In this work, we report on a single-pot synthesis route based on a polymeric precursor method used for successfully producing undoped and iron-doped CeO2 nanoparticles with iron contents up to 10.0 mol. %. The formation of high-crystalline nanoparticles with a cubic fluorite structure is determined for all the studied samples. Meanwhile, the magnetic measurements of the undoped ceria nanoparticles revealed the occurrence of ferromagnetism of bound magnetic polarons of a fraction of Ce3+ at room temperature, and only a paramagnetic behavior of Fe3+ ions was determined for Fe-doped ceria nanoparticles. A monotonous reduction of the effective magnetic moment of the Fe3+ ions was determined. It suggests a change from a high-spin to low-spin state of Fe ions as the Fe content is increased. The 3+ valence state of the iron ions has been confirmed by the Fe K-edge X-ray absorption near-edge structure (XANES) and Mössbauer spectroscopy measurements. X-ray photoelectron spectroscopy data analysis evidenced a coexistence of Ce3+ and Ce4+ ions and a decreasing tendency of the relative fraction of Ce3+ ions in the surface region of the particles as the iron content is increased. Although the coexistence of Ce3+ and Ce4+ is confirmed by results obtained via Ce L3-edge XANES measurements, any clear dependence of the relative relation of Ce3+ ions on the iron content is determined, suggesting a homogeneous distribution of Ce3+ and Ce4+-ions in the whole volume of the particles. Ce L3-edge extended X-ray absorption fine structure revealed that the Ce-O bond distance shows a monotonous decrease as the Fe content is increased, which is in good agreement with the shrinking of the unit cell volume with the iron content determined from XRD data analysis, reinforcing the substitutional solution of Ce and Fe ions in the CeO2 matrix.
We report on the study of the structural and magnetic properties of crystalline Fe-doped ZnO nanoparticles with Fe content up to 10% synthesized by a co-precipitation method. The Rietveld analysis indicates that the Fe-doped ZnO nanoparticles are formed in a single phase wurtzite structure. DC magnetization (M) vs. applied magnetic field (H) curves obtained at 5 K show the occurrence of a ferromagnetic behavior. The coercive field and saturation magnetization depend on the Fe content. At room temperature, M vs. H curves show features consistent with a superparamagnetic state of nanoscale system. The temperature dependence of the AC and DC magnetic susceptibilities show features related to the thermal relaxation of the nano-sized particles. From the AC data analysis, a magnetic transition from the superparamagnetic to cluster-glass state is determined.
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