Zn0.95Fe0.05O solutions were prepared by sol-gel synthesis using 2,4-pentanedionate and acetate precursors which were dissolved into the solvent and chelating agent. The nanoparticles were annealed at various temperatures (400, 450, 500, 550, and 600 C-ay) and times to reveal the temperature effect on structural and magnetic properties. The thermal behaviors of the xerogels were analyzed using differential thermal analysis and thermogravimetric analysis to determine the heat treatment temperatures. The crystal structure and particle morphology were characterized by X-ray diffraction method and scanning electron microscope measurement tools. Quantum design physical properties measurement system was used to examine the magnetic properties of synthesized nanoparticles. The temperature and applied field dependences of magnetization of nanoparticles were recorded by using a vibrating sample magnetometer. Zero-field cooling and field-cooling conditions for magnetization as a function of temperature were performed at the magnetic field of 0.5 kOe. The structure, particle size, particle morphology, and magnetic properties of nanoparticles with different doping ratio, temperature, and time of annealing process were presented.