ZnMn 2 O 4 Nanopyramids Fabrication by Hydrothermal Route: Effect of Reaction Time on the Structural, Morphological, and Electrochemical Properties

Souha Aouini, Afrah Bardaoui, Ana M. Ferraria, Diogo M. F. Santos and Radhouane Chtourou
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Souha Aouini: 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
Afrah Bardaoui: 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
Ana M. Ferraria: BSIRG, iBB—Institute for Bioengineering and Biosciences, Chemical Engineering Department, Instituto Superior Técnico, Universidade de Lisboa, 1049-001 Lisbon, Portugal
Diogo M. F. Santos: Center of Physics and Engineering of Advanced Materials, Laboratory for Physics of Materials and Emerging Technologies, Chemical Engineering Department, Instituto Superior Técnico, Universidade de Lisboa, 1049-001 Lisbon, Portugal
Radhouane Chtourou: 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

Energies, 2022, vol. 15, issue 24, 1-16

Abstract: ZnMn 2 O 4 spinels are prepared by a simple hydrothermal route with control of the reaction time, ranging from 6 h to 18 h. 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 ZnMn 2 O 4 spinel samples present a tetragonal structure with high crystallinity and an average crystallite size of 32.3 ± 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 ± 1.5 µm. EDS analysis of ZnMn 2 O 4 (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 ZnMn 2 O 4 samples formed at 18 h showed the most promising electrochemical properties, with a specific capacity of 102 F g −1 , offering great potential in supercapacitor applications.

Keywords: hydrothermal synthesis; ZnMn 2 O 4 spinel; nanopyramids; electrochemical performances (search for similar items in EconPapers)
JEL-codes: Q Q0 Q4 Q40 Q41 Q42 Q43 Q47 Q48 Q49 (search for similar items in EconPapers)
Date: 2022
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