Electrospinning of preceramic polymers offers the ability to produce oxide and non-oxide ceramic fibers with diameters several orders of magnitude smaller than those available by commercial methods enabling composite materials with new and unique properties. In this project fibers were produced at scales smaller than currently available by commercial processes. Ceramic precursor polymers were combined with polystyrene to prepare electrospun fibers that are subsequently pyrolized into SiC nanofibers. Sol-gel precursors were pyrolyzed into transition metal carbides and nitrides by applying the carbothermal reduction CTR process using pitch as a carbon source. Electron and X-ray diffractions, electron microscopy, and electron energy loss spectroscopy show crystalline fibers were produced with average diameters as small as 50nm. A variety of carbide and nitride nanofibers were produced based on silicon, titanium, zirconium, hafnium, vanadium, niobium, and tantalum. The CTR process was expanded to examine a wide range of metal-oxide powders to aid in predicting success or failure of more expensive sol-gel materials and pitch was found to be a better carbon source for CTR than graphite or amorphous carbon.