CN103408799A - Modified nano silicon dioxide used for LED organosilicon packaging material, and preparation method thereof - Google Patents
Modified nano silicon dioxide used for LED organosilicon packaging material, and preparation method thereof Download PDFInfo
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- CN103408799A CN103408799A CN2013103213306A CN201310321330A CN103408799A CN 103408799 A CN103408799 A CN 103408799A CN 2013103213306 A CN2013103213306 A CN 2013103213306A CN 201310321330 A CN201310321330 A CN 201310321330A CN 103408799 A CN103408799 A CN 103408799A
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Abstract
The invention belongs to the field of organosilicon packaging material and discloses modified nano silicon dioxide used for LED organosilicon packaging material, and a preparation method and the application of the modified nano silicon dioxide. The modified nano silicon dioxide comprises the following components in parts by weight: 50 parts of nano silicon dioxide, 2 to 20 parts of hydrogenous chlorosilane monomer, 0.5 to 20 parts of phenyl silicone monomer and 500 to 2000 parts of organic solvent. When the modified nano silicon dioxide is applied to LED organosilicon packaging basis material, the comprehensive effect of improving the strength, the refractive index, the light transmittance and other optical properties of the material can be achieved, so that the LED organosilicon packaging material has the excellent properties such as high refracting index, high transparency, ultraviolet aging resistance and thermal aging resistance.
Description
Technical field
The invention belongs to the organosilicon encapsulating material field, particularly a kind of LED used for packing material modified manometer silicon dioxide and preparation method thereof and application.
Background technology
The LED encapsulation refers to the encapsulation of luminescence chip, and comparing integrated antenna package has relatively big difference.The encapsulation of LED not only requirement can be protected wick, but also can printing opacity, so the encapsulation of LED has special requirement to packaged material.Along with the LED manufacturing technology is constantly perfect, its luminous efficiency, brightness and power all have increased significantly, and require packaged material to have the performances such as high optics, mechanics, electricity and resistance toheat.At present, the LED packaged material is mainly epoxy resin and organosilicon material both at home and abroad.Organosilicon material has the good transparency, weathering resistance, insulativity and strong hydrophobicity etc., be widely used as the LED packaged material, but its lower specific refractory power (1.40) and mechanical strength, limited again it conversely in the particularly application in high-end LED packaged material field of LED packaged material.
Nano silicon or titanium dioxide etc. carry out modification to organosilicon LED packaged material can effectively improve the performances such as its specific refractory power (1.40) and mechanical strength, but, nano silicon adopts the mode of physical blending more to the modification of LED packaged material at present, although this modification mode can make LED packaged material specific refractory power and mechanical property etc. be improved, but the increase along with the nano-silicon dioxide particle addition, because the homogeneity of Nano particles of silicon dioxide and organosilicon body material is poor, cause the optical properties such as the transparency of organosilicon encapsulating material obviously to descend.
Summary of the invention
For overcoming shortcoming and defect of the prior art, primary and foremost purpose of the present invention is to provide a kind of modified manometer silicon dioxide that can improve simultaneously LED organosilicon encapsulating material specific refractory power, transmissivity, mechanical strength.
Another object of the present invention is to provide the preparation method of above-mentioned LED organosilicon encapsulating material with modified manometer silicon dioxide.
A further object of the present invention is to provide the application of above-mentioned modified manometer silicon dioxide in the LED organosilicon encapsulating material.
Purpose of the present invention is achieved through the following technical solutions: a kind of LED organosilicon encapsulating material modified manometer silicon dioxide, and described LED organosilicon encapsulating material is comprised of the following component of meter by weight with modified manometer silicon dioxide:
The particle diameter of described nano silicon is 50～500nm.
The described silicon hydride chlorid monomer that contains has following structure:
Wherein, R is CH
3, CH
2CH
3Perhaps Ph.
The described phenyl siloxane monomer that contains is a kind of in phenyl three (dimethyl siloxane) silane, phenyl three (trimethylsiloxane group) silane, dimethoxydiphenylsilane, phenylbenzene diethoxy silane, phenyltrimethoxysila,e and phenyl triethoxysilane or at least two kinds.
Described organic solvent is a kind of in tetrahydrofuran (THF), benzene, toluene and butanone or at least two kinds.
The above-mentioned LED organosilicon encapsulating material preparation method of modified manometer silicon dioxide comprises following operation steps:
Contain the phenyl siloxane monomer, 500～2000 weight part organic solvents that contain silicon hydride chlorid monomer, 0.5～20 weight part of the nano silicon of 50 weight parts, 2～20 weight parts are packed in reactor, mix and stir, again mixture was reacted 3～10 hours under 30～100 ℃, at 40～100 ℃ of lower rotary evaporations, remove organic solvent, then adding triethylamine to regulate PH is 6～8, distilled water wash, finally obtain modified manometer silicon dioxide 50～80 ℃ of lower vacuum-dryings.
Described reactor is the reactor with stirrer, condensing reflux pipe and thermometer; The number of times of described distilled water wash is 5～10 times.
The application of above-mentioned modified manometer silicon dioxide in preparation LED organosilicon encapsulating material, described application is according to following operation steps: meter by weight, 0.5～60 part of modified manometer silicon dioxide, the containing hydrogen silicone oil of 5～100 parts, the vinyl silicone oil of 5～100 parts, the catalyzer of 0.0001～0.01 part are placed in to open container, under normal temperature, stir, under 60～150 ℃ of vacuum conditions, reacted 0.3～2 hour, obtain containing the LED organosilicon encapsulating material of modified manometer silicon dioxide.
Described catalyzer is Platinic chloride, H
2PtCl
6Tetrahydrofuran solution, H
2PtCl
6Aqueous isopropanol, Pt (PPh
3)
4, Cp
2The mixture of one or both in the platinum complex of the platinum complex of PtCl, the coordination of ethylene methacrylic radical siloxane, the platinum complex of diethyl phthalate coordination, dicyclopentadiene platinum dichloride and dichloro two (triphenylphosphine);
Described containing hydrogen silicone oil is more than one in Methyl Hydrogen Polysiloxane Fluid, methyl and phenyl hydrogen-containing silicon oil, and the molar content of hydrogen is 0.2%～1.45%;
Described vinyl silicone oil is more than one in methyl vinyl silicon oil, methyl phenyl vinyl silicone oil, and the molar content of vinyl is 0.1%～2.3%.
The present invention compared with prior art has following advantage and beneficial effect:
(1) adopt and have the silicon hydride chlorid of containing, the condensation that is hydrolyzed of phenyl siloxane and nano silicon obtains the modified manometer silicon dioxide of the high refractive index of siliceous-hydrogen bond, utilize the Si-H group on modified manometer silicon dioxide to participate in the addition reaction of silicon with hydrogen of LED organosilicon encapsulation matrix material, the agglomeration traits of having avoided nano silicon and the blend of LED organosilicon encapsulation matrix Material Physics to cause is more obvious to the organosilicon material reinforcement.
(2) adopt and have the silicon hydride chlorid of containing, the condensation that is hydrolyzed of phenyl siloxane and nano silicon obtains the modified manometer silicon dioxide of the high refractive index of siliceous-hydrogen bond, due to the phenyl siloxane of having introduced high refractive index in modified manometer silicon dioxide, therefore, with this modified manometer silicon dioxide, add in LED organosilicon encapsulating compound, overcome the problem of the optical property reduction that makes organosilicon encapsulating material adding of nano silicon.
(3) prepared modified manometer silicon dioxide is applied to the performance that the LED organosilicon encapsulating material has the excellences such as high refractive index, high-clarity, excellent ultraviolet aging resistance and heat-proof aging.
Embodiment
Below in conjunction with embodiment, the present invention is done to further detailed description, but embodiments of the present invention are not limited to this.
Embodiment 1
1, a kind of LED organosilicon encapsulating material preparation method of modified manometer silicon dioxide
The nano silicon of 50g (particle diameter is 50nm), the diphenyl dichlorosilane of 2g, the dimethoxydiphenylsilane of 10g, 1500g butanone are packed into possess stirrer, in the reactor of condensing reflux pipe and thermometer, mix and stir, then mixture was reacted 8 hours under 30 ℃, at 50 ℃ of lower rotary evaporations, remove organic solvent, then adding triethylamine to regulate PH is 6 rear distilled water wash 5 times, then 60 ℃ of lower vacuum-dryings, obtains modified manometer silicon dioxide.
2, the application of modified manometer silicon dioxide in the LED organosilicon encapsulating material
0.2%), (contents of ethylene is: for the methyl vinyl silicon oil of 80g 1.2%), the H of 0.0001g (hydrogen content is the methyl and phenyl hydrogen-containing silicon oil of modified manometer silicon dioxide 0.5g, the 100g of step 1 preparation:
2PtCl
6Tetrahydrofuran solution be placed in open container, under normal temperature, stir, reaction is 0.3 hour under 100 ℃ of lower vacuum conditions, obtains containing the cured article of the LED organosilicon encapsulating material of modified manometer silicon dioxide.The cured article that gained is contained to the LED organosilicon encapsulating material of modified manometer silicon dioxide carries out Performance Detection, and result is as follows:
Performance: refraction coefficient 1.50, transmittance 95%, hardness Shao Shi A35.
Transmissivity: press GB/T2410-2008 and measure; Specific refractory power: press GB/T6488-2008 and measure; Hardness: press GB/T2411-2008 and measure.
Embodiment 2
1, a kind of LED organosilicon encapsulating material preparation method of modified manometer silicon dioxide
The nano silicon of 50g (particle diameter is 500nm), the diphenyl chlorosilane of 10g, 10g dimethylchlorosilane, the dimethoxydiphenylsilane of 5g, 800g tetrahydrofuran (THF) are packed into possess stirrer, in the reactor of condensing reflux pipe and thermometer, mix and stir, then mixture was reacted 10 hours under 50 ℃, at 40 ℃ of lower rotary evaporations, remove organic solvent, then adding triethylamine to regulate PH is 8 rear distilled water wash 8 times, then 75 ℃ of lower vacuum-dryings, obtains modified manometer silicon dioxide.
2, the application of modified manometer silicon dioxide in the LED organosilicon encapsulating material
1.45%), (contents of ethylene is: for the phenyl-vinyl silicon oil of 8g 2.01%), the Pt (PPh of 0.0005g (hydrogen content is the methyl and phenyl hydrogen-containing silicon oil of modified manometer silicon dioxide 5g, the 5g of step 1 preparation:
3)
4Be placed in open container, stir under normal temperature, reaction is 0.5 hour under 70 ℃ of lower vacuum conditions, obtains containing the cured article of the LED organosilicon encapsulating material of modified manometer silicon dioxide.The cured article that gained is contained to the LED organosilicon encapsulating material of modified manometer silicon dioxide carries out Performance Detection, and result is as follows:
Performance: refraction coefficient 1.55, transmittance 96%, hardness Shao Shi A42.
Transmissivity: press GB/T2410-2008 and measure; Specific refractory power: press GB/T6488-2008 and measure; Hardness: press GB/T2411-2008 and measure.
Embodiment 3
1, a kind of LED organosilicon encapsulating material preparation method of modified manometer silicon dioxide
The dimethylchlorosilane of the nano silicon of 50g (particle diameter is 200nm), 5g, phenyl three (dimethyl siloxane) silane of 15g, 1000g toluene are packed into possess stirrer, in the reactor of condensing reflux pipe and thermometer, mix and stir, then mixture was reacted 3 hours under 100 ℃, at 80 ℃ of lower rotary evaporations, remove organic solvent, then adding triethylamine to regulate PH is 7 rear distilled water wash 5 times, then 80 ℃ of lower vacuum-dryings, obtains modified manometer silicon dioxide.
2, the application of modified manometer silicon dioxide in the LED organosilicon encapsulating material
1.23%), (contents of ethylene is: for the methyl vinyl silicon oil of 5g 1.52%), the Pt (PPh of 0.002g (hydrogen content is the Methyl Hydrogen Polysiloxane Fluid of modified manometer silicon dioxide 10g, the 20g of step 1 preparation:
3)
4, 0.003g Cp
2PtCl is placed in open container, stirs under normal temperature, and reaction is 1 hour under 60 ℃ of lower vacuum conditions, obtains containing the cured article of the LED organosilicon encapsulating material of modified manometer silicon dioxide.The cured article that gained is contained to the LED organosilicon encapsulating material of modified manometer silicon dioxide carries out Performance Detection, and result is as follows:
Performance: refraction coefficient 1.53, transmittance 93%, hardness Shao Shi A40.
Transmissivity: press GB/T2410-2008 and measure; Specific refractory power: press GB/T6488-2008 and measure; Hardness: press GB/T2411-2008 and measure.
Embodiment 4
1, a kind of LED organosilicon encapsulating material preparation method of modified manometer silicon dioxide
The nano silicon of 50g (particle diameter is 100nm), the ethyl dichlorosilane of 15g, the dimethoxydiphenylsilane list of 0.5g, 500g toluene are packed into possess stirrer, in the reactor of condensing reflux pipe and thermometer, mix and stir, then mixture was reacted 6 hours under 80 ℃, at 100 ℃ of lower rotary evaporations, remove organic solvent, then adding triethylamine to regulate PH is 7 rear distilled water wash 10 times, then 60 ℃ of lower vacuum-dryings, obtains modified manometer silicon dioxide.
2, the application of modified manometer silicon dioxide in the LED organosilicon encapsulating material
0.51%), (contents of ethylene is: for the methyl phenyl vinyl silicone oil of 30g 2.3%), the platinum complex of the diethyl phthalate coordination of 0.01g is placed in open container (hydrogen content is the methyl and phenyl hydrogen-containing silicon oil of modified manometer silicon dioxide 60g, the 40g of step 1 preparation:, under normal temperature, stir, reaction is 1.5 hours under 120 ℃ of vacuum conditions, obtains containing the cured article of the LED organosilicon encapsulating material of modified manometer silicon dioxide.The cured article that gained is contained to the LED organosilicon encapsulating material of modified manometer silicon dioxide carries out Performance Detection, and result is as follows:
Performance: refraction coefficient 1.51, transmittance 90%, hardness Shao Shi A50.
Transmissivity: press GB/T2410-2008 and measure; Specific refractory power: press GB/T6488-2008 and measure; Hardness: press GB/T2411-2008 and measure.
Embodiment 5
1, a kind of LED organosilicon encapsulating material preparation method of modified manometer silicon dioxide
By the nano silicon of 50g (particle diameter is 150nm), the diphenyl dichlorosilane of 5g, the diphenyl chlorosilane of 5g, the phenyltrimethoxysila,e of 5g, the 10g dimethoxydiphenylsilane, 5g phenylbenzene diethoxy silane, the 2000g tetrahydrofuran (THF) is packed into and is possessed stirrer, in the reactor of condensing reflux pipe and thermometer, mix and stir, then mixture was reacted 5 hours under 60 ℃, at 60 ℃ of lower rotary evaporations, remove organic solvent, then adding triethylamine to regulate PH is 6 rear distilled water wash 6 times, then 50 ℃ of lower vacuum-dryings, obtain modified manometer silicon dioxide.
2, the application of modified manometer silicon dioxide in the LED organosilicon encapsulating material
1.05%), (contents of ethylene is: for the methyl phenyl vinyl silicone oil of 100g 0.1%), the platinum complex of the ethylene methacrylic radical siloxane coordination of 0.008g is placed in open container (hydrogen content is the Methyl Hydrogen Polysiloxane Fluid of modified manometer silicon dioxide 20g, the 80g of step 1 preparation:, under normal temperature, stir, reaction is 2 hours under 150 ℃ of lower vacuum conditions, obtains containing the cured article of the LED organosilicon encapsulating material of modified manometer silicon dioxide.The cured article that gained is contained to the LED organosilicon encapsulating material of modified manometer silicon dioxide carries out Performance Detection, and result is as follows:
Performance: refraction coefficient 1.50, transmittance 93%, hardness Shao Shi A34.
Transmissivity: press GB/T2410-2008 and measure; Specific refractory power: press GB/T6488-2008 and measure; Hardness: press GB/T2411-2008 and measure.
Comparative Examples
1, nano-silicon dioxide modified LED organosilicon encapsulating material
Common nano silicon 20g(particle diameter is 200nm), 0.51%), (contents of ethylene is: for the methyl phenyl vinyl silicone oil of 50g 0.1%), the H of 0.006g (hydrogen content is: for the Methyl Hydrogen Polysiloxane Fluid of 30g
2PtCl
6Aqueous isopropanol be placed in open container, under normal temperature, stir, reaction is 0.8 hour under 120 ℃ of vacuum conditions, obtains containing the cured article of the LED organosilicon encapsulating material of modified manometer silicon dioxide.The cured article that gained is contained to the LED organosilicon encapsulating material of modified manometer silicon dioxide carries out Performance Detection, and result is as follows:
Performance: ultraviolet aging resistance is good, refraction coefficient 1.42, transmittance 86%, hardness Shao Shi A30.
Transmissivity: press GB/T2410-2008 and measure; Specific refractory power: press GB/T6488-2008 and measure; Hardness: press GB/T2411-2008 and measure.
Above-described embodiment is preferably embodiment of the present invention; but embodiments of the present invention are not restricted to the described embodiments; other any do not deviate from change, the modification done under spirit of the present invention and principle, substitutes, combination, simplify; all should be equivalent substitute mode, within being included in protection scope of the present invention.
Claims (9)
1. LED organosilicon encapsulating material modified manometer silicon dioxide is characterized in that: described LED organosilicon encapsulating material is comprised of the following component of meter by weight with modified manometer silicon dioxide:
2. LED organosilicon encapsulating material modified manometer silicon dioxide according to claim 1, it is characterized in that: the particle diameter of described nano silicon is 50～500nm.
3. LED organosilicon encapsulating material modified manometer silicon dioxide according to claim 1, it is characterized in that: the described silicon hydride chlorid monomer that contains has following structure:
Perhaps
In a kind of or mixture of two kinds;
Wherein, R is CH
3, CH
2CH
3Perhaps Ph.
4. LED organosilicon encapsulating material modified manometer silicon dioxide according to claim 1 is characterized in that: the described phenyl siloxane monomer that contains is a kind of in phenyl three (dimethyl siloxane) silane, phenyl three (trimethylsiloxane group) silane, dimethoxydiphenylsilane, phenylbenzene diethoxy silane, phenyltrimethoxysila,e and phenyl triethoxysilane or at least two kinds.
5. LED organosilicon encapsulating material modified manometer silicon dioxide according to claim 1 is characterized in that: described organic solvent is a kind of in tetrahydrofuran (THF), benzene, toluene and butanone or at least two kinds.
6. LED organosilicon encapsulating material according to claim 1 by the preparation method of modified manometer silicon dioxide, is characterized in that comprising following operation steps:
Contain the phenyl siloxane monomer, 500～2000 weight part organic solvents that contain silicon hydride chlorid monomer, 0.5～20 weight part of the nano silicon of 50 weight parts, 2～20 weight parts are packed in reactor, mix and stir, again mixture was reacted 3～10 hours under 30～100 ℃, at 40～100 ℃ of lower rotary evaporations, remove organic solvent, then adding triethylamine to regulate PH is 6～8, distilled water wash, finally obtain modified manometer silicon dioxide 50～80 ℃ of lower vacuum-dryings.
7. preparation method according to claim 6 is characterized in that: described reactor is the reactor with stirrer, condensing reflux pipe and thermometer; The number of times of described distilled water wash is 5～10 times.
8. the application of modified manometer silicon dioxide according to claim 1 in preparation LED organosilicon encapsulating material, it is characterized in that: described application is according to following operation steps: meter by weight, 0.5～60 part of modified manometer silicon dioxide, the containing hydrogen silicone oil of 5～100 parts, the vinyl silicone oil of 5～100 parts, the catalyzer of 0.0001～0.01 part are placed in to open container, under normal temperature, stir, under 60～150 ℃ of vacuum conditions, reacted 0.3～2 hour, obtain containing the LED organosilicon encapsulating material of modified manometer silicon dioxide.
9. application according to claim 8 is characterized in that: described catalyzer is Platinic chloride, H
2PtCl
6Tetrahydrofuran solution, H
2PtCl
6Aqueous isopropanol, Pt (PPh
3)
4, Cp
2The mixture of one or both in the platinum complex of the platinum complex of PtCl, the coordination of ethylene methacrylic radical siloxane, the platinum complex of diethyl phthalate coordination, dicyclopentadiene platinum dichloride and dichloro two (triphenylphosphine);
Described containing hydrogen silicone oil is more than one in Methyl Hydrogen Polysiloxane Fluid, methyl and phenyl hydrogen-containing silicon oil, and the molar content of hydrogen is 0.2%～1.45%;
Described vinyl silicone oil is more than one in methyl vinyl silicon oil, methyl phenyl vinyl silicone oil, and the molar content of vinyl is 0.1%～2.3%.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117819919A (en) * | 2024-03-04 | 2024-04-05 | 德州润德混凝土有限公司 | Light anti-cracking high-performance concrete and preparation method thereof |
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|---|---|---|---|---|
| US20090057699A1 (en) * | 2007-09-04 | 2009-03-05 | Philips Lumileds Lighting Company, Llc | LED with Particles in Encapsulant for Increased Light Extraction and Non-Yellow Off-State Color |
| CN101457022A (en) * | 2007-12-12 | 2009-06-17 | 深圳大学 | Production method of high refractive index nano modified organosilicon encapsulating material |
| CN102993753A (en) * | 2012-11-23 | 2013-03-27 | 中科院广州化学有限公司 | Composite hybrid organic silicon LED (Light Emitting Diode) packaging material, preparation method and applications thereof |
-
2013
- 2013-07-26 CN CN201310321330.6A patent/CN103408799B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20090057699A1 (en) * | 2007-09-04 | 2009-03-05 | Philips Lumileds Lighting Company, Llc | LED with Particles in Encapsulant for Increased Light Extraction and Non-Yellow Off-State Color |
| CN101457022A (en) * | 2007-12-12 | 2009-06-17 | 深圳大学 | Production method of high refractive index nano modified organosilicon encapsulating material |
| CN102993753A (en) * | 2012-11-23 | 2013-03-27 | 中科院广州化学有限公司 | Composite hybrid organic silicon LED (Light Emitting Diode) packaging material, preparation method and applications thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117819919A (en) * | 2024-03-04 | 2024-04-05 | 德州润德混凝土有限公司 | Light anti-cracking high-performance concrete and preparation method thereof |
| CN117819919B (en) * | 2024-03-04 | 2024-04-30 | 德州润德混凝土有限公司 | Light anti-cracking high-performance concrete and preparation method thereof |
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