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DOE OSTI2025

Experimental determination of the magnetic anisotropy in five-coordinated Co( II ) field-induced single molecule magnets

Magnetic anisotropy of the central metal atom is a crucial property of single molecule magnets (SMMs). Small structural changes can alter the magnetic properties, and accurate experimental methods to investigate magnetic anisotropy are therefore critical. Here, we investigate two five-coordinated Co( II ) SMMs, [CoCl 2 Cltpy] (1) and [CoBr 2 Cltpy] (2) (Cltpy = 4′-chloro-2,2′:6′,2′′-terpyridine), through multiple techniques. Ab initio theoretical calculations performed on the two compounds show that both possess axial magnetic anisotropy with the magnetic easy axis pointing towards one of the terminal halogen atoms. Theoretical calculations on SMMs are typically done on isolated molecular species, and to validate this approximation the magnetic anisotropy was further studied through experimental techniques. EPR measurements confirm an axial anisotropy of 1, and magnetic measurements provide experimental Zero-Field Splitting (ZFS) parameters, showing that the values from theoretical calculations are slightly overestimated. The X-ray electron density determined from 20 K single-crystal synchrotron X-ray diffraction data provides estimated d-orbital populations also suggesting axial magnetic anisotropy in both systems, and furthermore suggesting a more pronounced axiality in 1 compared to 2. This is in good agreement with the results obtained from both magnetic measurements and theoretical calculations. The magnetic anisotropy of 1 is quantified experimentally through polarized powder neutron diffraction via the site susceptibility method, confirming an axial magnetic anisotropy of the compound. A slight deviation in the easy axis direction is observed between experimental and theoretical results. This, together with the overestimation of the ZFS parameters from theoretical calculations, shows that experimental investigation of the magnetic anisotropy of SMMs is of high relevance. Magnetic anisotropy of the central metal atom is a crucial property of single molecule magnets (SMMs).

Slavensky, Hannah H. [Aarhus Univ. (Denmark)] (ORC↗

DOE OSTI2024

Innovative approaches to neutron beam optimization: A case study of FP14 at LANSCE

This paper describes an experimental method to acquire high resolution energy- and spatially- resolved neutron beam spots using the time-gated neutron imaging system with Teledyne Pi-MAX4 camera. These experimental data offer a unique opportunity for benchmarking beam spot simulations. High-quality simulations depend significantly on a high-fidelity geometry model, which can be challenging for legacy facilities. We informed our MCNPX geometry model by latest metrology survey employing Leica laser tracker ATS600. It gave us a high fidelity description of our facility geometry. Such a robust integration of novel tools and methods yields a previously unattainable level of accuracy in both predicting and capturing neutron beam spots, marking a notable advancement over traditional methods reliant on static image plates. Here, to demonstrate the practical application of these tools, we are showing a non-uniform beam spot challenge at our Flight Path 14 (FP14) at the Los Alamos Neutron Science Center (LANSCE). Our precise MCNPX prediction of beam spot shifting as function of neutron energy was confirmed by experimental beam spot measured with extremely high level of detail. Results of this research demonstrate a significant leap in neutron beam optimization at LANSCE and set a new benchmark in beam spot characterization. The advanced methods presented here have potential for adoption at similar research facilities worldwide, aiming at substantial improvement in neutron beam delivery for experiments.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

DOE OSTI2016

Magnetically insulated coaxial vacuum diode with partial space-charge-limited explosive emission from edge-type cathode

The vacuum current associated with any type of electron emission for arbitrary configuration of the diode depends on the combination of the applied electric field and vacuum space charge (VSC) field created by the current. Such fundamental statement should give very close links between the diode current and the normalized cathode field θ which has been introduced by Forbes in 2008 for planar diodes as a reduction in the cathode surface field: θ = field-with/field-without VSC. This article reports the universal approximation of the type of cos(πθ/2) that is the ratio of the actual current and the fully space-charge-limited current. Also, the theoretical treatment and the experimental method of determination of the dynamic emissive characteristics of the macroscopic explosive emission from edge-type cathodes in the coaxial diode are developed. The experimental results obtained with a picosecond time reference between the cathode voltage and the onset of the high-current electron beam exhibit a good coincidence with the theoretical predictions. The presented methods enable the analysis of a real-time-resolved dynamics associated with the dense, magnetized electron beam formation, acceleration and drift motion, including kinematic effects and the phase-stable excitation of high-power microwave oscillators.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

DOE OSTI2025

Theoretical and experimental quantification of Suzuki segregation enthalpy and strengthening mechanisms in a binary alloy

Solute segregation to planar defects in metallic alloys has been shown to drastically alter mechanical properties. While various works using first-principles and thermodynamic calculations have studied the fundamental driving forces for solute segregation via the Suzuki criterion, planar defect energy, or a comparison of energies of the HCP-like phase and FCC matrix, a quantitative experimental and computational comparison of equilibrium composition and segregation enthalpies has not yet been reported. In this work, we predict the equilibrium composition and segregation enthalpy to intrinsic stacking faults in a Ni-60Co (at.%) alloy and compare the results to two independent experimental methods. We observed that Co segregates to the innermost two planes of the intrinsic stacking fault, and we found that the experimental segregation enrichment, measured from transmission electron microscopy energy dispersive X-ray spectroscopy, of the faults is 6.8 at.% Co, which is 2.2 at.% less than the predicted value at the same temperature. We also find that the segregation enthalpy measured from the composition profile is −21.1 ± 6.4 meV/atom and separately from differential scanning calorimetry segregation enthalpy is −33.2 meV/atom, whereas the predicted enthalpy is −31 ± 1 meV/atom. Based on these results, we determine that segregation occurs very rapidly, within 8 min at temperatures as low as 36% of the homologous solidus temperature. Furthermore, this analysis provides an overview of the possible dislocation mechanisms responsible for strengthening effects due to solute segregation, and concludes that changes in room temperature hardness from local phase transformation is likely tied to post-segregation room temperature equilibrium partial separation distance.

Ab initio calculation↗

DOE OSTI2024

Exploring Quantum Materials with Resonant Inelastic X-Ray Scattering

Understanding quantum materials—solids in which interactions among constituent electrons yield a great variety of novel emergent quantum phenomena—is a forefront challenge in modern condensed matter physics. This goal has driven the invention and refinement of several experimental methods, which can spectroscopically determine the elementary excitations and correlation functions that determine material properties. Here we focus on the future experimental and theoretical trends of resonant inelastic x-ray scattering (RIXS), which is a remarkably versatile and rapidly growing technique for probing different charge, lattice, spin, and orbital excitations in quantum materials. We provide a forward-looking introduction to RIXS and outline how this technique is poised to deepen our insight into the nature of quantum materials and of their emergent electronic phenomena. Published by the American Physical Society 2024

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2021

Development of Standardized Property Requirements, Measurement Methods, and Reporting Guidance for Coatings

The diverse research programs presently in progress around the world have advanced a large number of coated cladding concepts to various stages of maturity. Industry teams have developed leading coating compositions and geometries, but significant disparity exists in the importance placed on different coating properties, as well as the applicability and standardization of the various methods used to measure these properties. This milestone report provides an initial assessment of the most important coating properties and the experimental methods available for their determination to lay the foundation for standardized reporting and development of comprehensive datasets for modeling efforts. This report has determined that the residual stress of the coating is the most crucial property to investigate, yet it has received minimal attention to date due to a knowledge gap about the growth and formation of the brittle Laves phase under reactor conditions. The significance of residual stress of the coating is further enhanced by its connection and interdependence with other important properties like creep and coating failure mechanisms. This milestone proposes an importance rating for residual stress properties and their associated measurement techniques to fill in knowledge. Furthermore, techniques to investigate the outlined properties are discussed, and their capabilities and limitations are illustrated to provide guidance on their use.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

DOE OSTI2021

Experimental Studies of the Dynamics of Adsorbed and Condensed Phase Iodine Species Formed in Severe Reactor Accidents (Final Project Report)

We have studied the chemical transformations of semi-volatile organic iodide species (RI) in the condensed phase as well as adsorbed onto the surfaces of environmentally relevant particles, e.g., soot (carbon) and dust (silica) under real-world conditions. The combination of chosen experimental methods provide a molecular-level insight into the chemical dynamics of organic iodides. Throughout this project, we have developed new experimental, quantum chemistry, and data analysis capabilities. All experimental work was performed with 127 I.

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗

DOE OSTI2024

Decarbonizing nitrogen fertilizer production via the electrochemical nitrogen oxidation reaction

Nitric acid is an important commodity chemical with extensive applications in both agricultural and industrial sectors. However, current production methods involve a combination of the Haber–Bosch and Ostwald processes, which are both energy and carbon emission intensive. The electrochemical nitrogen oxidation reaction (NOR) to produce nitric acid or nitrates shows great potential as an environmentally friendly method for producing fertilizers under mild conditions. The key to progress in this field lies in understanding the fundamental mechanistic insights and establishing robust experimental methods, which is essential for the efficient design and synthesis of electrocatalysts for NOR. Additionally, poor gas mass transport in conventional electrochemical reactors at present lead to lower NOR activity, thereby limiting the progress in this field. In this work, we present a synergistic computational and experimental approach to map out the potential chemical and electrochemical steps and determine the energetics on PtO 2 catalyst to gain mechanistic insights into NOR. Here, this study marks the first attempt to perform NOR in a vapor-fed reactor designed using advanced (additive) manufacturing. The vapor-fed reactor significantly improved the N 2 mass transport to the catalyst, allowing us to report the highest rate for nitrate production to date at 3.3 μmol cm -2 h -1 at 2.01 V vs RHE.

30 DIRECT ENERGY CONVERSION↗

DOE OSTI2025

An Investigation of Thermal Properties of 2D Materials [Dissertation]

Studying the thermal conductivity of 2D materials is important due to the applications of 2D materials in fields such as thermal management, thermoelectricity, renewable energy, and sensors. As such, measurements of the thermal conductivity of these 2D materials become important to measure. Thermal conductivity is often difficult to measure for 2D materials due to their atomically thin nature and many experimental methods for doing so requiring contact with the sample, which can alter the thermal properties. A non-contact method for calculating the thermal conductivity of 2D materials supported on substrates in order to model the thermal conductivity of 2D materials for devices, is proposed and experimentally performed in this dissertation. The optothermal Raman technique is a useful non-contact diagnostic technique useful in determining the thermal conductivity of 2D materials. The optothermal Raman typically does not account for heat losses due to convection or radiation or substrate resistance, which are shown to be important factors to consider when developing an optothermal Raman model. Additionally, the calculation of the interfacial thermal conductance between the bottom surface of the sample and the top surface of the substrate, plays an important role in determining the final value of the thermal conductivity of a supported sample, and will yield differing results based on whether or not the conductance is calculated using an approach such as the Diffuse Mismatch Model (DMM) or calculated directly by varying the laser heating profile (usually done by changing the laser objective). This is shown to be the case for both graphene on Ni, graphene on Cu, and SnSe 2 on Cu. In addition to experimentally calculating the thermal conductivity of a 2D material with the optothermal Raman technique, the thermal conductivity of 2D materials can also be calculated using computational methods. The three-phonon method is a method which can be used to simulate phonon scattering processes and determine the thermal conductivity of semiconductors, wherein phonon scattering is the dominant mechanism which determines the thermal conductivity. The three-phonon method uses relaxation times for phonon scattering with other phonons, electrons, and other material system elements, such as isotopes or material defects, in order to create a single-mode relaxation time approximation (SMRTA), which is used to calculate the final value of the thermal conductivity. An important consideration when determining the thermal conductivity of a 2D material using this method is the device geometry, which is reflected in this work as the phonon-boundary scattering relaxation time. This inclusion is important along with the inclusion of phonon-electron scattering in accurately determining the thermal conductivity of a 2D material. In both the optothermal Raman experiments and the three-phonon method computations, strain is shown to have a demonstrable effect on the thermal conductivity of 2D materials. When a 1.1% strain was applied to the mechanical properties of SnSe, the three-phonon processes yielded a lower thermal conductivity than the no-strain case. For the optothermal Raman experiments, the strain induced in the Cu substrate and transferred to a single-layer graphene (SLG) sample yields a trend where the thermal conductivity of the SLG decreases with respect to strain applied. In the case where the interfacial thermal conductance was calculated directly, the conductance increased with respect to strain applied. This presents strain as a reliable and viable method for tuning the thermal properties of 2D materials for device applications.

36 MATERIALS SCIENCE↗

DOE OSTI2011

Measurement of the photobleaching kinetics of semiconducting polymer films by the pump - probe method

A phenomenological model of the laser photobleaching dynamics of a semiconducting polymer in a dual-beam scheme for different wavelengths of the burning and probe beams is developed. An experimental method is implemented based on this model, which allows one to investigate materials with significantly different photodegradation rates. The photodegradation quantum yield in mixtures of a semiconducting polymer belonging to polyparaphenylene vinylenes (MEH-PPV) with a low-molecular electron acceptor 2,4,7-trinitrofluorenone (TNF) is measured at burning wavelengths of 488 and 514 nm for different component ratios of MEHPPV : TNF. It is found that adding the acceptor decreases the polymer photodegradation quantum yield by at least four orders of magnitude in the MEH-PPV : TNF = 1 : 0.4 mixture; the photodegradation quantum yields are the same at both wavelengths. It is shown that the photodegradation rates of the MEH-PPV : TNF films measured by laser photobleaching and IR spectroscopy are in good agreement.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

DOE OSTI2026

Experimental Quantification of Spin–Phonon Coupling in Molecular Qubits Using Inelastic Neutron Scattering

Electronic spin superposition states enable nanoscale sensing through their sensitivity to the local environment, yet their sensitivity to vibrational motion also limits their coherence times. In molecular spin systems, chemical tunability and atomicscale resolution are accompanied by a dense, thermally accessible phonon spectrum that introduces efficient spin relaxation pathways. Despite extensive theoretical work, there is little experimental consensus on which vibrational energies dominate spin relaxation or how molecular structure controls spin−phonon coupling (SPC). We present a fully experimental method to quantify SPC coefficients by combining temperature-dependent vibrational spectra from inelastic neutron scattering with spin relaxation rates measured by electron paramagnetic resonance. We apply this framework to two model S = 1/2 systems, copper(II) phthalocyanine (CuPc) and copper(II) octaethylporphyrin (CuOEP). Two distinct relaxation regimes emerge: below 40 K, weakly coupled lattice modes below 50 cm −1 dominate, whereas above 40 K, optical phonons above ∼185 cm −1 become thermally populated and drive relaxation with SPC coefficients nearly 3 orders of magnitude larger. Structural distortions in CuOEP that break planar symmetry soften the crystal lattice and enhance anharmonic scattering but also raise the energy of stretching modes at the molecular core where the spins reside. This redistributes vibrational energy toward the molecular periphery and out of plane, ultimately reducing SPC relative to CuPc and enabling room-temperature spin coherence in CuOEP. Although our method does not provide mode-specific SPC coefficients, it quantifies contributions from distinct spectral regions and establishes a broadly applicable, fully experimental link between crystal structure, lattice dynamics, and spin relaxation.

Lohaus, Stefan H. [California Institute of Technol↗

DOE OSTI2014

Geoelectrical Measurement of Multi-Scale Mass Transfer Parameters

Mass transfer affects contaminant transport and is thought to control the efficiency of aquifer remediation at a number of sites within the Department of Energy (DOE) complex. An improved understanding of mass transfer is critical to meeting the enormous scientific and engineering challenges currently facing DOE. Informed design of site remedies and long-term stewardship of radionuclide-contaminated sites will require new cost-effective laboratory and field techniques to measure the parameters controlling mass transfer spatially and across a range of scales. In this project, we sought to capitalize on the geophysical signatures of mass transfer. Previous numerical modeling and pilot-scale field experiments suggested that mass transfer produces a geoelectrical signature—a hysteretic relation between sampled (mobile-domain) fluid conductivity and bulk (mobile + immobile) conductivity—over a range of scales relevant to aquifer remediation. In this work, we investigated the geoelectrical signature of mass transfer during tracer transport in a series of controlled experiments to determine the operation of controlling parameters, and also investigated the use of complex-resistivity (CR) as a means of quantifying mass transfer parameters in situ without tracer experiments. In an add-on component to our grant, we additionally considered nuclear magnetic resonance (NMR) to help parse mobile from immobile porosities. Including the NMR component, our revised study objectives were to: 1. Develop and demonstrate geophysical approaches to measure mass-transfer parameters spatially and over a range of scales, including the combination of electrical resistivity monitoring, tracer tests, complex resistivity, nuclear magnetic resonance, and materials characterization; and 2. Provide mass-transfer estimates for improved understanding of contaminant fate and transport at DOE sites, such as uranium transport at the Hanford 300 Area. To achieve our objectives, we implemented a 3-part research plan involving (1) development of computer codes and techniques to estimate mass-transfer parameters from time-lapse electrical data; (2) bench-scale experiments on synthetic materials and materials from cores from the Hanford 300 Area; and (3) field demonstration experiments at the DOE’s Hanford 300 Area. In a synergistic add-on to our workplan, we analyzed data from field experiments performed at the DOE Naturita Site under a separate DOE SBR grant, on which PI Day-Lewis served as co-PI. Techniques developed for application to Hanford datasets also were applied to data from Naturita. 1. Introduction The Department of Energy (DOE) faces enormous scientific and engineering challenges associated with the remediation of legacy contamination at former nuclear weapons production facilities. Selection, design and optimization of appropriate site remedies (e.g., pump-and-treat, biostimulation, or monitored natural attenuation) requires reliable predictive models of radionuclide fate and transport; however, our current modeling capabilities are limited by an incomplete understanding of multi-scale mass transfer—its rates, scales, and the heterogeneity of controlling parameters. At many DOE sites, long “tailing” behavior, concentration rebound, and slower-than-expected cleanup are observed; these observations are all consistent with multi-scale mass transfer [Haggerty and Gorelick, 1995; Haggerty et al., 2000; 2004], which renders pump-and-treat remediation and biotransformation inefficient and slow [Haggerty and Gorelick, 1994; Harvey et al., 1994; Wilson, 1997]. Despite the importance of mass transfer, there are significant uncertainties associated with controlling parameters, and the prevalence of mass transfer remains a point of debate [e.g., Hill et al., 2006; Molz et al., 2006] for lack of experimental methods to verify and measure it in situ or independently of tracer breakthrough. There is a critical need for new field-experimental techniques to measure mass transfer in-situ and estimate multi-scale and spatially variable mass-transfer parameters. The current lack of such techniques results in large parameter uncertainty, which in turn translates into enormous prediction uncertainty and cost to DOE. In this project, we considered three hydrogeophysical approaches for providing information about mass-transfer parameters: (1) the combination of electrical-resistivity tomography (ERT) and ionic tracer experiments to explore rates of exchange and relative mobile and immobile porosities; (2) complex resistivity (CR) measurements to infer the distribution of diffusive length scales active in a porous medium; and (3) nuclear magnetic resonance (NMR) to estimate mobile and immobile porosity.

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗

DOE OSTI2019

Validation of RELAP-7 for Forced Convective and Natural Circulation Reactor Flows

New reactor designs such as small modular reactors and newly proposed passive safety systems rely on natural circulation two-phase flow cooling of the reactor core under accident conditions. Without a pump to drive the flow, the circulation rate is a strong function of void fraction. Under these conditions where the flow rate, pressure drop, and heat transfer are all closely coupled through the mixture density, the accurate prediction of void fraction is pivotal. Furthermore, while these passive systems boast a more reliable cooling option, the sensitivity of the system to two-phase flow instabilities is more likely than in forced convective cooling and can result in dangerous density wave or flow excursion conditions. Improvement of one-dimensional system codes and further development of three-dimensional code capability are all important efforts in addressing these issues. The proposed work is a critical step towards providing confidence through validation of the capability of thermal-hydraulic tools to meet the emerging challenges in reactor simulation. Historically, system analysis codes develop a stiffness over time due to fine-tuning of adjustable code parameters that result in a reluctance or inability to adopt improved models. Therefore, a rigorous effort should be invested in preparation for RELAP-7 to identify required modeling improvements of constitutive relations and validation of the code applicability to the wide range of possible reactor flow conditions. Part of this validation involves the uncertainty quantification which is a critical step in the Code Scaling, Applicability, and Uncertainty (CSAU) methodology and Best-Estimate Plus Uncertainty (BEPU) licensing method. BEPU allows recovery of safety margins and potentially optimizing plant performance, resulting in economic benefit for the reactor operators. Beginning with the collection of past experimental data covering prototypic LWR conditions, this document reviews three critical datasets available for the validation of system codes. The experimental methods, procedures, facilities, instrumentation, and supplementary information are consolidated to aid the validation efforts of this work and future projects. These three datasets (824 conditions) are chosen due to their wide acceptance and demonstrated application for code validation. Two experimental datasets from the Nuclear Power Engineering Corporation (NUPEC) span prototypic conditions of Boiling Water Reactors (BWR) and Pressurized Water Reactors (PWR). These datasets are labeled as the BFBT (BWR Full-size Fine-mesh Bundle Test) and the PSBT (PWR Subchannel and Bundle Test) datasets respectively. The third dataset is taken in an internally heated annulus that is scaled based on a BWR subassembly and includes two-phase flows important to post-blowdown analysis. Together, the datasets consider the full range of pressure and mass flux expected in LWR forced convective flows from steady-state to long term cooling conditions. Recognizing the deficiency of available data under low-pressure, low-flow, a new natural circulation dataset consisting of 107 conditions is obtained. With system pressures ranging between 145 and 950 kPa, natural circulation is driven by a heat flux up to 275 kW/m2 in a 3 m long heated region of the annulus test section which is followed by a 2 m long unheated region before entering a condenser. Stable natural circulation flow rates in this facility were measured to be between 182 and 590 kg/m2-s. Pressure and temperature are measured at ten locations in the facility. In addition, measurements of void fraction, interfacial area concentration, and gas velocity are obtained at five axial locations in the annulus test section. The RELAP5-3D code demonstrates good accuracy for void fraction predictions in BFBT and PSBT benchmarks, but shows relatively large discrepancy in the annulus experiments at lower pressures. In two-phase natural circulation, large oscillations are observed in many system parameters during the simulation of 19 experiment cases which were conducted at low pressures, and the model shows good predictive performance with the remaining 88 experiment cases. However, some discrepancies in void fraction and temperature predictions are found which may require improved constitutive modeling under these low-pressure, low-flow condition. The quantified uncertainty in void fraction predictions in three forced convection benchmarks due to uncertainties in boundary conditions and geometries are relatively small, except for a few cases in the annulus experiment. The output uncertainty of the natural circulation model is quantified by considering the measurement error in boundary conditions, and it is shown that the output uncertainty ranges are relatively small for the range of conditions considered. Through this work, a clear pathway is provided for validation of RELAP7 once the code is available.

42 ENGINEERING↗

DOE OSTI2023

An Effective Current Balancing Method for Inverters With Paralleled Silicon Carbide Power Modules

Silicon carbide (SiC) MOSFET has many superior characteristics in high power applications. Paralleling the SiC devices is an effective approach to increase the current capacity of the system, which also leads to current sharing issues. In this article, both transient and steady-state current sharing issues are studied for the high-power grid-tied inverters with paralleled SiC modules with an effective current balancing strategy proposed to address both issues simultaneously. The steady-state imbalance current due to the parameter mismatch is suppressed by the self-inductance of power cables used for paralleling connection. With the elimination of steady-state imbalance current, the transient imbalance current sensing is much simplified and can be realized by using low-cost current sensors. With the sensed imbalance current, a closed-loop control approach is proposed to adjust the modulation reference signal for each module to mitigate the remaining transient imbalance current. Furthermore, the proposed method is straightforward to implement with enhanced compatibility and flexibility compared to existing methods. Experimental studies are performed using inverters with 2 and 4 power modules paralleled in each phase to demonstrate the effectiveness of the proposed method.

42 ENGINEERING↗

DOE OSTI2017

An experimental topographic amplification study at Los Alamos National Laboratory using ambient vibrations

An experimental study aimed at investigating potential topographic amplification of seismic waves was conducted on a 50-m-tall and 185-m-wide soft-rock ridge located at Los Alamos National Laboratory near Los Alamos, New Mexico. Ten portable broadband seismograph stations were placed in arrays across the ridge and left to record ambient vibration data for ~9 hours. Clear evidence of topographic amplification was observed by comparing spectral ratios calculated from ambient noise recordings at the toe, slope, and crest of the instrumented ridge. The inferred resonance frequency of the ridge obtained from the experimental recordings was found to agree well with several simple estimates of the theoretical resonance frequency based on its geometry and stiffness. Results support the feasibility of quantifying the frequency range of topographic amplification solely using ambient vibrations, rather than strong or weak ground motions. Additionally, comparisons have been made between a number of widely used experimental methods for quantifying topographic effects, such as the standard spectral ratio, median reference method, and horizontal-to-vertical spectral ratio. As a result, differences in the amplification and frequency range of topographic effects indicated by these methods highlight the importance of choosing a reference condition that is appropriate for the site-specific conditions and goals associated with an experimental topographic amplification study.

58 GEOSCIENCES↗

DOE OSTI2022

Intact, Commercial Lithium-Polymer Batteries: Spatially Resolved Grating-Based Interferometry Imaging, Bragg Edge Imaging, and Neutron Diffraction

We survey several neutron imaging and diffraction methods for non-destructive testing and evaluation of intact, commercial lithium-ion batteries. Specifically, far-field interferometry was explored as an option to probe a wide range of autocorrelation lengths within the batteries via neutron imaging. The dark-field interferometry images change remarkably from fresh to worn batteries, and from charged to discharged batteries. When attempting to search for visual evidence of battery degradation, neutron Talbot-Lau grating interferometry exposed battery layering and particle scattering through dark-field imaging. Bragg edge imaging also reveals battery wear and state of charge. Neutron diffraction observed chemical changes between fresh and worn, charged and discharged batteries. However, the utility of these methods, for commercial batteries, is dependent upon battery size and shape, with 19 to 43 mAh prismatic batteries proving most convenient for these experimental methods. This study reports some of the first spatially resolved, small angle scattering (dark-field) images showing battery degradation.

36 MATERIALS SCIENCE↗

DOE OSTI2019

Comparing wall performance predicted from hygrothermal simulations to wall performance measured from environmental chamber experiments

To effectively mitigate prevailing perceptions of potential moisture risks in high-R wall assemblies, a comprehensive moisture durability assessment that incorporates BA team field evaluations, lab tests and simulations has been completed over the last couple years. In FY18, three stick-built walls were succumbed to typical Chicago weather in ORNL’s Heat, Air and Moisture chamber. The measured temperature, relative humidity and moisture content within these walls were compared to WUFI hygrothermal simulation results. In FY19, similar experiments and comparison to WUFI results were completed with two walls, a Structural Insulated Panel (SIP) based wall and a Concrete Masonry Unit (CMU) based wall. The following tasks were completed for these two walls: 1. Measure air permeance of each individual wall using ASTM E283 Standard Test Method. 2.Test walls in diffusion scenario as only moisture transport mechanism and compare measured transient temperature and relative humidity of select wall components to WUFI model results. Chicago summer and weather will be investigated. 3. Test walls in wetting event scenario and compare measured transient temperature and relative humidity of select wall components with Chicago summer weather to WUFI model results. 4. Test walls in diffusion/advection scenario. In addition to controlling outdoor chamber to match real outdoor weather, a pressure differential across the wall will be varied. Measured transient temperature and relative humidity of select wall components will be compared to WUFI model results. 5. Test walls in diffusion/advection with solar heating of cladding. In addition to the variables above, IR lamps will be used to heat the cladding on a diurnal cycle. Measured transient OSB MC and temperature will be compared to WUFI model results. This report documents the experimental method, results and comparison of the measured experimental hygrothermal performance of the two walls to simulations results.

42 ENGINEERING↗

DOE OSTI2021

Recent advances in the mechanical characterization of shales at nano-to micro-scales: A review

Understanding geomechanical properties of shales, such as stiffness properties and fracture toughness, is important in different areas of petroleum industry-related activities. Nanoscale to microscale experiments on shale samples require a much smaller sample compared to macroscale experiments. This is a major advantage because irregularly-shaped drill cuttings from shales can be used for experimental analyses, such as nanoindentation or atomic force microscopy (AFM). However, characterization of mechanical properties at the nano- to micro-scale is a relatively new addition to classical geomechanical experiments on shales, and there is still a lack of both fundamental knowledge and standard procedures for conducting experiments at this scale. The theoretical principles of nanoindentation-based (Gridded Nanoindentation and Modulus Mapping) and AFM-based experimental methods (PeakForce QNMTM and AFM-IR), a review of the literature results and the major findings are explained in Sections 2 and 3, respectively. These experimental techniques are compared in Section 4. Overall, nanoindentation experiments reveal the anisotropy of organic matter (OM)-rich shales at the nanoscale, and it is shown that gridded nanoindentation is capable of characterizing different minerals with respect to their stiffness properties. The capability of AFM (PeakForce QNMTM) to differentiate between different minerals within OM-rich shales with distinct mechanical properties, in particular stiffness, is also demonstrated. It is shown that AFM-based methods are more straightforward than gridded-nanoindentation to characterize OM-rich shales based on the stiffness of different constituent minerals of OM-rich shales, but nanoindentation can apply higher loads than AFM-based methods. Therefore, they can measure creep properties and fracture toughness of OM-rich shales. Here, it is shown that the OM is the most compliant part of the OM-rich shales, but it is still unclear if thermal maturation has an impact on the stiffness of OM. It is necessary to investigate if there is a relationship between the OM type (kerogen, bitumen, etc.) and mechanical properties such as Young’s modulus and Creep rate.

36 MATERIALS SCIENCE↗