) sebacic acid methyl esters; 2,2,6,6-pentamethyl-piperidines alcohol) ester (photostabilizer 582L), two (1,2; 2,6,6-pentamethyl-piperidines alcohol)-α-(3,5-di-tert-butyl-hydroxy phenyl methylene radical-α '-butyl-malonic ester) (photostabilizer 5144), N, N '-(2; 2,6,6 ,-tetramethyl-, 4-anilinic piperidines)-in the isophthaloyl amine (photostabilizer SU) one or more.Select the plural components of uv-absorbing agent and photostabilizer, can further improve weathering resistance and anti-UV property.
Scheme further is: said solidifying agent is methyl hexahydrophthalic anhydride or methyl hexahydrophthalic anhydride and HHPA compound system; Wherein the consumption of methyl hexahydrophthalic anhydride accounts for 20～99.9% of methyl hexahydrophthalic anhydride and HHPA compound system, and the consumption of HHPA accounts for 0～80% of methyl hexahydrophthalic anhydride and HHPA compound system.
In this patent, we regulate viscosity through adding solid cycloaliphatic epoxy resin EHPE3150.EHPE3150 has thermotolerance and the electrical property higher than liquid alicyclic epoxy resin, but owing to be solid-state under the normal temperature, uses manufacturability poor slightly separately.The consistency property is good when with liquid alicyclic epoxy resin and hydrogenated bisphenol A epoxy resin mixing, can prepare burden according to specific requirement, and the consumption of three kinds of resins can be selected between 1～99%, carries out the consumption combination according to concrete viscosity and processing requirement.
Three kinds of epoxy resin that use in this patent all do not contain phenyl ring, have higher anti-xanthochromia ability.Wherein low viscous liquid alicyclic epoxy resin mainly rises and improves thermotolerance and anti-xanthochromic effect, but the cross-linking density of itself is big, and fragility is bigger; It is many that the thermotolerance of hydrogenated bisphenol A epoxy resin has been compared the cycloaliphatic epoxy resin difference, and anti-xanthochromia is better under the situation with uv irradiating but it is heated, and anti-deflection and water tolerance are better; And the consistency of solid alicyclic resin EHPE3150 and above two kinds of resins is good, and good heat resistance, and photoelectric properties are excellent, and can prevent the sedimentation of complementary color agent and fluorescent material through adding the viscosity index of regulating mixture.
This patent can use outer release agent spraying separately, also can use inner pattern releasing agent applicable and outer release agent spraying simultaneously, also can use inner pattern releasing agent applicable separately.Inner pattern releasing agent applicable or outer release agent spraying that this patent uses all must be that transparency is high, and the inner pattern releasing agent applicable of use is requirement and epoxy and good liquid or solid compound or the mixture of anhydride system consistency also.
Through the mixing of three kinds of resins, the performance that both can guarantee this LED encapsulating epoxy resin mixture most critical promptly has the excellent fast light ability of declining, and lights secular that guaranteed performance can not be affected in the use; Secondly, glue has certain resistance to cracking, can in curing and high low temperature test process, not produce phenomenons such as dead lamp and cracking; And significantly, the use characteristics of glue such as viscosity, defoaming, anti-settling property etc. also are guaranteed.
Description of drawings
Fig. 1 is the ERL4221 structural formula;
Fig. 2 is the EHPE3150 structural formula;
Fig. 3 is Celloxide 2000 structural formulas;
Fig. 4 is the Celloxide2080 structural formula;
Fig. 5 is the cationic initiator structural formula; Wherein R is an alkyl, and Ar is a phenyl;
Fig. 6 is a LED light decay synoptic diagram of all kinds.
Embodiment
Embodiment 1
Performance before solidifying:
Processing condition:
Be weight mixing match such as A component and B component to be equivalent to 1:1 here mix to stir and be cured, solidifying then generally is to carry out stage by stage, the demoulding after 130 ℃ of half a hour to 1 hour, and 130 ℃ of 6-8 hour after fixing then, 150 ℃ heat up and solidify 1h then.
Solidify the back performance:
Comparative Examples 1
Comparative Examples 2
The Comparative Examples explanation:
For embodiment 1, this Comparative Examples has only been used liquid alicyclic epoxy resin, viscosity below 300cps, the complementary color agent meeting sedimentation of room temperature storage for some time, especially in summer, about 1 week just can see obviously that the complementary color agent precipitates under the room temperature more than 30 ℃; And the fluorescent material that in solidification process, adds owing to also can be very under the condition of high temperature fast sedimentation and can't homodisperse solidifying influence the quality after the curing.And pure ERL4221 system is very high owing to cross-linking density, and the Tg after the curing is up to 180 ℃, and fragility is big, breaks gold thread easily.
For embodiment 2, this Comparative Examples has only been used hydrogenated bisphenol A epoxy resin, and viscosity is below 500cps, and the complementary color agent of room temperature storage for some time also can sedimentation; And the fluorescent material that in solidification process, adds owing to also can be very under the condition of high temperature fast sedimentation and can't homodisperse solidifying influence the quality after the curing.And pure Hydrogenated Bisphenol A 99 system is very low owing to activity, and the Tg after the curing is very low, though pliability is good, thermotolerance is too poor, and Tg only about 100 ℃, all is prone to feel like jelly in use and solidification process.
Certainly, if be impossible certainly only with the solid alicyclic resin.
Embodiment 2
Explain:
The comparative example 1, and present embodiment has increased the consumption of solid alicyclic resin EHPE3150, so the viscosity of A component can be brought up to more than the 7000cps.
Embodiment 3
The comparative example 1, and present embodiment has reduced the consumption of solid alicyclic resin EHPE3150, so the viscosity of A component is reduced to below the 1000cps.
Claims (10)
1. a LED encapsulating epoxy resin mixture comprises following A component and B component, it is characterized in that:
The A component comprises:
The B component comprises:
2. according to the said LED encapsulating epoxy resin of claim 1 mixture, it is characterized in that: said solid cycloaliphatic epoxy resin is EHPE3150.
3. according to the said LED encapsulating epoxy resin of claim 1 mixture; It is characterized in that: said liquid alicyclic epoxy resin; Be 3,4-epoxycyclohexyl methyl 3, any one among 4-epoxycyclohexyl manthanoate, Celloxide 2000, the Celloxide 2080.
4. according to the said LED encapsulating epoxy resin of claim 1 mixture, it is characterized in that: said skimmer is any one among BYK-A530, Defom 5400, the BYK-141.
5. according to the said LED encapsulating epoxy resin of claim 1 mixture, it is characterized in that: blueness that the mixture that said complementary color agent is ultramarine and epoxy resin is mixed with or purple transparent liquid.
6. according to the said LED encapsulating epoxy resin of claim 1 mixture, it is characterized in that: said polyvalent alcohol is a glycerine, 1,4-butyleneglycol, 1, any one in 6-pinakon, the NSC 6366.
7. according to the said LED encapsulating epoxy resin of claim 1 mixture, it is characterized in that: any one in said promotor Wei quaternary alkylphosphonium salt, quaternary ammonium salt, DBU salt, imidazoles or the special-purpose cationic initiator.
8. according to the said LED encapsulating epoxy resin of claim 1 mixture; It is characterized in that: said oxidation inhibitor is two (3; The 5-di-tert-butyl-phenyl) pentaerythritol diphosphites; And phosphite antioxidant TP-10, TP-10H, 317,517, the polymerizability phosphite antioxidant TP-20 of the two key chemical companies in three (2, the 4-di-tert-butyl-phenyl) phosphorous acid ester, CGA12 or the Taiwan of Ciba, contain be obstructed the multiple functional radical phosphite antioxidant TP-80 of phenolic group and macromole base and their compound system.
9. according to the said LED encapsulating epoxy resin of claim 1 mixture; It is characterized in that: said uv-absorbing agent is 2-hydroxyl-4-methoxy benzophenone, 2-hydroxyl-4-octyloxy UVNUL MS-40,2-(2 '-hydroxyl-5 ' aminomethyl phenyl) benzotriazole, 2-(2 ' hydroxyl-5 ' uncle octyl phenyl) benzotriazole, 2; 4-dihydroxy benaophenonel, 2-Phenylbenzimidazole-5-sulfonic acid, 2-(2H-benzotriazole-2-yl)-4; 6-two (1-methyl-phenylethyl) phenol, 2-(2H-benzotriazole-2-yl)-6-(dodecyl)-4-methylphenol, 2-(2 '-hydroxyl-the 3 '-tertiary butyl-5 '-aminomethyl phenyl)-5-chlorinated benzotriazole, 2-(2 '-hydroxyl-3 '; 5 '-di-tert-butyl-phenyl)-and 5-chlorinated benzotriazole, 2 benzotriazole-2-base-4,6-DI-tert-butylphenol compounds, 2-(2H-benzotriazole-2-yl)-4,6-di-tert-pentyl phenol, 2-(2 '-hydroxyl-3 '-isobutyl--the 5 '-tertiary butyl) benzotriazole, 2-(2 '-hydroxyl-3 '-[1; The 1-3,5-dimethylphenyl]-5 '-[1; 1,3,3;-tetramethyl butyl]) benzotriazole, 2; 2 ' methylene radical-(6-(2H-benzotriazole)-uncle's 4-octyl group) phenol, 2-(2 '-hydroxyl-3 ' tertiary butyl, 5 '-n-octyl propionate)-benzotriazole, 2-cyano-3,3-diphenyl ethyl acrylate, 2-cyanic acid-3,3-diphenylacrylate monooctyl ester, N-(2-ethoxyl phenenyl)-N '-(4-ethylphenyl) oxalamide, N-(4 benzoic acid ethyl ester) N '; In N '-(methyl, phenyl) carbonamidine one or more; Said photostabilizer is Succinic Acid with (4-hydroxyl-2,2,6, the polymkeric substance of 6-tetramethyl--1-piperidines alcohol), two (2,2,6,6-tetramethyl--4-piperidyl) sebate, gather-{ [6-[(1; 1,3,3 ,-tetramethyl butyl)-amido] 1,3,5;-triazine-2,4-two bases] [(2,2,6, the 6-tetramethyl-piperidyl)-imido grpup]-1,6-hexane two bases-[(2; 2,6,6-tetramethyl-piperidyl)-imido grpup], two (3,5-di-t-butyl-4 hydroxybenzyl monoethyl phosphate) nickel, the two 1-octyloxies-2,2 of sebacic acid, 6; 6-tetramethyl piperidine alcohol ester, sebacic acid are two 1,2,2,6,6-pentamethyl-piperidines alcohol ester and (1,2; 2,6,6-pentamethyl-piperidines alcohol) mixture (3:1), the methylacrylic acid (1,2,2,6 of sebacic acid methyl esters; 6-pentamethyl-piperidines alcohol) ester, two (1,2,2,6,6-pentamethyl-piperidines alcohol)-α-(3,5-di-tert-butyl-hydroxy phenyl methylene radical-α '-butyl-malonic ester), N; In N '-(2,2,6,6 ,-tetramethyl-, 4-anilinic piperidines)-isophthaloyl amine one or more.
10. according to the said LED encapsulating epoxy resin of claim 1 mixture; It is characterized in that: said solidifying agent is methyl hexahydrophthalic anhydride or methyl hexahydrophthalic anhydride and HHPA compound system; Wherein the consumption of methyl hexahydrophthalic anhydride accounts for 20～99.9% of methyl hexahydrophthalic anhydride and HHPA compound system, and the consumption of HHPA accounts for 0～80% of methyl hexahydrophthalic anhydride and HHPA compound system.
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