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palladium nanoparticles (Pd NPs) are highly versatile catalysts for catalytic reactions in organic chemistry. They are used in a variety of applications including Suzuki and Heck coupling reactions, carbon-carbon bond formation and hydrogen storage.

To maximise their use, well-defined palladium NPs are required with a high degree of monodispersity. This aim is being achieved by a number of different methods ranging from physical to chemical.

The synthesis of monodisperse palladium NPs is a key area in the field of catalysis. A range of stabilising ligands, surfactants and sterically bulky host materials have been used to achieve this. However, the synthesis of stable and monodisperse Pd NPs remains a challenge.

Pd NPs have a very small size and a unique face-to-face octahedral geometry. This makes them more sensitive to adsorption of hydrogen gas. In the present work, the behaviour of octahedral Pd NPs under varying H concentrations and temperatures was studied using temperature-dependent cyclic voltammetry. This was accompanied by small angle X-ray scattering and single particle ICP-MS.

The octahedral Pd(acac)2 nanocrystals were prepared by reduction of the metal chloride with polyvinylpyrrolidone (PVP, g/mol, Alfa Aesar) in tetra ethylene glycol (TEG, g/mol, Merck). The particle sizes were analysed by scanning electron microscopy (SEM), small angle X-ray scattering and by single-particle ICP-MS. These measurements showed that the octahedral shape was retained, but that the crystalline structure had become more compact. This change was also confirmed by a 3D reconstruction based on the Pd X-ray crystallographic data, where a large portion of the octahedron was located within the scattering region of the isosurface (Figs 2a, b). The crystalline surface exhibited a high degree of homogeneity, but also contained areas with a more pronounced 111 reflection.

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