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研究生:周顯達
論文名稱:前驅溶液製備條件對溶膠-凝膠法製備之鋯鈦酸鉛溶膠及薄膜特性影響之探討
論文名稱(外文):Effects of the Preparation Conditions of the Precursor Solutions on the Characteristics of Sols and Thin Films of Sol-Gel Derived Lead Zirconate Titanates
指導教授:盧信
學位類別:碩士
校院名稱:長庚大學
系所名稱:化學工程研究所
學門:工程學門
學類:化學工程學類
論文種類:學術論文
論文出版年:2001
畢業學年度:89
語文別:中文
中文關鍵詞:鋯鈦酸鉛鐵電薄膜溶膠-凝膠法前驅溶液
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本論文之目的即想利用溶膠-凝膠法製備鋯鈦酸鉛及其薄膜,並探討溶膠-凝膠法前驅溶液製備條件,對鋯鈦酸鉛溶膠及粉末性質與燒結後鋯鈦酸鉛及其薄膜之特性的影響,並探討如何利用前驅溶液製備條件之控制,來調整溶膠及粉末之性質,進而改善燒結後鋯鈦酸鉛之特性。
實驗結果已證實,前驅溶液製備條件(反應物、水解量、濃度、溫度、pH值、Pb含量及酸觸媒種類),對以溶膠-凝膠法製備之鋯鈦酸鉛粉末及薄膜之結晶性、介電性及鐵電性皆有顯著之影響。在前驅溶液的製備條件之組合上,以選擇Pb(OAc)2-Zr(OPr)4-Ti(OPri)4 為反應物系統時,配合以濃度0.1M及在20℃下反應,並添加醋酸觸媒控制其pH值=5.43的環境下,可得到具最佳鈣鈦礦相結構的PZT薄膜及粉末,同時在此系統下,PZT薄膜的電性最佳(εr = 772.758,tanδ = 0.0552 at 100KHz;Pr = 40.5656μC/cm2,Ec = 56.8969kV/cm)。
The objective of this thesis is to prepare lead zirconium titanates(PZT) and their thin films by sol-gel method. In addition, the effects of the preparation conditions of the precursor solutions on the properties of the PZT sols and powders as well as the characteristics of the electro-ceramics and their thin film materials after sintering are also investigated.
From the experimental results obtained so far, it is proved that the preparation conditions of the precursor solutions (reactant selection, amounts of H2O, concentration, reaction temperature, pH value, lead content, acid catalyst selection, etc.) have prominent impacts on the crystallineity, the dielectrical properties, and the ferroelectrical properties of the sol-gel derived lead zirconium titanates. PZT powders and thin films with excellent perovskite structure can be produced from the 0.1 M precursor solution that was prepared by mixing Pb(OAc)2 solution with Zr(OPr)4 solution and Ti(OPri)4 solution at 20℃and pH=5.43 using acetic acid as catalyst. In this study, the PZT thin films prepared from this precursor solution also exhibited the best electrical properties (εr = 772.758,tanδ = 0.0552 at 100KHz;Pr = 40.5656μC/cm2,Ec = 56.8969kV/cm).
摘 要I
AbstractII
目錄III
圖目錄VII
表目錄XV
第1章 緒論1
第2章 文獻回顧6
2-1 鐵電特性6
2-2 PZT之晶體結構與性質12
2-3 非揮發性鐵電記憶體元件15
2-3-1 鐵電記憶體原理17
2-3-2 記憶陣列(以常見的1T-1C結構設計來說明)19
2-3-3 鐵電記憶體材料20
2-4 介電性質24
2-4-1 介電常數24
2-4-2 介電損失26
2-4-3 介電性的頻率特性28
2-5 疲勞30
2-6 時效34
2-7 漏電流機構35
2-8 依時介電崩潰41
2-9 溶膠-凝膠程序之原理及影響參數43
2-9-1 基本原理43
2-9-2主要影響因素50
2-10 研究目的57
第3章 實驗程序58
3-1 藥品來源及標定58
3-2前驅溶液之製備61
3-3 粉末的製備62
3-4 薄膜的製備63
3-5 性質的檢測68
3-5-1 粉末部分68
3-5-2薄膜部分69
3-5-3 PZT電容元件部分71
第4章 結果與討論73
4-1 PZT乾膠之熱處理條件之探討75
4-1-1 PZT4乾膠TGA&DTA之熱行為分析75
4-1-2 PZT4粉末XRD之分析78
4-1-3 PZT4粉末拉曼光譜之分析87
4-2 PZT陶瓷粉末性質之探討100
4-2-1 PZT乾膠TGA&DTA之熱行為分析100
4-2-2 PZT粉末XRD之分析130
4-2-3 PZT粉末拉曼光譜儀之分析145
4-3 PZT薄膜性質之探討159
4-3-1 PZT薄膜XRD之分析159
4-3-2 PZT薄膜之拉曼光譜的分析:167
4-3-3 PZT薄膜之ICP成分鑑定173
4-4 PZT薄膜介電及鐵電性質之量測與探討179
4-4-1 介電性質的量測179
4-4-2 PZT薄膜鐵電性質的量測187
4-4-3 PZT薄膜元件之疲勞曲線的量測192
第5章 結論196
未來展望198
參考文獻199
附錄207
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