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At least 1,135 records · Page 63

Ultra-high vacuum compatible optical chopper system for synchrotron x-ray scanning tunneling microscopy

High-speed beam choppers are a crucial part of time-resolved x-ray studies as well as a necessary component to enable elemental contrast in synchrotron x-ray scanning tunneling microscopy (SX-STM). However, many chopper systems are not capable of operation in vacuum, which restricts their application to x-ray studies with high photon energies, where air absorption does not present a significant problem. To overcome this limitation, we present a fully ultra-high vacuum (UHV) compatible chopper system capable of operating at variable chopping frequencies up to 4 kHz. The lightweight aluminum chopper disk is coated with Ti and Au films to provide the required beam attenuation for soft and hard x-rays with photon energies up to about 12 keV. The chopper is used for lock-in detection of x-ray enhanced signals in SX-STM.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

Patterning via optical-saturable transformations: A review and simple simulation model

Most of the nanoscale fabrication in the semiconductor industry is based on patterning with scanning-electron beam lithography (SEBL). Although this approach is very versatile and has very high resolution, it is intrinsically a serial writing process, and therefore, relatively slow. Our group has been investigating alternative nano-fabrication techniques, adapted from ideas of saturating optical transitions such as those used in stimulated emission-depletion microscopy and related methods, and optical interference lithography. Linewidths and resolutions on the scale of a few tens of nanometers and below are highly desirable for various applications in nanotechnology. However, the spatial resolution of optical lithography is restricted by diffraction. In the past, we developed absorbance modulation to overcome this limit. This approach utilizes photochromic molecules that can be optically switched between two thermally stable states, one opaque and the other transparent. However, absorbance modulation is limited to surface (2-D) patterning. Here, we report on an alternative approach that exploits unique combinations of spectrally selective reversible and irreversible photochemical transitions to achieve deep subwavelength resolution with potential extension to 3-dimensions. This approach, which we refer to as patterning via optical-saturable transformations have the potential for massive parallelism, enabling the creation of nanostructures and devices at a speed far surpassing what is possible with SEBL. The aim of our research is to translate the success in circumventing Abbe's diffraction limit in optical microscopy to optical lithography.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

Thermal melting and ablation of silicon by femtosecond laser radiation

The space-time dynamics of thermal melting, subsurface cavitation, spallative ablation, and fragmentation ablation of the silicon surface excited by single IR femtosecond laser pulses is studied by timeresolved optical reflection microscopy. This dynamics is revealed by monitoring picosecond and (sub)nanosecond oscillations of probe pulse reflection, which is modulated by picosecond acoustic reverberations in the dynamically growing surface melt subjected to ablation and having another acoustic impedance, and by optical interference between the probe pulse replicas reflected by the spalled layer surface and the layer retained on the target surface. The acoustic reverberation periods change during the growth and ablation of the surface melt film, which makes it possible to quantitatively estimate the contributions of these processes to the thermal dynamics of the material surface. The results on the thermal dynamics of laser excitation are supported by dynamic measurements of the ablation parameters using noncontact ultrasonic diagnostics, scanning electron microscopy, atomic force microscopy, and optical interference microscopy of the modified regions appearing on the silicon surface after ablation.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Confocal Raman Microscopy for Investigating Synthesis and Characterization of Individual Optically Trapped Vinyl-Polymerized Surfactant Particles

Small polymeric particles are increasingly employed as adsorbent materials, as molecular carriers, as delivery vehicles, and in preconcentration applications. The rational development of these materials requires in situ methods of analysis to characterize their synthesis, structure, and applications. Optical-trapping confocal Raman microscopy is a spectroscopic method capable of acquiring information at several stages of the development of such dispersed particulate materials. In the present study, an example material is developed and tested using confocal Raman microscopy for characterization at each stage of the process. Specifically, the method is used to investigate the synthesis, structure, and applications of individual polymeric surfactant particles produced by the vinyl polymerization of sodium 11-acrylamidoundecanoate (SAAU). The kinetics of polymerization can be monitored over time by measuring the loss of the acrylamide C=C functional groups using confocal Raman microscopy of particles optically trapped by the excitation laser, where, within the limits of detecting the vinyl functional group, the complete polymerization of the SAAU monomer was achieved. The polymerized SAAU particles are spherical, and they exhibit uniform access to water throughout their structure, as tested by the penetration of heavy water (D2O) and collection of spatially resolved Raman spectra from the interior of the particle. These porous particles contain hydrophobic domains that can be used to accumulate molecules for adsorption or carrier applications. This property was tested by using confocal Raman microscopy to measure the accumulation equilibria and kinetics of a model compound, dioxybenzone. The partitioning of this compound into the polymer surfactant could be determined on a quantitative basis using relative scattering cross sections of the SAAU monomer and the adsorbate. Furthermore, the study points out the utility of optical-trapping confocal Raman microscopy for investigating the synthesis, structure, and potential carrier applications of polymeric particle materials.

36 MATERIALS SCIENCE↗

Localization microscopy of DNA in situ using Vybrant{sup ®} DyeCycle™ Violet fluorescent probe: A new approach to study nuclear nanostructure at single molecule resolution

Higher order chromatin structure is not only required to compact and spatially arrange long chromatids within a nucleus, but have also important functional roles, including control of gene expression and DNA processing. However, studies of chromatin nanostructures cannot be performed using conventional widefield and confocal microscopy because of the limited optical resolution. Various methods of superresolution microscopy have been described to overcome this difficulty, like structured illumination and single molecule localization microscopy. We report here that the standard DNA dye Vybrant{sup ®} DyeCycle™ Violet can be used to provide single molecule localization microscopy (SMLM) images of DNA in nuclei of fixed mammalian cells. This SMLM method enabled optical isolation and localization of large numbers of DNA-bound molecules, usually in excess of 10{sup 6} signals in one cell nucleus. The technique yielded high-quality images of nuclear DNA density, revealing subdiffraction chromatin structures of the size in the order of 100 nm; the interchromatin compartment was visualized at unprecedented optical resolution. The approach offers several advantages over previously described high resolution DNA imaging methods, including high specificity, an ability to record images using a single wavelength excitation, and a higher density of single molecule signals than reported in previous SMLM studies. The method is compatible with DNA/multicolor SMLM imaging which employs simple staining methods suited also for conventional optical microscopy. - Highlights: • Super-resolution imaging of nuclear DNA with Vybrant Violet and blue excitation. • 90nm resolution images of DNA structures in optically thick eukaryotic nuclei. • Enhanced resolution confirms the existence of DNA-free regions inside the nucleus. • Optimized imaging conditions enable multicolor super-resolution imaging.

60 APPLIED LIFE SCIENCES↗

Ultrafast recovery time and broadband saturable absorption properties of black phosphorus suspension

As a new type of two-dimensional crystal material, black phosphorus (BP) exhibits excellent electronics and optical performance. Herein, we focus on carrier relaxation dynamics and nonlinear optical properties of BP suspension. Atomic force microscopy, transmission electron microscopy, and optical transmission spectrum are employed to characterize the structure and linear optical properties of the BP. Additionally, pump-probe experiments at wavelength of 1550 nm were carried out to study the carrier dynamics in BP suspension, and ultrafast recovery time was observed (τ{sub s} = 24 ± 2 fs). Furthermore, we demonstrate the saturable absorption signals by open aperture Z-scan experiments at wavelengths of 1550 nm, 532 nm, and 680 nm. The results indicate that BP has broadband saturable absorption properties and the nonlinear absorption coefficients were determined to be β{sub 2} = −0.20 ± 0.08 × 10{sup −3 }cm/GW (532 nm), β{sub 2} = −0.12 ± 0.05 × 10{sup −3 }cm/GW (680 nm), and β{sub 2} = −0.15 ± 0.09 × 10{sup −3 }cm/GW (1550 nm)

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

STORM Super-Resolution Visualization of Self-Assembled γPFD Chaperone Ultrastructures in Methanocaldococcus jannaschii

Gamma-prefoldin (γPFD), a unique chaperone found in the extremely thermophilic methanogen Methanocaldococcus jannaschii, self-assembles into filaments in vitro, which so far have been observed using transmission electron microscopy and cryo-electron microscopy. Utilizing three-dimensional stochastic optical reconstruction microscopy (3D-STORM), here we achieve ~20 nm resolution by precisely locating individual fluorescent molecules, hence resolving γPFD ultrastructure both in vitro and in vivo. Through CF647 NHS ester labeling, we first demonstrate the accurate visualization of filaments and bundles with purified γPFD. Next, by implementing immunofluorescence labeling after creating a 3xFLAG-tagged γPFD strain, we successfully visualize γPFD in M. jannaschii cells. Through 3D-STORM and two-color STORM imaging with DNA, we show the widespread distribution of filamentous γPFD structures within the cell. These findings provide valuable insights into the structure and localization of γPFD, opening up possibilities for studying intriguing nanoscale components not only in archaea but also in other microorganisms.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Breaking the Time Barrier in Kelvin Probe Force Microscopy: Fast Free Force Reconstruction Using the G-Mode Platform

The atomic force microscope (AFM) offers unparalleled insight into structure and material functionality across nanometer length scales. However, the spatial resolution afforded by the AFM tip is counterpoised by slow detection speeds compared to other common microscopy techniques (e.g. optical, scanning electron microscopy etc.). In this work, we develop an AFM imaging approach allowing ultrafast reconstruction of the tip-sample forces having ~2 orders of magnitude higher time resolution than standard detection methods. Fast free force recovery (F3R) overcomes the widely-viewed temporal bottleneck in AFM, i.e. the mechanical bandwidth of the cantilever, enabling time-resolved imaging at sub-bandwidth speeds. We demonstrate quantitative recovery of electrostatic forces with ~10 µs temporal resolution, free from cantilever ring-down effects. We further apply the F3R method to Kelvin probe force microscopy (KPFM) measurements. F3R-KPFM is an open loop imaging approach (i.e. no bias feedback), allowing ultrafast surface potential measurements (e.g. < 20 µs) to be performed at regular KPFM scan speeds. F3R-KPFM is demonstrated for exploration of ion migration in organometallic halide perovskites materials and shown to allow spatio-temporal imaging of positively charged ion migration under applied electric field, as well as subsequent formation of accumulated charges at the perovskite/electrode interface. In this work we demonstrate quantitative F3R-KPFM measurements – however, we fully expect the F3R approach to be valid for all modes of non-contact AFM operation, including non-invasive probing of ultrafast electrical and magnetic dynamics.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

Modulating above-room-temperature magnetism in Ga-implanted Fe 5 GeTe 2 van der Waals magnets

The creation of van der Waals (vdW) ferromagnets with tunable Curie temperature (T C ) and magnetic anisotropy is essential in developing vdW magnet-based devices. Here, we report an effective and reliable method for modulating the magnetic properties of vdW Fe 5 GeTe 2 by site-specific Ga + implantation. In this study, we report an easy axis in the ab-plane for bulk Fe 5 GeTe 2 (T C = 310 K) and an axis out of the plane for thin Fe 5 GeTe 2 flakes (T C = 290 K). Combining element-resolved photoemission electron microscopy and spatially resolved magneto-optic Kerr microscopy, we find that the implantation of a tiny amount of 10 –3 Ga + ·Å –3 in Fe 5 GeTe 2 greatly enhances the T C from 290 to 360 K and switches the magnetic easy axis from the out-of-plane c axis to the ab-plane. The room-temperature x-ray magnetic circular dichroism signal is enhanced from 0% to 9% at an implantation level of 10 –2 Ga + ·Å –3 . These results provide new opportunities for tailoring the magnetic properties of vdW materials beyond room temperature.

36 MATERIALS SCIENCE↗

Possibilities of Using Combined Optical and AFM Investigations of Albumin

The results of a complex study of 10% aqueous solution of human serum albumin using methods of optical and atomic force microscopy have been presented. The fine structure of main structures of albumin facies (vitreous matrix and concretions) has been revealed and some observed structural effects have been interpreted from the viewpoint of polymer materials science.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Intracellular distribution and stability of a luminescent rhenium( I ) tricarbonyl tetrazolato complex using epifluorescence microscopy in conjunction with X-ray fluorescence imaging

Optical fluorescence microscopy was used in conjunction with X-ray fluorescence microscopy to monitor the stability and intracellular distribution of the luminescent rhenium(I) complex fac -[Re(CO) 3 (phen)L], where phen = 1,10-phenathroline and L = 5-(4-iodophenyl)tetrazolato, in 22Rv1 cells. The rhenium complex showed no signs of ancillary ligand dissociation, a conclusion based on data obtained via X-ray fluorescence imaging aligning iodine and rhenium distributions. A diffuse reticular localisation was detected for the complex, in the nuclear/perinuclear region of cells, by either optical or X-ray fluorescence techniques. Furthermore, X-ray fluorescence also showed that the Re-I complex disrupted the homeostasis of some biologically relevant elements, such as chlorine, potassium and zinc.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

X-ray/EUV optics for astronomy and microscopy; Proceedings of the Meeting, San Diego, CA, Aug. 7-11, 1989

Topics included in these proceedings are on X-ray/EUV zone plates, filters, and windows; X-ray/EUV microscopes, telescopes, and monochromators; the design, characterization, and test of multilayer optics; the fabrication of X-ray/EUV multilayer optics; and the design, characterization, and test of grazing incidence X-ray optics. Other topics are on the fabrication of grazing incidence X-ray optics, X-ray/EUV space observatories and missions, the test and calibration of X-ray/EUV instruments, X-ray polarimetry, and X-ray/EUV spectroscopy and instruments. Papers are presented on 8-keV X-ray zone plates, a cylindrical X-ray multilayer monochromator, multilayer mirrors for 182 A, advanced flow polishing of exotic optical materials, and optical analysis of grazing incidence ring resonators for free-electron lasers. Attention is also given to X-ray mirrors for the European Synchrotron Radiation Facility, the XUV wide-field camera for Rosat, an optical test and alignment method for the XMM mirror module, Bragg crystal polarimeters, and a liftoff process for multilayer phase gratings.

Hoover, Richard B.↗

Near-field imaging of optical resonances in silicon metasurfaces using photoelectron microscopy

Precise control of light–matter interactions at the nanoscale lies at the heart of nanophotonics. However, experimental examination at this length scale is challenging since the corresponding electromagnetic near-field is often confined within volumes below the resolution of conventional optical microscopy. In semiconductor nanophotonics, electromagnetic fields are further restricted within the confines of individual subwavelength resonators, limiting access to critical light–matter interactions in these structures. In this work, we demonstrate that photoelectron emission microscopy (PEEM) can be used for polarization-resolved near-field spectroscopy and imaging of electromagnetic resonances supported by broken-symmetry silicon metasurfaces. We find that the photoemission results, enabled through an in situ potassium surface layer, are consistent with full-wave simulations and far-field reflectance measurements across visible and near-infrared wavelengths. In addition, we uncover a polarization-dependent evolution of collective resonances near the metasurface array edge taking advantage of the far-field excitation and full-field imaging of PEEM. Here, we deduce that coupling between eight resonators or more establishes the collective excitations of this metasurface. All told, we demonstrate that the high-spatial resolution hyperspectral imaging and far-field illumination of PEEM can be leveraged for the metrology of collective, non-local, optical resonances in semiconductor nanophotonic structures.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

Optical and Scanning Electron Microscopy of the Materials International Space Station Experiment (MISSE) Spacecraft Silicone Experiment

Under a microscope, atomic oxygen (AO) exposed silicone surfaces are crazed and seen as "islands" separated by numerous crack lines, much analogous to mud-tile cracks. This research characterized and compared the degree of AO degradation of silicones by analyzing optical microscope images of samples exposed to low Earth orbit (LEO) AO as part of the Spacecraft Silicone Experiment. The Spacecraft Silicone Experiment consisted of eight DC 93-500 silicone samples exposed to eight different AO fluence levels (ranged from 1.46 to 8.43 10(exp 21) atoms/sq cm) during two different Materials International Space Station Experiment (MISSE) missions. Image analysis software was used to analyze images taken using a digital camera. To describe the morphological degradation of each AO exposed flight sample, three different parameters were selected and estimated: (1) average area of islands was determined and found to be in the 1000 to 3100 sq mm range; (2) total length of crack lines per unit area of the sample surface were determined and found to be in the range of 27 to 59 mm of crack length per sq mm of sample surface; and (3) the fraction of sample surface area that is occupied by crack lines was determined and found to be in the 25 to 56 percent range. In addition, average crack width can be estimated from crack length and crack area measurements and was calculated to be about 10 mm. Among the parameters studied, the fraction of sample surface area that is occupied by crack lines is believed to be most useful in characterizing the degree of silicone conversion to silicates by AO because its value steadily increases with increasing fluence over the entire fluence range. A series of SEM images from the eight samples exposed to different AO fluences suggest a complex sequence of surface stress due to surface shrinkage and crack formation, followed by re-distribution of stress and shrinking rate on the sample surface. Energy dispersive spectra (EDS) indicated that upon AO exposure, carbon content on the surface decreased relatively quickly at the beginning, to 32 percent of the pristine value for the least exposed sample in this set of experiments (1.46 10(exp 21) atoms/sq cm), but then decreased slowly, to 22 percent of the pristine value for the most exposed sample in this set of experiment (8.43 10(exp 21) atoms/sq cm). The oxygen content appears to increase at a slower rate. The least and most AO exposed samples were, respectively, 52 and 150 percent above the pristine values. The silicone samples with the greater AO exposure (7.75 10(exp 21) atoms/sq cm and higher) appear to have a surface layer which contains SiO2 with perhaps small amounts of unreacted silicone, CO and CO2 sealed inside.

Hung, Ching-cheh↗

Final Technical Report - Rapid Surface Microanalysis using a Low Temperature Plasma

This project focused on improving our current understanding and scientific knowledge in the area of plasma-surface interactions and plasma assisted material synthesis related to advanced microelectronics and nanotechnology. Current challenges include: controlling the interaction of Low Temperature Plasma (LTP) with a single layer of atoms to manufacture integrated circuits, continued miniaturization of integrated circuits, LTP processing of material surfaces and thin films to enable industrial scale fabrication of advanced microelectronics, synthesis of new materials, nanomaterials, nanotubes, and complex materials, Technology developed in this subtopic is of value to either (i) enable scans of surfaces (~1 sq. cm area) using various microscopies (electron, optical, other) at high resolution (micron or sub-micron resolution) rapidly (hours or days rather than years to complete a high-resolution scan of such a large surface area), or (ii) enable scans of surfaces (~1 sq. cm area) using various microscopies (electron, optical, other) at relatively low resolution rapidly, then apply algorithms to select spots for micron-scale imaging. Sputtering occurs when particles of a solid material are ejected from its surface by energetic particles from a plasma. While the degradation of the solid material and the subsequent deposition of the ejected material onto vulnerable surfaces are the usual subjects of sputtering studies, plasma science has yet to be combined with sputtering to create new diagnostics devices and systems. Small changes in the design of the plasma discharge device make it possible to create broad plasma beams for rapid scanning or small plasma beams to obtain the distribution of ejected elements with micron resolution. In the high-resolution use, the ion flux is extracted from the gas-discharge plasma and focused by a spherical emission surface to micron sizes onto the target specimen, providing very local sputtering and local elemental analysis. We call this “self-focusing”. The radiation from the excited and ionized sputtered atoms is recorded by a spectrometer through a window and fiberglass cable and analyzed with standard software packages used for optical glow discharge spectroscopy. Computer simulations of beam formation were used to verify and optimize the designs to be tested. A prototype was designed, constructed, and used to start experiments of beam formation.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

Co-existence of a few and sub micron inhomogeneities in Al-rich AlGaN/AlN quantum wells

Inhomogeneity in Al-rich AlGaN/AlN quantum wells is directly observed using our custom-built confocal microscopy photoluminescence (μ-PL) apparatus with a reflective system. The μ-PL system can reach the AlN bandgap in the deep ultra-violet spectral range with a spatial resolution of 1.8 μm. In addition, cathodoluminescence (CL) measurements with a higher spatial resolution of about 100 nm are performed. A comparison of the μ-PL and CL measurements reveals that inhomogeneities, which have different spatial distributions of a few- and sub-micron scales that are superimposed, play key roles in determining the optical properties.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗