Preparation of the Bojarite Cu3(trz)3(µ3-OH)]Cl2.6H2O at low temperature. Physical and photo-electrochemical Characterization
摘要
Bojarite mineral [Cu3(trz)3(µ3-OH)]Cl2.6H2O was prepared at two temperatures (120 and 150 °C) by hydrothermal route for the first time. The sample was characterized by X-ray diffraction (XRD), thermal analysis (TG/DTG) and Raman spectroscopy. The XRD analysis shows peaks attributed to bojarite, crystallizing in a cubic structure. The Raman spectrum displays the characteristic bands of the bojarite. The TG/DTG profile shows that the product contains water and organic matter, consistent with the nominal composition. A direct optical transition of gap Eg (= 2.26 eV), determined from the diffuse reflectance, corresponds to the transition O2−:2p→Cu2+: t2g. The photoelectrochemical has also been undertaken. Voltammetry in Na2SO4 solution (0.1 M) exhibits low exchange current density (~ 2 mA cm−2) and good electrochemical stability. The variation of interfacial capacitance versus potential is typical of n-type behavior with an electron density of 3.12 × 1016 cm−3 and a flat band potential (Efb) of 0.17 VSCE. The electrochemical impedance spectroscopy (EIS) shows only the bulk contribution in the dark (22 kΩ cm−2), which decreases to 12.7 kΩ cm−2 under visible irradiation supporting the semiconductivity. The positioning of the conduction and valence bands allows us to conclude that this material can be used in electrolysis.