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DOE OSTI2024

General Applications for Hamilton Vantage (GenApps for Vantage) v0.6.1

General applications for Hamilton Vantage is a flexible liquid handling method used to automate the most widely applicable types of automated liquid transfers. General applications can also be used as a tool to onboard new fully-automated workflows by breaking them down step by step into single transfers. The goal of General Applications is to make using the Hamilton Vantage liquid handler as easy & practical as using a handheld pipette for the end user. The software supports plate-to-plate transfers for a variety of method types including: Stamp: One-to-One, Stamp: One-To-Many, Split, Combine, Hitpick, and Qtray plating. General Applications eliminates the need for automation engineers to customize individual methods for each new workflow that gets onboarded. Steps can be customized within GenApps according to the needs of the researcher. The software utilizes a GUI to prompt the users to input variables – Allowing for flexible control over plate types, transfer volumes, number of replicates, tip types, liquid classes, mixing steps, aspiration/dispense heights and more. General Applications also generates a deck image and setup instructions to guide the researcher on how to load the deck and start the instrument.

Yoder, Sam↗

DOE OSTI2024

Silicate coprecipitation reduces green rust crystal size and limits dissolution-precipitation during air oxidation

Green rusts (GR) are mixed-valence iron (Fe) hydroxides which form in reducing redox environments like riparian and wetland soils and shallow groundwater. In these environments, silicon (Si) can influence Fe oxides’ chemical and physical properties but its role in GR formation and subsequent oxidative transformation have not been studied starting at initial nucleation. Green rust sulfate [GR(SO 4 )] and green rust carbonate [GR(CO 3 )] were both coprecipitated from salts by base titration in increasing % mol Si (0, 1, 10, and 50). The minerals were characterized before and after rapid (24 h) aqueous air-oxidation by x-ray diffraction (XRD), scanning electron microscopy (SEM), Fe extended x-ray absorption fine structure spectroscopy (EXAFS), and N 2 -BET surface area. Results showed that only GR(SO4) or GR(CO3) was formed at every tested Si concentration. Increasing % mol Si caused decreased plate size and increased surface area in GR(CO3) but not GR(SO4). GR plate basal thickness was not changed at any condition indicating a lack of Si interlayering. Air oxidation of GR(SO4) at all % mol Si contents transformed by dissolution and reprecipitation into lepidocrocite and goethite, favoring ferrihydrite with higher % Si content. Air oxidation of GR(CO3) transformed into magnetite and goethite but increasing Si caused GR to oxidize while retaining its hexagonal plate structure via solid-state oxidation. Our results indicate that Si has the potential to cause GR to form in smaller particles and upon air oxidation, Si can either stabilize the plate structure or alter transformation to ferrihydrite.

36 MATERIALS SCIENCE↗

DOE OSTI2020

High-Temperature Particle Heat Exchanger for sCO2 Power Cycles [Award 30342]

This report describes the design, development, and testing of a prototype 100 kWt particle-to-supercritical CO 2 (sCO2) heat exchanger. An analytic hierarchy process was implemented to compare and evaluate alternative heat-exchanger designs (fluidized bed, shell-and-plate moving packed bed, and shell-and-tube moving packed bed) that could meet the high pressure (≥ 20 MPa) and high temperature (≥ 700 °C) operational requirements associated with sCO2 power cycles. Cost, heat-transfer coefficient, structural reliability, manufacturability, parasitics and heat losses, scalability, compatibility, erosion and corrosion, transient operation, and inspection ease were considered in the evaluation. A 100 kWt shell-and-plate design was selected for construction and integration with Sandia’s falling particle receiver system that heats the particles using concentrated sunlight. Sandia worked with industry to design and construct the moving packed-bed shell-and-plate heat exchanger. Tests were performed to evaluate its performance using both electrical heating and concentrated sunlight to heat the particles. Overall heat transfer coefficients at off-design conditions (reduced operating temperatures and only three stainless steel banks in the counter-crossflow heat exchanger) were measured to be approximately ~25 - 70 W/m 2 -K, significantly lower than simulated values of >100 W/m 2 -K. Tests using the falling particle receiver to heat the particles with concentrated sunlight yielded overall heat transfer coefficients of ~35 – 80 W/m 2 -K with four banks (including a nickel-alloy bank above the three stainless steel banks). The overall heat transfer coefficient was observed to decrease with increasing particle inlet temperatures, which contrasted the results of simulations that showed an increase in heat transfer coefficient with temperature due to increased effective particle-bed thermal conductivity from radiation. The likely cause of the discrepancy was particle-flow maldistributions and funnel flow within the heat exchanger caused by internal ledges and cross-bracing, which could have been exacerbated by increased particle-wall friction at higher temperatures. Additional heat loss at higher temperatures may also contribute to a lower overall heat-transfer coefficient. Design challenges including pressure drop, particle and sCO2 flow maldistribution, and reduced heat transfer coefficient are discussed with approaches for mitigation in future designs. Lessons learned regarding instrumentation, performance characterization, and operation of particle components and sCO2 flow loops are also discussed. Finally, a 200 MWt commercial-scale shell-and-plate heat-exchanger design based on the concepts investigated in this report is proposed.

14 SOLAR ENERGY↗

DOE OSTI2022

A User Guide to PARET/ANL

PARET was originally created in 1969 at what is now Idaho National Laboratory (INL), to analyze reactivity insertion events in research and test reactor cores cooled by light or heavy water, with fuel composed of either plates or pins. The use of PARET is also appropriate for fuel assemblies with curved fuel plates when their radii of curvatures are large with respect to the fuel plate thickness. The PARET/ANL version of the code has been developed at Argonne National Laboratory (ANL) under the sponsorship of the U.S. Department of Energy/NNSA since the inception of the Reactor Conversion Program. Since Reduced Enrichment for Research and Test Reactors (RERTR) began in 1978, PARET/ANL has been benchmarked to experimental data including SPERT testing, and used to determine the expected transient behavior of a large number of reactors regardless of enrichment both inside and outside the Reactor Conversion Program. This document provides the pertinent information for the use of PARET/ANL Version 7.6. PARET/ANL models the various fueled regions of a reactor core as channels. Each of these channels consists of a single flat fuel plate/pin (including cladding and, optionally, a gap) with water coolant on each side. In slab geometry the coolant channels for a given fuel plate are of identical dimensions (mirror symmetry), but they can be of different thickness in each channel. There can be many channels, but each channel is independent and coupled only through reactivity feedback effects to the whole core. The time-dependent differential equations that represent the system are replaced by an equivalent set of finite-difference equations in space and time, which are integrated numerically. PARET/ANL uses fundamentally the same numerical scheme as RELAP5 for the time-integration of the point-kinetics equations. The one-dimensional thermal-hydraulic model includes temperature-dependent thermal properties of the solid materials, such as heat capacity and thermal conductivity, as well as the transient heat production and heat transfer from the fuel meat to the coolant. Temperature- and pressure-dependent thermal properties of the coolant such as enthalpy, density, thermal conductivity, and viscosity are also used in determining parameters such as friction factors and heat transfer coefficients. The code first determines the steady-state solution for the initial state. Then the solution of the transient is obtained by integration in time and space. Multiple heat transfer, DNB and flow instability correlations are available. The code was originally developed to model reactors cooled by an open loop, which was adequate for rapid transients in pool-type cores. An external loop model appropriate for Miniature Neutron Source Reactors (MNSR’s) was also added to PARET/ANL to model natural circulation within the vessel, heat transfer from the vessel to pool and heat loss by evaporation from the pool. PARET/ANL also contains models for decay heat after shutdown, control rod reactivity versus time or position, time-dependent pump flow, and loss-of-flow event with flow reversal as well as logic for trips on period, power, and flow. Feedback reactivity effects from coolant density changes and temperature changes are represented by tables. Feedback reactivity from fuel heat-up (Doppler Effect) is represented by a four-term polynomial in powers of fuel temperature. Photo-neutrons produced in beryllium or in heavy water may be included in the point-kinetics equations by using additional delayed neutron groups.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

DOE OSTI2023

Tuning Organic Semiconductor Packing and Morphology through Non-equilibrium Solution Processing (Final Report)

Organic semiconductors (OSCs) are a promising candidate to produce low-cost, large area, and flexible electronics. There has previously been successful development of organic field effect transistors (OFETs), photovoltaics (OPV), and bioelectronics using OSCs. Solution processing of these materials allows for the fabrication of large-area devices in the kinetic crystallization regime. The charge transport capabilities have been shown to depend on the morphology and molecular packing of the OSC within thin films. Our hypothesis is that solution processing conditions may significantly impact OSC morphology and as a result the charge transport. Therefore, this work has focused on obtaining a fundamental understanding of the morphology and molecular packing of OSCs for optimal device performance. Through our work, we have gained a better understanding of how these structural conditions were influenced by the solution processing conditions. Our studies have led to a more systematic understanding of the various parameters that impact OSC morphology. Solution processing leads to non-equilibrium films, thus allowing for the formation of diverse morphologies that are inaccessible by other fabrication methods. Previously, our group has focused on tuning the morphology of small-molecular OSCs [53, 55-57]. However, little work had been devoted to polymer OSCs. There was a lack of detailed studies characterizing the solution-state of polymer OSCs in terms of their conformation, degree of entanglement, polymer aggregation, and chain relaxation dynamics. The solution state properties are also likely to be influenced by the rigidity and molecular weight of the polymer OSCs investigated. Thus, we have focused our attention on gaining a better insight of polymer OSC films and solution processing methods. Through this proposal, our approach is to investigate the correlation between solution-state properties and the morphology of the resulting polymer OSC films. We worked three specific aims: investigate the effects of 1) polymer OSC solution-state properties on final film morphology; 2) molecular additives on the solution-state and final film properties; 3) controlled pre-aggregation in the solution-state in the final film morphology. More rigid and planar polymer backbones should promote interchain charge transport and more efficient interchain hopping between polymer chains. Through tailoring the polymer backbone, polymer sidechains, and molecular weight, we expected the altered solution-state properties to affect the final film morphology. In addition, reducing the entanglements and promoting chain alignment will likely prevent charge carrier trapping through conformation disorders. We thus studied different mechanisms, such as molecular additives, to reduce entanglements in solution. Devices fabricated from these solutions were expected to have improved charge transport abilities. In addition to tailoring the solution-state characteristics of the polymer OSCs, we investigated the effect of solution processing methods on the molecular packing and morphology of polymer OSC films. Two main solution processing techniques, e.g., spin-coating and solution shearing, were employed to fabricate OFETs. Spin coating was employed to prepare OSC films, which produce isotropic films. This technique creates several parameters to tune such as spin coating speed, acceleration, and time. Additionally, our research group developed the solution shearing method, which consists of the solution initially sandwiched between two plates. By sliding the top plate, the solution front is exposed and drying begins. This technique allows for the creation of aligned large crystalline domains. Solution shearing consists of different processing parameters which can affect the final morphology, such as shearing speed, substrate temperature and temperature gradient, distance between both plates, and the tilt angle of the top plate. Due to the complexity of the polymer systems investigated, numerous techniques were employed to characterize the polymer OSC solution state and films. All the materials were characterized using the DOE supported synchrotron X-ray scattering facilities at the Stanford Synchrotron Radiation Lightsource (SSRL). Using grazing incidence X-ray scattering (GIXS) and Near Edge X-ray Absorption Fine Structure (NEXAFS) techniques, the crystalline structure and molecular orientations of the thin films were measured. Optical absorption (UV-Vis) spectroscopy was employed to determine the aggregation state in solution and films of the polymer systems. Polarized UV-Vis also allowed for the determination of the relative degree of polymer chain alignment for solution sheared films. Additionally, various other techniques were used to investigate other properties within the film, such as atomic force microscopy (AFM) and solution rheology. Finally, the device performance is quantified through the fabrication and characterization of OFETs, which will highlight the effects of morphology on charge transport.

36 MATERIALS SCIENCE↗

DOE OSTI2024

High-Energy Laser Direct Strike Assessment for NIF CryoXNBS Snout and Naiad SNM Container

An experimental IPT performed two NIF shots as an assessment of the effect of a direct laser beam strike impact on the NIF CryoXNBS snout and Naiad container. Four aligned NIF outer cone beams at best focus, 42 kJ total, struck a four millimeter thick stainless plate. In the first shot, the struck plate was followed by a 1.75 mm gap and a 2.0 millimeter stainless plate to create a surrogate geometry for the current CryoXNBS snout and Naiad container. There was minor plastic deformation of the rear plate rear surface with no evidence of bulk failure. The second shot tested a layered glass-filled polycarbonate and titanium shield placed in the gap. Nondestructive assay was sufficient to metrologize the beam strike area and the damage induced to the NIF target assemblies.

36 MATERIALS SCIENCE↗

DOE OSTI2023

Friction Experiment Data Analysis

The Spent Fuel Waste Disposition (SFWD) program under the U.S. Department of Energy (DOE) is planning a seismic shake table test of full-scale dry storage systems of spent nuclear fuel (SNF) to close the gap related to the seismic loads on the fuel assemblies in dry storage systems. This test will allow for quantifying the strains and accelerations on surrogate fuel assembly during representative earthquakes. A concrete layer will be installed on the shake table before the test to simulate conditions representative of an ISFSI pad. In the shake table tests with the vertical cask, the cask will be free-standing because this is representative of all, except two, ISFSIs in the U.S. with vertical dry storage casks. The static and dynamic friction coefficients between the steel bottom of the cask and the concrete layer on the shake table are important parameters that will affect cask behavior during the test. These parameters must be known for the pre- and post-test modelling, data analysis, and model validation. The friction experiment was performed at the Engineering Department of the University of New Mexico (UNM) to determine the friction coefficients between a steel plate with the same finish as the bottom of the vertical cask manufactured for the test and different concrete surfaces. In this experiment the steel plate was fixed and the concrete sample was pulled over the plate with a constant displacement rate using an MTS machine. This allowed for collecting continuous horizontal force data over the length of the steel plate. Four displacement rates and three vertical loads were used. The tests were performed with four concrete blocks with different degrees of the surface roughness - light sandblast, light to medium sandblast, medium bush hammer, and heavy sandblast. The total number of tests was 48. The data were used to calculate static and dynamic friction coefficients.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2024

Anisotropic Tensile Properties of a 14YWT Nanostructured Ferritic Alloy: On the Role of Cleavage Fracture

Two plates of nanostructured ferritic alloy NFA-1 were processed by ball milling atomized Fe-14Cr-3W-0.4Ti-0.2Y (wt.%) with FeO powders, canning, and hot-extrusion at 850 °C, followed by annealing and multipass cross-rolling at 1000 °C. This produces a severe (001) brittle cleavage texture on planes running parallel to the plate faces. In the first plate (P1), pre-existing microcracks (MCs) formed on the cleavage planes during cross-rolling. The second plate (P2) contained far fewer, if any, MCs. Here, we compare the tensile data for out-of-plane (S) and in-plane (L) tensile axis orientations, at temperatures from −196 °C to 800 °C. We also assess the tensile property differences between P1 and P2, and the effect of specimen size. The L-orientation strength and ductility were excellent; for example, the room temperature (RT) yield stress, σy ≈ 1042 ± 102 MPa, and the total elongation, εt ≈ 12.9 ± 1.5%. In contrast, the S-orientation RT σy ≈ 708 ± 57 MPa, and εt ≤ 0.2%. These differences were due to cleavage on the brittle (001) planes. Cleavage leads to beneficial delamination toughening, but is deleterious to deformation processing and through-wall heat transfer. Therefore, it is important to quantitatively characterize the pronounced NFA-1 strength anisotropy due to severe crystallographic texturing and cleavage fracture.

Crystallography↗

DOE OSTI2020

Fatigue-Crack Detection and Monitoring through the Scattered-Wave Two-Dimensional Cross-Correlation Imaging Method Using Piezoelectric Transducers

Piezoelectric transducers are convenient enablers for generating and receiving Lamb waves for damage detection. Fatigue cracks are one of the most common causes for the failure of metallic structures. Increasing emphasis on the integrity of critical structures creates an urgent need to monitor structures and to detect cracks at an early stage to prevent catastrophic failures. This paper presents a two-dimensional (2D) cross-correlation imaging technique that can not only detect a fatigue crack but can also precisely image the fatigue cracks in metallic structures. The imaging method was based on the cross-correlation algorithm that uses incident waves and the crack-scattered waves of all directions to generate the crack image. Fatigue testing for crack generation was then conducted in both an aluminum plate and a stainless-steel plate. Piezoelectric wafer transducer was used to actuate the interrogating Lamb wave. To obtain the scattered waves as well as the incident waves, a scanning laser Doppler vibrometer was adopted for acquiring time-space multidimensional wavefield, followed with frequency-wavenumber processing. The proof-of-concept study was conducted in an aluminum plate with a hairline fatigue crack. A frequency-wavenumber filtering method was used to obtain the incident wave and the scattered wave wavefields for the cross-correlation imaging. After this, the imaging method was applied to evaluate cracks on a stainless-steel plate generated during fatigue loading tests. The presented imaging method showed successful inspection and quantification results of the crack and its growth.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2020

Mechanical seal with high pressure high temperature secondary seal

A secondary seal of a mechanical seal comprises an annular sealing gasket and backing plate surrounding a cylindrical sealing surface, all of which can be made of the same metallic material. The gasket is C-shaped in cross section, and is axially pressed during operation into a C-shaped groove formed in the backing plate, the groove being shallower and larger in inner diameter than the gasket, so that the gasket, when pressed into the groove, deforms radially inward and seals against both the backing plate and the sealing surface. The contact area between the gasket and sealing surface increases with pressure. In embodiments, when the pressure is released, the gasket retracts from the sealing surface, allowing easy disassembly and allowing axial movement of the gasket and backing plate. Highly polished surfaces of the gasket and sealing surface can allow axial motion thereof during operation to maintain the seal face gap.

42 ENGINEERING↗

DOE OSTI2020

Multi-layer wearable body armor

A multi-layer body armor plate includes a strike plate; a mesh layer positioned over the strike plate, the mesh layer having a number of open cells; and an outer skin layer positioned over the mesh layer so as to encapsulate the open cells of the mesh layer between the strike plate and the outer skin layer. The open cells of the mesh layer may entrap air or may be filled with expandable, buoyant foam.

45 MILITARY TECHNOLOGY, WEAPONRY, AND NATIONAL DEF↗

DOE OSTI2020

Combustor with axially staged fuel injection

A combustor with axially staged fuel injection includes a plurality of nozzle segments annularly arranged about a center fuel nozzle. Each nozzle segment includes a fuel plenum partially defined between a forward plate and an aft plate and a plurality of tubes that extends through the fuel plenum and the aft plate. A panel fuel injector extends axially downstream from the aft plate and includes an outer wall, an inner wall, a plurality of outlets defined along at least one of the outer wall and the inner wall and a plurality of premix channels defined between the outer wall and the inner wall. Each premix channel is in fluid communication with a fuel supply, a compressed air supply and a respective outlet of the plurality of outlets.

42 ENGINEERING↗

DOE OSTI2020

High-frequency direct current bulk capacitors with interleaved busbar packages

Presented are electrical capacitors with interleaved busbar architectures, methods for making/operating such capacitors, and electric-drive vehicles equipped with such capacitors. A bulk capacitor includes multiple capacitor devices disposed within an outer housing and operable to modify electric current transmitted between a power source and an electrical load. An interleaved busbar package is interposed between the capacitor devices and outer housing. The interleaved busbar package includes a first busbar plate that electrically connects to first terminals of the capacitor devices and defines a busbar pocket. A second busbar plate is seated within the busbar pocket and electrically connects to second terminals of the capacitor devices. The second busbar plate includes a capacitor basin that seats therein the capacitor devices. An isolator sheet is interleaved between and electrically insulates the first and second busbar plates. The capacitor devices and interleaved busbar package may be partially submerged in an epoxy endfill composition.

42 ENGINEERING↗

DOE OSTI2020

Optical fiber receptacle cover

A cover for partially covering and protecting cables plugged into a receptacle is provided. The receptacle includes a face plate with a first hole through which a first fastener secures the face plate to a face of the receptacle. The cover comprises a plurality of walls at least partially defining a hollow chamber, a slot adjacent to the chamber and configured to receive the face plate when the cover is slid over the face plate, an opening that leads to the chamber and the slot, and a first channel extending partially through the chamber and configured to provide access to the fastener.

42 ENGINEERING↗

DOE OSTI2021

Multi-layer wearable body armor

Barr, Christian G.↗

DOE OSTI2022

Damage Evolution of Double-Sided Copper Conductor on Multi-layer Flexible Substrate Under Bending

Abstract—Thin-film conductors continue to play an important role in flexible electronics, and thus, the performance and reliability of such conductors under mechanical loading such as stretch, bend, and twist need to be studied through experiments as well as simulations. This paper focuses on the damage evolution of the thin-film conductors under cyclic bending. Four types of double-sided copper conductors: straight trace without coverlay, straight trace with coverlay, notched trace without coverlay, and notched trace with coverlay on multi-layer substrates were studied in this work. The adaptive curvature flexure test method, which is suitable for thin-film bending, was employed in this work. Adaptive curvature flexure test is one where the flexible substrate with its conductor is positioned between two parallel plates, and the parallel plates are moved relative to each other such that the gap distance between the parallel plates changes in one of the configurations of the adaptive curvature flexure test. Different strain levels can be achieved easily in such an adaptive curvature flexure test by controlling the gap distance between the parallel plates. By subjecting flexible substrates with thin conductors to such bend tests, the fatigue life of the specimen was determined for different magnitudes of strain ranges. The results were then compared among the four types of conductors. Specimens were designed such that the conductors were placed on both sides of the substrate so that the one of the conductors would undergo tensile straining, while the other one would undergo compressive straining. It was shown that the fatigue life was highly dependent on the magnitude of strain range, and that the conductor on the compressive side failed sooner than that on the tensile side. The failed specimens were examined in a microscope at different number of cycles. Also, the resistance of the conductors, which is directly related to the reliability of thin-film conductors, was monitored in-situ during bending. The resistance change with the strain range change as well as the resistance progression with the number of cycles in tensile as well as compressive mode were determined, and such information is then used to create failure prediction models for thin-film conductors on flexible substrates.

damage evolution, flexible conductor, multi-layer ↗

DOE OSTI2022

Alternative low cost electrodes for hybrid flow batteries

A redox flow battery may include: a membrane interposed between a first electrode positioned at a first side of the membrane and a second electrode positioned at a second side of the membrane opposite to the first side; a first flow field plate comprising a plurality of positive flow field ribs, each of the plurality of positive flow field ribs contacting the first electrode at first supporting regions on the first side; and the second electrode, including an electrode spacer positioned between the membrane and a second flow field plate, the electrode spacer comprising a plurality of main ribs, each of the plurality of main ribs contacting the second flow field plate at second supporting regions on the second side, each of the second supporting regions aligned opposite to one of the plurality of first supporting regions. As such, a current density distribution at a plating surface may be reduced.

Evans, Craig E.↗

DOE OSTI2022

Microstructural Characterization of A709 Commercial Heats with Precipitation Treatment

This report discusses work conducted at Idaho National Laboratory in fiscal year 2022 associated with the precipitates in Alloy 709 (A709). The purpose of this work is to support the development of the A709 Code Cases to qualify A709 in Section III, Division 5 of the American Society of Mechanical Engineers Boiler and Pressure Vessel Code. This would permit the use of A709 for elevated-temperature nuclear construction. This work encompassed two broad goals. The first goal was to understand the microstructure of the second commercial heat of plate A709 purchased through the Advanced Reactors Technologies Program in both the solution-annealed and precipitation-treated conditions. Transmission electron microscopy was utilized to characterize these microstructures. Direct comparisons were then made between the solution-annealed and precipitation-treated conditions as well as between the first and second commercial heats of plate A709. The second goal was to understand the impact of variations in the time and temperature of the precipitation treatment on the properties of A709. The precipitation treatment temperature was varied from 750°C to 800°C for times ranging from 3 hours to 30 hours. The hardness of each precipitation treatment variation was measured. All of the precipitation treatment variations investigated besides a specimen from the second commercial heat of plate A709 precipitation treated at 800? for 9 hours met the room-temperature hardness requirement specified in ASTM A213 and SA-213 for UNS S31025. The hardness measured for the specimen from the second commercial heat of plate A709 that was precipitation treated at 800? for 9 hours is considered an outlier. The next step is to look at the extremes of the precipitation treatment variations investigated and conduct elevated-temperature mechanical testing. The purpose of this testing would be to assess if these time and temperature variations have any impact on the mechanical performance.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗