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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
NASA NTRS1993

Ballistic-Electron-Emission Microscopy Techniques for Nanometer-scale Characterization of Interfaces

Semiconductor interface properties are among the most important phenomena in materials science and technology. The study of metal/semiconductor Schottky barrier interfaces has been the primary focus of a large research and development community for decades. Throughout the long history of interface investigation, the study of interface defect electronic properties have been seriously hindered by the fundamental experimental difficulty of probing subsurface structures. A new method, Ballistic-Electron-Emission Microscopy (BEEM), has been developed which not only enables spectroscopic probing of subsurface interface properties, but also, provides nanometer-resolution imaging capabilities. BEEM employs Scanning Tunneling Microscopy (STM) and a unique spatially localized ballistic electron spectroscopy method...

Bell, L. D.↗
DOE OSTI2024

Fingerprints of composite fermion Lambda levels in scanning tunneling microscopy

A composite fermion (CF) is a topological quasiparticle that emerges from a nonperturbative attachment of vortices to electrons in strongly correlated two-dimensional materials. Similar to noninteracting fermions that form Landau levels in a magnetic field, CFs can fill analogous “Lambda” levels, giving rise to the fractional quantum Hall (FQH) effect of electrons. Here, we show that Lambda levels can be directly visualized through the characteristic peak structure in the signal obtained via spectroscopy with scanning tunneling microscopy (STM) on a FQH state. Complementary to transport, which probes the low-energy properties of CFs, we show that high-energy features in STM spectra can be interpreted in terms of Lambda levels. We numerically demonstrate that STM spectra can be accurately modeled using Jain's CF theory. Our results show that STM provides a powerful tool for revealing the anatomy of FQH states and identifying physics beyond the noninteracting CF paradigm.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗
DOE OSTI2024

Microstructure, electrical resistivity, and tensile properties of neutron-irradiated Cu–Cr–Nb–Zr

High strength, high conductivity copper alloys that can resist creep at high temperatures are one of the primary candidates for efficient heat exchangers in fusion reactors. Cu–Cr–Nb–Zr (CCNZ) alloys, which were designed to improve the strength and creep life of ITER Cu–Cr–Zr (CCZ) reference alloys, have been found to have comparable electrical conductivity and tensile properties to CCZ alloys. The measured creep rupture times for these improved alloys is about ten times higher than the ITER reference alloys at 90–125 MPa at 500 °C. However, the effects of neutron irradiation on these alloys, and the ensuing material properties, have not been studied; thus, their utility in a fusion reactor environment is not well understood. This study characterizes the room temperature mechanical and electrical properties of a neutron-irradiated CCNZ alloy and compares them to a neutron-irradiated ITER reference heat sink CCZ alloy. Tensile specimens were neutron irradiated in the High Flux Isotope Reactor (HFIR) to 5 dpa between 250 °C and 325 °C. Post-irradiation characterization included electrical resistivity measurements, hardness, and tensile tests. Microstructural evaluation used scanning electron microscopy, energy dispersive x-ray spectroscopy, and atom probe tomography to characterize the irradiation-produced changes in the microstructure and investigate the mechanistic processes leading to post-irradiation properties. Transmutation calculations were validated with composition measurements from atom probe data and used to calculate contributions to the increased electrical resistivity measured after irradiation. Comparisons with CCZ alloys in the same irradiation heat found that the post-irradiated CCNZ and CCZ alloys had comparable electrical resistivity. Although CCNZ alloys suffered more irradiation hardening than CCZ, the overall tensile behavior deviated very little from non-irradiated values in the temperature range studied.

36 MATERIALS SCIENCE↗
NASA NTRS2007

Spray CVD for Making Solar-Cell Absorber Layers

Spray chemical vapor deposition (spray CVD) processes of a special type have been investigated for use in making CuInS2 absorber layers of thin-film solar photovoltaic cells from either of two subclasses of precursor compounds: [(PBu3) 2Cu(SEt)2In(SEt)2] or [(PPh3)2Cu(SEt)2 In(SEt)2]. The CuInS2 films produced in the experiments have been characterized by x-ray diffraction, scanning electron microscopy, energy-dispersive spectroscopy, and four-point-probe electrical tests.

Banger, Kulbinder K.↗
DOE OSTI2024

Formation of uranium nitride nanoparticles via mechanical alloying of uranium-molybdenum alloy fuels in gaseous nitrogen

Uranium-molybdenum (U-Mo) alloys show promise as a nuclear fuel system due to their high thermal conductivity and fuel loading capability. However, U-Mo systems are susceptible to irradiation induced swelling ultimately affecting the cladding via mechanical and chemical interactions. To address these shortcomings, this research investigated the formation of uranium mononitride (UN) nanoparticles within a 90 wt% U/10 wt% Mo (U-10Mo) matrix to act as a prospective defect sink for fission products at nanometric hetero-interfaces. To promote the formation of UN, U-10Mo powders were mechanically alloyed under a high purity nitrogen atmosphere. Variations of the milling process investigated included media size, duration of milling, and number of times the milling jar was re-aerated with nitrogen gas. Characterization of the fuel microstructure was completed using light element analysis, X-ray diffraction, scanning and transmission-electron microscopy, electron energy loss spectroscopy, and atom probe tomography. UN nanoparticles measuring 1–5 nm in radius were observed in the U-Mo matrix as early as 1 h into the mechanical alloying process. Milling time in excess of 10 h was found to lead to deleterious effects induced by the stainless-steel milling media.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2025

High spatial resolution charge sensing of quantum Hall states

Charge distribution offers a unique fingerprint of important properties of electronic systems, including dielectric response, charge ordering, and charge fractionalization. Here, we develop an architecture for charge sensing in two-dimensional electronic systems in a strong magnetic field. We probe local change of the chemical potential in a proximitized detector layer using scanning tunneling microscopy, allowing us to infer the chemical potential and the charge profile in the sample. Our technique has both high energy (<0.3 meV) and spatial (<10 nm) resolution exceeding that of previous studies by an order of magnitude. We apply our technique to study the chemical potential of quantum Hall liquids in monolayer graphene under high magnetic fields and their responses to charge impurities. The chemical potential measurement provides a local probe of the thermodynamic gap of quantum Hall ferromagnets and fractional quantum Hall states. The screening charge profile reveals spatially oscillatory response of the quantum Hall liquids to charge impurities and is consistent with the composite Fermi liquid picture close to the half-filling. Our technique also paves the way to map moiré potentials, probe Wigner crystals, and investigate fractional charges in quantum Hall and Chern insulators.

charge sensing↗
DOE OSTI2026

Understanding the structural and morphological effects of synthesis route on NpO 2

The availability of actinide standard materials for use in nuclear safeguard applications is critical, as is thorough characterization thereof. Although accurate trace element compositions and isotopic considerations are paramount for deployment of reference standards, structural characterization is also essential towards accurately describing the chemical form and potential matrix effects in candidate materials. Here, to this end, samples of NpO 2 were synthesized via a direct denitration (DD) method and probed with powder X-ray diffraction (PXRD), Raman spectroscopy, and scanning electron microscopy (SEM) for structural and morphological characterization and comparison with NpO 2 materials produced via modified direct denitration (MDD). PXRD confirmed the bulk identity of NpO 2 , and no additional phases were identified using this method. Analysis of Raman data collected using a 532 nm excitation wavelength indicates that samples are mostly phase pure; however, some variability in spectral features is observed. Analysis of additional spectroscopic data collected with a 785 nm excitation wavelength revealed variability in the relative intensity of spectral features. Raman spectroscopy indicates that the sample is primarily NpO 2 ; however, additional signals indicate possible structural disorder, oxidized species, or potential contributions from other Np phases. To further investigate the possibility of additional phase contributions within the sample of NpO 2 , Raman spectroscopic mapping was employed to examine the homogeneity of the sample produced via DD. From this analysis, we determined that despite variability in the intensity of Raman-active vibrational modes, consistent spectra are obtained throughout the area of the sample investigated. SEM images show aggregates with variable sizes and shapes, with rounded, primary particles possessing an average diameter of approximately 100 nm. Comparison of the results of these multimodal analyses to the literature indicates that the crystal chemical, spectroscopic, and microstructural properties of NpO 2 vary based on synthesis method, even if X-ray diffraction data indicate that the bulk phase is NpO 2 .

Direct denitration↗
NASA NTRS2010

Resonant difference-frequency atomic force ultrasonic microscope

A scanning probe microscope and methodology called resonant difference-frequency atomic force ultrasonic microscopy (RDF-AFUM), employs an ultrasonic wave launched from the bottom of a sample while the cantilever of an atomic force microscope, driven at a frequency differing from the ultrasonic frequency by one of the contact resonance frequencies of the cantilever, engages the sample top surface. The nonlinear mixing of the oscillating cantilever and the ultrasonic wave in the region defined by the cantilever tip-sample surface interaction force generates difference-frequency oscillations at the cantilever contact resonance. The resonance-enhanced difference-frequency signals are used to create images of nanoscale near-surface and subsurface features.

Cantrell, John H.↗
NASA NTRSDate not supplied

Quantative Measurements of Trace Elements and Three-Dimensional Atomic Scale Characterisation of Presolar O-rich Oxides and Silicates: An Atom Probe Tomography Approach

Presolar grains are recordsof a single moment in stellar evolution which have survived nebula and parent body processingwithin our Solar System. These grains condensed within a range of stellar envi-ronments including asymptotic giant branch stars, red giant branch stars, nova, supernova (SN) and hydrogen burning electron capture supernova(ECSN)[1,2]. Iso-topic and chemical compositions can be used to unravel details about environmental conditions at the time of their condensation and physical and chemical processes occurring at the time. For example,nucleosynthesis, stellar evolution, physical properties of stellar atmos-pheres, mixing from inner core to outer envelope, galac-tic chemical evolution, interstellar medium and parent body processing.NanoSIMS enables detailed characterisation of iso-topic compositions and rapid in situidentification of O-rich presolar oxides and silicates using their character-istic 17O/16O and 18O/16O isotopic ratios.Spectroscopic techniques e.g., auger spectroscopyand transmission electron microscopy, have provided additional details on major and minor chemical signatures. However, due tospatial resolution limitations,interaction volumes and interferencesfrom surrounding grains for in situtech-niques, attaining quantative characterisation of trace el-ements,hasproved challenging[1,3]. As the most sensitive geochemical tracers of envi-ronmental changes, trace elements are essential to un-ravelling the geochemical record of their parent stellar environments and evolutionary pathways[4].We car-ried out correlated in situisotopic and chemical analyses of 13 presolar grains to better understand stellar evolu-tion. In this work, we achieved this using a custom ap-proach, coordinating NanoSIMS, Scanning Electron Microscopy Energy Dispersive X-Ray Spectroscopy (SEM-EDX)and Atom Probe Tomography(APT).Our objective was to develop an approach which could ena-ble precise targeting of presolar grains for atom probe tomography and successfully execute atomic scale anal-yses of presolar oxides and silicates, to achieve quantative analysis of their trace elements for the first time.We also aimed to test the capability for Atom Probe tomography to measure isotopic compositions and stoichiometries of presolar oxide and silicate grains.

N D Nevill↗
DOE OSTI2026

Single-particle detection of enhanced polarizability in Au-decorated semiconducting nanorods via scanning dielectric microscopy

Hybrid nanostructures that combine semiconducting and metallic components offer great potential for photothermal therapy, optoelectronics, and sensing, by integrating tunable optical properties with enhanced light absorption and charge transport. Boosting the integrated performance of these hybrid systems demands techniques capable of probing local variations of the physical properties inaccessible to bulk analysis. Here, we report the single-particle dielectric characterization of hybrid, semiconducting bismuth sulfide (Bi 2 S 3 ) nanorods (NR) decorated with metallic Au nanoparticles (NP), employing scanning dielectric microscopy, which uses electrostatic force microscopy in combination with finite-element numerical simulations. We reveal a pronounced enhancement in the local dielectric response of Bi2S3 upon Au decoration, attributed to interfacial polarization and electron transfer from Au to the Bi 2 S 3 matrix, thus suggesting a enhanced metallic-like polarizability at the single-particle level. Numerical simulations show that the response is dominated by the vertical component of the permittivity and that the decorating metallic Au NP produce only moderate shielding of the semiconductor Bi 2 S 3 NR core, indicating that the large increase in the dielectric response originates primarily from intrinsic modifications within the NR. Overall, these findings provide direct insight into structure–property relationships at the single-particle level, supporting the rational design of advanced hybrid nanostructures with tailored electronic functionalities.

36 MATERIALS SCIENCE↗
NASA NTRS1988

Spatially resolved ballistic electron spectroscopy of subsurface interfaces

Buried interfaces have traditionally been inaccessible to direct investigation by surface-sensitive techniques. A unique and novel electronic probe, which is sensitive to subsurface electronic structure, has been utilized to probe Schottky barrier interfaces. The method, ballistic electron emission microscopy (BEEM), is based on scanning tunnelling microscopy (STM) techniques. A theoretical treatment has been developed to describe the ballistic electron spectra obtained by BEEM and this treatment is applied to data obtained on the Au-Si Schottky barrier interface system. Excellent agreement between experiment and theory is obtained. In addition, the treatment predicts nanometer spatial resolution for interface imaging by BEEM.

Bell, L. D.↗
NASA NTRS2003

Scanning Tunneling Optical Resonance Microscopy

Scanning tunneling optical resonance microscopy (STORM) is a method, now undergoing development, for measuring optoelectronic properties of materials and devices on the nanoscale by means of a combination of (1) traditional scanning tunneling microscopy (STM) with (2) tunable laser spectroscopy. In STORM, an STM tip probing a semiconductor is illuminated with modulated light at a wavelength in the visible-to-near-infrared range and the resulting photoenhancement of the tunneling current is measured as a function of the illuminating wavelength. The photoenhancement of tunneling current occurs when the laser photon energy is sufficient to excite charge carriers into the conduction band of the semiconductor. Figure 1 schematically depicts a proposed STORM apparatus. The light for illuminating the semiconductor specimen at the STM would be generated by a ring laser that would be tunable across the wavelength range of interest. The laser beam would be chopped by an achromatic liquid-crystal modulator. A polarization-maintaining optical fiber would couple the light to the tip/sample junction of a commercial STM. An STM can be operated in one of two modes: constant height or constant current. A STORM apparatus would be operated in the constant-current mode, in which the height of the tip relative to the specimen would be varied in order to keep the tunneling current constant. In this mode, a feedback control circuit adjusts the voltage applied to a piezoelectric actuator in the STM that adjusts the height of the STM tip to keep the tunneling current constant. The exponential relationship between the tunneling current and tip-to-sample distance makes it relatively easy to implement this mode of operation. The choice of method by which the photoenhanced portion of the tunneling current would be measured depends on choice of the frequency at which the input illumination would be modulated (chopped). If the frequency of modulation were low enough (typically < 10 Hz) that the feedback circuit could respond, then the voltage applied to the piezoelectric tip-height actuator could be measured by use of a lock-in amplifier locked to the modulation (chopping) signal. However, at a high modulation frequency (typically in the kilohertz range or higher), the feedback circuit would be unable to respond. In this case, the photoenhanced portion of the tunneling current could be measured directly. For this purpose, the tunneling current would be passed through a precise resistor and the voltage drop would be measured by use of the lock-in amplifier.

Bailey, Sheila↗
NASA NTRS1998

Analysis of a Memory Device Failure

The recent failure of a vintage memory device presented a unique challenge to failure analysts. Normally device layouts, fabrication parameters and other technical information were available to assist the analyst in the analysis. However, this device was out of production for many years and the manufacturer was no longer in business, so the information was not available. To further complicate this analysis, the package leads were all but removed making additional electrical testing difficult. Under these conditions, new and innovative methods were used to analyze the failure. The external visual exam, radiography, PIND, and leak testing were performed with nominal results. Since electrical testing was precluded by the short lead lengths, the device was delidded to expose the internal structures for microscopic examination. No failure mechanism was identified. The available electrical data suggested an ESD or low level EOS type mechanism which left no visible surface damage. Due to parallel electrical paths, electrical probing on the chip failed to locate the failure site. Two non-destructive Scanning Electron Microscopy techniques, CIVA (Charge Induced Voltage Alteration) and EBIC (Electron Beam Induced Current), and a liquid crystal decoration technique which detects localized heating were employed to aid in the analysis. CIVA and EBIC isolated two faults in the input circuitry, and the liquid crystal technique further localized two hot spots in regions on two input gates. Removal of the glassivation and metallization revealed multiple failure sites located in the gate oxide of two input transistors suggesting machine (testing) induced damage.

Nicolas, David P.↗
DOE OSTI2024

On-demand nanoengineering of in-plane ferroelectric topologies

Hierarchical assemblies of ferroelectric nanodomains, so-called super-domains, can exhibit exotic morphologies that lead to distinct behaviours. Controlling these super-domains reliably is critical for realizing states with desired functional properties. Here we reveal the super-switching mechanism by using a biased atomic force microscopy tip, that is, the switching of the in-plane super-domains, of a model ferroelectric Pb 0.6 Sr 0.4 TiO 3 . We demonstrate that the writing process is dominated by a super-domain nucleation and stabilization process. A complex scanning-probe trajectory enables on-demand formation of intricate centre-divergent, centre-convergent and flux-closure polar structures. Correlative piezoresponse force microscopy and optical spectroscopy confirm the topological nature and tunability of the emergent structures. The precise and versatile nanolithography in a ferroic material and the stability of the generated structures, also validated by phase-field modelling, suggests potential for reliable multi-state nanodevice architectures and, thereby, an alternative route for the creation of tunable topological structures for applications in neuromorphic circuits.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2026

Impacts of A‐Site Composition on the Cation Dissolution‐Mediated Surface Restructuring of Layered Nickelate Oxide Electrocatalysts During Alkaline Oxygen Evolution Reaction

The oxygen evolution reaction (OER) is a key anodic counter‐reaction for electrochemical production of fuels and chemicals. It is hindered by sluggish four‐electron transfer kinetics requiring highly oxidative operating potentials to achieve commercially relevant rates. NiFeO x H y electrocatalysts are among the most promising for OER in alkaline electrolytes. The Ni(OH) 2 /NiOOH redox couple has been reported as the active phase in Ni‐based electrocatalysts; however, its activity is often hindered by deactivation arising from the formation of OER‐inactive insulating species. Limited strategies exist for mitigating this deactivation. This study aims to address this by interrogating the evolution of OER active sites as a function of precatalyst composition and structural properties using a series of layered, crystalline Ni‐based Ruddlesden–Popper (RP) oxides (A 2 NiO 4+δ ). In situ evolution of the active NiO x H y surface is probed through Ni‐site OER turnover frequency analysis, and electrochemical impedance spectroscopy coupled with scanning transmission electron microscopy. We show that the stability of layered nickelate oxide electrocatalysts is governed by the dynamic competition between cation dissolution and Ni‐site reversibility, which can be tuned through the A‐site composition of RP oxides. These findings yield insights toward engineering OER oxide precatalysts that optimize the stability of in situ‐generated OER active phases.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2024

Atomic resolution scanning transmission electron microscopy at liquid helium temperatures for quantum materials

Fundamental quantum phenomena in condensed matter, ranging from correlated electron systems to quantum information processors, manifest their emergent characteristics and behaviors predominantly at low temperatures. This necessitates the use of liquid helium (LHe) cooling for experimental observation. Atomic resolution scanning transmission electron microscopy combined with LHe cooling (cryo-STEM) provides a powerful characterization technique to probe local atomic structural modulations and their coupling with charge, spin and orbital degrees-of-freedom in quantum materials. However, achieving atomic resolution in cryo-STEM is exceptionally challenging, primarily due to sample drifts arising from temperature changes and noises associated with LHe bubbling, turbulent gas flow, etc. In this work, we demonstrate atomic resolution cryo-STEM imaging at LHe temperatures using a commercial side-entry LHe cooling holder. Firstly, we examine STEM imaging performance as a function of He gas flow rate, identifying two primary noise sources: He-gas pulsing and He-gas bubbling. Secondly, we propose two strategies to achieve low noise conditions for atomic resolution STEM imaging: either by temporarily suppressing He gas flow rate using the needle valve or by acquiring images during the natural warming process. Lastly, we show the applications of image acquisition methods and image processing techniques in investigating structural phase transitions in Cr 2 Ge 2 Te 6 , CuIr 2 S 4 , and CrCl 3 . In conclusion, our findings represent an advance in the field of atomic resolution electron microscopy imaging for quantum materials and devices at LHe temperatures, which can be applied to other commercial side-entry LHe cooling TEM holders.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Experimental study of energy-dependent angular broadening of MeV electron beams for high-resolution imaging in thick samples

In scanning transmission electron microscopy (STEM), spatial resolution is primarily influenced by the projected size of the electron probe within the specimen. In thin samples, a large semi-convergence angle enables a tightly focused beam and sub-nanometer resolution. However, in thick specimens, resolution is fundamentally limited by transverse beam broadening from multiple large-angle scattering events—for example, a probe with 10 mrad angular divergence can broaden by ∼100 nm over a 10 μm path. Since this broadening scales inversely with beam energy, MeV-STEM offers a promising route for high-resolution imaging in thick materials. To quantitatively assess this effect, we performed high-precision measurements at UCLA’s PEGASUS beamline, characterizing beam divergence and intensity profiles for 3–8 MeV electrons transmitted through a wedged-silicon sample of varying thickness. Our results reconcile discrepancies among analytical models and validate Monte Carlo simulations. Here, we find that increasing beam energy from 3.0 to 5.8 MeV reduces angular broadening by a factor of 2.6, with diminishing returns observed at 7.6 MeV. These findings provide a quantitative framework for optimizing MeV-STEM parameters in high-resolution imaging of thick biological and microelectronic specimens, and for guiding beam energy selection in other advanced imaging modes beyond STEM.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Interface instabilities in hafnium hydride entrained iron metal matrix composites

The chemical interactions in Fe–HfH 2 metal matrix composites (MMCs) are studied across multiple length scales to elucidate the decomposition of the parent phases and corresponding reaction zone physics during direct current sintering. Fe–HfH 2 composites were synthesized with increasing as-mixed hydride contents of Fe–25% HfH 2 , Fe–40% HfH 2 , Fe–55% HfH 2 , and Fe–70% HfH 2 (all in vol. %) to demonstrate the ability to achieve sintered MMCs with target hydride contents. Samples were probed across multiple length scales through a multi-modal workflow employing x-ray diffraction, scanning electron microscopy and segmentation analysis, and synchrotron techniques including hard x-ray fluorescence mapping and nanoprobe x-ray absorption near-edge structure measurements. Under the selected sintering temperature and pressure conditions, hydrogen evolution is seen to evolve through parallel paths: thermal decomposition from during the transformation of HfH 2 to HfH x<2 and through subsequent reaction with the Fe matrix leading to intermetallic phase formation. Specifically, HfFe and HfFe 2 intermetallic formation accelerates the release of hydrogen with a subsequent HfO 2 phase forming at grain boundaries. For this MMC, the consumption or loss of hydrogen can be considerable in compacts with initial hydride loading of 25%–40% HfH 2 approaching 83% hydrogen loss for the lower volume fraction composites. Increasing the volume fraction of HfH 2 to 70% enhanced the retained hydrogen content to 53% and attributed to the reduced interfacial area intrinsic to the increased HfH 2 loading in this MMC.

36 MATERIALS SCIENCE↗