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SEM, EDS, and XPS characterization of coatings obtained on titanium during AC plasma electrolytic process enriched in magnesium

Rokosz K., Hryniewicz T., Raaen S., Matýsek D., Dudek Ł., Pietrzak K.

Advances in Materials Science

2018

Vol. 18, nr 3(57)

68--78

Plasma Electrolytic Oxidation (PEO) known also as Micro Arc Oxidation (MAO) process is widely used to fabricate porous coatings on titanium and its alloys mainly in water- and acid-based solutions to different applications, e.g. in biomaterials, catalysts, and sensors. In the present paper, the SEM, EDS, and XPS results of porous coatings obtained by PEO treatment on titanium in electrolytes based on concentrated phosphoric H3PO4 acid with calcium nitrate tetrahydrate Ca(NO3)2·4H2O, or magnesium nitrate hexahydrate Mg(NO3)2·6H2O, or zinc nitrate hexahydrate Zn(NO3)2·6H2O for 3 minutes at 200 Vpp (peak to peak) with frequency of 50 Hz, are presented. Based on EDS results, the Ca/P, Mg/P, and Zn/P ratios, which equal to 0.95, 0.176, and 0.231, respectively, were found out. The XPS studies of the top 10 nm of the porous layer clearly indicate that it contains mainly phosphates (PO4 3− and/or HPO4 2− and/or H2PO4 −, and/or P2O7 4−) with titanium (Ti4+) and calcium (Ca2+) or magnesium (Mg2+), or zinc (Zn2+).

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

Rokosz K., Hryniewicz T., Pietrzak K., Sadlak P., Valíček J.

Advances in Materials Science

2017

Vol. 17, nr 4(54)

55--67

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.