High speed synchrotron X-ray imaging and ultrafast tomography were used to study in situ and in real time the fragmentation and growth dynamics of dendritic microstructures of an Al-15%Cu alloy in solidification under ultrasound. An ultrasound of 30 kHz with vibration amplitude of 29 mu m was applied into the alloy melt and produced a strong swirling acoustic flow of similar to 0.3 m/s. Efficient dendrite fragmentation occurred due to the acoustic flow and the dominant mechanism is the thermal perturbation remelting plus mechanical fracture and separation effect. Acoustic flow fatigue impact and phase collision effects were found to play a minor role in causing dendrite fragmentation. Just 10 s of ultrasound application at the early stage of solidification produced similar to 100% more dendrite fragments compared to the case without ultrasound, resulting in 20 similar to 25% reduction in the average grain size in the solidified samples. Furthermore, the dendrite morphology and tip growth velocity were mainly affected by the initial dendrite fragment number density and their distribution. The systematic and real-time datasets obtained in near operando conditions provided valuable 4D information for validation of numerical models and assistance in developing optimisation strategy for ultrasound melt processing in industry. (C) 2021 The Authors. Published by Elsevier Ltd on behalf of Acta Materialia Inc. This is an open access article under the CC BY license (http://creativecommons.org/licenses/by/4.0/ )

PURPOSE:Subcutaneously or intramuscularly administered biodegradable microsphere formulations have been successfully exploited in the management of chronic conditions for over two decades, yet mechanistic understanding of the impact of formulation attributes on in vivo absorption rate from such systems is still in its infancy.METHODS:Suspension formulation physicochemical attributes may impact particulate deposition in subcutaneous (s.c.) tissue. Hence, the utility of synchrotron X-ray micro-computed tomography (μCT) for assessment of spatial distribution of suspension formulation components (PLG microspheres and vehicle) was evaluated in a porcine s.c. tissue model. Optical imaging of dyed vehicle and subsequent microscopic assessment of microsphere deposition was performed in parallel to compare the two approaches.RESULTS:Our findings demonstrate that synchrotron μCT can be applied to the assessment of microsphere and vehicle distribution in s.c. tissue, and that microspheres can also be visualised in the absence of contrast agent using this approach. The technique was deemed superior to optical imaging of macrotomy for the characterisation of microsphere deposition owing to its non-invasive nature and relatively rapid data acquisition time.CONCLUSIONS:The method outlined in this study provides a proof of concept feasibility for μCT application to determining the vehicle and suspended PLG microspheres fate following s.c. injection. A potential application for our findings is understanding the impact of injection, device and formulation variables on initial and temporal depot geometry in pre-clinical or ex-vivo models that can inform product design. Graphical abstract.

Synchrotron X-ray microtomography and skeletonisation method were used to study the true 3D network structures and morphologies of the Fe-rich intermetallic phases in recycled Al-5.0%Cu-0.6%Mn alloys with 0.5% and 1.0% Fe. It was found that, the Fe-phases in the 1.0%Fe alloy have node lengths of 5–25 μm; while those in the 0.5%Fe alloy are of 3–17 μm. The Fe-phases in the 1.0%Fe alloy also developed sharper mean curvature with wider distribution than those in the 0.5%Fe alloy. Combining SEM studies of the deeply-etched samples, the true 3D structures of 4 different type Fe phases in both alloys are also revealed and demonstrated.

Small angle x-ray scattering has been proven to be a valuable method for accessing structural information below the spatial resolution limit implied by direct imaging. Here, we theoretically derive the relation that links the subpixel differential phase signal provided by the sample to the moments of scattering distributions accessible by refraction sensitive x-ray imaging techniques. As an important special case we explain the scatter or dark-field contrast in terms of the sample's phase signal. Further, we establish that, for binary phase objects, the $n$th moment scales with the difference of the refractive index decrement to the power of $n$. Finally, we experimentally demonstrate the utility of the moments by quantitatively determining the particle sizes of a range of powders with a laboratory-based setup.

Segmentation is the process of isolating specific regions or objects within an imaged volume, so that further study can be undertaken on these areas of interest. When considering the analysis of complex biological systems, the segmentation of three-dimensional image data is a time consuming and labor intensive step. With the increased availability of many imaging modalities and with automated data collection schemes, this poses an increased challenge for the modern experimental biologist to move from data to knowledge. This publication describes the use of SuRVoS Workbench, a program designed to address these issues by providing methods to semi-automatically segment complex biological volumetric data. Three datasets of differing magnification and imaging modalities are presented here, each highlighting different strategies of segmenting with SuRVoS. Phase contrast X-ray tomography (microCT) of the fruiting body of a plant is used to demonstrate segmentation using model training, cryo electron tomography (cryoET) of human platelets is used to demonstrate segmentation using super- and megavoxels, and cryo soft X-ray tomography (cryoSXT) of a mammalian cell line is used to demonstrate the label splitting tools. Strategies and parameters for each datatype are also presented. By blending a selection of semi-automatic processes into a single interactive tool, SuRVoS provides several benefits. Overall time to segment volumetric data is reduced by a factor of five when compared to manual segmentation, a mainstay in many image processing fields. This is a significant savings when full manual segmentation can take weeks of effort. Additionally, subjectivity is addressed through the use of computationally identified boundaries, and splitting complex collections of objects by their calculated properties rather than on a case-by-case basis.

X-ray phase contrast enables weakly-attenuating structures to be imaged, with bright synchrotron sources adding the ability to capture time sequences and analyse sample dynamics. Here, we describe the translation of dynamical differential phase contrast imaging from the synchrotron to a compact x-ray source, in order to achieve this kind of time sequence imaging in the laboratory. We formulate broadly-applicable set-up guidelines for the single-grid, single-exposure imaging technique using a divergent source, exploring the experimental factors that restrict set-up size, imaging sensitivity and sample size. Experimental images are presented using the single-grid phase contrast technique with a steel attenuation grid and a liquid-metal-jet x-ray source, enabling exposure times as short as 0.5 s for dynamic imaging. Differential phase contrast images were retrieved from phantoms, incorporating noise filtering to improve the low-count images encountered when imaging dynamics using short exposures.

Data-constrained modeling is a method that enables three-dimensional distribution of mineral phases and porosity in a sample to be modeled based on micro-computed tomography scans acquired at different X-ray energies. Here we describe an alternative method for measuring porosity, synchrotron K-edge subtraction using xenon gas as a contrast agent. Results from both methods applied to the same Darai limestone sample are compared. Reasonable agreement between the two methods and with other porosity measurements is obtained. The possibility of a combination of data-constrained modeling and K-edge subtraction methods for more accurate sample characterization is discussed.

Floods can completely submerge terrestrial plants but some wetland species can sustain O2 and CO2 exchange with the environment via gas films forming on superhydrophobic leaf surfaces. We used high resolution synchrotron X-ray phase contrast micro-tomography in a novel approach to visualise gas films on submerged leaves of common cordgrass (Spartina anglica). 3D tomograms enabled a hitherto unmatched level of detail regarding the micro-topography of leaf gas films. Gas films formed only on the superhydrophobic adaxial leaf side (water droplet contact angle, Φ=162°) but not on the abaxial side (Φ=135°). The adaxial side of the leaves of common cordgrass is plicate with a longitudinal system of parallel grooves and ridges and the vast majority of the gas film volume was found in large ∼180μm deep elongated triangular volumes in the grooves and these volumes were connected to each neighbouring groove via a fine network of gas tubules (∼1.7μm diameter) across the ridges. In addition to the gas film retained on the leaf exterior, the X-ray phase contrast micro-tomography also successfully distinguished gas spaces internally in the leaf tissues, and the tissue porosity (gas volume per unit tissue volume) ranged from 6.3% to 20.3% in tip and base leaf segments, respectively. We conclude that X-ray phase contrast micro-tomography is a powerful tool to obtain quantitative data of exterior gas features on biological samples because of the significant difference in electron density between air, biological tissues and water.

Pore-scale events in multiphase flow in porous rock have been directly imaged in real time by using fast (15 to 60 seconds) synchrotron-based X-ray computed microtomography. In the past, pore-scale fluid displacements in porous media could only be imaged under quasistatic conditions where at scanning times of several minutes to hours, fluid distributions were subject to capillary redistribution. Here, pore-scale displacement events in porous rock were imaged in situ in real time in natural rock under dynamic flow conditions, where the pressure gradient and the viscocapillary balance were maintained during scanning. Two elementary processes, Haines jumps in drainage and snap-off in imbibition, were studied in detail for sintered glass, sandstone, and carbonate rock. We found that most Haines jump events do not displace the wetting phase pore-by-pore, but typically involve 10 to 20 individual pores and that filling events are cooperative. We also found that in sandstone rock 64% of the externally applied work is actually dissipated during these jumps and approximately 36% is converted into interfacial energy.

For dynamic samples and/or for simple ease-of-use experiments, single-image phase contrast tomography is a very effective method for the 3D visualization of materials which would otherwise be indiscernible in attenuation based x-ray imaging. With binary samples (e.g. air-material) and monochromatic wavefields a transport-of-intensity (TIE)-based phase retrieval algorithm is known to retrieve accurate quantitative maps of the phase distribution. For mixed material samples and/or white beam radiation the algorithm can still produce useful qualitative tomographic reconstructions with significantly improved area contrast. The stability of the algorithm comes with a recognized associated loss of spatial resolution due to its essential behaviour as a low-pass filter. One possible answer to this is an image fusion technique that merges the slices reconstructed from raw phase contrast images and those after phase retrieval, where the improved contrast may be acquired without the associated loss of high-frequency information. We present this technique as a simple few-parameter Fourier method, which is easily tunable and highly compatible with current reconstruction steps.

A data-constrained modelling (DCM) approach has been developed at CSIRO, which enables 3D characterisation of pores and mineral phase distributions using quantitative multi-energy synchrotron CT. For a tight reservoir, such as a carbonate limestone or a shale rock, DCM can generate microscopic partial volume distributions of materials and pores which are the effects of the fine length scales below X-ray CT resolution. Using this information, a quantitative relation between recoverable reserve and pore-throat size can be established for a rock sample. The technique can also be used for characterisation of other unconventional reservoir rocks.

In this report we show that synchrotron X-ray radiography is a powerful method to study liquid-air interface penetration through opaque microtextured surface roughness, leading to wetting transition. We investigate this wetting phenomenon in the context of sessile drop evaporation, and establish that liquid interface sinking into the surface texture is indeed dictated by the balance of capillary and Laplace pressures, where the intrinsically three-dimensional nature of the meniscus must be accounted for. Air bubble entrapment in the texture underneath impacting water drops is also visualized and the mechanisms of post-impact drop evaporation are discussed.

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 pore-scale 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, snap-off, and nonwetting phase entrapment, and it opens the way for a rigorous process for upscaling based on thermodynamic models.

In order to better understand the two phase properties of the porous GDL, the liquid water pattern and local saturation in the Toray 060 gas diffusion layer (GDL) is visualized in-situ in cells close to the optimal performance point at 80 {degree sign}C by X-ray tomographic microscopy. A recording time of about 10 s is achieved. At the optimal performance point (dew point of reactant gases 74 {degree sign}C) the water volume fraction observed depends on the rib width. A variation of {plus minus} 8 {degree sign}C of the feed gas dew point leads to significant saturation and performance changes. For different current densities the water volume fraction and permeability of the liquid phase of the cathode are determined and analyzed.

Starting from subfreezing temperatures presents a challenge for PEFC since ice may form in the gas flow channel, gas diffusion layer and catalyst layer and restrict the gas transport. Under non-isothermal conditions, a start-up is successful if the cell temperature rises above 0°C before freezing occurs. Under isothermal conditions below 0°C cells operate for a certain time followed by a sudden drop in power. The distribution of liquid/solid water during an isothermal start at subfreezing temperatures is quantitatively mapped by means of X-ray tomographic microscopy to improve understanding the circumstances at the phase transition and its effects on gas diffusion. Evidence was found that the produced water is in supercooled state at -10 °C initially and the drop of power is associated with freezing of the water in the cell at a GDL saturation of 20 to 30%.

Phase contrast x-ray imaging (PCXI) is a promising imaging modality, capable of sensitively differentiating soft tissue structures at high spatial resolution. However, high sensitivity often comes at the cost of a long exposure time or multiple exposures per image, limiting the imaging speed and possibly increasing the radiation dose. Here, we demonstrate a PCXI method that uses a single short exposure to sensitively capture sample phase information, permitting high speed x-ray movies and live animal imaging. The method illuminates a checkerboard phase grid to produce a fine grid-like intensity reference pattern at the detector, then spatially maps sample-induced distortions of this pattern to recover differential phase images of the sample. The use of a phase grid is an improvement on our previous absorption grid work in two ways. There is minimal loss in x-ray flux, permitting faster imaging, and, a very fine pattern is produced for homogenous high spatial resolution. We describe how this pattern permits retrieval of five images from a single exposure; the sample phase gradient images in the horizontal and vertical directions, a projected phase depth image, an edge-enhanced image, and a type of scattering image. Finally, we describe how the reconstruction technique can achieve subpixel distortion retrieval and study the behavior of the technique in regard to analysis technique, Talbot distance, and exposure time.

In near-field imaging with partially coherent x-rays, the phase shifting properties of the sample are encoded in the diffraction fringes that appear as an additional intensity modulation in the x-ray projection images. These Fresnel fringes are often regarded as purely an enhancement of the visibility at the interfaces. We show that retrieving the phase information contained in these patterns significantly advances the developments in fast micro-tomography. Improving temporal resolution without intensifying radiation damage implies a shortening of the exposure time rather than increasing the photon flux on the sample. Phase retrieval, to a large extent, compensates the consequent photon count moderation in the images, by fully exploiting the stronger refraction effect as compared with absorption. Two single-distance phase retrieval methods are evaluated for the case of an in situ 3 Hz micro-tomography of a rapidly evolving liquid foam, and an in vivo 6 Hz micro-tomography of a blowfly. A new dual-detector setup is introduced for simultaneous acquisition of two near-field diffraction patterns. Our goal is to couple high temporal, spatial and density resolution in a single imaging system in a dose-efficient manner, opening further options for dynamic four-dimensional studies.

Phase contrast imaging has been demonstrated to be advantageous in revealing detailed structures inside biological specimens without contrast agents. Grating-based differential phase contrast (DPC) and in-line phase contrast (ILPC) X-ray imaging are the two modalities frequently used at the beamline of TOmographic Microscopy and Coherent rAdiology experimenTs (TOMCAT) at the Swiss Light Source (SLS). In this paper, we preliminarily compared the abilities of two types of phase contrast imaging in distinguishing micro structures in mouse kidneys. The 3D reconstructions showed that the microstructures in kidney, such as micro vessels and renal tubules, were displayed clearly with both imaging modalities. The two techniques may be viewed as complementary. For larger features with very small density variations DPC is the desirable method. In cases where dose and time limits may prohibit the multiple steps required for DPC, and when the focus is on finer features, the ILPC method may be considered as a more viable alternative. Moreover, high resolution ILPC images are comparable with histological results.

Rats display little to no haversian remodeling of cortical bone. This fact, combined with the endochondral formation of cortical bone, means that rat femoral cortical bone contains highly mineralized cartilage islands in a central band of mid-femoral cross sections. We demonstrate that these islands have a significantly higher degree of mineralization than the surrounding bone, using quantitative backscattered electron imaging. The cartilaginous nature of the islands was verified by immunostaining for collagen type II. Toluidine blue staining of longitudinal sections and three-dimensional synchrotron radiation X-ray tomographic microscopy confirmed that the islands are elongated along the femoral long axis. Nanoindentation revealed significantly higher values of both reduced modulus and hardness in the islands compared to the surrounding bone, reflecting a higher degree of mineralization. The calcified cartilage islands were distributed in a central zone of the bone, from the growth plates through the mid-femoral bone. The presence of these cartilage islands and their possible effect on mechanical properties could be an additional reason why haversian remodeling is observed in higher-order species.

In this work, we used two techniques to study the deformation-induced whitening phenomenon that occurs when certain semicrystalline polymers (SCPs) are subjected to tensile drawing: (1) IPLST (Incoherent Polarized Steady Light Transport) was used for characterizing the light scatterers and in particular for determining their size. (2) SRXTM (Synchrotron Radiation X-Ray Tomographic Microscopy) was used to visualize the internal structure of the deformed SCPs. In particular, with this technique the possible presence of micrometric cavities can be detected. In the early whitening stage of a cavitating polypropylene (PP), the IPLST technique was found to show that the size of the light scatterers is larger than 1 m. At the same time, the SRXTM measurements showed that no void larger than 1 m was present in the material. The micrometric light scatterers responsible for the whitening phenomenon may thus not be simple cavities. In fact, this experimental study suggests that they correspond to areas where smaller objects (possibly nanovoids) are highly confined. At the scale of visible wavelengths, these regions could scatter visible light like individual entities of micrometric size. The study also showed that the size of cavities observable using SRXTM for a very deformed PP is dependent on the initial dimensions of the spherulites. Results previously obtained for a non-cavitating high density polyethylene are also briefly presented in this article to confirm the theory that deformation-induced-whitening phenomenon may have various origins for such complex microstructuring. (c) 2013 Wiley Periodicals, Inc. J Polym Sci Part B: Polym Phys., 2013, 51, 826-841