不同阳极氧化条件下TiO2纳米管阵列的制备及表征
Preparation and Characterization of TiO2 Nanotube Arrays by Anodic Oxidation Method
Received date: 2009-08-28
Revised date: 2009-11-28
Online published: 2010-05-12
分别在三种不同的电解液中, 以钛为基体采用阳极氧化的方法制备了TiO2纳米管阵列薄膜, 用SEM观察纳米管阵列薄膜的形貌、测量纳米管管径大小; 用XRD、拉曼光谱检测TiO2纳米管阵列薄膜热处理前后的晶型. 结果表明：不同的电解液体系和氧化电压下得到的纳米管形貌各不相同. 在0.24wt%HF水溶液中得到的TiO2纳米管排列整齐, 管径为110nm; 在0.5 wt%NaF+2.7wt% Na2SO4水溶液和0.88wt% NH4F的丙三醇水（体积比1∶1）混合溶液中得到的纳米管排列不规整, 管径为100nm; 在0.24wt%HF条件下生成的TiO2纳米管管径与氧化电压成线性关系：d=k×U+b, 其中, 系数k＝5.2nm/V, b=2.2nm, 0≤U≤25V. 经450℃热处理2h后TiO2纳米管结构由无定形态转变为锐钛矿.
李 荐 , 罗 佳 , 彭振文 , 郭 欣 . 不同阳极氧化条件下TiO2纳米管阵列的制备及表征[J]. 无机材料学报, 2010 , 25(5) : 490 -494 . DOI: 10.3724/SP.J.1077.2010.00490
Thin films of TiO2 nanotube arrays were fabricated by anodic oxidation method in different electrolyte solution. The morphology of the film and the diameter of the nanotubes were observed by scanning electronic microscope (SEM). The crystal type of the film before and after heattreatment were characterized by X-ray diffraction (XRD) and Laser Raman.The results show that the electrolyte solution and applied votage have great effect on microstructure of the films. High order-aligned TiO2 nanotube arrays of 110nm in outer diameter are prepared at 20V in the 0.24wt% HF aqueous solution. Films of nanotube arrays of 100nm in outer diameter are prepared at 20V in 0.5wt％NaF+2.7wt% Na2SO4 aqueous solution and 0.88wt% NH4F glycerol-water (vol ratio 1∶1) mixture solution. The outer diameter (d) of nanotubes increase linearly with applied voltage (U) in the range of 0-25V which can be described as d=k×U+b with k=5.2nm/V and b=2.2nm. TiO2 nanotube arrays with amorphous structure is transformed to anatase after annealed at 450℃ for 2h.
Key words： anodic oxidation; aligned TiO2 nanotubes; preparation; anneal
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