CN104073215A - Preparation method for nano silicon dioxide modified organic silicon sealant for packaging of light emitting diode (LED) - Google Patents
Preparation method for nano silicon dioxide modified organic silicon sealant for packaging of light emitting diode (LED) Download PDFInfo
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Abstract
The invention relates to a preparation method for a nano silicon dioxide modified organic silicon sealant for packaging of a light emitting diode (LED). As silane coupling agent modified nano silicon dioxide is added into chlorosilane hydrolysis and polycondensation system, the compatibility of the nano silicon dioxide and organic silicon resin is sharply improved; a small quantity of curing agent, catalyst and defoaming agent are added, the mixture is mixed uniformly and then is cured at room temperature so as to prepare the nano silicon dioxide modified organic silicon sealant. The preparation method is simple, has low cost, and can prepare a series of high refractive index and high transmittance packaging sealants for multiple LED electron components, and the operation conditions are easy to control.
Description
Technical field
The present invention relates to a kind of preparation method of organosilicon sealant, refer in particular to the preparation method of the nano-silicon dioxide modified organosilicon sealant of a kind of LED encapsulation.
Background technology
Power type light-emitting diode (Light Emitting Diode, LED), through the development of decades, be widely used in big area picture and text and show the aspects such as full-color screen, state instruction, mark illumination, signal show, backlight, Combined tail lamps of automobile and the room light of liquid-crystal display.LED has energy-saving and environmental protection, safety, life-span length, low consumption, low-heat, shockproof, waterproof, miniature, high brightness, easily light modulation, light beam is concentrated and reduces the advantages such as maintenance, be expected to become after incandescent light, luminescent lamp, high-intensity gas discharge lamp the 4th generation light source.
In general, the packaged material of LED has several as follows: epoxy resin, silica gel, silicone resin.But in conjunction with three kinds of LED packaged materials of existing market main flow, although epoxy resin encapsulating material has advantage on light transmission and cost, slightly inadequate at brightness decay, anti-UV, the aspect such as heat-resisting.Silicone resin is eager to excel at the Performance Ratio epoxy resin of the aspects such as heat-resisting, anti-UV and brightness decay, and and epoxy resin is in conjunction with obtaining better without interface problem, relatively be suitable for use in the encapsulation of white light and some low decay requirements (as display screen, wiring board, terminal box etc.), price is comparatively expensive.Silica gel relatively the above two, in anti-UV, heat-resisting and brightness decay, have larger advantage, be particularly suitable for being used on the low decay of heavy-power LED product and part and white light product, but it is poor that shortcoming is bonding force, easily produce interface problem with epoxy combination, easily moisture absorption, dirt resistance is poor.
Under hot environment, packaged material may cause carbonization, forms brown tectum at device surface, causes component failure.This research is compound to polymkeric substance and inorganic nano-particle, can make matrix material both have easy processing and the shock resistance of polymkeric substance, has again the characteristic such as high heat conduction and rub resistance of inorganic materials.Be a kind of not only practical but also easy method to adding heat-resisting additive in polysiloxane product, nano silicon is the most general a kind of filler of application in colourless Organosilicon Polymers system.
Summary of the invention
The technical problem to be solved in the present invention is: in order to overcome the problems of the prior art, the present invention adopts nano silicon to make filler, organic silica gel is played to thickening, thixotroping, reinforcement, increase physical strength, reached high gloss, high transparent, high-ductility moulding texts simultaneously.This sizing agent has excellent high-low temperature resistant, ageing-resistant, transparency is high, good moldability, the advantages such as condition of cure gentleness.
The technical solution adopted for the present invention to solve the technical problems is: 1. a LED encapsulates the preparation method with nano-silicon dioxide modified organosilicon sealant, and the concrete steps of the method are as follows:
1) nano-silicon dioxide modified processing: by a certain amount of silicon-dioxide and silane coupling agent 100:(0.01-1.00 in mass ratio) be dissolved in appropriate organic solvent, under constantly stirring at 110 DEG C of-150 DEG C of temperature reflux 3-8h, then cooling, and dry in baking oven, to vapor away remaining organic solvent; Organic solvent is benzene, toluene, any in dimethylbenzene;
2) preparation of modified organic silicon glue: the mixture of chlorosilane and improved silica is joined in the mixed solvent of toluene and water composition, DEG C Water Under solution 24h in temperature T=40, after reaction finishes, stratification is got supernatant liquid, with deionized water, supernatant liquid washing is extremely neutral, obtain hydrolysate silanol toluene solution;
3) add a certain amount of toluene solution dilution silanol toluene solution, add proper catalyst, back flow reaction 12h at temperature T=100 DEG C, be cooled to and add after room temperature 5% trimethylchlorosilane as end-capping reagent, to neutral, the product obtaining is concentrated to remove toluene and water with deionized water wash;
4) curing process of nano-silicon dioxide modified organic resin: add a certain amount of solidifying agent and catalyzer in nano-silicon dioxide modified silicone resin making, and a certain amount of defoamer, the amount of described catalyzer is benchmark by the quality of organic resin; After stirring, self-vulcanizing 6h, finally obtains the nano-silicon dioxide modified encapsulated with silicone resin glue solidifying.
As preferably, described silane coupling agent comprises γ aminopropyltriethoxy silane, gamma-amino propyl trimethoxy silicane, N-beta-aminoethyl-gamma-amino propyl group methyltrimethoxy silane, 2-ethyl trimethoxy silane, 3-ethyl trimethoxy silane, 4-ethyl trimethoxy silane, 2-epoxy cyclohexane base silane, 3-epoxy cyclohexane base silane, 4-epoxy cyclohexane base silane, γ-glycidyl ether oxygen base propyl group trimethoxy silane, γ propyltrimethoxy silane, γ-methacryloyl oxosilane, γ-propyl-triethoxysilicane, γ-methacryloyl oxosilane, γ-propyl group dimethoxy silane, the mixing of one or more coupling agents in γ-methacryloyl oxosilane.
As preferably, described chlorosilane is dichloromethyl phenylsilane, phenyl-trichloro-silicane, methyl ethylene dichlorosilane, dimethyldichlorosilane(DMCS).
As preferably, described catalyzer is sodium hydroxide, potassium hydroxide, sodium carbonate, Tetramethylammonium hydroxide, and mass concentration is 0.05%-0.2%.
As preferably, solidifying agent used is diethylenetriamine, triethylene tetramine, and mass concentration is 3%-5%.
As preferably, catalyzer used is the one in dibutyl tin laurate, two lauric acid two stannous octoates, two lauric acid two tin acetates, two neodecanoic acid tin methides, stannous octoate, and mass concentration is 0.1%-1%.
As preferably, defoamer used is polydimethylsiloxane, and mass concentration is 0.05%-1%.
The invention has the beneficial effects as follows: compared with prior art, mechanism and the feature of the inventive method are as described below:
(1) the present invention utilizes the performance of high thermal conductivity and the high refractive index improvement organic silicon packaging glue of nano silicon.Nano-silica surface after silane coupling agent surface treatment has covered one deck organism, makes between nano silicon and organosilicon, to have better consistency, and is conducive to the dispersion of nano silicon in organic silica gel matrix.
(2) the present invention adopts modified manometer silicon dioxide is directly dispersed in the polycondensation reaction system of silicone resin, has greatly improved the consistency of nano silicon and silicone resin;
(3) organosilicon sealant that prepared by method of the present invention, due to the good consistency that contains aminomethyl phenyl silica chain link and nano silicon and silicone resin; Refractive index and transmittance improve greatly;
(4) technique of the present invention is simple, and cost is low, and operational condition is easy to control, can obtain a series of high refractive index, high permeability for LED potting glue.
Embodiment
Below in conjunction with specific embodiment, further the present invention is set forth, should be understood that and quote embodiment only for the present invention is described, limit the scope of the invention and be not used in.
Embodiment 1
A preparation method for nano-silicon dioxide modified organosilicon sealant for LED encapsulation, the concrete steps of the method are as follows:
1) nano-silicon dioxide modified processing: by a certain amount of silicon-dioxide and γ aminopropyltriethoxy silane in mass ratio 100:1.00 be dissolved in appropriate benzene, under constantly stirring at 110 DEG C of-150 DEG C of temperature reflux 3-8h, then cooling, and dry in baking oven, to vapor away remaining benzene;
2) preparation of modified organic silicon glue: the mixture of dichloromethyl phenylsilane and improved silica is joined in the mixed solvent of toluene and water composition, DEG C Water Under solution 24h in temperature T=40, after reaction finishes, stratification is got supernatant liquid, with deionized water, supernatant liquid washing is extremely neutral, obtain hydrolysate silanol toluene solution;
3) add a certain amount of toluene solution dilution silanol toluene solution, add appropriate 0.2% sodium hydroxide, back flow reaction 12h at temperature T=100 DEG C, be cooled to and add after room temperature 5% trimethylchlorosilane as end-capping reagent, to neutral, the product obtaining is concentrated to remove toluene and water with deionized water wash;
4) curing process of nano-silicon dioxide modified organic resin: to add a certain amount of mass concentration in nano-silicon dioxide modified silicone resin be the dibutyl tin laurate that 5% diethylenetriamine and mass concentration are 1% making, and a certain amount of mass concentration is 1% polydimethylsiloxane, the amount of described catalyzer is benchmark by the quality of organic resin; After stirring, self-vulcanizing 6h, finally obtains the nano-silicon dioxide modified encapsulated with silicone resin glue solidifying.
Embodiment 2
A preparation method for nano-silicon dioxide modified organosilicon sealant for LED encapsulation, the concrete steps of the method are as follows:
1) nano-silicon dioxide modified processing: by a certain amount of silicon-dioxide and gamma-amino propyl trimethoxy silicane and N-beta-aminoethyl-gamma-amino propyl group methyltrimethoxy silane in mass ratio 100:1.00 be dissolved in appropriate toluene, under constantly stirring at 110 DEG C of-150 DEG C of temperature reflux 3-8h, then cooling, and dry in baking oven, to vapor away remaining toluene;
2) preparation of modified organic silicon glue: the mixture of phenyl-trichloro-silicane and improved silica is joined in the mixed solvent of toluene and water composition, DEG C Water Under solution 24h in temperature T=40, after reaction finishes, stratification is got supernatant liquid, with deionized water, supernatant liquid washing is extremely neutral, obtain hydrolysate silanol toluene solution;
3) add a certain amount of toluene solution dilution silanol toluene solution, add appropriate 0.2% potassium hydroxide, back flow reaction 12h at temperature T=100 DEG C, be cooled to and add after room temperature 5% trimethylchlorosilane as end-capping reagent, to neutral, the product obtaining is concentrated to remove toluene and water with deionized water wash;
4) curing process of nano-silicon dioxide modified organic resin: to add a certain amount of mass concentration in nano-silicon dioxide modified silicone resin be that 3% triethylene tetramine and mass concentration are 0.1% 2 lauric acid two stannous octoates making, and a certain amount of mass concentration is 0.05% polydimethylsiloxane, the amount of described catalyzer is benchmark by the quality of organic resin; After stirring, self-vulcanizing 6h, finally obtains the nano-silicon dioxide modified encapsulated with silicone resin glue solidifying.
Embodiment 3
A preparation method for nano-silicon dioxide modified organosilicon sealant for LED encapsulation, the concrete steps of the method are as follows:
1) nano-silicon dioxide modified processing: by a certain amount of silicon-dioxide and 2-ethyl trimethoxy silane and 3-ethyl trimethoxy silane in mass ratio 100:1.00 be dissolved in appropriate dimethylbenzene, under constantly stirring at 110 DEG C of-150 DEG C of temperature reflux 3-8h, then cooling, and dry in baking oven, to vapor away remaining dimethylbenzene;
2) preparation of modified organic silicon glue: the mixture of dichloromethyl phenylsilane, phenyl-trichloro-silicane, methyl ethylene dichlorosilane, dimethyldichlorosilane(DMCS) and improved silica is joined in the mixed solvent of toluene and water composition, DEG C Water Under solution 24h in temperature T=40, after reaction finishes, stratification is got supernatant liquid, with deionized water, supernatant liquid washing is extremely neutral, obtain hydrolysate silanol toluene solution;
3) add a certain amount of toluene solution dilution silanol toluene solution, add appropriate 0.2% Tetramethylammonium hydroxide, back flow reaction 12h at temperature T=100 DEG C, be cooled to and add after room temperature 5% trimethylchlorosilane as end-capping reagent, to neutral, the product obtaining is concentrated to remove toluene and water with deionized water wash;
4) curing process of nano-silicon dioxide modified organic resin: to add a certain amount of mass concentration in nano-silicon dioxide modified silicone resin be that 4% triethylene tetramine and mass concentration are 1% stannous octoate making, and a certain amount of mass concentration is 1% polydimethylsiloxane, the amount of described catalyzer is benchmark by the quality of organic resin; After stirring, self-vulcanizing 6h, finally obtains the nano-silicon dioxide modified encapsulated with silicone resin glue solidifying.
Taking above-mentioned foundation desirable embodiment of the present invention as enlightenment, by above-mentioned description, relevant staff can, not departing from the scope of this invention technological thought, carry out various change and amendment completely.The technical scope of this invention is not limited to the content on specification sheets, must determine its technical scope according to claim scope.
Claims (7)
1. a preparation method for nano-silicon dioxide modified organosilicon sealant for LED encapsulation, is characterized in that, the concrete steps of the method are as follows:
1) nano-silicon dioxide modified processing: by a certain amount of silicon-dioxide and silane coupling agent 100:(0.01-1.00 in mass ratio) be dissolved in appropriate organic solvent, under constantly stirring at 110 DEG C of-150 DEG C of temperature reflux 3-8h, then cooling, and dry in baking oven, to vapor away remaining organic solvent; Organic solvent is benzene, toluene, any in dimethylbenzene;
2) preparation of modified organic silicon glue: the mixture of chlorosilane and improved silica is joined in the mixed solvent of toluene and water composition, DEG C Water Under solution 24h in temperature T=40, after reaction finishes, stratification is got supernatant liquid, with deionized water, supernatant liquid washing is extremely neutral, obtain hydrolysate silanol toluene solution;
3) add a certain amount of toluene solution dilution silanol toluene solution, add proper catalyst, back flow reaction 12h at temperature T=100 DEG C, be cooled to and add after room temperature 5% trimethylchlorosilane as end-capping reagent, to neutral, the product obtaining is concentrated to remove toluene and water with deionized water wash;
4) curing process of nano-silicon dioxide modified organic resin: add a certain amount of solidifying agent and catalyzer in nano-silicon dioxide modified silicone resin making, and a certain amount of defoamer, the amount of described catalyzer is benchmark by the quality of organic resin; After stirring, self-vulcanizing 6h, finally obtains the nano-silicon dioxide modified encapsulated with silicone resin glue solidifying.
2. the preparation method of nano-silicon dioxide modified organosilicon sealant for a kind of LED encapsulation according to claim 1, it is characterized in that: described silane coupling agent comprises γ aminopropyltriethoxy silane, gamma-amino propyl trimethoxy silicane, N-beta-aminoethyl-gamma-amino propyl group methyltrimethoxy silane, 2-ethyl trimethoxy silane, 3-ethyl trimethoxy silane, 4-ethyl trimethoxy silane, 2-epoxy cyclohexane base silane, 3-epoxy cyclohexane base silane, 4-epoxy cyclohexane base silane, γ-glycidyl ether oxygen base propyl group trimethoxy silane, γ propyltrimethoxy silane, γ-methacryloyl oxosilane, γ-propyl-triethoxysilicane, γ-methacryloyl oxosilane, γ-propyl group dimethoxy silane, the mixing of one or more coupling agents in γ-methacryloyl oxosilane.
3. the preparation method of nano-silicon dioxide modified organosilicon sealant for a kind of LED encapsulation according to claim 1, is characterized in that: described chlorosilane is dichloromethyl phenylsilane, phenyl-trichloro-silicane, methyl ethylene dichlorosilane, dimethyldichlorosilane(DMCS).
4. the preparation method of nano-silicon dioxide modified organosilicon sealant for a kind of LED encapsulation according to claim 1, it is characterized in that: described catalyzer is sodium hydroxide, potassium hydroxide, sodium carbonate, Tetramethylammonium hydroxide, mass concentration is 0.05%-0.2%.
5. the preparation method of nano-silicon dioxide modified organosilicon sealant for a kind of LED encapsulation according to claim 1, is characterized in that: solidifying agent used is diethylenetriamine, triethylene tetramine, and mass concentration is 3%-5%.
6. the preparation method of nano-silicon dioxide modified organosilicon sealant for a kind of LED encapsulation according to claim 1, it is characterized in that: catalyzer used is the one in dibutyl tin laurate, two lauric acid two stannous octoates, two lauric acid two tin acetates, two neodecanoic acid tin methides, stannous octoate, and mass concentration is 0.1%-1%.
7. the preparation method of nano-silicon dioxide modified organosilicon sealant for a kind of LED encapsulation according to claim 1, is characterized in that: defoamer used is polydimethylsiloxane, and mass concentration is 0.05%-1%.
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| CN105060311A (en) * | 2015-08-25 | 2015-11-18 | 安徽良臣硅源材料有限公司 | Preparation method for waterproof silica gel bonded by hydrophilic groups |
| CN105968360A (en) * | 2016-05-31 | 2016-09-28 | 深圳市国华光电科技有限公司 | Organic-silicon ternary packaging material and preparation method thereof |
| CN107383894A (en) * | 2017-08-22 | 2017-11-24 | 成都新柯力化工科技有限公司 | The LED encapsulation material and preparation method of a kind of high transmission rate |
| CN107459963A (en) * | 2017-09-08 | 2017-12-12 | 常州市好利莱光电科技有限公司 | A kind of organic silicon potting adhesive |
| CN107572156A (en) * | 2017-08-22 | 2018-01-12 | 浙江海洋大学 | A kind of oil storage tank terrace leakage-resistant device |
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| CN108511584A (en) * | 2018-03-12 | 2018-09-07 | 合肥同佑电子科技有限公司 | A kind of special encapsulating material of light emitting diode and preparation method thereof |
| CN108517037A (en) * | 2018-04-13 | 2018-09-11 | 江苏芃湃新材料科技有限公司 | High heat conduction organosilicon composite material and preparation method |
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| CN110016242A (en) * | 2019-04-04 | 2019-07-16 | 深圳先进技术研究院 | The monolayer surface modifying method of nano silica |
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| CN115926493A (en) * | 2022-10-26 | 2023-04-07 | 中国科学院深圳先进技术研究院 | Preparation method and application of organic silicon composite material modified nano silicon dioxide with high oil phase compatibility and moisture curable film |
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| CN101343365A (en) * | 2008-08-28 | 2009-01-14 | 杭州师范大学 | Preparation method for methyl phenyl vinyl polysiloxane for packaging LED |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105060311A (en) * | 2015-08-25 | 2015-11-18 | 安徽良臣硅源材料有限公司 | Preparation method for waterproof silica gel bonded by hydrophilic groups |
| CN105968360B (en) * | 2016-05-31 | 2018-10-16 | 深圳市国华光电科技有限公司 | A kind of organosilicon ternary encapsulating material and preparation method thereof |
| CN105968360A (en) * | 2016-05-31 | 2016-09-28 | 深圳市国华光电科技有限公司 | Organic-silicon ternary packaging material and preparation method thereof |
| CN107955170B (en) * | 2016-10-14 | 2020-01-14 | 中昊晨光化工研究院有限公司 | Silicone elastomer for sealing and preparation method and application thereof |
| CN107955170A (en) * | 2016-10-14 | 2018-04-24 | 中昊晨光化工研究院有限公司 | A kind of silicone elastomer for being used to seal and its preparation method and application |
| CN107572156B (en) * | 2017-08-22 | 2019-06-25 | 浙江海洋大学 | A kind of oil storage tank terrace leakage-resistant device |
| CN107572156A (en) * | 2017-08-22 | 2018-01-12 | 浙江海洋大学 | A kind of oil storage tank terrace leakage-resistant device |
| CN107383894A (en) * | 2017-08-22 | 2017-11-24 | 成都新柯力化工科技有限公司 | The LED encapsulation material and preparation method of a kind of high transmission rate |
| CN107459963A (en) * | 2017-09-08 | 2017-12-12 | 常州市好利莱光电科技有限公司 | A kind of organic silicon potting adhesive |
| CN108511584A (en) * | 2018-03-12 | 2018-09-07 | 合肥同佑电子科技有限公司 | A kind of special encapsulating material of light emitting diode and preparation method thereof |
| CN108517037A (en) * | 2018-04-13 | 2018-09-11 | 江苏芃湃新材料科技有限公司 | High heat conduction organosilicon composite material and preparation method |
| CN108864785A (en) * | 2018-06-21 | 2018-11-23 | 镇江市益宝电气科技有限公司 | A kind of high-voltage insulated bus and coating process |
| CN110016242A (en) * | 2019-04-04 | 2019-07-16 | 深圳先进技术研究院 | The monolayer surface modifying method of nano silica |
| CN114248511A (en) * | 2021-12-22 | 2022-03-29 | 南通大学 | High-efficiency thermal protection aluminum foil glass fiber composite fabric |
| CN114686161A (en) * | 2022-06-02 | 2022-07-01 | 南宝光电材料(昆山)有限公司 | Organic silicon die bond adhesive and preparation method and application thereof |
| CN114686161B (en) * | 2022-06-02 | 2022-09-23 | 南宝光电材料(昆山)有限公司 | Organic silicon die bond adhesive and preparation method and application thereof |
| CN115926493A (en) * | 2022-10-26 | 2023-04-07 | 中国科学院深圳先进技术研究院 | Preparation method and application of organic silicon composite material modified nano silicon dioxide with high oil phase compatibility and moisture curable film |
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