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At least 973 records · Page 54

Investigating electrochemical corrosion at Mg alloy-steel joint interface using scanning electrochemical cell impedance microscopy (SECCIM)

Developing strategies to prevent corrosion at the interface of dissimilar metal alloys is challenging because of the presence of heterogenous distribution of galvanic couples and microstructural features that significantly change the corrosion rate. Devising strategies to mitigate this interfacial corrosion requires quantitative and correlative understanding of its surface electrochemical reaction. In this work, scanning electrochemical cell impedance microscopy (SECCIM) was employed to study location-specific corrosion in the interfacial region of dissimilar alloys, such as AZ31 (magnesium alloy) and DP590 (steel) welded using the Friction-stir Assisted Scribe Technique (FAST) processes. Herein, SECCM and SECCIM were used to perform correlative mapping of the local electrochemical impedance spectroscopic and potentiodynamic polarization to measure the effect of electronic and microstructural changes in the welded interfacial region on corrosion kinetics. Microstructural characterization including scanning electron microscopy and electron backscatter diffraction was performed to correlate changes in microstructural features and chemistry with the corresponding electronic properties that affect corrosion behavior. The variations in corrosion potential, corrosion current density, and electrochemical impedance spectroscopy behavior across the interface provide deeper insights on the interfacial region—which is chemically and microstructurally distinct from both bare AZ31 and DP590 that can help prevent corrosion in dissimilar metal structures.

59 BASIC BIOLOGICAL SCIENCES↗

Probing topological quantum matter with scanning tunnelling microscopy

The search for topological phases of matter is evolving towards strongly interacting systems, including magnets and superconductors, where exotic effects emerge from the quantum-level interplay between geometry, correlation and topology. Over the past decade or so, scanning tunnelling microscopy has become a powerful tool to probe and discover emergent topological matter, because of its unprecedented spatial resolution, high-precision electronic detection and magnetic tunability. Scanning tunnelling microscopy can be used to probe various topological phenomena, as well as complement results from other techniques. We discuss some of these proof-of-principle methodologies applied to probe topology, with particular attention to studies performed under a tunable vector magnetic field, which is a relatively new direction of recent focus. Finally, we then project the future possibilities for atomic-resolution tunnelling methods in providing new insights into topological matter.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Scanning photoelectron microscope for nanoscale three-dimensional spatial-resolved electron spectroscopy for chemical analysis

In order to achieve nondestructive observation of the three-dimensional spatially resolved electronic structure of solids, we have developed a scanning photoelectron microscope system with the capability of depth profiling in electron spectroscopy for chemical analysis (ESCA). We call this system 3D nano-ESCA. For focusing the x-ray, a Fresnel zone plate with a diameter of 200 {mu}m and an outermost zone width of 35 nm is used. In order to obtain the angular dependence of the photoelectron spectra for the depth-profile analysis without rotating the sample, we adopted a modified VG Scienta R3000 analyzer with an acceptance angle of 60 deg. as a high-resolution angle-resolved electron spectrometer. The system has been installed at the University-of-Tokyo Materials Science Outstation beamline, BL07LSU, at SPring-8. From the results of the line-scan profiles of the poly-Si/high-k gate patterns, we achieved a total spatial resolution better than 70 nm. The capability of our system for pinpoint depth-profile analysis and high-resolution chemical state analysis is demonstrated.

36 MATERIALS SCIENCE↗

Size dependent bandgap of molecular beam epitaxy grown InN quantum dots measured by scanning tunneling spectroscopy

InN quantum dots (QDs) were grown on Si (111) by epitaxial Stranski-Krastanow growth mode using plasma-assisted molecular beam epitaxy. Single-crystalline wurtzite structure of InN QDs was verified by the x-ray diffraction and transmission electron microscopy. Scanning tunneling microscopy has been used to probe the structural aspects of QDs. A surface bandgap of InN QDs was estimated from scanning tunneling spectroscopy (STS) I-V curves and found that it is strongly dependent on the size of QDs. The observed size-dependent STS bandgap energy shifts with diameter and height were theoretical explained based on an effective mass approximation with finite-depth square-well potential model.

36 MATERIALS SCIENCE↗

Measurement of Semiconductor Surface Potential using the Scanning Electron Microscope

We calibrate the secondary electron signal from a standard scanning electron microscope to voltage, yielding an image of the surface or near-surface potential. Data on both atomically abrupt heterojunction GaInP/GaAs and diffused homojunction Si solar cell devices clearly show the expected variation in potential with position and applied bias, giving depletion widths and locating metallurgical junctions to an accuracy better than 10 nm. In some images, distortion near the p-n junction is observed, seemingly consistent with the effects of lateral electric fields (patch fields). Reducing the tube bias removes this distortion. This approach results in rapid and straightforward collection of near-surface potential data using a standard scanning electron microscope.

14 SOLAR ENERGY↗

The material dependence of temperature measurement resolution in thermal scanning electron microscopy

Thermal scanning electron microscopy is a recently developed temperature mapping technique based on thermal diffuse scattering in electron backscatter diffraction in a scanning electron microscope. It provides nano-scale and non-contact temperature mapping capabilities. Due to the specific temperature sensitive mechanism inherent to this technique, the temperature resolution is highly material dependent. A thorough investigation of what material properties affect the temperature resolution is important for realizing the inherent temperature resolution limit for each material. In this paper, three material dependent parameters-the Debye-Waller B-factor temperature sensitivity, backscatter yield, and lattice constant-are shown to control the temperature resolution.

36 MATERIALS SCIENCE↗

Atomic resolution scanning tunneling microscopy in a cryogen free dilution refrigerator at 15 mK

Pulse tube refrigerators are becoming more common, because they are cost efficient and demand less handling than conventional (wet) refrigerators. However, a downside of a pulse tube system is the vibration level at the cold-head, which is in most designs several micrometers. We implemented vibration isolation techniques which significantly reduced vibration levels at the experiment. These optimizations were necessary for the vibration sensitive magnetic resonance force microscopy experiments at milli-kelvin temperatures for which the cryostat is intended. With these modifications we show atomic resolution scanning tunneling microscopy on graphite. This is promising for scanning probe microscopy applications at very low temperatures.

42 ENGINEERING↗

Imaging of buried phosphorus nanostructures in silicon using scanning tunneling microscopy

We demonstrate the locating and imaging of single phosphorus atoms and phosphorus dopant nanostructures, buried beneath the Si(001) surface using scanning tunneling microscopy. The buried dopant nanostructures have been fabricated in a bottom-up approach using scanning tunneling microscope lithography on Si(001). We find that current imaging tunneling spectroscopy is suited to locate and image buried nanostructures at room temperature and with residual surface roughness present. From these studies, we can place an upper limit on the lateral diffusion during encapsulation with low-temperature Si molecular beam epitaxy.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Plasma etching of superconducting Niobium tips for scanning tunneling microscopy

We have developed a reproducible technique for the fabrication of sharp superconducting Nb tips for scanning tunneling microscopy (STM) and scanning tunneling spectroscopy. Sections of Nb wire with 250 μm diameter are dry etched in an SF₆ plasma in a Reactive Ion Etcher. The gas pressure, etching time, and applied power are chosen to control the ratio of isotropic to anisotropic etch rates and produce the desired tip shape. The resulting tips are atomically sharp, with radii of less than 100 nm, mechanically stable, and superconducting. They generate good STM images and spectroscopy on single crystal samples of Au(111), Au(100), and Nb(100), as well as a doped topological insulator Bi₂Se₃ at temperatures ranging from 30 mK to 9 K.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Phase modulation mode of scanning ion conductance microscopy

This Letter reports a phase modulation (PM) mode of scanning ion conductance microscopy. In this mode, an AC current is directly generated by an AC voltage between the electrodes. The portion of the AC current in phase with the AC voltage, which is the current through the resistance path, is modulated by the tip-sample distance. It can be used as the input of feedback control to drive the scanner in Z direction. The PM mode, taking the advantages of both DC mode and traditional AC mode, is less prone to electronic noise and DC drift but maintains high scanning speed. The effectiveness of the PM mode has been proven by experiments.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

High-stability cryogenic scanning tunneling microscope based on a closed-cycle cryostat

We report on the design and operation of a cryogenic ultra-high vacuum (UHV) scanning tunneling microscope (STM) coupled to a closed-cycle cryostat (CCC). The STM is thermally linked to the CCC through helium exchange gas confined inside a volume enclosed by highly flexible rubber bellows. The STM is thus mechanically decoupled from the CCC, which results in a significant reduction of the mechanical noise transferred from the CCC to the STM. Noise analysis of the tunneling current shows current fluctuations up to 4% of the total current, which translates into tip-sample distance variations of up to 1.5 picometers. This noise level is sufficiently low for atomic-resolution imaging of a wide variety of surfaces. To demonstrate this, atomic-resolution images of Au(111) and NaCl(100)/Au(111) surfaces, as well as of carbon nanotubes deposited on Au(111), were obtained. Thermal drift analysis showed that under optimized conditions, the lateral stability of the STM scanner can be as low as 0.18 Å/h. Scanning Tunneling Spectroscopy measurements based on the lock-in technique were also carried out, and showed no detectable presence of noise from the closed-cycle cryostat. Using this cooling approach, temperatures as low as 16 K at the STM scanner have been achieved, with the complete cool-down of the system typically taking up to 12 h. These results demonstrate that the constructed CCC-coupled STM is a highly stable instrument capable of highly detailed spectroscopic investigations of materials and surfaces at the atomic scale.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Novel scanning electron microscope bulge test technique integrated with loading function

Membranes and film-on-substrate structures are critical elements for some devices in electronics industry and for Micro Electro Mechanical Systems devices. These structures are normally at the scale of micrometer or even nanometer. Thus, the measurement for the mechanical property of these membranes poses a challenge over the conventional measurements at macro-scales. In this study, a novel bulge test method is presented for the evaluation of mechanical property of micro thin membranes. Three aspects are discussed in the study: (a) A novel bulge test with a Scanning Electron Microscope system realizing the function of loading and measuring simultaneously; (b) a simplified Digital Image Correlation method for a height measurement; and (c) an imaging distortion correction by the introduction of a scanning Moiré method. Combined with the above techniques, biaxial modulus as well as Young's modulus of the polyimide film can be determined. Besides, a standard tensile test is conducted as an auxiliary experiment to validate the feasibility of the proposed method.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Investigation of surface defect states in CeO{sub 2-y} nanocrystals by Scanning−tunneling microscopy/spectroscopy and ellipsometry

Synthesis process strongly influences the nanocrystalline CeO{sub 2-y} defective structure. The presence of surface defects, in the form of oxygen vacancies in different charge states (F centers), can change the electronic properties of ceria nanocrystals. Nanocrystalline CeO{sub 2-y} samples were synthesized using three different methods (precipitation, self-propagating room temperature, and hydrothermal synthesis). Raman spectroscopy was used to identify the presence of oxygen vacancies which presumably were formed at the nanoparticle surface. The defect concentration depended on the crystallite size of differently prepared CeO{sub 2-y} samples. Scanning tunneling microscopy/spectroscopy and ellipsometry were employed to investigate the electronic band structure of defective CeO{sub 2-y} nanocrystals. Scanning tunneling spectroscopy measurements demonstrated that inside the band gap of CeO{sub 2-y} nanocrystals, besides the filled 4 f states, appeared additional states which were related to occupied and empty F center defect states. From the ellipsometric measurements, using the critical points model, the energy positions of different F centers states and the values of the reduced band gap energies were determined. The analysis of obtained data pointed out that depending on the synthesis method, different types of F centers (F{sup +} and F{sup 0}) can be formed in the CeO{sub 2-y} nanocrystals. The formation of different F center defect states inside the ceria gap have a strong impact on the electrical, optical, and magnetic properties of ceria nanocrystals.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

Three axis vector magnet set-up for cryogenic scanning probe microscopy

We describe a three axis vector magnet system for cryogenic scanning probe microscopy measurements. We discuss the magnet support system and the power supply, consisting of a compact three way 100 A current source. We obtain tilted magnetic fields in all directions with maximum value of 5T along z-axis and of 1.2T for XY-plane magnetic fields. We describe a scanning tunneling microscopy-spectroscopy (STM-STS) set-up, operating in a dilution refrigerator, which includes a new high voltage ultralow noise piezodrive electronics and discuss the noise level due to vibrations. STM images and STS maps show atomic resolution and the tilted vortex lattice at 150 mK in the superconductor β-Bi{sub 2}Pd. We observe a strongly elongated hexagonal lattice, which corresponds to the projection of the tilted hexagonal vortex lattice on the surface. We also discuss Magnetic Force Microscopy images in a variable temperature insert.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Atomic-scale electrochemistry on the surface of a manganite

The doped manganese oxides (manganites) have been widely studied for their colossal magnetoresistive effects, for potential applications in oxide spintronics, electroforming in resistive switching devices, and are materials of choice as cathodes in modern solid oxide fuel cells. However, little experimental knowledge of the dynamics of the surfaces of perovskite manganites at the atomic scale exists. Here, through in-situ scanning tunnelling microscopy (STM), we demonstrate atomic resolution on samples of La 0.625 Ca 0.375 MnO 3 grown on (001) SrTiO 3 by pulsed laser deposition (PLD). Furthermore, by applying triangular DC waveforms of increasing amplitude to the STM tip, and measuring the tunnelling current, we demonstrate the ability to both perform and monitor surface electrochemical processes at the atomic level, including, for the first time in a manganite, formation of single and multiple oxygen vacancies, disruption of the overlying manganite layers, and removal and deposition of individual atomic units or clusters. Our work paves the way for better understanding of surface oxygen reactions in these systems.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Influence of mechanical noise inside a scanning electron microscope

The scanning electron microscope is becoming a popular tool to perform tasks that require positioning, manipulation, characterization, and assembly of micro-components. However, some of these applications require a higher level of performance with respect to dynamics and precision of positioning. One limiting factor is the presence of unidentified noises and disturbances. This work aims to study the influence of mechanical disturbances generated by the environment and by the microscope, identifying how these can affect elements in the vacuum chamber. To achieve this objective, a dedicated setup, including a high-resolution vibrometer, was built inside the microscope. This work led to the identification and quantification of main disturbances and noise sources acting on a scanning electron microscope. Furthermore, the effects of external acoustic excitations were analysed. Potential applications of these results include noise compensation and real-time control for high accuracy tasks.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Surface characterization of InP trenches embedded in oxide using scanning probe microscopy

Metrology for structural and electrical analyses at device level has been identified as one of the major challenges to be resolved for the sub-14 nm technology nodes. In these advanced nodes, new high mobility semiconductors, such as III–V compounds, are grown in narrow trenches on a Si substrate. Probing the nature of the defects, the defect density, and the role of processing steps on the surface of such structures are prime metrology requirements. In order to enable defect analysis on a (III–V) surface, a proper sample preparation for oxide removal is of primary importance. In this work, the effectiveness of different chemical cleanings and thermal annealing procedures is investigated on both blanket InP and oxide embedded InP trenches by means of scanning probe microscopy techniques. It is found that the most effective approach is a combination of an HCl-based chemical cleaning combined with a low-temperature thermal annealing leading to an oxide free surface with atomically flat areas. Scanning tunneling microscopy (STM) has been the preferred method for such investigations on blanket films due to its intrinsic sub-nm spatial resolution. However, its application on oxide embedded structures is non-trivial. To perform STM on the trenches of interest (generally <20 nm wide), we propose a combination of non-contact atomic force microscopy and STM using the same conductive atomic force microscopy tip Our results prove that with these procedures, it is possible to perform STM in narrow InP trenches showing stacking faults and surface reconstruction. Significant differences in terms of roughness and terrace formation are also observed between the blanket and the oxide embedded InP.

36 MATERIALS SCIENCE↗

Spin-polarized scanning tunneling microscopy experiments on the rough surface of a polycrystalline NiFe film with a fine magnetic tip sensitive to a well-defined magnetization component

We developed a micrometer-sized magnetic tip integrated onto the write head of a hard disk drive for spin-polarized scanning tunneling microscopy (SP-STM) in the modulated tip magnetization mode. Using SP-STM, we measured a well-defined in-plane spin-component of the tunneling current of the rough surface of a polycrystalline NiFe film. The spin asymmetry of the NiFe film was about 1.3% within the bias voltage range of -3 to 1 V. We obtained the local spin component image of the sample surface, switching the magnetic field of the sample to reverse the sample magnetization during scanning. We also obtained a spin image of the rough surface of a polycrystalline NiFe film evaporated on the recording medium of a hard disk drive.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗