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研究生:吳弘仁
研究生(外文):Hung-Jen Wu
論文名稱:雙離子束濺鍍系統及後退火處理製備鐵鉑/氧化錳雙層膜之微結構與磁性質研究
論文名稱(外文):The microstructure and magnetism of FePt/Mn-Oxide thin films by ion-beam bombardment and annealing
指導教授:林克偉林克偉引用關係
口試委員:蔡佳霖孫安正
口試日期:2011-05-04
學位類別:碩士
校院名稱:國立中興大學
系所名稱:材料科學與工程學系所
學門:工程學門
學類:材料工程學類
論文種類:學術論文
論文出版年:2011
畢業學年度:99
語文別:中文
論文頁數:100
中文關鍵詞:鐵鉑磁性質雙離子束
外文關鍵詞:FePtmagnetismion-beam bombardment
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本實驗在超高真空下以磁控濺鍍的方式製備 10 nm 之磁性FePt 薄膜於熱氧化
的Si 基板上,爾後以雙離子束濺鍍系統(Dual Ion Beam Assisted Deposition)於其薄
膜表面上鍍置不同氧含量(8~41%O2/Ar)的氧化錳(MnOx 10nm),並將試片在超高真
空磁控濺鍍之腔體經過退火處理。
此研究主要第一部分在探討在離子濺鍍系統中改變氧含量時,氧化錳(MnOx)
薄膜對鐵鉑(FePt)磁性層微結構與磁性質方面的影響。根據X 光繞射的分析結果顯
示,其結構在經過550oC 退火之後,皆由非序化的面心立方(fcc 相)轉變為序化的
面心正方(fct 相)(a~3.80 Å , c~3.67 Å ),在序化度方面當氧含量為8%O2/Ar 有最大值
(S~0.85)。電子顯微鏡之明視野圖形與繞射圖形結果顯示在10 分鐘退火後,氧化
錳(MnOx)可能形成晶界(grain boundary)將鐵鉑(FePt)有效的分散。從磁性質分析顯
示,當氧含量為8%O2/Ar,具有最大矯頑磁力,其垂直膜面的矯頑磁力分別為7.8
kOe。而隨著氧含量的變化,晶格常數並無太大的變化。從研究結果發現,當氧含
量為較低時,其鐵鉑(FePt)晶格中的間隙位置可能會因為退火後被氧原子所占據,
因此內部的應力會使得序化度的提高,但是由電子顯微鏡圖及MFM 圖指出分散的
鐵鉑(FePt)顆粒由於在磁化過程中受到的阻礙有限,因此矯頑磁力有明顯的下降,
然而當氧含量過高時,會使得氧原子成為擴散阻礙,而限制鐵鉑晶粒的成長,而
當氧含量高於21%O2/Ar 時,過多的氧原子可視為一缺陷,而此缺陷的存在會造成
矯頑磁力些許的上升。
第二部分則主要在探討在超高真空磁控之腔體,當氧含量固定8%O2/Ar,經
過不同退火溫度變化時,氧化錳(MnOx)薄膜對FePt 磁性層微結構與磁性質方面的
影響。依據X 光繞射的分析結果顯示,其鐵鉑/氧化錳(FePt-MnOx 8%O2/Ar)結構於
350℃及400℃仍為非序化之面心立方(fcc 相),當退火溫度達550℃以上時,其結
構由非序化的fcc 相轉變為序化的面心正方(L10 FePt)相,在序化度方面當溫度為
550℃時有最大值(S~ 0.85),然而隨著退火溫度上升,序化度亦隨之下降。電子顯
微鏡明視野圖形結果顯示鐵鉑/氧化錳(FePt-MnOx)顯示在經過550oC、10 分鐘退火
後,其頂層MnOx 可能形成晶界(grain boundary)將FePt 有效的分散。在磁性質分
析顯示,具有最大矯頑磁力,其垂直膜面的矯頑磁力為6.9 kOe。從電子顯微鏡圖
形證實隨著退火溫度升高而鐵鉑(FePt)晶粒的成長(15~25nm),造成反向磁區
(reversed domain)聚集,而磁區結合(domain mucleation process)造成磁翻轉機制改變
(magnetization maechanism),因此才會造成隨著退火溫度的上升,其矯頑磁力亦隨
之下降。

In our research, the magnetic properties and structure of Fe-Pt thin on SiO2
substrate film are strongly affected by capped different layers prepared ion-beam
bombardment and post-annealing. In this study, the co-sputtered FePt films (10 nm) on
thermal oxide SiO2 substrates were prepared by a UHV magnetron sputtering System at
first. The capping Mn-oxide layers (10 nm) were deposited on top of FePt film by using
the dual ion-beam deposition technique in the mixture of O2/Ar gas varied from 8% to
41%O2/Ar. All samples were post annealed at 550oC for 10 mins in UHV chamber.
Then, the highest ordering parameter of samples is 8%O2/Ar FePt/MnOx bilayers, so
other samples prepared by IBAD with 8%O2/Ar were annealed in UHV chamber with
different heat treatment condition. The Effect of top oxide capped layer and annealing
temperature on microstructure and magnetism in FePt thin film was analyzed and
discussed.
As-deposited FePt/MnOx bilayer exhibited a magnetically soft fcc phase, and it
turned to an ordered fct FePt phase with large coercivity (~8 kOe) after annealing at 550
oC. Increasing the %O2/Ar in capped MnOx layer during deposition resulted in smaller
ordered FePt grains separated by grain boundaries of MnOx. We found that the
superlattice (001) peak was broadened considerably with larger amount of MnOx
incorporated into FePt, likely due to the hindered formation of hard phase.Our results
indicate that for FePt/MnOx films deposited with lower %O2/Ar, the oxygen atoms may
occupy the interstitial positions in the FePt lattice to induce a local strain thus enhancing
the FePt ordering. Further increase in %O2/Ar in capped MnOx layer will result in the
excess oxygen atoms acting as a diffusion barrier which effectively inhibits the FePt
grain growth and ordering.
In the part of different anneal temperature, the FePt-MnOx (8% O2/Ar) annealed at
300°C and 400oC show similar structure as as-deposited. Further increasing the
annealing temperatures from 400 to 550 oC resulted in structural phase transformation
from fcc FePt to fct FePt (a~3.80 Å ,c~3.69 Å ), indicating the onset of structural phase
transformation occurred at a temperature higher than 400 oC. In this study, the higher
annaealing temperature resulted that magnetization reversal mechanism is controlled by
domain nucleation process and leads to the formation of polycrystalline films, which
give more chances to nucleation of reversed domains. The decrease of Hc at Ta above
550oC may partly be attributed to change in reversal mechanisms.

致謝 .................................................................................................................................. I
摘要 .................................................................................................................................II
Abstract ........................................................................................................................... III
目錄 ............................................................................................................................... IV
圖目錄 ............................................................................................................................ VI
表目錄 ............................................................................................................................ XI
第一章 緒論 .................................................................................................................... 1
1-1 研究背景................................................................................................................... 1
1-2 研究動機................................................................................................................... 4
1-3 理論基礎................................................................................................................... 5
1-3-1 高密度磁記錄媒體之要求............................................................................... 5
1-3-2 垂直式記錄媒體方式與優點........................................................................... 6
1-3-3 FePt 合金的特性.............................................................................................. 8
1-3-4 合金化學序化(chemical ordering) ................................................................... 9
1-4 文獻回顧.................................................................................................................. 11
第二章 實驗方法與步驟 .............................................................................................. 22
2-1 實驗設計與流程...................................................................................................... 22
2-2 基材前處理.............................................................................................................. 23
2-3 試片準備與退火處理.............................................................................................. 23
2-4 磁控濺鍍系統簡介.................................................................................................. 25
2-5 雙離子束濺鍍系統簡介.......................................................................................... 26
第三章 儀器原理及分析原理簡介 .............................................................................. 32
3-1 結構量測與分析:.................................................................................................... 32
垂直面低略角 X 光繞射儀(In-Plan GID X-Ray Diffractometer)............................ 32
3-2 薄膜顯微結構分析................................................................................................. 35
高解析度穿透式電子顯微鏡(High-Resolution Transmission Electron Microscope,
HRTEM ) ................................................................................................................... 35
3-3 薄膜磁性分析......................................................................................................... 40
(1)震動樣品磁力計(Vibrating sample magnetometer-VSM)................................... 40
(2)震動樣品磁力計(初始曲線(initial curve)) .......................................................... 42
(3)磁力顯微鏡(Magnetic force microscopy-MFM) ................................................. 42
3-4 成份分析................................................................................................................. 46
X 射線光電子能譜儀(X-ray Photoelectron Spectroscope-XPS) ............................. 46
第四章 結果與討論 ...................................................................................................... 48
4-1 初鍍膜FePt-MnOx (8, 15, 21, 30, 41%O2/Ar)薄膜微結構之觀察....................... 48
4-1-1 XRD 繞射分析(初鍍FePt-MnOx)................................................................. 48
4-1-2 Lattice constant ................................................................................................ 48
4-1-3 HR-TEM 分析(初鍍膜FePt-MnOx)............................................................... 49
4-2 FePt(10nm) / MnOx(10nm)雙層薄膜之改變氧含量效應..................................... 51
4-2-1 氧含量效應對薄膜微結構的影響.................................................................. 53
4-2-2 HR-TEM 分析................................................................................................. 57
4-2-3 VSM 分析....................................................................................................... 62
4-2-4 AFM/MFM 分析.............................................................................................. 68
4-2-5 XPS 分析......................................................................................................... 70
4-3 FePt(10nm)/MnOx(10nm)(8%O2/Ar)雙層薄膜之改變不同退火溫度效應.......... 77
4-3-1 退火溫度效應對薄膜微結構的影響.............................................................. 77
4-3-2 HR-TEM 分析................................................................................................. 81
4-3-3 VSM 分析....................................................................................................... 87
4-3-4 AFM/MFM 分析.............................................................................................. 93
4-3-5 XPS 分析......................................................................................................... 95
第五章 結論 .................................................................................................................. 98
參考文獻 ...................................................................................................................... 100
附錄…………………………………………………………………………………...103

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