Abstract. Titanium nitride-carbon nanocomposites have been synthesized by the reaction of TiCl 4 and NaN 3 in supercritical benzene medium that also serves as a carbon source. The as-prepared precursor has been subjected to di erent heat treatments under ammonia and nitrogen atmospheres. The structure and chemical composition of the synthesized TiN-C nanocomposites are studied by X-Ray Di raction (XRD) and CHN elemental analysis. Meanwhile, the nature of carbonaceous species and the respective carbon phase transitions during supercritical process and following heat treatments are further investigated by Raman spectroscopy, Time of Flight Secondary Ion Mass Spectrometry (ToF-SIMS), and their charge-discharge characteristics with respect to lithium storage. After 10 h of NH3 treatment at 1000 C, carbonaceous phase transforms to graphene layered structure. The highly e cient mixed TiN conducting network and the internal defects between G layers induced by nitrogen doping improve rate capability and cycling performance of G sheets and provide a speci c capacity of 381 mAh g 1 at Charge/Discharge (C/D) rate of 0.2 C. The enhanced electrochemical performance of the SIV nanocomposite is mainly due to improving the electronic/ionic conductivity, reducing charge transfer coe cient, and increasing electrochemical surface area that are resulted from anchoring of TiN nanoparticles to graphene sheets.