Comparison of Velocimetry and Reflectometry to Investigate Time of Arrival Diagnostic (TOAD) Probe Function
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TOAD PDV Time of Arrival Diagnostic Photon Doppler↗
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Using Machine Learning to Detect and Locate Rogue Devices from Time-Domain Reflectometry
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Haas, Jason Juedes [Sandia National Laboratories (↗
NASA Hybrid Reflectometer Project
Time-domain and frequency-domain reflectometry have been used for about forty years to locate opens and shorts in cables. Interpretation of reflectometry data is as much art as science. Is there information in the data that is being missed? Can the reflectometers be improved to allow us to detect and locate defects in cables that are not outright shorts or opens? The Hybrid Reflectometer Project was begun this year at NASA Ames Research Center, initially to model wire physics, simulating time-domain reflectometry (TDR) signals in those models and validating the models against actual TDR data taken on testbed cables. Theoretical models of reflectometry in wires will give us an understanding of the merits and limits of these techniques and will guide the application of a proposed hybrid reflectometer with the aim of enhancing reflectometer sensitivity to the point that wire defects can be detected. We will point out efforts by some other researchers to apply wire physics models to the problem of defect detection in wires and we will describe our own initial efforts to create wire physics models and report on testbed validation of the TDR simulations.
Lynch, Dana↗
A SSTDR Methodology, Implementations, and Challenges
Sequence time-domain reflectometry (STDR) and spread spectrum time-domain reflectometry (SSTDR) detect, locate, and diagnose faults in live (energized) electrical systems. In this paper, we survey the present SSTDR literature for discussions on theory, algorithms used in its analysis, and its more prominent implementations and applications. Our review includes both scientific litera-ture and selected patents. We also discuss future applications of SSTDR.
14 SOLAR ENERGY↗
Studying Transient Phenomena in Thin Films with Reinforcement Learning
Neutron reflectometry has long been a powerful tool to study the interfacial properties of energy materials. Recently, time-resolved neutron reflectometry has been used to better understand transient phenomena in electrochemical systems. Those measurements often comprise a large number of reflectivity curves acquired over a narrow q range, with each individual curve having lower information content compared to a typical steady-state measurement. In this work, we present an approach that leverages existing reinforcement learning tools to model time-resolved data to extract the time evolution of structure parameters. Further, by mapping the reflectivity curves taken at different times as individual states, we use the Soft Actor-Critic algorithm to optimize the time series of structure parameters that best represent the evolution of an electrochemical system. We show that this approach constitutes an elegant solution to the modeling of time-resolved neutron reflectometry data.
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
In Situ Measurement of Buried Electrolyte–Electrode Interfaces for Solid State Batteries with Nanometer Level Precision
Many technologies including high-energy solid-state batteries rely on high quality solid–solid interfaces. Solid–solid interfaces are particularly difficult to study as their nature requires the interface to be buried. Here, in this work, we demonstrate the use of a combination of neutron reflectometry and in situ electrochemistry to measure the interface between Li metal and the solid electrolyte LiPON across an 8 cm 2 area. Neutron reflectometry measurements confirm the interphase to be less than 7 nm thick. The neutron reflectometry data further emphasize that the interphase that forms is a chemical gradient consisting of a Li-rich layer that gradually decreases in Li content until it blends into pure LiPON. Experimental confirmation that we can make ideal solid–solid interphases less than 10 nm thick will help facilitate the adoption of high efficiency next generation solid state batteries. Further this combination of complementary techniques provides a more general methodology for studying buried solid–solid interfaces across applications.
25 ENERGY STORAGE↗
Reconstructing the reflectivity of liquid surfaces from grazing incidence X-ray off-specular scattering data
The capillary wave model of a liquid surface predicts both the X-ray specular reflection and the diffuse scattering around it. A quantitative method is presented to obtain the X-ray reflectivity (XRR) from a liquid surface through the diffuse scattering data around the specular reflection measured using a grazing incidence X-ray off-specular scattering (GIXOS) geometry at a fixed horizontal offset angle with respect to the plane of incidence. With this approach the entire Q z -dependent reflectivity profile can be obtained at a single, fixed incident angle. This permits a much faster acquisition of the profile than with conventional reflectometry, where the incident angle must be scanned point by point to obtain a Q z -dependent profile. The XRR derived from the GIXOS-measured diffuse scattering, referred to in this paper as pseudo-reflectivity, provides a larger Q z range compared with the reflectivity measured by conventional reflectometry. Transforming the GIXOS-measured diffuse scattering profile to pseudo-XRR opens up the GIXOS method to widely available specular XRR analysis software tools. Here the GIXOS-derived pseudo-XRR is compared with the XRR measured by specular reflectometry from two simple vapor–liquid interfaces at different surface tension, and from a hexadecyltrimethylammonium bromide monolayer on a water surface. For the simple liquids, excellent agreement (beyond 11 orders of magnitude in signal) is found between the two methods, supporting the approach of using GIXOS-measured diffuse scattering to derive reflectivities. Pseudo-XRR obtained at different horizontal offset angles with respect to the plane of incidence yields indistinguishable results, and this supports the robustness of the GIXOS-XRR approach. The pseudo-XRR method can be extended to soft thin films on a liquid surface, and criteria are established for the applicability of the approach.
36 MATERIALS SCIENCE↗
Measuring a Fiber-Optic Delay Line Using a Mode-Locked Laser
The figure schematically depicts a laboratory setup for determining the optical length of a fiber-optic delay line at a precision greater than that obtainable by use of optical time-domain reflectometry or of mechanical measurement of length during the delay-line-winding process. In this setup, the delay line becomes part of the resonant optical cavity that governs the frequency of oscillation of a mode-locked laser. The length can then be determined from frequency-domain measurements, as described below. The laboratory setup is basically an all-fiber ring laser in which the delay line constitutes part of the ring. Another part of the ring - the laser gain medium - is an erbium-doped fiber amplifier pumped by a diode laser at a wavelength of 980 nm. The loop also includes an optical isolator, two polarization controllers, and a polarizing beam splitter. The optical isolator enforces unidirectional lasing. The polarization beam splitter allows light in only one polarization mode to pass through the ring; light in the orthogonal polarization mode is rejected from the ring and utilized as a diagnostic output, which is fed to an optical spectrum analyzer and a photodetector. The photodetector output is fed to a radio-frequency spectrum analyzer and an oscilloscope. The fiber ring laser can generate continuous-wave radiation in non-mode-locked operation or ultrashort optical pulses in mode-locked operation. The mode-locked operation exhibited by this ring is said to be passive in the sense that no electro-optical modulator or other active optical component is used to achieve it. Passive mode locking is achieved by exploiting optical nonlinearity of passive components in such a manner as to obtain ultra-short optical pulses. In this setup, the particular nonlinear optical property exploited to achieve passive mode locking is nonlinear polarization rotation. This or any ring laser can support oscillation in multiple modes as long as sufficient gain is present to overcome losses in the ring. When mode locking is achieved, oscillation occurs in all the modes having the same phase and same polarization. The frequency interval between modes, often denoted the free spectral range (FSR), is given by c/nL, where c is the speed of light in vacuum, n is the effective index of refraction of the fiber, and L is the total length of optical path around the ring. Therefore, the length of the fiber-optic delay line, as part of the length around the ring, can be calculated from the FSRs measured with and without the delay line incorporated into the ring. For this purpose, the FSR measurements are made by use of the optical and radio-frequency spectrum analyzers. In experimentation on a 10-km-long fiber-optic delay line, it was found that this setup made it possible to measure the length to within a fractional error of about 3 10(exp -6), corresponding to a length error of 3 cm. In contrast, measurements by optical time-domain reflectometry and mechanical measurement were found to be much less precise: For optical time-domain reflectometry, the fractional error was found no less than 10(exp -4) (corresponding to a length error of 1 m) and for mechanical measurement, the fractional error was found to be about 10(exp -2) (corresponding to a length error of 100 m).
Tu, Meirong↗
Influence of Grafting Density and the Ionic Environment on the Structure of Zwitterionic Brushes
Zwitterionic polymer brushes possess a high potential for applications as surface coatings, e.g., in antifouling applications. Their complex association behavior due to the coexistence of oppositely charged groups on the same monomeric unit allows for a broad variation of polarity, hydrophilicity, and the antipolyelectrolyte effect with the variation of the surrounding environment. In this study, planar polysulfobetaine brushes were investigated with neutron reflectometry (NR) and neutron spin–echo spectroscopy under grazing incidence (GINSES) to explore the brush structure and its inner dynamics perpendicular to the substrate. In particular, the effects of the substrate–initiator system and ionic strength on the structure were investigated with neutron reflectometry and a swelling by a factor of 3–5 was found in the presence of aqueous NaCl and MgCl 2 solutions compared to the dry state. During the data analysis, the applicability of a model-free evaluation was also demonstrated for the investigated polysulfobetaine brushes. Furthermore, it was found with GINSES that in contrast to neutral brushes, these polysulfobetaine brushes do not show the typical concentration fluctuations in the nanosecond time range when partially swollen with salt-free water.
36 MATERIALS SCIENCE↗
A high temperature cell for investigating interfacial structure on the molecular scale in molten salt/alloy systems
In this work, we describe the design and development of an in situ neutron reflectometry cell for high temperature investigations of structural changes occurring at the interface between inorganic salts, in their molten state up to 800 °C, and corrosion resistant alloys or other surfaces. In the cell, a molten salt is confined by an annular ring of single crystal sapphire constrained between the sample substrate and a sapphire plate using two gold O-rings, enclosing a liquid salt volume of 20 ml, along with a dynamic cell volume to accommodate expansion of the liquid with heating. Further, as a test case for the cell, we report on an in situ neutron reflectometry measurement of the interface between a eutectic salt mixture of MgCl 2 –KCl (32:68 molar ratio) and a single crystal sapphire substrate at 450 °C, resulting in the formation of a 60 Å layer having a scattering length density of 1.72 × 10 –6 Å –2 . While the origin of this layer is uncertain, it is likely to have resulted from the salt reacting with an existing impurity layer on the sapphire substrate.
46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
M-STAR: Magnetism second target advanced reflectometer at the Spallation Neutron Source
M-STAR is a next generation polarized neutron reflectometer with advanced capabilities. A new focusing guide concept is optimized for samples with dimensions down to a millimeter range. A proposed hybrid pulse-skipping chopper will enable experiments at constant geometry at one incident angle in a broad range of wavevector transfer Q up to 0.3 A –1 for specular, off-specular, and GISANS measurements. M-STAR will empower nanoscience and spintronics studies routinely on small samples (~2 × 2 mm 2 ) and of atomic-scale thickness using versatile experimental conditions of magnetic and/or electric fields, light, and temperature applied in situ to novel complex device-like nanosystems with multiple buried interfaces. M-STAR will enable improved grazing incidence diffraction measurements, as a surface-sensitive depth-resolved probe of, e.g., the out-of-plane component of atomic magnetic moments in ferromagnetic, antiferromagnetic, and more complex structures as well as in-plane atomic-scale structures inaccessible with contemporary diffractometry and reflectometry. New horizons will be opened by the development of an option to probe near-surface dynamics with inelastic grazing incidence scattering in the time-of-flight mode. These novel options in combination with ideally matched parameters of the second target station will place M-STAR in the world’s leading position for high resolution polarized reflectometry.
47 OTHER INSTRUMENTATION↗
SSTDR and FDR Detection of Un-Energized and Energized Cable Anomalies Including Thermal Degradation Using Machine Learning
Historically, cables are initially qualified for nuclear power plant use for 40 years. As plants extend their operating license to 60 and 80 years, continued use of these cables must shift to a performance-based approach since it is cost prohibitive to completely replace cables that are likely still capable of performing their design function. A variety of cable tests are available and are commonly applied during outages when the cables can be taken out of service. Frequency domain reflectometry (FDR) is one of these test methods that is being more broadly accepted and used because it not only detects anomalies along the cable with a low-voltage signal that does not stress the cable insulation, but the technique also locates the anomalies. This supports follow-up local inspection and local repair or partial replacement of a damaged cable segment. Currently, FDR testing is only applied to cables that are taken out of service since the test instrument would be damaged by operational voltages. A related technology that has found some acceptance in the aircraft and rail industry is spread spectrum time domain reflectometry (SSTDR). This technology has been implemented with a custom commercial instrument by LiveWire Innovation that is designed to operate on live cables up to 1000 volts and with a bandwidth of 48 MHz. Initial evaluation by the Pacific Northwest National Laboratory (PNNL) of the Live Wire system indicated that a broader bandwidth (BW) SSTDR may be better for many kinds of flaws. This led PNNL to develop an SSTDR laboratory instrument suitable for tests up to 500 MHz bandwidth. Testing on energized cables is also desirable for online monitoring systems so an inductive clamshell coupler was developed that allows energized cables to be tested up to at least 5 kV and likely higher voltage levels. Dielectric spectroscopy and tan delta testing plus various laboratory destructive tests were included in this data acquisition campaign directed to feed a machine learning (ML) study. With these kinds of developments, online energized cable tests may be possible with industrial adoption of such hardware advances but it will be completely impractical to have highly skilled data analysts continually examine these complex signals for indications of damage or compromised conditions. If online testing is to be implemented in new test hardware, it must be accompanied by software that can interpret the signals and alert plant operators of changing or degraded conditions. The thermally aged, shielded cable investigated here was separately treated for ML analysis. Visual analysis of electrical data showed generally increasing peaks where the cable entered and exited the oven. These peaks were not exactly aligned with expected locations, but these differences were attributed to velocity of propagation calibration errors. Only supervised ML was applied to the thermally aged data as this data was only available shortly before the committed publication date of this report. The supervised ML was structured to divide the 0 to 70-day responses as ‘normal’ from 0 to 35 days or ‘anomalous’ from 36 to 70 days, based on cable tensile elongation at break (EAB) insulation characterization. Using 80% of the data for training and 20% for testing, the supervised ML predicted normal versus anomalous was 70% accurate. Important conclusions include: • Accuracy to predict the presence of cable damage is improved from the 2023 effort by more training data. Weighted accuracies for comparisons among the instruments ranged from 67 to 89 % for unsupervised ML and 71 to 99% for supervised ML. • Based on the synthetic data tests, the unsupervised models are more generalizable to unseen anomalies. The Multi-Layer Perceptron classifier (MLP) model reported as high as 99.7% accuracy on the test data, but this dropped to 58.3% when tested on the synthetic data. In contrast, the unsupervised Pointwise model only achieved 89.7% accuracy on the experimental data but reported 78.3% accuracy on the synthetic data. • The best anomaly indicators are higher frequency (400 MHz BW) FDR data. Other tests may be interesting but for this study, this was the best predicter.
46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
Microstructural Underpinnings of Giant Intrinsic Exchange Bias in Epitaxial NiCo 2 O 4 Thin Films
Understanding intrinsic exchange bias in nominally single-component ferromagnetic or ferrimagnetic materials is crucial for simplifying related device architectures. However, the mechanisms behind this phenomenon and its tunability remain elusive, which hinders the efforts to achieve unidirectional magnetization for widespread applications. Inspired by the high tunability of ferrimagnetic inverse spinel NiCo 2 O 4 , the origin of intrinsic exchange bias in NiCo 2 O 4 (111) films deposited on Al 2 O 3 (0001) substrates are investigated. The comprehensive characterizations, including electron diffraction, X-ray reflectometry and spectroscopy, and polarized neutron reflectometry, reveal that intrinsic exchange bias in NiCo 2 O 4 (111)/Al 2 O 3 (0001) arises from a reconstructed antiferromagnetic rock-salt Ni x Co 1-x O layer at the interface between the film and the substrate due to a significant structural mismatch. Remarkably, by engineering the interfacial structure under optimal growth conditions, it can achieve exchange bias larger than coercivity, leading to unidirectional magnetization. Such giant intrinsic exchange bias can be utilized for realistic device applications. This work establishes a new material platform based on NiCo 2 O 4 , an emergent spintronics material, to study tunable interfacial magnetic and spintronic properties.
36 MATERIALS SCIENCE↗
Oxide structure of air-passivated U-6Nb alloy thin films
U-6Nb is a uranium alloy containing 6 wt% niobium that possesses high corrosion resistance. The structure and composition of the passivating oxide layer formed on air-aged U-6Nb, which gives the material its corrosion resistant properties, was characterized using surface scattering techniques. Stable oxide layers formed on the surface of a set of U-6Nb alloy thin films under ambient conditions were investigated using neutron reflectometry (NR), x-ray reflectometry (XRR) and grazing incidence x-ray diffraction (GIXD). The passivating oxide was composed of approximately 27% U, 5% Nb, and 68% O, primarily consisting of a thin niobium oxide layer (5.5 ± 0.4 nm) separating a thicker UO2 layer (27.1 ± 2.3 nm) from the underlying U-6Nb alloy. A critical density of enriched niobium oxide at the metal-oxide interface is hypothesized to limit oxygen diffusion and confer high corrosion resistance to the alloy.
36 MATERIALS SCIENCE↗
Steering Molecular Dynamics Simulations of Membrane-Associated Proteins with Neutron Reflection Results
Herein, we present a novel method to incorporate structural results from surface-sensitive scattering, such as X-ray or neutron reflectometry, into molecular dynamics simulations. While reflectometry techniques generally provide a means to determine the molecular-scale structures of organized interfacial films, they were recently shown to offer the capability to characterize the structures of protein-membrane complexes supported by a solid substrate. One-dimensional information inherent in the experimental results is used in the form of component volume occupancy (CVO) profiles, which describe the distribution of molecular components within an interfacial architecture, to construct real-space constraints in the form of a biasing potential for the simulation that vanishes when the simulated and experimental profiles agree. This approach improves the correspondence between simulation and experiment, as shown in the re-evaluation of an neutron-reflection-derived structure which was approximated by an independent molecular dynamics simulation in earlier work, and it also leads to faster equilibration of ensemble structures. We further show that time averaging the CVO profile that develops in the simulation while biasing with this approach permits fluctuations about the average that are necessary for conformational exploration of the system. This method is particularly valuable for studies of proteins at interfaces that contain disordered regions since the conformation of such regions is difficult to judge from the analysis of one-dimensional experimental profiles and may take prohibitively long to equilibrate in simulations.
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
X-ray and Neutron Reflectivity Studies of Styrene-Maleic Acid Copolymer Interactions with Galactolipid-Containing Monolayers
Styrene-maleic acid (SMA) copolymers have recently gained attention for their ability to facilitate the detergent-free solubilization of membrane protein complexes and their native boundary lipids into polymer-encapsulated, nanosized lipid particles, referred to as SMALPs. However, the interfacial interactions between SMA and lipids, which dictate the mechanism, efficiency, and selectivity of lipid and membrane protein extraction, are barely understood. Our recent finding has shown that SMA 1440, a chemical derivative of the SMA family with a functionalized butoxyethanol group, was most active in galactolipid-rich membranes, as opposed to phospholipid membranes. In the present work, we have performed X-ray reflectometry (XRR) and neutron reflectometry (NR) on the lipid monolayers at the liquid–air interface followed by the SMA copolymer adsorption. XRR and Langmuir Π–A isotherms captured the fluidifying effect of galactolipids, which allowed SMA copolymers to infiltrate easily into the lipid membranes. NR results revealed the detailed structural arrangement of SMA 1440 copolymers within the membranes and highlighted the partition of butoxyethanol group into the lipid tail region. In conclusion, this work allows us to propose a possible mechanism for the membrane solubilization by SMA.
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
Design of a low frequency, density profile reflectometer system for the MAST-U spherical tokamak
Validated and accurate edge profiles (temperature, density, etc.) are vitally important to the Mega Ampere Spherical Tokamak Upgrade (MAST-U) divertor and confinement effort. Density profile reflectometry has the potential to significantly add to the measurement capabilities currently available on MAST-U (e.g., Thomson scattering and Langmuir probes). This work presents the diagnostic requirements, problems, and solutions facing profile reflectometry in spherical tokamaks and MAST-U in particular. Requirements include density measurements near zero electron density in the scrape off layer region, coverage for a broad range of MAST-U plasma parameters, high time (≤10 microseconds) and spatial resolutions (≤1 cm), reliability, and identification of the plasma start frequency.
Instruments & Instrumentation↗