Laboratory X-ray Microtomography Research Articles

Crystal Analyzer Based Multispectral Microtomography Using CCD-Sensor.

To solve the problems of spectral tomography, an X-ray optical scheme was proposed, using a crystal analyzer in Laue geometry between the sample and the detector, which allowed for the selection of predetermined pairs of wavelengths from the incident polychromatic radiation to obtain projection images. On a laboratory X-ray microtomography setup, an experiment was carried out for the first time where a mixture of micro-granules of sodium chloride NaCl, silver behenate AgC22H43O2, and lithium niobate LiNbO3 was used as a test sample to identify their spatial arrangement. The elements were chosen based on the presence of absorption edges in two of the elements in the energy range of the polychromatic spectrum of the probing radiation. The method of projection distortion correction was used to preprocess the obtained projections. To interpret the obtained reconstruction results, the segmentation method based on the analysis of joint histograms was used. This allowed us to identify each of the three substances. To compare the results obtained, additional "reference" tomographic measurements were performed: one in polychromatic and two in monochromatic (MoKα-, MoKβ-lines) modes. It took three times less time for the tomographic experiment with the crystal analyzer, while the reconstruction accuracy was comparable to that of the "reference" tomography.

Tracking the Progression of the Simulated Bronze Disease-A Laboratory X-ray Microtomography Study.

The internal three-dimensional characteristics of X-ray microtomography (micro-CT) has great application potential in the field of bronze corrosion. This work presents a method of simulating bronze disease based on an in situ micro-CT image to study the characteristics of the oxidative hydrolysis reactions of copper(I) chloride and copper(II) chloride dihydrate. A series of high-resolution reconstruction images were obtained by carrying out micro-CT at three key points throughout the experiment. We found that the reactions of copper(I) chloride and copper(II) chloride dihydrate showed different characteristics at different stages of the simulation in the micro-CT view. The method proposed in this work specifically simulated one single type of bronze corrosion and characterized the evolution characteristics of simulated bronze disease. It provides a new perspective to investigate bronze disease and can help improve the subsequent use of micro-CT to distinguish real bronze corrosions.

Air-drying of 3D printed part made of ligno-cellulosic fibres: 3D real-time monitoring combining sub-minute laboratory X-ray microtomography and digital volume correlation

Air-drying of 3D printed part made of ligno-cellulosic fibres: 3D real-time monitoring combining sub-minute laboratory X-ray microtomography and digital volume correlation

Damage evolution during fracture by correlative microscopy with hyperspectral electron microscopy and laboratory-based microtomography.

Damage evolution during fracture of metals is a critical factor in determining the reliability and integrity of the infrastructure that the society relies upon. However, experimental techniques for directly observing these phenomena have remained challenged. We have addressed this gap by developing a correlative microscopy framework combining high-resolution hyperspectral electron microscopy with laboratory x-ray microtomography (XMT) and applied it to study fracture mechanisms in a steel inclusion system. We observed damage nucleation and growth to be inhomogeneous and anisotropic. Fracture resistance was observed to be controlled by inclusion distribution and the size scale of an inclusion-depleted zone. Furthermore, our studies demonstrate that laboratory XMT can characterize damage to the micrometer scale with a large field of view in dense metals like steel, offering a more accessible alternative to synchrotron-based tomography. The framework presented provides a means to broadly adopt correlative microscopy for studies of degradation phenomena and help accelerate discovery of new materials solutions.

Mapping the Pore Architecture of Structured Catalyst Monoliths from Nanometer to Centimeter Scale with Electron and X-ray Tomographies

The hierarchical pore systems of Pt/Al2O3 exhaust gas aftertreatment catalysts were analyzed with a collection of correlative imaging techniques to monitor changes induced by hydrothermal aging. Synergistic imaging with laboratory X-ray microtomography, synchrotron radiation ptychographic X-ray computed nanotomography, and electron tomography allowed quantitative observation of the catalyst pore architecture from centimeter to nanometer scale. Thermal aging at 750 °C in air and hydrothermal aging at 1050 °C in 10% H2O/air caused increasing structural degradation, which manifested as widespread sintering of Pt particles, increased volume and quantity of macropores (>20 nm), and reduction in effective surface area coupled with decreasing volume and frequency of mesopores (2-20 nm) and micropores (<2 nm). Electron tomography unraveled the three-dimensional (3D) structure with high resolution allowing visualization of meso- and macropores but with samples of maximum 300 nm thickness. To complement this, hard X-ray ptychographic tomography produced quantitative 3D electron density maps of 5 μm diameter samples with spatial resolution <50 nm, effectively filling the resolution gap between electron tomography and hard X-ray microtomography. The obtained 3D volumes are an essential input for future computational modeling of fluid dynamics, mass transport, or diffusion properties and may readily complement bulk one-dimensional porosimetry measurements or simulated porosity. (Less)

Laboratory X-ray Microtomography: Ways of Processing Experimental Data

Software is described for the preliminary processing of X-ray data that allow the spatial resolution of laboratory X-ray microtomographs to be improved.

Optimization of image quality and acquisition time for lab-based X-ray microtomography using an iterative reconstruction algorithm

Abstract Non-invasive laboratory-based X-ray microtomography has been widely applied in many industrial and research disciplines. However, the main barrier to the use of laboratory systems compared to a synchrotron beamline is its much longer image acquisition time (hours per scan compared to seconds to minutes at a synchrotron), which results in limited application for dynamic in situ processes. Therefore, the majority of existing laboratory X-ray microtomography is limited to static imaging; relatively fast imaging (tens of minutes per scan) can only be achieved by sacrificing imaging quality, e.g. reducing exposure time or number of projections. To alleviate this barrier, we introduce an optimized implementation of a well-known iterative reconstruction algorithm that allows users to reconstruct tomographic images with reasonable image quality, but requires lower X-ray signal counts and fewer projections than conventional methods. Quantitative analysis and comparison between the iterative and the conventional filtered back-projection reconstruction algorithm was performed using a sandstone rock sample with and without liquid phases in the pore space. Overall, by implementing the iterative reconstruction algorithm, the required image acquisition time for samples such as this, with sparse object structure, can be reduced by a factor of up to 4 without measurable loss of sharpness or signal to noise ratio.

Development and evaluation of an experimental protocol for 3-D visualization and characterization of the structure of bacterial biofilms in porous media using laboratory X-ray tomography

The development of a reliable model allowing accurate predictions of biofilm growth in porous media relies on a good knowledge of the temporal evolution of biofilm structure within the porous network. Since little is known about the real 3-D structure of biofilms in porous media, this work was aimed at developing a new experimental protocol to visualize the 3-D microstructure of the inside of a porous medium using laboratory X-ray microtomography. A reliable and reproducible methodology is proposed for (1) growing a biofilm inside a porous medium, and (2) X-ray tomography-based characterization of the temporal development of the biofilm at the inlet of the biofilter. The statistical analysis proposed here also validates the results presented in the literature based on a biofilm structure single measurement.

Reconstruction and quantitative characterization of the three dimensional microstructure model of TC6 titanium alloy based on dual-energy X-ray microtomography

In the present study, dual-energy micro-computed tomography (Micro-CT) imaging was employed to overcome the difficulty of low absorption contrast due to the low difference in density among the primary α phase, secondary α phase, and β phase of the annealed microstructure (annealing at 800°C for 2h followed by air cooling) of TC6 titanium alloy. The three dimensional microstructure model of TC6 titanium alloy was first achieved by laboratory X-ray microtomography, and then analyzed quantitatively. It is found that the volume fractions of the primary α phase, secondary α phase and β phase are 28.32%, 47.78% and 23.90%, respectively. Some complex microstructural features of TC6 titanium alloy such as spatial distribution, shapes, and interconnectivities that can hardly be described by the conventional two dimensional microscopy technique were successfully captured. In three dimensional space, the primary α phase is composed of discrete equiaxed grains and interconnected grains, and the fraction of the individual equiaxed grains is up to 50% and the average diameter is about 10µm; the secondary α phase interconnects with β phase forming a completely interconnected network.

Quantitative 3D characterisation of porous NiTi fabricated by self-propagating high temperature synthesis using X-ray microtomography

A porous NiTi specimen prepared by self-propagating high temperature synthesis for bone implant applications has been characterised by a laboratory X-ray microtomography instrument to reveal the three-dimensional (3D) structure of the internal porosity. The reconstructed slices obtained from the tomography scan showed open porosity as well as micropores in the matrix. The 3D renderings revealed that the open porosity is highly interconnected, tortuous structure. 3D quantitative estimates of the micropores in terms of their volume fraction, number density and size have been evaluated. Metrics have been developed based on skeletonised idealisation of the complex architecture of interconnected pores that reflect its structural properties.

Particle tracking during Ostwald ripening using time-resolved laboratory X-ray microtomography

Laboratory X-ray microtomography is investigated as a method for obtaining time-resolved images of microstructural coarsening of the semisolid state of Al–5wt.% Cu samples during Ostwald ripening. Owing to the 3D imaging capability of tomography, this technique uniquely provides access to the growth rates of individual particles, thereby not only allowing a statistical characterization of coarsening—as has long been possible by conventional metallography—but also enabling quantification of the influence of local environment on particle boundary migration. The latter information is crucial to understanding growth kinetics during Ostwald ripening at high volume fractions of the coarsening phase. Automated image processing and segmentation routines were developed to close gaps in the network of particle boundaries and to track individual particles from one annealing step to the next. The particle tracking success rate places an upper bound of only a few percent on the likelihood of segmentation errors for any given particle. The accuracy of particle size trajectories extracted from the time-resolved tomographic reconstructions is correspondingly high. Statistically averaged coarsening data and individual particle growth rates are in excellent agreement with the results of prior experimental studies and with computer simulations of Ostwald ripening.

A Regularized, Pyramidal Multi-grid Approach to Global 3D-Volume Digital Image Correlation Based on X-ray Micro-tomography

In this study a robust strategy for 3D-Volume Digital Image Correlation DIC is presented, apt to provide accurate kinematic measurements within a loaded sample on the basis of three-dimensional digital images by X-ray computed micro-tomography. In the framework of a Galerkin, finite element discretization of the displacement field, the inverse problem of estimating 3D motion inside the bulk material is solved recursively on a hierarchical family of grids, linked by suitable restriction and prolongation operators. Such structured grids are defined over an image pyramid, which is generated starting from the raw tomographic reconstructions by a reiterated application of average filters and sub-sampling operators. To achieve robust estimates of the underlying displacement fields, multi-grid cycles are performed ascending and descending along the pyramid in a selected sequence. At each scale, the least-square matching function for DIC is enriched by means of a penalty term in the spirit of Tychonoff regularization, including as a priori information the estimate achieved at the previous grid and transferred to the current scale. For each grid only one Newton iteration can be considered, implying important time savings. Results are presented concerning a laboratory X-ray micro-tomography experiment on a polymeric foam sample, subjected to loading by an apparatus ad-hoc realized.

Rectangular Beads from the Final Gravettian Level of the Abri Pataud: Raw Material Identification and its Archaeological Implications

The Final Gravettian level (level 2) of the abri Pataud (Dordogne, France) yielded a large assemblage of body ornaments that consists essentially of 85 quite standardized rectangular beads. Some uncertainty remained about the raw material in which these small beads were made: mammoth ivory, reindeer antler or bone? Non-invasive methods were employed in order to determine the raw material. First chemical analyses using microbeam Proton Induced X-ray Emission analysis (microPIXE) did not enable us to conclude definitively. Therefore, synchrotron and laboratory X-ray microtomography (microCT) were applied on eight beads and allowed us to identify ivory for all of them except for one, which shows slightly different morphological features.

Crack closure and stress intensity factor measurements in nodular graphite cast iron using three-dimensional correlation of laboratory X-ray microtomography images

Three-dimensional (3-D) tomographic images of a nodular graphite cast iron obtained using a laboratory X-ray source were used to analyze the opening of a fatigue crack during in situ mechanical loading. Direct image analysis and digital image correlation are utilized to obtain the 3-D morphology and front location of the crack, as well as the displacement fields in the bulk of the specimen. From digital image correlation results it is possible to extract the crack opening displacement (COD) map in the whole sample cross-section and to compute stress intensity factors (SIFs) all along the crack front, even for COD values that are less than the image resolution. The comparison of COD maps with local values of the SIF enabled for an estimation of the opening SIF ( K op ) equal to 6 MPa m 1/2.

Microtomographic characterization of columnar Al–Cu dendrites for fluid flow and flow stress determination

During the twin roll casting of Al alloys, the interdendritic liquid may flow as the two solidification fronts are compressed together between the rolls. This can lead to defects such as centerline segregation. To understand the flow properties of the interdendritic liquid, samples of Al–12wt.% Cu were solidified directionally in a Bridgman furnace and quenched to capture the growing columnar dendritic structures. The quenched samples were scanned using a laboratory X-ray microtomography (XMT) unit to obtain the 3D structure with a voxel resolution of 7.2μm. Image analysis was used to separate the Al dendrite from the interdendritic Al–Al2Cu eutectic. Flow between the dendrites was simulated by solving the Stokes equation to calculate the permeability tensor as a function of the fraction solid. The results were compared to prior experimental measurements and calculations using synchrotron tomography observations of equiaxed structures. Elasto–plastic finite element (FE) simulations were performed on the dendritic structures to determine flow stress behavior as a function of fraction solid. It was found that the standard approximations for the reduction in flow stress in the semi-solid have a variation in excess of 100% from that calculated using the true structure. Therefore, it is critical to simulate the actual dendrite for effective flow stress determination.

X-ray microtomography: Nondestructive three-dimensional imaging for in vitro endodontic studies

Article shows the application of a laboratory x-ray microtomography system, a miniaturized form of conventional computerized axial tomography, to the study of root canal morphologic characteristics and changes in the course of root canal treatment in extracted teeth. After reconstruction of the three-dimensional images, the IDL software package (Research Systems, Inc., Colorado) was used to obtain cross-sectional slices of the tooth and three-dimensional views of rendered surfaces of constant mineral density. The root canal systems and changes in these were imaged at a resolution (cubic voxel side-length) of ∼40 μm.