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At least 973 records · Page 54

Scalable Synthesis of Ti 3 C 2 T x MXene

Scaling the production of synthetic 2D materials to industrial quantities has faced significant challenges due to synthesis bottlenecks whereby few have been produced in large volumes. These challenges typically stem from bottom‐up approaches limiting the production to the substrate size or precursor availability for chemical synthesis and/or exfoliation. In contrast, MXenes, a large class of 2D transition metal carbides and/or nitrides, are produced via a top‐down synthesis approach. The selective wet etching process does not have similar synthesis constraints as some other 2D materials. The reaction occurs in the whole volume; therefore, the process can be readily scaled with reactor volume. Herein, the synthesis of 2D titanium carbide MXene (Ti 3 C 2 T x ) is studied in two batch sizes, 1 and 50 g, to determine if large‐volume synthesis affects the resultant structure or composition of MXene flakes. Characterization of the morphology and properties of the produced MXene using scanning electron microscopy, X‐ray diffraction, dynamic light scattering, Raman spectroscopy, X‐ray photoelectron spectroscopy, UV–visible spectroscopy, and conductivity measurements show that the materials produced in both batch sizes are essentially identical. This illustrates that MXenes experience no change in structure or properties when scaling synthesis, making them viable for further scale‐up and commercialization.

Shuck, Christopher E.↗

Overcoming the Intrinsic Limitations of Fast Charging Lithium‐Ion Batteries Using Integrated Acoustic Streaming

A lithium‐ion battery's maximum charge rate and energy density are intrinsically limited by the ion diffusion rate in the electrolyte. Most research focuses on materials science solutions to this problem, with gradual improvement over the years. A mechanical solution is proposed to integrate an MHz‐order frequency surface acoustic wave (SAW) device into an existing 1.8 Ah multilayered Li‐ion pouch cell to enhance the ion diffusion rate and the overall battery performance. Both the charging rate and cycling lifetime are improved from SAW. At a 6C (10 min) charge and C/3 discharge rate, typical of electric vehicle applications, integrating SAW into the Li‐ion cell doubles the energy density and maintains at least 72% of the battery's initial capacity after 2000 cycles. Moreover, using SAW quantifiably reduces battery degradation in these conditions as determined by optical imaging, scanning electron microscopy, X‐ray diffraction, and neutron diffraction. The use of SAW appears to offer a method to avoid undesirable Li metal plating on the graphite anode during charging, and leads to a much longer battery lifetime and good charge capacity, all despite rapid charging.

Huang, An↗

Enhancement of Thermoelectric Performance in CuSbSe 2 Nanoplate–Based Pellets by Texture Engineering and Carrier Concentration Optimization

This work reports the thermoelectric properties of the CuSbSe 2 -x mol% PtTe2 (x = 0, 0.5, 1.0, 1.5, and 2.0) pellets composed of highly oriented single crystalline nanoplates. CuSbSe 2 -PtTe 2 single crystalline nanoplates are prepared by a wet-chemical process, and the pellets are prepared through a bottom-up self-assembly of the CuSbSe 2 -PtTe 2 nanoplates and spark plasma sintering (SPS) process. X-ray diffraction and field emission scanning electron microscopic analyses show a highly textured nature with an orientation factor of ≈0.8 for (00l) facets along the primary surface of the pellets (in-plane, perpendicular to the SPS pressure). By this way, bulk-single-crystal-like electrical and thermal transport properties with a strong anisotropy are obtained, which results in an effective optimization on thermoelectric performance. The maximum in-plane thermoelectric figure-of-merit ZT value reaches 0.50 at 673 K for CuSbSe 2 -2.0 mol% PtTe 2 pellet, which is about five times higher than the in-plane ZT (0.10) for pure CuSbSe 2 .

36 MATERIALS SCIENCE↗

Structural, Electric and Magnetic Properties of Bi{sub 2}Sr{sub 2}Ag{sub 0.03}Ca{sub 1}Cu{sub 2}O{sub y} Ceramics Modified by Post-annealing

Polycrystalline Bi{sub 2}Sr{sub 2}Ag{sub 0.03}Ca{sub 1}Cu{sub 2}O{sub y} samples were fabricated using conventional solid-state reaction method. Then, post-annealing temperatures at 730, 780 and 830 {sup ∘}C were applied on samples while time was kept constant at 50 h. Both the x-ray diffraction (XRD) measurement and the scanning electron microscopy (SEM) showed that all samples have high amounts of Bi-2212 phase as the main phase, indicating that the selected starting composition is suitable to analyze the post-annealing effects on the flux pinning properties of Bi-2212 superconductors. In particular, flux pinning performance of Bi-2212 phase is observed from both the magnetic hysteresis loops and J{sub c} values calculated using Bean’s model. The highest J{sub c} value was obtained for sample which was not exposed to the post-annealing treatment. The results clearly show that post-annealing procedure in Bi{sub 2}Sr{sub 2}Ag{sub 0.03}Ca{sub 1}Cu{sub 2}O{sub y} system does not create artificial pinning centres, which lead to the improvements in J{sub c} at high magnetic fields.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

An Integrated Simulation of Multiple-Pass U-10Mo Alloy Hot Rolling and Static Recrystallization

To achieve a desired microstructure and minimize the thickness variation in rolled foils, researchers must understand the effects of foil fabrication process variables on microstructure evolution. We developed an integrated simulation of deformation and recrystallization that employs the finite element method (FEM) and the kinetic Monte Carlo (KMC) Potts model, respectively, to investigate microstructure evolution during multiple-pass hot rolling and heat treatment in polycrystalline U-10Mo fuel. Scanning electron microscopy and electron backscatter diffraction images of microstructures were directly used as input in FEM calculation of deformation, and the calculated strains were used to determine the driving force of nucleation and growth of recrystallized grains in the Potts model. Grain structures predicted by the Potts model were used to update the grain structure and material properties for FEM. Simulation alternated between FEM and the Potts model to simulate grain structure evolution during multiple rolling and heat treatments. The initial model parameters were determined by benchmarking the recrystallization kinetics against experimental data. Then, the model was applied to predict the grain structure evolution. Results showed that our model can capture the coupling between deformation and recrystallization and can quantitatively reproduce the observed U-10Mo recrystallization and grain growth kinetics. The simulation results demonstrated that the developed model can predict U-10Mo grain structures as a function of initial microstructure and foil fabrication parameters.

36 MATERIALS SCIENCE↗

Characterization and Rationalization of Microstructural Evolution in GRCop-84 Processed by Laser-Powder Bed Fusion (L-PBF)

In this study, prismatic geometries of GRCop-84 [Cu-8Cr-4Nb (at. pct)] were built with laser-powder bed fusion (L-PBF) process. The samples were sectioned parallel or perpendicular to the build direction and characterized in the as-built and after post-processing with a hot-isostatically pressing (HIP) treatment. The microstructure and phase evolutions were evaluated with optical microscopy, scanning electron microscopy (SEM), electron backscattered diffraction (EBSD), and high-temperature X-ray diffraction (HTXRD) up to 1223 K. The samples in the as-built conditions exhibited predominantly columnar epitaxial and misoriented Cu-FCC grains. The microstructure evolutions are discussed based on locations within the overall build geometry, the dynamics of small melt pool shape and sectioning effects. The above grain structure did not change significantly during post-process HIP treatment. The stability of this FCC grain structure is attributed to the formation of primary stable Cr 2 Nb (Laves phase) during L-PBF, even before the emergence of FCC grains from liquid. The stability of Cr 2 Nb in both as-built and HIPed samples were evaluated using high-temperature X-ray diffraction measurements and compared with that of gas-atomized powder. The significance of these results is discussed with reference to aerospace applications.

36 MATERIALS SCIENCE↗

Orientation Relationships of Pure Tin on Single Crystal Germanium Substrates

The limited number of independent β-Sn grain orientations resulting from the difficulty in nucleating β-Sn during solidification of Sn-based solders has a large effect on the resulting β-Sn grain size and, hence, on overall solder joint performance and reliability. This study analyzes the efficacy of Ge as a heterogeneous nucleation agent for β-Sn by observing the morphologies and orientation relationships of as-deposited, solid-state annealed, and liquid-state annealed pure Sn films on single crystal Ge (100), (110), and (111) substrates. Here, the results from scanning electron microscopy and electron backscatter diffraction showed that the as-deposited Sn films all deposited with a Sn (001)|| z-axis texture, regardless of the underlying Ge substrate orientation. Solid-state annealing at 150 °C for 5 min did not result in significant dewetting of the Sn films, and the films maintained their as-deposited texture of Sn (001)|| z-axis, regardless of the underlying Ge substrate orientation. Liquid-state annealing at 235 °C for 1 min resulted is large-scale dewetting of the Sn films and re-orientation of the Sn films on the various Ge substrates. After solidification, the Ge (100) and (110) single crystal substrates produced patches of dewetted grains of the same orientation but there were no consistent Sn grain textures after liquid-state annealing, suggesting no single orientation relationship. In contrast, solidification on Ge (111) single crystal substrates resulted in isolated grains with a single Sn film texture and an orientation relationship of (100) Sn ∥(111) Ge and [100] Sn ∥[110] Ge . Density Functional Theory simulations of the experimentally observed Ge (111) sample orientation relationship and the Ge/Sn cube-on-cube orientation relationship suggest favorable relative interfacial binding energies for both interface orientations.

36 MATERIALS SCIENCE↗

Electron Beam Welding of Nimonic 80A Superalloy: Microstructure Evolution and EBSD Study After Aging Heat Treatment

The purpose of this research was to evaluate integrity and microstructure changes of the electron beam-welded Nimonic 80A and the base metal after aging heat treatment process, i.e., 700 °C/72 h/air cooling. Here, microstructure, microhardness and tensile were investigated by various tools, i.e., scanning electron microscope with energy-dispersive spectroscopy and electron backscatter diffraction, x-ray diffraction analysis and Vickers hardness. Evaluation of microstructure shows that the weld zone mainly consists of columnar dendrites. The effect of aging heat treatment on the microstructure morphology and phase structure is very limited. Also, it was observed that there are obvious segregation and precipitates in intracrystalline and along the grain boundaries after aging heat treatment. Electron backscatter diffraction results show that the weld zone and base metal have a clear difference in the grain boundary characterization and kernel average misorientation at room temperature and after aging heat treatment, which leads to a difference in microhardness of the weld zone. In addition, the relationship between microhardness and tensile strength is discussed.

36 MATERIALS SCIENCE↗

Magnetic Behavior of Ni/NiO Core–Shell Nanoparticles under Electromagnetic Waves for Oil–Water Interfacial Tension Reduction

The increasing demand for oil and gas has led to a hope of developing more efficient recovery methods. It is well known that nanoparticles adsorbed at the oil–water interface, but there is no consensus that has been reached on whether magnetic nanoparticles under electromagnetic waves affect the interfacial tension. In this paper, nickel/nickel oxide nanoparticles have been synthesized using sol–gel auto combustion method. The product was characterized using x-ray diffraction, Raman spectroscopy, field emission scanning electron microscopy, Fourier transforms infrared spectroscopy and vibrating sample magnetometer. The results show the Ni/NiO phases and the ferromagnetic nature of the sample. The Ni/NiO nanofluids were prepared to investigate the effect on oil–water interfacial tension in enhanced oil recovery under electromagnetic waves using an inverted pendant drop method. The results show a significant decrease in interfacial tension under electromagnetic waves of frequency 2.2 kHz at low wt.% of Ni/NiO and at room temperature. The decrease in the interfacial tension has been observed by increasing the temperature to 90 °C using temperature controller. The decrease in the interfacial tension could be due to the interaction of oscillating B-field of waves and magnetic domains of adsorbing nanoparticles at the oil–water interface which disturbed the oil–water interface.

36 MATERIALS SCIENCE↗

Location-Specific Microstructure Characterization Within AM Bench 2022 Nickel Alloy 718 3D Builds

Abstract The Additive Manufacturing Benchmark Test Series (AM Bench) is a broad effort to produce rigorous measurement datasets for validating AM computer simulations across the range of processing, structure, and properties, for many additive manufacturing (AM) build methods and material classes. Here, the microstructures of nickel alloy 718 AM Bench 2022 test artifacts produced using laser-based powder bed fusion (PBF-LB), in both as-built and fully heat-treated conditions, are examined. Cross sections are primarily characterized using large area scanning electron microscopy (SEM) electron backscatter diffraction (EBSD) and example analyses of the crystallographic textures are described. These data are part of a large set of in situ and ex situ measurements from both three-dimensional builds and laser tracks on bare plates. All the measurement data are available online with download links at www.nist.gov/ambench .

Levine, L. E. (ORCID:0000000334484229)↗

Friction Stir Welding of ODS and RAFM Steels

Advanced structural materials such as oxide dispersion strengthened steels and reduced-activation ferritic/martensitic steels are desired in fusion reactors as primary candidate materials for first wall and blanket structures, due to their excellent radiation and high-temperature creep resistance. However, their poor fusion weldability has been the major technical challenge limiting practical applications. For this reason, solid-state friction stir welding (FSW) has been considered for such applications. In this paper, the effect of FSW parameters on joining similar and dissimilar advanced structural steels was investigated. Scanning electron microscopy and electron backscatter diffraction methods were used to reveal the effects of FSW on grain size, micro-texture distribution, and phase stability. Hardness mapping was performed to evaluate mechanical properties. Finally, post weld heat treatment was also performed to tailor the microstructure in the welds in order to match the weld zone mechanical properties to the base material.

36 MATERIALS SCIENCE↗

Effect of neutron and ion irradiation on the metal matrix and oxide corrosion layer on Zr-1.0Nb cladding alloys

A detailed study has been carried out on recrystallised Zr-1.0Nb alloys corroded and irradiated under different conditions, including ex-autoclave and ex-reactor samples. After 540 days in reactor and damage around 5 dpa, the neutron irradiated sample shows no serious evidence for radiation enhanced corrosion and is still in pre-transition stage. The good corrosion resistance of the neutron irradiated Zr-1.0Nb can be related to the higher volume fraction of tetragonal phase and fewer interconnected nano porosity/cracks in the oxide. This indicates less tetragonal to monoclinic transition, leads to more protective oxide in the neutron irradiated sample, containing little evidence for short circuit paths for the penetration of oxygen or water towards the metal-oxide interface. These observations on a sample with a slow overall oxidation rate are consistent with the hypothesis that interconnected porosity can lead to early transitions and rapid oxidation. Tetragonal oxide can be either stabilised by irradiation, or stabilised by local release of impurity species from SPPs such as dissolution of Fe from Zr-Nb-Fe precipitates or radiation introduced precipitates (RIPs) which is likely to be small β-Nb clusters. The oxide consists of well-aligned columnar-equiaxed microstructure in the autoclave sample while a more complex oxide grain structure was observed in the neutron-irradiated sample. As oxide continues to grow, there are more < a > and < c > loops, dissolved Fe and RIPs in the metal matrix, however, the corrosion rate is low enough for the tetragonal oxide to stabilise and suboxide + Zr(Osat) phases exist for protectiveness, so there is no enhanced corrosion after radiation. In situ ion irradiation in the TEM revealed no visible defect clusters or voids in the oxide, suggesting that radiation damage to the metal matrix rather than oxide may have a stronger effect on corrosion mechanisms after neutron irradiation, however, cascade damages are not visible in this case. Neutron irradiation also seems to have little effect on promoting fast oxidation or dissolution of β-Nb precipitates into the surrounding oxide or metal during irradiation. Furthermore, these results are discussed in the light of the current mechanisms for corrosion of nuclear fuel cladding alloys.

(S)TEM↗

Characteristics and mechanisms of hydrogen-induced quasi-cleavage fracture of lath martensitic steel

Here this study presents an in-depth characterization of the microstructures, crystallographic orientations, and dislocation characteristics beneath hydrogen-induced quasi-cleavage fracture features of an as-quenched, lath martensitic (α') 22MnB5 steel. The fracture surfaces of gaseous hydrogen-embrittled martensitic specimens were analyzed by a combination of multiple analytical tools: scanning electron microscopy (SEM), electron backscatter diffraction (EBSD), transmission electron microscopy (TEM), and transmission Kikuchi diffraction (TKD). The dominant fracture mode in the hydrogen-affected zones was quasi-cleavage fracture, which involved significant plasticity, evidenced by plastic zones near tear ridges and a high density of dislocations beneath the quasi-cleavage facets. The martensite constituent sizes, variant orientations, and boundaries influenced the quasi-cleavage surface morphologies. Fractography revealed the occurrence of {100} α' -type cleavage across martensitic laths, developing relatively “flat” quasi-cleavage surfaces, in addition to {110} α' -type cracking likely along lath and block boundaries, and fracture along non-cleavage planes. The likelihood of the formation of the relatively “flat” quasi-cleavage surfaces increased with increasing martensitic constituent sizes. Substantial dislocation bands formed on intersecting {112} α' slip planes within a martensite block below the hydrogen-induced cleavage fractures on {100} α' planes. River markings on the quasi-cleavage surfaces were found to originate from the complex, hierarchical lath martensitic microstructure. Steps and ridges on the quasi-cleavage facets generally linked with the various martensitic boundaries, suggesting that they were produced as a result of crack deviations at those boundaries. The fracture paths and martensite quasi-cleavage mechanisms are discussed in the context of the role of hydrogen and Cottrell cleavage model.

36 MATERIALS SCIENCE↗

Microwave-assisted ammonia decomposition over metal nitride catalysts at low temperatures

The negative environmental impact of fossil fuel-based energy systems has unveiled the need to develop a CO x -free sustainable hydrogen (H 2 ) economy. Employing a microwave-assisted route, a ternary metal nitride catalyst (i.e., Co 2 Mo 3 N), and a low-temperature-pressure NH 3 decomposition process, this study investigated the possibility of developing a distributed H 2 production process. Here, this study not only explored lower cost-based catalyst systems but also the use of a microwave reactor to increase the energy efficiency of the process. Results from catalytic NH 3 decomposition experiments, performed in microwave reactors on Co 2 Mo 3 N catalyst, demonstrated the peak energy efficiency (of ~0.006 kgH 2 /kWh) at 400 °C in ambient pressure (with an NH 3 conversion >90%) which was around ninety times (~90 x) more efficient than a conventional system. Activation energy calculation also displayed a 20% less energy requirement for the microwave-based process (~31 kJ mol -1 ) than the conventional system (~37 kJ mol -1 ), indicating the advantage of the microwave-based process. Further microwave-assisted catalytic measurements and characterization of the Co 2 Mo 3 N catalyst, using x-ray diffraction (XRD) technique and scanning electron microscopic (SEM) images, revealed the excellent stability of this material at its peak performance (at 400 °C) and illustrated the potential of using this catalyst for a sustainable, economic, and energy-efficient approach for producing CO x -free H 2 .

08 HYDROGEN↗

Structural and superconducting properties of Nb 3 Sn films grown by multilayer sequential magnetron sputtering

Nb 3 Sn thin films are fabricated by sequential sputtering followed by annealing at 850–1200°C in vacuum. The effects of the annealing temperature and time on the formation of Nb 3 Sn were examined. The film crystal structure, morphology, surface topography and composition were distinguished by X-ray diffraction, field-emission scanning electron microscopy, atomic force microscopy, and energy dispersive X-ray spectroscopy analysis. The superconducting properties of the films were characterized by measuring the surface resistivity by the four-point probe method. The highest critical temperature T c = 17.86 K was observed for the Nb 3 Sn films annealed at 950°C for 3 h. When the films were annealed above 1000°C for 3 h, Sn evaporation resulted in a Nb-rich film, degrading the superconducting performance. Annealing at 1200°C for 3 h resulted in evaporation of Sn leaving less than 1% Sn on the surface, as detected by energy dispersive spectroscopy, and for that film a T c of 7.9 K was observed.

36 MATERIALS SCIENCE↗

Investigating microstructural evolution in SolidStir™ extruded oxide dispersion strengthened 14YWT alloy fuel cladding tube

Structural components for extreme environments require advanced materials and manufacturing processes. One such advanced material is oxide dispersion strengthened (ODS) Fe–14 wt.%Cr–3W–0.4Ti–0.3Y 2 O 3 (14YWT), which is developed for components to be used in Gen IV and fusion nuclear reactors. However, the conventional manufacturing processes to produce components, such as fuel cladding tubes, either do not retain the desired microstructural attributes or are costly and less efficient. As a result, a more attractive option is a novel manufacturing process developed on the principle of friction stir welding or processing (FSW/P) and commercially referred to as SolidStir™ Extrusion (SSE). Here this study used the SSE technique to study the manufacturing and microstructural evolution of a fuel cladding tube made of ODS 14YWT alloy. The cladding extrusion by the SSE technique involved the use of ball-milled 14YWT powders with Y, Ti, and O in the solid solution and the use of a specially designed W-25Re-Hf tool for consolidation and extrusion of the powders. A scanning electron microscope (SEM), electron backscattered diffraction (EBSD), and transmission electron microscope (TEM) were utilized for microstructural characterization. A Keyence microscope captured macrostructural photographs of the extruded tube. EBSD examination of the extruded tube on both transverse and longitudinal cross-sections showed the presence of dynamically recrystallized grains and revealed that the average grain size of the transverse cross-section was smaller than that of the longitudinal cross-section. The texture was weak and consisted of some amount of shear texture. The presence of nano-oxide clusters or precipitates of Y, Ti, and O (pyrochlores) in the extruded tube was determined by TEM. Aging heat treatment caused the average precipitate size to decrease and the density to increase compared to the as-processed condition. The results indicated that SSE is a viable tool for manufacturing fuel cladding tubes with the desired microstructural attributes.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Formation of uranium nitride nanoparticles via mechanical alloying of uranium-molybdenum alloy fuels in gaseous nitrogen

Uranium-molybdenum (U-Mo) alloys show promise as a nuclear fuel system due to their high thermal conductivity and fuel loading capability. However, U-Mo systems are susceptible to irradiation induced swelling ultimately affecting the cladding via mechanical and chemical interactions. To address these shortcomings, this research investigated the formation of uranium mononitride (UN) nanoparticles within a 90 wt% U/10 wt% Mo (U-10Mo) matrix to act as a prospective defect sink for fission products at nanometric hetero-interfaces. To promote the formation of UN, U-10Mo powders were mechanically alloyed under a high purity nitrogen atmosphere. Variations of the milling process investigated included media size, duration of milling, and number of times the milling jar was re-aerated with nitrogen gas. Characterization of the fuel microstructure was completed using light element analysis, X-ray diffraction, scanning and transmission-electron microscopy, electron energy loss spectroscopy, and atom probe tomography. UN nanoparticles measuring 1–5 nm in radius were observed in the U-Mo matrix as early as 1 h into the mechanical alloying process. Milling time in excess of 10 h was found to lead to deleterious effects induced by the stainless-steel milling media.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗