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In this work, vanadium pentoxide (V2O5) and titanium-modified V2O5 thin films were synthesized using the sol-gel spin coating route. The effect of Ti-doping concentration on the electrochromic optical properties and atomic/electronic structures of V2O5 smart thin films is examined. As the doping concentration of Ti increases, the surface roughness of the films is reduced. The structure of the films is analyzed using X-ray diffraction (XRD) and Raman spectroscopy, while the electrochromic modulation of atomic and electronic structures is elucidated through Raman and X-ray absorption spectroscopy (XAS) conducted during lithiation and delithiation. The XRD patterns demonstrate that an increase in Ti concentration leads to a more amorphous structure of the films and a shift of the main diffraction peak to a lower angle, attributable to the enlarged spacing between the stacking layers resulting from the incorporation of Ti ions. Soft X-ray absorption spectroscopy (XAS) and in situ hard XAS of the V L-edge, the O K-edge, and the V K-edge revealed a reduction in the charge state of V and local atomic structural symmetry modification upon lithated coloration and delithiated bleaching process. The critical insights provided by in situ XAS provides reveal that a small amount of Ti has the ability to modify the interlayer distance and local atomic structure of V2O5, thereby improving its electrochromic switching rate and stability when utilized in smart windows.

The scarcity of fuels, high pollution levels, climate change, and other major environmental issues are critical challenges that modern societies are facing, mostly originating from fossil fuels-based economies. These challenges can be addressed by developing green, eco-friendly, inexpensive energy sources and energy storage devices. Electrochemical energy storage materials possess high capacitance and superior power density. To engineer highly efficient next-generation electrochemical energy storage devices, the mechanisms of electrochemical reactions and redox behavior must be probed in operational environments. They can be studied by investigating atomic and electronic structures using in situ x-ray absorption spectroscopy (XAS) analysis. Such a technique has attracted substantial research and development interest in the field of energy science for over a decade. The mechanisms of charge/discharge, carrier transport, and ion intercalation/deintercalation can be elucidated. Supercapacitors generally store energy by two specific mechanisms—pseudocapacitance and electrochemical double-layer capacitance. In situ XAS is a powerful tool for probing and understanding these mechanisms. In this Review, both soft and hard x rays are used for the in situ XAS analysis of various representative electrochemical energy storage systems. This Review also showcases some of the highly efficient energy and power density candidates. Furthermore, the importance of synchrotron-based x-ray spectroscopy characterization techniques is enlightened. The impact of the electronic structure, local atomic structure, and electronically active elements/sites of the typical electrochemical energy storage candidates in operational conditions is elucidated. Regarding electrochemical energy storage mechanisms in their respective working environments, the unknown valence states and reversible/irreversible nature of elements, local hybridization, delocalized d-electrons spin states, participation of coordination shells, disorder, and faradaic/non-faradaic behavior are thoroughly discussed. Finally, the future direction of in situ XAS analysis combined with spatial chemical mapping from operando scanning transmission x-ray microscopy and other emerging characterization techniques is presented and discussed. [ABSTRACT FROM AUTHOR]