In this work, the crystalline structure, chemical composition, size, and morphology of core@shell nanoparticles based on Zn-Mn ferrite nanocrystals were investigated. These materials have been proposed as promising candidates for multifunctional applications in biomedicine, catalysis, environmental remediation, among others. Those properties were probed by using several experimental techniques such as Synchrotron X-Ray Diffraction, Energy-Dispersive X-ray Spectroscopy, Transmission Electron Microscopy and Selected Area Electron Diffraction. Results show that all synthesized nanoparticles present a single crystalline spinel phase without the appearance of undesirable byproducts. The nanoparticles present a non-stoichiometric Zn-Mn ferrite core, due to a Fe enrichment and a Zn loss with respect to the synthesis medium. The surface treatment of the nanoparticles induces a greater iron enrichment, which occurs at the nanoparticles surface without changing the crystalline structure. Finally, modifications in lattice parameters and strain suggest a contribution of the Mn2+ cations, mainly related to their easy oxidation in the synthesis route, which increases the structural vacancies of Mn-richer ferrites.

We report on experimental observations of self-assemblies in colloidal dispersions of clay nanoplatelets and magnetic nanoparticles. Visual observations have been combined with small angle X-ray scattering (SAXS) in the study of several composites at a fixed clay concentration in the dilute regime, and varying ferrofluid concentrations. Our visual observations which encompass macroscopic separation in gravitational- and magnetic field, indicate that all samples present a concentrated phase and a diluted one. SAXS data obtained from each phase are consistent with the interpretation that the scattering contribution from the clay nano-platelets in the samples can be neglected in comparison with the magnetic particle contribution. The analysis of the scattered intensity is performed combining two models, one based on the global scattering function and the other allowing the extraction of the structure factor of the mixtures. The parameters of the size distribution of magnetic nanoparticles determined by both methods are in good agreement. The structure factor of the mixtures shows that on a local scale, the mixtures behave like a gas of isolated magnetic nanoparticles. It also indicates the presence of interactions between magnetic nanoparticles mediated by the presence of Laponite platelets. Such interactions could be attributed with a progressive partial phase separation between spheres and discs rather than to the formation of dense aggregates.