Journal articles on the topic 'In Situ X Ray Nano Tomography'
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1
Vanpeene, Victor, Isaac Martens, Jakub Drnec, Tobias Schulli, Ennio Capria, and Julie Villanova. "In Situ X-Ray Nano-Tomography at ID16B: A Practical Guide to Battery Analysis." ECS Meeting Abstracts MA2022-01, no. 1 (July 7, 2022): 119. http://dx.doi.org/10.1149/ma2022-011119mtgabs.
Abstract:
The past decade faced with rapid development of electric vehicles, portable electronic devices and green energy production, in which lithium-ion batteries (LiBs) technology plays a key role. In this context, extensive research has been made for increasing their energy density along with power density. This challenge requires pushing forward the resolution limits to probe degradation phenomena occurring at the active material level for a deeper understanding of the batter failure mechanism. In this context, X-ray techniques have been intensively used to probe in details the morphological/chemical evolution along cycling of various battery materials. For instance, X-ray computed tomography brings valuable 3D information for material structural analysis at scale ranging from the micrometre to the nanometre. High flux and high coherent X-ray nano-beams provided by the synchrotron sources, combined with the fast acquisition obtained thanks to the new generation of cMOS detectors, make it possible to carry out in situ and operando measurements at the nano-scale to 3D monitor dynamic phenomena. These developments present a real interest for the energy storage applications. This presentation will focus on the hard X-ray nano-tomography set-up developed at the ID16B beamline of the ESRF and its applications toward operando measurements applied to different case studies related to energy materials. This will be discussed as well in regards to the benefits and limitations brought by the extremely brilliant X-ray source EBS developed at the ESRF.
2
Antonelli, Stephen, Arthur Ronne, Insung Han, Mingyuan Ge, Bobby Layne, Ashwin J. Shahani, Kazuhiro Iwamatsu, et al. "Versatile compact heater design for in situ nano-tomography by transmission X-ray microscopy." Journal of Synchrotron Radiation 27, no. 3 (April 16, 2020): 746–52. http://dx.doi.org/10.1107/s1600577520004567.
Abstract:
A versatile, compact heater designed at National Synchrotron Light Source-II for in situ X-ray nano-imaging in a full-field transmission X-ray microscope is presented. Heater design for nano-imaging is challenging, combining tight spatial constraints with stringent design requirements for the temperature range and stability. Finite-element modeling and analytical calculations were used to determine the heater design parameters. Performance tests demonstrated reliable and stable performance, including maintaining the exterior casing close to room temperature while the heater is operating at above 1100°C, a homogenous heating zone and small temperature fluctuations. Two scientific experiments are presented to demonstrate the heater capabilities: (i) in situ 3D nano-tomography including a study of metal dealloying in a liquid molten salt extreme environment, and (ii) a study of pore formation in icosahedral quasicrystals. The progression of structural changes in both studies were clearly resolved in 3D, showing that the new heater enables powerful capabilities to directly visualize and quantify 3D morphological evolution of materials under real conditions by X-ray nano-imaging at elevated temperature during synthesis, fabrication and operation processes. This heater design concept can be applied to other applications where a precise, compact heater design is required.
3
Daemi, S. R., X. Lu, D. Sykes, J. Behnsen, C. Tan, A. Palacios-Padros, J. Cookson, et al. "4D visualisation of in situ nano-compression of Li-ion cathode materials to mimic early stage calendering." Materials Horizons 6, no. 3 (2019): 612–17. http://dx.doi.org/10.1039/c8mh01533c.
4
Costa, G. S. R., G. J. Q. Vasconcelos, and N. L. Archilha. "Fluid Injection System for X-ray Tomography Experiments." Journal of Physics: Conference Series 2380, no. 1 (December 1, 2022): 012110. http://dx.doi.org/10.1088/1742-6596/2380/1/012110.
Abstract:
Abstract Due to recent developments on synchrotron sources, time-resolved experiments are favored by fourth-generation machines. In particular, X-ray tomography beamlines can now perform complete experiments in less than one second. MOGNO, the nano and microtomography beamline at Sirius, is designed for in situ and operando experiments. The first designed and tested environmental cell is a complete injection system for porous media materials. This system is composed by a flow cell with fluid injection control and pressure feedback. The cell can be used for experiments with pore pressure up to 750 PSI. To increase the autonomy of the injection system, three syringe pumps with a volume of 15 ml are used, and the flow control is done through three independent step motors, and can vary between 30 to 10,000 µl/minute. A web application was developed to allow MOGNO users to easily control the system and read the pressure feedback.
5
Liu, Xiaoyang, Kaustubh Bawane, Yang Liu, Mingyuan Ge, Xiaoyin Zheng, Arthur Ronne, Anna Plonka, et al. "Revealing 3D Morphological Evolution and Reaction Kinetics of Metals and Alloys in Molten Salts Via Synchrotron X-Ray Nano-Tomography and Multimodal Studies." ECS Meeting Abstracts MA2022-02, no. 55 (October 9, 2022): 2057. http://dx.doi.org/10.1149/ma2022-02552057mtgabs.
Abstract:
The use of molten salts for large-scale solar concentrated power plants and molten salt reactors has been driving the research to better understand how metals and alloys interact with the molten salt. As the metals may undergo morphological, chemical, and structural change in molten salt environments, it is critical to understand the fundamental mechanisms in these changes. In this work, we will present how we utilized synchrotron X-ray nano-tomography to better understand the 3D morphological evolution of Ni, Cr, and their alloys in molten salt. The effects of temperature and additives in the salt on the morphological evolution will be discussed. At the higher temperature, a characteristic bicontinuous structure can form from molten salt dealloying a binary alloy. [1] This contrasts to the intergranular corrosion found in the same system reacted at a lower temperature. [2] Different additives in the salt were also found to alter the morphological changes of the alloys and can create planar corrosion, percolation dealloying, or redeposition. To complement the morphological studies by X-ray nano-tomography, a suite of X-ray and electron microscopy analyses were also carried out to better understand the chemical and structural (both short-and long-range ordering) evolution. Taking it as a multimodal approach, we will discuss how we couple the analysis from synchrotron operando X-ray absorption spectroscopy, diffraction, and imaging, as well as the multiscale imaging studies from both X-ray and electron microscopy. This work was supported as part of the Molten Salts in Extreme Environments (MSEE) Energy Frontier Research Center (EFRC), funded by the U.S. Department of Energy, Office of Science. References: [1] "Formation of three-dimensional bicontinuous structures via molten salt dealloying studied in real-time by in situ synchrotron X-ray nano-tomography" Xiaoyang Liu, Arthur Ronne*, Lin-Chieh Yu, Yang Liu, Mingyuan Ge, Cheng-Hung Lin, Bobby Layne, Phillip Halstenberg, Dmitry S. Maltsev, Alexander S. Ivanov, Stephen Antonelli, Sheng Dai, Wah-Keat Lee, Shannon M. Mahurin, Anatoly I. Frenkel, James F. Wishart, Xianghui Xiao & Yu-chen Karen Chen-Wiegart* Nature Communications (2021), DOI: 10.1038/s41467-021-23598-8 [2] "Visualizing time-dependent microstructural and chemical evolution during molten salt corrosion of Ni-20Cr model alloy using correlative quasi in situ TEM and in situ synchrotron X-ray nano-tomography" Kaustubh Bawane, Xiaoyang Liu, Ruchi Gakhar, Michael Woods, Mingyuan Ge, Xianghui Xiao, Wah-Keat Lee, Philip Halstenberg, Sheng Dai, Shannon Mahurin, Simon M. Pimblott, James F. Wishart, Yu-chen Karen Chen-Wiegart*, Lingfeng He* Corrosion Science (2021), DOI: 10.1016/j.corsci.2021.109962
6
Shapovalov, Viktor, Kristina Kutukova, Sebastian Maletti, Christian Heubner, Vera Butova, Igor Shukaev, Alexander Guda, Alexander Soldatov, and Ehrenfried Zschech. "Laboratory X-ray Microscopy Study of Microcrack Evolution in a Novel Sodium Iron Titanate-Based Cathode Material for Li-Ion Batteries." Crystals 12, no. 1 (December 21, 2021): 3. http://dx.doi.org/10.3390/cryst12010003.
Abstract:
The long-term performance of batteries depends strongly on the 3D morphology of electrode materials. Morphological changes, i.e., particle fracture and surface deterioration, are among the most prominent sources of electrode degradation. A profound understanding of the fracture mechanics of electrode materials in micro- and nanoscale dimensions requires the use of advanced in situ and operando techniques. In this paper, we demonstrate the capabilities of laboratory X-ray microscopy and nano X-ray computed tomography (nano-XCT) for the non-destructive study of the electrode material’s 3D morphology and defects, such as microcracks, at sub-micron resolution. We investigate the morphology of Na0.9Fe0.45Ti1.55O4 sodium iron titanate (NFTO) cathode material in Li-ion batteries using laboratory-based in situ and operando X-ray microscopy. The impact of the morphology on the degradation of battery materials, particularly the size- and density-dependence of the fracture behavior of the particles, is revealed based on a semi-quantitative analysis of the formation and propagation of microcracks in particles. Finally, we discuss design concepts of the operando cells for the study of electrochemical processes.
7
Chen, Liang, Lihui Wu, Yu Liu, and Wei Chen. "In situ observation of void evolution in 1,3,5-triamino-2,4,6-trinitrobenzene under compression by synchrotron radiation X-ray nano-computed tomography." Journal of Synchrotron Radiation 27, no. 1 (January 1, 2020): 127–33. http://dx.doi.org/10.1107/s1600577519014309.
Abstract:
The formation and development of voids in 1,3,5-triamino-2,4,6-trinitrobenzene crystals under compression were characterized in situ by X-ray nano-computed tomography. Benefiting from high spatial resolution (30 nm) and excellent imaging contrast, the X-ray nano-computed tomography images revealed the presence of a small fraction of inhomogeneous structures in the original crystal (volume ratio ∼1.2%). Such an inhomogeneity acts as a nucleation of voids and produces stress concentration during compression, which leads to continuous growth of the voids under loading. Meanwhile, the results further reveal that the developing voids are not isotropic: voids with higher surface roughness and irregular structures are easier to break and form new micro-voids. These new voids with higher irregular structures are weaker and easier to break into smaller ones compared with the originals, leading to the development of voids along these weak zones. Finally large voids form. The experiments allow direct investigation of void formation and development, which helps in studying the mechanisms of void development and energetic materials deterioration during manufacturing and transporting.
8
Schmid, Gregor, Fabian Zeitvogel, Likai Hao, Pablo Ingino, Wolfgang Kuerner, James J. Dynes, Chithra Karunakaran, et al. "Synchrotron-Based Chemical Nano-Tomography of Microbial Cell-Mineral Aggregates in their Natural, Hydrated State." Microscopy and Microanalysis 20, no. 2 (February 19, 2014): 531–36. http://dx.doi.org/10.1017/s1431927613014104.
Abstract:
AbstractChemical nano-tomography of microbial cells in their natural, hydrated state provides direct evidence of metabolic and chemical processes. Cells of the nitrate-reducing Acidovorax sp. strain BoFeN1 were cultured in the presence of ferrous iron. Bacterial reduction of nitrate causes precipitation of Fe(III)-(oxyhydr)oxides in the periplasm and in direct vicinity of the cells. Nanoliter aliquots of cell-suspension were injected into custom-designed sample holders wherein polyimide membranes collapse around the cells by capillary forces. The immobilized, hydrated cells were analyzed by synchrotron-based scanning transmission X-ray microscopy in combination with angle-scan tomography. This approach provides three-dimensional (3D) maps of the chemical species in the sample by employing their intrinsic near-edge X-ray absorption properties. The cells were scanned through the focus of a monochromatic soft X-ray beam at different, chemically specific X-ray energies to acquire projection images of their corresponding X-ray absorbance. Based on these images, chemical composition maps were then calculated. Acquiring projections at different tilt angles allowed for 3D reconstruction of the chemical composition. Our approach allows for 3D chemical mapping of hydrated samples and thus provides direct evidence for the localization of metabolic and chemical processes in situ.
9
Parks, Huw Christopher William, Aaron Wade, Thomas M. M. Heenan, Chun Tan, Alice V. Llewellyn, Hamish Thomas Reid, Ralf Ziesche, et al. "Crack Hysteresis Phenomena in Polycrystalline NMC811 Secondary Particles." ECS Meeting Abstracts MA2023-01, no. 7 (August 28, 2023): 2847. http://dx.doi.org/10.1149/ma2023-0172847mtgabs.
Abstract:
Using X-ray tomography, we can predict and study the factors that govern fracture behaviour and cracking in NMC811 particles as a function of potential. Cracking and fracturing is known to cause a decline in battery performance, as regions become disintegrated from the conductive matrix. However, electrochemically induced cracking can be difficult to assess due to complicated sample preparation methods required. An in-situ study that accurately determines the onset of cracking during delithiation from the layered structure is crucial to characterize voltage-induced fracturing in battery particles. Tomography has been extensively used to non-destructively image cracks in li-ion battery materials at the electrode and particle level, making it an ideal candidate for in-situ studies that preserve the electrode during charging and discharging. However, accurately, and reliably tracking operational cracking without the influence of pre-existing cracks is highly challenging, requiring the highest resolutions possible for 3D imaging techniques and small sample geometries while maintaining realistic electrochemical performance. In this study, we present a technique using in-situ synchrotron X-ray computed tomography (CT) and nano-scale CT to completely attribute particle cracking to electrochemical stimulation, corroborated with high-resolution imaging. We demonstrate the cracking hysteresis phenomenon that occurs in NMC811 secondary particles during the first cycle, using a rapid detection algorithm that calculates the extent of cracking in battery particles, even when cracking is not resolvable as compared to nano CT. The results show unprecedented material statistics for understanding and predicting fracture behaviour in battery particles. Figure 1
10
Parks, Huw Christopher William, Chun Tan, Aaron Wade, Thomas M. M. Heenan, Paul R. Shearing, Dan Brett, and Rhodri Jervis. "Nano Tomography of High Voltage Induced First Cycle Cracking in NMC811." ECS Meeting Abstracts MA2022-01, no. 2 (July 7, 2022): 345. http://dx.doi.org/10.1149/ma2022-012345mtgabs.
Abstract:
Lithium nickel-manganese-cobalt (NMC) oxide-based Li-ion batteries have emerged as the most promising successor to LiCoO2 chemistry and could potentially facilitate ubiquitous adoption of Li-ion in mobile and transport systems. High specific capacities, high-rate capability, and long-term cycling abilities are driving much research into these cathode materials, forcing a greater nickel content with each iteration. NMC811’s high specific capacity makes it highly attractive for battery suppliers and users; however, it suffers significant capacity fade via several degradation modes, one being crack formation within secondary particles. The fresh surface exposed by cracking has been linked with parasitic reactions that evolve oxygen and potentially initiate the formation of inactive crystal structures. [1] X-ray computed tomography (CT) has been utilised extensively to image the morphology of battery particles and with the advancement of lab-based tomography systems, resolution on the nano scale is readily available.[2] Whilst in-situ studies are becoming the standard experimental operation for appraising the dynamic nature of these materials, in-situ cells are complicated for use in lab-based instruments due to their low flux, low energy and reduced working space. Thus, nano tomography rarely provides information that deconvolutes chemo-mechanical cracking from manufacturing defects and calendaring. However, in this work we have developed a unique technique to follow the progression of cracking at the nanometre scale by sequential correlated imaging of a micro-sized tab cut from the electrode.[3,4] This method allows for images of the pristine material to be acquired ex-situ before electrochemical testing, and then sequential imaging of the same region of interest in subsequent scans. Here, nano-CT imaging of the same region of the electrode while fully-lithiated and charged to 4.5 V unveils the propagation of cracks as a function of voltage, and their relaxation phenomena upon discharge. [1] Li, Tianyu, Xiao-Zi Yuan, Lei Zhang, Datong Song, Kaiyuan Shi, and Christina Bock. "Degradation mechanisms and mitigation strategies of nickel-rich NMC-based lithium-ion batteries." Electrochemical Energy Reviews 3, no. 1 (2020): 43-80. [2] Heenan, Thomas MM, Chun Tan, Jennifer Hack, Dan JL Brett, and Paul R. Shearing. "Developments in X-ray tomography characterization for electrochemical devices." Materials Today 31 (2019): 69-85 [3] Tan, C., S. Daemi, T. Heenan, F. Iacoviello, A. S. Leach, L. Rasha, R. Jervis, D. J. L. Brett, and P. R. Shearing. "Rapid preparation of geometrically optimal battery electrode samples for nano scale X-ray characterisation." Journal of The Electrochemical Society 167, no. 6 (2020): 060512. [4] Tan, Chun, Andrew S. Leach, Thomas MM Heenan, Huw Parks, Rhodri Jervis, Johanna Nelson Weker, Daniel JL Brett, and Paul R. Shearing. "Nanoscale state-of-charge heterogeneities within polycrystalline nickel-rich layered oxide cathode materials." Cell Reports Physical Science (2021): 100647. Figure 1
11
Li, Qiong, Jürgen Gluch, Zhongquan Liao, Juliane Posseckardt, André Clausner, Magdalena Łępicka, Małgorzata Grądzka-Dahlke, and Ehrenfried Zschech. "Morphology and Mechanical Properties of Fossil Diatom Frustules from Genera of Ellerbeckia and Melosira." Nanomaterials 11, no. 6 (June 20, 2021): 1615. http://dx.doi.org/10.3390/nano11061615.
Abstract:
Fossil frustules of Ellerbeckia and Melosira were studied using laboratory-based nano X-ray tomography (nano-XCT), transmission electron microscopy (TEM) and energy-dispersive X-ray spectroscopy (EDS). Three-dimensional (3D) morphology characterization using nondestructive nano-XCT reveals the continuous connection of fultoportulae, tube processes and protrusions. The study confirms that Ellerbeckia is different from Melosira. Both genera reveal heavily silicified frustules with valve faces linking together and forming cylindrical chains. For this cylindrical architecture of both genera, valve face thickness, mantle wall thickness and copulae thickness change with the cylindrical diameter. Furthermore, EDS reveals that these fossil frustules contain Si and O only, with no other elements in the percentage concentration range. Nanopores with a diameter of approximately 15 nm were detected inside the biosilica of both genera using TEM. In situ micromechanical experiments with uniaxial loading were carried out within the nano-XCT on these fossil frustules to determine the maximal loading force under compression and to describe the fracture behavior. The fracture force of both genera is correlated to the dimension of the fossil frustules. The results from in situ mechanical tests show that the crack initiation starts either at very thin features or at linking structures of the frustules.
12
Kumar, R., P. Lhuissier, J. Villanova, L. Salvo, and J. J. Blandin. "Elementary growth mechanisms of creep cavities in AZ31 alloy revealed by in situ X-ray nano-tomography." Acta Materialia 228 (April 2022): 117760. http://dx.doi.org/10.1016/j.actamat.2022.117760.
13
Grünwald, Nikolas, Pierre Lhuissier, Luc Salvo, Julie Villanova, Norbert H. Menzler, Olivier Guillon, Christophe L. Martin, and Robert Vaßen. "In situ investigation of atmospheric plasma-sprayed Mn–Co–Fe–O by synchrotron X-ray nano-tomography." Journal of Materials Science 55, no. 27 (June 19, 2020): 12725–36. http://dx.doi.org/10.1007/s10853-020-04916-9.
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Hart, Abarasi, Mohamed Adam, John P. Robinson, Sean P. Rigby, and Joseph Wood. "Tetralin and Decalin H-Donor Effect on Catalytic Upgrading of Heavy Oil Inductively Heated with Steel Balls." Catalysts 10, no. 4 (April 3, 2020): 393. http://dx.doi.org/10.3390/catal10040393.
Abstract:
The Toe-to-Heel Air Injection (THAI) combined with catalytic upgrading process in situ (CAPRI) has demonstrated it can simultaneously extract and upgrade heavy oil in situ. This paper reports the investigation of augmenting temperature deficit and suppressing coke formation in the CAPRI section through the incorporation of induction heating and H-donor solvents. An induction-heated catalytic reactor was designed and developed, heated with steel balls in a mixed bed of NiMo/Al2O3 catalyst (66% v/v) to 425 °C temperature, 15 bar pressure and 0.75 h−1 LHSV (Liquid Hourly Space Velocity). The catalyst surface area, pore volume and pore size distribution were determined by using nitrogen adsorption–desorption, while the location of coke deposits within the microstructure of the pelleted spent catalyst was analyzed with X-ray nano-Computed Tomography (X-ray nano-CT). Findings showed that induction heating improved the catalyst performance, resulting in a 2.2° American Petroleum Institute (API) gravity increase of the upgraded oil over that achieved with the conventional heating method. The increment in API gravity and viscosity reduction in the upgraded oils with nitrogen gas only, N2 and H-donor solvents, and hydrogen gas environments can be summarized as follows: decalin > H2 gas >= tetralin > N2 gas. Meanwhile, the improvement in naphtha fraction, middle distillate fractions and suppression of coke formation are as follows: decalin > H2 gas > tetralin > N2 gas. The X-ray nano-CT of the spent catalyst revealed that the pellet suffers deactivation due to coke deposit at the external surface and pore-mouth blockage, signifying underutilization of the catalyst interior surface area.
15
Claro, Pedro I. C., Egon P. B. S. Borges, Gabriel R. Schleder, Nathaly L. Archilha, Allan Pinto, Murilo Carvalho, Carlos E. Driemeier, Adalberto Fazzio, and Rubia F. Gouveia. "From micro- to nano- and time-resolved x-ray computed tomography: Bio-based applications, synchrotron capabilities, and data-driven processing." Applied Physics Reviews 10, no. 2 (June 2023): 021302. http://dx.doi.org/10.1063/5.0129324.
Abstract:
X-ray computed microtomography (μCT) is an innovative and nondestructive versatile technique that has been used extensively to investigate bio-based systems in multiple application areas. Emerging progress in this field has brought countless studies using μCT characterization, revealing three-dimensional (3D) material structures and quantifying features such as defects, pores, secondary phases, filler dispersions, and internal interfaces. Recently, x-ray computed tomography (CT) beamlines coupled to synchrotron light sources have also enabled computed nanotomography (nCT) and four-dimensional (4D) characterization, allowing in situ, in vivo, and in operando characterization from the micro- to nanostructure. This increase in temporal and spatial resolutions produces a deluge of data to be processed, including real-time processing, to provide feedback during experiments. To overcome this issue, deep learning techniques have risen as a powerful tool that permits the automation of large amounts of data processing, availing the maximum beamline capabilities. In this context, this review outlines applications, synchrotron capabilities, and data-driven processing, focusing on the urgency of combining computational tools with experimental data. We bring a recent overview on this topic to researchers and professionals working not only in this and related areas but also to readers starting their contact with x-ray CT techniques and deep learning.
16
Weng, Yi-Tse, Chun-Chieh Wang, Cheng-Cheng Chiang, Heng Tsai, Yen-Fang Song, Shiuh-Tsuen Huang, and Biqing Liang. "In situ evidence of mineral physical protection and carbon stabilization revealed by nanoscale 3-D tomography." Biogeosciences 15, no. 10 (May 25, 2018): 3133–42. http://dx.doi.org/10.5194/bg-15-3133-2018.
Abstract:
Abstract. An approach for nanoscale 3-D tomography of organic carbon (OC) and associated mineral nanoparticles was developed to illustrate their spatial distribution and boundary interplay, using synchrotron-based transmission X-ray microscopy (TXM). The proposed 3-D tomography technique was first applied to in situ observation of a laboratory-made consortium of black carbon (BC) and nanomineral (TiO2, 15 nm), and its performance was evaluated using dual-scan (absorption contrast and phase contrast) modes. This novel tool was then successfully applied to a natural OC–mineral consortium from mountain soil at a spatial resolution of 60 nm, showing the fine structure and boundary of OC, the distribution of abundant nano-sized minerals, and the 3-D organo-mineral association in situ. The stabilization of 3500-year-old natural OC was mainly attributed to the physical protection of nano-sized iron (Fe)-containing minerals (Fe oxyhydroxides including ferrihydrite, goethite, and lepidocrocite), and the strong organo-mineral complexation. In situ evidence revealed an abundance of mineral nanoparticles, in dense thin layers or nano-aggregates/clusters, instead of crystalline clay-sized minerals on or near OC surfaces. The key working minerals for C stabilization were reactive short-range-order (SRO) mineral nanoparticles and poorly crystalline submicron-sized clay minerals. Spectroscopic analyses demonstrated that the studied OC was not merely in crisscross co-localization with reactive SRO minerals; there could be a significant degree of binding between OC and the minerals. The ubiquity and abundance of mineral nanoparticles on the OC surface, and their heterogeneity in the natural environment may have been severely underestimated by traditional research approaches. Our in situ description of organo-mineral interplay at the nanoscale provides direct evidence to substantiate the importance of mineral physical protection for the long-term stabilization of OC. This high-resolution 3-D tomography approach is a promising tool for generating new insight into the interior 3-D structure of micro-aggregates, the in situ interplay between OC and minerals, and the fate of mineral nanoparticles (including heavy metals) in natural environments.
17
Lhuissier, Pierre, Pauline Gravier, Richi Kumar, Alexis Burr, Alexandre Barthelemy, Fanny Mas, Armelle Philip, et al. "X-ray Computed Tomography for Pores Evolutions Under Thermo-mechanical Loading : In Situ Characterization at Nano and Micro Scale." Microscopy and Microanalysis 28, S1 (July 22, 2022): 326–27. http://dx.doi.org/10.1017/s1431927622002070.
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De Angelis, Salvatore, Julie Villanova, Peter Stanley Jørgensen, Vincenzo Esposito, and Jacob Ross Bowen. "Elucidating nickel oxide reduction in a Ni-YSZ solid oxide cell via in-situ X-ray nano holo-tomography." Acta Materialia 273 (July 2024): 119965. http://dx.doi.org/10.1016/j.actamat.2024.119965.
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Statnik, Eugene S., Alexey I. Salimon, Cyril Besnard, Jingwei Chen, Zifan Wang, Thomas Moxham, Igor P. Dolbnya, and Alexander M. Korsunsky. "Ovine Bone Morphology and Deformation Analysis Using Synchrotron X-ray Imaging and Scattering." Quantum Beam Science 4, no. 3 (August 9, 2020): 29. http://dx.doi.org/10.3390/qubs4030029.
Abstract:
Bone is a natural hierarchical composite tissue incorporating hard mineral nano-crystals of hydroxyapatite (HAp) and organic binding material containing elastic collagen fibers. In the study, we investigated the structure and deformation of ovine bone by the combination of high-energy synchrotron X-ray tomographic imaging and scattering. X-ray experiments were performed prior to and under three-point bending loading by using a specially developed in situ load cell constructed from aluminium alloy frame, fast-drying epoxy resin for sample fixation, and a titanium bolt for contact loading. Firstly, multiple radiographic projection images were acquired and tomographic reconstruction was performed using SAVU software, following segmentation using Avizo. Secondly, Wide Angle X-ray Scattering (WAXS) and Small Angle X-ray Scattering (SAXS) 2D scattering patterns were collected from HAp and collagen. Both sample shape and deformation affect the observed scattering. Novel combined tomographic and diffraction analysis presented below paves the way for advanced characterization of complex shape samples using the Dual Imaging and Diffraction (DIAD) paradigm.
20
Ikeda, Yuko, Atsushi Kato, Junichi Shimanuki, Shinzo Kohjiya, Masatoshi Tosaka, Sirilux Poompradub, Shigeyuki Toki, and Benjamin S. Hsiao. "Nano-Structural Elucidation in Carbon Black Loaded NR Vulcanizate by 3D-TEM and In Situ WAXD Measurements." Rubber Chemistry and Technology 80, no. 2 (May 1, 2007): 251–64. http://dx.doi.org/10.5254/1.3539405.
Abstract:
Abstract Three dimensional (3D) visualization of nanometer structure of carbon black dispersion in rubbery matrix has successfully been studied and reported in this paper. Use of 3D-TEM, which is computerized tomography combined with transmission electron microscopy (TEM), enabled us to reconstruct 3D images of carbon black aggregates in natural rubber (NR) matrix. The TEM measurements were conducted by a bright-field method on thin samples without any electron staining. The sample was subject to uni-axial tilting (+65 degree to −65 degree with 2 degree increment) in the sample chamber, and 66 TEM images were taken on each sample. These TEM images were used for computerized tomography to reconstruct the 3D image. This technique is designated as 3D-TEM. The nano-structural features observed by 3D-TEM were in conformity with the electron-conductivity results, and the percolation behavior was recognized. These results were further supplemented by in situ wide-angle X-ray diffraction (WAXD), i.e., simultaneous WAXD and tensile measurements on the sample to observe the strain-induced crystallization in NR vulcanizate. Upon tensile elongation, the crystallization was clearly observed in WAXD in the presence of carbon black, and it contributed to the tensile properties. In order to understand the performances of filled NR vulcanizates, it surely is necessary to know the structural states of the mixed nano-filler and the crystallites produced upon elongation.
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Kolb, Ute, Yasar Krysiak, Tatiana Gorelik, and Enrico Mugnaioli. "Electron and X-ray diffraction – two worlds united." Acta Crystallographica Section A Foundations and Advances 70, a1 (August 5, 2014): C926. http://dx.doi.org/10.1107/s2053273314090731.
Abstract:
Small crystals structure solution usually done with X-ray powder diffraction (XRPD) provides bulk information and is powerful for in-situ investigations. Peak overlap in the one-dimensional data causes problems e.g. for polyphasic or impure samples and large cell parameters thus peak indexing and intensity extraction are the main issues where x-ray powder data may be supported by extra information. Electrons sample smaller volumes but strong coulombic interaction cause multiple scattering effects changing intensities often so strong that a structure solution is becoming impossible. Nevertheless, oriented electron diffraction patterns may provide sufficient information to support indexing or the assignment of impurity peaks in the case of low quality x-ray powder pattern. Reciprocal space tomography [1] uses a series of non-oriented diffraction patterns for which dynamical effects are significantly reduced and an enhanced amount of independent reflections sampled allows "ab-initio" crystal structure solution using established X-ray structure solution packages. Although structure refinement based on kinematical intensities is stable, achievable R values of 10-30% are high and final refinement may be performed based on X-ray powder data. Scanning transmission electron microscopy (STEM) for crystal tracking and nano electron diffraction (NED) is suitable for beam sensitive material, agglomerated particles, twins or intergrown phases on crystals down to 30nm size [2, 3]. Interesting properties of nanocrystalline materials are driven mainly by twinning, defects, disorder in one or two dimensions down to the amorphous state. Here low data completeness or uncertain intensity determination causes problems in structure solution. Here a mean structure may be determinable serving as a basis for disorder description and being used as a starting model being refined onto X-ray powder data maybe supported by a combination of the diffraction methods or by adding extra information.
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Topal, Emre, Harishankaran Rajendran, Izabela Zgłobicka, Jürgen Gluch, Zhongquan Liao, André Clausner, Krzysztof Kurzydłowski, and Ehrenfried Zschech. "Numerical and Experimental Study of the Mechanical Response of Diatom Frustules." Nanomaterials 10, no. 5 (May 18, 2020): 959. http://dx.doi.org/10.3390/nano10050959.
Abstract:
Diatom frustules, with their hierarchical three-dimensional patterned silica structures at nano to micrometer dimensions, can be a paragon for the design of lightweight structural materials. However, the mechanical properties of frustules, especially the species with pennate symmetry, have not been studied systematically. A novel approach combining in situ micro-indentation and high-resolution X-ray computed tomography (XCT)-based finite element analysis (FEA) at the identical sample is developed and applied to Didymosphenia geminata frustule. Furthermore, scanning electron microscopy and transmission electron microscopy investigations are conducted to obtain detailed information regarding the resolvable structures and the composition. During the in situ micro-indentation studies of Didymosphenia geminata frustule, a mainly elastic deformation behavior with displacement discontinuities/non-linearities is observed. To extract material properties from obtained load-displacement curves in the elastic region, elastic finite element method (FEM) simulations are conducted. Young’s modulus is determined as 31.8 GPa. The method described in this paper allows understanding of the mechanical behavior of very complex structures.
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Yan, Zilin, Christophe L. Martin, Didier Bouvard, David Jauffrès, Pierre Lhuissier, Luc Salvo, Luis Olmos, Julie Villanova, and Olivier Guillon. "Coupling in-situ X-ray micro- and nano-tomography and discrete element method for investigating high temperature sintering of metal and ceramic powders." EPJ Web of Conferences 140 (2017): 13006. http://dx.doi.org/10.1051/epjconf/201714013006.
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Patterson, B. M., N. L. Cordes, R. Gilbertson, and Z. Smith. "The Application of X-ray Micro- and Nano- Scale Computed Tomography to the Morphological and In-situ Dynamic Study of Polymer Foam Materials." Microscopy and Microanalysis 19, S2 (August 2013): 398–99. http://dx.doi.org/10.1017/s143192761300398x.
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Bawane, Kaustubh, Xiaoyang Liu, Ruchi Gakhar, Michael Woods, Mingyuan Ge, Xianghui Xiao, Wah-Keat Lee, et al. "Visualizing time-dependent microstructural and chemical evolution during molten salt corrosion of Ni-20Cr model alloy using correlative quasi in situ TEM and in situ synchrotron X-ray nano-tomography." Corrosion Science 195 (February 2022): 109962. http://dx.doi.org/10.1016/j.corsci.2021.109962.
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Aliyah, Kinanti Hantiyana, Christian Appel, Christian Prehal, Manuel Guizar Sicairos, Lorenz Gubler, and Jens Eller. "Operando Liquid Water Saturation in PEFC Catalyst Layers Determined Via Small Angle X-Ray Scattering." ECS Meeting Abstracts MA2022-02, no. 39 (October 9, 2022): 1412. http://dx.doi.org/10.1149/ma2022-02391412mtgabs.
Abstract:
Various measurement techniques suitable with the length scale of PEFC components have been explored to address the PEFC water management challenge. For the gas diffusion layer (GDL), technological advances have permitted operando water saturation quantification and elucidation of its mechanism with X-ray tomography with few microns resolution 1-4. Furthermore, sub-voxel information contained in the X-ray tomography data has demonstrated accurate water quantification in the nano-porous microporous layer (MPL)5. However, in the nanoscale regime of the catalyst layer, the quantification of water and the mechanism of the water filling the pores remain nontrivial. Studies involving imaging techniques dedicated to understand the water management in the catalyst layer have been carried out albeit with limited spatial resolution6. Nevertheless, the pore-scale information has remained unresolved. Small angle X-ray scattering (SAXS) technique is proposed as a non-destructive diagnostic tool to investigate the catalyst layer saturation in operating conditions. SAXS is well suited for diagnosing the presence of liquid water during operando experiments because of its sensitivity to electron density contrast, nanoscale observation window, high temporal resolution and adequate spatial resolution to distinguish the components in PEFCs. Herein, SAXS intensity profiles measured at cSAXS, Swiss Light Source, Paul Scherrer Institut, Switzerland, with a recently developed SAXS-compatible operando PEFC (Figure 1 middle and right) are interpreted using representative morphology models and assuming different water filling mechanisms (Figure 1 middle and left). The presentation will provide insights into the wetting phenomena in the catalyst layer of PEFC during operation using a representative morphology modelling approach. This work has been presented in XVIII edition of the International Small-Angle Scattering Conference. (1) Xu, H.; Buhrer, M.; Marone, F.; Schmidt, T. J.; Buchi, F. N.; Eller, J. Effects of Gas Diffusion Layer Substrates on PEFC Water Management: Part I. Operando Liquid Water Saturation and Gas Diffusion Properties. J Electrochem Soc 2021, 168 (7). (2) Eller, J.; Rosen, T.; Marone, F.; Stampanoni, M.; Wokaun, A.; Buchi, F. N. Progress in In Situ X-Ray Tomographic Microscopy of Liquid Water in Gas Diffusion Layers of PEFC. J Electrochem Soc 2011, 158 (8), B963-B970. (3) Mularczyk, A.; Lin, Q. Y.; Niblett, D.; Vasile, A.; Blunt, M. J.; Niasar, V.; Marone, F.; Schmidt, T. J.; Buchi, F. N.; Eller, J. Operando Liquid Pressure Determination in Polymer Electrolyte Fuel Cells. Acs Appl Mater Inter 2021, 13 (29), 34003-34011. (4) Sabharwal, M.; Buchi, F. N.; Nagashima, S.; Marone, F.; Eller, J. Investigation of the transient freeze start behavior of polymer electrolyte fuel cells. J Power Sources 2021, 489. (5) Chen, Y. C.; Berger, A.; De Angelis, S.; Schuler, T.; Bozzetti, M.; Eller, J.; Tileli, V.; Schmidt, T. J.; Buchi, F. N. A Method for Spatial Quantification of Water in Microporous Layers of Polymer Electrolyte Fuel Cells by X-ray Tomographic Microscopy. Acs Appl Mater Inter 2021, 13 (14), 16227-16237. (6) Babu, S. K.; Spernjak, D.; Mukundan, R.; Hussey, D. S.; Jacobson, D. L.; Chung, H. T.; Wu, G.; Steinbach, A. J.; Litster, S.; Borup, R. L.; Zelenay, P. Understanding water management in platinum group metal-free electrodes using neutron imaging. J Power Sources 2020, 472. Figure 1
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Akhondzadeh, Hamed, Alireza Keshavarz, Faisal Ur Rahman Awan, Ahmed Z. Al-Yaseri, Stefan Iglauer, and Maxim Lebedev. "Coal fracturing through liquid nitrogen treatment: a micro-computed tomography study." APPEA Journal 60, no. 1 (2020): 67. http://dx.doi.org/10.1071/aj19105.
Abstract:
Low permeability of coal has been a constant obstacle to economic production from coalbed methane reservoirs, and liquid nitrogen (LN2) treatment has been investigated as one approach to address this issue. This study examined LN2 fracturing of a bituminous coal at pore-scale through 3D X-ray micro-computed tomography. For this purpose, a cylindrical sample was immersed into LN2 for 60 min. The micro-CT results clearly showed that the rapid freezing of the coal with LN2 generated fracture planes with large apertures originating from the pre-existing cleats in the rock. This treatment also connected original cleats with originally isolated pores and micro-cleats, thereby increasing pore network connectivity. Moreover, scanning electron microscopy highlighted the appearance of continuous wide conductive fractures with a maximum opening size of 9 µm. Furthermore, a nano-indentation technique was used to test the effect of LN2 on coal mechanical properties. The indentation moduli decreased by up to 14%, which was attributed to the increase in the cracked rock compressibility, showing considerable fracturing efficiency of the LN2 treatment. Through in-situ microscopic visualisation and surface investigation, this study quantified the pore structure and connectivity evolution of the rock based on the morphological alteration, and demonstrated the promising effect of LN2 freezing on fracturing of bituminous coals, thus aiding coalbed methane production. The significance of this study was investigating the mechanisms associated with and the efficiency of LN2 treatment of a coal rock in a 3D analysis inside the rock.
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Lin, Chien-Chou, Li-Hsuan Chiu, Walter H. Chang, Cheng-An J. Lin, Ruei-Ming Chen, Yuan-Soon Ho, Chun S. Zuo, Austin Changou, Yue-Fa Cheng, and Wen-Fu T. Lai. "A Non-Invasive Method for Monitoring Osteogenesis and Osseointegration Using Near-Infrared Fluorescent Imaging: A Model of Maxilla Implantation in Rats." International Journal of Molecular Sciences 24, no. 5 (March 6, 2023): 5032. http://dx.doi.org/10.3390/ijms24055032.
Abstract:
Currently, computed tomography and conventional X-ray radiography usually generate a micro-artifact around metal implants. This metal artifact frequently causes false positive or negative diagnoses of bone maturation or pathological peri-implantitis around implants. In an attempt to repair the artifacts, a highly specific nanoprobe, an osteogenic biomarker, and nano-Au-Pamidronate were designed to monitor the osteogenesis. In total, 12 Sprague Dawley rats were included in the study and could be chategorized in 3 groups: 4 rats in the X-ray and CT group, 4 rats in the NIRF group, and 4 rats in the sham group. A titanium alloy screw was implanted in the anterior hard palate. The X-ray, CT, and NIRF images were taken 28 days after implantation. The X-ray showed that the tissue surrounded the implant tightly; however, a gap of metal artifacts was noted around the interface between dental implants and palatal bone. Compared to the CT image, a fluorescence image was noted around the implant site in the NIRF group. Furthermore, the histological implant-bone tissue also exhibited a significant NIRF signal. In conclusion, this novel NIRF molecular imaging system precisely identifies the image loss caused by metal artifacts and can be applied to monitoring bone maturation around orthopedic implants. In addition, by observing the new bone formation, a new principle and timetable for an implant osseointegrated with bone can be established and a new type of implant fixture or surface treatment can be evaluated using this system.
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El-Zoka, Ayman A., Se-Ho Kim, Heena Khanchandani, Leigh T. Stephenson, and Baptiste Gault. "(Digital Presentation) Advances in Cryo-Atom Probe Tomography Studies on Formation of Nanoporous Metals By Dealloying." ECS Meeting Abstracts MA2022-01, no. 47 (July 7, 2022): 1983. http://dx.doi.org/10.1149/ma2022-01471983mtgabs.
Abstract:
The selective removal of a less noble (more chemically active) metal from a mixture of 2–3 metals can yield a bicontinuous, open-pore, 3D nanoporous metal (NPM), that is rich in the more noble metal(s)1. NPMs have been successfully developed by the intelligent use of the conventionally-undesired dealloying corrosion. The excellent properties of NPMs are attributed to the surface area-to-volume ratio, and high curvature of nanoligament surfaces 2,3 . Experimental work on NPMs revealed the formation of uniformly nanoporous structure by dealloying AgAu alloy in nitric acid, a method still widely used until today for making nanoporous gold (NPG). This dealloying process is complex: the selective dissolution of the less-noble element should lead to the creation of surface vacancies or adatoms, which migrate across the surface to form surface roughening features, and thus assisting the migration of the residual more-noble atoms, leading to island growth4. Ex-situ characterization cannot fully explain some intricate details at the dealloying interface and at the surface of the formed nanoligaments. Gaining insight into initial stages of dealloying, and the inherent competition between surface roughening from the dissolution of silver atoms, and surface smoothening from surface diffusion of gold atoms5, can only be done effectively by monitoring the changes occurring at the surfaces of alloys in-situ. Several notable in-situ methods were used to characterize formation of NPMs, such as TEM 6, often limited by the 2D nature of the analysis. Also, synchrotron-based methods such as X-ray nanotomography 7 and neutron scattering 8 were limited by resolution and lack of compositional contrast. APT is a powerful technique that provides 3D characterization9 and near-atomic-scale compositional analysis of materials, and could complement the abovementioned suite of techniques, yet the analysis of nanoporous structure comes with challenges. Aiming to develop a universal method for probing corrosion systems by APT, the concept of embedding frozen solutions in corroded systems was developed and reported in a recent reporting 10 of analyzing NPMs along with frozen water-based solutions. This involved the joint use of an ensemble of equipment and techniques that connect the frozen liquid to the atom probe, including a plasma-focused ion beam (PFIB) where the preparation of APT specimens uses a cryostage, and transfer of the frozen sample through ultra-high-vacuum suitcase11. This paved the way for many advances in characterization of corrosion processes, as the possibility of freezing corrosion reactions for APT (now known as cryo-APT) arises. Here, we further develop cryo-APT to probe into the mechanisms of dealloying in AgAu and how that leads to the formation of NPG using our in-situ approach. Nanoligament structure will be correlated with dealloying conditions by making observations at the solid-liquid interface in 3D. References Newman, R. C. 2.05 - Dealloying. in Shreir’s Corrosion (eds. Cottis, B. et al.) 801–809 (Elsevier, 2010). Zielasek, V. et al. Gold Catalysts: Nanoporous Gold Foams. Angew. Chemie Int. Ed. 45, 8241–8244 (2006). Xue, Y., Markmann, J., Duan, H., Weissmüller, J. & Huber, P. Switchable imbibition in nanoporous gold. Nat. Commun. 5, (2014). Forty, A. J. & Rowlands, G. A possible model for corrosion pitting and tunneling in noble-metal alloys. Philos. Mag. A Phys. Condens. Matter, Struct. Defects Mech. Prop. (1981) doi:10.1080/01418618108239399. Erlebacher, J., Newman, C. & Sieradzki, K. Fundamental physics and chemistry of nanoporosity evolution during dealloying. RSC Nanosci. Nanotechnol. 11–29 (2012) doi:10.1039/9781849735285-00011. Liu, P. et al. Dealloying Kinetics of AgAu Nanoparticles by In Situ Liquid-Cell Scanning Transmission Electron Microscopy. Nano Lett. 20, 1944–1951 (2020). Chen-Wiegart, Y. C. K. et al. In situ imaging of dealloying during nanoporous gold formation by transmission X-ray microscopy. Acta Mater. 61, 1118–1125 (2013). Corcoran, S. G., Wiesler, D. G. & Sieradzki, K. An in Situ Small Angle Neutron Scattering Investigation of Ag0.7Au0.3 Dealloying Under Potential Control. MRS Proc. 451, 93 (1996). Gault, B., Moody, M. P., Cairney, J. M. & Ringer, imon P. Atom Probe Microscopy. vol. 160 (Springer New York, 2012). El-Zoka, A. A. et al. Enabling near-atomic–scale analysis of frozen water. Sci. Adv. 6, eabd6324 (2020). Stephenson, L. T. et al. The LaplacE project: An integrated suite for preparing and transferring atom probe samples under cryogenic and UHV conditions. PLoS One (2018) doi:10.1371/journal.pone.0209211. Figure 1
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Wiseall, A. C., R. J. Cuss, C. C. Graham, and J. F. Harrington. "The visualization of flow paths in experimental studies of clay-rich materials." Mineralogical Magazine 79, no. 6 (November 2015): 1335–42. http://dx.doi.org/10.1180/minmag.2015.079.06.09.
Abstract:
AbstractOne of the most challenging aspects of understanding the flow of gas and water during testing in clay-rich low-permeability materials is the difficulty in visualizing localized flow. Whilst understanding has been increased using X-ray Computed-tomography (CT) scanning, synchrotron X-ray imaging and Nuclear Magnetic Resonance (NMR) imaging, real-time testing is problematic under realistic in situ conditions confining pressures, which require steel pressure vessels. These methods tend not to have the nano-metre scale resolution necessary for clay mineral visualization, and are generally not compatible with the long duration necessary to investigate flow in such materials. Therefore other methods are necessary to visualize flow paths during post-mortem analysis of test samples. Several methodologies have been established at the British Geological Survey (BGS), in order to visualize flow paths both directly and indirectly. These include: (1) the injection of fluorescein-stained water or deuterium oxide; (2) the introduction of nanoparticles that are transported by carrier gas; (3) the use of radiologically tagged gas; and (4) the development of apparatus for the direct visualization of clay. These methodologies have greatly increased our understanding of the transport of water and gas through intact and fractured clay-rich materials. The body of evidence for gas transport through the formation of dilatant pathways is now considerable. This study presents observations using a new apparatus to directly visualize the flow of gas in a kaolinite paste. The results presented provide an insight into the flow of gas in clay-rich rocks. The flow of gas through dilatant pathways has been shown in a number of argillaceous materials (Angeli et al., 2009; Autio et al., 2006; Cuss et al., 2014; Harrington et al., 2012). These pathways are pressure induced and an increase in gas pressure leads to the dilation of pathways. Once the gas breakthrough occurs, pressure decreases and pathways begin to close. This new approach is providing a unique insight into the complex processes involved during the onset, development and closure of these dilatant gas pathways.
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Wang, Heng, Rui Wang, and Michael F. L. De Volder. "Understanding the Expansion and Electrochemistry of Nickel-Rich NMC - Graphite Full Cells Using in-Situ Dilatometry." ECS Meeting Abstracts MA2023-01, no. 2 (August 28, 2023): 674. http://dx.doi.org/10.1149/ma2023-012674mtgabs.
Abstract:
The higher energy density and lower cost of Ni-rich lithium nickel manganese cobalt (NMC) have made them one of the best cathode materials for Li-Ion batteries (LIBs). Understanding the mechanical behaviour, particularly the volume changes during charging and discharging, is important for the cell design. So far, this has mainly been studied using X-ray diffraction (XRD), which is powerful in understanding the nanoscale crystal level of the material volume change. However, recent papers have shown that XRD is insufficient to capture macroscopic cell expansion [1]. It is also getting more important to consider the synergistic effect of cathodes and anodes in the context of full cells. It is therefore valuable to have in-situ dilatometry filling the gap and unravelling how nano and macro electrochemical and mechanical behaviour differs. Here, we coupled electrochemical analysis with in-situ electrochemical dilatometry to observe macroscopic dimensional changes of NMC811−graphite full cells during galvanostatic cycling under different pressure conditions, voltages, and cathode particle morphologies. Our setup uses a non-contact dilation sensor and independent control over the stack pressure to achieve highly accurate measurements of the electrode expansion, with a linearity of ≤ ±90 nm, resolution of ≤ 0.5 nm, and a drift of ≤ 100 nm/month. The initial investigations of graphite v.s. NMC811 pouch cells (220 mAh) have offered clear evidence of the strong correlation between dilation and electrochemistry, where reversible dilation features in every charge-discharge cycle can be assigned to cathode and anode phase transitions. In addition, our system can effectively isolate the reversible thickness change from the irreversible thickness change known to be potentially correlated to solid electrolyte interphase (SEI),[2] particle rearrangement,[3] and electrode delamination.[4] With different experimental conditions (C-rates, pressure and voltage windows), the full cells demonstrated different electrochemical performances alongside varied dilation behaviours. The observed in-situ dimensional changes improve our understanding of the physical and chemical processes happening while cycling NMC-Graphite full cells. [1] F. B. Spingler, S. Kücher, R. Phillips, E. Moyassari, and A. Jossen, “Electrochemically Stable In Situ Dilatometry of NMC, NCA and Graphite Electrodes for Lithium-Ion Cells Compared to XRD Measurements,” J. Electrochem. Soc., vol. 168, no. 4, p. 040515, 2021, doi: 10.1149/1945-7111/abf262. [2] A. J. Louli, L. D. Ellis, and J. R. Dahn, “Operando Pressure Measurements Reveal Solid Electrolyte Interphase Growth to Rank Li-Ion Cell Performance,” Joule, vol. 3, no. 3, pp. 745–761, 2019, doi: 10.1016/j.joule.2018.12.009. [3] D. Y. W. Yu, M. Zhao, and H. E. Hoster, “Suppressing Vertical Displacement of Lithiated Silicon Particles in High Volumetric Capacity Battery Electrodes,” ChemElectroChem, vol. 2, no. 8, pp. 1090–1095, 2015, doi: 10.1002/celc.201500133. [4] H. Michael et al., “A Dilatometric Study of Graphite Electrodes during Cycling with X-ray Computed Tomography,” J. Electrochem. Soc., vol. 168, no. 1, p. 010507, 2021, doi: 10.1149/1945-7111/abd648.
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Varga, Peter, Bernhard Hesse, Max Langer, Susanne Schrof, Nils Männicke, Heikki Suhonen, Alexandra Pacureanu, Dieter Pahr, Françoise Peyrin, and Kay Raum. "Synchrotron X-ray phase nano-tomography-based analysis of the lacunar–canalicular network morphology and its relation to the strains experienced by osteocytes in situ as predicted by case-specific finite element analysis." Biomechanics and Modeling in Mechanobiology 14, no. 2 (July 11, 2014): 267–82. http://dx.doi.org/10.1007/s10237-014-0601-9.
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An, Qi, Chunyang Hong, and Haitao Wen. "Fracture Patterns of Rocks Observed under Cryogenic Conditions Using Cryo-Scanning Electron Microscopy." Processes 11, no. 7 (July 7, 2023): 2038. http://dx.doi.org/10.3390/pr11072038.
Abstract:
Cryogenic fracturing, which uses liquid nitrogen (LN2) as a fracturing fluid, is a waterless fracturing method. However, previous attempts to investigate the fracture morphology of rocks after LN2 quenching have been mainly based on standard scanning electron microscopy (SEM) analysis at room temperature. This can be problematic since thermally-induced fractures created by temperature difference tend to close as a sample warms and thermal stress relaxes. To address this issue, we established a novel approach employing Cryo-scanning electron microscopy (Cryo-SEM) to investigate the fracture patterns induced by liquid nitrogen quenching under cryogenic conditions. This method can achieve in-situ visualization of fractures and pores with a nano-scale resolution at −190 °C. X-ray computed tomography (CT) is also employed to illustrate the fracture distribution inside samples. Cryo-SEM and standard SEM are compared, and statistical assessments are conducted to quantify fracture aperture size and closure scale. The results demonstrate that Cryo-SEM can more accurately preserve native fracture morphology and provide a more accurate means of evaluating fracture scales generated during LN2 quenching, particularly at higher temperature differences between rock and liquid nitrogen. Distinct fracture patterns and fracture width are observed for various rock types (i.e., coal, sandstone, shale, granite) by using these methods. More prominently, the maximum fracture width of coal, sandstone, shale and granite were 89.17 µm, 1.29 µm, 0.028 µm and 2.12 µm when the temperature difference between LN2 and rock samples were 296 °C. LN2 is shown to exhibit superior fracturing efficiency on coal and granite, characterized by complex fracture networks with branched fractures. This research contributes to our understanding of liquid nitrogen fracturing mechanisms and may offer effective approaches for unconventional reservoirs stimulation.
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Dumbryte, Irma, Donatas Narbutis, Maria Androulidaki, Arturas Vailionis, Saulius Juodkazis, and Mangirdas Malinauskas. "Teeth Microcracks Research: Towards Multi-Modal Imaging." Bioengineering 10, no. 12 (November 25, 2023): 1354. http://dx.doi.org/10.3390/bioengineering10121354.
Abstract:
This perspective is an overview of the recent advances in teeth microcrack (MC) research, where there is a clear tendency towards a shift from two-dimensional (2D) to three-dimensional (3D) examination techniques, enhanced with artificial intelligence models for data processing and image acquisition. X-ray micro-computed tomography combined with machine learning allows 3D characterization of all spatially resolved cracks, despite the locations within the tooth in which they begin and extend, and the arrangement of MCs and their structural properties. With photoluminescence and micro-/nano-Raman spectroscopy, optical properties and chemical and elemental composition of the material can be evaluated, thus helping to assess the structural integrity of the tooth at the MC site. Approaching tooth samples having cracks from different perspectives and using complementary laboratory techniques, there is a natural progression from 3D to multi-modal imaging, where the volumetric (passive: dimensions) information of the tooth sample can be supplemented by dynamic (active: composition, interaction) image data. Revelation of tooth cracks clearly shows the need to re-assess the role of these MCs and their effect on the structural integrity and longevity of the tooth. This provides insight into the nature of cracks in natural hard materials and contributes to a better understanding of how bio-inspired structures could be designed to foresee crack propagation in biosolids.
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Llewellyn, Alice V., Andrew S. Leach, Isabella Mombrini, Alessia Matruglio, Jiecheng Diao, Chun Tan, Thomas M. M. Heenan, et al. "Understanding the Degradation Mechanisms of Lithium Ion Batteries Using in-Situ Multi-Scale Diffraction Techniques." ECS Meeting Abstracts MA2022-01, no. 2 (July 7, 2022): 177. http://dx.doi.org/10.1149/ma2022-012177mtgabs.
Abstract:
Advanced Li-ion batteries adopting new cathode chemistries are required for the successful widespread transition to electric vehicles (EVs) and renewable energy sources, aiming for high energy density, long cycle life, and good rate capability. Commercial candidates for EV batteries include Ni-rich Li(NixMnyCo1−x-y)O2 (NMC) cathodes, with Ni:Mn:Co ratios of 8:1:1 (NMC811) and higher. These are favored because of their high specific capacity (~ 200 mAh g-1)and reduced cobalt content. Despite all of the advantages, these materials suffer from a range of degradation modes, many of which are associated with the redox and crystallographic behavior at high states of charge. In particular, Ni-rich cathodes suffer from several limitations, such as rapid capacity fade in comparison to NMC stoichiometries with lower Ni content. In addition, they also have a lower onset voltage for oxygen release and subsequent surface reconstruction leading to the formation of spinel and rock salt phases which impede (de)lithiation and therefore the achievable capacity of the cell.1 Crystallographic properties of electrode materials are intrinsically linked to the electrochemical performance of the cell. NMC materials suffer from anisotropic changes in the crystal structure during cycling which induces strain and leads to issues such as crack formation, expediting degradation. One method to tackle capacity fade is to switch to single-crystal morphologies (particle size 1-3 μm) which have better mechanical stability than conventional polycrystalline morphologies (secondary agglomerate particles ~ 10 μm made up of primary particles which are 100 nm – 1 μm in size) and have less propensity to form extensive rock-salt layers. It is thought that the single-crystal morphology helps to reduce stress in the material as the anisotropic stress in polycrystalline cathodes is concentrated at grain boundaries. However, there is still a limited understanding of the subtle mechanistic differences between the two materials during cycling.2 A multi-scale approach is required to gain a more comprehensive understanding of the degradation mechanisms at play and how they initiate and propagate. In this work, synchrotron diffraction methods were employed at the crystal, particle and cell scale using a variety of techniques including in-situ Bragg Coherent Diffraction Imaging (BCDI), 3D-XRD and operando high-resolution XRD. Intra-particle, inter-particle and electrode level heterogeneities were observed during cycling, both in pristine and aged samples. It is believed that these heterogeneities accelerate the loss of performance at the cell level by inducing crack formation which can then be observed in X-ray computed tomography data acquired in simultaneous lab studies. The overarching goal of these investigations is to add to the understanding of complex degradation mechanisms for Ni-rich layered transition metal oxide cathodes, ultimately aiding in the informed development of future battery electrode materials. References: 1] Xu, C. et al., Phase Behaviour during Electrochemical Cycling of Ni‐Rich Cathode Materials for Li‐Ion Batteries. Adv. Energy Mater. 2021, 11, 2003404. 2] Yin, S. et al., Fundamental and solutions of microcracks in Ni-rich layered oxide cathode materials of lithium-ion batteries. Nano Energy, 2021, 83, 105854.
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Paul, Partha P., Ji Hu, Robert Scott Young, Ludovic Broche, Alex Rettie, Marco DiMichiel, and Philip Withers. "Multimodal Characterization of Nucleation and Progression of Interfacial Degradation in All Solid-State Batteries." ECS Meeting Abstracts MA2023-02, no. 5 (December 22, 2023): 871. http://dx.doi.org/10.1149/ma2023-025871mtgabs.
Abstract:
We face an immediate need for more energy-dense batteries that are stable over long-term cycling, to address the increased electrification of the transportation sector. All-solid state batteries (ASSBs) that combine a solid-state electrolyte with a Li metal anode offer the potential to achieve this objective by replacing intercalation anodes such as graphite with Li metal. However, interfacial degradation at the Li | solid electrolyte interface currently compromises the safety and cycling stability of ASSBs [1]. This interfacial degradation is usually a combination of instabilities of mechanical, chemical or electrochemical origin. This in turn compromises the structural and morphological stability of ASSBs over cycling, causing them to fail in fewer cycles than required for implementation as next-generation batteries in automobiles [2]. Thus, in order to improve their cycling stability, the understanding of the origin and nature of these interfacial instabilities needs to be multimodal, to understand the interplay between the different degradation mechanisms. Argyrodite (Li6PS5Cl) is a particularly attractive solid-state electrolyte (SSE) due to a high ionic conductivity (comparable to liquid electrolytes), as well as potential for batch processing [3]. However, its brittle nature and chemical composition makes it susceptible to cracking and deleterious side reactions, which hamper its stability. This work will focus on elucidating the effect of (1) current density and (2) processing conditions on the cycling stability of Li | LPSCl | Li ASSBs. We use 4-D XRD-CT (X-ray diffraction computed tomography) combined with phase contrast micro-computed tomography (μCT) to conduct the multimodal investigation of interfacial degradation, under pseudo operando conditions. The methodology is to obtain a 3-D XRDCT scan around the interface in a particular cycled condition, followed by a higher-resolution 3D μCT scan on the same region. This sequence is repeated after every stripping/plating cycle, starting from the pristine cell up to cell failure. These experiments are conducted at a synchrotron source, to enable the acquisition at high spatial resolution (~5 μm) over large volumes (~mm3), in a reasonable amount of time. A standard swagelok-style cell is used for repeatability of results and optimal geometry for conducting tomography. XRD-CT can furnish quantitative phase maps of all phases (argyrodite and reaction by-products), as well as the elastic strain in the sample. The μCT on the other hand gives information on the evolution of morphology around the interface with cycling (cracks/voids). Thus, by correlating the two datasets together over cycling, we are able to connect mechanical instabilities to the chemical/electrochemical instabilities. Here, we focus on varying two specific processing parameters for argyrodite: the sintering temperature and pressure, and studying their effect on nucleation and propagation of interfacial instabilities over repeated cycling. Through cycling, we track the evolution of cracks/voids, chemical by-products such as LiCl, Li3P and Li2S using XRD-CT and μCT. Finally, we track the filling of metallic Li into certain cracks in dendritic form, which leads to shorting and failure of the cell. We find that both of these parameters heavily influence the behavior of the interface, with cells failing between 4-20 cycles, and a marked difference in how the degradation initiates and propagates. Finally, for the processing condition that shows the best cycling behavior, we do a C-rate study, by increasing the current density for plating/stripping with each cycle up to failure. This discusses the utility of a parameter such as critical current density for a cell, where the local current densities are very heterogeneous and different from the global current reading while cycling. We envisage these results being used as inputs into modeling studies to optimize strategies for interfacial stabilization in ASSBs going forward. [1] Paul, P. P. et al. Interfaces in all solid state Li-metal batteries: a review on instabilities, stabilization strategies, and scalability. Energy Storage Materials 2022, 45, 969-1001. [2] Hao, S. et al. Tracking lithium penetration in solid electrolytes in 3D by in-situ synchrotron X-ray computed tomography. Nano Energy 2021, 82, 105744. [3] Chen, Y-T. et al., Investigating dry room compatibility of sulfide solid-state electrolytes for scalable manufacturing, Journal of Materials Chemistry A 2022, 10, 7155-7164.
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Osmieri, Luigi, Tanvir Alam Arman, Guanxiong Wang, Hao Wang, Kenneth C. Neyerlin, Siddharth Komini Babu, and Jacob S. Spendelow. "Electrochemical Diagnostics and Innovative Electrode Architectures to Investigate and Improve Mass Transport in Platinum Group Metal-Free Catalyst Layers." ECS Meeting Abstracts MA2022-02, no. 39 (October 9, 2022): 1424. http://dx.doi.org/10.1149/ma2022-02391424mtgabs.
Abstract:
To efficiently and extensively utilize hydrogen for transportation and stationary power generation, the development of low-cost and efficient proton exchange membrane fuel cells (PEMFC) is essential.1 Platinum (Pt) is used as catalyst in PEMFC due to its high performance, but its high cost has been one of the major barriers to the extensive use of PEMFC systems for transportation. In particular, high loadings of Pt are required at the PEMFC cathode due to the sluggish kinetics of the oxygen reduction reaction (ORR).2 One of the strategies adopted to overcome this barrier, is the development of low-cost platinum group metal (PGM)-free catalysts.3 Both the ORR activity and durability of PGM-free catalysts has improved considerably in recent years,4 but the mass activity of these materials remains much lower compared to Pt-based catalysts, requiring the use of higher catalyst loadings on the electrode. As a direct consequence, typical PGM-free catalyst layers (CL) are about 1 order of magnitude thicker than Pt-based ones (~100 µm vs. ~10 µm), creating more challenging conditions for transport of O2 and H+ to the active sites and removal of liquid water within the CL.5 A series of in-situ electrochemical diagnostics methods to measure the mass transport resistance in PGM-fee CLs based on H2 and O2 limiting currents have been developed within the DOE-sponsored ElectroCat consortium.4,6 We will show the application of these methods, in conjunction to other well-established in-situ and ex-situ characterizations (cyclic voltammetry, impedance spectroscopy, SEM, X-ray tomography), to explain the performance trend observed in different PGM-free CLs. We examined the impact of different CL fabrication variables like the ionomer-to-catalyst (I/C) ratio, the ink solvent composition, and the ionomer equivalent weight (EW), evidencing the ones providing harsher conditions for mass transport. The results show the importance achieving optimal transport conditions by selecting a proper combination of these fabrication parameters.7,8 With the aim of improving mass transport and ionic conductivity and expanding the CL operational robustness over a broader range of operating conditions, we developed an innovative electrode architecture having differentiated and ordered domains.9 In particular, we designed a CL divided into alternated catalyst and void domains (grooves). We investigated the fabrication of the groovy CL using different methods and tested the performance under different relative humidity conditions. The results show how the groovy CL structure provides performance enhancements compared to a traditional planar CL in conditions more challenging for mass transport, e.g., at high relative humidity and for electrodes prepared with high I/C and low EW ionomer. In addition, we demonstrated that filling the grooves with a material more hydrophobic than the main catalyst domain (e.g., catalyst mixed with ionomer with high EW and low I/C, or carbon mixed with PTFE) we can largely expand the operational robustness in oversaturated conditions. References D. A. Cullen et al., Nat. Energy (2021). D. Banham et al., Sci. Adv., 4, 1–7 (2018). L. Osmieri et al., Curr. Opin. Electrochem., 25, 100627 (2020). P. Zelenay and D. J. Myers, DOE Annual Merit Review - ElectroCat 2.0 (Electrocatalysis Consortium) (2021). L. Osmieri and Q. Meyer, Curr. Opin. Electrochem., 31, 100847 (2021). A. G. Star, G. Wang, S. Medina, S. Pylypenko, and K. C. Neyerlin, J. Power Sources, 450, 227655 (2020). L. Osmieri et al., Nano Energy, 75, 104943 (2020). G. Wang, L. Osmieri, A. G. Star, J. Pfeilsticker, and K. C. Neyerlin, J. Electrochem. Soc., 167, 044519 (2020). J. S. Spendelow, DOE Annual Merit Review - Accessible PGM-free Catalysts and Electrodes (2021).
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Pauwels, Bart, and Alexander Sasov. "X-ray Nano- and Micro-tomography in an SEM." Microscopy Today 21, no. 2 (March 2013): 24–28. http://dx.doi.org/10.1017/s1551929513000047.
Abstract:
X-ray microfocus computer tomography (μ-CT) is a non-destructive experimental technique that reveals the 3D internal microstructure of the sample under study. The experimental set-up consists of an X-ray source, an X-ray detector, and set in between is a sample that is placed on a rotation stage. With this set-up multiple X-ray projection images can be obtained from the sample at different angles. In between the acquisition of two successive images, the sample is rotated over a small angle, typically between 0.2° and 1°. This set of projection images is then used as input for the reconstruction algorithm, which calculates a reconstruction of the internal microstructure of the sample with (sub-) micrometer sensitivity.
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Kuan, Aaron T., Jasper S. Phelps, Logan A. Thomas, Tri M. Nguyen, Julie Han, Chiao-Lin Chen, Anthony W. Azevedo, et al. "Dense neuronal reconstruction through X-ray holographic nano-tomography." Nature Neuroscience 23, no. 12 (September 14, 2020): 1637–43. http://dx.doi.org/10.1038/s41593-020-0704-9.
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Kuan, Aaron T. "Dense Neuronal Reconstruction through X-ray Holographic Nano-Tomography." Biophysical Journal 118, no. 3 (February 2020): 290a. http://dx.doi.org/10.1016/j.bpj.2019.11.1647.
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Weker, Johanna Nelson, Xiaojing Huang, and Michael F. Toney. "In situ X-ray-based imaging of nano materials." Current Opinion in Chemical Engineering 12 (May 2016): 14–21. http://dx.doi.org/10.1016/j.coche.2016.01.006.
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Merkle, Arno, Marijn Boone, and Denis Van Loo. "In situ Dynamic X-ray Tomography in the Laboratory." Microscopy and Microanalysis 24, S1 (August 2018): 998–99. http://dx.doi.org/10.1017/s1431927618005482.
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Patterson, Brian M., Nikolaus L. Cordes, Kevin Henderson, Xianghui Xiao, and Nikhilesh Chawla. "In situ Imaging of Materials using X-ray Tomography." Microscopy and Microanalysis 24, S1 (August 2018): 1002–3. http://dx.doi.org/10.1017/s1431927618005500.
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Vamvakeros, Antonios, Simon D. M. Jacques, Marco Di Michiel, Pierre Senecal, Vesna Middelkoop, Robert J. Cernik, and Andrew M. Beale. "Interlaced X-ray diffraction computed tomography." Journal of Applied Crystallography 49, no. 2 (March 1, 2016): 485–96. http://dx.doi.org/10.1107/s160057671600131x.
Abstract:
An X-ray diffraction computed tomography data-collection strategy that allows, post experiment, a choice between temporal and spatial resolution is reported. This strategy enables time-resolved studies on comparatively short timescales, or alternatively allows for improved spatial resolution if the system under study, or components within it, appear to be unchanging. The application of the method for studying an Mn–Na–W/SiO2 fixed-bed reactor in situ is demonstrated. Additionally, the opportunities to improve the data-collection strategy further, enabling post-collection tuning between statistical, temporal and spatial resolutions, are discussed. In principle, the interlaced scanning approach can also be applied to other pencil-beam tomographic techniques, like X-ray fluorescence computed tomography, X-ray absorption fine structure computed tomography, pair distribution function computed tomography and tomographic scanning transmission X-ray microscopy.
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José Querino de Vasconcelos, Gustavo, Eduardo Xavier Miqueles, and Gabriel Schubert Ruiz Costa. "Responsive alignment for X-ray tomography beamlines." Journal of Synchrotron Radiation 25, no. 6 (September 20, 2018): 1774–79. http://dx.doi.org/10.1107/s1600577518012201.
Abstract:
X-ray computed tomography (CT) is an imaging technique intended to obtain the internal structure and three-dimensional representation of a sample. In general, parallel-beam CT reconstruction algorithms require a precise angular alignment and knowledge of the exact axis of rotation position. Highly brilliant X-ray sources with ever-increasing data-acquisition rates demand optimized alignment techniques to avoid compromising in situ data analysis. This paper presents a method to automatically align the angular orientation and linear position of the rotation axis in a tomography setup, correlating image features from different X-ray projections.
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Chichón, Francisco Javier, Maria Josefa Rodríguez, Eva Pereiro, Michele Chiappi, Beatriz Perdiguero, Peter Guttmann, Stephan Werner, et al. "Cryo X-ray nano-tomography of vaccinia virus infected cells." Journal of Structural Biology 177, no. 2 (February 2012): 202–11. http://dx.doi.org/10.1016/j.jsb.2011.12.001.
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Maire, Éric, J. C. Grenier, and L. Babout. "Damage Investigation in Aluminium Alloys by X Ray Tomography." Materials Science Forum 519-521 (July 2006): 821–27. http://dx.doi.org/10.4028/www.scientific.net/msf.519-521.821.
Abstract:
X-ray tomography allows the microstruture of aluminum alloys to be imaged non destructively in three dimensions (3D). This paper shows different examples of the use of this technique for the quantification of damage in model and industrial Al based materials. The model materials are used to setup the technique. The spherical shape of their inclusions makes it easy to compare the measurements with the prediction of standard model for damage. The industrial materials are characterized during in situ tensile but also ex situ bulging and plane strain tension tests. The respective contribution of initiation and growth of damage is measured separately and discussed. The 3D data are also used to quantify the anisotropy of the effect of damage.
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Wu, Yanlin, Hidekazu Takano, Karol Vegso, Masato Hoshino, Koichi Matsuo, and Atsushi Momose. "X-Ray Phase Nano-tomography by FZP-based X-Ray Microscopy Combined with Talbot Interferometry." Microscopy and Microanalysis 24, S2 (August 2018): 226–27. http://dx.doi.org/10.1017/s1431927618013478.
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Hasçakir, B., G. Glatz, L. M. M. Castanier, and A. R. R. Kovscek. "In-Situ Combustion Dynamics Visualized With X-Ray Computed Tomography." SPE Journal 16, no. 03 (June 9, 2011): 524–36. http://dx.doi.org/10.2118/135186-pa.
Abstract:
Summary One method to access unconventional, heavy-oil resources is to apply in-situ combustion (ISC) to oxidize in place a small fraction of the hydrocarbon, thereby providing heat and pressure that enhances recovery. ISC is also attractive because it provides the opportunity to upgrade oil in situ by increasing the API gravity and decreasing, for instance, sulfur content. Despite a considerable literature on ISC dynamics, the propagation of a combustion front through porous media has never been visualized directly. We use X-ray computed tomography (CT) to monitor ISC movement, displacement-front shape, and thickness in a 1-m-long "combustion" tube. Temperature-profile history, liquid production, and effluent gas data are also obtained. Tests employ an 8.65°API heavy crude oil and representative sand. The general trend of saturation profiles is defined through spatially and temporally varying CT numbers. The role of initial oil and water saturations is examined by packing the combustion tube with either multiple samples with different saturations or by filling it with a uniform sample. Our work quantifies that ISC fronts display instabilities on a fine scale (cm). ISC reactions appear to add to front instability in comparison to inert gas advance. The pressure gradients during ISC appear to influence grain arrangement for loose packing. These grain arrangements cause combustion-front fingering, suggesting that the geomechanical state is relevant to combustion. These new data advance the knowledge base significantly by providing a data set for benchmarking of ISC simulations.
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Chu, Y. S., F. De Carlo, J. D. Almer, and D. C. Mancini. "Development of in situ x-ray tomography-diffraction technique (abstract)." Review of Scientific Instruments 73, no. 3 (March 2002): 1656. http://dx.doi.org/10.1063/1.1448133.