Rechargeable Lithium Sulfur batteries have attracted widespread attention due to their high theoretical energy density, which is of great importance due to growing energy demands. These batteries have not been commercialized due to the challenges caused by their complex electrochemical reactions such as the shuttle effect and solubility of higher order Polysulfides in the electrolytes. In this thesis, we discuss attempts to combat these technical issues by combining physical and chemical modifications of mesoporous carbon nanofibers as electrodes or interlayers, by incorporation of cyclic Nitrogen groups, using Gas-Assisted electrospinning and electrospraying techniques. We also compare the synergistic effects off all these features on battery performance and use various characterization tools to understand them.