鐵酸鉍複鐵式薄膜之晶體成長與分析｜國立清華大學博碩士論文庫

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研究生：	李奕賢 Yi-Hsien Lee
論文名稱：	鐵酸鉍複鐵式薄膜之晶體成長與分析 Crystal growth and characterizations of multiferroic BiFeO3 thin Films
指導教授：	吳振名 Jenn-Ming Wu
口試委員:
學位類別：	博士 Doctor
系所名稱：	工學院 - 材料科學工程學系 Materials Science and Engineering
論文出版年：	2005
畢業學年度：	94
語文別：	英文
論文頁數：	209
中文關鍵詞：	複鐵式、鐵電性、磁電、磊晶、鐵酸鉍
外文關鍵詞：	Multiferroic, Ferroelectric, Magnetoelectric, Epitaxial, Bismuth Ferrite
相關次數：	點閱：2 下載：0
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鐵酸鉍(BiFeO3，BFO)複鐵式材料，具結構、電、磁的序化而同時具有鐵電性(Tc~1100K)及反鐵磁特性(TN~640K)，其優異的鐵電/壓電性以及獨特的磁電共存特性，引起廣泛的研究。本文主要研究BFO薄膜之晶體結構、化學組態、電性、磁性及奈米檢測。藉由射頻磁控濺鍍法(RF-magnetron sputtering)低溫製備純鈣鈦礦結晶相之BFO薄膜，隨機晶向,(100)及(111)優選晶向之晶體結構分別於白金基版(Pt/TiOx/SiO2/Si，Pt)，鎳酸鑭基板(LaNiO3/Pt/TiOx/SiO2/Si，LNO)及鉛酸鋇基板(BaPbO3/Pt/TiOx/SiO2/Si，BPO)上多晶成長，於鎳酸鑭電極及鐵酸鑭緩衝層之氧化鎂單晶基版(LaNiO3/LaFeO3/MgO)異質磊晶成長(100)指向之磊晶薄膜，藉由改變基版及底電極材料得到不同晶體結構之純相BFO薄膜。
BFO薄膜之化學組態，明顯受到工作壓力及製程溫度的影響，藉由適當控制製程參數，可得到穩定的薄膜化學組態。並探討薄膜晶向對高優選BFO薄膜於晶體成長、表面形貌、電性及磁性的影響，藉由掃描式穿透顯微鏡之高角度環型暗場顯像術(Scanning Transmission Electron Microscope High-Angle Annular Dark-Field，STEM-HAADF)分析薄膜/電極介面及薄膜化學均勻性。藉由掃描式壓電力顯微鏡 (Scanning Probe Microscopy，SPM)，探討奈米尺度下的物性及電性。藉由添加鑭(La)元素，改善薄膜結晶性及表面粗糙度，部分取代鉍原子造成晶格體積的增加，造成介電、鐵電及磁特性的增進。

Multiferroics BiFeO3 (BFO), exhibiting simultaneously ferroelectricity (Tc~1100K) and anti-ferromagnetism (TN~640K), have attracted extensively attention for their coupled electric, magnetic, and structure order parameters in the same phase. The crystal structure, chemical configuration, nanoscale characterization, electric and magnetic properties were investigated is this study. The pure perovskite phase of BFO films were deposited by rf-magnetron sputtering at low processing temperature. The crystal structure of the BFO films was significantly influenced by the substrate and the bottom electrodes. The BFO film was grown with random orientation on Pt/TiOx/SiO2/Si (Pt), whereas highly (100)- and (111)-oriented ones were obtained on LaNiO3/Pt/TiOx/SiO2/Si (LNO) and BaPbO3/Pt/TiOx/SiO2/Si (BPO), respectively. The BFO-based films were hetero-epitaxially grown on the LaNiO3/LaFeO/MgO single crystal substrates.
The chemical configuration of the films, which significantly depended on working pressure and temperature, was enhanced by well-controlled processing parameters. The orientation dependence in the crystal growth, electric properties and magnetic behavior of BFO films were examined. The film/electrode interface and chemical homogeneity of the films were characterized by the scanning transmission electron microscope high-angle annular dark-field imaging (STEM-HAADF). Nanoscale characterization of the BFO films was studied by scanning probe microscopy (SPM). With the partial substitution of lanthanum (La) ions for bismuth ions, the significant enhancement in the dielectric, ferroelectric and magnetic performance of BFO films was attributed to the improved crystallinity, smooth surface, and increased lattice volume.

ABSTRCT (Chinese)                                         I
ABSTRCT (English)                                       III
ACKNOWLEDGEMENT (Chinese)                                 V
CONTENTS                                                VII
LIST OF TABLES                                         XIII
LIST OF FIGURES                                         XIV

1. Introduction                                            1
1.1 Multiferroic BiFeO3 materials                          1
1.2 Motivation                                             3
1.3 Outline of the Dissertation                            5

2. Background study                                        6
2.1 Electric properties of ferroelectric materials         7
2.1.1.Perovskite structure                                 7
2.1.2. Symmetry and electric properties in the perovskite  9
2.1.3. Ferroelectricity                                   10
2.1.4. Piezoelectricity                                   12
2.1.5. Dielectric and ferroelectric theory                13
2.1.6. Domain structure                                   15
2.1.7. Reliability of ferroelectric materials             17
2.2 Magnetism of materials                                19
2.2.1 Magnetism in transition-metal-based ionic crystals  19
2.2.2 Direct exchange                                     21
2.2.3 Super-exchange                                      23
2.2.4 Phenomenon of exchange bias                         23
2.3 Multiferroic materials                                25
2.3.1 The coexistence of ferroelectric and magnetic order 25
2.3.2 Single-phase multiferroic materials                 29
2.3.3 Multiferroic composite and heterostructure          30
2.3.4 Magnetoelectric coupling phenomenon                 32
2.4 BiFeO3 materials                                      33
2.4.1 Crystal structure                                   33
2.4.2 Electric characteristics                            34
2.4.3 Magnetic characteristics                            36
2.4.4 Major challenge                                     39

3. Experimental procedures                                51
3.1 Substrate system and sample structure                 51
3.1.1 Pt / TiOx / Ti / SiOx / Si substrate                51
3.1.2 Sample structure                                    51
3.2 Preparation of electrodes                             52
3.2.1 Platinum upper electrode                            52
3.2.2 LaNiO3 bottom electrode                             52
3.2.3 BaPbO3 bottom electrode                             53
3.3 Fabrication of BiFeO3–based thin films               53
3.4 Hetero-epitaxial growth                               54
3.4.1 BiFeO3/LaNiO3/ LaFeO3/MgO(100)                      54
3.4.2 BiFeO3/LaNiO3 / STO                                 54
3.3.3 BiFeO3/BaPbO3 / STO                                 54
3.5 Characterization                                      55
3.4.1 Structure analysis                                  55
A. X-ray Diffraction (XRD)                                55
B. Scanning Transmission Electron Microscopy (STEM)       55
C. Scanning Electron Microscope (SEM)                     56
3.4.2 Chemical analysis                                   56
A. Auger Electron Spectroscopy (AES)                      56
B. X-ray Photoelectron Spectroscopy (XPS)                 57
C. Energy Dispersive X-ray Spectroscopy (EDS)             57
3.4.3 Electric analysis                                   57
A. Leakage measurement                                    58
B. Dielectric measurement                                 58
C. Ferroelectric measurement                              58
3.4.4 Magnetic analysis                                   59
A. Vibration Sample Microscopy (VSM)                      59
3.4.5 Nano-scaled characterization                        59
A. Atomic Force Microscopy (AFM)                          59
B. Piezoresponse Force Microscopy (PFM)                   60

4. Low-temperature growth and surface chemistry of BiFeO3 thin films                                                69
4.1 Introduction                                          69
4.2 Experimental Details                                  70
4.3 Results and discussion                                72
4.3.1 Crystal growth and microstructure of BiFeO3 thin films                                                     72
A. Temperature effect                                     72
B. Working pressure effect                                73
C. Ar/O2 ratio effect                                     75
D. Target stoichiometry                                   76
4.3.2 Surface chemistry of BiFeO3 thin films              77
A. Temperature effect                                     77
B. Working pressure effect                                77
4.4 Conclusion.                                           79

5. Crystal growth, interface characterization and multiferroic   properties of the highly oriented BiFeO3 thin films                                                89
5.1 Introduction                                          89
5.2 Experimental Details                                  91
5.3 Results and discussion                                92
5.3.1 Crystal growth of highly oriented BiFeO3 films      92
5.3.2 Interface characterization of highly oriented BiFeO3 films                                                     93
5.3.3 Orientation effect in multiferroic properties       95
A. Leakage behavior                                       95
B. Dielectric properties                                  97
C. Ferroelectric properties                               97
D. Magnetic properties                                    98
E. NiFe/BFO heterostructure                               98
5.4 Conclusion                                           101

6. The influence of La-doping in multiferroic properties of BiFeO3 films                                             118
6.1 Introduction                                         118
6.2 Experimental Details                                 120
6.3 Results and discussion                               121
6.3.1 The La-substitution effect in crystal structure    121
6.3.2 The La-substitution effect in surface morphology   122
6.3.3 The La-substitution effect in electric properties  122
6.3.4 The La-substitution effect in ferroelectric reliability                                              124
6.3.5 The La-substitution effect in magnetic properties  125
6.4 Conclusion                                           125

7. Nanoscale characterizations of BiFeO3 thin films      134
7.1 Introduction                                         134
7.2 Experimental Details                                 135
7.3 Results and discussion                               137
7.3.1 Hysteresis measurement of randomly oriented BFO film                                                     137
7.3.2 The influence of crystalline orientation in domain structure of BiFeO3 films                                139
7.3.3 Poling of the BiFeO3 films                         141
7.4 Conclusion.                                          143

8. Epitaxial growth of the La-substituted BiFeO3/LaNiO3 hetero-structure films                                   153
8.1 Introduction                                         153
8.2 Experimental Details                                 155
8.3 Results and discussion                               155
8.3.1 Crystal structure of the of the hetero-structure films                                                    155
8.3.2 Surface morphology of the hetero-structure films   157
8.3.3 Multiferroic properties of the of the hetero-structure film                                           158
8.4 Conclusion                                           161

9. Conclusion                                            172

Appendix 1 Epitaxial growth of LaFeO3 thin films         176
A.1 Introduction                                         176
A.2 Experimental Details                                 178
A.3 Results and discussion                               180
A.3.1 Crystal structure                                  180
A.3.2 Chemical configurations                            182
A.3.3 Surface morphology                                 183
A.4 Conclusion                                           184


References                                               191
Publications                                             208

                                

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