物理化学学报 >> 2008, Vol. 24 >> Issue (12): 2191-2197.doi: 10.1016/S1872-1508(08)60082-0

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导电玻璃上室温沉积钛膜及TiO2纳米管阵列的制备与表征

汤育欣, 陶杰, 张焱焱, 吴涛, 陶海军, 包祖国   

  1. 南京航空航天大学材料科学与技术学院, 南京 210016
  • 收稿日期:2008-07-14 修回日期:2008-09-17 发布日期:2008-12-04
  • 通讯作者: 陶杰 E-mail:taojie@nuaa.edu.cn

Preparation and Characterization of TiO2 Nanotube Arrays via Anodization of Titanium Films Deposited on FTO Conducting Glass at Room Temperature

TANG Yu-Xin, TAO Jie, ZHANG Yan-Yan, WU Tao, TAO Hai-Jun, BAO Zu-Guo   

  1. College of Material Science and Technology, Nanjing University of Aeronautics and Astronautics, Nanjing 210016, P. R. China
  • Received:2008-07-14 Revised:2008-09-17 Published:2008-12-04
  • Contact: TAO Jie E-mail:taojie@nuaa.edu.cn

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摘要： 在掺氟的杂nO2(FTO)导电玻璃衬底上采用射频磁控溅射的方法室温沉积纯Ti薄膜, 以NH4F/甘油为电解液, 经电化学阳极氧化得到结构有序、微米级的TiO2纳米管阵列/FTO复合结构, 并通过场发射扫描电子显微镜(FESEM)、X射线衍射(XRD)以及光电化学的方法对纳米管阵列进行了表征. 研究表明, 在氩气气压为0.5 Pa, 功率为150 W, 时间为0.5 h条件下在导电玻璃上室温沉积获得钛膜的结构为晶带T型组织, 表面均匀性好且致密度较高; 在电压为30 V下, 随着阳极氧化时间从1 h延长至3 h, 纳米管的管径从50 nm增加到75 nm, 纳米管的长度从750 nm增至1100 nm后减至800 nm, 管壁由平滑变为波纹状; 随氧化电压的升高, 纳米管管径逐渐增大, 而表面覆盖物逐渐减少, 可通过在稀的HF溶液(0.05%(w, 质量分数))中超声清洗去除; 此外, 瞬态光电流测试表明结晶的电极表现出更好的光电转换性能, 紫外光照射下能促进TiO2光生载流子有效分离, 在热处理温度为450 ℃时, 具有较高的光电化学性能.

关键词: 射频磁控溅射, 室温, FTO 导电玻璃, TiO2纳米管阵列, NH4F/甘油

Abstract: Self-organized TiO2 nanotube arrays with micro-scale length were prepared on fluorine-doped tin oxide (FTO) conducting glass in NH4F/glycerol electrolyte by electrochemical anodization of pure titanium films deposited by radio frequency magnetron sputtering (RFMS) at roomtemperature. The samples were characterized by means of field emission scanning electron microscopy (FESEM), X-ray diffraction (XRD), and photoelectrochemistry methods. The results showed that Ti films prepared at the condition of Ar pressure 0.5 Pa, power 150 W, and 0.5 h at room temperature possessed the zone T model structure with good homogeneity and high denseness. When the anodization time was prolonged from 1 to 3 h at the voltage of 30 V, the pore diameter of TiO2 nanotubes increased from 50 to 75 nm, and the length increased from750 to 1100 nmand then gradually decreased to 800 nm, while their wall morphology changed from smooth to rough. Also with increasing the anodization voltage, the pore diameter became larger, and the remaining oxide layer reduced, which could be easily removed by ultrasonic-chemical cleaning in 0.05% (w, mass fraction) diluted HF solution. Moreover, the photocurrent response curves and electrochemical impedance spectroscopy (EIS) results indicated that UV-illumination clearly enhanced the effective separation of the electron-hole pairs and the crystallized electrodes from the annealing treatment of as-anodized electrodes at 450 ℃ exhibited a better photoelectrochemical performance.

Key words: Radio frequency magnetron sputtering, Roomtemperature, FTO conducting glass, TiO2 nanotube arrays, NH4F/glycerol

MSC2000: 

  • O646