Papers by Author: René Le Gall

Abstract: It was recently shown [1] that EMPA-WDS (Electron Probe MicroAnalysis by Wavelength Dispersive X-ray Spectroscopy) can be used to detect and to accurately quantify monolayer surface and grain boundary segregation. This paper presents the last developments of this application. It focuses on the measurement of sulphur grain boundary segregation in nickel on fractured surfaces. A special attention was paid to the quantification of the sulphur coverage, taking into account the non-normal incidence of the electron beam on a fracture surface. Sulphur grain boundary segregation kinetics was measured at 750°C in nickel to document the quantitative possibilities of the technique.

Abstract: It was previously reported that fatigue life of some alloys can be dramatically reduced if the grain boundaries contain a high level of impurity segregation before fatigue tests. In this paper the susceptibility of single phase brass samples (90Cu10Zn) to this form of damage is studied. After cold drawing of as cast brass bars, fatigue samples were heat treated at 800°C during 30min to promote recrystallization and impurity segregation at grain boundary. The samples were then tested under high frequency bending fatigue test at 200°C. After cracking, fracture surfaces were studied using both scanning electron microscopy (SEM) and electron probe microanalysis (EPMA). The SEM micrographs showed that the fractures were mostly intergranular. Chemical composition of intergranular cracks surface were analyzed using EPMA at low accelerating voltage. A high concentration of sulfur was found on most of grain boundary facets. The internal stress in alloys after fatigue was qualitatively estimated using electron backscattering diffraction in scanning electron microscopy. A high level of local misorientation was found near most grain boundaries. The mechanism of intergranular cracks formation during fatigue is discussed taking into account both the segregation of sulfur at grain boundaries and accumulation of plastic strain at grain boundaries

Abstract: Heat-resistant steels of HP series (Fe-25Cr-35Ni) are used as reformer tubes in petrochemical industries. Their composition includes Nb and Ti as strong carbide formers. In the ascast condition, alloys exhibit an austenite matrix with intergranular MC, M23C6 and/or M7C3 eutectic carbides. During exposure at high temperature, phase transformations occur: chromium carbides of M7C3 type transform into the more stable M23C6 type, intragranular M23C6 carbides precipitate, and a silicide, the G-phase (Ni16Nb6Si7), forms due to the instability of MC carbides (NbC). Thermodynamic simulation is of great help for understanding precipitate formation and transformations. Thermo-Calc and Dictra are used to simulate the precipitation of carbides in the austenite matrix during service. However, from an experimental point of view, M23C6 and M7C3 are not easy to distinguish in bulk alloys. Indeed, backscattered scanning electron microscopy does not bring any contrast between the two phases, and energy dispersive spectroscopy (EDS) analysis does not lead to carbon content and consequently to the distinction between M23C6 and M7C3. With transmission electron microscopy (TEM), sample preparation is difficult and the observed area is extremely small. In the present work, HP alloys are investigated by electron backscatter diffraction (EBSD) coupled to EDS. Carbides are identified on the basis of crystal structure, in the bulk, within their microstructural context, and the experimental procedure is both simpler and cheaper than TEM. Precipitates (M23C6, M7C3) could be identified by orientation mapping and single spot analysis.

Abstract: Impurity segregation at grain boundaries in polycrystalline alloys is known to have a tremendous impact on the material properties such as grain boundary mobility, cohesion... But direct measurement of grain boundary chemistry is quite complex and there are few results concerning polycrystals. In this paper we present an indirect method to measure segregationmisorientation dependence on polycrystalline Ni-S alloys using 3D reconstruction of etch grooves. Samples of Ni-S alloy (1 ppm at) have been cold rolled at respectively 0.3 and 0.9 Von Mises equivalent strain and then annealed at 455°C to promote recrystallization. Then they have been etched near the transpassive potential to form etch grooves, whose geometry depends on the sulfur segregation level. It is found that the sulfur concentration at grain boundary decreases significantly when the driving force for grain boundary migration (i.e. the initial strain) increases, as predicted by solute drag theory.