Characterisation of nickel–zinc ferrite/silica nanocomposites with low ferrite concentration obtained by an improved modified sol–gel method

The paper presents a study regarding the structure, morphology and magnetic behaviour of x% (Ni_0.65Zn_0.35Fe₂O₄)/(100 − x)% SiO₂ ferrimagnetic nanocomposites for low Ni–Zn ferrite concentration (x = 5, 10, 15, 20 and 30 mass percent) obtained by an improved modified sol–gel method. The obtained gels and nanocomposites have been characterized by fast Fourier transform-infrared (FT-IR) spectrometry, X-ray diffraction (XRD), transmission electron microscopy (TEM) and magnetic measurements (MM). The addition of a supplementary quantity of diol in the synthesis, corresponding to a molar ratio EG : TEOS = 1:1, and the control of the thermal treatment applied to the precursor xerogels tetraethylortosilicate (TEOS)–metal nitrates (MN)–ethylene glycol (EG) leads to fine (~2–9 nm), almost spherical Ni–Zn ferrite nanoparticles homogenously dispersed inside the amorphous SiO₂ matrix. TEM images reveal the fine nature and the narrow size distribution of the ferrite nanoparticles. Nanoparticles diameter increases with the ferrite concentration and with the annealing temperature. For all concentrations of ferrite in SiO₂ and all annealing temperature, we have obtained Ni_0.65Zn_0.35Fe₂O₄ ferrite as single phase (proven by XRD) in the amorphous silica matrix, only after a pre-treatment of synthesized gels, at 573 K, for 3 h. The magnetic behaviour of ferrite nanoparticles in quasi-static magnetic fields is very particular, depending on the annealing temperature and the ferrite content in silica matrix. We have obtained superparamagnetic behaviour for the nanocomposites, for a concentration of 30% ferrite in SiO₂ at high annealing temperature, of 1,273 K.