Natural and isotopically enriched KCl targets were prepared using specially formulated KCl solutions, deposited by electrospraying on thin (1.5μm) gold backings, followed by a short annealing in a preheated (350–450 °C) furnace. Various techniques, such as X-ray fluorescence (XRF), scanning electron microscopy (SEM) imaging, and energy-dispersive X-ray spectroscopy (EDS), were used to characterize the produced targets. A white neutron beam at the Los Alamos Neutron Science Center (LANSCE) facility was also used to verify the estimated atomic percentages of the enriched 40KCl targets. KCl was deposited relatively uniformly as large particles rather than films on the gold surface. This method can be broadly extended to make stable targets that are difficult to produce with other methods and more exotic radioactive targets required for research in fundamental sciences and applications.