{"status":"ok","message-type":"work","message-version":"1.0.0","message":{"indexed":{"date-parts":[[2026,8,19]],"date-time":"2026-08-19T19:56:22Z","timestamp":1787169382424,"version":"build-2736575974"},"reference-count":90,"publisher":"MDPI AG","issue":"20","license":[{"start":{"date-parts":[[2025,10,13]],"date-time":"2025-10-13T00:00:00Z","timestamp":1760313600000},"content-version":"vor","delay-in-days":0,"URL":"https:\/\/creativecommons.org\/licenses\/by\/4.0\/"}],"funder":[{"name":"Korea government","award":["RS-2019-NR040065"],"award-info":[{"award-number":["RS-2019-NR040065"]}]}],"content-domain":{"domain":[],"crossmark-restriction":false},"short-container-title":["Nanomaterials"],"abstract":"<jats:p>The rational design of multifunctional electrocatalysts requires synergistic integration of conductive scaffolds with redox-active components. Here, a hierarchical core\u2013shell NiCo2S4 grown\/anchored on Co9S8-loaded carbon nanofibers (NCS\/CS\/CNFs) was synthesized via an electrospinning and hydrothermal approach and systematically characterized. FESEM\/TEM confirmed a core-shell nanofiber structure with a NiCo2S4 shell thickness of ~30\u201370 nm, increasing the fiber diameter to ~290 \u00b1 30 nm, while BET analysis revealed a surface area of 24.84 m2 g\u22121 and pore volume of 0.042 cm3 g\u22121, surpassing CS\/CNFs (6.12 m2 g\u22121) and NCS (4.85 m2 g\u22121). XRD confirmed crystalline NiCo2S4 and Co9S8 phases, while XPS identified mixed Ni2+\/Ni3+ and Co2+\/Co3+ states with strong Ni-S\/Co-S bonding, indicating enhanced electron delocalization. Electrochemical measurements in 1 M KOH demonstrated outstanding OER activity, with NCS\/CS\/CNFs requiring only 324 mV overpotential at 10 mA cm\u22122, a Tafel slope of 125.7 mV dec\u22121, and low charge-transfer resistance (0.33 \u03a9 cm2). They also achieved a high areal capacitance of 1412.5 \u03bcF cm\u22122 and maintained a stable current density for &gt;5 h. For methanol oxidation, the composite delivered 150 mA cm\u22122 at 0.1 M methanol, ~1.6 times that of CS and 1.3 times that of NCS, while maintaining stability for 18,000 s. This bifunctional activity underscores the synergy between conductive CNFs and hierarchical sulfides, offering a scalable route to durable electrocatalysts for water splitting and direct methanol fuel cells.<\/jats:p>","DOI":"10.3390\/nano15201559","type":"journal-article","created":{"date-parts":[[2025,10,14]],"date-time":"2025-10-14T05:48:21Z","timestamp":1760420901000},"page":"1559","update-policy":"https:\/\/doi.org\/10.3390\/mdpi_crossmark_policy","source":"Crossref","is-referenced-by-count":5,"title":["Engineering 3D Heterostructured NiCo2S4\/Co9S8-CNFs via Electrospinning and Hydrothermal Strategies for Efficient Bifunctional Energy Conversion"],"prefix":"10.3390","volume":"15","author":[{"given":"Dhananjaya","family":"Merum","sequence":"first","affiliation":[{"name":"Department of Chemistry, College of Natural Sciences, Yeungnam University, 280 Daehak-Ro, Gyeongsan 38541, Gyeongbuk, Republic of Korea"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-7293-8899","authenticated-orcid":false,"given":"Rama Krishna","family":"Chava","sequence":"additional","affiliation":[{"name":"Department of Chemistry, College of Natural Sciences, Yeungnam University, 280 Daehak-Ro, Gyeongsan 38541, Gyeongbuk, Republic of Korea"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-7199-9881","authenticated-orcid":false,"given":"Misook","family":"Kang","sequence":"additional","affiliation":[{"name":"Department of Chemistry, College of Natural Sciences, Yeungnam University, 280 Daehak-Ro, Gyeongsan 38541, Gyeongbuk, Republic of Korea"}],"role":[{"vocabulary":"crossref","role":"author"}]}],"member":"1968","published-online":{"date-parts":[[2025,10,13]]},"reference":[{"key":"ref_1","doi-asserted-by":"crossref","first-page":"101873","DOI":"10.1016\/j.gsf.2024.101873","article-title":"Energy Access Challenge and the Role of Fossil Fuels in Meeting Electricity Demand: Promoting Renewable Energy Capacity for Sustainable Development","volume":"15","author":"Zhang","year":"2024","journal-title":"Geosci. 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