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This book examines the influence of polymeric binders on sol-gel electrospinning of nanofiber. The precursor nanofibers were calcined at high temperature to derive nanostructured oxide ceramic fibers. The morphological, compositional, spectral, structural and magnetic properties of the obtained ceramic nano-fibers were characterized using scanning electron microscopy, transmission electron microscopy, x-ray diffraction, Raman spectroscopy, Fourier transform infrared spectroscopy, UV-Vis-near IR spectroscopy, x-ray photoelectron spectroscopy, vibrating sample magnetometry and Brunauer-Emmett-Teller surface area analysis. The applicability of nickel oxide nanofibers was explored in sensing vapors of different alcohols and catalytic reduction of harmful species from diesel engine exhaust. The cobalt oxide nano-fibers developed were used for water splitting and electrochemical sensing of glucose and hydrogen peroxide. The properties of nano-materials are pertinent to their synthesis route as the surface atoms are sensitive to the contiguous medium of synthesis; it is true also in the case of sol-gel electrospinning.