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At least 793 records · Page 44

Bi aliovalent substitution in Li 7 La 3 Zr 2 O 12 garnets: Structural and ionic conductivity effects

We report on the synthesis of cubic-phase garnet-type solid-state electrolytes based on Bi-doped Li 7 La 3 Zr 2 O 12 (LLZO). Bi aliovalent substitution of Zr in LLZO utilizing the Pechini processing method is employed to synthesize Li 7-x La 3 Zr 2-x Bi x O 12 compounds. A strong dependence of the ionic conductivity on Bi content is observed, and under our synthesis and sintering conditions, a >100-fold increase over the un-doped sample is observed for x=0.75. Cubic-phase Li 6 La 3 Zr 1 BiO 12 compounds are generated upon annealing in air in the temperature range 650 °C-900 °C. In contrast, in the absence of Bi, the cubic garnet phase of Li 7 La 3 Zr 2 O 12 is not formed below 700 °C and a transformation to the tetragonal phase is observed at similar to 900 °C for this un-doped compound. The role of Bi in lowering the formation temperature of the garnet cubic phase and in the ionic conductivity improvements is investigated in this work. We ascribe the effect of Bi-doping on ionic conductivity increments to changes in Li + -site occupancy and lattice parameters and the reduction in the formation temperature for the cubic-phase formation to rate enhancements of the solid-state reaction. To identify the site occupancy of Bi in the garnet structure, we employ synchrotron extended x-ray absorption fine structure spectroscopy. Our results indicate that Bi additions occupy the Zr-type sites exclusively, to within the accuracy of the measurements.

36 MATERIALS SCIENCE↗

Magnetic and mechanical properties of grain-refined Dy-free Nd-Fe-B sintered magnets

In this work, the effects of grain size on magnetic and mechanical properties of Dy-free Nd-Fe-B sintered magnets were studied. The grain size of the sintered magnets was varied by using different sized Dy-free Nd-Fe-B alloy feedstock powders which were ball milled to different extents. Increasing the ball milling time from 7 to 11 h caused the average particle size of the powders to decrease from 3.6 to 2.1 µm, while the average grain size of the corresponding sintered magnets decreased from 5.0 to 4.0 µm. The intrinsic coercivity Hcj and maximum energy product (BH) max of these magnets increased from 11.6 to 13.7 kOe and 41.6 to 43.6 MGOe, respectively. The finer grain magnets exhibited better thermal stability, as indicated by a smaller temperature coefficient of H cj (-0.71%/°C). With extending ball milling time to 15 h, the magnetic properties of the magnets deteriorate, while the flexural strengths first decrease and then increase. The flexural strength improvement is attributed to the increased Oxygen content in the magnets due to finer grains. The coercivity enhancement by reduction of grain size is a promising approach to develop Dy-free Nd-Fe-B sintered magnets with better thermal stability. It is important to control the Oxygen contents in the magnets to compromise both magnetic and mechanical properties.

36 MATERIALS SCIENCE↗

Characterization of high thermal conductivity fuel surrogates before and after ion irradiation

High thermal conductivity nuclear fuels offer important potential advantages over traditional oxide-based fuels such as higher burnup, reduction in fission gas release, and better overall safety of the system. One proposed approach to high thermal conductivity fuels utilizes high thermal conductivity nonfissile additives with UO 2 fuel to lower the fuel operating temperature and thereby take advantage of the highly favorable radiation resistance of UO 2 at lower operating temperatures. However, differential swelling in the matrix and high conductivity additive phases during high dose irradiation could lead to internal cracking and poor performance. In the current study, ceria (CeO 2 ) and zirconia (ZrO 2 ) surrogate matrices were used to model UO2 behavior. Additives of 10 vol. % Al 2 O 3 or SiC in the form of short fibers or platelets were used for the high conductivity second phase. The nuclear fuel surrogates were sintered to achieve densities greater than 93% of the ideal values. Scanning electron microscopy (SEM) imaging and X-ray diffraction confirmed the uniform distribution of the second phase and that no intermetallic second phase was formed during sintering. The thermal conductivity of the sintered samples was measured from 50 °C to 900 °C and confirmed the desirable increase compared to pure CeO 2 /ZrO 2 pellets. Samples were irradiated with 20 MeV Ni 6+ ions at midrange doses ranging from 1 to 15 displacements per atom (dpa) and temperatures from 300 °C to 700 °C. Post irradiation characterization revealed a good stability of the samples at low to medium doses with matrix lattice parameter swelling of < 0.14 % but showed a significant microstructural deterioration and decrease of the mechanical properties at 15 dpa.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Novel refractory high-entropy metal-ceramic composites with superior mechanical properties

A new concept of refractory high-entropy metal-ceramic composites (HEMCC) has been proposed that combines the outstanding physical properties of both high-entropy alloy (HEA) and high-entropy ceramic (HEC). As the first HEMCC system, to the best of our knowledge, TiTaNbZr-(TiTaNbZr)C, has been developed by a powder metallurgy process. The HEA and HEC phases exhibit body-centered cubic (BCC) and rock-salt B1 crystal structures, respectively, and both phases have non-equimolar chemical compositions. Further, with the increase of the HEC phase in HEMCC, the hardness is enhanced while the density and fracture toughness are decreased. HEA50C sintered from 50vol% HEA and 50vol% HEC precursor powders shows a favorable combination of flexural strength (541±48MPa) and fracture toughness (6.93±0.27 MPa·m 1/2 ) at room temperature and a high compressive strength at 1300ºC (275MPa). The optimized mechanical performance of HEMCC might be attributed to the combination of the ductile HEA and strong HEC phases, smaller grain size, and crack arrest at HEC/HEA interfaces.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

High hardness and oxidation-resistant Cr-containing medium entropy ZrTaW diboride

This study reports the successful synthesis of a Cr-containing (Zr 0.30 Ta 0.34 Cr 0.06 W 0.30 )B 2 medium-entropy boride (MEB) via an in-situ reactive borothermal reduction route from oxide precursors. High-energy ball milling was employed to homogenize the precursor mixture prior to reactive densification. X-ray diffraction confirmed the formation of a predominantly AlB₂-type hexagonal diboride structure together with a secondary (W X , M 1-X )B monoboride phase. Microstructural characterization revealed compositional heterogeneity and localized W-rich regions associated with the secondary phase. The synthesized medium-entropy boride exhibited enhanced mechanical properties, which are attributed to lattice distortion and solid-solution strengthening effects. Thermogravimetric analysis revealed complex multistage oxidation behavior, and the oxidation resistance was compared with conventional ultra-high-temperature diborides. The results demonstrate the strong relationship between oxide-derived processing, compositional complexity, phase evolution, and oxidation behavior, highlighting the potential of medium-entropy borides for high-temperature structural applications

36 MATERIALS SCIENCE↗

Pressure sintering of Si3N4-Al2O3 /Sialon/

Essentially pore-free Sialon bodies were obtained by pressure sintering for three blends (mol ratios of 4:1, 2:3, and 3:2) of Si3N4 and Al2O3 powders under the conditions of 27.6 MN/sq m and a temperature of 1700 C for 2 h. These dense bodies consist mainly of a Sialon solid solution with a minor amount of a particular second phase. The higher the Al2O3 content (20 to 60 mol% range) in Sialon, the higher the densification rate. Fully dense bodies can be obtained at temperatures as low as 1500 C at 27.6 MN/sq m for 2 h with no second phase detectable by X-ray diffraction. A 100% dense body can be obtained by heating at 1700 C at 27.6 MN/sq m without a holding time.

Yeh, H. C.↗

Crystallization, flow and thermal histories of lunar and terrestrial compositions

Contents: a kinetic treatment of glass formation; effects of nucleating heterogeneities on glass formation; glass formation under continuous cooling conditions; crystallization statistics; kinetics of crystal nucleation; diffusion controlled crystal growth; crystallization of lunar compositions; crystallization between solidus and liquidus; crystallization on reheating a glass; temperature distributions during crystallization; crystallization of anorthite and anorthite-albite compositions; effect of oxidation state on viscosity; diffusive creep and viscous flow; high temperature flow behavior of glass-forming liquids, a free volume interpretation; viscous flow behavior of lunar compositions; thermal history of orange soil material; breccias formation by viscous sintering; viscous sintering; thermal histories of breccias; solute partitioning and thermal history of lunar rocks; heat flow in impact melts; and thermal histories of olivines.

Uhlmann, D. R.↗

Design, fabrication and test of liquid metal heat-pipe sandwich panels

Integral heat-pipe sandwich panels, which synergistically combine the thermal efficiency of heat pipes and the structural efficiency of honeycomb sandwich panel construction, were fabricated and tested. The designs utilize two different wickable honeycomb cores, facesheets with screen mesh sintered to the internal surfaces, and potassium or sodium as the working fluid. Panels were tested by radiant heating, and the results indicate successful heat pipe operation at temperatures of approximately 922 K (1200 F). These panels, in addition to solving potential thermal stress problems in an Airframe-Integrated Scramjet Engine, have potential applications as cold plates for electronic component cooling, as radiators for space platforms, and as low distortion, large area structures.

Basiulis, A.↗

Design, fabrication and test of liquid metal heat-pipe sandwich panels

Integral heat-pipe sandwich panels, which synergistically combine the thermal efficiency of heat pipes and the structural efficiency of honeycomb sandwich panel construction, were fabricated and tested. The designs utilize two different wickable honeycomb cores, facesheets with screen mesh sintered to the internal surfaces, and potassium or sodium as the working fluid. Panels were tested by radiant heating, and the results indicate successful heat pipe operation at temperatures of approximately 922K (1200F). These panels, in addition to solving potential thermal stress problems in an Airframe-Integrated Scramjet Engine, have potential applications as cold plates for electronic component cooling, as radiators for space platforms, and as low distortion, large area structures.

Basiulis, A.↗

Metallurgical and mechanical phenomena due to rubbing of titanium against sintered powder Nichrome

Metallurgical and mechanical changes occurring during high-speed rubbing of Ti-6Al-4V blade specimens against an abradable Nichrome aircraft engine seal material were studied using optical microscopy, electron microscopy, and microhardness techniques. Evidence of temperatures above the beta transus of Ti-6Al-4V (1000 C) and of thermal hardening was found on blade tips that exhibited undesirable abrading characteristics resulting in high forces of interaction, high temperatures, and smearing. The material within the layer of the corresponding seals was found to be work-hardened to a depth of about 0.1 mm and showed evidence of densification extending to a depth of about 0.5 mm below the rubbed surface. Wear particles produced by rub interactions that generated cleanly abraded seal surfaces were found to be several times larger than those produced during interactions which showed evidence of surface smearing and seal densification.

Zenas, R.↗

Flaw imaging and ultrasonic techniques for characterizing sintered silicon carbide

The capabilities were investigated of projection microfocus x-radiography, ultrasonic velocity and attenuation, and reflection scanning acoustic microscopy for characterizing silicon carbide specimens. Silicon carbide batches covered a range of densities and different microstructural characteristics. Room temperature, four point flexural strength tests were conducted. Fractography was used to identify types, sizes, and locations of fracture origins. Fracture toughness values were calculated from fracture strength and flaw characterization data. Detection capabilities of radiography and acoustic microscopy for fracture-causing flaws were evaluated. Applicability of ultrasonics for verifying material strength and toughness was examined.

Baaklini, George Y.↗

Radiographic and ultrasonic characterization of sintered silicon carbide

The capabilities were investigated of projection microfocus X-radiography, ultrasonic velocity and attenuation, and reflection scanning acoustic microscopy for characterizing silicon carbide specimens. Silicon carbide batches covered a range of densities and different microstructural characteristics. Room temperature, four point flexural strength tests were conducted. Fractography was used to identify types, sizes, and locations of fracture origins. Fracture toughness values were calculated from fracture strength and flaw characterization data. Detection capabilities of radiography and acoustic microscopy for fracture-causing flaws were evaluated. Applicability of ultrasonics for verifying material strength and toughness was examined.

Baaklini, G. Y.↗

Copper Chloride Cathode For Liquid-Sodium Cell

Rechargeable liquid-sodium cell with copper chloride cathode offers substantial increase in energy density over cells made with other cathode materials. Unit has theoretical maximum energy density of 1135 W.h/kg. Generates electricity by electrochemical reaction of molten sodium and solid copper chloride immersed in molten electrolyte, sodium tetrachloroaluminate at temperature of equal to or greater than 200 degrees C. Wall of alumina tube separates molten electrolyte from molten sodium anode. Copper chloride cathode embedded in pores of sintered nickel cylinder or directly sintered.

Bugga, Ratnakumar V.↗

Lithological Variation with Depth and Decoupling of Maturity Parameters in Apollo 16 Regolith Core 68001/2

Using FerroMagnetic Resonance (FMR) and Instrumental Neutron Activation Analysis (INAA), we have determined the maturity (surface exposure) parameter I(sub s)/FeO and concentrations of twenty- five chemical elements on samples taken every half centimeter down the 61-cm length of the 68001/2 regolith core (double drive tube) collected at station 8 on the Apollo 16 mission to the Moon. Contrary to premission expectations, no ejecta or other influence from South Ray crater is evident in the core, although a small inflection in the I(sub s)/FeO profile at 3 cm depth may be related the South Ray crater impact. Regolith maturity generally decreases with depth, as in several previously studied cores. We recognize five compositionally distinct units in the core, which we designate A through E, although all are similar in composition to each other and to other soils from the Cayley plains at the Apollo 16 site. Unit A (0-33 cm) is mature to submature throughout (I(sub s)/FeO: 89-34 units) and is indistinguishable in composition from surface soils collected at station 8. Unit B (33-37 cm) is enriched slightly in a component of anorthositic norite composition. Unit D (42-53 cm) is compositionally equivalent to 80 wt% Unit-A soil plus 20 wt% Apollo-16-type dimict breccia consisting of subequal parts anorthosite and impact-melt breccia. Compared to Unit A, Unit E (53-61 cm) contains a small proportion (up to 4%) of some component compositionally similar to Apollo 14 sample 14321. Unit C (37-42 cm) is unusual. For lithophile and siderophile elements, it is similar to Units A and D. However, I(sub s)/FeO is low throughout the unit (less than 30 units) and in a bluish-gray zone at 41 cm depth I(sub s)/FeO drops to 1.6 units, the lowest value that we have observed in several hundred Apollo 16 soil samples. Samples from the bluish-gray zone also have low Zn concentrations, less than 10 micro g/g, compared to 20-30 micro g/g for the rest of the core. Although both values are consistent with fragmented rock material that has received virtually no surface exposure, the abundance of agglutinates in the bluish-gray soil of Unit C is moderately high, typical of a submature soil that would ordinarily have I(sub s)/FeO - 30. We believe that the anomalously low values of I(sub s)/FeO and Zn concentration result because the soil was heated to -800-1000 'C, probably during an impact. This temperature range is sufficient to volatize the surface-correlated Zn and agglomerate the nanophase metal giving rise to the FMR signal but is not great enough to sinter the soil. Alternatively, the unusual soil interval may represent a disaggregated or incipient regolith breccia, although there is no significant difference in the texture or clast-matrix relationships between Unit C and adjacent units.

Korotev, Randy L.↗

Advancements in Binder Systems for Solid Freeform Fabrication

Paper will present recent developments in advanced material binder systems for solid freeform fabrication (SFF) technologies. The advantage of SFF is the capability to custom fabricate complex geometries directly from computer aided design data in layer- by-layer fashion, eliminated the need for traditional fixturing and tooling. Binders allow for the low temperature processing of 'green' structural materials, either metal, ceramic or composite, in traditional rapid prototyping machines. The greatest obstacle comes when green parts must then go through a sintering or burnout process to remove the binders and fully densify the parent material, without damaging or distorting the original part geometry. Critical issues and up-to-date assessments will be delivered on various material systems.

Cooper, Ken↗

Induction ultrafast sintering

This study proposes and demonstrates induction ultrafast sintering (IUS), which enables rapid densification of refractory and other materials via two contactless modalities: direct IUS (d-IUS), where heating occurs through electromagnetic coupling with the sample, and susceptor IUS (s-IUS), where heating is achieved indirectly via an induction-heated metal case. Ultrahigh heating rates of ∼75 to >450 °C/s and temperatures exceeding 2500 °C are readily achieved. Both d-IUS and s-IUS densify molybdenum to high densities within 120 s, with only ∼1–3 % porosity observed by image analysis. Similarly, 3 mol % yttria-stabilized zirconia (3YSZ) reaches ∼97 % relative density in 30 s via s-IUS. This study further demonstrates ultrafast reactive sintering of two difficult-to-sinter materials: a refractory compositionally complex alloy–carbide (RCCA–CCC) composite, NbMoTaW–(Nb 0.37 Mo 0.11 Ta 0.39 W 0.13 ) 2 C, using d-IUS, and a compositionally complex silicide (CCS), (Mo 1/3 Nb 1/3 Zr 1/3 )Si 2 , using s-IUS. This IUS platform offers a versatile route for high-throughput materials discovery and energy-efficient fabrication of bulk refractory materials.

36 MATERIALS SCIENCE↗

Amorphous complexion-aided sintering enables scalable processing of bulk nanocrystalline Cu-Zr with high strength and compressive plasticity

Nanocrystalline alloys can have exceptional strengths, yet due to limited microstructural stability it is difficult to fabricate bulk pieces through traditional processing routes that retain nanosized grains. In this study, centimeter-sized Cu-Zr alloy pellets were fabricated via a simple and improved powder metallurgy processing route. Different consolidation temperatures and times were employed to investigate the effect of amorphous grain boundary complexions on densification and the resulting mechanical properties. Bulk compression tests were carried out, with the samples that were hot pressed at 900 °C for 10 h exhibiting an excellent combination of average yield strength of 722 ± 45 MPa and average failure strain of 25.3 ± 2.4 %. Furthermore, we find that a powder processing route which enables amorphous complexion-assisted sintering leads to samples that (1) reach full density without requiring quenching treatments or other complex processing, (2) demonstrate appreciable plasticity, and (3) have strength that competes with commercially available high-strength Cu alloys.

Bulk nanocrystalline alloy↗

Wireless Passive Ceramic Sensor for Far-Field Temperature Measurement at High Temperatures

A passive wireless high-temperature sensor for far-field applications was developed for stable temperature sensing up to 1000 °C. The goal is to leverage the properties of electroceramic materials, including adequate electrical conductivity, high-temperature resilience, and chemical stability in harsh environments. Initial sensors were fabricated using Ag for operation to 600 °C to achieve a baseline understanding of temperature sensing principles using patch antenna designs. Fabrication then followed with higher temperature sensors made from (In, Sn) O2 (ITO) for evaluation up to 1000 °C. A patch antenna was modeled in ANSYS HFSS to operate in a high-frequency region (2.5–3.5 GHz) within a 50 × 50 mm2 confined geometric area using characteristic material properties. The sensor was fabricated on Al2O3 using screen printing methods and then sintered at 700 °C for Ag and 1200 °C for ITO in an ambient atmosphere. Sensors were evaluated at 600 °C for Ag and 1000 °C for ITO and analyzed at set interrogating distances up to 0.75 m using ultra-wideband slot antennas to collect scattering parameters. The sensitivity (average change in resonant frequency with respect to temperature) from 50 to 1000 °C was between 22 and 62 kHz/°C which decreased as interrogating distances reached 0.75 m.

47 OTHER INSTRUMENTATION↗