本研究目的為開發臨場加熱電子顯微技術，利用自行設計的加熱載具分別於掃描式/穿透式電子顯微鏡中建立一臨場加熱系統，用以觀察其材料於升溫過程中的動態反應，包含擴散、成核與成長過程。並搭配電子顯微鏡之能量散佈光譜儀對材料於反應前後做定性與定量分析。
參考其原廠載具規格並了解其內部構造後，分別針對熱燈絲掃描式電子顯微鏡與場發射穿透式電子顯微鏡設計一加熱載具。掃描式電子顯微鏡加熱系統為陶瓷加熱片接一配有溫度控制之直流電源，並利用K型熱電偶量測載台溫度。配合加熱片之尺寸自行設計一載具，其裝置可於室溫至500℃下臨場觀測其表面形貌之改變。而穿透式電子顯微鏡則使用一自行設計微型環狀螺旋熱阻絲搭配一直流電源供應器，並將其熱阻絲置於自製載具中，亦可於室溫至500℃下做臨場加熱之動態觀測。
而本實驗主要觀測材料為a-Si1-xGex/ AlOx/ Al/ Si substrate 堆疊結構，搭配商用加熱載具與自行設計之載具臨場觀測略低於共晶溫度下鋁誘發異矽鍺異質磊晶於矽基板之反應過程，並搭配能量散佈光譜儀之成分分析作為驗證。

The main goal of this research is to develop the in-situ heating electron microscopy applied on dynamic observation of material’s reaction process including atomic diffusion, nucleation, and grain growth. The in-situ heating systems are set up in scanning and transmission electron microscope respectively for dynamic analysis of aluminum-induced solid-phase epitaxy (Al-SPE).
Comparing with the specifications of commercial holders, the self-designed heating stage for scanning electron microscope (SEM) and heating holder for transmission electron microscope (TEM) are developed to each requirement of instrument respectively. The heating system for SEM is composed of the heat insulator, sample carrier and the ceramic heating element, equipped with a temperature control system. The temperature range of this self-designed SEM heating system is from room temperature to 500℃. On the other hand, the heating system for TEM is composed of the toroidal coils, put in self-designed heating holder, and a DC power supply, which can heat up to 500℃ for in situ analysis.
With commercial heating holder and self-designed heating system, the dynamic reaction of aluminum-induced heteroepitaxial SiGe on sc-Si (100) substrate at low temperature (lower than 725K) is observed and further verified the reaction mechanism of Al-SPE with EDS and motion images.

致謝 i
摘要 iii
Abstract iv
目錄 v
表目錄 viii
圖目錄 ix
第一章 緒論 1
1.1 顯微鏡的發展 1
1.1.1 光學顯微鏡的發展 1
1.1.2 電子顯微鏡的發展 3
1.1.3 掃描式電子顯微鏡 5
1.1.4 穿透式電子顯微鏡 7
1.2 研究動機與目的 8
第二章 文獻回顧 9
2.1 電子顯微鏡加熱載具設計 9
2.1.1 掃描式電子顯微鏡之加熱載具 10
2.1.2 穿透式電子顯微鏡之加熱載具 15
2.1.3 微機電製程之微型加熱器 19
2.2 臨場加熱電子顯微鏡之分析 23
2.2.1 高溫臨場相變化之分析 23
2.2.2 臨場觀測奈米結構成核與成長 26
2.2.3 臨場觀測原子擴散與電遷移現象 32
2.3 矽基太陽能電池 35
2.3.1 太陽能電池的發展 35
2.3.2 鋁誘發固相磊晶技術 39
2.3.2.1 金屬誘發結晶 39
2.3.2.2 金屬誘發異質磊晶矽鍺薄膜 40
2.3.3 鋁誘發磊晶機制與熱力學探討 43
第三章 載具開發與實驗方法 47
3.1 實驗大綱 47
3.2 掃描式電子顯微鏡臨場觀測之加熱系統架設 48
3.2.1 設備與裝置組件 48
3.2.2 實驗步驟 52
3.3 穿透式電子顯微鏡臨場觀測之加熱系統架設 53
3.3.1 設備與裝置組件 54
3.3.2 實驗步驟 56
3.4 鋁誘發固相磊晶技術低溫成長異質磊晶矽鍺薄膜 57
3.4.1 材料準備 57
3.4.2 樣品製備步驟 57
第四章 結果與討論 60
4.1 SEM加熱載具設計與製作 60
4.1.1 加熱系統的設計與儀器架設 60
4.1.2 升溫與影像擷取測試 62
4.1.3 載具設計與組裝 64
4.1.4 臨場觀測 66
4.2 TEM加熱載具設計與製作 68
4.2.1 加熱系統的設計&TEM樣品桿的製作 68
4.2.2 自製TEM樣品桿檢測 70
4.2.3 樣品載具的設計與製作 71
4.2.4 樣品位置與溫度分佈 72
4.3 鋁誘發矽鍺異質磊晶於TEM下臨場觀測 74
4.3.1 鋁誘發矽鍺異質磊晶於升溫過程之反應 75
4.3.2 由臨場觀測結果探討其反應機制 77
4.3.2.1 矽鍺自由原子的形成與擴散 77
4.3.2.2 鋁-矽界面成核點的產生 78
4.3.2.3 異質磊晶反應後堆疊結構之變化 80
4.3.3 鋁誘發異質磊晶之分析 81
4.4 自製TEM加熱載具臨場觀測鋁誘發異質磊晶 83
第五章 結論 84
第六章 參考文獻 85

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