Boone, Peter S. | Search NASA

DOE OSTI2024

Electrophoretic deposition for improved trace element homogeneity in silica reference materials

Spatially-resolved analysis requires homogeneous reference materials (RMs) to make reliable quantitative measurements. Here we previously developed an electrophoretic deposition (EPD) method for fabrication of glassy microanalytical RMs with superior platinum-group element homogeneity **[1], and now include further dopants. For 39 trace elements, we analyzed dopant homogeneity in sintered silica (SiO 2 ) samples consolidated either mechanically by die-pressing (DP) or by EPD. A set of EPD and DP samples was made from each of two nanoparticle feedstocks produced by variations of the Stöber process **[2]. Spatially-resolved dopant distribution was characterized in all samples by laser-ablation inductively-coupled plasma mass spectrometry (LA-ICP-MS). In both sample sets, homogeneity of most trace elements was substantially improved by EPD relative to their DP counterpart.

36 MATERIALS SCIENCE↗

DOE OSTI2022

The effect of oxygen concentration on the speciation of laser ablated uranium

Abstract In order to model the fate and transport of particles following a nuclear explosion, there must first be an understanding of individual physical and chemical processes that affect particle formation. One interaction pertinent to fireball chemistry and resultant debris formation is that between uranium and oxygen. In this study, we use laser ablation of uranium metal in different concentrations of oxygen gas, either 16 O 2 or 18 O 2 , to determine the influence of oxygen on rapidly cooling uranium. Analysis of recovered particulates using infrared absorption and Raman spectroscopies indicate that the micrometer-sized particulates are predominantly amorphous UO x (am-UO x , where 3 ≤ x ≤ 4) and UO 2 after ablation in 1 atm of pure O 2 and a 1% O 2 /Ar mixture, respectively. Energy dispersive X-ray spectroscopy (EDS) of particulates formed in pure O 2 suggest an O/U ratio of ~ 3.7, consistent with the vibrational spectroscopy analysis. Both am-UO x and UO 2 particulates convert to α-U 3 O 8 when heated. Lastly, experiments performed in 18 O 2 environments show the formation of 18 O-substituted uranium oxides; vibrational frequencies for am-U 18 O x are reported for the first time. When compared to literature, this work shows that cooling timescales can affect the structural composition of uranium oxides (i.e., crystalline vs. amorphous). This indicator can be used in current models of nuclear explosions to improve our predicative capabilities of chemical speciation.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗