CN103937445B - Preparation method of transparent organic silica gel with high refractive index for high brightness and large power COB-LED encapsulation - Google Patents
Preparation method of transparent organic silica gel with high refractive index for high brightness and large power COB-LED encapsulation Download PDFInfo
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Abstract
The invention relates to a preparation method of a transparent organic silica gel with a high refractive index for high brightness and large power COB-LED encapsulation, and belongs to the technical field of photoelectrical device encapsulation materials. The key points of the preparation method are that: phenyl vinyl resin (component A) and phenyl hydrogen-containing silicone oil (component B), which both have a high refractive index and are transparent, are synthesized firstly, then chloroplatinic acid or platinum complex is used as the catalyst, and finally the mixture of the component A and the component B is cured under a certain condition so as to obtain the transparent and high temperature resistant organic silicone encapsulating gel; wherein the mass ratio of the component A to the component B is (1-5):1. The preparation method comprises the following steps: mixing the component A and the component B, then adding a little amount of catalyst, or mixing the component B and the catalyst firstly, then adding a certain ratio of component A; fully mixing and blending the mixture, and curing under a certain condition so as to obtain the organic silicone encapsulation gel. The refractive index of the prepared organic silicone encapsulation gel is 1.5167 to 1.5577, the light transmittance at 450 nm is 95% or more, the thermal decomposition temperature at a nitrogen gas atmosphere can reach 404.63 DEG C, the hardness is 58 to 65, and the adhesive strength is 56.8 MPa.
Description
Technical field
The present invention relates to a kind of high brightness, high-power COB-LED（Chip on Board, chip on board encapsulates）The encapsulation preparation method of high folding transparent organic silicon glue, belongs to the encapsulating material technical field of photoelectric device.
Background technology
The unique chemical constitution of organosilicon material makes it have the characteristic of inorganic matters and Organic substance concurrently, there is the performances such as excellent heat-resisting, weather-proof, durable, low temperature flexibility, UV stable, high water vapor transmittance, it is a kind of new material being related to that technological innovation, the modernization of national defense, the national economic development and living standards of the people improve, be widely used in electric, semiconductor electronic, high light large power LED encapsulation etc..Organosilicon product is because having electric insulation, fire-retardant, radiation hardness, corrosion-resistant, high-low temperature resistant, and the good characteristic such as good biocompatibility, have a wide range of applications in space flight and aviation, military project apparatus, the electric, field such as health care, automobile, building, household chemicalss.In recent years, China's power-type and great power LED have reached international industry bleeding edge, and the epitaxial wafer of LED field and researching and producing of chip are quickly propelling, and but relatively ignore the research to encapsulating material.China's high brightness, high-power COB-LED encapsulation organic silica gel major part need to lean on import at present, expensive, this greatly limits the development further of LED industry.Because of the shortage of domestic funds and technology, product haves such problems as that refractive index is relatively low, transparent deficiency, thermostability be not good, poor mechanical property.
In order to solve the above problems, the present invention designs the transparent phenyl vinyl resin of the high folding of synthesis first（Component A）And phenyl hydrogen-containing silicon oil（B component）, between adjustment monomer, ratio can realize the Modulatory character of refraction index, change synthetic catalyst, control reaction condition etc. can synthesize the component of suitable molecular weight and molecular weight distribution；Then curing catalysts are made using chloroplatinic acid or platinum complex, under mild conditions, 25 ~ 120 C are curable, A, B component refraction index all more than 1.50, very well, catalyst amount is few for the compatibility of two kinds of components, curing reaction high conversion rate, no coupling product generates, internal and surface all energy completion of cures, and shrinkage factor is low（0~0.5%）Resistance to elevated temperatures is especially excellent, heat decomposition temperature reaches 404.63 C, 150 ~ 200 C can life-time service, this packaging plastic has the advantages that refraction index is high, condition of cure is gentle, solidification rate is fast, the transparency good, hardness is suitable, adhesion strength is high, high temperature resistant, ageing-resistant.
Content of the invention
It is an object of the invention to provide the preparation method of a kind of high brightness, high-power COB-LED encapsulation organic silica gel.It is another object of the present invention to preparing a kind of novel organosilicon high-temperature plastic, to improve the heat resistance of current organic silicon packaging glue, realize the Modulatory character of organic silicon packaging glue index of refraction simultaneously.
The present invention relates to a kind of high brightness, the preparation method of high-power COB-LED encapsulation high folding transparent organic silicon glue are it is characterised in that have following technical process and step：
A. the synthesis of phenyl vinyl resin（Component A）One of method：Weigh 8.6 ~ 10.9g 1,3,5,7- tetramethyl -1,3,5,7- tetraphenyl tetrasiloxane ring body (D4), 2.64 ~ 5.28g methylvinyldimethoxysilane, 0.5～2.0g γ-glycidyl ether oxygen propyl trimethoxy silicane (KH-560) be placed in three-necked bottle, add xylene solvent, be warming up to 90 C, add appropriate base catalyst, it is：Tetramethylammonium hydroxide (Me4) or potassium hydroxide NOH（KOH）, or eight hydrated sulfuric acid barium（Ba(OH)2·8H2O）；Temperature is maintained at 90 C ~ 110 C/4h；Vacuum distillation, the solvent in removing system and small-molecule substance；Obtain phenyl vinyl resin；
The synthesis of phenyl vinyl resin（Component A）The two of method：Weigh 8.6 ~ 10.9g 1,3,5,7- tetramethyl -1,3,5,7- tetraphenyl tetrasiloxane ring body (D4), 2.64 ~ 5.28g methylvinyldimethoxysilane, 0.5～2.0g γ-glycidyl ether oxygen propyl trimethoxy silicane (KH-560) be placed in three-necked bottle, add the appropriate dimethylbenzene that again steams as reaction dissolvent, then pass to N2And heat up, when temperature rises to 80 ~ 90 C, instill 0.1 ~ 1.0g DMF（DMF）As accelerator, then instill 0.1 ~ 1.5g Me again4The silicon alkoxide solution catalyst of NOH；Temperature is maintained at 85 ~ 95 C/2h, 96 ~ 105 C/2h, 106 ~ 115 C/2h, is then directly warming up to 150 ~ 180 C, and maintains 1 ~ 2h to make catalyst Me4NOH is decomposed；Then carry out vacuum distillation 3 ~ 5h at this temperature, small-molecule substance after removing the solvent in reaction system and decomposing；Finally obtain phenyl vinyl resin；
B. the synthesis of phenyl hydrogen-containing silicon oil（B component）：3.85 ~ 5.45g D is added in three-necked bottle4, 2.4 ~ 6.4g 1,3,5,7- tetrahydrochysene -1,3,5,7- tetramethyl-ring tetrasiloxane（Hydrogeneous ring body）, using dimethylbenzene with isopropanol as mixed solvent, it is uniformly mixed the dense H of rear Deca 0.1 ~ 2g2SO4Catalyst, is warming up to 50 ~ 60 C, back flow reaction 2 ~ 4h；Plus 0.2 ~ the tetramethyl two hydrogen-based disiloxane of 1.5g（Hydrogeneous double-seal head）, balancing response 3 ~ 5h；After dehydration, vacuum distillation, cooling, filtration, obtain phenyl hydrogen-containing silicon oil；
C. the curing process of high folding transparent organic silicon packaging plastic：Above two material is thoroughly mixed, A, the mass ratio of B component are (1 ~ 5):1, it is subsequently adding a certain amount of catalyst chloroplatinic acid or platinum complex, the ratio of A, B component quality summation and catalyst is：(3~10)：(0.003~0.01)；Or B component is mixed homogeneously with catalyst elder generation and adds a certain proportion of component A afterwards；After being thoroughly mixed uniformly, vacuum distillation aerofluxuss are steeped；After row finishes, cold curing 1 ~ 4h；Or heating 80 ~ 120 C solidification 1min ~ 120min；Finally give high brightness, the high-power COB-LED encapsulation high folding transparent organic silicon glue of solidification.
The mechanism of the inventive method and feature are as described below：
The present invention utilizes 1,3,5,7- tetramethyl -1,3, the open loop of 5,7- tetraphenyl tetrasiloxane ring bodies and methylvinyldimethoxysilane open loop, copolymerization introduce phenyl ring in organic silicon substrate, vinyl has higher refractive index and can carry out additive reaction with containing hydrogen silicone oil to ensure prepared packaging plastic, and preparation is high to roll over transparent, resistant to elevated temperatures phenyl organic silicon packaging glue.The organosilicon solidification temperature that the present invention adopts is fast compared with low rate, between 25 ~ 120 C.Present device is fairly simple, and cost is relatively low, and operating condition is easy to control.The philosophy and technique of the present invention is different from common organic silica gel curing.
Tested through abbe's refractometer, non-isothermal DSC test, ISOTHERMAL DSC test, ultraviolet spectrophotometer, durometer, electronic tension tester, TGA using the high folding transparent organic silicon packaging plastic of the inventive method preparation, 180 C/1000h characterize to its refraction index, condition of cure, solidification rate, the transparency, hardness, adhesion strength, thermostability, the performance such as ageing-resistant respectively.Its refraction index is 1.5167 ~ 1.5577；Can start to solidify in 36.35 C；It is 2min ~ 1min in 100 C ~ 120 C isothermal curing times；Light transmittance at 450nm is higher than 95%；Under room temperature condition, hardness is 58 ~ 65；Adhesion strength is 56.8MPa；Heat decomposition temperature in a nitrogen atmosphere reaches 404.63 C；The burn-in test of 180 C under air atmosphere, 1000h.
Advantages of the present invention is：The regulation and control of organic silicon packaging glue refraction index not only can be realized, the raising of heat resistance, light transmission, adhesion strength etc. can also be realized, be prepared for a kind of superior packaging plastic of combination property.
Specific embodiment
After now the specific embodiment of the present invention being specified in.
Embodiment one
Weigh 8.6g
D4, 2.64g methylvinyldimethoxysilane, 0.85g KH-560 be placed in three-necked bottle, add 30mL xylene solvent, it is warming up to 90 C, add 0.2g Tetramethylammonium hydroxide catalyst, temperature is maintained at 90 C ~ 110 C/4h, vacuum distillation, the solvent in removing system and small-molecule substance etc., obtain phenyl vinyl resin.
3.85gD is added in three-necked bottle4、2.5g
1,3,5,7- tetrahydrochysene -1,3,5,7- tetramethyl-ring tetrasiloxanes, 5mL dimethylbenzene and 20mL isopropanol, as mixed solvent, are uniformly mixed the dense H of rear Deca 0.4g2SO4Catalyst, is warming up to 50 ~ 60 C, back flow reaction 2 ~ 4h.Plus the hydrogeneous double-seal head of 0.3g, balancing response 4h.After dehydration, vacuum distillation, cooling, filtration, obtain phenyl hydrogen-containing silicon oil.
Synthesized 2g phenyl vinyl resin is mixed with 1g phenyl hydrogen-containing silicon oil, with 0.003g chloroplatinic acid as curing catalysts, mix homogeneously excludes bubble under vacuum condition；Or again with phenyl vinyl mixed with resin uniformly, evacuation excludes bubble by after firming agent and phenyl hydrogen-containing silicon oil mix homogeneously.Solidify 0.5h under the conditions of 80 C, solidify 1h under the conditions of 100 °C, that is, obtain based resin organic silica gel.
Organic silicon packaging glue refraction index manufactured in the present embodiment is 1.5167, and the light transmittance at 450nm reaches 95%.
Embodiment two
10.9gD is added first in 250mL three-necked bottle4, 5.28g methylvinyldimethoxysilane, 1.18g KH-560, and add 0.018g Ba (OH)2·8H2O, as catalyst, then measures 20mL toluene as the solvent of reaction with graduated cylinder, is uniformly mixed；To 80 C, flow back warming-in-water 4h, adds 0.28g vinyl double-seal head as the end-capping reagent of reaction, flow back 2h.After reaction terminates cooling, deionized water is washed till neutrality, vacuum distillation obtains colorless transparent viscous liquid after removing solvent and water, instill micro dilute sulfuric acid, after salt being layered with Organic substance with the method for centrifugation, remove supernatant liquid, finally use the politef membrane filtration of 0.45um, as phenyl vinyl resin.
5.45gD is added in three-necked bottle4、4.8g
1,3,5,7- tetrahydrochysene -1,3,5,7- tetramethyl-ring tetrasiloxanes, 5mL steams dimethylbenzene, 20mL isopropanol as solvent again, is uniformly mixed, the dense H of Deca 0.59g2SO4, it is warming up to 50 C, and stirring reaction 2 ~ 3h at this temperature.Plus the hydrogeneous double-seal head of 0.46g, as end-capping reagent, balancing response 3h, adds 10%（Mass fraction）Water continue stirring 0.5h to decompose sulfuric ester, stratification, go sour water layer, oil reservoir be washed to neutrality, then heat decompression and pull out low waste, cooling, be filtrated to get purpose product phenyl hydrogen-containing silicon oil.
Synthesized 3.5g phenyl vinyl resin is mixed with 1.5g phenyl hydrogen-containing silicon oil, with 0.005g chloroplatinic acid as curing catalysts, mix homogeneously excludes bubble under vacuum condition；Or again with phenyl vinyl mixed with resin uniformly, evacuation excludes bubble by after firming agent and phenyl hydrogen-containing silicon oil mix homogeneously.Solidify 2h under the conditions of 80 C, that is, obtain based resin organic silica gel.
Organic silicon packaging glue refraction index manufactured in the present embodiment is 1.5412, and the light transmittance at 450nm reaches 95.5%.
Embodiment three
Take 8.8g
D4, 4.35g methylvinyldimethoxysilane, 0.98g KH-560 be placed in there-necked flask, add 20mL to steam dimethylbenzene as reaction dissolvent again, then pass to N2And heat up, when temperature rises to 90 C, instill 0.2gDMF as accelerator, then instill 0.3g Me again4As polymerisation catalysts, temperature is maintained at 90 C/2h, 100 C/2h, 110 C/2h to the silanol saline solution of NOH, is then directly warming up to 165 C and maintains 1.5h to make catalyst Me4NOH is decomposed, and then carries out vacuum distillation 5h at this temperature, and after removing the solvent in reaction system and decomposing, small-molecule substance etc., finally obtains phenyl vinyl resin.
8.75g D is added in three-necked bottle4, 4.8g 1,3,5,7- tetrahydrochysene -1,3,5,7- tetramethyl-ring tetrasiloxanes, 10mL steams dimethylbenzene, 40mL isopropanol as solvent again, is uniformly mixed, the dense H of Deca 0.59g2SO4, it is warming up to 50 C, and stirring reaction 2 ~ 3 h at this temperature.Plus the hydrogeneous double-seal head of 0.80g is as end-capping reagent, balancing response 3h, stratification, go sour water layer, oil reservoir is washed to neutrality, then heats decompression and pull out low waste, cooling, it is filtrated to get purpose product phenyl hydrogen-containing silicon oil.
Synthesized 7g phenyl vinyl resin is mixed with 3g phenyl hydrogen-containing silicon oil, with 0.01g platinum complex as curing catalysts, mix homogeneously excludes bubble under vacuum condition；Or again with phenyl vinyl mixed with resin uniformly, evacuation excludes bubble by after firming agent and phenyl hydrogen-containing silicon oil mix homogeneously.Solidify 1h under the conditions of 80 C, solidify 1h under the conditions of 100 °C, that is, obtain based resin organic silica gel.
Organic silicon packaging glue refraction index manufactured in the present embodiment is 1.5577, and the light transmittance at 450nm reaches 96%.
Claims (1)
1. a kind of high brightness, the high-power COB-LED encapsulation high folding preparation method of transparent organic silicon glue are it is characterised in that comprising the following steps that of the method：
A. one of synthesis (component A) method of phenyl vinyl resin：Weigh 8.6～10.9g 1,3,5,7- tetramethyl -1,3,5,7- tetraphenyl tetrasiloxane ring body, 2.64～5.28g methylvinyldimethoxysilane, 0.5～2.0g γ-glycidyl ether oxygen propyl trimethoxy silicane (KH-560) is placed in three-necked bottle, adds xylene solvent, is warming up to 90 DEG C, add appropriate base catalyst, it is：Tetramethylammonium hydroxide (Me4) or potassium hydroxide (KOH) or barium hydroxide octahydrate (Ba (OH) NOH2·8H2O)；Temperature is maintained at 90 DEG C～110 DEG C/4h；Vacuum distillation, the solvent in removing system and small-molecule substance；Obtain phenyl vinyl resin；The two of synthesis (component A) method of phenyl vinyl resin：Weigh 8.6～10.9g 1,3,5,7- tetramethyl -1,3,5,7- tetraphenyl tetrasiloxane ring bodies, 2.64～5.28g methylvinyldimethoxysilane, 0.5～2.0g γ-glycidyl ether oxygen propyl trimethoxy silicane (KH-560) is placed in three-necked bottle, add the appropriate dimethylbenzene that again steams as reaction dissolvent, then pass to N2And heat up, when temperature rises to 80～90 DEG C, instill 0.1～1.0gN, dinethylformamide (DMF), as accelerator, then instills 0.1～1.5gMe again4The silicon alkoxide solution catalyst of NOH；Temperature is maintained at 85～95 DEG C/2h, 96～105 DEG C/2h, 106～115 DEG C/2h, is then directly warming up to 150～180 DEG C, and maintains 1～2h to make catalyst Me4NOH is decomposed；Then carry out vacuum distillation 3～5h at this temperature, small-molecule substance after removing the solvent in reaction system and decomposing；Finally obtain phenyl vinyl resin；
B. the synthesis (B component) of phenyl hydrogen-containing silicon oil：Addition 3.85～5.45g1 in three-necked bottle, 3,5,7- tetramethyl -1,3,5,7- tetraphenyl tetrasiloxane ring bodies, 2.4～6.4g 1,3,5,7- tetrahydrochysene -1,3,5,7- tetramethyl-ring tetrasiloxanes, using dimethylbenzene with isopropanol as mixed solvent, are uniformly mixed the dense H of rear Deca 0.1～2g2SO4Catalyst, is warming up to 50～60 DEG C, back flow reaction 2～4h；Plus 0.2～the tetramethyl two hydrogen-based disiloxane of 1.5g, balancing response 3～5h；After dehydration, vacuum distillation, cooling, filtration, obtain phenyl hydrogen-containing silicon oil；
C. the curing process of high folding transparent organic silicon packaging plastic：Above two component A and B component are thoroughly mixed, A, the mass ratio of B component are (1～5):1, it is subsequently adding a certain amount of catalyst chloroplatinic acid or platinum complex, the ratio of A, B component quality summation and catalyst is：(3～10)：(0.003～0.01)；Or B component is mixed homogeneously with catalyst elder generation and adds a certain proportion of component A afterwards, after being thoroughly mixed uniformly, vacuum distillation aerofluxuss are steeped, after row finishes, cold curing 1～4h；Or 80～120 DEG C of solidification 1min～120min of heating, finally give high brightness, the high-power COB-LED encapsulation high folding transparent organic silicon glue of solidification.
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| CN104212408B (en) * | 2014-08-15 | 2016-04-06 | 华中师范大学 | Filling glue of a kind of phenyl system high refractive index LED and preparation method thereof |
| CN104327273A (en) * | 2014-10-22 | 2015-02-04 | 上海大学 | Organic silicon potting adhesive containing POSS group and preparation method of organic silicon potting adhesive |
| CN105085826A (en) * | 2015-08-16 | 2015-11-25 | 朱志 | Metallic silicon powder mixed high-performance organic silicon resin-polymethyl methacrylate composite for LED packaging and preparation method thereof |
| CN110194946B (en) * | 2019-05-16 | 2021-10-12 | 上海大学 | Organic silicon packaging adhesive and preparation method thereof |
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