Aluminum sec-butoxide/polyvinylpyrrolidone (ASB/PVP) solutions, prepared by sol gel processing of a mixture of ASB and PVP, were electrospun to form ASB/PVP organic inorganic hybrid fibers. The diameter of alumina nanofibers was in the range of 200 nm to 500 nnn. Since the fibers cracked after calcinations at 1100 degrees C, they were cured at 300 degrees C, 400 degrees C and 500 degrees C for 24 h each. The calcination of these composite fibers at temperatures above 1000 degrees C resulted in pure rod-shaped a-alumina. It was analyzed by SEM, TG-DTA, FTIR, and XRD.