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The structural characterisation of actinide nanoparticles (NPs) is of primary importance and hard to achieve, especially for non‐homogeneous samples with NPs less than 3 nm. By combining high‐energy X‐ray scattering (HEXS) and high‐energy‐resolution fluorescence‐detected X‐ray absorption near‐edge structure (HERFD XANES) analysis, we have characterised for the first time both the short‐ and medium‐range order of ThO 2  NPs obtained by chemical precipitation. By using this methodology, a novel insight into the structures of NPs at different stages of their formation has been achieved. The pair distribution function revealed a high concentration of ThO 2  small units similar to thorium hexamer clusters mixed with 1 nm ThO 2  NPs in the initial steps of formation. Drying the precipitates at around 150 °C promoted the recrystallisation of the smallest units into more thermodynamically stable ThO 2  NPs. HERFD XANES analysis at the thorium M 4  edge, a direct probe for f states, showed variations that we have correlated with the breakdown of the local symmetry around the thorium atoms, which most likely concerns surface atoms. Together, HEXS and HERFD XANES are a powerful methodology for investigating actinide NPs and their formation mechanism.

The Application of HEXS and HERFD XANES for Accurate Structural Characterisation of Actinide Nanomaterials: The Case of ThO 2