Abstract
The one-step seed-mediated synthesis is widely used for the preparation of ferromagnetic metal nanoparticles (NPs) since it offers a good control of particle morphology. Nevertheless, this approach suffers from a lack of mechanistic studies because of the difficulties to follow in real time the heterogeneous nucleation and to predict structure effects with seeds that are generated in situ. Here, we propose a complete scheme of the hetero-nucleation process involved in one-pot seed-mediated syntheses of cobalt nanoparticles in liquid polyols, relying on geometrical phase analysis (GPA) of high-resolution HAADF-STEM images and in situ measurements of the molecular hydrogen evolution. Cobalt particles of different shapes (rods, platelets or hourglass like particles) were grown by reducing cobalt carboxylate in liquid polyols in presence of iridium or ruthenium chloride as nucleating agent. A reaction scheme was established by monitoring the H2 evolution resulting from the decomposition of metal hydrides, formed in situ by β-elimination of metal alkoxides, and from the polyol dehydrogenation, catalytically activated by the metal particles. This is a very good probe for both the noble metal nucleation and the heterogeneous