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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 559 records · Page 31
All sourcesNASA NTRSDOE OSTI
DOE OSTI2023

3D Visualization of Proteins within Metal–Organic Frameworks via Ferritin‐Enabled Electron Microscopy

Abstract Electron tomography holds great promise as a tool for investigating the 3D morphologies and internal structures of metal‐organic framework‐based protein biocomposites (protein@MOFs). Understanding the 3D spatial arrangement of proteins within protein@MOFs is paramount for developing synthetic methods to control their spatial localization and distribution patterns within the biocomposite crystals. In this study, the naturally occurring iron oxide mineral core of the protein horse spleen ferritin (Fn) is leveraged as a contrast agent to directly observe individual proteins once encapsulated into MOFs by electron microscopy techniques. This methodology couples scanning electron microscopy, transmission electron microscopy, and electron tomography to garner detailed 2D and 3D structural interpretations of where proteins spatially lie in Fn@MOF crystals, addressing the significant gaps in understanding how synthetic conditions relate to overall protein spatial localization and aggregation. These findings collectively reveal that adjusting the ligand‐to‐metal ratios, protein concentration, and the use of denaturing agents alters how proteins are arranged, localized, and aggregated within MOF crystals.

Chemistry↗
DOE OSTI2017

Characterization of Sulfur and Nanostructured Sulfur Battery Cathodes in Electron Microscopy Without Sublimation Artifacts

Abstract Lithium sulfur (Li–S) batteries have the potential to provide higher energy storage density at lower cost than conventional lithium ion batteries. A key challenge for Li–S batteries is the loss of sulfur to the electrolyte during cycling. This loss can be mitigated by sequestering the sulfur in nanostructured carbon–sulfur composites. The nanoscale characterization of the sulfur distribution within these complex nanostructured electrodes is normally performed by electron microscopy, but sulfur sublimates and redistributes in the high-vacuum conditions of conventional electron microscopes. The resulting sublimation artifacts render characterization of sulfur in conventional electron microscopes problematic and unreliable. Here, we demonstrate two techniques, cryogenic transmission electron microscopy (cryo-TEM) and scanning electron microscopy in air (airSEM), that enable the reliable characterization of sulfur across multiple length scales by suppressing sulfur sublimation. We use cryo-TEM and airSEM to examine carbon–sulfur composites synthesized for use as Li–S battery cathodes, noting several cases where the commonly employed sulfur melt infusion method is highly inefficient at infiltrating sulfur into porous carbon hosts.

25 ENERGY STORAGE↗
DOE OSTI2020

Solid-State Sintering of Core-Shell Ceramic Powders Fabricated by Particle Atomic Layer Deposition

The properties of technical ceramics are highly dependent on their microstructure, which evolves during sintering. Sintering is the process by which ceramic parts are subjected to high temperatures to activate chemical diffusion and the consumption of porosity. During the initial stage of sintering, interparticle necks between neighboring particles form and subsequently increase in size, consuming porosity as the particle centers move closer together. To experimentally determine how this process depends on particle surface composition, particle atomic layer deposition (ALD) was used to deposit a thin film of amorphous aluminum oxide (Al2O3) onto yttria-stabilized tetragonal zirconia (3YSZ) particles, producing core-shell structured powders. The uniformity of the Al2O3 film was confirmed with transmission electron microscopy and energy dispersive spectroscopy. Scanning electron microscopy was used to observe microstructural evolution during sintering, and the dihedral angles of Al2O3 and 3YSZ grains were measured to determine the ratio of interfacial energies between the 3YSZ|3YSZ, 3YSZ|Al2O3, and Al2O3|Al2O3 interfaces. Analysis of the densification kinetics revealed that the initial stage of densification is dependent on the material at the surface of the particles (ie, the Al2O3 film) and is controlled by the diffusion of Al3+ cations through Al2O3. Once the Al2O3 film has coalesced, the sintering behavior is controlled by the densification of the core material (3YSZ). Thus, core-shell powders fabricated by particle ALD sinter by a two-step process where the kinetics are dependent on the material present at interparticle contacts.

alumina↗
NASA NTRS2003

Individual Aerosol Particles from Biomass Burning in Southern Africa Compositions and Aging of Inorganic Particles: Compositions and Aging of Inorganic Particles - 2

Individual aerosol particles collected over southern Africa during the SAFARI 2000 field study were studied using transmission electron microscopy and field-emission scanning electron microscopy. The sizes, shapes, compositions, mixing states, surface coatings, and relative abundances of aerosol particles from biomass burning, in boundary layer hazes, and in the free troposphere were compared, with emphasis on aging and reactions of inorganic smoke particles. Potassium salts and organic particles were the predominant species in the smoke, and most were internally mixed. More KCl particles occur in young smoke, whereas more K2SO4 and KNO3 particles were present in aged smoke. This change indicates that with the aging of the smoke, KCl particles from the fires were converted to K2SO4 and KNO3 through reactions with sulfur- and nitrogen- bearing species from biomass burning as well as other sources. More soot was present in smoke from flaming grass fires than bush and wood fires, probably due to the predominance of flaming combustion in grass fires. The high abundance of organic particles and soluble salts can affect the hygroscopic properties of biomass-burning aerosols and therefore influence their role as cloud condensation nuclei. Particles from biomass burning were important constituents of the regional hazes.

Li, Jia↗
DOE OSTI2023

Operando Electrochemical Liquid-Cell Scanning Transmission Electron Microscopy (EC-STEM) Studies of Evolving Cu Nanocatalysts for CO 2 Electroreduction

The design and synthesis of nanocatalysts with well-defined sizes, compositions, and structures have revolutionized our accessibility to tunable catalyst activity and selectivity for a variety of energy-related electrochemical reactions. Nonetheless, establishing structure-(re)activity correlations requires the understanding of the dynamic evolution of pristine nanocatalysts and the identification of their active states under operating conditions. We previously communicated the operando observation of Cu nanocatalysts evolving into active metallic Cu nanograins for CO 2 electroreduction (Yang et al. Nature 2023, 614, 262–269). Here, we expand our discussion to the technical capabilities and further research applications of operando electrochemical liquid-cell scanning transmission electron microscopy (EC-STEM), which enables quantitative electrochemistry while tracking dynamic structural evolution of sub-10 nm Cu nanocatalysts. The coexistent H 2 bubbles, often disruptive to operando spectroscopy, are an effective approach to create a thin-liquid layer that significantly improves spatial resolution while remaining electrochemically accessible to Cu nanocatalysts. Operando four-dimensional (4D) STEM in liquids provides insights into the complex structure of active polycrystalline metallic Cu nanograins. With continuous technical developments, we anticipate that operando EC-STEM will evolve into a powerful electroanalytical method to advance our understanding of a variety of nanoscale electrocatalysts at solid/liquid interfaces.

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

Environmentally induced chemical and morphological heterogeneity of zinc oxide thin films

Zinc oxide (ZnO) thin films have been reported to suffer from degradation in electrical properties, when exposed to elevated heat and humidity, often leading to failures of electronic devices containing ZnO films. This degradation appears to be linked to water and oxygen penetration into the ZnO film. However, a direct observation in the ZnO film morphological evolution detailing structural and chemical changes has been lacking. Here, we systematically investigated the chemical and morphological heterogeneities of ZnO thin films caused by elevated heat and humidity, simulating an environmental aging. X-ray fluorescence microscopy, X-ray absorption spectroscopy, grazing incidence small angle and wide angle X-ray scattering, scanning electron microscopy (SEM), ultra-high-resolution SEM, and optical microscopy were carried out to examine ZnO and Al-doped ZnO thin films on two different substrates—silicon wafers and flexible polyethylene terephthalate (PET) films. In the un-doped ZnO thin film, the simulated environmental aging is resulting in pin-holes. In the Al-doped ZnO thin films, significant morphological changes occurred after the treatment, with an appearance of platelet-shaped structures that are 100–200 nm wide by 1μm long. Synchrotron x-ray characterization further confirmed the heterogeneity in the aged Al-doped ZnO, showing the formation of anisotropic structures and disordering. X-ray diffraction and X-ray absorption spectroscopy indicated the formation of a zinc hydroxide in the aged Al-doped films. In conclusion, utilizing advanced characterization methods, our studies provided information with an unprecedented level of details and revealed the chemical and morphologically heterogeneous nature of the degradation in ZnO thin films.

36 MATERIALS SCIENCE↗
NASA NTRS1992

Theory and application of scanning electron acoustic microscopy

A three-dimensional theoretical model based on the application of the thermal conduction and Navier equations to a chopped electron beam incident on a disk specimen is used to obtain the particle displacement field in the specimen. The results lead to a consideration of the signal generation, spatial resolution, and contrast mechanisms in scanning electron acoustic microscopy (SEAM). The model suggests that the time-variant heat source produced by the beam chopping generates driving source, thermal wave, and acoustic wave displacements simultaneously in the specimen. Evidence of the correctness of the prediction is obtained from the mathematically similar problem of pulsed laser light injection into a tank of water. High speed Schlieren photographs taken following laser injection show the simultaneous evolution of thermal and acoustic waveforms. Examples of contrast reversal, stress-induced contrast, and acoustic zone contrast and resolution with SEAM are presented and explained in terms of the model features.

Cantrell, John H.↗
DOE OSTI2021

A Focused Ion Beam-Scanning Transmission Electron Microscopy with Energy-Dispersive X-ray Spectroscopy Study on Technetium Incorporation within Iron Oxides through Fe(OH) 2 (s) Mineral Transformation

Incorporation of Tc(IV) into iron oxide/hydroxide minerals has been explored and proposed as a promising pathway to preventing Tc(IV) reoxidation to environmentally mobile pertechnetate (TcO 4 - ) and improving long-term immobilization of radioactive technetium-99 (Tc). However, visual evidence evaluating the distribution of Tc(IV) incorporated within iron oxide/hydroxide phases has not been available, until now, despite potential implications on Tc(IV) stability within the host phase. For the purpose of this study Tc(IV) incorporation into iron oxide/hydroxide phases was facilitated via Fe(OH) 2 (s) oxidation and mineral transformation to magnetite (Fe 3 O 4 ). Focused ion beam - scanning transmission electron microscopy equipped with energy-dispersive X-ray spectroscopy (FIB/STEM-EDS) methods were then combined with X-ray diffraction and absorption spectroscopy techniques to characterize and visually demonstrate that, for the first time, Tc(IV) is heterogeneously incorporated into different iron oxide/hydroxide phases as Tc(IV)-incorporated magnetite and/or TcO 2 ·2H 2 O(s) via different incorporation mechanisms. Heterogeneous distribution of Tc(IV) in magnetite suggests either (i) TcO4- is reduced quickly at the magnetite surface and then encapsulated into magnetite during continued octahedral crystal growth, or (ii) Tc(IV) alternatively partitioned into multiple layers of a blocky, plate-like morphological magnetite structure showing stratified Tc. With limited Tc-hematite (Fe 2 O 3 ) incorporation, the results suggest that TcO 2 ·2H 2 O(s) is formed and mainly associated/embedded in fibrous nanometer-sized polycrystalline hematite. This work highlights the power of modern state-of-the-art FIB/STEM-EDS approach to provide essential visual insights of the Tc-iron oxide/hydroxide incorporation and generate reliable mechanism-informed designs for waste forms relying on Tc mineral incorporation.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2022

Dynamics of the gold–silicon eutectic reaction studied at limited length scales using in situ $\mathrm{TEM}$ and $\mathrm{STEM}$

We report the dynamics of the gold–silicon eutectic reaction in limited dimensions were studied using in situ transmission electron microscopy and scanning transmission electron microscopy heating experiments. The phase transformation, viewed in both plan-view and cross-section of the film, occurs through a complex combination of dislocation and grain boundary motion and diffusion of silicon along gold grain boundaries, which results in a dramatic change in the microstructure of the film. The conversion observed in cross-section shows that the eutectic mixture forms at the Au–Si interface and proceeds into the Au film at a discontinuous growth rate. This complex process can lead to a variety of microstructures depending on sample geometry, heating temperature, and the ratio of gold to silicon which was found to have the largest impact on the eutectic microstructure. The eutectic morphology varied from dendrites to hollow rectangular structures to Au–Si eutectic agglomerates with increasing silicon to gold ratio.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Strain-driven oxygen vacancy ordering in LaNiO 3 thin films revealed by integrated differential phase contrast imaging in scanning transmission electron microscopy

Rare-earth nickelates, such as LaNiO 3 (LNO), exhibit complex electronic properties, with ordered oxygen vacancies (OOV) influencing conductivity and magnetic behavior. We investigate the structural stability of strain-induced OOV phases in LNO thin films grown on SrTiO 3 substrates and the impact of Ruddlesden–Popper (RP) faults. Using high-angle annular dark-field scanning transmission electron microscopy (HAADF-STEM) and integrated differential phase contrast (iDPC) STEM imaging, we conducted atomic-scale structural and compositional analyses of OOV. Geometric phase analysis (GPA) was employed to measure the strain in fault-free and RP fault regions, while density functional theory (DFT) calculations explored different OOV arrangements in the LNO phase. Simulated iDPC-STEM imaging of energy-stabilized structures was performed to correlate with experimental results. Here, our findings reveal superstructure modulation in the chemical composition and atomic-scale lattice structure in LNO, primarily due to the formation of the OOV in Ni–O layers of the LaNiO 2.5 phase. The out-of-plane compressive strain of about 2% stabilizes this phase, reducing the strain, diminishing OOV, and transforming them into LNO.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Measuring Mass-Based Hygroscopicity of Atmospheric Particles through in situ Imaging

Quantifying how atmospheric particles interact with water vapor is critical for understanding the effects of aerosols on climate. We present a novel method to measure the mass-based hygroscopicity of particles while characterizing their elemental and carbon functional group compositions. Since mass-based hygroscopicity is insensitive to particle geometry, it is advantageous for probing the hygroscopic behavior of atmospheric particles, which can have irregular morphologies. Combining scanning electron microscopy with energy dispersive X-ray analysis (SEM/EDX), scanning transmission X-ray microscopy (STXM) analysis, and in situ STXM humidification experiments, this method was validated using laboratory-generated, atmospherically relevant particles. Then, the hygroscopicity and elemental composition of 15 complex atmospheric particles were analyzed by leveraging quantification of C, N, and O from STXM, and complementary elemental quantification from SEM/EDX. We found three types of hygroscopic responses, and correlated high hygroscopicity with Na and Cl content. The mixing state determined for 158 particles broadly agreed with those of the humidified particles, indicating the potential to infer the atmospheric hygroscopic behavior from a selected subset of particles. These methods offer unique quantitative capabilities to characterize and correlate the hygroscopicity and chemistry of individual submicron atmospheric particles.

Environmental Molecular Sciences Laboratory↗
DOE OSTI2023

High-Energy X-ray Diffraction Microscopy for Nuclear Forensics (FY23 Project Report)

Morphological information on nuclear material has been identified using visible light and scanning electron microscopy. These identify qualitative differences in particle morphology. Three-dimensional imaging of materials through alternating scanning electron microscopy imaging and focused ion beam milling has also been used. Unfortunately, these techniques are time- and labor-intensive, with significant sample preparation required and lengthy analysis times. Further, the resulting 3D images are qualitative, require manual identification, and do not capture statistically-representative populations. High energy X-ray 3D imaging using a direct-beam or diffracted-beam (High-Energy Diffraction Microscopy) have been developed at the Advanced Photon Source and can produce quantitative information on grains (phase, location, etc.) and pores (size distribution, sphericity) in a material. These techniques require only minutes to characterize a sample volume and are non-destructive, thus suitable for a wide range of existing samples and for confirmatory analyses to be carried out using conventional microscopy techniques.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Size-Resolved Chemical Composition of Particles Collected Using STAC at the Ground Site During the SAIL Campaign in Gunnison, Colorado

Aerosol particles were collected using a four-stage Size and Time-resolved Aerosol Collector (STAC) during the SAIL field campaign. Each stage of STAC separates particles into distinct aerodynamic size fractions with 50% cut-off diameters: Stage A: 2.27 µm Stage B: 0.615 µm Stage C: 0.421 µm Stage D: 0.119 µm Each stage provides both size- and time-resolved sampling, enabling investigation of particle composition across different atmospheric regimes. Only a subset of samples was selected for analysis based on prevailing meteorological conditions (e.g., temperature, humidity, and air-mass influence) to capture representative aerosol types under distinct weather patterns. Collected substrates were first examined under Scanning Electron Microscopy (SEM) to evaluate particle loading, morphology, and spatial distribution. Subsequently, Computer-Controlled Scanning Electron Microscopy with Energy-Dispersive X-ray Spectroscopy (CCSEM/EDX) was performed to obtain size-resolved elemental composition of individual particles. A rule-based classification scheme was applied to categorize particles into major compositional groups (e.g., biological, carbonaceous, dust, sulfate, Na-rich, and mixed types). This dataset provides high-resolution morphological and chemical information on atmospheric particles collected during the SAIL campaign, offering insights into the influence of meteorology on aerosol composition and mixing state.

Size and Time-resolved Aerosol Collector↗
DOE OSTI2015

Ablation of (GeS{sub 2}){sub 0.3}(Sb{sub 2}S{sub 3}){sub 0.7} glass with an ultra-violet nano-second laser

Highlights: • The interaction of (GeS{sub 2}){sub 0.3}(Sb{sub 2}S{sub 3}){sub 0.7} bulk glass and film with UV nanosecond laser. • Ablation process, topography of crater and structure of the material were studied. • Ablation threshold fluencies changed with the spot diameter and number of pulses. • The photo-thermal expansion of the material occurred for low laser fluency. • Laser direct writing process applicable for fabrication of passive optical elements. - Abstract: The results of an experimental study of the laser ablation of bulk and thin films of a GeSbS chalcogenide glass using UV nanosecond pulses are reported. The response of the samples to illumination conditions was studied through the use of atomic force spectroscopy, digital holographic microscopy, Raman scattering and scanning electron microscopy. The multi-pulse ablation thresholds were determined for both the bulk and thin film samples for varying number of pulses and illuminated spot diameter. The possible application of direct laser writing into the bulk and thin films of this material is presented.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Exploring 3D leaf anatomical traits for C 4 photosynthesis: chloroplast and plasmodesmata pit field size in maize and sugarcane

Summary Volume and surface area of chloroplasts and surface area of plasmodesmata pit fields are presented for two C 4 species, maize and sugarcane, with respect to cell surface area and cell volume. Serial block face scanning electron microscopy (SBF‐SEM) and confocal laser scanning microscopy with the Airyscan system (LSM) were used. Chloroplast size estimates were much faster and easier using LSM than with SBF‐SEM; however, the results were more variable than SBF‐SEM. Mesophyll cells were lobed where chloroplasts were located, facilitating cell‐to‐cell connections while allowing for greater intercellular airspace exposure. Bundle sheath cells were cylindrical with chloroplasts arranged centrifugally. Chloroplasts occupied c. 30–50% of mesophyll cell volume, and 60–70% of bundle sheath cell volume. Roughly 2–3% of each cell surface area was covered by plasmodesmata pit fields for both bundle sheath and mesophyll cells. This work will aid future research to develop SBF‐SEM methodologies with the aim to better understand the effect of cell structure on C 4 photosynthesis.

3D leaf imaging↗
DOE OSTI2019

Atomic electrostatic maps of 1D channels in 2D semiconductors using 4D scanning transmission electron microscopy

Defects in materials give rise to fluctuations in electrostatic fields that reflect the local charge density, but imaging this with single atom sensitivity is challenging. However, if possible, this provides information about the energetics of adatom binding, localized conduction channels, molecular functionality and their relationship to individual bonds. Here, ultrastable electron-optics are combined with a high-speed 2D electron detector to map electrostatic fields around individual atoms in 2D monolayers using 4D scanning transmission electron microscopy. Simultaneous imaging of the electric field, phase, annular dark field and the total charge in 2D MoS 2 and WS 2 is demonstrated for pristine areas and regions with 1D wires. The in-gap states in sulphur line vacancies cause 1D electron-rich channels that are mapped experimentally and confirmed using density functional theory calculations. We show how electrostatic fields are sensitive in defective areas to changes of atomic bonding and structural determination beyond conventional imaging.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Scanning transmission electron microscopy (STEM) study on surface modified CVD diamond/Si(111) film post implanted Fe-B and NiFe-B related to GMR properties

Nanostructure investigation on the post implantation by Fe-B and NiFe-B on CVD diamond/Si(111) film have been studied by means of STEM related to their GMR phenomena. Two samples were investigated carefully, firstly sample is post NiFe-B at E=70keV and dose= 10{sup 15} ions/cm{sup 2} (denoted as A-E3D1). Secondly, is post FeB at E=20 keV and dose= 10{sup 15} ions/cm{sup 2} (denoted as B-E1D1). Based on FPP measurement at room temperature (RT) and H{sub applied} = 8 kOe, A-E3D1 sample has MR ratio almost 80% and MR ratio in B-E1D1 sample is 45%. Based on STEM-EDX investigation, there are two aspects of how MR ratio of A-E3D1 more higher than those of B-E1D1. Firstly, surface nanostructure on the top of A-E3D1 film is more grazing than on the top of B-E1D1. Analysis with Scanning Transmission Electron Microscope (STEM) equipped with Electron Energy Loss Spectroscopy (EELS) the growth of amorphous carbon layer on top of the implanted diamond film with thickness around 100 nm and only 20 nm on the no implanted sample have observed. Boron atoms were found inside the carbon amorphous layer distributed homogenously. Secondly, oxygen content at the interface between diamond film and silicon substrate in sample A-E3D1 was lower than those in B-E1D1 sample. This condition gives the resistance value in A-E3D1 lower than value in B-E1D1. This result is close to the Raman Spectroscopy data measurement which obviously suggests changes on the Raman spectrum due to implantation related to Oxygen excitation from B-E1D1 sample.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Surface plasmon resonance in nanostructured Ag incorporated ZnS films

Silver incorporated zinc sulfide thin films are prepared by RF magnetron sputtering technique and the influence of silver incorporation on the structural, optical and luminescence properties is analyzed using techniques like grazing incidence X-Ray diffraction (GIXRD), atomic force microscopy (AFM), field emission scanning electron microscopy (FESEM), energy dispersive X-ray spectroscopy (EDS), micro-Raman spectroscopy, UV-Vis spectroscopy and laser photoluminescence spectroscopy. XRD analysis presents hexagonal wurtzite structure for the films. A reduction of crystallinity of the films is observed due to Ag incorporation. The Raman spectral analysis confirms the reduction of crystallinity and increase of strain due to the Ag incorporation. AFM analysis reveals a rough surface morphology for the undoped film and Ag incorporation makes the films uniform, dense and smooth. A blue shift of band gap energy with increase in Ag incorporation is observed due to quantum confinement effect. An absorption band (450-650 nm region) due to surface plasmon resonance of the Ag clusters present in the ZnS matrix is observed for the samples with higher Ag incorporation. The complex dielectric constant, loss factor and distribution of volume and surface energy loss of the ZnS thin films are calculated. Laser photoluminescence measurements gives an intense bluish green emission from the ZnS films and a quenching of the PL emission is observed which can be due to the metal plasmonic absorption and non-radiative energy transfer due to Ag incorporation.

36 MATERIALS SCIENCE↗