硫化鐵礦物以各種不同的礦物相存在於自然界中，本研究利用水熱合成法合成硫化鐵礦物，先透過改變長晶的溫度及時間，觀察硫化鐵在不同溫度及時間下之礦物相變化；接著探討鐵/硫莫爾數比例之改變對其長晶過程之影響，本實驗使用X光繞射儀分析硫化鐵礦物之晶體結構及相轉變序列，同時利用國家同步輻射研究中心X光繞射技術，以即時方式分析硫化鐵相轉變之過程，並與非即時實驗之結果相互比較，再利用掃描式電子顯微鏡及穿透式電子顯微鏡觀察硫化鐵礦物之形貌及結晶度分析，最後探討其相轉變機制。接著利用超導量子干涉儀與震動樣品磁力儀量測硫化鐵礦物之巨觀磁特性，並使用磁力顯微鏡掃描磁力影像，且觀察其磁區分布及磁場方向等微觀磁特性，並探討巨觀與微觀尺度磁性特徵之異同。
在非即時實驗中，改變加熱溫度及持溫時間，觀察其相轉變序列為：四方硫鐵礦（FeS）→ 硫複鐵礦（Fe3S4）→ 菱硫鐵礦（Fe9S11）→ 磁黃鐵礦（Fe9S10）；而即時實驗結果顯示其相轉變序列為：四方硫鐵礦（FeS） → 硫複鐵礦（Fe3S4） → 磁黃鐵礦（Fe9S10）；然而非即時與即時實驗結果中，可以發現在非即時實驗中菱硫鐵礦（Fe9S11）的出現，進一步探討其原因較有可能為實驗之合成環境中，鐵與硫濃度分布不均所導致菱硫鐵礦（Fe9S11）的生成與否。改變鐵/硫莫爾數之比例，探討不同的鐵硫比例如何影響長晶過程，由非即時與即時之實驗結果可得知：鐵/硫莫爾數比例的差異的確會使長晶序列中硫化鐵礦物的生成時間有所差異。
由掃描式電子顯微鏡及穿透式電子顯微鏡之影像得知：硫複鐵礦（Fe3S4）的粒徑大小約為50 ~ 200 nm，形貌無特定形狀，結構中有明顯的缺陷存在；磁黃鐵礦（Fe9S10）的粒徑大小約為1 ~ 4 μm，呈現片狀六角形狀；硫複鐵礦（Fe3S4）與磁黃鐵礦（Fe9S10）皆為單晶結構。巨觀磁特性得知：硫複鐵礦（Fe3S4）為亞鐵磁性，且為單磁域/擬單磁域結構；磁黃鐵礦（Fe9S10）為反鐵磁性並含有少量亞鐵磁性，為單磁域結構。由微觀之磁力顯微鏡影像可得知：硫複鐵礦（Fe3S4）粒徑大小70 ~ 110 nm、磁域結構為單磁域；磁黃鐵礦（Fe9S10）則因為磁力訊號微弱，以表面形貌的凡德瓦力貢獻為主，看不出其磁性結構。
本研究透過探討長晶溫度及時間之變化與不同鐵/硫莫爾數比例，對硫化鐵長晶過程之影響，藉此長晶實驗模擬自然界中「溫度」、「時間」及「富鐵與富硫」等條件對硫化鐵礦物生成機制之影響；並同時討論硫複鐵礦與磁黃鐵礦在巨觀及微觀磁性量測之磁性參數及磁域結構之差異；此結果應可提供後續進行相關實驗之參考依據。

Iron sulphide minerals are present in Earth’s crust in various Fe-S phases. In this study, iron sulphide minerals were synthesized via a hydrothermal method and their phase transition mechanisms and magnetic properties were investigated. Ex situ and in situ X-ray diffraction results of the iron-sulphur system under hydrothermal conditions suggested that the transformation sequence followed the different order. Futher study the difference between the experimental method of ex situ and in situ. And the generate time of iron sulphide minerals were affected by the moore ratio of Fe-S. Greigite showed a granular morphology with particle diameters around 50 ~ 200 nm and the HRTEM showed few defects distributed throughout the crystal; pyrrhotite was comprised of stacked hexagonal sheets with thousands of nanometers in width. Magnetic properties of greigite showed ferromagnetic behavior and single/pseudo-single domain structure. Pyrrhotite was anti-ferromagnetic containing ferromagnetic behavior and single domain structure. Overall, this study provides new information on the phase transition mechanism, related reaction formulas, and magnetic properties of iron sulphides, and it emphasizes the important role played by temperature, time, and moore ratio in phase transitions.

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