Compared with traditional metal materials, carbon-based materials have the advantages of low density, high conductivity, good chemical stability, etc., and can be used as reliable alternative materials in various fields. Among them, the carbon fiber conductive network constructed by electrospinning technology has the advantages of high porosity, high specific surface area and rich heterogeneous interface. In order to further improve the conductivity and mechanical properties of pure carbon fiber films, tantalum carbide (TaC) nanoparticles were selected as conductive fillers. The crystallization degree, electrical and mechanical properties of electrospun TaC/C nanofibers at different temperatures were investigated. As the carbonization temperature increases, the crystallization degree and electrical conductivity of the sample also increases, while the growth trend of electrical conductivity is markedly slowed. The best mechanical properties of 12.39 MPa was achieved when the carbonization temperature was 1200 °C. Finally, through comprehensive analysis and comparison, it can be concluded that a carbonization temperature of 1200 °C is the optimum.