SYNTHESIS AND CHARACTERIZATION OF NANO CuO-ZrO_2 MIXED OXIDE

摘要

Nano CuO-ZrO_2 mixed oxides were prepared by wet chemical method by mixing equimolar solutions (0.45M) of cupric chloride (1.92g) and Zirconium oxychloride (3.63g) in aqueous Sodium hydroxide and refluxed at elevated temperature. The prepared nano CuO-ZrO_2 mixed oxides were characterized by FT-IR, SEM, EDAX, XRD, DSC and CV studies. From XRD studies the size of the nano CuO and ZrO_2 are found to be 25 and 9.5nm respectively through Debye-Scherrer's formula. The sizes of the CuO-ZrO_2 mixed oxide particles have also been characterized and the average grain size of the particles is found to be 24nm in diameter. The nano particle composition and morphology of CuO, ZrO_2 and mixed oxide have been analysed by EDAX set up attached with scanning electron microscope (SEM). EDAX analysis indicates the presence of Cu, Zr and O. SEM morphological studies of CuO, ZrO_2 and mixed CuO-ZrO_2 revealed the particle distribution with uniform granular structure. Cyclic Voltammetric studies exhibit good adherent behaviour on electrode surface and good electroactivity at pH 1.0. Nano CuO, ZrO_2 and mixed CuO-ZrO_2 under goes oxidation at 0.224V, 0.092V -0.072V and0.198V respectively. DSC thermogram of CuO, ZrO_2 and mixed CuO-ZrO_2 are recorded at the heating rate of 10°/ min. The glass transition temperature (Tg), the crystallization temperature (Tc) and melting point (T_(M)) of the mixed oxide are determined from the DSC curve. The Tg value of CuO-ZrO_2 mixed oxide is -50° C the Tc value is 20° C and melts at a temperature of 116° C.