▎ 摘　　要

Nanostructure of CuO plays a critical role in Li-ion battery (LIB) applications of CuO/graphene oxide (GO) nanocomposites. Morphological evolution of CuO/GO anode material provides essential information for developing the performance of LIBs. But, the nanostructural evolution of the CuO/GO anode materials have not been previously studied by in situ electrochemical-synchrotron radiation techniques. In this paper, different CuO morphology in preparation of CuO/GO nanocomposites could be controlled by increasing the reactive time at 83 degrees C. In situ synchrotron X-ray diffraction and small angle X-ray scattering (SAXS) are employed to characterize the structural behavior of CuO/GO samples during the first cycle. The CuO(-511) Bragg peak demonstrates a more significant shift toward higher angles due to the incorporation of Li+ in the CuO crystal lattice. SAXS indicates that the formation and growth of SEI are observed with lithiation dose, and subsequently some cracks occur. The in situ electrochemical-synchrotron techniques could be implemented to help further understand the electrochemical behaviors and conversion mechanism of anode materials.