<p>In this study, CuO-NiO-Mn<sub>3</sub>O<sub>4</sub> nanocomposites (NC) and their pristine materials were synthesized via the thermal decomposition method and characterized using XRD, Raman, SEM with EDX, TEM, XPS, UV-Vis and PL spectroscopy. XRD analysis confirmed the monoclinic, cubic and tetragonal phases of CuO, NiO and Mn<sub>3</sub>O<sub>4</sub>, respectively, in both pristine and composite forms. Raman spectroscopy validated the phase purity and vibrational characteristics such as Ag, Bg, TO, LO and A<sub>1</sub>g modes of all the prepared samples. SEM revealed distinct morphologies for the pristine NPs, showing spherical CuO, flaky clustered NiO, and bulk Mn<sub>3</sub>O<sub>4</sub>, while the NC displayed a mixed morphology of small and large particles, reflecting its composite nature. TEM analysis further confirmed particle size variation, with pristine NPs measuring 200–400&#xa0;nm and the NC showing a reduction to 50–100&#xa0;nm, indicating size refinement upon composite formation. EDX and XPS analysis verified the occurrence of Cu, Ni, Mn and O elements along with their chemical states. The CuO-NiO-Mn<sub>3</sub>O<sub>4</sub>NC exhibited a reduced energy gap (E<sub>g</sub> = 1.11&#xa0;eV) compared to CuO (2.41&#xa0;eV), NiO (2.67&#xa0;eV) and Mn<sub>3</sub>O<sub>4</sub> (1.21&#xa0;eV), enhancing its photocatalytic performance. Photocatalytic Cr(VI) reduction studies demonstrated that 30&#xa0;mg of CuO-NiO-Mn<sub>3</sub>O<sub>4</sub> NC achieved 93% reduction efficiency with a rate constant of k<sub>obs</sub> = 0.09286&#xa0;min<sup>− 1</sup>. The composite exhibited excellent cycling stability over five repeated cycles, with electrons (e<sup>−</sup>) and superoxide radicals (<sup>•</sup>O<sub>2</sub><sup>−</sup>) identified as key contributors to the reduction process at pH 3 ± 0.1.</p>

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Structural, Morphological and Optical Properties of CuO-NiO-Mn3O4Nanocomposite for Photocatalytic Cr(VI) Reduction

  • Elumalai Arulkumar,
  • Gopinath Dhamodaran,
  • Essam H. Ibrahim,
  • Mohd. Shkir

摘要

In this study, CuO-NiO-Mn3O4 nanocomposites (NC) and their pristine materials were synthesized via the thermal decomposition method and characterized using XRD, Raman, SEM with EDX, TEM, XPS, UV-Vis and PL spectroscopy. XRD analysis confirmed the monoclinic, cubic and tetragonal phases of CuO, NiO and Mn3O4, respectively, in both pristine and composite forms. Raman spectroscopy validated the phase purity and vibrational characteristics such as Ag, Bg, TO, LO and A1g modes of all the prepared samples. SEM revealed distinct morphologies for the pristine NPs, showing spherical CuO, flaky clustered NiO, and bulk Mn3O4, while the NC displayed a mixed morphology of small and large particles, reflecting its composite nature. TEM analysis further confirmed particle size variation, with pristine NPs measuring 200–400 nm and the NC showing a reduction to 50–100 nm, indicating size refinement upon composite formation. EDX and XPS analysis verified the occurrence of Cu, Ni, Mn and O elements along with their chemical states. The CuO-NiO-Mn3O4NC exhibited a reduced energy gap (Eg = 1.11 eV) compared to CuO (2.41 eV), NiO (2.67 eV) and Mn3O4 (1.21 eV), enhancing its photocatalytic performance. Photocatalytic Cr(VI) reduction studies demonstrated that 30 mg of CuO-NiO-Mn3O4 NC achieved 93% reduction efficiency with a rate constant of kobs = 0.09286 min− 1. The composite exhibited excellent cycling stability over five repeated cycles, with electrons (e) and superoxide radicals (O2) identified as key contributors to the reduction process at pH 3 ± 0.1.