The general theme of this work is broadly divided into three parts I.Synthesis of transition oxide nano materials of (NiO, Co3O4) and MgO by chemical combustion method for different fuel to oxidizer ratio (0<Ψ<2) in the steps of 0.25) and studies of their structural, electron paramagnetic resonance, optical and microscopic properties. II.Synthesis of diluted antiferromagnetic systems Mg1-xMxO (M=Ni, Co) (0<x<1) by chemical combustion method and studies of their structural, electron paramagnetic resonance and microscopic properties. III.Fabrication of transition oxide nano crystalline thin films by chemical bath deposition and studies of their structural, optical and microscopic properties Various experimental probes have been utilized for the following characterization studies such as, (1) Structural: X-ray diffraction (2) Microscopic: Scanning Electron Microscope (SEM), Atomic Force Microscope (AFM) (3) Susceptibility (magnetic studies): Electron Paramagnetic Resonance (EPR) (4) BET surface area: Specific surface area (5) Optical: UV-Visible spectrophotometer and FTIR