The controllable synthesis and structural tailoring of nanostructured metal-organic frameworks (MOFs) is of huge significance in boosting their potential for rechargeable batteries. We herein present the facile synthesis of cobalt-based ultrathin metal-organic framework nanosheets (referred to as "u-CoTDA") by using 2,5-thiophenedicarboxylic (H TDA) as the organic building block through a one-pot ultrasonic method for the first time. The obtained u-CoTDA exhibits high reversible capacity (790 mAh g after 400 cycles at 1 A g ) and excellent rate capability (694 mAh g at 2 A g ), which outperforms its bulk counterpart. Moreover, the detailed lithiation/delithiation processes of u-CoTDA were studied by the combination of Co K-edge X-ray absorption near edge structure (XANES), O K-edge soft X-ray spectroscopy (sXAS) and electron paramagnetic resonance (EPR) techniques, which demonstrate that both the Co centers and organic ligands of u-CoTDA are involved in the reduction/oxidation processes.
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