Search NASA⌕ Search

SEARCH · Search NASA

Results for “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.

Quote a phrase for an exact phrase match. Source license links do not imply unrestricted reuse.

At least 1,675 records · Page 93
All sourcesNASA NTRSDOE OSTI
DOE OSTI2014

The influence of C s /C c correction in analytical imaging and spectroscopy in scanning and transmission electron microscopy

Aberration correction in scanning/transmission electron microscopy (S/TEM) owes much to the efforts of a small dedicated group of innovators. Leading that frontier has been Prof. Harald Rose. To date his leadership and dynamic personality has spearheaded our ability to leave behind many of the limitations imposed by spherical aberration (C s ) in high resolution phase contrast imaging. Following shortly behind, has been the development of chromatic aberration correction (C c ) which augments those accomplishments. In this study we will review and summarize how the combination of C s /C c technology enhances our ability to conduct hyperspectral imaging and spectroscopy in today's and future computationally mediated experiments in both thin as well as realistic specimens in vacuo and during in-situ/environmental experiments.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
DOE OSTI2016

Current status and future directions for in situ transmission electron microscopy

This review article discusses the current and future possibilities for the application of in situ transmission electron microscopy to reveal synthesis pathways and functional mechanisms in complex and nanoscale materials. The findings of a group of scientists, representing academia, government labs and private sector entities (predominantly commercial vendors) during a workshop, held at the Center for Nanoscale Science and Technology-National Institute of Science and Technology (CNST-NIST), are discussed. We provide a comprehensive review of the scientific needs and future instrument and technique developments required to meet them.

Taheri, Mitra L.↗
DOE OSTI2017

A short story of imaging and spectroscopy of two-dimensional materials by scanning transmission electron microscopy

Here we present a short historical account of when single adatom impurities where first identified in two-dimensional materials by scanning transmission electron microscopy (STEM). We also present a study of the graphene low-loss (below 50 eV) response as a function of number of layers using electron energy-loss spectroscopy (EELS). The study shows that as few as three layers of graphene behave as bulk graphite for losses above 10 eV We also show examples of how point and extended defects can easily be resolved and structural dynamics can be readily capture by using aberration-corrected STEM imaging. Lastly, we show that the new generation of monochromators has opened up possibilities to explore new physics with an electron microscope. All these capabilities were enabled by the development of spherical aberration correctors and monochromators, where Ondrej Krivanek has played a key role.

2D materials↗
DOE OSTI2020

Variable voltage electron microscopy: Toward atom-by-atom fabrication in 2D materials

The precisely focused electron beam (e-beam) in scanning transmission electron microscopy has been found to be a versatile tool for patterning matter on the atomic level and enabling atom-by-atom fabrication, however, beam-induced phenomena are known to be extremely sensitive to the e-beam energy and are closely correlated with the proximity of the knock-on threshold. Here we provide a method to control the energy transferred to the sample while facilitating much faster changes in accelerating voltages by maintaining a nearly constant temperature in the electron microscope lenses. We use this method to demonstrate in-situ nano-milling of a graphene film followed rapidly by “gentler” imaging at lower energy. Additionally, the insertion and controlled movement of silicon dopants in graphene is demonstrated by employing a different e-beam energy during each process. We believe the incorporation of variable e-beam energy will broaden the potential for atomic scale e-beam fabrication.

36 MATERIALS SCIENCE↗
DOE OSTI2021

UEMtomaton: A Source-Available Platform to Aid in Start-up of Ultrafast Electron Microscopy Labs

The steady rise in the number of ultrafast electron microscopy (UEM) labs, in addition to the opacity and lack of detailed descriptions of current approaches that would enable point-by-point construction, has created an opportunity for sharing common methods and instrumentation for (for example) automating data acquisition to assist in efficient lab start-up and to learn about common and robust protocols. In the spirit of open sharing of methods, we provide here a description of an entry-level method and user interface (UI) for automating UEM experiments, and we provide access to the source code and scripts (source-available) for ease of implementation or as a starting reference point for those entering or seeking to enter the field (https://github.com/CEMSFlannigan/UEMtomaton/releases/tag/v1.0). Core instrumentation and physical connections in the UEM lab at Minnesota are described. Interface communication schemes consisting of duo server-client pairs between critical components – the optical delay stage and the UEM digital camera – are presented, with emphasis placed on describing the logic and communications sequence designed to conduct automated series acquisitions. An application designed and programmed with C++/CLI as Windows Forms in Microsoft Visual Studio – dubbed UEMtomaton – is also presented. Key to the UI layout is centralization of the automation tasks and establishment of communication within the software rather than by interfacing with each individual workstation. It is our hope that this note provides useful insight for current and future UEM researchers, particularly with respect to generalizability and portability of the approach to emerging labs. Here, we note that while this basic, entry-level approach is certainly not the most sophisticated or comprehensive of those currently in use, we feel there is nevertheless value in clearly communicating a proven straightforward method to hopefully lower the barrier to entry into the field.

47 OTHER INSTRUMENTATION↗
DOE OSTI2022

A Quantitative Method for In Situ Pump-Beam Metrology in 4D Ultrafast Electron Microscopy

In this work, we report a method for measuring spot size and focusing conditions of the femtosecond (fs) excitation laser in situ at the specimen location in 4D ultrafast electron microscopy (UEM). The method makes use of threshold laser ablation behaviors of thin amorphous carbon membranes. For Gaussian beam profiles and for ablation threshold fluence values, we analytically derive expressions describing the relationship between ablated hole size and the actual laser spot size. Using these expressions, we developed experimental procedures for characterizing the shape and spot size of the pump beam at the specimen. We demonstrate the viability of the approach for incident excitation wavelengths of 343 nm and 515 nm, thus illustrating the applicability of the method to a range of optical wavelengths without modification. Further, we show that by measuring ablated hole size as a function of focusing condition, a full metrological characterization of the Gaussian beam propagation properties can be performed. Finally, we find good agreement for spot sizes determined with this method and with those determined by extrapolation from measurements taken outside the microscope column. Overall, this method is a simple, cost-effective means for accurate and precise determination of key pump-beam parameters in situ at the specimen location in UEM experiments.

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

Reconstructing the exit wave of 2D materials in high-resolution transmission electron microscopy using machine learning

Reconstruction of the exit wave function is an important route to interpreting high-resolution transmission electron microscopy (HRTEM) images. Here we demonstrate that convolutional neural networks can be used to reconstruct the exit wave from a short focal series of HRTEM images, with a fidelity comparable to conventional exit wave reconstruction. We use a fully convolutional neural network based on the U-Net architecture, and demonstrate that we can train it on simulated exit waves and simulated HRTEM images of graphene-supported molybdenum disulphide (an industrial desulfurization catalyst). We then apply the trained network to analyse experimentally obtained images from similar samples, and obtain exit waves that clearly show the atomically resolved structure of both the MoS 2 nanoparticles and the graphene support. We also show that it is possible to successfully train the neural networks to reconstruct exit waves for 3400 different two-dimensional materials taken from the Computational 2D Materials Database of known and proposed two-dimensional materials.

2D materials↗
DOE OSTI2023

Circular dichroism in hard X-ray photoelectron diffraction observed by time-of-flight momentum microscopy

X-ray photoelectron diffraction (XPD) is a powerful technique that yields detailed structural information of solids and thin films that complements electronic structure measurements. Among the strongholds of XPD we can identify dopant sites, track structural phase transitions, and perform holographic reconstruction. High-resolution imaging of k ll -distributions (momentum microscopy) presents a new approach to core-level photoemission. It yields full-field k x -k y XPD patterns with unprecedented acquisition speed and richness in details. Here, we show that beyond the pure diffraction information, XPD patterns exhibit pronounced circular dichroism in the angular distribution (CDAD) with asymmetries up to 80%, alongside with rapid variations on a small k ll -scale (0.1 Å -1 ). Measurements with circularly-polarized hard X-rays (hν = 6 keV) for a number of core levels, including Si, Ge, Mo and W, prove that core-level CDAD is a general phenomenon that is independent of atomic number. The fine structure in CDAD is more pronounced compared to the corresponding intensity patterns. Additionally, they obey the same symmetry rules as found for atomic and molecular species, and valence bands. Further, the CD is antisymmetric with respect to the mirror planes of the crystal, whose signatures are sharp zero lines. Calculations using both the Bloch-wave approach and one-step photoemission reveal the origin of the fine structure that represents the signature of Kikuchi diffraction. To disentangle the roles of photoexcitation and diffraction, XPD has been implemented into the Munich SPRKKR package to unify the one-step model of photoemission and multiple scattering theory.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
DOE OSTI2025

Morphotype-resolved characterization of microalgal communities in a nutrient recovery process with ARTiMiS flow imaging microscopy

Microalgae-driven nutrient recovery represents a promising technology for phosphorus removal from wastewater while simultaneously generating biomass that can be valorized to offset treatment costs. As full-scale processes come online, system parameters including biomass composition must be carefully monitored to optimize performance and prevent culture crashes. In this study, flow imaging microscopy (FIM) was leveraged to characterize microalgal community composition in near real-time at a full-scale municipal wastewater treatment plant (WWTP) in Wisconsin, USA, and population and morphotype dynamics were examined to identify relationships between water chemistry, biomass composition, and system performance. Two FIM technologies, FlowCam and ARTiMiS, were evaluated as monitoring tools. ARTiMiS provided a more accurate estimate of total system biomass, and estimates derived from particle area as a proxy for biovolume yielded better approximations than particle counts. Deep learning classification models trained on annotated image libraries demonstrated equivalent performance between FlowCam and ARTiMiS, and convolutional neural network (CNN) classifiers proved significantly more accurate when compared to feature table-based dense neural network (DNN) models. Across a two-year study period, Scenedesmus spp. appeared most important for phosphorus removal, and were negatively impacted by elevated temperatures and increase in nitrite/nitrate concentrations. Chlorella and Monoraphidium also played an important role in phosphorus removal. For both Scenedesmus and Chlorella, smaller morphological types were more often associated with better system performance, whereas larger morphotypes likely associated with stress response(s) correlated with poor phosphorus recovery rates. Furthermore, these results demonstrate the potential of FIM as a critical technology for high-resolution characterization of industrial microalgal processes.

59 BASIC BIOLOGICAL SCIENCES↗
DOE OSTI2024

Nanoscopic lipid domains determined by microscopy and neutron scattering

Biological membranes are highly complex supramolecular assemblies, which play central roles in biology. However, their complexity makes them challenging to study their nanoscale structures. To overcome this challenge, model membranes assembled using reduced sets of membrane-associated biomolecules have been found to be both excellent and tractable proxies for biological membranes. Due to their relative simplicity, they have been studied using a range of biophysical characterization techniques. Here, in this review article, we will briefly detail the use of fluorescence and electron microscopies, and X-ray and neutron scattering techniques used over the past few decades to study the nanostructure of biological membranes.

59 BASIC BIOLOGICAL SCIENCES↗
DOE OSTI2012

A Transmission Electron Microscopy Study of the Effect of Interfaces on Bubble Formation in He-Implanted Cu-Nb Multilayers

Magnetron sputtered thin films of Cu, Nb, and Cu-Nb multilayers with 2.5 and 5 nm nominal layer thickness were deposited on Si and implanted with 4He+ and 3He+ ions. Secondary ion mass spectroscopy and nuclear reaction analysis, respectively, were used to measure the 4He+ and 3He+ concentration profile with depth inside the films. Cross-sectional transmission electron microscopy was used to characterize the helium bubbles. Analysis of the contrast from helium bubbles in defocused transmission electron microscope images showed a minimum bubble diameter of 1.25 nm. While pure Cu and Nb films showed bubble contrast over the entire range of helium implantation, the multilayers exhibited bubbles only above a critical He concentration that increased almost linearly with decreasing layer thickness. The work shows that large amounts of helium can be trapped at incoherent interfaces in the form of stable, nanometer-size bubbles.

36 MATERIALS SCIENCE↗
DOE OSTI2012

Atomic-Scale Imaging and Spectroscopy for In Situ Liquid Scanning Transmission Electron Microscopy

Observation of growth, synthesis, dynamics and electrochemical reactions in the liquid state is an important yet largely unstudied aspect of nanotechnology. The only techniques that can potentially provide the insights necessary to advance our understanding of these mechanisms is simultaneous atomic-scale imaging and quantitative chemical analysis (through spectroscopy) under environmental conditions in the transmission electron microscope (TEM). In this study we describe the experimental and technical conditions necessary to obtain electron energy loss (EEL) spectra from a nanoparticle in colloidal suspension using aberration corrected scanning transmission electron microscopy (STEM) combined with the environmental liquid stage. At a fluid path length below 400 nm, atomic resolution images can be obtained and simultaneous compositional analysis can be achieved. We show that EEL spectroscopy can be used to quantify the total fluid path length around the nanoparticle, and demonstrate characteristic core-loss signals from the suspended nanoparticles can be resolved and analyzed to provide information on the local interfacial chemistry with the surrounding environment. The combined approach using aberration corrected STEM and EEL spectra with the in situ fluid stage demonstrates a plenary platform for detailed investigations of solution based catalysis and biological research.

atomic resolution↗
DOE OSTI2014

Combined Scanning Transmission Electron Microscopy Tilt- and Focal Series

In this study, a combined tilt- and focal series is proposed as a new recording scheme for high-angle annular dark-field scanning transmission electron microscopy (STEM) tomography. Three-dimensional (3D) data were acquired by mechanically tilting the specimen, and recording a through-focal series at each tilt direction. The sample was a whole-mount macrophage cell with embedded gold nanoparticles. The tilt focal algebraic reconstruction technique (TF-ART) is introduced as a new algorithm to reconstruct tomograms from such combined tilt- and focal series. The feasibility of TF-ART was demonstrated by 3D reconstruction of the experimental 3D data. The results were compared with a conventional STEM tilt series of a similar sample. The combined tilt- and focal series led to smaller missing wedge artifacts, and a higher axial resolution than obtained for the STEM tilt series, thus improving on one of the main issues of tilt series-based electron tomography.

Dahmen, Tim↗
DOE OSTI2016

Picoliter Drop-On-Demand Dispensing for Multiplex Liquid Cell Transmission Electron Microscopy

Abstract Liquid cell transmission electron microscopy (LCTEM) provides a unique insight into the dynamics of nanomaterials in solution. Controlling the addition of multiple solutions to the liquid cell remains a key hurdle in our ability to increase throughput and to study processes dependent on solution mixing including chemical reactions. Here, we report that a piezo dispensing technique allows for mixing of multiple solutions directly within the viewing area. This technique permits deposition of 50 pL droplets of various aqueous solutions onto the liquid cell window, before assembly of the cell in a fully controlled manner. This proof-of-concept study highlights the great potential of picoliter dispensing in combination with LCTEM for observing nanoparticle mixing in the solution phase and the creation of chemical gradients.

Environmental Molecular Sciences Laboratory↗
DOE OSTI2017

Characterization of BiVO 4 Powders and Thin Films by Electron Microscopy and Electron Energy Loss Spectroscopy

BiVO4 (BVO) is a promising material for photoelectro-chemical water splitting by using visible light. It is formed by abundant and nontoxic elements i.e. low cost and environmentally friendly. BVO has three polymorphs: orthorhombic, tetragonal, and monoclinic. The monoclinic phase (m-BVO) phase exhibits a much higher photocatalytical activity due to its favorable band gap (2.4–2.5 eV) in the visible region of the electromagnetic spectrum, and a valence band position suitable for driving water oxidation under illumination. An earlier investigation using scanning transmission electron microscopy (STEM) and energy loss spectroscopy (EELS) has shown a pronounced surface reduction of monoclinic BVO particles i.e., within a 5 nm thick shell, the oxidation state of V is reduced from +5 to about +4 [1]. This demands for around 15% oxygen vacancies of charge neutrality is assumed.

74 ATOMIC AND MOLECULAR PHYSICS↗
DOE OSTI2017

High-Resolution Field Emission Scanning Electron Microscopy (FESEM) Imaging of Cellulose Microfibril Organization in Plant Primary Cell Walls

Abstract We have used field emission scanning electron microscopy (FESEM) to study the high-resolution organization of cellulose microfibrils in onion epidermal cell walls. We frequently found that conventional “rule of thumb” conditions for imaging of biological samples did not yield high-resolution images of cellulose organization and often resulted in artifacts or distortions of cell wall structure. Here we detail our method of one-step fixation and dehydration with 100% ethanol, followed by critical point drying, ultrathin iridium (Ir) sputter coating (3 s), and FESEM imaging at a moderate accelerating voltage (10 kV) with an In-lens detector. We compare results obtained with our improved protocol with images obtained with samples processed by conventional aldehyde fixation, graded dehydration, sputter coating with Au, Au/Pd, or carbon, and low-voltage FESEM imaging. The results demonstrated that our protocol is simpler, causes little artifact, and is more suitable for high-resolution imaging of cell wall cellulose microfibrils whereas such imaging is very challenging by conventional methods.

biofuels (including algae and biomass), bio-inspir↗
DOE OSTI2018

Atomic-Resolution Study of Grain Boundaries in CdTe Using Scanning Transmission Electron Microscopy

CdTe is one of the most promising photovoltaic materials due to its near optimum band gap and a high absorption coefficient. However, the efficiencies of both champion poly-crystalline CdTe photovoltaic cells as well as production line modules are still significantly below the theoretical Shockley-Queisser limit of ~30%. Reduction of non-radiative recombination at grain boundaries is believed to be the key to improving the efficiency of polycrystalline CdTe-based solar cells. Here, atomistic-level characterization, including scanning transmission electron microscopy (STEM) and first principles density functional theory (DFT) modeling, is crucial in developing a fundamental understanding of how grain boundaries affect the solar cells’ efficiency.

14 SOLAR ENERGY↗