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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 1,585 records · Page 88
All sourcesNASA NTRSDOE OSTI
DOE OSTI2014

The ReactorSTM: Atomically resolved scanning tunneling microscopy under high-pressure, high-temperature catalytic reaction conditions

To enable atomic-scale observations of model catalysts under conditions approaching those used by the chemical industry, we have developed a second generation, high-pressure, high-temperature scanning tunneling microscope (STM): the ReactorSTM. It consists of a compact STM scanner, of which the tip extends into a 0.5 ml reactor flow-cell, that is housed in a ultra-high vacuum (UHV) system. The STM can be operated from UHV to 6 bars and from room temperature up to 600 K. A gas mixing and analysis system optimized for fast response times allows us to directly correlate the surface structure observed by STM with reactivity measurements from a mass spectrometer. The in situ STM experiments can be combined with ex situ UHV sample preparation and analysis techniques, including ion bombardment, thin film deposition, low-energy electron diffraction and x-ray photoelectron spectroscopy. The performance of the instrument is demonstrated by atomically resolved images of Au(111) and atom-row resolution on Pt(110), both under high-pressure and high-temperature conditions.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
DOE OSTI2014

Scanning tunneling microscopy/spectroscopy of picene thin films formed on Ag(111)

Using ultrahigh-vacuum low-temperature scanning tunneling microscopy and spectroscopy combined with first principles density functional theory calculations, we have investigated structural and electronic properties of pristine and potassium (K)-deposited picene thin films formed in situ on a Ag(111) substrate. At low coverages, the molecules are uniformly distributed with the long axis aligned along the [112{sup ¯}] direction of the substrate. At higher coverages, ordered structures composed of monolayer molecules are observed, one of which is a monolayer with tilted and flat-lying molecules resembling a (11{sup ¯}0) plane of the bulk crystalline picene. Between the molecules and the substrate, the van der Waals interaction is dominant with negligible hybridization between their electronic states; a conclusion that contrasts with the chemisorption exhibited by pentacene molecules on the same substrate. We also observed a monolayer picene thin film in which all molecules were standing to form an intermolecular π stacking. Two-dimensional delocalized electronic states are found on the K-deposited π stacking structure.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2014

Characterization of gold nanoparticle films: Rutherford backscattering spectroscopy, scanning electron microscopy with image analysis, and atomic force microscopy

Gold nanoparticle films are of interest in several branches of science and technology, and accurate sample characterization is needed but technically demanding. We prepared such films by DC magnetron sputtering and recorded their mass thickness by Rutherford backscattering spectroscopy. The geometric thickness d{sub g}—from the substrate to the tops of the nanoparticles—was obtained by scanning electron microscopy (SEM) combined with image analysis as well as by atomic force microscopy (AFM). The various techniques yielded an internally consistent characterization of the films. In particular, very similar results for d{sub g} were obtained by SEM with image analysis and by AFM.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Copper intercalation at the interface of graphene and Ir(111) studied by scanning tunneling microscopy

We report on the intercalation of a submonolayer of copper at 775 K underneath graphene epitaxially grown on Ir(111) studied by means of low energy electron diffraction (LEED) and scanning tunneling microscopy (STM) at 77 K. Nucleation and growth dynamics of Cu below graphene have been investigated, and, most importantly, the intercalation mechanism has been identified. First, LEED patterns reveal the pseudomorphic growth of Cu on Ir under the topmost graphene layer resulting in a large Cu in-plane lattice parameter expansion of about 6% compared to Cu(111). Second, large-scale STM topographs as a function of Cu coverage show that Cu diffusion on Ir below graphene exhibits a low energy barrier resulting in Cu accumulation at Ir step edges. As a result, the graphene sheet undergoes a strong edges reshaping. Finally, atomically-resolved STM images reveal a damaged graphene sheet at the atomic scale after metal intercalation. Point defects in graphene were shown to be carbon vacancies. According to these results, a Cu penetration path beneath graphene is proposed to occur via metal aided defect formation with no or poor self healing of the graphene sheet. This work illustrates the fact that Cu intercalation is harmful for graphene grown on Ir(111) at the atomic scale.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Direct observation and analysis of yolk-shell materials using low-voltage high-resolution scanning electron microscopy: Nanometal-particles encapsulated in metal-oxide, carbon, and polymer

Nanometal particles show characteristic features in chemical and physical properties depending on their sizes and shapes. For keeping and further enhancing their features, the particles should be protected from coalescence or degradation. One approach is to encapsulate the nanometal particles inside pores with chemically inert or functional materials, such as carbon, polymer, and metal oxides, which contain mesopores to allow permeation of only chemicals not the nanometal particles. Recently developed low-voltage high-resolution scanning electron microscopy was applied to the study of structural, chemical, and electron state of both nanometal particles and encapsulating materials in yolk-shell materials of Au@C, Ru/Pt@C, Au@TiO{sub 2}, and Pt@Polymer. Progresses in the following categories were shown for the yolk-shell materials: (i) resolution of topographic image contrast by secondary electrons, of atomic-number contrast by back-scattered electrons, and of elemental mapping by X-ray energy dispersive spectroscopy; (ii) sample preparation for observing internal structures; and (iii) X-ray spectroscopy such as soft X-ray emission spectroscopy. Transmission electron microscopy was also used for characterization of Au@C.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Invited Article: Autonomous assembly of atomically perfect nanostructures using a scanning tunneling microscope

A major goal of nanotechnology is to develop the capability to arrange matter at will by placing individual atoms at desired locations in a predetermined configuration to build a nanostructure with specific properties or function. The scanning tunneling microscope has demonstrated the ability to arrange the basic building blocks of matter, single atoms, in two-dimensional configurations. An array of various nanostructures has been assembled, which display the quantum mechanics of quantum confined geometries. The level of human interaction needed to physically locate the atom and bring it to the desired location limits this atom assembly technology. Here we report the use of autonomous atom assembly via path planning technology; this allows atomically perfect nanostructures to be assembled without the need for human intervention, resulting in precise constructions in shorter times. We demonstrate autonomous assembly by assembling various quantum confinement geometries using atoms and molecules and describe the benefits of this approach.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
DOE OSTI2014

Monitoring Si growth on Ag(111) with scanning tunneling microscopy reveals that silicene structure involves silver atoms

Using scanning tunneling microscopy (STM), the elaboration of the so-called silicene layer on Ag(111) is monitored in real time during Si evaporation at different temperatures. It is shown that the growth of silicene is accompanied by the release of about 65% of the surface Ag atoms from the Si covered areas. We observe that Si islands develop on the Ag terraces and Si strips at the Ag step edges, progressively forming ordered (4×4), (√(13)×√(13)) R13.9°, and dotted phases. Meanwhile, displaced Ag atoms group to develop additional bare Ag terraces growing round the Si islands from the pristine Ag step edges. This indicates a strong interaction between Si and Ag atoms, with an important modification of the Ag substrate beneath the surface layer. This observation is in contradiction with the picture of a silicene layer weakly interacting with the unreconstructed Ag substrate, and strongly indicates that the structure of silicene on Ag(111) corresponds either to a Si-Ag surface alloy or to a Si plane covered with Ag atoms.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
DOE OSTI2014

A high stability and repeatability electrochemical scanning tunneling microscope

We present a home built electrochemical scanning tunneling microscope (ECSTM) with very high stability and repeatability. Its coarse approach is driven by a closely stacked piezo motor of GeckoDrive type with four rigid clamping points, which enhances the rigidity, compactness, and stability greatly. It can give high clarity atomic resolution images without sound and vibration isolations. Its drifting rates in XY and Z directions in solution are as low as 84 pm/min and 59 pm/min, respectively. In addition, repeatable coarse approaches in solution within 2 mm travel distance show a lateral deviation less than 50 nm. The gas environment can be well controlled to lower the evaporation rate of the cell, thus reducing the contamination and elongating the measurement time. Atomically resolved SO{sub 4}{sup 2−} image on Au (111) work electrode is demonstrated to show the performance of the ECSTM.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
DOE OSTI2015

Correction of absorption-edge artifacts in polychromatic X-ray tomography in a scanning electron microscope for 3D microelectronics

X-ray tomography is widely used in materials science. However, X-ray scanners are often based on polychromatic radiation that creates artifacts such as dark streaks. We show this artifact is not always due to beam hardening. It may appear when scanning samples with high-Z elements inside a low-Z matrix because of the high-Z element absorption edge: X-rays whose energy is above this edge are strongly absorbed, violating the exponential decay assumption for reconstruction algorithms and generating dark streaks. A method is proposed to limit the absorption edge effect and is applied on a microelectronic case to suppress dark streaks between interconnections.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
DOE OSTI2015

A nanoscale gigahertz source realized with Josephson scanning tunneling microscopy

Using the AC Josephson effect in the superconductor-vacuum-superconductor tunnel junction of a scanning tunneling microscope (STM), we demonstrate the generation of GHz radiation. With the macroscopic STM tip acting as a λ/4-monopole antenna, we first show that the atomic scale Josephson junction in the STM is sensitive to its frequency-dependent environmental impedance in the GHz regime. Further, enhancing Cooper pair tunneling via excitations of the tip eigenmodes, we are able to generate high-frequency radiation. We find that for vanadium junctions, the enhanced photon emission can be tuned from about 25 GHz to 200 GHz and that large photon flux in excess of 10{sup 20 }cm{sup −2} s{sup −1} is reached in the tunnel junction. These findings demonstrate that the atomic scale Josephson junction in an STM can be employed as a full spectroscopic tool for GHz frequencies on the atomic scale.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2015

Large area strain analysis using scanning transmission electron microscopy across multiple images

Here, we apply revolving scanning transmission electron microscopy to measure lattice strain across a sample using a single reference area. To do so, we remove image distortion introduced by sample drift, which usually restricts strain analysis to a single image. Overcoming this challenge, we show that it is possible to use strain reference areas elsewhere in the sample, thereby enabling reliable strain mapping across large areas. As a prototypical example, we determine the strain present within the microstructure of a Ni-based superalloy directly from atom column positions as well as geometric phase analysis. While maintaining atomic resolution, we quantify strain within nanoscale regions and demonstrate that large, unit-cell level strain fluctuations are present within the intermetallic phase.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
DOE OSTI2015

Observation of nonlinear bands in near-field scanning optical microscopy of a photonic-crystal waveguide

We have measured the photonic bandstructure of GaAs photonic-crystal waveguides with high resolution in energy as well as in momentum using near-field scanning optical microscopy. Intriguingly, we observe additional bands that are not predicted by eigenmode solvers, as was recently demonstrated by Huisman et al. [Phys. Rev. B 86, 155154 (2012)]. We study the presence of these additional bands by performing measurements of these bands while varying the incident light power, revealing a non-linear power dependence. Here, we demonstrate experimentally and theoretically that the observed additional bands are caused by a waveguide-specific near-field tip effect not previously reported, which can significantly phase-modulate the detected field.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2015

Note: Fabrication and characterization of molybdenum tips for scanning tunneling microscopy and spectroscopy

We present a method for the preparation of bulk molybdenum tips for Scanning Tunneling Microscopy and Spectroscopy and we assess their potential in performing high resolution imaging and local spectroscopy by measurements on different single crystal surfaces in UHV, namely, Au(111), Si(111)-7 × 7, and titanium oxide 2D ordered nanostructures supported on Au(111). The fabrication method is versatile and can be extended to other metals, e.g., cobalt.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
DOE OSTI2015

Temperature dependence of the superconducting proximity effect quantified by scanning tunneling spectroscopy

Here, we present the first systematic study on the temperature dependence of the extension of the superconducting proximity effect in a 1–2 atomic layer thin metallic film, surrounding a superconducting Pb island. Scanning tunneling microscopy/spectroscopy (STM/STS) measurements reveal the spatial variation of the local density of state on the film from 0.38 up to 1.8 K. In this temperature range the superconductivity of the island is almost unaffected and shows a constant gap of a 1.20 ± 0.03 meV. Using a superconducting Nb-tip a constant value of the proximity length of 17 ± 3 nm at 0.38 and 1.8 K is found. In contrast, experiments with a normal conductive W-tip indicate an apparent decrease of the proximity length with increasing temperature. This result is ascribed to the thermal broadening of the occupation of states of the tip, and it does not reflect an intrinsic temperature dependence of the proximity length. Our tunneling spectroscopy experiments shed fresh light on the fundamental issue of the temperature dependence of the proximity effect for atomic monolayers, where the intrinsic temperature dependence of the proximity effect is comparably weak.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Non-thermal plasma mills bacteria: Scanning electron microscopy observations

Non-thermal plasmas hold great promise for a variety of biomedical applications. To ensure safe clinical application of plasma, a rigorous analysis of plasma-induced effects on cell functions is required. Yet mechanisms of bacteria deactivation by non-thermal plasma remain largely unknown. We therefore analyzed the influence of low-temperature atmospheric plasma on Gram-positive and Gram-negative bacteria. Using scanning electron microscopy, we demonstrate that both Gram-positive and Gram-negative bacteria strains in a minute were completely destroyed by helium plasma. In contrast, mesenchymal stem cells (MSCs) were not affected by the same treatment. Furthermore, histopathological analysis of hematoxylin and eosin–stained rat skin sections from plasma–treated animals did not reveal any abnormalities in comparison to control ones. We discuss possible physical mechanisms leading to the shred of bacteria under non-thermal plasma irradiation. Our findings disclose how helium plasma destroys bacteria and demonstrates the safe use of plasma treatment for MSCs and skin cells, highlighting the favorability of plasma applications for chronic wound therapy.

60 APPLIED LIFE SCIENCES↗
DOE OSTI2015

Note: Advancement in tip etching for preparation of tunable size scanning tunneling microscopy tips

The two aspects of a scanning tunneling microscopy tip, the macroscopic profile and the nanoscale apex, can be tailored by controlling the tension during electrochemical etching and the solution-electrode contact area via acetone vapor. The apex diameter is shown to be proportional to the square root of the tension, and is demonstrated over apex diameters of 150-500 nm. The apex was found to be created in four distinct shapes where a secondary etching can reshape the tip into a single geometry. Improvement in tip height and stability of the profile are demonstrated versus a non-acetone fabrication control.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Charge collection microscopy of in-situ switchable PRAM line cells in a scanning electron microscope: Technique development and unique observations

An imaging method has been developed based on charge collection in a scanning electron microscope (SEM) that allows discrimination between the amorphous and crystalline states of Phase-change Random Access Memory (PRAM) line cells. During imaging, the cells are electrically connected and can be switched between the states and the resistance can be measured. This allows for electrical characterization of the line cells in-situ in the SEM. Details on sample and measurement system requirements are provided which turned out to be crucial for the successful development of this method. Results show that the amorphous or crystalline state of the line cells can be readily discerned, but the spatial resolution is relatively poor. Nevertheless, it is still possible to estimate the length of the amorphous mark, and also for the first time, we could directly observe the shift of the amorphous mark from one side of the line cell to the other side when the polarity of the applied (50 ns) RESET pulse was reversed.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
DOE OSTI2015

Large area fabrication of plasmonic nanoparticle grating structure by conventional scanning electron microscope

Plasmonic nanoparticle grating (PNG) structure of different periods has been fabricated by electron beam lithography using silver halide based transmission electron microscope film as a substrate. Conventional scanning electron microscope is used as a fabrication tool for electron beam lithography. Optical microscope and energy dispersive spectroscopy (EDS) have been used for its morphological and elemental characterization. Optical characterization is performed by UV-Vis absorption spectroscopic technique.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗