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At least 793 records · Page 44

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DOE OSTI2018

The Influence of the Cobalt Content on the Strength Properties of Tungsten Carbide Ceramics under Dynamic Loads

Based on the registration and analysis of the full wave profiles, the Hugoniot elastic limit and spall strength of ceramics based on tungsten carbide with different cobalt content are measured. We also study the influence of the cobalt content on the mechanical characteristics of tungsten carbide such as hardness, fracture strength, Young’s modulus, shear modulus, and sound velocity. It is shown that in the process of spalling, the failure stresses grow and the dynamic elastic limit decreases almost linearly within the scatter of their values with growing cobalt content; moreover, the value of the Hugoniot elastic limit is abruptly practically halved as the cobalt content grows from 0 to 2 wt %.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2015

Characterization of high level nuclear waste glass samples following extended melter idling

The Savannah River Site Defense Waste Processing Facility (DWPF) melter was recently idled with glass remaining in the melt pool and riser for approximately three months. This situation presented a unique opportunity to collect and analyze glass samples since outages of this duration are uncommon. The objective of this study was to obtain insight into the potential for crystal formation in the glass resulting from an extended idling period. The results will be used to support development of a crystal-tolerant approach for operation of the high-level waste melter at the Hanford Tank Waste Treatment and Immobilization Plant (WTP). Two glass pour stream samples were collected from DWPF when the melter was restarted after idling for three months. The samples did not contain crystallization that was detectible by X-ray diffraction. Electron microscopy identified occasional spinel and noble metal crystals of no practical significance. Occasional platinum particles were observed by microscopy as an artifact of the sample collection method. Reduction/oxidation measurements showed that the pour stream glasses were fully oxidized, which was expected after the extended idling period. Chemical analysis of the pour stream glasses revealed slight differences in the concentrations of some oxides relative to analyses of the melter feed composition prior to the idling period. While these differences may be within the analytical error of the laboratories, the trends indicate that there may have been some amount of volatility associated with some of the glass components, and that there may have been interaction of the glass with the refractory components of the melter. These changes in composition, although small, can be attributed to the idling of the melter for an extended period. The changes in glass composition resulted in a 70-100 °C increase in the predicted spinel liquidus temperature (TL) for the pour stream glass samples relative to the analysis of the melter feed prior to the outage. This indicates that the potential for spinel crystallization increased as a result of idling for an extended period. However, the predicted TL of the pour stream glasses remained 150-200 °C below the mean melt pool temperature of about 1125 °C during the idling period. Given the change in predicted TL over the three month outage, the results indicate that it is important to have a thorough understanding of spinel crystallization within the melter for WTP to operate with a volume percent crystallization constraint. This knowledge will enable process control routines to be developed that avoid bulk crystallization in the melter and allow for recovery from off-normal events. The current WTP crystal-tolerant glass program will develop an improved understanding of spinel crystallization in the WTP melter to allow for operation at maximum waste loading in glass composition systems limited by predictions of spinel crystallization.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2013

Reduced-temperature processing and consolidation of ultra-refractory Ta4HfC5

TaC, HfC, and WC powders were subjected to high-energy milling and hot pressing to produce Ta4HfC5, a composite of Ta(4)HfC5 + 30 vol.% WC, and a composite of Ta4HfC5 + 50 vol.% WC. Sub-micron powders were examined after four different milling intervals prior to hot pressing. XRD was used to verify proper phase formation. SEM, relative density, and hardness measurements were used to examine the resulting phases. Hot pressed compacts of Ta4HfC5 showed densification as high as 98.6% along with Vickers hardness values of 21.4 GPa. Similarly, Ta4HfC5 + 30 vol.% WC exhibited 99% densification with a Vickers hardness of 22.5 GPa. These levels of densification were achieved at 1500 degrees C, which is lower than any previously reported sintering temperature for Ta4HfC5. Microhardness values measured in this study were higher than those previously reported for Ta4HfC5. The WC additions to Ta4HfC5 were found to improve densification and increase microhardness. (C) 2013 Elsevier Ltd. All rights reserved.

36 MATERIALS SCIENCE↗

DOE OSTI2019

Neutron irradiation-induced microstructure damage in ultra-high temperature ceramic TiC

Titanium carbide (TiC) is an ultra-high temperature ceramic with potential as a structural material candidate for advanced reactor concepts. However, the irradiation tolerance of TiC is not well understood. Here, we reveal the key irradiation damage microstructure degradation processes in TiC using mixed spectrum neutron irradiations at dose of ~2 displacements per atom (dpa) at temperatures of ~220, 620, and 1115 °C, combined with state-of-art microstructure characterization using transmission electron microscopy (TEM) and high-resolution TEM (HRTEM). The helium injection (~65 atomic parts per million) produced by neutron transmutation also occurred in the sample. TiC was observed to form irradiation-induced interstitial-type dislocation loops and He-stabilized cavities. At 220 and 620 °C, the analysis of the electron diffraction patterns, rel-rod imaging and HRTEM revealed that the dislocation loops were faulted Frank loops with Burgers vector b Frank = 1/3<111> lying on {111} planes. A detailed Burgers vector identification performed by the g.b technique revealed that the dislocation loops forming at 1115 °C were unfaulted, edge-type, with Burgers vectors b = a<100> and a/2<110> with corresponding {100} and {110} habit planes. Using continuum mechanics, we estimated the critical radius at which a faulted dislocation loop transitions to a perfect loop to be 9 nm. Further, no amorphization occurred in TiC under-investigated irradiation conditions while macroscopic swelling under point defect swelling regime was observed. He-stabilized cavities were detected at 1115 °C, but not at lower temperature irradiation. These observations indicate the onset of long-range vacancy migration in TiC occurs between 620 and 1115 °C.

36 MATERIALS SCIENCE↗

DOE OSTI2022

Additive manufacturing of complex objects using refractory matrix materials

A method for the manufacture of a three-dimensional object using a refractory matrix material is provided. The method includes the additive manufacture of a green body from a powder-based refractory matrix material followed by densification via chemical vapor infiltration (CVI). The refractory matrix material can be a refractory ceramic (e.g., silicon carbide, zirconium carbide, or graphite) or a refractory metal (e.g., molybdenum or tungsten). In one embodiment, the matrix material is deposited according to a binder-jet printing process to produce a green body having a complex geometry. The CVI process increases its density, provides a hermetic seal, and yields an object with mechanical integrity. The residual binder content dissociates and is removed from the green body prior to the start of the CVI process as temperatures increase in the CVI reactor. The CVI process selective deposits a fully dense coating on all internal and external surfaces of the finished object.

Terrani, Kurt A.↗

DOE OSTI2024

Additive manufacturing of complex objects using refractory matrix materials

Terrani, Kurt A.↗

DOE OSTI2018

Effect of sintering temperature on structural, magnetic and electrical transport properties of La0.67Ca0.33MnO3 ceramics prepared by Plasma Activated Sintering

Highlights: • La{sub 0.67}Ca{sub 0.33}MnO{sub 3} were prepared by using Plasma Activated Sintering technology. • Detailed studies of sintering temperature effect on structural, magnetic and electrical transport behaviors were investigated. • The observed behaviors have been explained by oxygen vacancy effect in combination with grain size effect. - Abstract: La{sub 0.67}Ca{sub 0.33}MnO{sub 3} (LCMO) ceramics were prepared by Plasma Activated Sintering (PAS). The effect of sintering temperature on structural, magnetic and electrical transport properties of the LCMO ceramics were investigated. XRD and SEM characterizations of the LCMO ceramics indicated that all samples exhibited single orthorhombic phase. Also, through PAS dense LCMO ceramics were obtained. Certain interesting phenomena were observed from the PAS sintering temperature effect on the magnetic and transport behaviors of LCMO ceramics, which were significantly different from traditional sintering methods The magnetization decreased and the resistivity increased as the sintering temperature increased, whereas the T{sub C} and T{sub IM} shifted towards the lower temperature side. The conduction mechanism of all samples was electron-magnon scattering process in the ferromagnetic low-temperature region, while the paramagnetic high-temperature region mechanism was explained with the variable range hopping (VRH) model. All these behaviors were explained through the oxygen vacancy effect in combination with the grain size effect.

36 MATERIALS SCIENCE↗

DOE OSTI2018

Production Procedure and Characterization of Zn-Doped Y-123 Superconducting Samples Prepared by Sol-Gel Method

The superconducting YBa{sub 2}Cu{sub 3−x}Zn{sub x}O{sub 7} (Y-123) bulk materials have been synthesized by using the sol-gel method. Samples are produced as undoped Y-123 and transition metal (Zn)-doped Y-123. Before the final heat treatment, the samples are calcined at 850 °C for 24 h. This process is repeated three times. Then, samples are sintered at 950 °C for 24 h in an air environment and at 500 °C for 5 h in an oxygen atmosphere. The synthesized products are characterized by XRD, R-T, and Vickers microhardness tester. The XRD investigation revealed that the prepared sample has an orthorhombic structure. According to XRD measurements, an orthorhombic structure has not changed with Zn doping. It was observed that undoped and Zn-doped samples have superconductivity properties by electrical measurements. T{sub c}{sup onset} is 89 K for undoped Y-123 sample, and the T{sub c}{sup onset} value decreases monotically with Zn addition. All samples show metallic behavior above T{sub c}{sup onset} temperature. As a result of Vickers microhardness measurements, it is observed that all samples have reverse indentation size effect (RISE) behavior.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2015

Crystallization in high level waste (HLW) glass melters: Savannah River Site operational experience

This paper provides a review of the scaled melter testing that was completed for design input to the Defense Waste Processing Facility (DWPF) melter. Testing with prototype melters provided the data to define the DWPF operating limits to avoid bulk (volume) crystallization in the un-agitated DWPF melter and provided the data to distinguish between spinels generated by refractory corrosion versus spinels that precipitated from the HLW glass melt pool. A review of the crystallization observed with the prototype melters and the full-scale DWPF melters (DWPF Melter 1 and DWPF Melter 2) is included. Examples of actual DWPF melter attainment with Melter 2 are given. The intent is to provide an overview of lessons learned, including some example data, that can be used to advance the development and implementation of an empirical model and operating limit for crystal accumulation for a waste treatment and immobilization plant.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2022

High-surface-area corundum nanoparticles by resistive hotspot-induced phase transformation

Abstract High-surface-area α-Al 2 O 3 nanoparticles are used in high-strength ceramics and stable catalyst supports. The production of α-Al 2 O 3 by phase transformation from γ-Al 2 O 3 is hampered by a high activation energy barrier, which usually requires extended high-temperature annealing (~1500 K, > 10 h) and suffers from aggregation. Here, we report the synthesis of dehydrated α-Al 2 O 3 nanoparticles (phase purity ~100%, particle size ~23 nm, surface area ~65 m 2 g −1 ) by a pulsed direct current Joule heating of γ-Al 2 O 3 . The phase transformation is completed at a reduced bulk temperature and duration (~573 K, < 1 s) via an intermediate δʹ-Al 2 O 3 phase. Numerical simulations reveal the resistive hotspot-induced local heating in the pulsed current process enables the rapid transformation. Theoretical calculations show the topotactic transition (from γ- to δʹ- to α-Al 2 O 3 ) is driven by their surface energy differences. The α-Al 2 O 3 nanoparticles are sintered to nanograined ceramics with hardness superior to commercial alumina and approaching that of sapphire.

Deng, Bing (ORCID:0000000305308410)↗

DOE OSTI2017

Tin doped PrBaFe 2 O 5+δ anode material for solid oxide fuel cells

Ceramic anodes have many advantages over cermet anodes for solid oxide fuel cells. We report the synthesis and characterization of Sn doped double perovskite PrBaFe (2-x) Sn x O 5+δ (x = 0–0.3) anode materials. Different crystal structures were observed depending on the Sn doping level and gas atmosphere. The materials demonstrated excellent stability in both reducing and redox atmospheres at elevated temperatures. The oxygen content in the as-prepared PrBaFe (2-x) Sn x O 5+δ was nonlinearly correlated to the Sn doping level and reached maximum values around x = 0.1. After the reducing treatment, the oxygen content linearly decreased with increasing Sn doping level. The electrical conductivity of bulk PrBaFe (2-x) Sn x O 5+δ (x = 0.1) reached 63.6 S cm -1 at 800 °C in humidified hydrogen. At 750 °C, the surface exchange coefficient and bulk diffusivity of PrBaFe (2-x) Sn x O 5+δ reached the maximum values of 4.42 × 10 -6 m s -1 and 6.04 × 10 -7 m 2 s -1 , respectively, in the reducing process when the Sn doping level was x = 0.1. The activation energies of surface exchange coefficient and bulk diffusivity of PrBaFe (2-x) Sn x O 5+δ (x = 0.1) were 0.22 eV and 0.16 eV, respectively, in the reducing process. The area specific resistance of the PrBaFe (2-x) Sn x O 5+δ (x = 0.1) anode was 0.095–0.285 Ω cm 2 from 850–750 °C in humidified hydrogen, better than or comparable to the best ceramic anodes in the literature.

36 MATERIALS SCIENCE↗

DOE OSTI2013

Chemical Vapor Deposited Zinc Sulfide. SPIE Press Monograph

Zinc sulfide has shown unequaled utility for infrared windows that require a combination of long-wavelength infrared transparency, mechanical durability, and elevated-temperature performance. This book reviews the physical properties of chemical vapor deposited ZnS and their relationship to the CVD process that produced them. An in-depth look at the material microstructure is included, along with a discussion of the material's optical properties. Finally, because the CVD process itself is central to the development of this material, a brief history is presented.

ceramic↗

DOE OSTI2024

Methods of fabricating porous ceramic electrodes for solid state battery applications

Compositions and methods for the fabrication of electrode and porous lithium-garnet electrolyte scaffolds for use in solid state batteries and other devices are provided. The methods produce porous structures using phase inversion or high shear compaction processes to fabricate a solid-state battery electrode material from LLZO electrolytes. Engineered electrode structures with a porous scaffold of solid electrolyte material provide lower interfacial resistances and a mechanical support for a thin solid electrode layer improving performance.

Tucker, Michael↗

DOE OSTI2021

AOI [1]: Passive Wireless Sensor Systems Fabricated by Direct-Writing for Temperature and Health Monitoring of Energy Systems in Harsh-Environments (Final Report)

Researchers at West Virginia University (WVU) propose to demonstrate a wireless, high-temperature sensor system for monitoring the temperature and health of energy-system components. The active sensor and electronics for wireless communication will be composed entirely of an electroceramic materials (conductive ceramics) which are capable of withstanding the harsh-environments required for fossil energy-based technologies. This work will focus primarily on the fabrication and testing of temperature (thermocouples and thermistors) and health (strain/stress and crack propagation sensors) that function at extreme temperatures (up to 700-1700ºC). The electronics will accompany the high-temperature sensor, which will include a passive wireless communication circuit that allows the transmission of the data based on the LCR resonance principle to a near-by reader antenna. This passive transmission of data will reduce the need for interconnect wires near the active, and possibly rotating, energy-system component. The research will include process development to permit the 2D/3D direct-writing of the entire sensor and communication circuit onto the energy-system component. The direct-writing will be facilitated by using silicon-based polymer-derived precursors to form the high-temperature, stable electroceramic compositions. In addition, methods for direct-writing the circuit onto a fugitive carrier substrate will be completed, which will permit a “peel-and-stick”-like transfer of the sensor circuit to the energy-system component. This feature will allow the economical and precise placement of the sensor circuit onto components of various shapes and locations, without altering the geometry and active features of the manufactured component, or the removal (or decommissioning) of the component for installation. The proposed work will be directed at the following areas: 1) Investigation of phase formation, sintering/grain growth, and electrical properties of polymer-derived electroceramic composites; 2) Definition of processes to direct-write through ink-jet and robo-casting the polymer-derived electroceramic composites onto oxide and polymer surfaces; 3) Development of methods to form monolithic "peel-and-stick" preforms that will efficiently transfer the sensor circuit to ceramic surfaces after thermal treatment; 4) Design of passive wireless LCR circuits and receiver (reader) antennas for communication and testing at high temperatures; 5) Investigation of the passive wireless sensor system developed (and method of transferring sensor system) for temperature and stress/strain measurements on a SOFC repeat unit and a singular gas turbine blade prototype as example applications.

01 COAL, LIGNITE, AND PEAT↗

DOE OSTI2016

Initial Testing of Off-Gas Recycle Condensate Liquid from the WTP Low Activity Waste Vitrification Process - 16432

The Waste Treatment and Immobilization Plant (WTP) under construction at the Hanford site is designed to treat and immobilize the inventory of High-Level Waste stored in the 177 underground storage tanks. The WTP process flow was designed to pre-treat this waste, separating it into High Level Waste (HLW) and Low Activity Waste (LAW) fractions for vitrification. Vitrification of the waste generates a condensate stream from the off-gas processes originating from two off-gas treatment unit operations, the Submerged Bed Scrubber (SBS) and the Wet Electrostatic Precipitator (WESP). The baseline plan for disposition of the stream from the LAW melter is to recycle it to the Pretreatment facility where it gets evaporated and processed through the LAW melter again. If the Pretreatment facility is unavailable, this baseline disposition pathway is not viable. Additionally, chloride, fluoride, and sulfate are partially volatile in the melter, accumulating to high concentrations while recycling and impacting the glass waste loading and facility throughput. The primary radionuclide that volatizes and accumulates is {sup 99}Tc. The long half-life and environmental mobility of {sup 99}Tc complicates disposal options for this secondary aqueous waste stream. This task is investigating {sup 99}Tc removal to examine the potential for diverting this stream to an alternate disposition path and avoiding impacting the glass waste loading. Separation methods for {sup 99}Tc have focused on using inorganic precipitation agents that can remove it by reducing it from soluble pertechnetate ion, with a +7 oxidation state, to insoluble technetium dioxide in the +4 oxidation state. Stannous chloride (SnCl{sub 2}) has been found highly effective at causing the reduction and precipitating {sup 99}Tc for removal, but it also precipitates other components. The primary competitor that precipitates is chromium, which consumes the redox activity of the Sn(II), causing addition of more of the SnCl{sub 2}. Research has examined the optimum quantity of SnCl{sub 2}, mixing time, and the impact of other redox-active species. It is also important to know the stability of the precipitated {sup 99}Tc in process conditions, since it is expected it will eventually be re-oxidized by oxygen and dissolve. This work is expected to determine if a {sup 99}Tc removal step could be used to decontaminate the bulk of this stream, and make it suitable for other disposal paths so that the chloride, fluoride, and sulfate can be diverted away from the glass melter. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2013

Study of de-watering from the gelatinous precipitate formed during co-precipitation of Nd-YAG powder

Neodymium doped Yttrium Aluminium Garnet (Nd:YAG) ceramics have been synthesised using coprecipitation technique and high temperature vacuum sintering. Gelatinous like precipitates were obtained when precursors of Nd, Al and Yb-nitrate solutions are co-precipitated using ammonia co-precipitant. De-watering from the gelatinous like precipitates is a big challenge and it possesses difficulty in filtration. Evaporation of water by heating resulted in strong agglomerated powder. Different agents were used to ease the filtration process, which is correlated with the phase in the calcined powder.

36 MATERIALS SCIENCE↗

DOE OSTI2015

Electric-field-temperature phase diagram of Mn-doped Bi{sub 0.5}(Na{sub 0.9}K{sub 0.1}){sub 0.5}TiO{sub 3} ceramics

An electric field–temperature (E-T) phase diagram for a lead-free 0.5 mol. % Mn-doped Bi(Na{sub 0.1}K{sub 0.9})TiO{sub 3} ceramics was investigated. The x-ray diffraction, dielectric and polarization measurements revealed relaxor behavior and were used to characterize the stability regions of the non-ergodic relaxor, ergodic relaxor and electric field induced ferroelectric states. As indicated by the polarization–current density profiles, transformation between two electric fields, induced ferroelectric states with opposite polarization direction arise via a two-step process through an intermediate relaxor state. Interplay between the ferroelectric state conversion and intermediate relaxor state is governed by the dynamics of polarization relaxation. The presented E-T phase diagram revealed the effects of the applied electric field and temperature on stability regions. This is of special interest since the Bi{sub 0.5}(Na{sub 0.1}K{sub 0.9}){sub 0.5}TiO{sub 3} ceramics were proposed as a potential piezoceramic material.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

DOE OSTI2015

Deposition of Pd–Ag thin film membranes on ceramic supports for hydrogen purification/separation

Highlights: • Thin film Pd–Ag membranes have been produced for hydrogen selectivity. • Magnetron sputtering yields Pd–Ag compact films for atomic H diffusion. • The thin film Pd–Ag membranes yielded a selectivity of α (H{sub 2}/N{sub 2}) = 10. - Abstract: Pd–Ag based membranes supported on porous α-Al{sub 2}O{sub 3} (doped with yttria-stabilized zirconia) were studied for hydrogen selective separation. Magnetron sputtering technique was employed for the synthesis of thin film membranes. The hydrogen permeation flux is affected by the membrane columnar structure, which is formed during deposition. From scanning electron microscopy analysis, it was observed that different sputtering deposition pressures lead to distinct columnar structure growth. X-ray diffraction patterns provided evidence of a Pd–Ag solid solution with an average crystallite domain size of 21 nm, whose preferential growth can be altered by the deposition pressure. The gas-permeation results have shown that the Pd–Ag membrane supported on porous α-Al{sub 2}O{sub 3} is selective toward H{sub 2}. For optimized membrane synthesis conditions, the permeance toward N{sub 2} is 0.076 × 10{sup −6} mol m{sup −2} s{sup −1} Pa{sup −1} at room temperature, whereas for a pressure difference of 300 kPa the H{sub 2}-flux is of the order of ca. 0.21 mol m{sup −2} s{sup −1}, which corresponds to a permeance of 0.71 × 10{sup −6} mol m{sup −2} s{sup −1} Pa{sup −1}, yielding a selectivity of α (H{sub 2}/N{sub 2}) = 10. These findings suggest that the membrane has a reasonable capacity to selectively permeate this gas.

36 MATERIALS SCIENCE↗