scholarly journals Fabrication and characterisation of porous, calcium enriched coatings on titanium after plasma electrolytic oxidation under DC regime

2017 ◽  
Vol 17 (4) ◽  
pp. 55-67 ◽  
Author(s):  
K. Rokosz ◽  
T. Hryniewicz ◽  
K. Pietrzak ◽  
P. Sadlak ◽  
J. Valíček

Abstract The purpose of this work is to produce and characterize (chemical composition and roughness parameters) porous coatings enriched in calcium and phosphorus on the titanium (CP Titanium Grade 2) by plasma electrolytic oxidation. As an electrolyte, a mixture of phosphoric acid H3PO4 and calcium nitrate Ca(NO3)2·4H2O was used. Based on obtained EDS and roughness results of PEO coatings, the effect of PEO voltages on the chemical composition and surface roughness of porous coatings was determined. With voltage increasing from 450 V to 650 V, the calcium in PEO coatings obtained in freshly prepared electrolyte was also found to increase. In addition, the Ca/P ratio increased linearly with voltage increasing according to the formula Ca/P = 0.035·U+0.176 (by wt%) and Ca/P = 0.03·U+0.13 (by at%). It was also noticed that the surface roughness increases with the voltage increasing, what is related to the change in coating porosity, i.e. the higher is the surface roughness, the bigger are pores sizes obtained.

2017 ◽  
Vol 17 (2) ◽  
pp. 41-54 ◽  
Author(s):  
K. Rokosz ◽  
T. Hryniewicz ◽  
K. Pietrzak ◽  
W. Malorny

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.


Author(s):  
Krzysztof Rokosz ◽  
Tadeusz Hryniewicz ◽  
Steinar Raaen ◽  
Sofia Gaiaschi ◽  
Patrick Chapon ◽  
...  

In the paper, the effect of voltage increasing (from 500 VDC up to 650 VDC) on the structure and chemical composition of porous coating on titanium made by Plasma Electrolytic Oxidation, is presented. In the present paper, phosphates based coatings enriched with calcium, magnesium, zinc and copper in electrolyte based on 1 L of 85% concentrated H3PO4 with additions of Ca(NO3)2·4H2O, and Mg(NO3)2∙6H2O, and Zn(NO3)2∙6H2O, and Cu(NO3)2∙3H2O, are described. The morphology, chemical and phase composition, are evaluated using SEM, EDS, XRD, XPS, GDOES. Based on all the analyses, it was found out that the PEO coatings are porous and enriched with calcium, magnesium, zinc and copper. They consist mainly of the amorphous phase, which is more visible for higher voltages, and it is correlated with the increasing of the total PEO coating thickness (the higher the voltage, the thicker the PEO coating). However, for 650 VDC an amorphous phase and titanium substrate was also recorded with a signal from Ti2P2O7 crystalline, that was not observed for lower voltages. It was also found out that all the obtained coatings may be divided in three sub-layers, i.e. porous, semiporous, and transition one.


Metals ◽  
2017 ◽  
Vol 7 (9) ◽  
pp. 354 ◽  
Author(s):  
Krzysztof Rokosz ◽  
Tadeusz Hryniewicz ◽  
Sofia Gaiaschi ◽  
Patrick Chapon ◽  
Steinar Raaen ◽  
...  

2016 ◽  
Vol 2016 ◽  
pp. 1-7 ◽  
Author(s):  
Krzysztof Rokosz ◽  
Tadeusz Hryniewicz ◽  
Patrick Chapon ◽  
Steinar Raaen ◽  
Hugo Ricardo Zschommler Sandim

XPS and GDOES characterizations of porous coatings on tantalum after Plasma Electrolytic Oxidation (PEO) at 450 V for 3 minutes in electrolyte containing concentrated (85%) phosphoric acid with calcium nitrate and copper (II) nitrate are described. Based on the obtained data, it may be concluded that the PEO coating consists of tantalum (Ta5+), calcium (Ca2+), copper (Cu2+  and Cu+), and phosphates (PO43-). It has to be pointed out that copper and calcium are distributed throughout the volume. The authors also propose a new model of PEO, based on the derivative of GDOES signals with sputtering time.


Materials ◽  
2018 ◽  
Vol 11 (9) ◽  
pp. 1680 ◽  
Author(s):  
Krzysztof Rokosz ◽  
Tadeusz Hryniewicz ◽  
Sofia Gaiaschi ◽  
Patrick Chapon ◽  
Steinar Raaen ◽  
...  

In this paper, the characteristics of new porous coatings fabricated at three voltages in electrolytes based on H3PO4 with calcium nitrate tetrahydrate, magnesium nitrate hexahydrate, and copper(II) nitrate trihydrate are presented. The SEM, energy dispersive spectroscopy (EDS), glow discharge optical emission spectroscopy (GDOES), X-ray photoelectron spectroscopy (XPS), and XRD techniques for coating identification were used. It was found that the higher the plasma electrolytic oxidation (PEO) (micro arc oxidation (MAO)) voltage, the thicker the porous coating with higher amounts of built-in elements coming from the electrolyte and more amorphous phase with signals from crystalline Ca(H2PO4)2∙H2O and/or Ti(HPO4)2∙H2O. Additionally, the external parts of the obtained porous coatings formed on titanium consisted mainly of Ti4+, Ca2+, Mg2+ and PO43−, HPO42−, H2PO4−, P2O74− as well as Zn2+ or copper Cu+/Cu2+. The surface should be characterized by high biocompatibility, due to the presence of structures based on calcium and phosphates, and have bactericidal properties, due to the presence of zinc and copper ions. Furthermore, the addition of magnesium ions should accelerate the healing of postoperative wounds, which could lead to faster patient recovery.


2016 ◽  
Vol 16 (3) ◽  
pp. 15-25 ◽  
Author(s):  
K. Rokosz ◽  
T. Hryniewicz ◽  
Ł. Dudek ◽  
A. Schütz ◽  
J. Heeg ◽  
...  

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.


Nanomaterials ◽  
2021 ◽  
Vol 11 (6) ◽  
pp. 1375
Author(s):  
Soumya Sikdar ◽  
Pramod V. Menezes ◽  
Raven Maccione ◽  
Timo Jacob ◽  
Pradeep L. Menezes

Plasma electrolytic oxidation (PEO) is a novel surface treatment process to produce thick, dense metal oxide coatings, especially on light metals, primarily to improve their wear and corrosion resistance. The coating manufactured from the PEO process is relatively superior to normal anodic oxidation. It is widely employed in the fields of mechanical, petrochemical, and biomedical industries, to name a few. Several investigations have been carried out to study the coating performance developed through the PEO process in the past. This review attempts to summarize and explain some of the fundamental aspects of the PEO process, mechanism of coating formation, the processing conditions that impact the process, the main characteristics of the process, the microstructures evolved in the coating, the mechanical and tribological properties of the coating, and the influence of environmental conditions on the coating process. Recently, the PEO process has also been employed to produce nanocomposite coatings by incorporating nanoparticles in the electrolyte. This review also narrates some of the recent developments in the field of nanocomposite coatings with examples and their applications. Additionally, some of the applications of the PEO coatings have been demonstrated. Moreover, the significance of the PEO process, its current trends, and its scope of future work are highlighted.


Coatings ◽  
2021 ◽  
Vol 11 (4) ◽  
pp. 401
Author(s):  
Ruzil Farrakhov ◽  
Olga Melnichuk ◽  
Evgeny Parfenov ◽  
Veta Mukaeva ◽  
Arseniy Raab ◽  
...  

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.


Materials ◽  
2018 ◽  
Vol 11 (12) ◽  
pp. 2438 ◽  
Author(s):  
Myungwon Hwang ◽  
Wonsub Chung

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.


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