Nanotomography for Quantitative 3D Particle Reconstruction

Particulates are ubiquitous across fuel cycle operations and carry critical information about particle formation, processing, and potential proliferation-related activities. Traditional analytical techniques, including micro-Raman spectroscopy and standard electron microscopy, are often limited in spatial resolution or dimensionality, particularly when used to examine metallic or submicron-scale features. Understanding particle morphology, phase distribution, and internal porosity is essential for constraining formation conditions, thermodynamic environments, and material transport behavior. In this report, we demonstrate the application of plasma focused ion beam nanotomography to reconstruct micron-scale particulates at nanoscale resolution. Using high-resolution backscattered electron imaging and Avizo software, we obtained 3D reconstructions that enabled quantitative analysis of particle morphology, phase composition, and internal voids. Representative examples include a Ta particle with a large central void and a composite particle with embedded tetrahedral crystalline structures. These reconstructions reveal structural and compositional details that are inaccessible through conventional 2D imaging. The results demonstrate that nanotomography provides both qualitative and quantitative insights into particle formation and behavior. Using nanotomography, porosity and phase distributions can be quantified to inform models of particle density, transport, and solidification conditions. Beyond technical insights, the workflow developed here establishes a transferable capability for analyzing heterogeneous particles and has potential applications in bulk materials studies via x-ray computed tomography or other volumetric imaging modalities. Ongoing efforts are focused on optimizing the workflow to process multiple particles simultaneously, increasing throughput and statistical robustness. Overall, this work illustrates the power of nanotomography as a tool for connect. Authors: Moseley, Duncan H. [Oak Ridge National Laboratory (ORNL), Oak Ridge, TN (United States)] (ORCID:0000000343518347); Parish, Chad [Oak Ridge National Laboratory (ORNL), Oak Ridge, TN (United States)] (ORCID:0000000312097439); Beiswenger, Toya [Oak Ridge National Laboratory (ORNL), Oak Ridge, TN (United States)] (ORCID:0009000870421667); Petrova, Rumy [Oak Ridge National Laboratory (ORNL), Oak Ridge, TN (United States)]; Arregui Mena, Jose' (David) [Oak Ridge National Laboratory (ORNL), Oak Ridge, TN (United States)] (ORCID:0000000261313268). DOE Contract: AC05-00OR22725. Subjects: 11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS; 73 NUCLEAR PHYSICS AND RADIATION PHYSICS