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At least 73 records · Page 4

Design, Testing, and Implementation of the Marshall Grazing Incidence X-ray Spectrometer Slit-Jaw Context Imaging System

The Marshall Grazing Incidence X-ray Spectrometer (MaGIXS) is a NASA sounding rocket payload providing a 0.6 – 2.5 nm spectrum with unprecedented spatial and spectral resolution. The instrument is comprised of a novel optical design, featuring a Wolter 1 grazing mirror in the telescope module focusing the solar image on a slit plate; two corrective optics, a diffraction grating and a low-noise detector make up the spectrometer module. When MaGIXS flies on a suborbital launch in 2020, a slit-jaw camera system will image the sun in extreme ultraviolet (EUV) to soft x-ray wavelengths, providing a reference for pointing the telescope and aligning the data to supporting observations from satellites.

Phillip Wilkerson↗

The soft X-ray/EUV calibration facility at the University of Colorado

The components of the calibration facility at the University of Colorado are described. The system is capable of analyzing the performance of optical components in the wavelength range from 2.7 to 2500 A. The system uses two light sources: a water-cooled hollow cathode gas discharge source and a soft X-ray source. The 2.2-m grazing incidence monochrometer, slits, large chamber, and computer-controlled manipulator are examined. The NBS aluminum oxide photodiode, a flowing gas proportional counter, and an imaging microchannel plate device are employed to detect the light. The optics, detectors, and data acquisition system are computer controlled. The facility is applicable for evaluating the performance of diffraction gratings, multilayer mirrors, reflective coatings, spectrographs, surface roughness scattering, and absolute detector efficiencies. Examples demonstrating the capabilities of the facility and a diagram of the facility are presented.

Windt, David L.↗

Thin Film Synthesis of SrZn2P2 with SrI2 Post-Annealing for Enhanced Crystallinity and Optoelectronic Quality

Ternary Zintl phosphides are promising light-absorbing semiconductors for thin-film optoelectronic applications, but strategies for controlling their microstructure and optoelectronic quality remain underexplored. Here, we report the synthesis of phase-pure SrZn2P2 thin films using radio-frequency co-sputtering in a PH3 + Ar atmosphere and investigate the impact of post-growth processing on their structural and optical properties. Grazing-incidence X-ray scattering and Raman spectroscopy confirm the formation of crystalline SrZn2P2 films over a finite compositional window. Optical measurements reveal clear absorption near the direct-band-gap energy (~1.8 eV) and near-band-edge photoluminescence. Further, we have studied the effects of chemically compatible halide-assisted annealing. It is found that SrI2 treatments lead to pronounced grain growth and reduced diffraction peak broadening while preserving phase purity, in contrast to rapid thermal or forming-gas annealing. Notably, annealing with SrI2 at 450 degrees C significantly enhances both the intensity and spatial uniformity of the photoluminescence, thus connecting the observed microstructural consolidation with improved radiative recombination. Our study demonstrates that halide-assisted annealing provides an effective pathway for microstructural control in SrZn2P2 thin films and highlights a generalizable processing strategy for advancing Zintl phosphide semiconductors toward optoelectronic applications.

14 SOLAR ENERGY↗

Increased spatial coherence length from an asymmetric crystal reflection at grazing exit

Coherent X-ray imaging is an active field at synchrotron sources. The images rely on the available coherent flux over a limited field of view. At many synchrotron beamlines a double-crystal monochromator (DCM) is employed in a standard nondispersive arrangement. For coherent diffraction imaging it is advantageous to increase the available field of view by increasing the spatial coherence length (SCL) of a beam exiting such a DCM. Here, Talbot interferometry data together with ray-tracing simulations for a (+ − − +) four-reflection experimental arrangement are presented, wherein the first two reflections are in the DCM and the final fourth reflection is asymmetric at grazing exit. Analyses of the interferometry data combined with the simulations show that compared with the beam exiting the DCM a gain of 76% in the SCL was achieved, albeit with a factor of 20 reduction in flux density, which may not be a severe penalty at a synchrotron beamline. Previous efforts reported in the literature to increase the SCL that employed asymmetric crystal diffraction at grazing incidence are also discussed. A much reduced SCL is found presently in simulations wherein the same asymmetric crystal is set for grazing incidence instead of grazing exit. In addition, the present study is compared and contrasted with two other means of increasing the SCL. These are (i) focusing the beam onto an aperture to act as a secondary source, and (ii) allowing the beam to propagate in vacuum an additional distance along the beamline.

73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗

X-ray spectrographs using radial groove gratings

A high efficiency spectrograph design for the EUV and soft X rays is presented. This grazing incidence system uses a plane surface reflection grating with rulings that are radial, like the spokes of a wheel. The grating is placed in a beam of light that is converging to a focus. The single reflection off the grating is in the conical diffraction mount ensuring maximum performance from the system. Aberrations and performance levels are discussed. The gratings can be manufactured with existing ruling engines. Sample applications to an X-ray monochromator and an EUV stellar spectrograph are discussed.

Cash, W. C., Jr.↗

X-ray Interferometry with Transmissive Beam Combiners for Ultra-High Angular Resolution Astronomy

Abstract Interferometry provides one of the possible routes to ultra-high angular resolution for X-ray and gamma-ray astronomy. Sub-micro-arc-second angular resolution, necessary to achieve objectives such as imaging the regions around the event horizon of a super-massive black hole at the center of an active galaxy, can be achieved if beams from parts of the incoming wavefront separated by 100s of meters can be stably and accurately brought together at small angles. One way of achieving this is by using grazing incidence mirrors. We here investigate an alternative approach in which the beams are recombined by optical elements working in transmission. It is shown that the use of diffractive elements is a particularly attractive option. We report experimental results from a simple 2-beam interferometer using a low-cost commercially available profiled film as the diffractive elements. A rotationally symmetric filled (or mostly filled) aperture variant of such an interferometer, equivalent to an X-ray axicon, is shown to offer a much wider bandpass than either a Phase Fresnel Lens (PFL) or a PFL with a refractive lens in an achromatic pair. Simulations of an example system are presented.

Skinner, G. K.↗

X-ray optics - A technique for high resolution imaging

Both scattering and figure errors in grazing incidence optics are larger in the plane of incidence than out-of-plane by a factor equal to 1/sin theta, where theta is the graze angle. When the full annular aperture of a grazing incidence telescope is stopped down, the point spread function becomes highly elliptical with a width as much as sin theta times narrower than the full image. In practice, this means that improvements in resolution of up to 100 times can be achieved, and effective resolution can approach the diffraction limit. Laboratory data demonstrating the effect are presented.

Cash, Webster↗

Correlation of Processing and Structure in an Ethylene‐Glycol Side‐Chain Modified Polythiophene via Combined X‐Ray Scattering and 4D Scanning Transmission Electron Microscopy

The results of a combined grazing incidence wide-angle X-ray scattering (GIWAXS) and 4D scanning transmission microscopy (4D-STEM) analysis of the effects of thermal processing on poly(3[2-(2-methoxyethoxy)ethoxy]-methylthiophene-2,5-diyl) are reported, a conjugated semiconducting polymer used as the active layer in organic electrochemical transistor devices. GIWAXS provides a measure of overall crystallinity in the film, while 4D-STEM produces real-space maps of the morphology and orientation of individual crystallites along with their spatial extent and distribution. The sensitivity of the 4D-STEM detector allows for collection of electron diffraction patterns at each position in an image scan while limiting the imparted electron dose to below the damage threshold. In conclusion, the effects of heat treatment on the distribution and type of crystallites present in the films is determined.

36 MATERIALS SCIENCE↗

Astronomical X-Ray Optics Using Mono-Crystalline Silicon: High Resolution, Light Weight, and Low Cost

X-ray astronomy critically depends on X-ray optics. The capability of an X-ray telescope is largelydetermined by the point-spread function (PSF) and the photon-collection area of its mirrors, the same astelescopes in other wavelength bands. Since an X-ray telescope must be operated above the atmosphere inspace and that X-rays reflect only at grazing incidence, X-ray mirrors must be both lightweight and thin, bothof which add significant technical and engineering challenge to making an X-ray telescope. In this paper wereport our effort at NASA Goddard Space Flight Center (GSFC) of developing an approach to making an Xraymirror assembly that can be significantly better than the mirror assembly currently flying on the ChandraX-ray Observatory in each of the three aspects: PSF, effective area per unit mass, and production cost per uniteffective area. Our approach is based on the precision polishing of mono-crystalline silicon to fabricate thinand lightweight X-ray mirrors of the highest figure quality and micro-roughness, therefore, having thepotential of achieving diffraction-limited X-ray optics. When successfully developed, this approach will makeimplementable in the 2020s and 2030s many X-ray astronomical missions that are currently on the drawingboard, including sounding rocket flights such as OGRE, Explorer class missions such as STAR-X andFORCE, Probe class missions such as AXIS, TAP, and HEX-P, as well as large missions such as Lynx.

Zhang, William W.↗

Monocrystalline Silicon and the Meta-Shell Approach to Building X-Ray Astronomical Optics

Angular resolution and photon-collecting area are the two most important factors that determine the power of an X-ray astronomical telescope. The grazing incidence nature of X-ray optics means that even a modest photon-collecting area requires an extraordinarily large mirror area. This requirement for a large mirror area is compounded by the fact that X-ray telescopes must be launched into, and operated in, outer space, which means that the mirror must be both lightweight and thin. Meanwhile the production and integration cost of a large mirror area determines the economical feasibility of a telescope. In this paper we report on a technology development program whose objective is to meet this three-fold requirement of making astronomical X-ray optics: (1) angular resolution, (2) photon-collecting area, and (3) production cost. This technology is based on precision polishing of monocrystalline silicon for making a large number of mirror segments and on the meta-shell approach to integrate these mirror segments into a mirror assembly. The meta-shell approach takes advantage of the axial or rotational symmetry of an X-ray telescope to align and bond a large number of small, lightweight mirrors into a large mirror assembly. The most important features of this technology include: (1) potential to achieve the highest possible angular resolution dictated by optical design and diffraction; and (2) capable of implementing every conceivable optical design, such as Wolter-I, Wolter-Schwarzschild, as well as other variations to one or another aspect of a telescope. The simplicity and modular nature of the process makes it highly amenable to mass production, thereby making it possible to produce very large X-ray telescopes in a reasonable amount of time and at a reasonable cost. As of June 2017, the basic validity of this approach has been demonstrated by finite element analysis of its structural, thermal, and gravity release characteristics, and by the fabrication, alignment, bonding, and X-ray testing of mirror modules. Continued work in the coming years will raise the technical readiness of this technology for use by SMEX, MIDEX, Probe, as well as major flagship missions.

Zhang, William W.↗

Fabricating Radial Groove Gratings Using Projection Photolithography

Projection photolithography has been used as a fabrication method for radial grove gratings. Use of photolithographic method for diffraction grating fabrication represents the most significant breakthrough in grating technology in the last 60 years, since the introduction of holographic written gratings. Unlike traditional methods utilized for grating fabrication, this method has the advantage of producing complex diffractive groove contours that can be designed at pixel-by-pixel level, with pixel size currently at the level of 45 45 nm. Typical placement accuracy of the grating pixels is 10 nm over 30 nm. It is far superior to holographic, mechanically ruled or direct e-beam written gratings and results in high spatial coherence and low spectral cross-talk. Due to the smooth surface produced by reactive ion etch, such gratings have a low level of randomly scattered light. Also, due to high fidelity and good surface roughness, this method is ideally suited for fabrication of radial groove gratings. The projection mask is created using a laser writer. A single crystal silicon wafer is coated with photoresist, and then the projection mask, with its layer of photoresist, is exposed for patterning in a stepper or scanner. To develop the photoresist, the fabricator either removes the exposed areas (positive resist) of the unexposed areas (negative resist). Next, the patterned and developed photoresist silicon substrate is subjected to reactive ion etching. After this step, the substrate is cleaned. The projection mask is fabricated according to electronic design files that may be generated in GDS file format using any suitable CAD (computer-aided design) or other software program. Radial groove gratings in off-axis grazing angle of incidence mount are of special interest for x-ray spectroscopy, as they allow achieving higher spectral resolution for the same grating area and have lower alignment tolerances than traditional in-plane grating scheme. This is especially critical for NASA Constellation- X project that will utilize hundreds of gratings all of which need to be precisely aligned for x-ray observation of space.

Iazikov, Dmitri↗

GdWN 3 is a nitride perovskite

Nitride perovskites ABN3 are an emerging and highly underexplored class of materials that are of interest due to their intriguing calculated ferroelectric, optoelectronic, and other functional properties. Incorporating novel A-site cations is one strategy to tune and expand such properties; for example, Gd 3+ is compelling due to its large magnetic moment, potentially leading to multiferroic behavior. However, the theoretically predicted ground state of GdWN 3 was a non-perovskite monoclinic structure. Here, we experimentally show that GdWN 3-y crystallizes in a perovskite structure. High-throughput combinatorial sputtering with activated nitrogen is employed to synthesize thin films of Gd 2-x W x N 3-y O y with oxygen content y < 0.05. Ex situ annealing crystallizes a polycrystalline perovskite phase in a narrow composition window near x = 1. LeBail fits of synchrotron grazing incidence wide angle x-ray scattering data are consistent with a perovskite ground-state structure. Refined density functional theory calculations that included antiferromagnetic configurations confirm that the ground-state structure of GdWN 3 is a distorted Pnma perovskite with antiferromagnetic ordering, in contrast to prior predictions. Initial property measurements find that GdWN 3-y is paramagnetic down to T = 2 K with antiferromagnetic correlations and that the absorption onset depends on cation stoichiometry. This work provides an important path toward both the rapid expansion of the emerging family of nitride perovskites and understanding their potential multiferroic properties.

14 SOLAR ENERGY↗

Lamellar and Hexagonal Assemblies of PEG-Grafted Silver Nanoparticles: Implications for Plasmonics and Photonics

Assembly of silver nanoparticles (AgNPs) grafted with thiolated poly(ethylene glycol) (PEG-SH) with various molecular weights is reported. Synchrotron-based X-ray surface-sensitive diffraction methods are used to determine the nature of two-dimensional (2D) assemblies at liquid/vapor interfaces, and small-angle X-ray scattering (SAXS) is used to monitor the three-dimensional (3D) assemblies in bulk suspensions. We find that assembly can be induced either by the addition of K 2 CO 3 or polyacrylic acid (PAA) to the PEG-AgNP aqueous suspensions. The addition of K 2 CO 3 induces a 2D hexagonal structure at the liquid/vapor interface and a 3D hexagonal columnar structure in solutions, where the columns consist of tethered PEG-AgNP chains. On the other hand, the addition of PAA leads to the formation of a 2D lamella-like distorted hexagonal sheet at the liquid/vapor interface and a 3D lamellar superstructure formed by stacked 2D sheets in the PEG-AgNP suspension. Effects of the core type of nanoparticles on the assembly can be used to control structures for potential applications in plasmonics and photonics.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Ion Transport in 2D Nanostructured $\pi$-Conjugated Thieno[3,2- b ]thiophene-Based Liquid Crystal

Leveraging the self-assembling behavior of liquid crystals designed for controlling ion transport is of both fundamental and technological significance. Here, we have designed and prepared a liquid crystal that contains (2,5-bis(5-(2,5,8,11-tetraoxatridecan-13-yl)thiophen-2yl)thieno[3,2-b]thiophene (BTTT) as mesogenic core and conjugated segment and symmetric tetra(ethylene oxide) (EO4) as polar side chains for ionic conducting regions. Driven by the crystallization of the BTTT cores, BTTT/dEO4 exhibits well-ordered smectic phases below 71.5 °C as confirmed by differential scanning calorimetry, polarized optical microscope, temperature dependent wide-angle X-ray scattering and grazing incidence wide-angle X-ray scattering (GIWAXS). We adopted a combination of experimental GIWAXS and molecular dynamics (MD) simulations to better understand the molecular packing of BTTT/dEO4 films, particularly when loaded with the ion conducting salt, lithium bis(trifluoromethanesulfonyl)imide (LiTFSI). Ionic conduction of BTTT/dEO4 is realized by the addition of LiTFSI, with the material able to maintain smectic phases up to r = [Li + ]/[EO] = 0.1. In this work, The highest ionic conductivity of 8 × 10 -3 S/cm was attained at an intermedium salt concentration of r = 0.05. It was also found that ion conduction in BTTT/dEO4 is enhanced by forming a smectic layered structure with irregular interfaces between the BTTT and EO4 layers and by the lateral film expansion upon salt addition. This can be explained by the enhancement of the misalignment and configurational entropy of the side chains, which increase their local mobility and that of the solvated ions. Our molecular design thus illustrates how, beyond the favorable energetic interactions that drive the assembly and ion solvating domains, modulation of entropic effects can also be favorably harnessed to improve ion conduction.

thin film electrochemical impedance spectroscopy↗

Structural stability, elemental ordering, and transport properties of layered ScTaN 2

Ternary transition metal (TM) nitrides have gained significant attention in thin film research due to their promising properties for a broad range of applications. Particularly, some of the ternary TM nitrides have been predicted to adopt layered structures that make them interesting for thermoelectric conversion and quantum materials applications. Unfortunately, synthesis of TM ternary nitride films by physical vapor deposition often favors disordered 3D structures rather than the predicted 2D-like layered structure. In this study, we investigate the structural interplay in the Sc-Ta-N ternary system using a combinatorial approach. Combinatorial libraries S⁢c 𝑥 ⁢T⁢a 1−𝑥 ⁢N are synthesized following a two-step method: First, deposit film precursors by cosputtering and then process the resulting 3D-structured samples with rapid thermal annealing. Synchrotron grazing-incidence wide-angle x-ray scattering on films annealed at 1200 ⁢°⁢C for 20 min leads to the nucleation of ScTaN 2 layered structure (𝑃⁢6 3 /𝑚⁢𝑚⁢𝑐) near stoichiometry. We find that the layered structure can accommodate large off-stoichiometry in the Ta-rich region (𝑥 < 0.5), facilitated by the alloying with quasi-isostructural Ta 5 ⁢N 6 compound that exists on a composition tie line at 𝑥 = 0. While focusing on ScTaN 2 , we estimate the long-range order parameter in near-stoichiometric films to be 0.86, corresponding to a fraction of Sc/Ta antisites of 7%. Transport measurements on ScTaN 2 reveal a nearly temperature-independent high carrier density (10 21 c⁢m −3 ), suggesting a heavily doped semiconductor or semimetallic character, consistent with a small positive Seebeck coefficient of +19 µV/K. The carrier mobility at 2 K is relatively small (9.5c⁢m 2 V −1 s −1 ) and the residual-resistivity ratio is minor, suggesting that electrical conduction is dominated by defects or disorder. Measured magnetoresistance suggests possible weak antilocalization at 2 K. This paper highlights the interplay between ScTaN 2 and Ta 5 ⁢N 6 crystal structures in stabilizing layered materials, emphasizes the importance of cation order/disorder for potential tunable alloys, and suggests that ScTaN 2 is a promising platform for exploring electronic properties.

36 MATERIALS SCIENCE↗

Echelle spectrographs at grazing incidence

It is shown that by using the conical diffraction mount, existing echelle gratings can be used at grazing incidence to achieve high spectral resolution in the extreme UV and soft X rays. Design considerations for grazing incidence echelle spectrographs are examined, and two sample designs are discussed. The first, for use in the extreme UV, has a primary mirror and an entrance slit to the spectrograph. The system has a resolution of 10,000, operates at any wavelength longward of 100 A, and covers 30% of the spectrum at a single setting. The X-ray spectrograph uses objective gratings to obtain spectral resolution of 28,000 over any factor of 2 in. wavelength. It operates to wavelengths as short as 4 A.

Cash, W.↗

High efficiency spectrographs for the EUV and soft X-rays

The use of grazing incidence optics and reflection grating designs is shown to be a method that improves the performance of spectrographs at wavelengths shorter than 1200 A. Emphasis is laid on spectroscopic designs for X ray and EUV astronomy, with sample designs for an objective reflection grating spectrograph (ORGS) and an echelle spectrograph for wavelengths longer than 100 A. Conical diffraction allows operations at grazing incidence in the echelle spectrograph. In ORGS, the extreme distance of X ray objects aids in collimating the source radiation, which encounters conical diffraction within the instrument, proceeds parallel to the optical axis, and arrives at the detector. A series of gratings is used to achieve the effect. A grazing echelle is employed for EUV observations, and offers a resolution of 20,000 over a 300 A bandpass.

Cash, W.↗

Grazing incidence optics; Proceedings of the Meeting, Orlando, FL, Apr. 3, 4, 1986

Papers are presented on the diffraction-limited performance of grazing incidence optical systems; transverse ray aberrations of Wolter type 1 telescopes; hybrid X-ray telescope systems; surface characterization of grazing incidence optics in the extreme UV and X-ray regions; and the surface roughness properties of synchrotron radiation optics. Topics discussed include the simulation of free-abrasive grinding of grazing incidence mirrors with vertical-honing and flexible blades; mirrors for the Extreme Ultraviolet Explorer; the design and development of conical X-ray imaging mirrors; thermal loading considerations for synchrotron radiation mirrors; and grazing incidence optics for synchrotron radiation insertion-device beams. Consideration is given to the interpretation of glancing incidence scattering measurements; damage processes in short wavelength coated FEL optics; the replication of grain incidence optics; and the assembly and alignment of the Technology Mirror Assembly.

Osantowski, John F.↗