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Nano nickel ferrite particles were prepared at pH values 1.5, 4, 7, 10, 13 by a hydrothermal method using metal chlorides and NaOH as an oxidant and solution basicity controller. There is a phase transition from hematite to spinel ferrite that begins when the pH reaches 4. The lowest crystallite size (4 nm) was associated with a highest lattice constant (8.345 Å), at pH=4. Whereas maximum crystallite size 64.5 nm corresponds lattice constant of 8.298 Å at pH=10. The highest magnetization (48 emu/g) value was achieved for the sample prepared at pH=7, which at the same time has a lower coercivity. The samples synthesized at pH ≥4 show superparamagnetic behavior owing to its low particle size and to zero field cooling and field cooling measurements. The ferromagnetic resonance (FMR) cavity tests analysis show that the broadened linewidth (770 Oe) and high imaginary permeability or high microwave absorption which is linked to high magnetization and low coercivity of superparamagnetic particles and their aggregation. There was a shift in the resonance field due to internal fields and cation distribution.