Insights into Reaction Intermediates to Predict Synthetic Pathways for Shape-Controlled Metal Nanocrystals
Valeria Mantella a, Michal Strach a, James Pankhurst a, Raffaella Buonsanti a
a Ecole Polytechnique Federale de Lausanne (EPFL), Switzerland, Lausanne, Switzerland
Poster, Valeria Mantella, 023
Publication date: 6th May 2020

Understanding nucleation phenomena is of crucial importance to rationally predict synthetic pathways for shape-controlled nanocrystals (NCs), yet the lack of in situ set-up which can reproduce the same laboratory synthetic conditions limits such knowledge. In the present work, we report an integrated approach to study the nucleation mechanisms of Cu NCs with different shapes, such as spheres and cubes, by means of different techniques including X-ray absorption spectroscopy (XAS) at a synchrotron source. The measurements were carried out using a customized in-situ cell which mimics the typical synthesis environment. The observed compositional and structural changes allowed us to firstly identify the reaction intermediates forming during the synthesis at high temperatures. As next step, from the collected kinetic data, we could correlate the chemical nature of these intermediates to their conversion kinetics into Cu nuclei and eventually to the formation of Cu spheres and cubes. Thanks to these findings, we further explained the formation of Cu octahedra occurring at a higher temperature and we learned how to modulate the reaction conditions in a predictive manner to obtain Cu tetrahedra, which have not been previously synthesized

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