Phase-contrast x-ray tomography for soft and hard condensed matter

Abstract

Phase-Contrast Tomography (PCT) is becoming an important technique for nondestructive, in-situ characterization of soft and hard condensed matter. This thesis sheds light on our progress in developing novel tomographic reconstruction algorithms in combination with in-situ experimental approaches that employ propagation-based PCT. These developments are aimed to improve the spatial and temporal resolutions of in-situ studies of the soft and hard condensed matter. The mechanical properties of materials such as steel are, to a large extent, defined by its microstructure. Propagation-based PCT (i.e. holotomography) can be used to visualize the microstructures associated with small variations in density or composition in the bulk of the specimen. This imaging technique has the advantage of being non-destructive and allows to carry out in-situ, time-resolved observations of miscrostructural changes during dynamic processes such as solid-state phase transformations. Sufficient spatial and temporal resolution can be achieved only when an extremely bright x-ray source is used. In order to test whether a novel table-top x-ray source, the MIRRORCLE-6X, can be used for implementation of a propagation-based PCT system, we have carried out a series of experiments. The characteristics of a propagation-based PCI system that employs the MIRRORCLE-6X were analyzed. In our further research we have focused on the experiments that could be performed at the European Synchrotron Radiation Facility (ESRF) in Grenoble, France. We reported on the investigation of the cementite microstructure in carbon steel. In this work we present the reconstruction of the three-dimensional morphology of cementite grains in the bulk of steel using a non-destructive imaging technique – x-ray Phase-Contrast Tomography (PCT). Complementary information about the crystalline structure of the ferrite grains surrounding the cementite is obtained using x-ray Diffraction-Contrast Tomography (DCT). The work was continued by a time-resolved x-ray PCT investigation of the austenite grain growth during the ferrite-to-austenite phase transformation in low-carbon steel. Experimental data allows to visualize the evolution of the three-dimensional morphology of the austenite-ferrite interfaces with a spatial resolution on the order of 1 ?m and a time resolution of less than 9 minutes. The in-situ measurements show that the theory for grain growth during diffusional solid-state phase transformations needs to be extended in order to describe the drastically lower mobility that we observed for flat interfaces compared to curved interfaces. We observe that some flat interfaces are completely immobile, which is not predicted by the state-of-the-art theories and showed - for the first time - that new computational model for grain growth are needed. Quantitative image reconstruction based on PCT data requires solving two inverse problems: phase retrieval and tomographic reconstruction. In most cases, the problem of phase retrieval is ill-posed and requires that some type of a prior knowledge about the reconstructed image (i.e. particular regularization method) is used. We present a novel algebraic approach suitable for phase retrieval using various linear models. In this approach Total Variation (TV) minimization is used for regularization of the linearized inverse problem by promoting the solution with a sparse gradient magnitude (i.e. piece-wise constant solution). In that case prior knowledge about the reconstructed image may allow to (partially) recover the unknown spatial frequencies that are undefined by the experimental data. The problem of tomographic reconstruction based on PCT data can be solved using a similar approach. We conclude our investigation of the image reconstruction algorithms by introducing several algebraic approaches suitable for tomographic reconstruction based on PCT data. In these approaches TV minimization is used to find a regularized solution to an underdetermined linear system based on a linearized representation of the PCT. When the density of the reconstructed object is piece-wise constant (or close to it) a virtually artifact-free solution can be computed for the tomographic problem. The proposed approach can also be used to radically improve the accuracy of the tomographic reconstruction based on incomplete data (e.g. small number of projections) or data with low signal to noise ratio.