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Results for “transition electron microscopy”

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 37 records · Page 2
All sourcesNASA NTRSDOE OSTI
DOE OSTI2020

Energy considerations regarding pulsed arc production of nanomaterials

Atmospheric arc discharge volumes have been estimated from the light distribution emitted during evaporation of graphite and molybdenum disulphide (MoS 2 ) anodes. These data have been correlated to the peak power in the case of pulsed arc discharge held at different frequencies (1, 2 and 5 Hz). The measured power density values and the corresponding specific energies per particle have been compared to DC values, and showed that pulsed arc discharges deliver electrical power more efficiently than DC arc discharges do with yet lower thermal loads. In particular, the power density of ≈1 kW/cm 3 characteristic of pulsed arcs (10-20 kW/cm 3 in DC) suffices to provide 15 eV/particle to the arc plasma (≈10 eV/particle or less in DC). Such an energy balance resulted in high ionization rates of the ablated material and production yields of carbon nanotubes around 10 11 cm -2 kWh -1 . Lastly, in situ probe experiments showed that pulsed arcs enhance the transport to substrate of the generated nanoparticles, such as graphene and MoS 2 monolayers. Pulsed anodic arcs open the possibility to generate further nanomaterials thanks to a more rational power investment and a better control of the discharge region.

42 ENGINEERING↗
NASA NTRS1989

Sequentially evaporated thin Y-Ba-Co-O superconducting films on microwave substrates

The development of high T sub c superconducting thin films on various microwave substrates is of major interest in space electronic systems. Thin films of YBa2Cu3O(7-Delta) were formed on SrTiO3, MgO, ZrO2 coated Al2O3, and LaAlO3 substrates by multi-layer sequential evaporation and subsequent annealing in oxygen. The technique allows controlled deposition of Cu, BaF2 and Y layers, as well as the ZrO buffer layers, to achieve reproducibility for microwave circuit fabrication. The three layer structure of Cu/BaF2/Y is repeated a minimum of four times. The films were annealed in an ambient of oxygen bubbled through water at temperatures between 850 C and 900 C followed by slow cooling (-2 C/minute) to 450 C, a low temperature anneal, and slow cooling to room temperature. Annealing times ranged from 15 minutes to 5 hrs. at high temperature and 0 to 6 hr. at 450 C. Silver contacts for four probe electrical measurements were formed by evaporation followed with an anneal at 500 C. The films were characterized by resistance-temperature measurements, energy dispersive X-ray spectroscopy, X-ray diffraction, and scanning electron microscopy. Critical transition temperatures ranged from 30 K to 87 K as a function of the substrate, composition of the film, thicknesses of the layers, and annealing conditions. Microwave ring resonator circuits were also patterned on these MgO and LaAlO3 substrates.

Valco, G. J.↗
DOE OSTI2020

1D to 2D Transition in Tellurium Observed by 4D Electron Microscopy

A new microwave-enhanced synthesis method for the production of tellurium nanostructures is reported here—with control over products from the 1D regime (sub-5 nm diameter nanowires), to nanoribbons, to the 2D tellurene regime—along with a new methodology for local statistical quantification of the crystallographic parameters of these materials at the nanometer scale. Using a direct electron detector and image-corrected microscope, large and robust 4D scanning transmission electron microscopy datasets for accurate structural analysis are obtained. These datasets allow the adaptation of quantitative techniques originally developed for X-ray diffraction (XRD) refinement analyses to transmission electron microscopy, enabling the first demonstration of sub-picometer accuracy lattice parameter extraction while also obtaining both the size of the coherent crystallite domains and the nanostrain, which is observed to decrease as nanowires transition to tellurene. This new local analysis is commensurate with global powder XRD results, indicating the robustness of both the new synthesis approach and new structural analysis methodology for future scalable production of 2D tellurene and characterization of nanomaterials.

2D materials↗
DOE OSTI2021

Photo-exfoliation of MoS 2 quantum dots from nanosheets: an in-situ transmission electron microscopy study

Fabrication of transition metal dichalcogenide (TMD) quantum dots (QDs) is complex and requires submerging of powders in binary solvents and the constant tuning of wavelength and pulsed frequency of light to achieve a desired reaction. Here,iInstead of liquid state photoexfoliation, we utilize infrared laser irradiation of free-standing MoS 2 flakes in transmission electron microscope (TEM) to achieve solid-state multi-level photoexfoliation of QDs. By investigating the steps involved in photochemical reaction between the surface of MoS 2 and the laser beam, we gain insight into each step of the photoexfoliation mechanism and observe high yield production of QDs, led by an inhomogeneous crystalline size distribution. Additionally, by using a laser with a lower energy than the indirect optical transition of bulk MoS 2 , we conclude that the underlying phenomena behind the photoexfoliation is from multi-photon absorption achieved at high optical outputs from the laser source. These findings provide an environmentally friendly synthesis method to fabricate QDs for potential applications in biomedicine, optoelectronics, and fluorescence sensing.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Thermally driven phase transition of halide perovskites revealed by big data-powered in situ electron microscopy

Halide perovskites are promising light-absorbing materials for high-efficiency solar cells, while the crystalline phase of halide perovskites may influence the device’s efficiency and stability. In this work, we investigated the thermally driven phase transition of perovskite (CsPbIxBr3—x), which was confirmed by electron diffraction and high-resolution transmission electron microscopy results. CsPbIxBr3—x transitioned from δ phase to α phase when heated, and the γ phase was obtained when the sample was cooled down. The γ phase was stable as long as it was isolated from humidity and air. A template matching-based data analysis method enabled visualization of the thermally driven phase evolution of perovskite during heating. Here, we also proposed a possible atomic movement in the process of phase transition based on our in situ heating experimental data. The results presented here may improve our understanding of the thermally driven phase transition of perovskite as well as provide a protocol for big-data analysis of in situ experiments.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2024

Nanosecond Structural Dynamics during Electrical Melting of Charge Density Waves in 1⁢T-TaS 2

Electrical control of charge density waves has been of immense interest, as the strong underlying electron-lattice interactions potentially open new, efficient pathways for manipulating their ordering and, consequently, their electronic properties. However, the transition mechanisms are often unclear as electric field, current, carrier injection, heat, and strain can all contribute and play varying roles across length scales and timescales. Here, we provide insight on how electrical stimulation melts the room temperature charge density wave order in 1T-TaS 2 by visualizing the atomic and mesoscopic structural dynamics from quasistatic to nanosecond pulsed melting. Using a newly developed ultrafast electron microscope setup with electrical stimulation, we reveal the order and strain dynamics during voltage pulses as short as 20 ns. The order parameter dynamics across a range of pulse amplitudes and durations support a thermally driven mechanism even for fields as high as 19 kV cm -1 . In addition, time-resolved imaging reveals a heterogeneous, mesoscopic strain response across the flake, including MHz-scale acoustic resonances that emerge during sufficiently short pulsed excitation which may modulate the order. In conclusion, these results suggest that metallic charge density wave phases like studied here may be more robust to electronic switching pathways than insulating ones, motivating further investigations at higher fields and currents in this and other related systems.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Extending Interfaces in 3D to Achieve Superior Nanoscale Strength in Ti/Nb Nanolaminates

Tuning the atomic-level structure of nanolaminates enables high strength, increased deformability, and the ability to absorb and mitigate damage due to varied crystalline defects, including dislocations. Here, we present the enhanced strength of Ti/Nb nanolaminates containing thick 3D interfaces (3DIs), relative to their chemically abrupt 2D counterparts. We examine the effects of crystallographic alignment and compositional gradients on mechanical behavior via experiments and phase-field-dislocation dynamics (PFDD) modeling. Mechanical testing reveals that nanolaminates containing thicker 3DIs demonstrate a 28% hardness enhancement compared with sharp-interface nanolaminates. PFDD modeling shows that the critical resolved shear stress (CRSS) increases with the 3DI thickness. Gradual compositional transitions in 3DIs were confirmed via scanning transmission electron microscopy and high-resolution transmission electron microscopy, showing sharp crystallographic transitions and a heightened interface topography. The findings establish a positive function between the 3DI thickness and mechanical robustness for hexagonal-closest-packed-containing composites, emphasizing the role of defect–interface interactions in tailoring the mechanical performance and providing a foundation for future interfacial engineering.

36 MATERIALS SCIENCE↗
NASA NTRS1977

Characteristics of first order shock induced magnetic transitions in iron and discrimination from TRM

Reflected light microscopy provides information on first-order shock transitions in iron and iron-nickel and permits discrimination of microstructures due to shock transitions from those imparted by thermal transitions. In addition, thin-foil electron microscopy is used to characterize magnetic transitions in fine-particle iron. First-order magnetic phase changes, such as that from the antiferromagnetic face centered cubic state to the ferromagnetic body centered cubic state, are studied with the aim of calibrating the shock and thermal mechanisms of magnetization in iron with a particle size range between 250 and 1200 A. The efficiency of remanence due to shock transition is also estimated.

Wasilewski, P.↗
DOE OSTI2021

Topological Frustration as a New Parameter to Tune Morphology Revealed through Exploring the Continuum between A-B-C 3-Arm Star and Linear Triblock Polymers

Block polymers assemble into a variety of phase-separated morphologies based on volume fraction (φ) and interactions (χ) of the respective blocks. The arrangement of three different polymer blocks could either be a 3-arm star, with each block having one terminus attached to a common junction point or a linear A-B-C architecture. A versatile strategy is reported to synthesize a series of well-defined graft polymers that lie along the unexplored continuum between a 3-arm star and an A-B-C linear triblock polymer architecture. Using the technique of single-molecule insertion, precise control over the position of graft arm C along the B chain was achieved. A series of discrete graft polymers (PMMA-b-PS-g-PEO) with fixed φ and prescribed ω values that lie on the continuum between a 3-arm star (ω = 0) and linear triblock polymer (ω = 1) were synthesized. Morphological studies using small-angle X-ray scattering and conventional and energy-filtered transmission electron microscopy reveal the transition between lamellae, perforated lamellae, and cylindrical morphologies with systematic variation in the ω values, a trend attributed to the topological frustration and the associated χ values between the three blocks. Molecular dynamic simulations of coarse-grained models were found to predict phase diagrams that are consistent with the experimentally observed morphologies. Furthermore, our results suggest that changes in ω lead to topological frustration which is an important additional new design parameter that can be used to tune the morphology of multiblock polymers in addition to φ and χ.

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

Magnetic state switching in FeGa microstructures

This work demonstrates that magnetoelectric composite heterostructures can be designed at the length scale of 10µms that can be switched from a magnetized state to a vortex state, effectively switching the magnetization off, using electric field induced strain. This was accomplished using thin film magnetoelectric heterostructures of Fe 81.4 Ga 18.6 on a single crystal (011) [Pb(Mg 1/3 Nb 2/3 )O 3 ] 0.68 -[PbTiO 3 ] 0.32 (PMN-32PT) ferroelectric substrate. Here, the heterostructures were tripped from a multi-domain magnetized state to a flux closure vortex state using voltage induced strain in a piezoelectric substrate. FeGa heterostructures were deposited on a Si-substrate for superconducting quantum interference device magnetometry characterization of the magnetic properties. The magnetoelectric coupling of a FeGa continuous film on PMN-32PT was characterized using a magneto optical Kerr effect magnetometer with bi-axial strain gauges, and magnetic multi-domain heterostructures were imaged using x-ray magnetic circular dichroism—photoemission electron microscopy during the transition to the vortex state. The domain structures were modelled using MuMax 3 , a micromagnetics code, and compared with observations. The results provide considerable insight into designing magnetoelectric heterostructures that can be switched from an ‘on’ state to an ‘off’ state using electric field induced strain.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Chirality-induced zigzag domain wall in in-plane magnetized ultrathin films

In this report the domain structure in in-plane magnetized Fe/Ni/W(110) films is investigated using spin-polarized low-energy electron microscopy. A novel transition of the domain wall shape from a zigzaglike pattern to straight is observed as a function of the film thickness, which is triggered by the transition of the domain wall type from the out-of-plane chiral wall to the in-plane Néel wall. The contribution of the Dzyaloshinskii-Moriya interaction to the wall energy is proposed to explain the transition of the domain wall shape, which is supported by Monte Carlo simulations.

36 MATERIALS SCIENCE↗
NASA NTRS1991

Composition dependence of superconductivity in YBa2(Cu(3-x)Al(x))Oy

Eleven different compositions in the system YBa2(Cu(3-x)Al(x))O(y) (x = 0 to 0.3) have been synthesized and characterized by electrical resistivity measurements, powder x-ray diffraction, and scanning electron microscopy. The superconducting transition temperature T sub c (onset) was almost unaffected by the presence of alumina due to its limited solubility in YBa2Cu3O(7-x). However, T sub c(R = 0) gradually decreased, and the resistive tails became longer with increasing Al2O3 concentration. This was probably due to formation of BaAl2O4 and other impurity phases from chemical decomposition of the superconducting phase by reaction with Al2O3.

Bansal, Narottam P.↗
NASA NTRS1993

Composition dependence of superconductivity in YBa2(Cu(3-x)Al(x))O(y)

Eleven different compositions in the system YBa2(Cu(3-x)Al(x))O(y) (x = 0 to 0.3) have been synthesized and characterized by electrical resistivity measurements, powder X-ray diffraction, and scanning electron microscopy. The superconducting transition temperature T sub c (onset) was almost unaffected by the presence of alumina due to its limited solubility in YBa2Cu3O(7-x). However, T sub c(R = 0) gradually decreased, and the resistive tails became longer with increasing Al2O3 concentration. This was probably due to formation of BaAl2O4 and other impurity phases from chemical decomposition of the superconducting phase by reaction with Al2O3.

Bansal, N. P.↗
NASA NTRS1975

Fretting of titanium at temperatures to 650 C in air

Fretting wear experiments were conducted on high-purity titanium at temperatures up to 650 C. Results indicate that up to about 500 C, the fretting wear increases with temperature. A further increase in the temperature up to 650 C results in decreasing fretting wear. This change in trend of fretting wear with temperature is shown to be associated with a change in oxidation rate. Additional experiments at 650 C showed a transmission from a low rate of fretting wear to a higher rate occurred after exposure to a number of fretting cycles; the number of cycles required to cause this transition was dependent on the normal load. Scanning electron microscopy studies revealed that this transition was marked by cracking and disruption of the surface oxide film. A model was proposed that coupled the oxidation rate kinetics of titanium at 650 C with the occurrence of wear at the surface of the oxide film.

Bill, R. C.↗
DOE OSTI2022

Imaging Phase Segregation in Nanoscale Li x CoO 2 Single Particles

Li x CoO 2 (LCO) is a common battery cathode material that has recently emerged as a promising material for other applications including electrocatalysis and as electrochemical random access memory (ECRAM). During charge– discharge cycling LCO exhibits phase transformations that are significantly complicated by electron correlation. While the bulk phase diagram for an ensemble of battery particles has been studied extensively, it remains unclear how these phases scale to nanometer dimensions and the effects of strain and diffusional anisotropy at the single-particle scale. Understanding these effects is critical to modeling battery performance and for predicting the scalability and performance of electrocatalysts and ECRAM. Here we investigate isolated, epitaxial LiCoO 2 islands grown by pulsed laser deposition. After electrochemical cycling of the islands, conductive atomic force microscopy (c-AFM) is used to image the spatial distribution of conductive and insulating phases. Above 20 nm island thicknesses, we observe a kinetically arrested state in which the phase boundary is perpendicular to the Li-planes; we propose a model and present image analysis results that show smaller LCO islands have a higher conductive fraction than larger area islands, and the overall conductive fraction is consistent with the lithiation state. Thinner islands (14 nm), with a larger surface to volume ratio, are found to exhibit a striping pattern, which suggests surface energy can dominate below a critical dimension. When increasing force is applied through the AFM tip to strain the LCO islands, significant shifts in current flow are observed, and underlying mechanisms for this behavior are discussed. The c-AFM images are compared with photoemission electron microscopy images, which are used to acquire statistics across hundreds of particles. Finally, the results indicate that strain and morphology become more critical to electrochemical performance as particles approach nanometer dimensions.

25 ENERGY STORAGE↗
DOE OSTI2021

Morphological Transitions of a Photoswitchable Aramid Amphiphile Nanostructure

Self-assembly of small amphiphilic molecules in water can lead to nanostructures of varying geometries with pristine internal molecular organization. Here we introduce a photoswitchable aramid amphiphile (AA), designed to exhibit extensive hydrogen bonding and robust mechanical properties upon self-assembly, while containing a vinylnitrile group for photoinduced cis-trans isomerization. We demonstrate spontaneous self-assembly of the vinylnitrile-containing AA in water to form nanoribbons. Upon UV irradiation, trans-to-cis isomerizations occur concomitantly with a morphological transition from nanoribbons to nanotubes. The nanotube structure persists in water for over six months, stabilized by strong and collective intermolecular interactions. We demonstrate that the nanoribbon-to-nanotube transition is reversible upon heating and that switching between states can be achieved repeatedly. Finally, we use electron microscopy to capture the transition and propose mechanisms for nanoribbon-to-nanotube rearrangement and vice versa. This stability and switchability of photoresponsive AA nanostructures make them viable for a range of future applications.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2022

Structural transitions in the GTP cap visualized by cryo-electron microscopy of catalytically inactive microtubules

Microtubules (MTs) are nonequilibrium polymers that switch between states of growth and shrinkage. This property is critical for their function and is a consequence of GTP hydrolysis in the MT. The structure of the stable GTP part of the MT (the GTP cap) has previously been inferred from MTs polymerized with nonhydrolyzable GTP analogs. Here, we report high-resolution structures of MTs truly containing GTP, polymerized from mutated, hydrolysis-deficient tubulins. We find that GTP-MTs have an “expanded lattice” and a “closed seam,” structural characteristics possibly responsible for stabilizing the GTP cap. These results provide insight into the structural transitions at growing MT ends, furthering our understanding of the bistable nature of MTs.

59 BASIC BIOLOGICAL SCIENCES↗