CN103013433A - High-transparency, highly-refractive and self-bonding organic silicon material and preparation method thereof - Google Patents
High-transparency, highly-refractive and self-bonding organic silicon material and preparation method thereof Download PDFInfo
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- CN103013433A CN103013433A CN2012105773505A CN201210577350A CN103013433A CN 103013433 A CN103013433 A CN 103013433A CN 2012105773505 A CN2012105773505 A CN 2012105773505A CN 201210577350 A CN201210577350 A CN 201210577350A CN 103013433 A CN103013433 A CN 103013433A
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Abstract
The invention provides a high-transparency, highly-refractive and self-bonding organic silicon material for LED (Light-Emitting Diode) encapsulation and a preparation method thereof, in particular relates to a preparation method of the high-transparency, highly-refractive and self-bonding organic silicon material for LED encapsulation. The high-transparency, highly-refractive and self-bonding organic silicon material comprises the following mixed components in parts by weight: 50-95 parts of ethenyl polysiloxane component A, 5-40 parts of hydrogen-containing polysiloxane component B, 0.001-1 part of platinum catalyst component C, 0.001-1 part of inhibitor component D, 0.1-10 parts of tackifier component E and 0.01-1 part of anti-sludging agent component F. The encapsulation material provided by the invention is of an AB glue double-component type, has good cohesive force with PPA (Phenyl-Propanolamine) and high transparency. The refractive index of the encapsulation material can reach 1.54, and the lighting effect of the encapsulation material is higher than that of the common encapsulation material by 30%. The encapsulation material has an anti-sludging action, so that the sediments of fluorescent powder in the curing process are effectively reduced, the encapsulated lamp beads have the advantages of consistent light color and few product regions.
Description
Technical field
The present invention relates to electronic chemical product and organosilicon macromolecule technical field, relate in particular to the preparation method of the organosilicon material of high transparent, the high refractive power of a kind of LED encapsulation, self-adhesive.
Background technology
LED has light efficiency height, characteristics that current consumption is little, and it is than incandescent light power saving 80%, than electricity-saving lamp power saving 50%.Along with LED to high-power, integrated development, its optical throughput and working temperature than common LED high a lot of doubly, traditional epoxy packages material can serious aging under short-wave radiation and heat effect, and the flavescence phenomenon occurs, and can't satisfy the encapsulation requirement of LED again.And organosilicon material is the desirable packaged material of LED owing to have the advantages such as cold-hot impact, UV resistant radiation, water white transparency.
Common are in the market machine silicium encapsulating material refractive index about 1.4, according to Theoretical Calculation, refractive index is 1.5 packaged material, its light efficiency than refractive index be 1.4 high by 20%.Because silica gel and timbering material PPA thermal expansivity have gap, this just requires silica gel and timbering material PPA to have good cohesive force, and at present domestic organosilicon encapsulating material and PPA cohesive force are bad, and dead lamp phenomenon appears in the lamp pearl of encapsulation easily after crossing Reflow Soldering.In order to improve cohesive force, some producers add conventional silane coupling agent, but so that the packaged material outward appearance to become white translucent, cause light efficiency to descend.In addition, because the specific gravity difference of fluorescent material and silica gel is large, in the silica gel solidification process, fluorescent material can precipitate, and it is large to cause the lamp pearl to send the aberration of light, and the subregion of lamp pearl product is many.
Summary of the invention
Technical problem to be solved by this invention provides organosilicon encapsulating material of a kind of high transparent, high refractive power, self-adhesive and preparation method thereof.This packaged material is AB glue two-component-type, when having with PPA bonds well power, has high-clarity; This packaged material refractive index can reach 1.54, and its light efficiency is higher by 30% than common packaged material; This packaged material has the antisolvent precipitation effect, effectively reduces the precipitation of fluorescent material in the solidification process, and packaged lamp pearly-lustre look consistent, and the product subregion is few.
Organosilicon material for packaging provided by the present invention comprises containing vinyl polysiloxane component A, hydrogen containing siloxane B component, platinum catalyst component C, inhibitor component D, tackifier component E, anti-sludging agent component F mixing.
Each amounts of components mass fraction is as follows:
Component A:50～95
B component: 5～40
Component C:0.001～1
Component D:0.001～1
Component E:0.1～10
Component F:0.01～1
Above umber summation is 100 parts.
Described component A be refractive index 1.40 ~ 1.58 contain the vinyl polysiloxane, structural formula is as follows:
（R
1R
2R
3SiO
1/2）
a（R
1R
2SiO）
b（R
1SiO
3/2）
c（SiO
2）
d
R wherein
1, R
2, R
3Can be methyl, phenyl or vinyl, wherein a, b, c, d represent respectively more than or equal to 0 and less than 1 number, a+b+c+d=1 and c+d〉0;
Described B component is the hydrogen containing siloxane of refractive index 1.40 ~ 1.58, and structural formula is as follows:
（R
4R
5R
6SiO
1/2）
m（R
4R
5SiO）
n（R
4SiO
3/2）
o（SiO
2）
p
Wherein R4, R5, R6 can be methyl, phenyl or hydrogen base, wherein m, n, o, p represent respectively more than or equal to 0 its less than 1 number, m+n+o+p=1;
Described component C is isopropyl alcohol solution of chloroplatinic acid or platinum and vinyl polysiloxane inner complex;
Described component D is alkynol and vinyl cyclotetrasiloxane mixture.
Described component E is the compound that contains active function groups X and two parts of poly-silica chain link Y, and active function groups X can be epoxy group(ing), alkoxyl group, acryloxy, amino and different eyeball perester radical, and poly-silica chain link Y can be-R
7SiO ,-R
7R
8SiO
1/2,-SiO
3/2, R wherein
7, R
8Be methyl, phenyl or hydrogen.
Described component F is the gas phase White Carbon black, and preferred specific surface is greater than 300m
2/ g.
Organosilicon material for packaging provided by the present invention is that two-pack (A glue, B glue) form mixes, the A adhesive capacity is 3000 ~ 10000mPa.s, comprise component A, component C, component E, component F, the B adhesive capacity is that 100 ~ 2000mPa.s comprises component A, B component, component D.The ratio of A glue and B glue is in 10:1 to 1:10 scope, and ratio commonly used is 1:1.
Excellent effect of the present invention:
LED organosilicon material for packaging transmittance of the present invention can reach 99%, refractive index reaches 1.41～1.54, has good cohesive force with timbering materials such as PPA, and has an antisolvent precipitation effect, effectively reduce the precipitation of fluorescent material in the solidification process, packaged lamp pearly-lustre look consistent, and the product subregion is few.
Describe the present invention in detail below in conjunction with specific embodiment
Embodiment
Embodiment 1
Be (ViPh with the 47.4g structural formula
2SiO
1/2)
0.2(MePhSiO)
0.45(SiO
2)
0.35, viscosity is 8000mPa.s, and refractive index is 1.53 contains in the vinyl polysiloxane, and the platinum and vinyl polysiloxane inner complex, the 2g structural formula that add 0.1gPt content and be 5000ppm are
Compound, 0.5g specific surface area be 300m
2The gas phase White Carbon black of/g, stirring obtains A glue, and viscosity is 7000mPa.s; With the 22.5g same structure contain the vinyl polysiloxane, with the 27g structural formula be (Ph
2HSiO
1/2)
0.1(MePhSiO)
0.4(MeHSiO)
0.4(SiO
2)
0.1, viscosity is 80mPa.s, the hydrogen containing siloxane of refractive index 1.51, and 0.5g methyl ethylene cyclotetrasiloxane, stirring obtains B glue, and viscosity is 1000mPa.s.It is 3500mPa.s that A glue and B glue are mixed viscosity according to 1:1, detects hardness ShoreA60, transmittance 98.5%, refractive index 1.52 through 100 ℃ 1 hour, 150 ℃ after solidifying in 2 hours.128 on encapsulation SMD5050 lamp pearl carries out the experiment of thermal shock and fixed temperature and humidity, the rate 0 of turning off the light.
Embodiment 2
Basically consistent with embodiment 1, difference is to be (ViPh with the 49.82g structural formula
2SiO
1/2)
0.2(MePhSiO)
0.2(PhSiO
3/2)
0.6, viscosity is 6000mPa.s, refractive index be 1.55 contain the vinyl polysiloxane, with the platinum of 0.02gPt content 10000ppm and vinyl polysiloxane inner complex, 0.1g structural formula
For compound, 0.06g specific surface area are 400m
2The gas-phase silica of/g, stirring obtains A glue, and viscosity is 5600mPa.s; With the 34.9g same structure contain vinyl machine polysiloxane, with the 15g structural formula be (Ph
2HSiO
1/2)
0.2(MeHSiO)
0.6(PhSiO
3/2)
0.2, viscosity is 500mPa.s, and refractive index is that 1.48 hydrogen containing siloxane, 0.1g ethynylcyclohexanol stir, and obtains B glue, and viscosity is 1500mPa.s.It is 3800mPa.s that A glue and B glue are mixed viscosity according to 1:2, and row's bubble detects hardness ShoreA50, transmittance 99%, refractive index 1.51 after solidifying in 2 hours by 100 ℃ 1 hour, 150 ℃.128 on encapsulation SMD5050 lamp pearl carries out the experiment of thermal shock and fixed temperature and humidity, the rate 0 of turning off the light.
Embodiment 3
Basically consistent with embodiment 1, difference is to be (ViPh with the 45.99g structural formula
2SiO
1/2)
0.3(MePhSiO)
0.2(PhSiO
3/2)
0.3(SiO2)
0..2, viscosity is 7000mPa.s, refractive index be 1.52 contain the vinyl polysiloxane, with 1gPt content be that platinum and the vinyl polysiloxane inner complex of 300ppm is as catalyzer, 3g structural formula
Compound, 0.01g specific surface area be 300m
2The gas phase White Carbon black of/g, stirring obtains A glue, and viscosity is 5000mPa.s; With the 7.8g same structure contain the vinyl polysiloxane and the 42g structural formula is (Ph
2HSiO
1/2)
0.2(MePhSiO)
0.2(MeHSiO)
0.2(PhSiO
3/2)
0.2(SiO
2)
0.2, viscosity is 850mPa.s, the hydrogen containing siloxane of refractive index 1.52, and 0.2g methyl ethylene cyclotetrasiloxane and ethynylcyclohexanol mixture stir, and obtain B glue, and viscosity is 1100mPa.s.It is 3000mPa.s that A glue and B glue are mixed viscosity according to 2:1, detects hardness ShoreD30, transmittance 98%, refractive index 1.52 through 100 ℃ 1 hour, 150 ℃ after solidifying in 2 hours.128 on encapsulation SMD5050 lamp pearl carries out the experiment of thermal shock and fixed temperature and humidity, the rate 0 of turning off the light.
Embodiment 4
Basically consistent with embodiment 1, difference is to be (ViMe with the 49.5g structural formula
2SiO
1/2)
0.2(Ph
2SiO)
0.2(Me
2SiO)
0.2(PhSiO
3/2)
0.4, viscosity is 3000mPa.s, refractive index be 1.50 contain the vinyl polysiloxane, with 0.2gPt content be that platinum and the vinyl polysiloxane inner complex of 2500ppm is as catalyzer, 0.001g structural formula
Compound, 0.001g specific surface area be 400m
2The gas phase White Carbon black of/g, stirring obtains A glue, and viscosity is 2800mPa.s; With the 40.5g same structure contain the vinyl polysiloxane, with the 9g structural formula be (Me
2HSiO
1/2)
0.2(MePhSiO)
0.4(MeHSiO)
0.4, viscosity is 60mPa.s, the hydrogen containing siloxane of refractive index 1.50, and 0.5g methyl ethylene cyclotetrasiloxane, stirring obtains B glue, and viscosity is 400mPa.s.It is 1500mPa.s that A glue and B glue are mixed viscosity according to 3:1, detects hardness ShoreA20, transmittance 99%, refractive index 1.50 through 100 ℃ 1 hour, 150 ℃ after solidifying in 2 hours.Fill 60 on 1W band lens high-power lamp pearl with this product, carry out the experiment of thermal shock and fixed temperature and humidity, the rate 0 of turning off the light.
Embodiment 5
Basically consistent with embodiment 1, difference is to be (ViPh with the 45.78g structural formula
2SiO
1/2)
0.1(MeViSiO)
0.2(PhSiO
3/2)
0.3(SiO
2)
0..4, viscosity is 10000mPa.s, refractive index be 1.53 contain the vinyl polysiloxane, with 0.2gPt content be that platinum and vinyl polysiloxane inner complex, the 4g structural formula of 1500ppm is
Compound, 0.02g specific surface area be 400m
2The gas phase White Carbon black of/g, stirring obtains A glue, and viscosity is 6200mPa.s; With the 19.5g same structure contain the vinyl polysiloxane and the 30g structural formula is (Ph
2HSiO
1/2)
0.1(MePhSiO)
0.1(MeHSiO)
0.2(PhSiO
3/2)
0.4(SiO
2)
0.2, viscosity is 1200mPa.s, the hydrogen containing siloxane of refractive index 1.52, and 0.5g methyl ethylene cyclotetrasiloxane and ethynylcyclohexanol mixture, stirring obtains B glue, and viscosity is 2200mPa.s.A glue and B glue are mixed according to 1:4, and viscosity is 4000mPa.s, detects hardness ShoreD60, transmittance 98%, refractive index 1.52 after 100 ℃ 1 hour, 150 ℃ curing in 2 hours.128 on encapsulation SMD5050 lamp pearl carries out the experiment of thermal shock and fixed temperature and humidity, the rate 0 of turning off the light.
Claims (7)
1. a LED encapsulates the organosilicon material of using high transparent, high refractive power, self-adhesive, it is characterized in that including following component, and each amounts of components mass fraction is as follows:
Component A:50～95
B component: 5～40
Component C:0.001～1
Component D:0.001～1
Component E:0.1～10
Component F:0.01～1
Described component A is for containing the vinyl polysiloxane, and structural formula is as follows:
（R
1R
2R
3SiO
1/2）
a（R
1R
2SiO）
b（R
1SiO
3/2）
c（SiO
2）
d
R wherein
1, R
2, R
3Can be methyl, phenyl or vinyl, wherein a, b, c, d represent respectively more than or equal to 0 its less than 1 number, a+b+c+d=1 and c+d 0;
Described B component is hydrogen containing siloxane, and structural formula is as follows:
（R
4R
5R
6SiO
1/2）
m（R
4R
5SiO）
n（R
4SiO
3/2）
o（SiO
2）
p
R wherein
4, R
5, R
6Can be methyl, phenyl or hydrogen base, wherein m, n, o, p represent respectively more than or equal to 0 its less than 1 number, m+n+o+p=1;
Described component C is isopropyl alcohol solution of chloroplatinic acid or platinum and vinyl polysiloxane inner complex;
Described component D is alkynol and vinyl cyclotetrasiloxane mixture;
Described component E is the compound that contains active function groups X and two parts of poly-silica chain link Y, and active function groups X can be epoxy group(ing), alkoxyl group, acryloxy, amino and different eyeball perester radical, and poly-silica chain link Y can be-R
7SiO ,-R
7R
8SiO
1/2,-SiO
3/2, R wherein
7, R
8Be methyl, phenyl or hydrogen;
Described component F is the gas phase White Carbon black, and preferred specific surface is greater than 300m
2/ g.
2. the preparation method of LED organosilicon material for packaging according to claim 1, the two-pack form that it is characterized by A glue, B glue is mixed, wherein, A glue comprises said components A, component C, component E, component F, and B glue comprises above-mentioned component A, B component, the component D of comprising; The ratio of A glue and B glue is in 10:1 to 1:10 scope.
3. the preparation method of LED organosilicon material for packaging according to claim 2, the ratio that it is characterized in that described A glue and B glue is 1:1.
4. according to claim 1 and 2 or 3 described LED organosilicon material for packagings, it is characterized by and have high refractive index, reach 1.41～1.54.
5. according to claim 1 and 2 or 3 described LED organosilicon material for packagings, it is characterized by and have high transmission rate, when thickness was 1mm, transmittance reached 99%.
6. according to claim 1 and 2 or 3 described LED organosilicon material for packagings, it is characterized by with timbering materials such as PPA and have good cohesive force.
7. according to claim 1 and 2 or 3 described LED organosilicon material for packagings, it is characterized by and have the antisolvent precipitation effect, can effectively reduce the precipitation of fluorescent material in the solidification process, packaged lamp pearly-lustre look consistent, and the product subregion is few.
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| CN201210577350.5A CN103013433B (en) | 2012-12-27 | 2012-12-27 | High-transparency, highly-refractive and self-bonding organic silicon material and preparation method thereof |
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Cited By (8)
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| CN103242801A (en) * | 2013-05-14 | 2013-08-14 | 汕头市骏码凯撒有限公司 | Single-component high-refractivity LED (light-emitting diode) packaging adhesive and preparation method thereof |
| CN103865476A (en) * | 2014-03-28 | 2014-06-18 | 烟台德邦先进硅材料有限公司 | Organic silicon solid insulated crystal for low-power light-emitting diode (LED) encapsulated by surface mount technology (SMT) |
| CN104531056A (en) * | 2015-01-22 | 2015-04-22 | 烟台德邦先进硅材料有限公司 | Organosilicone packaging glue for packaging LED lamp filament |
| CN105428506A (en) * | 2015-11-16 | 2016-03-23 | 江西华柏节能照明科技协同创新有限公司 | High-luminous-efficiency and high-color-rendering-index fluorescent powder silica gel formula |
| CN106675506A (en) * | 2016-11-13 | 2017-05-17 | 复旦大学 | Organic silicon adhesive and preparation method thereof |
| CN106711311A (en) * | 2017-01-05 | 2017-05-24 | 永林电子有限公司 | Method for reducing fluorescent powder sedimentation rate of surface mount device |
| CN108997968A (en) * | 2017-06-06 | 2018-12-14 | 上海铜镑光电科技有限公司 | A kind of LED uniform in light emission glue |
| WO2023136188A1 (en) * | 2022-01-12 | 2023-07-20 | 信越化学工業株式会社 | Thixotropic silicone gel composition for spot potting, cured product thereof, and photocoupler |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103242801A (en) * | 2013-05-14 | 2013-08-14 | 汕头市骏码凯撒有限公司 | Single-component high-refractivity LED (light-emitting diode) packaging adhesive and preparation method thereof |
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| CN108997968A (en) * | 2017-06-06 | 2018-12-14 | 上海铜镑光电科技有限公司 | A kind of LED uniform in light emission glue |
| WO2023136188A1 (en) * | 2022-01-12 | 2023-07-20 | 信越化学工業株式会社 | Thixotropic silicone gel composition for spot potting, cured product thereof, and photocoupler |
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Effective date of registration: 20220118 Address after: 510760, Guangzhou, Guangdong province Whampoa District Po Po Industrial Zone, East Road, Tat Tat Road, No. 8 Patentee after: GUANGZHOU TINCI MATERIALS TECHNOLOGY Co.,Ltd. Address before: 510760 No. 5, Xingcheng Road, YUNPU Industrial Zone, Huangpu District, Guangzhou, Guangdong Patentee before: GUANGZHOU TIANCI ORGANIC SILICON TECHNOLOGY CO.,LTD. |