In the present research, nickel hydroxide, nickel oxide and nickel ferrites (NiFe2O4) nanoparticles, as well as NiFe2O4 / NiO nanostructures were prepared using a rapid and simple microwave method. The influence of power and pulses on the size and morphology of the produced nanostructures were investigated. The obtained nanostructure products were characterized via scanning electron microscopy (SEM), Fourier transform infrared (FT-IR) spectroscopy and X-ray diffraction (XRD) techniques. The magnetic property of the nanostructures was studied by a vibrating sample magnetometer (VSM). The results illustrate that by calcination of NiFe2O4 nanoparticles the magnetic behaviours of samples change from super-paramagnetic to ferromagnetic. The photo-catalytic behaviour of NiFe2O4-NiO nanocomposites was evaluated using the photo-degradation of congo-red in different pH conditions (pH=3 and pH=5) under the irradiation of ultraviolet light. These results show that prepared nanocomposites are applicable as magnetic and photo-catalytic material in UV lights.