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At least 1,063 records · Page 59

6 nm super-resolution optical transmission and scattering spectroscopic imaging of carbon nanotubes using a nanometer-scale white light source

Abstract Optical transmission and scattering spectroscopic microscopy at the visible and adjacent wavelengths denote one of the most informative and inclusive characterization methods in material research. Unfortunately, restricted by the diffraction limit of light, it cannot resolve the nanoscale variation in light absorption and scattering, diagnostics of the local inhomogeneity in material structure and properties. Moreover, a large quantity of nanomaterials has anisotropic optical properties that are appealing yet hard to characterize through conventional optical methods. There is an increasing demand to extend the optical hyperspectral imaging into the nanometer length scale. In this work, we report a super-resolution hyperspectral imaging technique that uses a nanoscale white light source generated by superfocusing the light from a tungsten-halogen lamp to simultaneously obtain optical transmission and scattering spectroscopic images. A 6-nm spatial resolution in the visible to near-infrared wavelength regime (415–980 nm) is demonstrated on an individual single-walled carbon nanotube (SW-CNT). Both the longitudinal and transverse optical electronic transitions are measured, and the SW-CNT chiral indices can be identified. The band structure modulation in a SW-CNT through strain engineering is mapped.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Comprehensive characterization of irradiation induced defects in ceria: Impact of point defects on vibrational and optical properties

Validation of multiscale microstructure evolution models can be improved when standard microstructure characterization tools are coupled with methods sensitive to individual point defects. We demonstrate how electronic and vibrational properties of defects revealed by optical absorption and Raman spectroscopies can be used to compliment transmission electron microscopy (TEM) and x-ray diffraction (XRD) in the characterization of microstructure evolution in ceria under non-equilibrium conditions. Experimental manifestation of non-equilibrium conditions was realized by exposing cerium dioxide (CeO2) to energetic protons at elevated temperature. Two sintered polycrystalline CeO2 samples were bombarded with protons accelerated to a few MeVs. These irradiation conditions produced a microstructure with resolvable extended defects and a significant concentration of point defects. A rate theory (RT) model was parametrized using the results of TEM, XRD, and thermal conductivity measurements to infer point defect concentrations. An abundance of cerium sublattice defects suggested by the RT model is supported by Raman spectroscopy measurements, which show peak shift and broadening of the intrinsic T2g peak and emergence of new defect peaks. Additionally, spectroscopic ellipsometry measurements performed in lieu of optical absorption reveals the presence of Ce3+ ions associated with oxygen vacancies. This work lays the foundation for a coupled approach that considers a multimodal characterization of microstructures to guide and validate complex defect evolution models.

Chauhan, Vinay S.↗

Quasi-optical beam tracing module development for millimeter-wave high-wavenumber collective scattering on the NSTX-U and EAST tokamaks

A Python3-based beam tracing code utilizing Quasi-Optics has been developed to track both incident and receiving beams in high-k collective millimeter wave scattering systems within magnetic fusion plasmas. In contrast to existing ray tracing codes that solely consider refraction, this beam tracing code incorporates diffraction phenomena, providing a more comprehensive calculation. Here, this enhanced capability allows for a more accurate calculation of the scattering volume and spatial resolution in high-k collective scattering systems, crucial for evaluating system performance and facilitating data analysis. Unlike Geometrical Optics, Quasi-Optics employs the complex eikonal method, representing a Gaussian beam as a collection of coupled rays to accurately preserve diffraction characteristics. The developed code is intended for application in NSTX-Upgrade and EAST high-k beam tracing analyses, targeting frequencies of 693 GHz and 270 GHz, respectively. The high-k system's primary objective is the observation of electron-scale instabilities. Employing a symplectic integrator, the code ensures numerical accuracy, assessed through the conservation of the Hamiltonian. With its precision and efficiency, the code facilitates rapid inter-shot analyses.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

Manufacturing Precise, Lightweight Paraboloidal Mirrors

A process for fabricating a precise, diffraction- limited, ultra-lightweight, composite- material (matrix/fiber) paraboloidal telescope mirror has been devised. Unlike the traditional process of fabrication of heavier glass-based mirrors, this process involves a minimum of manual steps and subjective judgment. Instead, this process involves objectively controllable, repeatable steps; hence, this process is better suited for mass production. Other processes that have been investigated for fabrication of precise composite-material lightweight mirrors have resulted in print-through of fiber patterns onto reflecting surfaces, and have not provided adequate structural support for maintenance of stable, diffraction-limited surface figures. In contrast, this process does not result in print-through of the fiber pattern onto the reflecting surface and does provide a lightweight, rigid structure capable of maintaining a diffraction-limited surface figure in the face of changing temperature, humidity, and air pressure. The process consists mainly of the following steps: 1. A precise glass mandrel is fabricated by conventional optical grinding and polishing. 2. The mandrel is coated with a release agent and covered with layers of a carbon- fiber composite material. 3. The outer surface of the outer layer of the carbon-fiber composite material is coated with a surfactant chosen to provide for the proper flow of an epoxy resin to be applied subsequently. 4. The mandrel as thus covered is mounted on a temperature-controlled spin table. 5. The table is heated to a suitable temperature and spun at a suitable speed as the epoxy resin is poured onto the coated carbon-fiber composite material. 6. The surface figure of the optic is monitored and adjusted by use of traditional Ronchi, Focault, and interferometric optical measurement techniques while the speed of rotation and the temperature are adjusted to obtain the desired figure. The proper selection of surfactant, speed or rotation, viscosity of the epoxy, and temperature make it possible to obtain the desired diffraction-limited, smooth (1/50th wave) parabolic outer surface, suitable for reflective coating. 7. A reflective coat is applied by use of conventional coating techniques. 8. Once the final figure is set, a lightweight structural foam is applied to the rear of the optic to ensure stability of the figure.

Hermann, Frederick Thomas↗

Micron-Accurate Laser Fresnel-Diffraction Ranging System

Two versions of an optoelectronic system undergoing development are depicted. The system is expected to be capable of measuring a distance between 2 and 10 m with an error of no more than 1 micrometer. The system would be designed to exploit Fresnel diffraction of a laser beam. In particular, it would be designed to take advantage of the fact that a Fresnel diffraction pattern is ultrasensitive to distance. The two versions would differ in the following respects: In version 1, the focus of the telescope would be in the Fresnel region, and the telescope would have a small depth of focus. As a consequence, the Fresnel pattern would be imaged directly onto the photodetector array; in version 2, a multielement lens module would displace the Fresnel region from the vicinity of the pinhole to the vicinity of the optical receiver. As the distance to be measured varied, the location of the receiver relative to the displaced Fresnel-diffraction region would vary, thereby causing the Fresnel diffraction pattern on the focal plane to vary. The multielement lens module would also correct for aberrations. The processing of the digitized Fresnel diffraction pattern in the computer might be accelerated by using only parts of the pattern or even only one small part - the central pixel. As the distance from the pinhole increased, the central pixel would rapidly cycle between maximum and minimum light intensity. This in itself would not be sufficient to uniquely determine the distance. However, by varying the size of the pinhole or the wavelength of the laser, one could obtain a second cycle of variation of intensity that, in conjunction with the first cycle, could enable a unique determination of distance. Alternatively, for a single wavelength and a single pinhole size, it should suffice to consider the data from only two different key pixels in the Fresnel pattern.

Lehner, David↗

Crystal Growth of Quaternary Rare Earth Selenosilicates by Using the Flux-Assisted Boron Chalcogen Mixture Method: Investigation of Their Magnetic and Optical Properties

A series of rare earth magnesium selenosilicates, RE3Mg 0.5 SiSe 7 (RE = Ce, Pr, Nd, Sm, Gd, Tb, Dy) were obtained as single crystal using the flux assisted boron chalcogen mixture (BCM) method. The structures of the crystals were determined by single-crystal X-ray diffraction. The RE3Mg 0.5 SiSe 7 series crystallizes in the hexagonal crystal system in the space group P6 3 . Polycrystalline powders were synthesized to perform physical property measurements. Magnetic measurements over the 2–300 K temperature range reveal that Ce 3 Mg 0.5 SiSe 7 and Gd 3 Mg 0.5 SiSe 7 exhibit paramagnetic behavior with negative Weiss constants (θ W = −14.50, θ W = −6.13 K, respectively). The optical properties of RE 3 Mg 0.5 SiSe 7 (RE = Ce, Pr, Nd, Sm, Gd) were measured by ultraviolet–visible (UV–vis) diffuse reflectance. Density functional theory (DFT) electronic structure calculations were performed. Furthermore, a second harmonic generation measurement was performed on a polycrystalline powder of Ce 3 Mg 0.5 SiSe 7 and was found to be SHG active with an efficiency of 0.11 times the standard potassium dihydrogen phosphate (KDP).

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Decoding THz‐Driven Dynamic Fingerprints of Ferroelectric Nanotwin Networks

Ultrafast polarization dynamics in ferroelectrics are of considerable interest for high-speed tunable dielectrics and electro-optics. Extended domain wall networks formed in ferroelectric twin nanodomains can support collective dynamics in the terahertz regime but require techniques that track polarization and strain evolution driven by ultrafast stimulus. Here, we use multi-modal probing of THz-pulse-driven excitations in PbTiO 3 /SrTiO 3 superlattices by combining X-ray free electron laser measurements that directly tracks lattice changes, with optical second harmonic generation that tracks the electronic potential coupled with the lattice potential. Dynamical phase-field modeling enables fingerprinting of these collective modes as superpositions of domain “breathing” through wall oscillations and polarization “rotations” with still walls. Ultrafast domain wall motion at 0.1–0.5 THz is observed at practical fields of 100 kV/cm with wall velocities of >4000 m/s, approaching typical speed of sound in PbTiO 3 . A unique “charging” mode is discovered that can electrically charge and discharge domain walls on ∼4 ps time scale thus dynamically tuning wall conductivity. Integrated experimental and theoretical fingerprinting of the dynamical landscape presented here enables ultrafast control of ferroics for high-speed microelectronics and optical applications.

THz dynamics↗

Using defects as a ‘fossil record’ to help interpret complex processes during additive manufacturing: as applied to raster-scanned electron beam powder bed additively manufactured Ti–6Al–4V

Abstract Defects in parts produced by additive manufacturing, instead of simply being perceived as deleterious, can act as important sources of information associated with the complex physical processes that occur during materials deposition and subsequent thermal cycles. Indeed, they act as materials-state ‘fossil’ records of the dynamic AM process. The approach of using defects as epoch-like records of prior history has been developed while studying additively manufactured Ti–6Al–4V and has given new insights into processes that may otherwise remain either obscured or unquantified. Analogous to ‘epochs,’ the evolution of these defects often is characterized by physics that span across a temporal length scale. To demonstrate this approach, a broad range of analyses including optical and electron microscopy, X-ray computed tomography, energy-dispersive spectroscopy, and electron backscatter diffraction have been used to characterize a raster-scanned electron beam Ti–6Al–4V sample. These analysis techniques provide key characteristics of defects such as their morphology, location within the part, complex compositional fields interacting with the defects, and structures on the free surfaces of defects. Observed defects have been classified as banding, spherical porosity, and lack of fusion. Banding is directly related to preferential evaporation of Al, which has an influence on mechanical properties. Lack-of-fusion defects can be used to understand columnar grain growth, fluid flow of melt pools, humping, and spattering events. Graphical abstract

36 MATERIALS SCIENCE↗

The Influence of Nonlocal Metal–Dielectric Environments on Physical and Chemical Processes

Plasmonic nanolayers and laminar metallic/dielectric multilayers were originally developed for optical cloaking applications and lensing applications that could potentially image objects whose size was below the diffraction limit. These assemblies were initially formed from gold or silver nanorods grown within an alumina mesh. However, more recently, assemblies with similar properties have also been prepared by sequential thin-layer deposition of alternating layers of gold and magnesium fluoride (MgF 2 ). These metal/dielectric composite materials enable control of the dielectric constant in the directions perpendicular to the layers and balance the real and imaginary dielectric constants of the assembly such that the speed and the amplitude of the waves traveling through the assembly are not attenuated. In this Account, we will also focus on a few of the applications ranging from surface wetting to fluorescence quenching to enhancement of photochemical reactions. First, we will share an introduction to processes used to create these materials, which are combinations of low refractive index metals and transparent higher index materials arranged in a scalable repeating fashion. Two fabrication methods were employed: an electrochemical deposition of Ag nanorods into an anodized alumina matrix which produced materials with an anisotropic negative refractive index material within the plane of the film and lamellar metal/dielectric layers in which the negative index perpendicular to the growth direction. These alternating layers of plasmonic metals and dielectric materials were ultimately chosen to prepare films for further testing, because of their relative ease of fabrication. We will continue with a discussion of a few of the applications of both of these nonlocal dielectric composite materials including more specialized plasmonic, composite, and hyperbolic metamaterials including fluorescence quenching, photochemical reactions, and surface wetting. In each of these applications, the unique response caused by the enhancement of the electric field and the interface between hyperbolic materials and plasmonic materials as they interact photophysically with their near neighbors is presented. In each of the applications, the enhanced electric field extends from the composite substrate layer to interact with its near neighbors and beyond. Furthermore, the presence of this extended interaction can be observed in the form of decreased emission lifetime, enhancement of photochemical reaction rates, and changes in the surface energies measured by contact angle goniometry. In this Account, all of these situations will be addressed. Finally, we will conclude with a summary and vision for the future as well as a discussion of the unique challenges and opportunities available as research active faculty at an HBCU.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Generation and detection of 50 GHz surface acoustic waves by extreme ultraviolet pulses

In this work, we use femtosecond extreme ultraviolet pulses derived from a free electron laser to excite and probe surface acoustic waves (SAWs) on the (001) surface of single crystal SrTiO 3 . SAWs are generated by a pair of 39.9 nm pulses crossed at the sample with the crossing angle defining the SAW wavelength at 84 nm. Detection of SAWs is performed via diffraction of a time-delayed 13.3 nm probe pulse by SAW-induced surface ripples. Despite the low reflectivity of the sample in the extreme ultraviolet range, the reflection mode detection is found to be efficient because of an increase in the diffraction efficiency for shorter wavelengths. We describe a methodology for extracting the SAW attenuation in the presence of a thermal grating, which is based on measuring the decay of oscillations at twice the SAW frequency. The proposed approach can be used to study ultrahigh frequency SAWs in a broad range of materials and will bridge the wave vector gap in surface phonon spectroscopy between Brillouin scattering and He atom scattering.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

Effect of grain size on damage and failure in two-phase materials: Homogenized CuPb

It is well known that spall failure strongly depends on the microstructure of a material. There have been numerous studies to study the effect of grain size on the overall spall strength and the total amount of damage in single element metals like copper. However, such systematic studies remain rare in two-phase materials and alloys. In this work, two incipient spall experiments were performed on a Cu–1%Pb alloy to understand the effect of grain size on the damage and failure in a two-phase material. Overall, these results showed that even though the spall strength did not change as a function of grain size, there were significant differences in the total amount of damage as a function of grain size. A clear increase in the total damage present in the material was seen as the grain size was increased from 32 to either 70 or 75 μm in either of the experiments. Furthermore, this difference was attributed to variations in the void growth rate as the grain size was increased.

36 MATERIALS SCIENCE↗

Dynamic and quasi-static strength of additively repaired aluminum

Additive manufacturing has the potential to repair high value components, saving significant time and resources; however, the level of reliability and performance of additive repairs is still relatively unknown. In this work, the structure–property and performance of laser wire additive manufacturing repairs in 1100 aluminum are investigated. Two types of intentional damage are inflicted on the samples and subsequently repaired with pulsed laser deposition additive manufacturing. Quasi-static (10 –3 s –1 ) and high strain-rate (10 –3 s –1 ) mechanical testing is carried out with in situ diagnostics and post-mortem imaging. The results show that while the quasi-static strength and ductility of samples with a repaired region are lower than a pristine sample, the dynamic strength under shock loading is comparable. This work highlights both the potential utility of additive manufacturing for repair purposes, the significant risk of compromised performance of additive parts under specific conditions, and the need to test at varying strain rates to fully characterize material performance.

36 MATERIALS SCIENCE↗

Sulfur Species in Zinc-Rich Condylar Zones of a Rat Temporomandibular Joint

We performed synchrotron-based micro-X-ray absorption near-edge spectroscopy (µ-XANES) coupled with micro-X-ray fluorescence (µ-XRF) for the identification of elements that included biometal zinc (Zn) and nonmetal sulfur (S) (and its species) in the condylar zones of a rat temporomandibular joint (TMJ). Zone-specific spatial localization of biometal Zn and nonmetal S from a materials viewpoint when correlated with hypoxia inducible factor-1α (HIF-1α) (a surrogate for tissue oxygenation) can provide insights into Zn-specific redox pathways at the vulnerable subchondral interface. Histologic localization of Zn, HIF-1α, and sulfur-rich proteoglycans (PGs) were mapped using an optical microscope. The µ-XRF maps coupled with site-specific micro-X-ray diffraction (µ-XRD) patterns were used to underline Zn-incorporated biological apatite in the subchondral bone and the bone of a rat TMJ condyle. Results demonstrated an association between Zn, PG, and HIF-1α histologic maps with µ-XRF, µ-XANES, and µ-XRD data and provided insights into plausible biological S species in Zn-enriched zones of a rat TMJ condyle. Spatially localized Zn and S underscore their roles in cell and tissue functions in a zone-specific manner. Elemental Zn with organic and inorganic S species at the cartilage-bone interface and the biomineral phase of Zn-enriched biological apatite from subchondral bone to condylar bone were ascertained using µ-XRF-XANES and µ-XRF-XRD. The coupled µ-XRF-XANES in situ complemented with µ-XRF-XRD in situ and immunohistochemistry provided valuable biological insights into zone-specific biological pathways in rat TMJ condyles. Based on these data, we present a workflow to reliably map and correlate S species within Zn-enriched regions of cartilage, bone, and their interface. We suggest the use of this correlative and complementary microspectroscopic spatial information for zone-specific localization of biometal Zn and nonmetal S to gain insights into plausible microanatomy-specific oxidative stress in the TMJ.

apatites↗

Single-frame far-field diffractive imaging with randomized illumination

We introduce a single-frame diffractive imaging method called randomized probe imaging (RPI). In RPI, a sample is illuminated by a structured probe field containing speckles smaller than the sample’s typical feature size. Quantitative amplitude and phase images are then reconstructed from the resulting far-field diffraction pattern. The experimental geometry of RPI is straightforward to implement, requires no near-field optics, and is applicable to extended samples. When the resulting data are analyzed with a complimentary algorithm, reliable reconstructions which are robust to missing data are achieved. To realize these benefits, a resolution limit associated with the numerical aperture of the probe-forming optics is imposed. RPI therefore offers an attractive modality for quantitative X-ray phase imaging when temporal resolution and reliability are critical but spatial resolution in the tens of nanometers is sufficient. We discuss the method, introduce a reconstruction algorithm, and present two proof-of-concept experiments: one using visible light, and one using soft X-rays.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

High-resolution ptychographic imaging enabled by high-speed multi-pass scanning

As a coherent diffraction imaging technique, ptychography provides high-spatial resolution beyond Rayleigh’s criterion of the focusing optics, but it is also sensitively affected by the decoherence coming from the spatial and temporal variations in the experiment. Here we show that high-speed ptychographic data acquisition with short exposure can effectively reduce the impact from experimental variations. To reach a cumulative dose required for a given resolution, we further demonstrate that a continuous multi-pass scan via high-speed ptychography can achieve high-resolution imaging. This low-dose scan strategy is shown to be more dose-efficient, and has potential for radiation-sensitive sample studies and time-resolved imaging.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗

X-Ray Performance of Critical-angle Transmission Grating Prototypes for the Arcus Mission

Arcus is a proposed Explorer Class soft X-ray grating spectrometer. It aims to explore cosmic feedback by mapping hot gases within and between galaxies and galaxy clusters and characterizing jets and winds from supermassive black holes and to investigate the dynamics of protoplanetary disks and stellar accretion. Arcus features 12 m focal-length grazing-incidence silicon pore optics (SPO) developed for the Athena mission. Critical-angle transmission (CAT) gratings efficiently disperse high diffraction orders onto CCDs. We report new and improved X-ray performance results for Arcus-like CAT gratings, including a record resolving power for two coaligned CAT gratings. Multiple Arcus prototype grating facets were illuminated by an SPO at the PANTER facility. The facets consist of 32 × 32.5 mm 2 patterned silicon membranes, bonded to metal frames. The bonding angle is adjusted according to the measured average tilt angle of the grating bars in the membrane. Two simultaneously illuminated facets show a minor broadening of the Al-K α doublet in the 18th and 21st orders with the best-fit record effective resolving power of ${R}_{G}\approx {1.3}_{-0.5}^{+\infty }\times {10}^{4}$ (3σ), about three to four times the Arcus requirement. We measured the diffraction efficiency of quasi-fully illuminated gratings at O-K wavelengths in orders 4–7 in an Arcus-like configuration and compare results with synchrotron spot measurements. After corrections for geometrical effects and bremsstrahlung continuum, we find agreement between full and spot illumination at the two different facilities, as well as with the models used for Arcus effective area predictions. We find that these flight-like gratings meet the diffraction efficiency and greatly exceed the resolving power Arcus requires.

79 ASTRONOMY AND ASTROPHYSICS↗

Ray tracing program with options for diffraction gratings

Diffraction theory, developed in vectorial form and coded into ray tracing routines, permits tracing rays of any wavelength through surfaces that are plane, spherical, conical, or aspheric polynomial. Ruled diffraction gratings may run in either X-direction or Y-direction, where Z is optical axis.

Howell, B. J.↗

Optical Signal Processing: Poisson Image Restoration and Shearing Interferometry

Optical signal processing can be performed in either digital or analog systems. Digital computers and coherent optical systems are discussed as they are used in optical signal processing. Topics include: image restoration; phase-object visualization; image contrast reversal; optical computation; image multiplexing; and fabrication of spatial filters. Digital optical data processing deals with restoration of images degraded by signal-dependent noise. When the input data of an image restoration system are the numbers of photoelectrons received from various areas of a photosensitive surface, the data are Poisson distributed with mean values proportional to the illuminance of the incoherently radiating object and background light. Optical signal processing using coherent optical systems is also discussed. Following a brief review of the pertinent details of Ronchi's diffraction grating interferometer, moire effect, carrier-frequency photography, and achromatic holography, two new shearing interferometers based on them are presented. Both interferometers can produce variable shear.

Hong, Yie-Ming↗