2026-10-14T21:16:54Z https://api.figshare.com/v2/oai

oai:figshare.com:article/33758380 2026-09-14T20:48:51Z portal_1197 item_type_3 month_year_09_2026

Data for Incorporation of Sb5+ into CeO2 : local structural distortion of the fluorite structure from a pentavalent substituent Craig I. Hiley (6086510) Janet M. Fisher (2133238) Reza J. Kashtiban (1423762) Giannantonio Cibin (1342398) David Thompsett (2101270) Richard I. Walton (1328463) Cerium oxides Catalysis Antimony compounds Migrated from ePrints Hydrothermal crystallisation of CeO2 from aqueous sodium hydroxide solution at 240 C using CeCl3·7H2O in the presence of hydrogen peroxide with addition of either SbCl3 or SbCl5 yields polycrystalline samples of antimony-containing ceria directly from solution. Powder X-ray diffraction sShows a contraction of the cubic lattice parameter with increasing Sb content, and also a broadening of Bragg peaks, from which Scherrer analysis yields crystallite domain sizes of 5 - 20 nm. Scanning transmission electron microscopy provides consistent results with observation of highly crystalline particles of a few nm in diameter. X-ay absorption near edge structure spectroscopy at the Ce LIII and Sb K edges reveals the presence of Ce4+ and Sb5+ in the solids. To balance charge the presence of co-included Na is proposed, corroborated by elemental analysis. The general chemical formula of the materials can thus be written as (Ce1 xSbx)1 yNayO2-δ (where x < 0.4 and y ≥ x/3). Sb K-edge extended X-ray absorption fine structure spectroscopy of the substituted ceria samples shows that the local structure of Sb resembles that in NaSbO3, where six-coordinate metal sites are found, but with evidence of a longer interatomic correlation due to surrounding Ce/Sb atoms in the fluorite structure; this implies that the Sb is displaced from the ideal eight-coordinate site of the fluorite structure. This structural distortion gives materials that are unstable under reducing conditions, coupled by the ease of reduction to elemental antimony, which is extruded leading to phase separation.<br><br>Data are organised in folders according to the figures they are plotted in (numbered as in the paper). Each folder contains sets of .txt files for each experimental data-set shown: each is a two-column ascii file labelled according to the material from which the data were recorded. 2018-07-05T00:00:00Z Dataset Dataset 10.82444/warw.33758380.v1 https://figshare.com/articles/dataset/Data_for_Incorporation_of_Sb5_into_CeO2_local_structural_distortion_of_the_fluorite_structure_from_a_pentavalent_substituent/33758380 CC BY 4.0