Fe 2 O 3 nanoparticles with sizes ranging from 15 to 53 nm were synthesized by a modified sol-gel method. Maghemite particles as well as particles with admixture of maghemite and hematite were obtained and characterized by XRD, FTIR, UV-Vis photoacoustic and M€ ossbauer spectroscopy, TEM, and magnetic measurements. The size and hematite/maghemite ratio of the nanoparticles were controlled by changing the Fe:PVA (poly (vinyl alcohol)) monomeric unit ratio used in the medium reaction (1:6, 1:12, 1:18, and 1:24). The average size of the nanoparticles decreases, and the maghemite content increases with increasing PVA amount until 1:18 ratio. The maghemite and hematite nanoparticles showed cubic and hexagonal morphology, respectively. Direct band gap energy were 1.77 and 1.91 eV for A6 and A18 samples. Zero-field-cooling-field-cooling curves show that samples present superparamagnetic behavior. Maghemite-hematite phase transition and hematite N eel transition were observed near 700 K and 1015 K, respectively. Magnetization of the particles increases consistently with the increase in the amount of PVA used in the synthesis. M€ ossbauer spectra were adjusted with a hematite sextet and maghemite distribution for A6, A12, and A24 and with maghemite distribution for A18, in agreement with XRD results. V