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At least 181 records · Page 10

Structure–property relations in graphitic pebbles for nuclear applications

This work presents an analytical approach for holistically characterizing graphitic matrix pebbles for nuclear applications whereby the macrostructure, microstructure, and thermophysical properties of pebbles are determined. A systematic sectioning method was applied to several pebbles to describe the regional properties of the samples. Intact matrix-only spheres and sections of spheres fabricated by Kairos Power were characterized via optical imaging, x-ray computed tomography, x-ray diffraction, and ellipsometry to determine 2D and 3D macrostructure and anisotropy. The thermophysical properties of these materials were determined via measurements of density, specific heat, thermal expansion, and thermal diffusivity. The results of this study indicate that the pebble fabrication methods and their resultant effect on microstructure have a nontrivial effect on thermophysical properties, confirming the importance of robust characterization of these components. A discussion of the characterization approach and its applicability to nuclear fuel development activities is also included.

42 ENGINEERING↗

Influence of Oxygen Flow and Stoichiometry on Optical Properties and Damage Resistance of Hafnium Oxide Thin Films

Hafnium oxide (HfO 2 ) is predominantly used as a high-index material in multi-layer dielectric coatings for high-peak- and high-average-power lasers, but laser damage often initiates within the HfO 2 layers despite their wide bandgap. Oxygen deficiency during deposition can introduce vacancy-related sub-bandgap states and absorptive defects, lowering damage resistance. This study investigates how oxygen flow during HfO 2 deposition with ion beam sputtering (IBS) affects its stoichiometry, defect formation, and nanosecond laser-induced damage threshold (LIDT) and whether single-layer trends predict multilayer performance. Single layers were deposited at varying oxygen flows, characterized for optical and structural properties, and tested for the LIDT at 1064 nm and 355 nm. Increasing oxygen flow drove the layer toward near-stoichiometric HfO 2 , reduced the refractive index, and altered the density of surface pinhole-like features. The single-layer LIDT at 355 nm increased with oxygen, whereas the 1064 nm LIDT was comparatively less sensitive to oxygen flow, consistent with the wavelength-dependent roles of absorptive precursors and microstructural defects. In contrast, a HfO 2 -based high-reflector (HR) showed a higher LIDT at lower oxygen flow, indicating that the family of damage precursors changes between single layers and multilayers; in stacks, structural properties such as stress, gas entrapment and thermal dissipation may outweigh the isolated absorptive defects found in single layers. These results demonstrate that the optimal oxygen flow condition depends on both LIDT wavelength and film architecture. We identified, for single layers, a 15–35 sccm window for maximizing the 1064 nm LIDT and a high-flow optimum (45 sccm) for the 355 nm LIDT and, for 355 nm HR stacks, a distinct lower-flow regime (~10 sccm).

Optics and optical instruments↗

Microporous structure in silicone polymers with polylactic acid and polyethylene glycol microspheres: Synthesis and characterization

Porosity in polymer parts could improve mechanical properties while reducing weight and density. Individual pores must be small enough that bulk mechanical properties are retained but significant enough to reduce the density of the material. Filler materials can be incorporated into polymer matrices and removed to create voids. Here, this paper focuses on creating spherical pores in silicone matrices by inserting and removing core materials or fillers during post-cure. A method was developed to incorporate pore formers into an uncured polymer resin and remove the pore former materials from the matrix. Polyethylene glycol (PEG) and polylactic acid (PLA) microspheres were created and incorporated into silicone matrices as pore formers. Microspheres with controllable size distributions were formed via an emulsion formation. Microspheres are removed from the matrix by solvent extraction and calcination. Thermogravimetric Analysis (TGA), Dynamic Mechanical Analysis (DMA), and optical imaging characterize and determine the successful creation of micropores in the polymer matrices.

36 MATERIALS SCIENCE↗

Demonstrating SolarPILOT’s Python API Through Heliostat Optimal Aimpoint Strategy Use Case

SolarPILOT is a software package that generates solar field layouts and characterizes the optical performance of concentrating solar power (CSP) tower systems. SolarPILOT was developed by the National Renewable Energy Laboratory (NREL) as a stand-alone desktop application but has also been incorporated into NREL’s1 System Advisor Model (SAM) in a simplified format. Prior means for user interaction with SolarPILOT have included the application’s graphical interface, the SAM routines with limited configurability, and through a built-in scripting language called “LK.” This paper presents a new, full-featured, Python-based application programmable interface (API) for SolarPILOT, which we hereafter refer to as CoPylot. CoPylot provides access to all SolarPILOT’s capabilities to generate and characterize power tower CSP systems seamlessly through Python. Supported capabilities include (i) creating and destroying a model instance with message reporting tools; (ii) accessing and setting any SolarPILOT variable including custom land boundaries for field layouts; (iii) programmatically managing receiver and heliostat objects with varied attributes for systems with multiple receiver or heliostat types; (iv) generating, assigning, and modifying solar field layouts including the ability to set individual heliostat locations, aimpoints, soiling rates, and reflectivity levels; (v) simulating solar field performance; (vi) returning detailed results describing performance of individual heliostats, the aggregate field, and receiver flux distribution; and, (vii) exporting Python-based model instances to multiple file formats. CoPylot enables Python users to perform detailed CSP tower analysis utilizing either the Hermite expansion technique (analytical) or the SolTrace ray-tracing engine. In addition to CoPylot’s functionality, Python users have access to the over 100,000 open-source libraries to develop, analyze, optimize, and visualize power tower CSP research. This enables CSP researchers to perform analysis that was previously not possible through SolarPILOT’s existing interfaces. This paper discusses the capabilities of CoPylot and presents a use case wherein we demonstrate optimal solar field aiming strategies.

41 EE - Solar Energy Technologies Office (EE-4S)↗

Demonstrating SolarPILOT's Python API Through Heliostat Optimal Aimpoint Strategy Use Case: Preprint

SolarPILOT is a software package that generates heliostat field layouts and characterizes the optical performance of concentrating solar power (CSP) tower systems. SolarPILOT was developed by the National Renewable Energy Laboratory (NREL) as a stand-alone desktop application but has also been incorporated into NREL's System Advisor Model (SAM) in a simplified format. Prior means for user interaction with SolarPILOT have included the application's graphical interface, the SAM routines with limited configurability, and through a built-in scripting language called "LK." This paper presents a new, full-featured Python-based application programmable interface (API) for SolarPILOT, which we hereafter refer to as CoPylot. CoPylot provides access to all SolarPILOT's capabilities to generate and characterize power tower CSP systems seamlessly through Python. Supported capabilities include (i) creating and destroying a model instances with message reporting tools; (ii) accessing and setting any SolarPILOT variable including custom land boundaries for field layout; (iii) programmatically managing receiver and heliostat objects with varied attributes for systems with multiple receiver or heliostat types; (iv) generating, assigning, and modifying heliostat field layouts including the ability to set individual heliostat locations, aimpoints, soiling rates, and reflectivity levels; (v) simulating heliostat field performance; (vi) returning detailed results describing performance of individual heliostats, the aggregate field, and receiver flux; and, (vii) exporting Python-based model instances to multiple file formats. CoPylot enables Python users to perform detailed tower CSP analysis utilizing either the Hermite expansion technique (analytical) or the SolTrace ray-tracing engine. In addition to CoPylot's functionality, Python users have access to the over 100,000 open-source libraries to develop, analyze, optimize, and visualize CSP tower research.

41 EE - Solar Energy Technologies Office (EE-4S)↗

Infrared Optical Anisotropy in Quasi‐1D Hexagonal Chalcogenide BaTiSe 3

Polarimetric infrared (IR) detection bolsters IR thermography by leveraging the polarization of light. Optical anisotropy, i.e., birefringence and dichroism, can be leveraged to achieve polarimetric detection. Recently, giant optical anisotropy is discovered in quasi-1D narrow-bandgap hexagonal perovskite sulfides, A 1+x TiS 3 , specifically BaTiS 3 and Sr 9/8 TiS 3 . In these materials, the critical role of atomic-scale structure modulations in the unconventional electrical, optical, and thermal properties raises the broader question of the nature of other materials that belong to this family. To address this issue, for the first time, high-quality single crystals of a largely unexplored member of the A 1+x TiX 3 (X = S, Se) family, BaTiSe 3 are synthesized. Single-crystal X-ray diffraction determined the room-temperature structure with the P31c space group, which is a superstructure of the earlier reported P6 3 /mmc structure. The crystal structure of BaTiSe 3 features antiparallel c-axis displacements similar to but of lower symmetry than BaTiS 3 , verified by the polarization dependent Raman spectroscopy. Fourier transform infrared (FTIR) spectroscopy is used to characterize the optical anisotropy of BaTiSe 3 , whose refractive index along the ordinary (E ⊥ c) and extraordinary (E ‖ c) optical axes is quantitatively determined by combining ellipsometry studies with FTIR. With a giant birefringence Δn ∼ 0.9, BaTiSe 3 emerges as a new candidate for miniaturized birefringent optics for mid-wave infrared to long-wave infrared imaging.

optical anisotropy↗

A Workflow for Accelerating Multimodal Data Collection for Electrodeposited Films

Abstract Future machine learning strategies for materials process optimization will likely replace human capital-intensive artisan research with autonomous and/or accelerated approaches. Such automation enables accelerated multimodal characterization that simultaneously minimizes human errors, lowers costs, enhances statistical sampling, and allows scientists to allocate their time to critical thinking instead of repetitive manual tasks. Previous acceleration efforts to synthesize and evaluate materials have often employed elaborate robotic self-driving laboratories or used specialized strategies that are difficult to generalize. Herein we describe an implemented workflow for accelerating the multimodal characterization of a combinatorial set of 915 electroplated Ni and Ni–Fe thin films resulting in a data cube with over 160,000 individual data files. Our acceleration strategies do not require manufacturing-scale resources and are thus amenable to typical materials research facilities in academic, government, or commercial laboratories. The workflow demonstrated the acceleration of six characterization modalities: optical microscopy, laser profilometry, X-ray diffraction, X-ray fluorescence, nanoindentation, and tribological (friction and wear) testing, each with speedup factors ranging from 13–46x. In addition, automated data upload to a repository using FAIR data principles was accelerated by 64x.

36 MATERIALS SCIENCE↗

Optical and mass-spectral characterization of mixed-gas flowing atmospheric-pressure afterglow sources

Plasma-based ambient desorption/ionization (ADI) sources for mass spectrometry (MS) often use helium as the primary discharge gas due to the large reaction cross section of excited helium species with atmospheric gases, which ultimately leads to efficient reagent-ion formation. However, some studies have shown that mixed-gas plasmas provide unique advantages. For instance, our group showed that a helium-oxygen flowing atmospheric-pressure afterglow (He:O 2 -FAPA) source yielded enhanced ion signals for small polar analytes, but compounds with aromatic rings underwent chemical modification to produce pyrylium species. Here, it is shown that the addition of H 2 to the helium FAPA gas significantly decreased the reagent-ion signals, but analyte-ion signal was not affected to the same degree. In addition, mass spectra obtained with He:H 2 -FAPA were chemically cleaner with fewer ions stemming from analyte species and produced less oxidation of analytes. Addition of nitrogen increased the abundance of negative reagent ions (e.g., NO 2 - and NO 3 - ) which led to enhanced ion signal for RDX. To better understand these unique advantages of a mixed-gas FAPA, the impact of molecular-gas (O 2 , N 2 , or H 2 ) addition on the optical-emission spectra from the discharge was also measured. Spatially resolved emission was obtained from the anode- and negative-glow regions. In general, addition of small fractions (~0.1%) of molecular gases decreased helium and OH emission intensities. Atomic oxygen and hydrogen emission increased with the addition of O 2 and H 2 , respectively. Furthermore, emission characteristics of N 2 , N 2 + , and NO with respect to molecular gas composition on He-FAPA were measured. Finally, fundamental plasma parameters, such as OH rotational temperature (T rot ), were also calculated for these mixed-gas systems.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Performance Assessment of Portable Optical Particle Spectrometer (POPS)

Accurate representation of atmospheric aerosol properties is a long-standing problem in atmospheric research. Modern pilotless aerial systems provide a new platform for atmospheric in situ measurement. However, small airborne platforms require miniaturized instrumentation due to apparent size, power, and weight limitations. A Portable Optical Particle Spectrometer (POPS) is an emerged instrument to measure ambient aerosol size distribution with high time and size resolution, designed for deployment on a small unmanned aerial system (UAS) or tethered balloon system (TBS) platforms. This study evaluates the performance of a POPS with an upgraded laser heater and additional temperature sensors in the aerosol pathway. POPS maintains its performance under different environmental conditions as long as the laser temperature remains above 25 °C and the aerosol flow temperature inside the optical chamber is 15 °C higher than the ambient temperature. The comparison between POPS and an Ultra-High Sensitivity Aerosol Spectrometer (UHSAS) suggests that the coincidence error is less than 25% when the number concentration is less than 4000 cm –3 . The size distributions measured by both of them remained unaffected up to 15,000 cm –3 . While both instruments’ sizing accuracy is affected by the aerosol chemical composition and morphology, the influence is more profound on the POPS.

47 OTHER INSTRUMENTATION↗

Boron‐Doped Nano‐Crystalline Coated Carbon Fibers for Phasic Dopamine Sensing

Real time, chronic electrochemical detection of neurotransmitters will provide a positive step in the treatment and understanding of neurological disease. However, current electrodes using carbon fibers (CF) fail to perform chronically. While diamond-based coatings show promise in improving their longevity, achieving a uniform layer of such coatings on CFs is challenging, and the electrodes often lose sensitivity after coating. In this work, a complete and uniform boron-doped nanocrystalline material grown in a diamond reactor (B-NCD) was developed to coat CF microelectrodes for neurochemical sensing. The coating was characterized electrically, optically, mechanically, and chemically. The B-NCD coated CF electrodes were able to detect phasic dopamine at a sensitivity comparable to the most widely used alternatives (uncoated and PEDOT:Nafion coated CFs). During biofouling testing, the B-NCD coated CF electrodes demonstrated better stability than uncoated CFs and comparable performance to PEDOT:Nafion coated CFs. Moreover, B-NCD exhibited no signs of degradation during consecutive FSCV applications, while uncoated and PEDOT:Nafion coated CF electrodes degraded significantly over time. Furthermore, the B-NCD coating supported the survival and development of neurons and astrocytes in vitro, exhibited excellent adhesion and durability during mechanical bending testing, and enabled successful in vivo recording of phasic dopamine release in the rat brain. Overall, B-NCD coated CFs present as an ideal candidate for chronic, flexible neural implantable electrodes for long-term neurochemical monitoring.

carbon fiber↗

Experimental Evidence of Free Carrier Generation in 2D Hybrid Organic–Inorganic Perovskites

Despite the significant potential of 2D hybrid organic–inorganic perovskites (2DHOIPs) for high-efficiency optoelectronics application-comparable to their 3D counterparts, the fundamental carrier photogeneration remains unclear. In contrast to conventional ultrafast optical property characterization, we use ultrafast photocurrent spectroscopy to investigate the early-time electrical properties of type-I and type-II 2DHOIPs by manipulating the quantum confinement and the dielectric quantum matching effect. We discovered that the high frequency dielectric quantum matching effect plays a major role in 2DHOIPs, demonstrated by their high carrier mobility (µ), near-unity photogeneration quantum yield (Φ), below-room temperature exciton binding energy (E b ), and approaching 3D space factor (DSF). Our work shows that the optoelectronic performances of 2DHOIPs are comparable to their counterparts of 3DHOIPs.

2D perovskite↗

Effects of weave path parameters on the geometry of wire arc additive manufactured features

Here, the present work investigates the effect of process parameters on the geometry of wire arc additive manufactured parts. The geometric accuracy of features produced with a weaving strategy is compared to what can be accomplished with a typical overlapping bead strategy. In this work, single-layer and multi-layer geometries were deposited under varying process and path parameters. The wavelength, amplitude, and torch speed of the weaving path were varied, while the power, wire feed speed, and contact tip to work distance remained constant. The geometric deposition efficiencies of several samples produced with a weave strategy are directly compared to samples generated with two parallel overlapping beads with torch speeds defined to match the deposition rate of the weave samples. Feature geometries were characterized using optical microscopy and laser scanning data. The results indicate that implementing a weave path strategy can improve the geometric accuracy of wire arc additive features, thus increasing the effective volumetric deposition rate of the process. It is shown that the most consistent improvements resulted from the combination of low wavelength and high amplitude, which correlate to wider and taller printed layers.

GMAW↗

Microstructure and Residual Stress in Functionally Graded 316L Stainless Steel/Inconel 625 Alloys Fabricated by Direct Energy Deposition

Functionally graded materials (FGMs) provide a unique solution to combine distinct properties within a single component to enhance its overall performance. Understanding the microstructure and residual stress distribution is particularly important as the material dissimilarity in FGMs can result in high residual stress that affects the mechanical integrity of structural components. Here, this work aims to study the microstructure and residual stress of additively manufactured FGMs and the effects of isothermal annealing. In this study, 316L stainless steel/Inconel 625 FGMs were built by direct energy deposition, and characterized by optical and electron microscopy as well as synchrotron-based X-ray diffraction. Our study reveals that thermal annealing at 500°C for 3 h has minimal effects on the microstructure and chemistry of the graded materials, but effectively relieves the residual stress and leads to a uniform distribution of residual stress.

36 MATERIALS SCIENCE↗

Large-scale additive manufacturing of self-heating molds

Large-scale material extrusion additive manufacturing technology is becoming the new mainstream technology for scaled-up composite mold and die applications. This paradigm shift in composite processing technology is primarily driven by out-of-autoclave tooling applications, in which fiber reinforced composite molds with scaled-up sizes and embedded heating elements are attractive. The present research describes the design, manufacturing, and testing of self-heating composite molds fabricated via a large-scale pellet extrusion 3D printing machine with an integrated wire co-extrusion tool. Polycarbonate (PC) composites reinforced with carbon fiber (PC/CF; 20 wt.%) and glass fiber (PC/GF; 20 wt.%) were used to fabricate mold parts. Joule heating thermal test results showed that uniform temperatures (~100 °C) were achieved for both PC/CF and PC/GF mold surfaces, using a custom-made feedback control power supply and infrared thermography. Mechanical characterizations, including tensile and flexural testing were performed on the wire-embedded and un-wired PC/CF and PC/GF base specimens to investigate the impact of the fiber reinforcement as well as the embedded wires. In the direction of extrusion, the ultimate tensile stress of PC/CF was 105 MPa, and that of PC/GF was 73 MPa, while the neat PC value was 64 MPa. Inner-bead voids and interfacial gaps were observed and characterized via optical and scanning electron microscopy. The embedded wires and inner bead impacted the mechanical properties of the composites. Furthermore, the stiffness of the wire-embedded mold was still satisfactory, proving that the technology can be used to fabricate additively manufactured out-of-oven/autoclave molds.

36 MATERIALS SCIENCE↗

Transverse impact by RCCs on S-glass and Kevlar® FRC strips

This study aims to isolate interactions between plies and tows and reveal fundamental physics involved in transverse impact on fiber-reinforced composite (FRC) structures. Composite strips were sectioned from large panels and characterized by optical photography, three-dimensional synchrotron X-ray computed tomography, and scanning electron microscopy (SEM). Each strip was impacted perpendicularly by a right circular cylinder (RCC) projectile at a velocity ranging from ~ 150 to 600 m/s. The global strip behavior, as well as localized deformation and failure of the strip near the projectile corner, were both captured by high-speed optical imaging. S-Glass FRC strips were observed to fail in tension ahead of the RCC projectiles’ flat surfaces while Kevlar® FRC strips fractured at the projectile corners. The concept of critical velocity region previously used for impact on yarns was introduced to define different failure modes of each composite strip type. The strip damage extent was found to increase with the impact velocity and reach the maximum at the upper limit of the critical velocity region. Above the critical velocity region, the damage extent decreased with impact velocity. Wave propagations and load histories in the composite strips during impact were quantified and compared with Smith’s theory. Finally, critical velocities of single fibers, yarns, and composite strips and ballistic limits of single-ply and multi-ply composite panels were compared to provide insight into the design of impact-resistant fabrics and composites.

42 ENGINEERING↗

A reactive wetting strategy improves lithium metal reversibility

The cycling of lithium metal (Li 0 ) anode is often accompanied by irregular lithium plating/stripping, leading to poor Li 0 reversibility, and posing a grand challenge to constructing reliable Li 0 batteries. Hereby, we report a reactive wetting strategy to enable conformal and highly reversible Li 0 plating/stripping through a lithium-reactive substrate. In this study, the reactive wetting, smooth nucleation, and conformal growth behaviors of Li 0 are visualized through in-situ transmission electron microscopy, ex-situ scanning electron microscope, and in-situ optical microscope characterizations. Based on the reactive wetting substrate, high average Coulombic efficiencies (99.0% at 0.5 mA cm -2 for 400 cycles) are realized for Li 0 anodes. By pre-plating Li 0 into the reactive wetting substrate as anodes and leveraging LiFePO 4 as cathodes, high capacity retention (76.0% after 200 cycles in low N/P ratio conditions) is also achieved in the as-constructed Li 0 full cells. This work establishes a fundamental understanding of reactive wetting dynamics of Li 0 and provides a drop-in solution to improving Li 0 reversibility.

25 ENERGY STORAGE↗

A process optimization framework for laser direct energy deposition: Densification, microstructure, and mechanical properties of an Fe-Cr alloy

Laser Direct Energy Deposition (DED) is a metal additive manufacturing technique with the ability to fabricate large and complex parts through deposition of metal powders. However, achieving high-density parts and targeted build heights using DED can be challenging due to the large number of highly sensitive process variables. This work proposes a robust fabrication parameter optimization framework to generate process maps for primary parameters in DED, including laser power, scan speed, mass flow rate, hatch spacing, and layer height. Simple single-track experiments were utilized to map out the parameter space, and a combination of geometric criteria for hatch spacing and layer height were proposed to determine parameter sets that achieve both targeted build heights and mitigate porosity formation. Using this framework, specimens with >99 % density and consistent mechanical properties were successfully fabricated over a wide range of process parameters for an Fe-9wt.%Cr (Fe9Cr) alloy, a surrogate for radiation damage-resistant reduced activation ferritic/martensitic (RAFM) steels. Processing these materials using DED is of particular interest in the development of plasma facing components for nuclear fusion applications. The microstructure and mechanical properties of as-printed Fe9Cr were characterized using optical and electron microscopy, X-ray diffraction, and uniaxial tensile tests. As-printed Fe9Cr displayed ~25 % elongation and ultimate tensile strengths of up to 475 MPa which is comparable to similar wrought alloys. Finally, the proposed framework will allow for accelerated DED parameter optimization for novel alloy systems, as well as open the possibility for local microstructure control while simultaneously mitigating defect formation.

42 ENGINEERING↗

On residual stress analysis and microstructural evolution for stainless steel type 304 spent nuclear fuel canisters weld joint: Numerical and experimental studies

Chloride-induced stress corrosion cracking (CISCC) in the weldments of austenitic stainless steel canisters is one of the primary safety concerns during the dry storage of used nuclear fuel at Independent Spent Fuel Storage Installations in coastal areas. In order to evaluate the CISCC behavior in the canister, a 3D sequentially coupled thermo-mechanical finite element model was built to simulate the residual stresses induced by two intersecting longitudinal and circumferential multi-pass welds in austenitic stainless steel mockup canister. Weld-induced residual stresses from simulation were in good agreement with the experimental measurement results by deep-hole drilling and contour methods. Through-wall high tensile axial and hoop stresses were observed in both the fusion zone and heat affected zone (HAZ) in the longitudinal and circumferential weld, respectively. On the other hand, the microstructure within the weldments of 304 stainless steel mockup was characterized using optical microscopy, scanning electron microscopy, electron back-scattered diffraction and energy dispersive X-ray spectroscopy methods. A few amount of MnS inclusions in both the base metal and HAZ, and a lot of (Mn,Si) x O y inclusions in the fusion zone were found. Meanwhile, there is some α'-martensite in the base metal, while the martensite was reversed in the HAZ. In the fusion zone, there is a lot of δ-ferrite. The martensite reversion phenomenon was also verified by the combination of Feritscope test and thermal simulation, which could predict a martensite reversion temperature as 400C°. The welding residual stresses and microstructure analysis results could offer the instructive information for the prediction of CISCC behavior of the spent nuclear fuel canisters.

36 MATERIALS SCIENCE↗