A comparative study of the electrical conductivity of intermetallic and corresponding nanocomposites at room and the subzero temperature was carried out by experimental and theoretical techniques. Four series of intermetallic compounds (IMCs) and nanocomposites (NCs) of Al2O3, ZnO, TiO2, and CuO were synthesized by high-temperature reactive synthesis and sol-gel technique, respectively. Heat treatment of NCs was carried out at 100, 200, 300, and 400°C. Characterization of NCs was carried out by UV-visible, FTIR, FE-SEM, and XRD techniques. Computational study (DMol3, CASTEP, Forcite, Reflex, and VAMP) was carried out to study the electronic and optical properties of metal nanoparticles. The influence of heat treatment, the addition of coinage metal and ferromagnetic material, effect of a decrease in temperature on the electrical conductivity of IMCs and NCs were thoroughly investigated. The electrical conductivity of NCs was found to increase with an increase in heat treatment temperature (up to 400°C) and with the decrease in temperature (-70°C). The addition of Hematite, α-Fe2O3, and coinage metal do not significantly increase the electrical conductivity of NCs at room temperature. The electrical conductivity of NCs was found to be higher than IMCs and coinage metals. Hence, synthesized NCs can have a large number of potential applications in nanowires, quantum dots, and nano cables with very low resistivity (10-6 ΩWm-1).