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Nanostructured H 2 V 3 O 8  is a promising high‐capacity cathode material, suitable not only for Li +  but also for Na+, Mg 2+ , and Zn 2+  insertion. However, the full theoretical capacity for Li +  insertion has not been demonstrated experimentally so far. In addition, improvement of cycling stability is desirable. Modifications like substitution or prelithiation are possibilities to enhance the electrochemical performance of electrode materials. Here, for the first time, the substitution of vanadium sites in H 2 V 3 O 8  with molybdenum was achieved while preserving the nanostructure by combining a soft chemical synthesis approach with a hydrothermal process. The obtained Mo‐substituted vanadate nanofibers were further modified by prelithiation. While pristine H 2 V 3 O 8  showed an initial capacity of 223 mAh g −1  and a retention of 79 % over 30 cycles, combining Mo substitution and prelithiation led to a superior initial capacity of 312 mAh g −1  and a capacity retention of 94 % after 30 cycles.

Modified H 2 V 3 O 8 to Enhance the Electrochemical Performance for Li‐ion Insertion: The Influence of Prelithiation and Mo‐Substitution