CN101457022A - Production method of high refractive index nano modified organosilicon encapsulating material - Google Patents
Production method of high refractive index nano modified organosilicon encapsulating material Download PDFInfo
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- CN101457022A CN101457022A CNA2007101249793A CN200710124979A CN101457022A CN 101457022 A CN101457022 A CN 101457022A CN A2007101249793 A CNA2007101249793 A CN A2007101249793A CN 200710124979 A CN200710124979 A CN 200710124979A CN 101457022 A CN101457022 A CN 101457022A
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Abstract
A producing method for a high-refractive index modified organic silicon sealing material adopts a two-pack route and uses a plurality kinds of organic silicon polymer bodies provided with special function genes and produces ropy nanometer modified organic silicon polymer sealing solution together with the inorganic nanometer oxide sol through a certain technique; a thick coat on the chip is produced in a simple method before the solidification and the sealing coat with the needed performance is gained after a certain temperature process. The gained sealing material is provided with the performances of high refractive index, high transmittance, high-temperature resistance, being UV resistant and aging resistant and strong caking, thus can be applied in the sealing of the power typed LED lighting fittings.
Description
Technical field
The preparation of nano modified organosilicon encapsulating material
Background technology
Semi-conductor white-light illuminating (white light LEDs) with advantages such as energy-efficient, environmental protections enjoys various countries to attract attention in the prospect of illumination market.And constantly perfect along with the power type white light LED manufacturing technology, its luminous efficiency, brightness and power all have increased significantly.But in the process of making the power type white light LED device, except chip fabrication techniques, fluorescent material manufacturing technology and heat dissipation technology, the performance of LED packaged material will be to its luminous efficiency, brightness and work-ing life also producing remarkable influence.Use the packaged material of high refractive index, high anti-ultraviolet ability and heat-proof aging ability, low-stress, optical output power and the work-ing life that can obviously improve illuminating device.
Traditional epoxy resin encapsulating material is in the requirement that can not satisfy encapsulation aspect reliability and anti-ultraviolet and the heat aging performance far away.And organosilicon material is considered to be used for the best materials of high-power LED encapsulation owing to the advantage on the above-mentioned performance.But, because the domestic R﹠D work of up to the present seldom carrying out related products cause the organosilicon material of high refractive index to yet there are no report at present at home, and its application in the LED encapsulation also can only depend on import.Therefore, development has the organosilicon encapsulating material of high-clarity, high refractive index, good ultraviolet aging resistance and thermal ageing ability and realizes industrialization, and the development and the large-scale production of power-type LED device had crucial meaning.
Summary of the invention
In order to solve the various technical problems of present power-type LED packaged material, this project proposes the new technological approaches of preparation one class LED packaged material (filling or adhesives).This technology adopts nano inorganic oxide colloidal sol and organosilicon polymer with high refractive index compound; technology by organo-silicone rubber and the double-deck encapsulation of silicone resin; can not only realize the high-clarity, high refractive index of packaged material, good ultraviolet aging resistance and thermal ageing ability; and have the good interface consistency, can play a very good protection to inside chip.
Method of the present invention has been utilized the advantage performance of organosilicon superpolymer and inorganic nano colloidal sol.Adopt the multiple organosilicon performed polymer that contains the specific function group, obtain heavy-gravity nano modification organic polymer encapsulation colloidal sol with inorganic nanometer oxide colloidal sol by certain process means, before curing, make thick coating on the chip, obtain desired properties encapsulation coating through certain Temperature Treatment by simple method.Organosilicon partly increases the flexibility of film forming properties and coating; Inorganic oxide sol and organosilicon are compound, improve the hardness and the sticking power of rete; Because nano-oxide mingling in structure makes the structure of rete enrich, thermotolerance and uvioresistant ability are further improved; Have the compound of the inorganic oxide of high refractive index and organic poly-silicon superpolymer, can realize high refractive index with specific function group, and controlled within the specific limits; The processing of temperature can increase the effect between the composition and the effect of composition and base material, improves the hardness and the sticking power of rete.
The invention provides a kind of preparation method of high refractive index nano modified organosilicon encapsulating material, comprising the preparation method of organosilicon performed polymer, the preparation method of high refractive index nano inorganic oxide sol and the preparation method of nano modified organosilicon encapsulating material.
The preparation method of organosilicon performed polymer is: by the sol-gel technique polycondensation that is hydrolyzed, obtain the organosilicon performed polymer of certain ingredients with multiple organosilane monomers such as phenyl-trichloro-silicane, vinyl dimethyl dichlorosilane (DMCS) and dimethyldichlorosilane(DMCS)s.The synthesis material of organosilicon performed polymer adopts multiple organosilane monomers such as phenyl-trichloro-silicane, vinyl dimethyl dichlorosilane (DMCS) and dimethyldichlorosilane(DMCS).Wherein the part by weight of phenyl-trichloro-silicane is 5%～80%, and the part by weight of vinyl dimethyl dichlorosilane (DMCS) is 1%～50%, and the part by weight of dimethyldichlorosilane(DMCS) is 3%～90%.The part by weight of phenyl is for being 2%～50% in the organosilicon performed polymer, and the part by weight of vinyl is 0.1%～30%.Solvent adopts toluene and water, and the part by weight of toluene is 20%～80%, and the part by weight of water is 10%～70%.Temperature of reaction is 110～160 ℃, and the reaction times is 0.5～5h.Heat-processed can adopt oil bath or carry out in reactor.Carry out underpressure distillation after reacting completely, remove toluene and organosilicon small molecules, pressure is 0.05 normal atmosphere, and temperature is 110～160 ℃.
The preparation method of high refractive index nano inorganic oxide sol is: pass through hydrolytic condensation under certain condition with more than one metals or nonmetal alkoxide, obtain nano inorganic oxide colloidal sol.Raw material adopts multiple alkoxide such as tetraethoxy, four butanols zirconiums.Wherein the part by weight of tetraethoxy is that the part by weight of 1%～40%, four butanols zirconiums is 1%～95%, and the part by weight of butyl (tetra) titanate is 0.5%～10%.The weight of water is with respect to 2%～70% of metal and nonmetal alkoxide total amount.The employing dehydrated alcohol is a solvent, and the part by weight of dehydrated alcohol is 20%～99%.The interpolation mineral acid is a catalyzer, and the mineral acid of interpolation is following any: hydrochloric acid, phosphoric acid or acetic acid, its consumption are 0.001%～3%.PH value scope is controlled at 4～8.
The preparation method of nano modified organosilicon encapsulating material is: the nano inorganic oxide colloidal sol and the organosilicon performed polymer that will prepare carry out complex reaction, obtain nano modified organosilicon encapsulating material.Wherein the part by weight of nano inorganic oxide diluent is 0.1%～70%, and the part by weight of organosilicon polymer is 30%～100%.(straight chain silicone oil, main chain are the methyl hydrogen base, and two ends are with methyl blocking, and the massfraction of SiH is 0.3～3wt%) as linking agent, are 1%～50% with respect to the part by weight of organosilicon performed polymer to add containing hydrogen silicone oil.Adopt platinum divinyl tetramethyl disiloxane complex compound as catalyzer, concentration is 2000ppm～3000ppm, and addition is 2ppm～40ppm.Solidification value is 30～150 ℃, and be 2min～2h set time.
Adopt the nano modified organosilicon encapsulating material of method of the present invention preparation to have high-clarity, high refractive index, good ultraviolet aging resistance and thermal ageing ability.Show that through experiment test the visible light transmissivity of nano modified organosilicon encapsulating material reaches 98%, specific refractory power reaches more than 1.5, and 150 ℃ of following thermal treatments are after 1000 hours, and visible light transmissivity is decayed less than 5%.
Embodiment
Implement will be further understood that the present invention from following illustrative:
(1) preparation of different elementary composition organosilicon performed polymer new systems
Embodiment 1
Proportioning raw materials is: in round-bottomed flask, mechanical stirring drips the mixture of phenyl-trichloro-silicane 10g, vinyl dimethyl dichlorosilane (DMCS) 10g and dimethyldichlorosilane(DMCS) 50g with 140g toluene and 100g water.140 ℃ of reaction 1.5h, toluene is removed in underpressure distillation, obtains water white thick liquid.
Embodiment 2
Proportioning raw materials is: in round-bottomed flask, mechanical stirring drips the mixture of phenyl-trichloro-silicane 60g, vinyl dimethyl dichlorosilane (DMCS) 30g and dimethyldichlorosilane(DMCS) 35g with 230g toluene and 210g water.140 ℃ of reaction 1.5h, toluene is removed in underpressure distillation, obtains water white thick liquid.
Embodiment 3
Proportioning raw materials is: in round-bottomed flask, mechanical stirring drips the mixture of phenyl-trichloro-silicane 120g, vinyl dimethyl dichlorosilane (DMCS) 30g and dimethyldichlorosilane(DMCS) 35g with 320g toluene and 310g water.140 ℃ of reaction 1.5h, toluene is removed in underpressure distillation, obtains water white thick liquid.
(2) technology of preparing of nano inorganic oxide colloidal sol
Embodiment 4
Proportioning raw materials is: 200g dehydrated alcohol, 6g deionized water and 0.1g mixed in hydrochloric acid is even, and tetraethoxy 8g, four butanols zirconium 30g are added drop-wise in the above-mentioned mixing solutions after butyl (tetra) titanate 1g mixes.The room temperature lower magnetic force stirs 1h, slowly is heated to 80 ℃ of backflow 2h.Obtain the nano inorganic oxide colloidal sol diluent of water white transparency high dispersing.
Embodiment 5
Proportioning raw materials is: 200g dehydrated alcohol, 5.5g deionized water and 0.1g mixed in hydrochloric acid is even, and tetraethoxy 4g, four butanols zirconium 30g are added drop-wise in the above-mentioned mixing solutions after butyl (tetra) titanate 1g mixes.The room temperature lower magnetic force stirs 1h, slowly is heated to 80 ℃ of backflow 2h.Obtain the nano inorganic oxide colloidal sol diluent of water white transparency high dispersing.
(3) preparation of nano modified organosilicon encapsulating material
Embodiment 6
Proportioning raw materials is: the inorganic nanometer oxide diluent 20g of the foregoing description 4 preparations, the organosilicon performed polymer 100g and the containing hydrogen silicone oil 20g of embodiment 2 preparations added in the there-necked flask, and stirring at room 1h, ethanol is removed in 55 ℃ of underpressure distillation.Obtain water white thick liquid.Add the 1g platinum catalyst in above-mentioned liquid, stirring at room is even.Obtain stand-by nano modified organosilicon encapsulating material.Condition of cure adopts 100 ℃ of heating 0.5h.Specific refractory power is 1.50, and visible light transmissivity is 98%.
Embodiment 7
Proportioning raw materials is: the inorganic nanometer oxide diluent 50g of the foregoing description 4 preparations, the organosilicon performed polymer 100g and the containing hydrogen silicone oil 20g of embodiment 3 preparations added in the there-necked flask, and stirring at room 1h, ethanol is removed in 55 ℃ of underpressure distillation.Obtain water white thick liquid.Add the 1g platinum catalyst in above-mentioned liquid, stirring at room is even.Obtain stand-by nano modified organosilicon encapsulating material.Condition of cure adopts 100 ℃ of heating 0.5h.Specific refractory power is 1.52, and visible light transmissivity is 98%.
Embodiment 8
Proportioning raw materials is: the organosilicon performed polymer 100g of the inorganic nanometer oxide diluent 80g of the foregoing description 4 preparation, embodiment 3 preparations mixed with containing hydrogen silicone oil 20g adds in the there-necked flask, and stirring at room 1h, ethanol is removed in 55 ℃ of underpressure distillation.Obtain water white thick liquid.Add the 1g platinum catalyst in above-mentioned liquid, stirring at room is even.Obtain stand-by nano modified organosilicon encapsulating material.Condition of cure adopts 100 ℃ of heating 0.5h.Specific refractory power is 1.55, and visible light transmissivity is 98%.
Claims (14)
1. method for preparing high refractive index nano modified organosilicon encapsulating material, it is characterized in that: inorganic nanometer oxide colloidal sol and organosilicon performed polymer is compound, be used for nano modified organosilicon encapsulating material, be mainly used in the encapsulation of power-type LED illuminating device.
2. according to the described preparation method of claim 1, it is characterized in that: the synthesis material of the organosilicon performed polymer of preparation adopts multiple organosilane monomers such as phenyl-trichloro-silicane, vinyl dimethyl dichlorosilane (DMCS) and dimethyldichlorosilane(DMCS).Wherein the part by weight of phenyl-trichloro-silicane is 5%～80%, and the part by weight of vinyl dimethyl dichlorosilane (DMCS) is 1%～50%, and the part by weight of dimethyldichlorosilane(DMCS) is 3%～90%,
3. according to the described preparation method of claim 1, it is characterized in that: the part by weight that the organosilicon performed polymer of preparation contains phenyl is 2%～50%, and the part by weight of vinyl is 0.1%～30%.
4. according to the described preparation method of claim 1, it is characterized in that: preparation organosilicon performed polymer solvent adopts toluene and water, and the part by weight of toluene is 20%～80%, and the part by weight of water is 10%～70%.
5. according to the described preparation method of claim 1, it is characterized in that: preparation organosilicon prepolymer reaction temperature is 110～160 ℃, and the reaction times is 0.5～5h.
6. according to the described preparation method of claim 1, it is characterized in that: preparation nano inorganic oxide colloidal sol, raw material adopts tetraethoxy, four butanols zirconium and butyl (tetra) titanates, wherein the part by weight of tetraethoxy is 1%～40%, the part by weight of four butanols zirconiums is 1%～95%, and the part by weight of butyl (tetra) titanate is 0.5%～10%.
7. according to the described preparation method of claim 1, it is characterized in that: preparation nano inorganic oxide colloidal sol, the weight of water is with respect to 2%～70% of metal and nonmetal alkoxide total amount.The employing dehydrated alcohol is a solvent, and the part by weight of dehydrated alcohol is 20%～99%.
8. according to the described preparation method of claim 1, it is characterized in that: preparation nano inorganic oxide colloidal sol, mineral acid is a catalyzer, the mineral acid of interpolation is following any: hydrochloric acid, phosphoric acid or acetic acid, its consumption are 0.001%～3%.PH value scope is controlled at 4～8.
9. according to the described preparation method of claim 1, it is characterized in that: the temperature of reaction of preparation nano inorganic oxide colloidal sol is controlled at 50～90 ℃, and the time is 1～4h.
10. according to the described preparation method of claim 1, it is characterized in that: preparation nano modified organosilicon envelope
10. according to the described preparation method of claim 1, it is characterized in that: the preparation nano modified organosilicon encapsulating material, the part by weight of nano inorganic oxide diluent is 0.1%～70%, the part by weight of organosilicon polymer is 30%～100%.
11. according to the described preparation method of claim 1, it is characterized in that: the preparation nano modified organosilicon encapsulating material adds containing hydrogen silicone oil as linking agent, and containing hydrogen silicone oil is 1%～50% with respect to the part by weight of organosilicon performed polymer.
12. according to the described preparation method of claim 1, it is characterized in that: the preparation nano modified organosilicon encapsulating material adds containing hydrogen silicone oil as linking agent, and containing hydrogen silicone oil is a straight chain silicone oil, and main chain is the methyl hydrogen base, and two ends are with methyl blocking.The massfraction of SiH is 0.3～3wt% in the containing hydrogen silicone oil.
13. according to the described preparation method of claim 1, it is characterized in that: the preparation nano modified organosilicon encapsulating material adopts platinum divinyl tetramethyl disiloxane complex compound as catalyzer, concentration is 1000ppm～3000ppm, and addition is 2ppm～40ppm.
14. according to the described preparation method of claim 1, it is characterized in that: preparation nano modified organosilicon encapsulating material solidification value is 30～150 ℃, and be 2min～2h set time.
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101924177A (en) * | 2010-08-03 | 2010-12-22 | 陕西科技大学 | Light-emitting diode with light distributing function and preparation method thereof |
| CN102391529A (en) * | 2011-07-14 | 2012-03-28 | 杭州师范大学 | Preparation method of silicone resin type organic/inorganic hybrid material for packaging |
| CN102952271A (en) * | 2012-06-07 | 2013-03-06 | 安徽众星新材料有限公司 | High-refraction-index silicon resin as well as preparation method and application thereof |
| CN103059573A (en) * | 2012-12-19 | 2013-04-24 | 中科院广州化学有限公司 | Inorganic/organic hybridization nanometer composite resin and light-emitting diode (LED) packaging materials prepared by the same |
| CN103131189A (en) * | 2013-01-05 | 2013-06-05 | 中科院广州化学有限公司 | Inorganic or organic hybridization nanocomposite for packaging light emitting diode (LED) and preparation method thereof |
| CN103265702A (en) * | 2013-05-28 | 2013-08-28 | 哈尔滨工业大学 | Preparation method of ultraviolet-resistant and high-temperature-resistant methyl silicone resin |
| CN103408799A (en) * | 2013-07-26 | 2013-11-27 | 中科院广州化学有限公司 | Modified nano silicon dioxide used for LED organosilicon packaging material, and preparation method thereof |
| CN104640946A (en) * | 2012-09-21 | 2015-05-20 | 道康宁东丽株式会社 | Highly refractive surface treatment agent, and fine member and optical material surface-treated using the same |
| JP2015531797A (en) * | 2012-07-13 | 2015-11-05 | ベーヨットエス・セラミクス・ゲーエムベーハー | Production method of polysilane |
| CN105399956A (en) * | 2015-11-25 | 2016-03-16 | 烟台德邦先进硅材料有限公司 | High-temperature-resistant high-refractive-index Ti-containing organic silicon resin and preparation method thereof |
| WO2017092412A1 (en) * | 2015-11-30 | 2017-06-08 | 苏州太湖电工新材料股份有限公司 | Nano-silica hybrid vinyl phenyl silicon intermediate, preparation method therefor and use thereof in environmentally-friendly insulating paint |
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- 2007-12-12 CN CNA2007101249793A patent/CN101457022A/en active Pending
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| CN101924177A (en) * | 2010-08-03 | 2010-12-22 | 陕西科技大学 | Light-emitting diode with light distributing function and preparation method thereof |
| CN102391529A (en) * | 2011-07-14 | 2012-03-28 | 杭州师范大学 | Preparation method of silicone resin type organic/inorganic hybrid material for packaging |
| CN102952271A (en) * | 2012-06-07 | 2013-03-06 | 安徽众星新材料有限公司 | High-refraction-index silicon resin as well as preparation method and application thereof |
| JP2015531797A (en) * | 2012-07-13 | 2015-11-05 | ベーヨットエス・セラミクス・ゲーエムベーハー | Production method of polysilane |
| CN104640946A (en) * | 2012-09-21 | 2015-05-20 | 道康宁东丽株式会社 | Highly refractive surface treatment agent, and fine member and optical material surface-treated using the same |
| CN103059573B (en) * | 2012-12-19 | 2015-08-05 | 中科院广州化学有限公司 | The LED material of inorganic/organic hybrid nanocomposite and preparation thereof |
| CN103059573A (en) * | 2012-12-19 | 2013-04-24 | 中科院广州化学有限公司 | Inorganic/organic hybridization nanometer composite resin and light-emitting diode (LED) packaging materials prepared by the same |
| CN103131189A (en) * | 2013-01-05 | 2013-06-05 | 中科院广州化学有限公司 | Inorganic or organic hybridization nanocomposite for packaging light emitting diode (LED) and preparation method thereof |
| CN103265702B (en) * | 2013-05-28 | 2015-04-22 | 哈尔滨工业大学 | Preparation method of ultraviolet-resistant and high-temperature-resistant methyl silicone resin |
| CN103265702A (en) * | 2013-05-28 | 2013-08-28 | 哈尔滨工业大学 | Preparation method of ultraviolet-resistant and high-temperature-resistant methyl silicone resin |
| CN103408799A (en) * | 2013-07-26 | 2013-11-27 | 中科院广州化学有限公司 | Modified nano silicon dioxide used for LED organosilicon packaging material, and preparation method thereof |
| CN105399956A (en) * | 2015-11-25 | 2016-03-16 | 烟台德邦先进硅材料有限公司 | High-temperature-resistant high-refractive-index Ti-containing organic silicon resin and preparation method thereof |
| WO2017092412A1 (en) * | 2015-11-30 | 2017-06-08 | 苏州太湖电工新材料股份有限公司 | Nano-silica hybrid vinyl phenyl silicon intermediate, preparation method therefor and use thereof in environmentally-friendly insulating paint |
| US10662291B2 (en) | 2015-11-30 | 2020-05-26 | Suzhou Taihu Electric Advanced Material Co, Ltd. | Nano-silica hybrid vinyl phenyl silicon intermediate, preparation method thereof and use thereof in environmentally-friendly insulating varnish |
| CN109943191A (en) * | 2019-03-14 | 2019-06-28 | 珠海市横琴新区贝格特实业有限公司 | Solvent-free heat-conducting resin preparation and coating processes |
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