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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 145 records · Page 8
All sourcesNASA NTRSDOE OSTI
DOE OSTI2024

Structural Complexities in Sodium Ion Conductive Antiperovskite Revealed by Cryogenic Transmission Electron Microscopy

Here we use low-dose cryogenic transmission electron microscopy (cryo-TEM) to investigate the atomic-scale structure of antiperovskite Na 2 NH 2 BH 4 crystals by preserving the room-temperature cubic phase and carefully monitoring the electron dose. Via quantitative analysis of electron beam damage using selected area electron diffraction, we find cryogenic imaging provides 6-fold improvement in beam stability for this solid electrolyte. Cryo-TEM images obtained from flat crystals revealed the presence of a new, long-range-ordered supercell with a cubic phase. The supercell exhibits doubled unit cell dimensions of 9.4 Å × 9.4 Å as compared to the cubic lattice structure revealed by X-ray crystallography of 4.7 Å × 4.7 Å. The comparison between the experimental image and simulated potential map indicates the origin of the supercell is a vacancy ordering of sodium atoms. This work demonstrates the potential of using cryo-TEM imaging to study the atomic-scale structure of air- and electron-beam-sensitive antiperovskite-type solid electrolytes.

36 MATERIALS SCIENCE↗
NASA NTRS2004

Large-Scale Fabrication of Carbon Nanotube Probe Tips For Atomic Force Microscopy Critical Dimension Imaging Applications

Carbon nanotube (CNT) probe tips for atomic force microscopy (AFM) offer several advantages over Si/Si3N4 probe tips, including improved resolution, shape, and mechanical properties. This viewgraph presentation discusses these advantages, and the drawbacks of existing methods for fabricating CNT probe tips for AFM. The presentation introduces a bottom up wafer scale fabrication method for CNT probe tips which integrates catalyst nanopatterning and nanomaterials synthesis with traditional silicon cantilever microfabrication technology. This method makes mass production of CNT AFM probe tips feasible, and can be applied to the fabrication of other nanodevices with CNT elements.

Ye, Qi Laura↗
DOE OSTI2014

Large-angle illumination STEM: Toward three-dimensional atom-by-atom imaging

To completely understand and control materials and their properties, it is of critical importance to determine their atomic structures in all three dimensions. Recent revolutionary advances in electron optics – the inventions of geometric and chromatic aberration correctors as well as electron source monochromators – have provided fertile ground for performing optical depth sectioning at atomic-scale dimensions. In this study we theoretically demonstrate the imaging of top/sub-surface atomic structures and identify the depth of single dopants, single vacancies and the other point defects within materials by large-angle illumination scanning transmission electron microscopy (LAI-STEM). The proposed method also allows us to measure specimen properties such as thickness or three-dimensional surface morphology using observations from a single crystallographic orientation.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Understanding and quantifying electron beam effects during in situ TEM nanomechanical tensile testing on metal thin films

Transmission electron microscopy (TEM) imaging relies on high energy electrons for atomic scale resolution, however, the electrons themselves interact with and may alter the material being imaged. Using an in situ TEM MEMS-based nanomechanical testing technique, the effect of the electron beam (e-beam) on the deformation behavior of nanocrystalline Al and ultrafine-grained Au is investigated and quantified. We show that the e-beam enhances plastic deformation, leading to an increase in plastic strain rate and a decrease in true activation volume V* in Al (28 to 21b 3 , with b being the Burgers vector length). The e-beam has a much weaker effect on Au. The e-beam effect is not caused by knock-on damage, but rather an effective temperature increase due to additional atomic fluctuations provided by the e-beam. The effective temperature increase is larger for Al than Au. This e-beam effect does not change the deformation mechanisms, but instead accelerates the stress-driven, thermally activated plastic deformation. These experiments provide insight into the effects of the e-beam on plastic deformation in different metals and underscore the importance of understanding and quantifying these effects for proper interpretation of measured mechanical properties during in situ TEM experiments.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Band Gap Engineering and Layer-by-Layer Band Gap Mapping of Selenium-doped Molybdenum Disulfide

Ternary two-dimensional dichalcogenide alloys exhibit compositionally modulated electronic structure and hence, control of dopant concentration within each layer of these layered compounds provides a powerful way to modify their properties. The challenge then becomes quantifying and locating the dopant atoms within each layer in order to better understand and fine-tune the desired properties. Here we report the synthesis of selenium substitutionally doped molybdenum disulfide atomic layers, with a broad range of selenium concentrations, resulting in band gap modulations of over 0.2 eV. Atomic scale chemical analysis using Z-contrast imaging provides direct maps of the dopant atom distribution in individual MoS2 layers and hence a measure of the local band gaps. Furthermore, in a bilayer structure, the dopant distribution of each layer is imaged independently. We demonstrate that each layer in the bilayer contains similar doping levels, randomly distributed, providing new insights into the growth mechanism and alloying behavior in two-dimensional dichalcogenide atomic layers. The results show that growth of uniform, ternary, two-dimensional dichalcogenide alloy films with tunable electronic properties is feasible.

Gong, Yongji↗
DOE OSTI2012

Atomically localized plasmon enhancement in monolayer graphene

Plasmons in graphene can be tuned by using electrostatic gating or chemical doping, and the ability to confine plasmons in very small regions could have applications in optoelectronics, plasmonics and transformation optics. However, little is known about how atomic-scale defects influence the plasmonic properties of graphene. Moreover, the smallest localized plasmon resonance observed in any material to date has been limited to around 10 nm. Here, we show that surface plasmon resonances in graphene can be enhanced locally at the atomic scale. Using electron energy-loss spectrum imaging in an aberration-corrected scanning transmission electron microscope, we find that a single point defect can act as an atomic antenna in the petahertz (10{sup 15} Hz) frequency range, leading to surface plasmon resonances at the subnanometer scale.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Relationship between molecular structure and corrugations in self-assembled polypeptoid nanosheets revealed by cryogenic electron microscopy

Designing conformationally dynamic molecules that self-assemble into predictable nanostructures remains an important unmet challenge. This paper describes how atomic-scale cryogenic transmission electron microscopy (cryo-TEM) can be used to explore the relationship between molecular structure and self-assembly of block copolymers. We examined sheetlike micelles formed in water using a series of diblock copolypeptoids with the same hydrophilic block and three distinct crystalline hydrophobic blocks. Our cryo-TEM images revealed all the structures share nansoscale features, but differ in their intermolecular packing geometries. Different molecular arrangements, parallel and antiparallel V-shaped crystal motifs, were revealed by two-dimensional atomic-scale through-plane images. However, images from tilted samples revealed an unexpected feature when the hydrophobic polypeptoid block comprised phenyl rings with substituted bromine atoms at the para position. The nanosheets contained atomic-scale corrugations that were absent in the other systems which comprised unsubstituted aliphatic and aromatic side chains. We hypothesize that these corrugations are due to the dipolar characteristics of the brominated phenyl group and interactions between this group and water molecules. Published by the American Physical Society 2024

36 MATERIALS SCIENCE↗
DOE OSTI2017

The Role of Gas in Determining Image Quality and Resolution During In Situ Scanning Transmission Electron Microscopy Experiments

As gas-solid heterogeneous catalytic reactions are molecular in nature, a full mechanistic understanding of the process requires atomic scale characterization under realistic operating conditions. While atomic resolution imaging has become a routine in modern high-vacuum (scanning) transmission electron microscopy ((S)TEM), both image quality and resolution nominally degrade when reaction gases are introduced. In this work, we systematically assess the effects of different gases at various pressures on the quality and resolution of images obtained at room temperature in the annular dark field STEM imaging mode using a differentially pumped (DP) gas cell. This imaging mode is largely free from inelastic scattering effects induced by the presence of gases and retains good imaging properties over a wide range of gas mass/pressures. We demonstrate the application of the ESTEM with atomic resolution images of a complex oxide alkane oxidation catalyst MoVNbTeOx (M1) immersed in light and heavy gas environments.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2018

Building Structures Atom by Atom via Electron Beam Manipulation

Building materials from the atom up is the pinnacle of materials fabrication. Until recently the only platform that offered single-atom manipulation was scanning tunneling microscopy. Here controlled manipulation and assembly of a few atom structures are demonstrated by bringing together single atoms using a scanning transmission electron microscope. An atomically focused electron beam is used to introduce Si substitutional defects and defect clusters in graphene with spatial control of a few nanometers and enable controlled motion of Si atoms. The Si substitutional defects are then further manipulated to form dimers, trimers, and more complex structures. The dynamics of a beam-induced atomic-scale chemical process is captured in a time-series of images at atomic resolution. In conclusion, these studies suggest that control of the e-beam-induced local processes offers the next step toward atom-by-atom nanofabrication, providing an enabling tool for the study of atomic-scale chemistry in 2D materials and fabrication of predefined structures and defects with atomic specificity.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Atomic Scale Studies of La/Sr Ordering in Colossal Magnetoresistant La 2-2x Sr 1+2x Mn 2 O 7 Single Crystals

To date, it is unclear whether chemical order (or disorder) is in any way connected to double exchange, electronic phase separation, or charge ordering (CO) in manganites. In this work, we carry out an atomic resolution study of the colossal magnetoresistant manganite La 2-2x Sr 1+2x Mn 2 O 7 (LSMO). We combine aberration-corrected electron microscopy and spectroscopy with spectroscopic image simulations, to analyze cation ordering at the atomic scale in real space in a number of LSMO single crystals. We compare three different compositions within the phase diagram: a ferromagnetic metallic material (x=0.36), an insulating, antiferromagnetic charge ordered (AF-CO) compound (x=0.5), which also exhibits orbital ordering, and an additional AF sample (x=0.56). Detailed image simulations are essential to accurately quantify the degree of chemical ordering of these samples. We find a significant degree of long-range chemical ordering in all cases, which increases in the AF-CO range. However, the degree of ordering is never complete nor can it explain the strongly correlated underlying ordering phenomena. Our results show that chemical ordering over distinct crystallographic sites is not needed for electronic ordering phenomena to appear in manganites, and cannot by itself explain the complex electronic behavior of LSMO.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Nanoscopic structure of borosilicate glass with additives for nuclear waste vitrification

In this report we investigated the nanoscopic structure of borosilicate glasses as a host for high-level radioactive liquid waste (HLLW) in the presence of the additives Na 2 O and CaO/ZnO with and without Li 2 O. These additives have been used to lower the glass melting point, suppress the macroscopic phase separation, and increase the chemical durability of glasses. Small-angle neutron scattering was used to elucidate the effect of the additives on the nanoscopic structure along with macro- and atomic-scale observations obtained using neutron imaging and X-ray diffraction, respectively. The borosilicate glass made without Na 2 O formed a microphase-separated structure of SiO 2 - and B 2 O 3 -rich domains approximately 100 nm in size, and the material was homogeneous at length scales up to millimeters. With the addition of increasing amounts of Na 2 O, the domain spacing decreased. Introducing CaO/ZnO additives induced inhomogeneities in the glass, such as void structures several nanometers in size, although the inhomogeneity was suppressed by the coaddition of Li 2 O. These results provide insights into the performance of host glasses for HLLW vitrification. Incorporating HLLW into glasses is likely to cause changes in the nanoscopic structure of host glasses similar to those revealed here.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2018

Electron-Beam-Induced Synthesis of Hexagonal 1 H -MoSe 2 from Square β-FeSe Decorated with Mo Adatoms

Two-dimensional (2D) materials have generated interest in the scientific community because of the advanced electronic applications they might offer. Powerful electron beam microscopes have been used not only to evaluate the structures of these materials but also to manipulate them by forming vacancies, nanofragments, and nanowires or joining nanoislands together. In this work, we show that the electron beam in a scanning transmission electron microscope (STEM) can be used in yet another way: to mediate the synthesis of 2D 1H-MoSe 2 from Mo-decorated 2D β-FeSe and simultaneously image the process on the atomic scale. This is quite remarkable given the different crystal structures of the reactant (square lattice β-FeSe) and the product (hexagonal lattice 1H-MoSe 2 ). Herein, the feasibility of the transformation was first explored by theoretical calculations that predicted that the reaction is exothermic. Furthermore, a theoretical reaction path to forming a stable 1H-MoSe 2 nucleation kernel within pure β-FeSe was found, demonstrating that the pertinent energy barriers are smaller than the energy supplied by the STEM electron beam.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2017

Learning through ferroelectric domain dynamics in solid-state synapses

In the brain, learning is achieved through the ability of synapses to reconfigure the strength by which they connect neurons (synaptic plasticity). In promising solid-state synapses called memristors, conductance can be finely tuned by voltage pulses and set to evolve according to a biological learning rule called spike-timing-dependent plasticity (STDP). Future neuromorphic architectures will comprise billions of such nanosynapses, which require a clear understanding of the physical mechanisms responsible for plasticity. Here we report on synapses based on ferroelectric tunnel junctions and show that STDP can be harnessed from inhomogeneous polarization switching. Through combined scanning probe imaging, electrical transport and atomic-scale molecular dynamics, we demonstrate that conductance variations can be modelled by the nucleation-dominated reversal of domains. Finally, based on this physical model, our simulations show that arrays of ferroelectric nanosynapses can autonomously learn to recognize patterns in a predictable way, opening the path towards unsupervised learning in spiking neural networks.

60 APPLIED LIFE SCIENCES↗
DOE OSTI2015

Direct observation of interlocked domain walls and topological four-state vortex-like domain patterns in multiferroic YMnO{sub 3} single crystal

Using the advanced spherical aberration-corrected high angle annular dark field scanning transmission electron microscope imaging techniques, we investigated atomic-scale structural features of domain walls and domain patterns in YMnO{sub 3} single crystal. Three different types of interlocked ferroelectric-antiphase domain walls and two abnormal topological four-state vortex-like domain patterns are identified. Each ferroelectric domain wall is accompanied by a translation vector, i.e., 1/6[210] or −1/6[210], demonstrating its interlocked nature. Different from the four-state vortex domain patterns caused by a partial edge dislocation, two four-state vortex-like domain configurations have been obtained at atomic level. These observed phenomena can further extend our understanding of the fascinating vortex domain patterns in multiferroic hexagonal rare-earth manganites.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2018

Defect-Induced Hedgehog Polarization States in Multiferroics

Continuous developments in nanotechnology require new approaches to materials synthesis that can produce novel functional structures. Here, we show that nanoscale defects, such as nonstoichiometric nanoregions (NSNRs), can act as nano-building blocks for creating complex electrical polarization structures in the prototypical multiferroic BiFeO 3 . An array of charged NSNRs are produced in BiFeO 3 thin films by tuning the substrate temperature during film growth. Atomic-scale scanning transmission electron microscopy imaging reveals exotic polarization rotation patterns around these NSNRs. These polarization patterns resemble hedgehog or vortex topologies and can cause local changes in lattice symmetries leading to mixed-phase structures resembling the morphotropic phase boundary with high piezoelectricity. Phase-field simulations indicate that the observed polarization configurations are mainly induced by charged states at the NSNRs. Engineering defects thus may provide a new route for developing ferroelectric-or multiferroic-based nanodevices.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2017

Bellerophon Environment for Analysis of Materials (BEAM)

Improvements in scientific instrumentation allow imaging at mesoscopic to atomic length scales, many spectroscopic modes, and now--with the rise of multimodal acquisition systems and the associated processing capability--the era of multidimensional, informationally dense data sets has arrived. Technical issues in these combinatorial scientific fields are exacerbated by computational challenges best summarized as a necessity for drastic improvement in the capability to transfer, store, and analyze large volumes of data. The Bellerophon Environment for Analysis of Materials (BEAM) platform provides material scientists the capability to directly leverage the integrated computational and analytical power of High Performance Computing (HPC) to perform scalable data analysis and simulation and manage uploaded data files via an intuitive, cross-platform client user interface. This framework delivers authenticated, "push-button" execution of complex user workflows that deploy data analysis algorithms and computational simulations utilizing compute-and-data cloud infrastructures and HPC environments like Titan at the Oak Ridge Leadershp Computing Facility (OLCF).

Lingerfelt, Eric J↗