Juan G. Castaño

Osseointegration improvement by plasma electrolytic oxidation of modified titanium alloys surfaces

Titanium (Ti) is a material frequently used in orthopedic applications, due to its good mechanical properties and high corrosion resistance. However, formation of a non-adherent fibrous tissue between material and bone drastically could affect the osseointegration process and, therefore, the mechanical stability of the implant. Modifications of topography and configuration of the tissue/material interface is one of the mechanisms to improve that process by manipulating parameters such as morphology and roughness. There are different techniques that can be used to modify the titanium surface; plasma electrolytic oxidation (PEO) is one of those alternatives, which consists of obtaining porous anodic coatings by controlling parameters such as voltage, current, anodizing solution and time of the reaction. From all of the above factors, and based on previous studies that demonstrated that bone cells sense substrates features to grow new tissue, in this work commercially pure Ti (c.p Ti) and Ti6Al4V alloy samples were modified at their surface by PEO in different anodizing solutions composed of H2SO4 and H3PO4 mixtures. Treated surfaces were characterized and used as platforms to grow osteoblasts; subsequently, cell behavior parameters like adhesion, proliferation and differentiation were also studied. Although the results showed no significant differences in proliferation, differentiation and cell biological activity, overall results showed an important influence of topography of the modified surfaces compared with polished untreated surfaces. Finally, this study offers an alternative protocol to modify surfaces of Ti and their alloys in a controlled and reproducible way in which biocompatibility of the material is not compromised and osseointegration would be improved.

CHARACTERIZATION OF DEPOSITS FORMED IN A WATER DISTRIBUTION SYSTEM

The development of unwanted deposits in any water distribution system is unavoidable under standard conditions. Knowing the composition of such deposits will help to establish the causes of deposit formation and consequently to be able to keep water quality as high as possible. This paper presents the results of an extensive study of deposits found in a water distribution system of a tropical city. Characterization of materials collected across the system was made by infrared spectroscopy (IR), X ray diffraction (XRD), energy dispersive spectroscopy (EDS) and scanning electron microscopy (SEM). Analysis of the samples taken at several sites of the system reveals the presence of three predominant deposits: a brown coloured deposit, tubercles and white deposits. Aluminosilicates and humic acids were found to be main constituents in brown deposits. Tubercles were mostly mixtures of magnetite, goethite and in some cases lepidocrocite. White deposits were formed by calcite, aluminosilicates and quartz. Organic matter as volatile solids were 14.0 ± 5.0% for brown deposits and 11.2 ± 2.0% for tubercles.

Formation of protective anodic oxides on aluminium by low voltage anodising in sulphuric acid with cerium nitrate and tartaric acid additions

Abstract The effects of the anodising potential and of the combined addition of tartaric acid and cerium nitrate to a sulphuric acid anodising bath on the corrosion behaviour of high purity aluminium and on AA2024T3 aerospace aluminium alloy have been systematically investigated. It is found that the anodising potential is critical in determining the anticorrosion performance; lower potential generates finer pores that provide enhanced corrosion protection compared with the larger pores generated at higher potentials. At both anodising potentials, the addition of cerium nitrate alone to the sulphuric acid bath does not increase significantly the anticorrosion performance. Conversely, the addition of tartaric acid alone is generally beneficial. Finally, when cerium nitrate is added in combination with tartaric acid a further improvement of the corrosion resistance is observed.

Modification of titanium alloys surface properties by plasma electrolytic oxidation (PEO) and influence on biological response

Surface characteristics can mediate biological interaction improving or affecting the tissue integration after implantation of a biomaterial. Features such as topography, wettability, surface energy and chemistry can be key determinants for interactions between cells and materials. Plasma electrolytic oxidation (PEO) is a technique used to control this kind of parameters by the addition of chemical species and the production of different morphologies on the surfaces of titanium and its alloys. With the purpose to improve the biological response, surfaces of c.p titanium and Ti6Al4V were modified by using PEO. Different electrolytes, voltages, current densities and anodizing times were tested in order to obtain surfaces with different characteristics. The obtained materials were characterized by different techniques such as X-ray diffraction (XRD), scanning electron microscopy (SEM) and glow discharge optical emission spectroscopy (GDOES). Wettability of the obtained surfaces were measured and the corresponding surface energies were calculated. Superhydrophilic surfaces with contact angles of about 0 degrees were obtained without any other treatment but PEO and this condition in some cases remains stable after several weeks of anodizing; crystal phase composition (anatase—rutile) of the anodic surface appears to be critical for obtaining this property. Finally, in order to verify the biological effect of these surfaces, osteoblast were seeded on the samples. It was found that cell behavior improves as SFE (surface free energy) and coating porosity increases whereas it is affected negatively by roughness.Graphical abstractTechniques for surface modification allow changes in the coatings such as surface energy, roughness and porosity. As a consequence of this, biological response can be altered. In this paper, surfaces of c.p Ti and Ti6Al4V were modified by using plasma electrolytic oxidation (PEO) in order to accelerate the cell adhesion process.

Effect of heat treatment on the tribological properties of Nickel-Boron electroless coating

Nickel-Boron autocatalytic coatings are widely used in several industries to improve mechanical properties of materials such as hardness and wear resistance. Tribological properties were evaluated in Ni-B autocatalytic coatings deposited on AISI/SAE 1018 carbon steel before and after a heat treatment at 450 °C for one hour. Tribological tests were carried out by dry sliding, using a load of 5 N and a sliding speed of 0.012 m/s, in a homemade ball-on-disk tribometer, which followed ASTM G99 standard. According to the tribological evaluation, the heat treatments applied to Ni-B coatings improved their tribological performance. This research corroborates that by applying an adequate heat treatment, hardness and wear resistance of Ni-B coatings can be improved significantly.

Formation of nanotubular TiO2 structures with varied surface characteristics for biomaterial applications

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, NH4 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 NH4 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 NH4 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.

High Resolution Morphological Changes of Cu, Ni, Al, and Au Surfaces Due to Atmospheric Corrosion

As atmospheric corrosion of electrical contacts is a common cause of failure in electronics industry and at the same time miniaturization is a requirement in any modern electronic device, it is important to study the effects of corrosion in the surface morphology of metals widely used in that industry sector, such as gold, copper, nickel, and aluminium. Here, atomic force microscopy (AFM) has been used with that purpose, analysing flat surfaces of those metals both before and after exposure by several weeks to the effects of a contaminated atmosphere containing both NO2 and SO2 at constant temperature and humidity. Results indicate all metals suffered changes both in surface morphology and roughness. AFM phase mode images also indicated the occurrence of different species on the Ni and Cu surfaces after 11 weeks of exposure. Evidence of defects due to the corrosion attack was only observed for Ni.

Electrochemical impedance study for modeling the anticorrosive performance of coatings based on accelerated tests and outdoor exposures

In this study, the atmospheric corrosive protection characteristics of four organic coatings were modeled based on the evolution of low-frequency impedance (|Z|ω→0) over time when subjected to accelerated tests and outdoor exposures. Environmental characteristics such as the time of wetness, chloride and sulfate depositions, and ultraviolet radiation were defined as explanatory variables. The results obtained helped to establish a relationship between |Z|ω→0, acquired from electrochemical impedance spectra, and the explanatory variables. An adjustment factor was calculated for each coating against the most aggressive natural exposure, resulting in a good prediction of |Z|ω→0 and the performance of the coatings for other outdoor tests.

Anodic oxidation of titanium for implants and prosthesis: processing, characterization and potential improvement of osteointegration

Among all biomaterials used for bone replacement, it is recognized that both commercially pure titanium (Ti c.p.) and Ti6Al4V alloy are the materials that show the best in vivo performance due to their excellent balance between mechanical, physical-chemical and biofunctional properties. However, one of its main drawbacks, which compromise the service reliability of the implants and its osteointegration capacity, is the thin film of fibrous tissue around the implant due to the bioinert behaviour of titanium. One of the alternatives more studied to improve the titanium osteointegration is the surface modification through the control of the roughness parameters within a specific range which is recognized that improve the osteoblasts adhesion. In this work is investigated the influence of different electrochemical processing conditions for surface modification of c.p. Ti, in their microstructural, morphological, topographical and mechanical properties, as well as in their biological behaviour. The electrochemical anodizing treatment was performed by using different electrolytes based on phosphoric acid (H3PO4), sulphuric acid (H2SO4) with a fluoride salt; and the Focused Ion Beam (FIB) technique, normally named as Nanolab, was used for the microstructural, chemical and morphological characterization, as well as the confocal laser microscopy technique which also served for roughness measurements. The mechanical response of the anodic layers was evaluated through the using of a scratch tester which showed the critical loads for the coating damages. The characterization results showed that both, concentrations and electrolyte species, clearly influenced the morphological and topographical features, as well as the chemical composition of the anodic layer. By using the FIB was possible to detect nanopores within both the surface and the bulk of the coating. Some of the conditions generated a very special coating morphology which promoted a better osteoblasts adhesion. Contrary to what it was a priory expected, all anodic coatings showed high critical loads for damages during scratch test, despite their high porosity, which could be related with some defects coalescence mechanism that allows dissipating the high stress concentration applied during the test.

Obtención y evaluación de recubrimientos ni-p modificados con magnetitas sintetizadas en presencia de al y ce

Se depositaron peliculas Ni-P modificadas con magnetitas puras y sintetizadas en presencia de Al y Ce. El oxido utilizado fue obtenido por via hidrotermal y en presencia de cationes Al y Ce. Los recubrimientos obtenidos fueron preparados mediante electroless plating y por deposicion simultanea de Ni-P y Fe3O4. La morfologia de los recubrimientos fue estudiada mediante microscopia electronica de barrido. La resistencia a la corrosion de las peliculas Ni-P modificadas con magnetita fue evaluada mediante espectroscopia de impedancia electroquimica, donde las peliculas compuestas exhibieron un mejor comportamiento.