Evaluation of elastic constants of M23C6 and M7C3 embedded in Fe-Cr-C alloys using in-situ XRD tensile test and self-consistent model
Not Available
Lee, Hoon (ORCID:0000000320040395)↗
Engineering topics
Almer, Jonathan
Publications and source records attributed to Almer, Jonathan.
FY24 accomplishments in preparation for startup of Activated Materials Laboratory (AML)
The Activated Materials Laboratory (AML) will be a new radiological facility at the Advanced Photon Source (APS) in Argonne National Laboratory (ANL), adjacent to the high-energy x-ray microscopy (HEXM) beamline in the long beamline building (LBB) constructed under the APS-upgrade (APS-U) project. The AML is a centralized facility to facilitate the safe conduct of experiments on activated materials at the APS. This report provides an overview of the status of the AML as a Nuclear Science User Facilities (NSUF) partner user facility in preparation for the general user access in 2025 upon the commissioning of the APS-U beamlines. The AML's scope, functionality and components are detailed. The NSUF partner beamlines’ commissioning status in the post-APS-U era is provided, along with the AML’s operational updates and operational plan.
73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗
Synchrotron micro-computed tomography analysis of neutron-irradiated U-Mo fuel
The three-dimensional (3D) microstructure of neutron-irradiated uranium-10 wt.% molybdenum (U-10Mo) fuel with a burn-up of 9.8 × 10 21 fissions/cm 3 was characterized using a novel, multi-modal synchrotron micro-computed tomography approach combining propagation-based phase-contrast enhanced and absorption contrast techniques. The porosity development, porosity interconnectedness, swelling, composition, local thickness of the zirconium (Zr) diffusion barrier, and the influence of the fuel–cladding interaction on the local composition and pore morphology, were uniquely determined in 3D. Two cuboids were produced using a focused ion beam-scanning electron microscope at the Zr diffusion barrier–fuel interface and in the bulk fuel. The bulk fuel sample swelled by 53.3 [+9.7/−3.1]%, while the fuel near the Zr–fuel interface swelled by 63.3 [+14.7/−7.2]%. The average local thickness of the Zr diffusion barrier decreased by 53 %, compared to the expected pre-irradiated thickness. Four pore morphology regions were identified initiating parallel to the fuel–Zr interaction region: (1) an interaction layer of suppressed porosity, (2) a layer of elongated and interconnected porosity, (3) a transition zone of low porosity, and (4) a layer of unoriented porosity representative of the bulk fuel behavior. The increase in porosity near the diffusion barrier corresponded to a higher U concentration compared to that in the bulk fuel. The interconnected porosity in the fuel near the diffusion barrier was extensive and oriented parallel to the diffusion barrier, while the bulk fuel had more compact and isolated pore networks. The interaction layer, despite having suppressed porosity, was nearly 100 wt.% U. Porosity suppression at the diffusion barrier corresponds to the expected reduction in radiation-driven diffusion of Xe at the interface despite the anticipated increase in fission product nucleation originating from a higher U concentration. In conclusion, the novel 3D insights of the porosity, swelling, and compositional variations characterized herein can improve the fidelity of fuel performance codes for proliferation-resistant fuels for research and test reactors.
11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
FY23 Status Report of the Activated Materials Laboratory at the Advanced Photon Source
The Activated Materials Laboratory (AML) is a new radiological facility located at the Advanced Photon Source (APS) in Argonne National Laboratory (ANL), adjacent to the high-energy x-ray microscopy (HEXM) beamline in the long beamline building (LBB) constructed under the APS-upgrade (APS-U) project. The AML is a centralized facility to facilitate the safe conduct of experiments on activated materials at the APS. This report provides an overview of the status of the AML as a Nuclear Science User Facilities (NSUF) partner user facility in preparation for the general user access in 2024 upon the commissioning of the APS-U beamlines. Specifically, details are provided regarding the laboratory's scope, functionality, components, operational blueprint, and data management approach. The plans on augmenting the instrumentation, refining operational procedures and developing a robust data management strategy for FY24 and beyond are also discussed.
43 PARTICLE ACCELERATORS↗
Dynamic In‐Plane Heterogeneous and Inverted Response of Graphite to Fast Charging and Discharging Conditions in Lithium‐Ion Pouch Cells
Solutions for improving fast charging of lithium‐ion batteries have largely focused on alleviating through‐plane lithiation gradients while little is understood about in‐plane heterogeneities and how to resolve them. Herein, high‐speed synchrotron X‐ray diffraction (XRD) resolves graphite lithiation spatially and temporally during 6 C charging and 2 C discharging. At every point during operation, considerable differences in the state of lithiation across the pouch cell are present. Some regions are more responsive to operation than others, reaching full lithiation early during charge and full delithiation during discharge. Other regions within the cell never fully delithiate during discharge, despite a prolonged voltage hold at 2.8 V. Using time‐resolved XRD data, the calculated local current density (mA cm −2 ) at the graphite surface shows an unexpected occurrence of local inverted current densities where regions of graphite are observed to delithiate during charging and lithiate during discharging. A pseudo‐3D model is developed for the graphite electrode with spatially varying microstructural tortuosity to show how microstructural heterogeneity could influence spatial charge dynamics. The model could not predict the complex in‐plane charge behavior observed within the cell. Consequently physics‐based charging protocols based on homogeneous electrode assumptions may underestimate the local variations in charge dynamics and occurrence of lithium plating.
25 ENERGY STORAGE↗
Thermally Grown Oxide Stress in PS-PVD and EB-PVD Thermal Barrier Coatings Observed at Various Lifetimes Via Synchrotron X-ray Diffraction
The current standard application method for thermal barrier coatings (TBCs) on turbine blades for jet engines is electron-beam physical vapor deposition (EB-PVD) due to its high strain tolerance and low thermal conductivity. An emerging deposition method, plasma-spray physical vapor deposition (PS-PVD), presents an opportunity for a tailorable microstructure, and non-line-of-sight deposition that is faster and less expensive. To compare the lifetime behavior of both PS-PVD and EB-PVD coatings, samples subjected to 300 and 600 thermal cycles were measured during a 1 h thermal cycle to determine the strains, which were converted to stress, in the thermally grown oxide (TGO) layer of the TBCs using synchrotron X-ray diffraction (XRD). Room temperature XRD measurements indicated among samples that PS-PVD coatings experienced greater variation in in-plane room temperature strain in the TGO after cycling than the EB-PVD coatings. In-situ XRD measurements indicated similar high-temperature strain and no spallation after 600 thermal cycles for both coatings. Further, microscopy imaging after cycling showed greater rumpling in PS-PVD coatings that led to different failure modes between the two coatings’ TGO layers. The tailorability of PS-PVD coatings allows for adjustments in the processing parameters to improve their overall performance after aging and bridge the differences between the two deposition methods.
36 MATERIALS SCIENCE↗
Polymorphism of garnet solid electrolytes and its implications for grain-level chemo-mechanics
Understanding and mitigating filament formation, short-circuit and solid electrolyte fracture is necessary for advanced all-solid-state batteries. Here, we employ a coupled far-field high-energy diffraction microscopy and tomography approach for assessing the chemo-mechanical behaviour for dense, polycrystalline garnet (Li 7 La 3 Zr 2 O 12 ) solid electrolytes with grain-level resolution. In situ monitoring of grain-level stress responses reveals that the failure mechanism is stochastic and affected by local microstructural heterogeneity. In this work, coupling high-energy X-ray diffraction and far-field high-energy diffraction microscopy measurements reveals the presence of phase heterogeneity that can alter local chemo-mechanics within the bulk solid electrolyte. These local regions are proposed to be regions with the presence of a cubic polymorph of LLZO, potentially arising from local dopant concentration variation. The coupled tomography and FF-HEDM experiments are combined with transport and mechanics modelling to illustrate the degradation of polycrystalline garnet solid electrolytes. The results showcase the pathways for processing high-performing solid-state batteries.
36 MATERIALS SCIENCE↗
Stresses within rare-earth doped yttria-stabilized zirconia thermal barrier coatings from in-situ synchrotron X-ray diffraction at high temperatures
There is a growing interest for smart coatings that can be integrated into turbine engines for in-situ temperature measurements or health monitoring. The addition of rare-earth dopants into standard thermal barrier ceramic top coat materials is used to obtain luminescent coatings that enable spectral measurements, for real-time temperature or health monitoring. The thermomechanical performance and durability of such novel coating compositions in extreme environments still remains to be evaluated. Consequently, the ability to manufacture sensor coatings which present suitable thermal properties needs to be demonstrated. For this study, highly luminescent erbium and europium doped yttria-stabilized zirconia and state-of-the-art yttria-stabilized zirconia coatings manufactured by air plasma spray were characterized to determine the effects of the embedded rareearth dopants on coating internal strain and stress and to quantify and compare their high temperature response using synchrotron X-ray diffraction. In-situ depth-resolved strain measurements were performed at 15 μm intervals along the depth of the coatings to evaluate materials response at key locations, specifically at layer interfaces. In-plane stress was calculated for the coatings and a finite element model was implemented to supplement the results and enable further predictions. The results show that the sensor coatings that were manufactured in this work revealed only minor variations in the strain response of sensor coatings under a typical thermal cycle and especially at temperatures closer to that of gas turbine operating conditions, compared to state-of-the-art coatings. This work demonstrates the viability of manufacturing rare-earth doped yttria-stabilized zirconia coatings that provide beneficial spectroscopic monitoring capabilities while having minimal impact on the thermomechanical response of the thermal barrier coatings.
Air plasma spray↗
Structural changes across thermodynamic maxima in supercooled liquid tellurium: a water-like scenario
Liquid polymorphism is an intriguing phenomenon which has been found in a few single-component systems, the most famous being water. By supercooling liquid Te to more than 130 K below its melting point and performing simultaneous small-angle and wide-angle X-ray scattering measurements, we observe clear maxima in its thermodynamic response functions around 615 K, suggesting the possible existence of liquid polymorphism. A close look at the underlying structural evolution shows the development of intermediate-range order upon cooling, most strongly around the thermodynamic maxima, which we attribute to bond-orientational ordering. The striking similarities between our results and those of water, despite the lack of hydrogen-bonding and tetrahedrality in tellurium, indicate that water-like anomalies may be a general phenomenon among liquid systems with competing bond- and density-ordering.
36 MATERIALS SCIENCE↗
In situ synchrotron tensile investigations on ultrasonic additive manufactured (UAM) zirconium
The microstructure evolution during room temperature uniaxial tensile straining of ultrasonic additive manufactured (UAM) zirconium was evaluated using the Advanced Photon Source (APS) facility. Miniature dog-bone tensile specimens of two orientations were cut from a UAM-fabricated zirconium bar for in situ synchrotron tensile tests. Wide-angle X-ray scattering (WAXS) scanning was used to unveil the changes in microstructure of the entire gauge regions throughout the straining. A series of WAXS data analysis methods were utilized to quantify both elastic and plastic deformation mechanisms within the strained specimens. Stress concentrations were identified during early stages of plastic deformation, which become candidate necking positions and eventually lead to failure. Additionally, fracture surface analysis implied that these stress concentration locations may be correlated to the fabrication defects, providing insightful guidance for future improvements of the UAM zirconium fabrication process.
36 MATERIALS SCIENCE↗
Mechanism of chlorine-induced stress corrosion cracking of two 304 SS heats in simulated marine environment through in situ X-ray tomography and diffraction: Role of deformation induced martensite and crack branching
In this work, In-situ synchrotron x-ray tomography and diffraction experiments were conducted on two heats of 304SS undergoing chlorine-induced stress-corrosion-cracking (CISCC) in a simulated marine environment. The role of deformation induced martensite on CISCC was investigated through diffraction analysis where no significant amount of martensite was found to form during CISCC, indicating that it may not play a significant role in affecting the process. Tomography combined with stress-intensity analysis revealed the influence of stress-intensity on branching types with single crack growth, micro-branching, and macro-branching. Post experimental electron microscopy characterization revealed the presence of FeCl 2 , CrCl 2 , and NiCl 2 ·6H 2 O compounds at the crack, which infers a dissolution mechanism during the experiment. A dissolution mechanism highlighting the synergy between stress and corrosion was proposed to explain chlorine-induced stress-corrosion-cracking and crack branching.
36 MATERIALS SCIENCE↗
Investigation of the fatigue crack behavior of 304 stainless steels using synchrotron X-ray tomography and diffraction: Influence of the martensite fraction and role of inclusions
Here, the effect of fatigue on the microstructure of four-point bend specimens of three variations of 304 stainless steels (Commercial 304, 304H, and 304 L) was investigated using synchrotron x-ray tomography and diffraction. X-ray tomography revealed the formation of the fatigue-induced microvoids and crack while the diffraction data was used to quantify the amount of deformation-induced martensite found after fatigue in all samples. Transmission electron microscopy evidenced the role of the precipitates/inclusions on the microvoid formation. It was found to depend on their chemical nature. The shape of the precipitates/inclusions was also found to have an effect on the microvoid shape.
304 stainless steel↗
Developing ductile and isotropic Ti alloy with tailored composition for laser powder bed fusion
Laser powder bed fusion (LPBF) is an advanced technology to create metallic components with complex geometry. Ti-6Al-4V (Ti64) is one of the most frequently used materials for LPBF. The intrinsic high cooling rates and ultra-high directional thermal gradient of melt, however, lead to a hierarchical structure composed of fine martensitic alpha' within columnar prior-beta grains in LPBF Ti64. This microstructure results in poor ductility and strong mechanical anisotropy in as-built Ti64 components, which largely limit their applications. Here, we report that the above shortcomings can be overcome by tailoring the alloy composition. Specifically, by reducing the aluminum content from 6 wt% to 4 wt%, the resultant LPBF Ti-4Al-4V (Ti44) alloy exhibits substantially improved ductility and mechanical isotropy. These improvements are attributed to grain refinement during solidification and the activation of multiple slip modes and twinning in the as-built material during deformation. This work offers a simple strategy to design new titanium alloys for LPBF with significantly improved ductility and isotropy.
36 MATERIALS SCIENCE↗
4D evolution of Cr 23 C 6 precipitates in neutron-irradiated and annealed HT-UPS steel observed via synchrotron micro-computed tomography
High-temperature-ultrafine precipitate strengthened (HT-UPS) steel is a potential structural material for advanced nuclear reactors; however, its irradiation response is not well understood. This research provides insight into irradiation-induced effects, such as precipitate evolution mechanisms and four-dimensional morphological evolution, in HT-UPS steel using synchrotron micro-computed tomography. Identical specimens were characterized pre-irradiation and post-irradiation following neutron exposure up to 0.3 displacements per atom at 600 °C. Irradiation effects were also differentiated from the annealing response of precipitates. Following neutron irradiation, the average Cr 23 C 6 precipitate size reduced, affected by the synergy of nucleation and growth, ballistic dissolution, and inverse coarsening, which was observed at fluences an order of magnitude lower than previously observed. Annealing at 600 °C for 32 h increased the average Cr 23 C 6 precipitate size and decreased the phase fraction, attributed to precipitate coarsening. The precipitate morphology evolution and resultant mechanisms can be utilized to parameterize and validate microstructural models simulating radiation damage or annealing.
36 MATERIALS SCIENCE↗
BraggNN : fast X-ray Bragg peak analysis using deep learning
X-ray diffraction based microscopy techniques such as high-energy diffraction microscopy (HEDM) rely on knowledge of the position of diffraction peaks with high precision. These positions are typically computed by fitting the observed intensities in detector data to a theoretical peak shape such as pseudo-Voigt. As experiments become more complex and detector technologies evolve, the computational cost of such peak-shape fitting becomes the biggest hurdle to the rapid analysis required for real-time feedback in experiments. To this end, we propose BraggNN, a deep-learning based method that can determine peak positions much more rapidly than conventional pseudo-Voigt peak fitting. When applied to a test dataset, peak center-of-mass positions obtained from BraggNN deviate less than 0.29 and 0.57 pixels for 75 and 95% of the peaks, respectively, from positions obtained using conventional pseudo-Voigt fitting (Euclidean distance). When applied to a real experimental dataset and using grain positions from near-field HEDM reconstruction as ground-truth, grain positions using BraggNN result in 15% smaller errors compared with those calculated using pseudo-Voigt. Recent advances in deep-learning method implementations and special-purpose model inference accelerators allow BraggNN to deliver enormous performance improvements relative to the conventional method, running, for example, more than 200 times faster on a consumer-class GPU card with out-of-the-box software.
36 MATERIALS SCIENCE↗
Global and local texture development during initial plastic deformation of cold-pilgered Zircaloy-4 tubing
In this work we present a thorough characterization of the texture development during the initial step of a cold pilgering process of a Zircaloy-4 TREX tube, on which the axial cross section is reduced by 80% over a 40cm length with an overall Q-ratio of 2.34, followed by a recrystallization thermal treatment. Texture across a tapered specimen representing this working zone was characterized by neutron diffraction and high energy synchrotron x-ray diffraction at 28 positions (4 locations along its length and 7 locations across its thickness with 0.3 mm spatial resolution), and on the deformed end after the thermal treatment. Results show that the starting material (TREX tube) presents a texture gradient through its wall thickness, with the c poles aligned to the hoop direction at the outer surface (with radial and hoop Kearns factors: f R =0.36, f H = 0.50), and gradually rotating around the axial direction to become a quasi-radial orientation (~35 o out of the radial direction) at the inner surface ( f R =0.43, f H =0.35). The overall texture becomes more radial due to the cold pilgering, but the texture gradient remains during the whole deformation process, being always more radial at the inner surface, ( f R =0.53, f H =0.37 at 80%) than at the outer surface ( f R =0.41, f H =0.50at 80%). The most remarkable changes in texture produced by the rolling process is a 30 o rotation of the grains around their c-axis, producing a marked increase of the <11 2 ¯ 0> // axial fiber texture at expenses of the original <10 1 ¯ 0> // axial fiber texture observed in the TREX tube. The observed changes in texture during deformation were correctly explained by visco-plastic self-consistent (VPSC) modelling. This was achieved after the inclusion of the basal <a> slip system, which plays a central role to explain the 30 o rotation around the c-axis during deformation. The texture evolution was correctly described after the inclusion of a drag effect to grain rotation due to the interaction with neighbouring grains. The through thickness texture differences are greatly reduced by the recrystallization thermal treatment, with similar Kearns factors at the inner surface ( f R =0.50, f H =0.28) and the outer surface ( f R =0.48, f H =0.39). The predominance of the <10 1 ¯ 0> // axial fiber texture is recovered after recrystallization.
36 MATERIALS SCIENCE↗