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研究生：	詹智忠 Chan, Chih-chung
論文名稱：	尋找軟磁性材料用與鐵酸鉍作磁交換作用 Finding soft magnetic material intended for magnetic exchange coupling with BFO
指導教授：	齊孝定 Qi, Xiao-ding
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：	2008
畢業學年度：	96
語文別：	中文
論文頁數：	93
中文關鍵詞：	鐵酸鉍、軟磁性材料
外文關鍵詞：	BiFeO3, soft magnetic material
相關次數：	點閱：69 下載：4
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鐵酸鉍(BiFeO3，BFO)為一種多鐵體材料，鐵酸鉍同時具有鐵電性(Tc~1100K)及反鐵磁特性(TN~640K)，比單一具有鐵電性或單一具有鐵磁性材料多出一個可控制之變數，因而引起高度的重視。本研究為設法找出一軟磁性氧化物，用與BFO做磁交換偶合，作為自旋閥門之應用，為了避免和BFO產生界面化學反應，適合使用具有(1)高的飽和磁化率 (2)小的矯頑場(3)高於室溫之居里溫度等條件之磁性氧化物。
實驗中以NiFe2O4、ZnFe2O4、Ni0.5Zn0.5Fe2O4、Ni0.2Zn0.3Fe2.5O4、Ni0.3Zn0.2Fe2.5O4、Ni0.7Zn0.3Fe2O4和Ni0.3Zn0.7Fe2O4等靶材，以磁控濺射法於室溫下沉積薄膜，再以高溫和不同氣氛下退火以促使相的形成。製備好之薄膜以X光繞射儀 (XRD)、振動樣品磁力計(VSM)和場發射式掃描式電子顯微鏡(FE-SEM)等儀器進行測試。結果發現成分為Ni0.3Zn0.7Fe2O4在空氣中10500C退火能得到最好之性質，飽合磁化率為986.3 emu/cm3，矯頑場為37 Oe，適於用來與BFO進行磁偶合作用。

BiFeO3 (BFO) is simultaneously ferroelectric (Tc~1100K) and antiferromagnetic (TN~640K). It has one more controllable variable for device applications than ordinary ferroelectrics or antiferromagnets and therefore has attracted a broad interest recently. This research was intended to find a soft oxide ferromagnet to be used for exchange interaction with BFO for spin valve applications. In order to avoid interface chemical reaction with BFO, an oxide ferromagnet is preferred, which also needs to be: (1) high saturated Magnetization,(2) low coercive field, and (3) above room temperature Curie temperature.
In this study, Ni0.5Zn0.5Fe2O4、NiFe2O4、ZnFe2O4、Ni0.2Zn0.3Fe2.5O4、Ni0.7Zn0.3Fe2O4,and Ni0.3Zn0.7Fe2O4 have been grown by magnetron sputtering. The films were first deposited at room temperature, and the desired phase was formed after sintering at high temperatures in various atmospheres, including air, argon and oxygen. The prepared films were characterized by x-ray diffraction, vibrating sample magnetrometry, scanning electron microscopy, etc. It was found that Ni0.3Zn0.7Fe2O4 sintered in air at 10500C had the best properties that we search for. The saturated magnetization was 986.3 emu/cm3 and the coercive field was 37 Oe, which is suitable for exchange bias with BFO.

中文摘要....................................................................................................................................................I
Abstract...................................................................................................................................................II
總目錄....................................................................................................................................................III
表目錄......................................................................................................................................................VI
圖目錄.....................................................................................................................................................VII
第一章  緒論................................................................................................................................................1
1-1前言.....................................................................................................................................................1
1-2 研究動機與目地..........................................................................................................................................4
第二章  文獻探討............................................................................................................................................5
2-1 簡介複鐵式材料（Multi-ferro Materials）....................................................................................................5
2-1-1  極化.................................................................................................................................................8
2-1-2 BFO基本特性..........................................................................................................................................10
2-2 鎳鋅鐵氧磁體...........................................................................................................................................13
2-3 磁性來源...............................................................................................................................................18
2-4 濺鍍原理...............................................................................................................................................21
2-5 薄膜沉積原理.....................................................................................................................................25
2-6 薄膜顯微結構...........................................................................................................................................27
2-7 晶格匹配...............................................................................................................................................30
2-8 自旋閥簡介.............................................................................................................................................32
第三章  實驗及儀器介紹.....................................................................................................................................35
3-1實驗規劃................................................................................................................................................35
3-2 靶材製作...............................................................................................................................................37
3-3  退火處理..............................................................................................................................................41
3-4 試片製作與清洗.........................................................................................................................................42
3-5 濺鍍設備...............................................................................................................................................43
3-6分析儀器................................................................................................................................................44
3-6-1 表面粗度儀...........................................................................................................................................44
3-6-2 X-ray繞射分析儀......................................................................................................................................45
3-6-3 低掠角X光薄膜繞射[27]................................................................................................................................46
3-6-4 場發射型掃描式電子顯微鏡（field emission scanning electron microscopy,FESEM）.............................50
3-6-5 原子力顯微鏡(Atomic Force Microscopy, AFM)....................................................................51
3-6-6 樣品震動磁力計（vibrating sample magnetometer, VSM）...................................................................52
3-6-7 化學分析電子光譜法(electron spectroscopy for chemical  analysis，ESCA):光電子光譜法(XPS)..............54
第四章  結果與討論.........................................................................................................................................55
4-1 靶材分析...............................................................................................................................................55
4-2 低掠角X光分析..........................................................................................................................................58
4-3 磁性分析...............................................................................................................................................63
4-3-1 改變靶材成份.........................................................................................................................................65
4-3-2 改變退火溫度.........................................................................................................................................69
4-3-3  改變氣氛對磁特性之影響....................................................................................................................73
4-4 SEM分析................................................................................................................................................74
4-5 膜厚分析...............................................................................................................................................78
4-6 AFM分析................................................................................................................................................81
4-7 ESCA...................................................................................................................................................84
第五章 結論................................................................................................................................................87
參考資料...................................................................................................................................................89

 
表目錄
Table 1-1 不同記憶體的特性比較[1]...............................................................................................2
Table 2-1 各種鐵氧體的主要特性和應用範圍比較[18]............................................................................13
Table 2-2 陶鐵磁體中陽離子位置...............................................................................................17
Table 2-3 電漿內所包含的各種反應...............................................................................................23
Table 3-1 鐵化學計量比等於2.5之靶材成分表...............................................................................................38
Table 3-2 鐵化學計量比等於2之靶材成分表...............................................................................................38
Table 4-1 Fe化學計量=2.5之飽和磁化及矯頑磁場.................................................................................66
Table 4-2 Fe化學計量=2之飽和磁化及矯頑磁場........................................................................................66
Table 4-3 Ni0.3Zn0.7Fe2O4不同退火溫度之飽和磁化及矯頑場比較...........................................................70
Table 4-4 Ni0.5-Zn0.5 ferrite隨溫度之MS、HC變化[36]................................................................................71
Table 4-5 不同氣氛之ＭＳ比較................................................................................................73
Table 4-6 不同成分濺鍍速率................................................................................................78
Table 4-7 Ni0.3Zn0.7Fe2O4靶濺鍍60分鐘氣體流量與膜厚之關係..........................................................79
Table 4-8 不同退火處理表面之粗糙度................................................................................................82

 
圖目錄
Fig.2-1 典型鐵電電滯曲線(hysteresis loop curve)和ABO3 鈣鈦礦結構圖[12]...............................................7
Fig.2-2 四種極化機制........................................................................................................................................9
Fig.3-1 實驗流程圖.........................................................................................................................................36
Fig.3-2 鎳鋅鐵氧體靶材製作流程........................................................................................................39
Fig.3-3 靶材燒結升溫曲線...................................................................................................................................40
Fig.3-4 基板清洗步驟.......................................................................................................................................42
Fig.3-5 低掠角X光繞射法的幾何關係示意圖...............................................................................................48
Fig.3-6 低掠角X光繞射法之西蒙-鮑林繞射裝置示意圖..................................................................................48
Fig.3-7 原子力顯微鏡原理示意圖...........................................................................................................51
Fig.3-8 樣品震動磁力計示意圖[28]........................................................................................................53
Fig.4-1 化學計量比Fe=2.5之靶材x-ray.........................................................................................................57
Fig.4-2 化學計量比Fe=2之靶材x-ray.........................................................................................................57
Fig.4-3 Ni0.2Zn0.3Fe2.5O4薄膜掠角X-RAY(A)空氣中 (B)Ar氣中 (C) Ar+H2混合氣體中退火800℃持溫兩小時..................................................................................................................................................................60
Fig.4-4 Ni0.3Zn0.7Fe2O4、Ni0.7Zn0.3Fe2O4 及Ni0.5Zn0.5Fe2O4空氣中1050℃持溫兩小時退火...........60
Fig.4-5 燒結1250℃晶格常數隨Fe比例之變化[33].................................................................................61
Fig.4-6 燒結1250℃晶格常數隨Ni比例之變化[33].................................................................................62
Fig.4-7 燒結1250℃晶格常數隨Zn比例之變化[33].................................................................................62
Fig.4-8 不同成分之磁滯曲線.................................................................................................................................65
Fig.4-9  Ms及Hc隨Zn2+濃度變化之曲線..................................................................................67
Fig.4-10 Yin Liu和Tai Qiu不同成分之比較[35]................................................................................67
Fig.4-11 不同退火溫度之M-H曲線及橫軸放大圖..................................................................................70
Fig.4-12 不同退火溫度之飽和磁化及矯頑場之比較...................................................................................71
Fig.4-13 根據Liu Yin和Qiu Tai所作之Table 4-4畫成之曲線圖[36].....................................................72
Fig.4-14 Ni0.5-Zn0.5 ferrite 不同溫度之磁滯曲線在室溫下所測[36]....................................................72
Fig.4-15 不同氣氛之M-H曲線.................................................................................................................................73
Fig.4-16 Ni0.2Zn0.3Fe2.5O4 40000倍及80000倍之SEM空氣中800℃持溫兩小時..............................................75
Fig.4-17 Ni0.3Zn0.7Fe2O4  650℃空氣中退火持溫兩小時之SEM圖.....................................................................75
Fig.4-18 Ni0.3Zn0.7Fe2O4 850℃空氣中退火持溫兩小時之SEM圖.....................................................................76
Fig.4-19 Ni0.3Zn0.7Fe2O4 1050℃空氣中退火持溫兩小時之SEM圖...................................................................76
Fig.4-20 Ni0.2Zn0.3Fe2.5O4  EDS分析，空氣中800℃持溫兩小時基板為SrTiO3.......................................77
Fig.4-21 濺鍍速率膜厚與濺鍍時間關係圖........................................................................................................79
Fig.4-22 (a) 300℃持溫2 HR (b) 300℃持溫0.5 HR (c)空氣中退火.................................................................81
Fig.4-23 不同退火處理之AFM圖片大小為3μm × 3μm (a) 56.8 nm，300℃ Ar+H2持溫2HR再升至850℃ (b) 18.05 nm，300℃ Ar+H2持溫0.5HR再升至850℃
         (c) 7.273 nm，空氣中850℃退火(d) 2.864 nm，未退火..............................................................83
Fig.4-24 Ni0.3Zn0.7Fe2O4 能譜圖.............................................................................................85
Fig.4-25 Ni0.3Zn0.7Fe2O4  Fe 2p 能譜圖及Fe2O3標準能譜圖[38]..........................................85
Fig.4-26 Ni0.3Zn0.7Fe2O4  Ni 2p 能譜圖及NiO標準能譜圖[38]....................................................86
Fig.4-27 Ni0.3Zn0.7Fe2O4  Zn 2p 能譜圖及ZnO標準能譜圖[38]....................................................86
                                    

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