CN102876282A - Preparation method of transparent organic silica glue for encapsulating nano SiO2 modified COB-LEDs - Google Patents
Preparation method of transparent organic silica glue for encapsulating nano SiO2 modified COB-LEDs Download PDFInfo
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- CN102876282A CN102876282A CN2012103374002A CN201210337400A CN102876282A CN 102876282 A CN102876282 A CN 102876282A CN 2012103374002 A CN2012103374002 A CN 2012103374002A CN 201210337400 A CN201210337400 A CN 201210337400A CN 102876282 A CN102876282 A CN 102876282A
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- nanometer sio
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Abstract
The invention relates to a preparation method of transparent organic silica glue for encapsulating nano SiO2 modified COB-LEDs. The method comprises the specific steps as follows: firstly, preparing surface treating agents (silane coupling agent solution) with certain concentration; adopting silane coupling agents to modify nano SiO2; and then, adding the modified nano SiO2 to the organic silica glue so as to obtain the organic silica packaging glue. The mass ratio of nano Si02 to the organic silica glue is (6.00 to 20.00) to 100. After being stirred for mixing the nano SiO2 and the organic silica glue, a small amount of curing agents and catalytic agents are added for evenly stirring and mixing so as to prepare the nano Si02 modified organic silica packaging glue. According to the invention, the thermal conductivity of the organic silica packaging glue prepared by the method can be improved by 5 to 23%, the refractive index can be improved by 0.1 to 3.3%, and the glue has good shaping performance. Compared with the traditional LED packaging, the cost can be reduced by about 30%. The glue is colourless and transparent, and can be widely used for fixing electron components, sealing electronic housings and plane light sources, and encapsulating various lamps.
Description
Technical field
The present invention relates to a kind of nanometer SiO
2The COB-LED(Chip on Board of modification, the chip on board encapsulation) the embedding preparation method of transparent organic silicon glue, belong to COB-LED light source mother plate packaging plastic technical field.
Background technology
Semiconductor LED is because having the characteristics such as long, energy-efficient, environmental protection of life-span aspect the illumination, LED substitutes the traditional lighting light source as the novel illumination light source and has sizable potentiality, is one of effective way that solves present energy dilemma.Constantly perfect along with the power type white light LED manufacturing technology, its luminous efficiency, brightness and power all are improved largely.Therefore, the LED packaged material begins to face huge challenge, prepares to have high refractive index high anti-ultraviolet ability and heat-proof aging ability, low-stress, the packaged material of high heat conductance, the optical output power and the work-ing life that are expected to improve illuminating device.Data show, led light source is than incandescent light economize on electricity 87%, than luminescent lamp economize on electricity 50%, and the life-span is longer 20～30 times than incandescent light, grow 10 times than luminescent lamp.Led light source because of have energy-saving and environmental protection, long lifetime, safety, response is fast, volume is little, rich color, a series of distinct advantages such as controlled, the best of falling energy consumption that is considered to economize on electricity realizes approach.The COB encapsulation is a kind of chip directly placed technology, is that bare chip is directly sticked on the printed circuit board (PCB), then carries out Bonding, with organic gel chip and lead-in wire is sealed the technique of protection again.The COB-LED light source has the advantages such as high-level efficiency, low-loss, long lifetime, photochromic pure, vibration resistance, fast response time.When the LED area source adopts the COB explained hereafter, abandoned the through metal encapsulation mode of straw hat pipe and SMD lamp pearl, can be directly with chip attachment on the splendid metal substrate of heat conductivility, radiating efficiency improves tens times than lamp pearl formula led light source, with the light decay of decrease led light source, effectively guarantee the work-ing life of LED light fixture.The LED area source is whole encapsulation, and advanced technique will perfectly solve the problem of LED lamp pearl coloured light inequality, whole bright dipping, and the equal light effect of illumination is good, is the only choosing that following interior lighting is used energy-conserving light source.
In general, the packaged material of LED has following several: Resins, epoxy, 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 in 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 Resins, epoxy of the aspects such as heat-resisting, anti-UV and brightness decay, and and Resins, epoxy is in conjunction with getting better without the interface problem, relatively be suitable for use in white light and some the low encapsulation that requires that decays (such as display screen, wiring board, terminal box etc.), but weak point is to be not suitable for being used in greater than on the high power products more than the 0.5W, and price is relatively also comparatively expensive.Silica gel relatively the above two, in anti-UV, heat-resisting and brightness decay larger advantage is arranged, be particularly suitable for being used on the low decay of heavy-power LED product and part and the white light product, but it is relatively poor that shortcoming is bonding force, easily produce interface problem with the epoxy combination, easily moisture absorption, dirt resistance is relatively poor.
Under hot environment, packaged material may cause carbonization, forms the brown tectum at device surface, causes component failure.This research is compound with polymkeric substance and inorganic nano-particle, can make matrix material both have easy processing and the shock resistance of polymkeric substance, has again the characteristics such as the high heat conduction of inorganic materials and rub resistance.Add heat-resisting additive in the polysiloxane product and be a kind of not only practical but also easy method, nano silicon is to use the most general a kind of filler in the colourless Organosilicon Polymers system.The present invention adopts nano silicon to make filler, and organic silica gel has been played thickening, thixotroping, reinforcement, increase physical strength, reaches simultaneously high gloss, high transparent, high-ductility moulding texts.This sizing agent has excellent high-low temperature resistant, ageing-resistant, transparency is high, good moldability, the advantages such as condition of cure gentleness.
Summary of the invention
Defective for prior art exists the object of the present invention is to provide a kind of nanometer SiO
2The COB-LED embedding of modification finally obtains the nanometer SiO that solidifies with the preparation method of organic silica gel
2The high brightness of modification, high-power COB-LED organic silicon packaging glue.
For achieving the above object, the present invention adopts following technical scheme:
A kind of nanometer SiO
2The COB-LED embedding of the modification preparation method of transparent organic silicon glue, concrete steps are as follows:
A. the preparation of surface treatment agent solution: with a certain amount of surface treatment agent, be that silane coupling agent is dissolved in an amount of organic solvent, surface treatment agent is any in γ-glycidoxypropyltrime,hoxysilane, γ aminopropyltriethoxy silane, vinyltrimethoxy silane, the vinyltriethoxysilane; Organic solvent is any in toluene, benzene, the ethanol, and its volume ratio is 1:(1.0～10.0);
B. nanometer SiO
2Modification: with a certain amount of nanometer SiO
2Mix with above-mentioned surface treatment agent solution; Nanometer SiO
2With surface treatment agent be that the quality proportioning of silane coupling agent is 100: (0.01～1.00); Under constantly stirring under 110～130 ℃ of temperature reflux 3～6 h; Then cooling, and dry in baking oven, to vapor away remaining small molecule organic compound;
C. the preparation of modified organic silicon glue: with above-mentioned a certain amount of nanometer SiO through modification
2Be added in a certain amount of organic silica gel; Nanometer SiO
2Add-on and described organic silica gel mass ratio between the two be (6.00～20.00): 100; Organic silica gel is α, alpha, omega-dihydroxy polydimethyl siloxane, α, any in the alpha, omega-dihydroxy polydimethyl hexichol siloxanes; Fully mix, make nanometer SiO
2The organic silicon packaging glue of modification;
D. nanometer SiO
2The curing process of the organic silicon packaging glue of modification: the nanometer SiO that is making
2Add a certain amount of solidifying agent methyl 3 third (fourth) ketoximinosilanes and vinyl 3 third (fourth) ketoximinosilanes in the organic silicon packaging glue of modification, and a certain amount of catalyzer dibutyl tin laurate; The add-on of described solidifying agent and catalyzer is benchmark by the quality of organic silica gel; The mass ratio of solidifying agent and organic silica gel is (3～6): 100; The mass ratio of catalyzer and organic silica gel is (0.2～0.6): 100; After fully mixing, underpressure distillation exhaust bubble, behind the drained bubble, self-vulcanizing 8～20 h; Perhaps be heated to 110～150 ℃ and solidify 30～60 min, finally obtain the nanometer SiO that solidifies
2The COB-LED embedding organic silicon packaging glue of modification.
Compared with prior art, the mechanism of the inventive method and characteristics are as described below:
The present invention utilizes nanometer SiO
2High thermal conductivity and the high refractive index performance of improving organic silicon packaging glue.Through the nanometer SiO after the silane coupling agent surface treatment
2Surface coverage one deck organism so that nanometer SiO
2And have better consistency between the organosilicon, and be conducive to nanometer SiO
2Dispersion in the organic silica gel matrix.Nanometer SiO
2Be dispersed in the rear heat conduction network that forms in the organic silica gel matrix, can improve the heat conductivility of organic silica gel.Simultaneously, by changing nanometer SiO
2Consumption can realize within the specific limits the regulation and control of organic silica gel refractive index.The present invention adopts silane coupler modified nanometer SiO
2The method of silica filled organopolysiloxane glue has overcome common SiO
2Though can improve the thermal conductivity of packaged material, loading level is large, the poor shortcoming of packaging plastic consistency, is difficult to realize the deficiency of thermal conductivity and the dual regulation and control of refractive index.The organosilicon solidification value that the present invention adopts is lower, between 25 ℃～140 ℃.Present device is fairly simple, and cost is lower, and operational condition is easy to control.Philosophy and technique of the present invention is different from common SiO
2The method of direct silica filled organopolysiloxane glue.
Adopt the nanometer SiO of the inventive method preparation
2The organosilicon of modification is thrown mirror glue and respectively its thermal conductivity and refractive index is characterized through thermal conductivity tester and Abbe refractometer, and its thermal conductivity can improve 5～23%, and refractive index can improve 0.1～3.3%.
The present invention not only can realize the improvement of organosilicon lens glue thermal conductivity, can also realize the control of organic silica gel formability.
Embodiment
After now specific embodiments of the invention being specified in.
Embodiment 1:
Get γ aminopropyltriethoxy silane 0.01g under the normal temperature and be dissolved in a certain amount of toluene, add nanometer SiO
2100g, 110 ℃ of 4 h that reflux under agitation, cooling is placed on and vapors away remaining organic molecule in the baking oven, obtains the nanometer SiO of modification
2
The nanometer SiO of modification learnt from else's experience
20.24g, α, alpha, omega-dihydroxy polydimethyl siloxane 100g, after both are fully mixed, add catalyzer dibutyl tin laurate 0.4g, solidifying agent methyl tributanoximo silane 2.86g and vinyl tributyl ketoximyl silane 1.14g after mixing pour into sample self-vulcanizing in the mould.
The thermal conductivity ratio of the organosilicon lens glue of the present embodiment preparation is not filled nanometer SiO
2The organosilicon lens glue that directly solidifies improves 5.8%, and its refractive index is than not filling nanometer SiO
2The organosilicon lens glue improve 0.1%, the constancy of glue is good.
Embodiment 2:
Get γ aminopropyltriethoxy silane 0.01g under the normal temperature and be dissolved in a certain amount of toluene, add nanometer SiO
2100g, 110 ℃ of 4 h that reflux under agitation, cooling is placed on and vapors away remaining organic molecule in the baking oven, obtains the nanometer SiO of modification
2
The nanometer SiO of modification learnt from else's experience
24.00g, α, alpha, omega-dihydroxy polydimethyl siloxane 100g, after both are fully mixed, add catalyzer dibutyl tin laurate 0.4g, solidifying agent methyl tributanoximo silane 2.86g and vinyl tributyl ketoximyl silane 1.14g after mixing pour into sample self-vulcanizing in the mould.
The thermal conductivity ratio of the organosilicon lens glue of the present embodiment preparation is not filled nanometer SiO
2The organosilicon lens glue that directly solidifies improves 10.4%, and its refractive index is than not filling nanometer SiO
2The organosilicon lens glue improve 2.1%, the constancy of glue is good.
Embodiment 3:
Get γ aminopropyltriethoxy silane 0.01g under the normal temperature and be dissolved in a certain amount of toluene, add nanometer SiO
2100g, 110 ℃ of 3 h that reflux under agitation, cooling is placed on and vapors away remaining organic molecule in the baking oven, obtains the nanometer SiO of modification
2
The nanometer SiO of modification learnt from else's experience
215.0g, α, alpha, omega-dihydroxy polydimethyl siloxane 100g, after both are fully mixed, add catalyzer dibutyl tin laurate 0.4g, solidifying agent methyl tributanoximo silane 2.86g and vinyl tributyl ketoximyl silane 1.14g after mixing pour into sample self-vulcanizing in the mould.
The thermal conductivity ratio of the organosilicon lens glue of the present embodiment preparation is not filled nanometer SiO
2The organosilicon lens glue that directly solidifies improves 19.5%, and its refractive index is than not filling nanometer SiO
2The organosilicon lens glue improve 2.9%, the constancy of glue is good.
Claims (1)
1. nanometer SiO
2The COB-LED embedding of the modification preparation method of transparent organic silicon glue is characterized in that, the concrete steps of the method are as follows:
A. the preparation of surface treatment agent solution: with a certain amount of surface treatment agent, be that silane coupling agent is dissolved in an amount of organic solvent, surface treatment agent is any in γ-glycidoxypropyltrime,hoxysilane, γ aminopropyltriethoxy silane, vinyltrimethoxy silane, the vinyltriethoxysilane; Organic solvent is any in toluene, benzene, the ethanol, and its volume ratio is 1:(1.0～10.0);
B. nanometer SiO
2Modification: with a certain amount of nanometer SiO
2Mix with above-mentioned surface treatment agent solution; Nanometer SiO
2With surface treatment agent be that the quality proportioning of silane coupling agent is 100: (0.01～1.00); Under constantly stirring under 110～130 ℃ of temperature reflux 3～6 h; Then cooling, and dry in baking oven, to vapor away remaining small molecule organic compound;
C. the preparation of modified organic silicon glue: with above-mentioned a certain amount of nanometer SiO through modification
2Be added in a certain amount of organic silica gel; Nanometer SiO
2Add-on and described organic silica gel mass ratio between the two be (6.00～20.00): 100; Organic silica gel is α, alpha, omega-dihydroxy polydimethyl siloxane, α, any in the alpha, omega-dihydroxy polydimethyl hexichol siloxanes; Fully mix, make nanometer SiO
2The organic silicon packaging glue of modification;
D. nanometer SiO
2The curing process of the organic silicon packaging glue of modification: the nanometer SiO that is making
2Add a certain amount of solidifying agent methyl 3 third (fourth) ketoximinosilanes and vinyl 3 third (fourth) ketoximinosilanes in the organic silicon packaging glue of modification, and a certain amount of catalyzer dibutyl tin laurate; The add-on of described solidifying agent and catalyzer is benchmark by the quality of organic silica gel; The mass ratio of solidifying agent and organic silica gel is (3～6): 100; The mass ratio of catalyzer and organic silica gel is (0.2～0.6): 100; After fully mixing, underpressure distillation exhaust bubble, behind the drained bubble, self-vulcanizing 8～20 h; Perhaps be heated to 110～150 ℃ and solidify 30～60 min, finally obtain the nanometer SiO that solidifies
2The COB-LED embedding organic silicon packaging glue of modification.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103122237A (en) * | 2013-02-20 | 2013-05-29 | 昆山宏凌电子有限公司 | Heat-conducting glue and preparation method thereof |
| CN103497760A (en) * | 2013-09-18 | 2014-01-08 | 深圳市晨日科技有限公司 | Anti-phosphor deposition high thixotropic LED (light-emitting diode) jelly glue |
| CN104073215A (en) * | 2014-06-30 | 2014-10-01 | 江苏华程光电科技有限公司 | Preparation method for nano silicon dioxide modified organic silicon sealant for packaging of light emitting diode (LED) |
| CN105176485A (en) * | 2015-10-29 | 2015-12-23 | 烟台德邦先进硅材料有限公司 | Preparation method of LED organosilicone packaging silica gel having high heat conductivity coefficient |
| CN105322072A (en) * | 2014-07-30 | 2016-02-10 | 高玉宇 | Fluorescent composite resin substrate white light light-emitting diode device and manufacture method thereof |
| CN105400470A (en) * | 2015-12-01 | 2016-03-16 | 杭州新湖电子有限公司 | Packaging adhesive for LED white-light nixie tube and preparation method of packaging adhesive |
| CN105895788A (en) * | 2014-05-08 | 2016-08-24 | 罗冠杰 | Sheet type white light emitting diode, method for preparing sheet type white light emitting diode and packaging adhesive material |
| CN107502000A (en) * | 2017-07-28 | 2017-12-22 | 北京航天控制仪器研究所 | A kind of silicon powder of surface chemical modification and preparation method and application |
| CN107793944A (en) * | 2017-11-06 | 2018-03-13 | 张永宏 | A kind of organic silica gel static-free glue band |
| CN111732932A (en) * | 2020-07-02 | 2020-10-02 | 深圳市新纶科技股份有限公司 | Organic silicon material and preparation method and application thereof |
| CN114133915A (en) * | 2021-11-26 | 2022-03-04 | 北京通美晶体技术股份有限公司 | Abrasive for polishing solution, polishing solution for fine polishing of indium phosphide crystals and preparation method of polishing solution |
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Cited By (16)
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| CN103122237A (en) * | 2013-02-20 | 2013-05-29 | 昆山宏凌电子有限公司 | Heat-conducting glue and preparation method thereof |
| CN103497760A (en) * | 2013-09-18 | 2014-01-08 | 深圳市晨日科技有限公司 | Anti-phosphor deposition high thixotropic LED (light-emitting diode) jelly glue |
| CN103497760B (en) * | 2013-09-18 | 2015-04-22 | 深圳市晨日科技有限公司 | Anti-phosphor deposition high thixotropic LED (light-emitting diode) jelly glue |
| CN105895788A (en) * | 2014-05-08 | 2016-08-24 | 罗冠杰 | Sheet type white light emitting diode, method for preparing sheet type white light emitting diode and packaging adhesive material |
| CN104073215A (en) * | 2014-06-30 | 2014-10-01 | 江苏华程光电科技有限公司 | Preparation method for nano silicon dioxide modified organic silicon sealant for packaging of light emitting diode (LED) |
| CN105322072B (en) * | 2014-07-30 | 2019-08-06 | 盛汉有限公司 | Fluorescent compound resin substrate white-light emitting second level pipe device and its manufacturing method |
| CN105322072A (en) * | 2014-07-30 | 2016-02-10 | 高玉宇 | Fluorescent composite resin substrate white light light-emitting diode device and manufacture method thereof |
| CN105176485A (en) * | 2015-10-29 | 2015-12-23 | 烟台德邦先进硅材料有限公司 | Preparation method of LED organosilicone packaging silica gel having high heat conductivity coefficient |
| CN105400470A (en) * | 2015-12-01 | 2016-03-16 | 杭州新湖电子有限公司 | Packaging adhesive for LED white-light nixie tube and preparation method of packaging adhesive |
| CN105400470B (en) * | 2015-12-01 | 2018-03-09 | 杭州新湖电子有限公司 | A kind of LED white-light nixie tubes packaging plastic and preparation method thereof |
| CN107502000A (en) * | 2017-07-28 | 2017-12-22 | 北京航天控制仪器研究所 | A kind of silicon powder of surface chemical modification and preparation method and application |
| CN107502000B (en) * | 2017-07-28 | 2019-09-06 | 北京航天控制仪器研究所 | A kind of silicon powder of surface chemical modification and the preparation method and application thereof |
| CN107793944A (en) * | 2017-11-06 | 2018-03-13 | 张永宏 | A kind of organic silica gel static-free glue band |
| CN111732932A (en) * | 2020-07-02 | 2020-10-02 | 深圳市新纶科技股份有限公司 | Organic silicon material and preparation method and application thereof |
| CN114133915A (en) * | 2021-11-26 | 2022-03-04 | 北京通美晶体技术股份有限公司 | Abrasive for polishing solution, polishing solution for fine polishing of indium phosphide crystals and preparation method of polishing solution |
| CN114133915B (en) * | 2021-11-26 | 2023-01-06 | 北京通美晶体技术股份有限公司 | Abrasive for polishing solution, polishing solution for fine polishing of indium phosphide crystal and preparation method of polishing solution |
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Application publication date: 20130116 |