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The evolution of the structural and morphological parameters under the effect of time was analyzed by XRD, ATR-FTIR, XPS, and SEM-EDS. The XRD results show that for longer reaction times (18 h), the ZnMn2O4 spinel samples present a tetragonal structure with high crystallinity and an average crystallite size of 32.3 \u00b1 1.7 nm, larger than those obtained for 6 h and 12 h. The ATR-FTIR spectra confirm the structural results, with well-defined peaks related to stretching vibrations of M-O (M = Zn, Mn) functional groups. XPS reveals the co-existence of several metal oxides and hydroxides at the outermost surface. SEM analysis shows that the samples present a pyramid morphology, better defined at 18 h, with an average particle size of 6.2 \u00b1 1.5 \u00b5m. EDS analysis of ZnMn2O4 (18 h) reveals atomic ratios of 0.45, 0.22, and 0.50 for Zn\/Mn, Zn\/O, and Mn\/O, respectively, in good agreement with the expected values. Based on the CVs, the synthesized ZnMn2O4 samples formed at 18 h showed the most promising electrochemical properties, with a specific capacity of 102 F g\u22121, offering great potential in supercapacitor applications.<\/jats:p>","DOI":"10.3390\/en15249352","type":"journal-article","created":{"date-parts":[[2022,12,12]],"date-time":"2022-12-12T05:10:19Z","timestamp":1670821819000},"page":"9352","update-policy":"https:\/\/doi.org\/10.3390\/mdpi_crossmark_policy","source":"Crossref","is-referenced-by-count":28,"title":["ZnMn2O4 Nanopyramids Fabrication by Hydrothermal Route: Effect of Reaction Time on the Structural, Morphological, and Electrochemical Properties"],"prefix":"10.3390","volume":"15","author":[{"ORCID":"https:\/\/orcid.org\/0000-0001-5943-4880","authenticated-orcid":false,"given":"Souha","family":"Aouini","sequence":"first","affiliation":[{"name":"Laboratory of Nanomaterials and Systems for Renewable Energies (LaNSER), Research and Technology Center of Energy (CRTEn), Techno-Park Borj Cedria, Bp 95, Hammam-Lif, Tunis 2050, Tunisia"},{"name":"Faculty of Science of Tunis, University of Tunis, El Manar, Tunis 2092, Tunisia"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-3295-7897","authenticated-orcid":false,"given":"Afrah","family":"Bardaoui","sequence":"additional","affiliation":[{"name":"Laboratory of Nanomaterials and Systems for Renewable Energies (LaNSER), Research and Technology Center of Energy (CRTEn), Techno-Park Borj Cedria, Bp 95, Hammam-Lif, Tunis 2050, Tunisia"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-6784-6540","authenticated-orcid":false,"given":"Ana","family":"Ferraria","sequence":"additional","affiliation":[{"name":"BSIRG, iBB\u2014Institute for Bioengineering and Biosciences, Chemical Engineering Department, Instituto Superior T\u00e9cnico, Universidade de Lisboa, 1049-001 Lisbon, Portugal"},{"name":"Associate Laboratory i4HB\u2014Institute for Health and Bioeconomy, Instituto Superior T\u00e9cnico, Universidade de Lisboa, 1049-001 Lisbon, Portugal"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-7920-2638","authenticated-orcid":false,"given":"Diogo","family":"Santos","sequence":"additional","affiliation":[{"name":"Center of Physics and Engineering of Advanced Materials, Laboratory for Physics of Materials and Emerging Technologies, Chemical Engineering Department, Instituto Superior T\u00e9cnico, Universidade de Lisboa, 1049-001 Lisbon, Portugal"}]},{"given":"Radhouane","family":"Chtourou","sequence":"additional","affiliation":[{"name":"Laboratory of Nanomaterials and Systems for Renewable Energies (LaNSER), Research and Technology Center of Energy (CRTEn), Techno-Park Borj Cedria, Bp 95, Hammam-Lif, Tunis 2050, Tunisia"}]}],"member":"1968","published-online":{"date-parts":[[2022,12,10]]},"reference":[{"key":"ref_1","doi-asserted-by":"crossref","first-page":"100214","DOI":"10.1016\/j.mtsust.2022.100214","article-title":"Hydrothermal Synthesis of Transition Metal Oxides, Transition Metal Oxide\/Carbonaceous Material Nanocomposites for Supercapacitor Applications","volume":"19","author":"Nandagudi","year":"2022","journal-title":"Mater. 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