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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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At least 721 records · Page 40
All sourcesNASA NTRSDOE OSTI
DOE OSTI2019

W/TaC/SiC sandwich stack for high temperature applications

High-temperature stability of the tungsten/tantalum carbide/silicon carbide (W/TaC/SiC) system was examined and compared to the tungsten/silicon carbide (W/SiC) system. Interfacial reactions, surface morphology, and roughness evolutions on thermal annealing at 1000 °C were systematically investigated by X-ray diffraction (XRD), scanning electron microscopy (SEM) and atomic force microscopy (AFM). For the W/SiC system, WC, W 2 C and W 5 Si 3 phases were observed due to severe chemical reaction after 24 h annealing, which led to an inhomogeneous surface structure with several large craters and small pores, thereby increasing surface roughness greatly. On the other hand, there was no tungsten silicide and/or carbide formation upon annealing with a TaC diffusion barrier. The surface structure remained nearly unchanged, and small changes in surface roughness with annealing time, which could be due to the growth of W grains, were noted. Furthermore, both the as-deposited and the 24 h annealed W/TaC/SiC samples presented an excellent interfacial bonding with a dense uniform interface. The results indicate that TaC is a promising diffusion barrier in the W/SiC system for high temperature applications.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Structural properties of aqueous grown polydopamine thin films determined by neutron reflectometry

Here, in this work, neutron reflectometry (NR) studies of the bio-mimetic polymer, polydopamine (PDA), deposited from differing initial concentrations of precursor material dopamine hydrochloride for a range of polymerization times, is reported. PDA can form a complex and highly versatile polymer film, with many structure studies having been performed previously, but a comprehensive structural determination of PDA by NR is lacking in the literature. It was found that simple box models were incapable of fully explaining the observed data, necessitating the use of a composite model consisting of the weighted average of both the 1 and 2 box models to fully capture the heterogeneous nature of the PDA film structure. Confocal laser scanning microscopy (CLSM) and atomic force microscopy (AFM) were performed to capture the surface structure and relative mechanical difference between the separate domains of the PDA. The CLSM results provide evidence that the PDA domains are larger than the coherent scattering length of a neutron used in these measurements, 10μm, supporting the need for a composite model. The AFM measurements show complex structure below the coherence length provide physical justification for the two box model. It was determined that film structure and quality are both heavily impacted by the initial concentration of dopamine hydrochloride and the polymerization time, giving confidence to the highly customizable nature of PDA as an adhesion promoting interface treatment in composite systems, such as plastic bonded explosives (PBX).

36 MATERIALS SCIENCE↗
DOE OSTI2024

Corrosion protection of mild steel by superhydrophobic magnetite coating

Corrosion-resistant hydrophobic magnetite coatings on mild steel surfaces were developed by immersion method. The effect of steel surface roughness (R a ) on its hydrophobicity was systematically studied using contact angle measurement (CAM), scanning electron microscopy (SEM), and atomic force microscopy (AFM). The corrosion resistance of hydrophobic magnetite coatings was evaluated using a potentiodynamic polarization test. The durability of the coatings was assessed in air, tap water, and 3.5 wt% NaCl environments. Hydrophobic magnetite coating with a water contact angle of 146-152° showed excellent resistance to corrosion, longevity in atmospheric air, and significant self-cleaning properties. The primary focus of this study was to develop a quick and simple immersion technique to create hydrophobic surfaces on mild steel. Finally, results suggest that surface roughness plays a significant role in surface hydrophobicity, and enhancing the hydrophobicity of mild steel improves its corrosion resistance.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Determination of the Maturation Status of Dendritic Cells by Applying Pattern Recognition to High-Resolution Images

The maturation or activation status of dendritic cells (DCs) directly correlates with their behavior and immunofunction. A common means to determine the maturity of dendritic cells is from high-resolution images acquired via scanning electron microscopy (SEM) or atomic force microscopy (AFM). While direct and visual, the determination has been made by directly looking at the images by researchers. Here we report a machine learning approach using pattern recognition in conjunction with cellular biophysical knowledge of dendritic cells to determine the maturation status of dendritic cells automatically. The determination from AFM images reaches 100% accuracy. The results from SEM images reaches 94.9%. The results demonstrate the accuracy of using machine learning for accelerating data analysis, extracting information, and drawing conclusions from high-resolution cellular images, paving the way for future applications requiring high-throughput and automation, such as cellular sorting and selection based on morphology, quantification of cellular structure, and DC-based immunotherapy.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2025

Tailoring the Physicochemical Properties of Nb Thin Films via Surface Engineering Methods

The modification of surface oxide layers formed on niobium (Nb) thin films via chemical mechanical planarization (CMP) and accelerated neutral atom beam (ANAB) processing provides a promising route toward tailoring their emergent properties and performance when used as superconducting qubits. Here, in this study, we show that CMP- and ANAB-formed Nb oxides are significantly thinner and smoother than the native oxide, as revealed by transmission electron microscopy (TEM) and atomic force microscopy. Scanning TEM and energy-dispersive X-ray spectroscopy along with X-ray photoelectron spectroscopy identified an oxidation gradient within the native and surface-engineered oxides. The topside layer is dominated by Nb 5+ (Nb 2 O 5 ), with various Nb suboxides present closer to the oxide/metal interface. Time-of-flight secondary ion mass spectrometry (ToF-SIMS) depth profiling confirmed the presence of an oxygen content gradient and demonstrated the enhanced resistance of the CMP- and ANAB-formed oxides to oxygen surface exchange and subsequent diffusion via 18 O 2 isotopic labeling experiments. ToF-SIMS also identified an interfacial layer containing trapped hydrogen (H)-containing species at the Nb oxide/metal interface. In situ ToF-SIMS and TEM revealed migration of the H/OH interfacial layer coinciding with decomposition of the surface oxide. Furthermore, our density functional theory calculations indicated that both H from moisture present in ambient air and bulk H in Nb films tend to segregate at the interface. These findings underscore the importance of understanding surface oxidation mechanisms, hydrogen incorporation, and their impact on the designed functionalities of Nb-based devices.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Two-step route to size and shape controlled gibbsite nanoplates and the crystal growth mechanism

Mastery of gibbsite (α-Al(OH) 3 ) nucleation and crystal growth is significant in fundamental aluminum chemistry and also beneficial for industrial applications and the remediation of nuclear waste. Herein, we developed an additive-free two-step route to size and morphology controlled synthesis of gibbsite nanoplates. Independent temperature manipulation of nucleation and crystal growth regimes was used to control the efficacy and yield of the process, producing gibbsite nanoplates with tunable morphologies and sizes. We achieve morphologies ranging from hexagon, pseudo hexagon, truncated triangle to rhombic, and average basal plane diameters from 120 to 850 nm, with thicknesses between 8 and 45 nm. Analysis of gibbsite structure, size and morphology with techniques including powder X-ray diffraction (p-XRD), 27 Al magic angle spinning nuclear magnetic resonance spectroscopy (MAS NMR), scanning electron microscopy (SEM), and atomic force microscopy (AFM) provided key details on the nucleation and crystal growth mechanisms. The results indicate the temperature of the nucleation aging step is the most important factor controlling the final particle size. Particularly small nanoplates were obtained with a low nucleation aging temperature followed by high crystal growth temperature, suggesting that gibbsite growth can be approximated via a LaMer-type burst nucleation and crystal growth mechanism. Scalability was demonstrated by triplicate of 2 L experiments which prepared gibbsite nanoplates of ~200 nm size and with an average yield of ~55% after 84 h. Compared to existing techniques, this improved two-step route is cheaper, more efficient and environmentally friendly.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2020

A combined SECM and electrochemical AFM approach to probe interfacial processes affecting molecular reactivity at redox flow battery electrodes

Redox flow batteries are attractive technologies for grid energy storage since they use solutions of redox-active molecules that enable a superior scalability and the decoupling of power and energy density. However, the reaction mechanisms of the redox active components at RFB electrodes are complex, and there is currently a pressing need to understand how interfacial processes impact the kinetics and operational reversibility of RFB systems. Here, we developed a combined electrochemical imaging methodology rooted in scanning electrochemical microscopy (SECM) and atomic force microscopy (AFM) for exploring the impact of electrode structure and conditioning on the electron transfer properties of model redox-active dialkoxybenzene derivatives, 2,5-di-tert-butyl-1,4-bis(2-methoxyethoxy)benzene (C1) and 2,3-dimethyl-1,4-dialkoxybenzene (C7). Using AFM and secondary-ion mass spectrometry (SIMS), we observed the formation of interfacial films with distinct mechanical properties compared to those of cleaved graphitic surfaces, and exclusively during reduction of electrogenerated radical cations. These films had an impact on the median rate and distribution of the electron transfer rate constant at the basal plane of multilayer and single layer graphene electrodes, displaying kinetically-limited values that did not yield the activation expected per the Butler–Volmer model with a transfer coefficient ~0.5. These changes were dependent on redoxmer structure: furthermore, SECM showed strong attenuation of C7 kinetics by a surface layer on MLG and SLG, while C1 kinetics were only affected by SLG. SECM and AFM results together show that these limiting films operate exclusively on the basal plane of graphite, with the edge plane showing a relative insensitivity to cycling and operation potential. Ultimately, this integrated electrochemical imaging methodology creates new opportunities to understand the unique role of interfacial processes on the heterogeneous reactivity of redoxmers at electrodes for RFBs, with a future role in elucidating phenomena at high active concentrations and spatiotemporal variations in electrode dynamics.

25 ENERGY STORAGE↗
DOE OSTI2026

Laser interference structuring of Cu for adhesive joining of HVAC equipment

Due to potential energy and cost savings benefits, adhesive joining has been recently considered for heating, ventilation, air conditioning, and refrigeration (HVAC&R) systems. HVAC adhesive bonding requires cost-effective and adequate surface preparations of adherents. Here, this article investigates the use of abrasion, traditional single-beam laser, and a laser-interference technique as surface preparations of copper surfaces. Surface morphology is characterized using scanning electron microscopy (SEM) and atomic force microscopy (AFM). Effective submicrometer peak-to-valley structuring with a periodicity of ∼2.7μ⁢m was demonstrated for laser-interference processing. Single-lap shear tests were conducted for 89 joints made with bondline thicknesses of 0.15 and 0.3 mm. Data on process variables and measured variables included open-time, bond length, maximum load, displacement at failure, shear lap strength, and failure mode. A statistical analysis was conducted on each lot to determine the lower limit with 95% confidence intervals for displacements at failure and shear lap strengths. A comparison is presented between the properties of laser-structured joints with respect to those prepared by abrasion, which is considered the baseline surface preparation technique. Based on this comparison, one single-beam laser technique and two laser-interference techniques were shown to exhibit vastly superior performance over the joints made with abraded specimens.

Sabau, Adrian S. [Oak Ridge National Laboratory (O↗
DOE OSTI2013

Subsurface Synthesis and Characterization of Ag Nanoparticles Embedded in MgO

Metal nanoparticles exhibit localized surface plasmon resonance (LSPR) which is very sensitive to the size and shape of the nanoparticle and the dielectric medium surrounding it. LSPR causes field enhancement near the surface of the nanoparticle making them interesting candidates for plasmonic applications. In particular, partially exposed metallic nanoparticles distributed in a dielectric matrix form hotspots which are prime locations for LSPR spectroscopy and sensing. This study involves synthesizing partially buried Ag nanoparticles in MgO and investigating the characteristics of this material system. Ag nanoparticles of different shapes and size distributions were synthesized below the surface of MgO by implanting 200 keV Ag+ ions followed by annealing at 10000C for 10 and 30 hours. A detailed optical and structural characterization was carried out to understand the evolution of Ag nanoparticle microstructure and size distribution inside the MgO matrix. Micro x-ray diffraction (MicroXRD) was employed to investigate the structural properties and estimate the crystallite size. The nanoparticles evolved from a spherical to faceted morphology with annealing time, assuming an octahedral shape truncated at the (001) planes as seen from aberration corrected transmission electron microscopy (TEM) images. The nanoparticles embedded in MgO were shown to be pure metallic Ag using atom probe tomography (APT). The nanoparticles were partially exposed to the surface employing plasma etch techniques to remove the overlaying MgO. Scanning electron microscopy (SEM) and atomic force microscopy (AFM) were employed to study the surface morphology and obtain a height distribution for the partially exposed nanoparticles.

Environmental Molecular Sciences Laboratory↗
DOE OSTI2017

Applying Pattern Recognition to High-Resolution Images to Determine Cellular Signaling Status

Two frequently used tools to acquire high-resolution images of cells are scanning electron microscopy (SEM) and atomic force microscopy (AFM). The former provides a nanometer resolution view of cellular features rapidly and with high throughput, while the latter enables visualizing hydrated and living cells. In current practice, these images are viewed by eye to determine cellular status, e.g. activated versus resting. Automatic and quantitative data analysis is lacking. This work develops an algorithm of pattern recognition that works very effectively for AFM and SEM images. Using rat basophilic leukemia (RBL) cells, our approach creates a support vector machine (SVM) to automatically classify resting and activated cells. 10-fold cross-validation with cells that are known to be activated or resting gives a good estimate of the generalized classification results. The pattern recognition of AFM images achieves 100% accuracy, while SEM reaches 95.4% for our images as well as images published in prior literature. This outcome suggests that our methodology could become an important and frequently used tool for researchers utilizing AFM and SEM for structural characterization as well as determining cellular signaling status and function.

60 APPLIED LIFE SCIENCES↗
DOE OSTI2025

Hybrid chemical characterization of latent images in EUV resist with 12 nm half-pitch features

With the advancement of high numerical aperture extreme ultraviolet (EUV) lithography, the new platform will enable chipmakers to achieve critical dimensions of 8 nm. However, resist materials face significant challenges in delivering increased sensitivity while managing rising stochastic variations. We aim to develop comprehensive techniques to characterize the chemical profile of latent images, stored in EUV resists after exposure and postexposure baking, which is essential for understanding the origin of stochastic effects. Infrared photo-induced force microscopy (IR PiFM) is a bimodal atomic force microscopy technique combined with an infrared light source, allowing for simultaneous sub-5 nm topographic and chemical characterization within a localized environment. Critical-dimension resonant soft X-ray scatterometry (CD-RSoXS) provides statistical data that reveal structural and chemical information for comparative analysis. For the first time, IR PiFM has been used to chemically map the latent images of EUV resists (after exposure and postexposure baking) at a record high resolution of 12 nm half-pitch, enabling nondestructive analysis of patterns prior to development. Furthermore, CD-RSoXS offers direct experimental observation and comparison of exposed, postexposure baked, and developed patterns, which align with the IR PiFM results. We demonstrate that the IR PiFM technique offers valuable insights into both high spatial resolution and local chemical information simultaneously. In addition, CD-RSoXS provides statistical results that support our main findings. This hybrid metrology approach leverages a multifaceted dataset by combining the most reliable information from each source, which is essential for a comprehensive understanding of the stochastic effects in EUV lithography processes.

O’Reilly, Padraic↗
DOE OSTI2015

Nitrogen and silicon defect incorporation during homoepitaxial CVD diamond growth on (111) surfaces

Chemical Vapor Deposited (CVD) diamond growth on (111)-diamond surfaces has received increased attention lately because of the use of N-V related centers in quantum computing as well as application of these defect centers in sensing nano-Tesla strength magnetic fields. We have carried out a detailed study of homoepitaxial diamond deposition on (111)-single crystal diamond (SCD) surfaces using a 1.2 kW microwave plasma CVD (MPCVD) system employing methane/hydrogen/nitrogen/oxygen gas phase chemistry. We have utilized Type Ib (111)-oriented single crystal diamonds as seed crystals in our study. The homoepitaxially grown diamond films were analyzed by Raman spectroscopy, Photoluminescence Spectroscopy (PL), X-ray Photoelectron Spectroscopy (XPS), Scanning Electron Microscopy (SEM) and Atomic Force Microscopy (AFM). The nitrogen concentration in the plasma was carefully varied between 0 and 1500 ppm while a ppm level of silicon impurity is present in the plasma from the quartz bell jar. The concentration of N-V defect centers with PL zero phonon lines (ZPL) at 575nm and 637nm and the Si-defect center with a ZPL at 737nm were experimentally detected from a variation in CVD growth conditions and were quantitatively studied. As a result, altering nitrogen and oxygen concentration in the plasma was observed to directly affect N-V and Si-defect incorporation into the (111)-oriented diamond lattice and these findings are presented.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Developing Quantum Levitation of ICF Capsules Coated with MgB 2 Thin Films

Current inertial confinement fusion (ICF) capsule support technologies create implosion perturbations which reduce fusion yield, driving the search for new support paradigms. Quantum levitation of the capsule will eliminate the requirement of a physical support structure, increasing fusion yield. The application of an external magnetic field to a capsule coated with a superconducting film can provide the necessary conditions for levitation. Magnesium diboride (MgB 2 ) is an attractive option for ICF applications as it has a high reported superconducting transition temperature of 39 K and is a low Z compound. This project is part of an ongoing effort which seeks to coat ICF capsules with a thin layer of superconducting MgB 2 . This project studied the synthesis of MgB 2 and diffusion/reaction kinetics of B/Mg/B m ultilayer thin films. These films were sputter deposited on flat glassy carbon substrates. Films were annealed in a tube furnace at temperatures between 400 °C and 650 °C for a total of 29 hours with film characterization done at predetermined intervals. At each interval, superconducting properties of the samples were evaluated with superconducting quantum interference device (SQUID) magnetometry, while Rutherford backscattering (RBS) with 2 MeV 4 He + ions was done to determine the composition and depth profile of the films. Scanning electron microscopy (SEM) and atomic force microscopy (AFM) were used to characterize surface morphology. Superconducting behavior was observed in thin films annealed at and above 450 °C. Formation of superconducting MgB 2 at 450 °C h as not been previously reported below 500 °C. The surface of the samples annealed at 500 °C and below was smooth with a measured roughness of ~3 nm. After 29 hours of annealing time, the 450 °C sample had a transition temperature of 27.3 K. The highest transition temperature measured was 30.9 K and was associated with a sample annealed for 29 hours at 650 °C. Transition temperatures were weakly positively correlated with annealing temperature and showed dependence on initial structural quality and oxygen contamination. Current research is attempting to synthesize superconducting MgB 2 coatings on spherical Si beads with the findings of this study. Future efforts are focused on the construction and testing of a levitation apparatus.

36 MATERIALS SCIENCE↗
NASA NTRS1993

Imaging Genetic Molecules At Atomic Resolution

Proposed method of imaging informational polymeric biological molecules at atomic resolution enables determination of sequences of component monomers about 10 to the 3rd power to 10 to the 4th power times as fast as conventional methods do. Accelerates research on genetic structures of animals and plants. Also contributes significantly to imaging processes like scanning electron microscopy (SEM), atomic-force microscopy (AFM), and scanning tunneling microscopy (STM) in cases in which necessary to locate or identify small specimens on relatively large backgrounds and subtract background images to obtain images of specimens in isolation. V-grooves on silicon wafer laid out in square pattern, intersections of which marked to identify coordinates. Specimen molecules held in grooves for reproducible positioning and scanning by AFM or STM.

Coles, L. Stephen↗
NASA NTRS1998

Vapor Growth and Characterization of Cr-Doped ZnSe Crystals

Cr-doped ZnSe single crystals were grown by self-seeded physical vapor transport technique under both vertical (stabilized) and horizontal configurations. The source materials were mixtures of ZnSe and CrSe. The growth temperatures were in the range of 1140 to 1150C and the furnace translation rates were 1.9 to 2.2 mm/day. The surface morphology of the as-grown crystals was examined by scanning electron microscopy (SEM) and atomic force microscopy (AFM). The different features on the as-grown surface of the vertically and horizontally grown crystals suggests that different growth mechanisms were involved for the two growth configurations. The [Cr] doping levels were determined to be in the range of 1.8 to 8.3 x 10(exp 19)/cubic centimeter from optical absorption measurements. The crystalline quality of the grown crystals were examined by high resolution triple crystal X-ray diffraction (HRTXD) analysis.

Su, Ching-Hua↗
NASA NTRS1999

Vapor Growth and Characterization of Cr-Doped ZnSe Crystals

Cr-doped ZnSe single crystals were grown by a self-seeded physical vapor transport technique in both vertical (stabilized) and horizontal configurations. The source materials were mixtures of ZnSe and CrSe. Growth temperatures were in the range of 1140-1150 C and the furnace translation rates were 1.9-2.2 mm/day. The surface morphology of the as-grown crystals was examined by scanning electron microscopy (SEM) and atomic force microscopy (AFM). Different features of the as-grown surface of the vertically and horizontally grown crystals suggest that different growth mechanisms were involved in the two growth configurations. The [Cr] doping levels were determined to be in the range of 1.8-8.3 x 10 (exp 19) cm (exp -3) from optical absorption measurements. The crystalline quality of the grown crystals were examined by high-resolution triple-crystal X-ray diffraction (HRTXD) analysis.

Su, Ching-Hua↗
NASA NTRS2000

Investigations into an unknown organism on the martian meteorite Allan Hills 84001

Examination of fracture surfaces near the fusion crust of the martian meteorite Allan Hills (ALH) 84001 have been conducted using scanning electron microscopy (SEM) and atomic force microscopy (AFM) and has revealed structures strongly resembling mycelium. These structures were compared with similar structures found in Antarctic cryptoendolithic communities. On morphology alone, we conclude that these features are not only terrestrial in origin but probably belong to a member of the Actinomycetales, which we consider was introduced during the Antarctic residency of this meteorite. If true, this is the first documented account of terrestrial microbial activity within a meteorite from the Antarctic blue ice fields. These structures, however, do not bear any resemblance to those postulated to be martian biota, although they are a probable source of the organic contaminants previously reported in this meteorite.

NASA Center JSC↗
NASA NTRS1994

(abstract) Optical Scattering and Surface Microroughness of Ion Beam Deposited Au and Pt Thin Films

Thin films of gold and platinum have been deposited onto superpolished fused silica substrates using thermal evaporation, ion assisted deposition (IAD), and ion assisted sputtering. The influence of ion beam flux, thin film material, and deposition rate on the films microroughness have been investigated. Short range surface microroughness of the films has been examined using scanning tunneling microscopy (STM) and atomic force microscopy (AFM). Long range surface microroughness has been characterized using an angle resolved optical scatterometer. Results indicate that ion beam deposited coatings have improved microstructure over thermally evaporated films.

assisted sputtering fused silica ion beam microrou↗