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At least 667 records · Page 37

Macromolecule Crystal Quality Improvement in Microgravity: The Role of Impurities

While macromolecule impurities may affect crystal size and morphology the over-riding question is; "How do macromolecule impurities effect crystal X-ray quality and diffraction resolution?" In the case of chicken egg white lysozyme, crystals can be grown in the presence of a number of impurities without affecting diffraction resolution. One impurity however, the lysozyme dimer, does negatively impact the X-ray crystal properties. Crystal quality improvement as a result of better partitioning of this impurity during crystallization in microgravity has been reported'. In our recent experimental work dimer partitioning was found to be not significantly different between the two environments. Mosaicity analysis of pure crystals showed a reduced mosaicity and increased signal to noise for the microgravity grown crystals. Dimer incorporation however, did greatly reduce the resolution limit in both ground and microgravity grown crystals. These results indicate that impurity effects in microgravity are complex and may rely on the conditions or techniques employed.

Judge, Russell A.↗

Hydrogen tolerance of a Ti3Al-based alloy

The Ti-24Al-11Nb (Ti-24-11) alloy heat-treated to the fine basketweave microstructure was shown previously to be hydrogen-tolerant. In order to assess its limit of hydrogen tolerance, the tensile, creep, fracture toughness, and sustained-load crack growth behaviors of this alloy were studied as a function of hydrogen content. The mechanical test results indicated that the fine basketweave microstructure was tolerant to hydride embrittlement for hydrogen contents up to about 1500 wppm. On the other hand, hydrogen charging experiments indicated that the Ti-24-11 alloy was severely cracked and pulverized under zero load when the hydrogen content exceeded 3000 wppm. X-ray diffraction results revealed that the dichotomous behaviors might be due to the formation of face-centered cubic (fcc) delta-type hydrides at higher hydrogen contents but face-centered tetragonal (fct) gamma-type hydrides at lower hydrogen contents.

Chan, Kwai S.↗

CVD silicon carbide monofilament reinforced SrO-Al2O3-2SiO2 (SAS) glass-ceramic composites

Unidirectional CVD SiC fiber-reinforced SrO.Al2O3.2SiO2 (SAS) glass-ceramic matrix composites have been fabricated by hot pressing at various combinations of temperature, pressure and time. Both carbon-rich surface coated SCS-6 and uncoated SCS-0 fibers were used as reinforcements. Almost fully dense composites have been obtained. Monoclinic celsian, SrAl2Si2O8, was the only crystalline phase observed in the matrix from x-ray diffraction. During three point flexure testing of composites, a test span to thickness ratio of approximately 25 or greater was necessary to avoid sample delamination. Strong and tough SCS-6/SAS composites having a first matrix crack stress of approximately 300 MPa and an ultimate bend strength of approximately 825 MPa were fabricated. No chemical reaction between the SCS-6 fibers and the SAS matrix was observed after high temperature processing. The uncoated SCS-0 fiber-reinforced SAS composites showed only limited improvement in strength over SAS monolithic. The SCS-0/SAS composite having a fiber volume fraction of 0.24 and hot pressed at 1400 deg C exhibited a first matrix cracking stress of approximately 231 +/- 20 MPa and ultimate strength of 265 +/- 17 MPa. From fiber push-out tests, the fiber/matrix interfacial debonding strength (tau(sub debond)) and frictional sliding stress (tau(sub friction)) in the SCS-6/SAS system were evaluated to be approximately 6.7 +/- 2.3 MPa and 4.3 +/- 0.6 MPa, respectively, indicating a weak interface. However, for the SCS-0/SAS composite, much higher values of approximately 17.5 +/- 2.7 MPa for tau(sub debond) and 11.3 +/- 1.6 MPa for tau(sub friction) respectively, were observed; some of the fibers were so strongly bonded to the matrix that they could not be pushed out. Examination of fracture surfaces revealed limited short pull-out length of SCS-0 fibers. The applicability of various micromechanical models for predicting the values of first matrix cracking stress and ultimate strength of these composites were examined.

Bansal, Narottam P.↗

End-to-end Modeling of Lyot Coronagraph for LUVOIR: Sensitivity to Segment-Level Aberrations

Direct imaging and spectroscopic characterization of atmospheres of Earth-like exoplanets require starlight suppression to detect a faint planetary signal at small angular separations. Future space telescopes will require segmentation to survey a statistically significant population of nearby stars systems by increasing aperture size beyond the limits set by traditional monolithic apertures; however, segmentation also represents an additional challenge due to the introduction of temporal pupil discontinuities in terms of both phase and amplitude. For this study, a baseline Lyot coronagraph is used with the Large UV / Optical /Infrared (LUVOIR) mission’s 15-m on-axis, segmented optical telescope assembly (OTA). We present a high-fidelity, end-to-end modeling approach developed as part of the Segmented Coronagraph Design and Analysis (SCDA) group that includes diffractive optical propagations at the 1e-10 contrast level across the entire optical train including the OTA and intermediate re-imaging optics inside the coronagraph instrument. We perform a tolerancing analysis to assess the contrast sensitivity to wavefront perturbations for a set of key telescope terms including segment-level low-order and mid-spatial frequency aberrations. As an input to the end-to-end telescope model, we use two industry-provided segment-level wavefront aberration datasets pertaining: (1) thermal gradients and accelerations (courtesy of Ball-Aerospace and L3-Harris), and (2) telescope dynamics including line-of-sight and segment jitter (courtesy of Lockheed-Martin). Contrast performance outputs of the coronagraph are fed into a mission design reference simulator to assess the scientific yield sensitivity. End-to-end modeling will incorporate performance improvements due to active wavefront sensing and control and/or segment-level metrology to improve system performance.

Optics↗

Spin glass freezing and superconductivity in YBa2(Cu(1-x)Fe(x))3O7 alloys

The dynamics were studied of the iron spins in superconducting YBa2(Cu(0.94)Fe(0.06))3O7 by neutron time of flight measurements. Two samples were studied with slightly different characteristics, as shown by resistivity and neutron diffraction measurements. The same dynamical anomalies are observed by neutrons in both samples. Differences appear qualitative but not quantitative. In the whole temperature range, the q-dependence of the magnetic intensity mainly reflects the magnetic form factor of iron which shows that the iron spins are almost uncorrelated. The elastic and quasielastic intensities strongly vary with temperature. A spin glass like freezing is revealed at low temperature by a sharp decrease of the quasielastic intensity, an increase of the 'elastic' or resolution limited intensity and a minimum in the quasielastic width. The freezing temperature (T sub f - 18 K) corresponds to that already determined by a magnetic splitting in Mossbauer experiments. Above T sub f, the relaxation of the iron spins in the paramagnetic state is modified by the occurrence of superconductivity. An increase was observed of the quasielastic intensity and of the quasielastic width at the superconducting transition.

Mirebeau, I.↗

X-ray diffractometer studies of shocked materials

This study explores the utility of X-ray diffractometer scans for determination of shock pressure histories of geological materials from meteorite impact sites. The technique is based on quantification of increased crystal lattice disorder with increasing shock pressure as expressed by decreasing diffraction peak amplitude and pronounced line-broadening caused by decreasing mosaic domain size and increasing strain. The ratio of peak height (PH) to half width (HW) decreases systematically with increasing shock pressure. Data are given for experimentally shocked quartz, feldspars, pyroxene and olivine along with data for granitic materials from the Piledriver nuclear event and from the Ries Crater, Germany. Although the technique in principle may be capable of yielding relatively accurate pressure determinations, its application to naturally shocked materials may be severely limited.

Hanss, R. E.↗

A laboratory verification sensor

The use of a variant of the Hartmann test is described to sense the coalignment of the 36 primary mirror segments of the Keck 10-meter Telescope. The Shack-Hartmann alignment camera is a surface-tilt-error-sensing device, operable with high sensitivity over a wide range of tilt errors. An interferometer, on the other hand, is a surface-height-error-sensing device. In general, if the surface height error exceeds a few wavelengths of the incident illumination, an interferogram is difficult to interpret and loses utility. The Shack-Hartmann aligment camera is, therefore, likely to be attractive as a development tool for segmented mirror telescopes, particularly at early stages of development in which the surface quality of developmental segments may be too poor to justify interferometric testing. The constraints are examined which would define the first-order properties of a Shack-Hartmann alignment camera and the precision and range of measurement one could expect to achieve with it are investigated. Fundamental constraints do arise, however, from consideration of geometrical imaging, diffraction, and the density of sampling of images at the detector array. Geometrical imagining determines the linear size of the image, and depends on the primary mirror diameter and the f-number of a lenslet. Diffraction is another constraint; it depends on the lenslet aperture. Finally, the sampling density at the detector array is important since the number of pixels in the image determines how accurately the centroid of the image can be measured. When these factors are considered under realistic assumptions it is apparent that the first order design of a Shack-Hartmann alignment camera is completely determined by the first-order constraints considered, and that in the case of a 20-meter telescope with seeing-limited imaging, such a camera, used with a suitable detector array, will achieve useful precision.

Vaughan, Arthur H.↗

Evolved Gas Analysis and X-Ray Diffraction of Carbonate Samples from the 2009 Arctic Mars Analog Svalbard Expedition: Implications for Mineralogical Inferences from the Mars Science Laboratory

The 2009 Arctic Mars Analog Svalbard Expedition (AMASE) investigated several geologic settings using methodologies and techniques being developed or considered for future Mars missions, such as the Mars Science Laboratory (MSL), ExoMars, and Mars Sample Return (MSR). AMASE-related research comprises both analyses conducted during the expedition and further analyses of collected samples using laboratory facilities at a variety of institutions. The Sample Analysis at Mars (SAM) instrument suite, which will be part of the Analytical Laboratory on MSL, consists of a quadrupole mass spectrometer (QMS), a gas chromatograph (GC), and a tunable laser spectrometer (TLS). An Evolved Gas Analysis Mass Spectrometer (EGA-MS) was used during AMASE to represent part of the capabilities of SAM. The other instrument included in the MSL Analytical Laboratory is CheMin, which uses X-Ray Diffraction (XRD) and X-Ray Fluorescence (XRF) to perform quantitative mineralogical characterization of samples. Field-portable versions of CheMin were used during the AMASE 2009. Here, we discuss the preliminary interpretation of EGA and XRD analyses of selected AMASE carbonate samples and implications for mineralogical interpretations from MSL. Though CheMin will be the primary mineralogical tool on MSL, SAM EGA could be used to support XRD identifications or indicate the presence of volatile-bearing minerals which may be near or below XRD detection limits. Data collected with instruments in the field and in comparable laboratory setups (e.g., the SAM breadboard) will be discussed.

McAdam, A. C.↗

Orbiter environment at S- and Ku-band frequencies

Detailed measurements of the electric field strength associated with the Ku-band radar and S-band communication link were made by the Plasma Diagnostics Package (PDP) on STS 51F. These measurements were made while the PDP was attached to the Remote Manipulation System arm and again while the PDP was released as a subsatellite. The results indicate that cargo elements that remain inside of the scan limits of the radar should experience fields less than 2 V/m and that elements that may encounter the main beam can use 300 V/m as a design guideline with adequate safety margin. S-band fields tended to be several dB lower than worst-case predictions. Safe design practice indicates that an electric field E = 100/r (r in meters) should be used as a guideline for deployable systems. S-band electric fields within the cargo bay envelope should be less than 2 V/m even with edge diffraction effects and reflections from other payloads taken into account. The absolute accuracy of these measurements is about 2 dB.

Murphy, G. B.↗

Statistics for ionospherically diffracted VHF/UHF signals.

In this paper, a general characterization of the statistics for an ionospherically diffracted, monochromatic plane wave is presented. The main results are restricted to weak scatter, although two possible extensions that accommodate large phase perturbations and multiple scatter are discussed. A detailed discussion of the first-order statistics of amplitude is given. The general Gaussian distribution is discussed together with its Nakagami-distribution approximation and the log-normal distribution. By using a segment of ATS-3 satellite data recorded at Lima, Peru, we show equally good fits to Gaussian and log-normal distributions at least for the limited dynamic range available. The Nakagami distribution provides only a poor approximation.

Rino, C. L.↗

Consolidation of Si3N4 by hot isostatic pressing

Silicon nitride (Si3N4) is being considered for gas turbine engine applications because present-day metallic alloys are rapidly approaching the limits of their temperature capabilities. The present investigation was undertaken to determine the feasibility of producing a sound, dense Si3N4 body without additives, using conventional gas hot-isostatic-pressing techniques and an uncommon hydraulic hot-isostatic-pressing technique. These two hot-isostatic-pressing (HIP) techniques produce much higher pressure (275-413 MN/sq m) than conventional hot-pressing techniques and have the potential of producing large bodies of desirable shapes. Evaluation was based on density measurement, microscopic examination, both optical and electron, and X-ray diffraction analysis.

Yeh, H. C.↗

Using Multiplicative Algebraic Reconstruction Techniques (MART) to Derive Instrument Requirements for Computed Tomography Imaging Spectrographs

Computed Tomography Imaging Spectrographs (CTISs), which are generally slitless or large-aperture spectrographs that observe a wide, dispersed field of view in multiple dispersion angles or diffraction orders, provide a unique opportunity to capture spectral information over an extended source, such as the Sun, but require software reconstruction techniques to be fully utilized. A useful data product that can be recovered from CTIS observations is intensity maps of solar features in single spectral lines. These intensity maps can then be used to determine temperature, density, abundance, and equilibrium properties of the emitting plasma. We apply the multiplicative algebraic reconstruction technique (MART) to example data from a variety of CTIS configurations to determine the capability and limitations of the method to return spectrally-pure maps. By completing this study, we aim to establish a path to derive requirements for CTIS instruments that rely on reconstruction techniques to meet their science objectives.

Amy Winebarger↗

Advanced protein crystal growth flight hardware for the Space Station

The operational environment of the Space Station will differ considerably from the previous short term missions such as the Spacelabs. Limited crew availability combined with the near continuous operation of Space Station facilities will require a high degree of facility automation. This paper will discuss current efforts to develop automated flight hardware for advanced protein crystal growth on the Space Station. Particular areas discussed will be the automated monitoring of key growth parameters for vapor diffusion growth and proposed mechanisms for control of these parameters. A history of protein crystal growth efforts will be presented in addition to the rationale and need for improved protein crystals for X-ray diffraction. The facility will be capable of simultaneously processing several hundred protein samples at various temperatures, pH's, concentrations etc., and provide allowances for real time variance of growth parameters.

Herrmann, Frederick T.↗

Coordinated Analyses of Antarctic Sediments as Mars Analog Materials Using Reflectance Spectroscopy and Current Flight-Like Instruments for CheMin, SAM and MOMA

Coordinated analyses of mineralogy and chemistry of sediments from the Antarctic Dry Valleys illustrate how data obtained using flight-ready technology of current NASA and ESA missions can be combined for greater understanding of the samples. Mineralogy was measured by X-ray diffraction (XRD) and visible/ near-infrared (VNIR) reflectance spectroscopy. Chemical analyses utilized a quadrupole mass spectrometer (QMS) to perform pyrolysis-evolved gas analysis (EGA) and gas chromatography-mass spectrometry (GC/MS) both with and without derivatization, as well as laser desorption-mass spectrometry (LD/MS) techniques. These analyses are designed to demonstrate some of the capabilities of near-term landed Mars missions, to provide ground truthing of VNIR reflectance data acquired from orbit by the Compact Reconnaissance Imaging Spectrometer for Mars (CRISM) on MRO and to provide detection limits for surface- operated instruments: the Chemistry and Mineralogy (CheMin) and Sample Analysis at Mars (SAM) instrument suites onboard Mars Science Laboratory (MSL) and the Mars Organic Molecule Analyzer (MOMA) onboard ExoMars-2018. The new data from this study are compared with previous analyses of the sediments performed with other techniques. Tremolite was found in the oxic region samples for the first time using the CheMin-like XRD instrument. The NIR spectral features of tremolite are consistent with those observed in these samples. Although the tremolite bands are weak in spectra of these samples, spectral features near 2.32 and 2.39 micrometers could be detected by CRISM if tremolite is present on the martian surface. Allophane was found to be a good match to weak NIR features at 1.37-1.41, 1.92, and 2.19 micrometers in spectra of the oxic region sediments and is a common component of immature volcanic soils. Biogenic methane was found to be associated with calcite in the oxic region samples by the SAM/EGA instrument and a phosphoric acid derivative was found in the anoxic region sample using the SAM/MTBSTFA technique.

Mars↗

Convective flow effects on protein crystal growth

A high-resolution microscopic interferometric setup for the monitoring of protein morphologies has been developed. Growth or dissolution of a crystal can be resolved with a long-term depth resolution of 200 A and a lateral resolution of 2 microns. This capability of simultaneously monitoring the interfacial displacement with high local depth resolution has yielded several novel results. We have found with lysozyme that (1) the normal growth rate is oscillatory, and (2) depending on the impurity content of the solution, the growth step density is either greater or lower at the periphery of a facet than in its center. The repartitioning of Na plus and Cl minus ions between lysozyme solutions and crystals was studied for a wide range of crystallization conditions. A nucleation-growth-repartitioning model was developed, to interpret the large body of data in unified way. The results strongly suggest that (1) the ion to lysozyne ratio in the crystal depends mostly on kinetic rather than crystallographic parameters, and (2) lysozyme crystals possess a salt-rich core with a diameter electron microscopy results appear to confirm this finding, which could have far-reaching consequences for x-ray diffraction studies. A computational model for diffusive-convective transport in protein crystallization has been applied to a realistic growth cell geometry, taking into account the findings of the above repartitioning studies and our kinetics data for the growth of lysozyme. The results show that even in the small cell employed, protein concentration nonuniformities and gravity-driven solutal convection can be significant. The calculated convection velocities are of the same order to magnitude as those found in earlier experiments. As expected, convective transport, i.e., at Og, lysozyme crystal growth remains kinetically limited. The salt distribution in the crystal is predicted to be non-uniform at both 1g and 0g, as a consequence of protein depletion in the solution. Static and dynamic light scattering studies in undersaturated and supersaturated solutions have been performed. Diffusivities in undersaturated solutions, were found to vary with lysozyme concentrations. Depending on the salt concentration, the diffusivities either increase or decrease. Interestingly, the corresponding static scattering intensities behave oppositely, Our current analysis indicates that these changes are inconsistent with aggregation in undersaturated solutions. However, the data are compatible with concentration-dependent changes of the interactions between protein and salt.

Rosenberger, Franz↗

SAM-Like Evolved Gas Analyses of Phyllosilicate Minerals and Applications to SAM Analyses of the Sheepbed Mudstone, Gale Crater, Mars

While in Yellowknife Bay, the Mars Science Laboratory Curiosity rover collected two drilled samples, John Klein (hereafter "JK") and Cumberland ("CB"), from the Sheepbed mudstone, as well as a scooped sample from the Rocknest aeolian bedform ("RN"). These samples were sieved by Curiosity's sample processing system and then several subsamples of these materials were delivered to the Sample Analysis at Mars (SAM) instrument suite and the CheMin X-ray diffraction/X-ray fluorescence instrument. CheMin provided the first in situ X-ray diffraction-based evidence of clay minerals on Mars, which are likely trioctahedral smectites (e.g., Fe-saponite) and comprise ~20 wt% of the mudstone samples [1]. SAM's evolved gas analysis (EGA) mass spectrometry analyses of JK and CB subsamples, as well as RN subsamples, detected H2O, CO2, O2, H2, SO2, H2S, HCl, NO, OCS, CS2 and other trace gases evolved during pyrolysis. The identity of evolved gases and temperature( s) of evolution can augment mineral detection by CheMin and place constraints on trace volatile-bearing phases present below the CheMin detection limit or those phases difficult to characterize with XRD (e.g., X-ray amorphous phases). Here we will focus on the SAM H2O data, in the context of CheMin analyses, and comparisons to laboratory SAM-like analyses of several phyllosilicate minerals including smectites.

McAdam, A. C.↗

Effect of starting powder characteristics on density, microstructure and low temperature oxidation behavior of a Si3N48w/o Y2O3 ceramic

The densification and oxidation behavior of Si3N4 - 8w/oY2O3 prepared from three commercial starting powders were studied. Bars of SN 402, SN 502, and CP 85/15 were sintered for 3 to 4.5 hours at 1750 C. A second set was hot pressed for 2 hours at 1750 C. The microstructures were studied by transmission electron microscopy and scanning electron microscopy, densities were determined, and the phase compositions were determined by X-ray diffraction. Densification and microstructure were greatly influenced by the starting powder morphology and impurity content. Although SN 402 exhibited the maximum weight lose, the highest sintered and hot pressed densities were obtained with this powder. All powders had both equiaxed and elongated grains. Sintered bars were composed of beta silicon nitride and n-melelite. In contrast, hot pressed bars contained beta silicon nitride, H-phase, and J-phase, but no melelite. Yttria distribution in sintered bars was related to the presence of cation impurities such as Ca, Fe, and Mg. A limited oxidation study at 750 C in air showed no instability in these Si3N4 - 8 w/oY2O3 specimens, regardless of startin powder.

Schuon, S.↗

The effect of alloying on gamma and gamma prime in nickel-base superalloys

An investigation was conducted to determine the compositional limits of gamma and gamma prime phases in nickel-base superalloys. Fifty-one nickel-base alloys were melted under vacuum and heat treated for 4 hours at 1190 C followed by 1008 hours at 850 C. The alloys had the following composition ranges: A1 4.0 to 13 atomic percent, Cr 6.5 to 20.5 percent, Ti 0.25 to 4.75 percent, Mo 0.0 to 6.0 percent, and W 0.0 to 4.0 percent. The residues from the ammonium sulfate electrolytic extraction for the two-phase alloys were analyzed chemically and by X-ray diffraction. The results of the investigation were used to assemble a mathematical model of the gamma-gamma prime region of the Ni-Al-Cr-Ti-Mo-W system. A computer program was written to analyze the model of the phase diagram. Some of these results are also presented graphically. The resulting model is capable of satisfactorily predicting the compositions of conjugate gamma-gamma prime phases in the alloys investigated and twelve of fifteen commercial superalloys studied.

Dreshfield, R. L.↗