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At least 19 records

XRD, TEM, IR, Raman and NMR Spectroscopy of In Situ Crystallization of Lithium Disilicate Glass

The structure of a Li2O-2SiO2 (LS2) glass was investigated as a function of pressure and temperature up to 6 GPa and 750 C respectively, using XRD, TEM, IR, Raman and NMR spectroscopy. Glass densified at 6 GPa has an average Si-O-Si bond angle approx.7deg lower than that found in glass processed at 4.5 GPa. At 4.5 GPa, lithium disilicate crystallizes from the glass, while at 6 GPa a new high pressure form of lithium metasilicate crystallizes. The new phase, while having lithium metasilicate crystal symmetry, contains at least 4 different Si sites. NMR results for 6 GPa sample indicate the presence of Q4 species with (Q(sup 4))Si-O-Si(Q(sup 4)) bond angles of approx.157deg. This is the first reported occurrence of Q(sup 4) species with such large bond angles in alumina free alkali silicate glass. No five- or six- coordinated Si are found.

Fuss, T.↗

In-Situ Crystallization of a Lithium Disilicate Glass--Effect of Pressure on Crystal Growth Rate

Crystallization of a Li2O.2SiO2 (LS2) glass subjected to a uniform hydrostatic pressure of 4.5 GPa and 6 GPa was investigated up to a temperature of 750 C. The density of the compressed glass is about 2% greater at 4.5 GPa than at 1 atm and, depending upon the processing temperature, up to 10% greater at 6 GPa. Crystal growth rates investigated as a function of temperature and pressure show that lithium disilicate crystal growth is an order of magnitude slower at 4.5 GPa than 1 atm resulting in a shift of +45 C (plus or minus 10 C) in the growth rate curve at high pressure compared to 1 atm condition. At 6 GPa lithium disilicate crystallization is suppressed entirely, while a new high pressure lithium metasilicate crystallizes at temperatures 95 C (plus or minus 10 C) higher than those reported for lithium disilicate crystallization at 1 atm. The decrease in crystal growth rate with increasing pressure for lithium disilicate glass up to 750 C is related to an increase in viscosity with pressure associated with fundamental changes in glass structure accommodating densification.

Fuss, T.↗

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.↗

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↗

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↗

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.↗

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↗

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↗

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↗

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↗

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.↗

In situ observation of mono-molecular growth steps on aqueous solution grown crystals and the transport of molecules to the crystals

Direct in situ observation of mono-molecular growth steps on a crystal growing in an aqueous solution became possible. The combination of this method with high resolution Schlieren methods or interferometry, permits the growth mechanism of crystals to be investigated directly. Since the observation of growth steps on crystals is the most direct and sensitive way for investigating a crystal growth mechanism, it would contribute to revealing fundamental differences between the growth in space and on Earth. The method was recently extended to in situ observation of the growth processes at high temperatures (1800K).

Tsukamoto, Katsuo↗

Evaluation of a New Cloud Droplet Activation Parameterization wtih in Situ Data from CRYSTAL-FACE and CSTRIPE

The accuracy of the 2003 prognostic, physically based aerosol activation parameterization of A. Nenes and J. H. Seinfeld (NS) with modification introduced by C. Fountoukis and A. Nenes in 2005 (modified NS) is evaluated against extensive microphysical data sets collected on board the Center for Interdisciplinary Remotely Piloted Aircraft Studies (CIRPAS) Twin Otter aircraft for cumuliform and stratiform clouds of marine and continental origin. The cumuliform cloud data were collected during NASA's Cirrus Regional Study of Tropical Anvils and Cirrus Layers-Florida Area Cirrus Experiment (CRYSTAL-FACE, Key West, Florida, July 2002), while the stratiform cloud data were gathered during Coastal Stratocumulus Imposed Perturbation Experiment (CSTRIPE, Monterey, California, July 2003). In situ data sets of aerosol size distribution, chemical composition, and updraft velocities are used as input for the NS parameterization, and the evaluation is carried out by comparing predicted cloud droplet number concentrations (CDNC) with observations. This is the first known study in which a prognostic cloud droplet activation parameterization has been evaluated against a wide range of observations. On average, predicted droplet concentration in adiabatic regions is within -20% of observations at the base of cumuliform clouds and -30% of observations at different altitudes throughout the stratiform clouds, all within experimental uncertainty. Furthermore, CDNC is well parameterized using either a single mean updraft velocity w or by weighting droplet nucleation rates with a Gaussian probability density function of w. This study suggests that for nonprecipitating warm clouds of variable microphysics, aerosol composition, and size distribution the modified NS parameterization can accurately predict cloud droplet activation and can be successfully implemented for describing the aerosol activation process in global climate models.

Meskhidze, Nicholas↗

Classification of Particle Shapes from Lidar Depolarization Ratios in Convective Ice Clouds Compared to in situ Observations During CRYSTAL-FACE

This manuscript describes a method to class@ cirrus cloud ice particle shape using lidar depolarization measurements as a basis for segregating different particle shape regimes. Measurements from the ER-2 Cloud Physics Lidar (CPL) system during CRYSTAL-FACE provide the basis for this work. While the CPL onboard the ER-2 aircraft was providing remote sensing measurements of cirrus clouds, the Cloud Particle Imager (CPI) onboard the WB-57 aircraft was flying inside those same clouds to sample particle sizes. The results of classifying particle shapes using the CPL data are compared to the in situ measurements made using the CPI , and there is found to be good agreement between the particle shape inferred from the CPL data and that actually measured by the CPI. If proven practical, application of this technique to spaceborne observations could lead to large-scale classification of cirrus cloud particle shapes.

Noel, Vincent↗

Simultaneous in situ Optical Monitoring Techniques during Crystal Growth of ZnSe by Physical Vapor Transport

ZnSe crystals grown in sealed ampoules by the physical vapor transport method were monitored in situ using three techniques, simultaneously. A Michelson interferometer was set-up to observe the growth rate and surface morphological evolution. An interference pattern (interferogram) is formed by the interaction between the reflection of a HeNe laser (632.8 nm wavelength) off the crystal-vapor interface and a reference beam from the same laser. Preliminary results indicate that the rate of growth/thermal-etching can be calculated using analog data acquisition and simple fringe counting techniques. Gross surface features may also be observed using a digital frame grabber and fringe analysis software. The second in situ technique uses optical absorption to determine the partial pressures of the vapor species. The Se2 and Zn vapor species present in the sealed ampoule absorb light at characteristic wavelengths. The optical absorption is determined by monitoring the light intensity difference between the sample and reference beams. The Se2 Partial pressure profile along the length of the ampoule was estimated from the vibronic absorption peaks at 340.5, 350.8, 361.3 and 379.2 nm using the Beer's law constants established in the calibration runs of pure Se. Finally, because the high temperature crystal growth furnace contains windows, in situ visual observation of the growing crystal is also possible. The use of these techniques not only permits in situ investigation of high temperature vapor growth of semiconductors, but also offers the potential for real time feed back on the growing crystal and allows the possibility of actively controlling the growth process.

Su, C.- H.↗