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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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At least 289 records · Page 16
All sourcesNASA NTRSDOE OSTI
DOE OSTI2020

Glass waste form options for rare-earth fission products from electrochemical reprocessing

Herein, we describe a first-of-a-kind study where lead tellurite (Pb-Te-O), iron phosphate (Fe-P-O), and lanthanide aluminoborosilicate (LABS) waste forms are evaluated for treating and/or immobilizing waste streams containing high rare-earth (RE) content, e.g., RECl 3 , REOCl, and/or REO x . Results from this study show that NdOCl can be immobilized in 78TeO 2 -22PbO glass at up to 10 mass%. Higher loadings of up to 15 mass% were demonstrated, but with a small fraction of crystallization. Two Fe-P-O glasses produced from either RECl 3 (RE = Nd,Ce) or NdOCl revealed products with very similar properties, demonstrating that the phosphate process can be used to chlorinate a variety of RE-containing waste streams. Two LABS glasses produced from Nd 2 O 3 or NdOCl showed similar properties, but the LABS-NdOCl glass did have some residual Cl present. Characterization is provided for all waste forms including chemical analysis, X-ray diffraction, and bulk density.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2020

Sol–gel synthesis of iodosodalite precursors and subsequent consolidation with a glass binder made from oxides and sol–gel routes

Radioiodine accumulates in aqueous solutions and off-gas streams during nuclear fuel reprocessing due to its solubility in aqueous solutions and volatility, respectively. Additionally, radioiodine is highly mobile in geological environments and iodine-129 has been found to be one of the largest long-term contributors to chronic dose to humans in scenarios of radionuclide migration from geological repositories. Most of the radioiodine can be captured during fuel reprocessing in off-gas streams using solid sorbents and scrubbing solutions. Once iodine is captured, it must be stored in a durable form for eventual disposal. Iodosodalite has been investigated as a waste form for radioiodine, however these synthesis processes typically result in mixed products and iodine volatilization during consolidation. Therefore, this paper proposes a novel approach to synthesizing iodosodalite utilizing a sol-gel method. This method was chosen to lower processing temperatures and improve product yield. Preliminary experiments conducted to determine the viability of this synthetic method are presented. Additionally, consolidation of sol-gel derived iodosodalite with a glass-binder was explored using three different methods: 1) incorporating the glass-binder during gel preparation using alkoxide precursors; 2) separately preparing the glass binder using a sol-gel method; and 3) separately preparing the glass-binder using a melt-quench technique. Glass-bonded iodosodalite was successfully synthesized using these novel sol-gel approaches.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Feldspar-based CaO–K 2 O–Na 2 O–BaO silicate glass sealant for solid oxide fuel cells

Sealants have been widely used in solid oxide fuel cells (SOFCs), and glass sealants have shown considerable potentials due to their low leakage rate. In this paper, we report a type of feldspar-based glass sealant, mainly composed of CaO-K 2 O-Na 2 O-BaO, with a coefficient of thermal expansion (CTE) of 10.11×10 -6 k -1 , a glass transition temperature at 528°C, and a softening temperature at 573°C. Using this sealant to seal anode-supported SOFCs, the open-circuit voltage (OCV) remains at 1.08V after five thermal cycles and 50-hour aging at 750°C, close to the theoretical OCV value. The SEM and EDS reveal stable interface between the glass sealant and the anode, indicating excellent performance of the CaO-K 2 O-Na 2 O-BaO glass sealant for SOFC sealing applications.

25 ENERGY STORAGE↗
DOE OSTI2024

Sources of Li isotope bias during SIMS analysis of standard glasses

The 7 Li/ 6 Li ratios in fourteen USGS, MPI-DING, and NIST glass reference materials (RMs) were analyzed by LG-SIMS to assess compositional matrix effects, evaluate RM δ 7 Li homogeneity, and calculate the useful yield of lithium in silicate glasses. The analyzed RMs cover a range of SiO 2 contents from 45.5 to 75.6% (komatiite to rhyolite), the largest compositional range yet evaluated for δ 7 Li matrix effects. We observe a matrix-induced bias (matrix effect) of up to 18‰ over the studied range that linearly correlates with SiO 2 content, demonstrating that SiO 2 content is a critical factor that must be considered when using silicate glasses to standardize for silicate samples of unknown δ 7 Li composition. All RMs were found to be sufficiently reproducible to aid in standardization of variable SiO 2 contents and appear isotopically homogeneous at the precision of our measurements. Lithium ionizes very efficiently in these RMs, with measurable yields >5% in all fused-rock RMs and >15% in low SiO 2 fused-rock RMs measured at high beam intensities. Finally, fused-rock RMs ionize lithium 2-3x more efficiently than synthetic glass RMs, which may be related to differences in major oxide chemistry and the reduced nature of the synthetic glasses relative to their fused counterparts.

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

Characterizing major and trace element compositions in fallout melt glass from a near-surface nuclear test

We report the chemical and isotopic compositions of fallout melt glasses from nuclear tests contain a range of information constraining the physical conditions within the fireball and the mechanisms of fallout formation but historic studies tended to exclude the behavior of stable major and trace elements. Here, we present a large study specifically focused on major and trace element relationships within a population of macroscale fallout samples from a single event. We interpret these data to better constrain how fallout melt glass formation in near surface environments is influenced by that environment and demonstrate how major and trace element abundances can provide useful insights into chemical processes within the fireball. Data confirm that the uranium in the fallout glass population derives from two isotopically distinct endmembers: isotopically enriched uranium (presumably from the weapon), and natural composition uranium that may be a combination of anthropogenic and environmental materials from within the blast zone. The similarity between major and trace element concentrations in fallout and corresponding local soils from the event site confirm the local soils as the most probable source of entrained material into the fireball and the source of carrier material into which the bomb vapor was incorporated. The lack of correlation between major and trace element abundances with size indicates that volatility driven processes, such as condensation from the fireball, do not control the composition of macroscale fallout melt glass. Although the fallout has major and trace element chemical characteristics broadly similar to those of the local, associated soils, some systematic differences are observed between the two populations. Fallout melt glass is depleted in volatile elements such as K, Na, Tl and Pb, consistent with heating to temperatures above ~1000 °C for 3-10 s. This is supported by the results of laser heating experiments performed on rhyolitic soil at temperatures (1600-2200 °C) and timescales (1-120 s) that are broadly relevant to fallout formation conditions. Relative enrichments of metals such as Cu and Co do not correlate with the abundance of uranium, suggesting that fallout also records input of near field anthropogenic materials. Our observations suggest that major chemical features can be related to processing in the fireball and used to inform the thermal-chemical evolution of the system. Ultimately, these data are consistent with a fallout formation mechanism that involves rapid melting of surface materials to form carrier material melts with minor incorporation of bomb vapor and a degree of volumetric volatile loss due to heating.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2020

Ruthenium solubility and its impact on the crystallization behavior and electrical conductivity of MoO 3 -containing borosilicate-based model high-level nuclear waste glasses

The present study focuses on investigating the solubility of RuO 2 in a borosilicate-based model high-level waste glass and understanding its impact on the crystallization behavior and electrical conductivity of the resulting vitrified waste forms. The solubility limit of RuO 2 in the investigated glass composition has been determined to be 460 ppm by weight. The higher concentration of RuO 2 results in sub-micron sized Ru-rich inclusions in the glassy matrix, which eventually agglomerate to form needle-like and polyhedral RuO 2 crystals. It is observed that RuO 2 selectively promotes the crystallization of the rare-earth apatite phase over the powellite phase. The as-synthesized RuO 2 -containing glasses exhibit semiconducting behavior with a similar level of electrical conductivity below the glass transition. Here, the percolation of non-uniformly distributed RuO 2 inclusions may result in a formation of short-range low-resistive conduction pathways in the host glass matrix leading to an apparent metallic-like behavior of selected thin samples with the highest ruthenium content.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Predicting boron coordination in multicomponent borate and borosilicate glasses using analytical models and machine learning

Accurate prediction of boron coordination in multicomponent glasses is critical in glass science and technology as it strongly affects the properties of borate and borosilicate glasses. We have collected a dataset containing 657 glasses from literature with boron coordination values and developed models using analytical functions based on the well accepted Dell, Xiao and Bray model. Good prediction of boron coordination with a R 2 value higher than 0.8 was obtained. The large variation of boron coordination from experiments, originated from sample preparations and characterizations, led to difficulties in obtaining models with better prediction performance. Various machine learning (ML) algorithms were evaluated and slightly better prediction performance was observed; however, interpretation of the ML models is less straight forward. In conclusion, this study developed various models capable of providing quantitative boron coordination predictions, providing insights into its structural roles in multi-component glasses, and suggesting fruitful areas for future research.

36 MATERIALS SCIENCE↗
DOE OSTI2022

In-situ investigation of the vibrational properties of H 2 O CO 2 -bearing and dry K-rich basaltic glasses at high pressure by mid infrared spectroscopy

Here, the vibrational properties of CO 2 –H 2 O-bearing and dry synthetic K-rich basaltic glasses were investigated at room temperature and pressures between 0.0001–5.5 GPa using the diamond anvil cell combined with in situ reflectance and transmittance Fourier Transform infrared micro-spectroscopy. The absorption coefficient a(v) calculated from the Kramers-Kronig relation shows that glasses are dominated by the Q 2 aluminosilicate unit followed by Q 1 , Q 3 . The variation in Q n concentration upon compression suggests that glasses undergo polymerization from ambient pressure to 2 GPa followed by less marked structural changes up to 4 GPa, above which the structure is further polymerized. Once decompressed, glasses retained a polymerized structure. Our results show that 1.03 wt% CO 2 -1.42 wt% H 2 O in a glass with 3.10 wt% K 2 O and 46.77 wt% SiO 2 prevent the formation of fully polymerized connections when cold-compressed. Our results can be used to explain the effect of volatiles and alkali on the rheology of natural basaltic magmas.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Viscosity anomaly of a metallic glass-forming liquid under high pressure

Viscosity, as a critical property closely associated with the glass-forming ability of a liquid, has been extensively studied with varying temperatures. However, its pressure dependence has not been well explored yet due to experimental difficulties. Here, we measured the viscosity of a metallic glass-forming liquid, Zr 46 Cu 37.6 Ag 8.4 Al 8 , at pressures up to 6.1 GPa above the melting points by falling-sphere viscometry with ultrafast synchrotron x-ray imaging. Overall, the viscosity increases with pressure, while surprisingly, there is an abrupt drop between 3.2 GPa and 3.7 GPa, indicating the possible existence of a pressure-induced liquid-to-liquid transition. Pressure could change the short- and medium-range orders in the multicomponent glass-forming liquid, as suggested by the different crystalline outcomes after cooling to room temperature at high- and low-pressure ranges. In conclusion, our work extended the viscosity investigation of metallic glass-forming liquids to the high-pressure regime, which will expand our understanding of liquid-liquid transitions and metallic glass formation.

36 MATERIALS SCIENCE↗
DOE OSTI2026

Impact of Crystalline Phases on Low-Activity Waste Glass Durability: Insights from PCT and VHT

During vitrification of nuclear wastes, slow cooling along the container centerline promotes crystalline phase formation, which can alter residual glass composition and reduce chemical durability. This study investigates the effects of crystalline phases on the chemical durability of low-activity waste (LAW) borosilicate glasses using the product consistency test (PCT) and vapor hydration test (VHT) on container centerline cooled (CCC) samples. A preliminary model (R2 = 0.88) was developed to predict CCC PCT responses based on glass composition, PCT data from quenched glasses, and measured crystal fractions. Using the latest LAW glass dataset, the feasibility of predictive modeling is evaluated, limitations in current data and methods are identified, and challenges for improving model accuracy are discussed to guide future data collection and model development.

borosilicate glass↗
DOE OSTI2024

Infinitely rugged intra-cage potential energy landscape in metallic glasses caused by many-body interaction

The absence of translational symmetry in glassy materials poses a significant challenge in establishing effective structure-property relationships in real space. Consequently, the potential energy landscape (PEL) in phase space is widely utilized to comprehend the complex phenomena in glasses. The classical PEL features a two-scale profile comprising mega-basins and sub-basins, corresponding to α-relaxations (e.g. glass transition) and β-relaxations (e.g. local cage-breaking atomic rearrangements), respectively. Recent studies, however, reveal that sub-basins are not smooth and contain finer structures, the origins of which remain elusive. Here we probe the smoothness of sub-basin bottoms in glasses' PEL by introducing small intra-cage cyclic loading and then measuring the net changes in atomic-level stresses. Compared to glasses with pair interaction, glasses with many-body interaction exhibit orders-of-magnitude larger and loading-dependent stress changes even before the first cage-breaking event takes place, which reflect much more feature-rich sub-basins. We further demonstrate this stark contrast stems from the spatial distribution of individual atom's constraining force field. Specifically, at vanishing perturbations, many-body interactions disrupt the positive-definite synchrony in energy variations of the perturbed atom and the whole system, causing inherently less confined atomic responses and infinitely rugged sub-basins. The implications of these findings for the selective addition or removal of fine structures in the PEL and the subsequent tuning of glassy materials' responses to external stimuli are also explored.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Impacts of constraints and uncertainties on projected amount of Hanford low-activity waste glasses

A systematic evaluation of Hanford low-activity waste (LAW) loading in alkali-aluminoborosilicate glasses was performed. A set of 22 waste compositions were selected to represent the range of wastes anticipated across the Hanford mission. Glass composition was formulated for each waste to simultaneously satisfy a full cadre of property and composition constraints while maximizing waste loading. Glass properties were estimated using property models recently developed for Hanford LAW Facility operation. The impacts from the property and composition constraints on the glass mass to be produced were calculated and compared. Electrical conductivity, Vapor Hydration Test and SO 3 melter tolerance, and canister-centerline cooling crystal constraints have a large effect on reducing total glass mass, while the impact from Product Consistency Test, viscosity, and isothermal crystal constraints is relatively small. Additionally, effects of model prediction and process/composition uncertainties were quantified. The results identified areas of future research that could be useful to improve the efficiency of plant operation.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2021

Combinatorial measurement of critical cooling rates in aluminum-base metallic glass forming alloys

Direct measurement of critical cooling rates has been challenging and only determined for a minute fraction of the reported metallic glass forming alloys. Here, we report a method that directly measures critical cooling rate of thin film metallic glass forming alloys in a combinatorial fashion. Based on a universal heating architecture using indirect laser heating and a microstructure analysis this method offers itself as a rapid screening technique to quantify glass forming ability. We use this method to identify glass forming alloys and study the composition effect on the critical cooling rate in the Al–Ni–Ge system where we identified Al 51 Ge 35 Ni 14 as the best glass forming composition with a critical cooling rate of 10 4 K/s.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Introduction of Chalcogenide Glasses to Additive Manufacturing: Nanoparticle Ink Formulation, Inkjet Printing, and Phase Change Devices Fabrication

Abstract Chalcogenide glasses are one of the most versatile materials that have been widely researched because of their flexible optical, chemical, electronic, and phase change properties. Their application is usually in the form of thin films, which work as active layers in sensors and memory devices. In this work, we investigate the formulation of nanoparticle ink of Ge–Se chalcogenide glasses and its potential applications. The process steps reported in this work describe nanoparticle ink formulation from chalcogenide glasses, its application via inkjet printing and dip-coating methods and sintering to manufacture phase change devices. We report data regarding nanoparticle production by ball milling and ultrasonication along with the essential characteristics of the formed inks, like contact angle and viscosity. The printed chalcogenide glass films were characterized by Raman spectroscopy, X-ray diffraction, energy dispersive spectroscopy and atomic force microscopy. The printed films exhibited similar compositional, structural, electronic and optical properties as the thermally evaporated thin films. The crystallization processes of the printed films are discussed compared to those obtained by vacuum thermal deposition. We demonstrate the formation of printed thin films using nanoparticle inks, low-temperature sintering and proof for the first time, their application in electronic and photonic temperature sensors utilizing their phase change property. This work adds chalcogenide glasses to the list of inkjet printable materials, thus offering an easy way to form arbitrary device structures for optical and electronic applications.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2020

Fast-current-heating devices to study in situ phase formation in metallic glasses by using high-energy synchrotron radiation

Details of fast-resistive-heating setups, controlled heating ranging from ~10 1 K s –1 to ~10 3 K s –1 , to study in situ phase transformations (on heating and on cooling) in metallic glasses by high-energy synchrotron x-ray diffraction are discussed here. Both setups were designed and custom built at the Leibniz Institute for Solid State and Materials Research Dresden (IFW Dresden) and have been implemented at the P02.1 Powder Diffraction and Total Scattering Beamline and the P21.1 Swedish Materials Science Beamline at PETRA III storage ring, DESY, Hamburg. The devices are interchangeable at both beamlines. Joule heating is triggered automatically and is timed with the incident beam and detector. The crystallization process can be controlled via a feedback circuit by monitoring the change in the time-dependent resistivity and temperature of glasses. Different ambient atmospheres, such as vacuum and inert gases (He and Ar), can be used to control oxidation and cooling. The main focus of these devices is on understanding the crystallization mechanism and kinetics in metallic glasses, which are brittle and for which fast heating gives defined glass–crystal composites with enhanced plasticity. As an example, phase-transformation sequence(s) in a prototyped Cu–Zr-based metallic glass is described on heating, and a crystalline phase beneficial to the plasticity is identified.

47 OTHER INSTRUMENTATION↗
DOE OSTI2021

Glasses denser than the supercooled liquid

When aged below the glass transition temperature, T g , the density of a glass cannot exceed that of the metastable supercooled liquid (SCL) state, unless crystals are nucleated. The only exception is when another polyamorphic SCL state exists, with a density higher than that of the ordinary SCL. Experimentally, such polyamorphic states and their corresponding liquid–liquid phase transitions have only been observed in network-forming systems or those with polymorphic crystalline states. In otherwise simple liquids, such phase transitions have not been observed, either in aged or vapor-deposited stable glasses, even near the Kauzmann temperature. Here, we report that the density of thin vapor-deposited films of N,N'-bis(3-methylphenyl)-N,N'-diphenylbenzidine (TPD) can exceed their corresponding SCL density by as much as 3.5% and can even exceed the crystal density under certain deposition conditions. We identify a previously unidentified high-density supercooled liquid (HD-SCL) phase with a liquid–liquid phase transition temperature (T LL ) ~35 K below the nominal glass transition temperature of the ordinary SCL. Additionally, the HD-SCL state is observed in glasses deposited in the thickness range of 25 to 55 nm, where thin films of the ordinary SCL have exceptionally enhanced surface mobility with large mobility gradients. The enhanced mobility enables vapor-deposited thin films to overcome kinetic barriers for relaxation and access the HD-SCL state. The HD-SCL state is only thermodynamically favored in thin films and transforms rapidly to the ordinary SCL when the vapor deposition is continued to form films with thicknesses more than 60 nm.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Spin-glass dynamics in the presence of a magnetic field: exploration of microscopic properties

The synergy between experiment, theory, and simulations enables a microscopic analysis of spin-glass dynamics in a magnetic field in the vicinity of and below the spin-glass transition temperature T g . The spin-glass correlation length, ξ(t, t w ; T), is analysed both in experiments and in simulations in terms of the waiting time t w after the spin glass has been cooled down to a stabilised measuring temperature T < T g and of the time t after the magnetic field is changed. This correlation length is extracted experimentally for a CuMn 6 at. % single crystal, as well as for simulations on the Janus II special-purpose supercomputer, the latter with time and length scales comparable to experiment. The non-linear magnetic susceptibility is reported from experiment and simulations, using ξ(t, t w ; T) as the scaling variable. Previous experiments are reanalysed, and disagreements about the nature of the Zeeman energy are resolved. The growth of the spin-glass magnetisation in zero-field magnetisation experiments, M ZFC (t, t w ; T), is measured from simulations, verifying the scaling relationships in the dynamical or non-equilibrium regime. Lastly, our preliminary search for the de Almeida–Thouless line in D = 3 is discussed.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Atom Probe Tomography Investigation of Clustering in Model P 2 O 5 -Doped Borosilicate Glasses for Nuclear Waste Vitrification

Atom probe tomography (APT) has been utilized to investigate the microstructure of two model borosilicate glasses designed to understand the solubility limits of phosphorous pentoxide (P 2 O 5 ). This component is found in certain high-level radioactive defence wastes destined for vitrification, where phase separation can potentially lead to a number of issues relating to the processing of the glass and its long-term chemical and structural stability. The development of suitable focused ion beam (FIB)-preparation routes and APT analysis conditions were initially determined for the model glasses, before examining their detailed microstructures. In a 3.0 mol% P 2 O 5 -doped glass, both visual inspection and sensitive statistical analysis of the APT data show homogeneous microstructures, while raising the content to 4.0 mol% initiates the formation of phosphorus-enriched nanoscale precipitates. This study confirms the expected inhomogeneities and phase separation of these glasses and offers routes to characterizing these at near-atomic scale resolution using APT.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗