Iron oxide thin films were prepared by spin-coating a gel solution of iron(III) nitrate dissolved in 2-methoxyethanol and acetylacetone on glass and quartz substrates. The film thickness was adjusted by changing the spinning rate of the spin coater, Annealing was carried out between 300 degrees C to 600 degrees C to investigate the phases present in the films. Viscosity of the main solution was found as 0.0035 Pa (.) s by viscosity measurement. TGA/DTA analyses showed that heat treatment should be done between 330 degrees C and 440 degrees C in order to produce maghemite thin films. SEM studies showed that single layer thickness of the films were between 65 and 80 nm. The structural characteristics were evaluated by changing the experimental parameters which are annealing temperature, annealing time and thickness of the films. From the X-ray diffraction analysis, maghemite formation was observed with decreasing annealing temperature, annealing time and film thickness. TEM results verified the presence of the maghemite phase by electron diffraction and selected area electron diffraction (SAED) methods. According to UV-Vis results transmittance of the films decreases with increasing annealing temperature.