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At least 685 records · Page 38
All sourcesNASA NTRSDOE OSTI
DOE OSTI2023

Voltage‐Modulated Untwist Deformations and Multispectral Optical Effects from Ion Intercalation into Chiral Ceramic Nanoparticles

Abstract Reconfiguration of chiral ceramic nanostructures after ion intercalation should favor specific nanoscale twists leading to strong chiroptical effects. In this work, V 2 O 3 nanoparticles are shown to have “built‐in” chiral distortions caused by binding of tartaric acid enantiomers to the nanoparticle surface. As evidenced by spectroscopy/microscopy techniques and calculations of nanoscale chirality measures, the intercalation of Zn 2+ ions into the V 2 O 3 lattice results in particle expansion, untwist deformations, and chirality reduction. Coherent deformations in the particle ensemble manifest as changes in sign and positions of circular polarization bands at ultraviolet, visible, mid‐infrared (IR), near‐IR (NIR), and IR wavelengths. The g‐ factors observed for IR and NIR spectral diapasons are ≈100–400 times higher than those for previously reported dielectric, semiconductor, and plasmonic nanoparticles. Nanocomposite films layer‐by‐layer assembled (LBL) from V 2 O 3 nanoparticles reveal cyclic‐voltage‐driven modulation of optical activity. Device prototypes for IR and NIR range problematic for liquid crystals and other organic materials are demonstrated. High optical activity, synthetic simplicity, sustainable processability, and environmental robustness of the chiral LBL nanocomposites provide a versatile platform for photonic devices. Similar reconfigurations of particle shapes are expected for multiple chiral ceramic nanostructures, leading to unique optical, electrical, and magnetic properties.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Evolution of Shock Waves in Hot-Pressed Ceramics of Boron Carbide and Silicon Carbide

In this paper we studied the evolution of shock compression waves in hot-pressed ceramics based on boron carbide and silicon carbide at a maximum compressive stress of 32 and 34 GPa, respectively, to determine the possible contribution of relaxation processes to the resistance to high-rate deformation. At a change in sample thickness from 0.5 to 8 mm, an appreciable decay of the elastic precursor was observed in boron carbide while an insignificant anomalous growth of the elastic precursor with a sample thickness was observed in the experiments with silicon carbide samples of various thickness. The measured value of the Hugoniot elastic limit of samples with a thickness of 8 mm was σ{sub HEL} = 17.2 ± 1.3 GPa for boron carbide and σ{sub HEL} = 15 ± 0.1 GPa for silicon carbide.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2023

Testing and Processing of Pre-production 325 MHz Single Spoke Resonator Power Couplers for PIP-II Project

Fundamental 325 MHz power couplers are designed, built and tested for SSR cavities in PIP-II project. Couplers should work in CW mode at power level 7.5kW w/o beam and ~15 kW with the 2 mA beam. At pre-production stage we built and tested 6 couplers, produced by CPI (FNAL) and PMB (IJCLab) and 4 more couplers will be tested soon. Two of tested couplers had TiN coated ceramic window. In warm test stand two couplers were mounted on the coupling chamber and tested in SW regime at full reflection with phase controlled by position of short and reflection insert. Couplers were tested at pulse mode (up to 25kW) and cw mode (12kW) with HV bias or without bias. Test results demonstrated that 3.5 kV DC bias completely suppresses multipactor in coupler. Vacuum activity in coupler was controlled by e-pickups and build-in vacuum gauges, located near the vacuum side of window. Power processing without DC bias was done for several couplers with and without TiN coating on ceramic window. Test results are presented and discussing in paper.

43 PARTICLE ACCELERATORS↗
DOE OSTI2026

Chemical and Radiological Compatibility Testing of 3D Printed Materials

To dramatically increase the adaptability, performance, and safety of processes in support of the Defense Waste Processing Facility (DWPF), Savannah River National Lab (SRNL) plans to perform chemical and radiological compatibility testing on a wide variety of 3D printed materials of interest. The 3D printing process provides numerous strategic operational benefits such as rapid prototyping of complex designs and geometry specific to the needs of the nuclear waste disposition process, as well as on-demand rapid prototyping and iteration with materials that aren’t as accessible through traditional manufacturing methods. Reaction chemistry in simulated waste batches can be matched closely to its radioactive counterpart, but glass reactor vessels have limitations. Vessel geometry can play a big factor in mixing transport limitations, process chemistry, and degradation reaction kinetics. In addition, additive manufacturing allows for much more detailed vessel design than traditional alternatives. Waste processing techniques in DWPF also encounter extreme chemical environments including high pH, strong acids, abrasive slurries, and significant irradiation. To meet these challenges, a matrix of various polymer, ceramic, and metal additive manufacturing materials have been exposed to a suite of chemical environments of interest as well as radioactive dose (such as gamma radiation from 60 Co) to properly test their durability under these conditions. Mass change has been monitored over a period of up to a week in these conditions, as well as added characterization for surface modification through Scanning Electron Microscopy/Electron Dispersive X-ray analysis (SEM/EDX). Further chemical characterization has been monitored through Fourier-Transform InfraRed Spectroscopy (FTIR), with planned investigation via thermal and tensile strength degradation. While the direct product of this research is identification of material(s) that can withstand specific hazardous environments encountered by the mercury water wash tank in DWPF process simulation experiments, the reference base of materials will be used for many other nuclear processes in the pursuit of rapidly developed, cost-efficient, and highly specific devices for environmental remediation and much more.

Wilson, Nathan W. [Savannah River National Laborat↗
DOE OSTI2023

TESTING AND PROCESSING OF PRE-PRODUCTION 325 MHZ SINGLE SPOKE RESONATOR POWER COUPLERS FOR PIP-II PROJECT

Fundamental 325 MHz power couplers are designed, built and tested for SSR cavities in PIP-II project [1]. Couplers should work in CW mode at power level 7.5kW w/o beam and ~15 kW with the 2 mA beam. At pre-production stage we built and tested 6 couplers, produced by CPI (FNAL) and PMB (IJCLab) and 4 more couplers will be tested soon. Two of tested couplers had TiN coated ceramic window. In warm test stand two couplers were mounted on the coupling chamber and tested in SW regime at full reflection with phase controlled by position of short and reflection insert. Couplers were tested at pulse mode (up to 25kW) and cw mode (12kW) with HV bias or without bias. Test results demonstrated that 3.5 kV DC bias completely suppresses multipactor in coupler. Vacuum activity in coupler was controlled by e-pickups and build-in vacuum gauges, located near the vacuum side of window. Power processing without DC bias was done for several couplers with and without TiN coating on ceramic window. Test results are presented and discussing in paper.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗
DOE OSTI2018

Flake Formation in Phase Layers of a Cutting Ceramic

Flake formation (cracking) is observed in inserts of untreated cutting ceramic and also during diffusional strengthening of the inserts’ surface layer by nitrogen on heating in a muffle furnace to 450–500°C, with the creation of γ-phase (a protective layer), the removal of carbon from the atomic cells, and the formation of titanium nitride. Heat-treatment conditions for inserts of cutting ceramic are established such that the flake content at their surface is reduced. Treatment to prevent flake formation is proposed: heating in a sealed muffle furnace with a nitrogen atmosphere to 250–280°C at a pressure of 0.25 MPa. In this process, the titanium carbide at the surface of the inserts is converted to titanium nitride as a result of carbon diffusion, with the formation of a protective γ-phase layer. By removing carbon from the surface layer of the inserts and ensuring the diffusion of nitrogen into the cutting ceramic, with the formation of titanium nitride in the γphase, the durability and performance of the inserts are improved, along with their mechanical properties.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Scalable, Infiltration-Free Ceramic Matrix Composite (SIF-CMC) manufacturing for Molten Salt Receiver: Investigation of particle-loaded preceramic resin

Due to their unique combination of high temperature, corrosion resistance, and toughness, Ceramic Matrix Composites (CMC) are the optimal materials to be used in the next generation of Concentrated Solar Power (CSP), which will operate at working temperatures up to 800 °C. However, today, CMC is too costly to be used in CSP applications due to its complex manufacturing process based on repeated infiltration-pyrolysis cycles. To solve this issue, PARC is developing a scalable, infiltration-free method (SIF) to manufacture CMC, which can reduce the production cost, increase batch consistency, and leverage all of the intrinsic advantages of current CMCs. The key to the SIF method is using a flowable preceramic resin with high loading of functional components. The formulation impregnates the fiber during curing and leads to high-density, low-shrinkage parts upon pyrolysis. In this paper, we demonstrate a proof-of-concept of the SIF process and report the relationships between key process parameters in the manufacturing process: functional material loading in the resin vs. resin’s flowability and morphology changes upon pyrolysis.

ceramic matrix composite, concentrated solar power↗
DOE OSTI2020

Design of functional composite and all-inorganic nanostructured materials via infiltration of polymer templates with inorganic precursors

Robust and efficient approaches for the synthesis of materials with structure, porosity, and composition controlled at the nanoscale are highly important for a wide range of applications. Polymer templates are promising platforms to achieve such control. The self-assembly process of polymers provides access to diverse structures that can serve as templates for the deposition of inorganic materials. By infiltrating metal precursors from gas or liquid phases, using sequential infiltration synthesis (SIS) or swelling-based infiltration (SBI), respectively, into the polymer templates, one can create finely-tuned texturing of the surface films and bulk materials. In this review, we outline the specifics and dynamics of the polymer infiltration process and characterize the structure and properties of the synthesized materials. Finally, we highlight recent progress in implementing polymer infiltration-based nanoporous ceramics for many applications, including sensors, antireflective coatings, oil-absorbing foams, nanolithographic patterns, and catalytic materials.

Berman, Diana↗
DOE OSTI2016

High temperature x-ray micro-tomography

There is increasing demand for 3D micro-scale time-resolved imaging of samples in realistic - and in many cases extreme environments. The data is used to understand material response, validate and refine computational models which, in turn, can be used to reduce development time for new materials and processes. Here we present the results of high temperature experiments carried out at the x-ray micro-tomography beamline 8.3.2 at the Advanced Light Source. The themes involve material failure and processing at temperatures up to 1750°C. The experimental configurations required to achieve the requisite conditions for imaging are described, with examples of ceramic matrix composites, spacecraft ablative heat shields and nuclear reactor core Gilsocarbon graphite.

43 PARTICLE ACCELERATORS↗
DOE OSTI2022

Electrochemical Aging and Halogen Oxides Formation on Multiwalled Carbon Nanotubes and Fe 3 O 4 @g-C 3 N 4 Coated Conductive Membranes

Electrochemical membrane filtration is widely reported to enhance water contaminants' degradation or rejection via anodic oxidation or cathodic repulsion. Despite their advances, electrochemical membranes or electrocatalysts often suffer from corrosion or passivation, especially under strong electrode potentials or reactions. Moreover, the formation of toxic byproducts, such as chlorinated organic compounds and oxyhalides (e.g., ClO 4 - ) is another major concern. This study investigated the membrane aging processes of two types of conductive membranes, multiwalled carbon nanotubes (MWCNTs) and ferrite/graphitic carbon nitride hybrids (Fe 3 O 4 @g-C 3 N 4 ) coated on ceramic membranes. Under high current densities (~ 20 mA∙cm -2 ) with anodic potentials (~10 V), MWCNTs and Fe 3 O 4 @g-C 3 N 4 catalysts underwent evident oxidation as indicated by an increase of the intensity ratio of the Raman spectral bands (I D /I G ) and charge transfer resistance (R ct ) of two electrochemical membranes. Under variations of electrode potentials, chloride or bromide were shown to be oxidized to bromate (BrO 3 - ) and chlorate (ClO 3 - ) at levels of 1-10 mmol∙L -1 . The formation of BrO 3 - and ClO 3 - was dependent on the solution pH, current densities (1-20 mA∙cm -2 ), and initial concentrations of Br or Cl ions. Finally, to warrant a safe and rational design and operation of electrochemically reactive membrane processes, membrane aging and toxic byproduct's formation deserve careful characterization under relevant water filtration environments.

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

Exploring the structural uniformity and integrity of protonic ceramic thin film electrolyte using wet powder spraying

Thin protonic ceramic electrolyte contributes to lower ohmic resistance and enhances electrochemical performance of protonic ceramic electrochemical cells. However, manufacturing of large-scale thin electrolyte remains a challenge. Wet powder spraying is an attractive technique to deposit <10 µm thin electrolyte when advanced atomizing techniques and optimized spraying process are integrated. Here ultrasonic atomization is integrated in the wet powder spray technique to reduce the thickness of electrolyte. Moreover, a parametric study is conducted to optimize the wet powder spray process to deposit uniform and crack-free electrolyte film. It is illustrated that tuning of solid loading rates and spray passes can affect the morphology of the as-sprayed electrolyte film, enabling the structural compactness of the sintered electrolyte layer. To maintain chemical stability of the electrolyte layer during sintering, effect of sintering temperature is further investigated to produce a physically thin, structurally dense, and chemically homogeneous electrolyte layer. The protonic ceramic electrochemical cells fabricated with optimized spraying and sintering parameters demonstrate excellent performance under both fuel cell and electrolysis modes. In addition, the cells exhibit remarkable structural integrity during redox and long-term stability tests.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Dry in-pile fracture test (DRIFT) for separate-effects validation of ceramic fuel fracture models

Fracture is an important component of nuclear fuel behavior, and significant efforts have been invested into developing fuel performance models that are capable of accurately representing fracture. Usable data on the process of fracture propagation in nuclear fuel under realistic service conditions are very limited. To address this need, a series of separate-effects experiments were developed and performed at Idaho National Laboratory's Transient Reactor Test (TREAT) facility. These experiments employ a heat sink to radially remove heat from the fuel in a manner that approximates the effect of coolant in an operating light-water reactor (LWR). The test holder for these experiments is known as the Dry In-pile Fracture Test (DRIFT). A series of experiments employing DRIFT and TREAT were performed to provide data on the extent and nature of fracture in fresh fuel at various points during a ramp to full power. Novel aspects of these experiments include the way they employ a heat sink to replicate steady-state LWR conditions, as well as the use of fiber optic sensors for in-reactor thermal instrumentation. Details on the development of this experiment, experimental conditions, and resulting data (including in situ thermal measurements and post-irradiation imaging of fracture) are provided in this work. LWR-equivalent powers ranging from 10 to 25 kW/m were tested using this apparatus. Cracking was visible at all power levels, with increasing cracking extent as the power level increased, although there was little difference in the cracking between the two highest-power tests, which had LWR-equivalent powers of 20 and 25 kW/m.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2020

Ion irradiation and modification: The role of coupled electronic and nuclear energy dissipation and subsequent nonequilibrium processes in materials

Understanding material responses to energy deposition from energetic charged particles is important for defect engineering, ion-beam processing, ion-beam analysis and modification, geologic aging, space exploration, and nuclear applications. As an incident ion penetrates a solid, its energy is transferred to electrons and to atomic nuclei of the solid. Much of this electronic energy deposition is subsequently transferred to the atomic structure via electron–phonon (e–ph) coupling, leading to local inelastic thermal spikes in which energy dissipation is influenced by the local environment. In addition, intense ionization can lead to high densities of localized electronic excitations in wide-bandgap materials and ceramics that can affect defect dynamics and atomic mobility. Specifically, energy exchange between electrons and atomic nuclei, along with localized electronic excitations, can lead to substantial competitive (ionization-induced annealing), additive (both electronic and nuclear energy depositions contributing to damage production), and synergistic (more damage than the sums of separate damage processes) effects. Although nonmonotonic effects of the e–ph coupling strength and athermal processes are demonstrated for pre-existing defects and residual damage during ion–solid interactions, there is limited understanding of when such electronic effects must be considered in atomic-scale models of damage production and evolution in a broad variety of materials. Complex ceramics and chemically disordered solid solution alloys with different constituent elements allow a systematic evaluation of defect dynamics and irradiation performance with increasing complexity. Current knowledge regarding tuning of bonding characteristics and chemical disorder to control atomic-level dynamics is reviewed. Although a lack of fundamental understanding obstructs the advancement of reliable predictions for ion beam material modification, it highlights challenges and opens research opportunities. Insights into the complex electronic and atomic correlations with extreme energy deposition will strengthen our ability to design materials and predict ion-irradiation-induced damage in a radiation environment, and they may pave the way to better control fundamental processes and design new material functionalities for advanced technologies.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Advanced waste form and Melter development for treatment of troublesome high-level wastes

A number of waste components in US defense high level radioactive wastes (HLW) have proven challenging for current Joule heated ceramic melter (JHCM) operations and have limited the ability to increase waste loadings beyond already realized levels. Many of these “troublesome" waste species cause crystallization in the glass melt that can negatively impact product quality or have a deleterious effect on melter processing. Recent efforts at US Department of Energy laboratories have focused on understanding crystallization behavior within HLW glass melts and investigating approaches to mitigate the impacts of crystallization so that increases in waste loading can be realized. Advanced glass formulations have been developed to highlight the unique benefits of next-generation melter technologies such as the Cold Crucible Induction Melter (CCIM). Crystal-tolerant HLW glasses have been investigated to allow sparingly soluble components such as chromium to crystallize in the melter but pass out of the melter before accumulating.The Hanford site AZ-101 tank waste composition represents a waste group that is waste loading limited primarily due to high concentrations of Fe 2 O 3 (also with high Al 2 O 3 concentrations). Systematic glass formulation development utilizing slightly higher process temperatures and higher tolerance to spinel crystals demonstrated that an increase in waste loading of more than 20% could be achieved for this waste composition, and by extension higher loadings for wastes in the same group. An extended duration CCIM melter test was conducted on an AZ-101 waste simulant using the CCIM platform at the Idaho National Laboratory (INL). The melter was continually operated for approximately 80 hours demonstrating that the AZ-101 high waste loading glass composition could be readily processed using the CCIM technology. The resulting glass was close to the targeted composition and exhibited excellent durability in both the as poured state and after being slowly cooled according to the canister centerline cooling (CCC) profile. Glass formulation development was also completed on other Hanford tank wastes that were identified to further challenge waste loading due to the presence of appreciable quantities (>750 g) of plutonium in the waste tanks. In addition to containing appreciable Pu quantities, the C-102 waste tank and the 244-TX waste tank contain high concentrations of aluminum and iron, respectively that will further challenge vitrification processing. Glass formulation testing also demonstrated that high waste loadings could be achieved with these tank compositions using the attributes afforded by the CCIM technology.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2019

Nanoscale stacking fault–assisted room temperature plasticity in flash-sintered TiO 2

Ceramic materials have been widely used for structural applications. However, most ceramics have rather limited plasticity at low temperatures and fracture well before the onset of plastic yielding. The brittle nature of ceramics arises from the lack of dislocation activity and the need for high stress to nucleate dislocations. Here, we have investigated the deformability of TiO 2 prepared by a flash-sintering technique. Our in situ studies show that the flash-sintered TiO 2 can be compressed to ~10% strain under room temperature without noticeable crack formation. The room temperature plasticity in flash-sintered TiO 2 is attributed to the formation of nanoscale stacking faults and nanotwins, which may be assisted by the high-density preexisting defects and oxygen vacancies introduced by the flash-sintering process. Distinct deformation behaviors have been observed in flash-sintered TiO 2 deformed at different testing temperatures, ranging from room temperature to 600°C. Potential mechanisms that may render ductile ceramic materials are discussed.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Reliability and Durability Testing of Glass Ceramic Seals for Praxair’s Oxygen Transport Membranes

Praxair has been developing Oxygen Transport Membrane (OTM) systems for the efficient conversion of natural gas to syngas which can subsequently be used in chemical synthesis, generation of industrial gases (H2, CO) or synthesis of liquid fuels. One of the technical barriers for commercialization of this technology is the reliability of key components of OTM systems – Seals and Membranes. Praxair has been testing these components at the process conditions expected for commercial systems. However, long-term durability data is currently limited and is not sufficiently available to make well informed predictions of OTM reliability which represents one of the major risks that could prevent the technology from being fully commercialized. Pacific Northwest National Laboratory (PNNL) has been developing high temperature seals and ceramic membranes for applications similar to OTM systems such as Solid Oxide Fuel Cells. The goal of the cooperative development between Praxair and PNNL is to generate long-term data such that there is sufficient confidence in the OTM seal and membrane reliability predictions to enable the process technology to be fully commercialized.

03 NATURAL GAS↗
DOE OSTI2025

Accelerated Fuel Qualification of Fast Modular Reactor Fuel in a Thermal Reactor: Modeling and Simulation Paired with Irradiation Testing

The accelerated fuel qualification (AFQ) methodology is applied by simulating accelerated fuel tests of the General Atomics Electromagnetic Systems’ fuel system for its 44-MW(electric) gas-cooled, fast-spectrum fast modular reactor (FMR). This fuel is comprised of UO 2 pellets in SiGA® cladding, a silicon carbide ceramic matrix composite. Fast reactors, like the FMR, offer many benefits, including high fuel utilization and flexibility, but may require a lengthy material design process if tests are performed using fast neutron irradiation alone. A thermal neutron irradiation can instead be used to rapidly test how well key components of the current material models extend to high burnup. Thermal neutrons produce a different radial power distribution within the pin than fast neutrons. However, the temperature and burnup values for the two neutron types are comparable, and the differences between the simulated fuel responses are relatively small, demonstrating the weak sensitivity of the physics-based fuel model calculations on the neutron type and the irradiation rate. Furthermore, the deformation of the SiGA cladding saturates after about 1 displacement per atom for both neutron spectra. In an accelerated fuel test, the irradiation time required to reach the target fuel burnup can be reduced by a factor of 3 by using a small rodlet with a 45% smaller pellet diameter while maintaining the same linear power. Therefore, the time for data collection up to high burnup can be significantly reduced while maintaining the same temperature profile, which largely determines the material response. Tests of fuel rodlets of standard and compact size will be carried out in the Idaho National Laboratory’s Advanced Test Reactor (ATR), including full size and compact rodlets with varying gap sizes. By applying physics-based mechanistic modeling and simulation in accordance with the AFQ methodology, this type of compact rodlet testing in a thermal test reactor captures the necessary phenomena to test fuel material models up to high burnup and to simulate the expected impact of fast neutron radiation on the fuel in FMR operations. Finally, this approach to testing fast reactor fuels in existing thermal test reactors, paired with advanced physics-based mechanistic modeling and simulation, is expected to be applicable to a range of advanced fuels and will decrease the overall fuel qualification timeframe from decades to years.

Advanced test reactor (ATR)↗
DOE OSTI2018

Scalable measurements of tow architecture variability in braided ceramic composite tubes

Abstract The performance of braided ceramic matrix composites has been shown to depend on the spatial arrangement of tows; therefore, a new class of tools is required to measure irregularities in the composite architecture for components with intricate geometries. We report a scalable and robust reconstruction technique built upon stereoscopic digital image correlation that is able to efficiently measure the position of tows in arbitrarily shaped composites. This method was applied to triaxially braided ceramic matrix composite tubes intended for use as nuclear fuel cladding, which revealed both long‐range “systematic” tow packing defects associated with the manufacturing process and short‐range “intrinsic” defects due to the braid architecture. These findings suggested that the character of tow spacing variation in braided composite tubes was substantially more complex than in planar woven composites. These measurements are expected to lead to improved processing of braided composites and to facilitate the design of statistically representative virtual specimens for finite element modeling.

Heim, Frederick M.↗