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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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At least 19 records
All sourcesNASA NTRSDOE OSTI
NASA NTRS2001

Laboratory multiple-crystal X-ray topography and reciprocal-space mapping of protein crystals: influence of impurities on crystal perfection

Double-axis multiple-crystal X-ray topography, rocking-curve measurements and triple-axis reciprocal-space mapping have been combined to characterize protein crystals using a laboratory source. Crystals of lysozyme and lysozyme crystals doped with acetylated lysozyme impurities were examined. It was shown that the incorporation of acetylated lysozyme into crystals of lysozyme induces mosaic domains that are responsible for the broadening and/or splitting of rocking curves and diffraction-space maps along the direction normal to the reciprocal-lattice vector, while the overall elastic lattice strain of the impurity-doped crystals does not appear to be appreciable in high angular resolution reciprocal-space maps. Multiple-crystal monochromatic X-ray topography, which is highly sensitive to lattice distortions, was used to reveal the spatial distribution of mosaic domains in crystals which correlates with the diffraction features in reciprocal space. Discussions of the influence of acetylated lysozyme on crystal perfection are given in terms of our observations.

Muramidase/chemistry↗
DOE OSTI2021

Macromolecular phasing using diffraction from multiple crystal forms

A phasing algorithm for macromolecular crystallography is proposed that utilizes diffraction data from multiple crystal forms – crystals of the same molecule with different unit-cell packings (different unit-cell parameters or space-group symmetries). The approach is based on the method of iterated projections, starting with no initial phase information. The practicality of the method is demonstrated by simulation using known structures that exist in multiple crystal forms, assuming some information on the molecular envelope and positional relationships between the molecules in the different unit cells. With incorporation of new or existing methods for determination of these parameters, the approach has potential as a method for ab initio phasing.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
NASA NTRS2022

High-precision predictions of properties of chemically disordered crystals

Multiple scattering theory (MST) combined with density functional theory (DFT) allows to predict properties of chemically disordered materials from the first principles. However, such predictions often suffer from the systematic errors, which depend on crystal geometry. Each computed property of a particular crystal structure typically has a relatively small random error and a larger systematic error. Cancellation of systematic errors allows more accurate predictions. We propose a computational methodology based on the subtraction of the systematic errors in MST. To exemplify it, we apply it to the precipitated alloys. Considering precipitation strengthening in Ni superalloys, we compute the relative enthalpies of the competing Ni_3(Al_{1-x}Ti_x)_1 crystal structures with a chemical disorder on the Al+Ti sublattice. Such predicted composition-structure-property dependencies are useful for the guided design of the next-generation alloys with improved strength. Our predictions are validated by comparison with the results of other DFT methods (having a higher computational cost) and with experiment.

density functional theory↗
NASA NTRSDate not supplied

High-precision predictions of properties of chemically disordered crystals

Multiple scattering theory (MST) combined with density functional theory (DFT) allows to predict properties of chemically disordered materials from the first principles. However, such predictions often suffer from the systematic errors, which depend on crystal geometry. Each computed property of a particular crystal structure typically has a relatively small random error and a larger systematic error. Cancellation of systematic errors allows more accurate predictions. We propose a computational methodology based on the subtraction of the systematic errors in MST. To exemplify it, we apply it to the precipitated alloys. Considering precipitation strengthening in Ni superalloys, we compute the relative enthalpies of the competing Ni3(Al,Ti)1 crystal structures with a chemical disorder on the Al+Ti sublattice. Such predicted composition-structure-property dependencies are useful for the guided design of the next-generation alloys with improved strength. Our predictions are validated by comparison with the results of other DFT methods (having a higher computational cost) and with experiment. We acknowledge funding of the guided design of stronger superalloys for airspace by NASA Aeronautics Research Mission Directorate (ARMD) via Transformational Tools and Technologies (TTT) Project.

Computational↗
DOE OSTI2023

Efficient structure-factor modeling for crystals with multiple components

Diffraction intensities from a crystallographic experiment include contributions from the entire unit cell of the crystal: the macromolecule, the solvent around it and eventually other compounds. These contributions cannot typically be well described by an atomic model alone, i.e . using point scatterers. Indeed, entities such as disordered (bulk) solvent, semi-ordered solvent ( e.g. lipid belts in membrane proteins, ligands, ion channels) and disordered polymer loops require other types of modeling than a collection of individual atoms. This results in the model structure factors containing multiple contributions. Most macromolecular applications assume two-component structure factors: one component arising from the atomic model and the second one describing the bulk solvent. A more accurate and detailed modeling of the disordered regions of the crystal will naturally require more than two components in the structure factors, which presents algorithmic and computational challenges. Here an efficient solution of this problem is proposed. All algorithms described in this work have been implemented in the computational crystallography toolbox ( CCTBX ) and are also available within Phenix software. These algorithms are rather general and do not use any assumptions about molecule type or size nor about those of its components.

59 BASIC BIOLOGICAL SCIENCES↗
DOE OSTI2022

Titrating Controlled Defects into Si-LTA Zeolite Crystals Using Multiple Organic Structure-Directing Agents

Controlling defects in zeolites is crucial for tuning their adsorption and catalytic properties. In this work, we have performed an integrated zeolite synthesis, spectroscopy, and density functional theory study to test the limit of F– as a charge-balancing agent that mitigates defects in siliceous zeolites. We focused on the synthesis of siliceous zeolite LTA at 150 °C with 1,2-dimethyl-3-(4-methylbenzyl) imidazolium as the primary organic structure-directing agent (OSDA) and tetramethyl ammonium (TMA) as the secondary OSDA. By varying the amount of TMA in the synthesis gel, positive charges were titrated into the resulting as-made Si-LTA. Surprisingly, we found that greater TMA concentration does not induce more F– to enter into the zeolite. 29Si solid-state MAS NMR, Raman spectroscopy, and density functional theory suggest that this system has surpassed its capacity for F– to balance OSDA charge, and additional positive charge is balanced by Si–O– framework defects. The number of defects in the as-made Si-LTA can be precisely titrated by the amount of TMA in the zeolite structures. For the Si-LTA synthesized without TMA, framework defects formed in the early stage of crystal growth were found to heal during later crystallization, leading to defect-free Si-LTA. However, for the Si-LTA synthesized with TMA, the defects formed in early stages do not heal. A DFT thermodynamic analysis explains that crowding of Si-LTA pores by TMA impedes defect healing; this prediction is corroborated by synthesis experiments at an elevated temperature (170 °C). These results indicate that F– can have a limited capacity to balance OSDA charge in zeolite synthesis, opening up a third route to zeolite synthesis intermediate between the fluoride and hydroxide routes.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2021

Absolute throughput calibration of multiple spherical crystals for the Orion High-REsolution X-ray spectrometer (OHREX)

We present absolute throughput analysis of several crystals for the Orion High-REsolution X-ray (OHREX) imaging crystal spectrometer using ray tracing and experimental measurements. The OHREX spectrometer is a high-resolution x-ray spectrometer designed to measure spectral line shapes at the Orion laser facility. The spectrometer is fielded with up to two spherical crystals simultaneously covering two independent spectral ranges. Each crystal has a nominal radius of curvature of R = 67.2 cm and is fielded at a nominal Bragg angle of 51.3°. To cover different bands of interest, several different crystals are available, including Ge (111), KAP, and several cuts of quartz, whose resolving power λ/Δλ exceeds 10 000. The calibrated response of the available crystals has previously been reported from measurements at the EBIT-I electron beam ion trap at Lawrence Livermore National Laboratory. Here, we model the absolute throughput of each crystal using ray tracing and verify the results using experimental data for the quartz $(10\bar{1}1)$ crystal.

47 OTHER INSTRUMENTATION↗
NASA NTRS2021

Absolute throughput calibration of multiple spherical crystals for the Orion High-REsolution X-ray spectrometer (OHREX)

We present absolute throughput analysis of several crystals for the Orion High-REsolution X-ray (OHREX) imaging crystal spectrometer using ray tracing and experimental measurements. The OHREX spectrometer is a high-resolution x-ray spectrometer designed to measure spectral line shapes at the Orion laser facility. The spectrometer is fielded with up to two spherical crystals simultaneously covering two independent spectral ranges. Each crystal has a nominal radius of curvature of R = 67.2 cm and is fielded at a nominal Bragg angle of 51.3°. To cover different bands of interest, several different crystals are available, including Ge (111), KAP, and several cuts of quartz, whose resolving power λ/Δλ exceeds 10 000. The calibrated response of the available crystals has previously been reported from measurements at the EBIT-I electron beam ion trap at Lawrence Livermore National Laboratory. Here, we model the absolute throughput of each crystal using ray tracing and verify the results using experimental data for the quartz (10¯11) crystal.

M. J. MacDonald↗
DOE OSTI2023

Calcite Twinning in Mollusk Shells and Carrara Marble

Mollusk shells protect the animals that form and inhabit them. They are composites of minerals and organics, with diverse mesostructures, including nacre, prismatic calcite, crossed-lamellar aragonite, and foliated calcite. Twins, that is, crystals mirror symmetric with respect to their coherent interface, occurring as formation or deformation twins, are observed in all mollusk shell mesostructures but never within calcite prisms. Here, nanotwins and microwins within single calcite prisms are observed in different shells. Using Polarization-dependent Imaging Contrast (PIC) mapping with 20–60 nm resolution, twins are observed to be 0.2–3 µm thick layers of differently oriented and colored crystals with respect to the main prism crystal. Multiple twins are interspersed with the prism crystal, parallel to one another, and similarly oriented. When comparing images of calcite prisms and twins obtained by PIC mapping and by Electron Back-Scattered Diffraction (EBSD), the images correspond precisely. All twins are e-twin types, with 127° angular distance between c-axes. E-twins are the most common deformation twins in geologic calcite, as also observed here in Carrara marble. Location of all twins near the outer surface of all shells and e-twin type both suggest that twins within calcite prisms in mollusk shells result from deformation twinning.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Disorder and diffuse scattering in single-chirality (TaSe 4 ) 2 ⁢I crystals

The quasi-one-dimensional chiral compound (TaSe 4 ) 2 I has been extensively studied as a prime example of a topological Weyl semimetal. Upon crossing its phase transition temperature $T$ CDW ≈263K, (TaSe 4 ) 2 I exhibits incommensurate charge density wave (CDW) modulations described by the well-defined propagation vector ∼(0.05,0.05,0.11), oblique to the TaSe 4 chains. Although optical and transport properties greatly depend on chirality, there is no systematic report about chiral domain size for (TaSe 4 ) 2 I. In this study, our single-crystal scattering refinements reveal a bulk iodine deficiency, and Flack parameter measurements on multiple crystals demonstrate that separate (TaSe 4 ) 2 I crystals have uniform handedness, supported by direct imaging and helicity-dependent terahertz emission spectroscopy. Our single-crystal x-ray scattering and calculated diffraction patterns identify multiple diffuse features and create a real-space picture of the temperature-dependent (TaSe 4 ) 2 I crystal structure. Further, the short-range diffuse features are present at room temperature and decrease in intensity as the CDW modulation develops. These transverse displacements, along with electron pinning from the iodine deficiency, help explain why (TaSe 4 ) 2 I behaves as an electronic semiconductor at temperatures above and below $T$ CDW , despite a metallic band structure calculated from density functional theory of the ideal structure.

36 MATERIALS SCIENCE↗
DOE OSTI2022

The mechanisms of catalysis and ligand binding for the SARS-CoV-2 NSP3 macrodomain from neutron and x-ray diffraction at room temperature

The nonstructural protein 3 (NSP3) macrodomain of severe acute respiratory syndrome coronavirus 2 (SARS-CoV-2) (Mac1) removes adenosine diphosphate (ADP) ribosylation posttranslational modifications, playing a key role in the immune evasion capabilities of the virus responsible for the coronavirus disease 2019 pandemic. Here, we determined neutron and x-ray crystal structures of the SARS-CoV-2 NSP3 macrodomain using multiple crystal forms, temperatures, and pHs, across the apo and ADP-ribose–bound states. We characterize extensive solvation in the Mac1 active site and visualize how water networks reorganize upon binding of ADP-ribose and non-native ligands, inspiring strategies for displacing waters to increase the potency of Mac1 inhibitors. Determining the precise orientations of active site water molecules and the protonation states of key catalytic site residues by neutron crystallography suggests a catalytic mechanism for coronavirus macrodomains distinct from the substrate-assisted mechanism proposed for human MacroD2. These data provoke a reevaluation of macrodomain catalytic mechanisms and will guide the optimization of Mac1 inhibitors.

60 APPLIED LIFE SCIENCES↗
DOE OSTI2021

Temporal prepulse contrast degradation in high-intensity CPA lasers from anisotropy of amplifier gain media

Here, we present a study of the temporal pre-pulse contrast degradation of high focused intensity pulses produced in CPA laser systems due to imperfections in amplifier design, alignment of amplifier components, and crystal inhomogeneity. Using an extended cross-polarized imaging technique, we demonstrate the presence of multiple crystal domains inside Ti:sapphire slabs with ≈10 cm diameter. Furthermore, the results of our numerical calculations show that crystalline c-axis orientation inhomogeneity caused by these crystal domains can lead to generation of pre-pulses with relative contrast >10 -10 within several picoseconds before the main pulse. In a multiple-slab amplifier head configuration sometimes used in high repetition rate systems, the misalignment of the amplifier slabs crystalline c-axes with respect to each other can lead to the generation of pre-pulses with relative contrast as high as 10 -6 , depending on the magnitude of misalignment.

47 OTHER INSTRUMENTATION↗
DOE OSTI2024

Imaging extended single crystal lattice distortion fields with multi-peak Bragg ptychography

Recent advances in phase-retrieval-based x-ray imaging methods have demonstrated the ability to reconstruct 3D distortion vector fields within a nanocrystal by using coherent diffraction information from multiple crystal Bragg reflections. However, these works do not provide a solution to the challenges encountered in imaging lattice distortions in crystals with significant defect content that result in phase wrapping. Moreover, these methods only apply to isolated crystals smaller than the x-ray illumination, and therefore cannot be used for imaging of distortions in extended crystals. We introduce multi-peak Bragg ptychography which addresses both challenges via an optimization framework that combines stochastic gradient descent and phase unwrapping methods for robust image reconstruction of lattice distortions and defects in extended crystals. Our work uses modern automatic differentiation toolsets so that the method is easy to extend to other settings and easy to implement in high-performance computers. This work is particularly timely given the broad interest in using the increased coherent flux in fourth-generation synchrotrons for innovative material research.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Toward In Situ Synchrotron Mapping of Crystal Selection Processes during Crystal Growth

In this work, we present an automated and rapid method for non-destructive mapping of crystal grains in a rod-shaped sample. The approach was designed for application to in situ float-zone crystal growth experiments at an x-ray synchrotron source, but could be useful in other applications. The methods have been tested on a TiO 2 boule grown in an optical float zone furnace. The approach applies a statistical filter to polycrystalline diffraction patterns on 2D detectors to rapidly determine the degree of powder-quality 1of the signal. When larger crystals emerge in the growth, their position, size and shape can be tracked using an automated blob-tracking algorithm that follows individual Bragg peaks as a function of position in a grid-scan, even when multiple crystals are contributing spots to diffraction images. This method is found to be robust as the same crystal shape can be independently reconstructed using different sets of Bragg reflections. Image segmentation methods are then used to map out the polycrystalline grains. We also note that other information about crystal quality, such as mosaicity or strain state, may be inferred and mapped from the intensity variation of the Bragg peaks at different locations within the sample.

36 MATERIALS SCIENCE↗
NASA NTRS1982

Atmosphere Analyzer

California Measurements, Inc.'s model PC-2 Aerosol Particle Analyzer is produced in both airborne and ground-use versions. Originating from NASA technology, it is a quick and accurate method of detecting minute amounts of mass loadings on a quartz crystal -- offers utility as highly sensitive detector of fine particles suspended in air. When combined with suitable air delivery system, it provides immediate information on the size distribution and mass concentrations of aerosols. William Chiang, obtained a NASA license for multiple crystal oscillator technology, and initially developed a particle analyzer for NASA use with Langley Research Center assistance. Later his company produced the modified PC-2 for commercial applications Brunswick Corporation uses the device for atmospheric research and in studies of smoke particles in Fires. PC-2 is used by pharmaceutical and chemical companies in research on inhalation toxicology and environmental health. Also useful in testing various filters for safety masks and nuclear installations.

Source record↗
DOE OSTI2024

In-situ relative calibration of Bragg crystals with Monte Carlo line ratio analysis

X-ray line emission spectra can thoroughly characterize hot plasmas, especially when line shapes and ratios convey distinct aspects of plasma conditions. However, the high spectral resolution required for observing line shapes is often at odds with the large bandwidth required to observe many line ratios across a wide spectral range. One strategy to obtain high spectral resolution over a wide bandwidth is to use multiple crystals with calibrated reflectivity so that line intensities across different crystals can be compared. Here, we explore the use of a low-resolution, wide-bandwidth mica survey spectrometer to infer relative reflectivity of two high-resolution, narrow-bandwidth quartz crystals. Finally, a Monte Carlo error analysis determines comparable x-ray line ratios measured from both spectrometers, resulting in an in situ calibration factor and associated uncertainty for the relative reflectivity of the high-resolution crystals.

47 OTHER INSTRUMENTATION↗