Cr3C2-NiCr/NiAl coating on the CuCo2Be alloy was prepared by a plasma spraying technique. The high temperature dry sliding friction and wear characteristics of Cr3C2-NiCr/NiAl coating and CuCo2Be were investigated at UMT-2 tribometer using Al2O3 ceramic ball as dual material. The formation mechanism, the microstructure and the high temperature friction and wear behavior of the Cr3C2-NiCr/NiAl coating were studied by Olympus confocal laser scanning microscope, SEM, EDS, and XRD. The results show that the coating is layered and compact. Nickel-aluminum compounds are angular. The phase composition of the coating is amorphous. During the friction and wear process at 500 oC, the wear mechanisms of the coating and CuCo2Be alloy are abrasive wear and adhesive wear as well as a small amount of oxidation wear. Through observing the wear volume morphology, it would find that the wear of substrate materials with the coating is significantly less than CuCo2Be before spraying, so the high-temperature wear resistance of CuCo2Be alloy is improved by plasma spraying.