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The nano and micro sized particles play a very important role in different sectors. In recent years, an electrochemical method has aroused a considerable interest in the synthesis of nano and microsized metal oxide powder and films because of its simplicity, low temperature operation process and viability of commercial production. Therefore, This book is mainly directed towards the Synthesis, Characterization and Applications of different Nano and Micro sized metal oxide particles by different methods like electrochemical generation and solution combustion method. The synthesized particles are characterized by using powder X-ray diffraction (XRD), Thermal analysis (TG-DTA), Scanning electron microscopy (SEM), Energy dispersive X-ray diffraction spectroscopy (EDX), X-ray photoelectron spectroscopy (XPS), Transmission electron microscopy (TEM), Fourier transform infrared (FT-IR) and UV-Vis spectroscopic techniques.