CN103183963B - Organic silicon resin packaging material for LED - Google Patents
Organic silicon resin packaging material for LED Download PDFInfo
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- CN103183963B CN103183963B CN201310114668.4A CN201310114668A CN103183963B CN 103183963 B CN103183963 B CN 103183963B CN 201310114668 A CN201310114668 A CN 201310114668A CN 103183963 B CN103183963 B CN 103183963B
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Abstract
The invention relates to an organic silicon resin packaging material for an LED, which comprises 1) silicon resin A at least consisting of alkenyl, phenyl or hydroxyl directly connected with silicon per molecule, 2) silicon resin B which is a product obtained by further condensation of the silicon resin A under base catalysis, 3) polysiloxane C at least consisting of hydrogen or phenyl directly connected with silicon per molecule, 4) platinum catalyst D, and 5) inhibitor E. According to the organic silicon resin packaging material for the LED, the silicon resin A and the silicon resin B with similar structure and different viscosity are adopted to mix with hydrogen containing polysiloxane C to prepare the LED materials with different viscosities; and condensate has good structure homogeneity, small stress and excellent mechanical property.
Description
Technical field
The present invention relates to a kind of organic silicon resin encapsulant, be particularly useful for power LED package.
Background technology
Semiconductor light-emitting-diode (LED) illumination is considered to one of 21 century high-tech sector most with prospects, and it is while initiation illumination revolution, also will for promotion energy-saving and emission-reduction, set up conservation-minded society and make major contribution.
Tradition low-power LED generally adopts epoxy resin as encapsulating compound, but this kind of material weathering resistance is poor, and under high temperature and uv-radiation, easy xanthochromia, affects life-time service reliability.Along with the increase of luminous power, the temperature contrast aggravation of environment for use, proposes higher adaptability to LED encapsulation material and requires and choice criteria.
Organosilicon material, due to himself molecular structure feature, has excellent weathering resistance and cold-hot impact characteristics, becomes the first-selected packaged material of power led device at present gradually.Silicone resin containing phenyl not only has high refractive index, the light extraction efficiency of LED can be significantly improved, and the introducing of phenyl ring can reduce the ventilation property of encapsulating compound, effectively improve the sulfuration degree of protection of LED, thus become the Research Emphasis of relevant enterprise both at home and abroad instantly.
LED organic silicon resin encapsulant is made up of vinyl polysiloxane and hydrogen containing siloxane usually, under certain baking condition, carry out crosslinking curing through addition reaction.For regulating the characteristics such as glue viscosity, cured article hardness, usually also need to add other components such as vinyl silicone oil.When multiple vinyl component and when depositing, due to the difference of molecular structure, contents of ethylene and distribution, often there is larger difference in its reactive behavior, cause cured article structural homogeneity poor, solidification internal stress and fragility are greatly, easy to crack under thermal shock, affect the life-time service reliability of LED.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, provide a kind of LED organic silicon resin encapsulant, the viscosity of this encapsulating compound can flexible modulation, and after solidification, structural homogeneity is good, stress is little, excellent in mechanical performance.
For achieving the above object, the present invention is by the following technical solutions:
LED organic silicon resin encapsulant of the present invention, comprises following component:
(1) 10 ~ 90 weight part silicone resin A, per molecule at least contains the alkenyl, phenyl and the hydroxyl that are directly connected with silicon, and its structural formula is as follows:
R
1 aR
2 b(OH)
cSiO
(4-a-b-c)/2
Wherein R
1the alkenyl with 2 ~ 10 carbon atoms, R
2substituted or unsubstituted univalence hydrocarbyl and alkoxyl group, wherein at least 30mol% R
2for phenyl, a is 0.05 ~ 0.2, b be 0.8 ~ 2, c be 0.05 ~ 0.5, a+b+c is 1 ~ 2.5;
(2) 10 ~ 90 weight part silicone resin B, it be silicone resin A under alkali or its aqueous solution catalysis, the product that condensation reaction obtains occurs further, and per molecule is at least containing the alkenyl be directly connected with silicon and phenyl, and its structural formula is as follows:
R
1 aR
3 d(OH)
eSiO
(4-a-d-e)/2
Wherein R
1the alkenyl with 2 ~ 10 carbon atoms, R
3substituted or unsubstituted univalence hydrocarbyl and alkoxyl group, wherein at least 30mol% R
3for phenyl, a is 0.05 ~ 0.2, d be 0.8 ~ 2.2, e be 0 ~ 0.3, a+d+e is 1 ~ 2.5;
(3) 5 ~ 50 weight part polysiloxane C, per molecule at least contains the hydrogen and phenyl that are directly connected with silicon, and its structural formula is as follows:
H
fR
4 gSiO
(4-f-g)/2
Wherein R
4substituted or unsubstituted univalence hydrocarbyl, wherein at least 10mol% R
4for phenyl, f is 0.2 ~ 0.8, g is 0.5 ~ 2;
(4) 0.01 ~ 0.5 weight part platinum catalyst D;
(5) 0.01 ~ 0.5 weight part inhibitor E.
In order to improve the sticking power of encapsulating compound and support, can add tackifier in encapsulating compound, the weight of tackifier is 0.1 ~ 5% of encapsulating compound gross weight.
Organic silicon resin encapsulant of the present invention, wherein silicone resin A and silicone resin B are host, and polysiloxane C is solidifying agent, and platinum catalyst D is used for promoting host and solidifying agent reaction, and inhibitor E is used for extending operable time when encapsulating compound uses.
Silicone resin B in the present invention is that silicone resin A is under the alkali such as sodium hydroxide, potassium hydroxide, sodium bicarbonate, sodium carbonate, salt of wormwood or its aqueous solution catalysis, the product that further generation condensation reaction obtains, thus there is similar structure composition, but there is relatively low hydroxy radical content, relatively high viscosity.Under room temperature (25 ° of C), silicone resin A is the liquid of viscosity 1000mPas ~ 100Pas, silicone resin B be viscosity be greater than 2000 mPas liquid or for solid.The temperature of described condensation reaction is 30 ~ 90 ° of C, and be preferably 40 ~ 80 ° of C, the reaction times is 0.1 ~ 100h, is preferably 0.5 ~ 10h.
In the present invention, described platinum catalyst is the complex compound that platinum and vinyl gather silica thing, and wherein the content of platinum is 500 ~ 10000ppm.
In the present invention, described inhibitor is one or more in alkynol compound and many vinyl polysiloxane, wherein the carbon atom of alkynol compound is less than 15, as ethynylcyclohexanol, 3-Phenyl-1-butyn-3-ol, 3-methyl isophthalic acid-butine-3-alcohol, methylpentynol, 3,5-dimethyl-1-hexin-3-alcohol.
The preparation method of LED organic silicon resin encapsulant of the present invention: get each component by weight, be uniformly mixed, namely obtains described LED organic silicon resin encapsulant.
The preparation method of silicone resin A: add in reaction unit by methylsiloxane, methyl vinyl silicone, phenyl siloxane, four-functional group organosilane monomer, end-capping reagent, catalyzer, drip water while stirring, is added dropwise to complete post-heating reaction 2 ~ 20h.Cooling, add toluene and water, separatory, organic layers with water is washed till neutrality, and under 150 ° of C, vacuum sloughs low-boiling-point substance, obtains water white transparency product.
In preparation method, methylsiloxane is methyltrimethoxy silane, Union carbide A-162, dimethyldimethoxysil,ne, dimethyldiethoxysilane, octamethylcyclotetrasiloxane etc.
Methyl vinyl silicone is methylvinyldimethoxysilane, methyl vinyl diethoxysilane, t etram-ethyltetravinylcyclotetrasiloxane etc.
Phenyl siloxane is phenyltrimethoxysila,e, phenyl triethoxysilane, aminomethyl phenyl dimethoxysilane, aminomethyl phenyl diethoxy silane, dimethoxydiphenylsilane, diphenyl diethoxy silane etc.
Four-functional group organosilane monomer is tetraethoxy, water glass, tetramethoxy-silicane etc.
End-capping reagent is divinyl tetramethyl disiloxane, hexamethyldisiloxane etc.Catalyzer is hydrochloric acid, sulfuric acid, trifluoromethayl sulfonic acid etc.
The preparation method of silicone resin B: silicone resin A, after washing, adds alkali or its aqueous solution, is heated to 30 ~ 90 ° of C, reaction 0.1 ~ 100h, cooling, separatory, is washed to neutrality, and under 150 ° of C, vacuum sloughs low-boiling-point substance, obtains water white transparency product.Described alkali is sodium hydroxide, potassium hydroxide, sodium bicarbonate, sodium carbonate or salt of wormwood.
The use of LED organic silicon resin encapsulant of the present invention: generally solidify under heating, Heating temperature is 50 ~ 180 ° of C, is preferably 70 ~ 160 ° of C, and heat-up time is 0.5 ~ 10h, and be preferably 1 ~ 4h, also sectional is cured.
Compared with prior art, the invention has the beneficial effects as follows:
The viscosity of described encapsulating compound can flexible modulation, meet various processing request, cured article structural homogeneity be good, toughness and cold-hot impact property excellent.
Embodiment
Below by way of example, the present invention is further described.
Synthetic example 1
By 52g phenyltrimethoxysila,e, 42g aminomethyl phenyl diethoxy silane, 10g methyltrimethoxy silane, 7g tetraethoxy, 9g divinyl tetramethyl disiloxane, the 1g vitriol oil adds in there-necked flask, stirs lower dropping 50g water.Reactant is warming up to 60 ° of C and reacts 5h.Cooling, add toluene and water, separatory, organic layers with water is washed till neutrality, and under 150 ° of C, vacuum sloughs low-boiling-point substance, obtains water white Vinylphenyl silicon resin A, viscosity 6200 mPas.
Synthetic example 2
Synthetic method is with embodiment 1, and product is after washing, and add 50g 5% sodium bicarbonate aqueous solution, reflux 1h under 75 ° of C, cooling, separatory, is washed to neutrality, under 150 ° of C, vacuum sloughs low-boiling-point substance, obtains water white Vinylphenyl silicon resin B1, viscosity 13000 mPas.
Synthetic example 3
Synthetic method is with embodiment 1, and product is after washing, and add 0.1g potassium hydroxide, reflux 1h under 60 ° of C, and cooling, separatory, is washed to neutrality, and under 150 ° of C, vacuum sloughs low-boiling-point substance, obtains water white Vinylphenyl silicon resin B2, viscosity 46000 mPas.
Synthetic example 4
Synthetic method is with embodiment 1, and product is after washing, and add 0.1g potassium hydroxide, reflux 5h under 75 ° of C, cooling, and separatory, is washed to neutrality, and under 150 ° of C, vacuum sloughs low-boiling-point substance, obtains water white Vinylphenyl silicon resin B3, is solid after cooling.
Embodiment 5
Get above-mentioned silicone resin A 20 g, silicone resin B1 70g, viscosity is poly-methyl hydrogen phenyl siloxane 16 g of 100 mPas, catalyzer 0.18 g of platiniferous 3000ppm, ethynylcyclohexanol 0.1g, tackifier 1g, be uniformly mixed, obtain the organic silicon resin encapsulant that viscosity is 5200 mPas.This encapsulating compound toasts through 150 ° of C 3h, becomes the cured article that hardness is D30, tensile strength 4.5MPa, elongation 70%.
Embodiment 6
Get above-mentioned silicone resin A 50g, silicone resin B2 30g, viscosity is the poly-methyl hydrogen phenyl siloxane 20g of 45 mPas, the catalyzer 0.3g of platiniferous 3000ppm, 3-Phenyl-1-butyn-3-ol 0.2g, is uniformly mixed, and obtains the organic silicon resin encapsulant that viscosity is 3500 mPas.This encapsulating compound is through 80 ° of C 1h, and 150 ° of C 3h toast, and become the cured article that hardness is D42, tensile strength 6.5MPa, elongation 62%.
Embodiment 7
Get above-mentioned silicone resin A 60g, silicone resin B3 20g, viscosity is the poly-methyl hydrogen phenyl siloxane 20g of 45 mPas, catalyzer 0.25 g of platiniferous 3000ppm, ethynylcyclohexanol 0.15g, tackifier 1g, be uniformly mixed, obtain the organic silicon resin encapsulant that viscosity is 4000 mPas.This encapsulating compound is through 80 ° of C 1h, and 150 ° of C 2h toast, and become the cured article that hardness is D35, tensile strength 6.2MPa, elongation 76%.
Organic silicon resin encapsulant of the present invention, viscosity can flexible, and after solidification, structure is homogeneous, and good toughness, is conducive to protecting luminescence chip better.
What more than enumerate is only specific embodiments of the invention.Obviously, the invention is not restricted to above examples of implementation, in the protection domain of spirit of the present invention and claim, any amendment make the present invention and change, all should think protection scope of the present invention.
Claims (7)
1. a LED organic silicon resin encapsulant, is characterized in that described encapsulating compound comprises following component:
(1) 10 ~ 90 weight part silicone resin A, per molecule at least contains the alkenyl, phenyl and the hydroxyl that are directly connected with silicon, and its structural formula is as follows:
R
1 aR
2 b(OH)
cSiO
(4-a-b-c)/2
Wherein R
1the alkenyl with 2 ~ 10 carbon atoms, R
2substituted or unsubstituted univalence hydrocarbyl and alkoxyl group, wherein at least 30mol% R
2for phenyl, a is 0.05 ~ 0.2, b be 0.8 ~ 2, c be 0.05 ~ 0.5, a+b+c is 1 ~ 2.5;
(2) 10 ~ 90 weight part silicone resin B, it be silicone resin A under alkali or its aqueous solution catalysis, the product that condensation reaction obtains occurs further, and per molecule is at least containing the alkenyl be directly connected with silicon and phenyl, and its structural formula is as follows:
R
1 aR
3 d(OH)
eSiO
(4-a-d-e)/2
Wherein R
1the alkenyl with 2 ~ 10 carbon atoms, R
3substituted or unsubstituted univalence hydrocarbyl and alkoxyl group, wherein at least 30mol% R
3for phenyl, a is 0.05 ~ 0.2, d be 0.8 ~ 2.2, e be 0 ~ 0.3, a+d+e is 1 ~ 2.5;
(3) 5 ~ 50 weight part polysiloxane C, per molecule at least contains the hydrogen and phenyl that are directly connected with silicon, and its structural formula is as follows:
H
fR
4 gSiO
(4-f-g)/2
Wherein R
4substituted or unsubstituted univalence hydrocarbyl, wherein at least 10mol% R
4for phenyl, f is 0.2 ~ 0.8, g is 0.5 ~ 2;
(4) 0.01 ~ 0.5 weight part platinum catalyst D;
(5) 0.01 ~ 0.5 weight part inhibitor E.
2. LED organic silicon resin encapsulant according to claim 1, is characterized in that: encapsulating compound also comprises tackifier, and the weight of tackifier is 0.1 ~ 5% of encapsulating compound gross weight.
3. LED organic silicon resin encapsulant according to claim 1, it is characterized in that: described silicone resin B is that silicone resin A is under alkali or its aqueous solution catalysis, the product that further generation condensation reaction obtains, alkali used is sodium hydroxide, potassium hydroxide, sodium carbonate, sodium bicarbonate or salt of wormwood, temperature of reaction is 30 ~ 90 ° of C, and the reaction times is 0.1 ~ 100h.
4. LED organic silicon resin encapsulant according to claim 1, is characterized in that: under 25 ° of C, and silicone resin A is the liquid of viscosity 1000mPas ~ 100Pas, silicone resin B be viscosity be greater than 2000mPas liquid or for solid.
5. LED organic silicon resin encapsulant according to claim 1, is characterized in that: described platinum catalyst is the complex compound that platinum and vinyl gather silica thing, and wherein the content of platinum is 500 ~ 10000ppm.
6. LED organic silicon resin encapsulant according to claim 1, is characterized in that: described inhibitor is one or more in alkynol compound and many vinyl polysiloxane.
7. LED organic silicon resin encapsulant according to claim 6, is characterized in that: the carbon atom of described alkynol compound is less than 15.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310114668.4A CN103183963B (en) | 2013-04-03 | 2013-04-03 | Organic silicon resin packaging material for LED |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310114668.4A CN103183963B (en) | 2013-04-03 | 2013-04-03 | Organic silicon resin packaging material for LED |
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| CN103183963A CN103183963A (en) | 2013-07-03 |
| CN103183963B true CN103183963B (en) | 2015-03-18 |
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| CN110317343B (en) * | 2019-07-04 | 2021-10-22 | 中蓝晨光化工有限公司 | Single-component room-temperature curing organic silicon resin containing MQ structural unit and preparation method thereof |
| CN112341821B (en) * | 2019-08-06 | 2022-06-14 | 北京科化新材料科技有限公司 | Solid silicon resin compound and preparation method and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101665572A (en) * | 2009-08-24 | 2010-03-10 | 常州市源恩合成材料有限公司 | Organic silicon resin for encapsulating LED and preparation method thereof |
| CN102863799A (en) * | 2012-10-17 | 2013-01-09 | 东莞市贝特利新材料有限公司 | High-refractive-index organosilicon material for light-emitting diode (LED) packaging and preparation method of high-refractive-index organosilicon material |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101665572A (en) * | 2009-08-24 | 2010-03-10 | 常州市源恩合成材料有限公司 | Organic silicon resin for encapsulating LED and preparation method thereof |
| CN102863799A (en) * | 2012-10-17 | 2013-01-09 | 东莞市贝特利新材料有限公司 | High-refractive-index organosilicon material for light-emitting diode (LED) packaging and preparation method of high-refractive-index organosilicon material |
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Address after: Hangzhou City, Zhejiang province 311122 Yuhang District Xianlin Street Xian Xing Lu 31, No. 33 Applicant after: Hangzhou Hangke Photoelectric Co., Ltd. Address before: Hangzhou City, Zhejiang province 310011 Dengyun Road No. 425 Lilda Building 5 floor Applicant before: Hangzhou Hangke Photoelectric Co., Ltd. |
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Address after: Hangzhou City, Zhejiang province 311122 Yuhang District Xianlin Street Xian Xing Lu 31, No. 33 Patentee after: Hangzhou Hangzhou Ke optoelectronic group Limited by Share Ltd Address before: Hangzhou City, Zhejiang province 311122 Yuhang District Xianlin Street Xian Xing Lu 31, No. 33 Patentee before: Hangzhou Hangke Photoelectric Co., Ltd. |