Quantifying Impurity Effects on the Surface Morphology of α‑U3O8

• Published in: Analytical chemistry (Washington) Vol. 91; no. 15; pp. 10081 - 10087
• Main Authors: Hanson, Alexa B, Lee, Rachel Nicholls, Vachet, Clement, Schwerdt, Ian J, Tasdizen, Tolga
• Format: Journal Article
• Language: English
• Published: Washington American Chemical Society 06.08.2019
• Subjects: Calcium; Chemistry; Crystallography; Imagery; Impurities; Impurity effects; Inductively coupled plasma mass spectrometry; Learning algorithms; Machine learning; Magnesium; Mass spectrometry; Mass spectroscopy; Morphology; Nitrates; Peroxide; Scanning electron microscopy; Synthesis; Uranium oxides; Water purification; X ray powder diffraction; X-ray diffraction; X-ray spectroscopy; Zirconium
• ISSN: 0003-2700; 1520-6882
• DOI: 10.1021/acs.analchem.9b02013

The morphological effect of impurities on α-U3O8 has been investigated. This study provides the first evidence that the presence of impurities can alter nuclear material morphology, and these changes can be quantified to aid in revealing processing history. Four elements: Ca, Mg, V, and Zr were implemented in the uranyl peroxide synthesis route and studied individually within the α-U3O8. Six total replicates were synthesized, and replicates 1–3 were filtered and washed with Millipore water (18.2 MΩ) to remove any residual nitrates. Replicates 4–6 were filtered but not washed to determine the amount of impurities removed during washing. Inductively coupled plasma mass spectrometry (ICP-MS) was employed at key points during the synthesis to quantify incorporation of the impurity. Each sample was characterized using powder X-ray diffraction (p-XRD), high-resolution scanning electron microscopy (HRSEM), and SEM with energy dispersive X-ray spectroscopy (SEM-EDS). p-XRD was utilized to evaluate any crystallographic changes due to the impurities; HRSEM imagery was analyzed with Morphological Analysis for MAterials (MAMA) software and machine learning classification for quantification of the morphology; and SEM-EDS was utilized to locate the impurity within the α-U3O8. All samples were found to be quantifiably distinguishable, further demonstrating the utility of quantitative morphology as a signature for the processing history of nuclear material.