Anodic oxide coatings with a hierarchical micronanostructure on sintered titanium powders

Natalia M. Yakovleva; Alisa M. Shul’ga; Irina V. Lukiyanchuk; Kristina V. Stepanova; Alexander N. Kokatev; Elena S. Chubieva

doi:10.17308/kcmf.2022.24/10561

Natalia M. Yakovleva Petrozavodsk State University, 33 Lenina prospekt, Petrozavodsk 185910, Russian Federation https://orcid.org/0000-0003-4294-0183
Alisa M. Shul’ga Petrozavodsk State University, 33 Lenina prospekt, Petrozavodsk 185910, Russian Federation https://orcid.org/0000-0002-3844-7110
Irina V. Lukiyanchuk Institute of Chemistry of the Far Eastern Branch of the Russian Academy of Sciences, 159 100-Letiya Oktyabrya ul., Vladivistik 690022, Russian Federation https://orcid.org/0000-0003-1680-4882
Kristina V. Stepanova Petrozavodsk State University, 33 Lenina prospekt, Petrozavodsk 185910, Russian Federation https://orcid.org/0000-0002-4737-497X
Alexander N. Kokatev Petrozavodsk State University, 33 Lenina prospekt, Petrozavodsk 185910, Russian Federation https://orcid.org/0000-0002-9449-1482
Elena S. Chubieva Petrozavodsk State University, 33 Lenina prospekt, Petrozavodsk 185910, Russian Federation https://orcid.org/0000-0001-6782-8089

DOI: https://doi.org/10.17308/kcmf.2022.24/10561

Keywords: Sintered powders, Porous powder materials, Titanium sponge, Anodic oxide coatings, Structure hierarchy, Microcones, Crystalline, Nanostructured titanium dioxide, Scanning electron microscopy, Atomic force microscopy

Abstract

TiO₂ nanotubes formed by electrochemical anodising of Ti (titanium foil) are normally X-ray amorphous. To improve their functional properties, they are usually converted into crystalline nanotubes by annealing at T ≈ 400–500 °С. What is more, under certain conditions, oxide films with a hierarchical micronanostructure can be formed on titanium foil by anodising in fluorine-containing electrolytes. Such films contain nanostructured microcones whose atomic structure corresponds to anatase (a-TiO₂). It is interesting to find out whether it is possible to form anodic oxide coatings with a hierarchical micronanostructure on the surface of sintered powders of titanium sponge, which should have much larger specific surfaces and a wider range of applications. This paper is aimed at the study of the process of anodising porous samples of sintered
powders of titanium sponge in an aqueous electrolyte (1 М Н₂SO₄ + 0.15 wt % HF).
The object of our study were sintered titanium powders in the form of samples of porous powder materials with a specific area of Ssp = 1,350 cm²/g. Anodising was conducted in a 1 М Н₂SO₄ + 0.15 wt % HF electrolyte at various values of current density (jm). Surface morphology before and after anodising was investigated by scanning electron microscopy and atomic force microscopy. X-ray diffractometry was used to study the phase composition.
The research involved the study of the influence of conditions for the galvanostatic anodising of samples of porous powder materials made from titanium sponge on the growth, morphology, and atomic structure of anodic oxide coatings. For the first time, it was shown that anodising at the values of current density jm = (230÷1,890) mA/g leads to the appearance of nanostructured a-TiO₂ microcones (with base diameters and heights of up to 4 μm) in an amorphous nanoporous/nanotube oxide matrix (with an effective pore/tube diameter of about 50 nm). Since such coatings have a high specific area and a hierarchical micronanostructure, they are promising for the design of devices for photocatalytic environment purification
and production of superhydrophobic surfaces.

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Author Biographies

Natalia M. Yakovleva, Petrozavodsk State University, 33 Lenina prospekt, Petrozavodsk 185910, Russian Federation

Dr. Sci. (Phys.–Math.), Full
Professor, Professor at the Department of Information –
Measuring Systems and Physical Electronics,
Petrozavodsk State University (Petrozavodsk, Republic
of Karelia, Russian Federation)

Alisa M. Shul’ga, Petrozavodsk State University, 33 Lenina prospekt, Petrozavodsk 185910, Russian Federation

Engineer, Petrozavodsk State
University (Petrozavodsk, Republic of Karelia, Russian
Federation)

Irina V. Lukiyanchuk, Institute of Chemistry of the Far Eastern Branch of the Russian Academy of Sciences, 159 100-Letiya Oktyabrya ul., Vladivistik 690022, Russian Federation

Cand. Sci. (Chem.), Senior
Researcher, Institute of Chemistry, Far-Eastern
Branch, Russian Academy of Sciences V(ladivostok,
Russian Federation)

Kristina V. Stepanova, Petrozavodsk State University, 33 Lenina prospekt, Petrozavodsk 185910, Russian Federation

Cand. Sci. (Tech.), Associate
Professor, Petrozavodsk State University, (Petrozavodsk,
Republic of Karelia, Russian Federation)

Alexander N. Kokatev, Petrozavodsk State University, 33 Lenina prospekt, Petrozavodsk 185910, Russian Federation

Cand. Sci. (Tech.), Engineer,
Petrozavodsk State University (Petrozavodsk, Republic
of Karelia, Russian Federation)

Elena S. Chubieva, Petrozavodsk State University, 33 Lenina prospekt, Petrozavodsk 185910, Russian Federation

Engineer, Petrozavodsk State
University (Petrozavodsk, Republic of Karelia, Russian
Federation)

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