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At least 1,189 records · Page 66
All sourcesNASA NTRSDOE OSTI
DOE OSTI2023

Will high-entropy carbides and borides be enabling materials for extreme environments?

Abstract The concept of multi-principal component has created promising opportunities for the development of novel high-entropy ceramics for extreme environments encountered in advanced turbine engines, nuclear reactors, and hypersonic vehicles, as it expands the compositional space of ceramic materials with tailored properties within a single-phase solid solution. The unique physical properties of some high-entropy carbides and borides, such as higher hardness, high-temperature strength, lower thermal conductivity, and improved irradiation resistance than the constitute ceramics, have been observed. These promising properties may be attributed to the compositional complexity, atomic-level disorder, lattice distortion, and other fundamental processes related to defect formation and phonon scattering. This manuscript serves as a critical review of the recent progress in high-entropy carbides and borides, focusing on synthesis and evaluations of their performance in extreme high-temperature, irradiation, and gaseous environments.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Individual pore and interconnection size analysis of macroporous ceramic scaffolds using high-resolution X-ray tomography

The pore interconnection size of β-tricalcium phosphate scaffolds plays an essential role in the bone repair process. Although, the μCT technique is widely used in the biomaterial community, it is rarely used to measure the interconnection size because of the lack of algorithms. In addition, discrete nature of the μCT introduces large systematic errors due to the convex geometry of interconnections. We proposed, verified and validated a novel pore-level algorithm to accurately characterize the individual pores and interconnections. Specifically, pores and interconnections were isolated, labeled, and individually analyzed with high accuracy. The technique was verified thoroughly by visually inspecting and verifying over 3474 properties of randomly selected pores. This extensive verification process has passed a one-percent accuracy criterion. Scanning errors inherent in the discretization, which lead to both dummy and significantly overestimated interconnections, have been examined using computer-based simulations and additional high-resolution scanning. Then accurate correction charts were developed and used to reduce the scanning errors. Only after the corrections, both the μCT and SEM-based results converged, and the novel algorithm was validated. Material scientists with access to all geometrical properties of individual pores and interconnections, using the novel algorithm, will have a more-detailed and accurate description of the substitute architecture and a potentially deeper understanding of the link between the geometric and biological interaction. - Highlights: •An algorithm is developed to analyze individually all pores and interconnections. •After pore isolating, the discretization errors in interconnections were corrected. •Dummy interconnections and overestimated sizes were due to thin material walls. •The isolating algorithm was verified through visual inspection (99% accurate). •After correcting for the systematic errors, algorithm was validated successfully.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Evaluation of a recycling process for printed circuit board by physical separation and heat treatment

Highlights: • The parts mounted on printed circuit board (PCB) were liberated by underwater explosion and mechanical crushing. • The crushed PCB without surface-mounted parts was carbonized under inert atmosphere at 873 K to recover copper. • The multi-layered ceramic capacitors including nickel was carbonized at 873 K to recover nickel by the magnetic separation. • The tantalum powders were recovered from the molded resins by heat treatment at 723 and 823 K in air atmosphere and screening. • Energy and treatment cost of new process increased, however, the environmental burden decreased comparing conventional one. - Abstract: Printed circuit boards (PCBs) from discarded personal computer (PC) and hard disk drive were crushed by explosion in water or mechanical comminution in order to disintegrate the attached parts. More parts were stripped from PCB of PC, composed of epoxy resin; than from PCB of household appliance, composed of phenol resin. In an attempt to raise the copper grade of PCB by removing other components, a carbonization treatment was investigated. The crushed PCB without surface-mounted parts was carbonized under a nitrogen atmosphere at 873–1073 K. After screening, the char was classified by size into oversized pieces, undersized pieces and powder. The copper foil and glass fiber pieces were liberated and collected in undersized fraction. The copper foil was liberated easily from glass fiber by stamping treatment. As one of the mounted parts, the multi-layered ceramic capacitors (MLCCs), which contain nickel, were carbonized at 873 K. The magnetic separation is carried out at a lower magnetic field strength of 0.1 T and then at 0.8 T. In the +0.5 mm size fraction the nickel grade in magnetic product was increased from 0.16% to 6.7% and the nickel recovery is 74%. The other useful mounted parts are tantalum capacitors. The tantalum capacitors were collected from mounted parts. The tantalum-sintered bodies were separated from molded resins by heat treatment at 723–773 K in air atmosphere and screening of 0.5 mm. Silica was removed and 70% of tantalum grade was obtained after more than 823 K heating and separation. Next, the evaluation of Cu recycling in PCB is estimated. Energy consumption of new process increased and the treatment cost becomes 3 times higher comparing the conventional process, while the environmental burden of new process decreased comparing conventional process. The nickel recovery process in fine ground particles increased energy and energy cost comparing those of the conventional process. However, the environmental burden decreased than the conventional one. The process for recovering tantalum used more heat for the treatment and therefore the energy consumption increased by 50%, when comparing with conventional process. However, the market price for tantalum is very large; the profit for tantalum recovery is added. Also the environmental burden decreased by the recycling of tantalum recovery. Therefore, the tantalum recovery is very important step in the PCB recycling. If there is no tantalum, the consumed energy and treatment cost increase in the new process, though the environmental burden decreases.

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

Influence of Carbides and Alloying Elements on Intercrystallite Corrosion in Cutting-Ceramic Inserts

It is established that intercrystallite corrosion of cutting-ceramic inserts arises when the chromium content in the peripheral zone of the grains is depleted by the deposition of chromium carbides at the grain boundaries, in the presence of stress due to the fast cooling of the inserts from high temperatures. This is especially apparent when 12Kh18N10Т, 40Kh13, 14Kh17N2, and other steels that are hard to machine are worked by a tool equipped with inserts of VOK-60M modified cutting ceramic. Research shows that the intercrystallite corrosion of cutting-ceramic inserts may be attributed to the stress arising in the surface layers of the grains as a result of carbide or nitride deposition. Heating cutting-ceramic inserts at 650–800°С lowers this stress and restores their resistance to intercrystallite corrosion. Research also shows that chromomanganese cutting-ceramic inserts are less susceptible to intercrystallite corrosion than are chromium–manganese–nickel inserts, while chromium–manganese–nickel cutting-ceramic inserts are less susceptible than are chromonickel inserts. The benefits of chromium–manganese–nickel cutting-ceramic inserts are especially pronounced with relatively brief machining of 12Kh18N10Т, 40Kh13, 14Kh17N2, and other such steels, in rigorous conditions, with a temperature of 600–650°С in the workpiece–tool contact zone. A new theory of the intercrystallite corrosion of VOK-60M modified cutting ceramic is based on the role of the kinetic factor at the relatively low tempering temperatures associated with the deposition of metastable carbide, although this does not lead to maximum change in free energy of the system but only to a relative change. In the cutting ceramic, this carbide may be chromium carbide (Cr, Тi){sub 23}C{sub 6}, which is greatly enriched with titanium. With increase in tempering temperature, the deposited carbide tends toward the stable composition Cr{sub 23}С{sub 6}. Prolonged holding at the tempering temperature also tends to favor thermodynamic equilibrium. In other word, the chromium carbide is gradually enriched to reach the stable composition Cr{sub 23}С{sub 6}. This process is more rapid at higher temperatures. Obviously, the variation in composition of the carbide deposited at the grain boundaries in VOK-60M cutting ceramic with change in temperature and holding time will affect the kinetics of electrochemical solution of the system consisting of the carbide in contact with a solid solution. Research shows that vacuum sintering and annealing markedly improve the thermal stability. For the cutting ceramic, this is explained not only by the removal of fusible impurities but also by the larger quantity of aluminum and other alloying elements that remain in the strengthening phase, rather than being bound in oxides. Sintering in vacuum ensures greater plasticity of cutting ceramic based on nickel and cobalt in cutting 12Kh18N10Т and 14Kh17N2 steel at high speeds, with high temperatures in the machining zone. In addition, on sintering in vacuum furnaces, the content of small nonmetallic inclusions in the basic structure is 5–7 times less than in regular cutting ceramic. That significantly improves the deformability of the ceramic inserts.

36 MATERIALS SCIENCE↗
DOE OSTI2024

System and method for engineered ceramic packages for use in fluid treatment technologies

The present disclosure relates to a method for making a ceramic mini-tube configured for use in a fluid modification system. The method involves using an electrospinning system to receive a quantity of precursor solution. The electrospinning system creates an electric field which causes the precursor solution, when emitted, to be stretched into a fiber jet. The fiber jet is deposited on a collector resulting in a fiber mat. The fiber mat is removed from the collector, wherein the fiber mat is formed into a shape. The fiber mat is further processed so that the fiber mat retains a desired shape. A heat treatment operation is then performed to convert the fiber mat into a ceramic structure having the desired shape.

Kelly, James Patrick↗
DOE OSTI2018

Insight into the BiFeO 3 flash sintering process by in-situ energy dispersive X-ray diffraction (ED-XRD)

The sintering mechanism of BiFeO 3 has been investigated in-situ by energy dispersive X-ray diffraction (ED-XRD) using a high-energy white collimated X-ray beam from the Advanced Photon Source (Argonne National Laboratories). Such radiation is very penetrating thereby allowing measurements of the sample even when placed inside the flash sintering set up. Additionally, the fast ED-XRD measurements permit monitoring the flash sintering process by providing information about phase composition and sample temperature in real time. Moreover, profile scans, obtained by moving the stage vertically while recording the ED-XRD spectra, permit investigating the homogeneity of the flash for the entire length of the sample. All experiments have been complemented by ex-situ studies. Here, it has been concluded that flash sintering of BiFeO 3 is a homogeneous process without any directionality effects. Furthermore, flash sintering takes place at quite low temperatures (below the Tc ≈ 830 °C), which may be related to the high quality of the samples, as pure, highly insulating ceramics without evidence of secondary phases with a homogenous nanostructured grain size distribution are obtained by this technique. Moreover, it is also evidenced that the rapid heating of the sample does not seem to justify, at least by itself, the densification process. Therefore, it appears that the electric current should play a role in the enhanced mobility during the sintering process.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Composition dependence of electric-field-induced structure of Bi{sub 1/2}(Na{sub 1−x}K{sub x}){sub 1/2}TiO{sub 3} lead-free piezoelectric ceramics

Microscopic origins of the electric-field-induced strain for three compositions of Bi{sub 1/2}(Na{sub 1−x}K{sub x}){sub 1/2}TiO{sub 3} (x = 0.14, 0.18, and 0.22) (BNKT100x) ceramics have been compared using in situ high-energy (87.12 keV) X-ray diffraction. In the as-processed state, average crystallographic structure of BNKT14 and BNKT18 were found to be of rhombohedral symmetry, while BNKT22 was tetragonal. Diffraction data collected under electric field showed that both the BNKT14 and BNKT18 exhibit induced lattice strain and non-180° ferroelectric domain switching without any apparent phase transformation. The BNKT22 composition, in addition to the lattice strain and domain switching, showed an electric-field-induced transformation from a tetragonal to mixed tetragonal-rhombohedral state. Despite the difference in the origin of microscopic strain responses in these compositions, the measured macroscopic poling strains of 0.46% (BNKT14), 0.43% (BNKT18), and 0.44% (BNKT22) are similar. In addition, the application of a second poling field of opposite polarity to the first increased the magnitude of non-180° ferroelectric domain texture. This was suggested to be related to the existence of an asymmetric internal bias field.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
NASA NTRS2015

Additive Manufacturing of SiC Based Ceramics and Ceramic Matrix Composites

Silicon carbide (SiC) ceramics and SiC fiber reinforcedSiC ceramic matrix composites (SiCSiC CMCs) offer high payoff as replacements for metals in turbine engine applications due to their lighter weight, higher temperature capability, and lower cooling requirements. Additive manufacturing approaches can offer game changing technologies for the quick and low cost fabrication of parts with much greater design freedom and geometric complexity. Four approaches for developing these materials are presented. The first two utilize low cost 3D printers. The first uses pre-ceramic pastes developed as feed materials which are converted to SiC after firing. The second uses wood containing filament to print a carbonaceous preform which is infiltrated with a pre-ceramic polymer and converted to SiC. The other two approaches pursue the AM of CMCs. The first is binder jet SiC powder processing in collaboration with rp+m (Rapid Prototyping+Manufacturing). Processing optimization was pursued through SiC powder blending, infiltration with and without SiC nano powder loading, and integration of nanofibers into the powder bed. The second approach was laminated object manufacturing (LOM) in which fiber prepregs and laminates are cut to shape by a laser and stacked to form the desired part. Scanning electron microscopy was conducted on materials from all approaches with select approaches also characterized with XRD, TGA, and bend testing.

3-D printing↗
DOE OSTI2018

Fabrication and microstructural analysis of ceramic fuel derived from sol-gel and powder routes

Within the Advanced Fuels Campaign the Oak Ridge National Laboratory is looking into the fabrication of enhanced UO 2 fuel candidates. Early in FY18 an open-port glove box line was set up enabling the fabrication and initial characterization of potentially enhanced fuel candidates. The fabrication processes available at the Oak Ridge National Laboratory are unique owing to its UO 3 microsphere feedstock compared to commonly used powder feedstocks. The reported activities demonstrate the feasibility of fabricating advanced UO 2 -Molybdenum ceramics with an enhanced thermal conductivity and high densities. Further development of the fabrication routes and a variety of different dopants is expected to result in a matrix of different advanced fuel candidates. Following initial property screening, the in-reactor performance and suitability of these fuel candidates will be probed in the MiniFuel irradiation set-up at the Oak Ridge National Laboratory.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2020

Developing new alkaline ceramics as possible CO 2 chemisorbents at high temperatures: The lithium and sodium yttriates (LiYO 2 and NaYO 2 ) cases

In this work, lithium and sodium yttriates (LiYO 2 and NaYO 2 ) were synthesized, characterized and tested as possible carbon dioxide (CO 2 ) captors. All the experimental syntheses and analyses were supported by the theoretical thermodynamic calculations, showing that both ceramics would be able to chemisorb CO 2 in a wide temperature range. Therefore, both ceramics were prepared by solid-state reaction and structurally characterized. In fact, the structural characterization evidenced that sodium atoms are located in a octahedral close-packed structure, while lithium ions are not so packed. The lithium ions are, indeed, in a highly distorted tetrahedron, tending to square-planar coordination. Then, based on the theoretical and structural analysis, LiYO 2 and NaYO 2 samples were investigated for the CO 2 capture process through dynamic and isothermal thermogravimetric experiments. All these experiments showed that LiYO 2 has better CO 2 capture properties than NaYO 2 , which was further correlated with the crystal structures of each ceramic. Furthermore, both ceramics presented similar CO 2 capture efficiencies regardless of the CO 2 concentration. Finally, LiYO 2 sample was tested for cyclic CO 2 chemisorption-desorption processes. The obtained results showed that the CO 2 capture efficiency is maintained high at least through 10 cycles. Therefore, these alkaline yttriates seem to present interesting alternatives as high and moderate temperature CO 2 captors, applicable for post-combustion industrial capture processes.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2022

The influence of the processing parameters on the reactive flash sintering of ZrO 2 -CeO 2

Reactive flash sintering (RFS) is a method that was recently developed to produce dense single-phase bulk ceramic parts through solid-state reactions in a single-step that only takes a few minutes. The influence of the RFS parameters on the phase purity of a simple mixed oxide, (Zr 0.8 ,Ce 0.2 )O 2 , was investigated. Parameters such as furnace temperature, furnace atmosphere, electric current density, and alternating current (AC) or direct current (DC) were examined. It was found that (Zr 0.8 ,Ce 0.2 )O 2 pellets with high densities, above 90% of its theoretical density, can be produced by RFS in a few minutes when RFS occurs under oxidizing atmospheres, AC fields with current densities of 100 mA·mm –2 , and at a furnace temperature of 1200°C. Reducing conditions such as Ar-H 2 atmosphere and DC fields, low furnace temperatures, and low current densities resulted in phase impurities and poor reactions between the ZrO 2 and the CeO 2 powders. These results show that RFS is a useful method to produce mixed oxides, but it is very sensitive to the processing parameters. This is the first time that the influence of most of the RFS processing parameters has been studied systematically. Thus, the present work aims to provide guidelines on selecting the right processing parameters when exploring RFS.

36 MATERIALS SCIENCE↗
DOE OSTI2020

A Novel Laser 3D Printing Method for the Advanced Manufacturing of Protonic Ceramics

Protonic ceramics (PCs) with high proton conductivity at intermediate temperatures (300–600 °C) have attracted many applications in energy conversion and storage devices such as PC fuel/electrolysis cells, PC membrane reactors, hydrogen pump, hydrogen or water-permeable membranes, and gas sensors. One of the essential steps for fulfilling the practical utilization of these intermediate-temperature PC energy devices is the successful development of advanced manufacturing methods for cost-effectively and rapidly fabricating them with high energy density and efficiency in a customized demand. In this work, we developed a new laser 3D printing (L3DP) technique by integrating digital microextrusion-based 3D printing and precise and rapid laser processing (sintering, drying, cutting, and polishing), which showed the capability of manufacturing PCs with desired complex geometries, crystal structures, and microstructures. The L3DP method allowed the fabrication of PC parts such as pellets, cylinders, cones, films, straight/lobed tubes with sealed endings, microchannel membranes, and half cells for assembling PC energy devices. The preliminary measurement of the L3DP electrolyte film showed a high proton conductivity of ≈7 × 10−3 S/cm. This L3DP technique not only demonstrated the potential to bring the PCs into practical use but also made it possible for the rapid direct digital manufacturing of ceramic-based devices.

08 HYDROGEN↗
DOE OSTI2021

Unconventional Materials Processing Using Spark Plasma Sintering

Spark plasma sintering (SPS) has gained recognition in the last 20 years for its rapid densification of hard-to-sinter conventional and advanced materials, including metals, ceramics, polymers, and composites. Herein, we describe the unconventional usages of the SPS technique developed in the field. The potential of various new modifications in the SPS technique, from pressureless to the integration of a novel gas quenching system to extrusion, has led to SPS’ evolution into a completely new manufacturing tool. The SPS technique’s modifications have broadened its usability from merely a densification tool to the fabrication of complex-shaped components, advanced functional materials, functionally gradient materials, interconnected materials, and porous filter materials for real-life applications. The broader application achieved by modification of the SPS technique can provide an alternative to conventional powder metallurgy methods as a scalable manufacturing process. The future challenges and opportunities in this emerging research field have also been identified and presented.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Coaxial Ceramic Direct Ink Writing on Heterogenous and Rough Surfaces: Investigation of Core–Shell Interactions

In this work, coaxial conductor–ceramic direct ink writing enables the printing of sensitive or encapsulated materials onto heterogeneous and rough substrates. While encasing the core fluid within a stiff ceramic shell, continuity may be maintained, even while printing onto conventionally challenging substrates. Here, we report the development of a coaxial ceramic direct ink writing suite and explore coflow interrelationships based on microfluidic principles. A coaxial nozzle is designed to facilitate the coextrusion of an alumina shell, whereas indium–tin-oxide inks constitute the core. In this manner, a core–shell ceramic element may be printed onto rough substrates for future high-temperature applications. Colloidal inks are engineered to provide the required rheological and sintering performance. Moreover, flow simulations in conjunction with microfluidic coflow principles are used to explore the coaxial printing processing space, thus controlling the core–shell architectures. Physical modeling is further used to analyze core deformations and eccentricity. As a result, simulations are validated experimentally, and the analyses are used to deposit coaxial ceramic features onto heterogeneous, high-temperature ceramic substrates.

20 FOSSIL-FUELED POWER PLANTS↗
DOE OSTI2026

Refractory-based thermal energy storage for industrial process heat: one-dimensional modeling, control, and optimization

The variable and weather-dependent output of wind and solar power plants present a substantial challenge for planning and operating electricity-systems, particularly in the absence of cost-effective and dispatchable energy storage technologies. This study investigates a high-temperature, electrically heated, refractory-based thermal energy storage (RTES) system that stores electrical energy as sensible heat in dense ceramic bricks over the 950–1800 °C range. The stored heat can be discharged as a controlled hot-gas stream for industrial heating, fuel substitution in high-temperature processes, or electricity generation. The main novelty is a comprehensive modelling, control, mapping, and optimization framework that integrates one-dimensional transient gas–solid heat transfer, fan-assisted discharge, bypass-flow regulation, reheating logic, fan-power evaluation, insulation-loss assessment, and genetic-algorithm-based design optimization. The model uses feedback from outlet temperature and delivered power to regulate discharge, while a two-stage genetic algorithm optimizes brick-channel geometry, gas-flow operation, and multilayer insulation thicknesses. Storage capacities below 50 MWh and discharge powers of 5–30 MW are analyzed to evaluate hold time, thermal delivery, fan-power penalty, heat loss, state-of-charge evolution, and indicative capital cost. Results demonstrate that optimized and well-insulated refractory-based thermal energy storage units can provide stable, efficient, and repeatable heat delivery over multiple discharge cycles. The generated performance and cost maps support modular refractory thermal energy storage as a practical option for large-scale integration of wind and solar generation and for high-temperature industrial process heat.

25 ENERGY STORAGE↗
DOE OSTI2022

Laser 3D printing of highly compacted protonic ceramic electrolyzer stack

Solid oxide electrolysis cells (SOECs) for H 2 production is a core technology for H2@scale. However, its conventional manufacturing methods adapted from the manufacture of solid oxide fuel cells (SOFC) need high cost, especially for small-volume production. The emerging laser 3D printing (L3DP) technology with computer-aided 3D printing and computer-controlled laser processing can fulfill layer-by-layer digital shaping and rapid in-situ consolidating feedstock into complicated geometries. L3DP, a promising additive manufacturing (AM) technology, has achieved significant success in manufacturing plastic and metal parts, which is currently attracting considerable attention for the cost-effective, rapid, and flexible manufacturing of heterogeneous multilayered ceramic devices (e.g., SOECs, SOFCs, and solid-state batteries). It is believed that the L3DP can integrate the advantages of selective consolidation of heterogeneous layers, accurate control of layer microstructures, high processing heat efficiency, high processing speed, high stack compactness, high stack design flexibility, and low stack sealing area for cost-effective, rapid, and flexible manufacturing of SOECs to meet DOE’s electrolyzer target.

08 HYDROGEN↗
NASA NTRS1993

Production of Ultrafine, High-purity Ceramic Powders Using the US Bureau of Mines Developed Turbomill

Turbomilling, an innovative grinding technology developed by the U.S. Bureau of Mines in the early 1960's for delaminating filler-grade kaolinitic clays, has been expanded into the areas of particle size reduction, material mixing, and process reaction kinetics. The turbomill, originally called an attrition grinder, has been used for particle size reduction of many minerals, including natural and synthetic mica, pyrophyllite, talc, and marble. In recent years, an all-polymer version of the turbomill has been used to produce ultrafine, high-purity, advanced ceramic powders such as SiC, Si3N4, TiB2, and ZrO2. In addition to particle size reduction, the turbomill has been used to produce intimate mixtures of high surface area powders and whiskers. Raw materials, TiN, AlN, and Al2O3, used to produce a titanium nitride/aluminum oxynitride (TiN/AlON) composite, were mixed in the turbomill, resulting in strength increases over samples prepared by dry ball milling. Using the turbomill as a leach vessel, it was found that 90.4 pct of the copper was extracted from the chalcopyrite during a 4-hour leach test in ferric sulfate versus conventional processing which involves either roasting of the ore for Cu recovery or leaching of the ore for several days.

Hoyer, Jesse L.↗