高折射率奈米二氧化鋯�矽樹脂複合材料之製備及其在LED封裝材料的應用

Preparation of High Refractive Index Zirconium Dioxide / Silicone Resin Composite Materials and Its Application on LED Encapsulating Materials

賴岱甫(Dai-Fu Lai)

指導教授 ： 邱文英

國立臺灣大學/工學院/化學工程學研究所/碩士(2012年)

https://doi.org/10.6342/NTU.2012.01962

摘要

本研究分為兩個部分，第一部分是利用溶膠凝膠法，直接在LED矽樹脂封裝材料中，合成具有高折射率之二氧化鋯奈米顆粒，使用醋酸當作螯合劑來控制二氧化鋯的顆粒大小和改質二氧化鋯的表面，將二氧化鋯顆粒導入商用LED矽樹脂中，並在合成二氧化鋯之溶膠凝膠過程中，選用適當的溶劑防止二氧化鋯聚集。
　　將二氧化鋯/矽樹脂複合材料製備成具有高折射率以及高透明度之光學薄膜，並製備下層為高折射率薄膜，上層為A/B劑之折射率漸進式複合膜，藉由折射率的層層遞減，以期後續應用在LED封裝中能達到較高的取光效率；並量測含高折射率二氧化鋯A/B劑之折射率、薄膜之穿透度，以及複合膜之穿透度、吸水性、耐熱性與耐UV光性，以符合LED封裝材料之需求。
　　第二部分欲探討加入二氧化鋯奈米顆粒對矽樹脂之A/B劑硬化交聯程度的影響，由DSC的反應熱探討二氧化鋯濃度及其顆粒大小，影響矽樹脂之A/B劑聚合之情形。並利用DSC探討含二氧化鋯A/B劑複合膜之聚合情形。

關鍵字

二氧化鋯 ； 溶膠凝膠法 ； LED封裝材料 ； 高折射率 ； 有機/無機複合材料

並列摘要

The research was divided into two parts. Zirconium dioxide (ZrO2) nanoparticles with high refractive index were introduced into commercial-grade silicone resin by an in-situ sol gel reaction in the first part. The acetic acid was used as chelating agent to control the particle size of ZrO2 and modified the surface of ZrO2 to provide linkages between the water phase of ZrO2 and the oil phase of silicone resins. Moreover, butanol and methyl ethyl ketone were chosen as the co-solvent system to prevent ZrO2 particles from aggregation during the sol-gel process.
Then we synthesized optical films with high refractive index and high transmittance and synthesized composite films with high refractive index thin film on the bottom and encapsulating material on the top of the composite film. Through using the encapsulating materials with decreasing refractive index layer-by-layer, LEDs could achieve higher light extraction efficiency. In order to achieve the requirements of LED encapsulating materials, optical thin films and composite films were synthesized and measured in terms of refractive index, transmittance, water uptake, thermal resistance and UV resistance.
The curing degree of the silicone resin after introducing zirconium dioxide nanoparticles was investigated in the second part. The influences of the concentration and the size domain of the zirconium dioxide on the degree of curing degree was studied by DSC measurement, and the curing degree of the composite film was investigated by DSC measurement as well.

並列關鍵字

zirconium dioxide (ZrO2) ； sol-gel method ； LED encapsulating materials ； high refractive index ； organic/inorganic hybrid materials

參考文獻

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