In the present investigation, spherical nanoparticles of nickel ferrite with uniform structure were successfully produced by hydrothermal method in the presence of polyethylene glycol (PEG) as a polymeric surfactant at 180°C for 12 hour aging time and the effects of the synthesis time, temperature and surfactant were investigated. According to the X-ray analysis, conversion of nickel oxide and hematite to nickel ferrite was a way to produce NiFe2O4. At 140‌°C, agglomerated particles without specific shape were formed, but at 180°C particles were homogenous with spherical shape. Saturation magnetization increased by increasing the hydrothermal process aging time.