ZnO/Ni/C 磁性光觸媒粉體經由水熱技術製備而成。起始溶液中醋酸鋅、硝酸鎳與檸檬酸的莫爾比為6：1：4，且總金屬離子的莫爾濃度為0.1 M。藉由2 M 氨水調整起始溶液之pH值後，在180 ℃進行2 個小時的水熱反應，接著等冷卻至室溫後再藉由離心與冷凍乾燥之方式得到固態前驅粉體。藉熱分析探討前驅粉體之熱行為表現，並以此分析結果決定粉體在氮氣氣氛中煆燒的溫度。煆燒之樣品以X-ray 繞射分析儀(XRD)、同步熱重與熱示差掃描分析儀(TG-DSC)、傅立葉轉換紅外線光譜儀(FTIR)、光致螢光光譜儀(PL) 和掃描式電子顯微鏡(SEM) 來分析其粉體特性，並對MB 水溶液進行光催化能力測試。由實驗結果發現起始溶液之pH 值與煆燒溫度會影響ZnO 的結晶度和ZnO 與Ni 之重量比。最後結果指出ZnO/Ni/C 磁性光觸媒粉體在起始溶液之pH 值為4 (未添加氨水)，且煆燒溫度為600 ℃ 時擁有最佳的光催化效果(0.017 m3/(kg．s))。

ZnO/Ni/C magnetic photocatalytic particles were prepared using a hydrothermal technique. The aqueous solutions, having the molar ratios of Zn(CH3COO)2‧2H2O：Ni(NO3)2‧6H2O：C3H4OH(COOH)3 = 6：1：4 and the molar concentration of the total metallic ions (Zn2+ and Ni2+) = 0.1 M, were prepared. The pH of the solution was adjusted using 2 M NH4OH(aq). The solutions were then hydrothermally treated at 180 ℃ for 2 h. After centrifugally filtering and freeze-drying, the dried solid precursors were obtained and then thermally analyzed to investigate their thermal behavior, followed by calcining the solid precursors in N2 atmosphere at different temperatures. The calcined specimens were characterized using x-ray diffractometer (XRD), fourier transform infrared spectroscope (FTIR), scanning electron microscope (SEM) and photoluminescence spectroscope (PL). The photocatalytic performance of the prepared ZnO/Ni/C particles was evaluated by monitoring the ability to photocatalytically decompose the methylene blue in water under the irradiation of 365 nm UV light. Effects of pH values of the aqueous solution and calcination temperatures on the degree of crystallinity of ZnO and the weight ratio of ZnO to Ni in the ZnO/Ni/C magnetic photocatalytic particles were studied. The results indicated that the ZnO/Ni/C magnetic photocatalytic particles prepared by calcining the solid precursor obtained from the solution of pH = 4 (without NH4OH additions) in the nitrogen atmosphere at 600 ℃ possessed the best photocatalytic ability to decompose methylene, having a specific reaction rate, based on the mass of the photocatalyst used, 0.017 m3/(kg．s).

主目錄
論文提要內容：	I
Abstract:	II
主目錄	III
圖目錄	V
表目錄	VII
第一章	緒論	1
第二章	文獻回顧	5
2-1.	光觸媒與光催化的原理	5
(1).	摻雜(doping)	6
(2).	複合(coupling)	6
2-2.	氧化鋅(ZnO) 基本性質、晶體結構	7
2-3.	ZnO 粉體之製備	10
2-3-1.	水熱/溶劑熱法(Hydrothermal / Solvothermal method)	10
2-3-2.	溶膠-凝膠法(Sol-Gel method)	12
2-3-3.	多元醇法(Polyol method)	14
2-3-4.	噴霧熱解法(Spray Pyrolysis method)	15
2-4.	磁性光觸媒粉體之發展及製備	15
第三章	實驗步驟	23
3-1.	實驗藥品	23
3-2.	ZnO/Ni/C磁性光觸媒粉體之製備	24
3-3.	特性分析	26
3-4-1.	X-ray 繞射分析儀(X-ray diffractometer, XRD)	26
3-4-2.	同步熱重與熱示差掃描分析儀(Simultaneous thermogravimetry-differential scanning calorimetry, TG-DSC)	27
3-4-3.	掃描式電子顯微鏡(scanning electron microscope, SEM) 	28
3-4-4.	傅立葉轉換紅外線光譜儀(Fourier transform infrared spectroscopy, FTIR)	28
3-4-5.	光致螢光光譜儀(photoluminescence spectroscopy, PL)	29
3-4.	光催化活性實驗	29
第四章	結果與討論	32
4-1.	水熱法製備之ZnO/Ni/C粉體之特性分析與光催化能力	32
(a).	粉體特性分析	32
(b).	光催化能力	41
4-2.	pH 值對ZnO/Ni/C 粉體之影響	46
4-3.	ZnO/Ni/C 粉體之磁性值	56
第五章	結論	57
第六章	參考文獻	58

 
圖目錄
圖1-1. 不同光觸媒半導體於pH=1 之能隙分佈圖	2
圖1-2. 光觸媒相關研究領域	3
圖1-3. 金屬氧化反應之Ellingham plot	4
圖2-1. 六方晶系纖鋅礦結構	9
圖2-2. ZnO-MNs 成長示意圖 (a) ZnO 的生成、(b) ZnO-MNs的生成、(c) 洗滌後之ZnO-MNs、(d) ZnO-MNs的SEM和(e)物質間形成之關係鍵結	12
圖3-1. ZnO/Ni/C粉體製備之流程圖	25
圖4-1. P4 (未添加氨水) 前驅粉體之熱分析圖。	34
圖4-2. P4 (未添加氨水) 所得前驅粉體加熱至不同溫度下之FTIR 圖。	35
圖4-3. P4 (未添加氨水) 前驅粉體在氮氣氣氛下加熱至不同溫度之XRD 圖。	37
圖4-4. 平均晶粒尺寸與ZnO/Ni 重量分率對P4 (未添加氨水) 在不同煆燒溫度之關係圖。	38
圖4-5. P4 (未添加氨水) 於不同煆燒溫度之PL 圖。	38
圖4-6. P4 (未添加氨水) 所得前驅粉體於不同煆燒溫度下之SEM 圖(倍率為100 k)：(a) 前驅粉體、(b) 500 oC、(c) 550 oC、(d) 600 oC。	40
圖4-7. 不同煆燒溫度的P4 粉體於365-nm 紫外光照射30 分鐘時MB 濃度之關係圖。	41
圖4-8. P4 煆燒粉體於不同煆燒溫度之光降解的MB 濃度隨時間變化。	42
圖4-9. P4 粉體之kAm 值對煆燒溫度之變化關係。	45
圖4-10. 不同起始溶液之pH 值經水熱反應後所製得前驅物粉體之FTIR 圖。	47
圖4-11. 不同起始溶液pH 值經水熱反應後所製得前驅物粉體之熱分析圖，(a) DSC 圖和(b) TG 圖。	49
圖4-12.起始溶液之pH 值經水熱法再經過氮氣氣氛下煆燒600 oC之XRD 圖。	51
圖4-13. 起始溶液之pH 值經水熱法後在氮氣氣氛下煆燒600 oC 之ZnO 晶粒尺寸關係圖。	52
圖4-15. 起始溶液之pH 值經水熱法後在氮氣氣氛下煆燒600 oC 之SEM 圖(倍率為100 k)：(a) pH= 4、(b) pH= 7 和(c) pH= 9。	54
圖4-16. 前驅粉體經過氮氣氮氣氣氛下煆燒600 oC 後光催化反應之kAm 值對起始溶液之pH 值。	55
圖4-17. P4 (未添加氨水) 於不同煆燒溫度：(a) 500 oC(N2)、(b) 550 oC(N2)、(c) 600 oC(N2) 與起始溶液之pH 值經水熱法再經過氮氣氣氛下煆燒600 oC：(d) P7-600 oC(N2)、(e) P9-600 oC(N2) 之磁性表現圖。	56

 
表目錄
表2-1. ZnO物理性質	9
表3-1. 實驗使用之主要化學藥品	23
表3-2. 所有材料的莫爾配比	24
表3-3. 反應溶液於水熱反應前後之pH 值變化	25
表3-4. 所使用分析儀器的用途	26
表4-1. 為P4 (未添加氨水) 傅氏紅外線吸收光譜(FT-IR) 之官能基吸收峰	36
表4-2. P4 (未添加氨水)、P7 和P9 之前驅乾燥粉體的傅氏紅外線吸收光譜(FT-IR) 之官能基	48

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