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研究生：	林建龍 Lin, Chain-Long
論文名稱：	鉍含量、氧化鉍緩衝層及鉭摻雜對化學溶液鍍著法生長鉍鑭鈦膜鐵電性質之影響 Effects of excess Bi concentration,buffered Bi2O3 layers,and Ta doping on the ferroelectricity of Bi3.25La0.75Ti3O12 Films Grown by chemical solution deposition
指導教授：	林文台 Lin, Wen-Tai
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：	2003
畢業學年度：	91
語文別：	中文
論文頁數：	124
中文關鍵詞：	鐵電性質、化學溶液鍍著法
外文關鍵詞：	chemical solution deposition, ferroelectricity
相關次數：	點閱：103 下載：1
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研究以化學溶液鍍著法生長Bi3.25La0.75Ti3O12(BLT)薄膜在不同過量百分比的鉍、Bi2O3緩衝層和添加不同計量比的鉭在退火溫度550-800度對其鐵電性之影響，同時添加鉭的部分又和射頻濺鍍法所長的互相比較。BLT薄膜在過量10 mol %有最佳鐵電性，而無Bi2O3緩衝層的BLT薄膜在550-800度為(117)而850度為c軸，當有Bi2O3在550-650度是顯著的(117)和(200)峰值而700則是c軸取向，除了Bi2O3緩衝層外，有機殘留物和在(001)BLT/Pt的低界面能是促使a-和c-軸生長的決定因素，在本實驗中塗有Bi2O3緩衝層採二階段退火可以製備最佳a-軸取向之BLT膜，此過程為第一次在550-650度而後在700-850度退火，a軸取向的BLT膜比任意或c-軸取向的BLT膜分別有較大的殘餘極化（2Pr）和較小的矯頑電場（2Ec）。這個結果可解釋沿a-軸有大的極化和Bi2O3緩衝層補償BLT膜在退火過程中鉍的損失，以CSD和sputter生長的BLT膜其殘餘極化（2Pr）隨添加鉭而減少，這個結果可被解釋由於鉭的添加而導致晶粒的變小。

Effects of excess Bi concentrations, buffered Bi2O3 layers, and Ta doping on the ferroelectricity of chemical-solution-deposited (CSD) Bi3.25La0.75Ti3O12 (BLT) films were studied as a function of annealing temperature in the range of 550-800℃. Meanwhile, Some Ta-doped BLT films were prepared using sputtered deposition for comparison. The BLT films with excess 10 mol % Bi showed the best ferroelectricity. The BLT films without buffered Bi2O3 layers showed a prominent (117) peak at 550-800℃ and c-axis-oriented growth at 850℃, while the BLT films with buffered Bi2O3 layers showed prominent (117) and (200) peaks at 550-650℃ and c-axis-oriented growth at 700℃. In addition to the buffered Bi2O3 layer, the hydrocarbon residue in the CSD BLT films and the lower interfacial energy of (001)BLT/Pt appear to be the crucial factors in enhancing the a- and c-axis-oriented growth of BLT films, respectively. In the present study, deposition of buffered Bi2O3 layers in conjunction with two-step annealing, i.e., first annealed at 550-650℃ and then annealed at 700-850℃, is a viable processing to fabricate well-crystallized BLT films with a-axis orientation. The BLT films with a-axis orientation showed a larger remanent polarization and a smaller coercive field than those with random or c-axis orientation, respectively. This result can be explained in terms of the large polarization along the a-axis orienation and buffered Bi2O3 layers which compensate the BLT films for Bi evaporation during annealing. For the CSD and sputtered BLT films the remanent polarization decreased with the doping concentration of Ta. This result can be explained in terms of the reduction of the grain size of the films due to Ta doping.

中文摘要……………………………………………………………Ⅰ
英文摘要……………………………………………………………Ⅱ
誌謝感言……………………………………………………Ⅲ
本文目錄……………………………………………………………Ⅳ
表目錄……………………………………………………………Ⅶ
圖目錄……………………………………………………………Ⅷ

本文	
第一章 簡介…………………………………………………1
1.前言…………………………………………………………1
1-1.電子記憶體………………………………………….....1
1-2.鐵電材料 ..…………………………………………….1
2.基本理論……………………………………………………6
2-1.極化理論……………..…………………………………6
    2-2.脈衝極化及疲勞量測………………………………8
    2-3.鐵電記憶體的讀寫原理……………………………9
3.Bi4-XLaXTi3O12（BLT）之基本結構………………………………10
4. 化學溶液鍍著法………………………………….…………………11
5.射頻濺鍍法…………………………….………………………12
5-1.濺鍍沈積原理 ..…….……………………………… 12
5-2.射頻濺鍍沈積 ..…….……………………………… 14
6.電子槍蒸鍍系統……………………………………………14
7.拉賽福背向散射儀 …………………………………..….…..16
8.研究理論基礎與動機..…………………………………….... 18
8-1. SBT鐵電薄膜 ………………………………………18
8-2.BTO與BLT鐵電薄膜……………………………….19
8-3.SBT與BTO和BLT鐵電薄膜………………………21
8-4.BTW與BTV鐵電薄膜………………………………21
8-5.本實驗研究動機—BLT和BLTT鐵電薄膜……….22
第二章 實驗步驟與方法……………………………………23
 1.實驗流程圖………………………………………...…….23
 2.溶液與靶材配置 ……..…………………………………….24
 3.基板（底電極）Pt/Ta/SiO2/Si製備…………………………25
 4.BLT和BLTT鐵電薄膜製備………………………………..25
 5.薄膜退火 .……………………………………………………26
 6.上電極製作 …………………………………………………26
 7.接觸退火 …………………………………………………….27
 8.鐵電性質量測與分析……………………………………….27
8-1.結晶相鑑定……………………………………………27
8-2.成分分析………………………………………………27
8-3.薄膜厚度與粗糙度測定……………………………..28
8-4.遲滯曲線、時效與疲勞量測………………………..28
8-5.漏電流量測……………………………………………28
第三章 結果與討論……………………………….……….....30
 1.不同百分比過量的鉍(Bi)………………………………….…..30
 2. 不同Bi2O3緩衝層對BLT薄膜方向性生長之影響………..….31
    2-1. Pt/BLT/Pt……….………………………………………31
    2-2. Pt/Bi2O3/BLT/ Bi2O3/Pt、Pt/Bi2O3/BLT/ Pt、Pt /BLT/ Bi2 O3 /Pt ………………………………………………………32
    2-3.不同方向性生長BLT薄膜之鐵電性質……….…………35
    2-4.不同厚度Bi2O3緩衝層對BLT膜鐵電性之影響………….36
 3.摻雜鉭對BLT薄膜鐵電性之影響………..…………………….37
    3-1.Pt/BLTT/Pt………………………………………..…….37
    3-2.Pt/Bi2O3/BLTTa/Bi2O3/Pt……………………………..….39
第四章 結論……………………………….………..........….42
參考文獻………………………………………….…...........44

表   目   錄
表（一）各種用於鐵電薄膜製作技術之特徵比較……………50
表（二）PZT,SBT,BLT薄膜以Pt為電極之鐵電性質比較…51

圖   目   錄
圖（一）遲滯曲線……………………………………………………...52
圖（二）製備鐵電薄膜的各種技術之發展…………………………...53
圖（三）鐵電陶瓷薄膜在元件上之應用……………………………...54
圖（四）鈦離子偏離中心形成電偶極………………………………...55
圖（五）（a）P-E遲滯曲線之操作電壓（b）脈衝極化測量之操作電壓（c）疲勞測試之操作電壓……………………………….56
圖（六）脈衝極化量測…………………………………………………57
圖（七）不同DRO記憶體電路構造，Cf, Cf1, Cf2為鐵電電容，T1,    T2, P1, P2, 1N1～N6為MOSFET …………………………..58
圖（八）2T-1C記憶晶胞電路圖………………………………………59
圖（九）讀寫電壓脈衝之操作………………………………………...60
圖（十）（a）PbBi2Nb2O9,（b）Bi4Ti3O12（c）BaBi4Ti4O15之一半擬正方晶體構造…………………………………………………..61
圖（十一）Bi3.25La0.75Ti3O12的晶格結構……………………………...62
圖 (十二) 旋轉器和執行程式………………………………………...62
圖（十三）（a）射頻濺鍍系統的示意圖（b）拉賽福背向散射儀俯視示意圖………………..........................................................63
圖（十四）10 mol %BLT試片退火後之RBS………………………...64
圖（十五）不同過量鉍之試片經700度退火之遲滯曲線比較圖….…65
圖（十六）不同過量鉍之試片經725度退火之遲滯曲線比較圖…….66
圖（十七）不同過量鉍之試片經750度退火之遲滯曲線比較圖……67
圖（十八）不同過量鉍之試片經725和750度退火下之2Pr和2Ec比較圖……………….……………………………………….68
圖（十九）10和30mol%鉍過量在750度退火後之晶粒TEM比較圖……….....……………………………………………….69
圖（二十）不同過量鉍之試片經725度退火之XRD圖…………...70
圖（二十一）不同過量鉍之試片經750度退火之XRD圖…………71
圖（二十二）0.075M十層Bi2O3緩衝層之TEM横截面圖……………72
圖（二十三） 10 mol%鉍過量Pt/BLT/Pt試片在不同溫度退火之XRD繞射圖….....…………………………………………….73
圖（二十四） 10 mol%鉍過量Pt/BLT/Pt試片二階段式退火先650度再不同溫度退火之XRD繞射圖……….……………74
圖（二十五） 10 mol%鉍過量Pt/BLT/Pt試片二階段式退火先650度再不同溫度退火之XRD繞射圖……………………75
圖（二十六）0.075M純Bi2O3膜在不同溫度退火之XRD繞射圖……76
圖（二十七）10 mol%鉍過量Pt/Bi2O3/BLT/Bi2O3/Pt試片在不同溫度退火之XRD繞射圖……………………………………77
圖（二十八）10 mol%鉍過量試片550度退火之(117)繞射綘的放大比較圖……………………………………………………..72
圖（二十九）10 mol%鉍過量不同Bi2O3緩衝層試片經700退火之XRD繞射圖…………………………………………………...78
圖（三十） 10 mol%鉍過量不同Bi2O3緩衝層試片的方向性程度和2Pr之比較圖……..…………………………………………79
圖（三十一）10 mol%鉍過量不同Bi2O3緩衝層試片(無上電極)經700度退火之XRD繞射圖…………………………………80
圖（三十二）以濺鍍法生長的BLT試片在不同溫度退火XRD繞射圖………………………………………………………..81
圖（三十三）10 mol%鉍過量不同優選方向試片之SEM圖………… 82
圖（三十四）10 mol%鉍過量Pt/Bi2O3/BLT/Bi2O3 Pt試片二階段式退火先650度再高溫退火XRD繞射圖….…….………..83
圖（三十五）10 mol%鉍過量不同優選取向在外加電場750kV/cm750度退火之遲滯曲線比較圖……………………………..84
圖（三十六）10 mol%鉍過量Pt/BLT/Pt試片750度退火之AES圖…..……………………………………………………85
圖（三十七）10 mol%鉍過量Pt/Bi2O3/BLT/Bi2O3 Pt試片750度退火之AES圖……………………………………………….86
圖（三十八）10 mol%鉍過量不同優選取向試片725度退火外加電壓5V之疲勞比較圖………………………………….…...87
圖（三十九）10 mol%鉍過量Pt/Bi2O 3/BLT/Bi2O/Pt試片725度退火電場5V之疲勞量測前後的遲滯曲線比較圖…………88
圖（四十） 10 mol%鉍過量Pt/BLT/Pt試片725度退火電壓5V之疲勞量測前後的遲滯曲線比較圖………………………..89
圖（四十一）10 mol%鉍過量Pt/Bi2O 3/BLT/Bi2O/Pt試片725度退火電壓5V之疲勞量測前後的遲滯曲線比較圖…………90
圖（四十二）10 mol%鉍過量不同優選取向試片750度退火外加電壓5V之疲勞比較圖………………………………………91
圖（四十三）10 mol%鉍過量Pt/Bi2O3/BLT/Bi2O3/Pt試片750度退火外加電壓5V之疲勞量測前後的遲滯曲線比較圖……92
圖（四十四）10 mol%鉍過量Pt/BLT/Pt試片750度退火外加電壓5V之疲勞量測前後的遲滯曲線比較圖...………………...93
圖（四十五）10 mol%鉍過量Pt/Bi2O3/BLT/Bi2O3/Pt試片750度退火外加電壓5V之疲勞量測前後的遲滯曲線比較圖……94
圖（四十六）10 mol%鉍過量有和無Bi2O3緩衝層試片750退火之漏電流比較圖………………..……………………………95
圖（四十七）10 mol%鉍過量不同厚度緩衝層在不同溫度的2Pr比較圖………………..……..………………………………..96
圖（四十八）10 mol%鉍過量不同厚度緩衝層試片經700度退火之XRD繞射圖…………………………………………………..97
圖（四十九）10 mol%鉍過量不同厚度緩衝層試片經700度退火之遲滯曲線比較圖…………………………………………..98
圖（五十） 10 mol%鉍過量不同厚度緩衝層試片經725度退火之XRD繞射圖…………………………………………………..99
圖（五十一）10 mol%鉍過量不同厚度緩衝層試片經725度退火之遲滯曲線比較圖…………………………………………100
圖（五十二）10 mol%鉍過量不同厚度緩衝層試片經750度退火之XRD繞射圖….……………………………………………...101
圖（五十三）10 mol%鉍過量不同厚度緩衝層試片經750度退火之遲滯曲線比較圖…………………………………………102
圖（五十四）10 mol%鉍過量不同厚度緩衝層試片經750度退火之SEM圖………………………………………………………104
圖（五十五）化學溶液鍍著法10 mol%鉍過量不同鉭含量試片經750度退火之SEM圖…………..…………………………105
圖（五十六）濺鍍法生長不同鉭含量試片經750度退火之SEM圖…107
圖（五十七）化學溶液鍍著法生長10 mol%鉍過量不同鉭含量試片經700度退火之XRD繞射圖……………………………108
圖（五十八）濺鍍法生長不同鉭含量試片經700度退火之XRD繞射圖………………………………………………………109
圖（五十九）化學溶液鍍著法生長10 mol%鉍過量不同鉭含量試片700和750度退火之2Pr比較圖………………………….110
圖（六十）濺鍍法生長不同鉭含量試片700和750度退火之2Pr比較圖………………………………………………………111
圖（六十一）化學溶液鍍著法生長不同含量試片700度退火之(117)繞射峰的放大比較圖…………………………………112
圖（六十二）濺鍍法生長不同鉭含量試不同Ta含量之試片700度退火之(117)繞射峰的放大比較圖………………………112
圖（六十三）化學溶液鍍著法BLT和BLTT 0.03兩試片750oC退火外加電壓5V之疲勞比較圖……………………………..113
圖（六十四）濺鍍法BLT和BLTT0.05兩試片750oC退火外加電壓5V之疲勞比較圖………….…………………….………..114
圖（六十五）化學溶液鍍著法BLT試片750度退火外加電場5V之疲勞量測前後的遲滯曲線比較圖………………………115
圖（六十六） 化學溶液鍍著法BLTT0.03試片750度退火外加電壓5V在疲勞量測前後之遲滯曲線比較圖…………………116
圖（六十七） 濺鍍法BLTT試片750度退火外加電壓5V在疲勞量測前後之遲滯曲線比較圖………………………………117
圖（六十八）濺鍍法BLTT0.05試片750度退火外加電壓5V在疲勞量測前後之遲滯曲線比較圖……………………………118
圖（六十九）濺鍍法BLTT0.01試片750度退火在外加電壓5V之漏電流圖形……….………….……………………………..119
圖（七十）濺鍍法BLTT0.01試片不同溫度退火之XRD繞射圖……120
圖（七十一） 濺鍍法BLTT0.01試片不同Bi2O3緩衝層經700度退火之XRD繞射圖…………...………………………………121
圖（七十二）濺鍍法BLTT0.01試片不同Bi2O3緩衝層其方向性程度和2Pr之比較圖………..…………………………………122
圖（七十三）濺鍍法Pt/Bi2O3/BLTT/ Bi2O3/Pt試片二階段退火先低溫再700度退火之XRD繞射圖…………………………123
圖（七十四）濺鍍法BLTT0.01試片不同Bi2O3緩衝層經750度退火之SEM圖………………………………………………...124
                                    

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