▎ 摘　　要

Ultrasmall Cu/Ni-NiOx nanoparticles (NPs) had been successfully prepared by attaching and growing Ni-NiOx NPs on the surface of Cu NPs and then uniformly dispersed onto graphene (G) surface. High-angle annular dark-field-scanning transmission electron microscopy (HAADF-STEM) characterization confirmed that Ni-NiOx NPs were uniformly distributed on the surface of Cu NPs. The catalytic methanolysis of ammonia borane (AB) proved that Cu/Ni-NiOx NPs possessed high catalytic hydrogen (H-2) evolution activity, and the highest turnover frequency (TOF) was 17.72 mol H-2 center dot mol(-1) Cu center dot min(-1). Comparative experiments revealed that the high catalytic activity originated from the abundant catalytic active sites of Cu/Ni-NiOx NPs. The attachment of Ni-NiOx on the surface of Cu NPs that dispersed on G (G-Cu/Ni-NiOx) can not only effectively improve the antioxidative performance of Cu NPs under ambient conditions but also promote the methanolysis of AB to produce H-2.