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Chemically preintercalated dopamine (DOPA) molecules were used as both reducing agent and carbon precursor to prepare δ-V2O5∙nH2O/C, H2V3O8/C, VO2(B)/C and V2O3/C nanocomposites via hydrothermal treatment or hydrothermal treatment followed by annealing under Ar flow. We found that the phase composition and morphology of the produced composites are influenced by the DOPA:V2O5 ratio used to synthesize (DOPA)xV2O5 precursors through DOPA diffusion into the interlayer region of δ-V2O5∙nH2O framework. The increase of DOPA concentration in the reaction mixture led to more pronounced reduction of vanadium and a higher fraction of carbon in the composites’ structure, as evidenced by XPS and Raman spectroscopy measurements. The electrochemical charge storage properties of the synthesized nanocomposites were evaluated in Li-ion cells with non-aqueous electrolyte. δ-V2O5∙nH2O/C, H2V3O8/C, VO2(B)/C, and V2O3/C electrodes delivered high initial capacities of 214, 252, 279, and 637 mAh·g–1, respectively. The insights provided by this investigation open up the possibility of creating new nanocomposite oxide/carbon electrodes for a variety of applications such as energy storage, sensing and electrochromic devices. 

A capacitance increase phenomenon is observed for MoO 3 electrodes synthesized via a sol-gel process in the presence of dopamine hydrochloride (Dopa HCl) as compared to α-MoO 3 electrodes in 5M ZnCl 2 aqueous electrolyte. The synthesis approach is based on a hydrogen peroxide-initiated sol-gel reaction to which the Dopa HCl is added. The powder precursor (Dopa) x MoO y , is isolated from the metastable gel using freeze-drying. Hydrothermal treatment (HT) of the precursor results in the formation of MoO 3 accompanied by carbonization of the organic molecules; designated as HT-MoO 3 /C. HT of the precipitate formed in the absence of dopamine in the reaction produced α-MoO 3 , which was used as a reference material in this study (α-MoO 3 -ref). Scanning electron microscopy (SEM) images show a nanobelt morphology for both HT-MoO 3 /C and α-MoO 3 -ref powders, but with distinct differences in the shape of the nanobelts. The presence of carbonaceous content in the structure of HT-MoO 3 /C is confirmed by FTIR and Raman spectroscopy measurements. X-ray diffraction (XRD) and Rietveld refinement analysis demonstrate the presence of α-MoO 3 and h-MoO 3 phases in the structure of HT-MoO 3 /C. The increased specific capacitance delivered by the HT-MoO 3 /C electrode as compared to the α-MoO 3 -ref electrode in 5M ZnCl 2 electrolyte in a −0.25–0.70 V vs. Ag/AgCl potential window triggered a more detailed study in an expanded potential window. In the 5M ZnCl 2 electrolyte at a scan rate of 2 mV s −1 , the HT-MoO 3 /C electrode shows a second cycle capacitance of 347.6 F g −1 . The higher electrochemical performance of the HT-MoO 3 /C electrode can be attributed to the presence of carbon in its structure, which can facilitate electron transport. Our study provides a new route for further development of metal oxides for energy storage applications. 

MXenes offer high metallic conductivity and redox capacitance that are attractive for high‐power, high‐energy storage devices. However, they operate limitedly under high anodic potentials due to irreversible oxidation. Pairing them with oxides to design asymmetric supercapacitors may expand the voltage window and increase the energy storage capabilities. Hydrated lithium preintercalated bilayered V₂O₅(δ‐Li_xV₂O₅·nH₂O) is attractive for aqueous energy storage due to its high Li capacity at high potentials; however, its poor cyclability remains a challenge. To overcome its limitations and achieve a wide voltage window and excellent cyclability, it is combined with V₂C and Nb₄C₃MXenes. Asymmetric supercapacitors employing lithium intercalated V₂C (Li‐V₂C) or tetramethylammonium intercalated Nb₄C₃(TMA‐Nb₄C₃) MXenes as the negative electrode, and aδ‐Li_xV₂O₅·nH₂O composite with carbon nanotubes as the positive electrode in 5 mLiCl electrolyte operate over wide voltage windows of 2 and 1.6 V, respectively. The latter shows remarkably high cyclability—capacitance retention of ≈95% after 10 000 cycles. This work highlights the importance of selecting appropriate MXenes to achieve a wide voltage window and a long cycle life in combination with oxide anodes to demonstrate the potential of MXenes beyond Ti₃C₂in energy storage.