NiFe2O4(NFO) is synthesized by the hydrothermal technique where the salts of nickel and iron are mixed in a stoichiometric ratio and kept in autoclave for different times, i.e., 12 h, 15 h, 18 h, and 21 h, but the temperature is kept the same which is 180 °C for all samples. This technique is very useful to fabricate nanomaterials with many advantages like low-temperature synthesis, cheap, simple, and easy sample processing. The material was characterized using X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), and vibrating sample magnetometer (VSM) to study its structural and magnetic properties. XRD confirms the presence of all characteristic peaks corresponding to NFO but the exact pure phase of nickel ferrite forms under the condition of 15 h; in other three samples, an extra impurity peak of hematite (α-Fe2O3) is also present. Further, FESEM studies represent the uniformity and homogeneity in the material. VSM reveals Magnetization-Magnetic (M-H) field loop results in which the highest saturation magnetization comes out to be ~ 50 emu. g−1 for 15 h sample. So, for this particular condition, nickel ferrite is optimized to get a pure phase along with maximum saturation magnetization. The positive impact of the processing on the magnetic properties could be used for the development of soft ferrites for various magnetoelectric applications.