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Journal article
Solid-State Nuclear Magnetic Resonance Insights into the Precursor-Dependent Structure and Na-Ion Storage Behavior of Na-Preintercalated Bilayered Vanadium Oxides
Chemistry of Materials, Forthcoming
23 Apr 2026
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Abstract
Chemically preintercalated bilayered vanadium oxide (BVO) electrodes derived from V2CTx MXene exhibit superior Na-ion storage performance compared to compositionally similar BVO counterparts synthesized from α-V2O5 powder. Here, we report for the first time the precursor-dependent structural differences in Na-preintercalated BVO electrodes (δ-NaxV2O5·nH2O) synthesized from α-V2O5 powder (AD-NVO) and V2CTx MXene nanoflakes (MD-NVO) and show how these differences govern their electrochemical behavior in a nonaqueous Na-ion energy storage system. Our analyses show that AD-NVO and MD-NVO exhibit distinct compositions of δ-Na0.37V2O5·0.46H2O and δ-Na0.33V2O5·0.21H2O, respectively, along with pronounced differences in morphology, electronic structure, and interlayer chemistry. Scanning electron microscopy reveals the formation of 1D nanobelts for AD-NVO, whereas MD-NVO consists of 2D nanoflakes assembled into nanoflower-like agglomerates. X-ray photoelectron spectroscopy indicates that Na preintercalation led to different extents of V5+ to V4+ reduction in AD-NVO and MD-NVO, attributed to differences in the structural water content, which was further supported by the V4+ content quantification via electron paramagnetic resonance. Electrochemical measurements show fundamentally different charge storage behaviors: AD-NVO exhibits largely capacitive responses, while MD-NVO displays pronounced Na+ redox activity and delivers a higher specific capacity, improved rate capability, and superior cycling stability. Magic-angle spinning 23Na solid-state NMR identifies two distinct interlayer Na environments in MD-NVO, in contrast to a single Na site in AD-NVO. These sites play complementary roles, with one facilitating Na+ transport and the other acting as stabilizing pillars, as confirmed by ex situ X-ray diffraction. This study reveals how precursor-dependent structural evolution in chemically preintercalated layered oxides governs interlayer chemistry and electrochemical function, providing design principles for engineering layered metal oxides for advanced energy storage.
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Details
- Title
- Solid-State Nuclear Magnetic Resonance Insights into the Precursor-Dependent Structure and Na-Ion Storage Behavior of Na-Preintercalated Bilayered Vanadium Oxides
- Creators
- Xinle Zhang - Drexel University, Materials Science and EngineeringTimofey Kirillovich Averianov - Drexel University, Materials Science and EngineeringMina Mozafari - Hunter CollegePhillip Stallworth - Hunter CollegeDmitri V Barbash - Drexel University, Materials Characterization CoreSteven G Greenbaum - Hunter CollegeEkaterina A Pomerantseva (Corresponding Author) - Drexel University, Materials Science and Engineering
- Publication Details
- Chemistry of Materials, Forthcoming
- Publisher
- ACS Publications
- Number of pages
- 11
- Grant note
- Division of Materials Research: DMR-2106445
This work was supported by the National Science Foundation grant DMR-2106445. The XRD, SEM, and XPS analyses in this work were carried out using facilities in the Materials Characterization Core (MCC) at Drexel University. We thank Prof. Kevin Owens from the Department of Chemistry at Drexel University for providing us with access to the atomic absorption spectroscopy (AAS) analysis in the Instrumental Analytical Laboratory. The NMR and EPR work at Hunter College was supported in part by the U.S. National Aeronautics and Space Administration (NASA) via the NASA-Hunter Center for Advanced Energy Storage for Space under cooperative agreement #80NSSC24M0177.
- Resource Type
- Journal article
- Language
- English
- Academic Unit
- Materials Science and Engineering; Materials Characterization Core
- Web of Science ID
- WOS:001748998600001
- Other Identifier
- 991022172968204721