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).