Synthesis and characterization of the NiFe2O4/Ni3Fe nanocomposite powder and compacts obtained by mechanical milling and spark plasma sintering

Nanocomposite powder and compacts of NiFe2O4/Ni3Fe type were synthesized using mechanical milling and spark plasma sintering (SPS) techniques. The samples have been investigated by X-ray diffraction (XRD), laser particles size analysis, differential scanning calorimetry (DSC), scanning electron microscopy (SEM) and energy dispersive X-ray spectrometry (EDX). The nanocomposite powder was obtained by mechanical milling in a high planetary ball mill of nanocrystalline NiFe2O4 and nanocrystalline Ni3Fe powders. The nanocomposite powder consists from Ni3Fe particles covered at the surface with a layer of NiFe2O4 fine particles and NiFe2O4 particles. The nanocomposite particles have the median diameter d50 of 1.6 μm. The sintering in 400–600 °C temperature range preserve the nanocomposite phases but lead to a high porosity. The nanocomposite compacts consist in Ni3Fe clusters surrounded by NiFe2O4. A sintering temperature of 800 °C leads to a good density for the nanocomposite compacts and to the new phase formation. The new phase is a wustite type (Fe1−xNixO) and is formed at the metal/ceramic interface. A change in the Ni/Fe ratio, in the spinel structure, was evidenced during sintering. Sintering at a temperature of 800 °C, leads to the formation of a mixed iron–nickel ferrite with a very small amount of nickel, Ni1−xFexFe2O4.