奈米氧化鉍是用熱蒸鍍法將金屬鉍(99.999%)於1 Torr的環境下製成奈米鉍粉末，並將粉末放入高溫爐管退火製成，並分別從50°C到800°C於大氣壓下恆溫退火兩個小時。可以從外觀上看到粉末會有從黑色→亮黃色→淺黃色→深黃色的顏色變化，使用掃描式電子顯微鏡(FE-SEM)、X光繞射分析(XRD)和室溫的光致發光分析(PL)來探討退火對奈米氧化鉍的形貌、粒徑、晶體結構與光學性質的影響。FE-SEM的結果顯示奈米氧化鉍粒子的平均粒徑隨著退火溫度的上升而增加，粒子表面的形貌在退火溫度超過300°C時改變。XRD的結果顯示退火溫度在250°C時會轉變成純四方結構的β-Bi2O3，退火溫度在550°C時會轉變成純體心立方結構的γ- Bi2O3，退火溫度在700°C時會轉變成單斜結構的α- Bi2O3和三斜結構ω- Bi2O3，晶粒大小也隨著退火溫度上升而增加。室溫PL的結果顯示在He-Cd雷射(325nm)的激發下，在紫光、藍-綠光波段、黃-橘波段、紅光波段出現五個發射波峰，且紅光的強度占了大部分的發光強度，顯示出奈米氧化鉍的發光主要是鉍原子的間隙缺陷，隨著退火溫度上升，主峰值位置幾乎沒有變化，代表粒徑大小與晶格結構不會影響奈米氧化鉍主要的發光性質。

Bismuth nanoparticles were prepared by thermal evaporation method with purity 99.999% bismuth bulk. The as-prepared bismuth nanoparticles were annealed in air with high temperature tube furnace from 50°C to 800°C for two hours to obtain bismuth oxide nanoparticle. The color change can be seen from appearance of powder from black → bright yellow → pale yellow → red-brown. Using Scanning Electron Microscope (SEM)、X-Ray diffractometer (XRD) and room temperature Photoluminescence (PL) to analyze the effect of annealing on morphology、particle size、crystal structure and optical properties of bismuth oxide. The result of SEM show that the mean size of bismuth oxide nanoparticles increases with anneal temperature rise. The morphology of particles changes with anneal temperature above 300°C. The result of XRD shows that the crystal structure transform to pure tetragonal of β-Bi2O3 in anneal temperature 250°C, pure body-centered cubic γ- Bi2O3 in anneal temperature 550°C, monoclinic α- Bi2O3 and Triclinic ω- Bi2O3 in anneal temperature 700°C. The crystallite size increase with the anneal temperature rise. The result of room temperature PL shows that emission band is observed in Violet region (390-450nm)、blue-green region(490-580nm)、yellow-orange region ( 550-640nm ) and red region (650~800nm) under excited by He-Cd laser (325 nm). The intensity of red emission band occupied most of luminescence of bismuth oxide nanoparticle indicate that the existence of visible emission band can be attributed to the bismuth interstitials. The position of emission band of red region do not change also indicate that the change of grain size and crystal structure will not change the optical properties of bismuth oxide nanoparticles.

第一章 緒論 1
1-1 簡介 1
1-2 研究動機 1

第二章 基礎理論 3
2-1 退火 3
2-2 鉍的晶體結構與性質 4
2-3 氧化鉍的晶體結構與性質 5
2-4 氧化鉍的發光性質 7

第三章 樣品的製備 9
3-1 奈米鉍的製備 9
3-2 奈米氧化鉍的製備 11

第四章 實驗儀器介紹 13
4-1 掃描式電子顯微鏡(SEM) 13
4-2 X-射線繞射儀(XRD) 15
4-3 光致發光光譜儀(PL) 17

第五章 奈米氧化鉍之測量與分析 21
5-1 樣品表面形態與粒徑分析 21
5-2 不同退火溫度的晶體結構分析 30
5-2-1 GASA精算軟體晶體結構擬合分析 30
5-2-2 寬化效應與晶體粒徑尺寸(grain size)分析 44
5-3 光致發光(PL)光譜分析 48

第六章 結論 65

第七章 參考文獻 67

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