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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 1,621 records · Page 90
All sourcesNASA NTRSDOE OSTI
DOE OSTI2020

A microchip microcontroller-based transducer controller for non-contact scanning probe microscopy with phase-locked loop, amplitude, and Q control

An inexpensive yet versatile transducer controller for non-contact scanning probe microscopy (SPM) based on a PIC32 microcontroller from Microchip Technology, Inc is described. In addition to feedback control using the amplitude or phase of the signal from the non-contact transducer, the controller includes a phase-locked loop for frequency-shift feedback, as well as fixed-amplitude, quality factor (Q) control, and self-excitation modes. Apart from the input amplifiers, output buffers, and the Q-control circuit, all other functions of the controller are instantiated in software on the microchip, enabling rapid changes in operating parameters if needed. The controller communicates with a host personal computer via a simple serial connection. The controller has been tested with a quartz tuning-fork transducer but can be used with any oscillating non-contact transducer.

47 OTHER INSTRUMENTATION↗
DOE OSTI2020

A modular ultra-high vacuum millikelvin scanning tunneling microscope

We describe the design, construction, and performance of an ultra-high vacuum (UHV) scanning tunneling microscope (STM) capable of imaging at dilution-refrigerator temperatures and equipped with a vector magnet. The primary objective of our design is to achieve a high level of modularity by partitioning the STM system into a set of easily separable, interchangeable components. This naturally segregates the UHV needs of STM instrumentation from the typically non-UHV construction of a dilution refrigerator, facilitating the usage of non-UHV materials while maintaining a fully bakeable UHV chamber that houses the STM. Here, the modular design also permits speedy removal of the microscope head from the rest of the system, allowing for repairs, modifications, and even replacement of the entire microscope head to be made at any time without warming the cryostat or compromising the vacuum. Without using cryogenic filters, we measured an electron temperature of 184 mK on a superconducting Al(100) single crystal.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2020

Bayesian inference in band excitation scanning probe microscopy for optimal dynamic model selection in imaging

The universal tendency in scanning probe microscopy (SPM) over the last two decades is to transition from simple 2D imaging to complex detection and spectroscopic imaging modes. The emergence of complex SPM engines brings forth the challenge of reliable data interpretation, i.e., conversion from detected signals to descriptors specific to tip–surface interactions and subsequently to material’s properties. In this work, we implemented a Bayesian inference approach for the analysis of the image formation mechanisms in band excitation SPM. Compared to the point estimates in classical functional fit approaches, Bayesian inference allows for the incorporation of extant knowledge of materials and probe behavior in the form of corresponding prior distribution and return the information on the material functionality in the form of readily interpretable posterior distributions. We explore the nonlinear mechanical behaviors spatially in a classical ferroelectric material, PbTiO 3 . We observe the non-trivial evolution of the Duffing stiffness term and the nonlinearity of the sample surface, determine spatial clustering of the nonlinear response, and perform a Landau analysis on predicting the nonlinear coefficient, which indicates that ferroelectric behavior can be a cause of the observed results. These observations suggest that the spectrum of anomalous behaviors at the ferroelectric domain walls may be broader than previously believed and can extend to non-conventional mechanical properties in addition to static and microwave conductance.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Revisiting heat treatment and surface activation of GaAs photocathodes: In situ studies using scanning tunneling microscopy and photoelectron spectroscopy

The lifetime of GaAs photocathodes in polarized electron guns is limited due to the delicate activation layer. An atomically clean and smooth GaAs surface is needed to deposit a robust activation layer, such as Cs 2 Te, with longer lifetime compared to traditional (Cs,O) activation. A previous experiment with Cs 2 Te activation on GaAs used heat cleaning temperatures around 400°C to avoid an increase in surface roughness [Bae et al., Appl. Phys. Lett. 112, 154101 (2018)]. Furthermore, high-temperature heat cleaning around 580°C, which results in a relatively contamination-free surface, could be one possible way to improve quantum efficiency. However, one should be cautious about surface roughness degradation during high-temperature heat cleaning. In this paper, we report results of surface roughness measurements on native, heat cleaned, and (Cs,O) activated GaAs photocathodes under vacuum. The results, measured by ultrahigh vacuum scanning tunneling microscopy, show that the surface roughness improves as the heat cleaning temperature is increased, by at least a factor of three for 580°C heat cleaning, compared to the native sample. Activation with (Cs,O) is shown to increase surface roughness by a factor of four compared to a 580°C heat cleaned sample. This confirms that high-temperature heat cleaning can be useful for depositing good quality robust activation layers on GaAs. Additionally, we also report chemical analysis for each step of preparation for p-doped GaAs photocathodes using X-ray photoelectron spectroscopy (XPS), angle-resolved XPS, and ultraviolet photoelectron spectroscopy. Our results indicate that the (Cs,O) activation layer forms a sandwich structure consists of Cs and oxygen. We found no formation of any specific compound such as Cs 2 O or Cs 11 O 3 .

43 PARTICLE ACCELERATORS↗
DOE OSTI2021

Scanning SQUID microscopy in a cryogen-free dilution refrigerator

We report a scanning superconducting quantum interference device (SQUID) microscope in a cryogen-free dilution refrigerator with a base temperature at the sample stage of at least 30 mK. The microscope is rigidly mounted to the mixing chamber plate to optimize thermal anchoring of the sample. The microscope housing fits into the bore of a superconducting vector magnet, and our design accommodates a large number of wires connecting the sample and sensor. Through a combination of vibration isolation in the cryostat and a rigid microscope housing, we achieve relative vibrations between the SQUID and the sample that allow us to image with micrometer resolution over a 150 μm range while the sample stage temperature remains at base temperature. To demonstrate the capabilities of our system, we show images acquired simultaneously of the static magnetic field, magnetic susceptibility, and magnetic fields produced by a current above a superconducting micrometer-scale device.

47 OTHER INSTRUMENTATION↗
DOE OSTI2022

Scattering-type scanning near-field optical microscopy with Akiyama piezo-probes

Recent developments of the scattering-type scanning near-field optical microscope at cryogenic temperatures (cryogenic s-SNOM or cryo-SNOM) have led to many breakthroughs in the studies of low energy excitations in quantum materials. However, the simultaneous demands on vibration isolation, low base temperature, precise nano-positioning, and optical access make the construction of a cryo-SNOM a daunting task. Adding to the overhead space required for a cryo-SNOM is the atomic force microscopy control, which predominantly utilizes a laser-based detection scheme for determining the cantilever tapping motion. In this work, we provide an alternative and straightforward route to performing s-SNOM using metal-coated Akiyama probes, where the cantilever tapping motion is detected through a piezoelectric signal. We show that the Akiyama-based cryo-SNOM attains high spatial resolution, good near-field contrast, and is able to perform imaging with a significantly more compact system compared to other cryo-SNOM implementations. Our results firmly establish the potential of s-SNOM based on self-sensing piezo-probes, which can easily accommodate far-infrared wavelengths and high magnetic fields in the future.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
DOE OSTI2024

Unraveling the impact of initial choices and in-loop interventions on learning dynamics in autonomous scanning probe microscopy

The current focus in Autonomous Experimentation (AE) is on developing robust workflows to conduct the AE effectively. This entails the need for well-defined approaches to guide the AE process, including strategies for hyperparameter tuning and high-level human interventions within the workflow loop. This paper presents a comprehensive analysis of the influence of initial experimental conditions and in-loop interventions on the learning dynamics of Deep Kernel Learning (DKL) within the realm of AE in scanning probe microscopy. We explore the concept of the “seed effect,” where the initial experiment setup has a substantial impact on the subsequent learning trajectory. Additionally, we introduce an approach of the seed point interventions in AE allowing the operator to influence the exploration process. Using a dataset from Piezoresponse Force Microscopy on PbTiO 3 thin films, we illustrate the impact of the “seed effect” and in-loop seed interventions on the effectiveness of DKL in predicting material properties. The study highlights the importance of initial choices and adaptive interventions in optimizing learning rates and enhancing the efficiency of automated material characterization. This work offers valuable insights into designing more robust and effective AE workflows in microscopy with potential applications across various characterization techniques.

47 OTHER INSTRUMENTATION↗
DOE OSTI2024

Cooling rate dependence of charge density wave phases in 1 T -TaS 2 studied by scanning tunneling microscopy and x-ray diffraction

The role of dynamics in the charge density wave (CDW) phases of 1T-TaS 2 , especially in accessing metastable phases, is still under scrutiny. We investigated cooling rate dependence on low-temperature CDW phases in this material by scanning tunneling microscopy and x-ray diffraction. In the majority of cases, we found the typical low temperature commensurate CDW and identified no other differences between samples that were fast cooled vs slow cooled from room temperature. In rare cases (1/18 STM experiments and 1/30 XRD experiments), we found a multi-domain structure in the low temperature CDW. The domain structure and metallic behavior revealed by STM and STS measurements of this phase are in excellent agreement with the previously reported metallic mosaic CDW phase.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
DOE OSTI2024

Integration of scanning probe microscope with high-performance computing: Fixed-policy and reward-driven workflows implementation

The rapid development of computation power and machine learning algorithms has paved the way for automating scientific discovery with a scanning probe microscope (SPM). The key elements toward operationalization of the automated SPM are the interface to enable SPM control from Python codes, availability of high computing power, and development of workflows for scientific discovery. Here, we build a Python interface library that enables controlling an SPM from either a local computer or a remote high-performance computer, which satisfies the high computation power need of machine learning algorithms in autonomous workflows. We further introduce a general platform to abstract the operations of SPM in scientific discovery into fixed-policy or reward-driven workflows. Furthermore, our work provides a full infrastructure to build automated SPM workflows for both routine operations and autonomous scientific discovery with machine learning.

47 OTHER INSTRUMENTATION↗
DOE OSTI2024

Analysis of differential scanning calorimetry data for aged plutonium

Differential scanning calorimetry data for samples of a 52 year old plutonium alloy with 3.3 at. % Ga that were heated beyond the melting point is analyzed using transition state theory to find activation energies for the δ to ε and ε to liquid phase transitions. A Bayesian statistical method involving a Gaussian process model is used to find mean values and confidence intervals for the activation energies. The activation energy for the δ to ε phase transition increases by 3.3 ± 3.8% per decade, relative to the case when all age related plutonium lattice point defects have been removed through annealing. The corresponding increase in activation energy for the ε to liquid transition is shown to be 7.1 ± 1.8% per decade. It is postulated that the change in activation energy with age for both phase transitions is caused, in part, by the accumulation of the same type of lattice point defects associated with the observed increase in elastic bulk modulus over time.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2025

Nm-scale electrical resistance imaging on CdTe by scanning spreading resistance microscopy

Local resistance imaging can provide information on nm-scale carrier distribution in semiconductor devices. Scanning spreading resistance microscopy (SSRM), an atomic force microscopy-based nm-scale resistance mapping technique, has been developed for carrier delineation in Si microdevices. We report on the development and validation of SSRM on CdTe materials, by testing on molecular beam epitaxy (MBE) grown CdTe films. The probe/CdTe contact resistance was suppressed sufficiently below sample's spreading resistance by pressing the probe into the sample with ∼mN contact force and applying a large sample/probe forward bias voltage (V s ), which was understood by analyzing current-voltage (I-V) involving a serially connected insulating top layer with underlying spreading resistance. The carrier concentration as deduced from the resistance measurement, using a single mobility value, is consistent with Hall measurement with a standard deviation of 14% based on a set of MBE films with carrier concentrations in the range of 10 15 –10 16 /cm 3 . The doping polarity was readily identified by flipping V s polarity, where the resistance with reverse V s is orders of magnitude larger than forward V s . While focusing on the SSRM technique validation, we also show an example on an As-doped Cd(Se,Te) polycrystalline thin film of a high-performance CdTe solar cell, which illustrates the local resistance nonuniformity with up to two orders of magnitude differences, indicating if local mobility is roughly constant, local carrier concentration can have significant nonuniformity.

14 SOLAR ENERGY↗
DOE OSTI2016

Probing plasmons in three dimensions by combining complementary spectroscopies in a scanning transmission electron microscope

The nanoscale optical response of surface plasmons in three-dimensional metallic nanostructures plays an important role in many nanotechnology applications, where precise spatial and spectral characteristics of plasmonic elements control device performance. Electron energy loss spectroscopy (EELS) and cathodoluminescence (CL) within a scanning transmission electron microscope have proven to be valuable tools for studying plasmonics at the nanoscale. Each technique has been used separately, producing three-dimensional reconstructions through tomography, often aided by simulations for complete characterization. Here we demonstrate that the complementary nature of the two techniques, namely that EELS probes beam-induced electronic excitations while CL probes radiative decay, allows us to directly obtain a spatially- and spectrally-resolved picture of the plasmonic characteristics of nanostructures in three dimensions. Furthermore, the approach enables nanoparticle-by-nanoparticle plasmonic analysis in three dimensions to aid in the design of diverse nanoplasmonic applications.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Imaging via complete cantilever dynamic detection: General dynamic mode imaging and spectroscopy in scanning probe microscopy

We develop and implement a multifrequency spectroscopy and spectroscopic imaging mode, referred to as general dynamic mode (GDM), that captures the complete spatially- and stimulus dependent information on nonlinear cantilever dynamics in scanning probe microscopy (SPM). GDM acquires the cantilever response including harmonics and mode mixing products across the entire broadband cantilever spectrum as a function of excitation frequency. GDM spectra substitute the classical measurements in SPM, e.g. amplitude and phase in lock-in detection. Here, GDM is used to investigate the response of a purely capacitively driven cantilever. We use information theory techniques to mine the data and verify the findings with governing equations and classical lock-in based approaches. We explore the dependence of the cantilever dynamics on the tip–sample distance, AC and DC driving bias. This approach can be applied to investigate the dynamic behavior of other systems within and beyond dynamic SPM. In conclusion, GDM is expected to be useful for separating the contribution of different physical phenomena in the cantilever response and understanding the role of cantilever dynamics in dynamic AFM techniques.

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

Advanced techniques in automated high-resolution scanning transmission electron microscopy

Scanning transmission electron microscopy is a common tool used to study the atomic structure of materials. It is an inherently multimodal tool allowing for the simultaneous acquisition of multiple information channels. Despite its versatility, however, experimental workflows currently rely heavily on experienced human operators and can only acquire data from small regions of a sample at a time. Here, we demonstrate a flexible pipeline-based system for high-throughput acquisition of atomic-resolution structural data using an all-piezo sample stage applied to large-scale imaging of nanoparticles and multimodal data acquisition. As a result, the system is available as part of the user program of the Molecular Foundry at Lawrence Berkeley National Laboratory.

4D-STEM↗
DOE OSTI2016

Imaging electronic states on topological semimetals using scanning tunneling microscopy

Following the intense studies on topological insulators, significant efforts have recently been devoted to the search for gapless topological systems. These materials not only broaden the topological classification of matter but also provide a condensed matter realization of various relativistic particles and phenomena previously discussed mainly in high energy physics. Weyl semimetals host massless, chiral, low-energy excitations in the bulk electronic band structure, whereas a symmetry protected pair of Weyl fermions gives rise to massless Dirac fermions. We employed scanning tunneling microscopy/spectroscopy to explore the behavior of electronic states both on the surface and in the bulk of topological semimetal phases. By mapping the quasiparticle interference (QPI) and emerging Landau levels at high magnetic field in Dirac semimetals Cd 3 As 2 and Na 3 Bi, we observed extended Dirac-like bulk electronic bands. QPI imaged on Weyl semimetal TaAs demonstrated the predicted momentum dependent delocalization of Fermi arc surface states in the vicinity of the surface projected Weyl nodes.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Scanning Transmission Electron Microscopy–Atom Probe Tomography Correlative Analysis for the Characterization of Solute-defect Interactions

Atom probe tomography (APT) and (scanning) transmission electron microscopy ((S)TEM) are complementary techniques that provide spatially resolved chemical and structural information at the atomic scale. Here, in this study, we employ two different STEM/APT correlative analysis methods to investigate Cr segregation at dislocation loops in ultra-high purity Fe–Cr alloys. APT needles for the correlative analysis were extracted either from bulk material or from thinned TEM lamellae. STEM analysis was used to determine the Burgers vectors of ion-irradiation-induced dislocation loops, while APT reconstruction of the same region revealed the Cr segregation to these loops. We extended the g•b = 0 invisibility criterion of dislocation loops from TEM mode in a lamella to STEM mode in a needle-shaped specimen. STEM and APT analysis on the same needle provide straightforward correlative analysis, although it is limited by a small observation volume. In contrast, iterative STEM analysis of TEM lamellae, followed by the selective extraction of specific regions of interest for APT analysis, expands the observation area by up to 100 times but requires additional time-consuming steps for APT needle extraction from the lamellae.

47 OTHER INSTRUMENTATION↗
DOE OSTI2025

Advancing Cross-Sectional Scanning Electron Microscopy of Perovskite Solar Cells

Organic–inorganic perovskites are an emerging class of photovoltaic materials. Despite achieving power conversion efficiencies surpassing 26%, the challenge of perovskite stability including degradation during exposure to operational conditions such as light, heat, humidity, water, oxygen, and electric fields is well known. Related, perovskite instability has limited high-resolution electron imaging and characterization techniques that can be used for understanding degradation mechanisms. Furthermore, we demonstrate perovskite device cross-section preparation using mechanical polishing in a water-free environment with cryogenic Ar ion milling. Scanning electron microscopy was then used in both backscattered electron and secondary electron imaging modes to obtain information about layer structure, grain aggregate structure, and compositional heterogeneity. Monte Carlo CASINO simulations inform optimum beam conditions and image acquisition parameters and the effects of accelerating voltage, dwell times, and frame averaging for practical image acquisition are reported.

14 SOLAR ENERGY↗
DOE OSTI2023

Design of Electrostatic Aberration Correctors for Scanning Transmission Electron Microscopy

Abstract In a scanning transmission electron microscope (STEM), producing a high-resolution image generally requires an electron beam focused to the smallest point possible. However, the magnetic lenses used to focus the beam are unavoidably imperfect, introducing aberrations that limit resolution. Modern STEMs overcome this by using hardware aberration correctors comprised of many multipole elements, but these devices are complex, expensive, and can be difficult to tune. We demonstrate a design for an electrostatic phase plate that can act as an aberration corrector. The corrector is comprised of annular segments, each of which is an independent two-terminal device that can apply a constant or ramped phase shift to a portion of the electron beam. We show the improvement in image resolution using an electrostatic corrector. Engineering criteria impose that much of the beam within the probe-forming aperture be blocked by support bars, leading to large probe tails for the corrected probe that sample the specimen beyond the central lobe. We also show how this device can be used to create other STEM beam profiles such as vortex beams and probes with a high degree of phase diversity, which improve information transfer in ptychographic reconstructions.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗