Copper/nickel nanoparticle-decorated N-doped graphene (Cu/ Ni/N-graphene) hybrids were prepared by using a solvothermal method, and further employed as a sensing material for fabricating a sensitive non-enzymatic glucose and ethanol sensor. Compared with Cu, Cu/N-graphene, Ni, Ni/N-graphene, Cu 50 /Ni 50 nanoparticles, and Cu 51 /Ni 49 /graphene, the Cu 52 /Ni 48 /Ngraphene showed enhanced electrochemical activity to glucose and ethanol oxidation, owing to the synergetic effects of Cu and Ni together with N-graphene sheets in the hybrids. The results showed that the Cu 52 /Ni 48 /N-graphene hybrid-modified electrode exhibited excellent performance for glucose detection with a wider linear range (from 0.5 mM to 4.6 mM), lower limit of detection (0.2 mM, S/N = 3), and higher sensitivity (1847.56 mA mM À1 cm À2 ) than other modified electrodes. Furthermore, the presented non-enzymatic sensor also displayed a good response toward ethanol oxidation with a wide linear range from 0.2 to 37.1 mM, lower detection limit of 0.1 mM (S/ N = 3), and faster response time (5 s). These results indicated that the excellent properties could promote the potential application of the bimetals and N-graphene sheets as enhanced materials in constructing non-enzymatic sensors for electrochemical analysis.