Advanced synchrotron characterization techniques for fusion materials science
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99 GENERAL AND MISCELLANEOUS↗
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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.
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Advancing Battery Manufacturing: Synchrotron Characterization for Industry
Large-scale battery manufacturing requires understanding the fundamental principles of materials and interfaces and relies on advanced techniques for detailed interrogation. Despite advancements in the industrial scale production and their associated quality control tools, challenges such as electrode heterogeneity, internal defects, and largescale material waste (e.g., scrap) can hamper manufacturing. Synchrotron X-ray characterization techniques offer spatial, temporal, and chemical resolution that can provide diagnostic insights for metrology across various manufacturing steps. This review examines the use of synchrotron tools to advance understanding of key steps in the battery manufacturing process. Recent examples demonstrate how synchrotron methods resolve manufacturing challenges and uncover degradation pathways that are otherwise inaccessible. Future directions for advancing battery manufacturing emphasize collaboration between academia and industry through the use of synchrotron X-ray techniques.
Batteries↗
Synchrotron characterization of high-Z, current-mode x-ray detectors
Fast x-ray detectors are critical tools in pulsed power and fusion applications, where detector impulse response of a nanosecond or better is often required. Semiconductor detectors can create fast, sensitive devices with extensive operational flexibility. There is typically a trade-off between detector sensitivity and speed, but higher atomic number absorbers can increase hard x-ray absorption without increasing the charge collection time, provided carriers achieve high velocity. This paper presents x-ray pulse characterization conducted at the Advanced Photon Source of x-ray absorption efficiency and temporal impulse response of current-mode semiconductor x-ray detectors composed of Si, GaAs, and CdTe.
47 OTHER INSTRUMENTATION↗
Synchrotron Characterization of Hydrogen and Ferric Iron in Martian Meteorites
The hydrogen budget of the Martian interior is distributed among several phases: melts, hydrous minerals, and nominally anhydrous minerals like olivine, pyroxene, and garnet. All these phases are vulnerable to loss of hydrogen during shock, excavation and transport via the mechanism of dehydrogenation, in which the charge on the H protons is left behind as polarons on Fe atoms. Thus, both H and F(3x) must be analyzed in order to reconstruct hydrogen and oxygen fugacities on Mars. To date, SIMS data have elucidated D/H and H contents of hydrous phases in SNC meteorites, but anhydrous martian minerals have not been systematically examined for trace hydrogen. Ferric iron has been quantified using XANES in many marital phases, but integrated studies of both Fe(3x) and H on the same spots are really needed to address the H budget. Here, we measure and profile H and Fe(3x) abundances in and across individual grains of glass and silicates in Martian meteorites. We use the new technology of synchrotron microFI'lR spectroscopy to measure the hydrogen contents of hydrous and nominally anhydrous minerals in martian meteorites on 30-100 microns thick, doubly polished thin sections on spots down to 3 x 3 microns. Synchrotron microXANES was used to analyze Fe(3x) on the same scale, and complementary SIMS D/H data will be collected where possible, though at a slightly larger scale. Development of this combination of techniques is critical because future sample return missions will generate only microscopic samples for study. Results have been used to quantitatively assess the distribution of hydrogen and ferric iron among phases in the martian interior, which will better constrain the geodynamic processes of the interior, as well as the overall hydrogen and water budgets on Mars.
Dyar, Melinda D.↗
Micromechanical and fatigue in situ synchrotron characterization of an additively manufactured superalloy with porosity
Additive manufacturing (AM) has the potential to transform component production, but its widespread adoption is constrained by defects, such as pores, that compromise structural integrity. Here, this study investigates the influence of porosity on the micromechanical and fatigue response of AM Inconel 718 (IN718), a widely used aerospace superalloy. One baseline specimen with minimal stochastic porosity and another intentionally seeded with lack of fusion (LOF) pores were examined using high-energy X-ray diffraction microscopy (HEDM) and micro-computed tomography during cyclic loading. Fatigue cracks in the LOF specimen initiated more frequently and at lower cycle counts than in the baseline specimen. The number fraction of fatigue cracks that grew was comparatively higher in the LOF specimen. Grain-level metrics, including stress and diffraction spot widths, were quantified using far-field HEDM. Across the thousands of grains detected in both specimens, the pores in the LOF specimen increased the variability of stress and spot width evolution in the azimuthal direction, the latter serving as a surrogate measure of plastic deformation. However, no correlations emerged between these metrics and grain proximity to fatigue crack initiation sites or pores, underscoring the limitations of grain-averaged metrics for predicting fatigue. Nonetheless, the rich dataset reported here provides a foundation for future modeling efforts.
High-energy X-ray diffraction microscopy↗
Elucidating Cathode Degradation Mechanisms in LiNi 0.8 Mn 0.1 Co 0.1 O 2 (NMC811)/Graphite Cells Under Fast Charge Rates Using Operando Synchrotron Characterization
Li-ion batteries capable of extreme fast charging (XFC) are in demand to facilitate widespread electric vehicle (EV) adoption. While the impact of fast charge on the negative electrode has been studied, degradation of state-of-the-art NMC811 under XFC conditions has not been studied in detail. Herein, cathode degradation is probed in NMC811/graphite batteries by analysis of structural and chemical changes for recovered samples previously cycled under XFC conditions and during typical cycling. NMC surface reconstruction, as determined by soft X-ray absorption, was not detected for recovered electrodes. Furthermore, bulk redox activity from X-ray absorption near edge structure measurements showed more change in the oxidation state of Ni and Co under the 1C charge rate compared to the 4C rate consistent with the electrochemistry. Increased unit cell volume contraction under the 1C rate as determined by operando X-ray diffraction suggests that higher charge rates may provide a protective effect on the cathode by reducing structural distortion due to less delithiation.
25 ENERGY STORAGE↗
Multi-Modal Synchrotron Characterization: Modern Techniques and Data Analysis
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36 MATERIALS SCIENCE↗
Advanced synchrotron characterization techniques for fusion materials science
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99 GENERAL AND MISCELLANEOUS↗
Synchrotron-based Characterization Techniques for Radiation Detection Materials and Devices: An Overview
High-performance room-temperature radiation detectors (high energy resolution for spectrometers, high spatial resolution for imaging devices, and low defect-density for high flux applications) are needed for photon energies (>20 keV) that are not well suited for silicon detectors. Applications for such radiation detectors include nonproliferation, synchrotron, medical, astrophysics, and homeland security. Material- and device- characterization to understand and solve the limiting factors of radiation detection materials and devices is a core element of a radiation detector development R&D program. This presentation will give an overview on the two main synchrotron-based characterization techniques that have been employed by the authors in the last ~20 years: (1) White Beam X-ray Diffraction Topography and (2) Micron-scale detector mapping. A perfect (one domain) crystal (radiation detection material) is a requirement to achieve a highperformance radiation detector. White Beam X-ray Diffraction Topography (WBXDT) allows the rapid screening of the crystallinity of the detector material. With WBXDT we can quickly screen CZT and other crystals to make sure they have only one domain, and to see the presence of extended defects and strain fields.
Camarda, Giuseppe S.↗
In situ synchrotron X-ray imaging and mechanical properties characterization of additively manufactured high-entropy alloy composites
Laser beam directed energy deposition has become an increasingly popular advanced manufacturing technique for materials discovery as a result of the in situ alloying capability. In this study, we leverage an additive manufacturing enabled high throughput materials discovery approach to explore the composition space of a graded W x (CoCrFeMnNi) 100–x sample spanning 0 ≤ x ≤ 21 at%. In addition to microstructural and mechanical characterization, synchrotron high speed x-ray computer aided tomography was conducted on a W 20 (CoCrFeMnNi) 80 composition to visualize melting dynamics, powder-laser interactions, and remelting effects of previously consolidated material. Results reveal the formation of the Fe 7 W 6 intermetallic phase at W concentrations> 6 at%, despite the high configurational entropy. Unincorporated W particles also occurred at W concentrations> 10 at% accompanied by a dissolution band of Fe 7 W 6 at the W/matrix interface and hardness values greater than 400 HV. In this work, the primary strengthening mechanism is attributed to the reinforcement of the Fe 7 W 6 and W phases as a metal matrix composite. The in situ high speed x-ray imaging during remelting showed that an additional laser pass did not promote further mixing of the Fe 7 W 6 or W phases suggesting that, despite the dissolution of the W into the Fe 7 W 6 phase being thermodynamically favored, it is kinetically limited by the thickness/diffusivity of the intermetallic phase, and the rapid solidification of the laser-based process.
36 MATERIALS SCIENCE↗
The formation and evolution of Ni 2 Cr precipitates in Ni–Cr model alloys as a function of stoichiometry characterized by synchrotron x-ray diffraction
Ni-based alloys containing significant amounts of Cr, may precipitate new phases during long-term service at elevated temperatures. In Ni–Cr model alloys, the formation of Ni 2 Cr has been found to impact the material properties, including the strength and ductility after isothermal aging below the critical temperature of 590°C. In this work, we quantify the formation and evolution of long-range ordering in four Ni–Cr binary model alloys (Ni/Cr = 1.8, 2.0, 2.2, 2.4) after isothermal aging up to 10,000h at temperatures between 373 and 475°C. The alloys were characterized by hardness testing and synchrotron-based x-ray diffraction to quantify the impact of Ni 2 Cr phase fraction and precipitate size on mechanical properties. After 500h of isothermal aging, the formation of Ni 2 Cr was detected in all four alloys at 475°C. In the stochiometric alloy samples (Ni/Cr = 2.0), the formation of Ni 2 Cr was found after 500 and 3000h aging at 418 and 373°C, respectively. We found that the matrix lattice contraction and Ni 2 Cr phase fraction both saturate after early aging times. This is in stark contrast to the hardness and Ni 2 Cr precipitate size that both continue to increase with increasing aging time. Our results highlight that changes in hardness correlate linearly with Ni 2 Cr precipitate size rather than phase fraction. This important structure-property relationship can potentially help define Ni–Cr-based component lifetimes directly through an understanding of how Ni 2 Cr formation impacts strength and ductility. Here, we find that a precipitation hardening model for critical resolved shear stress with weakly coupled dislocations shows good agreement with the material property changes quantified from experimental measurements.
36 MATERIALS SCIENCE↗
Synchrotron Microanalytical Characterization and K/Ar Dating of the GL-O-1 Glauconite Reference Material at the Single Pellet Scale and Reassessment of the Age of Visually Mature Pellets
The K/Ar chronology of glauconite pellets is a long-used method for directly dating marine sedimentary deposits. Many papers have explored the processes that form glauconite and the factors that lead to greater reliability in the ages. Although K/Ar ages of glauconite are generally in agreement with other measures of stratigraphic age, there are examples of occurrences with ages too old and examples with ages too young. This paper seeks to build on the accumulated knowledge of glauconite, using synchrotron radiation to non-destructively characterize individual pellets and then consecutively measure the argon and potassium to obtain a K/Ar age. This strategy provides the advantage of measurements on a single aliquot while avoiding recoil loss of 40 Ar in the nuclear reactor during irradiation for 40 Ar/ 39 Ar dating. We have used the glauconite reference material GL-O-1 to showcase several non-destructive methods for evaluating the maturity of individual pellets. In our argon measurements, we have found that the radiogenic argon concentration of large bulk samples underestimates the values for individual visually mature pellets, and we determined a K/Ar age of 101.0 ± 0.3 Ma (1σ SEM), M.S.W.D. 0.54 from 15 of 16 visually mature individual pellets. This age is 6% older than the reference value of 95.03 ± 1.11 Ma (1σ), and it is in good agreement with constraints from the U-Pb dating of volcanic minerals near the Albian–Cenomanian boundary.
36 MATERIALS SCIENCE↗
Synchrotron-based techniques for characterizing STCH water-splitting materials
Understanding the role of oxygen vacancy–induced atomic and electronic structural changes to complex metal oxides during water-splitting processes is paramount to advancing the field of solar thermochemical hydrogen production (STCH). The formulation and confirmation of a mechanism for these types of chemical reactions necessitate a multifaceted experimental approach, featuring advanced structural characterization methods. Synchrotron X-ray techniques are essential to the rapidly advancing field of STCH in part due to properties such as high brilliance, high coherence, and variable energy that provide sensitivity, resolution, and rapid data acquisition times required for the characterization of complex metal oxides during water-splitting cycles. X-ray diffraction (XRD) is commonly used for determining the structures and phase purity of new materials synthesized by solid-state techniques and monitoring the structural integrity of oxides during water-splitting processes (e.g., oxygen vacancy–induced lattice expansion). X-ray absorption spectroscopy (XAS) is an element-specific technique and is sensitive to local atomic and electronic changes encountered around metal coordination centers during redox. While in operando measurements are desirable, the experimental conditions required for such measurements (high temperatures, controlled oxygen partial pressures, and H 2 O) practically necessitate in situ measurements that do not meet all operating conditions or ex situ measurements. Here, we highlight the application of synchrotron X-ray scattering and spectroscopic techniques using both in situ and ex situ measurements, emphasizing the advantages and limitations of each method as they relate to water-splitting processes. The best practices are discussed for preparing quenched states of reduction and performing synchrotron measurements, which focus on XRD and XAS at soft (e.g., oxygen K-edge, transition metal L-edges, and lanthanide M-edges) and hard (e.g., transition metal K-edges and lanthanide L-edges) X-ray energies. The X-ray absorption spectra of these complex oxides are a convolution of multiple contributions with accurate interpretation being contingent on computational methods. The state-of-the-art methods are discussed that enable peak positions and intensities to be related to material electronic and structural properties. Through careful experimental design, these studies can elucidate complex structure–property relationships as they pertain to nonstoichiometric water splitting. A survey of modern approaches for the evaluation of water-splitting materials at synchrotron sources under various experimental conditions is provided, and available software for data analysis is discussed.
08 HYDROGEN↗
In situ probing of interfacial roughness and transient phases during ceramic cold sintering process
The ceramic cold sintering process (CSP) offers an eco-friendly approach to producing fully dense ceramics at low temperatures. However, an incomplete mechanistic understanding hinders its optimization and widespread adoption. In this study, we analyze the microstructural and structural changes in ZnO, a model CSP system, using in situ synchrotron-based high-energy small-angle X-ray scattering and X-ray diffraction techniques. Our results reveal the time evolution of ZnO particles' surface area and roughness, reflecting the dissolution and re precipitation processes that enable densification. The in situ measurements supply valuable kinetic data for these stages of CSP. Alongside microstructural changes and densification, we observed the evolution of secondary phases representing reaction products between ZnO and acetic acid, the solvent used. The initial ZnO/solvent mixture's dominant secondary phase is attributed to zinc acetate, which is gradually replaced by a zinc soap-type structure during CSP. This structure has a large (≈ 21 Å) lattice parameter and is assumed to have a layered nature. The formation of this soap phase, which is retained in the sintered product as an intergranular component, appears to be a signature of successful cold sintering as it facilitates mass transport, leading to densification. Here, our study underscores the potential of in situ synchrotron characterization for revealing microstructural and phase-evolution details during CSP. These findings, which would be challenging to obtain through ex situ measurements, provide crucial data to guide and validate theoretical models, ultimately enhancing CSP's effectiveness and adoption.
36 MATERIALS SCIENCE↗
Bimetallic-Derived Catalytic Structures for CO 2 -Assisted Ethane Activation
In recent years, the simultaneous upgrading of CO 2 and ethane has emerged as a promising approach for generating valuable gaseous (CO, H 2 , and ethylene) and liquid (aromatics and C 3 oxygenates) chemicals from the greenhouse gas CO 2 and large-reserved shale gas. The key challenges for controlling product selectivity lie in the selective C-H and C-C bond cleavage of ethane with the assistance of CO 2 . Bimetallic-derived catalysts likely undergo alloying or oxygen-induced segregation under reaction conditions, thus providing diverse types of interfacial sites, e.g., metal/support (M/M'O x ) interface and metal oxide/metal (M'O x /M) inverse interface, that are beneficial for selective CO 2 -assisted ethane upgrading. The alloying extent can be initially predicted by cohesive energy and atomic radius (or Wigner-Seitz radius), while the preference for segregation to form the on-top suboxide can be approximated using the work function, electronegativity, and binding strength of adsorbed oxygen. Furthermore, bimetallic-derived catalysts are typically supported on high surface area oxides. Modifying the reducibility and acidity/basicity of the oxide supports and introducing surface defects facilitate CO 2 activation and oxygen supplies for ethane activation. Using in situ synchrotron characterization and density functional theory (DFT) calculations, we found that the electronic properties of oxygen species influence the selective cleavage of C-H/C-C bonds in ethane, with electron-deficient oxygen over the metal (or alloy) surface promoting nonselective bond scission to produce syngas and electron-enriched oxygen over the metal oxide/metal interface enhancing selective C-H scission to yield ethylene. Here, we further demonstrate that the preferred structures of the catalyst surfaces, either alloy surfaces or metal oxide/metal inverse interfaces, can be controlled through the appropriate choice of metal combinations and their atomic ratios. Through a comprehensive comparison of experimental results and DFT calculations, the selectivity of C-C/C-H bond scission is correlated with the thermodynamically favorable bimetallic-derived structures (i.e., alloy surfaces or metal oxide/metal inverse interfaces) under reaction conditions over a wide range of bimetallic catalysts. These findings not only offer structural and mechanistic insights into bimetallic-derived catalysts but also provide design principles for selective catalysts for CO 2 -assisted activation of ethane and other light alkanes. This Account concludes by discussing challenges and opportunities in designing advanced bimetallic-derived catalysts, incorporating new reaction chemistries for other products, employing precise synthesis strategies for well-defined structures with optimized site densities, and leveraging time/spatial/energy-resolved in situ spectroscopy/scattering/microscopy techniques for comprehensive structural analysis. The research methodologies established here are helpful for the investigation of dynamic alloy and interfacial structures and should inspire more efforts toward the simultaneous upgrading of CO 2 and shale gas.
03 NATURAL GAS↗
Elucidating a dissolution–deposition reaction mechanism by multimodal synchrotron X-ray characterization in aqueous Zn/MnO 2 batteries
Aqueous Zn/MnO 2 batteries with their environmental sustainability and competitive cost, are becoming a promising, safe alternative for grid-scale electrochemical energy storage. Here, presented as a promising design principle to deliver a higher theoretical capacity, this work offers fundamental understanding of the dissolution–deposition mechanism of Zn/β-MnO 2 . A multimodal synchrotron characterization approach including three operando X-ray techniques (powder diffraction, absorption spectroscopy, and fluorescence microscopy) is coupled with elementally resolved synchrotron X-ray nano-tomography. Together they provide a direct correlation between structural evolution, reaction chemistry, and 3D morphological changes. Operando synchrotron X-ray diffraction and spectroscopy show a crystalline-to-amorphous phase transition. Quantitative modeling of the operando data by Rietveld refinement for X-ray diffraction and multivariate curve resolution (MCR) for X-ray absorption spectroscopy are used in a complementary fashion to track the structural and chemical transitions of both the long-range (crystalline phases) and short-range (including amorphous phases) ordering upon cycling. Scanning X-ray microscopy and full-field nano-tomography visualizes the morphology of electrodes at different electrochemical states with elemental sensitivity to spatially resolve the formation of the Zn- and Mn-containing phases. Overall, this work critically indicates that for Zn/MnO 2 aqueous batteries, the reaction pathways involving Zn–Mn complex formation upon cycling become independent of the polymorphs of the initial electrode and sheds light on the interplay among structural, chemical, and morphological evolution for electrochemically driven phase transitions.
36 MATERIALS SCIENCE↗
Synchrotron X-ray topographic characterization of dislocations in 6H-SiC axial samples
Not Available
Peng, Hongyu↗
Synchrotron X-ray topography characterization of high quality ammonothermal-grown gallium nitride substrates
Abstract not provided
Liu, Yafei↗