Methods for Calibrating the Electrochemical Quartz Crystal Microbalance: Frequency to Mass and Compensation for Viscous Load

The main output from an Electrochemical Quartz Crystal Microbalance is a frequency shift. This note describes how to separate the mass- and viscous load contributions to this shift by a calibration procedure. The mass calibration is made by electroplating from a copper sulfate solution in ethanol/water with 100% current efficiency. An estimate of viscous load is obtained by measuring the energy dissipation and is related to frequency change using the Kanazawa–Gordon equation. Two approaches are discussed: either by performing calibration experiments in a series of water–glycerol mixtures or by following oscillations in frequency and dissipation by collecting data during the stabilization phase of the experiment

Modeling Current Transients in a Reciprocal Motion Tribocorrosion Experiment

Tribocorrosion of passivating metals is a dynamic phenomenon causing degradation of materials by a combination of mechanical wear and electrochemical dissolution. The mechanical action typically produces a local removal of particles, metal as well as oxides, resulting in an exposure of the metal surface and is followed by a repassivation process, of which the time-dependent current response is a direct measure. Kinetics for interface-limited film growth were used to find an analytical expression for the current transients, including the conductivity of the electrolyte as well as the contribution from the confined geometry within the mechanical contact. The solution gave a good experimental fit to a series of experiments with a range of electrolyte conductivities, and also to correlate well with values obtained using electrochemical impedance spectroscopy. Parameters from the rubbing experiment were used to calculate curves that compared well with passivation transients recorded on a bare metal surface for the same electrolyte series. The evaluation procedure made it possible to assess the relative resistance contributions from the growing passive film, the confined mechanical contact geometry, and the electrolyte

Early Precipitation Stages of Sigma Phase in Alloy 28 Studied with Scanning Electron Microscopy and Atom Probe Tomography

This study deals with early stages of sigma phase growth in a high end austenitic stainless steel - Alloy 28 (EN 1.4563/UNS N08028). Its precipitation kinetics was followed by a series of heat treatments at 800 degrees C for holding times up to 30 000 s. The samples were studied with high resolution scanning electron microscopy and atom probe tomography. Detailed image analysis of the micrographs made it possible to quantify the growth rate of the precipitates. It was shown that diffusion limited growth along grain boundaries was about 15 times faster than growth perpendicular to a grain face. By combining the image data with quantitative chemical analysis of the phase boundaries, it was possible to estimate diffusion coefficients in the lattice and in the grain boundaries; grain boundary diffusion coefficients were about 250 times those of the lattice

Detergent Induced Removal of b-Lactoglobulin from Stainless Steel Surfaces at Influenced by Surface Pretreatment

The adsorption of β-lactoglobulin to stainless steel and its subsequent removal were followed using in situ null ellipsometry. The influence of the surface pretreatment on the protein removal by the surfactant SDS and by sodium hydroxide was studied. All surfaces were precleaned in strongly alkaline solution. Some surfaces received no further pretreatment, while others were either passivated in nitric acid or plasma-cleaned prior to experiments. Stainless steel surfaces subjected to different surface pretreatments showed considerable differences in cleaning behavior. Cleaning, using NaOH, of surfaces which had been precleaned with alkali only or with plasma resulted in practically complete β-lactoglobulin removal. In contrast, appreciable amounts of protein remained on passivated stainless steel. Protein removal by SDS was limited and comparable for all three surface pretreatments investigated. Only minor effects on the protein adsorption tendency were observed. The amounts of β-lactoglobulin adsorbed tended to be somewhat lower on the passivated surfaces

The Electrochemical Behavior of Ti in Human Synovial Fluids

In this study, we report results of the interaction of titanium (Ti) with human synovial fluids. A wide palette of electrochemical techniques was used, including open circuit potential, potentiodynamic methods, and electrochemical impedance. After the electrochemical testing, selected surfaces were analyzed using Auger Electron Spectroscopy to provide laterally resolved information on surface chemistry. For comparison purposes, similar tests were conducted in a series of simulated body fluids. This study shows that compared to the tested simulated body fluids, synovial liquids show a large patient variability up to one order of magnitude for some crucial electrochemical parameters such as corrosion current density. The electrochemical behavior of Ti exposed to human synovial fluids seems to be controlled by the interaction with organic molecules rather than with reactive oxygen species

The Electrochemical Behavior of Ti in Human Synovial Fluids

In this study, we report results of the interaction of titanium (Ti) with human synovial fluids. A wide palette of electrochemical techniques was used, including open circuit potential, potentiodynamic methods, and electrochemical impedance. After the electrochemical testing, selected surfaces were analyzed using Auger Electron Spectroscopy to provide laterally resolved information on surface chemistry. For comparison purposes, similar tests were conducted in a series of simulated body fluids. This study shows that compared to the tested simulated body fluids, synovial liquids show a large patient variability up to one order of magnitude for some crucial electrochemical parameters such as corrosion current density. The electrochemical behavior of Ti exposed to human synovial fluids seems to be controlled by the interaction with organic molecules rather than with reactive oxygen species