scholarly journals Plasma Electrolytic Oxidation of Titanium in H2SO4–H3PO4 Mixtures

Coatings ◽  
2020 ◽  
Vol 10 (2) ◽  
pp. 116 ◽  
Author(s):  
Bernd Engelkamp ◽  
Björn Fischer ◽  
Klaus Schierbaum
Keyword(s):  
Sulfuric Acid ◽  
Phosphoric Acid ◽  
Oxide Layer ◽  
Plasma Electrolytic Oxidation ◽  
Phase Changes ◽  
Crystal Phase ◽  
Plasma Discharges ◽  
X Ray ◽  
Electrolytic Oxidation ◽  
Plasma Electrolytic

Oxide layers on titanium foils were produced by galvanostatically controlled plasma electrolytic oxidation in 12.9 M sulfuric acid with small amounts of phosphoric acid added up to a 3% mole fraction. In pure sulfuric acid, the oxide layer is distinctly modified by plasma discharges. As the time of the process increases, rough surfaces with typical circular pores evolve. The predominant crystal phase of the titanium dioxide material is rutile. With the addition of phosphoric acid, discharge effects become less pronounced, and the predominant crystal phase changes to anatase. Furthermore, the oxide layer thickness and mass gain both increase. Already small amounts of phosphoric acid induce these effects. Our findings suggest that anions of phosphoric acid preferentially adsorb to the anodic area and suppress plasma discharges, and conventional anodization is promoted. The process was systematically investigated at different stages, and voltage and oxide formation efficiency were determined. Oxide surfaces and their cross-sections were studied by scanning electron microscopy and energy-dispersive X-ray spectroscopy. The phase composition was determined by X-ray diffraction and confocal Raman microscopy.

scholarly journals Ag Nanoparticle-Decorated Oxide Coatings Formed via Plasma Electrolytic Oxidation on ZrNb Alloy

Materials ◽  
2019 ◽  
Vol 12 (22) ◽  
pp. 3742 ◽  
Author(s):  
Oleksandr Oleshko ◽  
Volodymyr Deineka V ◽  
Yevgeniia Husak ◽  
Viktoriia Korniienko ◽  
Oleg Mishchenko ◽  
...  
Keyword(s):  
Oxide Layer ◽  
Photoelectron Spectroscopy ◽  
Bacterial Adhesion ◽  
Plasma Electrolytic Oxidation ◽  
Infectious Complications ◽  
Osteoblast Cell ◽  
Effective Prevention ◽  
X Ray ◽  
Electrolytic Oxidation ◽  
Plasma Electrolytic

Plasma electrolytic oxidation (PEO) can provide an ideal surface for osteogenic cell attachment and proliferation with further successful osteointegration. However, the same surface is attractive for bacteria due to similar mechanisms of adhesion in prokaryotic and eukaryotic cells. This issue requires the application of additional surface treatments for effective prevention of postoperative infectious complications. In the present work, ZrNb alloy was treated in a Ca-P solution with Ag nanoparticles (AgNPs) for the development of a new oxide layer that hosted osteogenic cells and prevented bacterial adhesion. For the PEO, 0.5 M Ca(H2PO2)2 solution with 264 mg L−1 of round-shaped AgNPs was used. Scanning electron microscopy with energy-dispersive x-ray and x-ray photoelectron spectroscopy were used for morphology and chemical analysis of the obtained samples; the SBF immersion test, bacteria adhesion test, and osteoblast cell culture were used for biological investigation. PEO in a Ca-P bath with AgNPs provides the formation of a mesoporous oxide layer that supports osteoblast cell adhesion and proliferation. Additionally, the obtained surface with incorporated Ag prevents bacterial adhesion in the first 6 h after immersion in a pathogen suspension, which can be an effective approach to prevent infectious complications after implantation.

INCORPORATION OF MULTI-WALLED CARBON NANOTUBES INTO OXIDE LAYER FORMED ON AL ALLOY BY PLASMA ELECTROLYTIC OXIDATION

2020 ◽  
Vol 27 (11) ◽  
pp. 2050007
Author(s):  
KOANGYONG HYUN ◽  
JUNG-HYUNG LEE ◽  
SEONG-JONG KIM
Keyword(s):  
Carbon Nanotubes ◽  
Oxide Layer ◽  
Plasma Electrolytic Oxidation ◽  
Aqueous Suspension ◽  
Al Alloy ◽  
Time Curve ◽  
Oxide Layers ◽  
X Ray ◽  
Electrolytic Oxidation ◽  
Plasma Electrolytic

Plasma electrolytic oxidation (PEO) is an electrochemical-based surface modification technique that produces oxide layers on valve metals. The PEO process is performed in an electrolyte solution, which offers the possibility of particles’ incorporation into the growing oxide layer. In this study, we employed a PEO technique on a commercial Al alloy in an aqueous suspension of carbon nanotubes (CNTs) to fabricate CNT-incorporated oxide layer. The voltage–time response was recorded during the process. The surface of the resulting oxide layer was characterized by means of a scanning electron microscope (SEM), an energy-dispersive X-ray spectrometer (EDS), and X-ray diffraction (XRD). It was found from the SEM observation that the CNTs were successfully incorporated into the oxide layer. The PEO with the addition of CNTs led to a delay in time to breakdown (50[Formula: see text][Formula: see text][Formula: see text]s) and a decrease in breakdown voltage (442[Formula: see text][Formula: see text][Formula: see text]V) in the voltage–time curve. The microstructural feature was clearly distinguishable between the oxide layers produced with and without CNTs: a pancake-like structure for PEO without CNTs, and a doughnut-like structure for PEO with CNTs. However, neither the results of the structure analysis nor the elemental analysis provides a clear indication of carbon, even though the presence of CNTs in the oxide layer is evident, suggesting that further optimization of CNT concentration is required.

scholarly journals Energy-Dispersive X-Ray Spectroscopy Mapping of Porous Coatings Obtained on Titanium by Plasma Electrolytic Oxidation in a Solution Containing Concentrated Phosphoric Acid with Copper Nitrate

2016 ◽  
Vol 16 (3) ◽  
pp. 15-25 ◽  
Author(s):  
K. Rokosz ◽  
T. Hryniewicz ◽  
Ł. Dudek ◽  
A. Schütz ◽  
J. Heeg ◽  
...  
Keyword(s):  
Chemical Composition ◽  
Phosphoric Acid ◽  
Plasma Electrolytic Oxidation ◽  
Copper Nitrate ◽  
Energy Dispersive ◽  
Porous Coatings ◽  
X Ray ◽  
Study Results ◽  
Electrolytic Oxidation ◽  
Plasma Electrolytic

Abstract The SEM and EDS study results of coatings obtained on titanium by Plasma Electrolytic Oxidation (PEO) in the electrolytes containing of 600 g copper nitrate in 1 liter of concentrated phosphoric acid at 450 V for 1 and 3 minutes, are presented. The obtained coatings are porous and consist mainly of phosphorus within titanium and copper. It was found that the time of PEO oxidation has impact on the chemical composition of the coatings. The longer time of PEO treatment, the higher amount of copper inside coating. The PEO oxidation of titanium for 1 minute has resulted in the creation of coating, on which 3 phases where found, which contained up to 13.4 wt% (9 at%) of copper inside the phosphate structure. In case of 1 minute PEO treatment of titanium, the 2 phases were found, which contained up to 13 wt% (8 at%) of copper inside the phosphate structure. The copper-to-phosphorus ratios after 1 minute processing belong to the range from 0.28 by wt% (0.14 by at%) to 0.47 by wt% (0.23 by at%), while after 3 minutes the same ratios belong to the range from 0.27 by wt% (0.13 by at%) to 0.35 by wt% (0.17 by at%). In summary, it should be stated that the higher amounts of phosphorus and copper were recorded on titanium after PEO oxidation for 3 minutes than these after 1 minute.

ffect of Na2WO4 in electrolyte on mechanical properties of oxide layer on Al alloy via plasma electrolytic oxidation

2015 ◽  
Vol 53 (8) ◽  
pp. 535-540 ◽  
Author(s):  
Young Gun Ko ◽  
Dong Hyuk Shin ◽  
Hae Woong Yang ◽  
Yeon Sung Kim ◽  
Joo Hyun Park ◽  
...  
Keyword(s):  
Mechanical Properties ◽  
Oxide Layer ◽  
Plasma Electrolytic Oxidation ◽  
Al Alloy ◽  
Electrolytic Oxidation ◽  
Plasma Electrolytic

scholarly journals Comparison of Biocompatible Coatings Produced by Plasma Electrolytic Oxidation on cp-Ti and Ti-Zr-Nb Superelastic Alloy

Coatings ◽  
2021 ◽  
Vol 11 (4) ◽  
pp. 401
Author(s):  
Ruzil Farrakhov ◽  
Olga Melnichuk ◽  
Evgeny Parfenov ◽  
Veta Mukaeva ◽  
Arseniy Raab ◽  
...  
Keyword(s):  
Plasma Electrolytic Oxidation ◽  
Electrochemical Impedance ◽  
Pure Titanium ◽  
Commercially Pure Titanium ◽  
X Ray ◽  
Kinetic Coefficients ◽  
Electrolytic Oxidation ◽  
Plasma Electrolytic ◽  
Cp Ti ◽  
Peo Coatings

The paper compares the coatings produced by plasma electrolytic oxidation (PEO) on commercially pure titanium and a novel superelastic alloy Ti-18Zr-15Nb (at. %) for implant applications. The PEO coatings were produced on both alloys in the identical pulsed bipolar regime. The properties of the coatings were examined using scanning electron microscopy (SEM), X-ray diffraction (XRD), and energy-dispersive X-ray spectroscopy (EDX), potentiodynamic polarization (PDP), and electrochemical impedance spectroscopy (EIS). The PEO process kinetics was modeled based on the Avrami theorem and Cottrell equation using a relaxation method. The resultant coatings contain TiO2, for both alloys, and NbO2, Nb2O5, ZrO2 for Ti-18Zr-15Nb alloy. The coating on the Ti-18Zr-15Nb alloy has a higher thickness, porosity, and roughness compared to that on cp-Ti. The values of the kinetic coefficients of the PEO process—higher diffusion coefficient and lower time constant for the processing of Ti-18Zr-15Nb—explain this effect. According to the electrochemical studies, PEO coatings on Ti-18Zr-15Nb alloy provide better corrosion protection. Higher corrosion resistance, porosity, and roughness contribute to better biocompatibility of the PEO coating on Ti-18Zr-15Nb alloy compared to cp-Ti.

scholarly journals Bioactivity Performance of Pure Mg after Plasma Electrolytic Oxidation in Silicate-Based Solutions

Molecules ◽  
2021 ◽  
Vol 26 (7) ◽  
pp. 2094
Author(s):  
Yevheniia Husak ◽  
Joanna Michalska ◽  
Oleksandr Oleshko ◽  
Viktoriia Korniienko ◽  
Karlis Grundsteins ◽  
...  
Keyword(s):  
Cell Culture ◽  
Oxide Layer ◽  
Plasma Electrolytic Oxidation ◽  
Oxide Coating ◽  
Mg Alloy ◽  
Aureus Strain ◽  
Active Surface Area ◽  
Corrosion Properties ◽  
Electrolytic Oxidation ◽  
Plasma Electrolytic

The biodegradable metals, including magnesium (Mg), are a convenient alternative to permanent metals but fast uncontrolled corrosion limited wide clinical application. Formation of a barrier coating on Mg alloys could be a successful strategy for the production of a stable external layer that prevents fast corrosion. Our research was aimed to develop an Mg stable oxide coating using plasma electrolytic oxidation (PEO) in silicate-based solutions. 99.9% pure Mg alloy was anodized in electrolytes contained mixtures of sodium silicate and sodium fluoride, calcium hydroxide and sodium hydroxide. Scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDX), contact angle (CA), Photoluminescence analysis and immersion tests were performed to assess structural and long-term corrosion properties of the new coating. Biocompatibility and antibacterial potential of the new coating were evaluated using U2OS cell culture and the gram-positive Staphylococcus aureus (S. aureus, strain B 918). PEO provided the formation of a porous oxide layer with relatively high roughness. It was shown that Ca(OH)2 was a crucial compound for oxidation and surface modification of Mg implants, treated with the PEO method. The addition of Ca2+ ions resulted in more intense oxidation of the Mg surface and growth of the oxide layer with a higher active surface area. Cell culture experiments demonstrated appropriate cell adhesion to all investigated coatings with a significantly better proliferation rate for the samples treated in Ca(OH)2-containing electrolyte. In contrast, NaOH-based electrolyte provided more relevant antibacterial effects but did not support cell proliferation. In conclusion, it should be noted that PEO of Mg alloy in silicate baths containing Ca(OH)2 provided the formation of stable biocompatible oxide coatings that could be used in the development of commercial degradable implants.

scholarly journals SEM and EDS Characterization of Porous Coatings Obtained On Titaniumby Plasma Electrolytic Oxidation in Electrolyte Containing Concentrated Phosphoric Acid with Zinc Nitrate

2017 ◽  
Vol 17 (2) ◽  
pp. 41-54 ◽  
Author(s):  
K. Rokosz ◽  
T. Hryniewicz ◽  
K. Pietrzak ◽  
W. Malorny
Keyword(s):  
Phosphoric Acid ◽  
Plasma Electrolytic Oxidation ◽  
Pure Titanium ◽  
Zinc Nitrate ◽  
Porous Coatings ◽  
Electrolytic Oxidation ◽  
Micro Arc Oxidation ◽  
Plasma Electrolytic ◽  
Peo Coatings

AbstractThe SEM and EDS results of porous coatings formed on pure titanium by Plasma Electrolytic Oxidation (Micro Arc Oxidation) under DC regime of voltage in the electrolytes containing of 500 g zinc nitrate Zn(NO3)2·6H2O in 1000 mL of concentrated phosphoric acid H3PO4at three voltages, i.e. 450 V, 550 V, 650 V for 3 minutes, are presented. The PEO coatings with pores, which have different shapes and the diameters, consist mainly of phosphorus, titanium and zinc. The maximum of zinc-to-phosphorus (Zn/P) ratio was found for treatment at 650 V and it equals 0.43 (wt%) | 0.20 (at%), while the minimum of that coefficient was recorded for the voltage of 450 V and equaling 0.26 (wt%) | 0.12 (at%). Performed studies have shown a possible way to form the porous coatings enriched with zinc by Plasma Electrolytic Oxidation in electrolyte containing concentrated phosphoric acid H3PO4with zinc nitrate Zn(NO3)2·6H2O.

scholarly journals Effects of a Carbon Nanotube Additive on the Corrosion-Resistance and Heat-Dissipation Properties of Plasma Electrolytic Oxidation on AZ31 Magnesium Alloy

Materials ◽  
2018 ◽  
Vol 11 (12) ◽  
pp. 2438 ◽  
Author(s):  
Myungwon Hwang ◽  
Wonsub Chung
Keyword(s):  
Corrosion Resistance ◽  
Carbon Nanotube ◽  
Plasma Electrolytic Oxidation ◽  
Heat Dissipation ◽  
X Ray ◽  
Steady State Method ◽  
Electrolytic Oxidation ◽  
Plasma Electrolytic ◽  
Dissipation Property ◽  
Peo Coatings

Plasma electrolytic oxidation (PEO) coating was obtained on AZ31 Mg alloy using a direct current in a sodium silicate-based electrolyte with and without a carbon nanotube (CNT) additive. The surface morphology and phase composition of the PEO coatings were investigated through field emission scanning electron microscopy (SEM), X-ray diffraction (XRD), and X-ray photoelectron spectroscopy (XPS). The corrosion-resistance properties of the PEO coatings were evaluated using potentiodynamic polarization measurements and electrochemical impedance spectroscopy (EIS) in a 3.5 wt.% NaCl solution. Furthermore, the heat-dissipation property was evaluated by a heat-flux measurement setup using a modified steady-state method and Fourier transform infrared spectroscopy (FT-IR). The results demonstrate that, by increasing the concentration of CNT additive in the electrolyte, the micropores and cracks of the PEO coatings are greatly decreased. In addition, the anticorrosion performance of the PEO coatings that incorporated CNT for the protection of the Mg substrate was improved. Finally, the coating’s heat-dissipation property was improved by the incorporation of CNT with high thermal conductivity and high thermal emissivity.

scholarly journals Nanodesigned coatings obtained by plasma electrolytic oxidation of titanium implant and their cytotoxicity

2021 ◽  
Vol 19 ◽  
pp. 228080001882225
Author(s):  
Marko Magić ◽  
Božana Čolović ◽  
Saša Vasilijić ◽  
Nenad Tadić ◽  
Stevan Stojadinović ◽  
...  
Keyword(s):  
Plasma Electrolytic Oxidation ◽  
Cell Attachment ◽  
Titanium Implant ◽  
Ionic Exchange ◽  
X Ray Diffraction ◽  
X Ray ◽  
Electrolytic Oxidation ◽  
Plasma Electrolytic ◽  
The Given ◽  
Scanning Electron

The titanium implant was treated with plasma electrolytic oxidation and subsequent ionic exchange and thermal treatment in order to obtain bioactive layer consisting of titanium oxide, calcium and sodium titanates and hydroxyapatite, as confirmed by X-ray diffraction (XRD). Scanning electron microscopy (SEM) revealed that the given method, besides corresponding phase composition, enables suitable nanotopology for cell attachment and proliferation. Cytotoxicity investigations by MTT, LDH and propidium iodide assays and light microscopy showed that these coatings were not toxic to L929 cells.

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