| Summary: | We report here the first synthesis of mixed oxide U1-xPuxO2(+y) nanoparticles. The obtained nanopowders were characterized by X-ray diffraction, thermal ionization mass spectrometry, transmission electron microscopy, Raman spectroscopy, and U M4 edge high-energy-resolution X-ray absorption near edge structure (HR-XANES). The HR-XANES spectra give evidence for the partial oxidation of UIV to UV. This novel route toward the formation of actinide–actinide solid solution opens research opportunities that are not accessible using bulk materials. We give details on the X-ray diffraction study on plutonium oxalate hexahydrate, as a reagent for the synthesis of such nanoparticles.
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