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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.
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We present a new analytical platform that uses a tilted and Peltier cooling stage interfaced with an environmental scanning electron microscope to directly observe and assess the phase state of individual particles as a function of relative humidity.
Ground water sources used as coolant fluids in a variety of thermal systems such as heat exchangers and power plant condensers contain silica particles that accrete on heat transfer surfaces over time leading to reduction in thermal performance, a problem that is particularly exacerbated with temperature. Nonwetting superhydrophobic, lubricant-infused, and a new class of solid-infused surfaces introduced in this work are candidates for fouling mitigation, by virtue of their water repellency, but little is known about fouling of silica on the surfaces, especially under dynamic flow conditions and as a function of temperature. This article presents, for the first time, a systematic study of dynamic flow fouling of silica on nonwetting surfaces vis-à-vis conventional copper surface over a temperature range 20–50°C. The mechanism of silica aggregate formation and its adherence to the different surfaces is elucidated by scanning electron microscope (SEM) imaging. Sigmoidal growth model is used to describe the time evolution of fouling thermal resistance and an Arrhenius model is presented for the temperature-dependent increase in the asymptotic fouling resistance on nonwetting and conventional surfaces alike. Lubricant-infused and solid-infused surfaces are shown to reduce fouling thermal resistance by up to 25% and 13%, respectively, compared to a conventional surface, whereas superhydrophobic surfaces lose their non-wettability under flow conditions, leading to an adverse increase in the fouling resistance by up to 13%. Considering the possible lubricant depletion in lubricant-infused surfaces over prolonged exposure to a flowing fluid, solid-infused surfaces present a robust alternative.
Recent studies have shown that solvated amphiphiles can form nanostructured self-assemblies called dynamic binary complexes (DBCs) in the presence of ions. Since the nanostructures of DBCs are directly related to their viscoelastic properties, it is important to understand how the nanostructures change under different solution conditions. However, it is challenging to obtain a three-dimensional molecular description of these nanostructures by utilizing conventional experimental characterization techniques or thermodynamic models. To this end, we combined the structural data from small angle X-ray scattering (SAXS) experiments and thermodynamic knowledge from coarse-grained Monte Carlo (CGMC) simulations to identify the detailed three-dimensional nanostructure of DBCs. Specifically, unbiased CGMC simulations are performed with SAXS-guided initial conditions, which aids us to sample accurate nanostructures in a computationally efficient fashion. As a result, an elliptical bilayer nanostructure is obtained as the most probable nanostructure of DBCs whose dimensions are validated by scanning electron microscope (SEM) images. Then, utilizing the obtained molecular model of DBCs, here we could also explain the pH tunability of the system. Overall, our results from SAXS-guided unbiased CGMC simulations highlight that using potential energy combined with SAXS data, we can distinguish otherwise degenerate nanostructures resulting from the inherent ambiguity of SAXS patterns.
Organometal halide perovskites are promising materials for optoelectronic applications, whose commercial realization depends critically on their stability under multiple environmental factors. In this study, a methylammonium lead bromide (MAPbBr 3 ) single crystal was cleaved and exposed to simultaneous oxygen and light illumination under ultrahigh vacuum (UHV). The exposure process was monitored using X-ray photoelectron spectroscopy (XPS) with precise control of the exposure time and oxygen pressure. It was found that the combination of oxygen and light accelerated the degradation of MAPbBr 3 , which could not be viewed as a simple addition of that by oxygen-only and light-only exposures. The XPS spectra showed significant loss of carbon, bromine, and nitrogen at an oxygen exposure of 10 10 Langmuir with light illumination, approximately 17 times of the additive effects of oxygen-only and light-only exposures. It was also found that the photoluminescence (PL) emission was much weakened by oxygen and light co-exposure, while previous reports had shown that PL was substantially enhanced by oxygen-only exposure. Measurements using a scanning electron microscope (SEM) and focused ion beam (FIB) demonstrated that the crystal surface was much roughened by the co-exposure. Furthermore, Density functional theory (DFT) calculations revealed the formation of superoxide and oxygen induced gap state, suggesting the creation of oxygen radicals by light illumination as a possible microscopic driving force for enhanced degradation.
Electric Field Assisted Sintering (EFAS, also referred to as spark plasma sintering) is a powerful technology for the consolidation of powder materials. The high heating rate during the sintering process is critical for minimizing energy consumption, but it can also cause microstructure heterogeneities in sintered parts, such as spatially varied porosity. The examination of localized porosity usually requires the use of a scanning electron microscope with a carefully prepared surface. In this paper, photothermal radiometry is used to measure local thermal diffusivity and extract localized porosity of EFAS-sintered parts by using a percolation-threshold model. Applying this approach, we identified the radial position-dependent porosity variation in EFAS parts, which is likely formed due to the large temperature gradient during the sintering process. This approach has a unique advantage because it can measure samples with minimal or no surface preparation, enabling the possibility of in situ characterization in EFAS with proper system modification. Necessary modifications on the measurement approach for EFAS deployment and in situ characterization are also discussed.
Alloying additions are introduced into U-Zr fuel in order to bind lanthanides (e.g., cerium) and prevent their migration to the fuel-cladding interface. Antimony (Sb) is being investigated as a candidate additive. The present study focuses on the diffusion couple behavior of U-10Zr (wt%) alloy with Sb against cladding (iron or HT9) at 640°C. The diffusion cross sections were analyzed using a scanning electron microscope and X-ray diffraction. Zr-rind was found at the interface of the fuel alloy, Sb was found to be bound in Sb-Zr precipitates or Sb-Ce precipitates, and no reaction was found between Sb precipitates and the cladding materials.
Cost- and resource-efficient growth is necessary for many applications of semiconductor nanowires. We here present the design, operational details and theory behind Aerotaxy, a scalable alternative technology for producing quality crystalline nanowires at a remarkably high growth rate and throughput. Using size-controlled Au seed particles and organometallic precursors, Aerotaxy can produce nanowires with perfect crystallinity and controllable dimensions, and the method is suitable to meet industrial production requirements. Here, we explain why Aerotaxy is an efficient method for fabricating semiconductor nanowires and explain the technical aspects of our custom-built Aerotaxy system. Investigations using SEM (Scanning Electron Microscope), TEM (Transmission Electron Microscope)and other characterization methods are used to support the claim that Aerotaxy is indeed a scalable method capable of producing nanowires with reproducible properties. We have investigated both binary and ternary III–V semiconductor material systems like GaAs and GaAsP. In addition, common aspects of Aerotaxy nanowires deduced from experimental observations are used to validate the Aerotaxy growth model, based on a computational flow dynamics (CFD) approach. We compare the experimental results with the model behaviour to better understand Aerotaxy growth.
The controlled fabrication of vertical, tapered, and high-aspect ratio GaN nanowires via a two-step top-down process consisting of an inductively coupled plasma reactive ion etch followed by a hot, 85% H 3 PO 4 crystallographic wet etch is explored. The vertical nanowires are oriented in the $[0001]$ direction and are bound by sidewalls comprising of $\{33\bar{6}2\}$ semipolar planes which are at a 12° angle from the [0001] axis. High temperature H3PO4 etching between 60 °C and 95 °C result in smooth semipolar faceting with no visible micro-faceting, whereas a 50 °C etch reveals a micro-faceted etch evolution. High-angle annular dark-field scanning transmission electron microscopy imaging confirms nanowire tip dimensions down to 8–12 nanometers. The activation energy associated with the etch process is 0.90 ± 0.09 eV, which is consistent with a reaction-rate limited dissolution process. The exposure of the $\{33\bar{6}2\}$ type planes is consistent with etching barrier index calculations. The field emission properties of the nanowires were investigated via a nanoprobe in a scanning electron microscope as well as by a vacuum field emission electron microscope. Finally, the measurements show a gap size dependent turn-on voltage, with a maximum current of 33 nA and turn-on field of 1.92 V nm -1 for a 50 nm gap, and uniform emission across the array.
Abstract Machine learning (ML) and artificial intelligence have proven to be an invaluable tool in tackling a vast array of scientific, engineering, and societal problems. The main drivers behind the recent proliferation of ML in practically all aspects of science and technology can be attributed to: (a) improved data acquisition and inexpensive data storage; (b) exponential growth in computing power; and (c) availability of open-source software and resources that have made the use of state-of-the-art ML algorithms widely accessible. The impact of ML on the field of low-temperature plasmas (LTPs) could be particularly significant in the emerging applications that involve plasma treatment of complex interfaces in areas ranging from the manufacture of microelectronics and processing of quantum materials, to the LTP-driven electrification of the chemical industry, and to medicine and biotechnology. This is primarily due to the complex and poorly-understood nature of the plasma-surface interactions in these applications that pose unique challenges to the modeling, diagnostics, and predictive control of LTPs. As the use of ML is becoming more prevalent, it is increasingly paramount for the LTP community to be able to critically analyze and assess the concepts and techniques behind data-driven approaches. To this end, the goal of this paper is to provide a tutorial overview of some of the widely-used ML methods that can be useful, amongst others, for discovering and correlating patterns in the data that may be otherwise impractical to decipher by human intuition alone, for learning multivariable nonlinear data-driven prediction models that are capable of describing the complex behavior of plasma interacting with interfaces, and for guiding the design of experiments to explore the parameter space of plasma-assisted processes in a systematic and resource-efficient manner. We illustrate the utility of various supervised, unsupervised and active learning methods using LTP datasets consisting of commonly-available, information-rich measurements (e.g. optical emission spectra, current–voltage characteristics, scanning electron microscope images, infrared surface temperature measurements, Fourier transform infrared spectra). All the ML demonstrations presented in this paper are carried out using open-source software; the datasets and codes are made publicly available. The FAIR guiding principles for scientific data management and stewardship can accelerate the adoption and development of ML in the LTP community.
The operating temperature window of solid tungsten (W) is dictated by its Ductile to Brittle Transition Temperature (DBTT) and re-crystallization temperature; roughly between 300-1300 °C. The brittleness of W at lower temperatures is exasperated when it undergoes recrystallization. We investigate here the thermal shock resistance of micro-porous W as a meta-material fabricated in a 3D open-cell network structure. We present experimental results for the effects of cyclic high-enthalpy arc-jet plasma on surface damage in three testing categories. Observed damage includes surface ablation of asperities, melting and solidification of W-fuzz on samples that have been exposed to a prior helium plasma, and micro-cracks at ligament triple junctions. Scanning electron microscope (SEM) observations show more micro-cracking on 54% and 23% foams compared to the 43% ones. In all tested samples, thermal expansion/contraction displacements were accommodated by ligament rotation and a network of micro-cracks. Furthermore, no large through-thickness crack were observed.
The extreme sensitivity of 2D materials to defects and nanostructure requires precise imaging techniques to verify presence of desirable and absence of undesirable features in the atomic geometry. Helium-ion beams have emerged as a promising materials imaging tool, achieving up to 20 times higher resolution and 10 times larger depth-of-field than conventional or environmental scanning electron microscopes. Here, we offer first-principles theoretical insights to advance ion-beam imaging of atomically thin materials by performing real-time time-dependent density functional theory simulations of single impacts of 10–200 keV light ions in free-standing graphene. Here we predict that detecting electrons emitted from the back of the material (the side from which the ion exits) would result in up to three times higher signal and up to five times higher contrast images, making 2D materials especially compelling targets for ion-beam microscopy. This predicted superiority of exit-side emission likely arises from anisotropic kinetic emission. The charge induced in the graphene equilibrates on a sub-fs time scale, leading to only slight disturbances in the carbon lattice that are unlikely to damage the atomic structure for any of the beam parameters investigated here.
Abstract Polyurethane (PU) foams reinforced with bamboo fiber sources in China, i.e. , bamboo fiber, bamboo α -cellulose fiber, and bamboo nanocellulose fiber, were prepared and their physico-mechanical properties were analyzed in this work. The bamboo fiber sources and PU foams were characterized by Fourier transform infrared spectroscopy (FTIR), Scanning electron microscope (SEM), Thermal gravimetric analysis (TGA) and universal compression testing. The results indicated that the hydroxyl groups on the fiber surfaces were enhanced by removing non-celluloses in the preparation of α -cellulose and nanocellulose. With the addition of small particle size α -cellulose and nanocellulose, the cell sizes of PU foams were reduced due to more nucleating agents being introduced. The FTIR spectra confirmed that the bamboo fiber sources were involved in the foaming reaction. The PU foams with bamboo fiber sources had a higher thermal stability than neat foam, and they were satisfactory enough to be used as insulation. PU foams reinforced with 5% bamboo fiber, 3% α -cellulose fiber and 3% nanocellulose fiber had better physico-mechanical performance than other foams. The reinforcement performance of 3% bamboo α -cellulose fiber on PU foam was comparable with that of high-cost nanocellulose. Accordingly, bamboo α -cellulose fiber was demonstrated to be a promising candidate to reinforce PU foam, which could be used in the reinforcement of foam insulation.
Monolayer graphene growth on liquid copper (Cu) has attracted attention due to advantages of a flat/smooth catalytic growth surface, high synthesis temperature (>1080 °C) as well as the possibility of forming graphene domains that are mobile on the liquid Cu with potential to minimize grain boundary defects and self-assemble into a continuous monolayer film. However, the quality of monolayer graphene grown on liquid copper and its suitability for size-selective ionic/molecular membrane separations has not been evaluated/studied. Here, we probe the quality of monolayer graphene grown on liquid Cu (via a metallurgical process, HSMG ® ) using Scanning Electron Microscope (SEM), High-resolution transmission electron microscope (HR-TEM), Raman spectroscopy and report on a facile approach to assess intrinsic sub-nanometer to nanometer-scale defects over centimeter-scale areas. We demonstrate high transfer yields of monolayer graphene (>93% coverage) from the growth substrate to polyimide track etched membrane (PITEM, pore diameter ~200 nm) supports to form centimeter-scale atomically thin membranes. Next, we use pressure-driven transport of ethanol to probe defects > 60 nm and diffusion-driven transport of analytes (KCl ~0.66 nm, L-Tryptophan ~0.7–0.9 nm, Vitamin B12 ~1–1.5 nm and Lysozyme ~3.8–4 nm) to probe nanoscale and sub-nanometer scale defects. Diffusive transport confirms the presence of intrinsic sub-nanometer to nanometer scale defects in monolayer graphene grown on liquid Cu are no less than that in high-quality graphene synthesized via chemical vapor deposition (CVD) on solid Cu. Our work not only benchmarks quality of graphene grown on liquid copper for membrane applications but also provides fundamental insights into the origin of intrinsic defects in large-area graphene synthesized via bottom-up processes for membrane applications.
Abstract The femtosecond laser has emerged as a powerful tool for micro- and nanoscale device fabrication. Through nonlinear ionization processes, nanometer-sized material modifications can be inscribed in transparent materials for device fabrication. This paper describes femtosecond precision inscription of nanograting in silica fiber cores to form both distributed and point fiber sensors for sensing applications in extreme environmental conditions. Through the use of scanning electron microscope imaging and laser processing optimization, high-temperature stable, Type II femtosecond laser modifications were continuously inscribed, point by point, with only an insertion loss at 1 dB m −1 or 0.001 dB per point sensor device. High-temperature performance of fiber sensors was tested at 1000 °C, which showed a temperature fluctuation of ±5.5 °C over 5 days. The low laser-induced insertion loss in optical fibers enabled the fabrication of a 1.4 m, radiation-resilient distributed fiber sensor. The in-pile testing of the distributed fiber sensor further showed that fiber sensors can execute stable and distributed temperature measurements in extreme radiation environments. Overall, this paper demonstrates that femtosecond-laser-fabricated fiber sensors are suitable measurement devices for applications in extreme environments.
We present an experimental analysis of the change in the electric field enhancement factor with varying gap size and penetration depth (P.D) of cathode into anode for a coaxial vacuum gap, diagnosed using Fowler–Nordheim analysis and optical imaging via scanning electron microscope (SEM) and time integrated Digital single lens reflex camera (DSLR). Data were collected on the Coaxial Gap Breakdown Machine (240 A, 25 kV, 150 ns, 0.1 Hz). Experiments using five different gap sizes at nine different P.Ds are compared over runs comprising 50 shots for each case. The results show a strong link between enhancement factor and gap size, with P.D and surface topology. For large gap sizes, 150, 330, and 700 μm, the average enhancement factor value increases with increasing P.D. For smaller gap sizes, 50 and 100 μm, the average enhancement factor decreases with P.D. SEM imaging before and after plasma formation for each gap size allows for quantifying surface finish, microprotrusion growth, average blast diameter, and an estimation of the surface area breakdowns occupy. Time integrated DSLR imaging analysis of the gap at each shot allows for a determination of the distribution of breakdowns about the circumference of the gap for each case tested. Here, the Fowler–Nordheim analysis allows for a quantitative analysis of the surface roughness of all gap sizes tested. Results show that for large gap sizes, the gap geometry and increasing area of breakdown is the main cause for increasing average enhancement factor. For small gap sizes, the dominant driving factor for small average enhancement factors—that subsequently decrease with P.D—is significant changes in surface topology due to an increased number of breakdowns.
Mechanical strength of a 94 wt% debased alumina was measured using ASTM-C1161 specimens fabricated via conventional and lithography-based ceramic manufacturing (LCM) methods. The effects of build orientation and a 1500°C wet hydrogen fire added to the LCM firing sequence on strength were evaluated. Additionally, a Weibull fit to the conventional flexural specimen data yielded 20 and 356 MPa for the modulus and characteristic strength, respectively. Weibull fits of the data from the LCM specimens yielded moduli between 7.5 and 11.3 and characteristics strengths between 333 and 339 MPa. A Weibull fit to data from LCM specimens subjected to the wet hydrogen fire yielded 14.2 and 376 MPa for the modulus and characteristic strength, respectively. The 95% confidence intervals for all Weibull parameters are reported. Average Archimedes bulk densities of LCM and conventional specimens were 3.732 and 3.730 g/cm 3 , respectively. Process dependent differences in surface morphology were observed in scanning electron microscope (SEM) images of specimen surfaces. SEM images of LCM specimen cross-sections showed alumina grain texture dependent on build direction, but no evidence of porosity concentrated in planes between printed layers. Fracture surfaces of LCM and conventionally processed specimens revealed hackle lines and mirror regions indicative of fracture initiation at the sample surface rather than the interior.
Environmental barrier coatings (EBCs) protect advanced ceramics and ceramic matrix composites (CMCs) from oxidation and corrosion in gas turbine engine environments. Foreign object damage (FOD), where debris impact the protective coatings, is a critical hazard which limits the turbine durability. Despite previous efforts to understand FOD in EBCs, a detailed understanding of the fundamental transient damage mechanisms is still lacking. In the current work, the real-time FOD behavior of a Mullite / Silicon EBC was visualized via a dynamic synchrotron X-ray source in phase contrast imaging (PCI) configuration. Prior to the in situ FOD experiments, the microstructure and composition of the coating were respectively characterized using a scanning electron microscope (SEM) and X-ray diffraction (XRD). The variation in the properties of the debris was modeled by ~ 1.5 mm diameter Partially Stabilized Zirconia (PSZ) and Silicon Nitride (Si 3 N 4 ) spheres. A modified light-gas gun setup, synchronized with the X-ray beam, was used to propel the projectiles at velocities ranging between 300 and 355 m·s -1 . Coated samples were impacted under a fully backed support configuration and at normal incidence. Coating penetration and delamination, as well as projectile deformation at the bond coat resulted for FOD by PSZ spheres. Comparatively, projectile fracture, with subsequent rebound of fragments, as well as complete coating penetration and delamination at the substrate interface occurred for FOD by Si 3 N 4 spheres. It should be noted that only cone cracking was observed for FOD by PSZ spheres while back surface cracking was present for both projectile types. Qualitative understanding of the driving forces for the observed damage mechanisms were provided.
Compositional analysis of boron carbide on nanometer length scales to examine or interpret atomic mechanisms, for example, solid-state amorphization or grain-boundary segregation, is challenging. This work reviews advancements in high-resolution microanalysis to characterize multiple generations of boron carbide. First, ζ-factor microanalysis will be introduced as a powerful (scanning) transmission electron microscopy ((S)TEM) analytical framework to accurately characterize boron carbide. Three case studies involving the application of ζ-factor microanalysis will then be presented: (1) accurate stoichiometry determination of B-doped boron carbide using ζ-factor microanalysis and electron energy loss spectroscopy, (2) normalized quantification of silicon grain-boundary segregation in Si-doped boron carbide, and (3) calibration of a scanning electron microscope X-ray energy-dispersive spectroscopy (XEDS) system to measure compositional homogeneity differences of B/Si-doped arc-melted boron carbides in the as-melted and annealed conditions. Overall, the improvement and application of advanced analytical tools have helped better understand processing–microstructure–property relationships and successfully manufacture high-performance ceramics.