The orthorhombic MoO 3 micro-strips sample was synthesized using microwave assisted chemical co-precipitation technique. Synchrotron X-ray Diffraction (SXRD) pattern and Rietveld Refinement was used to estimate structural parameter, crystallite size of sample. It reveals that the synthesized sample MoO 3 crystallized as an orthorhombic phase. X-ray Absorption Spectroscopy (XAS) measurement, which comprises both X-ray Absorption Near Edge Structure (XANES) and Extended X-ray Absorption Fine Structure (EXAFS) techniques, have been carried out on Mo K-edge to probe the local structure of samples. Local structure is also confirmed from the SXRD and Raman spectra of sample. XAS measurement reveals that the first bond length of Mo-O and Mo-Mo is 1.69 and 3.42 Å in orthorhombic MoO 3 respectively. Transmission electron microscopy and SAED patterns showed stripe-like structure and single-crystal formation of MoO 3 respectively.