臺灣博碩士論文加值系統

本研究以氣相凝結法在不同氧分壓下（50、100、150 mbar）生成奈米氧化鐵粉，並將所得粉體進行無電鍍鎳處理；此外，也選用商用奈米氧化鐵粉進行相同無電鍍鎳處理，做為實驗對照組。研究過程所使用之奈米氧化鐵或其改質粉體以X光繞射分析、穿透式電子顯微鏡、熱重分析儀、同步幅射X光與磁性檢測等分析技術進行其相關性質檢測。
實驗結果顯示，氣相凝結法生成奈米氧化鐵粉末內含有Fe及γ-Fe2O3相，由TEM觀察粉體型態發現奈米氧化鐵粉末，由表面開始氧化，且容易團聚為鏈狀，150 mbar氧氣氛下所得粉體，氧化最均勻；由X光吸收光譜分析發現150 mbar氧氣氛所得之γ-Fe2O3粉體延伸微精細結構訊號明顯高於氧含量50及100 mbar，顯示其氧化程度較為完全，熱重分析結果顯示，氣凝粉體在溫度100℃時，Fe轉變至γ-Fe2O3，而當溫度達到400℃時，γ-Fe2O3相再轉換成α-Fe2O3相。無電鍍鎳處理後之氧化鐵粉，在pH值6之酸性環境下析鍍30分鐘披覆性較佳，但pH值為8時，無電鍍過程中鎳離子還原效果則最佳。
氣凝合成氧化鐵粉保磁力較佳，Hc值為458.63 Oe。經無電鍍鎳處理後，pH值控制在8時，由於還原成鎳金屬效果最佳，所得到的Ms值為74.51emu/g 。

In the present study, nanocrystalline iron oxide powders were prepared by an inert gas condensation technique under different oxygen partial pressure, i.e., 50, 100, and 150 mbar, respectively. Surface modification of nanocrystalline iron oxide powders and commercial available nanocrystalline iron powders was preformed by electroless nickel plating. The original and modified powders where characterized by X-ray diffraction, transmission electron microscopy, thermogravimetric analysis, and synchrotron X-ray absorption techniques.
The experimental results showed that nanocrystalline iron oxide powders prepared by gas condensation technique exhibit a mixture of Fe and γ-Fe2O3 phase. TEM observation revealed that oxidation began from the surface of the gas-condensed iron powders. The amount of oxidation increased with increasing oxygen partial pressure and was confirmed by synchrotron X-ray absorption examination. Thermal analysis showed that Fe transformed intoγ-Fe2O3 at 100 oC, and further transformed into α-Fe2O3 at 400 oC. The iron oxide powders can be modified by electroless nickel plating in a solution with ph value ranged from 6 to 8.
The coercivity of the nanocrystalline iron oxide powders as-prepared by gas-condensation technique was 458.63 Oe. After electroless nickel plating in a solution with ph=8, the saturated magnetization (Ms) was 74.51 emu/g.

中文摘要 I
Abstract II
總目錄 IV
表目錄 VII
圖目錄 VIII
第一章 前言 1
第二章 文獻回顧 3
2-1 奈米粉末的合成法 3
2-1-1 物理方法 3
2-1-2氣相凝結合成法原理及製程參數 4
2-1-3 化學方法 8
2-2 奈米複合粉體之合成 10
2-2-1 奈米複合粉體的組成與結構特性 10
2-2-2 奈米複合粉末的類型 12
2-3 奈米微粒之磁特性 13
2-3-1 奈米粒子與磁矩的關係 13
2-3-2 鐵氧化物之構造與特性 14
2-4 無電鍍鎳原理 17
2-4-1 無電鍍鎳的組成與特性 18
2-4-2 無電鍍鎳的反應機構 20
2-4-3無電鍍的前處理特性 21
2-5 鎳磷的添加對鐵粉性質的影響 22
第三章 實驗步驟及方法 25
3-1 氣凝合成法合成奈米氧化鐵粉 25
3-2 奈米氧化鐵粉之無電鍍鎳改質 28
3-3 粉末特性分析 31
3-3-1 X光繞射分析 31
3-3-2 氧化鐵粉體熱重損失分析 31
3-3-3 穿透式電子顯微鏡觀察 31
3-3-4 X光吸收光譜分析 32
3-3-5 VSM磁性檢測 33
第四章 結果與討論 34
4-1 氣凝奈米氧化鐵粉之合成與分析 34
4-1-1 氣凝粉體XRD分析 34
4-1-2 氧化鐵粉TEM粒徑分析與形貌觀察 36
4-1-3 氣凝合成之氧化鐵粉TGA分析 38
4-1-4 In Situ加熱繞射分析 40
4-1-5 X光吸收光譜分析 44
4-2無電鍍鎳改質之奈米氧化鐵粉分析 49
4-2-1 改質粉末XRD分析 49
4-2-2 改質粉末之TEM / EDS分析 54
4-2-3 改質粉末之X光吸收光譜分析 64
4-2-4 VSM磁性分析 69
第五章 結論 76
參考文獻 77

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