高性能改質二氧化鈦/環氧樹脂奈米複合材料應用於LED封裝之製備與性質研究

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题名:	高性能改質二氧化鈦/環氧樹脂奈米複合材料應用於LED封裝之製備與性質研究 Preparation and Characterization of High Performance Modified TiO2/Epoxy for LED Encapsulation
作者:	何偉碩
贡献者:	化學工程與材料工程學系奈米材料碩士班
关键词:	二氧化鈦環氧樹脂 LED封裝奈米複合材料 TiO2 Epoxy LED Encapsulation nanocomposites
日期:	2017
上传时间:	2017-09-27 10:50:05 (UTC+8)
摘要:	本研究旨在製備高性能矽氧烷改質二氧化鈦/環氧樹脂奈米複合材料，並檢測其物理性質、熱性質、機械性質、光學性質、形態學與穩定性性質，將此性能優異之環氧樹脂奈米複合材料應用於LED封裝膠。此種環氧樹脂具有高透明度，良好的耐候性、耐高溫特性、抗龜裂性、極佳的電氣特性與低放熱反應性，為LED封裝材料之主要原料。為了提升環氧樹脂在折射率、熱尺寸穩定性及提升其耐黃變性質，本研究利用奈米二氧化鈦(TiO2)作為補強材添加於環氧樹脂中，藉由奈米二氧化鈦之高折射率、高機械性質與良好吸收UV光之性質，以達到補強環氧樹脂材料之效果。本研究利用溶膠-凝膠(sol-gel)法將矽氧烷偶合劑(3-Aminopropyltrimethoxysilane)接枝於奈米二氧化鈦表面以進行改質，成功製備出良好分散性之改質奈米二氧化鈦(APTMS-m-TiO2)，利用原位聚合法將TiO2與APTMS-m-TiO2摻混至環氧樹脂(Epoxy)中，將混和後還氧樹酯複合材料注入模具，在100 ℃先烘烤1小時，再使用120 ℃烘烤4小時製備成改質二氧化鈦/環氧樹脂奈米複合材料。並探討不同TiO2與APTMS-m-TiO2 之phr (每100克的樹脂所含該之成份克數)對環氧樹脂奈米複合材料形態學(SEM)、物理性質(接觸角及密度)、機械性質(硬度、耐磨耗指數、耐衝擊強度、抗折強度及黏合強度)、熱性質(TGA、TMA、CTE、HDT及VST)與光學性質(透光率、折射率)之性能和影響的差異程度。實驗結果得知，經由TGA、FTIR、XRD及XPS測試，可以證明矽烷偶合劑接枝的成功，並在粒徑分析下，也證明經由改質後之奈米二氧化鈦粒徑較改質前之粒徑大小要更大，證實矽氧烷偶合劑改質成功。在二氧化鈦/環氧樹脂奈米複合材料添加TiO2與APTMS-m-TiO2部分，物理性質的測試，密度與接觸角度皆上升；在機械性質測試結果，硬度、磨耗指數、抗折模數與黏合強度，皆為上升，而耐衝擊強度與抗折強度則下降；在熱性質方面，VST與HDT皆上升；光學性質結果得知，折射率隨著奈米二氧化鈦添加量的增加而上升，當APTMS-m-TiO2添加量為0.010phr時，在波長為589 nm處，環氧樹脂奈米複合材料之折射率由1.6562提升至1.6568。添加量0.001 phr之APTMS-m-TiO2 / Epoxy奈米複合材料於450 nm處之光穿透率為76.311 %、添加量0.003 phr為75.122 %、添加量0.005 phr為74.011 %與添加量0.010 phr為70.048 %，比相同添加量之 pristine TiO2/ Epoxy奈米複合材料，光穿透率為76.554 %、75.753 %、74.685 %與71.333%。透光老化測試中，熱穩定性與UV光照穩定性效果也都提升。以上結果顯示出添加奈米二氧化鈦粉末，有助於提升環氧樹脂奈米複合材料之各項性質。改質二氧化鈦比上未改質二氧化鈦於環氧樹脂奈米複合材料中各性質表現都更加良好，顯示出改質後奈米二氧化鈦 / 環氧樹脂奈米複合材料之分散性較為良好。從長時間高溫烘烤與長時間UV光照試驗結果得知，添加奈米二氧化鈦透光率損失，隨著添加量之增加而減少，改質後較未改質之環氧樹脂奈米複合材料，損失率又更低，顯示出添加奈米二氧化鈦有助於提升材料之耐熱性與UV光照之耐候性，改質後又比未改質之環氧樹脂奈米複合材料效果更顯著。 The aim of this study is to develop a high performance and high light transparent titanium oxide (TiO2) / Epoxy　resin(Epoxy) nanocomposite for light-emitting diode(LED)　encapsulant. Determinev　properties　about physical properties, mechanical properties, electrical properties, optical properties, thermalproperties, characterization, morphology and reliability. This kind of epoxy resin has high transparency, good weatherability, high temperature resistance, crack resistance, excellent electrical characteristics and low exothermic reaction, the main raw material for LED encapsulant. Anatase TiO2 nanoparticles were used as high refractive index filler to fabricate excellent UV resistance, high mechanical properties and high refractive index epoxy nanocomposites. In this study, using 3-Aminopropyltrimethoxysilane(APTMS) grafted nano titanium surface modification by a sol-gel method and TiO2 and APTMS-m-TiO2 were mixed into epoxy resin (Epoxy) by in-situ polymerization. After mixing, the epoxy resin nanocomposite was injected into the mold, baked at 100℃ for 1 hour, and then baked at 120℃ for 4 hours to prepare a transparent modified titanium dioxide(TiO2) / epoxy resin(Epoxy) nanocomposite. For Epoxy Add prepared TiO2 and MPS-m-TiO2 nanocomposites with a different number of grams of composition (per 100 grams of resin contained in the composition of the number of grams). Explore the different components of the number of grams of TiO2 and MPS-m-TiO2 nanometer morphology of Epoxy composites(SEM), physical properties (density and contact angle), mechanical properties (hardness, abrasion index, flexural strength, impact strength and adhesive strengh), thermal properties (TGA, CTE, HDT and VST), the optical properties (transmittance, refractive index), reliability of the performance and impact. The experimental results that, through test of TGA, FT-IR, XRD and XPS can prove the success of silane coupling agent grafted via.And at particle size analysis, also can prove APTMS-m-TiO2 is bigger than TiO2. The TiO2 and APTMS-TiO2 were added to the Epoxy nanocomposite parts, a test of physical properties (density and porosity) effectively increasing, in mechanical properties test results, hardness and abrasion index are rising, while the impact of strength is fall；thermal properties, heat resistance improving effect is more significant. In optical properties test, refractive index is rising. The above results indicate that adding TiO2 is beneficial to promote each characteristic of Epoxy nanocomposite。APTMS-m-TiO2 is better than TiO2 on Epoxy nanocomposite, it shows that APTMS-m-TiO2 diversion is better. It can be proved that in a long period of high temperature and UV light that add transmittance of TiO2 the loss of rate .It shows that add TiO2 is conducive to enhance both of the heat resistant of materials and the UV exposure,TPTMS-m-TiO2 / Epoxy nanocomposite is better than TiO2 / Epoxy nanocomposite effect more remarkable.
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