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研究生：	林千琪 Lin, Chien-chi
論文名稱：	摻雜矽之鉍釹鈦鐵電薄膜製備與特性 Fabrication and Characterization of Si-doped Bi3.5Nd0.5Ti3O12 Ferroelectric 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：	2007
畢業學年度：	95
語文別：	中文
論文頁數：	129
中文關鍵詞：	矽、鉍釹鈦、鐵電薄膜
外文關鍵詞：	Bi3.5Nd0.5Ti4O12, ferroelectric thin film, Si
相關次數：	點閱：87 下載：1
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中文摘要
鉍釹鈦(Bi3.5Nd0.5Ti3O12 ,BNT)為一種層狀鈣鈦礦結構之鐵電薄膜，具有優異的鐵電性質，多用於非揮發性記憶體元件。本文主要研究摻雜矽之鉍釹鈦鐵電薄膜製備與特性。利用化學溶液鍍膜法(Chemical solution deposition，CSD)於鎳酸鑭電極基板(LaNiO3/Si)上鍍覆所得到之鐵電薄膜，探討Si摻雜對於薄膜晶體結構、介電特性、漏電流特性以及鐵電性質之影響。
Si摻雜於BNT薄膜可使結晶溫度降低、晶粒細化、表面粗糙度下降。而薄膜之電性易受結晶指向之影響，所以本研究再利用分層結晶(layer-by-layer crystallization)的熱處理方式，於鎳酸鑭電極基板上可製作出具有(117)與(200)優選指向之薄膜。藉由Si摻雜以及分層結晶熱處理製作出的BNT薄膜，漏電流明顯的獲得改善(J<10-8)。於650℃分層結晶熱處理溫度下Si摻雜量為x=0.01時，可得到較佳的鐵電以及介電性質，殘存極化量(2Pr)為6.0(μC/cm2)，矯頑電場(Ec)為29.2kV/cm，於頻率1MHz下介電常數為236，而散逸因子0.015。

Abstract
Bi3.5Nd0.5Ti3O12(BNT) thin films of layered perovskite structure, which is currently used as capacitor material in ferroelectric memory. Si-doped BNT ferroelectric thin films was investigated in this research. The thin films were prepared on LaNiO3/Si using chemical solution deposition (CSD) technique. The crystal structure, dielectric, leakage current and ferroelectric properties of Si-doped BNT thin films were examined in this work.
Silicon (Si)-substituted BNT thin films are expected to reduce the processing temperature and show good surface morphology with relatively small grain. The electric properties of thin films depended on crystal orientation. The Bi3.5Nd0.5Ti3-xSixO12(BNTS) thin films grown on LNO/Si substrate derived with layer-by-layer crystallization exhibit preferred (117) and (200) orientation and reduce leakage current densities about 10-8 A/cm2.
The best ferroelectric and dielectric properties were observed for Bi3.5Nd0.5Ti2.99Si0.01 O12 thin films derived with layer-by-layer crystallization annealed at 650℃, was measured to have a dielectric constant of 236, dielectric loss of 0.015, remanent polarization (2Pr) of 6.0(μC/cm2), and coercive field of 29.2kV/cm.

總目錄
中文摘要…………………………………………………………………Ⅰ
英文摘要…………………………………………………………………Ⅱ
誌謝感言…………………………………………………………………Ⅲ
總目錄……………………………………………………………………Ⅳ
圖目錄……………………………………………………………………Ⅷ
表目錄……………………………………………………………………ⅩⅣ

第一章  緒論……………………………………………………………1
   1-1  簡介……………………………………………………………1
   1-2  鐵電材料的發展………………………………………………1
   1-3  研究動機………………………………………………………2
第二章  文獻回顧………………………………………………………5
   2-1  鐵電材料………………………………………………………5
      2-1-1 晶體結構與特性…………………………………………5
      2-1-2 鐵電材料的特性…………………………………………7
      2-1-3 鈣鈦礦結構………………………………………………8
      2-1-4 鐵電晶域與電滯曲線……………………………………10
      2-1-5 鐵電記憶體的操作原理…………………………………12
   2-2  層狀鈣鈦礦結構………………………………………………16
      2-2-1 鉭酸鍶鉍鐵電薄膜………………………………………16
      2-2-2 鈦酸鉍鐵電薄膜…………………………………………16
        2-2-2-1 鈦酸鉍添加鑭系元素………………………………19
        2-2-2-2 Si摻雜………………………………………………20  
   2-3  鐵電薄膜的製作方式…………………………………………21
   2-4  電極……………………………………………………………23
      2-4-1 金屬電極…………………………………………………23
      2-4-2 鈣鈦礦結構之氧化物電極………………………………23
   2-5  極化現象與介電特性…………………………………………25
      2-5-1 介電損耗…………………………………………………29
   2-6  漏電流機制……………………………………………………31
第三章  實驗方法與步驟………………………………………………34
3-1  實驗流程圖……………………………………………………34
3-2  鐵電電容下電極基板之製備…………………………………35
3-2-1  LaNiO3/Si基板之製備…………………………………35
3-3  Bi3.5Nd0.5Ti3-xSixO12鐵電薄膜的製備 …………………………38
3-3-1  Bi3.5Nd0.5Ti3-xSixO12溶液的配製…………………………38
3-3-2  Bi3.5Nd0.5Ti3-xSixO12鍍膜被覆與熱處理…………………39
   3-4  Pt上電極之製作………………………………………………43
3-5  鐵電薄膜的特性檢測 …………………………………………44
   3-5-1 多功能X光薄膜繞射儀(XRD)……………………………44
   3-5-2 場發射掃描式電子顯微鏡(SEM)…………………………44
   3-5-3 歐傑電子光譜儀(AES)……………………………………44
      3-5-4 原子力顯微鏡(AFM)………………………………………45
      3-5-5 熱重/熱差分析(TG/DTA)…………………………………45
   3-6  Pt/BNTS/LNO鐵電電容之電性量測……………………………46
      3-6-1 漏電流量測…………………………………………………46
      3-6-2 介電特性量測………………………………………………46
      3-6-3 電滯量測……………………………………………………46
第四章  問題與討論………………………………………………………49
  4-1  Si摻雜Bi3.5Nd0.5Ti3O12薄膜性質…………………………………49
      4-1-1 Bi3.5Nd0.5Ti3-xSixO12晶體之熱性質…………………………49
      4-1-2 Bi3.5Nd0.5Ti3-xSixO12薄膜晶體結構…………………………53
      4-1-3 Bi3.5Nd0.5Ti3-xSixO12薄膜表面微結構………………………59
      4-1-4 Bi3.5Nd0.5Ti3-xSixO12薄膜漏電流……………………………70
  4-2  分層結晶製備BNTSx薄膜 ………………………………………75
      4-2-1 分層結晶BNTSx薄膜的晶體結構…………………………76
      4-2-2 分層結晶BNTSx薄膜表面微結構…………………………82
      4-2-3 分層結晶BNTSx薄膜漏電流特性…………………………87
      4-2-4 分層結晶BNTSx薄膜之介電特性…………………………90
      4-2-5 分層結晶BNTSx薄膜之鐵電特性…………………………95
第五章  結論 ……………………………………………………………100
參考資料..……………….…………………………………………………102













圖目錄
Fig.2-1 The relationship of paraelectricity, piezoelectricity, pyroelectricity 
      and ferroelectricity…………………………………………………6
Fig.2-2 ABO3 perovskite unit cell …………………………………………9
Fig.2-3 Ionic displacements in PZT ……………………………………….9
Fig.2-4 Hysteresis loop of a ferroelectric material ………………………..14
Fig2-5 One Transistor-One Capacitor (1T-1C) of FRAM cell structure……15
Fig.2-6 Lattice structure of the Strontium bismuth tantalite ………………17
Fig.2-7 Lattice structure of the bismuth titanate…………………………...18
Fig.2-8 Schematic representation of different mechanisms of polarization.
       …………………………………………………….………………26
Fig.2-9 Frequency dependence of several contributions to the polarization.
       …………………………………………………….………………28
Fig.2-10 I-V phase of dielectric material……………………………………30
Fig.3-1 The process for preparing Pt/BNTS/LNO/Si ferroelectric device.
       ……………………………………………………………………..34
Fig.3-2 The cleaning process of silscon wafer  ……………………………35
Fig.3-3 The process for preparing LNO electrode by chemical solution
method………….……………………………………………………37
Fig.3-4 The spin coating process...…………………………………………..40
Fig.3-5 The process for preparing BNTSx thin films by chemical solution 
      method…………………….…………………………………………41
Fig.3-6 The process for preparing BNTS thin films prepared with 
      layer-by-layer crystallization..……………………………………….42
Fig.3-7 The final structural drawing of BNTS device...……………………..43
Fig.3-8 Schematic drawing of HP-4140 testingsystem .…………………….47
Fig.3-9 Schematic drawing of HP-4284A multi-frequency LCR meter.
      …………………………………………………….…………………47
Fig.3-10 Schematic drawing of IBM computer controlled RT-66A testing 
       system………………………………………………………………48
Fig.4-1 DTA/TG analysis of BNT with a heating rate of 10℃/min in air.
       ………………………………………….…………………………..51
Fig.4-2 DTA/TG analysis of BNTSx (x=0.1) with a heating rate of 
      10℃/min in air…………………………………..…………………..52
Fig.4-3 X-ray diffraction patterns of BNTSx (x=0, 0.03, 0.05, 0.1) thin   
      films grown on LNO/Si substrate as annealed at 600℃ for 1 hr. 
      ………………………………………………………………………55
Fig.4-4 X-ray diffraction patterns of BNTSx (x=0, 0.03, 0.05, 0.1) thin   
      films grown on LNO/Si substrate as annealed at 650℃ for 1 hr. 
      ………………………………………………………………………56
Fig.4-5 X-ray diffraction patterns of BNTSx (x=0, 0.03, 0.05, 0.1) thin   
      films grown on LNO/Si substrate as annealed at 700℃ for 1 hr. 
      ………………………………………………………………………57
Fig.4-6 The α intensity of BNTS(x=0, 0.03, 0.05, 0.1) thin films grown on
      LNO/Si substrate as annealed at different temperature for 1 hr. 
      ………………………………………………………………………58
Fig.4-7 SEM surface and cross section micrographs of (a) BNT (b) BNTSx 
(x=0.03) (c) BNTSx (x=0.05) (d) BNTSx (x=0.1) thin films grown on 
LNO/Si substrate as annealed at 600℃ for 1 hr……………………..61
Fig.4-8 AFM 2-D images and surface roughness of (a) BNT (b) BNTSx 
(x=0.03) (c) BNTSx (x=0.05) (d) BNTSx (x=0.1) thin films grown on LNO/Si substrate as annealed at 600℃ for 1 hr……………...……...63 
Fig.4-9 SEM surface and cross section micrographs of (a) BNT (b) BNTSx 
(x=0.03) (c) BNTSx (x=0.05) (d) BNTSx (x=0.1) thin films grown on 
LNO/Si substrate as annealed at 650℃ for 1 hr……………………..64 
Fig.4-10 AFM 2-D images and surface roughness of (a) BNT (b) BNTSx 
(x=0.03) (c) BNTSx (x=0.05) (d) BNTSx (x=0.1) thin films grown on 
LNO/Si substrate as annealed at 650℃ for 1 hr………………...….66 
Fig.4-11 SEM surface and cross section micrographs of (a) BNT (b) BNTSx 
(x=0.03) (c) BNTSx (x=0.05) (d) BNTSx (x=0.1) thin films grown on 
LNO/Si substrate as annealed at 700℃ for 1 hr..…………………..67 
Fig.4-12 AFM 2-D images and surface roughness of (a) BNT (b) BNTSx 
(x=0.03) (c) BNTSx (x=0.05) (d) BNTSx (x=0.1) thin films grown on 
LNO/Si substrate as annealed at 700℃ for 1 hr………..…………..69
Fig.4-13 The leakage current density-electric field(J-E) behavior of 
       BNTS(x=0, 0.03, 0.05, 0.1) thin films grown on LNO/Si 
       substrate as annealed at 600℃ for 1 hr………………………...…..72
Fig.4-14 The leakage current density-electric field(J-E) behavior of 
       BNTS(x=0, 0.03, 0.05, 0.1) thin films grown on LNO/Si 
       substrate as annealed at 650℃ for 1 hr………………………...…..73
Fig.4-15 The leakage current density-electric field(J-E) behavior of 
       BNTS(x=0, 0.03, 0.05, 0.1) thin films grown on LNO/Si 
       substrate as annealed at 700℃ for 1 hr……………………...……..74 
Fig4-16 X-ray diffraction patterns of BNTSx (x=0, 0.01, 0.03, 0.1) thin   
      films grown on LNO/Si substrate derived with layer-by-layer crystallization annealed at 650℃………………………………...….78
Fig4-17 X-ray diffraction patterns of BNTSx (x=0, 0.01, 0.03, 0.1) thin   
      films grown on LNO/Si substrate derived with layer-by-layer crystallization annealed at 700℃………………………………...….79
Fig 4-18 The detail scan of (117) diffraction of BNTSx (x=0, 0.01, 0.03, 0.1) 
       thin films annealed at (a) 650℃ (b) 700℃ on LNO/Si substrate 
       derived with layer-by-layer crystallization…………………...…….80
Fig.4-19 SEM micrographs of (a) BNT (b) BNTSx (x=0.01) (c) BNTSx 
(x=0.03) (d) BNTSx (x=0.1) thin films grown on LNO/Si substrate 
derived with layer-by-layer crystallization annealed at 650℃.
       ………………………………………………………………..…….83
Fig.4-20 AFM 2-D images and surface roughness of (a) BNT (b) BNTSx 
(x=0.01) (c) BNTSx (x=0.03) (d) BNTSx (x=0.1) thin films 
derived with layer-by-layer crystallization annealed at 650℃. 
       …………………………………………………………………...…84
Fig.4-21 SEM micrographs of (a) BNT (b) BNTSx (x=0.01) (c) BNTSx 
(x=0.03) (d) BNTSx (x=0.1) thin films grown on LNO/Si substrate 
derived with layer-by-layer crystallization annealed at 700℃.
       ………………………………………………………………….….85
Fig.4-22 AFM 2-D images and surface roughness of (a) BNT, (b) BNTS(x=0.01), (c) BNTS(x=0.03), (d) BNTS(x=0.1) thin
 films derived with layer-by-layer crystallization annealed at 700℃. 
       …………………………………………………………………..….86
Fig.4-23 The leakage current density-electric field(J-E) behavior of 
       BNTS(x=0, 0.01, 0.03, 0.1) thin films derived with layer-by-layer 
       crystallization annealed at 650℃…………………………….…….88 
Fig.4-24 The leakage current density-electric field(J-E) behavior of 
       BNTS(x=0, 0.01, 0.03, 0.1) thin films derived with layer-by-layer 
       crystallization annealed at 700℃……………………………..……89 
Fig.4-25 Dielectric properties of BNTS(x=0, 0.01, 0.03, 0.1) thin films 
       grown on LNO/Si substrate derived with layer-by-layer 
       crystallization annealed at 650℃……………………………….….92
Fig.4-26 Dielectric properties of BNTS(x=0, 0.01, 0.03, 0.1) thin films 
       grown on LNO/Si substrate derived with layer-by-layer 
       crystallization annealed at 700℃…………………………………..93
Fig.4-27 Dielectric constant of BNTS(x=0, 0.01, 0.03, 0.1) thin films 
       grown on LNO/Si substrate derived with layer-by-layer 
       crystallization annealed at different temperature………………..…94
Fig.4-28 Polarization hysteresis loops for (a) BNT, (b) BNTS(x=0.01), 
       (c) BNTS(x=0.03), (d) BNTS(x=0.1) thin films derived with
layer-by-layer crystallization annealed at 650℃……………….…..96
Fig.4-29 The relation between double remanent polarization (2Pr) for BNTS(x=0, 0.01, 0.03, 0.1) thin films annealed at 650℃…………97 
Fig.4-30 Polarization hysteresis loops for (a) BNT, (b) BNTS(x=0.01), 
       (c) BNTS(x=0.03), (d) BNTS(x=0.1) thin films derived with
layer-by-layer crystallization annealed at 700℃……………….…..98 
Fig.4-31 The AES images of BNTS(x=0.1) thin films derived with
layer-by-layer crystallization annealed at 700℃ …………………99














表目錄
Table 1-1 Comparison between FRAM and other Memories…………...…4
Table 2-1 The technology requirements of FeRAM……………………..…13
Table 3-1 Detail chemical information about the precursors of LNO…..….36
Table 3-2 Detail chemical information about the precursors of BNTSx……38
Table 4-1 The lattice constant of BNTS(x=0, 0.01, 0.03, 0.1)  
        thin films annealed at 650℃……………………………….……81
Table 4-2 The lattice constant of BNTS(x=0, 0.01, 0.03, 0.1)  
        thin films annealed at 700℃………………………………….…81
                                    

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