Microwave-assisted chemical precipitation was used to prepare CuxCd1–xS (x = 0.8, 0.6, 0.4, and 0.2) nanoparticles mixture. The crystal structure, size, and surface morphology of the as-synthesized nanoparticles were studied using X-ray diffraction and SEM. Presence of copper, cadmium, and sulphur in proper ratios in the samples was confirmed by energy-dispersed X-ray analysis. DC electrical resistance measurements of all the samples in the temperature range of 300…500 K showed phase transition above a certain temperature.