In this work the effect of a SiO2 coating on the magnetic properties of Fe3O4 nanoparticles obtained by the sol-gel method is analyzed. Two sets of samples were prepared: Fe3O4 nanoparticles and Fe3O4@SiO2 core-shell composites. The samples display the characteristic spinel structure associated with the magnetite Fe3O4 phase, with the majority of grain sizes around 5-10 nm. At room temperature the nanoparticles show the characteristic superparamagnetic behavior with mean blocking temperatures around 160 and 120 K for Fe3O4 and Fe3O4@SiO2, respectively. The main effect of the SiO2 coating is reflected in the temperature dependence of the high field magnetization (μ(0)H = 6 T), i.e. deviations from the Bloch law at low temperatures (T < 20 K). Such deviations, enhanced by the introduction of the SiO2 coating, are associated with the occurrence of surface spin disordered effects. The induction heating effects (magnetic hyperthermia) are analyzed under the application of an AC magnetic field. Maximum specific absorption rate (SAR) values around 1.5 W g(-1) were achieved for the Fe3O4 nanoparticles. A significant decrease (around 26%) is found in the SAR values of the SiO2 coated nanocomposite. The different heating response is analyzed in terms of the decrease of the effective nanoparticle magnetization in the Fe3O4@SiO2 core-shell composites at room temperature.
The most stable form of iron oxide is Hematite (α-Fe2O3), which has interesting electronic, catalytic, and magnetic properties showing size dependent characteristics. At room temperature, Hematite is weakly ferromagnetic with a rhombohedral corundum structure. Upon cooling, the structure undergoes a first order spin reorientation, in which the net magnetic moment is lost. This transition is called the Morin transition. In this work, the first order Morin transition has been analyzed as a function of the temperature and applied magnetic field in Hematite nanoparticles. The magnetization was measured in the temperature range of the transformation at different applied magnetic fields to evaluate the entropy change linked to the Morin transition. The magnetic field promotes a shift of the transformation temperature. The change of entropy has been estimated on the basis of Clausius-Clapeyron type equation.
Fe 2 O 3 nanoparticles with sizes ranging from 15 to 53 nm were synthesized by a modified sol-gel method. Maghemite particles as well as particles with admixture of maghemite and hematite were obtained and characterized by XRD, FTIR, UV-Vis photoacoustic and M€ ossbauer spectroscopy, TEM, and magnetic measurements. The size and hematite/maghemite ratio of the nanoparticles were controlled by changing the Fe:PVA (poly (vinyl alcohol)) monomeric unit ratio used in the medium reaction (1:6, 1:12, 1:18, and 1:24). The average size of the nanoparticles decreases, and the maghemite content increases with increasing PVA amount until 1:18 ratio. The maghemite and hematite nanoparticles showed cubic and hexagonal morphology, respectively. Direct band gap energy were 1.77 and 1.91 eV for A6 and A18 samples. Zero-field-cooling-field-cooling curves show that samples present superparamagnetic behavior. Maghemite-hematite phase transition and hematite N eel transition were observed near 700 K and 1015 K, respectively. Magnetization of the particles increases consistently with the increase in the amount of PVA used in the synthesis. M€ ossbauer spectra were adjusted with a hematite sextet and maghemite distribution for A6, A12, and A24 and with maghemite distribution for A18, in agreement with XRD results. V
Room-temperature ferromagnetism in non-magnetic doped TiO2 semiconductor nanoparticles is analyzed in the present work. Undoped and N-doped TiO2 nanoparticles were obtained employing sol-gel procedure using urea as the nitrogen source. The obtained gels were first dried at 70 °C and afterwards calcined in air at 300 °C. A residual carbon concentration was retained in the samples as a consequence of the organic decomposition process. Post-annealing treatments at 300 °C under air and vacuum conditions were also performed. The crystallographic structure of nanoparticles was analyzed by X-ray diffraction, obtaining a single anatase crystalline phase after the calcinations (mean nanoparticle diameters around 5–8 nm). SQUID magnetometry was employed to analyze the magnetic response of the samples. Whereas for the undoped samples synthesized with hydrolysis rate h = 6, paramagnetic like behavior is observed at room temperature, the N-doped nanoparticles (h = 3) show a weak ferromagnetic response (saturation magnetization ≈10−3 emu/g). Moreover, a clear reinforcement of the room-temperature ferromagnetism response is found with the post-annealing treatments, in particular that performed in vacuum. Thus, the results indicate the dominant role of the oxygen stoichiometry and the oxygen vacancies in the room temperature ferromagnetic response of these TiO2 nanoparticles.
NiFe2O4 and NiFe2O4-SiO2 nanoparticles were synthesized by a sol-gel method using citric acid as fuel, giving rise its combustion to the crystallization of the spinel phase. Different synthesis conditions were analyzed with the aim of obtaining stoichiometric NiFe2O4 nanoparticles. The spinel structure in the calcined nanoparticles (400 °C, 2 h) was evaluated by x-ray diffraction. Their nanometer size (mean diameters around 10–15 nm) was confirmed through electron microscopy (field emission scanning electron microscopy and transmission electron microscopy). Rietveld refinement indicates the existence of a small percentage of NiO and Fe3O4 phases and a certain degree of structural disorder. The main effect of the silica coating is to enhance the disorder effects and prevent the crystalline growth after post-annealing treatments. Due to the small particle size, the nanoparticles display characteristic superparamagnetic behaviour and surface effects associated to a spin-glass like state: i.e., reduction in the saturation magnetization values and splitting of the zero field cooled (ZFC)-field cooled (FC) high field magnetization curves. The fitting of the field dependence of the ZFC-FC irreversibility temperatures to the Almeida—Thouless equation confirms the spin-glass nature of the detected magnetic phenomena. Exchange bias effects (shifts in the FC hysteresis loops) detected below the estimated freezing temperature support the spin-glass nature of the spin disorder effects.
The induction heating effects in amorphous and nanocrystalline wires, Fe73.5-xCrxSi13.5Cu1B9Nb3 (x = 3, 7, and 10), are analyzed in this work. In these alloys, the Curie temperature of the amorphous phase, TC, can be tailored through the Cr content of the alloy or the volume crystalline fraction after nanocrystallization. Four samples were selected; amorphous with x = 0 and 10 and nanocrystalline x = 7 with different crystalline fractions. The Curie temperature of the residual amorphous phase, TCa, was experimentally determined by the temperature dependence of the self-inductance of the samples. The analysis of the frequency dependence of the complex magnetic susceptibility enabled the estimation of the magnetic power losses in the samples. The heating effects on the wires were analyzed under the application of an ac magnetic field employing a home-made hyperthermia set-up. A single piece of a wire was immersed in a water bath (initial temperature from 291 K to 325 K) and subjected to the ac magnetic field. The specific absorption rate (SAR) was estimated through the initial slope of the temperature increase as a function of time. Maximum SAR values were obtained in the amorphous sample (x = 3) with the highest TC and enhanced magnetic power losses. In the nanocrystalline samples (x = 7), the detected heating effects above TCa are interpreted as a consequence of the magnetization process of the ferromagnetic grains. However, in spite of the low SAR displayed by the amorphous wire with TC ≈ 300 K (x = 10), interesting self-regulated characteristics are observed in this sample.
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