本研究採用陽極氧化法,雙電極連接直流電源供應器,在含氟化物溶液中,鈦板為陽極,鉑片為陰極,使鈦金屬氧化成氧化鈦層並受氟離子腐蝕成為奈米管陣列膜。接著以電化學蝕刻技術,形成自身支持(free-standing)的高縱橫比TiO2奈米管陣列貫通(both-ends opened)膜,再利用此透過膜進行甲基橙染料的光(電)催化反應。 本研究分別採用一步陽極氧化與酸蝕法(草酸及氫氟酸)、二步升壓陽極氧化法、二步降壓陽極氧化法、三步陽極氧化法,嘗試製備二氧化鈦奈米管陣列貫通膜。結果顯示,一步法的酸蝕操作條件嚴苛;二步法製備的薄膜不易從基板剝離且易脆;三步陽極氧化法則製備出可資後續光催化應用的奈米管陣列貫通膜。接著進行染料光催化反應,探討溶液pH(2~10)及UV光強度(5~20mW/cm2)對奈米管陣列貫通膜光催化反應速率常數之影響。結果顯示,染料溶液pH 2時有最佳的反應效應,且反應速率常數隨光強度增加而增高。光電催化的反應速率常數,為光催化的2.25倍。
In this study, anodic oxidation method was used to prepare titanium dioxide nanotube. A power supply was connected with two electrodes that immerged in fluoride solution. A titanium plate acts as anode and a platinum plate as cathode. The titanium dioxide layer grows on the titanium plate and sequentially corroded by fluoride to form nanotubes. Anodic growth of self-organized, high-aspect-ratio and highly ordered TiO2 nanotubes arrays membrane was prepared and nanotubes on the membrane were penetrated sequentially by electrochemical etching technique to remove the titanium barrier layer. The titanium plate finally forms a both-ends opened membrane. The membrane was then used as a photocatalyst for the degradation of methylene orange by photocatalytic and photoelectrocatalytic reaction. We used three methods to prepare the membranes including one-step with acid etching method, two-step with increasing voltage method, two-step with decreasing voltage method and three-step anodic oxidation method. The acid etching parameters are too critical to from a penetrated membrane. The membrane prepared by two-step methods was very brittle and can not peel off from titanium plate. The successfully penetrated membrane was prepared by three-step anodic oxidation method. The temporal varieties of degradation ratio were studied throughout two parameters including solution pH and UV light intensities. The results showed degradation ratios decrease as solution pH increase within the range from 2 to 10. The degradation ratios increase as UV light intensities increase within the range from 5 to 20mW/cm2. Furthermore, the reaction rate constant of photoelectrocatalysis is 2.25 times that of photocatalysis.