CN103980714A - High-refraction-index LED (Light Emitting Diode) organic silicon packaging material and preparation method thereof - Google Patents
High-refraction-index LED (Light Emitting Diode) organic silicon packaging material and preparation method thereof Download PDFInfo
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- CN103980714A CN103980714A CN201410243296.XA CN201410243296A CN103980714A CN 103980714 A CN103980714 A CN 103980714A CN 201410243296 A CN201410243296 A CN 201410243296A CN 103980714 A CN103980714 A CN 103980714A
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Abstract
The invention discloses a high-refraction-index LED (Light Emitting Diode) organic silicon packaging material and a preparation method thereof. The material consists of a component A and a component B, wherein the mass ratio of the component A to the component B is 5:1; the component A is prepared from the following raw materials in parts by mass: 140-160 parts of methyl high-phenyl vinyl silicon resin, 90-110 parts of vinyl phenyl silicon oil and 0.2-0.6 parts of platinum catalyst; the component B comprises 25-35 parts of high-phenyl vinyl silicon resin, 15-25 parts of methyl phenyl hydrogen silicon resin and 0.3-1 part of inhibitor. The methyl high-phenyl vinyl silicon resin is adopted to be reasonably combined with the vinyl phenyl silicon oil to provide silicon-vinyl, the high-phenyl vinyl silicon resin is adopted to be reasonably combined with the methyl phenyl hydrogen silicon resin to provide silicon hydrogen, in the presence of the catalyst and the inhibitor, the organic silicon packaging material obtained by uniformly mixing and stirring the components can have addition curing reaction when being heated, and can be applied to LED packaging to achieve the purpose of high light emission rate of an LED.
Description
Technical field
The present invention relates to LED organosilicon encapsulating material technical field, espespecially a kind of high refractive index LED organosilicon encapsulating material and preparation method thereof.
Background technology
LED is by chip, wire, support, conductive resin, the compositions such as packaged material, its encapsulation is to take to fill, the mode of embedding or mold pressing pours into liquid sizing material in the device that electronic component and circuit are housed, organosilyl main chain is that Si-O-Si side group is methyl, whole molecular chain in the shape of a spiral, this special heterochain molecular structure is given its many excellent properties, as: Si-O bond distance and bond angle are all relatively large, the steric hindrance that key rotates side group is little, segment is very submissive, thereby there is good resistance to low temperature, Si-O bond energy is relatively high simultaneously, make it have good thermostability and weathering resistance, can in wide temperature range, (50 ~ 250 °) work, low surface energy (21 ~ 22mN/m) makes it have good hydrophobicity, low surface tension and kindliness can increase the rate of permeation of polymeric system.These characteristics makes that organosilicon transmittance is high, Heat stability is good, ultraviolet resistance is strong, internal stress is little, water absorbability is low, performance is obviously better than epoxy resin, become the ideal chose of LED packaged material, but, the specific refractory power of organosilicon material is lower, the low light emission rate that can affect LED of specific refractory power, in order to improve specific refractory power and the radiation resistance of material, general selection prepared organosilicon encapsulating material containing vinyl polysiloxane and the containing hydrogen silicone oil of a certain amount of phenylbenzene silica chain link or aminomethyl phenyl silica chain link,, this class material contracts rate is low, cold-hot impact property is better.
Summary of the invention
A kind of high refractive index LED organosilicon encapsulating material of the present invention and preparation method thereof, it is characterized in that, provide a kind of high phenyl vinyl polysiloxane reasonable coordination of methyl vinyl phenyl silicone oil that utilizes to provide silicon-vinyl, high phenyl-based hydrogen-based silicone resin reasonable coordination aminomethyl phenyl based hydrogen-based silicone resin that silicon hydrogen base is provided, under catalyzer and inhibitor existence, can there is addition curing reaction in this organosilicon encapsulating material after mixing and stirring, encapsulate to realize the object of LED high light-emitting rate for LED through heating.
To achieve these goals, technical solution of the present invention is: a kind of high refractive index LED organosilicon encapsulating material is comprised of A component and B component, wherein, described A component and the mass ratio of B component are 5 ﹕ 1, and described A component comprises the raw material of following mass parts: 140～160 parts of the high phenyl vinyl polysiloxanes of methyl, 90～110 parts of vinyl phenyl silicone oils, 0.2～0.6 part of platinum group catalyst; Described B component comprises 25～35 parts of high phenyl-based hydrogen-based silicone resins, 15～25 parts of aminomethyl phenyl based hydrogen-based silicone resins, 0.3～1 part, inhibitor.
On the basis of such scheme, the present invention further can do following improvement:
Further, the high phenyl vinyl polysiloxane of described methyl is that to have chemical general formula be (PhSiO
3/2)
x1(Ph
2siO)
x2(Me
2siO)
x3(ViMe
2siO
1/2)
x4compound, the PhSiO in formula
3/2tri functional chain, the Ph in formula
2siO, Me
2siO is difunctionality chain link, ViMe
2siO
1/2it is simple function chain link; Ph in formula is phenyl, and Me is methyl, and Vi is vinyl, x1=0.55～0.60, x2=0.02～0.04, x3=0.02～0.04, x4=0.35～0.45 in formula, and its sum is satisfied with x1+x2+x3+x4=1;
Described vinyl phenyl silicone oil is that chemical general formula is ViMe
2siO (Si Me
2o)
m(SiPh
2o)
nsi Me
2the compound of Vi, the Ph in formula is phenyl, and Me is methyl, and Vi is vinyl, and the m in formula, n are and are greater than 10 and the m+n integer that is less than 50, and vinyl molecular fraction is 0.78%; Phenyl molecular fraction is 35%, and viscosity is 3050mPa ﹒ s;
Described high phenyl-based hydrogen-based silicone resin is the MDT resin with the viscosity higher of tri functional chain, difunctionality chain link and simple function chain link; Having chemical general formula is (PhSiO
3/2)
y1(Ph
2siO)
y2(Ph
3siO
1/2)
y3(HMe
2siO
1/2)
y4compound, the PhSiO in formula
3/2tri functional chain, the Ph in formula
2siO is difunctionality chain link, Ph
3siO
1/2, HMe
2siO
1/2it is simple function chain link; Ph in formula is phenyl, and Me is methyl, and Vi is vinyl, y1=0.5～0.6, y2=0.02～0.03, y3=0.02～0.03, y4=0.3～0.4 in formula, and its sum is satisfied with y1+y2+y3+y4=1;
Described aminomethyl phenyl based hydrogen-based silicone resin is the more low viscous MDT resin with tri functional chain, difunctionality chain link and simple function chain link; Having chemical general formula is (PhSiO
3/2)
z1(Me
2siO)
z2(Me
3siO
1/2)
z3(HMe
2siO
1/2)
z4compound, the PhSiO in formula
3/2tri functional chain, the Me in formula
2siO is difunctionality chain link, (Me
3siO
1/2), (HMe
2siO
1/2) be simple function chain link; Ph in formula is phenyl, and Me is methyl, and Vi is vinyl, z1=0.45～0.55, z2=0.08～0.09, z3=0.06～0.07, z4=0.30～0.35 in formula, and its sum is satisfied with z1+z2+z3+z4=1;
Described platinum group catalyst is to be selected from platinum-1,3-dimethyl-1,3-phenylbenzene-1,3-divinylsiloxanes title complex, platinum-1,1,3,3-tetramethyl--1, a kind of in 3-divinyl-sily oxide title complex, Platinic chloride-divinyl tetramethyl disiloxane title complex;
Described inhibitor is to be selected from 1-ethynylcyclohexanol, 3,3-phenylbenzene-1,5-divinyl-1,1,5,5-tetramethyl-trisiloxanes, 3-phenyl-1,5-divinyl-1,1,3, one or more in 5,5-pentamethyl-trisiloxanes, phenyl three (dimethyl vinyl siloxy) silane.
The preparation method of a kind of high refractive index LED organosilicon encapsulating material of the present invention comprises the preparation of A component and the preparation of B component; Wherein,
The preparation of described A component: be that the high phenyl vinyl polysiloxane of methyl of 140～160 parts, the vinyl phenyl silicone oil that mass parts is 90～110 parts, the platinum group catalyst that mass parts is 0.2～0.6 part join in agitator successively by mass parts, after stirring, obtain described A component;
The preparation of described B component: be the high phenyl-based hydrogen-based silicone resin of 25～35 parts, the aminomethyl phenyl based hydrogen-based silicone resin that mass parts is 15～25 parts, the inhibitor that mass parts is 0.1～0.3 part by mass parts, join successively in agitator, after stirring, obtain described B component;
During use, by described A component and the B component ratio of 5 ﹕ 1 in mass ratio, mix vacuum defoamation 30～45 minutes, point glue or filling on LED chip part to be packaged, is slowly heated to 150 ℃, and in 150 ℃ of isothermal curings 2～3 hours, stop heating, cooling, completes curing.
Advantage and disadvantage of the present invention is: silicon-vinyl and inhibition side reaction in order to addition reaction when the A component of a kind of high refractive index LED organosilicon encapsulating material of the present invention provides curing reaction occur, the platinum group catalyst of avoiding atrament to generate; When B component provides curing reaction in order to silicon-hydrogen base and the inhibitor of addition reaction; A component and B component all provide the phenyl that can improve specific refractory power and the silicone resin that increases cohesiveness and sticking power; Scheme after improvement, the high phenyl-based hydrogen-based silicone resin high viscosity of A component medium-high viscosity and more low viscous vinyl phenyl silicone oil are used in conjunction with, and B component medium-high viscosity and low viscous MDT resin be used in conjunction with, and are beneficial to each component Agitation and mixing even.
Embodiment
Embodiment 1
The preparation of A component: be the high phenyl vinyl polysiloxane of methyl of 160 grams, the vinyl phenyl silicone oil that mass parts is 90 grams, platinum-1 that mass parts is 0.6 gram by mass parts, 3-dimethyl-1,3-phenylbenzene-1,3-divinylsiloxanes title complex, join successively in agitator, after stirring, obtain described A component;
The preparation of described B component: be the high phenyl-based hydrogen-based silicone resin of 32 grams, the aminomethyl phenyl based hydrogen-based silicone resin that mass parts is 20 grams, 3-phenyl-1 that mass parts is 0.2 gram by mass parts, 5-divinyl-1,1,3,5,5-pentamethyl-trisiloxanes, joins in agitator successively, after stirring, obtain described B component;
During use, by described A component and the B component ratio of 5 ﹕ 1 in mass ratio, mix vacuum defoamation 30～45 minutes, point glue or filling on LED chip part to be packaged, is slowly heated to 150 ℃, and in 150 ℃ of isothermal curings 2～3 hours, stop heating, cooling, completes curing.
Embodiment 2
The preparation of A component: be the high phenyl vinyl polysiloxane of methyl of 140 grams, the vinyl phenyl silicone oil that mass parts is 110 grams, Platinic chloride-divinyl tetramethyl disiloxane title complex that mass parts is 0.2 gram by mass parts, join successively in agitator, after stirring, obtain described A component;
The preparation of described B component: be the high phenyl-based hydrogen-based silicone resin of 25 grams, the aminomethyl phenyl based hydrogen-based silicone resin that mass parts is 25 grams, the 1-ethynylcyclohexanol that mass parts is 0.1 gram by mass parts, join successively in agitator, after stirring, obtain described B component;
During use, by described A component and the B component ratio of 5 ﹕ 1 in mass ratio, mix vacuum defoamation 30～45 minutes, point glue or filling on LED chip part to be packaged, is slowly heated to 150 ℃, and in 150 ℃ of isothermal curings 2～3 hours, stop heating, cooling, completes curing.
Embodiment 3
The preparation of A component: be the high phenyl vinyl polysiloxane of methyl of 150 grams, the vinyl phenyl silicone oil that mass parts is 100 grams, platinum-1 that mass parts is 0.4 gram by mass parts, 1,3,3-tetramethyl--1,3-divinyl-sily oxide title complex, join successively in agitator, after stirring, obtain described A component;
The preparation of described B component: be the high phenyl-based hydrogen-based silicone resin of 35 grams, the aminomethyl phenyl based hydrogen-based silicone resin that mass parts is 15 grams, phenyl three (the dimethyl vinyl siloxy) silane that mass parts is 0.3 gram by mass parts, join successively in agitator, after stirring, obtain described B component;
During use, by described A component and the B component ratio of 5 ﹕ 1 in mass ratio, mix vacuum defoamation 30～45 minutes, point glue or filling on LED chip part to be packaged, is slowly heated to 150 ℃, and in 150 ℃ of isothermal curings 2～3 hours, stop heating, cooling, completes curing.
A component described in embodiment 1,2,3 and B component are mixed by mass ratio separately, vacuum defoamation 30 minutes, respectively according to the requirement of GB/T528-2009, by mixture levelling in mold slots, be slowly heated to 130 ℃, and in 130 ℃ of isothermal curings 2～3 hours, stop heating, cooling, completes curingly, makes sheet material.Test one: according to GB2410-80
The transmittance of test samples of sheets; Test two: require to make dumbbell shaped silica gel sample according to GB/T528-2009, test silica gel sample tensile strength, test three: according to GB/T2411-2008 test silica gel sample hardness; Test three: the specific refractory power of utilizing Abbe refractometer test silica gel sample.
Table one: performance index table
| Performance index ﹨ sample | Embodiment 1 | Embodiment 2 | Embodiment 3 |
| Transmittance (%) after solidifying | 95.5/(585nm) | 95.3/(585nm) | 95.7/(585nm) |
| Tensile strength (MPa) | 6.55 | 6.17 | 6.39 |
| Hardness (A) after solidifying | 65 | 69 | 67 |
| Specific refractory power | 1.51 | 1.52 | 1.51 |
By table one, can find out, samples of sheets (1mm is thick) after the sample solidifies of embodiment 1,2,3, at 585 its transmittances of nm wavelength all more than 95%, tensile strength is more than 6.17MPa, hardness 66A～69A after solidifying, specific refractory power, more than 1.51, has all reached re-set target, is suitable for the encapsulation of power LED.
The above; embodiment is only that the preferred embodiment of the present invention is described; not scope of the present invention is limited; under the prerequisite of spirit that does not depart from the technology of the present invention; various distortion and improvement that this area engineering technical personnel make technical scheme of the present invention, all should fall in the definite protection domain of claims of the present invention.
Claims (2)
1. high refractive index LED organosilicon encapsulating material and preparation method thereof, it is characterized in that: described a kind of high refractive index LED organosilicon encapsulating material is comprised of A component and B component, wherein, described A component and the mass ratio of B component are 5 ﹕ 1, and described A component comprises the raw material of following mass parts: 140～160 parts of the high phenyl vinyl polysiloxanes of methyl, 90～110 parts of vinyl phenyl silicone oils, 0.2～0.6 part of platinum group catalyst; Described B component comprises 25～35 parts of high phenyl-based hydrogen-based silicone resins, 15～25 parts of aminomethyl phenyl based hydrogen-based silicone resins, 0.3～1 part, inhibitor;
The preparation method of described a kind of high refractive index LED organosilicon encapsulating material comprises the preparation of A component and the preparation of B component; Wherein,
The preparation of described A component: be that the high phenyl vinyl polysiloxane of methyl of 140～160 parts, the vinyl phenyl silicone oil that mass parts is 90～110 parts, the platinum group catalyst that mass parts is 0.2～0.6 part join in agitator successively by mass parts, after stirring, obtain described A component;
The preparation of described B component: be the high phenyl-based hydrogen-based silicone resin of 25～35 parts, the aminomethyl phenyl based hydrogen-based silicone resin that mass parts is 15～25 parts, the inhibitor that mass parts is 0.1～0.3 part by mass parts, join successively in agitator, after stirring, obtain described B component.
2. a kind of high refractive index LED organosilicon encapsulating material according to claim 1 and preparation method thereof, is characterized in that: the high phenyl vinyl polysiloxane of described methyl is that to have chemical general formula be (PhSiO
3/2)
x1(Ph
2siO)
x2(Me
2siO)
x3(ViMe
2siO
1/2)
x4compound, the PhSiO in formula
3/2tri functional chain, the Ph in formula
2siO, Me
2siO is difunctionality chain link, ViMe
2siO
1/2it is simple function chain link; Ph in formula is phenyl, and Me is methyl, and Vi is vinyl, x1=0.55～0.60, x2=0.02～0.04, x3=0.02～0.04, x4=0.35～0.45 in formula, and its sum is satisfied with x1+x2+x3+x4=1; Described vinyl phenyl silicone oil is that chemical general formula is ViMe
2siO (Si Me
2o)
m(SiPh
2o)
nsi Me
2the compound of Vi, the Ph in formula is phenyl, and Me is methyl, and Vi is vinyl, and the m in formula, n are and are greater than 10 and the m+n integer that is less than 50, and vinyl molecular fraction is 0.78%; Phenyl molecular fraction is 35%, and viscosity is 3050mPa ﹒ s; Described high phenyl-based hydrogen-based silicone resin is the MDT resin with the viscosity higher of tri functional chain, difunctionality chain link and simple function chain link; Having chemical general formula is (PhSiO
3/2)
y1(Ph
2siO)
y2(Ph
3siO
1/2)
y3(HMe
2siO
1/2)
y4compound, the PhSiO in formula
3/2tri functional chain, the Ph in formula
2siO is difunctionality chain link, Ph
3siO
1/2, HMe
2siO
1/2it is simple function chain link; Ph in formula is phenyl, and Me is methyl, and Vi is vinyl, y1=0.5～0.6, y2=0.02～0.03, y3=0.02～0.03, y4=0.3～0.4 in formula, and its sum is satisfied with y1+y2+y3+y4=1; Described aminomethyl phenyl based hydrogen-based silicone resin is the more low viscous MDT resin with tri functional chain, difunctionality chain link and simple function chain link; Having chemical general formula is (PhSiO
3/2)
z1(Me
2siO)
z2(Me
3siO
1/2)
z3(HMe
2siO
1/2)
z4compound, the PhSiO in formula
3/2tri functional chain, the Me in formula
2siO is difunctionality chain link, (Me
3siO
1/2), (HMe
2siO
1/2) be simple function chain link; Ph in formula is phenyl, and Me is methyl, and Vi is vinyl, z1=0.45～0.55, z2=0.08～0.09, z3=0.06～0.07, z4=0.30～0.35 in formula, and its sum is satisfied with z1+z2+z3+z4=1; Described platinum group catalyst is to be selected from platinum-1,3-dimethyl-1,3-phenylbenzene-1,3-divinylsiloxanes title complex, platinum-1,1,3,3-tetramethyl--1, a kind of in 3-divinyl-sily oxide title complex, Platinic chloride-divinyl tetramethyl disiloxane title complex; Described inhibitor is to be selected from 1-ethynylcyclohexanol, 3,3-phenylbenzene-1,5-divinyl-1,1,5,5-tetramethyl-trisiloxanes, 3-phenyl-1,5-divinyl-1,1,3, one or more in 5,5-pentamethyl-trisiloxanes, phenyl three (dimethyl vinyl siloxy) silane.
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