Abstarct: In this experimental thesis, α-Fe2O3 thin films and nano-powders were synthesized using spray pyrolysis and hydrothermal techniques and the structural, optical and surface morphology of samples were studied. Characterization of samples were performed using field emission scanning electron microscope (FE-SEM), X-ray diffraction (XRD), optical spectroscopy (UV-Vis), photoluminescence (PL) and Energy Dispersive Spectroscopy (EDAX). In the case of synthesis using spray pyrolysis method, the effect of precursor solution concentration on samples was studied. XRD pattern analysis of samples showed that crystallite size increases with increasing in the precursor solution concentration. Calculated band gap of samples decreased from 3.57 to 2.09 eV. Also, surface morphology revealed increasing the concentration of sheets and decreasing grain boundaries. In the case of synthesis using hydrothermal method, effects of temperature, hydrothermal process time, type of substrate and surfactant (SDS) were investigated. Investigating the effect of process temperature, XRD pattern analysis showed an improvement in crystallinity when the temperature raised from 120 to 180 °C. Band gap of samples was increased from 1.97 to 2.07 eV. With increasing the process time from 6 to 24 hrs, mean crystallite sizes were increased from 32.35 to 27.53 nm and the band gap decreased from 2.08 to 2.06 eV. For the effect of surfactant, XRD pattern showed the lowest mean crystallite size for the highest amount of surfactant in the precursor solution. For the samples prepared using the lowest and highest amounts of SDS, the bad gap was estimated to be about 1.88 and 1.93 eV, respectively. Our research revealed that using seed laxyer causes better growth of samples than using bare glass substrate, and the mean crysttllite size increases from 29.69 to 39.21 nm, using seed laxyer. FESEM images revealed the formation of nano rice-like morphology for samples grown on seed laxyer. These nano rice-like shapes had a mean diameter of about 30 nm. XRD pattern showed the formation of hexagonal crystal structure for all α-Fe2O3 samples.