Papers by Author: Henning Friis Poulsen

Abstract: Within the last decade a number of x-ray diffraction methods have been presented for non-destructive 3D characterization of polycrystalline materials. 3DXRD [1] and Diffraction Contrast Tomography [2,3,4] are examples of such methods providing full spatial and crystallographic information of the individual grains. Both methods rely on specially designed high-resolution near-field detectors for acquire the shape of the illuminated grains, and therefore the spatial resolution is for both methods limited by the resolution of the detector, currently ~2 micrometers. Applying these methods using conventional far-field detectors provides information on centre of mass, crystallographic orientation and stress state of the individual grains [5], at the expense of high spatial resolution. However, far-field detectors have much higher efficiency than near-field detectors, and as such are suitable for dynamic studies requiring high temporal resolution and set-ups involving bulky sample environments (e.g. furnaces, stress-rigs etc.)

Abstract: An algorithm is presented for characterization of the grain resolved (type II) stress states in a polycrystalline sample based on monochromatic X-ray diffraction data. The algorithm is a robust 12-parameter-per-grain fit of the centre-of-mass grain positions, orientations and stress tensors including error estimation and outlier rejection. As examples of use results from two experiments – one on interstitial free (IF) steel and one on copper – will be presented. In the first experiment 96 grains in one layer of IF steel were monitored during elastic loading and unloading. Very consistent results were obtained, with resolutions for each grain of approximately 10 μm in position, 0.05˚ in orientation and 80 μstrain. When averaging over all grains a resolution of 10 μstrain was obtained. In the second experiment it was demonstrated that the strain states of more than 1000 grains in a plastically deformed Cu specimen could be determined to an accuracy of 100 μstrain.

Abstract: The synchrotron based X-ray diffraction method “High angular resolution 3DXRD” is briefly introduced. The technique enables the investigation of individual dislocation free regions in a dislocation structure, in-situ within the bulk. Results on the strain distribution within a single grain in a copper sample deformed in tension to 2%, and kept under load, are presented. It is found that the dislocation free regions of the dislocation structure on average are subjected to compressive strain with respect to the mean (tensile) strain in the grain. Results on the dynamics of individual dislocation free regions during straining are further reviewed, with special focus on the observation of intermittent behaviour.

Abstract: Ferrite formation during austenite decomposition in carbon-manganese steel is studied during slow continuous cooling by three-dimensional x-ray diffraction microscopy at a synchrotron source. The ferrite fraction and nucleation rate are measured simultaneously and independently in real time in the bulk of the specimen. Thermodynamic calculations involving both ortho- and paraequilibrium have been performed to determine the driving force for nucleation. From the experiments and thermodynamic calculations the activation energies are estimated for nucleation and the transfer of iron atoms across the interface of the cluster during ferrite nucleation in steel.

Abstract: The implementation of 3-Dimensional X-Ray Diffraction (3DXRD) Microscopy at the Advanced Photon Source is described. The technique enables the non-destructive structural characterization of polycrystalline bulk materials and is therefore suitable for in situ studies during thermo-mechanical processing. High energy synchrotron radiation and area detectors are employed. First, a forward modeling approach for the reconstruction of grain boundaries from high resolution diffraction images is described. Second, a high resolution reciprocal space mapping technique of individual grains is presented.

Abstract: A method for in-situ studies of the dynamics of individual embedded subgrains during recovery is introduced. The method is an extension of 3DXRD principles for studies of grain dynamics in connection with recrystallisation. It is limited to studies of foils with a sample thickness of 10-100 subgrains due to diffraction spot overlap. The volume evolution during recovery (annealing at 300°C for 181 minutes) of nine individual subgrains in a deformed sample (38% cold rolled Aluminium) is presented.

Abstract: 3-Dimensional X-Ray Diffraction (3DXRD) microscopy is a tool for fast and non-destructive characterization of the individual grains, sub-grains and domains inside bulk materials. The method is based on diffraction with highly penetrating hard x-rays, enabling 3D studies of millimeter - centimeter thick specimens. The position, volume, orientation, elastic and plastic strain can be derived for hundreds of grains simultaneously. Furthermore, by applying novel reconstruction methods 3D maps of the grain boundaries can be generated. With the present 3DXRD microscope set-up at the European Synchrotron Radiation Facility, the spatial resolution is ~ 5 µm, while grains of size 100 nm can be detected. 3DXRD microscopy enables, for the first time, dynamic studies of the individual grains and sub-grains within polycrystalline materials. The methodology is reviewed with emphasis on recent advances in grain mapping. Based on this a series of general 3DXRD approaches are identified for studies of nucleation and growth phenomena such as recovery, recrystallisation and grain growth in metals.

Abstract: A new method for in-situ studies of nucleation in bulk metals based on high energy synchrotron radiation is presented. Copper samples cold rolled 20% are investigated. The crystallographic orientations near triple junctions are characterized using non-destructive 3DXRD microscopy before, during, and after annealing for 1 hour at 290°C. This method allows in-situ identification of new nuclei and the deformed material, which spawns the nuclei. Also, since data is acquired during annealing nucleation kinetics can be studied.