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. 2023 Jan 27;13(3):511.
doi: 10.3390/nano13030511.

Enhancement of Hydrophilicity of Nano-Pitted TiO2 Surface Using Phosphoric Acid Etching

Ferenc Koppány  1 , Krisztián Benedek Csomó  1 , Edvárd Márton Varmuzsa  1 , Eszter Bognár  2 , Liza Pelyhe  2 , Péter Nagy  2 , Imre Kientzl  2 , Dániel Szabó  2 , Miklós Weszl  3 , Gábor Dobos  4 , Sándor Lenk  4 , Gábor Erdei  4 , Gábor Kiss  4 , Lilien Nagy  5 , Attila Sréter  6 , Andrea Alexandra Belik  7 , Zsuzsanna Tóth  8 , János Vág  8 , Árpád Joób-Fancsaly  1 , Zsolt Németh  1
Affiliations

Enhancement of Hydrophilicity of Nano-Pitted TiO2 Surface Using Phosphoric Acid Etching

Ferenc Koppány et al. Nanomaterials (Basel). .

Abstract

Our research group developed a novel nano-pitted (NP) TiO2 surface on grade 2 titanium that showed good mechanical, osteogenic, and antibacterial properties; however, it showed weak hydrophilicity. Our objective was to develop a surface treatment method to enhance the hydrophilicity of the NP TiO2 surface without the destruction of the nano-topography. The effects of dilute and concentrated orthophosphoric (H3PO4) and nitric acids were investigated on wettability using contact angle measurement. Optical profilometry and atomic force microscopy were used for surface roughness measurement. The chemical composition of the TiO2 surface and the oxidation state of Ti was investigated using X-ray photoelectron spectroscopy. The ccH3PO4 treatment significantly increased the wettability of the NP TiO2 surfaces (30°) compared to the untreated control (88°). The quantity of the absorbed phosphorus significantly increased following ccH3PO4 treatment compared to the control and caused the oxidation state of titanium to decrease (Ti4+ → Ti3+). Owing to its simplicity and robustness the presented surface treatment method may be utilized in the industrial-scale manufacturing of titanium implants.

Keywords: hydrophilicity; implant; nano; phosphoric acid; titanium-dioxide.

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Conflict of interest statement

The authors declare no conflict of interest.

Figures

Figure 1
Figure 1
The effect of surface treatments on the wettability of NP surface. The treatment of the NP surface using ccH3PO4 has significantly increased the wettability compared to the untreated control (p * = 0.00). The other etchants did not cause an apparent effect on the wettability of the NP surface.
Figure 2
Figure 2
Proportion of elements on the untreated control and the ccH3PO4-treated NP surfaces. Panel A shows that the concentrations of phosphorus and oxygen are higher on the ccH3PO4-treated NP surface than on the untreated control. Panel B shows that the proportion of phosphorus did not change on the control or on the ccH3PO4-treated NP surfaces after sputtering. Carbon concentration is intentionally omitted because it would have caused the visualization of the other elements to be difficult (see Table 3 for data).
Figure 3
Figure 3
XPS spectra of untreated control (A) and ccH3PO4-treated NP surfaces (B) after sputtering. The Ti 2p3/2 peak appeared at 459.1 eV (blue curve) for the untreated NP surface, indicating fully coordinated Ti4+ ions, suggesting the oxide layer was solely constituted of TiO2. (The black curve is the corresponding Ti 2p1/2 component of the doublet peak.) On panel B, an additional doublet peak appeared at 458.8 eV binding energy, which indicates the presence of Ti3+ beside Ti4+ in the oxide layer. (Here the blue curve is Ti3+ 2p3/2, the green one is Ti4+ 2p3/2, while the black and purple curves are the corresponding Ti3+ 2p1/2 and Ti4+ 2p1/2 components of the doublets).
See this image and copyright information in PMC

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