We report on the synthesis of titanium dioxide by titanium carbide for the preparation of hybrid material reinforced with polyaniline (PANI@TiO2–TiC) using the in situ polymerization technique. The effectiveness of the samples on the thermal, optical and electrochemical properties was investigated. The XRD, XPS, FTIR, SEM and TEM results confirm the successful synthesis of the PANI, PANI@TiC and PANI@TiO2–TiC samples. Through this, a good connection, an excellent relationship between the structures and the properties of the synthesized hybrid materials were obtained. Moreover, the electrical conductivity and optical bandgap were also tested. Remarkably good electrochemical characteristics were identified by cyclic voltammetry. Moreover, the galvanostatic charge–discharge (GCD) of the supercapacitor was remarkably high. Cyclic stability showed good retention after 1500 cycles at 1.5 A·g−1.
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