NiFe2O4 ferrite was synthesized by sol-gel method. Its structural characteristics, morphology, electromagnetic and microwave absorption properties were analyzed by X-ray diffraction, scanning electron microscope and network analyzer, and analyzed the influence of the combustion temperature and citric acid. The results indicated that the particle size be enlarged with an increased combustion temperature and be diminished first, then increased with the increased of citric acid, and the best ratio of citric acid with metal ions for nCA: nFe: nNi = 4:2:1. Its microwave absorbing property is increased with the increased combustion temperature. Its complex permittivity imaginary part first decreases with temperature increases and then increases, the imaginary part of complex permeability with increasing temperature increases, indicating that the increase of calcination temperature, help to improve the sample microwave absorbing properties.