鈦相關氧化物成長機制及其性質之研究｜國立清華大學博碩士論文庫

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研究生：	黃奕仁 Huang, Yi-Jen
論文名稱：	鈦相關氧化物成長機制及其性質之研究 Titanium Related Metal Oxides - Growth Behaviors and Properties
指導教授：	李紫原 Lee, Chi-Young 裘性天 Chiu, Hsin-Tien
口試委員:
學位類別：	博士 Doctor
系所名稱：	工學院 - 材料科學工程學系 Materials Science and Engineering
論文出版年：	2010
畢業學年度：	98
語文別：	英文
論文頁數：	107
中文關鍵詞：	鈦、鈣鈦礦、成長
外文關鍵詞：	Ti, perovskite, growth
相關次數：	點閱：2 下載：0
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當材料縮小至奈米等級時，因其表面積增大或特定晶面的外露，常有不同於塊材的性質。近幾年來利用「由下而上」的合成方法來操控奈米材料的形貌和結構吸引了科學家們的目光。一般而言，材料的形貌深深受到成長行為的影響，在非平衡系統下，溫度梯度和濃度梯度是晶體成長的驅動力，導致了樹枝狀的成長。而在平衡系統下，原子的堆積傾向於讓熱力學穩的面外露，進而造成多面體的晶體。本研究以鹼處理方式在不同條件下合成出鈦酸鋇，鈦酸鍶，鈦酸鈣，以及稀有礦物-kassite等鈦相關氧化物，其多樣化的形貌和結構起因於不同的成長的行為。
首先，我們使用鈦前驅物和相關的氫氧化物在強鹼環境下來合成出多種鈣鈦礦結構(A2+B4+O2-3)，由於鋇、鍶和鈣這三者離子的電荷密度不同，造成原子堆積於 {111} 和 {100} 面上的速率不同，進而導致鈦酸鋇的形貌為圓球狀，鈦酸鍶為有著圓邊和{100}外露面的立方體，鈦酸鈣則為菱菱角角的立方體。利用其立方體的邊和角能量較高的特性，我們選用氟化鈉奈米立方體當作模板，讓四異丙氧基化鈦 (titanium tetraisopropoxide)水解成長於能量高的地方，再去除其模板，即可以得到鳥籠狀的奈米二氧化鈦。
當鈦酸鈣於弱鹼環境下合成時，由於系統中的濃度梯度增加而導致系統遠離平衡狀態，造成動力學產物-樹枝狀晶體的形成，此樹枝狀晶體主幹沿(012)面的法線向量，而兩個分枝分別沿(102)和面的法線向量成長。此外，使用鈦前驅物和氫氧化鈣在短時間下反應時，另一種動力學產物 – kassite 第一次以人工合成的方法得到。以穿透式電子顯微鏡配合同步輻射X光圖譜解析出其結構為六方晶系P312 並有著a = b = 0.52451(2) 和 c = 0.47844(3) nm. 在大部分的實驗中，常伴隨有鈦酸鈣的形成，這是因為kassite的形成是動力學控制下的產物，是經由溶於鹼中的氫氧化鈦和固體的氫氧化鈣反應而得到。而相對的，鈦酸鈣是熱力學控制下的產物，是經由溶於鹼中的氫氧化鈦和溶於水中的鈣離子反應所得到。當調整氫氧化鈣和二氧化鈦的莫耳比例為2:1，並且在10 M的濃氫氧化鈉下反應，再藉由鹽酸浸泡產物就可以得到純的片狀kassite。我們進一步的對此材料於不同溫度下做熱處理，從相對應的X光繞射圖譜和熱重損失-質譜圖譜分析得知加熱在500 °C 以上，結構中的水會完全的被去除而原子重新排列，溫度升至700 °C時則完全變成鈦酸鈣結構，其形貌仍然保持在片狀但在表面出現非晶質的二氧化鈦。當加熱至更高溫約1000°C時，非晶質的二氧化鈦轉換為金紅石(rutile) 並且晶粒聚集成長變大使得片狀結構崩解。
當鈦酸鋇和鈦酸鍶於短時間下合成時，並無法得到任何動力學產物，只有伴隨著殘留二氧化鈦。此複合材料為天然的hetrojunction 能夠抑制電子-電洞的再結合。本實驗以合成TiO2/BaTiO3 複合材料當作染料敏化電池的陽極材料，相較於純的二氧化鈦，其電池的轉換效率增加了1.7倍。

Tables of Contents
Abstract    I
中文摘要    IV
誌謝    VI
Lists of Figure Captions    XI
Lists of Table Captions    XV
Chapter 1    Introduction and Literature Review    1
1    Introduction    2
2    Literature reviews    5
2.1    Synthesis of metal oxide by alkali treatment    5
2.2    Kassite    12
2.3    Perovskite    15
2.4    Denedrite    17
2.5    Dye-sensitized solar cell    24
Chapter 2     Motivation    30
Chapter 3    Experimental Procedure    33
1    Materials    34
1.1    Reagents for synthesis    34
1.2    Electrolyte    35
1.3   Conducting substrate    35
2    Synthesis of calcium titanate    35
3    Synthesis of kassite (CaTi2O4(OH)2)    36
4    Synthesis perovskite related materials    36
5    Synthesis of TiO2/BaTiO3 composite    36
6    Fabrication of dye-sensitized solar cells.    37
6.1    Photoelectrode    37
6.2    Counter electrode    37
6.3    Electrolyte    37
6.4    Fabrication    37
7    Characterization and analysis    38
7.1    Morphological and structural characterization    38
7.2    Measurement of solar cell efficiency    39
7.3    Software of XRD refinement    39
7.4    Other analysis    39
Chapter 4     Growth of CaTiO3 Dendrites and Rectangular Prisms through a Wet Chemical Method    41
1    Abstract    42
2    Morphological and structural characterizations    43
3    Growth direction of dendrites    46
4    Growth mechanism of dendrites    50
5    Growth mechanism of rectangular prisms    51
6    Conclusion    56
Chapter 5    Artificial Synthesis of Platelet-like Kassite and Its Transformation  to CaTiO3    57
1    Abstract    58
2    Morphological and structural characterization    59
3    XRD refinement    63
4    Thermostability of kassite    64
5    Formation mechanism of kassite    70
6    Conclusion    74
Chapter 6     Manipulating the Shapes of Metal Oxides by Surface Stability    75
1    Abstract    76
2    Morphological and structural characterizations    77
3    Growth mechanism    79
4    Synthesis of nanocages    81
5    Conclusion    84
Chapter 7     A Simple Route to Synthesize TiO2/BaTiO3 Hetrojunction for Dye-sensitized Solar Cells    85
1    Abstract    86
2    Morphological and structural characterizations    86
3    Performance of DSSCs    88
4    Charge transport resistance and lifetime    90
5    Conclusion    93
Chapter 8  Future Work    94
Appendix.    96
References    97
Publication list    107

                                

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Chapter 7
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