High-resolution characterization of the diffusion of light chemical elements in metallic components by scanning microwave microscopy

International audienceAn original sub-surface, high spatial resolution tomographic technique based on scanning microwave microscopy (SMM) is used to visualize in-depth materials with different chemical compositions. A significant phase difference in SMM between aluminum and chromium buried patterns has been observed. Moreover this technique was used to characterize a solid solution of a light chemical element (oxygen) in a metal lattice (zirconium). The large solubility of the oxygen in zirconium leads to modifications of the properties of the solid solution that can be measured by the phase shift signal in the SMM technique. The signal obtained in cross-section of an oxidized Zr sample shows the excellent agreement between phase shift profiles measured at different depths. Such a profile can reveal the length of diffusion of the oxygen in zirconium under the surface. The comparison with the oxygen concentration measured by nuclear reaction analysis shows excellent agreement in terms of length of diffusion and spatial distribution of the oxygen. A rapid calibration shows a linear dependence between the phase shift and the oxygen concentration. The SMM method opens up new possibilities for indirect measurements of the oxygen concentration dissolved in the metal lattic

High temperature oxidation resistance and microstructure of laser-shock peened Ti-Beta-21S

Improving the high temperature (HT) resistance of titanium alloys is currently a technological challenge for extending their use in aerospace engines. Ti-Beta-21S is a metastable β titanium alloy specifically designed for high temperature applications up to 593 °C. We report the effect of a surface treatment by laser-shock peening (LSP) on the high temperature behavior of Ti-Beta-21S in order to increase further its maximum service temperature. The oxidation kinetics at 700 °C for duration up to 3000 h showed that the LSP treatment increases the oxidation resistance of Ti-Beta-21S. The effects of the LSP treatment on the alloy microstructure, its evolution at high temperature and the diffusion of light atmospheric elements (oxygen and nitrogen) are also reported

Effect of laser shock peening on the high temperature oxidation resistance of titanium

The effect of laser shock peening on the high temperature oxidation resistance of commercial pure titanium at high temperature (700 °C) was studied in long-time (3000 h) exposure under dry air. A reduction of the gain mass by a factor 4 was found for laser-shock peened (LSP) samples compared to untreated titanium, which supports the interest of laser-shock treatment for the improvement of high temperature resistance. Short-durations (10 h and 100 h) oxidation experiments, devoted to investigate the influence of the LSP treatment on the first stages of the oxidation process, were also carried out by TGA. Several techniques as scanning electron microscopy, hardness and roughness measurements, X-ray diffraction and X-ray photoelectron spectrometry, micro-Raman spectroscopy, nuclear reaction analysis and electron backscattered diffraction were used to characterize the sample after laser treatment and oxidations. The formation of a continuous nitrogen-rich layer between the oxide layer and the α-case area in LSP samples appears to be the key factor to explain the reduction of oxygen diffusion, and thus the improvement of the oxidation resistance of laser shocked titanium. Moreover, the grain-texture of LSP samples after oxidation can also explain the improvement of the high temperature oxidation resistance after long times exposures

Mechano-Chemical Aspects of High Temperature Oxidation: A Mesoscopic Model Applied to Zirconium Alloys

International audienc

Coupled Modelling of ZrO2/α-Zr(O) Layers Growth under Thermal and Mechanical Gradients

The oxidation process of a nuclear reactor fuel rod clad made of zirconium is simulated. It is assumed that the oxygen is transported by anionic diffusion in the zirconia layer (ZrO2). Part of this oxygen reacts at the interface between the zirconia layer and the metal, while the rest diffuses in the oxygen-enriched metal volume (a-Zr(O)) to the core of the metal by an interstitial mechanism. The model is based on the thermodynamics of irreversible processes and takes into account the influence of driving forces on the oxygen migration in the metal such as the oxygen concentration gradient, the temperature gradient [1] and the mechanical stress gradient [2]. The growth of both ZrO2 and a-Zr(O) layers are simulated using the finite element software CAST3M. This model has been applied on an axisymmetric geometry by imposing a heat flow on the fuel side and a constant temperature on the waterside of the clad. The differences obtained in the inner and outer sides of the nuclear clad concerning the oxidation kinetics and oxygen distribution are related to some coupling parameters. Several values of those parameters are used in the simulations to highlight their influence on the oxidation behavior. Thus, we show that negative values for the heat of transport, which relates the gradient of ocncentration and the gradient of temperature, give coherent results with experimental observations on oxidation kinetics for both sides of the clad

An empirical method to determine the free surface energy of solids at different deformations and temperature regimes : An application to Al.

We have performed molecular dynamics (MD) simulations using the three low index surfaces of Al to determine the variation of the surface energy as a function of deformation and temperature. We have also developed an empirical formulation for the surface free energy as a function of deformation. The observed difference between the numerical and analytical results has led us to divide the deformation into a mechanical and a thermal contribution. From this observation, we have obtained an expression for the surface free energy placing the temperature dependence on the bulk and surface elastic constants. Our simulations permitted us to analyze the multilayer relaxation for the particular surfaces studied. Namely, we found the first atomic layer of the Al(1 00) surface to be in slight contraction, an alternation between contraction and expansion in the first atomic layers of the Al(110) surface and slight expansion in the first atomic layer of the Al(1 11) surface

The chemical constitution and biocompatibility of accelerated Portland cement for endodontic use

Aim To evaluate the biocompatibility of mineral trioxide aggregate and accelerated Portland cement and their eluants by assessing cell metabolic function and proliferation. Methodology The chemical constitution of grey and white Portland cement, grey and white mineral trioxide aggregate (MTA) and accelerated Portland cement produced by excluding gypsum from the manufacturing process (Aalborg White) was determined using both energy dispersive analysis with X-ray and X-ray diffraction analysis. Biocompatibility of the materials was assessed using a direct test method where cell proliferation was measured quantitatively using Alamar Blue TM dye and an indirect test method where cells were grown on material elutions and cell proliferation was assessed using methyltetrazolium assay as recommended by the International standard guidelines, ISO 10993-Part 5 for in vitro testing. Results The chemical constitution of all the materials tested was similar. Indirect studies of the eluants showed an increase in cell activity after 24 h compared with the control in culture medium (P < 0.05). Direct cell contact with the cements resulted in a fall in cell viability for all time points studied (P < 0.001). Conclusions Biocompatibility testing of the cement eluants showed the presence of no toxic leachables from the grey or white MTA, and that the addition of bismuth oxide to the accelerated Portland cement did not interfere with biocompatibility. The new accelerated Portland cement showed similar results. Cell growth was poor when seeded in direct contact with the test cements. However, the elution made up of calcium hydroxide produced during the hydration reaction was shown to induce cell proliferation

An empirical model for free surface energy of strained solids at different temperature regimes.

We have developed an empirical formulation, based on the elastic theory, to calculate the variation of the surface free energy when a crystal is strained in the elastic regime. The model permits to obtain the variation of the surface energy at different strains and temperatures when are known the thermal dependence on the bulk and surface elastic constants. Molecular dynamics (MD) simulations were performed using the three low index surfaces of Al, to validate the accuracy of the model. The comparison between the empirical model and the MD simulations shows a good agreement for temperatures ranging between 0 and 900 K, and for deformation between 2% and 2%