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.
In this work, the effect of nickel doping on the structural and magnetic properties of Fe3O4 nanoparticles is analysed. Ni(x)Fe(3-x)O4 nanoparticles (x = 0, 0.04, 0.06 and 0.11) were obtained by chemical co-precipitation method, starting from a mixture of FeCl2 x 4H2O and Ni(AcO)2 x 4H2O salts. The analysis of the structure and composition of the synthesized nanoparticles confirms their nanometer size (main sizes around 10 nm) and the inclusion of the Ni atoms in the characteristic spinel structure of the magnetite Fe3O4 phase. In order to characterize in detail the structure of the samples, X-ray absorption (XANES) measurements were performed on the Ni and Fe K-edges. The results indicate the oxidation of the Ni atoms to the 2+ state and the location of the Ni2+ cations in the Fe2+ octahedral sites. With respect to the magnetic properties, the samples display the characteristic superparamagnetic behaviour, with anhysteretic magnetic response at room temperature. The estimated magnetic moment confirms the partial substitution of the Fe2+ cations by Ni2+ atoms in the octahedral sites of the spinel structure.
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.
This paper reports the use of the electrospinning technique for the synthesis of nanocomposite micro/nanofibers by combining a polymeric precursor with hydrophobic behavior like polyvinyl chloride (PVC) with nanoparticles of a corrosion inhibitor like ZnO. These electrospun fibers were deposited on substrates of the aluminum alloy 6061T6 until forming a coating around 100 μm. The effect of varying the different electrospinning deposition parameters (mostly applied voltage and flow-rate) was exhaustively analyzed in order to optimize the coating properties. Several microscopy and analysis techniques have been employed, including optical microscopy (OM), field emission scanning electron microscopy (FE-SEM), atomic force microscopy (AFM), thermogravimetric analysis (TGA), and differential scanning calorimetry (DSC). Water contact angle (WCA) measurements have been carried out in order to corroborate the coating hydrophobicity. Finally, their corrosion behavior has been evaluated by electrochemical tests (Tafel curves and pitting potential measurements), showing a relevant improvement in the resultant corrosion resistance of the coated aluminum alloys.
In this work, polymeric fibers of polystyrene (PS) with incorporated ZnO nanoparticles have been deposited onto an aluminum alloy substrate (6061T6) by using the electrospinning technique. In order to optimize the deposition process, the applied voltage and flow rate have been evaluated in order to obtain micrometric electrospun fibers with a high average roughness and superhydrophobic behavior. Thermogravimetric analysis (TGA) has also been employed in order to corroborate the amount of ZnO incorporated into the electrospun fibers, whereas differential scanning calorimetry (DSC) has been performed in order to determine the glass transition temperature (T g ) of the polymeric electrospun fibers. In addition, a specific thermal treatment (T g + 20 • C) of the synthesized electrospun fibers has been evaluated in the resultant corrosion resistance. A comparative study with previously reported results corresponding to polyvinyl chloride (PVC) fibers is carried out along this paper to show the changes in behavior due to the different compositions and fiber diameters. The coating has produced an important reduction of the corrosion current of the aluminum substrate in two orders of magnitude, showing also an important enhancement against pitting corrosion resistance. Finally, this deposition technique can be used as an innovative way for the design of both superhydrophobic and anticorrosive surfaces in one unique step over metallic substrates with arbitrary geometry.
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.
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