CN101787255B - Preparation method of light-emitting diode insulation crystal-bonding adhesive - Google Patents

Preparation method of light-emitting diode insulation crystal-bonding adhesive Download PDF

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Publication number
CN101787255B
CN101787255B CN2009102337042A CN200910233704A CN101787255B CN 101787255 B CN101787255 B CN 101787255B CN 2009102337042 A CN2009102337042 A CN 2009102337042A CN 200910233704 A CN200910233704 A CN 200910233704A CN 101787255 B CN101787255 B CN 101787255B
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bonding adhesive
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percentage composition
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CN101787255A (en
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胡建红
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Jiangsu Wenrun Optoelectronic Co Ltd
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Joint Venture Jiangsu Wenrun Optoelectronics Co Ltd
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Abstract

The invention discloses a preparation method of light-emitting diode (LED) insulation crystal-bonding adhesive. The raw materials comprise 10-20wt% of inorganic nanometer material, 10-20wt% of nano-AlN and the balance polysiloxane resin mixed by component A and component B. The preparation method comprises the following steps: (1) adopting polysiloxane resin containing component A and component B, mixing component A and component B in a weight ratio of 1:1, stirring evenly; (2) adding inorganic nanometer material, then stirring to mix evenly and ensure that the viscosity is not less than 35000cps; and (3) then adding nano-AlN, and stirring the mixed system evenly to obtain the finished product. The insulation crystal-bonding adhesive prepared by the method of the invention has excellent heat conductivity; and as polysiloxane resin is used as base material, the yellowing resistance and blackening resistance are greatly increased and the LED insulation crystal-bonding adhesive of the invention is far superior to the insulation crystal-bonding adhesive using epoxy resin as base material.

Description

A kind of preparation method of LED insulation crystal-bonding adhesive
Technical field
The present invention relates to a kind of preparation method of LED insulation crystal-bonding adhesive.
Background technology
Along with electronic devices and components and electronics develop to thin, light, little aspect, heat conduction, radiating insulating material just become a vital problem.When general electronic devices and components, 8 ℃ of working temperatures that surpass to allow when temperature, the life-span will reduce by 50%.Hence one can see that, and the quality of thermal design will produce very important influence to the life-span and the safety of electronic devices and components, electronics.In thermal design, the material of some good heat conductive insulatings and the process method of use if can be provided, will produce very considerable economic so.At present, the small power white light LEDs all adopts epoxy resins insulation glue as crystal-bonding adhesive, because the thermal conductivity of this insulation crystal-bonding adhesive is lower; Generally have only about 0.2w/m.k, cause LED when work, the heat that is produced can't fast and effeciently be derived and dispel the heat; Again because insulation paste is to adopt the epoxy resin base material to process, in secular use, insulation crystal-bonding adhesive xanthochromia, melanism are serious; The white light LEDs optical attenuation is increased greatly, when serious, when 25 spend, use 1000h; Light decay reaches more than 50%, can't satisfy the requirement of illumination level LED to light decay.
Summary of the invention
Technical problem
The object of the present invention is to provide a kind of preparation method of LED insulation crystal-bonding adhesive, prepared insulation crystal-bonding adhesive heat conductivility is excellent, and anti-xanthochromia, melanism performance also improve greatly.
Technical scheme
The present invention is achieved through following technical scheme.
A kind of preparation method of LED insulation crystal-bonding adhesive; Its raw material consists of: the quality percentage composition is 10～20% inorganic nano material; The quality percentage composition is 10～20% nanometer AlN, and all the other are A, B two-pack blended polyorganosiloxane resin, and its preparation process is following: the polyorganosiloxane resin of A, B two-pack is adopted in (1); The A component is mixed with the mass ratio of B component by 1: 1, and stir; (2) add inorganic nano material, stir then, mix, make its viscosity >=35000cps; (3) add nanometer AlN more therein, mixed system is stirred to get final product.
The preparation method of above-mentioned a kind of LED insulation crystal-bonding adhesive; Wherein, Said inorganic nano material is one or more the mixture in nano aluminium oxide, nano silicon, nano titanium oxide, nano magnesia or the nano oxidized gallium, and the particle size range of said inorganic nano material is 10～50nm.
The preparation method of above-mentioned a kind of LED insulation crystal-bonding adhesive, wherein, the particle size range of said nanometer AlN is 10～50nm.
The preparation method of above-mentioned a kind of LED insulation crystal-bonding adhesive, wherein, said A component is that the methyl phenyl vinyl polyorganosiloxane resin of 99.9%-99.98% and platinum catalyst that the quality percentage composition is 0.02%-0.1% are formed by the quality percentage composition.Said methyl phenyl vinyl polyorganosiloxane resin comprises C 6H 5SiO 3/2Unit and CH 2=CH (CH 3) 2SiO 1/2The unit.
The preparation method of above-mentioned a kind of LED insulation crystal-bonding adhesive; Wherein, said B component is that silica gel, the quality percentage composition of 80%-85% is that 5%-15% dimethyl hydrogen siloxy-phenyl silane and quality percentage composition are that two (dimethylvinylsiloxy) silane of phenylbenzene of 5%-10% are formed by the quality percentage composition.Said dimethyl hydrogen siloxy-phenyl silane chemical formula is [H (CH 3) 2SiO] 2Si (C 6H 5) 2Or [H (CH 3) 2SiO] 3Si (C 6H 5).
Beneficial effect
Insulation crystal-bonding adhesive heat conductivility by the method for the invention preparation is excellent; The thermal conductivity of the insulation crystal-bonding adhesive of epoxy resin-matrix has only 0.2W/m.K in the prior art; And the thermal conductivity of the insulation crystal-bonding adhesive of the method for the invention preparation reaches more than the 1.2W/m.K; Improve the heat conductivility of traditional insulation crystal-bonding adhesive greatly, also taken into account the balance of light transmission and thermal conductivity simultaneously, do not influenced the light extraction efficiency of original white light LEDs.Because adopt polyorganosiloxane resin as base material, its anti-xanthochromia, melanism performance improve greatly, are superior to the insulation crystal-bonding adhesive of epoxy resin base material greatly.As adopt traditional straight cutting retort stand encapsulation, and can produce and can use 1000h down at 25 ℃, average attenuation is 0 white light LEDs product.Epoxy resins insulation crystal-bonding adhesive point glue encapsulation operation technology is identical in the some glue packaging process of the insulation crystal-bonding adhesive of the method for the invention preparation and the prior art, also need not to change relevant device.
Description of drawings
Fig. 1 is the normal temperature longevity test reliability test report of polyorganosiloxane resin based insulation crystal-bonding adhesive of the present invention (WR-26 crystal-bonding adhesive);
Fig. 2 is the normal temperature longevity test reliability test report of the insulation crystal-bonding adhesive (DX-20-4 crystal-bonding adhesive) of epoxy resin-matrix;
Fig. 3 is the hot and humid test reliability trial report of lighting of polyorganosiloxane resin based insulation crystal-bonding adhesive of the present invention (WR-26 crystal-bonding adhesive);
Fig. 4 is the hot and humid test reliability trial report of lighting of the insulation crystal-bonding adhesive (DX-20-4 crystal-bonding adhesive) of epoxy resin-matrix.
Embodiment
Below through embodiment the present invention is described further:
A kind of preparation method of LED insulation crystal-bonding adhesive; Its raw material consists of: the quality percentage composition is 10～20% inorganic nano material; The quality percentage composition is 10～20% nanometer AlN, and all the other are A, B two-pack blended polyorganosiloxane resin, and its preparation process is following: the polyorganosiloxane resin of A, B two-pack is adopted in (1); The A component is mixed with the mass ratio of B component by 1: 1, and stir; (2) add inorganic nano material, stir then, mix, make its viscosity >=35000cps; (3) add nanometer AlN more therein, mixed system is stirred to get final product.
Embodiment 1
A kind of preparation method of LED insulation crystal-bonding adhesive; Its raw material consists of: the quality percentage composition is 15% nano aluminium oxide; The quality percentage composition is 10% nanometer AlN; All the other are A, B two-pack blended polyorganosiloxane resin; Its preparation process is following: the polyorganosiloxane resin of A, B two-pack is adopted in (1), and the A component is made up of the methyl phenyl vinyl polyorganosiloxane resin of 99.9wt% and the platinum catalyst of 0.1wt%, and the B component is made up of two (dimethylvinylsiloxy) silane of the phenylbenzene of silica gel, 15wt% dimethyl hydrogen siloxy-phenyl silane and the 5wt% of 80wt%; The A component is mixed with the mass ratio of B component by 1: 1, and stir; (2) nano aluminium oxide of adding 15wt% stirs then, mixes, and makes its viscosity >=35000cps; (3) and then add the nanometer AlN of 10wt%, mixed system is stirred to get final product.
Embodiment 2
A kind of preparation method of LED insulation crystal-bonding adhesive; Its raw material consists of: the quality percentage composition is 5% nano titanium oxide; The quality percentage composition is 5% nano magnesia; The quality percentage composition is 15% nanometer AlN, and all the other are A, B two-pack blended polyorganosiloxane resin, and its preparation process is following: the polyorganosiloxane resin of A, B two-pack is adopted in (1); The A component is made up of the methyl phenyl vinyl polyorganosiloxane resin of 99.92wt% and the platinum catalyst of 0.08wt%; The B component is made up of two (dimethylvinylsiloxy) silane of the phenylbenzene of silica gel, 10wt% dimethyl hydrogen siloxy-phenyl silane and the 7wt% of 83wt%, the A component is mixed with the mass ratio of B component by 1: 1, and stir; (2) add the nano titanium oxide of 5wt% and the nano magnesia of 5wt% and stir then, mix, make its viscosity >=35000cps; (3) and then add the nanometer AlN of 15wt%, mixed system is stirred to get final product.
Embodiment 3
A kind of preparation method of LED insulation crystal-bonding adhesive; Its raw material consists of: the quality percentage composition is 10% nano aluminium oxide; The quality percentage composition is 5% nano silicon; The quality percentage composition is 10% nanometer AlN, and all the other are A, B two-pack blended polyorganosiloxane resin, and its preparation process is following: the polyorganosiloxane resin of A, B two-pack is adopted in (1); The A component is made up of the methyl phenyl vinyl polyorganosiloxane resin of 99.98wt% and the platinum catalyst of 0.02wt%; The B component is made up of two (dimethylvinylsiloxy) silane of the phenylbenzene of silica gel, 15wt% dimethyl hydrogen siloxy-phenyl silane and the 5wt% of 80wt%, the A component is mixed with the mass ratio of B component by 1: 1, and stir; (2) add the nano aluminium oxide of 10wt% and the nano silicon of 5wt% and stir then, mix, make its viscosity >=35000cps; (3) and then add the nanometer AlN of 10wt%, mixed system is stirred to get final product.
Embodiment 4
A kind of preparation method of LED insulation crystal-bonding adhesive; Its raw material consists of: the quality percentage composition is 15% nano aluminium oxide; The quality percentage composition is 5% nano oxidized gallium; The quality percentage composition is 20% nanometer AlN, and all the other are A, B two-pack blended polyorganosiloxane resin, and its preparation process is following: the polyorganosiloxane resin of A, B two-pack is adopted in (1); The A component is made up of the methyl phenyl vinyl polyorganosiloxane resin of 99.9wt% and the platinum catalyst of 0.1wt%; The B component is made up of two (dimethylvinylsiloxy) silane of the phenylbenzene of silica gel, 5wt% dimethyl hydrogen siloxy-phenyl silane and the 10wt% of 85wt%, the A component is mixed with the mass ratio of B component by 1: 1, and stir; (2) add the nano aluminium oxide of 15wt% and the nano oxidized gallium of 5wt% and stir then, mix, make its viscosity >=35000cps; (3) and then add the nanometer AlN of 20wt%, mixed system is stirred to get final product.
The insulation crystal-bonding adhesive of the method for the invention preparation when not using, is stored in the refrigerator-freezer of 40 degrees below zero; During use, take out and at room temperature place 1～2 hour, and stir, can carry out a glue operation, be used for fixedly usefulness of LED wafer, baking condition:, toasted 1～2 hour at 120～150 ℃.

Claims (3)

1. the preparation method of a LED insulation crystal-bonding adhesive; It is characterized in that; Its raw material consists of: the quality percentage composition is one or more the mixture in 10～20% nano aluminium oxide, nano silicon, nano titanium oxide, nano magnesia or the nano oxidized gallium; The quality percentage composition is 10～20% nanometer AlN; All the other are A, B two-pack blended polyorganosiloxane resin, and said A component is that the methyl phenyl vinyl polyorganosiloxane resin of 99.9%-99.98% and platinum catalyst that the quality percentage composition is 0.02%-0.1% are formed by the quality percentage composition, and said methyl phenyl vinyl polyorganosiloxane resin comprises C 6H 5SiO 3/2Unit and CH 2=CH (CH 3) 2SiO 1/2The unit; Said B component is that silica gel, the quality percentage composition of 80%-85% is that 5%-15% dimethyl hydrogen siloxy-phenyl silane and quality percentage composition are that two (dimethylvinylsiloxy) silane of phenylbenzene of 5%-10% are formed by the quality percentage composition, and said dimethyl hydrogen siloxy-phenyl silane chemical formula is [H (CH 3) 2SiO] 2Si (C 6H 5) 2Or [H (CH 3) 2SiO] 3Si (C 6H 5), its preparation process is following: the polyorganosiloxane resin that A, B two-pack are adopted in (1), mix the A component, and stir with the mass ratio of B component by 1: 1; (2) mixture of one or more in adding nano aluminium oxide, nano silicon, nano titanium oxide, nano magnesia or the nano oxidized gallium stirs then, mixes, and makes its viscosity>=35000cps; (3) add nanometer AlN more therein, mixed system is stirred to get final product.
2. the preparation method of a kind of LED insulation crystal-bonding adhesive as claimed in claim 1 is characterized in that, the particle size range of said nano aluminium oxide, nano silicon, nano titanium oxide, nano magnesia or nano oxidized gallium is 10～50nm.
3. the preparation method of a kind of LED insulation crystal-bonding adhesive as claimed in claim 1 is characterized in that, the particle size range of said nanometer AlN is 10～50nm.
CN2009102337042A 2009-10-23 2009-10-23 Preparation method of light-emitting diode insulation crystal-bonding adhesive Active CN101787255B (en)

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US11131431B2 (en) 2014-09-28 2021-09-28 Jiaxing Super Lighting Electric Appliance Co., Ltd LED tube lamp
CN102775954B (en) * 2012-08-18 2013-10-30 邵成芬 LED (Light-Emitting Diode) packaging silica gel with high refractive index, light transmittance and power, and method for preparing same
CN103013491B (en) * 2012-12-20 2015-06-10 纳晶科技股份有限公司 Silica gel fitting and fabrication method thereof, and LED lamp provided with silica gel fitting
CN205979260U (en) 2014-09-28 2017-02-22 嘉兴山蒲照明电器有限公司 LED (Light -emitting diode) straight lamp
US10560989B2 (en) 2014-09-28 2020-02-11 Jiaxing Super Lighting Electric Appliance Co., Ltd LED tube lamp
CN204693095U (en) * 2014-09-28 2015-10-07 嘉兴山蒲照明电器有限公司 Led daylight lamp
US10514134B2 (en) 2014-12-05 2019-12-24 Jiaxing Super Lighting Electric Appliance Co., Ltd LED tube lamp
CN104592922B (en) * 2014-12-31 2016-04-20 湖北绿色家园精细化工股份有限公司 A kind of transparent, high rigidity, color inhibition epoxy ornaments glue and preparation technology thereof
US9897265B2 (en) 2015-03-10 2018-02-20 Jiaxing Super Lighting Electric Appliance Co., Ltd. LED tube lamp having LED light strip
US10161569B2 (en) 2015-09-02 2018-12-25 Jiaxing Super Lighting Electric Appliance Co., Ltd LED tube lamp
CN112608583A (en) * 2020-12-04 2021-04-06 东莞智昊光电科技有限公司 Thermosetting composite material, application, LED bracket, preparation method of LED bracket and LED product

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