Metallic nanoparticles (NPs), either supported on a porous oxide framework or finely dispersed within an oxide matrix, find applications in catalysis, plasmonics, nanomagnetism and energy conversion, among others. The development of synthetic routes that enable to control the morphology, chemical composition, crystal structure and mutual interaction of metallic and oxide phases is necessary in order to tailor the properties of this class of nanomaterials. With this work, we aim at developing a novel method for the synthesis of metal/oxide nanocomposites based on the assembly of NPs formed by gas phase condensation of metal vapors in a He/O 2 atmosphere. This new approach relies on the independent evaporation of two metallic precursors with strongly different oxidation enthalpies. Our goal is to show that the precursor with less negative enthalpy gives birth to metallic NPs, while the other to oxide NPs. The selected case study for this work is the synthesis of a Fe-Co/TiO x nanocomposite, a system of great interest for its catalytic and magnetic properties. By exploiting the new concept, we achieve the desired target, ie, a nanoscale dispersion of metallic alloy NPs within titanium oxide NPs, the structure of which can be tailored into TiO 1-δ or TiO 2 by controlling the synthesis and processing atmosphere. The proposed synthesis technique is versatile and scalable for the production of many NPs-assembled metal/oxide nanocomposites. View Full-Text