The construction of gold electrodes using 3 kinds of gold recordable compact discs (CDtrodes) and characterization by electrochemical and spectroscopic techniques are herein reported. Following a surface pretreatment in 0.5 mol L-1 sulfuric acid (H2SO4), the electrochemical experiments were performed in the presence of redox couple ferro/ferricyanide [Fe(CN)6]3-/4-. The immobilization of an oligopeptide bio-inspired by acetylcholinesterase onto the CDtrode was also evaluated. Surface characterization was done by cyclic voltammetry, electrochemical impedance spectroscopy, diffuse reflectance infrared Fourier transform spectroscopy and atomic force microscopy. CDtrodes are known to be of low cost, fast and simple construction. They are suitable for immobilizing biological molecules and could be used as disposable transducer for the construction of biosensors.

The surface intermediates formed on the Mg-La catalyst (molar ratio 1:1) were studied through temperature-programmed desorption (TPD) and diffuse reflectance infrared Fourier transform spectroscopy coupled to mass spectrometry (DRIFTS-MS) using methanol (MeOH) and ethyl acetate (EA) as probe molecules. TPD results showed that the products formed from adsorbed MeOH were hydrogen and formaldehyde, whereas EA produced hydrogen, ethanol, and acetone. DRIFTS-MS of a MeOH and EA mixture results showed that methanol adsorbs as methoxy species on the catalyst surface, and EA adsorbs through the oxygen of carbonyl groups forming ethoxy and acetate species. The reaction of the adsorbed intermediate species resulted in the formation of methane, CO2 gas phase, ethanol, and methyl acetate. Also, methanol adsorbed preferentially on the basic site and EA in a dissociative form. Surface intermediates identification allowed to confirm that the Eley-Rideal type mechanism was predominant on the catalyst surface studied.

The deposition of Diamond-like carbon (DLC) films brings excellent mechanical, chemical, optical and electronic properties to a large range of materials. However, a problem to be overcome is its poor adhesion on metallic substrates. Usually, a silicon layer must be deposited on the surface of metals previous to DLC film deposition. In fact, in our experiments using conventional Magnetron Sputtering (MS) technique for deposition of DLC film on metal surfaces (AISI 304 stainless steel, Al 2024, Ti-6Al-4V), the silicon interlayer was crucial to avoid delamination. However, a combined process using MS and high frequency and moderate energy pulses (2.5kV/6µs/1.25 kHz), was successful to grow DLC film without the interlayer. Additionally, by monitoring the stress and the thickness in silicon samples after the processes, it was possible to correlate the conditions of operation with such characteristics. Stress measurements carried out by a profilometer and calculated by Stoney's equation varied from 2 GPa to 10.5 GPa depending on the conditions of operation of the process (pressure, distance source-substrate, frequency, length and intensity of the pulse). The thickness, the composition, the structure and the morphology of DLC coatings deposited in such metallic surfaces were obtained. Tribological and corrosion tests were also performed.

The aim of this study was to determine the effect of the oral environment on the corrosion of dental alloys with different compositions, using electrochemical methods. The corrosion rates were obtained from the current-potential curves and electrochemical impedance spectroscopy (EIS). The effect of artificial saliva on the corrosion of dental alloys was dependent on alloy composition. Dissolution of the ions occurred in all tested dental alloys and the results were strongly dependent on the general alloy composition. Regarding the alloys containing nickel, the Ni-Cr and Ni-Cr-Ti alloys released 0.62 mg/L of Ni on average, while the Co-Cr dental alloy released ions between 0.01 and 0.03 mg/L of Co and Cr, respectively.The open-circuit potential stabilized at a higher level with lower deviation (standard deviation: Ni-Cr-6Ti = 32 mV/SCE and Co-Cr = 54 mV/SCE). The potenciodynamic curves of the dental alloys showed that the Ni-based dental alloy with >70 wt% of Ni had a similar curve and the Co-Cr dental alloy showed a low current density and hence a high resistance to corrosion compared with the Ni-based dental alloys. Some changes in microstructure were observed and this fact influenced the corrosion behavior for the alloys. The lower corrosion resistance also led to greater release of nickel ions to the medium. The quantity of Co ions released from the Co-Cr-Mo alloy was relatively small in the solutions. In addition, the quantity of Cr ions released into the artificial saliva from the Co-Cr alloy was lower than Cr release from the Ni-based dental alloys.

Abstract In order to evaluate its application as a dental prosthesis material, a CoCrW alloy was subjected to in vitro cytotoxicity test, surface characterization and electrochemical studies performed in artificial saliva and 0.15 mol.L-1 NaCl medium. The used techniques were: anodic polarization curves, chronoamperometric measurements, electrochemical impedance spectroscopy (EIS), scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDS) analysis and X-ray photoelectron spectroscopy (XPS). Cytotoxicity test was also performed. The electrochemical behavior of CoCrW alloy was compared in both studied media, from corrosion potential (Ecorr) to a 600 mV anodic overvoltage. From the electrochemical measurements it was observed that the CoCrW alloy in both media presents only generalized corrosion. SEM and EDS analysis showed that the alloy presents carbide niobium and silicon and manganese oxides as nonmetallic inclusions. XPS results indicated that cobalt does not significantly contribute to the passivating film formation. Cytotoxicity test showed no cytotoxic character of CoCrW alloy. These results suggest that the CoCrW alloy can be used as biomaterial to be applied as prosthesis in dental implants.

Modifications in texture and surface chemistry are commonly used to increase the biologic response to implants. We evaluated the influence of five different acid etching treatments on the chemical and topographical superficial characteristics of cpTi grade IV discs (test groups). One group of samples were only polished (control group). The samples were analyzed by electron microscopy (SEM, EDS), atomic force microscopy, and grazing incidence XRD. The acid etching treatments which produced higher values for the amplitude roughness parameters showed a combination of strong acids (HF and HCl/H2SO4) at high concentrations, with a relatively high temperature (≥ 60 °C) for a considerable time (≥ 60 min). Titanium and oxygen were the only elements detected by EDS on the surface in all groups, whereas titanium hydride was detected when the samples were analyzed by GIXRD. Only the group subjected to thermal treatment showed presence of rutile phase on the surface.

AbstractWe evaluated the influence of the etching time and temperature of an acid solution (HCl/H2SO4) on the chemical and topographical superficial characteristics of cpTi grade IV. Samples were analyzed by electron microscopy, interferometry, and grazing incidence XRD. The surfaces kept the irregularity aspect when submitted to the same etching temperature. On the other hand, the irregularities increased in size and depth with increasing etching time. The etching treatments that produced higher values for roughness parameters showed a combination of high temperature for a longer etching time. Some treatments produced very large irregularities, with a brittle surface in some regions. According to statistical correlation, the temperature made the strongest contribution in the variance of the mean values of the surface roughness parameters when compared to the etching time. Titanium and oxygen were the only elements on the surface in all groups. All test group samples showed the presence of titanium hydride.

Ti-6Al-4V alloy is employed in implants because of its good mechanical strength, excellent biocompatibility, and good resistance to corrosion in biological environments. Herein, a composite (HAp-TiO2, 50% by volume of both components) coating surface employing Ti-6Al-4V was characterized. Samples were analyzed post fabrication and post heat treatment to analyze the coating recrystallization, phases, crystallinity, porosity, and roughness. The coating showed rutile crystalline and amorphous Hap phases with crystallinity, porosity, and roughness of 55.6%, 13.6 ± 1.0%, and 4.2 ± 0.6 µm; whereas, after heat treatment, it showed a rutile hydroxyapatite phase and β-TCP with values 75.6%, 13.9 ± 1.9%, and 3.8 ± 0.2 µm, respectively. The composite exhibited 874 ± 26 HV100 hardness and 30 ± 2 MPa adhesion strength after heat treatment, which agree with previously reported data on other bioactive coatings. Therefore, this composite becomes much more crystalline after heating at 750 °C for 1 h.

The conditions of chemical synthesis can be crucial for polymerization of styrene in such a way that it can be produced latex beads at nanometric range (ϕ < 400nm). In this work, it will be analyzed how the absence of N2 and surfactant will result in colloidal particles with high affinity to agglomerate forming two kinds of nanostructured assemblies: colloidal crystals and nanowires. Four syntheses were realized and four parameters were changed: temperature, impeller speed, and initiator and styrene concentrations. The dispersion was filtered and coated on glass slides by evaporation induced self-assembly (EISA) process. Morphology and topography were observed at Scanning Electron Microscopy (SEM) and Atomic Force Microscope (AFM) respectively. They show how the synthesis conditions play a vital a role on the formation of self assembly nanostructures that can be applied as templates for sensors and biomaterials devices.

This paper presents insights into surfaces properties of sputter-deposited titania modified with bisphosphonates, including zeta potential measurements in a pH range. Functionalization was investigated through simulation and experimental approaches to model the adsorbate and evaluate structure-response relationships. Molecules of etidronic, alendronic, and risedronic acids were investigated through density functional theory. The molecules vary their reactivity through similar structures considering different scenarios. X-ray photoelectron spectroscopy of titania/BP systems demonstrated that functionalization occurs in a short time and resulted in a predominantly “side-on” adsorbate configuration after two hours of immersion. Zeta potential showed the predominancy of negative charges deprotonated free phosphonates. Water contact angle demonstrated that titania surfaces are hydrophilic after overnight functionalization. Atomic force measurements of bisphosphonates layers suggested that the molecular anions follow the surface topography, unchanging the surface roughness.