采用阳极氧化法在丙三醇+NH4F+5vol％ H2O的电解液中制备了高度有序的ZrO2纳米管阵列,详细考察了溶液中F含量(0.1～1.1 mol/L)对纳米管形貌、相结构和化学组成的影响.利用扫描电子显微镜(SEM),X射线衍射仪(XRD)和X射线光电子能谱仪(XPS)对不同条件下制备的管径约90～130 nm,管长约4.8～9.1 μm的纳米管形貌和结构进行了表征.结果显示,在含有0.7 mol/L NH4F的电解液中获得了高度有序且垂直导向的四方相ZrO2纳米管阵列,而在较低浓度的电解液中制备的纳米管阵列为无定形结构,较高浓度下纳米管阵列出现坍塌.此外,纳米管近表层处F/O原子比也随F浓度的变化而变化.
The present research demonstrates the significant influence of fluoride content on the morphology,phase structure and chemical composition of ZrO2 nanotube arrays which were prepared via a direct electrochemical anodization of zirconium foil in glycerol-based electrolytes composed of 5vo1％ H2O and different contents of NH4F from 0.1 mol/L to 1.1 mol/L.The as-prepared nanotube arrays with external diameter of 90-130 nm and length of 4.89.1 μm were characterized by scanning electron microscope (SEM),X-ray diffraction (XRD) and X-ray photoelectron spectrum (XPS).The results show that the highly ordered and vertically aligned tetragonal ZrO2 nanotube arrays can be obtained in the electrolyte containing 0.7 mol/L NH4F,and they become amorphous at lower NH4F concentration and collapse at higher NH4F concentration.Moreover,the F/O atomic ratio near the top surface of nanotubes is also dependent on the F concentration in the electrolyte.
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