Energy selective neutron imaging for the characterization of polycrystalline materials

This multipart dissertation focuses on the development and evaluation of advanced methods for material testing and characterization using neutron diffraction and imaging techniques. A major focus is on exploiting diffraction contrast in energy selective neutron imaging (often referred to as Bragg edge imaging) for strain and phase mapping of crystalline materials. The dissertation also evaluates the use of neutron diffraction to study the effect of multi-axial loading, in particular the role of applying directly shear strains from the application of torsion. A portable tension-torsion-tomography loading system has been developed for in-situ measurements and integrated at major user facilities around the world. Promising applications for the Bragg edge technique are implemented at the neutron imaging facility CONRAD at the reactor source BER-II as well as at neutron time of flight instruments. Strain mapping is successfully demonstrated for all cases to yield quantifiable results, but is limited in practicality due to limitations in choice of the scattering vector (direction of probed strain tensor component) and the gauge volume selection. The use of Bragg edge imaging for crystalline phase mapping was explored and appears to be a very promising technique. The extension to three-dimensionally resolved tomography is presented for samples exhibiting the TRansfomation Induced Plasticity (TRIP) effect, while challenges with characterizing textured samples are discussed. Individual crystallites within a polycrystalline material exhibit elastic anisotropy which is significant as that can lead to stress concentrations and inhomogeneities during plastic deformation. Characterization of elastic anisotropy is important to understand the effects of texture on the macroscopic mechanical properties. Diffraction methods can do this, by probing the response of individual lattice planes to externally applied mechanical stress. Past experimental data using diffraction based methods have largely been limited to uni‑axial tensile and/or compressive loading conditions, even though shear dominates most common failure mechanisms for structural materials. Within this dissertation, experimental techniques have been established for the measurement of lattice strains under applied torsion (pure shear) and lattice specific shear moduli are reported. This is accomplished using a (traditional) neutron diffractometer instrument, in conjunction with special alignment procedures and the specifically designed axial-torsional loading system

Investigation of dissimilar metal welds by energy-resolved neutron imaging

A nondestructive study of the internal structure and compositional gradient of dissimilar metal-alloy welds through energy-resolved neutron imaging is described in this paper. The ability of neutrons to penetrate thick metal objects (up to several cm) provides a unique possibility to examine samples which are opaque to other conventional techniques. The presence of Bragg edges in the measured neutron transmission spectra can be used to characterize the internal residual strain within the samples and some microstructural features, e.g. texture within the grains, while neutron resonance absorption provides the possibility to map the degree of uniformity in mixing of the participating alloys and intermetallic formation within the welds. In addition, voids and other defects can be revealed by the variation of neutron attenuation across the samples. This paper demonstrates the potential of neutron energy-resolved imaging to measure all these characteristics simultaneously in a single experiment with sub-mm spatial resolution. Two dissimilar alloy welds are used in this study: Al autogenously laser welded to steel, and Ti gas metal arc welded (GMAW) to stainless steel using Cu as a filler alloy. The cold metal transfer variant of the GMAW process was used in joining the Ti to the stainless steel in order to minimize the heat input. The distributions of the lattice parameter and texture variation in these welds as well as the presence of voids and defects in the melt region are mapped across the welds. The depth of the thermal front in the Al–steel weld is clearly resolved and could be used to optimize the welding process. A highly textured structure is revealed in the Ti to stainless steel joint where copper was used as a filler wire. The limited diffusion of Ti into the weld region is also verified by the resonance absorption

Neutron diffraction and diffraction contrast imaging for mapping the TRIP effect under load path change

The transformation induced plasticity (TRIP) effect is investigated during a load path change using a cruciform sample. The transformation properties are followed by in-situ neutron diffraction derived from the central area of the cruciform sample. Additionally, the spatial distribution of the TRIP effect triggered by stress concentrations is visualized using neutron Bragg edge imaging including, e.g., weak positions of the cruciform geometry. The results demonstrate that neutron diffraction contrast imaging offers the possibility to capture the TRIP effect in objects with complex geometries under complex stress states.Fil: Polatidis, Efthymios. Paul Scherrer Institute; SuizaFil: Morgano, Manuel. Paul Scherrer Institute; SuizaFil: Malamud, Florencia. Comision Nacional de Energia Atomica. Gerencia D/area Invest y Aplicaciones No Nucleares. Departamento Haces de Neutrones del Ra10 - Cab.; Argentina. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - Patagonia Norte; ArgentinaFil: Bacak, Michael. Paul Scherrer Institute; SuizaFil: Panzner, Tobias. Paul Scherrer Institute; Suiza. Swissneutronics; SuizaFil: Van Swygenhoven, Helena. Paul Scherrer Institute; Suiza. École Polytechnique Fédérale de Lausanne; SuizaFil: Strobl, Markus. Paul Scherrer Institute; Suiz

4D Bragg Edge Tomography of Directional Ice Templated Graphite Electrodes

Bragg edge tomography was carried out on novel, ultra-thick, directional ice templated graphite electrodes for Li-ion battery cells to visualise the distribution of graphite and stable lithiation phases, namely LiC12 and LiC6. The four-dimensional Bragg edge, wavelength-resolved neutron tomography technique allowed the investigation of the crystallographic lithiation states and comparison with the electrode state of charge. The tomographic imaging technique provided insight into the crystallographic changes during de-/lithiation over the electrode thickness by mapping the attenuation curves and Bragg edge parameters with a spatial resolution of approximately 300 µm. This feasibility study was performed on the IMAT beamline at the ISIS pulsed neutron spallation source, UK, and was the first time the 4D Bragg edge tomography method was applied to Li-ion battery electrodes. The utility of the technique was further enhanced by correlation with corresponding X-ray tomography data obtained at the Diamond Light Source, UK

Energy-resolved neutron imaging for reconstruction of strain introduced by cold working

Energy-resolved neutron transmission imaging is used to reconstruct maps of residual strains in drilled and cold-expanded holes in 5-mm and 6.4-mm-thick aluminum plates. The possibility of measuring the positions of Bragg edges in the transmission spectrum in each 55 × 55 µm2 pixel is utilized in the reconstruction of the strain distribution within the entire imaged area of the sample, all from a single measurement. Although the reconstructed strain is averaged through the sample thickness, this technique reveals strain asymmetries within the sample and thus provides information complementary to other well-established non-destructive testing methods

Crystalline phase discriminating neutron tomography using advanced reconstruction methods

Time-of-flight neutron imaging offers complementary attenuation contrast to X-ray computed tomography (CT), coupled with the ability to extract additional information from the variation in attenuation as a function of neutron energy (time of flight) at every point (voxel) in the image. In particular Bragg edge positions provide crystallographic information and therefore enable the identification of crystalline phases directly. Here we demonstrate Bragg edge tomography with high spatial and spectral resolution. We propose a new iterative tomographic reconstruction method with a tailored regularisation term to achieve high quality reconstruction from low-count data, where conventional filtered back-projection (FBP) fails. The regularisation acts in a separated mode for spatial and spectral dimensions and favours characteristic piece-wise constant and piece-wise smooth behaviour in the respective dimensions. The proposed method is compared against FBP and a state-of-the-art regulariser for multi-channel tomography on a multi-material phantom. The proposed new regulariser which accommodates specific image properties outperforms both conventional and state-of-the-art methods and therefore facilitates Bragg edge fitting at the voxel level. The proposed method requires significantly shorter exposure to retrieve features of interest. This in turn facilitates more efficient usage of expensive neutron beamline time and enables the full utilisation of state-of-the-art high resolution detectors

Time-of-Flight Three Dimensional Neutron Diffraction in Transmission Mode for Mapping Crystal Grain Structures

The physical properties of polycrystalline materials depend on their microstructure, which is the nano-to centimeter scale arrangement of phases and defects in their interior. Such microstructure depends on the shape, crystallographic phase and orientation, and interfacing of the grains constituting the material. This article presents a new non-destructive 3D technique to study centimeter-sized bulk samples with a spatial resolution of hundred micrometers: time-of-flight three-dimensional neutron diffraction (ToF 3DND). Compared to existing analogous X-ray diffraction techniques, ToF 3DND enables studies of samples that can be both larger in size and made of heavier elements. Moreover, ToF 3DND facilitates the use of complicated sample environments. The basic ToF 3DND setup, utilizing an imaging detector with high spatial and temporal resolution, can easily be implemented at a time-of-flight neutron beamline. The technique was developed and tested with data collected at the Materials and Life Science Experimental Facility of the Japan Proton Accelerator Complex (J-PARC) for an iron sample. We successfully reconstructed the shape of 108 grains and developed an indexing procedure. The reconstruction algorithms have been validated by reconstructing two stacked Co-Ni-Ga single crystals, and by comparison with a grain map obtained by post-mortem electron backscatter diffraction (EBSD)