The ISOL method is an efficient way to produce radioisotope ion beams of good quality. In this technique, a high-energy beam (e.g., protons) hits a target to produce the radioisotopes of interest through different nuclear reactions. However, the radioisotopes must be quickly released from the target, which can be done by optimisation of the target microstructure and increasing temperature. Uranium carbide is among the best target materials due to its high temperature stability and good thermal conductivity. Aiming at increasing the release rates, nanostructured materials are being tested. In this context, YCx nanofibers were prepared by electrospinning and studied the effects of the solution characteristics and electrospinning process parameters on the as-spun materials. It was concluded that the slowly heating (1oC/ min) of fibers up to 600oC is of fundamental importance to keep the fiber morphology upon polymer decomposition.