臺灣博碩士論文加值系統

本論文探討不同起始原料對奈米赤鐵礦形成奈米粒、奈米柱、奈米管、奈米環等形貌之影響，並解釋其長晶機制；之後，奈米赤鐵礦以碳熱還原法生成奈米磁鐵礦，奈米磁鐵礦再利用煆燒氧化得到磁赤鐵礦。接著觀察與討論氧化鐵奈米礦物巨觀與微觀磁特性之差異，並藉由外加磁場對氧化鐵奈米礦物磁性質之影響，進一步推測磁性礦物受到地磁的影響。本篇論文運用X光繞射儀分析產物的結晶構造，用原子力顯微鏡觀察微觀表面形貌，用磁力顯微鏡量測微觀尺度單顆奈米礦物的磁域分佈，並使用超導量子干涉儀量測其巨觀磁性變化（矯頑磁場、殘磁比、飽和磁化量…等）。
　　實驗結果發現：當溶液中所含磷酸根離子的濃度較低時，會傾向吸附在晶體的非c軸方向上，使奈米赤鐵礦在生長過程中沿c軸方向生長(生成柱狀形貌)；而當磷酸根離子濃度較高時，奈米赤鐵礦生長會受抑制，且在反應過程中生長環境為強酸下，酸會沿著未吸附磷酸根離子的面產生侵蝕，使其最終產物有管狀與環狀形貌的生成；並藉由穿透式電子顯微鏡更可釐清奈米赤鐵礦之單晶特性及其長晶生長機制。巨觀磁特性量測得知：除奈米赤鐵礦為弱的鐵磁性外，其他二者為亞鐵磁性；由殘磁量對應在微觀磁特性量測，奈米赤鐵礦訊號極微弱（幾乎量測到背景訊號），而奈米磁鐵礦與奈米磁赤鐵礦則有較強的訊號，請稍微描述微觀磁結構之差別…..；故可知：不同晶體形貌之奈米礦物其磁結構迥異。當外加磁場使奈米礦物達到飽和狀態，可觀察到磁性奈米礦物中的磁矩方向確實會受到外在的磁場方向與時間影響；由此可進一步推測：天然磁性礦物會受到地球磁場之作用時間與地磁方向所影響。本實驗欲推廣MFM微觀磁特性量測技術，輔助巨觀尺度所無法量測到之微觀磁區結構，加以解釋還無法解釋的地磁異常現象。

This objective of this study is to use distinct synthesis methods to manufacture nano-hematite, nano-magnetite and nano-maghemite, than the iron oxide nano-minerals preparation time to add different starting material, so that various morphologies including nano-particle, nano-rod, nano-tube, and nano-ring were synthesized, that using different synthesis parameters (such us concentration, temperature and time) to investigate the magnetic properties of iron oxide nano-minerals, that effect of external magnetic field samples phenomenon, further speculated that the magnetic substance affected by geomagnetism. It is observed that the compositions of raw materials during synthesis have an impact on crystal morphologies. Anion-bonded configuration on the vertical or on [001] facets of nano-hematite was the most important factor for the Fe3+ ions occupied on c-axis. Its major morphologies depend on PO4- anions concentration. Different mole concentration has various molecule-sizes and favorite bonding-facets. Therefore, the morphologies (nanoparticle, nanorod, nanotube, and nanoring) of nano-hematite could be controlled via the starting reaction-compositions. Magnetic properties of three minerals receive effect of magnetic field have distinct domain. It indicates that the substances domain will be subject to external magnetic fields. This phenomenon we hope to employ to nature of the magnetic minerals by magnetic force microscopy (MFM) technique and could be supply more accurate information of geomagnetism.

第一章、緒論..............................1

第二章、背景資料............................2

2.1洋底之磁性礦物...........................2

2.2材料介紹.................................4

2.2.1 奈米赤鐵礦.............................4

2.2.2 奈米磁鐵礦..............................5

2.2.3 奈米磁赤鐵礦.................................6

2.3 合成方法...............................7

2.4氧化鐵奈米礦物之合成方法.........................8

2.5晶體成核生長機制.........................9

2.6磁性介紹.............................11

2.6.1磁性物質分類.............................11

2.6.2磁之相關定義及特性.......................16

2.7磁力顯微鏡之成像原理.....................20

2.8磁域之相關文獻整理.....................23

第三章、研究方法與實驗步驟.....................30

3.1實驗材料與儀器.........................30

3.2實驗流程............................32

3.2.1合成奈米赤鐵礦.........................33

3.2.2合成奈米磁鐵礦.........................38

3.2.3合成奈米磁赤鐵礦........................39

3.3特性分析之儀器.........................40

3.3.1 X-ray繞射儀.....................40

3.3.2 穿透式電子顯微鏡.....................41

3.3.3 X光光電子能譜儀.....................42

3.3.4超導量子干涉儀.......................42

3.3.5原子力顯微鏡........................43

3.3.6電磁鐵(外加磁場)..........................45

第四章、結果與討論.........................46

4.1礦物特性分析..........................47

4.1.1晶相分析............................47

4.1.2晶粒大小分析..........................51

4.1.3 化學價態分析.........................54

4.1.4表面形貌分析..........................56

4.1.5比較起始原料對奈米赤鐵礦合成之影響..............60

4.1.6奈米磁鐵礦與奈米磁赤鐵礦之表面形貌分析............63

4.1.7結晶與生長方向之分析.......................65

4.2礦物磁特性分析.........................68

4.2.1巨觀磁性量測..........................68

4.2.2微觀磁性量測..........................74

4.3外加磁場對磁特性之影響........................85

4.3.1奈米粒子............................85

4.3.2奈米柱............................88

4.3.3奈米管............................91

4.3.4奈米環............................94

4.4磁特性之討論..........................97

4.5微觀磁量測技術在地質領域之展望..................100

第五章、結論.............................107

參考資料.............................109

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