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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4.8~9.1μm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.
Highly ordered ZrO2 nanotube arrays were prepared by the anodic oxidation method in the presence of glycerol + NH4F + 5vol% H2O. The effect of F content (0.1 ~ 1.1 mol / L) on the nanotube morphology, Phase structure and chemical composition.Using scanning electron microscopy (SEM), X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS) 4.8 ~ 9.1μm nanotube morphology and structure were characterized.The results showed that highly ordered and vertically oriented tetragonal ZrO2 nanotube arrays were obtained in the electrolyte containing 0.7 mol / L NH4F, while in the lower concentration The nanotube arrays fabricated in the electrolyte were amorphous and the nanotube arrays collapsed at higher concentrations.In addition, the F / O atomic ratio at the near surface of the nanotubes also changed with the concentration of F-.