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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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At least 109 records · Page 6
All sourcesNASA NTRSDOE OSTI
DOE OSTI2018

The effect of scanning jitter on geometric phase analysis in STEM images

Geometric phase analysis (GPA) is a useful method to map strain distribution in atomically resolved scanning/transmission electron microscopy (S/TEM) images. Nevertheless, the inevitable periodic jitter of electron probe in STEM along the scanning direction due to the interference of electric power supply, including grounding, can give rise to major artifacts, as evidenced by the appearance of satellite spots surrounding all main peaks in the power spectrum of the images. Here we reveal the origin of the image artifacts related to the probe jitter by mapping the image distortion component εxx using the GPA algorithm. The effect is verified by introducing a periodic displacement field to a STEM image simulated from a perfect crystal structure, and the calculated εxx maps show very good agreement with the experimental observations. Based on the quantitative analysis of the images distortion, we propose and test a feasible strategy to eliminate the effect of probe jitter from STEM images. Successful examples illustrate that the approach can help improve the accuracy in quantification of STEM images.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
NASA NTRS2013

Design and Application of Hybrid Magnetic Field-Eddy Current Probe

The incorporation of magnetic field sensors into eddy current probes can result in novel probe designs with unique performance characteristics. One such example is a recently developed electromagnetic probe consisting of a two-channel magnetoresistive sensor with an embedded single-strand eddy current inducer. Magnetic flux leakage maps of ferrous materials are generated from the DC sensor response while high-resolution eddy current imaging is simultaneously performed at frequencies up to 5 megahertz. In this work the design and optimization of this probe will be presented, along with an application toward analysis of sensory materials with embedded ferromagnetic shape-memory alloy (FSMA) particles. The sensory material is designed to produce a paramagnetic to ferromagnetic transition in the FSMA particles under strain. Mapping of the stray magnetic field and eddy current response of the sample with the hybrid probe can thereby image locations in the structure which have experienced an overstrain condition. Numerical modeling of the probe response is performed with good agreement with experimental results.

Wincheski, Buzz↗
DOE OSTI2017

Tailoring the Properties of a Ni-Based Superalloy via Modification of the Forging Process: an ICME Approach to Fatigue Performance

Traditionally, material design and property modifications are usually associated with compositional changes. However, subtle changes in the manufacturing process parameters can also have a dramatic effect on the resulting material properties. In this work, an integrated computational materials engineering (ICME) framework is adopted to tailor the fatigue performance of a Ni-based superalloy, RR1000. An existing fatigue model is used to identify microstructural features that promote enhanced fatigue life, namely a uniform, fine grain size distribution, random orientation, a distinct grain boundary distribution (specifically high twin boundary density and limited low-angle grain boundaries). A deformation mechanism map and process models for grain boundary engineering of RR1000 are used to identify the optimal thermo-mechanical processing parameters to realize these desirable microstructural features. For validation, small-scale forgings of RR1000 were produced and heat-treated to attain fine grain and coarse grain microstructures that represent the conventionally processed and grain boundary engineered (GBE) conditions, respectively. For each of the four microstructural variants of RR1000, the twin density and grain size were characterized and were in agreement with the desired microstructural attributes. In order to validate the deformation mechanisms and fatigue behavior of the material, high-resolution digital image correlation was performed to generate strain maps relative to the microstructural features. The high density of twin boundaries was confirmed to inhibit the length of slip bands, which is directly attributed to extended fatigue life. Thus, this study demonstrated the successful role of models, both process and performance, in the design and manufacture of Ni-based superalloy disk forgings.

36 MATERIALS SCIENCE↗
DOE OSTI2023

The physics of desiccation cracks 2: Modeling and prediction of the crack patterns

Here, this paper extends the experimental results of our companion paper by modeling and predicting the onset and pattern formation of desiccation cracks in geomaterials (Ruoyu et al., 2023). Thin-layer silt samples in controlled atmospheric conditions were tested to obtain the surface strain maps with the digital image correlation (DIC) method during dehydration. Support experiments, including consolidation and displacement-controlled triaxial tests, were conducted for the properties of geomaterials. These experimental results were used to validate a viscoplastic theoretical model by comparing cracks and singularities locations that distribute following the Cnoidal wave pattern. A critical value exists in the viscoplastic model that determines the number of singularities, which accurately predicts the number of cracks in the experiment. The critical values contain two crucial parameters: rate sensitivity and λ. Rate sensitivity describes the rate-dependent stress–strain relation, while λ shows the ability of pore pressure redistribution under the external mechanical loading rate. These results provide a new view to analyze the desiccation cracks considering the rate-dependent viscoplasticity.

42 ENGINEERING↗
DOE OSTI2023

HFTS-1 (Final Report)

Despite the long history of hydraulic fracturing, the optimal number of fracturing stages during multi-stage fracture stimulation in horizontal wells can be a complex subject. In addition to the increased expense of multistage fracturing in horizontal wells, increasing the number of fracturing stages does not always correlate with a commensurate increase in production. The problem is the application of a uniform fracture stimulation design to all stages with no consideration for geological variations along the wellbore. The result is an inefficient use and costly waste of energy and water. Optimization of the fracturing process requires an understanding of the cause-and-effect relationship between fracturing parameters and local geological properties at a given location along the wellbore. Realizing that the generalized rock mechanics theories and hypotheses are not truly applicable to fractured and laminated shales, quantifiable impacts of a shale’s geomechanical and depositional features are a prerequisite for design and implementation of optimized hydraulic fractures. The overarching goal of this project is to understand and define the relationships of shale geology and fracture dynamics using detailed field data that includes coring of the fracture domain. Finally, resource recovery from shale formations is estimated to be less than fifteen percent. Research proposed in this project will establish the foundations for investigating enhanced recovery techniques for increased resource recovery in existing fracture treated wells. Natural gas as an EOR fluid is in the initial stages of being used broadly in the oil and gas industry and as such, many aspects of the process need to be researched and addressed prior to widespread acceptance. In addition, re-fracturing techniques, particularly using cemented liners also need to be further investigated. This project explores several of these EOR techniques in greater detail, not just at the theoretical level, but through actual field test sites. This report delves into the research program, identified tasks, several studies, observations, results, and conclusions under the Hydraulic Fracturing Test Site (HFTS) project. This test project is subdivided into three distinct phases and each phase is discussed in detail under separate sections. The original test site for Phase 1 as well as the Phase 2 site are in Midland Basin in Texas and operated by Laredo Petroleum. In the first two phases, the program targeted the Wolfcamp formation in Midland Basin. Phase 3 of the study targeted the EagleFord play in South Texas with Devon Energy as the operator. Significant conclusions from this study include: 1) lateral and vertical fracture growth mapping as well as proppant transport behavior, 2) Use of field gas and its applicability for huff n puff EOR injection in the Midland Basin, 3) Development and validation of proppant log, both at core scale as well as in-fill well implementation by analyzing drilling mud return samples, 4) Applicability of liner refracturing including best practices for enhanced unit level productivity. This report will detail all these studies as well as technical results and conclusions from said studies. These include general subsurface characterization work, completion designs as implemented, studies looking at fracture geometry, high resolution microseismic study, advanced crosswell strain mapping studies including drainage characterization, core characterization results, proppant analysis (core and observation wells), geochemistry, etc. to name a few.

02 PETROLEUM↗
DOE OSTI2023

Application of Distributed Fiber Optic Strain Sensors to LMQXFA Cold Mass Welding

The future High Luminosity upgrade of the Large Hadron Collider (HL-LHC) at CERN will include the low-beta inner triplets (Q1, Q2a/b, Q3) for two LHC insertion regions. The Q1, Q3 components consist of eight 10 m-long LMQXFA cryo-assemblies fabricated by the HL-LHC Accelerator Upgrade Project. Each LMQXFA Cold mass contains two Nb 3 Sn magnets connected in series. A stainless-steel shell is welded around the two magnets before the insertion into the cryostat. There is a limit on how much coil preload increase induced by the shell welding is allowed. Distributed Rayleigh backscattering fiber optics sensors were used for the first time to obtain a strain map over a wide area of a Nb 3 Sn magnet cold mass shell. Finally, data were collected during welding of the first LMQXFA cold mass and the results confirm that the increase of the coil pole azimuthal pre-stress after welding do not exceed requirements.

43 PARTICLE ACCELERATORS↗
DOE OSTI2021

Beamline K11 DIAD: a new instrument for dual imaging and diffraction at Diamond Light Source

The Dual Imaging and Diffraction (DIAD) beamline at Diamond Light Source is a new dual-beam instrument for full-field imaging/tomography and powder diffraction. This instrument provides the user community with the capability to dynamically image 2D and 3D complex structures and perform phase identification and/or strain mapping using micro-diffraction. The aim is to enable in situ and in operando experiments that require spatially correlated results from both techniques, by providing measurements from the same specimen location quasi-simultaneously. Using an unusual optical layout, DIAD has two independent beams originating from one source that operate in the medium energy range (7–38 keV) and are combined at one sample position. Here, either radiography or tomography can be performed using monochromatic or pink beam, with a 1.4 mm × 1.2 mm field of view and a feature resolution of 1.2 µm. Micro-diffraction is possible with a variable beam size between 13 µm × 4 µm and 50 µm × 50 µm. One key functionality of the beamline is image-guided diffraction, a setup in which the micro-diffraction beam can be scanned over the complete area of the imaging field-of-view. This moving beam setup enables the collection of location-specific information about the phase composition and/or strains at any given position within the image/tomography field of view. The dual beam design allows fast switching between imaging and diffraction mode without the need of complicated and time-consuming mode switches. Real-time selection of areas of interest for diffraction measurements as well as the simultaneous collection of both imaging and diffraction data of (irreversible) in situ and in operando experiments are possible.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Poisson’s ratio of eTPU molded bead foams in compression via in situ synchrotron X-ray microtomography

In situ synchrotron X-ray microtomography was used to characterize the bulk deformation behavior by computing the Poisson's ratio of expanded thermoplastic polyurethane (eTPU) molded bead foams used in footwear midsole during compression. Quantitative data on morphological characteristics were obtained using an iterative image processing workflow. Image correlation on the 4D datasets using DVC was performed to calculate the volumetric and axial strain to estimate the Poisson ratio. Strain maps from DVC showed the influence of variability in ligament thickness distribution on the global mechanical behavior exhibited which dominated the response seen in these bead foams. Lastly, our results showed a strong correlation between Poisson ratio and distribution of ligament thickness in foams.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Elucidating the role of Cr migration in Ni-Cr exposed to molten FLiNaK via multiscale characterization

Structural materials used in nuclear reactor environments are subjected to coupled extremes such as high temperature, irradiation, and corrosion which act in concert to degrade their functional performance. Connecting alloy microstructure such as grain boundaries, and accumulating point defects with corrosion attack and pore morphology is critical to understanding underlying mechanisms. We uncover the compositional variations and morphology at multiple length scales in corrosion-damaged Ni-Cr alloy after exposure to oxidants in molten fluoride salts. A complex network of dense corrosion pores is detected by surface-level SEM observations. The corrosion pores take on a 1-dimensional morphology and are enriched with Ni and depleted of Cr 1–5 µm from the pore surface. STEM-EDS and 4D-STEM strain maps acquired simultaneously highlight the local variations in composition and structure of a ≤ 200 nm Cr-rich layer identified from a cross-section taken at the bottom of an isolated corrosion pore between the Ni-Cr alloy matrix and the embedded salt. However, the absence of an observed interface between the Ni-Cr alloy matrix and the FCC-structured Cr-rich layer suggests that Cr plating from the salt did not transpire. These findings support a proposed Cr lattice diffusion mechanism rather than Cr-precipitation from the salt to accommodate temperature transient conditions during sample cooling. Through the development of a 1D phase field model, these results are rationalized by formation energies for the Ni- and Cr-oxidation into the molten salt. This study reveals the locally altered microstructure caused by high temperature corrosion in non-steady-state molten salt nuclear reactor environments.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Deformation fields near a steady fatigue crack with anisotropic plasticity

In this work, from finite element simulations based on an irreversible, hysteretic cohesive interface model, a steady fatigue crack can be realized if the crack extension exceeds about twice the plastic zone size, and both the crack increment per loading cycle and the crack bridging zone size are smaller than the plastic zone size. The corresponding deformation fields develop a plastic wake behind the crack tip and a compressive residual stress field ahead of the crack tip. In addition, the Hill’s plasticity model is used to study the role of plastic anisotropy on the retardation of fatigue crack growth and the elastic strain fields. It is found that for Mode-I cyclic loading, an enhanced yield stress in directions that are inclined from the crack plane will lead to slower crack growth rate, but this retardation is insignificant for typical degrees of plastic anisotropy. Furthermore, these results provide key inputs for future comparisons to neutron and synchrotron diffraction measurements that provide full-field lattice strain mapping near fracture and fatigue crack tips, especially in textured materials such as wrought or rolled Mg alloys.

36 MATERIALS SCIENCE↗
DOE OSTI2023

The physics of desiccation cracks 1: Ductile fracturing and dependence on relative humidity

Ductile deformation is ubiquitously found in the shrinkage of geomaterials. The existence of ductility requires elastoplastic mechanics when analyzing the structure deformation under external stress. Here, in this work, we explore the physics of ductile fracturing based on the results from desiccation experiments and triaxial tests. By using the digital image correlation (DIC) method to generate the strain maps of samples undergoing desiccation cracking under different relative humidities, we obtain results showing the previously postulated Cnoidal Wave ductile failure patterns propagating under atmospheric condition-controlled crack velocities. We then correlate these observations with rate-dependent plasticity models calibrated through triaxial tests undergoing several unloading–reloading cycles and velocity stepping. This work demonstrates the necessity to consider ductility in soil cracking, indicating that the formation of crack patterns in soil desiccation is a slow and predictable process.

58 GEOSCIENCES↗
DOE OSTI2024

Correlating microstructure and mechanical properties of harvested high dose Zorita light water reactor internals

Here, in this study, microstructural studies and micro-mechanical testing of an ex-plant material harvested from the decommissioned pressurized water reactor (PWR) is carried out. Irradiated 304 stainless steel (SS) components were harvested by the Electric Power Research Institute, U.S. Nuclear Regulatory Commission, and members of the José Cabrera Nuclear Power Station (Zorita) in Spain. The bi-crystalline micro-tensile specimens, atom probe tomography (APT) tips, and transmission electron microscopy (TEM) lamellae were fabricated from the baffle plate materials irradiated to 0.05, 15 and 50 dpa to elucidate microstructural, microchemical, and local mechanical properties changes as a function of dose. TEM and APT studies reveal radiation induced Ni, Cr, and Si rich precipitates in the 15 dpa sample that become smaller and partially redissolve into the matrix of the 50 dpa sample (decreasing size and number density). Dislocation loop and cavity number density and size were quantified as a function of dose as well as swelling. Intergranular Ni and Si enrichments with concomitant Fe and Cr depletion were observed in the 15 dpa sample and were more pronounced in the 50 dpa sample. Micro-tensile testing performed in the scanning electron microscope (SEM) at room temperature and 300 °C shows that the material's local yield strength and ultimate tensile strength decreases with increased dose and elevated test temperature and provides further insights via localized strain mapping. Current and previous mechanical data was compared with calculated values using the dispersed barrier hardening model with inputs of dislocation loops, precipitates, and cavities from microstructural characterization.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Identification and correction of temporal and spatial distortions in scanning transmission electron microscopy

Scanning transmission electron microscopy (STEM) has become the technique of choice for quantitative characterization of atomic structure of materials, where the minute displacements of atomic columns from high-symmetry positions can be used to map strain, polarization, octahedra tilts, and other physical and chemical order parameter fields. The latter can be used as inputs into mesoscopic and atomistic models, providing insight into the correlative relationships and generative physics of materials on the atomic level. However, these quantitative applications of STEM necessitate understanding the microscope induced image distortions and developing the pathways to compensate them both as part of a rapid calibration procedure for in situ imaging, and the post-experimental data analysis stage. Here, we explore the spatiotemporal structure of the microscopic distortions in STEM using multivariate analysis of the atomic trajectories in the image stacks. Based on the behavior of principal component analysis (PCA), we develop the Gaussian process (GP)-based regression method for quantification of the distortion function. The limitations of such an approach and possible strategies for implementation as a part of in-line data acquisition in STEM are discussed. Here, the analysis workflow is summarized in a Jupyter notebook that can be used to retrace the analysis and analyze the reader's data.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Real Space Visualization of Competing Phases in La 0.6 Sr 2.4 Mn 2 O 7 Single Crystals

We report that correlated quantum materials are expected to provide the foundation for the next generation of information or energy technologies. A key feature of these materials is the proximity of multiple ground states close in energy, which results in the ability to tune properties with small changes in an external parameter such as magnetic field, composition, or temperature. For example, the colossal magnetoresistance exhibited by manganites is related to charge and orbital ordering and results from a metallic ferromagnetic phase in proximity to a paramagnetic insulating phase. The presence of competing ground states, at the heart of the physics and functionality of these materials, often results in nanoscale phase separation. Probing nanoscale phase separation with conventional diffraction techniques alone is not adequate, particularly when the domains are small or nanosized. In the present work we use a scanning transmission electron microscopy image-based technique of picometer precision strain maps (PPSM) to directly visualize the competing nanoscale phases with charge and orbital ordering in a double-layer manganite. Finally, this work underscores the role of subtle structural distortions in determining the electron physics in correlated quantum materials and provides insights into designing new functionalities via spatially tuning multiple competing ground states.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Epitaxial Templating of Two-Dimensional Metal Chloride Nanocrystals on Monolayer Molybdenum Disulfide

We demonstrate the formation of ionic metal chloride (CuCl) two-dimensional (2D) nanocrystals epitaxially templated on the surface of monolayer molybdenum disulfide (MoS 2 ). These 2D CuCl nanocrystals are single atomic planes from a nonlayered bulk CuCl structure. They are stabilized as a 2D monolayer on the surface of the MoS 2 through interactions with the uniform periodic surface of the MoS 2 . The heterostructure 2D system is studied at the atomic level using aberration-corrected transmission electron microscopy at 80 kV. Dynamics of discrete rotations of the CuCl nanocrystals are observed, maintaining two types of preferential alignments to the MoS 2 lattice, confirming that the strong interlayer interactions drive the stable CuCl structure. Strain maps are produced from displacement maps and used to track real-time variations of local atomic bonding and defect production. Density functional theory calculations interpret the formation of two types of energetically advantageous commensurate superlattices via strong chemical bonds at interfaces and predict their corresponding electronic structures. These results show how vertical heterostructured 2D nanoscale systems can be formed beyond the simple assembly of preformed layered materials and provide indications about how different 2D components and their interfacial coupling mode could influence the overall property of the heterostructures.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Atomic intercalation to measure adhesion of graphene on graphite

The interest in mechanical properties of layered and 2D materials has reemerged in light of device concepts that take advantage of flexing, adhesion and friction in such systems. Here we provide an effective measurement of the nanoscale elastic adhesion of a graphene sheet atop highly ordered pyrolytic graphite (HOPG) based on the analysis of atomic intercalates in graphite. Atomic intercalation is carried out using conventional ion sputtering, creating blisters in the top-most layer of the HOPG surface. Scanning tunneling microscopy coupled with image analysis and density functional theory are used to reconstruct the atomic positions and the strain map within the deformed graphene sheet, as well as to demonstrate subsurface diffusion of the ions creating such blisters. To estimate the adhesion energy we invoke an analytical model originally devised for macroscopic deformations of graphene. This model yields a value of 0.221 ± 0.011 J/m -2 for the adhesion energy of graphite, which is in surprisingly good agreement with reported experimental and theoretical values. This implies that macroscopic mechanical properties of graphene scale down to at least a few nanometers length. The simplicity of our method, compared to the macroscale characterization, enables analysis of elastic mechanical properties in two-dimensional layered materials and provides a unique opportunity to investigate the local variability of mechanical properties on the nanoscale.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Atomic and electronic structure of Lomer dislocations at CdTe bicrystal interface

Extended defects are of considerable importance in determining the electronic properties of semiconductors, especially in photovoltaics (PVs), due to their effects on electron-hole recombination. We employ model systems to study the effects of dislocations in CdTe by constructing grain boundaries using wafer bonding. Atomic-resolution scanning transmission electron microscopy (STEM) of a [1–10]/ (110) 4.8° tilt grain boundary reveals that the interface is composed of three distinct types of Lomer dislocations. Geometrical phase analysis is used to map strain fields, while STEM and density functional theory (DFT) modeling determine the atomic structure at the interface. The electronic structure of the dislocation cores calculated using DFT shows significant mid-gap states and different charge-channeling tendencies. Cl-doping is shown to reduce the midgap states, while maintaining the charge separation effects. In conclusion, this report offers novel avenues for exploring grain boundary effects in CdTe-based solar cells by fabricating controlled bicrystal interfaces and systematic atomic-scale analysis.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Three-dimensional optical trapping and orientation of microparticles for coherent X-ray diffraction imaging

Optical trapping has been implemented in many areas of physics and biology as a noncontact sample manipulation technique to study the structure and dynamics of nano-andmesoscale objects. It provides a unique approach for manipulating microscopic objects without inducing undesired changes in structure. Combining optical trapping with hard X-ray microscopy techniques, such as coherent diffraction imaging and crystallography, provides a nonperturbing environment where electronic and structural dynamics of an individual particle in solution can be followed in situ. It was previously shown that optical trapping allows the manipulation of micrometer-sized objects for Xray fluorescence imaging. However, questions remain over the ability of optical trapping to position objects for X-ray diffraction measurements, which have stringent requirements for angular stability. Our work demonstrates that dynamic holographic optical tweezers are capable of manipulating single micrometer-scale anisotropic particles in a microfluidic environment with the precision and stability required for X-ray Bragg diffraction experiments-thus functioning as an "optical goniometer." The methodology can be extended to a variety of X-ray experiments and the Bragg coherent diffractive imaging of individual particles in solution, as demonstrated here, will be markedly enhanced with the advent of brighter, coherent X-ray sources.

Gao, Yuan↗