Metallic oxide materials with AB2O4 structure are very interesting for technological applications. Nickel ferrite (NiFe2O4), for example, attracts considerable attention due to its chemical stability and mechanical hardness. These characteristics make it a suitable material for magnetic and magneto-optical applications. The properties of NiFe2O4 have a strong dependence on the crystallite size and microstructure. Due to this dependence, it is necessary to develop effective methods that allow controlling these variables. The aim of this work is to investigate the effect of time, temperature of isothermal treatment and choice of organic precursor during the production of NiFe2O4 samples employing the proteic sol-gel method have on crystallite size and microstructure. Two kinds of organic precursors were used: coconut water and pectin extracted from aple peel. Temperatures of 873 and 1173 K; 2, 4, 6, 8, 24 and 30 hours of isothermal treatment were also used. The samples produced were analyzed employing X-ray Diffraction.