Method for auto-alignment and determination of parameter space in dual-phase grating interferometry.

X-ray dual-phase grating interferometry provides quantitative micro-structural information beyond the optical resolution through its tunable correlation length. Ensuring optimal performance of the set-up requires accurate correlation length estimation and precise alignment of the gratings. This paper presents an automated procedure for determining the complete geometrical parameters of the interferometer set-up with a high degree of precision. The algorithm's effectiveness is then evaluated through a series of experimental tests, illustrating its accuracy and robustness.

4D microvelocimetry reveals multiphase flow field perturbations in porous media.

Many environmental and industrial processes depend on how fluids displace each other in porous materials. However, the flow dynamics that govern this process are still poorly understood, hampered by the lack of methods to measure flows in optically opaque, microscopic geometries. We introduce a 4D microvelocimetry method based on high-resolution X-ray computed tomography with fast imaging rates (up to 4 Hz). We use this to measure flow fields during unsteady-state drainage, injecting a viscous fluid into rock and filter samples. This provides experimental insight into the nonequilibrium energy dynamics of this process. We show that fluid displacements convert surface energy into kinetic energy. The latter corresponds to velocity perturbations in the pore-scale flow field behind the invading fluid front, reaching local velocities more than 40 times faster than the constant pump rate. The characteristic length scale of these perturbations exceeds the characteristic pore size by more than an order of magnitude. These flow field observations suggest that nonlocal dynamic effects may be long-ranged even at low capillary numbers, impacting the local viscous-capillary force balance and the representative elementary volume. Furthermore, the velocity perturbations can enhance unsaturated dispersive mixing and colloid transport and yet, are not accounted for in current models. Overall, this work shows that 4D X-ray velocimetry opens the way to solve long-standing fundamental questions regarding flow and transport in porous materials, underlying models of, e.g., groundwater pollution remediation and subsurface storage of CO2 and hydrogen.

Detailed analysis of the interference patterns measured in lab-based X-ray dual-phase grating interferometry through wave propagation simulation.

In this work, we analyze the interference patterns measured in lab-based dual-phase grating interferometry and for the first time explain the spatial dependencies of the measured interference patterns and the large visibility deviations between the theoretical prediction and the experimental results. To achieve this, a simulator based on wave propagation is developed. This work proves that the experimental results can be simulated with high accuracy by including the effective grating thickness profile induced by the cone-beam geometry, the measured detector response function and a non-ideal grating shape. With the comprehensive understanding of dual-phase grating interferometry, this provides the foundations for a more efficient and accurate algorithm to retrieve sample's structure information, and the realistic simulator is a useful tool for optimizing the set-up.

Improving image quality in fast, time-resolved micro-CT by weighted back projection.

Time-resolved micro-CT is an increasingly powerful technique for studying dynamic processes in materials and structures. However, it is still difficult to study very fast processes with this technique, since fast scanning is typically associated with high image noise levels. We present weighted back projection, a technique applicable in iterative reconstruction methods using two types of prior knowledge: (1) a virtual starting volume resembling the sample, for example obtained from a scan before the dynamic process was initiated, and (2) knowledge on which regions in the sample are more likely to undergo the dynamic process. Therefore, processes on which this technique is applicable are preferably occurring within a static grid. Weighted back projection has the ability to handle small errors in the prior knowledge, while similar 4D micro-CT techniques require the prior knowledge to be exactly correct. It incorporates the prior knowledge within the reconstruction by using a weight volume, representing for each voxel its probability of undergoing the dynamic process. Qualitative analysis on a sparse subset of projection data from a real micro-CT experiment indicates that this method requires significantly fewer projection angles to converge to a correct volume. This can lead to an improved temporal resolution.

In-Situ X-ray Imaging Of Sublimating Spin-Frozen Solutions.

Spin-freeze-drying is a promising technique to enable long-term storage of pharmaceutical unit doses of aqueous drug solutions. To investigate the sublimation of the ice during the primary phase of freeze-drying, X-ray imaging can yield crucial temporally resolved information on the local dynamics. In this paper, we describe a methodology to investigate the sublimation front during single unit-dose freeze-drying using 4D in-situ X-ray imaging. Three spin-frozen samples of different solutions were imaged using this methodology and the process characteristics were analysed and reduced to two-dimensional feature maps.

4D Micro-Computed X-ray Tomography as a Tool to Determine Critical Process and Product Information of Spin Freeze-Dried Unit Doses.

Maintaining chemical and physical stability of the product during freeze-drying is important but challenging. In addition, freeze-drying is typically associated with long process times. Therefore, mechanistic models have been developed to maximize drying efficiency without altering the chemical or physical stability of the product. Dried product mass transfer resistance ( R p ) is a critical input for these mechanistic models. Currently available techniques to determine R p only provide an estimation of the mean R p and do not allow measuring and determining essential local (i.e., intra-vial) R p differences. In this study, we present an analytical method, based on four-dimensional micro-computed tomography (4D- µ CT), which enables the possibility to determine intra-vial R p differences. Subsequently, these obtained R p values are used in a mechanistic model to predict the drying time distribution of a spin-frozen vial. Finally, this predicted primary drying time distribution is experimentally verified via thermal imaging during drying. It was further found during this study that 4D- µ CT uniquely allows measuring and determining other essential freeze-drying process parameters such as the moving direction(s) of the sublimation front and frozen product layer thickness, which allows gaining accurate process knowledge. To conclude, the study reveals that the variation in the end of primary drying time of a single vial could be predicted accurately using 4D- µ CT as similar results were found during the verification using thermal imaging.