Using a high-efficiency grating interferometer for hard X rays (10-30 keV) and a phase-stepping technique, separate radiographs of the phase and absorption profiles of bulk samples can be obtained from a single set of measurements. Tomographic reconstruction yields quantitative three-dimensional maps of the X-ray refractive index, with a spatial resolution down to a few microns. The method is mechanically robust, requires little spatial coherence and monochromaticity, and can be scaled up to large fields of view, with a detector of correspondingly moderate spatial resolution. These are important prerequisites for use with laboratory X-ray sources.
High-energy-density materials that undergo conversion and/or alloying reactions hold promise for next-generation lithium (Li) ion batteries. However, these materials experience substantial volume change during electrochemical operation, which causes mechanical fracture of the material and structural disintegration of the electrode, leading to capacity loss. In this work, we use x-ray tomography during battery operation to visualize and quantify the origins and evolution of electrochemical and mechanical degradation. Tomography provides the time-resolved, three-dimensional chemical composition and morphology within individual particles and throughout the electrode. In the model material tin(II) oxide, we witness distributions in onset and rate of core-shell lithiation, crack initiation and growth along preexisting defects, and irreversible distortion of the electrode, highlighting tomography as a tool to guide the development of durable materials and strain-tolerant electrodes.
Newly developed high-speed, synchrotron-based X-ray computed microtomography enabled us to directly image pore-scale displacement events in porous rock in real time. Common approaches to modeling macroscopic fluid behavior are phenomenological, have many shortcomings, and lack consistent links to elementary porescale displacement processes, such as Haines jumps and snap-off. Unlike the common singular pore jump paradigm based on observations of restricted artificial capillaries, we found that Haines jumps typically cascade through 10-20 geometrically defined pores per event, accounting for 64% of the energy dissipation. Real-time imaging provided a more detailed fundamental understanding of the elementary processes in porous media, such as hysteresis, snapoff, and nonwetting phase entrapment, and it opens the way for a rigorous process for upscaling based on thermodynamic models.hydrology | oil recovery | multiphase flow
We report the use of synchrotron radiation X-ray tomographic microscopy (SRXTM) to obtain statistically signifi cant volume ( ∼ 700 × 700 × 70 μ m 3 ) 3D reconstructions of porous electrode microstructures of transition metal oxide based electrodes. [ 1 ] We implement a segmentation algorithm that allows identifi cation of individual particles and validate it by showing that the calculated particle size distribution (PSD) is in agreement with experimentally determined PSD obtained with laser diffraction. We study the microstructure of LiNi 1/3 Mn 1/3 Co 1/3 O 2 (NMC)-based cathodes, prepared with varying weight percent of carbon black and binder (2-5 wt%) and different compressions (0-2000 bar), and their electrochemical performance. Tomographic data (raw and processed with particles identifi ed and labeled) and the corresponding electrochemical data for 16 different cathodes is provided open source. [ 2 ] The microstructure datasets can be used to study electrode properties like porosity, tortuosity, electrode anisotropy, and homogeneity, or as realistic geometries for three dimensional (3D) electrochemical simulations. The electrochemical data is intended to aid in the verifi cation of simulation models. The large number of studied particles (approx. 7000-19000 per electrode) allows us to investigate spatially resolved PSD and shows that the vicinity of electrode boundaries is populated by smaller particles than the bulk electrode. In addition to insight into electrode morphology, we demonstrate that the technique is capable of resolving features on the sub-particle level such as particle fracture, which is observed here under high compression conditions. It is becoming increasingly clear that the development of next generation, higher performance lithium ion batteries (LIB) will require a concerted effort between experimentalists and simulation experts. In addition to the development of predictive tools for the selection of active materials, realization of LIBs with high C-rate capabilities and energy density will require the development of roadmaps for achieving favorable porous electrode microstructures. [ 3 , 4 ] However, due to the lack of publically available microstructural data on porous electrodes to date, there exists a disconnect between the experimental and simulation communities. The simulation community, despite significant advances in computation over the past decades, must rely on simplifi ed pictures of porous electrode microstructure or computer generated microstructures that bear an as-of-yet unquantifi ed relationship to real battery microstructures.While one-dimensional (1D) simulations are appealing for their simplicity and computational effi ciency, there are significant limitations. Newman-type models rely on the representation of the electrode's complexity by effective medium approximations. [ 5 ] For systems featuring a broad PSD, as often found in real LIB electrodes, the validity of the Bruggeman relation, which is widely used to estimate the electrode's tortuosity from porosity, ha...
Sub-second temporal-resolution tomographic microscopy is becoming a reality at third-generation synchrotron sources. Efficient data handling and postprocessing is, however, difficult when the data rates are close to 10 GB s À1. This bottleneck still hinders exploitation of the full potential inherent in the ultrafast acquisition speed. In this paper the fast reconstruction algorithm gridrec, highly optimized for conventional CPU technology, is presented. It is shown that gridrec is a valuable alternative to standard filtered back-projection routines, despite being based on the Fourier transform method. In fact, the regridding procedure used for resampling the Fourier space from polar to Cartesian coordinates couples excellent performance with negligible accuracy degradation. The stronger dependence of the observed signal-to-noise ratio for gridrec reconstructions on the number of angular views makes the presented algorithm even superior to filtered back-projection when the tomographic problem is well sampled. Gridrec not only guarantees high-quality results but it provides up to 20-fold performance increase, making real-time monitoring of the sub-second acquisition process a reality.
Synchrotron-based X-ray Tomographic Microscopy (SRXTM) is nowadays a powerful technique for non-destructive, high-resolution investigations of a broad kind of materials. High-brilliance and high-coherence third generation synchrotron radiation facilities allow micrometer and sub-micrometer, quantitative, three-dimensional imaging within very short time and extend the traditional absorption imaging technique to edge-enhanced and phase-sensitive measurements. At the Swiss Light Source TOMCAT, a new beamline for TOmographic Microscopy and Coherent rAdiology experimenTs, has been recently built and started regular user operation in June 2006. The new beamline get photons from a 2.9 T superbend with a critical energy of 11.1 keV. This makes energies above 20 keV easily accessible. To guarantee the best beam quality (stability and homogeneity), the number of optical elements has been kept to a minimum. A Double Crystal Multilayer Monochromator (DCMM) covers an energy range between 8 and 45 keV with a bandwidth of a few percent down to 10 −4 . The beamline can also be operated in white-beam mode, providing the ideal conditions for real-time coherent radiology. This article presents the beamline design, its optical components and the endstation. It further illustrates two recently developed phase contrast techniques and finally gives an overview of recent research topics which make intense use of SRXTM.
We present the first ex vivo images of fresh, native breast tissue obtained from mastectomy specimens using grating interferometry. This technique yields improved diagnostic capabilities when compared with conventional mammography, especially when discerning the type of malignant conversions and their breadth within normal breast tissue. These promising results advance us toward the ultimate goal, using grating interferometry in vivo on humans in a clinical setting.
According to the current view, the formation of new alveolar septa from preexisting ones ceases due to the reduction of a double- to a single-layered capillaries network inside the alveolar septa (microvasculature maturation postnatal days 14-21 in rats). We challenged this view by measuring stereologically the appearance of new alveolar septa and by studying the alveolar capillary network in three-dimensional (3-D) visualizations obtained by high-resolution synchrotron radiation X-ray tomographic microscopy. We observed that new septa are formed at least until young adulthood (rats, days 4-60) and that roughly half of the new septa are lifted off of mature septa containing single-layered capillary networks. At the basis of newly forming septa, we detected a local duplication of the capillary network. We conclude that new alveoli may be formed in principle at any time and at any location inside the lung parenchyma and that lung development continues into young adulthood. We define two phases during developmental alveolarization. Phase one (days 4-21), lifting off of new septa from immature preexisting septa, and phase two (day 14 through young adulthood), formation of septa from mature preexisting septa. Clinically, our results ask for precautions using drugs influencing structural lung development during both phases of alveolarization.
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