Sacrificial Synthesis of Supported Ru Single Atoms and Clusters on N-doped Carbon Derived from Covalent Triazine Frameworks: A Charge Modulation Approach
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99 GENERAL AND MISCELLANEOUS↗
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Twisted-layer boron nitride ceramic with high deformability and strength
Moiré superlattices formed by twisted stacking in van der Waals materials have emerged as a new platform for exploring the physics of strongly correlated materials and other emergent phenomena. However, there remains a lack of research on the mechanical properties of twisted-layer van der Waals materials, owing to a lack of suitable strategies for making three-dimensional bulk materials. Here we report the successful synthesis of a polycrystalline boron nitride bulk ceramic with high room-temperature deformability and strength. This ceramic, synthesized from an onion-like boron nitride nanoprecursor with conventional spark plasma sintering and hot-pressing sintering, consists of interlocked laminated nanoplates in which parallel laminae are stacked with varying twist angles. The compressive strain of this bulk ceramic can reach 14% before fracture, about one order of magnitude higher compared with traditional ceramics (less than 1% in general), whereas the compressive strength is about six times that of ordinary hexagonal boron nitride layered ceramics. The exceptional mechanical properties are due to a combination of the elevated intrinsic deformability of the twisted layering in the nanoplates and the three-dimensional interlocked architecture that restricts deformation from propagating across individual nanoplates. The advent of this twisted-layer boron nitride bulk ceramic opens a gate to the fabrication of highly deformable bulk ceramics.
36 MATERIALS SCIENCE↗
Diminiode thermionic energy conversion with lanthanum-hexaboride electrodes
Thermionic conversion data obtained from a variable gap cesium diminiode with a hot pressed, sintered lanthanum hexaboride emitter and an arc melted lanthanum hexaboride collector are presented. Performance curves cover a range of temperatures: emitter 1500 to 1700 K, collector 750 to 1000 K, and cesium reservoir 370 to 510 K. Calculated values of emitter and collector work functions and barrier index are also given.
Kroeger, E. W.↗
Opacified silica reusable surface insulation /RSI/ for thermal protection of the Space Shuttle Orbiter
The present paper deals with a second-generation reusable surface insulation (RSI) material, termed LI-2200, which has been chosen for use on limited areas of the Orbiter heat shield. It is a rigid sintered fibrous silica containing about 3% by weight 1200 grit silicon carbide powder, capable of surviving multiple reentries at temperatures on the order of 1400 C. The lower thermal conductivity achieved by opacification with silicon carbide is demonstrated by radiant transmission measurements and thermal response tests.
Goldstein, H. E.↗
Research on ultra-high-temperature materials, monolithic ceramics, ceramic matrix composites and carbon/carbon composites
Research on three classes of materials that show potential for allowing significant increases in operating temperatures in gas turbine engines is discussed. Monolithic ceramics, ceramic matrix composites, and carbon-carbon composites are discussed. Sintering, hot pressing, and densification are discussed.
T. J. Miller↗
New Technology for Microfabrication and Testing of a Thermoelectric Device for Generating Mobile Electrical Power
Thermoelectric (TE) power generation is an increasingly important power generation technology. Major advantages include: no moving parts, low-weight, modularity, covertness/silence, high power density, low amortized cost, and long service life with minimum or no required maintenance. Despite low efficiency of power generation, there are many specialized needs for electrical power that TE technologies can uniquely and successfully address. Recent advances in thermoelectric materials technology have rekindled acute interest in thermoelectric power generation. We have developed single crystalline n- and p- type PbTe crystals and are also, developing PbTe bulk nanocomposites using PbTe nano powders and emerging filed assisted sintering technology (FAST). We will discuss the materials requirements for efficient thermoelectric power generation using waste heat at intermediate temperature range (6500 to 8500 K). We will present our recent results on production of n- and p- type PbTe crystals and their thermoelectric characterization. Relative characteristics and performance of PbTe bulk single crystals and nano composites for thermoelectric power generation will be discussed.
Prasad, Narasimha S.↗
Electron Bombardment on Dione: Surface Compositional Effects and Temperature Anomalies
Saturn’s icy moons are composed primarily of water ice with minor other “contaminants,” such as CO2 ice, and a dark component thought to be organics, hematite and/or metallic Fe [1]. The space weathering process of electron bombardment is expected to be particularly important on the surfaces of Saturn’s inner moons (Mimas, Tethys, Dione, and Rhea), as they orbit within Saturn’s inner magnetosphere. Terrains exhibiting thermal anomalies (i.e., colder temperatures in the day and warmer temperatures at night than surrounding areas) correspond to regions of high energy electron bombardment [2; 3; 4; 5]. Energetic electrons impact the surfaces, sintering ice grains together, and this process becomes more effective for increasing particle energies [6]. Solar UV radiation, cosmic rays, dust in-fall, and cold plasma particles trapped in Saturn’s magnetic field also play an important role in altering the nature and the structure of the native surface ices by the implantation of contaminants, ionization, sputtering, and dissociation of water ice molecules [7]. Additionally, CO2 could be sourced from irradiation of dark organic material [8]. Many of these surface alterations are observable in Cassini’s Visible and Infrared Mapping Spectrometer (VIMS) spectra [9]. We used similar methodologies as have been employed in previous works [e.g., 10] to derive surface temperatures from Cassini’s Composite Infrared Spectrometer (CIRS), which helped to isolate areas where space weathering due to electron bombardment is more predominant. The subtle changes in VIMS spectra were investigated using machine learning techniques. We present here our results for Dione.
Cindy Lee Young↗
Electron Bombardment on Dione: Surface Compositional Effects and Temperature Abnormalities
Saturn’s icy moons are composed primarily of water ice with minor other “contaminants,” such as CO2 ice, and a dark component thought to be organics, hematite and/or metallic Fe [1]. The space weathering process of electron bombardment is expected to be particularly important on the surfaces of Saturn’s inner moons (Mimas, Tethys, Dione, and Rhea), as they orbit within Saturn’s inner magnetosphere. Terrains exhibiting thermal anomalies (i.e., colder temperatures in the day and warmer temperatures at night than surrounding areas) correspond to regions of high energy electron bombardment [2; 3; 4; 5]. Energetic electrons impact the surfaces, sintering ice grains together, and this process becomes more effective for increasing particle energies [6]. Solar UV radiation, cosmic rays, dust in-fall, and cold plasma particles trapped in Saturn’s magnetic field also play an important role in altering the nature and the structure of the native surface ices by the implantation of contaminants, ionization, sputtering, and dissociation of water ice molecules [7]. Additionally, CO2 could be sourced from irradiation of dark organic material [8]. Many of these surface alterations are observable in Cassini’s Visible and Infrared Mapping Spectrometer (VIMS) spectra [9]. We used similar methodologies as have been employed in previous works [e.g., 10] to derive surface temperatures from Cassini’s Composite Infrared Spectrometer (CIRS), which helped to isolate areas where space weathering due to electron bombardment is more predominant. The subtle changes in VIMS spectra were investigated using machine learning techniques. We present here our results for Dione. [1] Clark, R. N., et al. (2012) Icarus, 218, 831–860 [2] Howett, C. J. A., et al. (2020) Icarus, 113745 [3] Nordheim, T. A., et al. (2017) Icarus, 286, 56-68 [4] Paranicas, C., et al. (2012) Planetary and Space Science, 61, 60–65 [5] Paranicas, C., et al. (2014) Icarus, 234, 155–161 [6] Schaible, M. J., et al. (2016) Icarus, 0, 1–13 [7] Baragiola, R. A., et al., (2013) Astrophysics and Space Science Library, vol. 356. Springer [8] Mennella, V., et al. (2006) The Astrophysical Journal, 643(2), 923 [9] Scipioni, F., et al. (2017) Icarus, 290, 183-200 [10] Howett, C. J. A., et al. (2014) Icarus, 241, 239-247
C L Young↗
Revealing Sintering Kinetics of MoS 2 -Supported Metal Nanocatalysts in Atmospheric Gas Environments via Operando Transmission Electron Microscopy
The decoration of two-dimensional (2D) substrates with nanoparticles (NPs) serve as heterostructures for various catalysis applications. Deep understanding of catalyst degradation mechanisms during service conditions is crucial to improve the catalyst durability. In this work, we studied the sintering behavior of Pt and bimetallic Au-core Pt-shell (Au@Pt core–shell) NPs on MoS 2 supports at high temperatures under vacuum, nitrogen (N 2 ), hydrogen (H 2 ), and air environments by in situ gas-cell transmission electron microscopy (TEM). The key observations are summarized as effect of environment: while particle migration and coalescence (PMC) was the main mechanism that led to Pt and Au@Pt NPs degradation under vacuum, N 2 , and H 2 environments, the degradation of MoS 2 substrate was prominent under exposure to air at high temperatures. Pt NPs were less stable in H 2 environment when compared with the Pt NPs under vacuum or N 2 , due to Pt–H interactions that weakened the adhesion of Pt on MoS 2 . Effect of NP composition: under H 2 , the stability of Au@Pt NPs was higher in comparison to Pt NPs. This is because H 2 promotes the alloying of Pt–Au, thus reducing the number of Pt at the surface (reducing H 2 interactions) and increasing Pt atoms in contact with MoS 2 . Effect of NP size: The alloying effect promoted by H 2 was more pronounced in small size Au@Pt NPs resulting in their higher sintering resistance in comparison to large size Au@Pt NPs and similar size Pt NPs. The present work provides key insights into the parameters affecting the catalyst degradation mechanisms on 2D supports.
2D materials↗
Development of Si3N4 and SiC of improved toughness
The application of energy absorbing surface layers to Si3N4 and SiC was investigated. Among the layers studied were microcracked materials such as iron titanate and a silica-zircon mixture and porous materials such as reaction sintered Si3N4. Energy absorption due to microcrack extension upon impact was found not to be an important mechanism. Instead, the fivefold improvement in Charpy and ballistic impact at elevated temperature (1250 C and 1370 C) found for Fe2TiO5 was due to plastic deformation while similar improvement found for silica-zircon mixtures at RT was due to crushing of the porous material. Due to thermal expansion mismatch, these two materials could not withstand thermal cycling when used as energy absorbing surface layers on Si3N4. Reaction sintered Si3N4 layers on dense Si3N4 were found to give up to a sevenfold increase in ballistic impact resistance due to crushing of the layer upon impact. High porosity (45%), large particle size R.S. Si3N4 layers fabricated from -100, +200 mesh Si powder gave better impact improvement than less porous (30%), small particle size layers fabricated from -325 mesh Si powder.
Brennan, J. J.↗
Static and dynamical Meissner force fields
The coupling between copper-based high temperature superconductors (HTS) and magnets is represented by a force field. Zero-field cooled experiments were performed with several forms of superconductors: 1) cold-pressed sintered cylindrical disks; 2) small particles fixed in epoxy polymers; and 3) small particles suspended in hydrocarbon waxes. Using magnets with axial field symmetries, direct spatial force measurements in the range of 0.1 to 10(exp 4) dynes were performed with an analytical balance and force constants were obtained from mechanical vibrational resonances. Force constants increase dramatically with decreasing spatial displacement. The force field displays a strong temperature dependence between 20 and 90 K and decreases exponentially with increasing distance of separation. Distinct slope changes suggest the presence of B-field and temperature-activated processes that define the forces. Hysteresis measurements indicated that the magnitude of force scales roughly with the volume fraction of HTS in composite structures. Thus, the net force resulting from the field interaction appears to arise from regions as small or smaller than the grain size and does not depend on contiguous electron transport over large areas. Results of these experiments are discussed.
Weinberger, B. R.↗
Mechanical Behavior of Neutron Irradiated Refractory Multi-Principal Element Alloys Processed via Spark Plasma Sintering
The search for advanced materials capable of withstanding the extreme conditions of Generation IV reactors is a critical area in materials science research. These reactors operate under severe environments, including high temperatures, corrosion, stress, and irradiation damage. Consequently, there is a need for innovative alloy systems to ensure the reliability and longevity of proposed Generation IV reactor components. Refractory multi-principal-element alloys (RMPEA) have emerged as a promising candidate due to their exceptional properties. These alloys, characterized by their composition of multiple principal elements in near-equiatomic ratios, exhibit superior resistance to irradiation damage, reduced void swelling, enhanced microstructural stability, and minimal irradiation-induced hardening. While initial studies on RMPEAs have shown promising results, most research has been limited to thin films, nanocrystalline microstructures, and ion irradiation, which do not accurately represent the behavior of bulk materials. To address this gap, our research focused on the neutron irradiation of bulk RMPEAs. We aim to conduct comprehensive post-irradiation examinations (PIE) of RMPEAs irradiated at the Advanced Test Reactor at Idaho National Laboratory. The RMPEAs were synthesized using spark plasma sintering (SPS) with mechanically alloyed metallurgical powder. The RMPEA specimens are a MoNbTi alloy system with additions of -Zr, and -ZrV. Furthermore, PIE consisted of mechanical testing and advanced materials characterization. The mechanical testing consisted of sub-sized tensile testing, micro- and nano- indentation. Microstructural characterization included scanning electron microscopy and transmission electron microscopy. Mechanical testing coupled with advanced microscopy techniques provides insight into phase morphology and its effects on the mechanical properties of the RMPEA specimens. The results indicate that both pristine and irradiated RMPEA specimens exhibited brittle behavior during tensile testing, which can be attributed to their heterogeneous microstructure. The SPS manufacturing process did not include any post treatment, which resulted in a heterogeneous microstructure. Energy-dispersive X-ray spectroscopy revealed the presence of intermetallic such as laves phases within the microstructure. Specifically, Ti-rich precipitates were observed in the MoNbTi specimen, while Mo-rich precipitates were found in the MoNbTiZrV specimen. Nano-hardness testing of pristine samples showed that the laves phases exhibited higher hardness values compared to the matrix phase, suggesting that precipitate hardening is likely the dominant hardening mechanism in these specimens. The results from this work will be used to build a finite element model to predict mechanical behavior of future MPEA compositions. Thus, enabling for a streamlined approach to developing novel MPEAs for the nuclear industry.
36 - MATERIALS SCIENCE↗
Effect of Ni content in Cu 1-x Ni x coating on microstructure evolution and mechanical properties of W/Mo joint via low-temperature diffusion bonding
The 93W and Mo1 refractory metals were bonded with different Cu 1- x Ni x coating interlayers of various Ni content using plasma-activated sintering at 700 °C. The effects of the Ni content in the Cu 1- x Ni x coating interlayer on the interfacial microstructure evolution and mechanical properties of the W/Mo joints were studied. The maximum average shear strength of the W/Mo joint was 316.5 MPa when the Ni content of the Cu 1- x Ni x coating interlayer was 25 %. When the Ni content of the Cu 1- x Ni x coating interlayer was below 50 %, the atomic diffusion at the W/Mo joint interface was adequate without the formation of intermetallic compounds, as demonstrated by the High Resolution Transmission Electron Microscope analyses of the joints. The presence of Ni in Cu 1- x Ni x promoted diffusion bonding at the interface, which contributed to the high mechanical properties of the W/Mo joint. With an increase in the Ni content of the Cu 1- x Ni x coating interlayer, the MoNi intermetallic compound (IMC) nucleated and grew at the Cu 1- x Ni x coating/Mo1 interface. When the Ni content of the Cu 1- x Ni x coating interlayer was above 50 %, the generation of a brittle MoNi IMC weakened the shear strength of the W/Mo joint dramatically.
36 MATERIALS SCIENCE↗
Grain growth kinetics in liquid-phase-sintered zinc oxide-barium oxide ceramics
Grain growth of ZnO in the presence of a liquid phase of the ZnO-BaO system has been studied for temperatures from 1300 to 1400 C. The specimens were treated in boiling water and the grains were separated by dissolving the matrix phase in an ultrasonic bath. As a consequence 3D grain size measurements were possible. Microstructural examination shows some grain coalescence with a wide range of neck size ratios and corresponding dihedral angles, however, most grains are isolated. Lognormal grain size distributions show similar shapes, indicating that the growth mechanism is invariant over this time and temperature. All regressions between G exp n and time for n = 2 and 3 proved statistically significant. The rate constants calculated with the growth exponent set to n = 3 are on the same order of magnitude as in metallic systems. The apparent activation energy for growth is estimated between 355 and 458 kJ/mol.
Yang, Sung-Chul↗
Feasibility of Actively Cooled Silicon Nitride Airfoil for Turbine Applications Demonstrated
Nickel-base superalloys currently limit gas turbine engine performance. Active cooling has extended the temperature range of service of nickel-base superalloys in current gas turbine engines, but the margin for further improvement appears modest. Therefore, significant advancements in materials technology are needed to raise turbine inlet temperatures above 2400 F to increase engine specific thrust and operating efficiency. Because of their low density and high-temperature strength and thermal conductivity, in situ toughened silicon nitride ceramics have received a great deal of attention for cooled structures. However, the high processing costs and low impact resistance of silicon nitride ceramics have proven to be major obstacles for widespread applications. Advanced rapid prototyping technology in combination with conventional gel casting and sintering can reduce high processing costs and may offer an affordable manufacturing approach. Researchers at the NASA Glenn Research Center, in cooperation with a local university and an aerospace company, are developing actively cooled and functionally graded ceramic structures. The objective of this program is to develop cost-effective manufacturing technology and experimental and analytical capabilities for environmentally stable, aerodynamically efficient, foreign-object-damage-resistant, in situ toughened silicon nitride turbine nozzle vanes, and to test these vanes under simulated engine conditions. Starting with computer aided design (CAD) files of an airfoil and a flat plate with internal cooling passages, the permanent and removable mold components for gel casting ceramic slips were made by stereolithography and Sanders machines, respectively. The gel-cast part was dried and sintered to final shape. Several in situ toughened silicon nitride generic airfoils with internal cooling passages have been fabricated. The uncoated and thermal barrier coated airfoils and flat plates were burner rig tested for 30 min without and with air cooling. Without cooling, the surface temperature of the flat plate reached approximately 2350 F. Starting with computer aided design (CAD) files of an airfoil and a flat plate with internal cooling passages, the permanent and removable mold components for gel casting ceramic slips were made by stereolithography and Sanders machines, respectively. The gel-cast part was dried and sintered to final shape. Several in situ toughened silicon nitride generic airfoils with internal cooling passages have been fabricated. The uncoated and thermal barrier coated airfoils and flat plates were burner rig tested for 30 min without and with air cooling. Without cooling, the surface temperature of the flat plate reached approximately 2350 F. With cooling, the surface temperature decreased to approximately 1910 F--a drop of approximately 440 F. This preliminary study demonstrates that a near-net-shape silicon nitride airfoil can be fabricated and that silicon nitride can sustain severe thermal shock and the thermal gradients induced by cooling and, thus, is a viable candidate for cooled components.
Bhatt, Ramakrishna T.↗
Producing Zirconium Diboride Components with Complex, Near-Net Shape Geometries by Aqueous Room-Temperature Injection Molding
Room-temperature injection molding is proposed as a novel, low-cost and more energy efficient manufacturing process capable of forming complex-shaped zirconium diboride (ZrB2) parts. This innovative processing method utilized aqueous suspensions with high powder loading and a minimal amount (5 vol.) of water-soluble polyvinylpyrrolidone (PVP), which was used as a viscosity modifier. Rheological characterization was performed to evaluate the room-temperature flow properties of ZrB2-PVP suspensions. ZrB2 specimens were fabricated with high green body strength and were machinable prior to binder removal despite their low polymer content. After binder burnout and pressureless sintering, the bulk density and microstructure of specimens were characterized using Archimedes technique and scanning electron microscopy. X-Ray Diffraction was used to determine the phase compositions present in sintered specimens. Ultimate strength of sintered specimens will be determined using ASTM C1323-10 compressive C-ring test.
Near-Net Shape Forming↗
Development of a Laser Ultrasonics-based Approach for Rapid Screening of High Entropy Alloys
This project utilized a laser ultrasonic technique to systematically study temperature-induced evolution of material properties in a set of interrelated binary alloys and a high entropy alloy (HEA) fabricated using arc-melting and spark plasma sintering processes. This technique involved the use of a nanosecond duration, high-intensity pulsed laser to thermo-elastically generate ultrasonic waves that propagate in the bulk of the metal alloy. Sub-nanometer-scale displacements associated with the propagating bulk ultrasonic waves were detected along the epicenter on the opposite surface of the sample using a 1 GHz bandwidth photorefractive interferometer. Phase transformations and microstructural changes were inferred from the temperature-dependent trends in the bulk acoustic velocities and features in the ultrasonic epicentral waveforms measured in the binary alloys. These inferences were then correlated with electron/optical microscopy observations and predictions using calculations of phase diagrams (CALPHAD). The results showed that the laser-generated ultrasonic pulses were strongly influenced by changes in material microstructure and could accurately track thermally driven phase transformations and detect the presence of microscale heterogeneities (grain boundaries, dendritic structures, etc.) in the set of binary alloy samples. The measurement approach was then applied to a quinary HEA sample for estimating phase transition temperature and determining microstructural heterogeneity. The rapid, non-contact and non-destructive ultrasonic testing approach demonstrated here is amenable to high throughput combinatorial investigations that can be applied to graded composition HEAs produced using advanced manufacturing methods. When paired with atomistic simulations and CALPHAD modeling, this approach can overcome the bottlenecks faced by current material characterization methods in efficiently screening the vast discovery space of HEAs that spans over a hundred million unique quinary alloy compositions.
36 MATERIALS SCIENCE↗
Spark plasma sintering of fuel meats for U 3 O 8 based dispersion fuels
Research and test reactors often use dispersion-type fuel due to its increased thermal conductivity and burn-up capabilities compared to conventional fuel. Al-U 3 O 8 (aluminumtriuranium octaoxide) dispersion fuels have several advantages over their competitors, such as higher service temperature and better stability of oxygen stoichiometry. However, the two-step fabrication of dispersion fuel causes undesirable porosity in cold-pressed fuel meats that is preserved in co-extruded fuel plates. To combat this, spark plasma sintering (SPS) was used for the fabrication of Al-15, 20, and 30 vol% U 3 O 8 and 8 and 12 vol% Mo-U 3 O 8 fuel meats for the Al-U 3 O 8 time. The in situ SPS data was used to construct and validate Master Sintering Curves (MSCs) with accuracies in Al fuels at 0.02 g/cm 3 , and Mo fuels at 0.07 and 0.17 g/cm 3 . The as-sintered fuel meats were characterised using x-ray diffraction (XRD) and scanning electron microscopy (SEM) to understand chemical and physical changes following the SPS process. The pellets exhibited very high relative densities, the U 3 O 8 was observed to undergo reduction to UO 2 .
Aluminium↗