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a b s t r a c t a r t i c l e i n f o Available online xxxxThe paper reports a change in the morphology of coatings formed galvanostatically on titanium by plasma electrolytic oxidation in phosphoric/sulfuric acid mixtures, and investigated using scanning electron microscopy, X-ray diffraction, and glow discharge optical emission spectroscopy. An initial grooved morphology, containing anatase, is transformed to a more usual porous morphology, which may also contain rutile. The coatings also contain phosphorus species, but comparatively small amounts of sulfur species. The morphological change occurs over a range of cell charge that is strongly dependent on the molar ratio of the acids but weakly dependent on the applied current. With the change in the coating morphology, the efficiency of coating formation reduces and the sparking becomes more localized and intense. Lap shear tests show that the grooved morphology provides a~60% increase in the strength of adhesively bonded joints compared with a porous morphology.

The optimal mechanical properties render magnesium widely used in industrial and biomedical applications. However, magnesium is highly reactive and unstable in aqueous solutions, which can be modulated to increase stability of reactive metals that include the use of alloys or by altering the surface with coatings. Plasma electrolytic oxidation is an efficient and tuneable method to apply a surface coating. By varying the plasma electrolytic oxidation parameters voltage, current density, time and (additives in the) electrolytic solution, the morphology, composition and surface energy of surface coatings are set. In the present study, we evaluated the influence on surface coatings of two solute additives, i.e. hexamethylenetetramine and mannitol, to base solutes silicate and potassium hydroxide. Results from in vitro studies in NaCl demonstrated an improvement in the corrosion resistance. In addition, coatings were obtained by a two-step anodization procedure, firstly anodizing in an electrolyte solution containing sodium fluoride and secondly in an electrolyte solution with hexamethylenetetramine and mannitol, respectively. Results showed that the first layer acts as a protective layer which improves the corrosion resistance in comparison with the samples with a single anodizing step. In conclusion, these coatings are promising candidates to be used in biomedical applications in particular because the components are non-toxic for the body and the rate of degradation of the surface coating is lower than that of pure magnesium.

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Nanotubular structures were generated on the surface of titanium c.p. by anodization technique in an aqueous solution of acetic acid (14% v/v) with different sources of fluoride ion (HF, NaF, NH F). The aim of using these three different compounds is to study the effect of the counterion (H , Na and NH4+) on the morphology, wettability and surface free energy of the modified surface. Nanotubes were generated at 10 and 15 V for each anodizing solution. To further improve surface characteristics, the samples were heat-treated at 600°C for 4 h and at 560°C for 3 h. SEM images revealed the formation of nanotubes in all anodizing conditions, while their diameter increased proportionally to the electric potential. X-ray diffraction and micro-Raman spectroscopy results showed the presence of both anatase and rutile phases, with a higher content of rutile in the coatings obtained using NH F and an applied potential of 10 V. The heat-treatment significantly increased the wettability of the anodic coatings, especially for the coating obtained at 15 V with HF, which showed values < 7 degrees of contact angle. Besides, the nanotubes show a decrease in diameter due to the heat treatment, except for the nanotubes formed in NH F. Depending on their surface properties (e.g. low contact angle and high surface free energy), these coatings potentially have great potential in biomedical applications, sensors devices, and catalytic applications among others. © 2018 Wiley Periodicals, Inc. J Biomed Mater Res Part A: 106A: 1341-1354, 2018.