Naica’s Giant Crystals: Characterization and Evolution of the Wall–Crystal Interface
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Crystals of Cd(1-x)Zn(x)Te with x = 0.2 and 40 g in weight were grown on monocrystalline cadmium-zinc telluride seeds by closed-ampoule physical vapor transport with or without excess (Cd + Zn) in the vapor phase. Two post-growth cool-down rates were used. The crystals were characterized using low temperature photoluminescence, atomic force microscopy, chemical etching, X-ray diffraction and electrical measurements. No formation of a second, ZnTe-rich phase was observed.
The solubility measurement system and the laser scattering microscope system were designed, built, and utilized for the study of crystal growth solutions and crystal characterization measurements. Solubility measurements and crystal defect maps were made with this equipment for a number of new materials. In some cases, where there have been published solubility data (i.e., TGS), more accurate measurements were made and discrepancies in the published data were resolved. The design of these instruments is presented along with a description of their use and some typical data generated using them.
NASA Glenn's Propulsion Systems Lab (PSL), an altitude engine test facility, was outfitted with a spray system to generate ice crystals. The first ice crystal characterization test occurred in 2012. At PSL, turbine engines and driven rigs can experience ice crystal icing at flight altitudes, temperatures and Mach numbers. To support these tests, four ice crystal characterizations have been conducted in two different facility configurations. In addition, super-cooled liquid and mixed phase clouds have also been generated. This paper will discuss the recent learning from the previous two calibrations. It will describe some of the 12-parameter calibration space, and how those parameters interact with each other, the instrumentation used to characterize the cloud and present a sample of the cloud characterization results.
Characterizing the fundamental micromechanisms activated during plastic deformation is critical to explain the macroscopic shock response of materials and develop accurate material models. In this paper, we investigate the orientation dependence, and the mediated slip and twin systems on [100] and [111] bcc molybdenum single crystals shock compressed up to 18 GPa with real-time Laue x-ray diffraction measurements. We report that dislocation slip along the {110} < 111 > and {112} < 111 > systems is the governing deformation mechanism during compression with negligible anisotropy observed at the Hugoniot state. Here, we provide real-time evidence that molybdenum undergoes deformation twinning along {11¯2} < 111 > during shock release.
NASA Glenn's Propulsion Systems Lab, an altitude engine test facility, was outfitted with a spray system to generate ice crystals in 2011. Turbine engines and driven rigs can experience ice crystal icing at flight altitudes, temperatures and Mach numbers. To support these tests, four ice crystal characterizations have been conducted in two different facility configurations. In addition, super-cooled liquid and mixed phase clouds have also been generated. This paper represents a work in progress. It will describe some of the 11-parameter calibration space, and how those parameters interact with each other, the instrumentation used to characterize the cloud and present a sample of the cloud characterization results.
Characterization of defects and/or disorder in biological macromolecular crystals presents much greater challenges than in conventional small-molecule crystals. The lack of sufficient contrast of defects is often a limiting factor in x-ray diffraction topography of protein crystals. This has seriously hampered efforts to understand mechanisms and origins of formation of imperfections, and the role of defects as essential entities in the bulk of macromolecular crystals. In this report, we employ a phase sensitive x-ray diffraction imaging approach for augmenting the contrast of defects in protein crystals.
The High-Speed Growth and Characterization of Crystals for Solar Cells Research Forum was held on July 25-27, 1983, at the Sandpiper Bay Hotel in ort St. Lucie, Florida. The Research Forum was arranged into eight interactive sessions and addressed theoretical and experimental phenomena, applications, and characterization including stress/strain and other problem areas that limit the rate of growth of crystals suitable for processing into efficient, cost-effective solar cells. The Flat-Plate Solar Array Project of the Jet Propulsion Laboratory sponsored the meeting: Thirty-five invited papers were presented. Discussion periods followed each presentation. These Proceedings are a record of the papers and the discussions.
NASA Glenn's Propulsion Systems Laboratory (PSL) is an altitude engine research test facility capable of producing ice-crystal and supercooled liquid clouds. The cloud characterization parameter space is fairly large and complex, but the phase of the cloud seems primarily governed by wet bulb temperature. The presentation will discuss some of the issues uncovered through four cloud characterization efforts to date, as well as some of instrumentation that has been used to characterize cloud parameters including cloud uniformity, bulk total water content, median volumetric diameter and max-diameter, percent freeze-out, relative humidity, and an update on the NASA Glenn PSL Ice Crystal Cloud Characterization (2016).
Elemental and compound semiconductors were characterized using new optical approach based on NIR microscopy in conjunction with computational image analysis and contrast enhancement. The approach made it possible to perform a quantitative microsegregation analysis of GaAs and InP. NIR dark file illumination in transmission mode makes it possible to detect submicron precipitates in semiinsulating GaAs.
Abstract Multimodal multiscale characterization provide opportunities to study organic semiconducting thin films with multiple length scales, across multiple platforms, to elucidate crystallization mechanisms of the various microstructures that impact functionality. With polarized scanning transmission X‐ray and 4D‐scanning transmission electron microscopy, hybrid crystalline structures in rubrene thin films in which large crystalline domains surround a common nucleus and transition to a spherulite morphology at larger radii is observed. These high‐resolution techniques reveal how azimuthal orientational discontinuities at smaller radii are erased as spherulite morphology takes hold. In situ crystallization in the films with optical microscopy is also captured, discovering the importance of considering the initial temperature increase of a film during thermal annealing over the crystallization timescale. This kinetic information of the radial crystallization rate and of corresponding film heating kinetics is used to estimate the temperature at which the larger crystalline regions transition into a spherulite. By combining the results obtained from the different characterization modes, it is learned that thermal conditions can sensitively affect the crystallization of rubrene and other organic thin films. The observations suggest opportunities for more complex temperature‐dependent processing to maximize hybrid structures’ functionality in organic thin films and demonstrate that multimodal studies deepen the understanding of structure‐function dynamics.
NASA Glenn's Propulsion Systems Lab, an altitude engine test facility, generates icing clouds with a spray system. While the spray system is used mostly to create ice crystal clouds (Appendix D/P), the 2017 cloud characterization effort added the requirement to produce exactly supercooled liquid clouds in Appendix C and Appendix O. Success was demonstrated to supercool the largest drops at the warmest conditions, but not freeze out the smallest drops at the coldest conditions. This paper documents primarily the total water content characterization methodology and results from an Iso-Kinetic Probe in ice crystals and Multi-Wire sensor in supercooled liquid, along with the cloud uniformity provided by light extinction tomography. Particle size distribution results from High Speed Imaging probes and a Phase Doppler Interferometer are discussed. Also, a new numerical model for tracking the thermodynamics of the air-drop interactions in PSL from the plenum toward the cloud characterization plane are noted. Both of these latter topic are more fully documented in companion papers.
CdZnTe-based detectors are highly valued because of their high spectral resolution, which is an essential feature for nuclear medical imaging. However, this resolution is compromised when there are substantial defects in the CdZnTe crystals. In this study, we present a learning-based approach to determine the spatially dependent bulk properties and defects in semiconductor detectors. This characterization allows us to mitigate and compensate for the undesired effects caused by crystal impurities. We tested our model with computer-generated noise-free input data, where it showed excellent accuracy, achieving an average RMSE of 0.43% between the predicted and the ground truth crystal properties. In addition, a sensitivity analysis was performed to determine the effect of noisy data on the accuracy of the model.
The behavior of protein crystal growth is estimated from measurements performed at both the microscopic and molecular levels. In the absence of solutal flow, it was determined that a model that balances the macromolecular flux toward the crystal surface with the flux of the crystal surface well characterizes crystal growth observed using microscopic methods. Namely, it was determined that the model provides accurate estimates for the crystal-growth velocities upon evaluation of crystal-growth measurements obtained in time. Growth velocities thus determined as a function of solution supersaturation were further interpreted using established deterministic models. From analyses of crystal-growth velocities, it was found that the mode of crystal growth varies with respect to increasing solution supersaturation, possibly owing to kinetic roughening. To verify further the hypothesis of kinetic roughening, crystal growth at the molecular level was examined using atomic force microscopy (AFM). From the AFM measurements, it was found that the magnitude of surface-height fluctuations, h(x), increases with increasing solution supersaturation. In contrast, the estimated characteristic length, xi, decreases rapidly upon increasing solution supersaturation. It was conjectured that the magnitude of both h(x) and xi could possibly determine the mode of crystal growth. Although the data precede any exact theory, the non-critical divergence of h(x) and xi with respect to increasing solution supersaturation was nevertheless preliminarily established. Moreover, approximate models to account for behavior of both h(x) and xi are also presented.
Glasses in the yttria-silica system with 20-40 mol pct Y2O3 have been subjected to recrystallization studies after melting at 1900-2100 C in W crucibles in 1 and 50 atm N2. The TEM and XRD results obtained indicate the presence of the delta, gamma, gamma-prime, and beta-Y2Si2O7 crystalline phases, depending on melting and quenching conditions. Heat-treatment in air at 1100-1600 C increased the amount of crystallization, and led to the formation of Y2SiO5, cristobalite, and polymorphs of Y2Si2O7. Also investigated were the effects of 5 and 10 wt pct zirconia additions.
Glasses in the yttria-silica system with 20 to 40 mol pct Y2O3 were subjected to recrystallization studies after melting at 1900 to 2100 C in W crucibles in 1 and 50 atm N2. The TEM and XRD results obtained indicate the presence of the delta, gamma, gamma prime, and beta-Y2Si2O7 crystalline phases, depending on melting and quenching conditions. Heat treatment in air at 1100 to 1600 C increased the amount of crystallization, and led to the formation of Y2SiO5, cristabalite, and polymorphs of Y2Si2O7. Also investigated were the effects of 5 and 10 wt pct zirconia additions.
Fluorescence is one of the most versatile and powerful tools for the study of macromolecules. While most proteins are intrinsically fluorescent, working at crystallization concentrations require the use of covalently prepared derivatives added as tracers. This approach requires derivatives that do not markedly affect the crystal packing. We have prepared fluorescent derivatives of chicken egg white lysozyme with probes bound to one of two different sites on the protein molecule. Lucifer yellow and 5-(2-aminoethyl)aminonapthalene-1-sulfonic acid (EDANS) have been attached to the side chain carboxyl of Asp(sup 101) using a carbodiimide coupling procedure. Asp(sup 101) lies within the active site cleft, and it is believed that the probes are "buried" within that cleft. Lucifer yellow and MANS probes with iodoacetamide reactive groups have been bound to His(sup 15), located on the "back side" of the molecule relative to the active site. All the derivatives fluoresce in the solution and the crystalline states. Fluorescence characterization has focused on determination of binding effects on the probe quantum yield, lifetime, absorption and emission spectra, and quenching by added solutes. Quenching studies show that, as postulated, the Asp(sup 101)-bound probes are partially sheltered from the bulk solution by their location within the active site cleft. Probes bound to His(sup 15) have quenching constants about equal to those for the free probes, indicating that this site is highly exposed to the bulk solution.