Titanium carbide exhibits exceptional electrical conductivity (1.5 × 104 S/cm) and thermal stability, along with impressive mechanical properties, including hardness (28–35 GPa). This makes it a promising candidate for structural materials in next-generation fuel cell electrodes. Utilizing TiC as a support to reduce platinum loading presents a significant opportunity for cost savings in fuel cell technology. Nanosized titanium carbide powders were produced through a sol-gel process. This process facilitates the production of extremely uniform materials with precise control over composition and structure at the molecular scale, leading to more reliable properties. Also, the sol-gel process may be more economically viable than conventional high-temperature synthesis techniques, especially for large-scale production. The precursor gels (Ti-O-C) were synthesized using titanium tetra isopropoxide, sucrose (C12H22O11), and acetic acid (CH3COOH). The produced xerogels were then subjected to calcination in a consistent argon environment at temperatures range from 800 °C to 1350 °C, maintaining this condition for 1 h. A range of analytical methods, such as TGA-DSC, XRD, SEM, and cyclic voltammetry, were utilized to characterize this during the entire process. The cyclic voltammetry result refers to the material’s ability to maintain its electrochemical performance over multiple charge-discharge cycles without significant degradation. The TiC nanoparticles produced were approximately 45 nm in size. The formation of TiC structure was confirmed by XRD, alongside trace amounts of TiO2 and free carbon, with fluctuations in oxygen and carbon content influenced by the synthesis parameters.