Nickel ferrite/multi-walled carbon nanotubes (NiFe 2 O 4 /MWCNTs) composite has been rapidly synthesized via microwave irradiation technique. The structural properties of the product was investigated by X-ray diffraction (XRD), N 2 adsorption/desorption isotherms, thermogravimetric analysis (TGA), Raman spectroscopy and, scanning electron microscopy (SEM). Catalytic behavior of the composite material on the advanced photo-Fenton degradation of Amaranth dye was evaluated. The synthesis conditions employed on the microwave system were: temperature (235 °C), power (500 W), pressure (600 psi) and irradiation time (30 min). Characterization results showed the formation of hybrid material, containing a predominantly microporous structure, with surface area and total pore volume of 54 m 2 g -1 and 0.2249 cm 3 g -1 , respectively. The composite exhibited higher catalytic activity compared to the pure NiFe 2 O 4 , reaching 100% of decolorization at 60 min of reaction, which can be attributed to a synergism between NiFe 2 O 4 and MWCNTs. Therefore, NiFe 2 O 4 /MWCNTs composite can be used as a promising photo-Fenton catalyst to degrade Amaranth dye from aqueous solutions.