▎ 摘 要
The ultrathin peroxoantimonate coating of graphene oxide from hydrogen peroxide-rich solutions of hydroxoantimonate is demonstrated. An amorphous 1-2 nm Sb (V) oxide film is formed and can be further crystallized by exposure to an electron beam to give a 2-5 nm thick supported Sb6O33 particulate coating. Heat treatment of the peroxoantimonate yielded different crystalline oxides, whereas in the presence of the graphene support only trigonal Sb (0) was produced by heat treatment in vacuum or an argon atmosphere. The graphene oxide support is essential for the formation of the Sb (0) phase and even in air a substantial elemental antimony was obtained. Whereas heat treatment of uncoated graphene oxide in an inert atmosphere produces reduced graphene oxide, the antimony oxide coated graphene oxide is not reduced by the heat treatment. Only after the supported antimony oxide is reduced to give the trigonal Sb (0) phase the graphene oxide was reduced by the heat treatment. The phases before and after the different heat treatments are characterized by electron and X-ray diffraction, thermal analysis, XPS studies, electron microscopy and wet chemistry. (C) 2012 Elsevier Ltd. All rights reserved.