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At least 19 records

On the Use of Monochromators for the Calibration of AXAF

Data acquired, during the AXAF calibration at MSFC's X-Ray Calibration Facility (XRCF), using monochromators requires special analysis owing to potentially large spatial variations in the monochromators' beams and to higher-order contributions to the spectral content. A description of the monochromators -- the Double-Crystal Monochromator (DCM) and the HIgh-Resolution Erect-Field Spectrometer (HIREFS\TM) reflection-grating monochromator --- is given, followed by a discussion of the spectral and spatial content as monitored by Beam-Normalization Detector (BND) flow proportional counters (FPCs). Emphasis is given to the methodology employed in determining the spatial content through fits to Beam Uniformity (BU) measurements made nonsimultaneously, either during calibration or during pre-calibration source characterization. We present an interpolation scheme which adequately represents the beam properties over a wide range of source conditions.

Swartz, Douglas A.↗

Growth and characterization of large YBa2Cu3O(7-x) single crystals

Centimeter-sized crystal plates of YBa2Cu3O(7-x) have been obtained using a bulk composition and method described by Schneemeyer at al. (1987) modified for growth in a pure oxygen atmosphere. A porous MgO crucible and long soak time promote large crystals. Mg was not detectable in the crystals. Electron microbeam analysis using a 60 A monochromator crystal for the oxygen determination gave the composition Y(1.05)Ba(2.02)Cu(2.94)O(6.52 + or - 0.06). As-grown crystals from the melt surface exhibit a fairly sharp Tc with zero resistance at 80 K, and show complex twinning and crack patterns. Optical micrographs of a lightly polished surface normal to the c-axis of a 3-mm crystal delineate twinning and fine scale microcracking; this crystal surface now has a zero resistance at 68 K. Microhardness measurements and microfracture observations indicate intrinsic properties that may inhibit or impede large scale manufacture of electronic ceramics.

Keester, Kenneth L.↗

Electron escape depth variation in thin SiO2 films measured with variable photon energy

A double crystal monochromator at the Stanford Synchrotron Radiation Laboratory is used to study the Si/SiO2 interface, using photon energies of hv = 1950-3700 eV. This photon energy range allows interfaces to be observed through oxide layers 50 A thick or more. Variations in electron escape depth and/or oxide density as a function of distance from the interface are observed over the entire kinetic energy range (100-3600 eV). These differences are attributed to a strained oxide layer near the interface.

Hecht, M. H.↗

Soft X-ray photoemission with the SSX-100 spectrometer

Photoemission and SEXAFS experiments were conducted using a double crystal monochromator at the Stanford Synchrotron Radiation Laboratory. Photoelectrons were detected using a Surface Science Laboratories SSX-100 electron analyzer, which employs a magnetic/electrostatic lens, hemispherical geometry, and a two-dimensional position-sensitive detector. In the kinetic energy range of interest (1000-2000 eV), a significant improvement in count rate was observed over a single channel cylindrical mirror analyzer system. Ten second scans of the KLL silicon Auger peak manifold were recorded at a large number of photon energies for subsequent determination of SEXAFS spectra.

Hecht, M. H.↗

Reciprocal Space Mapping of Macromolecular Crystals in the Laboratory

The technique of reciprocal space mapping applied to the physical measurement of macromolecular crystals will be described. This technique uses a triple axis diffractometer setup whereby the monochromator is the first crystal, the sample is the second and the third crystal (of the same material as the monochromator) analyzes the diffracted beam. The geometry is such that it is possible to separate mosaic volume effects from lattice strain effects. The deconvolution of the instrument parameters will also be addressed. Results from measurements at Brookhaven National Synchrotron Radiation Source carried out on microgravity and ground-grown crystals will be presented. The required beam characteristics for reciprocal space mapping are also ideal for topographic studies and the first topographs ever recorded from microgravity protein crystal samples will be shown. We are now working on a system which will enable reciprocal space mapping, mosaicity and topography studies to be carried out in the home laboratory. This system uses a rotating anode X-ray source to provide an intense beam then a Bartels double crystal, four reflection monochromator to provide the spectral and geometric beam conditioning necessary such that the instrument characteristics do not mask the measurement. This is coupled to a high precision diffractometer and sensitive detector. Commissioning data and first results from the system will be presented.

Snell, Edward H.↗

A Compact X-Ray System for Support of High Throughput Crystallography

Standard x-ray systems for crystallography rely on massive generators coupled with optics that guide X-ray beams onto the crystal sample. Optics for single-crystal diffractometry include total reflection mirrors, polycapillary optics or graded multilayer monochromators. The benefit of using polycapillary optic is that it can collect x-rays over tile greatest solid angle, and thus most efficiently, utilize the greatest portion of X-rays emitted from the Source, The x-ray generator has to have a small anode spot, and thus its size and power requirements can be substantially reduced We present the design and results from the first high flux x-ray system for crystallography that combine's a microfocus X-ray generator (40microns FWHM Spot size at a power of 45 W) and a collimating, polycapillary optic. Diffraction data collected from small test crystals with cell dimensions up to 160A (lysozyme and thaumatin) are of high quality. For example, diffraction data collected from a lysozyme crystal at RT yielded R=5.0% for data extending to 1.70A. We compare these results with measurements taken from standard crystallographic systems. Our current microfocus X-ray diffraction system is attractive for supporting crystal growth research in the standard crystallography laboratory as well as in remote, automated crystal growth laboratory. Its small volume, light-weight, and low power requirements are sufficient to have it installed in unique environments, i.e.. on-board International Space Station.

Ciszak, Ewa↗

An integrated control panel utilizing a programmable varistor-multiplexed dichroic liquid crystal display

Due to the conflicting demands of modern aircraft for increased systems/sensors and the decrease in cockpit panel size, weight, volume, and power, conventional discrete/dedicated methods of display and control are fast becoming obsolete. A means is sought to integrate the control and display into multifunctional programmable devices, thus giving the ability to increase system functions and yet conserve panel space. A potential solution to the control portion of the problem has come to be known as the Integrated Control Panel (ICP) approach. Flat panel display technology and controls using programmable flat panel displays with transparent capacitive touch control overlays offer the largest potential advantages. The flat panel display made of varistor-multiplexed dichroic liquid crystal (LCD) developed by GE in recent years appears to offer the ideal monochrome solution.

Whitton, I. J.↗

Back in Time

Under a Jet Propulsion Laboratory SBIR (Small Business Innovative Research), Cambridge Research and Instrumentation Inc., developed a new class of filters for the construction of small, low-cost multispectral imagers. The VariSpec liquid crystal enables users to obtain multi-spectral, ultra-high resolution images using a monochrome CCD (charge coupled device) camera. Application areas include biomedical imaging, remote sensing, and machine vision.

Source record↗

A new method for focusing and imaging X-rays and gamma-rays with diffraction crystals

Bent diffraction crystals in which the intercrystalline-plane spacing is varied as a function of position in the crystal are used to focus monochromatic radiation from a point source or parallel beam down to a point image. Conversely, radiation from a point source can be focused into an outgoing parallel beam. The Bragg angle for diffraction of monochromatic radiation will now vary as a function of position in the crystal and this new degree of freedom is used to obtain focusing and imaging of the diffracted beam. This approach to focusing and imaging is applied to the design of a large-area, high resolution X-ray telescope that is also a high resolution monochromator with the unique feature that the width of the energy increment that is diffracted can be controlled and varied during the operation of the instrument. The field can be scanned with a wide energy increment and then switched to a narrow energy increment for the high resolution work. Both transmission and reflection type diffraction crystals can be used.

Smither, R. K.↗

A Compact X-Ray System for Macromolecular Crystallography

We describe the design and performance of a high flux x-ray system for macromolecular crystallography that combines a microfocus x-ray generator (40 gm FWHM spot size at a power level of 46.5Watts) and a 5.5 mm focal distance polycapillary optic. The Cu K(sub alpha) X-ray flux produced by this optimized system is 7.0 times above the X-ray flux previously reported. The X-ray flux from the microfocus system is also 3.2 times higher than that produced by the rotating anode generator equipped with a long focal distance graded multilayer monochromator (Green optic; CMF24-48-Cu6) and 30% less than that produced by the rotating anode generator with the newest design of graded multilayer monochromator (Blue optic; CMF12-38-Cu6). Both rotating anode generators operate at a power level of 5000 Watts, dissipating more than 100 times the power of our microfocus x-ray system. Diffraction data collected from small test crystals are of high quality. For example, 42,540 reflections collected at ambient temperature from a lysozyme crystal yielded R(sub sym) 5.0% for the data extending to 1.7A, and 4.8% for the complete set of data to 1.85A. The amplitudes of the reflections were used to calculate difference electron density maps that revealed positions of structurally important ions and water molecules in the crystal of lysozyme using the phases calculated from the protein model.

Gubarev, Mikhail↗

Microfocus/Polycapillary-Optic Crystallographic X-Ray System

A system that generates an intense, nearly collimated, nearly monochromatic, small-diameter x-ray beam has been developed for use in macromolecular crystallography. A conventional x-ray system for macromolecular crystallography includes a rotating-anode x-ray source, which is massive (.500 kg), large (approximately 2 by 2 by 1 m), and power-hungry (between 2 and 18 kW). In contrast, the present system generates a beam of the required brightness from a microfocus source, which is small and light enough to be mounted on a laboratory bench, and operates at a power level of only tens of watts. The figure schematically depicts the system as configured for observing x-ray diffraction from a macromolecular crystal. In addition to the microfocus x-ray source, the system includes a polycapillary optic . a monolithic block (typically a bundle of fused glass tubes) that contains thousands of straight or gently curved capillary channels, along which x-rays propagate with multiple reflections. This particular polycapillary optic is configured to act as a collimator; the x-ray beam that emerges from its output face consists of quasi-parallel subbeams with a small angular divergence and a diameter comparable to the size of a crystal to be studied. The gap between the microfocus x-ray source and the input face of the polycapillary optic is chosen consistently with the focal length of the polycapillary optic and the need to maximize the solid angle subtended by the optic in order to maximize the collimated x-ray flux. The spectrum from the source contains a significant component of Cu K (photon energy is 8.08 keV) radiation. The beam is monochromatized (for Cu K ) by a nickel filter 10 m thick. In a test, this system was operated at a power of 40 W (current of 897 A at an accelerating potential of 45 kV), with an anode x-ray spot size of 41+/-2 microns. Also tested, in order to provide a standard for comparison, was a commercial rotating-anode x-ray crystallographic system with a pyrolytic graphite monochromator and a 250-micron pinhole collimator, operating at a power of 3.15 kW (current of 70 mA at an accelerating potential of 45 kV). The flux of collimated Cu K radiation in this system was found to be approximately 16 times that in the rotatinganode system. Data on x-ray diffraction from crystals of tetragonal form of lysozyme (protein) in this system were found to be of high quality and to be reducible by use of standard crystallographic software.

Joy, Marshall↗

A Compact X-Ray System for Macromolecular Crystallography

We describe the design and performance of a high flux x-ray system for a macromolecular crystallography that combines a microfocus x-ray generator (40 micrometer full width at half maximum spot size at a power level of 46.5 W) and a collimating polycapillary optic. The Cu Ka lpha x-ray flux produced by this optimized system through a 500,um diam orifice is 7.0 times greater than the x-ray flux previously reported by Gubarev et al. [M. Gubarev et al., J. Appl. Crystallogr. 33, 882 (2000)]. The x-ray flux from the microfocus system is also 2.6 times higher than that produced by a rotating anode generator equipped with a graded multilayer monochromator (green optic, Osmic Inc. CMF24-48-Cu6) and 40% less than that produced by a rotating anode generator with the newest design of graded multilayer monochromator (blue optic, Osmic, Inc. CMF12-38-Cu6). Both rotating anode generators operate at a power level of 5000 W, dissipating more than 100 times the power of our microfocus x-ray system. Diffraction data collected from small test crystals are of high quality. For example, 42 540 reflections collected at ambient temperature from a lysozyme crystal yielded R(sub sym)=5.0% for data extending to 1.70 A, and 4.8% for the complete set of data to 1.85 A. The amplitudes of the observed reflections were used to calculate difference electron density maps that revealed positions of structurally important ions and water molecules in the crystal of lysozyme using the phases calculated from the protein model.

Gubarev, Mikhail↗

Laboratory and In-Flight In-Situ X-ray Imaging and Scattering Facility for Materials, Biotechnology and Life Sciences

We propose a multifunctional X-ray facility for the Materials, Biotechnology and Life Sciences Programs to visualize formation and behavior dynamics of materials, biomaterials, and living organisms, tissues and cells. The facility will combine X-ray topography, phase micro-imaging and scattering capabilities with sample units installed on the goniometer. This should allow, for the first time, to monitor under well defined conditions, in situ, in real time: creation of imperfections during growth of semiconductors, metal, dielectric and biomacromolecular crystals and films, high-precision diffraction from crystals within a wide range of temperatures and vapor, melt, solution conditions, internal morphology and changes in living organisms, tissues and cells, diffraction on biominerals, nanotubes and particles, radiation damage, also under controlled formation/life conditions. The system will include an ultrabright X-ray source, X-ray mirror, monochromator, image-recording unit, detectors, and multipurpose diffractometer that fully accommodate and integrate furnaces and samples with other experimental environments. The easily adjustable laboratory and flight versions will allow monitoring processes under terrestrial and microgravity conditions. The flight version can be made available using a microsource combined with multilayer or capillary optics.

Source record↗

Compact X-Ray And Extreme-Ultraviolet Monochromator

Monochromator for x-ray and extreme-ultraviolet radiation provides higher spectral resolution than achieved with thin-metal-foil broad-band-pass filters. Uses Bragg reflection to band-pass-filter radiation from high-intensity, broad-spectrum source. Operates over much broader x-ray and extreme-ultraviolet spectrum than devices based upon natural crystals. Intended to filter continuum radiation from sources like synchrotrons, laser plasma sources, free-electron lasers, and wigglers to produce monochromatic beams for testing and analysis of x-ray and extreme-ultraviolet telescopes and microscopes, for calibration of photographic films and detectors, for biological and biomedical research, for x-ray lithography, for processing of materials, and for research in properties of materials.

Hoover, Richard B.↗

X-ray/EUV optics for astronomy and microscopy; Proceedings of the Meeting, San Diego, CA, Aug. 7-11, 1989

Topics included in these proceedings are on X-ray/EUV zone plates, filters, and windows; X-ray/EUV microscopes, telescopes, and monochromators; the design, characterization, and test of multilayer optics; the fabrication of X-ray/EUV multilayer optics; and the design, characterization, and test of grazing incidence X-ray optics. Other topics are on the fabrication of grazing incidence X-ray optics, X-ray/EUV space observatories and missions, the test and calibration of X-ray/EUV instruments, X-ray polarimetry, and X-ray/EUV spectroscopy and instruments. Papers are presented on 8-keV X-ray zone plates, a cylindrical X-ray multilayer monochromator, multilayer mirrors for 182 A, advanced flow polishing of exotic optical materials, and optical analysis of grazing incidence ring resonators for free-electron lasers. Attention is also given to X-ray mirrors for the European Synchrotron Radiation Facility, the XUV wide-field camera for Rosat, an optical test and alignment method for the XMM mirror module, Bragg crystal polarimeters, and a liftoff process for multilayer phase gratings.

Hoover, Richard B.↗

Wavelength tunable liquid crystal imaging filters for remote sensing from geosynchronous platforms

Recent advances in liquid crystal technology have enabled us to construct tunable birefringent filters with bandwidths between approximately 0.1 nm and 50 nm. The center wavelength of these filters can be selected electronically, in a few tens of milliseconds, with no moving parts. These liquid crystal tunable filters (LCTF's), together with existing CCD detectors, make possible a new generation of lightweight, rugged, high-resolution imaging spectrophotometers. Such instruments would be particularly interesting for remote sensing applications from geosynchronous platforms. Important advantages exist in the aperture, absence of image shift, power consumption, size, weight, and absence of high drive frequencies, compared to current instruments used or considered for multispectral scene analysis. In the present work, we have reviewed spectral requirements of planned NASA geosynchronous remote sensing missions and identified several applications of the liquid crystal tunable filter technology. We have modeled the LCTF performance in the visible and near-infrared, and carried out a literature study on space-hardening of the filter components, to evaluate the suitability of LCTF's for geosynchronous missions. We have also compared the power consumption, weight, size, reliability, and optical performance of an imaging spectrophotometer using a LCTF monochromator, to other instruments that have been put forward for remote sensing from geosynchronous platforms. We put forward some conceptual designs for LCTF's that seem to offer important reliability, over the mechanical filter wheels presently baselined for the HEPI and ALM experiments. The extremely wide acceptance angle achievable with LCTF's could also avoid the present need for large-aperture interference filters in the ALM (and LIS) experiments. Thermal vacuum testing and radiation damage analysis is required to investigate the space hardening of these new filters for geosynchronous flight.

Foukal, Peter↗

Experiment 1: Orbital Processing of High-Quality Zn-Alloyed CdTe Compound Semiconductors

Zinc-alloyed cadmium telluride (Zn:CdTe) crystals were grown in unit gravity and in microgravity for comparative analysis. Two crystals were grown on USML-1/STS-50 in 1992, and two additional crystals were grown on USML-2/STS-73 in 1995. The Crystal Growth Furnace (CGF) in the seeded Bridgman-Stockbarger crystal growth geometry was utilized on both missions. Crystals grown on USML-1/STS-50 were found to have solidified with partial wall contact due to the near-absence of the hydrostatic pressure in microgravity, a residual g-vector that was not axial, and the nonwetting sample/ampoule wetting conditions. Crystals grown on USML-2/STS-73 included: a sample/ampoule identical to the USML-1/STS-73 sample/ampoule, with the addition of a restraining spring to simulate hydrostatic pressure internally, and a tapered ampoule which accomplished 2.2 cm of crystal growth without wall contact. Infrared transmission of all ground and flight samples was found to be 63-66 percent, very close to the theoretical 66 percent, suggesting good stoichiometric control. Infrared microscopy confirmed that the primary precipitates were Te and their size (1-10 microns) and density suggested that the flight- and ground-base samples experienced similar thermal histories. Longitudinal macrosegregation, calculated using scaling analysis, was predicted to be low. Nearly diffusion controlled growth was achieved even in unit gravity and macrosegregation data could be fit with a diffusion controlled model. Radial segregation was monitored and was found to vary with fraction solidified, particularly through the shoulder region, where the sample cross section was varying significantly. It was also disturbed in the flight samples in regions where asymmetric wall contact was noted. In regions where a steady state was established, the radial segregation was invariant within our experimental measurement error. Flight samples were found to be much higher in structural perfection than samples processed in unit gravity under identical growth conditions. In regions where solidification had occurred without wall contact, the free surfaces evidenced virtually no twinning, although twins appeared in the flight samples in regions of wall contact and were pervasive in the ground samples. These results were confirmed using optical microscopy and synchrotron x-ray white beam topography. Full-width half-maximum rocking curve widths (FWHM), recorded in arc-seconds, were significantly reduced from 20 a-s (1 g) to 9 a-s (micro-g) for the best regions of the crystals. The 9 a-s (FWHM) rocking curve value in the unconfined flight samples equals the best value reported terrestrially for this material. The ground samples exhibited a fully developed (111)[110] dislocation mosaic structure, whereas dislocations within the flight samples were discrete and no mosaic structure was evident. The defect density was quantitatively reduced from 75,000 (1 g) to 800 (micro-g) +/-50 percent. Dislocation etch pit density results were confirmed using transmission synchrotron white beam and monochromated beam topography. The low defect density is thought to have resulted from the near absence of hydrostatic pressure, which allowed the molten boule to solidify with little or no wall contact. This minimized the transfer of hoop stresses during solidification and post-solidification processing.

Larson, D. J., Jr.↗

First Results from a Microfocus X-Ray System for Macromolecular Crystallography

The design and performance of a 40 Watt laboratory crystallography system optimized for the structure determination of small protein crystals are described. This system combines a microfocus x-ray generator (40 microns FWHM spot size at a power level of 40 Watts) and a short focal length (F = 2.6 mm) polycapillary collimating optic, and produces a small diameter quasi-parallel x-ray beam. Measurements of x-ray flux, divergence and spectral purity of the resulting x-ray beam are presented. The x-ray flux in a 250 microns diameter aperture produced by the microfocus system is 14.7 times higher .than that from a 3.15 kW rotating anode generator equipped with graphite monochromator. Crystallography data taken with the microfocus system are presented, and indicate that the divergence and spectral purity of the x-ray are sufficient to refine the diffraction data using a standard crystallographic software. Significant additional improvements in flux and beam divergence are possible, and plans for achieving these coals are discussed.

Gubarev, Mikhail↗