In the current paper, the production of homogeneous mixed nanocrystals based on Fe and Cu was successfully accomplished despite these two transition metals exhibiting extremely low miscibility in their phase diagram. The synthesis was carried out by the laser-mediated reduction of metal salts that were dissolved in different kinds of solvents, water, acetone and ethylene glycol. The greatest value of the methodology is that it allows the generation of mixed nanocrystals formed by transition metals with low miscibility in the presence of different solvents, taking metal salts as precursor agents, which are conventionally used in traditional wet synthesis techniques, but in contrast with the most popular approaches, the process requires neither special conditions nor hazardous reducing agents. Therefore, the presented methodology represents a clean and promising alternative for the synthesis of mixed nanocrystals composed of materials with low miscibility.