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At least 667 records · Page 37
All sourcesNASA NTRSDOE OSTI
DOE OSTI2019

Supramolecular Nanosheets Assembled from Poly(ethylene glycol)- b -poly( N -(2-phenylethyl)glycine) Diblock Copolymer Containing Crystallizable Hydrophobic Polypeptoid: Crystallization Driven Assembly Transition from Filaments to Nanosheets

Supramolecular two-dimensional (2D) nanomaterials from block copolymers have received great interest for their unique structure and properties. In this work, we report the formation of ultrathin nanosheets from self-assembly of amphiphilic poly(ethylene glycol)- b -poly( N -(2-phenylethyl)glycine) (PEG- b -PNPE) diblock copolymers, which contain rigid crystallizable polypeptoid segment. The PEG- b -PNPE copolymers were synthesized via ring opening polymerization (ROP). The obtained PEG- b -PNPE diblock copolymers can spontaneously form highly ordered structures in PEG selective solvents such as water and methanol. The copolymers with short PNPE segment can directly form nanosheets in water, and the obtained 2D nanosheets have a uniform thickness of 4-5 nm. In contrast, the copolymers with relatively long PNPE segment can only assemble into nanosheets with the assistance of methanol. It is anticpated that the crystallization and π-π stacking of PNPE blocks play critical roles in the formation of the nanosheet as suggested by grazing incidence wide-angle X-ray scattering (GIWAXS). During the process of adding water into copolymer methanol solution, the nanosheets were observed to evolve from individual nanofibers, to parallel aligning nanofibers, and eventually to the nanosheet structures verified by transmission electron microscopy (TEM) and cryo-TEM characterizations. We demonstrated that the preassembled filament behave as a fundamental packing motif to align laterally and further fuse into platelet-like structures. The assembly structure evolution process was tracked by TEM, atomic force microscopy, and cryo-TEM techniques. The understandings of supramolecular 2D nanosheet formation offer a new opportunity to make hierarchical nanostructures from polypeptoids containing copolymers.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Shape Dependence of Pressure-Induced Phase Transition in CdS Semiconductor Nanocrystals

Understanding structural stability and phase transformation of nanoparticles under high pressure is of great scientific interest, as it is one of the crucial factors for design, synthesis, and application of materials. Even though high-pressure research on nanomaterials has been widely conducted, their shape-dependent phase transition behavior still remains unclear. Examples of phase transitions of CdS nanoparticles are very limited, despite the fact that it is one of the most studied wide band gap semiconductors. Here we have employed in-situ synchrotron wide-angle X-ray scattering (WAXS) and transmission electron microscopy (TEM) to investigate the high-pressure behaviors of CdS nanoparticles as a function of particle shapes. We observed that CdS nanoparticles transform from wurtzite to rocksalt phase at elevated pressure in comparison to their bulk counterpart. Phase transitions also vary with particle shape—rod-shaped particles show a partially reversible phase transition and the onset of the structural phase transition pressure decreases with decreasing surface-to-volume ratios, while spherical particles undergo irreversible phase transition with relatively low phase transition pressure. Additionally, TEM images of spherical particles exhibited sintering-induced morphology change after high-pressure compression. Calculations of the bulk modulus reveals that spheres are more compressible than rods in the wurtzite phase. These results indicate that the shape of the particle plays an important role in determining their high-pressure properties. Our study provides important insights into understanding of the phase-structure-property relationship, guiding future design and synthesis of nanoparticles for promising applications.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Insights into the Structure and Dynamics of Metal–Organic Frameworks via Transmission Electron Microscopy

Metal–organic frameworks (MOFs) are hybrid materials composed of metal ions and organic linkers featuring high porosity, crystallinity, and chemical tunability at multiple length scales. Here, a recent advancement in transmission electron microscopy (TEM) and its direct application to MOF structure–property relationships have changed how we consider rational MOF design and development. Herein, we provide a perspective on TEM studies of MOFs and highlight the utilization of state-of-the-art TEM technologies to explore dynamic MOF processes and host–guest interactions. Additionally, we provide thoughts on what the future holds for TEM in the study of MOFs.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2021

Elucidating the Role of Halides and Iron during Radiolysis-Driven Oxidative Etching of Gold Nanocrystals Using Liquid Cell Transmission Electron Microscopy and Pulse Radiolysis

Graphene liquid cell transmission electron microscopy (TEM) has enabled the observation of a variety of nanoscale transformations. Yet understanding the chemistry of the liquid cell solution and its impact on the observed transformations remains an important step toward translating insights from liquid cell TEM to benchtop chemistry. Gold nanocrystal etching can be used as a model system to probe the reactivity of the solution. FeCl 3 has been widely used to promote gold oxidation in bulk and liquid cell TEM studies, but the roles of the halide and iron species have not been fully elucidated. In this work, we observed the etching trajectories of gold nanocrystals in different iron halide solutions. We observed an increase in gold nanocrystal etch rate going from Cl - - to Br - - to I - -containing solutions. Furthermore, this is consistent with a mechanism in which the dominant role of halides is as complexation agents for oxidized gold species. Additionally, the mechanism through which FeCl 3 induces etching in liquid cell TEM remains unclear. Ground-state bleaching of the Fe(III) absorption band observed through pulse radiolysis indicates that iron may react with Cl 2 · - radicals to form an oxidized transient species under irradiation. Complete active space self-consistent field (CASSCF) calculations indicate that the FeCl 3 complex is oxidized to an Fe species with an OH radical ligand. Together our data indicate that an oxidized Fe species may be the active oxidant, while halides modulate the etch rate by tuning the reduction potential of gold nanocrystals.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2014

Correlative Electron and Fluorescence Microscopy of Magnetotactic Bacteria in Liquid: Toward In Vivo Imaging

Magnetotactic bacteria biomineralize ordered chains of uniform, membrane-bound magnetite or greigite nanocrystals that exhibit nearly perfect crystal structures and species-specific morphologies. Transmission electron microscopy (TEM) is a critical technique for providing information regarding the organization of cellular and magnetite structures in these microorganisms. However, conventional TEM can only be used to image air-dried or vitrified bacteria removed from their natural environment. Here we present a correlative scanning TEM (STEM) and fluorescence microscopy technique for imaging viable cells of Magnetospirillum magneticum strain AMB-1 in liquid using an in situ fluid cell TEM holder. Fluorescently labeled cells were immobilized on microchip window surfaces and visualized in a fluid cell with STEM, followed by correlative fluorescence imaging to verify their membrane integrity. Notably, the post-STEM fluorescence imaging indicated that the bacterial cell wall membrane did not sustain radiation damage during STEM imaging at low electron dose conditions. We investigated the effects of radiation damage and sample preparation on the bacteria viability and found that approximately 50% of the bacterial membranes remained intact after an hour in the fluid cell, decreasing to ~30% after two hours. These results represent a first step toward in vivo studies of magnetite biomineralization in magnetotactic bacteria.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
DOE OSTI2025

Charges on a suspended silicon nitride membrane under a high-energy electron beam

Thin silicon nitride (SiN x ) membranes are widely used in gas and liquid phase transmission electron microscopy (TEM) and as phase plates to enhance imaging contrast. SiN x contains trap sites for both positive and negative charges, which can be manipulated by high-energy electron irradiation, external potential biasing, or light exposure. Charge accumulation on the membrane can significantly affect in situ TEM processes, including chemical and electrochemical reactions, nanoparticle dynamics, and catalytic activity, or introduce unwanted phase shifts when used as a phase plate. Here, in this study, charge accumulation on suspended SiN x membranes was investigated using off-axis electron holography combined with model-free charge analysis, supported by custom finite element analysis (FEA) simulations. An average residual positive charge density of approximately 2.8 × 10 −4 C m −2 was measured. Localized and stable regions of both positive and negative charges were identified on the membrane. The global positive and localized positive/negative charges give rise to strong electric fields and electroosmotic slip velocities at the membrane surface, which are sufficient to induce non-Brownian particle behavior and directional fluid flow, offering a physical explanation for previously observed anomalies in particle dynamics, nucleation, and growth during gas and liquid phase TEM experiments. These results provide a benchmark for understanding charge behavior at SiNx interfaces in gas and liquid phase TEM. Furthermore, the FEA simulations establish a framework for future investigations into charge distribution, electrostatic potentials, and electrical double layers at solid–liquid interfaces, particularly in complex geometries and chemically dynamic environments.

Suspended silicon↗
DOE OSTI2014

Microstructure of multistage annealed nanocrystalline SmCo 2 Fe 2 B alloy with enhanced magnetic properties

The microstructure and chemistry of SmCo 2 Fe 2 B melt-spun alloy after multistage annealing was investigated using high resolution transmission electron microscopy (HRTEM) and 3D atom probe tomography. The multistage annealing resulted in an increase in both the coercivity and magnetization. The presence of Sm(Co,Fe) 4 B (1:4:1) and Sm 2 (Co,Fe) 17 B x (2:17:x) magnetic phases were confirmed using both techniques. Fe 2 B at a scale of -5 nm was found by HRTEM precipitating within the 1:4:1 phase after the second-stage annealing. Ordering within the 2:17:x phase was directly identified both by the presence of antiphase boundaries observed by TEM and the interconnected isocomposition surface network found in 3D atom probe results in addition to radial distribution function analysis. The variations in the local chemistry after the secondary annealing were considered pivotal in improving the magnetic properties.

Environmental Molecular Sciences Laboratory↗
DOE OSTI2014

Small-displacement measurements using high-order Hermite-Gauss modes

We present a scheme for small-displacement measurements using high-order Hermite-Gauss modes and balanced homodyne detection. We demonstrate its use with experimental results of displacement measurements using fundamental transverse mode TEM{sub 00} and first order transverse mode TEM{sub 10} as signal modes. The results show a factor of 1.41 improvement in measurement precision with the TEM{sub 10} mode compared with that with the TEM{sub 00} mode. This scheme has potential applications in precision metrology, atomic force microscopy, and optical imaging.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
DOE OSTI2014

Role of the interface on radiation damage in the SrTiO{sub 3}/LaAlO{sub 3} heterostructure under Ne{sup 2+} ion irradiation

We systematically investigated the microstructural evolution of heteroepitaxial SrTiO{sub 3} (STO) thin films grown on a single crystal LaAlO{sub 3} (LAO) (001) substrate, focusing on the response of the STO/LAO interface to Ne{sup 2+} irradiation at room temperature. Cross sectional transmission electron microscope (TEM) analysis reveals that the LAO crystal amorphizes first after a relatively low dose of damage followed by the amorphization of the STO film after irradiation to a higher dose. While the critical dose to amorphize differs between each material, amorphization begins at the interface and proceeds outward in both cases. Thus, a crystalline/amorphous interface first forms at the STO/LAO interface by a dose of 1 dpa, and then an amorphous/amorphous interface forms when the dose reaches 3 dpa. Scanning TEM and x-ray energy dispersive spectroscopy indicate no significant heavy cation elemental diffusion, though electron energy loss spectroscopy reveals a redistribution of oxygen across the film/substrate interface after Ne{sup 2+} irradiation. Atomistic calculations are used to interpret the experimental findings in terms of the defect properties in each of the two component phases.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2014

Thermoelectric magnetic flows in melt during directional solidification

Thermoelectric magnetic (TEM) flows in melts, which are generated by TEM forces in liquids, were uncovered by the shape evolution of the planar solid/liquid interface during directional solidification. The solid/liquid interface developing from an initially tilted shape to a nearly flat one has been in situ and real-time observed by means of synchrotron X-ray radiography. The corresponding numerical 3D simulations and velocity measurements of flows in the melt confirm that TEM flows exist and respond to this interface shape change. This observation provides visible evidence for TEM flows in melt and their influence on the solid/liquid interface dynamics when directional solidification is conducted in a magnetic field.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2014

Regulation of electron temperature gradient turbulence by zonal flows driven by trapped electron modes

Turbulent transport caused by electron temperature gradient (ETG) modes was investigated by means of gyrokinetic simulations. It was found that the ETG turbulence can be regulated by meso-scale zonal flows driven by trapped electron modes (TEMs), which are excited with much smaller growth rates than those of ETG modes. The zonal flows of which radial wavelengths are in between the ion and the electron banana widths are not shielded by trapped ions nor electrons, and hence they are effectively driven by the TEMs. It was also shown that an E × B shearing rate of the TEM-driven zonal flows is larger than or comparable to the growth rates of long-wavelength ETG modes and TEMs, which make a main contribution to the turbulent transport before excitation of the zonal flows.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗
DOE OSTI2014

Phase transition from fcc to bcc structure of the Cu-clusters during nanocrystallization of Fe{sub 85.2}Si{sub 1}B{sub 9}P{sub 4}Cu{sub 0.8} soft magnetic alloy

A role of Cu on the nanocrystallization of an Fe{sub 85.2}Si{sub 1}B{sub 9}P{sub 4}Cu{sub 0.8} alloy was investigated by X-ray absorption fine structure (XAFS) and transmission electron microscopy (TEM). The Cu K-edge XAFS results show that local structure around Cu is disordered for the as-quenched sample whereas it changes to fcc-like structure at 613 K. The fcc Cu-clusters are, however, thermodynamically unstable and begin to transform into bcc structure at 638 K. An explicit bcc structure is observed for the sample annealed at 693 K for 600 s in which TEM observation shows that precipitated bcc-Fe crystallites with ∼12 nm are homogeneously distributed. The bcc structure of the Cu-clusters transforms into the fcc-type again at 973 K, which can be explained by the TEM observations; Cu segregates at grain boundaries between bcc-Fe crystallites and Fe{sub 3}(B,P) compounds. Combining the XAFS results with the TEM observations, the structure transition of the Cu-clusters from fcc to bcc is highly correlated with the preliminary precipitation of the bcc-Fe which takes place prior to the onset of the first crystallization temperature, T{sub x1} = 707 K. Thermodynamic analysis suggests that an interfacial energy density γ between an fcc-Cu cluster and bcc-Fe matrix dominates at a certain case over the structural energy between fcc and bcc Cu, ΔG{sub fcc} {sub −} {sub bcc}, which causes phase transition of the Cu clusters from fcc to bcc structure.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Observation of atomic ordering of triple-period-A and -B type in GaAsBi

We report the observation of atomic ordering of triple-period (TP)-A and -B type in low temperature (LT) grown GaAsBi alloy using transmission electron microscopy (TEM). In addition to previous reports, where only TP-A ordering was identified in III-V alloys, here, we confirm by electron diffraction, high-resolution (HR) TEM, and HR Z-contrast scanning TEM that two ordering variants coexists for LT-GaAsBi. We find that the TP-A ordering variant dominates over the TP-B variant. TP-A domains extend over 50–100 nm (projected lateral width) and are of higher perfection compared to TP-B domains. HR Z-contrast scanning TEM on different domains reveals a variation in the Bi occupancy in the (111) planes with triple period sequence. Since the formation of ordered phases has been directly linked to the occurrence of specific surface reconstructions, our results suggest a correlation between the TP-A and B type domains and the multiple stability of n × 3 and 3 × n reconstructions on the (001) surface of GaAsBi under low temperature growth.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2014

Electric field enhancement in a self-assembled 2D array of silver nanospheres

We investigate the plasmonic properties of a self-assembled 2D array of Ag nanospheres (average particle diameter/inter-particle separation distance of 9/3.7 nm). The structures of the individual particles and their assemblies are characterized using high-resolution transmission electron microscopy (HR-TEM). The plasmonic response of the nanoparticle network is probed using two-photon photoemission electron microscopy (TP-PEEM). HR-TEM and TP-PEEM statistics reveal the structure and plasmonic response of the network to be homogeneous on average. This translates into a relatively uniform surface-enhanced Raman scattering (SERS) response from biphenyl,4-4{sup ′}-dithiol (BPDT) molecules adsorbed onto different sites of the network. Reproducible, bright, and low-background SERS spectra are recorded and assigned on the basis of density functional theory calculations in which BPDT is chemisorbed onto the vertex of a finite tetrahedral Ag cluster consisting of 20 Ag atoms. A notable agreement between experiment and theory allows us to rigorously account for the observable vibrational states of BPDT in the ∼200–2200 cm{sup −1} region of the spectrum. Finite difference time domain simulations further reveal that physical enhancement factors on the order of 10{sup 6} are attainable at the nanogaps formed between the silver nanospheres in the 2D array. Combined with modest chemical enhancement factors, this study paves the way for reproducible single molecule signals from an easily self-assembled SERS substrate.

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

Correlative transmission electron microscopy and electrical properties study of switchable phase-change random access memory line cells

Phase-change memory line cells, where the active material has a thickness of 15 nm, were prepared for transmission electron microscopy (TEM) observation such that they still could be switched and characterized electrically after the preparation. The result of these observations in comparison with detailed electrical characterization showed (i) normal behavior for relatively long amorphous marks, resulting in a hyperbolic dependence between SET resistance and SET current, indicating a switching mechanism based on initially long and thin nanoscale crystalline filaments which thicken gradually, and (ii) anomalous behavior, which holds for relatively short amorphous marks, where initially directly a massive crystalline filament is formed that consumes most of the width of the amorphous mark only leaving minor residual amorphous regions at its edges. The present results demonstrate that even in (purposely) thick TEM samples, the TEM sample preparation hampers the probability to observe normal behavior and it can be debated whether it is possible to produce electrically switchable TEM specimen in which the memory cells behave the same as in their original bulk embedded state.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2016

Resolution enhancement in transmission electron microscopy with 60-kV monochromated electron source

Transmission electron microscopy (TEM) at low accelerating voltages is useful to obtain images with low irradiation damage. For a low accelerating voltage, linear information transfer, which determines the resolution for observation of single-layered materials, is largely limited by defocus spread, which improves when a narrow energy spread is used in the electron source. In this study, we have evaluated the resolution of images obtained at 60 kV by TEM performed with a monochromated electron source. The defocus spread has been evaluated by comparing diffractogram tableaux from TEM images obtained under nonmonochromated and monochromated illumination. The information limits for different energy spreads were precisely measured by using diffractograms with a large beam tilt. The result shows that the information limit reaches 0.1 nm with an energy width of 0.10 eV. With this monochromated source and a higher-order aberration corrector, we have obtained images of single carbon atoms in a graphene sheet by TEM at 60 kV.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
DOE OSTI2016

Crossover from disordered to core-shell structures of nano-oxide Y 2 O 3 dispersed particles in Fe

Here, molecular dynamic simulations of Y 2 O 3 in bcc Fe and transmission electron microscopy (TEM) observations were used to understand the structure of Y 2 O 3 nano-clusters in an oxide dispersion strengthened steel matrix. The study showed that Y 2 O 3 nano-clusters below 2 nm were completely disordered. Y 2 O 3 nano-clusters above 2 nm, however, form a core-shell structure, with a shell thickness of 0.5–0.7 nm that is independent of nano-cluster size. Y 2 O 3 nano-clusters were surrounded by off-lattice Fe atoms, further increasing the stability of these nano-clusters. TEM was used to corroborate our simulation results and showed a crossover from a disordered nano-cluster to a core-shell structure.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Deformation of Néel-type skyrmions revealed by Lorentz transmission electron microscopy

Néel-type magnetic skyrmions in multilayers are promising candidates for ultra-low power spintronic devices. To image the Néel-type skyrmions using Lorentz transmission electron microscopy (L-TEM), the samples must be tilted. Thus, the external magnetic field consists of both in-plane and out-of-plane components. To date, it is still not well known on the effect of the in-plane magnetic field on the L-TEM images, leading to ambiguities in retrieving the structure of Néel-type skyrmions. Here, Néel-type skyrmions in three [Pt/Co/Ta]$_{20}$ multilayer samples, with the easy magnetization axis being tuned from the out-of-plane to the in-plane direction by increasing the Co thickness from 1.8 to 2.2 nm, are imaged. When using a smaller defocus value (-2 mm) and a higher magnification (×9100) of L-TEM, a surprising dark-bright-dark-bright double contrasted pattern, instead of the previously reported dark-bright contrasted pattern, is observed. The additional dark-bright contrasted pattern becomes more evident for thicker Co layer samples in which the magnetization axis tilts more toward the in-plane direction. Further analysis, via a combination of magnetic force microscopy experiments, micromagnetic simulations, and micromagnetic analysis to Lorentz TEM simulation, shows that the additional dark-bright features originate from the deformation of the Néel-type skyrmions within an in-plane magnetic field.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗