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Tetragonal to monoclinic phase transition observed during Zr anodisation

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Abstract

Plasma electrolytic oxidation (PEO) is a coating procedure that utilises anodic oxidation in aqueous electrolytes above the dielectric breakdown voltage to produce oxide coatings that have specific properties. These conditions facilitate oxide formation under localised high temperatures and pressures that originate from short-lived microdischarges at sites over the metal surface and have fast oxide volume expansion. Anodic ZrO2 films were prepared by subjecting metallic zirconium to PEO in acid solutions (H2C2O4 and H3PO4) using a galvanostatic DC regime. The ZrO2 microstructure was investigated in films that were prepared at different charge densities. During the anodic breakdown, an important change in the amplitude of the voltage oscillations at a specific charge density was observed (i.e., the transition charge density (Q T)). We verified that this transition charge is a monotonic function of both the current density and temperature applied during the anodisation, which indicated that Q T is an intrinsic response of this system. The oxide morphology and microstructure were characterised using SEM and X-ray diffraction experiments (XRD) techniques. X-ray diffraction analysis revealed that the change in voltage oscillation was correlated with oxide microstructure changes during the breakdown process.

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Acknowledgements

The authors gratefully acknowledge the financial support from the Brazilian research funding agencies FAPESP and CNPq.

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  1. Donizete X. da Silva

    Present address: Universidade Federal de Tocantins, Palmas, TO, Brazil

Authors and Affiliations

  1. Departamento de Física, Química e Matemática, Universidade Federal de São Carlos, São Carlos, SP, Brazil

    Francisco Trivinho-Strixino

  2. Laboratório Computacional de Análises Cristalográficas e Cristalinas, Depto de Físico-Química, Instituto de Química, Universidade Estadual Paulista, Araraquara, SP, Brazil

    Carlos O. Paiva-Santos

  3. Departamento de Química, Universidade Federal de São Carlos, Rod. Washington Luis Km 235, Cx 676, São Carlos, SP, Brazil

    Ernesto C. Pereira

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  1. Francisco Trivinho-Strixino
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Trivinho-Strixino, F., da Silva, D.X., Paiva-Santos, C.O. et al. Tetragonal to monoclinic phase transition observed during Zr anodisation. J Solid State Electrochem 17, 191–199 (2013). https://doi.org/10.1007/s10008-012-1883-4

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