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Optical science and technology concepts for a large deployable reflector for far-infrared and submillimeter astronomy from above the earth's atmosphere are discussed. Requirements given at the Asilomar Conference are reviewed. The technical challenges of this large-aperture (about 20-meter) telescope, which will be diffraction limited in the infrared, are highlighted in a brief discussion of one particular configuration.
Three phase plates were designed to simulate the JWST segmented primary mirror wavefront at three on-orbit alignment stages: coarse phasing, intermediate phasing, and fine phasing. The purpose is to verify JWST's on-orbit wavefront sensing capability. Amongst the three stages, coarse alignment is defined to have piston error between adjacent segments being 30 m to 300 m, intermediate being 0.4 m to 10 m, and fine is below 0.4 m. The phase plates were made of fused silica, and were assembled in JWST Optical Simulator (OSIM). The piston difference was realized by the thickness difference of two adjacent segments. The two important parameters to phase plates are piston and wavefront errors. Dispersed Fringe Sensor (DFS) method was used for initial coarse piston evaluation, which is the emphasis of this paper. Point Diffraction Interferometer (PDI) is used for fine piston and wavefront error. In order to remove piston's 2 pi uncertainty with PDI, three laser wavelengths, 640nm, 660nm, and 780nm, are used for the measurement. The DHS test setup, analysis algorithm and results are presented. The phase plate design concept and its application (i.e. verifying the JWST on-orbit alignment algorithm) are described. The layout of JWST OSIM and the function of phase plates in OSIM are also addressed briefly.
This dataset features petrographic, X-Ray Diffraction (XRD), and Scanning Electron Microscopy Analyses of core samples from well 16A(78)-32, which serves as the injection well for the Utah FORGE Enhanced Geothermal System (EGS) project. In addition to an overview of the analysis, the following items have been included here: images of 21 entire thin sections in plane-polarized and cross-polarized light from 16 depths, scanning electron microscope back scatter electron photomosaic maps of 21 thin sections from 16 depths, bulk XRD data from 16 depths, clay-sized XRD patterns from 16 depths, an optical petrography report, and scanning electron microscopy and energy dispersive spectroscopy analyses of eight selected samples.
Photonic crystals are extensively explored to replace inorganic pigments and organic dyes as coloring elements in printing, painting, sensing, and anti-counterfeiting due to their brilliant structural colors, chemical stability, and environmental friendliness. However, most existing photonic-crystal-based pigments can only display monochromatic colors once made, and generating multicolors has to start with designing different building blocks. In this work, a novel photonic pigment featuring highly tunable structural colors in the entire visible spectrum, made by the magnetic assembly of monodisperse nanorods into body-centered-tetragonal photonic crystals, is reported. Their prominent magnetic and crystal anisotropy makes it efficient to generate multicolors using one photonic pigment by magnetically controlling the crystal orientation. Further, the combination of angle-dependent diffraction and magnetic orientation control enables the design of rotation-asymmetric photonic films that display distinct patterns and encrypted information in response to rotation. The efficient multicolor generation through precise orientational control makes this novel photonic pigment promising in developing high-performance structural-colored materials and optical devices.
The development of large pore single-crystalline covalently linked organic frameworks is critical in revealing the detailed structure-property relationship with substrates. One emergent approach is to photo-crosslink hydrogen-bonded molecular crystals. Introducing complementary hydrogen-bonded carboxylic acid building blocks is promising to construct large pore networks, but these molecules often form interpenetrated networks or non-porous solids. In this report we introduced heteromeric carboxylic acid dimers to construct a non-interpenetrated molecular crystal. Crosslinking this crystal precursor with dithiols afforded a large pore single-crystalline hydrogen-bonded crosslinked organic framework H C OF-101. X-ray diffraction analysis revealed H C OF-101 as an interlayer connected hexagonal network, which possesses flexible linkages and large porous channels to host a hydrazone photoswitch. Multicycle Z/E-isomerization of the hydrazone took place reversibly within H C OF-101, showcasing the potential use of H C OF-101 for optical information storage.
Understanding build-scale microstructural variation in wire arc additive manufacturing (WAAM) of low-carbon steels is essential for ensuring consistent structure–property relationships throughout large components. Conventional destructive characterization techniques, such as scanning electron microscopy (SEM) and electron backscatter diffraction (EBSD), are time-intensive and limited to localized regions, making comprehensive evaluation of large WAAM structures challenging. In this study, a nondestructive ultrasonic approach was employed to characterize a 252 mm tall ER70S-6 S-curved WAAM wall produced using a triple-bead deposition strategy. Optical and SEM analysis revealed a repeating dual-region microstructure consisting of uniform polygonal ferrite at melt pool centers and heterogeneous ferrite with coarse and fine grains near melt pool boundaries, attributed to cyclic thermal conditions. Longitudinal ultrasonic backscatter imaging was used to evaluate the continuity of this periodicity along the full build height. The ultrasonic response exhibited a consistent repeating pattern that correlated with the observed layer-wise microstructural variation. X-ray computed tomography confirmed the absence of detectable porosity, indicating that ultrasonic contrast is primarily governed by grain morphology. Overall, the results indicate that longitudinal backscatter ultrasound is a promising nondestructive characterization technique for validating microstructural variations along the s-curved WAAM wall, with significant potential for microstructure optimization and process control.
Conjugated polymer (CP) materials that are considered as an attractive choice for various electronic and optoelectronic applications possess highly heterogeneous complex structures that can span several orders of magnitude in length scale. This is due to the intricate coupling effects of weak secondary interactions and entropic forces that determine molecular organization in bulk polymer materials. Understanding the influence of molecular interactions on the emergence and evolution of nano- and microscale structures is of paramount importance to the guided design and development of condensed CP materials. Such understanding is even more critical for the rational design of hierarchical systems away from equilibrium, where weak molecular interactions can guide the system along competing kinetic pathways toward local energy minima and metastable architectures. In this work, we studied a promising concept for accessing various kinetically stabilized semi-crystalline CP nanostructures that are formed in the process of controlled chain-growth Kumada catalyst-transfer polymerization initiated by a small-molecule catalytic species which can exist in equilibrium between free and aggregated states. Specifically, we chose a small-molecule perylenedicarboximide (PDCI) polymerization catalytic initiator which has a strong tendency toward reversible supramolecular assembly–disassembly that can be controlled by temperature. Addition of a thiophene monomer to a solution of the PDCI initiator starts the chain-growth polymerization process, which produces distinct nanoscale semi-crystalline polythiophene structures formed under predominant kinetic control. Furthermore, we demonstrated that, depending on the reaction temperature (which affects the fine balance between the position of PDCI assembly–disassembly equilibrium, rate of polymerization, and solvent–solute interactions for the growing polythiophene chains), a range of kinetically trapped hierarchically organized semi-crystalline CP systems with substantially varying optoelectronic properties could be obtained. In addition to spectroscopic and electron microscopic studies, in order to better reveal the structural aspects of the generated polymer nanoscale systems, we carried out a series of X-ray diffraction and neutron scattering experiments which indicated complex hierarchical organization in these kinetically stabilized CP assembled materials. We expect that this in situ polymerization-based approach can lead to a general way to expand access to various semi-crystalline CP nanostructured materials with broadly tunable electronic and optical properties.
Perovskite cobaltites have emerged as archetypes for electrochemical control of materials properties in electrolyte-gate devices. Voltage-driven redox cycling can be performed between fully oxygenated perovskite and oxygen-vacancy-ordered brownmillerite phases, enabling exceptional modulation of the crystal structure, electronic transport, thermal transport, magnetism, and optical properties. The vast majority of studies, however, have focused heavily on the perovskite and brownmillerite end points. In contrast, here we focus on hysteresis and reversibility across the entire perovskite ↔ brownmillerite topotactic transformation, combining gate-voltage hysteresis loops, minor hysteresis loops, quantitative operando synchrotron X-ray diffraction, and temperature-dependent (magneto)transport, on ion-gel-gated ultrathin (10-unit-cell) epitaxial La 0.5 Sr 0.5 CoO 3-δ films. Further, gate-voltage hysteresis loops combined with operando diffraction reveal a wealth of new mechanistic findings, including asymmetric redox kinetics due to differing oxygen diffusivities in the two phases, nonmonotonic transformation rates due to the first-order nature of the transformation, and limits on reversibility due to first-cycle structural degradation. Minor loops additionally enable the first rational design of an optimal gate-voltage cycle. Combining this knowledge, we demonstrate state-of-the-art nonvolatile cycling of electronic and magnetic properties, encompassing >10 5 transport ON/OFF ratios at room temperature, and reversible metal-insulator-metal and ferromagnet-nonferromagnet-ferromagnet cycling, all at 10-unit-cell thickness with high room-temperature stability. This paves the way for future work to establish the ultimate cycling frequency and endurance of such devices.
X-ray crystallography is one of the leading tools to analyze the 3-D structure, and therefore, function of proteins and other biological macromolecules. Traditional methods of mounting individual crystals for X-ray diffraction analysis can be tedious and result in damage to fragile protein crystals. Furthermore, the advent of multi-crystal and serial crystallography methods explicitly require the mounting of larger numbers of crystals. To address this need, we have developed a device that facilitates the straightforward mounting of protein crystals for diffraction analysis, and that can be easily manufactured at scale. Inspired by grid-style devices that have been reported in the literature, we have developed an X-ray compatible microfluidic device that can be used to trap protein crystals in an array configuration, while also providing excellent optical transparency, a low X-ray background, and compatibility with the robotic sample handling and environmental controls used at synchrotron macromolecular crystallography beamlines. At the Stanford Synchrotron Radiation Lightsource (SSRL), these capabilities allow for fully remote-access data collection at controlled humidity conditions. Furthermore, we have demonstrated continuous manufacturing of these devices via roll-to-roll fabrication to enable cost-effective and efficient large-scale production.
Controlling the multi-level assembly and morphological properties of conjugated polymers through structural manipulation has contributed significantly to the advancement of organic electronics. In this work, a redox active conjugated polymer, TPT–TT, composed of alternating 1,4-(2-thienyl)-2,5-dialkoxyphenylene (TPT) and thienothiophene (TT) units is reported with non-covalent intramolecular S⋯O and S⋯H–C interactions that induce controlled main-chain planarity and solid-state order. As confirmed by density functional theory (DFT) calculations, these intramolecular interactions influence the main chain conformation, promoting backbone planarization, while still allowing dihedral rotations at higher kinetic energies (higher temperature), and give rise to temperature-dependent aggregation properties. Thermotropic liquid crystalline (LC) behavior is confirmed by cross-polarized optical microscopy (CPOM) and closely correlated with multiple thermal transitions observed by differential scanning calorimetry (DSC). This LC behavior allows us to develop and utilize a thermal annealing treatment that results in thin films with notable long-range order, as shown by grazing-incidence X-ray diffraction (GIXD). Specifically, we identified a first LC phase, ranging from 218 °C to 107 °C, as a nematic phase featuring preferential face-on π–π stacking and edge-on lamellar stacking exhibiting a large extent of disorder and broad orientation distribution. A second LC phase is observed from 107 °C to 48 °C, as a smectic A phase featuring sharp, highly ordered out-of-plane lamellar stacking features and sharp tilted backbone stacking peaks, while the structure of a third LC phase with a transition at 48 °C remains unclear, but resembles that of the solid state at ambient temperature. Furthermore, the significance of thermal annealing is evident in the ∼3-fold enhancement of the electrical conductivity of ferric tosylate-doped annealed films reaching 55 S cm −1 . More importantly, thermally annealed TPT–TT films exhibit both a narrow distribution of charge-carrier mobilities (1.4 ± 0.1) × 10 −2 cm 2 V −1 s −1 along with a remarkable device yield of 100% in an organic field-effect transistor (OFET) configuration. This molecular design approach to obtain highly ordered conjugated polymers in the solid state affords a deeper understanding of how intramolecular interactions and repeat-unit symmetry impact liquid crystallinity, solution aggregation, solution to solid-state transformation, solid-state morphology, and ultimately device applications.
Precision optics have been widely required in many advanced technological applications. X-ray mirrors, as an example, serve as the key optical components at synchrotron radiation and free electron laser facilities. They are rectangular silicon or glass substrates where a rectangular Clear Aperture (CA) needs to be polished to sub-nanometer Root Mean Squared (RMS) to keep the imaging capability of the incoming X-ray wavefront at the diffraction limit. The convolutional polishing model requires a CA to be extended with extra data, from which the dwell time is calculated via deconvolution. However, since deconvolution is very sensitive to boundary errors and noise, the existing surface extension methods can hardly fulfill the sub-nanometer requirement. On one hand, the figure errors in a CA were improperly modeled during the extension, leading to continuity issues along the boundary. On the other hand, uncorrectable high-frequency errors and noise were also extended. In this study, we propose a novel Robust Iterative Surface Extension (RISE) method that resolves these problems with a data fitting strategy. RISE models the figure errors in a CA with orthogonal polynomials and ensures that only correctable errors are fit and extended. Combined with boundary conditions, an iterative refinement of dwell time is then proposed to compensate the errors brought by the extension and deconvolution, which drastically reduces the estimated figure error residuals in a CA while the increase of total dwell time is negligible. To our best knowledge, RISE is the first data fitting-based surface extension method and is the first to optimize dwell time based on iterative extension. An experimental verification of RISE is given by fabricating two elliptic cylinders (10 mm × 80 mm CAs) starting from a sphere with a radius of curvature around 173 m using ion beam figuring. The figure errors in the two CAs greatly improved from 204.96 nm RMS and 190.28 nm RMS to 0.62 nm RMS and 0.71 nm RMS, respectively, which proves that RISE is an effective method for sub-nanometer level X-ray mirror fabrication.
A Uniform Theory of Diffraction (UTD) model for the principal-plane radar cross section (RCS) of a perfectly conducting, rectangular plate coated on one side with an electrically thin (t much less than lambda), lossy dielectric is presented. The incorporation of higher-order, multiple diffractions and of multiply diffracted surface-waves is discussed in detail. It is demonstrated that these terms are crucial to obtaining an accurate model. Approximations that are used in the model are discussed. Suggestions for improvements to the model are made. Validation is provided via comparison with experimental data and a physical optics (PO) model.
The WFIRST/AFTA 2.4 m space telescope currently under study includes a stellar coronagraph for the imaging and spectral characterization of extrasolar planets. Based largely on performance predictions from end-to-end optical propagation modeling, promising coronagraphic methods were selected in late 2013 for further consideration for use on AFTA. Since those downselect analyses further modeling work has been done on evaluating refined coronagraph designs, wavefront sensing and control, detector representation, and time-dependent effects. Thermal, structural, ray trace, and diffraction propagation models are used in these studies. Presented here is the progress to date and plans for future analyses.
Colloidal quantum dots (QDs) and their thin films are increasingly used in electronic and photonic devices replacing traditional bulk semiconductors. However, thermal properties of QDs remain underexplored relative to device development efforts. This study shows the use of time-resolved X-ray diffraction as a contact-free method to probe the thermal response of QDs in environments representative of the active layer in QD optoelectronic devices, providing in situ insights for future thermal management strategies. Through the extraction of Debye–Waller factors on a subnanosecond time scale, we directly capture the heating and cooling of core/shell CdSe/CdS QDs following pulsed optical excitation. In a QD thin film that actively provides optical gain, the thermal conductivity is found to be as low as 0.13 W m –1 K –1 , because of the poor heat flow between close-packed QD solids. For QDs dispersed in liquids, interfacial thermal conductance dominates thermal relaxation, with a conductance of 15 MW m –2 K –1 .
Ptychography is a rapidly developing scanning microscopy which is able to view the internal structures of samples at a high resolution beyond the illumination size. The achieved spatial resolution is theoretically dose-limited. A broadband source can provide much higher flux compared with a monochromatic source; however, it conflicts with the necessary coherence requirements of this coherent diffraction imaging technique. In this paper, a multi-wavelength reconstruction algorithm has been developed to deal with the broad bandwidth in ptychography. Compared with the latest development of mixed-state reconstruction approach, this multi-wavelength approach is more accurate in the physical model, and also considers the spot size variation as a function of energy due to the chromatic focusing optics. Therefore, this method has been proved in both simulation and experiment to significantly improve the reconstruction when the source bandwidth, illumination size and scan step size increase. It is worth mentioning that the accurate and detailed information of the energy spectrum for the incident beam is not required in advance for the proposed method. Further, we combine multi-wavelength and mixed-state approaches to jointly solve temporal and spatial partial coherence in ptychography so that it can handle various disadvantageous experimental effects. The significant relaxation in coherence requirements by our approaches allows the use of high-flux broadband X-ray sources for high-efficient and high-resolution ptychographic imaging.
A majority of Sun-like stars have at least one stellar companion that can introduce additional noise into the field of view of any high-contrast imaging instrument, limiting the achievable contrast. These include high-quality target stars such as the A and B components of Alpha Centauri, our nearest stellar neighbor. Enabling direct imaging of binary stars has the potential to increase the scientific yield for coronagraphic instruments planned on NASA's future space missions and concepts, including the Roman Space Telescope and the Astro2020 IR/O/UV flagship. Multi-Star Wavefront Control (MSWC) is a wavefront-control technique that simultaneously removes the (mutually incoherent) stellar leakage from both stellar components, enabling direct imaging of planets in many binary star systems. MSWC is an algorithmic technique and can be used with existing wavefront control systems on coronagraphic instruments (as well as starshades if a deformable mirror is available in the optical path) including planned observations on the upcoming PICTURE-D balloon flight. We report on the latest experimental and numerical results obtained with MSWC as part of the technology development effort to demonstrate compatibility with existing high-contrast imaging platforms for this technique. We first report on functional tests carried out at Subaru's SCExAO instrument operating in-air and showing the sub-Nyquist mode at 4.1e-6 contrast in monochromatic light. The Super-Nyquist regime of MSWC was recently tested in vacuum at JPL's High Contrast Imaging Testbed (HCIT) on the Decadal Survey Testbed (DST) reaching 8.6e-9 contrast in a 10% band. We also report on results for the current stage of vacuum testing at HCIT's Occulting Mask Coronagraph (OMC) testbed using a mask similar to the contributed MSWC mask on the Roman Space Telescope's coronagraph instrument which has demonstrated suppression at the 9.8e-9 contrast at Super-Nyquist separations around the 3rd diffraction order and is planned to use a novel binary source simulator.
Abstract The structures, strain fields, and defect distributions in solid materials underlie the mechanical and physical properties across numerous applications. Many modern microstructural microscopy tools characterize crystal grains, domains and defects required to map lattice distortions or deformation, but are limited to studies of the (near) surface. Generally speaking, such tools cannot probe the structural dynamics in a way that is representative of bulk behavior. Synchrotron X-ray diffraction based imaging has long mapped the deeply embedded structural elements, and with enhanced resolution, dark field X-ray microscopy (DFXM) can now map those features with the requisite nm-resolution. However, these techniques still suffer from the required integration times due to limitations from the source and optics. This work extends DFXM to X-ray free electron lasers, showing how the $$10^{12}$$ 10 12 photons per pulse available at these sources offer structural characterization down to 100 fs resolution (orders of magnitude faster than current synchrotron images). We introduce the XFEL DFXM setup with simultaneous bright field microscopy to probe density changes within the same volume. This work presents a comprehensive guide to the multi-modal ultrafast high-resolution X-ray microscope that we constructed and tested at two XFELs, and shows initial data demonstrating two timing strategies to study associated reversible or irreversible lattice dynamics.
In the present study, two industry primary and secondary zinc dialkyldithiophosphate standards, ZDDP1 and ZDDP2, respectively, are evaluated for their impact on the performance of Pd-based three-way catalyst and bench-marked against two mixed lubricant additives formed from either ZDDP1 or ZDDP2 with a second-generation oil-miscible phosphoric-containing ionic liquid (IL). The three-way catalysts (TWCs) are exposed to the lubricant additives in an engine bench under four different scenarios: a base case with no additive (NA), ZDDP1, IL+ZDDP1, ZDDP2, and IL+ZDDP2. The engine-aged TWC samples are characterized through a variety of analytical techniques, including evaluation of catalyst reactivity in a bench-flow reactor. With respect to the water–gas shift reaction and the oxygen storage capacity, the ZDDP2- and IL+ZDDP2-aged TWC samples are more degraded than the ZDDP1- and IL+ZDDP1-aged TWC samples. X-ray diffraction (XRD) patterns indicate that phosphorus in the form of CePO4 was found to be present in the washcoat of all TWC samples, with the highest amount found in the ZDDP2-aged TWC sample. The results obtained from XRD are further confirmed by those from inductively coupled plasma-optical emission spectroscopy (ICP-OES), which show that more phosphorus is detected in the washcoat of ZDDP2- and IL+ZDDP2-aged TWC samples than in the ZDDP1- and IL+ZDDP1-aged TWC samples.