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Herein, a self-supported VS2-V2O5(x:y)@NF composite electrode was constructed through a stepwise hydrothermal strategy. In this design, vertically grown VS2 on nickel foam provides a conductive and open scaffold, while V2O5-derived oxygen-containing domains are introduced into the surface and inter-array spaces to increase accessible reaction sites and regulate the local adsorption environment. Among the investigated compositions, VS2-V2O5(1:1)@NF exhibits the most balanced bifunctional response within the sample series, requiring overpotentials of 272.2 mV for HER and 292.8 mV for OER at 10 mA cm\u20132 in 1 M KOH. In a two-electrode overall water-splitting configuration, the symmetric electrolyzer requires cell voltages of 1.88 V and 2.27 V to deliver 10 and 100 mA cm\u20132, respectively. The performance variation among the samples prepared with different V2O5 precursor-feeding amounts is correlated with the self-supported sulfide\/oxide architecture, electrochemically accessible interface, apparent charge-transfer behavior, wettability, and surface reconstruction. The present results do not directly establish Fermi-level equilibration or quantitative interfacial charge redistribution.<\/jats:p>","DOI":"10.1021\/acsami.6c18277","type":"journal-article","created":{"date-parts":[[2026,10,13]],"date-time":"2026-10-13T08:01:59Z","timestamp":1791878519000},"source":"Crossref","is-referenced-by-count":0,"title":["Stepwise Construction of a Self-Supported VS2\u2013V2O5@NF Sulfide\/Oxide Composite Electrode for Alkaline Overall Water Splitting"],"prefix":"10.1021","author":[{"given":"Bo","family":"Dou","sequence":"first","affiliation":[{"name":"Jiamusi University , , , ,","place":["Jiamusi, Heilongjiang, China, 154007"]},{"name":"Dongguan University of Technology , , ,","place":["Dongguan, China, 523808"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Lige","family":"Bi","sequence":"additional","affiliation":[{"name":"Jiamusi University , , , ,","place":["Jiamusi, Heilongjiang, China, 154007"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Meili","family":"Qi","sequence":"additional","affiliation":[{"name":"Jiamusi University , , , ,","place":["Jiamusi, Heilongjiang, China, 154007"]},{"name":"Jiamusi University , , , ,","place":["Jiamusi, Heilongjiang, China, 154007"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Qiuqi","family":"Li","sequence":"additional","affiliation":[{"name":"Dongguan University of Technology , , ,","place":["Dongguan, China, 523808"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Yutong","family":"Yu","sequence":"additional","affiliation":[{"name":"Dongguan University of Technology , , ,","place":["Dongguan, China, 523808"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Xinyi","family":"Wu","sequence":"additional","affiliation":[{"name":"Dongguan University of Technology , , ,","place":["Dongguan, China, 523808"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Min","family":"Zhang","sequence":"additional","affiliation":[{"name":"Dongguan University of Technology , , ,","place":["Dongguan, China, 523808"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-4335-5234","authenticated-orcid":true,"given":"Shilei","family":"Xie","sequence":"additional","affiliation":[{"name":"Dongguan University of Technology , , ,","place":["Dongguan, China, 523808"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Faliang","family":"Cheng","sequence":"additional","affiliation":[{"name":"Dongguan University of Technology , , ,","place":["Dongguan, China, 523808"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-5610-0607","authenticated-orcid":true,"given":"Dong","family":"Xie","sequence":"additional","affiliation":[{"name":"Dongguan University of Technology , , ,","place":["Dongguan, China, 523808"]}],"role":[{"vocabulary":"crossref","role":"author"}]}],"member":"316","published-online":{"date-parts":[[2026,10,13]]},"reference":[{"issue":"11","key":"2026101304015288000_cit1","doi-asserted-by":"publisher","first-page":"3351","DOI":"10.1039\/D3CY00298E","article-title":"A Z-Scheme ZnIn2S4\/ZnS Heterojunction Catalyst: Insight into Enhanced Photocatalytic Performance and Mechanism","volume":"13","author":"Liu","year":"2023","journal-title":"Catal. 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