[[alternative]]Synthesis and property of lanthanum hexaboride

碩士[[abstract]]本研究使用七莫耳結晶水之氯化鑭、硼氫化鈉與鎂粉末於高溫(600、800及1000℃)低壓(10-2torr)條件下成功合成出六硼化鑭顆粒，六硼化鑭的結晶程度隨合成溫度增加而上升。將合成的六硼化鑭顆粒均勻混入壓克力系感光UV膠內，且經球磨混練及粒徑微細化後製得的隔熱膠，經光譜儀分析知近紅外光遮蔽效果隨合成溫度增加及粒徑減小而增加；隔熱膠固化及接著於6mm單層玻璃基材後再濺鍍約30nm金鍍層及6mm單層玻璃基材濺鍍金鍍層後再與固化隔熱膠接著，發現前者之結構模組俱較低的遮蔽係數。3mm單層玻璃間膠合固化隔熱膠及金鍍層後，由於光在界面間的多重反射及吸收，近紅外光遮蔽效果較隔熱膠固化於6mm單層玻璃基材後再濺鍍金鍍層佳。[[abstract]]This study has successfully synthesized lanthanum hexaboride by using magnesium powder, NaBH4 and LaCl3·7H2O at high temperature (600、800、1000℃) and low pressure (10-2 torr). The crystalline degree of lanthanum hexaboride increased with raisingsynthesizing temperature. The heat-insulating resin was prepared by uniformly blending synthesized lanthanum hexaboride particulates into UV-curing acrylic resin, then thelanthanum hexaboride particulates of the mixture was ball-milled to nano-scaled meter. The spectrum analysis showed that the near-infrared shielding effect increased accordingto increased synthesizing temperature and decreased particle size. Comparing two modules of different layer sequence on the surface of the 6mm thickness-glass substrate：(1)curing heat-insulating resin before sputtering a about 30nm gold layer ；and (2)sputtering a about 30nm gold layer before coating and curing a heat-insulating resin, respectively which alower shading coefficient was obtained on the module of former structure. Thenear-infrared shielding effect of the module with laminated a cured heat-insulating resin and then sputtering a about 30nm gold layer between 3mm-thickness glasses is better than the module with cured a heat-insulating resin on the surface of the 6mm-thickness glass substrate and then sputtering a about 30nm gold layer . The positive effect is due to the multiple reflection and absorption of light between interfaces.[[tableofcontents]]目錄 摘要····················································Ⅰ Abstract················································Ⅱ 總目錄·························· III 圖目錄··························VⅠ 表目錄··························VⅡ 壹、導論··························1 1-1 前言················································1 1-2 文獻回顧············································4 1-2.1折射與反射於近紅外光遮蔽機制·······················4 1-2.2 吸收於近紅外光遮蔽機制····························7 1-2.3六硼化鑭··········································11 1-2.4 紫外光硬化技術···································14 1-2.5節能玻璃··········································15 1-3 研究範疇···········································18 貳、實驗設計···········································29 2-1實驗藥品器材與實驗設備······························29 2-1.1 實驗材料······················29 2-1.2 實驗設備及分析儀器·······························30 2-2 實驗程序···········································32 2-2.1合成藥品之熱重分析測試····························32 2-2.2 LaB6奈米粉末合成·································32 2-2.3 LaB6奈米粉末之淨化·······························33 2-2.4 形態觀察·········································34 2-2.5 X光能量散佈分析儀(EDS) ··························34 2-2.6 粒徑分析·········································35 2-2.7 X-Ray繞射分析····································35 2-3 性質測試···········································36 2-3.1光譜測試··········································36 2-3.2隔熱玻璃製作及隔熱性能測試························37 參、結果與討論······················36 3-1 粉末性質分析·······································45 3-1.1 LaCl3·7H2O與NaBH4脫水及熱解聚分析················45 3-1.2 LaB6 XRD與EDS分析································45 3-1.3 LaB6之顯微結構···································47 3-1.4 LaB6之奈米化·····································47 3-2 光學性質分析·······································48 3-2.1 薄膜與平板玻璃之穿透率、反射率與吸收率計算········48 3-2.2 日光輻射熱取得率··················50 3-2.3 近紅外光遮蔽膠膜光譜分析·························51 3-2.4 節能膠合玻璃性能分析·····························53 肆、結論··························70 伍、參考文獻···········································72 圖目錄 圖 1-1、不同厚度的鍍膜層在反射率上的表現[8]············20 圖1-2、3M 240層光學隔熱膜膜示意[7]·····················21 圖 1-3、菁染料結構與其吸收光譜[14]·····················22 圖1-4、多次甲基菁染料結構[15]··························22 圖1-5、錯合物之結構與其吸收光譜[21]····················23 圖 1-6、六硼化鑭之結構[22]·····························24 圖2-1、合成反應系統與反應式示意························39 圖2-2、HITACHI U-4100分光光譜儀外觀····················40 圖2-3、6mm隔熱單層玻璃功能層設計示意···················41 圖2-4、3mm膠合隔熱雙層玻璃功能層設計示意···············42 圖3-1、原料熱脫水TGA分析·······························57 圖3-2、粉末成品在各燒結溫度條件下之XRD繞射分析·········58 圖3-3、合成粉末成品之EDS分析···························59 圖3-4、ALDRICH LaB6粉末之SEM照片·······················60 圖 3-5、不同條件下製備之近紅外光遮蔽膠膜光譜分析·······65 圖 3-6、SEM照片及條件下粒徑分析························67 表目錄 表一、氧化物具有電致變色性質的之過渡金屬元素[19] ······25 表二、UV-Curing與 Heat Curing之比較[35]················26 表三、紫外光硬化材料的基本組成及其功能[36]·············26 表四、商業上常用的光起始劑與生產公司[34]···············27 表五、玻璃綠建材之評估基準表[37] ······················28 表六、功能性隔熱膠膜之製備條件·························43 表七、節能玻璃之製備條件·······························44 表八、合成粉末成品之粒徑分析···························61 表九、可見光穿透率及反射率計算之Dλ．Vλ係數[41]·········62 表十、日光穿透率、反射率及吸收率計算之Eλ．△λ係數[41]··63 表十一、熱輻射光譜分佈對應值值 [41] ···················64 表十二、室內與室外之表面轉換係數 [42] ·······································64 表十三、各條件隔熱膠膜之可見光與日光(熱)穿透率分析··············66 表十四、各條件隔熱膠膜之粒徑分析················································66 表十五、各條件下節能膠合玻璃之光學性質量測分析結果···········68 表十六、各條件下節能膠合玻璃之遮蔽係數····································69[[note]]學號: 696370427, 學年度: 9