本論文係以鈦鐵礦結構之鈦酸鎳(NiTiO3)及鈦酸鈷(CoTiO3)材料作為光觸媒之研究，並進一步以銀離子分別取代鎳或鈷離子，製備成(Ag1-XNiX)TiO3及(Ag1-XCoX)TiO3之奈米光觸媒材料。本研究主要由五個部份所構成：(1) 有機酸前導物製程之參數探討；(2) 以檸檬酸前導物法合成 NiTiO3粉末及其基礎特性探討；(3) 以檸檬酸前導物法合成摻雜銀之NiTiO3粉末及其光催化特性研究；(4) 以檸檬酸前導物法合成CoTiO3粉末及其基礎特性探討;(5) 以檸檬酸前導物法合成摻雜銀之CoTiO3粉末及其光催化特性研究。
實驗結果顯示，以檸檬酸前導物法製備NiTiO3及CoTiO3粉末，其前導物於煆燒過程中，可分為脫水反應、燃燒分解反應與鈦鐵礦結晶化三個步驟。其中，NiTiO3與CoTiO3之結晶溫度分別為620C及588C，而最適合作為光觸媒之煆燒條件則為600C下持溫3小時，於此條件下之表面型態為球狀顆粒且分散較均勻並擁有最大之比表面積，因此晶粒很容易為了降低表面能而進一步經由Ostwald Ripening及Oriented Attachment之成長機制成長為一顆顆大單晶。經計算，NiTiO3及CoTiO3之結晶活化能分別為3896與2532 kJ/mol；晶粒成長活化能則分別為 8.84與13.23 kJ/mol。利用1-10 at%銀離子取代鈦鐵礦結構中之鎳離子或鈷離子後發現，對於典型光催化試劑-亞甲基藍之吸附能力而言，係隨銀離子之摻雜而有所提升，且對亞甲基藍之光降解效應亦有相當程度之影響。NiTiO3與CoTiO3摻雜銀系列之試樣於紫外光下以10W、365 nm之光源照射12小時後最高可分別解降63.71%及32.42%之亞甲基藍；而於可見光下以0.5W、400-500 nm之光源照射60小時後，對亞甲基藍之光降解效率分別可達65.74%及35.59%。進一步計算包含吸附於光觸媒表面之亞甲基藍，經摻雜7-10 at%銀離子之NiTiO3光觸媒催化後，其於紫外光及可見光下之整體光解降效率可分別高達97.48%與99.84%，而亞甲基藍溶液於摻雜銀之CoTiO3系列光觸媒催化下之最大效率分別為57.05%與57.28%，效率遠較純NiTiO3 和CoTiO3光觸媒為高，足見摻雜銀能有效提升光催化之效益。

The present investigation mainly focused on the ilmenite structure materials, NiTiO3 and CoTiO3, which may be the potential materials for photocatalysis. In advanced, the silver ions were used to substitute for part of nickel or cobalt ions, so as to prepare the photocatalysts as (Ag1-XNiX)TiO3 and (Ag1-XCoX)TiO3 nano-sized powders. This research can be divided into five sections, including changing the parameters of the organic acid precursor method which was modified from the Pechini process, preparing NiTiO3 and CoTiO3 powders by the citric acid precursor method, and also investigating the photocatalytic properties of silver doped NiTiO3 and CoTiO3 powders for the degradation of methylene blue (MB). In the experiments, nano-sized NiTiO3 and CoTiO3 powders were successfully prepared by the citric acid precursor method and the crystalline temperature of NiTiO3 and CoTiO3 powders were 620C and 588C. It is also found that NiTiO3 and CoTiO3 powders heated to 600C for 3 hours in air would be the candidates for photocatalysts. Moreover, the crystalline activation energy of NiTiO3 and CoTiO3 was estimated as 383 and 251 kJ/mol; the activation energy of grain growth was also calculated as 8.84 and 13.23 kJ/mol for NiTiO3 and CoTiO3.
When silver ions were in substitution for nickel or cobalt ions, the ability for NiTiO3 and CoTiO3 to adsorb MB molecules was improved, and the photo-degradation of MB was also influenced by the dopants of silver ions. Silver-doped NiTiO3 and CoTiO3 photocatalysts shows the best photodegradation rate of MB up to 63.71% and 32.42% under the UV light irradiation for 12 hours, and also presents the best photodegradation rate of MB as 65.74% and 35.59% under the visible light irradiation for 60 hours. Including the degradation of MB from the adsorbability of NiTiO3 and CoTiO3 in the dark, the concentration of the reacted MB solution was mostly decreased about 97.48% and 99.84% of the initial MB concentration for Ag-NiTiO3 series, and also decreased about 57.05% and 57.28% for Ag-CoTiO3 series after the UV and visble light irradiation. Therefore, silver ions used to place nickel or cobalt ions can substantially improve the photocatalysis for the degradation of MB.

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