In this paper, Al0.6CoCrFeNi/5052 aluminum matrix composites were prepared at different sintering temperatures (550–700 °C) by vacuum hot-pressing sintering. The effects of sintering temperature on composites were studied by testing the morphology, phase composition and mechanical properties of the composites, which were characterized by uniaxial compression experiments, X-ray diffraction, scanning electron microscope, electron probe and nanoindentation. The results show that the prepared composites have high strength and very good ductility with sintering temperature lower than 700 °C. When the sintering temperature is above 550 °C, the interface layer is formed in the composite material. As the sintering temperature increases, the formation method of the interface layer changes. The generation of the interface layer has a significant effect on the mechanical properties of the composites.