Florent Bridier

Experimental study of the Ca-Mg-Zn system using diffusion couples and key alloys

Abstract Nine diffusion couples and 32 key samples were prepared to map the phase diagram of the Ca–Mg–Zn system. Phase relations and solubility limits were determined for binary and ternary compounds using scanning electron microscopy, electron probe microanalysis and x-ray diffraction (XRD). The crystal structure of the ternary compounds was studied by XRD and electron backscatter diffraction. Four ternary intermetallic (IM) compounds were identified in this system: Ca3MgxZn15−x (4.6x12 at 335 °C, IM1), Ca14.5Mg15.8Zn69.7 (IM2), Ca2Mg5Zn13 (IM3) and Ca1.5Mg55.3Zn43.2 (IM4). Three binary compounds were found to have extended solid solubility into ternary systems: CaZn11, CaZn13 and Mg2Ca form substitutional solid solutions where Mg substitutes for Zn atoms in the first two compounds, and Zn substitutes for both Ca and Mg atoms in Mg2Ca. The isothermal section of the Ca–Mg–Zn phase diagram at 335 °C was constructed on the basis of the obtained experimental results. The morphologies of the diffusion couples in the Ca–Mg–Zn phase diagram at 335 °C were studied. Depending on the terminal compositions of the diffusion couples, the two-phase regions in the diffusion zone have either a tooth-like morphology or contain a matrix phase with isolated and/or dendritic precipitates.

Microscopic Strain and Crystal Rotation Measurement within Metallurgical Grains

This work describes an experimental procedure to measure the progressive strain localization and crystal lattice rotation within metallurgical grains. A digital image correlation software was implemented and associated with mechanical tests carried out inside a scanning electron microscope on specimens exhibiting nanometric grainy patterns. Cross-correlation analyzes between electron backscattering diffraction maps were also developed to quantify the corresponding local crystal rotation relative to the original structure. The microscale strain and rotation fields on the surface of a tensile-loaded specimen made of austenitic stainless steel 316L are presented as an illustration. Their direct spatial correlation between strain heterogeneities and the progressive activation of slip systems is put into evidence and discussed.

On the Measurement of Residual Stress in Induction Hardened Parts

It is well known that induction surface heating followed by rapid quenching generally increases the fatigue life of steel components subjected to bending loads by significantly postponing the micro-crack nucleation and propagation processes. The phase transformation volume change combined with severe thermal gradients leave a hard surface layer under relatively high and deep compressive residual stresses. In this paper, residual stress measurements are done on induction hardened AMS6414 martensitic steel (aerospace grade of AISI4340) cylinders using two techniques: the so-called contour method and X-ray diffraction. For both methods, induction hardened parts raise many challenges. The contour method hardly describes high stress gradients near the surface while the diffraction technique accuracy appears limited considering the strong microstructural variation and the high depth of the stresses to be measured. For the contour method, a CMM and an optical pen using the confocal chromatic imaging principle were used to measure the surface after precision WEDM cutting. The effect of data filtering and smoothing on the calculated stresses are discussed. For X-ray analysis, the effect of stress relaxation during layer removal and analysis technique is explained. The difference between the residual stress measurements done with the two techniques is discussed with emphasis on both the surface and the in-depth measurements.

Inter- and intragranular delta phase quantitative characterization in Inconel 718 by means of image analysis.

This paper describes an image processing method for discriminating the inter‐ and intragranular delta phase precipitates in Inconel 718 (IN 718). The successive practical operations and the motivations of their choices are presented in detail. The method was applied to IN 718 specimens heat treated with different parameters to produce microstructures containing various amounts of both types of precipitates. They were characterized by electron microscopy in backscattered electron imaging. The main difficulty arose from the fact that the brightness distributions of inter‐ and intragranular precipitates partially overlap. Additional information on their morphology and their spatial distribution had to be exploited in order to differentiate them. The shape and the orientation of the precipitates were evaluated using the structure tensor, an operator that quantifies the directionality of the intensity distribution in an image. The distance between parallel precipitates was also used as an additional property to identify clusters of intragranular precipitates.

Measuring in-depth Residual Stress Gradients: The Challenge of Induction Hardened Parts

Highly stressed machine parts such as gears and shafts are often surface treated to increase wear and fatigue resistance at critical locations. For example, induction surface hardening (ISH) is increasingly used in the automotive and aerospace industries thanks to the availability of modern multiple frequencies generators and complex shaped coils that provide a great flexibility in process control. With similar end-results in terms of hardened depths, very different residual stress profiles may be obtained, and optimized by modifying both heating and quenching kinetics. If hardness and microstructures variations are routinely verified, some challenges raise for the measurement of the residual stress gradients within complex geometry parts, in particular for the case of deep hardened layers. The most commonly used technique is X-ray diffraction (XRD). It requires using successive layer removal to get access to in-depth stresses. The measurements must therefore be corrected for the stress redistribution occurring during layer removal. However, industrial geometries are often not covered by traditional correction methods. The present work aims at applying XRD to precisely measure in-depth residual stress profiles in induction hardened thin discs made of martensitic steel. Both issues of microstructural variations and redistribution of stresses during layer removal are tackled. First, X-ray elastic constants were determined experimentally using a miniature custom-made tensile machine with specimens heat treated to simulate different microstructures found in ISH parts. Second, a recently introduced finite elements based layer removal correction method was applied. The proposed methodology is used to show the impact of preheating and core hardness on the residual stresses obtained after induction hardening.

Morphological and Crystallographic Characterizations of the Ca-Mg-Zn Intermetallics Appearing in Ternary Diffusion Couples

In the present research, seven multi-phase diffusion couples, with terminal alloys having different microstructural features, were prepared and annealed for 4 weeks at 335°C. The phase relations and change of morphological characteristics of each phase were studied along the diffusion zone by means of scanning electron microscopy/energy dispersive X-ray spectroscopy and quantitative electron probe microanalysis. Depending on the different terminal compositions of the diffusion couples, the morphological evolution in the diffusion zone can be: tooth-like, matrix phase with isolated and/or dendritic precipitates. Electron back-scattered diffraction analysis was carried out to investigate the crystal orientation of the ternary compounds and the crystal orientation relations at the interface of the diffusion zones.

Numerical simulation of low-cycle fatigue behavior of welded joints for naval applications: influence of residual stresses

A methodology is described and evaluated for the numerical prediction of the low-cycle fatigue strength of welded assemblies taking into account the effect of local residual stresses. The methodology involves (i) modeling the cyclic behavior of base metal and heat affected zone materials of welded joints, (ii) establishing a simplified method to analytically predict the local notch fatigue behavior, (iii) defining a crack initiation criterion including mean stress effect. Notched specimens are first designed to produce a first configuration without residual stresses, a second one with tensile residual stresses, and a third one with compressive residual stresses. Cyclic tests are performed under repeated tensile loading. These tests allowed describing the influence of the initial residual stress states on the fatigue life quantified and analyzed on the basis of experiments. The application of the simplified method managed to capture the impact of residual stresses on the local cyclic behavior and the crack initiation resistance. Finally, the fatigue life prediction method is applied on thick welded T-joints. The deep hole drilling and the contour method are used to determine residual stresses in the weld toe. The proposed modeling approach is finally evaluated and discussed by correlating numerical predictions with experimental results obtained on T-joints loaded in four-point bending fatigue.

Mechanical and metallurgical evolution of stainless steel 321 in a multi-step forming process

This paper examines the metallurgical evolution of AISI Stainless Steel 321 (SS 321) during multi-step forming, a process that involves cycles of deformation with intermediate heat treatment steps. The multi-step forming process was simulated by implementing interrupted uniaxial tensile testing experiments. Evolution of the mechanical properties as well as the microstructural features, such as twins and textures of the austenite and martensite phases, was studied as a function of the multi-step forming process. The characteristics of the Strain-Induced Martensite (SIM) were also documented for each deformation step and intermediate stress relief heat treatment. The results indicated that the intermediate heat treatments considerably increased the formability of SS 321. Texture analysis showed that the effect of the intermediate heat treatment on the austenite was minor and led to partial recrystallization, while deformation was observed to reinforce the crystallographic texture of austenite. For the SIM, an Olson-Cohen equation type was identified to analytically predict its formation during the multi-step forming process. The generated SIM was textured and weakened with increasing deformation.

Experimental Comparison of In-Depth Residual Stresses Measured with Neutron and X-Ray Diffraction with a Numerical Stress Relaxation Correction Method

This study is an experimental comparison of in-depth X-ray diffraction residual stress measurements with neutron diffraction measurements. The goal is to evaluate the relevance of the Savaria-Bridier-Bocher [1] stress relaxation correction method. Neutron diffraction are performed on a bent notched specimen. Destructive X-ray diffraction is performed until 5.25mm below the surface by polishing the material. This polishing induces stress relaxation and X-ray diffraction results have to be corrected. For that purpose, a finite element analysis is realised and show good correlation with neutron measurements results. The application of the stress correction method improves the X-ray measurements especially after 2 mm below the surface. The differences between measured and corrected residual stresses from both diffraction techniques are analyzed and discussed.