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296 records · Page 17
All sourcesNASA NTRSDOE OSTI
DOE OSTI2023

Bismuth-Polyoxocation Coordination Networks: Controlling Nuclearity and Dimension-Dependent Photocatalysis

Bismuth-oxocluster nodes for metal–organic frameworks (MOFs) and coordination networks/polymers are less prolific than other families featuring zinc, zirconium, titanium, lanthanides, etc. However, Bi 3+ is non-toxic, it readily forms polyoxocations, and its oxides are exploited in photocatalysis. This family of compounds provides opportunity in medicinal and energy applications. Here, we show that Bi node nuclearity depends on solvent polarity, leading to a family of Bi x -sulfonate/carboxylate coordination networks with x = 1–38. Larger nuclearity-node networks were obtained from polar and strongly coordinating solvents, and we attribute the solvent’s ability to stabilize larger species in solution. Here, the strong role of the solvent and the lesser role of the linker in defining node topologies differ from other MOF syntheses, and this is due to the Bi 3+ intrinsic lone pair that leads to weak node–linker interactions. We describe this family by single-crystal X-ray diffraction (eleven structures), obtained in pure forms and high yields. Ditopic linkers include NDS (1,5-naphthalenedisulfonate), DDBS (2,2'-[biphenyl-4,4'-diylchethane-2,1-diyl] dibenzenesulphonate), and NH 2 -benzendicarboxylate (BDC). While the BDC and NDS linkers yield more open-framework topologies that resemble those obtained by carboxylate linkers, topologies with DDBS linkers appear to be in part driven by association between DDBS molecules. An in situ small-angle X-ray scattering study of Bi 38 -DDBS reveals stepwise formation, including Bi 38 -assembly, pre-organization in solution, followed by crystallization, confirming the less important role of the linker. We demonstrate photocatalytic hydrogen (H 2 ) generation with select members of the synthesized materials without the benefit of a co-catalyst. Band gap determination from X-ray photoelectron spectroscopy (XPS) and UV–vis data suggest the DDBS linker effectively absorbs in the visible range with ligand-to-Bi-node charge transfer. In addition, materials containing more Bi (larger Bi 38 -nodes or Bi 6 inorganic chains) exhibit strong UV absorption, also contributing to effective photocatalysis by a different mechanism. All tested materials became black with extensive UV–vis exposure, and XPS, transmission electron microscopy, and X-ray scattering of the black Bi 38 -framework suggest that Bi o is formed in situ, without phase segregation. This evolution leads to enhanced photocatalytic performance, perhaps due to increased light absorption.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2021

Interaction of radio frequency waves with cylindrical density filaments: scattering and radiation pressure

The propagation of radio-frequency (RF) waves in tokamaks can be affected by filamentary structures, or blobs, that are present in the edge plasma and the scrape-off layer. The difference in the permittivity between the surrounding plasma and interior of a filament leads to reflection, refraction and diffraction of the waves. This, in turn, can affect the power flow into the core of the plasma and reduce the efficiency of heating and/or current generation. The scattering of RF waves, lower hybrid, helicon and ion cyclotron waves, by a single cylindrical filament, embedded in a background plasma, is studied using a full-wave analytical theory developed previously (Ram & Hizanidis, Phys. Plasmas , vol. 23, 2016, 022504). The theory assumes that the plasma in and around a filament is homogeneous and cold. A detailed scattering analysis reveals a variety of common features that exist among the three distinctly different RF waves. These common attributes can be inferred intuitively based on an examination of the cold plasma dispersion relation. The physical intuition is a useful step to understanding experimental observations on scattering, as well as results from simulations that include general forms of edge plasma turbulence. While a filament can affect the propagation of RF waves, the radiation force exerted by the waves can influence the filament. The force on a filament is determined using the Maxwell stress tensor. In 1905, Poynting was the first to evaluate and measure the radiation force on an interface separating two different dielectric media (Poynting, London Edinburgh Dublin Philos. Mag. J. Sci. , vol. 9, 1905, pp. 393–406). For ordinary light propagating in vacuum and incident on a glass surface, Poynting noted that the surface is ‘pulled’ towards the vacuum. In a magnetized cold plasma, there are two independent wave modes. Even if only one of these modes is excited by an RF antenna, a filament will couple power to the other mode: a consequence of electromagnetic boundary conditions. This facet of scattering has consequences on the radiation force that go beyond Poynting's seminal contribution. The direction of the force depends on the polarization of the incident wave and on the mode structure of the waves inside and in the vicinity of a filament. It can either pull the filament toward the RF source or push it away. For slow lower hybrid waves, filaments with densities greater than the ambient density are pulled in, while filaments with lower densities are pushed out, thereby enhancing the density in front of the antenna. In the case of fast helicon and ion cyclotron waves, the direction of the force depends on the plasma and wave parameters; in particular, on the ambient density. The radiation force, in all three frequency ranges, is large enough to affect the motion of a filament and could be measured experimentally. This also suggests the possibility of modifying the edge turbulence using RF waves.

Physics↗
DOE OSTI2022

Interaction of radio frequency waves with cylindrical density filaments -- scattering and radiation pressure

The propagation of radio-frequency (RF) waves in tokamaks can be affected by filamentary structures, or blobs, that are present in the edge plasma and the scrape-off layer. The difference in the permittivity between the surrounding plasma and interior of a filament leads to reflection, refraction and diffraction of the waves. This, in turn, can affect the power flow into the core of the plasma and reduce the efficiency of heating and/or current generation. The scattering of RF waves, lower hybrid, helicon and ion cyclotron waves, by a single cylindrical filament, embedded in a background plasma, is studied using a full-wave analytical theory developed previously (Ram & Hizanidis, Phys. Plasmas, vol. 23, 2016, 022504). The theory assumes that the plasma in and around a filament is homogeneous and cold. A detailed scattering analysis reveals a variety of common features that exist among the three distinctly different RF waves. These common attributes can be inferred intuitively based on an examination of the cold plasma dispersion relation. The physical intuition is a useful step to understanding experimental observations on scattering, as well as results from simulations that include general forms of edge plasma turbulence. While a filament can affect the propagation of RF waves, the radiation force exerted by the waves can influence the filament. The force on a filament is determined using the Maxwell stress tensor. In 1905, Poynting was the first to evaluate and measure the radiation force on an interface separating two different dielectric media (Poynting, London Edinburgh Dublin Philos. Mag. J. Sci., vol. 9, 1905, pp. 393–406). For ordinary light propagating in vacuum and incident on a glass surface, Poynting noted that the surface is ‘pulled’ towards the vacuum. In a magnetized cold plasma, there are two independent wave modes. Even if only one of these modes is excited by an RF antenna, a filament will couple power to the other mode: a consequence of electromagnetic boundary conditions. This facet of scattering has consequences on the radiation force that go beyond Poynting's seminal contribution. The direction of the force depends on the polarization of the incident wave and on the mode structure of the waves inside and in the vicinity of a filament. It can either pull the filament toward the RF source or push it away. For slow lower hybrid waves, filaments with densities greater than the ambient density are pulled in, while filaments with lower densities are pushed out, thereby enhancing the density in front of the antenna. In the case of fast helicon and ion cyclotron waves, the direction of the force depends on the plasma and wave parameters; in particular, on the ambient density. The radiation force, in all three frequency ranges, is large enough to affect the motion of a filament and could be measured experimentally. This also suggests the possibility of modifying the edge turbulence using RF waves.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗
DOE OSTI2026

Fragile-to-strong transition in liquid As 2 S 3 under pressure: The effect of melt metallization

The well-known classification of glass-forming melts into fragile and strong liquids has several notable exceptions, including water, silica, and certain phase-change materials (PCMs). These exceptional fluid systems exhibit a fragile-to-strong transition (FST) upon cooling: a transformation from a high-temperature liquid with fast atomic dynamics, low viscosity, and low flow activation energy, to a viscous supercooled melt with high energy barriers near the glass transition temperature T g . This behavior is critically important for non-volatile memories, photonic tensor cores, reconfigurable metamaterials, and other devices, that use PCMs, enabling nanosecond-scale crystallization in the fragile regime and long data retention in the strong regime near or below T g . A significant structural transformation is expected between these two viscosity regimes, along with a semiconductor-metal (SC-M) transition upon heating, driven by high internal pressure and associated density increase. By applying high external pressure to the canonical low-conducting chalcogenide melt As 2 S 3 , we observed both the FST and the SC-M transition, occurring simultaneously within the same domain of the P, T−phase space. These findings suggest that the FST is not limited to a few exceptional liquids but is a common phenomenon, at least in systems that exhibit melt metallization within specific regions of their P, T−phase diagrams.

first-principles molecular dynamics↗
DOE OSTI2021

Suppression of the vacuum space-charge effect in fs-photoemission by a retarding electrostatic front lens

The performance of time-resolved photoemission experiments at fs-pulsed photon sources is ultimately limited by the e–e Coulomb interaction, downgrading energy and momentum resolution. Here, we present an approach to effectively suppress space-charge artifacts in momentum microscopes and photoemission microscopes. A retarding electrostatic field generated by a special objective lens repels slow electrons, retaining the k-image of the fast photoelectrons. The suppression of space-charge effects scales with the ratio of the photoelectron velocities of fast and slow electrons. Fields in the range from -20 to 01100 V/mm for E kin = 100 eV to 4 keV direct secondaries and pump-induced slow electrons back to the sample surface. Ray tracing simulations reveal that this happens within the first 40 to 3 μm above the sample surface for E kin = 100 eV to 4 keV. An optimized front-lens design allows switching between the conventional accelerating and the new retarding mode. Time-resolved experiments at E kin = 107 eV using fs extreme ultraviolet probe pulses from the free-electron laser FLASH reveal that the width of the Fermi edge increases by just 30 meV at an incident pump fluence of 22 mJ/cm2 (retarding field -21 V/mm). For an accelerating field of +2 kV/mm and a pump fluence of only 5 mJ/cm 2 , it increases by 0.5 eV (pump wavelength 1030 nm). At the given conditions, the suppression mode permits increasing the slow-electron yield by three to four orders of magnitude. The feasibility of the method at high energies is demonstrated without a pump beam at E kin = 3830 eV using hard x rays from the storage ring PETRA III. The approach opens up a previously inaccessible regime of pump fluences for photoemission experiments.

47 OTHER INSTRUMENTATION↗
DOE OSTI2024

Effect of Heat Treatment on Microstructure and Mechanical Property of 316L Stainless Steel Produced by Laser Powder Bed Fusion

The advanced non-light water reactor designs (Gen IV reactors), including molten salt/ very high temperature/ sodium-cooled and lead-cooled fast reactors, typically operate at higher temperatures and more extreme radiation conditions than light water reactors. An intrinsic part of the deployment and progress of Gen IV reactor designs is selecting the most suitable structural material for a specific application. Additive manufacturing (AM), a fairly new process of making physical, three-dimensional objects from a computer design file, is going to completely change the way of design, build and certify nuclear systems. It offers a range of opportunities to produce complex geometries from existing materials, offers new routes for processing of previously difficult to process materials, allows for design of new high-performance materials, and finally facilitates hybridization of dissimilar materials. This emerging technology has successfully produced cars, wind turbine blade molds and even live cells. It could also open up big opportunities for the nuclear industry to quickly deploy technologies at a fraction of the cost. So far, AM techniques have been preliminarily applied in the field of nuclear reactors, including the classical parts such as the pressure vessel of a small reactor with 508-III steel, the bottom nozzle of a fuel assembly with 304L steel, the fuel cladding with zirconium alloy and the integrated impeller of a pump and the multi-channel valve body with 316L steel [6,7]. The AM applications for operating nuclear reactors started in auxiliary plant components and have slowly migrated to metallic reactors and core components, but many of these are not safety critical components. Although many parts used for nuclear reactors have been fabricated by AM techniques, practical applications in engineering are still a long way off due to the uncertainty factors focused on the processing, material properties, analysis methods and application standards, which feeds the safety and life-cycle of the nuclear reactor. Due to rapid, repeated heating and cooling during production, a high dislocation density was present in the AM material. This microstructure feature is unstable at elevated temperature while high temperature is one of the typical operation environments for nuclear reactors. Thus, it is important to understand the thermal effect on the microstructure of AM material. The objectives of this study are to investigate the effect of heat treatment on the microstructure and mechanical properties of 316L stainless steel produced by laser powder bed fusion additive manufacturing, and to determine an appropriate heat treatment practice that will be applied to the lightweight AM lattice-structured material with the same chemistry. The heat treatment study consisted of annealing the samples at a temperature range of 800 to 1200 oC with a 50 oC increment for different times (1-24 hours), followed by vacuum or air cooling. Microstructural characterization was carried out by Scanning Electron Microscope (SEM). Grain size and crystallographic orientation were investigated by Electron Backscatter Diffraction (EBSD). Vickers hardness tests with a 0.5 kg load were employed to determine the hardness of samples after different heat treatments. After heat treatment, the random crystallographic orientation was preserved, and the volume fraction of high-angle grain boundaries (grain boundary misorientation =15 oC) remained the same. The dislocation density decreased with annealing temperature due to recovery. The fine subgrain structures in the as-printed specimen were quite stable up to 1200 oC. Minimal recrystallization was observed up to 1200 oC. Recrystallization initiated only after 8.5 hours at 1200 oC. The SEM images did not show obvious dependence of microstructure on cooling rate. The hardness of the specimens decreased with increasing annealing temperature as a result of the decrease in dislocation density. It is interesting to note that the AM material showed very similar hardness to the wrought material when annealing at similar temperature, although the microstructures are very different. Annealing at 1050 oC for 1 hour followed by air cooling was selected as the heat treatment procedure for the lattice designed lightweight AM 316L material.

36 MATERIALS SCIENCE↗
DOE OSTI2025

A 28 nm multiply-accumulate ASIC architecture for on-chip data compression in MHz frame rate X-ray and electron pixel detectors

Modern X-ray detector systems urgently require compact, efficient, and fast data compression schemes to handle the transmission of big data from pixel arrays, enabling frame rates in the MHz regime. Here, in this work, a data compression ASIC that implements a streaming fixed-length lossy compression scheme is introduced and analyzed, proving the feasibility and benefits of on-chip compression. The compression scheme utilizes a vector matrix product logic, which performs a number of floating-point multiplications, additions, and accumulations. The logic is verified, synthesized, and shown to fit in the area resource available for the X-ray detector under study, which comprises 192 × 168 pixels each of 12-bit width, and having a total area of 20 mm× 20 mm, about 2 mm× 20 mm of which are available for the digital logic. Several system architectures, precisions, and compression ratios ranging from 100 to 250 were analyzed to pave the way for on-chip fixed-length compression (e.g., principal component analysis, singular value decomposition) and data reduction (e.g., azimuthal integration) for X-ray and electron detectors.

Data compression↗