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Here, a hydrothermal route on carbon fibre paper is used as a model platform to prepare nickel-cobalt hydroxide\/carbonate-hydroxide nanostructures across a controlled composition series. Rather than introducing new catalyst chemistry, this work establishes an image-based morphology map linking mesoscale structural parameters to the apparent oxygen evolution reaction response. Scanning electron microscopy reveals a systematic evolution from Co-rich nanofibre coatings to Ni-rich nanoplate architectures. The nanostructures are quantified through the fibre diameter,\n                    <jats:italic>D<\/jats:italic>\n                    , and the nanoplate thickness and length,\n                    <jats:italic>t<\/jats:italic>\n                    and\n                    <jats:italic>L<\/jats:italic>\n                    . These parameters capture trends that nominal composition alone does not explain: the apparent Tafel slope decreases as the fibre diameter is reduced and the fibrous morphology is replaced by plates, while the apparent charge-transfer resistance follows the evolution of the nanoplate dimensions. The 1:1 Ni:Co electrode deviates from a simple composition-based trend, being consistent with its mixed fibre\/plate architecture and comparatively large plate dimensions. The best Ni-rich electrode reaches an overpotential of 365 mV at 10 mAcm\n                    <jats:sup>\u22122<\/jats:sup>\n                    after conditioning and operates at 20 mAcm\n                    <jats:sup>\u22122<\/jats:sup>\n                    for 50 h with negligible morphological degradation. These results provide a practical morphology design rule for carbon-supported Ni\u2013Co hydroxide-derived electrodes.\n                  <\/jats:p>","DOI":"10.1088\/1361-6528\/aea333","type":"journal-article","created":{"date-parts":[[2026,9,7]],"date-time":"2026-09-07T22:48:14Z","timestamp":1788821294000},"page":"385601","update-policy":"https:\/\/doi.org\/10.1088\/crossmark-policy","source":"Crossref","is-referenced-by-count":0,"title":["Morphology mapping of nickel-cobalt\/carbonate hydroxide nanostructures on carbon fibre electrodes for oxygen evolution reaction"],"prefix":"10.1088","volume":"37","author":[{"ORCID":"https:\/\/orcid.org\/0000-0002-9244-9512","authenticated-orcid":true,"given":"Sofia","family":"Ferreira-Teixeira","sequence":"first","affiliation":[{"name":"CIC nanoGUNE BRTA"},{"name":"INL\u2014International Iberian Nanotechnology Laboratory"}],"role":[{"vocabulary":"crossref","role":"author"},{"role":"conceptualization","vocabulary":"credit"},{"role":"formal-analysis","vocabulary":"credit"},{"role":"funding-acquisition","vocabulary":"credit"},{"role":"investigation","vocabulary":"credit"},{"role":"methodology","vocabulary":"credit"},{"role":"validation","vocabulary":"credit"},{"role":"writing-original-draft","vocabulary":"credit"},{"role":"writing-review-editing","vocabulary":"credit"}]}],"member":"266","published-online":{"date-parts":[[2026,9,21]]},"reference":[{"key":"nanoaea333bib1","doi-asserted-by":"publisher","first-page":"972","DOI":"10.1126\/science.1103197","type":"journal-article","article-title":"Sustainable hydrogen production","volume":"305","author":"Turner","year":"2004","journal-title":"Science"},{"key":"nanoaea333bib2","doi-asserted-by":"publisher","first-page":"6446","DOI":"10.1021\/cr1002326","type":"journal-article","article-title":"Solar water splitting cells","volume":"110","author":"Walter","year":"2010","journal-title":"Chem. 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