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系統識別號 U0026-0812200911491527
論文名稱(中文) 複合型鈣鈦礦Ba1-xAx(Fe0.5Nb0.5)1-x/4O3 (A=La、Bi)之介電性質研究
論文名稱(英文) The Dielectric Properties of Complex Perovskite Oxide of Ba1-xAx(Fe0.5Nb0.5)1-x/4O3 (A=La、Bi) at Low Frequencies
校院名稱 成功大學
系所名稱(中) 材料科學及工程學系碩博士班
系所名稱(英) Department of Materials Science and Engineering
學年度 94
學期 1
出版年 95
研究生(中文) 鍾朝宇
研究生(英文) Chao-Yu Chung
電子信箱 n5890113@ccmail.ncku.edu.tw
學號 n5890113
學位類別 博士
語文別 中文
論文頁數 133頁
口試委員 指導教授-張炎輝
口試委員-林諭男
口試委員-王木琴
口試委員-楊文都
口試委員-吳南均
口試委員-陳引幹
口試委員-洪茂鋒
中文關鍵字 超高電容  鐵電性質  介電材料 
英文關鍵字 High capacitor  Ferroelectric properties  Dielectric material 
學科別分類
中文摘要 本研究是以複合型鈣鈦礦結構之Ba(Fe0.5Nb0.5)O3(BFN)材料為探討對象,並以高價數之La及Bi離子來取代Ba離子,製備成Ba1-xAx(Fe0.5Nb0.5)1-x/4O3(A=La、Bi)之複合型鈣鈦礦鐵電陶瓷體。本研究主要由三個部分所組成:(1)以溶膠-凝膠法合成Ba(Fe0.5Nb0.5)O3粉末並以旋轉塗佈法製備成薄膜;(2)以固態反應法製備Ba1-xLax(Fe0.5Nb0.5)1-x/4O3及其性質研究;(3)以固態反應法製備Ba1-xBix(Fe0.5 Nb0.5)1-x/4O3及其性質研究。
本研究成功的以溶膠-凝膠法合成Ba(Fe0.5Nb0.5)O3之複合型鈣鈦礦鐵電陶瓷。膠體在550℃煅燒5小時後即開始形成BFN相結構,而溫度提高到850℃則會得到單一的BFN之鈣鈦礦結構,且粉末的顆粒大小均約35nm,其結晶活化能與晶體成長活化能分別為64.25 kJ/mol和32.94 kJ/mole。此外,Ba(Fe0.5Nb0.5)O3鐵電陶瓷在1150℃~1250℃的燒結溫度下發現,鐵電性質的變化會受晶粒大小所影響,晶粒越大則鐵電性質越佳,其介電常數及介電損失在100Hz下,分別為12000與0.3。在薄膜方面,利用旋轉塗佈方式將Ba(Fe0.5Nb0.5)O3鐵電陶瓷沈積在Pt/Ti/SiO2/Si基板上,經550℃熱處理後形成單一之鈣鈦礦之結構,並且Ba(Fe0.5Nb0.5)O3鐵電薄膜經過550℃~700℃熱處理後,其殘留極化為0.3μC/cm2,而矯頑電場會隨著熱處理溫度增加而電場從160 kV/cm下降至120 kV/cm。
以兩階段固態反應法合成Ba1-xAx(Fe0.5Nb0.5)1-x/4O3(A=La、Bi)之複合型的鈣鈦礦鐵電陶瓷。BLFN及BBFN陶瓷分別在1350℃燒結4小時以及1250℃燒結1小時皆可獲得最佳的介電性質。Ba0.92La0.08(Fe0.5Nb0.5)0.98O3陶瓷在頻率1kHz及溫度在233~470K之介電常數為4x104~8x105,而Ba0.9Bi0.1(Fe0.5Nb0.5)0.975O3陶瓷在1kHz及溫度在233~470K之介電常數為2x104~3x105。不論是BLFN或BBFN其介電性質均隨頻率的減少而增加,這意味著這兩種介電陶瓷均為典型之鐵電材料,且在低頻範圍時擁有大量的方向極化以及空間電荷極化。此外在燒結過程中由於氧空缺在晶界或在晶粒的擴散速度不同,導致晶界的阻抗遠大於晶粒,因此而形成所謂晶界層電容。
英文摘要 The present investigation focused on the Ba(Fe0.5Nb0.5)O3, which has an perovskite structure. The ferroelectric ceramic Ba(Fe0.5Nb0.5)O3 powders doped with trivalence La and Bi ions (BLFN、BBFN) were synthesized. The experimentation consists of three parts as: Ba(Fe0.5Nb0.5)O3 powders prepared using sol-gel method, Ba(Fe0.5Nb0.5)O3 prepared by solid state reaction, synthesis and characterization of Ba1-xLax(Fe0.5Nb0.5)1-x/4O3 and Ba1-xBix (Fe0.5Nb0.5)1-x/4O3.
The Ba(Fe0.5Nb0.5)O3 ferroelectric ceramic has been successful synthesized by sol- gel method. In experiment, the crystallization of Ba(Fe0.5Nb0.5)O3 powders begins at 550℃ and the pure perovskite phase was obtained as the powder heat-treated at 850℃. The average grain size of Ba(Fe0.5Nb0.5)O3 powders were about 35 nm. The activation energy of crystallization and grain growth for Ba(Fe0.5Nb0.5)O3 is 64.25 kJ/mol and 32.94 kJ/mole, respectively. In addition, increase sintering temperature can be found a large grain size and it has better ferroelectric properties. As the samples were sintered at 1250℃, a dielectric constant, ε’max, of ~12000 and loss tangent of ~0.3 were obtained at 100 Hz. The Ba(Fe0.5Nb0.5)O3 gel was then spin-coated on the Pt/Ti/SiO2/Si substrates. The single phase was obtained as the thin films annealed at 550℃ for 30 min. The Ba(Fe0.5Nb0.5)O3 ferroelectric thin film annealed at 550℃~ 700℃, the remnant polarization keep around 0.3 μC/cm2, but coercive field decreases from 160 kV/cm to 120 kV/cm.
The complex perovskite oxides, Ba1-xAx(Fe0.5Nb0.5)1-x/4O3 (A=La,Bi), were fabricated by two stages solid-state reaction. In this experimental data obtained show very high values of dielectric permittivity in a wide temperature range that is inherent to so-called high-k materials. The dielectric constant is about 4x104~8x105 at 300~440K with a low dissipation factor for the sample with La=8 mole% sintered at 1350℃ for 4h, measured at 1 kHz. For the sample with Bi=10mole% sintered at 1250℃ for 1h the dielectric constant of about 2x104~3x105 with a low dissipation factor were obtained. The dielectric behavior of both the BLFN and BBFN increase with decreasing frequency. The dielectric behaviours of these materials were contributed by orientational and space charge polarizations. High oxygen diffusion coefficient at the grain boundaries leads to the extent of oxidation and higher resistivities in the grain boundary layers. The grain boundary-layeral capacitance was thus produced.
論文目次 摘要………………………………………………………………………I
Abstract……………………………………………………………………III
致謝………………………………………………………………………V
目錄………………………………………………………………………VI
表目錄……………………………………………………………………IX
圖目錄……………………………………………………………………X
第一章 諸論………………………………………………………………1
1-1.前言……………………………………………………………………1
1-2.鈦酸鋇之介電材料……………………………………………………2
1-3.研究動機………………………………………………………………3
1-4.研究目的………………………………………………………………4
第二章 基礎理論……………………………………………………………7
2-1.介電理論…………………………………………………………………7
2-1-1.介電特性……………………………………………………………7
2-1-2.極化機構……………………………………………………………7
2-1-3.介電損失……………………………………………………………8
2-2.鐵電理論…………………………………………………………………9
2-2-1.基本特性……………………………………………………………9
2-2-2.結構變化對鐵電性質的影響………………………………………10
2-2-3.鐵電材料應用………………………………………………………11
2-3.複合型鈣鈦礦之結構…………………………………………………12
2-3-1.有序-無序排列………………………………………………………12
2-3-2.弛緩性質……………………………………………………………13
2-4.能障型電容……………………………………………………………14
2-5 阻抗分析原理……………………………………………………………15
2-6 溶膠-凝膠法……………………………………………………………19
2-6-1 基本原理……………………………………………………………19
2-6-2 溶膠-凝膠製成主要步驟……………………………………………20
2-6-3 Pechini …Process……………………………………………………21
2-6-4 鍍膜方式……………………………………………………………22
2-6-5 溶膠-凝膠製程之憂缺點……………………………………………22
2-7 固態反應法……………………………………………………………23
2-7-1 固態反應機構………………………………………………………23
2-7-2 固態反應法之優點…………………………………………………24
2-8 晶粒大小測定…………………………………………………………24
第三章 實驗方法……………………………………………………………38
3-1 實驗方法………………………………………………………………38
3-2 實驗藥品………………………………………………………………38
3-3 溶膠-凝膠製程…………………………………………………………38
3-4 鐵電薄膜的製作………………………………………………………38
3-4-1. Pt/Ti/SiO2/Si 基板之準備……………………………………………39
3-4-2. 薄膜之旋鍍…………………………………………………………39
3-4-3. 上電極之製作………………………………………………………39
3-5. 固態反應法………………………………………………………………40
3-6. 結構與成份分析…………………………………………………………40
3-6-1. X光繞射分析………………………………………………………40
3-6-2. 密度量測………………………………………………………………40
3-6-3. 掃瞄式電子顯微鏡分析……………………………………………41
3-6-4. 穿透式電子顯微鏡分析……………………………………………41
3-6-5. 傅立葉轉紅外線光譜分析…………………………………………41
3-6-6. 熱差/熱重及示差掃瞄熱量分析……………………………………42
3-7. 性質量測…………………………………………………………………42
3-7-1. 介電性質量測………………………………………………………43
3-7-2. 阻抗分析量測………………………………………………………43
3-7-3. 電阻率量測…………………………………………………………43
3-7-4. P-E曲線量測…………………………………………………………43
第四章 結果與討論…………………………………………………………48
4-1. 以溶膠-凝膠法製備Ba(Fe0.5Nb0.5)O3…………………………………48
4-1-1. 傅立葉轉紅外線光譜分析…………………………………………48
4-1-2. 熱差/熱重分析………………………………………………………49
4-1-3. Ba(Fe0.5Nb0.5)O3粉末之X光繞射分析……………………………50
4-1-4. 結晶活化能分析……………………………………………………51
4-1-5. 晶粒尺寸與晶粒成長活化能…………………………………………51
4-1-6. 穿透式電子顯微鏡分析……………………………………………52
4-1-7. 鐵電性質分析……………………………………………………53
4-1-8. Ba(Fe0.5Nb0.5)O3薄膜之X光繞射分析……………………………54
4-1-9. SEM截面及表面分析………………………………………………55
4-1-10. 介電性質分析………………………………………………………56
4-1-11. 結論…………………………………………………………………57
4-2. 以固態反應法製備Ba1-xLax(Fe0.5Nb0.5)1-x/4O3………………………79
4-2-1. Ba1-xLax(Fe0.5Nb0.5)1-x/4O3之X光繞射分析………………………79
4-2-2. 密度量測…………………………………………………………….80
4-2-3. SEM表面微結構分析………………………………………………81
4-2-4. 介電性質分析……………………………………………………….82
4-2-5. 阻抗分析量測……………………………………………………….85
4-2-6. 結論…………………………………………………………………86
4-3. 以固態反應法製備Ba1-xBix(Fe0.5Nb0.5)1-x/4O3……………………96
4-3.1. Ba1-xBix(Fe0.5Nb0.5)1-x/4O3之結晶結構…………………………96
4-3.2. 掃瞄式電子顯微鏡分析……………………………………………97
4-3.3. 穿透式電子顯微鏡分析……………………………………………98
4-3.4. 介電性質分析………………………………………………………99
4-3.5. 阻抗分析量測………………………………………………………102
4-3.6. 結論…………………………………………………………………103
4-4. 綜合討論………………………………………………………………120
第五章 總結論………………………………………………………………122
參考文獻.……………………………………………………………………124
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