This seminar delves into the synthesis of heterostructured nanoparticles via pulsed laser irradiation of colloidal transition metals and their oxides. This non-equilibrium process induces physical perturbations within the colloidal environment, driving phase transformations, oxidation state variations, and surface modifications that boost catalytic activity. By tuning laser parameters, it is possible to control microstructural evolution, enabling the design of nanoparticles with tailored electronic and chemical properties. Experimental findings will be presented, with a particular focus on synchrotron-based X-ray absorption spectroscopy and electron microscopy techniques for characterizing oxidation states and local atomic structures. Complementary theoretical insights from ab initio calculations and atomistic simulations will provide a mechanistic understanding of phase formation and surface dynamics. Finally, the functional relevance of these heterostructures will be demonstrated in ethanol oxidation reactions, highlighting their potential in electrocatalytic fuel cells and sustainable energy applications.