CN105400487B - A kind of high brightness, high index of refraction LED packaging silicon rubbers and preparation method thereof - Google Patents
A kind of high brightness, high index of refraction LED packaging silicon rubbers and preparation method thereof Download PDFInfo
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- CN105400487B CN105400487B CN201510795643.4A CN201510795643A CN105400487B CN 105400487 B CN105400487 B CN 105400487B CN 201510795643 A CN201510795643 A CN 201510795643A CN 105400487 B CN105400487 B CN 105400487B
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Abstract
The invention belongs to encapsulating material fields, are related to a kind of high brightness, high index of refraction LED packaging silicon rubbers and preparation method thereof, by A, B component according to mass ratio 2:1 composition；Component A is made of following raw material by mass parts：Methyl phenyl vinyl polysiloxane 85 95, crosslinking agent 4.5 15, inhibitor 0.1~0.5, the B component are made of following raw material by mass parts：Vinyl silicone oil 75 85, methyl phenyl vinyl polysiloxane 10 20, chain extender 15, bonding agent 15, catalyst 0.1 0.5.The LED packaging silicon rubbers of the present invention have the characteristics that high brightness, high index of refraction, cementability are strong, weatherability is strong, and the light transmittance of silica gel is more than 99%, and preparation process is easy to operate, is easy to volume production, is suitable for LED packaging silicon rubbers.
Description
Technical field
The invention belongs to encapsulating material fields, are related to a kind of high brightness, high index of refraction LED packaging silicon rubbers and its preparation side
Method.
Background technology
LED packaging silicon rubbers are mainly used for light emitting diode（LED）Encapsulation, for protecting, sealed electronic element, may be used also
For electrical equipment embedding, the embedding of high voltage component, the moisture-proof coating of circuit board, electronics industry LED indoor outer display board, LED are handed over
Encapsulation, isolation protection of messenger etc. etc..The effect of packaging silicon rubber includes carrying out mechanical protection, stress release to chip, and makees
For a kind of guide structure, strengthen heat dissipation, to reduce junction temperature of chip, improve LED performances.
The silica gel of low-refraction is low due to refractive index（1.40）, with chip refractive index（2-4）Contrast causes greatly total reflection to be sent out
It is raw, light is made not export effectively；The photon loss that refractive index physical barriers are brought can effectively be reduced by improving silica gel refractive index, be carried
High external quantum efficiency, but silica gel performance is influenced by environmental temperature.As temperature raises, the thermal stress inside silica gel increases,
Cause the refractive index of silica gel to reduce, so as to influence LED light effect and light distribution.Therefore, the brightness for improving LED is a kind of comprehensive
The upgrading of energy is not limited only to improve refractive index.Silica gel with high brightness and high index of refraction can improve the luminous flux of LED, make
LED has preferable durability and reliability.
Although 102382618 A of patent CN improve a lot in the refractive index of packaging silicon rubber, LED luminance is a kind of
Comprehensive performance as a result, it there is no comprehensive consideration LED luminance situation.The present invention relates to a kind of high brightness, highs index of refraction to seal
Fill silica gel.
The content of the invention
It is an object of the invention to provide a kind of high brightness, the LED packaging silicon rubbers and preparation method thereof of high index of refraction.
To achieve the above object, the present invention uses following technical scheme：
A kind of high brightness, high index of refraction LED packaging silicon rubbers, it is characterised in that：By A, B component according to mass ratio 2:1 composition；
The component A is made of following raw material by mass parts：
Methyl phenyl vinyl polysiloxane 85-95
Crosslinking agent 4.5-15
Inhibitor 0.1~0.5
The B component is made of following raw material by mass parts：
Vinyl silicone oil 75-85
Methyl phenyl vinyl polysiloxane 10-20
Chain extender 1-5
Bonding agent 1-5
Catalyst 0.1-0.5
The beneficial effects of the invention are as follows：The present invention is made of A, B component, and two components are uniformly mixed according to a ratio during use, is led to
It crosses carry out hydrosilylation and completes solidification process.The LED packaging silicon rubbers of the present invention have high brightness, high index of refraction, cementability
By force, the characteristics of weatherability is strong, the light transmittance of silica gel is more than 99%, and preparation process is easy to operate, is easy to volume production, is suitable for LED encapsulation
Silica gel.
It is (ViMe that the methyl phenyl vinyl polysiloxane, which is selected from general formula,2SiO1/2 )3(PhSiO3/2)7Silicones,
Wherein Me is methyl, and Ph is phenyl, and Vi is vinyl.
The bonding agent is selected from the polymer containing epoxy and acryloxy functionality, and structural formula is（1）：
（1）
Wherein, Me is methyl, and Et is ethyl, n1For the integer of 10-20, n2For the integer of 10-20, n3For the whole of 20-40
Number.
The catalyst is platinum group catalyst, selected from chloroplatinic acid in alcohol, platinum-methyl phenyl silicone, platinum-alkene
Any one or more than one in complex.
The crosslinking agent is hydrogeneous silicones, and general formula is (HMe2SiO1/2)3(PhSiO3/2)5, Me is methyl, and Ph is
Phenyl.
The inhibitor is any one or one kind in ethynylcyclohexanol, 1,1,3- triphenyl -2- propine -1- alcohol
More than.
The chain extender is containing hydrogen silicone oil, and structural formula is（2）：
（2）
A kind of high brightness, high index of refraction LED packaging silicon rubbers preparation method, which is characterized in that preparation process is as follows：
The preparation process of the component A：By methyl phenyl vinyl polysiloxane of the mass parts for 85~95,4.5~15 matter
The crosslinking agent, the inhibitor of 0.1~0.5 mass parts of part are measured, is mixed evenly using machine, is filled with nitrogen, sealed storage, i.e.,
Obtain component A；
The preparation process of the B component：It is 75~85 parts of vinyl silicone oil by mass parts, the methyl of 10~20 mass parts
The catalysis of phenyl vinyl polysiloxane, the chain extender of 1~5 mass parts, the bonding agent of 1~5 mass parts, 0.1~0.5 mass parts
Agent is mixed evenly using machine, is filled with nitrogen protection, sealed storage is to get B component；
In use, by A, B component according to mass ratio 2:1 is uniformly mixed, 5~30min of vacuum defoamation, dispensing or encapsulating in
On part to be packaged, condition of cure：When+150 DEG C of curings 3 are small when 80 DEG C of curings 1 are small.
Specific embodiment
With reference to specific implementation case, the invention will be further described.
Embodiment 1
The preparation of component A：It is accurate weigh the hydrogeneous silicones of 85g methyl phenyl vinyl polysiloxanes, 14.9g crosslinking agents,
0.1g inhibitor ethynylcyclohexanols, are mixed evenly using machine to get component A；
The preparation of B component：Accurately 85g vinyl silicone oils, 10g methyl phenyl vinyl polysiloxanes, 2g chain extenders is weighed to contain
Hydrogen silicone oil（Structural formula 2）, 2.5g bonding agents（Structural formula 1）, 0.5g catalyst platinums-methyl phenyl silicone, drifted along or through using machine
Conjunction is stirred evenly to get B component；
In use, by A, B component according to mass ratio 2:1 is uniformly mixed, vacuum defoamation 5min, and dispensing or encapsulating are in waiting to seal
In piece installing, when+150 DEG C of curings 3 are small when 80 DEG C of curings 1 are small, you can.
The transmittance data of embodiment 1 is shown in Table 1.
Embodiment 2
The preparation of component A：It is accurate weigh the hydrogeneous silicones of 95g methyl phenyl vinyl polysiloxanes, 4.5g crosslinking agents,
1,1,3- triphenyl -2- propine -1- alcohol of 0.5g inhibitor, is mixed evenly using machine to get component A；
The preparation of B component：Accurately 75g vinyl silicone oils, 15g methyl phenyl vinyl polysiloxanes, 5g chain extenders is weighed to contain
Hydrogen silicone oil（Structural formula 2）, 4.7g bonding agents（Structural formula 1）, 0.3g catalyst platinums-olefin complex, utilize machine be mixed
Uniformly to get B component；
In use, by A, B component according to mass ratio 2:1 is uniformly mixed, vacuum defoamation 10min, and dispensing or encapsulating are in waiting to seal
In piece installing, when+150 DEG C of curings 3 are small when 80 DEG C of curings 1 are small, you can.
The transmittance data of embodiment 2 is shown in Table 1.
Embodiment 3
The preparation of component A：It is accurate weigh the hydrogeneous silicones of 90g methyl phenyl vinyl polysiloxanes, 9.8g crosslinking agents,
The mixture of 0.2g inhibitor ethynylcyclohexanol and 1,1,3- triphenyl -2- propine -1- alcohol（Mass ratio 1:1）, mixed using machine
It is mixed evenly to get component A；
The preparation of B component：Accurately 85g vinyl silicone oils, 10g methyl phenyl vinyl polysiloxanes, 2g chain extenders is weighed to contain
Hydrogen silicone oil（Structural formula 2）, 2.5g bonding agents（Structural formula 1）, 0.5g catalyst chloroplatinic acid in alcohol, be mixed using machine equal
It is even to get B component；
In use, by A, B component according to mass ratio 2:1 is uniformly mixed, vacuum defoamation 15min, and dispensing or encapsulating are in waiting to seal
In piece installing, when+150 DEG C of curings 3 are small when 80 DEG C of curings 1 are small, you can.
The transmittance data of embodiment 3 is shown in Table 1.
Embodiment 4
The preparation of component A：It is accurate weigh the hydrogeneous silicones of 92g methyl phenyl vinyl polysiloxanes, 7.6g crosslinking agents,
The mixture of 0.4g inhibitor ethynylcyclohexanol and 1,1,3- triphenyl -2- propine -1- alcohol（Mass ratio 2:1）, mixed using machine
It is mixed evenly to get component A；
The preparation of B component：Accurately 85g vinyl silicone oils, 10g methyl phenyl vinyl polysiloxanes, 2g chain extenders is weighed to contain
Hydrogen silicone oil（Structural formula 2）, 2.5g bonding agents（Structural formula 1）, 0.5g catalyst platinums-methyl phenyl silicone and platinum-alkene matches somebody with somebody
Polymer mixtures（Mass ratio is 1:1）, it is mixed evenly using machine to get B component；
In use, by A, B component according to mass ratio 2:1 is uniformly mixed, vacuum defoamation 25min, and dispensing or encapsulating are in waiting to seal
In piece installing, when+150 DEG C of curings 3 are small when 80 DEG C of curings 1 are small, you can.
The transmittance data of embodiment 4 is shown in Table 1.
Embodiment 5
The preparation of component A：It is accurate weigh the hydrogeneous silicones of 88g methyl phenyl vinyl polysiloxanes, 11.7g crosslinking agents,
0.3g inhibitor ethynylcyclohexanols, are mixed evenly using machine to get component A；
The preparation of B component：Accurately 85g vinyl silicone oils, 10g methyl phenyl vinyl polysiloxanes, 2g chain extenders is weighed to contain
Hydrogen silicone oil（Structural formula 2）, 2.5g bonding agents（Structural formula 1）, 0.5g catalyst platinums-methyl phenyl silicone and platinum-alkene matches somebody with somebody
Polymer mixtures（Mass ratio is 3:1）, it is mixed evenly using machine to get B component；
In use, by A, B component according to mass ratio 2:1 is uniformly mixed, vacuum defoamation 30min, and dispensing or encapsulating are in waiting to seal
In piece installing, when+150 DEG C of curings 3 are small when 80 DEG C of curings 1 are small, you can.
The transmittance data of embodiment 5 is shown in Table 1.
Light transmittance test, thickness of sample 3mm, test result are carried out to LED packaging silicon rubbers obtained in above-described embodiment 1-5
Such as table 1：
The test of 1 embodiment light transmittance of table
It is excellent to can be seen that the packaging silicon rubber light transmittance of the method for the present invention preparation from the test data in table 1,99%
More than.The present invention is to complete solidification process by carrying out hydrosilylation by A, B component.The LED packaging silicon rubbers of the present invention
Have the characteristics that high brightness, high index of refraction, cementability are strong, weatherability is strong, encapsulated suitable for LED.
It is understood that the above description of the embodiments is intended to facilitate those skilled in the art and using this hair
It is bright.Person skilled in the art obviously easily can make various modifications to these embodiments, and described herein
General Principle is applied in other embodiment without having to go through creative labor.Therefore, the invention is not restricted to implementations here
Example, those skilled in the art's announcement according to the present invention, improvement and modification made without departing from the scope of the present invention all should be
Within protection scope of the present invention.
Claims (7)
1. a kind of high brightness, high index of refraction LED packaging silicon rubbers, it is characterised in that：By A, B component according to mass ratio 2:1 composition；Institute
Component A is stated to be made of by mass parts following raw material：Methyl phenyl vinyl polysiloxane 85-95, crosslinking agent 4.5-15, inhibitor
0.1~0.5；The B component is made of following raw material by mass parts：Vinyl silicone oil 75-85, methyl phenyl vinyl polysiloxane
10-20, chain extender 1-5, bonding agent 1-5, catalyst 0.1-0.5；The wherein described bonding agent, which is selected from, contains epoxy and acryloyl
The polymer of oxy functional groups, structural formula are（1）；The chain extender is containing hydrogen silicone oil, and structural formula is（2）；Wherein, Me is first
Base, Et are ethyl, n1For the integer of 10-20, n2For the integer of 10-20, n3For the integer of 20-40,
（1）
（2）.
2. a kind of high brightness according to claim 1, high index of refraction LED packaging silicon rubbers, it is characterised in that：The methyl
It is (ViMe that phenyl vinyl polysiloxane, which is selected from general formula,2SiO1/2 )3(PhSiO3/2)7Silicones, wherein Me be methyl, Ph is benzene
Base, Vi are vinyl.
3. a kind of high brightness according to claim 1, high index of refraction LED packaging silicon rubbers, it is characterised in that：The catalysis
Agent is platinum group catalyst, any one in chloroplatinic acid in alcohol, platinum-methyl phenyl silicone, platinum-olefin complex
Or more than one.
4. a kind of high brightness according to claim 1, high index of refraction LED packaging silicon rubbers, it is characterised in that：The crosslinking
Agent is hydrogeneous silicones, and general formula is (HMe2SiO1/2)3(PhSiO3/2)5, Me is methyl, and Ph is phenyl.
5. a kind of high brightness according to claim 1, high index of refraction LED packaging silicon rubbers, it is characterised in that：The inhibition
Any one or more than one of the agent for ethynylcyclohexanol, in 1,1,3- triphenyl -2- propine -1- alcohol.
6. preparing a kind of any high brightness of claim 1-5, the method for high index of refraction LED packaging silicon rubbers, feature exists
In comprising the following steps：
The preparation of component A：By mass parts be 85~95 methyl phenyl vinyl polysiloxane, 4.5~15 mass parts crosslinking agent,
The inhibitor of 0.1~0.5 mass parts, is mixed evenly using machine, is filled with nitrogen, sealed storage is to get component A；
The preparation of B component：It is 75~85 parts of vinyl silicone oil by mass parts, the methyl phenyl vinyl silicon of 10~20 mass parts
Resin, the chain extender of 1~5 mass parts, the bonding agent of 1~5 mass parts, the catalyst of 0.1~0.5 mass parts, are drifted along or through using machine
Conjunction stirs evenly, and is filled with nitrogen protection, sealed storage is to get B component.
7. a kind of any high brightness of claim 1-5, the application method of high index of refraction LED packaging silicon rubbers, feature exist
In in use, by A, B component according to mass ratio 2:1 is uniformly mixed, and 5~30min of vacuum defoamation, dispensing or encapsulating are in be packaged
On part, condition of cure：When+150 DEG C of curings 3 are small when 80 DEG C of curings 1 are small.
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| CN106336849B (en) * | 2016-09-05 | 2019-09-17 | 烟台德邦科技有限公司 | A kind of high folding LED packaging silicon rubber of high temperature resistant low light attenuation |
| CN106433546A (en) * | 2016-09-13 | 2017-02-22 | 烟台德邦科技有限公司 | Solvent-free unfoamed polyurethane structured adhesive and preparation method thereof |
| CN108285644B (en) * | 2017-01-09 | 2021-03-16 | 青岛科技大学 | LED packaging liquid silicone rubber composition and preparation method thereof |
| CN107674635A (en) * | 2017-09-19 | 2018-02-09 | 合肥惠科金扬科技有限公司 | A kind of AMOLED of resistance to vulcanization packaging silicon rubbers of high temperature resistant high tenacity |
| CN109251723A (en) * | 2018-08-24 | 2019-01-22 | 烟台德邦先进硅材料有限公司 | A kind of Molding high folding LED packaging silicon rubber |
| CN109054732B (en) * | 2018-09-18 | 2021-02-09 | 烟台德邦科技股份有限公司 | LED packaging silica gel with excellent bonding performance and preparation method thereof |
| CN113563851A (en) * | 2021-07-20 | 2021-10-29 | 深圳先进电子材料国际创新研究院 | In-situ modified low-viscosity high-performance heat-conducting gel and preparation method and application thereof |
| CN115895274A (en) * | 2022-11-24 | 2023-04-04 | 惠州市众恺新材料有限公司 | High-reflection organic silicon composite material composition and preparation method thereof |
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| CN103013431A (en) * | 2012-12-03 | 2013-04-03 | 烟台德邦先进硅材料有限公司 | High-refractivity LED (Light-Emitting Diode) package silica gel |
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| CN103013431A (en) * | 2012-12-03 | 2013-04-03 | 烟台德邦先进硅材料有限公司 | High-refractivity LED (Light-Emitting Diode) package silica gel |
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Effective date of registration: 20190415 Address after: 264006 Kaifeng Road 3-3 Renewable Resource Processing Demonstration Zone, Yantai Development Zone, Shandong Province Patentee after: Yantai Darbond Technology Co., Ltd. Address before: 264006 No. 98 Jinshajiang Road, Yantai Development Zone, Shandong Province Patentee before: Yantai Debang Advanced Silicon Materials Co.,Ltd. |
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