A comparative study of X-ray tomographic microscopy on shales at different synchrotron facilities: ALS, APS and SLS.

Synchrotron radiation X-ray tomographic microscopy (SRXTM) was used to characterize the three-dimensional microstructure, geometry and distribution of different phases in two shale samples obtained from the North Sea (sample N1) and the Upper Barnett Formation in Texas (sample B1). Shale is a challenging material because of its multiphase composition, small grain size, low but significant amount of porosity, as well as strong shape- and lattice-preferred orientation. The goals of this round-robin project were to (i) characterize microstructures and porosity on the micrometer scale, (ii) compare results measured at three synchrotron facilities, and (iii) identify optimal experimental conditions of high-resolution SRXTM for fine-grained materials. SRXTM data of these shales were acquired under similar conditions at the Advanced Light Source (ALS) of Lawrence Berkeley National Laboratory, USA, the Advanced Photon Source (APS) of Argonne National Laboratory, USA, and the Swiss Light Source (SLS) of the Paul Scherrer Institut, Switzerland. The data reconstruction of all datasets was handled under the same procedures in order to compare the data quality and determine phase proportions and microstructures. With a 10× objective lens the spatial resolution is approximately 2 µm. The sharpness of phase boundaries in the reconstructed data collected from the APS and SLS was comparable and slightly more refined than in the data obtained from the ALS. Important internal features, such as pyrite (high-absorbing), and low-density features, including pores, fractures and organic matter or kerogen (low-absorbing), were adequately segmented on the same basis. The average volume fractions of low-density features for sample N1 and B1 were estimated at 6.3 (6)% and 4.5 (4)%, while those of pyrite were calculated to be 5.6 (6)% and 2.0 (3)%, respectively. The discrepancy of data quality and volume fractions were mainly due to different types of optical instruments and varying technical set-ups at the ALS, APS and SLS

Scalable Freeze-Tape-Casting Fabrication and Pore Structure Analysis of 3D LLZO Solid-State Electrolytes.

Nonflammable solid-state electrolytes can potentially address the reliability and energy density limitations of lithium-ion batteries. Garnet-structured oxides such as Li7La3Zr2O12 (LLZO) are some of the most promising candidates for solid-state devices. Here, three-dimensional (3D) solid-state LLZO frameworks with low tortuosity pore channels are proposed as scaffolds, into which active materials and other components can be infiltrated to make composite electrodes for solid-state batteries. To make the scaffolds, we employed aqueous freeze tape casting (FTC), a scalable and environmentally friendly method to produce porous LLZO structures. Using synchrotron radiation hard X-ray microcomputed tomography, we confirmed that LLZO films with porosities of up to 75% were successfully fabricated from slurries with a relatively wide concentration range. The acicular pore size and shape at different depths of scaffolds were quantified by fitting the pore shapes with ellipses, determining the long and short axes and their ratios, and investigating the equivalent diameter distribution. The results show that relatively homogeneous pore sizes and shapes were sustained over a long range along the thickness of the scaffold. Additionally, these pores had low tortuosity and the wall thickness distributions were found to be highly homogeneous. These are desirable characteristics for 3D solid electrolytes for composite electrodes, in terms of both the ease of active material infiltration and also minimization of Li diffusion distances in electrodes. The advantages of the FTC scaffolds are demonstrated by the improved conductivity of LLZO scaffolds infiltrated with poly(ethylene oxide)/lithium bis(trifluoromethanesulfonyl)imide (PEO/LITFSI) compared to those of PEO/LiTFSI films alone or composites containing LLZO particles

Lithium Dendrite Growth in Glassy and Rubbery Nanostructured Block Copolymer Electrolytes

Enabling the use of lithium metal anodes is a critical step required to dramatically increase the energy density of rechargeable batteries. However, dendrite growth in lithium metal batteries, and a lack of fundamental understanding of the factors governing this growth, is a limiting factor preventing their adoption. Herein we present the effect of battery cycling temperature, ranging from 90 to 120°C, on dendrite growth through a polystyrene-block-poly(ethylene oxide)-based electrolyte. This temperature range encompasses the glass transition temperature of polystyrene (107°C). A slight increase in the cycling temperature of symmetric lithium-polymer-lithium cells from 90 to 105°C results in a factor of five decrease in the amount of charge that can be passed before short circuit. Synchrotron hard X-ray microtomography experiments reveal a shift in dendrite location from primarily within the lithium electrode at 90°C, to primarily within the electrolyte at 105°C. Rheological measurements show a large change in mechanical properties over this temperature window. Time-temperature superposition was used to interpret the rheological data. Dendrite growth characteristics and cell lifetimes correlate with the temperature-dependent shift factors used for time-temperature superposition. Our work represents a step toward understanding the factors that govern lithium dendrite growth in viscoelastic electrolytes

X-ray Micro-Tomography of Ablative Heat Shield Materials

X-ray micro-tomography is a non-destructive characterization technique that allows imaging of materials structures with voxel sizes in the micrometer range. This level of resolution makes the technique very attractive for imaging porous ablators used in hypersonic entry systems. Besides providing a high fidelity description of the material architecture, micro-tomography enables computations of bulk material properties and simulations of micro-scale phenomena. This presentation provides an overview of a collaborative effort between NASA Ames Research Center and Lawrence Berkeley National Laboratory, aimed at developing micro-tomography experiments and simulations for porous ablative materials. Measurements are carried using x-rays from the Advanced Light Source at Berkeley Lab on different classes of ablative materials used in NASA entry systems. Challenges, strengths and limitations of the technique for imaging materials such as lightweight carbon-phenolic systems and woven textiles are discussed. Computational tools developed to perform numerical simulations based on micro-tomography are described. These enable computations of material properties such as permeability, thermal and radiative conductivity, tortuosity and other parameters that are used in ablator response models. Finally, we present the design of environmental cells that enable imaging materials under simulated operational conditions, such as high temperature, mechanical loads and oxidizing atmospheres.Keywords: Micro-tomography, Porous media, Ablatio

Observation of two-dimensional yttrium oxide nanoparticles in mealworm beetles ( Tenebrio molitor )

Nanomaterials are being used in medicine, manufacturing and consumer products, but their effects on organisms and the environment are not well understood because of the difficulty in detecting them. Here dual-energy X-rayK-edge subtraction was used to track two-dimensional yttrium oxide nanoparticles (which can be found in such household objects as color televisions) in adult mealworms (Tenebrio molitor). The insects ingested nanoparticle-infused feed for different time periods, up to 24 h, and the nanoparticles could then be identified at several locations in the insects' head, thorax and abdomen, mostly within the digestive tract. In time, all particles were excreted.</jats:p

X-Ray Micro-Tomography Applied to Nasa's Materials Research: Heat Shields, Parachutes and Asteroids

X-ray micro-tomography is used to support the research on materials carried out at NASA Ames Research Center. The technique is applied to a variety of applications, including the ability to characterize heat shield materials for planetary entry, to study the Earth- impacting asteroids, and to improve broadcloths of spacecraft parachutes. From micro-tomography images, relevant morphological and transport properties are determined and validated against experimental data

A New Approach To Light-Weight Ablators Analysis: From Micro-Tomography Measurements to Statistical Analysis and Modeling

The morphology characteristics and ablation behavior of a highly porous carbon fiber preform are studied using a combined experimental/numerical approach. Morphological characterization of the three-dimensional structure of the material is performed by hard X-rays synchrotron micro-tomography at the Advanced Light Source of Lawrence Berkeley National Laboratory. The resulting micro-tomography voxels are used to compute geometrical properties of the carbon preform, like porosity, specific surface area and tortuosity, that are otherwise indirectly measured through experimental techniques. The reconstructed volumes are used to build a computational grid for numerical simulations of the fibers\u27 ablation. By modeling the diffusion of oxygen through the porous medium using Lagrangian methods, and the oxidation at the carbon fibers\u27 surface using a reactivity model, the ablation of the carbon fibers are simulated for a range of Thiele numbers. It is shown that in the diffusion limited regime (large Thiele number), the ablation of the fibers occurs at the surface of the material. In the reaction limited regime (low Thiele number), the oxygen penetrates into the fibers, resulting in volumetric ablation and high material spallation

Observation of yttrium oxide nanoparticles in cabbage (Brassica oleracea) through dual energy K-edge subtraction imaging

BACKGROUND: The potential transfer of engineered nanoparticles (ENPs) from plants into the food chain has raised widespread concerns. In order to investigate the effects of ENPs on plants, young cabbage plants (Brassica oleracea) were exposed to a hydroponic system containing yttrium oxide (yttria) ENPs. The objective of this study was to reveal the impacts of NPs on plants by using K-edge subtraction imaging technique. RESULTS: Using synchrotron dual-energy X-ray micro-tomography with K-edge subtraction technique, we studied the uptake, accumulation, distribution and concentration mapping of yttria ENPs in cabbage plants. It was found that yttria ENPs were uptaken by the cabbage roots but did not effectively transferred and mobilized through the cabbage stem and leaves. This could be due to the accumulation of yttria ENPs blocked at primary-lateral-root junction. Instead, non-yttria minerals were found in the xylem vessels of roots and stem. CONCLUSIONS: Synchrotron dual-energy X-ray micro-tomography is an effective method to observe yttria NPs inside the cabbage plants in both whole body and microscale level. Furthermore, the blockage of a plant’s roots by nanoparticles is likely the first and potentially fatal environmental effect of such type of nanoparticles

High resolution fluorescence bio-imaging upconversion nanoparticles in insects

Imaging fluorescent markers with brightness, photostability, and continuous emission with auto fluorescence background suppression in biological samples has always been challenging due to limitations of available and economical techniques. Here we report a new approach, to achieve high contrast imaging inside small and difficult biological systems with special geometry such as fire ants, an important agricultural pest, using a homemade cost-effective optical system. Unlike the commonly used rare-earth doped fluoride nanoparticles, we utilized nanoparticles with a high upconversion efficiency in water. Specifically Y_2O_3:Er^(+3),Yb^(+3) nanoparticles (40-50 nm diameter) were fed to fire ants as food and then a simple illuminating experiment was conducted at 980 nm wavelength at relatively low pump intensity 8 kW.cm^(−2). The locations were further confirmed by X-ray tomography, where most particles aggregated inside the ant’s mouth. High resolution, fast, and economical optical imaging system opens the door for studying more complex biological system