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Transparent epoxy nanometer composite material, preparation method and application thereof

A technology of nano-composite material and transparent ring, applied in the field of transparent epoxy nano-composite material and its preparation, can solve the problems of increased interface force between filler and matrix, decreased light transmittance of material, decreased transmittance of visible light region, etc. The effect of overcoming light scattering phenomena, good fluorescence and phosphorescence effects

Inactive Publication Date: 2009-01-07
TECHNICAL INST OF PHYSICS & CHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this compensation is limited when the prepared material is a thick block, and it is impossible to prepare a nanocomposite with a high filler content. For example, we have prepared a transparent epoxy / ZnO nanocomposite (Polymer, 47( 2006) 2127-2132), when the ZnO content is lower than 0.07%, the addition of fillers has little effect on the visible light transmittance of the composite material, and when the ZnO content exceeds 0.07%, the visible light transmittance drops sharply
In addition, if the particle size of the filler is too small (such as less than 20nm), the specific surface area of ​​the filler will increase sharply, and the agglomeration phenomenon will also intensify. After adding the epoxy prepolymer, the viscosity of the mixture will increase, and the force between the filler and the matrix interface will increase. effect, resulting in severe agglomeration of nanofillers and inability to effectively disperse in the epoxy matrix
These agglomerated particles will cause light scattering in the composite material, resulting in a decrease in the light transmittance of the material

Method used

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  • Transparent epoxy nanometer composite material, preparation method and application thereof
  • Transparent epoxy nanometer composite material, preparation method and application thereof
  • Transparent epoxy nanometer composite material, preparation method and application thereof

Examples

Experimental program
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Embodiment 1

[0039] Add 0.0270mol tetraethyl orthosilicate (TEOS) to 200ml ethanol solution (0.1M) containing zinc oxide quantum dots with a particle size of 2nm under stirring, and magnetically stir for 3 hours; Down reaction 16 hours;

[0040] The resulting substance was washed twice with ethanol to obtain a white precipitate; then the resulting white precipitate was dried in air at 80°C for 6 hours, and calcined at 300°C for 0.5 hour to obtain zinc oxide quantum dots with a core / shell structure / Silicon dioxide (ZnO-QD / SiO 2 ) nanocomposite particles;

[0041] The prepared (ZnO-QD / SiO 2 ) Nanocomposite particle 4.3g joins in 6.0g epoxy solidifying agent (hexahydrophthalic anhydride, including 1.0wt% tetraethylammonium bromide) and after dispersing evenly, add 4.0g bisphenol A type epoxy resin (Epon828, DER 331, DER332 or E51), mixed uniformly, injected into the LED mold, cured and molded to obtain the LED encapsulated by transparent epoxy / S-T-S nanocomposite material (filler content is...

Embodiment 2

[0043] Add 0.120mol tetraethyl orthosilicate (TEOS) to 200ml ethanol solution (0.1M) containing zinc oxide quantum dots with a particle size of 6nm under stirring, and magnetically stir for 5 hours; Down reaction 22 hours;

[0044] The resulting material was washed twice by centrifugation with ethanol to obtain a white precipitate; then the resulting white precipitate was dried in air at 80°C for 6 hours, and calcined at 550°C for 1.0 hour to obtain zinc oxide quantum dots with a core / shell structure / Silicon dioxide (ZnO-QD / SiO 2 ) nanocomposite particles;

[0045] The prepared (ZnO-QD / SiO 2 ) Nanocomposite particle 1g joins in the 25g epoxy solidifying agent (methyl hexahydrophthalic anhydride, including 2wt% tetrabutyl ammonium bromide) and after dispersing evenly, add 25g bisphenol A epoxy resin (Epon828, DER 331, DER332 or E51 ). After mixing evenly, pour it into an LED mold, and solidify and shape it to obtain an LED encapsulated by a transparent epoxy / S-T-S nanocomp...

Embodiment 3

[0047] 0.243mol tetraethyl orthosilicate (TEOS) was added under the condition of stirring to 200ml of ethanol solution (0.1M) containing zinc oxide quantum dots with a particle size of 10nm, and magnetically stirred for 8 hours; Down reaction 28 hours;

[0048] The resulting material was centrifuged twice with ethanol to obtain a white precipitate; then the resulting white precipitate was dried in air at 80°C for 6 hours, and calcined at 800°C for 2.0 hours to obtain zinc oxide quantum dots / Silicon dioxide (ZnO-QD / SiO 2 ) nanocomposite particles;

[0049] The prepared (ZnO-QD / SiO 2 ) Nanocomposite particles 0.1g join in 40g epoxy curing agent (methyl hexahydrophthalic anhydride, including 5wt% imidazole, also can replace imidazole with 5wt% 2-methylimidazole), add 60g hydrogenated bis Phenol A epoxy resin (YX8000). After mixing evenly, pour it into an LED mold, and solidify and shape it to obtain an LED encapsulated by a transparent epoxy / S-T-S nanocomposite material (wit...

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Abstract

The invention relates to transparent epoxy nano composite material, and a preparation method and purposes thereof. The composite material comprises epoxy resin matrix material and composite nano inorganic filler which is evenly distributed in the epoxy resin matrix material; the composite nano inorganic filler consists of a zinc oxide quantum dot which is taken as a core and has grain size of 2nm to 10nm and a silicon dioxide outer layer which is taken as a shell and coated on the zinc oxide quantum dot; the epoxy resin matrix material consists of epoxy resin and epoxy curing agent; the epoxy resin is bisphenol-A epoxy resin or hydrogenated bisphenol-A epoxy resin; the epoxy curing agent is estolide curing agent which contains 1.0 weight percent to 5.0 weight percent of curing accelerator; the curing accelerator is amine curing accelerator or imidazole curing accelerator. The transparent epoxy nano composite material of the invention has excellent transparency, good fluorescence and phosphorescence effect compared with common pure transparent epoxy, and can replace traditional fluorescent powder. The invention is applicable in packaging LED and other luminescent semiconductor devices.

Description

technical field [0001] The present invention relates to a kind of transparent epoxy nano-composite material and its preparation method and application, more specifically, the present invention relates to a kind of transparent epoxy nano-composite material whose filler is the composite nanoparticle with core-shell structure and its preparation method and uses. Background technique [0002] Current scientific research has found that photoaging in white light emitting diodes (Light emitting diodes, LEDs) is not the only reason for the aging of epoxy resins, and another reason for the shortened lifespan of white light LEDs is the scattering effect of phosphors. In the actual application of LEDs, the main way to avoid the aging of epoxy resin caused by phosphor scattering is to keep the phosphor layer as far away from the LED chip as possible. However, although this method can alleviate the negative impact caused by phosphor light scattering to a certain extent, it cannot comple...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L63/02C08K9/02C09K3/10C08K5/3445C08K5/09C08K5/17
Inventor 付绍云李元庆肖红梅杨洋
Owner TECHNICAL INST OF PHYSICS & CHEMISTRY - CHINESE ACAD OF SCI
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