以价廉的Ni板代替常用的Pt片为阴极,纯钛为阳极,采用电化学阳极氧化法在NH4F-H3PO4体系中制备出TiO2纳米管阵列.详细研究了制备参数(溶液酸度、氟离子浓度、外加电压和氧化时间)对所获纳米管阵列形貌的影响.采用场发射扫描电镜(FE-SEM)和X射线衍射(XRD)对样品的形貌和晶相结构进行了表征.在最优化的条件下,可以获得形貌规整、表面干净、有序的TiO2纳米管阵列.纳米管阵列的平均管径为60 nm.管长约530 nm.采用阳极氧化法制备的纳米管阵列是非晶态的.经400℃热处理2 h后,可以转变为锐钛矿相.实验结果还发现,经过热处理后,纳米管阵列变得更为有序,管径扩大至约95 nm.%TiO2 nanotube arrays were fabricated by anodization of titanium in aqueous electrolyte solution of NH4F+H3PO4 using a Nickel sheet of low cost as cathode instead of conventionally used noble Platinum. The effects of preparation parameters, i.e., concentration of H3PO4 and F-, applied voltage and anodization time, on the morphology of as-prepared nanotube arrays were systematically studied. Field emission scanning electron microscope(FE-SEM) and X-ray dittraction(XRD) analysis were carried out to characterize the morphology and structure of the samples. The results showed that the self-ordered TiO2 nanotube arrays with an average pore size of 60 nm and a length of 530 nm could be obtained under optimum conditions. The as-prepared nanotube arrays were amorphous and transformed to an anatase crystal structure after being annealed at 400 ℃ for 2 h. It was also found that the freshly-prepared nanotube arrays got more ordered after calcination, with a pore size of ca. 95 nm.
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