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In metal nanoparticles (NPs) supracrystals, the metallic core provides somekey properties, e.g. magnetization, plasmonic response or conductivity, withthe ligand molecules giving rise to others like solubility, assembly orinteraction with biomolecules. The formation of these supracrystals depends ona complex interplay between many forces, some stemming from the core, some fromthe ligands. At present, there is no known approach to characterize the localorder of ligand molecules or their dynamics with atomic spatial resolution.Here, we develop a methodology based on small-angle ultrafast electrondiffraction combined with angular cross-correlation analysis to characterize atwo-dimensional supracrystal of dodecanethiol-coated gold NPs. We retrieve thestatic arrangement of the ligands, showing that at equilibrium they order in apreferential orientation on the NPs surface and throughout the two-dimensionalsupracrystal. Upon light excitation, positional disorder is induced in thesupracrystal, while its overall homogeneity is surprisingly found totransiently increase. This suggests that transient annealing of thesupracrystal takes place within few picoseconds (ps). This methodology willenable the systematic investigation of the dynamical structural properties ofnano-assembled materials containing light elements, relevant for biologicalapplications.

Order/disorder dynamics in a dodecanethiol-capped gold nanoparticles supracrystal by small-angle ultrafast electron diffraction