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  • Artigo IPEN-doc 25614
    Low temperature synthesis of pure and Fe-doped HfSiO4: Determination of Si and Fe fractions by neutron activation analysis
    2019 - SALES, T.N.S.; BOSCH-SANTOS, B.; SAIKI, M.; BURIMOVA, A.; PEREIRA, L.F.D.; SAXENA, R.N.; CARBONARI, A.W.
    A new method of synthesis of hafnium silicate HfSiO4 (also known as hafnon) is reported. We observed a selfcontrolled incorporation of SiO2 from the quartz tube in which a sample of hafnium oxide nanoparticles was heated. This approach was then adapted to Fe-doped hafnon production. Sample structure, morphology and composition were characterized by X-ray diffraction, electron microscopy and neutron activation analysis. Diffraction data has shown that lattice parameters of doped HfSiO4 thus obtained are very close to those previously known for bare hafnon. The hafnon-like phase stabilized at T=900 °C which is about 500 °C lower than the corresponding transition of bare bulk hafnium silicate. The fractions of Si and Fe in the composite matrices were determined with neutron activation analysis. These results completed by X-ray diffraction data allowed to assume that (i) Fe initially substituted Hf in the HfO2 lattice; (ii) there was no migration of iron atoms from Hf to Si sites at the formation of hafnon-like phase; (iii) doped and undoped hafnium oxide has taken as much Si from the quartz as was needed for the arrangement of Fe1-xHfxSiO4 tetragonal system, 0≤x<0.2. Our results are consistent with those obtained for similar materials, such as metal (Fe,V) doped zircon, where the dopant also demonstrated catalytic effect on phase stabilization.
  • Artigo IPEN-doc 23107
    Stable tetragonal phase and magnetic properties of Fe-doped HfO2 nanoparticles
    2017 - SALES, T.S.N.; CAVALCANTE, F.H.M.; BOSCH-SANTOS, B.; PEREIRA, L.F.D.; CABRERA-PASCA, G.A.; FREITAS, R.S.; SAXENA, R.N.; CARBONARI, A.W.
    In this paper, the effect in structural and magnetic properties of iron doping with concentration of 20% in hafnium dioxide (HfO2) nanoparticles is investigated. HfO2 is a wide band gap oxide with great potential to be used as high-permittivity gate dielectrics, which can be improved by doping. Nanoparticle samples were prepared by sol-gel chemical method and had their structure, morphology, and magnetic properties, respectively, investigated by X-ray diffraction (XRD), transmission electron microscopy (TEM) and scanning electron microscopy (SEM) with electron back scattering diffraction (EBSD), and magnetization measurements. TEM and SEM results show size distribution of particles in the range from 30 nm to 40 nm with small dispersion. Magnetization measurements show the blocking temperature at around 90 K with a strong paramagnetic contribution. XRD results show a major tetragonal phase (94%).
  • Artigo IPEN-doc 24061
    Effect of silicon doping in HFO2 nanoparticles from an atomic view
    2017 - SALES, TATIANE S.N.; CARBONARI, ARTUR W.
    We have prepared the Hafnium Oxide (HfO2) nanoparticles (NPs) doped with 5% at. of silicon (Si) using the sol-gel chemical method. Nuclear quadrupole interactions at Hf sites were investigated by perturbed γ–γ angular correlations (PAC) spectroscopy using 181Ta as probe nuclei. This method is based on the hyperfine interactions between the nuclear moments of the probe nuclei with extra-nuclear magnetic fields or electric field gradients (EFGs). In the case of quadrupolar electric interactions, experimental measurements give the quadrupole frequency Q with respective distribution () as well the asymmetry parameter  of of of the EFG. The hyperfine parameters were measured within the range from 200°C to 900°C. The structural and morphological characterization of the samples were carried out by X-ray diffraction and scanning electron microscopy (SEM) with electron back scattering diffraction (EBSD). PAC results show a major site fraction of probe nuclei, that was assigned to the monoclinic phase of HfO2, with approximately 60% population, which increases when the temperature of heat treatment increases. The XRD results showed a single phase with the expected monoclinic structure for the as-prepared samples indicating that Si atoms are at substitutional Hf sites.