Evolution of the phase state of paramagnetic additions at various stages of synthesis and subsequent thermal treatment of glasses of the system Al 2 O 3-K 2 O-B 2 O 3 simultaneously doped with Fe 2 O 3 and MnO is studied by means of a combination of experimental techniques: Faraday rotation ͑FR͒, electron magnetic resonance ͑EMR͒, transmission electron microscopy ͑TEM͒, Mössbauer spectroscopy, and magnetic measurements. Both FR and EMR show that magnetically ordered clusters occur already at the first stage of the glass preparation. In particular, for the ratio of the Fe and Mn oxides in the charge close to 3:2, fine magnetic nanoparticles are formed with characteristics similar to those of manganese ferrite. By computer simulating the EMR spectra at variable temperatures, a superparamagnetic nature of these nanoparticles is confirmed and their mean diameter is estimated as approximately 3.2 nm. In the thermally treated glasses larger magnetic nanoparticles are formed, giving rise to FR spectra, characteristic of magnetically ordered systems, and the EMR spectra different from those in as-prepared glasses but also showing superparamagnetic narrowing. The Mössbauer spectroscopy corroborates the manganese ferrite structure of the nanoparticles and indicates their coexistence in the ferrimagnetic and superparamagnetic states. The TEM shows the presence of polydisperse nanoparticles on the background of the glass matrix, and electron diffraction of a selected region containing larger particles indicates a crystal structure close to that of MnFe 2 O 4. Energy-dispersive atomic x-ray spectra confirm that the major part of Fe and Mn introduced to the glass composition is gathered in the particles, with the concentration ratio close to 2:1, characteristic of bulk MnFe 2 O 4. Magnetic hysteresis loops of samples subjected to an additional thermal treatment demonstrate a strong increase in the coercive force, remnant magnetization, and high-field magnetic susceptibility with temperature decrease. The consistent results obtained using various techniques demonstrate that the formation of nanoparticles with characteristics close to those of MnFe 2 O 4 confers to these glasses magnetic and magneto-optical properties typical of substances possessing magnetic order.
In this study, NiFe2O4@Au core–shell nanoparticles were prepared by the direct reduction of gold on the magnetic surface using amino acid methionine as a reducer and a stabilizing agent simultaneously. The obtained nanoparticles after three steps of gold deposition had an average size of about 120 nm. The analysis of particles was performed by X-ray diffraction, transmission electron microscopy, X-ray photoelectron spectroscopy, and UV-Vis spectroscopy techniques. The results indicate successful synthesis of core–shell particles with the magnetic core, which consists of a few agglomerated nickel ferrite crystals with an average size 25.2 ± 2.0 nm, and the thick gold shell consists of fused Au0 nanoparticles (NPs). Magnetic properties of the obtained nanoparticles were examined with magnetic circular dichroism. It was shown that the magnetic behavior of NiFe2O4@Au NPs is typical for superparamagnetic NPs and corresponds to that for NiFe2O4 NPs without a gold shell. The results indicate the successful synthesis of core–shell particles with the magnetic nickel ferrite core and thick gold shell, and open the potential for the application of the investigated hybrid nanoparticles in hyperthermia, targeted drug delivery, magnetic resonance imaging, or cell separation. The developed synthesis strategy can be extended to other metal ferrites and iron oxides.
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