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通过二次阳极氧化法在H2O+H3PO4+NH4F+乙二醇电解液中恒电压阳极氧化纯钛片,制备出管结构可控、重复性好的TiO2纳米管阵列。利用FESEM、XRD对TiO2纳米管阵列的形貌、管结构、相组成进行表征。探讨了TiO2纳米管阵列的形成机制,研究阳极氧化电压、电解质水含量与磷酸含量等因素对纳米管的管径、管长的影响。正交实验结果表明,在实验条件下,TiO2纳米管的管径和管长随阳极氧化电压增加而增加;TiO2纳米管管径随水含量0%~4%(体积分数)、磷酸含量的增加而增加,管长随水含量2%~6%(体积分数)、磷酸含量的增加而减少;TiO2纳米管的形貌随氟化铵含量和阳极氧化时间的影响较小。TiO2纳米管阵列在400℃退火3h后,由无定形态转变为锐钛矿相。
TiO2 nanotube array with controlled tube structure and good repeatability was prepared by anodic oxidation of H2O2 + H3PO4 + NH4F + ethylene glycol electrolyte. The morphology, tube structure and phase composition of TiO2 nanotube arrays were characterized by FESEM and XRD. The formation mechanism of TiO2 nanotube arrays was discussed. The effects of anodic oxidation voltage, electrolyte water content and phosphoric acid content on the nanotube diameter and tube length were investigated. The results of orthogonal experiment show that the diameter and tube length of TiO2 nanotubes increase with the increase of anodization voltage under the experimental conditions. The diameter of TiO2 nanotubes increases with the increase of water content from 0% to 4% (volume fraction) and phosphoric acid While the tube length decreases with the increase of water content from 2% to 6% (volume fraction) and phosphoric acid content. The morphology of TiO2 nanotubes has little influence on the content of ammonium fluoride and the time of anodization. TiO2 nanotube arrays annealed at 400 ℃ for 3h, the amorphous nanotubes transformed into anatase phase.