RESUMO
CeO2 nanorods were synthesized by a hydrothermal method and used as the support for preparing a series of Ni/CeO2 nanorod catalysts. The surface area of the catalysts decreased when the Ni percent over the CeO2 nanorods was increased. SEM results showed that the CeO2 is formed by nanorods approximately 1 µm in length. TEM and HREM revealed that the width of the nanorods is about 8 nm and it grew along the [1 1 1¯] axis. The catalytic activity of the catalysts was improved as the Ni was loaded onto CeO2 nanorods. The exposed planes of the CeO2 nanorod structure along the zone axis [0 1 1] for Ni impregnation were (1¯ 1¯ 1), (1 1 1¯), (1 1¯ 1), (1¯ 1 1¯), (2 0 0) and (2¯ 0 0) and they were more reactive for methanol conversion than (2¯ 2¯ 0), (2¯ 0 2¯), (0 2 2¯), (0 2¯ 2), (2 0 2) and (2 2 0) planes from the [1 1 1¯] axis (growth direction of the nanorod). This finding is mainly ascribed to the synergistic effect of the CeO2 nanorods and the Ni.
RESUMO
Silver nanowires were used as templates to synthesize silver-doped CeO(2) (Ag-CeO(2)) nanotubes by the precipitation method. The precipitated solid was dried at 100 °C for 24 h and calcined at 500 °C for 5 h. A TEM, HRTEM, LV-SEM and XRD study was carried out to determine the micro and nanostructural characteristics of the samples. LV-SEM analysis allowed us to observe microtubular empty structures constituted by Ce, O and Ag as indicated by EDS. These tubular structures, with an external diameter from 120 to 280 nm and an internal diameter from 40 to 80 nm, were mainly composed of 11 nm ceria nanoparticles. This kind of structures was obtained when CeO(2) nanoparticles covered the Ag nanowires during the synthesis. Due to the presence of ammonium hydroxide used during the synthesis, a fraction of the silver nanowire reacts and Ag atoms begin to migrate outside the ceria microtube. When the sintering process is applied, the Kirkendall effect can occur. So, out-diffusion of the remnant Ag through the interface is faster than the in-diffusion of the shell material (CeO(2)), which eventually results in a coaxial nanotube on completion of the non-equilibrium interdiffusion, leaving the central core completely empty, driving the formation of hollow tubular Ag-CeO(2) structures as a result.
RESUMO
The goal of this work was to analyse ZrO(2) in the pure state and when doped with Ag nanoparticles, by electron microscopy, x-ray diffraction and thermoluminescence methods. According to the results obtained, Ag nanoparticles did not modify the morphology or the crystalline structure of the ZrO(2). The thermoluminescent (TL) response of pure ZrO(2) showed two peaks, one at 334 K and the other at 417 K, when it was exposed to ultraviolet (UV) radiation, and at 342 and 397 K when gamma radiation was used. For ZrO(2) impregnated with Ag nanoparticles a diminished TL intensity due to nanoparticle shielding was observed, but the glow curve shape was similar. However, when Ag nanoparticles were added during the ZrO(2) synthesis, a shift of the TL peaks towards higher temperature values with reference to pure ZrO(2) was observed. A linear dependence of the integrated TL signal as a function of the irradiation dose was observed in all analysed samples. It was possible to determine some kinetic parameters, such as activation energy, kinetic order and frequency factor, using the sequential quadratic programming glow curve deconvolution; it was found that these values are highly dependent on the type of radiation used. Ag nanoparticles present in ZrO(2) also modified the kinetic parameters, mainly when they were added during the synthesis of ZrO(2). Our results reinforce the possibilities of using pure and doped ZrO(2) as an appropriate dosimetric material in radiation physics.