CN105176485A - Preparation method of LED organosilicone packaging silica gel having high heat conductivity coefficient - Google Patents
Preparation method of LED organosilicone packaging silica gel having high heat conductivity coefficient Download PDFInfo
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- CN105176485A CN105176485A CN201510718452.8A CN201510718452A CN105176485A CN 105176485 A CN105176485 A CN 105176485A CN 201510718452 A CN201510718452 A CN 201510718452A CN 105176485 A CN105176485 A CN 105176485A
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Abstract
The invention provides a preparation method of LED organosilicone packaging silica gel having high heat conductivity coefficient. The preparation method comprises the steps that 1, nano quartz surface treatment is performed, namely 100 parts by mass of nano quartz, 100 parts by mass of methyl vinyl silicon oil and 10-20 parts by mass of silane coupling agent are added into a vacuum kneading machine, are kneaded at the 140-150 DEG C temperature at the rotating speed of 30-50 r/min for 3-4 hours and then are cooled, dried and stored to obtain base gel A; 2, the organosilicone packaging silica gel is prepared, namely 100 parts by mass of methyl vinyl silicon oil, 1-10 parts by mass of base gel A, 50 parts by mass of methyl hydrogen silicone oil, 0.1-0.2 part by mass of catalyst platinum-vinyl silicone oil complex and 0.2-0.4 part by mass of inhibitor ethynol are subjected to full vacuum stirring and even mixing to prepare the organosilicone packaging silica gel. The heat conductivity of the packaging silica gel prepared by means of the preparation method can be improved by 6-38%, luminous flux can be improved by 5-20%, and luminous attenuation can be reduced by 5-10%.
Description
Technical field
The present invention relates to a kind of preparation method of LED organosilicon packaging silicon rubber of high thermal conductivity coefficient, belong to optical package technical field.
Background technology
The efficiency of electric energy conversion luminous energy is higher more greatly, then for the optical throughput that LED light source unit electric power sends, and namely light efficiency is higher.At present, have 40% to be used for luminescence in the energy consumption of LED, the energy consumption of 60% is scattered and disappeared with the form of heat, if these thermal lossess can not distribute the performance that can have a strong impact on packaged material timely, main manifestations is, easy aging, poor heat resistance, easy to crack etc., have impact on the life-span of LED component.Traditional heat-removal modalities is, by the aluminium base at back, heat is passed to away reduction working temperature, the shortcoming of this method is, because the thermal conductivity of organic silicon packaging glue is lower, so the temperature on packaging plastic surface can not be effectively reduced, fundamentally do not solve the heat dissipation problem of packaging plastic.
Patent of invention CN200810203983.3 describes a kind of encapsulation glue, and take nano zine oxide as heat conductive filler, its curing mode is dealcoholizing-type, has small molecules to generate in the curing process, and construction process exists the resistance to air loss affecting glue.What the present invention adopted is nanometer quartzite is heat conductive filler, and curing mode is Si―H addition reaction type, produces in solidification process without small molecules.
Summary of the invention
LED organosilicon packaging silicon rubber of high thermal conductivity coefficient provided by the invention and preparation method thereof, comprise a kind for the treatment of process of nanometer quartzite surface, another object prepares a kind of organic silicon packaging glue, to improve the lower heat conductivility of current organic silicon packaging glue, improves refractive index optical throughput simultaneously.
The preparation method of the LED organosilicon packaging silicon rubber of a kind of high thermal conductivity coefficient of the present invention, has following technological process and step:
1) surface treatment of nanometer quartzite: by mass parts, 100 parts of nanometer quartzites (particle diameter 50-100nm), 100 parts of methyl vinyl silicon oils, 10-20 part silane coupling agent, joins in vacuum kneader, at 140 ~ 150 DEG C of temperature, mediate 3-4 hour, rotating speed is 30-50r/min, then cool, kept dry, as base glue A;
Wherein silane coupling agent is any one in γ-glycidoxypropyltrime,hoxysilane, vinyltrimethoxy silane, vinyltriethoxysilane;
2) preparation of organosilicon packaging silicon rubber: by mass parts, 100 parts of methyl vinyl silicon oils, 1-10 part base glue A, 50 parts of Methyl Hydrogen Polysiloxane Fluids, 0.1-0.2 part catalyst platinum-vinyl silicone oil complex compound, platinum content 3000-5000ppm, 0.2-0.4 part inhibitor acetylene alcohol, after abundant vacuum stirring mixes, obtain organic silicon packaging glue.With pneumatic point gum machine by packaging plastic point on lamp pearl, by lamp pearl as toasting h solidification under 1-2 in 150 DEG C of baking ovens.
In said process 1,2, methyl vinyl silicon oil is, end ethene silicone oil, its viscosity is: 1000-5000mpa.s.In said process 2, Methyl Hydrogen Polysiloxane Fluid structural formula is as follows:
Mechanism of the present invention and feature as described below: the high thermal conductivity of nanometer silica powder significantly can improve the heat conductivility of packaging plastic, and simultaneously high refractive index can also improve the refractive index of packaging plastic thus reach better light efficiency.Surface treatment mode of the present invention is different from nano material and is with an organic solvent carrying out the direct process of silane coupling agent as medium, the present invention in treating processes without the need for machine solvent, adopt vinyl silicone oil as medium, in kneading process, make silane coupling agent and nanometer quartzite produce chemical reaction reach surface-treated result, nanometer quartzite can be made well to be dispersed in vinyl silicone oil simultaneously, be prepared into base glue and facilitate follow-up adding, avoid the secondary of nano particle to add.Involved in the present invention to the curing mode of packaging plastic be addition reaction of silicon with hydrogen, produce without small molecules in solidify reaction process, belong to environmentally friendly.Present device is comparatively simple, and cost is lower, and operational condition is easy to control.
The LED organosilicon packaging silicon rubber of high thermal conductivity coefficient adopting the inventive method to prepare is through thermal conductivity tester and Abbe refractometer respectively to its thermal conductivity, and its thermal conductivity can improve 6 ~ 38%; The LED organosilicon packaging silicon rubber of the high thermal conductivity coefficient adopting the inventive method to prepare is packaged into lamp pearl, and have its light efficiency of integrating sphere measurement, its optical throughput can improve 5-20%, and finished product lamp pearl has carried out lighting light decay experiment for a long time, its light decay decline 5-10% at led ageing device
Embodiment
Embodiment 1
1) 100g nanometer quartzite, the methyl vinyl silicon oil viscosity of 100g is the vinyltriethoxysilane of 1000mpa.s, 10g, joins in vacuum kneader, at 140 DEG C of temperature, mediate 3h, and rotating speed is 30r/min; Then cool, kept dry, as base glue 1.
2) the methyl vinyl silicon oil silicon oil viscosity of 100g is the Methyl Hydrogen Polysiloxane Fluid n=8 of the base glue 1,50g of 5000mpa.s, 1g, 0.1g catalyst platinum-vinyl silicone oil complex compound platinum content 3000ppm, the acetylene alcohol of 0.2g, after abundant vacuum stirring mixes, obtains organic silicon packaging glue.With pneumatic point gum machine by packaging plastic point on lamp pearl, by lamp pearl as toast in 150 DEG C of baking ovens 1h solidification.
Embodiment 2
1) 100g nanometer quartzite, 100g methyl vinyl silicon oil, viscosity is 5000mpa.s; 10g vinyltrimethoxy silane, joins in vacuum kneader, at 150 DEG C of temperature, mediate 4h, and rotating speed is 40r/min; Then cool, kept dry, as base glue 2.
2) methyl vinyl silicon oil of 100g, its viscosity is the base glue 2 of 3000mpa.s, 5g, the Methyl Hydrogen Polysiloxane Fluid n=8 of 50g, 0.15g catalyst platinum-vinyl silicone oil complex compound platinum content 4000ppm, the acetylene alcohol of 0.3g, after abundant vacuum stirring mixes, obtain organic silicon packaging glue.With pneumatic point gum machine by packaging plastic point on lamp pearl, by lamp pearl as toast in 150 DEG C of baking ovens 2h solidification.
Embodiment 3
1) 100g nanometer quartzite, the methyl vinyl silicon oil viscosity of 100g is the γ-glycidoxypropyltrime,hoxysilane of 3000mpa.s, 10g, joins in vacuum kneader, at 150 DEG C of temperature, mediates 4h, and rotating speed is 40r/min; Then cool, kept dry, as base glue 3.
2) methyl vinyl silicon oil of 100g, its viscosity is the base glue 3 of 5000mpa.s, 10g, the Methyl Hydrogen Polysiloxane Fluid n=10 of 50g, 0.2g catalyst platinum-vinyl silicone oil complex compound platinum content 5000ppm, the acetylene alcohol of 0.4g, after abundant vacuum stirring mixes, obtain organic silicon packaging glue.With pneumatic point gum machine by packaging plastic point on lamp pearl, by lamp pearl as toast in 150 DEG C of baking ovens 2h solidification.
Comparative example
Comparative example is by the proportioning in embodiment 1, does not add the comparative example that base glue 1 draws.
The test result of embodiment 1-3 sees the following form:
| Thermal conductivity (W/mk) | Initial luminous flux (lm) | Aging rear optical throughput (lm) | |
| Comparative example | 0.2 | 20.8 | 18.5 |
| Embodiment 1 | 0.21 | 22.2 | 21.9 |
| Embodiment 2 | 0.25 | 24.3 | 24.2 |
| Embodiment 3 | 0.3 | 25.8 | 25.4 |
Above-mentioned experimental result shows, the thermal conductivity that with the addition of the packaging plastic of nanometer silica powder improves 5%-50%, and the thermal diffusivity of packaging plastic improves greatly; Optical throughput is also improve 6.7%-24% by the high refractive index of nanometer silica powder; Do not add the lamp pearl of the filament glue of nanometer silica powder after lighting for a long time through 1000h, optical throughput conservation rate only has 88%, and the optical throughput conservation rate in embodiment is more than 98%, thus extends the work-ing life of lamp pearl.
Claims (6)
1. a preparation method for the LED organosilicon packaging silicon rubber of high thermal conductivity coefficient, it is characterized in that, step comprises:
1) surface treatment of nanometer quartzite: by mass parts, 100 parts of nanometer quartzites, 100 parts of methyl vinyl silicon oils, 10-20 part silane coupling agent, joins in vacuum kneader, at 140 ~ 150 DEG C of temperature, mediate 3-4 hour, rotating speed is 30-50r/min, then cool, kept dry, as base glue A;
2) preparation of organosilicon packaging silicon rubber: by mass parts, 100 parts of methyl vinyl silicon oils, 1-10 part base glue A, 50 parts of Methyl Hydrogen Polysiloxane Fluids, 0.1-0.2 part catalyst platinum-vinyl silicone oil complex compound, 0.2-0.4 part inhibitor acetylene alcohol, after abundant vacuum stirring mixes, obtains organic silicon packaging glue.
2. preparation method according to claim 1, is characterized in that, described silane coupling agent is any one in γ-glycidoxypropyltrime,hoxysilane, vinyltrimethoxy silane, vinyltriethoxysilane.
3. preparation method according to claim 1, is characterized in that, the particle diameter of described nanometer quartzite is 50-100nm.
4. preparation method according to claim 1, is characterized in that, described methyl vinyl silicon oil is end ethene silicone oil, and viscosity is 1000-5000mpa.s.
5. preparation method according to claim 1, is characterized in that, described Methyl Hydrogen Polysiloxane Fluid structural formula is as follows:
Wherein n=5-10.
6. preparation method according to claim 1, is characterized in that, in described catalyst platinum-vinyl silicone oil complex compound, platinum content is 3000-5000ppm.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102876282A (en) * | 2012-09-13 | 2013-01-16 | 上海大学 | Preparation method of transparent organic silica glue for encapsulating nano SiO2 modified COB-LEDs |
| CN102952403A (en) * | 2011-08-30 | 2013-03-06 | 上海尤耐有机硅材料有限公司 | Additive organosilicon heat-conducting electronic potting adhesive and manufacturing method thereof |
-
2015
- 2015-10-29 CN CN201510718452.8A patent/CN105176485A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102952403A (en) * | 2011-08-30 | 2013-03-06 | 上海尤耐有机硅材料有限公司 | Additive organosilicon heat-conducting electronic potting adhesive and manufacturing method thereof |
| CN102876282A (en) * | 2012-09-13 | 2013-01-16 | 上海大学 | Preparation method of transparent organic silica glue for encapsulating nano SiO2 modified COB-LEDs |
Non-Patent Citations (1)
| Title |
|---|
| 李广宇等: "《胶黏剂原材料手册》", 31 August 2004, 国防工业出版社 * |
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