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DOE OSTI2019

Correlated spin canting in ordered core-shell Fe 3 O 4 / Mn x Fe 3 - x O 4 nanoparticle assemblies

Polarization-analyzed small-angle neutron-scattering methods are used to determine the spin arrangements and experimental length scales of magnetic correlations in ordered three-dimensional assemblies of ~7.4-nm-diam core-shell Fe 3 O 4 /Mn x Fe 3–x O 4 nanoparticles. In moderate to high magnetic fields, the assemblies display a canted magnetic structure where the canting direction is coherent from nanoparticle to nanoparticle, in contrast to the less extended, more single-particle-like behavior for similar ferrite assemblies. The observed magnetic scattering is modeled by assuming that the interparticle dipolar coupling combined with Zeeman effects in a field leads to nanoparticle domains with preferred net spin alignments relative to packing symmetry axes. Over a range of fields and temperatures, the model qualitatively explains the observed scattering anomalies in terms of clusters that vary in area and thickness, highlighting the complex structures adopted in real, dense nanoparticle systems. Here, the clusters often have a strong two-dimensional magnetic character which is attributed to structural stacking faults and the resulting influence of interparticle dipolar interactions for these magnetically soft nanoparticles.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2025

Understanding the deformation behavior of the γ rich transformative Fe 38.5 Mn 20 Co 20 Cr 15 Si 5 Cu 1.5 complex concentrated alloy using in situ synchrotron diffraction

In situ tensile testing coupled with synchrotron x-ray diffraction was used to study the deformation behavior of metastability-engineered Fe 38.5 Mn 20 Co 20 Cr 15 Si 5 Cu 1.5 complex concentrated alloy. Monitoring the evolution of phase fraction and strain hardening response allowed the determination of true critical stress for the onset of the transformation-induced plasticity (TRIP) to be ∼375 MPa, preceded by slip starting at ∼255 MPa. In situ EBSD was used to validate the critical stress for transformation at the microstructure level and observe slip traces to confirm prior slip activity before the transformation. Further, a modeling framework based on stacking fault energy (SFE) was developed to predict the critical stress for transformation. Modeling suggested the SFE of the alloy to fall nearly 15 mJ/m 2 , which agrees well with SFE values calculated using synchrotron peak shifting (12 mJ/m 2 ) and thermodynamic calculation (11 mJ/m 2 ). As a result of γ-fcc to ε-hcp phase transformation, new {0002} ε planes emerged parallel to unaligned {111} γ planes with the tensile loading following S-N orientation relationship. Such selective emergence of new diffraction rings corresponding to ε phase is understood based on the reorientation of γ crystals with reference to tensile axis. In conclusion, this approach can be extended to effectively design alloys based on critical stress required for activating different deformation mechanisms to further push the limits of the strength-ductility envelope.

Complex concentrated alloy↗

DOE OSTI2024

Reduced-dimension Bayesian optimization for model calibration of transient vapor compression cycles

Development and calibration of first-principles dynamic models of vapor compression cycles (VCCs) is of critical importance for applications that include control design and fault detection and diagnostics. Nevertheless, the inherent complexity of models that are represented by large systems of differential–algebraic equations leads to significant challenges for model calibration processes that utilize classical gradient-based methods. Bayesian optimization (BO) is a sample-efficient and gradient-free approach using a probabilistic surrogate model and optimal search over a feasible parameter space. Despite the benefits of BO in reducing computational costs, challenges remain in dealing with a high-dimensional calibration task resulting from a large set of parameters that have significant impacts on system behavior and need to be calibrated simultaneously. This paper presents a reduced-dimension BO framework for calibrating transient VCCs models where the calibration space is projected to a low-dimensional subspace for accelerating convergence of the solution algorithm and consequently reducing the number of transient simulations. The proposed approach was demonstrated via two case studies associated with different VCC applications where 10 parameters were calibrated in each case using laboratory measurements. The reduced-dimension BO framework only required 1 / 8 th of the iterations associated with a standard BO method that deals with high-dimensional calibration parameters for converged solutions and yielded comparable accuracy. Furthermore, both calibrated models revealed significant accuracy improvements compared to uncalibrated models.

Ma, Jiacheng↗

DOE OSTI2015

Nonlinear Time Domain Seismic Soil-Structure Interaction (SSI) Deep Soil Site Methodology Development

Currently the Department of Energy (DOE) and the nuclear industry perform seismic soil-structure interaction (SSI) analysis using equivalent linear numerical analysis tools. For lower levels of ground motion, these tools should produce reasonable in-structure response values for evaluation of existing and new facilities. For larger levels of ground motion these tools likely overestimate the in-structure response (and therefore structural demand) since they do not consider geometric nonlinearities (such as gaping and sliding between the soil and structure) and are limited in the ability to model nonlinear soil behavior. The current equivalent linear SSI (SASSI) analysis approach either joins the soil and structure together in both tension and compression or releases the soil from the structure for both tension and compression. It also makes linear approximations for material nonlinearities and generalizes energy absorption with viscous damping. This produces the potential for inaccurately establishing where the structural concerns exist and/or inaccurately establishing the amplitude of the in-structure responses. Seismic hazard curves at nuclear facilities have continued to increase over the years as more information has been developed on seismic sources (i.e. faults), additional information gathered on seismic events, and additional research performed to determine local site effects. Seismic hazard curves are used to develop design basis earthquakes (DBE) that are used to evaluate nuclear facility response. As the seismic hazard curves increase, the input ground motions (DBE’s) used to numerically evaluation nuclear facility response increase causing larger in-structure response. As ground motions increase so does the importance of including nonlinear effects in numerical SSI models. To include material nonlinearity in the soil and geometric nonlinearity using contact (gaping and sliding) it is necessary to develop a nonlinear time domain methodology. This methodology will be known as, NonLinear Soil-Structure Interaction (NLSSI). In general NLSSI analysis should provide a more accurate representation of the seismic demands on nuclear facilities their systems and components. INL, in collaboration with a Nuclear Power Plant Vender (NPP-V), will develop a generic Nuclear Power Plant (NPP) structural design to be used in development of the methodology and for comparison with SASSI. This generic NPP design has been evaluated for the INL soil site because of the ease of access and quality of the site specific data. It is now being evaluated for a second site at Vogtle which is located approximately 15 miles East-Northeast of Waynesboro, Georgia and adjacent to Savanna River. The Vogtle site consists of many soil layers spanning down to a depth of 1058 feet. The reason that two soil sites are chosen is to demonstrate the methodology across multiple soil sites. The project will drive the models (soil and structure) using successively increasing acceleration time histories with amplitudes. The models will be run in time domain codes such as ABAQUS, LS-DYNA, and/or ESSI and compared with the same models run in SASSI. The project is focused on developing and documenting a method for performing time domain, non-linear seismic soil structure interaction (SSI) analysis. Development of this method will provide the Department of Energy (DOE) and industry with another tool to perform seismic SSI analysis.

58 GEOSCIENCES↗

NASA NTRS2011

Model Checking a Self-Stabilizing Distributed Clock Synchronization Protocol for Arbitrary Digraphs

This report presents the mechanical verification of a self-stabilizing distributed clock synchronization protocol for arbitrary digraphs in the absence of faults. This protocol does not rely on assumptions about the initial state of the system, other than the presence of at least one node, and no central clock or a centrally generated signal, pulse, or message is used. The system under study is an arbitrary, non-partitioned digraph ranging from fully connected to 1-connected networks of nodes while allowing for differences in the network elements. Nodes are anonymous, i.e., they do not have unique identities. There is no theoretical limit on the maximum number of participating nodes. The only constraint on the behavior of the node is that the interactions with other nodes are restricted to defined links and interfaces. This protocol deterministically converges within a time bound that is a linear function of the self-stabilization period.

Malekpour, Mahyar R.↗

NASA NTRS2012

Model Checking A Self-Stabilizing Synchronization Protocol for Arbitrary Digraphs

Malekpour, Mahyar R.↗

DOE OSTI2022

Deformation behavior of crystalline/amorphous Al-Si nanocomposites with nanolaminate or nanofibrous microstructures

Deformation mechanisms in sputter-deposited crystalline Al/amorphous Si nanocomposites with nanolaminate or nanofibrous morphology are characterized by nanoindentation, micropillar compression testing and transmission electron microscopy (TEM). The nanofibrous composite having crystalline Al nanofibers with ~40–50 nm in length and 15–20 nm in diameter embedded in amorphous Si exhibits strain hardening to a maximum flow stress of 2.9 GPa and no shear band (SB) formation in compression up to plastic strain exceeding 24%. On the other hand, nanolaminate composite that is composed of 80 nm crystalline Al layers and 20 nm amorphous Si layers exhibits catastrophic SBs starting at plastic strains in the range of 5–10%. Cross-sectional TEM of the deformed samples reveals a high density of stacking faults and twin boundaries in Al nanofibers and no microshear bands in the nanofibrous composite, suggesting plastic deformation in amorphous Si phase and crystalline Al nanofibers. Further, molecular dynamics simulations revealed that the plastic deformation in amorphous Si phase in the cosputtered films could be favored by the decrease in flow strength of amorphous Si with increasing Al solute concentration trapped in Si.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2021

TQEA: Temporal Quantum Error Analysis

For the last few years quantum computers have captured researchers’ interest in solving complicated problems in finance, chemistry, machine learning, and many other NP problems. Quantum computing benefits from parallel computation, entanglement, and calculation speedup compared to classical computing. Even though the operations and number of qubits in quantum computers are limited, previous research showed that using quantum computers can be beneficial. These benefits gained researchers’ interest to work on the improvement of quantum computers and overcome the limitations by building more advanced quantum computers with fault tolerance capability, more physical qubits, and better operational gates. In practice, Quantum applications would be translated into Quantum Circuits and each circuit can contain one or many entanglements (s), single qubits operations, and readouts. The importance of running Quantum applications with controlled errors or without errors is critical to the desired result from Quantum readout. In this paper, we study the characteristics of superconducting quantum machines along with the previously proposed methods of Quantum error detection/correction and in order to build a better error model we propose a temporal method for analyzing the the behavior of qubits errors (T1 and T2), frequency of operation, entanglement errors, and readout errors. In order to detect and predict the behavior of each machine, we use simple exponential smoothing analysis on heuristic calibration data. Finally, based on observation, we show that based on frequency, qubits, readout and single operation errors we can build a temporal based model to study and predict the outcome of runs on each Quantum machine.

Baheri, Betis↗

DOE OSTI2016

Impact of Micro-to Meso-scale Fractures on Sealing Behavior of Argillaceous Cap Rocks For CO 2 Sequestration

This multi-disciplinary project evaluated seal lithologies for the safety and security of long-term geosequestration of CO 2 . We used integrated studies to provide qualitative risk for potential seal failure; we integrated data sets from outcrop, core, geochemical analysis, rock failure properties from mechanical testing, geophysical wireline log analysis, and geomechanical modeling to understand the effects of lithologic heterogeneity and changing mechanical properties have on the mechanical properties of the seal. The objectives of this study were to characterize cap rock seals using natural field analogs, available drillhole logging data and whole-rock core, geochemical and isotopic analyses. Rock deformation experiments were carried out on collected samples to develop better models of risk estimation for potential cap rock seal failure. We also sampled variably faulted and fractured cap rocks to examine the impacts of mineralization and/or alteration on the mechanical properties. We compared CO 2 reacted systems to non-CO 2 reacted seal rock types to determine response of each to increased pore fluid pressures and potential for the creation of unintentional hydrofractures at depth.

58 GEOSCIENCES↗

NASA NTRS2008

NASA Tech Briefs, February 2008

Topics discussed include: Optical Measurement of Mass Flow of a Two-Phase Fluid; Selectable-Tip Corrosion-Testing Electrochemical Cell; Piezoelectric Bolt Breakers and Bolt Fatigue Testers; Improved Measurement of B(sub 22) of Macromolecules in a Flow Cell; Measurements by a Vector Network Analyzer at 325 to 508 GHz; Using Light to Treat Mucositis and Help Wounds Heal; Increasing Discharge Capacities of Li-(CF)(sub n) Cells; Dot-in-Well Quantum-Dot Infrared Photodetectors; Integrated Microbatteries for Implantable Medical Devices; Oxidation Behavior of Carbon Fiber-Reinforced Composites; GIDEP Batching Tool; Generic Spacecraft Model for Real-Time Simulation; Parallel-Processing Software for Creating Mosaic Images; Software for Verifying Image-Correlation Tie Points; Flexcam Image Capture Viewing and Spot Tracking; Low-Pt-Content Anode Catalyst for Direct Methanol Fuel Cells; Graphite/Cyanate Ester Face Sheets for Adaptive Optics; Atomized BaF2-CaF7 for Better-Flowing Plasma-Spray Feedstock; Nanophase Nickel-Zirconium Alloys for Fuel Cells; Vacuum Packaging of MEMS With Multiple Internal Seal Rings; Compact Two-Dimensional Spectrometer Optics; and Fault-Tolerant Coding for State Machines.

Source record↗

DOE OSTI2015

Pressure-induced stiffness of Au nanoparticles to 71 GPa under quasi-hydrostatic loading

The compressibility of nanocrystalline gold (n-Au, 20 nm) has been studied by x-ray total scattering using high-energy monochromatic x-rays in the diamond anvil cell under quasi-hydrostatic conditions up to 71 GPa. The bulk modulus, K 0 , of the n-Au obtained from fitting to a Vinet equation of state is ~196(3) GPa, which is about 17% higher than for the corresponding bulk materials (K 0 : 167 GPa). At low pressures (<7 GPa), the compression behavior of n-Au shows little difference from that of bulk Au. With increasing pressure, the compressive behavior of n-Au gradually deviates from the equation of state (EOS) of bulk gold. Analysis of the pair distribution function, peak broadening and Rietveld refinement reveals that the microstructure of n-Au is nearly a single-grain/domain at ambient conditions, but undergoes substantial pressure-induced reduction in grain size until 10 GPa. The results indicate that the nature of the internal microstructure in n-Au is associated with the observed EOS difference from bulk Au at high pressure. Full-pattern analysis confirms that significant changes in grain size, stacking faults, grain orientation and texture occur in n-Au at high pressure. We have observed direct experimental evidence of a transition in compressional mechanism for n-Au at ~20 GPa, i.e. from a deformation dominated by nucleation and motion of lattice dislocations (dislocation-mediated) to a prominent grain boundary mediated response to external pressure. In conclusion, the internal microstructure inside the nanoparticle (nanocrystallinity) plays a critical role for the macro-mechanical properties of nano-Au.

high pressure DAC↗

NASA NTRS2013

Application Agreement and Integration Services

Application agreement and integration services are required by distributed, fault-tolerant, safety critical systems to assure required performance. An analysis of distributed and hierarchical agreement strategies are developed against the backdrop of observed agreement failures in fielded systems. The documented work was performed under NASA Task Order NNL10AB32T, Validation And Verification of Safety-Critical Integrated Distributed Systems Area 2. This document is intended to satisfy the requirements for deliverable 5.2.11 under Task 4.2.2.3. This report discusses the challenges of maintaining application agreement and integration services. A literature search is presented that documents previous work in the area of replica determinism. Sources of non-deterministic behavior are identified and examples are presented where system level agreement failed to be achieved. We then explore how TTEthernet services can be extended to supply some interesting application agreement frameworks. This document assumes that the reader is familiar with the TTEthernet protocol. The reader is advised to read the TTEthernet protocol standard [1] before reading this document. This document does not re-iterate the content of the standard.

Driscoll, Kevin R.↗

NASA NTRS2000

Directionally Solidified NiAl-Based Alloys Studied for Improved Elevated-Temperature Strength and Room-Temperature Fracture Toughness

Efforts are underway to replace superalloys used in the hot sections of gas turbine engines with materials possessing better mechanical and physical properties. Alloys based on the intermetallic NiAl have demonstrated potential; however, they generally suffer from low fracture resistance (toughness) at room temperature and from poor strength at elevated temperatures. Directional solidification of NiAl alloyed with both Cr and Mo has yielded materials with useful toughness and elevated-temperature strength values. The intermetallic alloy NiAl has been proposed as an advanced material to extend the maximum operational temperature of gas turbine engines by several hundred degrees centigrade. This intermetallic alloy displays a lower density (approximately 30-percent less) and a higher thermal conductivity (4 to 8 times greater) than conventional superalloys as well as good high-temperature oxidation resistance. Unfortunately, unalloyed NiAl has poor elevated temperature strength (approximately 50 MPa at 1027 C) and low room-temperature fracture toughness (about 5 MPa). Directionally solidified NiAl eutectic alloys are known to possess a combination of high elevated-temperature strength and good room-temperature fracture toughness. Research has demonstrated that a NiAl matrix containing a uniform distribution of very thin Cr plates alloyed with Mo possessed both increased fracture toughness and elevated-temperature creep strength. Although attractive properties were obtained, these alloys were formed at low growth rates (greater than 19 mm/hr), which are considered to be economically unviable. Hence, an investigation was warranted of the strength and toughness behavior of NiAl-(Cr,Mo) directionally solidified at faster growth rates. If the mechanical properties did not deteriorate with increased growth rates, directional solidification could offer an economical means to produce NiAl-based alloys commercially for gas turbine engines. An investigation at the NASA Glenn Research Center at Lewis Field was undertaken to study the effect of the directional solidification growth rate on the microstructure, room temperature fracture toughness, and strength at 1027 C of a Ni-33Al-31Cr-3Mo eutectic alloy. The directionally solidified rates varied between 7.6 and 508 millimeters per hour Essentially fault-free, alternating (Cr, Mo)/NiAl lamellar plate microstructures (left photograph) were formed during growth at and below 12.7 mm/hr, whereas cellular microstructures (right photograph) with the (Cr, Mo) phase in a radial spokelike pattern were developed at faster growth rates. The compressive strength at 1027 C continuously increased with increasing growth rate and did not indicate a maxima as was reported for directionally solidified Ni-33Al-34Cr. Surprisingly, samples with the lamellar plate microstructure (left photograph) possessed a room-temperature fracture toughness of approximately 12 MPa(sup square root of m), whereas all the alloys with a cellular microstructure had a toughness of about 17 MPa(sup square root of m). These results are significant since they clearly demonstrate that Ni-33Al-31Cr-3Mo can be directionally solidified at much faster growth rates without any observable deterioration in its mechanical properties. Thus, the potential to produce strong, tough NiAl-based eutectics at commercially acceptable growth rates exists. Additional testing and alloy optimization studies are underway.

Whittenberger, J. Daniel↗

NASA NTRS2021

Assuring Intelligent Systems: Contingency Management for UAS

Unmanned aircraft systems (UAS) collaborate with humans to operate in diverse, safety-critical applications. However, assurance technologies need to be integrated into the design process in order to guarantee safe behavior, thereby enabling UAS operations in the National Airspace System (NAS). In this paper, formal methods are integrated with learning-enabled systems representations. The generation and representation of knowledge are captured via monadic second-order logic rules in the cognitive architecture Soar. These rules are translated into timed automata, and a proof of correctness for the translation is provided so that safety and liveness properties can be checked in the formal verification environment Uppaal. This approach is agnostic to the learning mechanism used to generate the learned rules (e.g., chunking, etc.). An example of a fault-tolerant, learning-enabled UAS deciding which of four contingency procedures to execute under a lost link scenario while overflying an urban area is used to illustrate the approach.

Intelligent Systems↗

DOE OSTI2017

Field-assisted sintering and phase transition of ZnS-CaLa 2 S 4 composite ceramics

In the present study, zinc sulfide (ZnS) and calcium lanthanum sulfide (CaLa 2 S 4 , CLS) composite ceramics were consolidated via field-assisted sintering of 0.5ZnS-0.5CLS (volume ratio) composite powders at 800–1050 °C. Through sintering curve analyses and microstructural observations, it was determined that between 800 and 1000 °C, grain boundary diffusion was the main mechanism controlling grain growth for both the ZnS and CLS phases within the composite ceramics. The consolidated composite ceramics were determined to be composed of sphalerite ZnS, wurtzite ZnS and thorium phosphate CLS. The sphalerite-wurtzite phase transition of ZnS was further demonstrated to be accompanied by the formation of stacking faults and twins in the ceramics. Furthermore, it was also found that the addition of the CLS phase improved the indentation hardness of the ceramics relative to pure ZnS by homogeneous dispersion of ZnS and CLS small grains.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

DOE OSTI2024

Compositional effect on pressure-induced polymorphism in high-entropy alloys

Recently, pressure-induced polymorphic phase transitions were discovered in several fragmented high-entropy alloys (HEAs), offering a valuable opportunity to deepen our understanding of these materials. However, the chemical and physical factors that govern these transitions are still unclear. Here, in this work, we combined in situ high-pressure synchrotron X-ray diffraction, X-ray emission spectroscopy (XES), and high-resolution transmission electron microscopy (HRTEM) to systematically study the evolution of the atomic and electronic structures in the Cantor alloy and its face-centered-cubic ( fcc ) subset alloys (CoCrFeMnNi, CoCrFeNi, CoCrMnNi, CoFeMnNi, CoCrNi, CoFeNi, CoMnNi, CrFeNi, and FeMnNi). Surprisingly, diverse behavior was observed among these closely related alloys during compression and decompression, which includes irreversible, reversible fcc to hexagonal close-packed (hcp) phase transitions, or even no detectable phase transitions up to ∼40 GPa. HRTEM measurements confirmed that the fcc and hcp phases abided by the classic Shoji-Nishiyama orientation relationship during the transitions. XES data indicated that high-pressure suppresses the local magnetic moments in all the studied alloys, suggesting that magnetic states do not significantly influence the polymorphic transitions. By comparing the effects of the atomic size difference, entropy, valence electron concentration, and stacking fault energy across all the compositions studied, only the stacking fault energy shows a strong correlation with the phase transitions, indicating it plays a key role in inducing polymorphism in HEAs.

36 MATERIALS SCIENCE↗

NASA NTRS1991

Strain accommodation beneath structures on Mars

A recent review of tectonic features on Mars shows that most of their subsurface structures can be confidently extended only a few kilometers deep (exceptions are rifts, in which bounding normal faults penetrate the entire brittle lithosphere, with ductile flow at deeper levels). Nevertheless, a variety of estimates of elastic lithosphere thickness and application of accepted failure criteria under likely conditions on Mars suggest a brittle lithosphere that is many tens of kilometers thick. This raises the question of how the strain (extension or shortening) accommodated by grabens and wrinkle ridges within the upper few kilometers is being accommodated at deeper levels in the lithosphere. Herein, the nonrift tectonic features present on Mars are briefly reviewed, along with their likely subsurface structures, and some inferences and implications are presented for behavior of the deeper lithosphere.

Golombek, M. P.↗

DOE OSTI2017

INDUCED MICROEARTHQUAKES AND SEISMICITY-PERMEABILITY RELATIONSHIPS IN FRACTURES

In the past several years, induced microearthquakes (MEQs) related to energy development projects have garnered public attention. Large-scale fluid injection in geoengineering activities, such as enhanced geothermal reservoir stimulation, geological storage of CO2, shale reservoir stimulation, and deep disposal of wastewater can generate significant fluid overpressures and induce microearthquakes by reactivating preexisting faults and fractures that are widely distributed throughout the upper crust. The monitoring of fluid-injection-induced microearthquakes can provide significant information (e.g., timing, special distribution, and moment magnitude) in evaluating reservoir development (e.g., fracture distribution and reservoir hydraulic conductivity evolution), in informing production strategies (e.g., accommodation of production wells), and in assessing the risks of fluid injection activities (e.g., caprock integrity of CO2 reservoir). The following questions are addressed in this study: (1) what are the mechanisms and implications of in-situ feedbacks (e.g., monitored fluid-injection-induced MEQs distribution, seismic moment magnitudes, and fracture behaviors) in geothermal stimulation? (2) What information can be derived from MEQs to inform geothermal reservoir stimulation strategies? (3) Are there any potential relationships between induced seismic or aseismic slip and permeability evolution of fractures in such unconventional reservoirs and caprocks? (4) What factors play an important role in controlling these relationships? These questions are addressed in the five individual chapters of this thesis.

58 GEOSCIENCES↗