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A conversion reaction mechanism of Cu 3 B 2 O 6 during the electrochemical reduction in a Li-ion battery test cell was revealed. Different experimental techniques were used: X-ray diffraction (XRD), in situ synchrotron diffraction, quasi in situ X-ray photoelectron and Auger-electron spectroscopy (XPS and AES), and ex situ scanning electron microscopy (SEM). The reduction process changes the initial oxidation state of copper from Cu(II) to Cu(0). After the subsequent oxidation, only the Cu(I)doi:10.1149/1.3597612 fatcat:7he5i6acgbfc7fvrdb36ef7d6i