CN103013431B - High-refractivity LED (Light-Emitting Diode) package silica gel - Google Patents

High-refractivity LED (Light-Emitting Diode) package silica gel Download PDF

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CN103013431B
CN103013431B CN201210508506.4A CN201210508506A CN103013431B CN 103013431 B CN103013431 B CN 103013431B CN 201210508506 A CN201210508506 A CN 201210508506A CN 103013431 B CN103013431 B CN 103013431B
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methyl phenyl
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refractive index
high refractive
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CN103013431A (en
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陈维
庄恒冬
王建斌
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YANTAI DEBANG ADVANCED SILICON MATERIALS CO Ltd
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YANTAI DEBANG ADVANCED SILICON MATERIALS CO Ltd
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Abstract

The invention relates to a high-refractivity LED (Light-Emitting Diode) package silica gel. The high-refractivity LED package silica gel comprises components A and B, the weight ratio of which is 1:1, wherein the component A comprises the following raw materials in parts by weight: 50-60 parts of methyl phenyl vinyl silicon resin, 35-45 parts of methyl phenyl vinyl polysiloxane, 0.1-0.3 part of platinum catalyst, and 1-5 parts of adhesive; and the component B comprises the following raw materials in parts by weight: 50-70 parts of crosslinking agent methyl phenyl hydrogen-containing silicon resin, 30-50 parts of methyl phenyl vinyl silicon resin, and 0.1-0.3 part of inhibitor. The high-refractivity LED package silica gel has high refractivity, high strength and high adhesion.

Description

A kind of LED packaging silicon rubber of high refractive index
Technical field
The present invention relates to a kind of LED packaging silicon rubber of high refractive index, particularly relate to the LED packaging silicon rubber of a kind of high refractive index, high strength, high adhesion, belong to adhesive technology field.
Background technology
Along with LED application is more and more extensive, also more and more higher to the requirement of LED packaged material.The current packaged material used of LED mainly contains epoxy resin and organosilicon material, epoxy resin internal stress is excessive, xanthochromia, and high and low temperature resistance is poor, loss of properties on aging, the organosilicon material of low-refraction, internal stress is little, and high and low temperature resistance is good, xanthochromia not, over-all properties is obviously better than epoxy resin, and therefore rapid substituted epoxy resin, is widely used in LED encapsulation field.
But the organosilicon material of the low-refraction encapsulating for LED is due to specific refractory power lower (1.40), differ larger with chip specific refractory power (2~4), excessive causing of refractive index difference can occur in total reflection, light reflection is returned to chip internal and cannot effectively derive, therefore improve the specific refractory power of packaged material, can reduce the generation of total reflection, thereby improved, get optical efficiency.
Although the LED packaging silicon rubber specific refractory power of current domestic high refractive index can reach between 1.50~1.55, but owing to generally adopting and only containing phenyl vinyl polysiloxane in formulating of recipe, linking agent is not resinous, silicone resin content is low, and do not contain caking agent, so there is the feature that intensity is low, poor to substrate bonding.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of LED packaging silicon rubber of high refractive index.
The technical scheme that the present invention solves the problems of the technologies described above is as follows: a kind of LED packaging silicon rubber of high refractive index, comprise component A and B component, and the weight ratio of described component A and B component is 1:1;
Wherein, described component A comprises the raw material of following weight part: 50~60 parts of methyl phenyl vinyl polysiloxanes, 35~45 parts of methyl phenyl vinyl polysiloxane, 0.1~0.3 part of platinum group catalyst, 1~5 part of caking agent; Described B component comprises the raw material of following weight part: 50~70 parts of linking agent aminomethyl phenyl Silicon Containing Hydrogen resins, 30~50 parts of methyl phenyl vinyl polysiloxanes, 0.1~0.3 part, inhibitor.
The invention has the beneficial effects as follows: the LED packaging silicon rubber of high refractive index of the present invention is by A, B component forms, A component provides high-intensity resin in reaction, vinyl, catalyzer and caking agent, B component provides high-intensity resin, linking agent, vinyl and inhibitor, the LED packaging silicon rubber of high refractive index of the present invention, except methyl phenyl vinyl polysiloxane contains silicone resin, its linking agent aminomethyl phenyl Silicon Containing Hydrogen resin substitutes aminomethyl phenyl hydrogen containing siloxane, the content of silicone resin increases, and added the caking agent of special construction, thereby improved intensity after solidifying, and excellent to base material sticking power.
On the basis of technique scheme, the present invention can also do following improvement.
Further, described methyl phenyl vinyl polysiloxane molecular formula is: (ViMe 2siO 1/2) 3(PhSiO 3/2) 7, wherein, described Me is methyl, and Vi is vinyl, and Ph is phenyl.
Adopting the beneficial effect of above-mentioned further scheme to be, as matrix resin, is a kind of silicone resin, has both contained vinyl and can participate in crosslinking reaction, also contains phenyl, can improve product specific refractory power.
Further, the molecular formula of described methyl phenyl vinyl polysiloxane is: ViMePhSiO 1/2, wherein, described Me is methyl, and Vi is vinyl, and Ph is phenyl.
Adopt the beneficial effect of above-mentioned further scheme to be, provide the adding of methyl phenyl vinyl polysiloxane can improve specific refractory power phenyl, can participate in the vinyl of reaction, and reduced the viscosity of system.
Further, described caking agent contains phenyl, epoxy and acryloxy functional group, and its structural formula is:
Figure GDA0000452817720000021
N wherein 1scope is 10~20, n 2scope is 10~20, n 3scope be 20~40.
Further, described platinum group catalyst is any one in platinum-methyl phenyl silicone title complex or platinum-olefin(e)complex.Be preferably platinum-methyl phenyl silicone title complex, wherein, platinum content is 3000~7000ppm.
Further, described linking agent is hydrogeneous silicone resin, and wherein, the molecular formula of described Silicon Containing Hydrogen resin is: (HMe 2siO 1/2) 3(PhSiO 3/2) 7, described Me is methyl, Ph is phenyl.
Adopting the beneficial effect of above-mentioned further scheme to be, as linking agent, is also a kind of silicone resin, not only provide reactive hydrogen to participate in crosslinking reaction, phenyl can improve whole system intensity and specific refractory power, and viscosity is low, for whole system, play reduced viscosity, the effect that intensity improves.
Further, described inhibitor is any one in ethynylcyclohexanol or 1,1,3-triphenyl-2-propine-1-alcohol.Be preferably 1,1,3-triphenyl-2-propine-1-alcohol, its structural formula is as follows:
Figure GDA0000452817720000031
The preparation method of the LED packaging silicon rubber of high refractive index of the present invention comprises the preparation process of A component and the preparation process of B component; Wherein,
The preparation process of described A component is as follows: by parts by weight, be 0.1~0.3 part of 35~45 parts of methyl phenyl vinyl polysiloxane, methyl phenyl vinyl polysiloxane, catalyzer, 1~5 part of the caking agent of 50~60 parts, add successively in stirrer, mixing and stirring, obtains described A component;
The preparation process of described B component is as follows: 10~30 parts of methyl phenyl vinyl polysiloxanes, 70~90 parts of aminomethyl phenyl Silicon Containing Hydrogen resins, and 0.1~0.3 part, inhibitor, adds in stirrer successively, and mixing and stirring obtains described B component;
During use, by described A component, B component by weight for the proportioning of 1:1 mixes, vacuum defoamation 20~40 minutes, point glue or encapsulating are on to be packaged, first at 100~120 ℃ of temperature, heat 0.5~1.5 hour, then 100~200 ℃ of heating 3~5 hours, solidify.
Embodiment
Below principle of the present invention and feature are described, example, only for explaining the present invention, is not intended to limit scope of the present invention.
A LED packaging silicon rubber for high refractive index, comprises component A and B component, and the weight ratio of described component A and B component is 1:1;
Wherein, described component A comprises the raw material of following weight part: 50~60 parts of methyl phenyl vinyl polysiloxanes, 35~45 parts of methyl phenyl vinyl polysiloxane, 0.1~0.3 part of platinum group catalyst, 1~5 part of caking agent; Described B component comprises the raw material of following weight part: 50~70 parts of linking agent aminomethyl phenyl Silicon Containing Hydrogen resins, 30~50 parts of methyl phenyl vinyl polysiloxanes, 0.1~0.3 part, inhibitor.
Below by several concrete preparation method embodiment to illustrate the present invention.(above parts by weight represent by grams in specific embodiment)
Embodiment 1
The preparation of A component: take methyl phenyl vinyl polysiloxane 50g, methyl phenyl vinyl polysiloxane 48.9g, caking agent 1g(structural formula), catalyst platinum-methyl phenyl silicone title complex 0.1g, platinum content 7000ppm, add successively in stirrer, mixing and stirring, obtains described A component;
The preparation of B component: take methyl phenyl vinyl polysiloxane 29.9g, linking agent aminomethyl phenyl Silicon Containing Hydrogen resin 70g, inhibitor 1,1,3-triphenyl-2-propine-1-alcohol 0.1g, adds in stirrer successively, and mixing and stirring, obtains described B component;
During use, by described A component, B component by weight for the proportioning of 1:1 mixes, vacuum defoamation 20 minutes, some glue or encapsulating in to be packaged upper, first 120 ℃ of heating 1 hour, then heat 4 hours at 150 ℃.
Embodiment 2
The preparation of A component: take methyl phenyl vinyl polysiloxane 60g, methyl phenyl vinyl polysiloxane 34.7g, caking agent 5g(structural formula), catalyst platinum-methyl phenyl silicone title complex 0.3g, platinum content 7000ppm, add successively in stirrer, mixing and stirring, obtains described A component;
The preparation of B component: take methyl phenyl vinyl polysiloxane 9.7g, linking agent aminomethyl phenyl Silicon Containing Hydrogen resin 90g, inhibitor 1,1,3-triphenyl-2-propine-1-alcohol 0.3g, adds in stirrer successively, and mixing and stirring, obtains described B component;
During use, by described A component, B component by weight for the proportioning of 1:1 mixes, vacuum defoamation 20 minutes, some glue or encapsulating in to be packaged upper, first 120 ℃ of heating 1 hour, then heat 4 hours at 150 ℃.
Embodiment 3
The preparation of A component: take methyl phenyl vinyl polysiloxane 55g, methyl phenyl vinyl polysiloxane 41.8g, caking agent 3g(structural formula), catalyst platinum-methyl phenyl silicone title complex 0.2g, platinum content 7000ppm, add successively in stirrer, mixing and stirring, obtains described A component;
The preparation of B component: take methyl phenyl vinyl polysiloxane 19.8g, linking agent aminomethyl phenyl Silicon Containing Hydrogen resin 80g, inhibitor 1,1,3-triphenyl-2-propine-1-alcohol 0.2g, adds in stirrer successively, and mixing and stirring, obtains described B component;
During use, by described A component, B component by weight for the proportioning of 1:1 mixes, vacuum defoamation 20 minutes, some glue or encapsulating in to be packaged upper, first 120 ℃ of heating 1 hour, then heat 4 hours at 150 ℃.
Comparative example 1
The preparation of A component: take methyl phenyl vinyl polysiloxane 55g, methyl phenyl vinyl polysiloxane 41.8g, caking agent 3g(structural formula), catalyst platinum-methyl phenyl silicone title complex 0.2g, platinum content 7000ppm, add successively in stirrer, mixing and stirring, obtains described A component;
The preparation of B component: take methyl phenyl vinyl polysiloxane 19.8g, linking agent aminomethyl phenyl hydrogen containing siloxane 80g, inhibitor 1,1,3-triphenyl-2-propine-1-alcohol 0.2g, adds in stirrer successively, and mixing and stirring, obtains described B component;
During use, by described A component, B component by weight for the proportioning of 1:1 mixes, vacuum defoamation 20 minutes, some glue or encapsulating in to be packaged upper, first 120 ℃ of heating 1 hour, then heat 4 hours at 150 ℃.
Comparative example 2
The preparation of A component: take methyl phenyl vinyl polysiloxane 55g, methyl phenyl vinyl polysiloxane 44.8g, catalyst platinum-methyl phenyl silicone title complex 0.2g, platinum content 7000ppm, add successively in stirrer, mixing and stirring, obtains described A component;
The preparation of B component: take methyl phenyl vinyl polysiloxane 19.8g, linking agent aminomethyl phenyl hydrogen containing siloxane 80g, inhibitor 1,1,3-triphenyl-2-propine-1-alcohol 0.2g, adds in stirrer successively, and mixing and stirring, obtains described B component;
During use, by described A component, B component by weight for the proportioning of 1:1 mixes, vacuum defoamation 20 minutes, some glue or encapsulating in to be packaged upper, first 120 ℃ of heating 1 hour, then heat 4 hours at 150 ℃.
Embodiment 1,2,3 and comparative example's 1,2 A, B component are weighed by weight the ratio of 1:1, then mix, deaeration 30 minutes, the one: according to GB/T7124-2008 tackiness agent tensile shear strength, require to make the test piece of 45# steel; The 2nd: according to GB/T528-2009, require to make sheet material, by mixture levelling in mould.Condition of cure: first 120 ℃ of heating 1 hour, then 150 ℃ of heating 4 hours.Test one: require to make dumbbell shaped silica gel exemplar according to GB/T528-2009, use puller system test tensile strength; Test two: the shearing resistance of making test piece with puller system test, testing method is according to GB/T7124-2008.
Table 1 performance index table
Figure GDA0000452817720000061
By table 1, can find out, embodiment 1,2,3 and comparative example 1 relatively can find out, aminomethyl phenyl Silicon Containing Hydrogen resin for linking agent, than obviously improving by the intensity of aminomethyl phenyl hydrogen containing siloxane; Embodiment 1,2,3 and comparative example 2 relatively can find out, adding of caking agent improved shearing resistance, namely improved the sticking power to base material.
The foregoing is only preferred embodiment of the present invention, in order to limit the present invention, within the spirit and principles in the present invention not all, any modification of doing, be equal to replacement, improvement etc., within all should being included in protection scope of the present invention.

Claims (7)

1. a LED packaging silicon rubber for high refractive index, is characterized in that, comprises component A and B component, and the weight ratio of described component A and B component is 1:1;
Wherein, described component A comprises the raw material of following weight part: 50~60 parts of methyl phenyl vinyl polysiloxanes, 35~45 parts of methyl phenyl vinyl polysiloxane, 0.1~0.3 part of platinum group catalyst, 1~5 part of caking agent; Described B component comprises the raw material of following weight part: 50~70 parts of linking agent aminomethyl phenyl Silicon Containing Hydrogen resins, and 30~50 parts of methyl phenyl vinyl polysiloxanes, 0.1~0.3 part, inhibitor,
Described caking agent contains phenyl, epoxy and acryloxy functional group, and its structural formula is:
Figure FDA0000456153740000011
Wherein, described n 1scope is 10~20, n 2scope is 10~20, n 3scope be 20~40.
2. the LED packaging silicon rubber of high refractive index according to claim 1, is characterized in that, described methyl phenyl vinyl polysiloxane molecular formula is: (ViMe 2siO 1/2) 3(PhSiO 3/2) 7, wherein, described Me is methyl, and Vi is vinyl, and Ph is phenyl.
3. the LED packaging silicon rubber of high refractive index according to claim 1, is characterized in that: described platinum group catalyst is any one in platinum-methyl phenyl silicone title complex or platinum-olefin(e)complex.
4. the LED packaging silicon rubber of high refractive index according to claim 3, is characterized in that: described platinum group catalyst is platinum-methyl phenyl silicone title complex, and wherein, platinum content is 3000~7000ppm.
5. the LED packaging silicon rubber of high refractive index according to claim 1, is characterized in that: described linking agent is hydrogeneous silicone resin, and wherein, the molecular formula of described Silicon Containing Hydrogen resin is: (HMe 2siO 1/2) 3(PhSiO 3/2) 7, described Me is methyl, Ph is phenyl.
6. the LED packaging silicon rubber of high refractive index according to claim 1, is characterized in that, described inhibitor is any one in ethynylcyclohexanol or 1,1,3-triphenyl-2-propine-1-alcohol.
7. the LED packaging silicon rubber of high refractive index according to claim 6, is characterized in that, described inhibitor is 1,1,3-triphenyl-2-propine-1-alcohol, and its structural formula is as follows:
Figure FDA0000456153740000021
CN201210508506.4A 2012-12-03 2012-12-03 High-refractivity LED (Light-Emitting Diode) package silica gel Expired - Fee Related CN103013431B (en)

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