We report here the first synthesis of mixed oxide U$_{1-x}$Pu$_{x}$O$_{2(+y)}$ nanoparticles. The obtained nanopowders were characterized by X-ray diffraction, thermal ionization mass spectrometry, transmission electron microscopy, Raman spectroscopy, and U M$_{4}$ edge high-energy-resolution X-ray absorption near edge structure (HR-XANES). The HR-XANES spectra give evidence for the partial oxidation of U$^{IV}$ to U$^{V}$. This novel route toward the formation of actinide–actinide solid

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... n 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.