Sophie Berveiller

Inter- and Intragranular Stress Determination with Kossel Microdiffraction in a Scanning Electron Microscope

A Kossel microdiffraction experimental set up is under development inside a Scanning Electron Microscope (SEM) in order to determine the crystallographic orientation as well as the inter- and intragranular strains and stresses on the micron scale, using a one cubic micrometer spot. The experimental Kossel line patterns are obtained by way of a CCD camera and are then fully indexed using a home-made simulation program. The so-determined orientation is compared with Electron Back-Scattered Diffraction (EBSD) results, and in-situ tests are performed inside the SEM using a tensile/compressive machine. The aim is to verify a 50MPa stress sensitivity for this technique and to take advantage from this microscope environment to associate microstructure observations (slip lines, particle decohesion, crack initiation) with determined stress analyses.

Strain resolution of scanning electron microscopy based Kossel microdiffraction

Kossel microdiffraction in a scanning electron microscope enables determination of local elastic strains. With Kossel patterns recorded by a CCD camera and some automation of the strain determination process, this technique may become a convenient tool for analysis of strains. As for all strain determination methods, critical for the applicability of the Kossel technique is its strain resolution. The resolution was estimated in a number of ways: from the simplest tests based on simulated patterns (of an Ni alloy), through analysis of sharp experimental patterns of Ge, to estimates obtained by in situ tensile straining of single crystals of the Ni-based superalloy. In the latter case, the results were compared with those of conventional X-ray diffraction and synchrotron-based Kossel diffraction. In the case of high-quality Ge patterns, a resolution of 1 × 10−4 was reached for all strain tensor components; this corresponds to a stress of about 10 MPa. With relatively diffuse patterns from the strained Ni-based superalloy, under the assumption of plane stress, the strain and stress resolutions were 3 × 10−4 and 60 MPa, respectively. Experimental and computational conditions for achieving these resolutions are described. The study shows potential perspectives and limits of the applicability of semiautomatic Kossel microdiffraction as a method of local strain determination.

Estimation of the electron beam-induced specimen heating and the emitted X-rays spatial resolution by Kossel microdiffraction in a scanning electron microscope

A Kossel microdiffraction experimental setup has been developed inside a Scanning Electron Microscope for crystallographic orientation, strain and stress determination at a micrometer scale. This paper reports an estimation of copper and germanium specimens heating due to the electron beam bombardment. The temperature rise is calculated from precise lattice parameters measurement considering different currents induced in the specimens. The spatial resolution of the technique is then deduced.

Residual Stress State at Different Scales in Deep Drawn Cup of Unstable Austenitic Steel

In this study, residual stresses state at different scales in the 301LN unstable austenitic steel after deep drawing was determined. The first part of the work deals with the characterization of the martensitic transformation during uniaxial loading. The austenite/martensite content which was determined by X-Ray Diffraction increases until a maximum of 0.6 for 30% strain. Internal stress distribution was determined by coupling in-situ tensile tests with sin²ψ method. As soon as martensite appears, the magnitudes of the internal stresses in this phase were found to be 400 MPa higher than in the austenite. To establish a relation between the complex loading path effect and the phase stress state, deep drawing tests were carried out for different drawing ratios. Both macroscopic tangential residual stresses and residual stresses in the martensite were determined. It appears that the macroscopic tangential residual stresses are positive and increase with increasing drawing ratios and the maximum value is located at middle height of the cup. It is about 850MPa for the Drawing Ratio (DR)=2.00. The tangential residual stresses in the martensite were found to be positive in the external face and have a same evolution as the macroscopic ones.

Inter and Intra Granular Strain Analysis by Microdiffraction Kossel

We have developed a new convenient tool for local stress and strain analysis in the scanning electron microscope. It is based on the Kossel diffraction, physical phenomenon that is known for a long time because of its high accuracy for lattice constant determination in micron regions. The pattern is recorded on a CCD camera allowing a fast and reliable analysis. This technique has been applied to several materials. In-situ tensile tests were performed on a shape memory alloy. During loading, we observe clearly a shift of Kossel lines on the diagram, whose magnitude depends on the (hkl) crystallographic planes. The stress can be deduced from the diffracting plane strain measurement using a single crystal stress analysis.

Micromechanical Modeling of Brittle Fracture of French RPV Steel: A Comprehensive Study of Stress Triaxiality Effect

The present study describes a multiscale representation of mechanisms involved in brittle fracture of a french Reactor Pressure Vessel (RPV) steel (16MND5 equ. ASTM A508 Cl.3) at low temperatures. Attention will be focused on the representation of stress heterogeneities inside the ferritic matrix during plastic straining, which is considered as critical for further micromechanical approach of brittle fracture. This representation is tuned on experimental results. Modeling involves micromechanical a description of plastic glide, a mean field (MF) model and a realistic three-dimensional aggregates Finite Element (FE) simulation, all put together inside a multiscale approach. Calibration is done on macroscopic stress-strain curves at different low temperatures, and modeling reproduces experimental stress heterogeneities. This modeling allows to apply a local micromechanical fracture criterion of crystallographic cleavage for triaxial loadings on the Representative Volume Element (RVE). Deterministic computations of time to fracture for different carbide sizes random selection provide a probability of fracture for an Elementary Volume (EV) consistant with the local approach. Results are in good agreement with hypothesis made by local approach to fracture. Hence, the main difference is that no phenomenological dependence on loading or microstructure is supposed for probability of fracture on the EV : this dependence is naturally introduced by the micromechanical description. Further information on ASME publications can be found at : http://asmedl.org As per ASMEs policy there must not be any outside charge or fee for distribution. This is for reference only. Anyone who wishes to use any part of this article must contact ASME for permission at permissions@asme.org.

Stress determination during the mechanically-induced martensite phase transformation in the superelastic alloy CuAlBe by neutron diffraction

This paper focuses on the study of the superelastic behavior associated to the stress induced martensite transformation in a Cu-12.5%Al-0.5%Be [wt. %] shape memory alloy. Neutron diffraction was used to track the evolution of stress in the (β1) austenitic phase during the onset of the stress-induced martensite phase change. A thin flat and a cylindrical specimen was analyzed, allowing us firstly to evaluate the stress evolution in the austenite phase during martensitic transformation with laboratory X-ray and neutron diffraction and secondly to compare differences between methods (sin2ψ, principal stress) for in-situ neutron diffraction experiments.

Influence of Temperature on Stress Distribution in Bainitic Steels - Application to 16 MND5-A508 Pressure Vessel Steel

In this study, the internal stress evolution of the ferrite phase of 16MND5-A508 has been determined using X-Ray Diffraction (XRD). The results of in situ tests combined with XRD analyses and performed at different temperatures (-150°C and 22°C) exhibit a difference of about 200MPa between the macroscopic stress and the ferrite one. The stress state in the cementite is determined by a mixture law; it reaches very high values up to 9000MPa. These results highlight the need to analyze the stress directly in the cementite phase by using appropriate tools, since its volume fraction does not allow it using XRD.

Plastic Heterogeneities Characterisation in 16MND5 RPV Steel by X-Ray Diffraction, Comparison with Finite-Element Approach

This paper reports experimental characterisation of stress heterogeneities in a French RPV bainitic steel (16MND5) determined by X-Ray diffraction during in-situ tensile testing at low temperature (until –150°C). Results are compared successfully to simulation results, obtained by post-processing of Finite Elements computations of realistic 3D aggregates.

Determination of Residual Stresses after Tensile Tests and Deep Drawing of Unstable Austenitic Steel

The main objective of this work is to contribute to the study of the 301LN unstable austenitic stainless steel by determining the distribution of residual stresses after deep drawing, taking into account the phase transformation. In the first part, kinetics of martensitic transformation are determined for uniaxial loading. Tensile tests are performed at different pre-strains at room temperature for two different strain rates. The austenite/martensite content is measured by X-ray diffraction and is coupled with the determination of residual stresses distribution. In addition, to establish a relation between the complex loading path effect and the residual stresses state, deep drawing are done for different drawing ratios for two different temperatures. Macroscopic tangential residual stresses are determined by the separation technique. It appears that the residual stresses increase with increasing drawing ratios and the maximum value is located at middle height of the cup.