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Single-step, High Pressure, and Two-Step Spark Plasma Sintering of UO2 nanopowders

de Bona, E.; Balice, L.; Cognini, L.; Holzhaeuser, M.; Popa, K.; Walter, O.; Cologna, M.; Prieur, D.; Wiss, T.; Baldinozzi, G.

Three different Spark Plasma Sintering (SPS) treatments were applied to highly sinteractive, near-stoichiometric UO2.04 nanocrystalline (5 nm) powders produced by U(IV) oxalate hydrothermal decomposition at 170 °C. The sintering conditions for reaching 95 % Theoretical Density (TD) in regular SPS, high pressure SPS (HP-SPS), and, for the first time, two-step SPS (2S-SPS), were found. Densification to 95 % TD was achieved at 1000 °C in regular SPS (70 MPa applied pressure), 660 °C in HP-SPS (500 MPa), and 650-550 °C in 2S-SPS (70 MPa). With the goal of minimising the grain growth during densification, the sintering treatments were optimised to favour densification over coarsening, and the final microstructures thus obtained are compared. Otherwise identical, stochiometric UO2 samples of different grain sizes, ranging from 3.08 μm to 163 nm, were produced. Room-temperature oxidation of the powders could not be avoided due to their nanometric dimensions, and a final annealing treatment was designed to reduce hyper stoichiometric samples to UO2.00.

Keywords: Spark Plasma Sintering; Uranium Dioxide; Microstructure; Coarsening; Two Step Sintering

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Publ.-Id: 31285