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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 1,099 records · Page 61
All sourcesNASA NTRSDOE OSTI
DOE OSTI2017

Etching of Cr tips for scanning tunneling microscopy of cleavable oxides

Here, we report a detailed three-step roadmap for the fabrication and characterization of bulk Cr tips for spin-polarized scanning tunneling microscopy. Our strategy uniquely circumvents the need for ultra-high vacuum preparation of clean surfaces or films. First, we demonstrate the role of ex situ electrochemical etch parameters on Cr tip apex geometry, using scanning electron micrographs of over 70 etched tips. Second, we describe the suitability of the in situ cleaved surface of the layered antiferromagnet La 1.4 Sr 1.6 Mn 2 O 7 to evaluate the spin characteristics of the Cr tip, replacing the ultra-high vacuum-prepared test samples that have been used in prior studies. Third, we outline a statistical algorithm that can effectively delineate closely spaced or irregular cleaved step edges, to maximize the accuracy of step height and spin-polarization measurements.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Time-resolved correlative optical microscopy of charge-carrier transport, recombination, and space-charge fields in CdTe heterostructures

From time- and spatially resolved optical measurements, we show that extended defects can have a large effect on the charge-carrier recombination in II-VI semiconductors. In CdTe double heterostructures grown by molecular beam epitaxy on the InSb (100)-orientation substrates, we characterized the extended defects and found that near stacking faults the space-charge field extends by 2-5 μm. Charge carriers drift (with the space-charge field strength of 730-1,360 V cm -1 ) and diffuse (with the mobility of 260 ± 30 cm 2 V -1 s -1 ) toward the extended defects, where the minority-carrier lifetime is reduced from 560 ns to 0.25 ns. Furthermore, the extended defects are nonradiative recombination sinks that affect areas significantly larger than the typical crystalline grains in II-VI solar cells. From the correlative time-resolved photoluminescence and second-harmonic generation microscopy data, we developed a band-diagram model that can be used to analyze the impact of extended defects on solar cells and other electronic devices.

14 SOLAR ENERGY↗
DOE OSTI2017

Filling fraction of Yb in CoSb 3 Skutterudite studied by electron microscopy

We report the filling fraction limit in filled Skutterudites plays a critical role in thermoelectric properties; however, the exact filling fraction limit for certain fillers is still in debate. In this work, we observed the lattice distortion, where lattice parameters a and b are unequal, in the annealed Yb-filled CoSb 3 . Microstructure characterization by advanced spherical aberration-corrected (C S -corrected) electron microscopy, energy-dispersive X-ray spectroscopy, and electron energy loss spectroscopy in conjunction with thermoelectric characterization clearly proves that the Yb filling fraction is higher in the annealed sample (with lattice distortion) than in the ball-milled sample (without lattice distortion). Therefore, the results indicate that lattice distortion appears when the Yb filling fraction reaches a certain critical value in CoSb 3 Skutterudites. Lastly, the observed lattice distortion provides an alternative approach to probe the filling fraction in filled Skutterudites.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Direct characterization of the Li intercalation mechanism into α-V 2 O 5 nanowires using in-situ transmission electron microscopy

The Li-V 2 O 5 system has been well studied electrochemically, but there is a lack of systematic in-situ studies involving direct investigations of the structural changes that accompany the lithiation process. The open-cell battery setup inside a transmission electron microscope is ideal for studying the reaction pathway of intercalation of Li + into nanowire cathodes. Here, in this work, we utilize in-situ transmission electron microscopy to study the Li-V 2 O 5 system. More specifically, we employ electron beam diffraction and electron energy-loss spectroscopy (EELS) in an open-cell battery setup to examine the phase changes within α-V 2 O 5 nanowire cathodes upon in-situ lithiation. Our results suggest that the pristine α-V 2 O 5 nanowire forms a Li oxide shell which then acts as a solid state electrolyte to conduct Li + ions, and the bulk of the V 2 O 5 nanowire undergoes transformation to the γ-Li 2 V 2 O 5 phase.

25 ENERGY STORAGE↗
DOE OSTI2017

Artifact mitigation of ptychography integrated with on-the-fly scanning probe microscopy

In this paper, we report our experiences with conducting ptychography simultaneously with the X-ray fluorescence measurement using the on-the-fly mode for efficient multi-modality imaging. We demonstrate that the periodic artifact inherent to the raster scan pattern can be mitigated using a sufficiently fine scan step size to provide an overlap ratio of >70%. This allows us to obtain transmitted phase contrast images with enhanced spatial resolution from ptychography while maintaining the fluorescence imaging with continuous-motion scans on pixelated grids. Lastly, this capability will greatly improve the competence and throughput of scanning probe X-ray microscopy.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Size analysis of sub-resolution objects by Kerr microscopy

Here, a Kerr microscopy method for the quantitative measurement of the size of magnetic objects that are smaller than the resolution limit is proposed. It can be applied to domain walls, bubble domains and magnetic skyrmion-bubble hybrid microstructures. The method is based on the integral contrast, determined by proper line scans across the object, which turns out to be independent from the resolution of the microscope after normalization to the maximum domain contrast.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
DOE OSTI2018

Temperature dependence of secondary electron emission: A new route to nanoscale temperature measurement using scanning electron microscopy

Scanning electron microscopy (SEM) is ubiquitous for imaging but is not generally regarded as a tool for thermal measurements. Here, the temperature dependence of secondary electron (SE) emission from a sample's surface is investigated. Spatially uniform SEM images and the net charge flowing through a sample were recorded at different temperatures to quantify the temperature dependence of SE emission and electron absorption. The measurements also demonstrated charge conservation during thermal cycling by placing the sample inside a Faraday cup to capture the emitted SEs and back-scattered electrons from the sample. The temperature dependence of SE emission was measured for four semiconducting materials (Si, GaP, InP, and GaAs) with response coefficients found to be of magnitudes ~100-1000 ppm/K. The detection limits for temperature changes were no more than ±8 °C for 60 s acquisition time.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
DOE OSTI2019

Multiple parameter dynamic photoresponse microscopy for data-intensive optoelectronic measurements of van der Waals heterostructures

Quantum devices made from van der Waals (vdW) heterostructures of two dimensional (2D) materials may herald a new frontier in designer materials that exhibit novel electronic properties and unusual electronic phases. However, due to the complexity of layered atomic structures and the physics that emerges, experimental realization of devices with tailored physical properties will require comprehensive measurements across a large domain of material and device parameters. Such multi-parameter measurements require new strategies that combine data-intensive techniques—often applied in astronomy and high energy physics—with the experimental tools of solid state physics and materials science. We discuss the challenges of comprehensive experimental science and present a technique, called Multi-Parameter Dynamic Photoresponse Microscopy (MPDPM), which utilizes ultrafast lasers, diffraction limited scanning beam optics, and hardware automation to characterize the photoresponse of 2D heterostructures in a time efficient manner. Using comprehensive methods on vdW heterostructures results in large and complicated data sets; in the case of MPDPM, we measure a large set of images requiring advanced image analysis to extract the underlying physics. We discuss how to approach such data sets in general and in the specific case of a graphene–boron nitride–graphite heterostructure photocell.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Radiation furnace for synchrotron dark-field x-ray microscopy experiments

We present a multi-purpose radiation furnace designed for x-ray experiments at synchrotrons. The furnace is optimized specifically for dark-field x-ray microscopy (DFXM) of crystalline materials at beamline ID06 of the European Synchrotron Radiation Facility. The furnace can reach temperatures above 1200 °C with a thermal stability better than 10 °C, with heating and cooling rates up to 30 K/s. The non-contact heating design enables samples to be heated either in air or in a controlled atmosphere contained within a capillary tube. The temperature was calibrated via the thermal expansion of an α-iron grain. Temperature profiles in the y and z axes were measured by scanning a thermocouple through the focal spot of the radiation furnace. In the current configuration of the beamline, this furnace can be used for DFXM, near-field x-ray topography, bright-field x-ray nanotomography, high-resolution reciprocal space mapping, and limited powder diffraction experiments. As a first application, we present a DFXM case study on isothermal heating of a commercially pure single crystal of aluminum.

Yildirim, C. (ORCID:0000000249690685)↗
DOE OSTI2020

Investigating the effect of electric fields on lead halide perovskites by scanning tunneling microscopy

Lead halide perovskites have emerged as promising absorber materials over the last decade to increase the efficiency of photovoltaics beyond its current limits. However, to further optimize the performance of perovskites, more detailed studies need to be performed which allow for the correlation of film morphology and local electronic properties at the nanoscale. In this paper, we present a scanning tunneling microscopy (STM) approach to probe the effect of an applied electric field of a methylammonium formamidinium lead triiodide perovskite thin film on the film response by current-voltage spectroscopy, current imaging tunneling spectroscopy, differential conductance mapping and X-ray absorption spectroscopy (XAS) by means of synchrotron X-ray STM (SX-STM). We find a strong correlation between the measurement conditions and the obtained current-voltage characteristics when imaging under opposite applied bias polarities. In particular, we find similarities to already observed poling effects for perovskites which result in either a positively or negatively charged interface due to ion and vacancy migration. Our results provide insight into the influence of measurement conditions such as bias polarity on the performance assessment of perovskite thin films by STM.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2020

Isotope effects on the high pressure viscosity of liquid water measured by differential dynamic microscopy

In this paper, differential dynamic microscopy is performed in diamond anvil cells to measure the viscosity of water along the 24 °C isotherm to high-pressure by determination of the tracer diffusion coefficient of monodisperse silica spheres of known diameter and application of the Stokes-Einstein-Sutherland equation. This technique allows liquid samples to be compressed to greater pressure prior to freezing than with other viscometry methods. The highest-pressure measurement was made at 1.67 GPa, considerably deeper into the supercompressed regime than previously reported. The effect of isotopic composition is investigated with samples of normal water, heavy water, and partially deuterated water. When data below 0.25 GPa are excluded a free volume model fits the observed viscosities well yielding a theoretical glass transition density close to that observed in very-high-density amorphous ice. The improved fit above 0.25 GPa coincides with the loss of other anomalous behaviors in liquid water caused by hydrogen bonding and represents a transition to properties closer to those of a simple liquid.

74 ATOMIC AND MOLECULAR PHYSICS↗
DOE OSTI2020

Super-resolution and signal separation in contact Kelvin probe force microscopy of electrochemically active ferroelectric materials

In this work, imaging mechanisms in contact Kelvin probe force microscopy (cKPFM) are explored via information theory-based methods. Gaussian processes are used to achieve super-resolution in the cKPFM signal, effectively extrapolating across the spatial and parameter space. Tensor factorization is applied to reduce the multidimensional signal to the tensor convolution of the scalar functions that show a clear trending behavior with the imaging parameters. These methods establish a workflow for the analysis of the multidimensional datasets that can then be related to the relevant physical mechanisms. We also provide an interactive Google Colab notebook that goes through all the analyses discussed in the paper.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Local characterization of a heavy-fermion superconductor via sub-Kelvin magnetic force microscopy

Using magnetic force microscopy operating at sub-Kelvin temperatures, we characterize the heavy fermion superconductor CeCoIn5. We pinpoint the absolute London penetration depth of λ(0)=435 ± 20 nm and report its temperature dependence, which is closely linked to the symmetry of the superconducting gap. In addition, we directly measure the pinning force of individual Abrikosov vortices and estimate the critical current density of jc=9×104 A/cm2. In contrast to the related, well-established tunnel diode oscillator technique, our method is capable of resolving inhomogeneities locally on the micrometer scale at ultra-low temperature.

Wulferding, Dirk (ORCID:0000000342792109)↗
DOE OSTI2021

Prospects for sub-nanometer scale imaging of optical phenomena using electron microscopy

Imaging of optical phenomena at the sub-nanometer scale can offer fundamental insights into the electronic or vibrational states in atomic-scale defects, molecules, and nanoparticles, which are important in quantum information, heterogeneous catalysis, optoelectronics, and structural biology. Several techniques have surpassed the traditional Abbe diffraction limit and attained spatial resolutions down to a few nanometers, but sub-nanometer scale optics has remained elusive. Here, we propose an approach that combines spectrally specific photoabsorption with sub-nanometer scale resolution transmission electron microscopy (TEM) of photoexcited electrons. We first estimate the signal level and conditions required for imaging nanoscale optical phenomena in core-shell quantum dots (QDs) like CdS/CdTe. Furthermore, we show the possibility of imaging photoexcited states of atomic-scale defects in a monolayer hexagonal boron nitride (h-BN) using ab initio and high resolution (HR)TEM simulations. The ability to directly visualize photoexcited states at the sub-nanometer scale opens opportunities to study properties of individual quantum dots and atomic defects.

74 ATOMIC AND MOLECULAR PHYSICS↗
DOE OSTI2021

Probing polarization dynamics at specific domain configurations: Computer-vision based automated experiment in piezoresponse force microscopy

Topological defects in ferroelectric materials have attracted much attention due to the emergence of conductive, ferroic, and magnetic functionalities. However, many topological configurations dynamically evolve during the switching processes, making them a challenge to characterize via traditional techniques. Here, we implement an automated experimentation approach for the exploration of functional properties in BiFeO 3 thin films. Specifically, we visualize the ferroelectric domain structures via single frequency piezoresponse force microscopy and implement a computer vision-based algorithm to discover features of interest at which spectroscopic measurements are taken. Subsequently, we employ dimensionality reduction techniques to reveal characteristic polarization behaviors at these features. This approach can be extended to other spectroscopies and modalities to probe only specific features of interest, ultimately enabling dynamical processes in ferroelectrics to be studied.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Non-destructive depth-resolved characterization of residual strain fields in high electron mobility transistors using differential aperture x-ray microscopy

Localized residual stress and elastic strain concentrations in microelectronic devices often affect the electronic performance, resistance to thermomechanical damage, and, likely, radiation tolerance. A primary challenge for the characterization of these concentrations is that they exist over sub-μm length-scales, precluding their characterization by more traditional residual stress measurement techniques. Here, in this study, we demonstrate the use of synchrotron x-ray-based differential aperture x-ray microscopy (DAXM) as a viable, non-destructive means to characterize these stress and strain concentrations in a depth-resolved manner. DAXM is used to map two-dimensional strain fields between the source and the drain in a gallium nitride (GaN) layer within high electron mobility transistors (HEMTs) with sub-μm spatial resolution. Strain fields at various positions in both pristine and irradiated HEMT specimens are presented in addition to a preliminary stress analysis to estimate the distribution of various stress components within the GaN layer. γ-irradiation is found to significantly reduce the lattice plane spacing in the GaN along the sample normal direction, which is attributed to radiation damage in transistor components bonded to the GaN during irradiation.

42 ENGINEERING↗
DOE OSTI2022

Low Repetition-Rate, High-Resolution Femtosecond Transmission Electron Microscopy

Spatial and energy resolutions of state-of-the-art transmission electron microscopes (TEMs) have surpassed 50 pm and 5 meV. However, with respect to the time domain, even the fastest detectors combined with the brightest sources may only be able to reach the microsecond timescale. Thus, conventional methods are incapable of resolving myriad fundamental ultrafast (i.e., attosecond to picosecond) atomic-scale dynamics. The successful demonstration of femtosecond (fs) laser-based (LB) ultrafast transmission electron microscopy (UEM) nearly 20 years ago provided a means to span this nearly 10-order-of-magnitude temporal gap. While nanometer-picosecond UEM studies of dynamics are now well established, ultrafast Å-scale imaging has gone largely unrealized. Further, while instrument development has rightly been an emphasis, and while new modalities and uses of pulsed-beam TEM continue to emerge, the overall chemical and materials application space has been only modestly explored to date. In this Perspectives article, we argue that these apparent shortfalls can be attributed to a simple lack of data and detail. We speculate that present work and continued growth of the field will ultimately lead to the realization that Å-scale fs dynamics can indeed be imaged with minimally modified UEM instrumentation and with repetition rates (f rep ) below - and perhaps even well below - 1 MHz. We further argue that use of low f rep , whether for LB UEM or for chopped/bunched beams, significantly expands the accessible application space. Furthermore, this calls for systematically establishing modality-specific limits so that especially promising technologies can be pursued, thus ultimately facilitating broader adoption as individual instrument capabilities expand.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2023

Scanning tunneling microscopy and spectroscopy characterization of Nb films for quantum applications

Niobium thin films are key components of superconducting microwave resonators. Interest in these devices has increased dramatically because of their application in quantum systems. Despite tremendous effort to improve their performance, loss mechanisms are still not well understood. Nb/substrate and Nb/air interfaces are likely culprits in contributing to decoherence and ultimately limiting the performance of superconducting devices. Here, we investigate the Nb/substrate interface by studying the effect of hydrogen-passivated H:Si(111) substrates on the local superconducting properties of ∼40 nm thick Nb films compared to Nb films grown on typical Si(001) substrates. Specifically, low-temperature scanning tunneling microscopy and spectroscopy are employed to compare nanoscale material properties. Further, the atomically flat monohydride H:Si(111) substrates are found to yield a smoother and less defective interface with the Nb film. Correspondingly, the Nb films grown on H:Si(111) substrates present more uniform superconducting properties and exhibit less quasiparticle broadening.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗