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Article

Ultra-Rapid Synthesis of Co3O4 Nanostructures with Tunable Morphology via Nickel-Assisted Anodization

by
Leydi Julieta Cardenas Flechas
1,2,
Jorge Bautista-Ruiz
3,
Paulo Tarso Cavalcante Freire
4,
Elaine Cristina Paris
5 and
Miryam Rincón Joya
6,*
1
Departamento de Ingeniería, Mecánica y Mecatrónica, Universidad Nacional de Colombia, Carrera 45 N 26-85, Bogotá 111321, Colombia
2
Departamento de Ingeniería, Mecánica y Mecatrónica, Fundación Universidad de América, Bogotá 111321, Colombia
3
Departamento de Ingeniería, Investigación de Materiales Cerámicos, Universidad Francisco de Paula Santander, San José de Cúcuta 540003, Colombia
4
Departamento de Física, Universidade Federal do Ceará, Fortaleza 60455-760, CE, Brazil
5
Embrapa Instrumentação, Rua XV de Novembro, 1452, São Carlos 13560-970, SP, Brazil
6
Departamento de Física, Universidad Nacional de Colombia, Carrera 45 N 26-85, Bogotá 11001, Colombia
*
Author to whom correspondence should be addressed.
Inorganics 2025, 13(11), 350; https://doi.org/10.3390/inorganics13110350 (registering DOI)
Submission received: 7 October 2025 / Revised: 20 October 2025 / Accepted: 24 October 2025 / Published: 26 October 2025

Abstract

Various morphologies of cobalt oxide Co3O4 films on cobalt (Co) foils were obtained via anodization followed by a thermal treatment at 350 °C. This study introduces a rapid and cost-effective synthesis route, achieving well-defined spinel structures in only 30 min. The novelty of this work lies in exploring nickel (Ni) as a morphological modifier in the anodization electrolyte. FESEM analysis revealed that, while anodization without Ni produced nanoflake structures, the inclusion of Ni transformed the morphology into larger cubic crystals and rice grain–shaped nanoparticles. XPS confirmed the presence of oxygen vacancies during phase formation, TEM showed spinel grains smaller than 20 nm, and Raman spectroscopy exhibited characteristic peak shifts influenced by both anodization and Ni addition. These results demonstrate that Ni not only accelerates the formation of spinel Co3O4 but also plays a decisive role in tailoring morphology, highlighting the efficiency and novelty of this approach.
Keywords: anodizing; Co film; Co3O4; nickel; various microstructural forms anodizing; Co film; Co3O4; nickel; various microstructural forms

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MDPI and ACS Style

Cardenas Flechas, L.J.; Bautista-Ruiz, J.; Freire, P.T.C.; Paris, E.C.; Joya, M.R. Ultra-Rapid Synthesis of Co3O4 Nanostructures with Tunable Morphology via Nickel-Assisted Anodization. Inorganics 2025, 13, 350. https://doi.org/10.3390/inorganics13110350

AMA Style

Cardenas Flechas LJ, Bautista-Ruiz J, Freire PTC, Paris EC, Joya MR. Ultra-Rapid Synthesis of Co3O4 Nanostructures with Tunable Morphology via Nickel-Assisted Anodization. Inorganics. 2025; 13(11):350. https://doi.org/10.3390/inorganics13110350

Chicago/Turabian Style

Cardenas Flechas, Leydi Julieta, Jorge Bautista-Ruiz, Paulo Tarso Cavalcante Freire, Elaine Cristina Paris, and Miryam Rincón Joya. 2025. "Ultra-Rapid Synthesis of Co3O4 Nanostructures with Tunable Morphology via Nickel-Assisted Anodization" Inorganics 13, no. 11: 350. https://doi.org/10.3390/inorganics13110350

APA Style

Cardenas Flechas, L. J., Bautista-Ruiz, J., Freire, P. T. C., Paris, E. C., & Joya, M. R. (2025). Ultra-Rapid Synthesis of Co3O4 Nanostructures with Tunable Morphology via Nickel-Assisted Anodization. Inorganics, 13(11), 350. https://doi.org/10.3390/inorganics13110350

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