Denis Bouscaud

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.

External Reference Samples for Residual Stress Analysis by X-Ray Diffraction

The GFAC (French Association for residual stress analysis) decided in 2007 to work on external reference samples for residual stress analysis by X-ray diffraction as defined in the XPA 09-285 and EN 15305-2009 standards. Seven materials are studied: ferritic steel, martensitic steel, aluminium alloy, titanium alloy, 2 types of Nickel-Chromium alloy and tungsten thin layers deposited on silicon wafers. The purpose of this external round robin campaign is threefold: (i) to give possibilities for each laboratory involved in the campaign test to obtain external reference samples for each material tested, (ii) to validate a common procedure for qualification of external samples and (iii) to commercialise validated external reference samples through the GFAC association. A common approach of X-Ray diffraction parameters, samples geometry and standard procedure has been chosen and adopted by each laboratory involved in these tests. No indication in terms of residual stress calculation method is given; the choice of the method (centroid, middle point, maximum of peak, fitting…) is the choice of the laboratory according to their X-ray diffraction set-ups, softwares and experience. Once all samples are analysed, values given by each laboratory are compared and analysed.

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.

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.

Stress Analysis by Kossel Microdiffraction on a Nickel-Based Single Crystal Superalloy during an In Situ Tensile Test – Comparison with Classical X-Ray Diffraction

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. An area of about one cubic micrometer can be analysed using the microscope probe, which enables to study different kinds of elements such as a grain boundary, a crack, a microelectronic component, etc. The diffraction pattern is recorded by a high resolution Charge-Coupled Device (CCD) camera. The crystallographic orientation, the lattice parameters and the elastic strain tensor of the probed area are deduced from the pattern indexation using a homemade software. The purpose of this paper is to report some results achieved up to now to estimate the reliability of the Kossel microdiffraction technique.