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At least 163 records · Page 9

Wear in particle based CSP systems from particle abrasion and attrition at high temperature

High temperature particle-based receivers offer distinct advantages over conventional molten salt receivers due to their ability to achieve temperatures above 700 ºC, direct absorption of solar energy as they fall through a beam of concentrated sunlight, and the relative ease of storage (and retrieval using a secondary working fluid) in insulated storage tanks. The use of particles, however, also raises concerns with material degradation from the flow of hot or cold particles through discharge hoppers or along the inner receiver surfaces and other system components (e.g. tubes, valves etc.), depending on operating mode of the receiver. The flow of particles over surfaces may result in loss of material from abrasive wear, impact erosion from impingement under gravitational fall and particle attrition as particles fall and move on top of each other. In the present study, the performance of candidate materials and particles were evaluated through a series of abrasion erosion and particle attrition experiments at room temperature as well as at 800 °C. Candidate materials were subject to abrasive wear from particles at low particle to material velocities inside a resistance heated kiln, and analyzed for changes in mass and surface morphology using cross-sectional scanning electron microscopy (SEM) and energy dispersive x-ray spectroscopy (EDS) tests. The wear rate for different specimens was noted to be largely driven by the strength of chromia scales built on the specimens from exposure to high temperature. Particle attrition measurements explored the susceptibility of particles to breakdown from particle to particle interaction and the generation of fines from this process. At the low velocities expected in particle based CSP plants, the particles tested exhibited near negligible breakdown. However, changes in the particle hardness at 800 ºC resulted in a significantly higher particle breakdown to sizes <40 microns raising potential environmental concerns. In addition to particle breakdown, it was also noted that the sample had oxides from the stainless steel test setup mixed in with the particles. Similar oxides can be expected to turn up in the utility scale particle based CSP plants as well. The presence of oxide was also noted to affect the solar absorptivity of the mixture compared to a clean initial specimen, potentially resulting in a change in the overall efficiency of the CSP plant.

14 SOLAR ENERGY↗

Precursor Identity and Surfactant Concentration Influence Shape of UO 2 Nanoparticles

A fundamental step toward studying the unique properties of actinide nanomaterials is control over the shape of actinide nanoparticles. Toward this goal, this work demonstrates the effects of precursor identity and surfactant concentration on the shape of uranium dioxide (UO 2 ) nanoparticles. UO 2 nanoparticles were synthesized by thermal decomposition of different precursors in the presence of oleylamine and oleic acid as surfactants. The size, shape, phase, and chemical composition of the nanoparticles was evaluated using transmission electron microscopy (TEM), energy dispersive X-ray spectroscopy (EDS), electron diffraction (ED), and U L 3 -edge X-ray absorption fine-structure (XAFS) spectroscopy. Anisotropic UO 2 nanocubes of ∼ 4 nm were obtained only with low surfactant concentrations, while increasing the surfactant concentration resulted in formation of nanoparticles with an isotropic, sphere morphology. The importance of precursor identity was also investigated by employing U(hfa) 4 , U(acac) 4 , UO 2 (acac) 2 , and UO 2 (hfa) 2 ·H 2 O (where hfa = hexafluoracetylacetone and acac = acetylacetone) as precursors. The nanocube morphology was only observed when U(hfa) 4 was used as a precursor. XAS allowed for comparison of the disorder in anisotropic vs isotropic UO 2 nanoparticles.

Nanocubes↗

Reduced trap state density in AlGaN/GaN HEMTs with low-temperature CVD-grown BN gate dielectric

In this Letter, low-temperature (400 °C) chemical vapor deposition-grown boron nitride (BN) was investigated as the gate dielectric for AlGaN/GaN metal–insulator–semiconductor high electron mobility transistors (MISHEMTs) on a Si substrate. Comprehensive characterizations using x-ray photoelectron spectroscopy, reflection electron energy loss spectroscopy, atomic force microscope, high-resolution transmission electron microscopy, and time-of-flight secondary ion mass spectrometry were conducted to analyze the deposited BN dielectric. Compared with conventional Schottky-gate HEMTs, the MISHEMTs exhibited significantly enhanced performance with 3 orders of magnitude lower reverse gate leakage current, a lower off-state current of 1 × 10−7 mA/mm, a higher on/off current ratio of 108, and lower on-resistance of 5.40 Ω mm. The frequency-dependent conductance measurement was performed to analyze the BN/HEMT interface, unveiling a low interface trap state density (Dit) on the order of 5 × 1011–6 × 1011 cm−2 eV−1. This work shows the effectiveness of low-temperature BN dielectrics and their potential for advancing GaN MISHEMTs toward high-performance power and RF electronics applications.

Physics↗

Order-disorder phase transition driven by interlayer sliding in lead iodides

A variety of phase transitions have been found in two-dimensional layered materials, but some of their atomic-scale mechanisms are hard to clearly understand. Here, we report the discovery of a phase transition whose mechanism is identified as interlayer sliding in lead iodides, a layered material widely used to synthesize lead halide perovskites. The low-temperature crystal structure of lead iodides is found not 2H polytype as known before, but non-centrosymmetric 4H polytype. This undergoes the order-disorder phase transition characterized by the abrupt spectral broadening of valence bands, taken by angle-resolved photoemission, at the critical temperature of 120 K. It is accompanied by drastic changes in simultaneously taken photocurrent and photoluminescence. The transmission electron microscopy is used to reveal that lead iodide layers stacked in the form of 4H polytype at low temperatures irregularly slide over each other above 120 K, which can be explained by the low energy barrier of only 10.6 meV/atom estimated by first principles calculations. Our findings suggest that interlayer sliding is a key mechanism of the phase transitions in layered materials, which can significantly affect optoelectronic and optical characteristics.

36 MATERIALS SCIENCE↗

Effect of substrate preparation on the structure and chemisorption properties of Pd/MgO model catalyst

Pd/MgO model catalysts are prepared by vapor deposition of Pd particles on MgO thin films which are deposited, at different temperatures, on UHV cleaved mica. MgO films and Pd particles are characterized in situ by Auger electron spectroscopy and energy-loss spectroscopy and ex situ by transmission electron microscopy. Succesive temperature programmed desorption (TPD) of CO shows a different evolution of the morphology of the Pd particles deposited on MgO films prepared at low and high temperature. In addition, on MgO prepared at low temperature, the smallest particles show a continuous decay of CO adsorption during TPD due to contamination by support species.

Henry, C. R.↗

Evaluation and Selection of Replacement Thermal Control Materials for the Hubble Space Telescope

The mechanical and optical properties of the metallized Teflon(Registered Trademark) FEP thermal control materials on the Hubble Space Telescope (HST) have degraded over the nearly seven years the telescope has been in orbit. Given the damage to the outer layer of the multi-layer insulation (MLI) that was apparent during the second servicing mission (SM2), the decision was made to replace the outer layer during subsequent servicing missions. A Failure Review Board was established to investigate the damage to the MLI and identify a replacement material. The replacement material had to meet the stringent thermal requirements of the spacecraft and maintain structural integrity for at least ten years. Ten candidate materials were selected and exposed to ten-year HST-equivalent doses of simulated orbital environments. Samples of the candidates were exposed sequentially to low and high energy electrons and protons, atomic oxygen, x-ray radiation, ultraviolet radiation and thermal cycling. Following the exposures, the mechanical integrity and optical properties of the candidates were investigated using Optical Microscopy, Scanning Electron Microscopy (SEM), and a Laboratory Portable Spectroreflectometer (LPSR). Based on the results of these simulations and analyses, the FRB selected a replacement material and two alternates that showed the highest likelihood of providing the requisite thermal properties and surviving for ten years in orbit.q

Townsend, Jacqueline A.↗

Ground-Based Testing of Replacement Thermal Control Materials for the Hubble Space Telescope

The mechanical and optical properties of the metallized Teflon FEP thermal control materials on the Hubble Space Telescope (HST) have degraded over the nearly seven years the telescope has been in orbit. Given the damage to the outer layer of the multi-layer insulation (MLI) that was apparent during the second servicing mission (SM2), the decision was made to replace the outer layer during subsequent servicing missions. A Failure Review Board was established to investigate the damage to the MLI and identify a replacement material. The replacement material had to meet the stringent thermal requirements of the spacecraft and maintain mechanical integrity for at least ten years. Ten candidate materials were selected and exposed to ten-year HST-equivalent doses of simulated orbital environments. Samples of the candidates were exposed sequentially to low and high energy electrons and protons, atomic oxygen, x-ray radiation, ultraviolet radiation and thermal cycling. Following the exposures, the mechanical integrity and optical properties of the candidates were investigated using Optical Microscopy, Scanning Electron Microscopy (SEM), a Laboratory Portable Spectroreflectometer (LPSR) and a Lambda 9 Spectroreflectometer. Based on the results of these simulations and analyses, the Failure Review Board selected a replacement material and two alternates that showed the highest likelihood of providing the requisite thermal properties and surviving for ten years in orbit.

Townsend, Jacqueline A.↗

Effects of a refractory metal protective barrier on uranium carbonitride ceramic–metallic composites exposed to a high temperature hydrogen environment

Uranium nitride has been under consideration at NASA and the Department of Energy for nuclear thermal propulsion applications intended for deep space exploration vehicles. It is critical to the success of the technology development that the behavior of the fuel system is properly characterized in operational environments. This body of work fabricated ceramic metal composites consisting of uranium ceramic fuel in a molybdenum and molybdenum–tungsten metal matrix, both with and without an exterior molybdenum barrier. Specimens were introduced to a high temperature hydrogen environment and characterized through x-ray diffraction, scanning electron microscopy, and energy dispersive spectroscopy to identify characteristic changes. A portion of the specimens was fabricated with a 1.27 mm thick molybdenum barrier in order to isolate the material from the hydrogen environment. Instability of the uranium nitride occurred as low as 2073 K, leading to aggressive instability approaching 2658 K. Carbon reactions with the metal matrix were observed as well as alloying between the uranium and metal matrix constituents. The liquid uranium resulting from the instability of the uranium nitride was observed to attack the grain boundaries of the refractory metal, resulting in the formation of a liquid uranium molybdenum eutectic melt. Specimens encased in a barrier experienced similar results. The authors conclude this is a significant challenge to applications of this cermet at these temperatures. Alternate configurations with resilient hermetic seals or lower temperature applications such as power reactors may have more success.

36 MATERIALS SCIENCE↗

Nanoconfinement of Molecular Magnesium Borohydride Captured in a Bipyridine-Functionalized Metal-Organic Framework

The lower limit of metal hydride nanoconfinement is demonstrated through the coordination of a molecular hydride species to binding sites inside the pores of a metal-organic framework (MOF). Magnesium borohydride, which has a high hydrogen capacity, is incorporated into the pores of UiO-67bpy (Zr6O4(OH)4(bpydc)6 with bpydc2- = 2,2'-bipyridine-5,5'- dicarboxylate) by solvent impregnation. The MOF retained its long-range order, and transmission electron microscopy and elemental mapping confirmed the retention of the crystal morphology and revealed a homogeneous distribution of the hydride within the MOF host. Notably, the B-, N-, and Mg-edge XAS data confirm the coordination of Mg(II) to the N atoms of the chelating bipyridine groups. In situ 11B MAS NMR studies helped elucidate the reaction mechanism and revealed that complete hydrogen release from Mg(BH4)2 occurs as low as 200 °C. Sieverts and thermogravimetric measurements indicate an increase in the rate of hydrogen release, with the onset of hydrogen desorption as low as 120 °C, which is approximately 150 °C lower than that of the bulk material. Furthermore, density functional theory calculations support the improved dehydrogenation properties and confirm the drastically lower activation energy for B-H bond dissociation.

Nanoconfinement, Metal Hydrides, Metal-Organic Fra↗

Nanoscale imaging of quantum dot dimers using time-resolved super-resolution microscopy combined with scanning electron microscopy

Abstract Time-resolved super-resolution microscopy was used in conjunction with scanning electron microscopy to image individual colloidal CdSe/CdS semiconductor quantum dots (QD) and QD dimers. The photoluminescence (PL) lifetimes, intensities, and structural parameters were acquired with nanometer scale spatial resolution and sub-nanosecond time resolution. The combination of these two techniques was more powerful than either alone, enabling us to resolve the PL properties of individual QDs within QD dimers as they blinked on and off, measure interparticle distances, and identify QDs that may be participating in energy transfer. The localization precision of our optical imaging technique was ∼3 nm, low enough that the emission from individual QDs within the dimers could be spatially resolved. While the majority of QDs within dimers acted as independent emitters, at least one pair of QDs in our study exhibited lifetime and intensity behaviors consistent with resonance energy transfer from a shorter lifetime and lower intensity donor QD to a longer lifetime and higher intensity acceptor QD. For this case, we demonstrate how the combined super-resolution optical imaging and scanning electron microscopy data can be used to characterize the energy transfer rate.

36 MATERIALS SCIENCE↗

An Automated Scanning Transmission Electron Microscope Guided by Sparse Data Analytics

Abstract Artificial intelligence (AI) promises to reshape scientific inquiry and enable breakthrough discoveries in areas such as energy storage, quantum computing, and biomedicine. Scanning transmission electron microscopy (STEM), a cornerstone of the study of chemical and materials systems, stands to benefit greatly from AI-driven automation. However, present barriers to low-level instrument control, as well as generalizable and interpretable feature detection, make truly automated microscopy impractical. Here, we discuss the design of a closed-loop instrument control platform guided by emerging sparse data analytics. We hypothesize that a centralized controller, informed by machine learning combining limited a priori knowledge and task-based discrimination, could drive on-the-fly experimental decision-making. This platform may unlock practical, automated analysis of a variety of material features, enabling new high-throughput and statistical studies.

47 OTHER INSTRUMENTATION↗

Effect of Carbon Nanofiber Clustering on the Micromechanical Properties of a Cement Paste

The use of carbon nanofibers (CNFs) in cement systems has received significant interest over the last decade due to their nanoscale reinforcing potential. However, despite many reports on the formation of localized CNF clusters, their effect on the cement paste micromechanical properties and relation to the mechanical response at the macroscopic scale are still not fully understood. In this study, grid nanoindentation coupled with scanning electron microscopy and energy dispersive spectroscopy was used to determine the local elastic indentation modulus and hardness of a portland cement paste containing 0.2% CNFs with sub-micro and microscale CNF clusters. The presence of low stiffness and porous assemblage of phases (modulus of 15–25 GPa) was identified in the cement paste with CNFs and was attributed primarily to the interfacial zone surrounding the CNF clusters. The CNFs favored the formation of higher modulus C–S–H phases (>30 GPa) in the bulk paste at the expense of the lower stiffness C–S–H. Nanoindentation results combined with a microscale–macroscale upscaling homogenization method further revealed an elastic modulus of the CNF clusters in the range from 18 to 21 GPa, indicating that the CNF clusters acted as compliant inclusions relative to the cement paste.

36 MATERIALS SCIENCE↗

Evolution of TiS and TiN in Fe-40 MassPctNi Austenitic Alloy During Heating at 1273 K (1000 °C)

Evolution of TiS in composition and morphology as well as the change in size distribution of TiS and TiN in Fe-40 masspctNi austenitic alloy during heating at 1273 K (1000 °C) was investigated using manual/automatic scanning electron microscopy energy-dispersive X-ray spectroscopy (SEM/EDS). Two types of TiS morphologies, spindle and spherical, were maintained during heating. The molar ratio of Ti/S of TiS increased while the aspect ratio of TiS was maintained in both alloys during heating. The number density of TiN inclusions was low compared with TiS in each alloy during heating. The pinning effect of TiS during heating was confirmed, and was stronger in alloy with a larger volume fraction of TiS. The results contribute to the establishment of optimum heat treatment processes for austenitic stainless steel to obtain better pitting corrosion resistance.

36 MATERIALS SCIENCE↗

Control of polymorphism during epitaxial growth of hyperferroelectric candidate LiZnSb on GaSb (111)B

A major challenge for ferroelectric devices is the depolarization field, which competes with and often destroys long-range polar order in the limit of ultrathin films. Recent theoretical predictions suggest a new class of materials, termed hyperferroelectics, that should be robust against the depolarization field and enable ferroelectricity down to the monolayer limit. Here, the authors demonstrate the epitaxial growth of hexagonal LiZnSb, one of the hyperferroelectric candidate materials, by molecular-beam epitaxy on GaSb (111)B substrates. Due to the high volatility of all three atomic species, they find that LiZnSb can be grown in an adsorption-controlled window, using an excess zinc flux. Within this window, the desired polar hexagonal phase is stabilized with respect to a competing cubic polymorph, as revealed by x-ray diffraction and transmission electron microscopy measurements. First-principles calculations show that for moderate amounts of epitaxial strain and moderate concentrations of Li vacancies, the cubic LiZnSb phase is lower in formation energy than the hexagonal phase, but only by a few millielectronvolts per formula unit. Therefore, they suggest that kinetics plays a role in stabilizing the desired hexagonal phase at low temperatures. Their results provide a path toward experimentally demonstrating ferroelectricity and hyperferroelectricity in a new class of ternary intermetallic compounds.

42 ENGINEERING↗

Field Emission Properties of Cu-Filled Vertically Aligned Carbon Nanotubes Grown Directly on Thin Cu Foils

Copper-filled vertically aligned carbon nanotubes (Cu@VACNTs) were grown directly on Cu foil substrates of 0.1 mm thicknesses at different temperatures via plasma-enhanced chemical vapor deposition (PECVD). By circumventing the need for additional catalyst layers or intensive substrate treatments, our in-situ technique offers a simplified and potentially scalable route for fabricating Cu@VACNTs with enhanced electrical and thermal properties on thin Cu foils. Comprehensive analysis using field emission scanning microscopy (FESEM), transmission electron microscopy (TEM), energy-dispersive X-ray spectroscopy (EDS) mappings, and X-ray diffraction (XRD) revealed uniform Cu filling within the VACNTs across a range of synthesis temperatures (650 °C, 700 °C, and 760 °C). Field emission (FE) measurements of the sample synthesized at 700 °C (S700) showed low turn-on and threshold fields of 2.33 V/μm and 3.29 V/μm, respectively. The findings demonstrate the viability of thin Cu substrates in creating dense and highly conductive Cu-filled VACNT arrays for advanced electronic and nanoelectronics applications.

36 MATERIALS SCIENCE↗

Mitigating Battery Cell Failure: Role of Ag‐Nanoparticle Fillers in Solid Electrolyte Dendrite Suppression

Abstract The development of solid‐state batteries (SSBs) with lithium Li metal anodes holds significant promise for enhancing the energy density and safety of next‐generation energy storage systems. However, their commercialization is hindered by challenges related to Li dendrite formation, which can lead to short circuits and battery failure. In this study, the role of Ag nanoparticles embedded within solid electrolytes (SE) is investigated in suppressing dendrite propagation. The results demonstrate that Ag nanoparticles effectively mitigate two key failure mechanisms: (1) dendrite growth within porous networks at low current densities and (2) stress intensification‐induced SE fracture at higher current densities (12 mA cm −2 ). Ex situ characterization using focused‐ion beam – scanning electron microscopy (FIB–SEM) and energy dispersive X‐ray spectroscopy (EDS,) reveals that Ag nanoparticles migrate alongside advancing Li dendrites, promoting homogeneous dendrite growth and reducing the likelihood of localized stress concentrations. Additionally, the incorporation of Ag nanoparticles is shown to facilitate a more uniform Li distribution toward the anode side, which can potentially enable the use of higher charging rates in SSBs. This study provides a new perspective on Li dendrite suppression and presents new opportunities for enhancing the performance and safety of SSBs.

Diallo, Mouhamad Said↗

Activating dislocation mediated plasticity in boron carbide through Al-doping

Dislocation slip, deformation twinning, phase transformations, and fast fracture are energy dissipation mechanisms that accommodate mechanical loading in materials. The energetically unfavorable formation of dislocation attributes to the ease of cracking and the low damage tolerance observed in superhard ceramics, notably boron carbide. Here, this work demonstrates that room temperature dislocation slip can be enabled in boron carbide by altering its chemistry through Al doping. The activation of dislocation slip is mechanistically explained by quantum mechanics simulations and electron microscopy, which indicate that strain energy is released through basal icosahedral slip facilitated by icosahedral rotation and chain bond breaking and reconfiguring. The new insight gained through this work suggests that atomic doping could be an effective strategy to tune deformation mechanisms in boron carbide, which provides a significant potential for limiting amorphization and catastrophic failure, and opens a new strategy to enhance damage tolerance in brittle ceramics.

36 MATERIALS SCIENCE↗

Nanohybrid of Silver‐MXene: A Promising Sorbent for Iodine Gas Capture from Nuclear Waste

The increasing reliance on nuclear energy as a significant low-carbon power source necessitates effective solutions for managing radioactive emissions. This study introduces a novel application of MXene nanohybrids, specifically silver-MXene (Ag-Ti 3 C 2 T x ), as an effective sorbent for radioiodine off-gas capture at an operating temperature of 150 °C. Through comprehensive material characterization, including X-ray diffraction, scanning and transmission electron microscopies, energy-dispersive X-ray spectroscopy, Raman spectroscopy, thermogravimetric analysis, inductively coupled plasma optical emission spectroscopy, and gas sorption analyses, the successful loading of Ag nanoparticles onto Ti 3 C 2 T x is confirmed and the subsequent formation of AgI upon iodine capture. The results demonstrate that Ag-Ti 3 C 2 T x exhibits superior iodine uptake compared to traditional silver-based sorbents such as silver mordenite zeolite (AgZ) and silver-functionalized silica aerogel (AgAero). The Ag-Ti 3 C 2 T x achieves an iodine loading of 946 mg g −1 , significantly outperforming AgZ (131 mg g −1 ). These findings highlight the potential of Ag-Ti 3 C 2 T x as a highly efficient, thermally stable sorbent for radioiodine capture, and potentially addressing key limitations of existing materials.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗