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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 91 records · Page 5
All sourcesNASA NTRSDOE OSTI
DOE OSTI2014

Observing gas-catalyst dynamics at atomic resolution and single-atom sensitivity

Transmission electron microscopy (TEM) has become an indispensable technique for studying heterogeneous catalysts. Specifically, advancements of aberration-corrected electron optics and data acquisition schemes have made TEM capable of delivering images of catalysts with sub-Ångström resolution and single-atom sensitivity. Parallel developments of differentially pumped electron microscopes and of gas cells enable in situ observations of catalysts during the exposure to reactive gas environments at pressures of up to atmospheric levels and temperatures of up to several hundred centigrade. Here, we outline how to take advantage of the emerging state-of-the-art instrumentation and methodologies to study surface structures and dynamics to improve the understanding of structure-sensitive catalytic functionality. The idea of using low electron dose-rates in TEM in conjunction with in-line holography and aberration-correction at low voltage (80kV) is introduced to allow maintaining atomic resolution and sensitivity during in situ observations of catalysts. Benefits are demonstrated by exit wave reconstructions of TEM images of a nanocrystalline Co 3 O 4 catalyst material acquired in situ during their exposure to either a reducing or oxidizing gas environment.

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

Tensile behavior and microstructural evolution of a Fe-25Ni-20Cr austenitic stainless steel (alloy 709) from room to elevated temperatures through in-situ synchrotron X-ray diffraction characterization and transmission electron microscopy

Uniaxial tensile tests were done on Fe-25Ni-20Cr Austenitic Stainless Steel (Alloy 709) along with in-situ synchrotron measurement at different temperatures (25 degrees C, 500 degrees C, 700 degrees C and 900 degrees C). The X-Ray diffraction data was collected in-situ in order to follow the phases present as well as to derive the dislocation density as a function of strain through peak broadening analysis based on the modified Williamson-Hall method and see how trends are affected as a function of temperature. The XRD data were complemented by TEM and STEM-EDX characterization done on the post-experiment samples to observe the deformed microstructures. Finally, the paper presents a depiction of the tensile behavior of this advanced steel by interpreting the stress-strain curves and the effect of temperature through the information gained by in-situ XRD and TEM observations as well as fractography done ex-situ on the samples tested to rupture.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Facile synthesis of B-type carbonated nanoapatite with tailored microstructure

Nanolime and a phosphate-based chelating agent were used to synthesize B-type carbonated apatite. Developed Rietveld refinement strategies allowed one to determine process yield, product crystallinity as well as structural (unit cell) and microstructural (size, strain) parameters. The effect of synthesis temperature (20–60 °C) as well as Ca/P ratio (1.5–2.5) and solid content (10–30 wt%) of the starting batch on these properties were investigated. FTIR, TEM and gas adsorption data provided supporting evidence. The process yield was 42–60 wt% and found to be governed by the Ca/P ratio. The purified products had high specific surface area (107–186 m{sup 2}/g) and crystallinity (76–97%). The unit cell parameters, correlated to the degree of structural carbonate, were sensitive to the Ca/P ratio. Instead, temperature governed the microstructural parameters. Less strained and larger crystals were obtained at higher temperatures. Long-term aging up to 6 months at 20 °C compensated for higher crystal growth kinetics at higher temperature. - Graphical abstract: Controlled synthesis of carbonated apatite at moderate temperatures using nanolime and sodiumhexametaphosphate as starting reagent. - Highlights: • Chemical synthesis of nano-sized apatite with tailored microstructure was performed. • Colloidal Ca(OH){sub 2} and a phosphorus-based chelating agents were used as reagents. • The method is simple and reproducible which facilitate industrial process scale-up. • Rietveld refinement strategies for product characterization were developed. • Rietveld analyses provided yield, microstructural and structure information.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2016

Photocatalytic activity of SnO{sub 2} nanoparticles in methylene blue degradation

Highlights: • Nanosized SnO{sub 2} photocatalysts were prepared with a precipitation method. • SnO{sub 2} nanoparticles displayed high photocatalytic activities for the MB degradation. • OH radicals are the main active species in photocatalysis on the SnO{sub 2} nanoparticles. - Abstract: Nanosized SnO{sub 2} photocatalysts were prepared with a precipitation method and were characterized by performing transmission electron microscopy (TEM), powder X-ray diffraction (XRD), and X-ray absorption spectroscopy (XAS). The powder XRD results revealed that the SnO{sub 2} nanoparticles have a typical tetragonal rutile (cassiterite) structure and the average crystallite size was found to be approximately 4.5 nm by using the Debye–Scherrer equation. The prepared SnO{sub 2} nanoparticles consist of agglomerated particles with a mean diameter of around 4–5 nm according to the analysis of TEM images. The XAS data confirmed that the prepared samples have cassiterite structures with tin oxidation state of +4. The prepared SnO{sub 2} nanoparticles were found to exhibit approximately 3.8 times higher activity than bulk SnO{sub 2} in the photodegradation of methylene blue. On the basis of a trapping experiment, we developed a possible mechanism for the photodegradation on SnO{sub 2} nanoparticles.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Significant increase of Curie temperature in nano-scale BaTiO{sub 3}

The low Curie temperature (T{sub c} = 130 °C) of bulk BaTiO{sub 3} greatly limits its applications. In this work, the phase structures of BaTiO{sub 3} nanoparticles with sizes ranging from 2.5 nm to 10 nm were studied at various temperatures by using aberration-corrected transmission electron microscopy (TEM) equipped with an in-situ heating holder. The results implied that each BaTiO{sub 3} nanoparticle was composed of different phases, and the ferroelectric ones were observed in the shells due to the complicated surface structure. The ferroelectric phases in BaTiO{sub 3} nanoparticles remained at 600 °C, suggesting a significant increase of T{sub c}. Based on the in-situ TEM results and the data reported by others, temperature-size phase diagrams for BaTiO{sub 3} particles and ceramics were proposed, showing that the phase transition became diffused and the T{sub c} obviously increased with decreasing size. The present work sheds light on the design and fabrication of advanced devices for high temperature applications.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2016

Study of static and dynamic magnetic properties of Fe nanoparticles composited with activated carbon

Nanocomposite of Fe nanoparticles with activated carbon has been synthesized to alter the magnetic spin-spin interaction and hence study the dilution effect on the static and dynamic magnetic properties of the Fe nanoparticle system. Transmission electron microscopic (TEM) image shows the spherical Fe nanoparticles dispersed in carbon matrix with 13.8 nm particle size. Temperature dependent magnetization measurement does not show any blocking temperature at all, right up to the room temperature. Magnetic hysteresis curve, taken at 300 K, shows small value of the coercivity and this small hysteresis indicates the presence of an energy barrier and inherent magnetization dynamics. Langevin function fitting of the hysteresis curve gives almost similar value of particle size as obtained from TEM analysis. Magnetic relaxation data, taken at a temperature of 100 K, were fitted with a combination of two exponentially decaying function. This diluted form of nanoparticle system, which has particles size in the superparamagnetic limit, behaves like a dilute ensemble of superspins with large value of the magnetic anisotropic barrier.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2016

Synthesis micro-scale boron nitride nanotubes at low substrate temperature

High temperature synthesis methods produce defects in 1D nanomaterials, which ultimately limit their applications. We report here the synthesis of micro-scale boron nitride nanotubes (BNNT) at low substrate temperature (300 {sup o}C) using a pulsed CO{sub 2} laser deposition technique in the presence of catalyst. The electron microscopic analyses have shown the nanotubes distributed randomly on the surface of the substrate. The average diameter (∼0.25 μm) of a nanotube, which is the highest reported value to date, is estimated by SEM data and confirmed by TEM measurements. These nanotubes are promising for high response deep-UV photo-luminescent devices. A detailed synthesis mechanism is presented and correlated with the experimental results.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2015

Ecosystem biogeochemistry model parameterization: Do more flux data result in a better model in predicting carbon flux?

Reliability of terrestrial ecosystem models highly depends on the quantity and quality of thedata that have been used to calibrate the models. Nowadays, in situ observations of carbon fluxes areabundant. However, the knowledge of how much data (data length) and which subset of the time seriesdata (data period) should be used to effectively calibrate the model is still lacking. This study uses theAmeriFlux carbon flux data to parameterize the Terrestrial Ecosystem Model (TEM) with an adjoint-baseddata assimilation technique for various ecosystem types. Parameterization experiments are thus conductedto explore the impact of both data length and data period on the uncertainty reduction of the posteriormodel parameters and the quantification of site and regional carbon dynamics. We find that: the modelis better constrained when it uses two-year data comparing to using one-year data. Further, two-year datais sufficient in calibrating TEM’s carbon dynamics, since using three-year data could only marginallyimprove the model performance at our study sites; the model is better constrained with the data thathave a higher‘‘climate variability’’than that having a lower one. The climate variability is used to measurethe overall possibility of the ecosystem to experience all climatic conditions including drought and extremeair temperatures and radiation; the U.S. regional simulations indicate that the effect of calibration datalength on carbon dynamics is amplified at regional and temporal scales, leading to large discrepanciesamong different parameterization experiments, especially in July and August. Our findings areconditioned on the specific model we used and the calibration sites we selected. The optimal calibrationdata length may not be suitable for other models. However, this study demonstrates that there may exist athreshold for calibration data length and simply using more data would not guarantee a better modelparameterization and prediction. More importantly, climate variability might be an effective indicator ofinformation within the data, which could help data selection for model parameterization. As a result, we believe ourfindings will benefit the ecosystem modeling community in using multiple-year data to improve modelpredictability.

59 BASIC BIOLOGICAL SCIENCES↗
DOE OSTI2016

Green synthesis of ZnO nanoparticles via complex formation by using Curcuma longa extract

Synthesis of ZnO nanoparticles(NPs) were conducted via Zn(II) complex formation by using Curcuma longa extract as template. Curcuma longa extract has the ability to form zinc ions complex with curcumin as ligating agent. Study on synthesis was conducted by monitoring thermal degradation of the material. Successful formation of zinc oxide nanoparticles was confirmed by employing x-ray diffraction, surface area analysis and transmission electron microscopy(TEM) studies. From the XRD analysis it is denoted that ZnO in hexagonal wurtzite phase was formed and particle size was varied as varied temperature. The data are also confirmed by TEM analysis which shows the particle sie at the range 20-80nm. The NPs exhibited excelent photocatalytic activity for methylene blue degradation and also significant antibacterial activity for Eschericia coli. The activity in methylene blue degradation was also confirmed from fast chemical oxygen demand (COD) reduction.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2015

Investigation of defect clusters in ion-irradiated Ni and NiCo using diffuse X-ray scattering and electron microscopy

The nature of defect clusters in Ni and Ni$_{50}$Co$_{50}$ (NiCo) irradiated at room temperature with 2–16 MeV Ni ions is studied using asymptotic diffuse X-ray scattering and transmission electron microscopy (TEM). Analysis of the scattering data provides separate size distributions for vacancy and interstitial type defect clusters, showing that both types of defect clusters have a smaller size and higher density in NiCo than in Ni. Diffuse scattering results show good quantitative agreement with TEM results for cluster sizes greater than 4 nm diameter, but find that the majority of vacancy clusters are under 2 nm in NiCo, which, if not detected, would lead to the conclusion that defect density was actually lower in the alloy. Interstitial dislocation loops and stacking fault tetrahedra are identified by TEM. Lastly comparison of diffuse scattering lineshapes to those calculated for dislocation loops and SFTs indicates that most of the vacancy clusters are SFTs.

36 MATERIALS SCIENCE↗
DOE OSTI2025

MultiTaskDeltaNet: change detection-based image segmentation for operando ETEM with application to carbon gasification kinetics

Transforming in situ transmission electron microscopy (TEM) imaging into a tool for spatially-resolved operando characterization of solid-state reactions requires automated, high-precision semantic segmentation of dynamically evolving features. However, traditional deep learning methods for semantic segmentation often face limitations due to the scarcity of labeled data, visually ambiguous features of interest, and scenarios involving small objects. To tackle these challenges, we introduce MultiTaskDeltaNet (MTDN), a novel deep learning architecture that creatively reconceptualizes the segmentation task as a change detection problem. By implementing a unique Siamese network with a U-Net backbone and using paired images to capture feature changes, MTDN effectively leverages minimal data to produce high-quality segmentations. Furthermore, MTDN utilizes a multi-task learning strategy to exploit correlations between physical features of interest. In an evaluation using data from in situ environmental TEM (ETEM) videos of filamentous carbon gasification, MTDN demonstrated a significant advantage over conventional segmentation models, particularly in accurately delineating fine structural features. Notably, MTDN achieved a 10.22% performance improvement over conventional segmentation models in predicting small and visually ambiguous physical features. This work bridges key gaps between deep learning and practical TEM image analysis, advancing automated characterization of nanomaterials in complex experimental settings.

08 HYDROGEN↗
NASA NTRS1993

The EET87513 clast N: A CM2 fragment in an HED polymict breccia

Xenoliths of material resembling carbonaceous chondrites have been found in several HED polymict breccias. Most workers concluded that these clasts are related to CM2 meteorites on the basis of texture, bulk composition, and mineralogy. Data on clast N, a carbonaceous chondrite fragment from the howardite EET87513 large enough (approximately 4x5mm on the surface of the slab from which it was separated) to extract bulk samples for INAA and oxygen isotope analysis and to provide a thin section for electron microprobe, SEM, and TEM analysis is reported. Preliminary data for this clast were previously reported. INAA was performed at Oregon State University and bulk oxygen isotopic composition was determined at the University of Chicago. These data confirm that EET87513 clast N is a fragment of CM2 material.

Buchanan, P. C.↗
DOE OSTI2017

Aggregation of cyclic polypeptoids bearing zwitterionic end-groups with attractive dipole–dipole and solvophobic interactions: a study by small-angle neutron scattering and molecular dynamics simulation

Aggregation behavior of cyclic polypeptoids bearing zwitterionic end-groups in methanol has been studied using a combination of experimental and simulation techniques. Here, the data from SANS and cryo-TEM indicate that the solution contains small clusters of these cyclic polypeptoids, ranging from a single polypeptoid chain to small oligomers, while the linear counterpart shows no cluster formation. Atomistic molecular dynamics simulations reveal that the driving force for this clustering behavior is due to the interplay between the effective repulsion due to the solvation of the dipoles formed by the charged end-groups in each polypeptoid chain and the attractive forces due to dipole–dipole interactions and the solvophobic effect.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2022

Crystallization kinetics and thermodynamics of an Ag–In–Sb–Te phase change material using complementary in situ microscopic techniques

The crystallization of an amorphous Ag–In–Sb–Te (AIST) phase change material (PCM) is studied using multiple in situ imaging techniques to directly quantify crystal growth rates over a broad range of temperatures. The measurable growth rates span from ≈ 10 –9 to ≈ 20 m/s. Recent results using dynamic transmission electron microscopy (TEM), a photoemission TEM technique, and TEM with sub-framed imaging are reported here and placed into the context of previous growth rate measurements on AIST. Dynamic TEM experiments show a maximum observed crystal growth rate for as-deposited films to be > 20 m/s. It is shown that crystal growth above the glass transition can be imaged in a TEM through use of subframing and a high-frame-rate direct electron detection camera. Challenges associated with the determination of temperature during in situ TEM experiments are described. Finally, preliminary nanocalorimetry results demonstrate the feasibility of collecting thermodynamic data for crystallization of PCMs with simultaneous TEM imaging.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Cu Doping Increases Capacity Retention in LiNi 0.6 Mn 0.2 Co 0.2 O 2 (NMC622) by Altering the Potential of the Ni-Based Redox Couple and Inhibiting Particle Pulverization

To discern the influence of Cu 2+ as a dopant on both the structural and electrochemical characteristics of LiNi 0.6 Mn 0.2 Co 0.2 O 2 (NMC622), Cu 2+ (aq) was added to the coprecipitation synthesis from the constituent ions. At 5 mol % Cu 2+ , a single-phase Cu-NMC product results, evidenced by an increase in d-spacing along the [003] and [104] directions and a slight increase in the crystal volume of the R–3m hexagonal (rock-salt superstructure) lattice. XRD data and high-resolution TEM imaging support Cu 2+ doping primarily on the transition metal 3b Wyckoff sites. Here, galvanostatic cycling of Cu-NMC shows a reversible gravimetric capacity of 102 mAh/g compared to 136 mAh/g for undoped NMC. Despite the lower capacity, the discharge capacity retention of Cu-NMC is 89% after 100 cycles compared to only 70% for NMC. XPS analysis reveals that this lower capacity is due to an increase in the concentration of Ni 3+ ions at the surface, while XRD data collected at the top and bottom of charge show a smaller decrease in crystalline domain size for Cu-NMC (40.5% decrease) compared to NMC (74.7% decrease), translating to pulverization of the secondary particles.

25 ENERGY STORAGE↗
DOE OSTI2016

In Situ TEM Microcompression Pillar Size Effects in Fe-9Cr ODS

The objective of this paper is to ascertain the existence of a specimen size threshold, below which the material no longer exhibits bulk mechanical behavior when tested using in situ transmission electron microscopic (TEM) micro-compression pillars. In this work, sub-micron sized pillars of a model Fe-9Cr oxide dispersion strengthened (ODS) alloy were compressed in TEM in situ at room temperature, and attempts have been made to quantify the resulting data. Results are compared to mechanical property values in the archival literature, and a discussion on the validity of quantitative in situ TEM micro-compression data for ODS steel is included. In situ TEM mechanical testing is a relatively new technique enabling concurrent TEM imaging and mechanical testing of sub-micron-sized electron-transparent specimens. Due to limited sample volume of many nuclear materials, in situ TEM mechanical testing holds great promise for advancing our understanding of deformation phenomena. But it is well known that the dramatically reduced specimen size required for in situ testing can affect quantitative and qualitative deformation behaviors. However, Kiener, et al. used in situ TEM micro-compression pillars on irradiated and unirradiated single-crystal copper. They observed size independence in the irradiated material, while the unnirradiated material displayed a size threshold below which the mechanical properties deviated from those of bulk Cu. They assert that the more densely-spaced obstacles in irradiated Cu allow it to display bulk properties even in specimens having ∼ 100 nm dimensions. Similar to Kiener's findings, we hypothesize that unirradiated ODS will demonstrate a size threshold, but the in situ TEM micro-compression technique can be extended from single crystal materials to engineering alloys. An Fe-9Cr model ODS alloy was chosen for this study because of the broad interest in ODS for advanced nuclear reactors. ODS alloys exhibit high irradiation tolerance and high temperature creep resistance. New insight into deformation processes gained through in situ TEM mechanical testing could be valuable for the validation of ODS alloys for next generation nuclear reactors. The fact that the compressive yield stress and elastic modulus do not follow distinct trends as a function of specimen size is likely due to the high density of obstacles to dislocation motion. The ODS microstructure contains such obstacles as oxide nanoparticles, a fine grain structure, a high density of dislocation lines, and carbide precipitates. Since the deformation behavior is governed by the minimum separation distance between obstacles [1], it is plausible that the high obstacle density enables ODS alloy micropillars to exhibit bulk-like mechanical properties even prior to irradiation. Future work will focus on: (1) developing finite element models to help explain the difference in elastic moduli between bulk and micropillar tests, (2) understanding the spread in yield stress measurements at fixed micropillar volumes, and (3) extending this study to irradiated ODS. (authors)

36 MATERIALS SCIENCE↗
DOE OSTI2018

Investigation of Superparamagnetism in Microwave and Conventional Processed Mn{sub 0.5}Zn{sub 0.5}Fe{sub 2}O{sub 4} Nanoparticles

Nanoparticles of spinel cubic Mn{sub 0.5}Zn{sub 0.5}Fe{sub 2}O{sub 4} are first prepared by the coprecipitation method and then subjected to conventional solid-state sintering and microwave processing techniques. Particle sizes are estimated by field emission scanning electron microscopy (FESEM) to be in the nanometer (5–13 nm) range. Transmission electron microscopy (TEM) also supports the FESEM data. The magnetization measurement by vibration sample magnetometry of the conventionally sintered sample shows a paramagnetic nature at room temperature, a superparamagnetic behaviour at low temperature, and a ferromagnetic nature at even lower temperature. The blocking temperature is estimated to be nearly 110 K. Microwave-processed samples show a superparamagnetic nature even at room temperature. The Fe{sup 3+} cations are found at both the sites confirmed by X-ray photoelectron spectroscopy (XPS), are prepared by microwave processing, and have better magnetic properties as compared to the conventionally sintered particles.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2015

The impact of aqueous medium on zeolite framework integrity

Understanding the zeolite framework stability in aqueous phase is crucial to develop stable catalysts. Al K–edge, extended X–ray absorption fine structure and 27Al MAS NMR spectroscopies in combination with DFT calculations have been used to monitor both qualitative and quantitative structural changes of two well–characterized samples with BEA structure. The effects of various properties on stability were explored, including Al concentration, Al distribution, particle size and structural defects. As the samples were degraded by treatment in hot liquid water, the local structure about the Al T–site remained mostly intact, including the Al–O–Si angles and bond distances, while the nano–scale crystalline structure as measured by XRD and TEM was disrupted. The combined data suggest a three–step mechanism in which, initially, the HBEA framework crystallinity decreases via hydrolysis of T–O bonds along polymorph stacking faults and inter–grain boundaries in a mode similar to crack propagation in glass. With prolonged exposure, amorphization occurs via hydrolysis of surface Si–OH groups propagating inward through the zeolite lattice. In parallel, cracks propagate within the crystalline micro–domains along paths through specific T–O–T groups. Authors thank B. W. Arey (PNNL) for HIM measurements, T. Huthwelker for support during Al XAFS measurements at the Swiss Light Source (PSI, Switzerland) and M. Y. Hu (PNNL) for support during NMR experiments. This work was supported by the U. S. Department of Energy (DOE), Office of Science, Office of Basic Energy Sciences, Division of Chemical Sciences, Geosciences & Biosciences. NMR experiments were performed at the Environmental Molecular Science Laboratory, a national scientific user facility sponsored by the DOE’s Office of Biological and Environmental Research, and Physical Science Laboratory both located at Pacific Northwest National Laboratory (PNNL). PNNL is a multi–program national laboratory operated for DOE by Battelle under Contract No. DE–AC05–76RL01830.

Environmental Molecular Sciences Laboratory↗