Modification of niobium surfaces using plasma electrolytic oxidation in silicate solutions

Herein, a study of the plasma electrolytic oxidation (PEO) of niobium in an anodising bath composed of potassium silicate (K2SiO3) and potassium hydroxide (KOH) is reported. The effects of the K2SiO3 concentration in the bath and the process voltage on the characteristics of the obtained oxide layers were assessed. Compact, barrier-type oxide layers were obtained when the process voltage did not exceed the breakdown potential of the oxide layer. When this threshold was breached, the morphology of the oxide layer changed markedly, which is typical of PEO. A significant amount of silicon, in the form of amorphous silica, was incorporated into the oxide coatings under these conditions compared with the amount obtained with conventional anodising. This surface modification technique led to an improvement in the corrosion resistance of niobium in Ringer’s solution, regardless of the imposed process conditions

Formation of a Bacteriostatic Surface on ZrNb Alloy via Anodization in a Solution Containing Cu Nanoparticles

High strength, excellent corrosion resistance, high biocompatibility, osseointegration ability, and low bacteria adhesion are critical properties of metal implants. Additionally, the implant surface plays a critical role as the cell and bacteria host, and the development of a simultaneously antibacterial and biocompatible implant is still a crucial challenge. Copper nanoparticles (CuNPs) could be a promising alternative to silver in antibacterial surface engineering due to low cell toxicity. In our study, we assessed the biocompatibility and antibacterial properties of a PEO (plasma electrolytic oxidation) coating incorporated with CuNPs (Cu nanoparticles). The structural and chemical parameters of the CuNP and PEO coating were studied with TEM/SEM (Transmission Electron Microscopy/Scanning Electron Microscopy), EDX (Energy-Dispersive X-ray Dpectroscopy), and XRD (X-ray Diffraction) methods. Cell toxicity and bacteria adhesion tests were used to prove the surface safety and antibacterial properties. We can conclude that PEO on a ZrNb alloy in Ca–P solution with CuNPs formed a stable ceramic layer incorporated with Cu nanoparticles. The new surface provided better osteoblast adhesion in all time-points compared with the nontreated metal and showed medium grade antibacterial activities. PEO at 450 V provided better antibacterial properties that are recommended for further investigation

In Vitro Biological Characterization of Silver-Doped Anodic Oxide Coating on Titanium

Despite the high biocompatibility and clinical effectiveness of Ti-based implants, surface functionalization (with complex osteointegrative/antibacterial strategies) is still required. To enhance the dental implant surface and to provide additional osteoinductive and antibacterial properties, plasma electrolytic oxidation of a pure Ti was performed using a nitrilotriacetic acid (NTA)-based Ag nanoparticles (AgNP)-loaded calcium–phosphate solution. Chemical and structural properties of the surface-modified titanium were assessed using scanning electron microscopy (SEM) with energy dispersive X-ray (EDX) and contact angle measurement. A bacterial adhesion test and cell culture biocompatibility with collagen production were performed to evaluate biological effectiveness of the Ti after the plasma electrolytic process. The NTA-based calcium–phosphate solution with Ag nanoparticles (AgNPs) can provide formation of a thick, porous plasma electrolytic oxidation (PEO) layer enriched in silver oxide. Voltage elevation leads to increased porosity and a hydrophilic nature of the newly formed ceramic coating. The silver-enriched PEO layer exhibits an effective antibacterial effect with high biocompatibility and increased collagen production that could be an effective complex strategy for dental and orthopedic implant development

PEO layers on Mg-based metallic glass to control hydrogen evolution rate

The amorphous Mg-based alloys may be used as metallic biomaterials for resorbable orthopedic implants. The Mg-Zn-Ca metallic glasses demonstrate variable in time degradation rate in simulated body fluid. In this work the Mg66Zn30Ca4 alloy was chosen as a substrate for coatings. This paper reports on the surface modification of a Mg66Zn30Ca4 metallic glass by plasma electrolytic oxidation (PEO). The structure characterization of uncoated Mg66Zn30Ca4 alloy was performed by using TEMand XRD method. The immersion tests of coated and uncoated Mg66Zn30Ca4 alloy were carried out in Ringer’s solutionat 37°C. The volume of released hydrogen by immersion tests was determined. The coatings structure and chemical composition after immersion tests by SEM/EDS were studied. Based on SEM images of surface structure samples, immersion tests results and hydrogen evolution measurement was proposed the course of corrosion process in Ringer’s solution for Mg-based metallic glasses with PEO coating. Results of immersion tests in Ringer’s solution allowed to determine the amount of evolved hydrogen in a function of time for Mg66Zn30Ca4 metallic glass and sample with PEO coating. In comparison to the non-coated Mg66Zn30Ca4 alloy, the sample with PEO layer showed a significantly decreased hydrogen evolution volume

On influence of anodic oxidation on thrombogenicity and bioactivity of the Ti-13Nb- 13Zr alloy

Purpose: This paper reports the results of investigations of the blood response of the modified titanium alloys surfaces. Methods: To enhance biocompatibility of the Ti-13Nb-13Zr alloy, anodisation was performed at 80 and 150 V. The oxidation process was carried out in a solution containing 4 mol dm−3 H3PO4 and 0.59 mol dm−3 Ca(H2PO2)2. Results: The haemolytic activity of the titanium alloy surface was not altered much by the anodisation. The obtained values of the percentage of haemolysis were well below the levels required for the materials intended for blood contact. The clotting time of the blood was similar for the as-ground sample and the sample anodised at 80 V. For the sample anodised at 150 V the clotting time was shorter. The differences between these samples were observed in partial thromboplastin time after activation, prothrombin time and thrombin time, after 24 h. Extracts taken from the samples were not toxic towards the L-929 mouse fibroblast cells. Conclusions: The proposed treatment might be appropriate for the preparation of the modified Ti-13Nb-13Zr surfaces intended for bone reconstruction or cardiovascular implants depending on process parameters

Shaping the Structure and Properties of TiO2-ZnO Oxide Coatings Produced by Plasma Electrolytic Oxidation on Titanium Substrate

У статті наведено результати попередніх досліджень можливості синтезу змішаних покриттів ZnO-TiO2 методом плазмового електрохімічного оксидування (ПЕО). Метою роботи був синтез змішаних покриттів TiO2-ZnO на титановій підкладці з електроліту, що містить наночастинки (НЧ) ZnO, та оцінка параметрів ПЕО на структуру, хімічний склад і властивості отриманих оксидних покриттів. Процес ПЕО здійснювався за різних вольт-амперних режимів з використанням різних сигналів: постійного струму, постійного імпульсу та змінного струму. У даній роботі визначено оптимальні умови процесу ПЕО для отримання добре зчіпних оксидних покриттів з максимально можливим вмістом ZnO. Досліджено структуру та морфологію отриманих оксидних покриттів, комплексно досліджено їх хімічний та фазовий склад (EDX, XRD, XPS та GD-OES). Крім того, оцінювали їх основні оптичні властивості. Показано, що в імпульсному процесі PEO DC можна отримати оксидні покриття, що характеризуються високим ступенем впорядкованості структури, високим вмістом ZnO в оксидному покритті (3,6 ат.%, XPS) і перспективним застосуванням для фотокаталітичних цілей. (3,12 еВ).The paper presents the results of preliminary research on the possibility of synthesizing ZnO-TiO2 mixed coatings by plasma electrochemical oxidation (PEO). The aim of the work was to synthesize TiO2-ZnO mixed coatings on a titanium substrate from an electrolyte containing ZnO nanoparticles (NPs) and to assess the parameters of PEO on the structure, chemical composition, and properties of the obtained oxide coatings. The PEO process was carried out under various current–voltage conditions using different signals: DC, DC pulse, and AC. In this work, optimal conditions for the PEO process were determined to obtain well-adhering oxide coatings with the highest possible content of ZnO. The structure and morphology of the resulting oxide coatings were investigated, and their chemical and phase composition was comprehensively examined (EDX, XRD, XPS, and GD-OES). In addition, their basic optical properties were assessed. It has been shown that in the PEO DC pulse process, it is possible to obtain oxide coatings characterized by a high degree of structure order, high ZnO content in the oxide coating (3.6 at.%, XPS), and prospective applications for photocatalytic purposes (3.12 eV).This research was funded by the Silesian University of Technology, grant number 04/010/BKM23/1071