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研究生：	張志嘉 Chang, Chih-Chia
論文名稱：	摻雜鑭、矽之鐵酸鉍多鐵性薄膜製備與特性之研究 Fabrication and Characterization of Si-doped or La-doped BiFeO3 Multiferroics Thin Films
指導教授：	洪敏雄 Hon, Min-Hsiung
學位類別：	碩士 Master
系所名稱：	工學院 - 材料科學及工程學系 Department of Materials Science and Engineering
論文出版年：	2006
畢業學年度：	94
語文別：	中文
論文頁數：	119
中文關鍵詞：	多鐵性、鐵酸鉍
外文關鍵詞：	Multiferroic, BiFeO3
相關次數：	點閱：60 下載：2
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鐵酸鉍(BiFeO3，BFO)之多鐵性薄膜，具有優異磁電共存特性可用於記憶體、可調式感測器以及自旋電晶體，尤其在記憶體設計上引起廣泛的興趣。由於BFO 有極高的漏電流導致無法在室溫下量測到飽和電滯曲線，故本研究利用化學溶液鍍膜法(chemical solution deposition)製備Si與La摻雜之BFO 薄膜於鎳酸鑭下電極基板(LaNiO3/Si)，以期降低漏電流的產生，並探討摻雜對薄膜之晶體結構、介電特性、鐵電性質、鐵磁性質之影響。
由於Si 離子半徑與Fe 離子半徑差異太大，導致Si 摻雜之BFO 薄膜需於高溫熱處理後，才可驅使Si4+離子取代Fe3+離子於B site 位置。從XRD結果得知650℃熱處理下易有Bi2Fe4O9 雜相生成於BFO 薄膜中，且Si 之溶
解度約為5 mole%。Si 摻雜可使BFO 薄膜緻密化、晶粒細化、降低孔洞生成以及表面粗糙度，導致其低頻介電損耗遠小於BFO，而具有較低之孔洞與缺陷存在，故5 mole% Si 摻雜可使BFO 薄膜漏電流密度從1.58×10-4
(A/cm2) 降至 1.09×10-7 (A/cm2)，因而在室溫下可量測到BFO 薄膜之電滯曲線，其殘留極化值與矯頑場分別為2.94 μm/cm2 以及100.1 kV/cm。此外亦發現殘留磁化率與矯頑磁場隨著Si 摻雜量上升而顯著增加的趨勢。
La 的摻雜可抑制Bi2Fe4O9 雜相生成而使介電常數呈現上升趨勢；但當La 摻雜量達15 mole% 時，由於晶粒呈現不連續性導致低頻之介電損耗大幅增加，最終使得漏電流大幅增加。10BLFO 可得到La 摻雜之BFO 系列的最低漏電流為2.02×10-5(A/cm2)，但僅較BFO 薄膜之漏電流小一個數量級，因而無法在室溫下量測到完整的電滯曲線。薄膜的殘留磁化量隨著La 摻雜量的增加而提升，但矯頑磁場則呈現下降趨勢。

Multiferroics BiFeO3 (BFO) thin films which simultaneously coexists ferroelectricity and antiferromagnetism, have attracted extensively attention to applying on memory, tunable sensor and spin transistor. Because of the significant leakage of BiFeO3, the ferroelectric hysteresis can’t measure at room temperature. Si-doped and La-doped BFO thin films were deposited LaNiO3/Si
substrates by chemical solution method in this study. Doping effects on crystal structure, leakage current, dielectric, ferroelectric and magnetic properties were investigated.
Because the radius of Si4+ ion was much smaller than that of Fe3+, a high temperature annealing process was necessary to induce Si4+ ion to substitute Fe3+ ion. The annealing temperature for Si-doped BFO thin films was 650℃, but the impurity phase (Bi2Fe4O9) was always occured in BFO thin films. The solubility
of Si ion was about 5 mole%. Si-doped in BFO thin films would make films dense, reduce crystal size, vacancies, and surface roughness. From dielectric analyses, 5BFSO thin films got a smallest tanδ at low frequency. That’s why
leakage current densities of 5BFSO thin films were reduced from 1.58×10-4 (A/cm2) to 1.09×10-7 (A/cm2). The remnant polarization and coercive field of 5BFSO thin films which measured at room temperature were 2.94 (μm/cm2) and 100.1(kV/cm), respectively. The remnant magnetization and coercive magnetic field were increased with increasing the amounts of Si-doped in BFO thin films.
The dopant of La would inhibit the formation of Bi2Fe4O9 phase, resulting in increasing dielectric constant. But as the amounts of La-doped in BFO thin films were increased to 15 mole%, grains appeared to be discontinuous. That’s the reason why 15BLFO had a large leakage current density. 10BLFO had the
lowest leakage current density of 2.02×10-5(A/cm2) for La-doped in BFO thin films. But this value was still too high to have complete P-E analyses. The remnant magnetization increased as the amounts of La-doped in BFO thin films
increased, but the coercive magnetic field was decreased as the amounts of La-doped in BFO thin films increased.

第一章 緒論...................................................................1
1-1 前言..................................................................... 1
1-2 研究動機................................................................. 2
第二章 文獻回顧...............................................................3
2-1 鐵電材料簡介............................................................. 3
2-1-1 鈣鈦礦型之鐵電材料..................................................... 3
2-1-2 鐵電晶域與電滯曲線..................................................... 6
2-2 磁性物質簡介............................................................. 8
2-3 極化現象與介電特性...................................................... 12
2-4 漏電流機制.............................................................. 15
2-5 氧化物LaNiO3 電極....................................................... 17
2-6 多鐵性材料.............................................................. 19
2-7 BiFeO3 材料簡介......................................................... 22
2-7-1 BiFeO3 晶體結構....................................................... 22
2-7-2 BiFeO3 電性簡介....................................................... 25
2-7-3 BiFeO3 磁性簡介....................................................... 28
第三章 實驗方法與步驟........................................................30
3-1 實驗材料................................................................ 30
3-1-1 實驗藥品.............................................................. 30
3-1-2 基材清洗.............................................................. 31
3-2 LaNiO3（LNO）下電極製備................................................. 32
3-3 BiFeO3 (BFO) 薄膜製備方法............................................... 33
3-3-1 BiFeO3 化學溶液調配................................................... 33
3-3-2 旋轉塗佈與熱處理...................................................... 33
3-3-3 Pt/BFO/LNO 與 Pt/BFO/Pt 鐵電電容元件製作.............................. 34
3-4 BFO 薄膜特性檢測........................................................ 37
3-4-1 低掠角X-ray (Glancing angle XRD，GIXRD)............................... 37
3-4-2 場發掃描式電子顯微鏡(FESEM)........................................... 37
3-4-3 光電子能譜分析儀(X-ray Photo-electron Spectroscopy，XPS).............. 38
3-4-4 原子力顯微鏡(AFM)..................................................... 38
3-4-5 熱重/熱差分析(TG/DTA)................................................. 38
3-5 Pt/BFO/LNO 與Pt/BFO/Pt 鐵電電容電性檢測................................. 39
3-5-1 漏電流(I-V)測試....................................................... 39
3-5-2 介電常數-介電損耗測試(C-F)............................................ 39
3-5-3 電滯曲線 (P-E)........................................................ 39
3-6 磁性量測................................................................ 41
3-6-1 超導量子干涉儀 (SQUID) ............................................... 41
第四章 矽離子與鑭離子摻雜對BiFeO3 (BFO) .....................................42
薄膜性質之影響...............................................................42
4-1 熱處理溫度對LNO 下電極之影響............................................ 42
4-2 基板對BiFeO3 薄膜性質之影響............................................. 46
4-2-1 基板對BiFeO3 薄膜之晶體結構影響....................................... 46
4-2-2 基板對BiFeO3 薄膜微觀型態之影響....................................... 47
4-2-3 基板對BiFeO3 薄膜介電特性之影響....................................... 49
4-2-4 基板對BiFeO3 薄膜漏電流之影響......................................... 57
4-3 矽離子摻雜對BFO 薄膜之多鐵性質之影響.................................... 59
4-3-1 BiFe1-xSxO3 的熱性質.................................................. 59
4-3-2 BiFe1-xSixO3 薄膜晶體結構與分析....................................... 61
4-3-3 矽摻雜對BFO 薄膜表面形貌之影響........................................ 66
4-3-4 BiFe1-xSixO3 薄膜化學鍵結分析......................................... 72
4-3-5 BiFe1-xSixO3 薄膜之介電特性........................................... 78
4-3-6 BiFe1-xSixO3 薄膜的漏電流分析......................................... 82
4-3-7 BiFe1-xSixO3 薄膜的鐵電性質........................................... 84
4-3-8 BiFe1-xSixO3 薄膜之磁性性質........................................... 88
4-4 鑭離子摻雜對BFO 薄膜之影響.............................................. 92
4-4-1 Bi1-xLaxFeO3 薄膜之晶體結構與分析..................................... 92
4-4-2 Bi1-xLaxFeO3 薄膜之微觀結構........................................... 93
4-4-3 Bi1-xLaxFeO3 薄膜之介電特性........................................... 97
4-4-4 Bi1-xLaxFeO3 薄膜的漏電流分析......................................... 99
4-4-5 Bi1-xLaxFeO3 薄膜的鐵電性質.......................................... 100
4-4-6 Bi1-xLaxFeO3 薄膜之磁性性質.......................................... 100
4-4-7 熱處理溫度對Bi1-xLaxFeO3 薄膜之影響.................................. 105
第五章 結論.................................................................110
第六章 參考資料.............................................................112
                                    

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