Er2O3 doped calcia stabilized zirconia based inert matrix fuel containing CeO2 as a surrogate for PuO2 was fabricated for a wide range of concentration using the polymer-to-ceramic conversion technique via metal acetate preceramic hybrid polymer solutions. Samples were characterized by XRD, SEM and AFM techniques. Nanocrystallite size variation in the samples was evaluated using peak broadening values by means of the Scherrer formula. The smallest lattice constant was obtained for the sample containing Zr/Ca/Ce/Er atomic weight ratio of 74/11/10/5. The average grain diameters varied between 64 nm and 129 nm. SEM results show that, the smallest grain size was obtained for the sample containing Zr/Ce/Er atomic weight ratio of 22/2/1. Moreover, surface roughness characteristics of the samples were evaluated by different definitions using intermittent contact mode AFM. © 2012 Springer Science+Business Media New York.