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At least 793 records · Page 44

Multiple-Zone Diffractive Optic Element for Laser Ranging Applications

A diffractive optic element (DOE) can be used as a beam splitter to generate multiple laser beams from a single input laser beam. This technology has been recently used in LRO s Lunar Orbiter Laser Altimeter (LOLA) instrument to generate five laser beams that measure the lunar topography from a 50-km nominal mapping orbit (see figure). An extension of this approach is to use a multiple-zone DOE to allow a laser altimeter instrument to operate over a wider range of distances. In particular, a multiple-zone DOE could be used for applications that require both mapping and landing on a planetary body. In this case, the laser altimeter operating range would need to extend from several hundred kilometers down to a few meters. The innovator was recently involved in an investigation how to modify the LOLA instrument for the OSIRIS asteroid mapping and sample return mission. One approach is to replace the DOE in the LOLA laser beam expander assembly with a multiple-zone DOE that would allow for the simultaneous illumination of the asteroid with mapping and landing laser beams. The proposed OSIRIS multiple-zone DOE would generate the same LOLA five-beam output pattern for high-altitude topographic mapping, but would simultaneously generate a wide divergence angle beam using a small portion of the total laser energy for the approach and landing portion of the mission. Only a few percent of the total laser energy is required for approach and landing operations as the return signal increases as the inverse square of the ranging height. A wide divergence beam could be implemented by making the center of the DOE a diffractive or refractive negative lens. The beam energy and beam divergence characteristics of a multiple-zone DOE could be easily tailored to meet the requirements of other missions that require laser ranging data. Current single-zone DOE lithographic manufacturing techniques could also be used to fabricate a multiple-zone DOE by masking the different DOE zones during the manufacturing process, and the same space-compatible DOE substrates (fused silica, sapphire) that are used on standard DOE s could be used for multiple- zone DOE s. DOEs are an elegant and cost-effective optical design option for spacebased laser altimeters that require multiple output laser beams. The use of multiple-zone DOEs would allow for the design and optimization of a laser altimeter instrument required to operate over a large range of target distances, such as those designed to both map and land on a planetary body. In addition to space-based laser altimeters, this technology could find applications in military or commercial unmanned aerial vehicles (UAVs) that fly at an altitude of several kilometers and need to land. It is also conceivable that variations of this approach could be used in land-based applications such as collision avoidance and robotic control of cars, trains, and ships.

Ramos-Izquierdo, Luis A.↗

Fabricating Blazed Diffraction Gratings by X-Ray Lithography

Gray-scale x-ray lithography is undergoing development as a technique for fabricating blazed diffraction gratings. As such, gray-scale x-ray lithography now complements such other grating-fabrication techniques as mechanical ruling, holography, ion etching, laser ablation, laser writing, and electron-beam lithography. Each of these techniques offers advantages and disadvantages for implementing specific grating designs; no single one of these techniques can satisfy the design requirements for all applications. Gray-scale x-ray lithography is expected to be advantageous for making gratings on steeper substrates than those that can be made by electron-beam lithography. This technique is not limited to sawtooth groove profiles and flat substrates: various groove profiles can be generated on arbitrarily shaped (including highly curved) substrates with the same ease as sawtooth profiles can be generated on flat substrates. Moreover, the gratings fabricated by this technique can be made free of ghosts (spurious diffraction components attributable to small spurious periodicities in the locations of grooves). The first step in gray-scale x-ray lithography is to conformally coat a substrate with a suitable photoresist. An x-ray mask (see Figure 1) is generated, placed between the substrate and a source of collimated x-rays, and scanned over the substrate so as to create a spatial modulation in the exposure of the photoresist. Development of the exposed photoresist results in a surface corrugation that corresponds to the spatial modulation and that defines the grating surface. The grating pattern is generated by scanning an appropriately shaped x-ray area mask along the substrate. The mask example of Figure 1 would generate a blazed grating profile when scanned in the perpendicular direction at constant speed, assuming the photoresist responds linearly to incident radiation. If the resist response is nonlinear, then the mask shape can be modified to account for the nonlinearity and produce a desired groove profile. An example of grating grooves generated by this technique is shown in Figure 2. A maximum relative efficiency of 88 percent has been demonstrated.

Mouroulis, Pantazis↗

First X-Ray Diffraction Results from Mars Science Laboratory: Mineralogy of Rocknest Aeolian Bedform at Gale Crater

Numerous orbital and landed observations of the martian surface suggest a reasonably uniform martian soil composition, likely as a result of global aeolian mixing [1, 2]. Chemical data for martian soils are abundant [e.g., 2, 3], and phase information has been provided by lander thermal emission and Moessbauer spectroscopic measurements [3, 4, 5, 6]. However, until now no X-ray diffraction (XRD) data were available for martian soil nor has XRD ever been used on another body apart from Earth. XRD is generally considered the most definitive method for determining the crystalline phases in solid samples, and it is the method of choice for determining mineralogy. CheMin s first XRD analysis on Mars coincided with the 100th anniversary of the discovery of X-ray diffraction by von Laue. Curiosity delivered scooped samples of loose, unconsolidated material ("soil") acquired from an aeolian bedform at the Rocknest locality to instruments in the body of the rover (the laboratory). Imaging shows that the soil has a range of particle sizes, of 1-2 mm and smaller, presumably representing contributions from global, regional, and local sources.

Bish, D. L.↗

Impedance Matched to Vacuum, Invisible Edge, Diffraction Suppressed Mirror

Diffraction suppressed mirrors having an invisible edge are disclosed for incident light at both targeted wavelengths and broadband incident light. The mirrors have a first having at least one discontiguous portion having a plurality of nanostructured apertures. The discontiguous mirror portion impedance matches a relatively high impedance portion of the mirror to a relatively low impedance portion of the mirror, thereby reducing the diffraction edge effect otherwise present in a conventional mirror.

Hagopian, John G.↗

Reaching the Diffraction Limit - Differential Speckle and Wide-Field Imaging for the WIYN Telescope

Speckle imaging allows telescopes to achieve diffraction limited imaging performance. The technique requires cameras capable of reading out frames at a very fast rate, effectively 'freezing out' atmospheric seeing. The resulting speckles can be correlated and images reconstructed that are at the diffraction limit of the telescope. These new instruments are based on the successful performance and design of the Differential Speckle Survey Instrument (DSSI).The instruments are being built for the Gemini-N and WIYN telescopes and will be made available to the community via the peer review proposal process. We envision their primary use to be validation and characterization of exoplanet targets from the NASA, K2 and TESS missions and RV discovered exoplanets. Such targets will provide excellent follow-up candidates for both the WIYN and Gemini telescopes. We expect similar data quality in speckle imaging mode with the new instruments. Additionally, both cameras will have a wide-field mode and standard SDSS filters. They will be highly versatile instruments and it is that likely many other science programs will request time on the cameras. The limiting magnitude for speckle observations will remain around 13-14th at WIYN and 16-17th at Gemini, while wide-field, normal CCD imaging operation should be able to go to much fainter, providing usual CCD imaging and photometric capabilities. The instruments will also have high utility as scoring cameras for telescope engineering purposes, or other applications where high time resolution is needed. Instrument support will be provided, including a software pipeline that takes raw speckle data to fully reconstructed images.

detector↗

Crystallographic Characterization of Extraterrestrial Materials by Energy-Scanning X-ray Diffraction

We have continued our long-term project using X-ray diffraction to characterize a wide range of extraterrestrial samples. The stationary sample method with polychromatic X-rays is advantageous because the irradiated area of the sample is always same and fixed, meaning that all diffraction spots occur from the same area of the sample, however, unit cell parameters cannot be directly obtained by this method though they are very important for identification of mineral and for determination of crystal structures. In order to obtain the cell parameters even in the case of the sample stationary method, we apply energy scanning of a micro-beam of monochromatic SR at SPring-8.

Hagiya, Kenji↗

Curved Diffractive X-ray Optics for X-ray Astronomy

We report on a concept for curved diffractive X-ray optics (CDXO). CDXO would enable potential new optical designs for X-ray instruments, such as a two element spectrometer, in which the secondary element of an X-ray mirror pair is patterned with an X-ray grating. A two-element spectrometer design eliminates the grating assembly, resulting in decreased instrument mass and reduced power requirements. In addition, a two-element spectrometer may realize cost/schedule savings by eliminating a separate grating alignment effort, and yield increased effective area over three element designs. We present a raytrace concept study of a two-element spectrometer compact enough to fit within a sounding rocket payload. We also review the progress made in electron-beam lithography (EBL) techniques that would enable curved diffractive X-ray optics to be patterned, and outline a procedure by which the accuracy of the EBL patterning process can be measured interferometrically.

Casey T. DeRoo↗

Materials Characterization Using X-Ray Diffraction

This talk for the Spring Meeting of the Ohio Section of the American Association of Physics Teachers begins with a brief description of what X-Ray diffraction is, and relates 2D diffraction (grating equation) to 3D (Bragg’s law). Various examples of how XRD can be used to answer a variety of materials science questions will be discussed along with some of how XRD has been used at NASA Glenn.

Laura Wilson↗

Development of Large-Volume-Diamond Anvil Cell for Neutron Diffraction: The Neutron Diamond Anvil Cell Project at ORNL

10 years ago, Dave Mao, director of EFree (energy frontier research in extreme environments), a DOE energy frontier recognized the importance of neutron science for energy research. The subsequent establishment of a neutron group within EFree lead to the establishment of an “Instrument Development Team” for SNAP, the High-Pressure beamline at the Spallation Neutron Source at Oak Ridge National Laboratory in Tennessee. The idea was to develop novel high pressure techniques to expand the pressure range for neutron diffraction. A goal was set to reach half megabar levels (50 GPa), which at the time was considered as extremely challenging. Here we will give a brief overview of the developments during the last decade in this novel area of research. Fortunately, during this period multi carat diamond anvils have become available mainly by the chemical vapor deposition process (CVD), making research in this pressure range and beyond rather routine. This paper shows the latest developments in large anvil designs, compact multiple ton diamond cells and some examples of high-quality neutron diffraction patterns of sample sizes far below conventional levels.

Boehler, Reinhard↗

Using In Situ High-Energy X-ray Diffraction to Quantify Electrode Behavior of Li-Ion Batteries from Extreme Fast Charging

Extreme fast charging (XFC, =15 min charging time) of Li-ion batteries (LIBs) has been proposed as an immediate target to increase the commercial appeal of electric vehicles. However, XFC of LIBs is associated with the degradation of battery performance and safety concerns. Quantitative and simultaneous characterization of various components during cell degradation represents a major experimental challenge. In this work, we outline a methodology for the use of spatially resolved, high-energy X-ray diffraction as a quantitative, in situ method of mapping the degradation of LIBs. We use this approach to study the battery cell capacity loss, both locally (mm scale) and globally over the entire cell (cm scale). Specifically, our workflow allows us to quantify the total amount of plated Li on the anode, as well as its spatial correlation to the structural properties of the anode and cathode. The method complements existing optical methods to resolve the spatial heterogeneity of local degradation mechanisms such as Li plating and provides simultaneous insights into concomitant anode state-of-charge variability. We apply it to commercially relevant single-layer pouch cells with the graphite anode and the LiNi 0.5 Mn 0.3 Co 0.2 O 2 cathode. Our results show that Li plating occurs heterogeneously on the graphite anode and that it is spatially correlated to the extent of anode lithiation. In this work, we anticipate that the described workflow will allow for understanding multiscale degradation in energy-storage devices beyond LIBs, where quantitative analysis at a local and global length scale can be performed without the necessity to tear down the device, due to the applicability of high-energy X-rays to probe in situ degradation.

25 ENERGY STORAGE↗

Utah FORGE Well 16A(78)-32 X-ray Diffraction Data

This submission contains x-ray diffraction data taken from 3,600 to 10,987 feet deep in well 16A(78)-32 in the Roosevelt Hot Springs Geothermal Area as part of the Utah FORGE project. 78 rock samples were taken. Samples are taken in a range of ten feet at 100 foot increments. Mineral abundances are given in weight percent of the sample, with results rounded to the nearest whole number. Fields marked with tr (trace) indicate that mineral is present, but that its abundance calculated from the Rietveld refinement was less than one weight percent; that it was observed in the clay-sized fraction, but not the bulk; and/or that it was observed in low abundance during petrographic analyses. The samples were taken between 10/29/2020 and 12/24/2020 during the drilling of well 16A(78)-32.

15 GEOTHERMAL ENERGY↗

A New Residual Strain Mapping Program Using Energy Dispersive X-Ray Diffraction at the Advanced Photon Source

Here, the ability to non-destructively map the residual strain field inside an engineering component is important for predicting its fatigue life or developing processing methods to prevent failure or enhance performance. In this paper, we describe a new residual strain mapping program at the Advanced Photon Source, Argonne National Laboratory. The new program is based on energy dispersive x-ray diffraction (EDXRD). It is capable of non-destructively penetrating a several- cm thick polycrystalline sample fabricated from engineering alloys using high-energy x-rays and measuring the residual strain field with mm or better spatial resolution and approximately ±1 x 10 -4 strain resolution. A multi-element detector array is employed to measure multiple strain components simultaneously. The residual strain mapping setup is augmented with a high-energy tomography capability, allowing precise alignment of the material volume of interest for residual strain mapping and providing a complementary view of the structure to understand the measured strain field. These measurement capabilities are demonstrated using several strain mapping examples ranging from polycrystalline structural alloys to biological materials. We also provide some guidance for the future users of the program for a successful residual strain mapping experiment. We are expanding the capabilities of the new setup with various in situ capabilities including thermo-mechanical loading.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Direct measurement of the effective properties of an additively manufactured titanium octet truss unit cell using high energy X-ray diffraction

Additively manufactured lattice structures offer a high specific strength-to-density ratio in comparison to conventional, fully dense parts. The small feature size and intricate geometry of lattice structures make it challenging to directly characterize their mechanical properties. This study presents direct measurement of the elastic mechanical properties of an additively manufactured titanium alloy octet truss unit cell. Strut stress and strain were measured using high-energy X-ray diffraction during quasi-static compressive loading. The crystallographic stress-strain relationship was converted into the stress-strain relationship of the octet truss lattice unit cell using the known symmetry of the struts. The sample studied herein was best fit by an orthorhombic linear elastic stress-strain relationship. In conclusion, this technique shows promise for studying additively manufactured lattice structures at length scales not previously reported.

36 MATERIALS SCIENCE↗

Multicycle flash sintering of cubic Y 2 O 3 -stabilized ZrO 2 : An in situ energy dispersive synchrotron x-ray diffraction study with high temporal resolution

The current induced unit cell volume changes, (111) Bragg peak full width at half maximum (FWHM) and its integrated intensity in 8 % Y 2 O 3 stabilized ZrO 2 (8 %YSZ) solid state electrolyte was monitored during a triple-flash sintering experiment by in situ energy dispersive x-ray diffraction using a polychromatic synchrotron probe (max, photon energy 200 keV) with 2 second temporal resolution. The first spontaneous singularity in the unit cell volume (+0.54 %) was observed at 899 °C under 15 V/mm applied field intensity, which was associated with 13 mA/mm 2 current draw and an increase in density to 97 %. Following anelastic relaxation of the unit cell volume under open circuit conditions, the same applied field was applied twice in a row which resulted in additional induced singularities at 925 °C (+0.48 %) and 944 °C (+0.42 %). A floating baseline, which was above the thermal expansion baseline, was observed from 833 to 969 °C and was attributed to Joule heating. In conclusion, the singularity at 899 °C is associated with a sharp change in (111) FWHM and a 34 % decrease in integrated peak area that was attributed to changes in the distribution of oxygen vacancies and the changes in their concentration as induced by the applied field in the spontaneous transient stage of flash sintering.

36 MATERIALS SCIENCE↗

Valence Electron Distributions from Sub-Angstrom Convergent Beam Electron Diffraction

Modern aberration-corrected scanning transmission electron microscopes can acquire four-dimensional data sets (“4D STEM”) by recording convergent beam electron diffraction (CBED) patterns, using precisely positioned, sub-angstrom probes. Here, we demonstrate that these patterns can probe the site symmetry, atomic displacements, and valence electron distributions at individual atomic columns. To this end, 4D STEM CBED patterns were acquired from SrTiO 3 single crystals and compared with patterns calculated using scattering potentials derived from density functional theory. Here, we show that an aspherical valence electron charge build-up at the oxygen sites causes intensity asymmetries in the low-angle scattering portion of the patterns. Using strained SrTiO 3 films containing subtle polar displacements within nanometer-sized domains, it is shown that the high-angle scattering portion in each pattern is sensitive to atomic displacements.

36 MATERIALS SCIENCE↗

Photodissociation of aqueous I3− observed with liquid-phase ultrafast mega-electron-volt electron diffraction

Developing femtosecond resolution methods for directly observing structural dynamics is critical to understanding complex photochemical reaction mechanisms in solution. We have used two recent developments, ultrafast mega-electron-volt electron sources and vacuum compatible sub-micron thick liquid sheet jets, to enable liquid-phase ultrafast electron diffraction (LUED). We have demonstrated the viability of LUED by investigating the photodissociation of tri-iodide initiated with a 400 nm laser pulse. This has enabled the average speed of the bond expansion to be measured during the first 750 fs of dissociation and the geminate recombination to be directly captured on the picosecond time scale.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Imaging the Renner–Teller effect using laser-induced electron diffraction

Structural information on electronically excited neutral molecules can be indirectly retrieved, largely through pump–probe and rotational spectroscopy measurements with the aid of calculations. Here, we demonstrate the direct structural retrieval of neutral carbonyl disulfide (CS 2 ) in the B ~ 1 B 2 excited electronic state using laser-induced electron diffraction (LIED). We unambiguously identify the ultrafast symmetric stretching and bending of the field-dressed neutral CS 2 molecule with combined picometer and attosecond resolution using intrapulse pump–probe excitation and measurement. We invoke the Renner–Teller effect to populate the B ~ 1 B 2 excited state in neutral CS 2 , leading to bending and stretching of the molecule. Our results demonstrate the sensitivity of LIED in retrieving the geometric structure of CS 2 , which is known to appear as a two-center scatterer.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗

X-ray diffraction study of phase transformation dynamics of Fe and Fe-Si alloys along the shock Hugoniot using an x-ray free electron laser

The x-ray free electron laser (XFEL) enables probing a highly compressed material response at the subnanosecond timescale. Here we exploit the ultrafast XFEL pulse to combine reflection x-ray diffraction and laser-driven shock compression to perform a study of the phase transformation and stability in Fe and Fe-Si alloys. Our approach enables us to observe that solid-solid phase transformations occur in Fe and Fe- Si 8.5 wt % in ≤ 130 ps at ~ 130 GPa; no transformation is observed in Fe- Si 16 wt % up to 110 GPa. Density functional theory calculations predict similar phase relations.

36 MATERIALS SCIENCE↗