A. García-Ruiz

Hydrolysis, Condensation, and Tetragonal Phase Formation in Sol-Gel Zirconia Prepared with Electron-Irradiated Alkoxide Solutions

Sol-gel zirconia precursor, zirconium n-butoxide in ter-butanol, was irradiated with 1.3 MeV electrons to a dose of 330 KGy. Gelling was instantaneously produced when an aqueous solution of sulfuric, hydrochloric or acetic acid was added to the irradiated solution; no hydrolysis catalyst was required. Samples were characterized with X-ray powder diffraction, infrared spectroscopy, and electron paramagnetic resonance. The electron irradiation accelerated hydrolysis and condensation, which avoided the stabilization of the tetragonal phase via carboxyls, and decreased the capability of sulfate ions to stabilize it. These results suggest that the stabilization of the tetragonal phase of sol-gel zirconia via carboxyl and sulfate ions depends on their diffusion in the sol.

Characterization of Pt-Pd bimetallic nanoparticles by Cs-corrected STEM.

Pt-Pd bimetallic nanoparticles were characterized using aberration (Cs) corrected scanning transmission electron microscopy (STEM) along with molecular dynamics simulations. The nanoparticles were synthesized through a microwave-assisted process. This technique has been applied to synthesize metallic nanoparticles at relatively short times, allowing a good control of size distribution. The structure of the bimetallic nanoparticles is fcc-like with an average size of 5 nm. To understand the properties of the bimetallic nanoparticles, it is necessary to know the positions of all the atoms in the nanostructure. We have used a recent quantitative method to analyze HAADF STEM images which allowed us to measure the total intensity of the scattered electrons for each atomic column. Beside with the characterization of the nanoparticles, we have performed classical molecular dynamics simulation for the structural and dynamical analysis of the cuboctahedral Pt-Pd bimetallic nanoparticles.

Rietveld Structure Refinement of Hydrothermally Grown Zinc Peroxide Nanoparticles

Nanocrystals of zinc oxides have demonstrated to be very important materials for several applications in many fields, particularly in catalysis. Nanocrystalline zinc peroxide (ZnO2), which is a precursor of zinc oxide (ZnO), has been prepared by means of a hydrothermal process from zinc acetate dehydrates. On the other hand, it is of great interest to have a detailed structural characterization, in order to correlate it with the catalytic properties of the synthesized material. In this work, some results are presented about the nanostructure of the prepared zinc peroxide. By using X-ray diffraction followed of a pattern refinement by the Rietveld techniques, refined average cell parameters and crystallite size were calculated and, from these refined values, crystallite morphology was simulated in an averaged manner. With the aim to get a more complete characterization, besides these results, some micrographs of the crystalline structure of ZnO2, observed by TEM, were also included in this work.