La0.9K0.1CoO3 perovskite type oxide fibers have been prepared by a sol-gel process combined with electrospinning procedure. The reactions during the calcination process of fibers have been tracked and characterized by TG, IR, and XRD. The prepared La0.9K0.1CoO3 fibers are composed of nanoparticles and the BET surface area is 7.1 m(2)/g. The scanning electron microscopy (SEM) results indicate that each individual fiber is uniform in cross section, and the average diameter of this sample is 600 nm. The catalytic activity for the combustion of soot particulate is evaluated by the technique of the temperature-programmed reaction, and the combustion temperature of carbon is indeed significantly lower than that of noncatalytic combustion under loose contact conditions.