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At least 37 records · Page 2

Aberration corrected 1.2-MV cold field-emission transmission electron microscope with a sub-50-pm resolution

Atomic-resolution electromagnetic field observation is critical to the development of advanced materials and to the unveiling of their fundamental physics. For this purpose, a spherical-aberration corrected 1.2-MV cold field-emission transmission electron microscope has been developed. The microscope has the following superior properties: stabilized accelerating voltage, minimized electrical and mechanical fluctuation, and coherent electron emission. These properties have enabled to obtain 43-pm information transfer. On the bases of these performances, a 43-pm resolution has been obtained by correcting lens aberrations up to the third order. Observations of GaN [411] thin crystal showed a projected atomic locations with a separation of 44 pm.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

In Situ Study of the Impact of Aberration-Corrected Electron-Beam Lithography on the Electronic Transport of Suspended Graphene Devices

The implementation of aberration-corrected electron beam lithography (AC-EBL) in a 200 keV scanning transmission electron microscope (STEM) is a novel technique that could be used for the fabrication of quantum devices based on 2D atomic crystals with single nanometer critical dimensions, allowing to observe more robust quantum effects. In this work we study electron beam sculpturing of nanostructures on suspended graphene field effect transistors using AC-EBL, focusing on the in situ characterization of the impact of electron beam exposure on device electronic transport quality. When AC-EBL is performed on a graphene channel (local exposure) or on the outside vicinity of a graphene channel (non-local exposure), the charge transport characteristics of graphene can be significantly affected due to charge doping and scattering. While the detrimental effect of non-local exposure can be largely removed by vigorous annealing, local-exposure induced damage is irreversible and cannot be fixed by annealing. We discuss the possible causes of the observed exposure effects. Our results provide guidance to the future development of high-energy electron beam lithography for nanomaterial device fabrication.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

Nanofocusing with aberration-corrected rotationally parabolic refractive X-ray lenses

Wavefront errors of rotationally parabolic refractive X-ray lenses made of beryllium (Be CRLs) have been recovered for various lens sets and X-ray beam configurations. Due to manufacturing via an embossing process, aberrations of individual lenses within the investigated ensemble are very similar. By deriving a mean single-lens deformation for the ensemble, aberrations of any arbitrary lens stack can be predicted from the ensemble with σ¯ = 0.034λ. Using these findings the expected focusing performance of current Be CRLs are modeled for relevant X-ray energies and bandwidths and it is shown that a correction of aberrations can be realised without prior lens characterization but simply based on the derived lens deformation. As a result, the performance of aberration-corrected Be CRLs is discussed and the applicability of aberration-correction demonstrated over wide X-ray energy ranges.

73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗

Investigation of focusing and correcting aberrations with binary amplitude and polarization modulation

Here, we investigate the focusing and correcting wavefront aberration of an optical wave using binary amplitude and polarization modulation. Focusing is performed by selectively modulating the field in different zones of the pupil to obtain on-axis constructive interference at a given distance. The conventional Soret zone plate (binary amplitude profile) is expanded to a polarization Soret zone plate with twice the focusing efficiency. Binary pixelated devices that approximate the sinusoidal transmission profile of a Gabor zone plate by spatial dithering are also investigated with amplitude and polarization modulation. Wavefront aberrations are corrected by modulation of the field in the pupil plane to prevent destructive interference in the focal plane of an ideal focusing element. Polarization modulation improves the efficiency obtained by amplitude-only modulation, with a gain that depends on the aberration. Experimental results obtained with Cr-on-glass devices for amplitude modulation and liquid crystal devices operating in the Mauguin condition for polarization modulation are in very good agreement with simulations.

47 OTHER INSTRUMENTATION↗

Single-Digit Nanometer Electron-Beam Lithography with an Aberration-Corrected Scanning Transmission Electron Microscope

Here, we demonstrate extension of electron-beam lithography using conventional resists and pattern transfer processes to single-digit nanometer dimensions by employing an aberration-corrected scanning transmission electron microscope as the exposure tool. Here, we present results of single-digit nanometer patterning of two widely used electron-beam resists: poly (methyl methacrylate) and hydrogen silsesquioxane. The method achieves sub-5 nanometer features in poly (methyl methacrylate) and sub-10 nanometer resolution in hydrogen silsesquioxane. High-fidelity transfer of these patterns into target materials of choice can be performed using metal lift-off, plasma etch, and resist infiltration with organometallics.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

New insights on ion track morphology in pyrochlores by aberration corrected scanning transmission electron microscopy

Here we demonstrate the enhanced imaging capabilities of an aberration corrected scanning transmission electron microscope to advance the understanding of ion track structure in pyrochlore structured materials (i.e., Gd 2 Ti 2 O 7 and Gd 2 TiZrO 7 ). Track formation occurs due to the inelastic transfer of energy from incident ions to electrons, and atomic-level details of track morphology as a function of energy-loss are revealed in the present work. A comparison of imaging details obtained by varying collection angles of detectors is discussed in the present work. A quantitative analysis of phase identification using high-angle annular dark field imaging is performed on the ion tracks. Finally, a novel 3-dimensional track reconstruction method is provided that is based on depth dependent imaging of the ion tracks. The technique is used in extracting the atomic-level details of nanoscale features, such as the disordered ion tracks, which are embedded in relatively thicker matrix. Another relevance of the method is shown by measuring the tilt of the ion tracks relative to the electron beam incidence that helps in knowing the structure and geometry of ion tracks quantitatively.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗

Nanowire growth kinetics in aberration corrected environmental transmission electron microscopy

Here, we visualize atomic level dynamics during Si nanowire growth using aberration corrected environmental transmission electron microscopy, and compare with lower pressure results from ultra-high vacuum microscopy. We discuss the importance of higher pressure observations for understanding growth mechanisms and describe protocols to minimize effects of the higher pressure background gas.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

Separating strain from composition in unit cell parameter maps obtained from aberration corrected high resolution transmission electron microscopy imaging

Based on the evaluation of lattice parameter maps in aberration corrected high resolution transmission electron microscopy images, we propose a simple method that allows quantifying the composition and disorder of a semiconductor alloy at the unit cell scale with high accuracy. This is realized by considering, next to the out-of-plane, also the in-plane lattice parameter component allowing to separate the chemical composition from the strain field. Considering only the out-of-plane lattice parameter component not only yields large deviations from the true local alloy content but also carries the risk of identifying false ordering phenomena like formations of chains or platelets. Our method is demonstrated on image simulations of relaxed supercells, as well as on experimental images of an In{sub 0.20}Ga{sub 0.80}N quantum well. Principally, our approach is applicable to all epitaxially strained compounds in the form of quantum wells, free standing islands, quantum dots, or wires.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Patterning Si at the 1 nm Length Scale with Aberration-Corrected Electron-Beam Lithography: Tuning of Plasmonic Properties by Design

Patterning of materials at single nanometer resolution allows engineering of quantum confinement effects, as these effects are significant at these length scales, and yields direct control over electro-optical properties. Silicon is by far the most important material in electronics, and the ability to fabricate Si-based devices of the smallest dimensions for novel device engineering is highly desirable. Here, the work presented here uses aberration-corrected electron-beam lithography combined with dry reactive ion etching to achieve both: patterning of 1-nm features and surface and volume plasmon engineering in Si. The nanofabrication technique employed here produces nanowires with a line edge roughness (LER) of 1 nm (3σ). In addition, this work demonstrates tuning of the Si volume plasmon energy by 1.2 eV from the bulk value, which is one order of magnitude higher than previous attempts of volume plasmon engineering using lithographic methods.

29 ENERGY PLANNING, POLICY, AND ECONOMY↗

Aberration‐Corrected Transmission Electron Microscopy and In Situ XAFS Structural Characterization of Pt/γ‐Al 2 O 3 Nanoparticles

Abstract Aberration‐corrected (AC) STEM, AC TEM and in situ X‐ray absorption fine structure spectroscopy (XAFS) were used to characterize the Pt clusters present on a 0.35 wt % Pt on γ‐alumina support after reduction in hydrogen at 700 °C. STEM high‐angle annular dark field imaging shows that cluster formation takes place at temperatures up to approximately 350 °C, and this is followed by gradual growth in cluster size for heat treatments in hydrogen up to 700 °C. The STEM data show that after 700 °C reduction the Pt clusters are present in a narrow size distribution centered at 0.88 nm, and using a method involving a redistribution of the Pt atoms using a high electron dosage in the STEM, it is shown that the clusters are present in two‐dimensional morphology. This conclusion is verified using intensity line scans. The in situ extended X‐ray absorption fine structure data are in good agreement with these observations. High‐resolution AC–TEM, which uses a broad coherent electron beam, and can thus offer advantages relative to STEM for structure determination of fine clusters, supported by image simulations of through‐focus series, were used to analyze the structures of Pt particles. The structures determined by using AC–TEM are consistent with STEM and EXAFS data in having a flat two‐dimensional morphology. Comparison of AC–STEM and AC TEM data for the same 700 °C reduced sample suggests that parallel‐beam TEM mode of imaging may be advantageous because of the less pronounced beam‐induced structural rearrangements that occur when imaging with a fine STEM probe.

Sinkler, Wharton↗

Nanocompression of 20 nm Silver Nanoparticles: In situ Aberration‐Corrected TEM and Atomistic Simulations

Single‐crystalline nanoparticles play an increasingly important role in a wide variety of fields including pharmaceuticals, advanced materials, catalysts for fuel cells, energy materials, as well as environmental detection and monitoring. Yet, the deformation mechanisms of very small nanoparticles are still poorly understood, in particular the role played by single dislocations and their interaction with surfaces. Here, in this work, silver nanoparticles with particularly small dimensions (≈20 nanometers in diameter) are compressed in situ in an aberration‐corrected transmission electron microscopy (TEM) and molecular dynamics (MD) simulations. During compression, the emergence of both dislocations and nanotwins are observed. However, these defects prove to be unstable and disappear upon removal of the indenter. Atomistic simulations confirm the role played by image stresses associated with the nearby surfaces and the reduction in dislocation line length as it approaches the free surface, thereby supporting the experimental observations. These results provide justification for the frequent observation of the absence of dislocations in nanoparticles of a few nanometers in size during in situ experiments, even after significant deformation. This phenomenon contributes to the self‐healing of samples through dislocation ejection toward the surfaces.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Direct imaging of light elements by annular dark-field aberration-corrected scanning transmission electron microscopy

In this report, we show that an annular dark-field detector in an aberration-corrected scanning transmission electron microscope allows the direct observation of light element columns in crystalline lattices. At specific imaging conditions, an enhancement of the intensities of light element columns in the presence of heavy element columns is observed. Experimental results are presented for imaging the nitrogen and carbon atomic columns at the GaN-SiC interface and within the GaN and SiC compounds. The crystal polarity of GaN at the interface is identified. The obtained findings are discussed and are well supported by image simulations.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Chromatic-aberration-corrected diffractive lenses for ultra-broadband focusing

We exploit the inherent dispersion in diffractive optics to demonstrate planar chromatic-aberration-corrected lenses. Specifically, we designed, fabricated and characterized cylindrical diffractive lenses that efficiently focus the entire visible band (450 nm to 700 nm) onto a single line. These devices are essentially pixelated, multi-level microstructures. Experiments confirm an average optical efficiency of 25% for a three-wavelength apochromatic lens whose chromatic focus shift is only 1.3 μm and 25 μm in the lateral and axial directions, respectively. Super-achromatic performance over the continuous visible band is also demonstrated with averaged lateral and axial focus shifts of only 1.65 μm and 73.6 μm, respectively. These lenses are easy to fabricate using single-step grayscale lithography and can be inexpensively replicated. Furthermore, these devices are thin (<3 μm), error tolerant, has low aspect ratio (<1:1) and offer polarization-insensitive focusing, all significant advantages compared to alternatives that rely on metasurfaces. Lastly, our design methodology offers high design flexibility in numerical aperture and focal length, and is readily extended to 2D.

36 MATERIALS SCIENCE↗

Controlled polarity of sputter-deposited aluminum nitride on metals observed by aberration corrected scanning transmission electron microscopy

The polarity determination process of sputter-deposited aluminum nitride (AlN) on metals has been analyzed using aberration corrected atomic resolution scanning transmission electron microscope. Direct growth of c-axis orientated AlN on face centered cubic metals (fcc) (111) with the local epitaxy has been observed, and the polarity was determined at the AlN/metal interface. We found that the AlN polarity can be controlled by the base metal layer: N-polarity AlN grows on Pt(111) while Al-polarity AlN forms on Al(111). Based on these results, the growth mechanism of AlN on metals is discussed.

36 MATERIALS SCIENCE↗

Evaluation of stacking faults and associated partial dislocations in AlSb/GaAs (001) interface by aberration-corrected high-resolution transmission electron microscopy

The stacking faults (SFs) in an AlSb/GaAs (001) interface were investigated using a 300 kV spherical aberration-corrected high-resolution transmission electron microscope (HRTEM). The structure and strain distribution of the single and intersecting (V-shaped) SFs associated with partial dislocations (PDs) were characterized by the [110] HRTEM images and geometric phase analysis, respectively. In the biaxial strain maps ε{sub xx} and ε{sub yy}, a SF can be divided into several sections under different strain states (positive or negative strain values). Furthermore, the strain state for the same section of a SF is in contrast to each other in ε{sub xx} and ε{sub yy} strain maps. The modification in the strain states was attributed to the variation in the local atomic displacements for the SF in the AlSb film on the GaAs substrate recorded in the lattice image. Finally, the single SF was found to be bounded by two 30° PDs. A pair of 30° PDs near the heteroepitaxial interface reacted to form a Lomer-Cottrell sessile dislocation located at the vertices of V-shaped SFs with opposite screw components. The roles of misfit dislocations, such as the PDs, in strain relaxation were also discussed.

36 MATERIALS SCIENCE↗

Experimental demonstration of passive acoustic imaging in the human skull cavity using CT-based aberration corrections

Purpose: Experimentally verify a previously described technique for performing passive acoustic imaging through an intact human skull using noninvasive, computed tomography (CT)-based aberration corrections Jones et al. [Phys. Med. Biol. 58, 4981–5005 (2013)]. Methods: A sparse hemispherical receiver array (30 cm diameter) consisting of 128 piezoceramic discs (2.5 mm diameter, 612 kHz center frequency) was used to passively listen through ex vivo human skullcaps (n = 4) to acoustic emissions from a narrow-band fixed source (1 mm diameter, 516 kHz center frequency) and from ultrasound-stimulated (5 cycle bursts, 1 Hz pulse repetition frequency, estimated in situ peak negative pressure 0.11–0.33 MPa, 306 kHz driving frequency) Definity™ microbubbles flowing through a thin-walled tube phantom. Initial in vivo feasibility testing of the method was performed. The performance of the method was assessed through comparisons to images generated without skull corrections, with invasive source-based corrections, and with water-path control images. Results: For source locations at least 25 mm from the inner skull surface, the modified reconstruction algorithm successfully restored a single focus within the skull cavity at a location within 1.25 mm from the true position of the narrow-band source. The results obtained from imaging single bubbles are in good agreement with numerical simulations of point source emitters and the authors’ previous experimental measurements using source-based skull corrections O’Reilly et al. [IEEE Trans. Biomed. Eng. 61, 1285–1294 (2014)]. In a rat model, microbubble activity was mapped through an intact human skull at pressure levels below and above the threshold for focused ultrasound-induced blood–brain barrier opening. During bursts that led to coherent bubble activity, the location of maximum intensity in images generated with CT-based skull corrections was found to deviate by less than 1 mm, on average, from the position obtained using source-based corrections. Conclusions: Taken together, these results demonstrate the feasibility of using the method to guide bubble-mediated ultrasound therapies in the brain. The technique may also have application in ultrasound-based cerebral angiography.

60 APPLIED LIFE SCIENCES↗

Aberration-corrected STEM imaging of 2D materials: Artifacts and practical applications of threefold astigmatism

High-resolution scanning transmission electron microscopy (HR-STEM) with spherical aberration correction enables researchers to peer into two-dimensional (2D) materials and correlate the material properties with those of single atoms. The maximum intensity of corrected electron beam is confined in the area having sub-angstrom size. Meanwhile, the residual threefold astigmatism of the electron probe implies a triangular shape distribution of the intensity, whereas its tails overlap and thus interact with several atomic species simultaneously. The result is the resonant modulation of contrast that interferes the determination of phase transition of 2D materials. Here, we theoretically reveal and experimentally determine the origin of resonant modulation of contrast and its unintended impact on violating the power-law dependence of contrast on coordination modes between transition metal and chalcogenide atoms. The finding illuminates the correlation between atomic contrast, spatially inequivalent chalcogenide orientation, and residual threefold astigmatism on determining the atomic structure of emerging 2D materials.

36 MATERIALS SCIENCE↗

In situ observation on hydrogenation of Mg-Ni films using environmental transmission electron microscope with aberration correction

In situ transmission electron microscopy (TEM) was performed to observe the hydrogenation of Mg-Ni films in a hydrogen atmosphere of 80–100 Pa. An aberration-corrected environmental TEM with a differential pumping system allows us to reveal the Angstrom-scale structure of the films in the initial stage of hydrogenation: first, nucleation and growth of Mg{sub 2}NiH{sub 4} crystals with a lattice spacing of 0.22 nm in an Mg-rich amorphous matrix of the film occurs within 20 s after the start of the high-resolution observation, then crystallization of MgH{sub 2} with a smaller spacing of 0.15 nm happens after approximately 1 min. Our in situ TEM method is also applicable to the analysis of other hydrogen-related materials.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗