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Results for “in situ crystallization”

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 37 records · Page 2
All sourcesNASA NTRSDOE OSTI
NASA NTRS1992

Fiber/matrix adhesion in graphite/PEKK composites

Experiments with poly ether ketone ketone (PEKK) resin and AS-4, IM-7, and G30-500 fibers showed excellent correlation between resin/fiber contact angle and composite transverse flexural strength as measures of resin/fiber interfacial strength. Both tests indicate the strongest interface for G30-500/PEKK followed by IM-7/PEKK and AS-4/PEKK. Also discussed are fiber effects on interlaminar fracture and on the in situ crystallization of the matrix during composite fabrication.

Bucher, R. A.↗
NASA NTRS1991

Airborne Measurements of Cirrus Reflectance and Heights with Comparison to Polder Observations

The NASA ER-2 high altitude aircraft cloud observation experiment includes visible, infrared and microwave radiometric imaging of cloud tops and combined lidar profiling of cloud tops. A special instrument is the Tilt Scan CCD Camera (TSCC) for measurements of cloud top multidirectional reflectance and polarization. Data have been acquired on the bi-directional reflectance of cirrus in the FIRE, TOGA/COARE, SUCCESS and WINCE cloud observation experiments. The FIRE, TOGA/COARE and SUCCESS observations include some cases of combined in situ crystal measurements and in all measurements, multispectral visible/IR cirrus microphysics retrievals are possible. The results for bi-directional reflectance for mid-latitude cirrus in the FIRE and SUCCESS missions are consistent with models for complex, multi-type crystal structure. These may be contrasted with tropical cirrus observation for which results are more typical of simple crystal structure. The cirrus multidirectional results may be compared and contrasted with those available from POLDER. In addition, during the WINCE experiment of January 1997 there were several targeted ER-2 for cloud observation underflights of POLDER on ADEOS, Comparison of direct cloud height measurement and multispectral radiometer analysis from ER-2 data with POLDER results are made.

Spinhirne, James↗
NASA NTRS1999

In Situ Monitoring of Crystal Growth Using MEPHISTO, Mission STS 87-Program USMP-4: Experimental Analysis

This report summarizes the results of the In situ Monitoring of Crystal Growth Using MEPHISTO (Material por l'Etude des Phenomenes Interessant de la Solidification sur Terre et en Orbite) experiment on USMP-4. The report includes microstructural and compositional data obtained during the first year of the post flight analysis, as well as numerical simulation of the flight experiment. Additional analyses are being continued and will be reported in the near future. The experiments utilized MEPHISTO hardware to study the solidification and melting behavior of bismuth alloyed with 1 at% tin. The experiments involved repeated melting and solidification of three samples, each approximately 90 cm long and 6mm in diameter. Half of each sample also included a 2 mm. diameter growth capillary, to assist in the formation of single grain inside. One sample provided the Seebeck voltage generated during melting and freezing processes. Another one provided temperature data and Peltier pulsed demarcation of the interface shape for post flight analysis. The third sample provided resistance and velocity measurements, as well as additional thermal data. The third sample was also quenched at the end of the mission to preserve the interface composition for post flight determination. A total of more than 45cm of directionally solidified alloy were directionally solidified at the end of the flight for post mission structural and compositional characterization. Metallurgical analysis of the samples has shown that the interfacial kinetics play a key role in controlling the morphological stability of faceted alloys. Substantial differences were observed in the Seebeck signal between the ground-based experiments and the space-based experiments. The temperature gradient in the liquid for the ground-based experiments was also significantly lower than the temperature gradient in the liquid for the space-based experiments. Both of these observations indicate significant influence of liquid convection for the ground-based experiments.

Abbaschian, Reza↗
NASA NTRS2004

Quartz Crystal Microbalance Operation and In Situ Calibration

Quartz crystal microbalances (QCMs) are commonly used to measure the rate of deposition of molecular species on a surface. The measurement is often used to select materials with a low outgassing rate for applications where the material has a line of sight to a contamination-sensitive surface. A quantitative, in situ calibration of the balance, or balances, using a pure material for which the enthalpy of sublimation is known, is described in this Technical Memorandum. Supporting calculations for surface dwell times of deposited materials and the effusion cell Clausing factor are presented along with examples of multiple QCM measurements of outgassing from a common source.

Albyn, K. C.↗
DOE OSTI2022

Deformation twinning and detwinning in extruded Mg-4Al: In-situ experiment and crystal plasticity simulation

Deformation twinning and detwinning in extruded Mg-4Al were investigated using in-situ SEM-DIC experiments and crystal plasticity finite element (CPFE) simulation. In this study, the in-situ SEM-DIC method was used to provide a unique set of data including twin/detwin characteristics and twin area fraction in addition to strain maps. A statistical analysis of the activation of twin variants and twin area fraction during both twinning and detwinning was conducted. A strong correlation was found between twin growth/shrinkage and the Schmid Factor (SF) for individual twin variants Higher twin SF during loading and unloading led to higher twin growth and shrinkage, respectively. However, after the applied compressive strain was removed, the pattern of the twin area fractions of the residual twin variants versus their nominal SFs did not follow the trend observed at the maximum compressive strain. Using a systematic methodology and an advanced twin/detwin model, the PRISMS-Plasticity CPFE simulation was calibrated using experimentally determined stress versus strain and twin area fraction versus strain information. A comprehensive evaluation of the CPFE model was conducted to determine its ability to capture the statistics of twin variants activation and twin area fraction. CPFE accurately captured the statistical aspects of both twinning and detwinning. Finally, it also predicted the first dominant twin variant for 47.5% of the grains and at least one of the two dominant twin variants for 80% of the grains at maximum compressive strain.

36 MATERIALS SCIENCE↗
NASA NTRS1990

Stratospheric ice crystals

In situ sampling of the crystals is described with a NASA high-altitude aircraft to characterize the presence of ice particles and their role in Antarctic ozone chemistry. A NASA wire impactor was employed to collect the crystals, and the device was modified to permit Formvar crystal replication. The size distributions of the columnar crystals show that at the highest altitude the the smallest crystals are collected. The crystals provide surface area for heterogeneous chemical reactions as well as the removal of moisture and particles from the stratosphere and its ozone-related components.

Goodman, Jindra↗
DOE OSTI2023

Polymer-based microfluidic device for on-chip counter-diffusive crystallization and in situ X-ray crystallography at room temperature

Proteins are long chains of amino acid residues that perform a myriad of functions in living organisms, including enzymatic reactions, signalling, and maintaining structural integrity. Protein function is determined directly by the protein structure. X-ray crystallography is the primary technique for determining the 3D structure of proteins, and facilitates understanding the effects of protein structure on function. The first step towards structure determination is crystallizing the protein of interest. We have developed a centrifugally-actuated microfluidic device that incorporates the fluid handling and metering necessary for protein crystallization. Liquid handling takes advantage of surface forces to control fluid flow and enable metering, without the need for any fluidic or pump connections. Our approach requires only the simple steps of pipetting the crystallization reagents into the device followed by either spinning or shaking to set up counter-diffusive protein crystallization trials. The use of thin, UV-curable polymers with a high level of X-ray transparency allows for in situ X-ray crystallography, eliminating the manual handling of fragile protein crystals and streamlining the process of protein structure analysis. We demonstrate the utility of our device using hen egg white lysozyme as a model system, followed by the crystallization and in situ, room temperature structural analysis of the hub domain of calcium–calmodulin dependent kinase II (CaMKIIβ).

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2020

Soft crystal martensites: An in situ resonant soft x-ray scattering study of a liquid crystal martensitic transformation

Liquid crystal blue phases (BPs) are three-dimensional soft crystals with unit cell sizes orders of magnitude larger than those of classic, atomic crystals. The directed self-assembly of BPs on chemically patterned surfaces uniquely enables detailed in situ resonant soft x-ray scattering measurements of martensitic phase transformations in these systems. The formation of twin lamellae is explicitly identified during the BPII-to-BPI transformation, further corroborating the martensitic nature of this transformation and broadening the analogy between soft and atomic crystal diffusionless phase transformations to include their strain-release mechanisms.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Evaporation of a Reactive Nanofluid Sessile Drop: Capturing Rapid Emergence of Surface Crystals with In Situ Synchrotron X-ray Diffraction

Mechanisms for surface pattern formation from evaporation of a reactive nanofluid sessile drop are not well understood. In contrast to the coffee-ring effect from inert particles, rapid chemical and morphological transformation of reactive nanoparticles upon rapid evaporative drying are challenging to probe experimentally. Here, using grazing-incidence X-ray surface scattering, the nanostructure of nascent surface patterns has been probed as a ZnO nanofluid sessile drop rapidly dries. The high temporal resolution enabled by the high flux of synchrotron X-rays allows the observation of the emergence of Zn(OH) 2 surface crystals from the onset of evaporation and their rapid evolution into the final residual surface pattern, via transient layered complexes evident from the temporary appearance of X-ray diffraction peaks preceding Zn(OH) 2 formation. The results offer mechanistic insights of morphogenesis of surface patterns from evaporation-induced self-assembly and self-organization of reactive nanofluids, previously untenable using other experimental methods.

36 MATERIALS SCIENCE↗
DOE OSTI2021

In situ study of Crystal Surface Interactions Guided by Biomolecules or Ligands

Ligands or biomolecules commonly exist and play a key role in particle-mediated materials growth, leading to a wide variety of structures. However, it is not fully understood how these organic molecules control forces interacting between particles and thus the dynamics of particle assembly. Herein, the overall goal of this project is to gain an understanding of the role of surface-coating materials (ligands and biomolecules) in particle assembly processes; that is, how surface-coating materials determine the interfacial structures of solvent/ligand (biomolecule)/crystal surface and thus the interaction forces.

36 MATERIALS SCIENCE↗
NASA NTRS1994

In-Situ Monitoring of Crystal Growth Using MEPHISTO

This experiment flew on STS-62 and is the continuation of a collaborative US-French study of the process of crystal formation. Knowledge from this experiment will support the development of techniques to grow higher quality semiconductor crystals on Earth.

Source record↗
NASA NTRS2001

In Situ Monitoring of Crystal Growth Using Mephisto

Experiments were carried out to study the morphological stability of Bi-1atomic% Sn alloys using the MEPHISTO directional solidification apparatus aboard Space Shuttle Columbia (STS-87, launched November 19, 1997). The research program involved collaboration of the University of Florida, Centre National d'Etudes Spatiales (France), NASA/Glenn Research Center, the National Institute of Standards and Technology, and the University of New South Wales (Australia). The experiments made use of the Seebeck technique to measure the interface temperature, the resistance change across the sample for determination of the interface velocity, and Peltier current pulsing for demarcation of the interface shape. These data were obtained in real-time during various melting/solidification cycles, and the experiments were controlled via telecommands. The Seebeck signal and temperature measurements in the space experiments, as well as morphological behavior of the solid/liquid interface, were found to be significantly different than those obtained from ground-based studies. For the space-based experiments, interface breakdown was observed at growth velocities of 6.7, 27, and 40 micrometers/s, but not at 1.8 and 3.3 micrometers/s. The results further indicate that the morphological stability threshold for some grain orientations is significantly enhanced, resulting in a staggered planar to cellular transition front. This report summarizes some of these findings.

Abbaschian, Reza↗
NASA NTRS2001

Shuttle Flight Experiment on USMP-4: In Situ Monitoring of Crystal Growth Using MEPHISTO

This reports on the MEPHISTO-4 experiment on the Space Shuttle Columbia, STS-87, November 19-December 5, 1997. Involved were NASA; the University of Florida at Gainesville; groups from France that developed and built the furnace; the National Institute of Standards and Technology; The University of New South Wales, Australia; and Purdue University. This was a solidification study in which three long rods of Bismuth- 1 at.% Tin were directionally solidified. The goals were to solidify in an environment free of natural convection; to determine the relationship among solidification growth velocity, growth mode, and temperature; and determine the diffusivity of Sn in Bi. The flight samples grew with a planar solid/liquid interface at velocities less than 3.4 gm/s, and cellular growth was present at velocities greater than 6.7 um/s; grain orientation influenced the planar to cellular transition. The temperature gradient in the liquid was 204 K/cm. The s/l interface was flat with slight concavity. Diffusion-dominated conditions were present during MEPHISTO-4. The Seebeck technique was used to determine the s/I interface temperature during growth, however, to date, analysis of the Seebeck results has not yielded a reliable measurement of the interface temperature. The partition coefficient for Bi alloyed with Sn was measured, k = 0.029.

Abbaschian, Reza↗
DOE OSTI2024

Thermodynamic and Kinetic Modulation of Methylammonium Lead Bromide Crystallization Revealed by In Situ Monitoring

Hybrid organic–inorganic perovskite (HOIP) crystals are promising optoelectronic materials, but little is known about either the thermodynamic and kinetic controls on crystal growth or the underlying growth mechanism(s). Herein, we use fluid cell atomic force microscopy (AFM) and solution nuclear magnetic resonance (NMR) spectroscopy to investigate growth of the model HOIP crystal CH 3 NH 3 PbBr 3 (MAPbBr 3 ) and to determine how formic acid (HCOOH) modulates the thermodynamics and kinetics of growth. The results show that growth of MAPbBr 3 in dimethylformamide (DMF) proceeds through the classical pathway by the spreading of atomic crystal steps generated at screw dislocations on the {100} surface. Temperature dependent step velocity measurements demonstrate that with increasing concentration, HCOOH decreases both the solubility of MAPbBr 3 and the kinetic coefficient (b) of step movement. 1 H-NMR measurements indicate that HCOOH increases the lifetime of the methylammonium (MA + ) ions and promotes the association of MAPbBr 3 , thus tuning the solubility of the perovskite. HCOOH also alters the molecular tumbling motion and bulk diffusion of the MA + ions, possibly via H-bonding. Further, our findings establish a direct correlation between the mesoscale crystal growth kinetics and the molecular-scale interactions between organic additives and constituent ions, providing unprecedented insights for developing predictive syntheses of HOIP crystals with defined size, crystal habit and shape, and defect distribution.

36 MATERIALS SCIENCE↗
NASA NTRS2001

Characterization and In-Situ Monitoring of ZnSe Crystal Growth by Seeded PVT for Microgravity Applications

Crystal growth from the vapor phase continues to play a significant role in the production of II-VI semiconductor compounds (ZnO, ZnTe, CdTe, etc.) and SiC. As compared to melt growth methods (where available) the advantages are: (1) lower growth temperature(s); (2) reduction in defect concentration; (3) additional purification; and (4) enhanced crystal perfection. A powerful tool in determining the mechanism of PVT is microgravity. Under normal gravity conditions the transport mechanism is a superposition of diffusive and convective fluxes. Microgravity offers the possibility of studying the transport properties without the influence of convective effects. Research on the crystal growth of ZnSe by PVT (P.I.: Su of NASA/MSFC) will help to clarify the effects of convection on crystal growth. A crystal growth furnace with in-situ and real time optical monitoring capabilities was constructed and used to monitor the vapor composition and growing crystal surface morphology during the PVT growth of ZnSe. Using photoluminescence and SIMS, ex-situ, the incorporation of point defects (Zn vacancy) and impurities was found to be correlated to the gravity vector due to the influence of the convective flow. A summary of the results to date will be presented.

Feth, Shari T.↗
DOE OSTI2022

Micro-strains, local stresses, and coherently diffracting domain size in shock compressed Al(100) single crystals

In situ x-ray diffraction (XRD) measurements and their analysis in Al single crystals shock compressed along the [100]-direction were utilized to examine shock wave induced microstructural heterogeneities. High-resolution XRD line profiles for the 200, 400, and 600 Al peaks were measured in uniaxial strain compression states to either 5.6 or 11.7 GPa and partial stress release to 3.5 or 6.6 GPa, respectively. Broadening of the XRD line profiles was analyzed to determine the magnitude of the longitudinal micro-strain distribution (0.195% and 0.28% full width at half maximum for 3.5 and 6.6 GPa stresses, respectively) and the size of coherently diffracting domains (CDDs) (0.125 and 0.07 μm for 3.5 and 6.6 GPa stresses, respectively). From the longitudinal micro-strain distributions, the distribution of local stress differences (or stress deviators) was obtained in the shocked state. The full width at half maximum of this distribution, a measure of the local stress inhomogeneities, is greater than half of the macroscopic stress difference for both 3.5 and 6.6 GPa peak stresses, suggesting considerable variation in local stress deviators. The CDD sizes determined here are comparable to characteristic length scales for defect-free regions determined from defect density measurements in post-shock recovery experiments. As a result, the present work represents an important step in understanding material microstructure and inhomogeneities in the shock-compressed state.

36 MATERIALS SCIENCE↗