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NASA NTRS2003

Comparison of Synchrotron MicroXANES Determination of Fe(3+)/Sigma Fe with Moessbauer Values for Clean Mineral Separates of Pyroxene from Martian Meteorites

The oxidation state of Fe in Martian meteorites is a parameter of great interest and the ability to determine this value in micrometer scale samples is important. Intense, tunable x-ray sources at large synchrotron storage rings are being exploited to examine the Fe K-absorption edge with energy resolution of approx. 1-1.5eV in spots of 10x15 microns on thin sections of a wide variety of materials including several Martian meteorites. Synchrotron microXANES (SmX) spectroscopy is the technique that provides the most flexible capability for investigating Fe(3+)/Sigma Fe. Variation of Fe(3+)/Sigma Fe is manifested as a function of the energy of the pre-edge to the Fe absorption edge produced by the sample. SmX is at present the only technique that can be used with conventional polished thin sections. Data for a broad spectrum of minerals have been produced and indicate that SmX can be used with a large variety of samples types.

Delaney, J. S.↗
NASA NTRS1999

Characterization of ZnSe Single Crystals Grown by Physical Vapor Transport

ZnSe bulk crystals were grown by self-seeded physical vapor transport technique in horizontal and vertical configurations. The impurities and defects in the grown crystals were studied by glow discharge mass spectroscopy (GDMS) and low temperature photoluminescence (PL) measurements. The PL results on the starting material and the grown crystals are consistent with the low impurity levels measured by GDMS. The crystalline quality of the grown crystals were examined by synchrotron white beam X-ray topography (SWBXT) and high resolution triple X-ray diffraction (HRTXD). The SWBXT shows that, aside from twins, the overall crystalline quality of the vapor grown ZnSe crystals, especially in the contactless grown region, was quite high. The HRTXD results are in line with the SWBXT findings. The comparison between the HRTXD on a chemical-mechanically polished and a cleaved surface seems to indicate that polishing damage can obscure the true microstructure in the as-grown ZnSe crystals.

Su, Ching-Hua↗
NASA NTRS1999

Growth of II-VI Solid Solutions in the Presence of a Rotating Magnetic Field

The application of a rotating magnetic field (RMF)in the frequency range 60-400 Hz and field strength of the order of 2-8 mT to crystal growth has received increasing attention in recent years. To take full advantage of the control of fluid flow by the forces applied by the field, the liquid column must be electrically conducting. Also, the application of RMF to the directional solidification of a column of liquid can result in complete mixing in the resultant solid. Thus, the technique of RMF is suited to solvent zones and float zones where the composition of the liquid is more readily controlled. In the work we report on, numerical modeling has been applied to II-VI systems, particularly tellurium based traveling heater techniques (THM). Results for a spectrum of field strengths and acceleration levels will be presented. These show clearly the effects of competing buoyancy forces and electromagnetic stirring. Crystals of cadmium zinc telluride and mercury cadmium telluride have been grown terrestrially from a tellurium solvent zone. The effects of the RMF during these experiments will be demonstrated with micrographs showing etch pits, white beam x-ray synchrotron topographs and triple axis x-ray diffraction.

Gillies, D. C↗
NASA NTRS1987

Nuclear techniques in studies of condensed matter

Nuclear techniques have played an important role in the studies of materials over the past several decades. For example, X-ray diffraction, neutron diffraction, neutron activation, and particle- or photon-induced X-ray emission techniques have been used extensively for the elucidation of structural and compositional details of materials. Several new techniques have been developed recently. Four such techniques are briefly reviewed which have great potential in the study and development of new materials. Of these four, Mossbauer spectroscopy, muon spin rotation, and positron annihilation spectroscopy techniques exploit their great sensitivity to the local atomic environments in the test materials. Interest in synchrotron radiation, on the other hand, stems from its special properties, such as high intensity, high degree of polarization, and high monochromaticity. It is hoped that this brief review will stimulate interest in the exploitation of these newer techniques for the development of improved materials.

Singh, Jag J.↗
NASA NTRS1981

Radiometry using synchrotron radiation

It is possible to use synchrotron radiation from electron synchrotrons and electron storage rings as an absolute source, especially in the VUV and soft X-ray regions where other standards are difficult to find. At the NBS, an electron storage ring (SURF-II) has been used to calibrate spectrometers and photometers utilized in solar and aeronomy research and in fusion plasma diagnostics. The radiation incident on these spectrometers can be calculated to uncertainties of 3%, and a technique to exactly determine the number of electrons orbiting in the ring is currently being developed to reduce this uncertainty. Detector calibrations between 5 and 55 nm are routinely performed at SURF-II and transfer standard detectors with 6-10% uncertainties over the range 5-254 nm are supplied.

Saloman, E. B.↗
NASA NTRS1993

Growth of ZnTe by Physical Vapor Transport and Traveling Heater Method

ZnTe crystals were grown by horizontal physical vapor transport (PVT) and a Te-solution vertical traveling heater method (THM). The grown crystals were examined by X-ray Laue diffraction technique and Hall measurements to determine the growth orientation and the electrical properties of the crystals. They were also characterized by low temperature infrared (IR) absorption measurements. Several sets of distinct peaks were observed in the IR absorption spectra for the THM samples and were identified as resulting from CU(2+) impurities. Similar measurements on vapor grown ZnTe showed featureless absorption spectra. Chemical analyses were carried out to measure the impurity content in various ZnTe samples and synchrotron radiation topography was used to Study crystalline microstructure of the (111) ZnTe single crystals grown by PVT.

Su, Ching-Hua↗
NASA NTRS1993

Synchrotron/crystal sample preparation

The Center for Applied Optics (CAO) of the University of Alabama in Huntsville (UAH) prepared this final report entitled 'Synchrotron/Crystal Sample Preparation' in completion of contract NAS8-38609, Delivery Order No. 53. Hughes Danbury Optical Systems (HDOS) is manufacturing the Advanced X-ray Astrophysics Facility (AXAF) mirrors. These thin-walled, grazing incidence, Wolter Type-1 mirrors, varying in diameter from 1.2 to 0.68 meters, must be ground and polished using state-of-the-art techniques in order to prevent undue stress due to damage or the presence of crystals and inclusions. The effect of crystals on the polishing and grinding process must also be understood. This involves coating special samples of Zerodur and measuring the reflectivity of the coatings in a synchrotron system. In order to gain the understanding needed on the effect of the Zerodur crystals by the grinding and polishing process, UAH prepared glass samples by cutting, grinding, etching, and polishing as required to meet specifications for witness bars for synchrotron measurements and for investigations of crystals embedded in Zerodur. UAH then characterized these samples for subsurface damage and surface roughness and figure.

Johnson, R. Barry↗
NASA NTRS1983

In situ trace element microanalysis

The use of particle-track-radiography and X-ray- fluorescence techniques in the in situ measurement of trace (less than 1000 ppm) elements in single mineral phases of polished sections is surveyed, and examples of their application to ordinary, carbonaceous and enstatite chondrites are provided. Radiographic methods surveyed include fission-track radiography (for U, Th, and Pu-244), alpha radiography using nuclear reactions (for Li and B), alpha autoradiography (for Bi and Pb), and beta autoradiography (for several elements in synthetic or biological samples). Two X-ray-fluorescence methods are compared: (1) photon-induced X-ray emission (PIXE), and (2) the potential use of synchrotron radiation. The latter is shown to allow much greater sensitivity than current PIXE technology and a much broader range of elements than particle-track radiography: the ppm analysis of 10-micron grains for all elements heavier than Na. These advantages are seen as balancing the high cost of accelerator use.

Burnett, D. S.↗
NASA NTRS1992

The x ray reflectivity of the AXAF VETA-I optics

The x-ray reflectivity of the VETA-I optic, the outermost shell of the AXAF x-ray telescope, with a bare Zerodur surface, is measured and compared with theoretical predictions. Measurements made at energies of 0.28, 0.9, 1.5, 2.1, and 2.3 keV are compared with predictions based on ray trace calculations. The data were obtained at the x-ray calibrations facility at Marshall Space Flight Center with an electron impact x-ray source located 528 m from the grazing incidence mirror. The source used photoelectric absorption filters to eliminate bremsstrahlung continuum. The mirror has a diameter of 1.2 m and a focal length of 10 m. The incident and reflected x-ray flux are detected using two proportional counters, one located in the incident beam of x-rays at the entrance aperture of the VETA-I, and the other in the focal plane behind an aperture of variable size. Results on the variation of the reflectivity with energy as well as the absolute value of the reflectivity are presented. We also present a synchrotron reflectivity measurement with high energy resolution over the range 0.26 to 1.8 keV on a flat Zerodur sample, done at NSLS. We present evidence for contamination of the flat by a thin layer of carbon on the surface, and the possibility of alteration of the surface composition of the VETA-I mirror perhaps by the polishing technique. The overall agreement between the measured and calculated effective area of VETA-I is between 2.6 percent and 10 percent, depending on which model for the surface composition is adopted. Measurements at individual energies deviate from the best-fitting calculation to 0.3 to 0.8 percent, averaging 0.6 percent at energies below the high energy cutoff of the mirror reflectivity, and are as high as 20.7 percent at the cutoff. We also discuss the approach to the final preflight calibration of the full AXAF flight mirror.

Kellogg, Edwin M.↗
NASA NTRS1998

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.↗
NASA NTRS2004

Oxygen Fugacity of Mare Basalts and the Lunar Mantle Application of a New Microscale Oxybarometer Based on the Valence State of Vanadium

The ability to estimate oxygen fugacities for mare basalts and to extend these observations to the lunar mantle is limited using bulk analysis techniques based on buffering assemblages or the valence state of iron. These limitations are due to reequilibration of mineral assemblages at subsolidus conditions, deviations of mineral compositions from thermodynamic ideality, size requirements, and the limits of the iron valence at very low fO2. Still, these approaches have been helpful and indicate that mare basalts crystallized at fO2 between the iron-w stite buffer (IW) and the ilmenite breakdown reaction (ilmenite = rutile + iron). It has also been inferred from these estimates that the lunar mantle is also highly reduced lying at conditions below IW. Generally, these data cannot be used to determine if the mare basalts become increasingly reduced during transport from their mantle source and eruption at the lunar surface and if there are differences in fO2 among mare basalts or mantle sources. One promising approach to determining the fO2 of mare basalts is using the mean valence of vanadium (2+, 3+, 4+, 5+) determined on spots of a few micrometers in diameter using synchrotron x-ray absorption fine structure (XAFS) spectroscopy. The average valence state of V in basaltic glasses is a function of fO2, temperature, V coordination, and melt composition. Here, we report the initial results of this approach applied to lunar pyroclastic glasses.

Shearer, C. K.↗
NASA NTRS1995

Multiwavelength monitoring of the BL Lacertae object PKS 2155-304. 4: Multiwavelength analysis

Simultaneous X-ray, ultraviolet, optical, infrared, and radio monitoring data were used to test and constrain models of continuum emission from the BL Lacertae object PKS 2155-304. Intensively sampled ultraviolet and soft X-ray light curves showed a clear temporal correlation with the X-rays leading the ultraviolet by 2-3 hr. This lag was found to be significantly different from zero after an exhaustive comparison of four different techniques for measuring temporal correlations. Variations in the ultraviolet trough optical wave bands were also strongly correlated, with no measurable lag down to limiting timescales of approximately less than 1-2 hr. This strong correlation extends to the near-infrared, but the less intensive sampling precludes measurement of any lag beyomnd an upper limit of approximately less than 1 day. These lags and limits of the order of hours are much shorter than most rapid observed single-band variations. Because of the very sparse radio sampling, it was not possible to measure quantitatively the correlation and lag with shorter wavelengths, but the data do suggest that the radio may lag the optical/ultraviolet by approximately 1 week, with longer delays and weaker variations to longer radio wavelengths. The epoch-folding Q(exp 2) statistic was used to test for periodicity, and no evidence for strict or quasi-periodicity was found in any of the light curves. Because they lead the lower frequencies, the soft X-rays (approximately less than 1 keV) cannot arise from synchrotron self-Compton scattering. These results also rule out the accretion disk model, which predicts a measurable lag between ultraviolet/optical wavelength bands and a correlation between hardness and brightness, neither of which were seen. They are consistent with the entire radio through X-ray continuum arising from direct synchrotron emission from a relativistic jet. However, the tapered jet model, in which the X-ray emission is produced closer in, has problems explaining the magnitude of the ultraviolet/X-ray lag, because the X-ray-emitting electrons have very short lifetimes (t(sub 1/2) much less than 1 s). The result that the lag is much smaller than the variability timescale suggests instead that the radiation may be produced in a flattened region such as a shock front.

Edelson, R.↗
NASA NTRS2003

Robust Extraction and Multi-Technique Analysis of Micrometeoroids Captured in Low Earth Orbit

The use of low-density silica aerogel as the primary capture cell technology for the NASA Discovery mission Stardust to Comet Wild-2 [1] is a strong motivation for researchers within the Meteoritics community to develop techniques to handle this material. The unique properties of silica aerogel allow dust particles to be captured at hypervelocity speeds and to remain partially intact. The same unique properties present difficulties in the preparation of particles for analysis. Using tools borrowed from microbiologists, we have developed techniques for robustly extracting captured hypervelocity dust particles and their residues from aerogel collectors[2-3]. It is important not only to refine these extraction techniques but also to develop protocols for analyzing the captured particles. Since Stardust does not return material to Earth until 2006, researchers must either analyze particles that are impacted in the laboratory using light-gasgun facilities [e.g. 41 or examine aerogel collectors that have been exposed in low-Earth orbit (LEO) [5]. While there are certainly benefits in laboratory shots, i.e. accelerating known compositions of projectiles into aerogel, the LEO capture particles offer the opportunity to investigate real particles captured under real conditions. The aerogel collectors used in this research are part of the NASA Orbital Debris Collection Experiment that was exposed on the MIR Space Station for 18 months [5]. We have developed the capability at the UCB Space Sciences Laboratory to extract tiny volumes of aerogel that completely contain each impact event, and to mount them on micromachined fixtures so that they can be analyzed with no interfering support (Fig.1). These aerogel keystones simultaneously bring the terminal particle and the particle track to within 10 m (15 g cm- ) of the nearest aerogel surface. The extracted aerogel wedges containing both the impact tracks and the captured particles have been characterized using the synchrotron total external reflection X-ray fluorescence (TXRF) microprobe at SSRL, the Nuclear Microprobe at LLNL, synchrotron infrared microscopy at the ALS facility at LBL and the NSLS at BNL, and the Total Reflection X-ray Fluorescence (TXRF) facility at SLAC.

Westphal, A. J.↗
NASA NTRS1999

Solidification of II-VI Compounds in a Rotating Magnetic Field

This project is aimed at using a rotating magnetic field (RMF) to control fluid flow and transport during directional solidification of elemental and compound melts. Microgravity experiments have demonstrated that small amounts of residual acceleration of less than a micro-g can initiate and prolong fluid flow, particularly when there is a static component of the field perpendicular to the liquid solid interface. Thus a true diffusion boundary layer is not formed, and it becomes difficult to verify theories of solidification or to achieve diffusion controlled solidification. The RMF superimposes a stirring effect on an electrically conducting liquid, and with appropriate field strengths and frequencies, controlled transport of material through a liquid column can be obtained. As diffusion conditions are precluded and complete mixing conditions prevail, the technique is appropriate for traveling solvent zone or float zone growth methods in which the overall composition of the liquid can be maintained throughout the growth experiment. Crystals grown by RMF techniques in microgravity in previous, unrelated missions have shown exceptional properties. The objective of the project is two-fold, namely (1) using numerical modeling to simulate the behavior of a solvent zone with applied thermal boundary conditions and demonstrate the effects of decreasing gravity levels, or an increasing applied RMF, or both, and (2) to grow elements and II-VI compounds from traveling solvent zones both with and without applied RMFs, and to determine objectively how well the modeling predicts solidification parameters. Numerical modeling has demonstrated that, in the growth of CdTe from a tellurium solution, a rotating magnetic field can advantageously modify the shape of the liquid solid interface such that the interface is convex as seen from the liquid. Under such circumstances, the defect structure is reduced as any defects which are formed tend to grow out and not propagate. The flow of liquid, however, is complex due to the competing flow induced by the rotating magnetic field and the buoyancy driven convection. When the acceleration forces are reduced to one thousandth of gravity, the flow pattern is much simplified and well controlled material transport through the solvent zone can be readily achieved. Triple axis diffractometry and x-ray synchrotron topography have demonstrated that there is no significant improvement in crystal quality for HgCdTe grown on earth from a tellurium solution when a rotating magnetic field is applied. However, modeling shows that the flow in microgravity with a rotating magnetic field would produce a superior product.

Gillies, D. C.↗
NASA NTRS1994

Relativistic particle acceleration in plerions

We discuss recent research on the structure and particle acceleration properties of relativistic shock waves in which the magnetic field is transverse to the flow direction in the upstream medium, and whose composition is either pure electrons and positrons or primarily electrons and positrons with an admixture of heavy ions. Particle-in-cell simulation techniques as well as analytic theory have been used to show that such shocks in pure pair plasmas are fully thermalized -- the downstream particle spectra are relativistic Maxwellians at the temperature expected from the jump conditions. On the other hand, shocks containing heavy ions which are a minority constituent by number but which carry most of the energy density in the upstream medium do put approximately 20% of the flow energy into a nonthermal population of pairs downstream, whose distribution in energy space is N(E) varies as E(exp -2), where N(E)dE is the number of particles with energy between E and E+dE. The mechanism of thermalization and particle acceleration is found to be synchrotron maser activity in the shock front, stimulated by the quasi-coherent gyration of the whole particle population as the plasma flowing into the shock reflects from the magnetic field in the shock front. The synchrotron maser modes radiated by the heavy ions are absorbed by the pairs at their (relativistic) cyclotron frequencies, allowing the maximum energy achievable by the pairs to be gamma(sub +/-)m(sub +/-)c squared = m(sub i)c squared gamma(sub 1)/Z(sub i), where gamma(sub 1) is the Lorentz factor of the upstream flow and Z(sub i) is the atomic number of the ions. The shock's spatial structure is shown to contain a series of 'overshoots' in the magnetic field, regions where the gyrating heavy ions compress the magnetic field to levels in excess of the eventual downstream value. This shock model is applied to an interpretation of the structure of the inner regions of the Crab Nebula, in particular to the 'wisps,' surface brightness enhancements near the pulsar. We argue that these surface brightness enhancements are the regions of magnetic overshoot, which appear brighter because the small Larmor radius pairs are compressed and radiate more efficiently in the regions of more intense magnetic field. This interpretation suggests that the structure of the shock terminating the pulsar's wind in the Crab Nebula is spatially resolved, and allows one to measure gamma(sub 1) and a number of other properties of the pulsar's wind. We also discuss applications of the shock theory to the termination shocks of the winds from rotation-powered pulsars embedded in compact binaries. We show that this model adequately accounts for (and indeed predicted) the recently discovered X-ray flux from PSR 1957+20, and we discuss several other applications to other examples of these systems.

Arons, Jonathan↗
NASA NTRS1977

Very high-energy gamma ray astronomy

Recent results in ground-based very high-energy (less than 10 to the eleventh power eV) gamma-ray astronomy are reviewed. The various modes of the atmospheric Cerenkov technique are described, and the importance of cosmic ray rejection methods is stressed. The positive detections (at approximately less than 10 to the 12th power eV) of the Crab pulsar that suggest a very flat spectrum and time-variable pulse phase are discussed. Observations of other pulsars (particularly Vela) suggest that these features may be general. The steady flux upper limits for the Crab Nebula are thus reconsidered, and a new value of the implied (Compton-synchrotron) magnetic field in the Nebula is reported. Evidence that a 4.8-hour modulated effect was detected at E sub gamma is less than 10 to the 12th power eV from Cyg X-3 is strengthened in that the exact period originally proposed agrees well with a recent determination of the X-ray period. The southern sky observations are reviewed, and the significance of the detection of an active galaxy (NGC 5128) is considered for source models and future observations.

Grindlay, J. E.↗
NASA NTRS1993

The X-ray reflectivity of the AXAF VETA-I optics

The study measures the X-ray reflectivity of the AXAF VETA-I optic and compares it with theoretical predictions. Measurements made at energies of 0.28, 0.9, 1.5, 2.1, and 2.3 keV are compared with predictions based on ray trace calculations. Results on the variation of the reflectivity with energy as well as the absolute value of the reflectivity are presented. A synchrotron reflectivity measurement with a high-energy resolution over the range 0.26 to 1.8 keV on a flat Zerodur sample is also reported. Evidence is found for contamination of the flat by a thin layer of carbon on the surface, and the possibility of alteration of the surface composition of the VETA-I mirror, perhaps by the polishing technique. The overall agreement between the measured and calculated effective area of VETA-I is between 2.6 and 10 percent. Measurements at individual energies deviate from the best-fitting calculation to 0.3 to 0.8 percent, averaging 0.6 percent at energies below the high energy cutoff of the mirror reflectivity, and are as high as 20.7 percent at the cutoff.

Kellogg, E.↗
NASA NTRS1994

Gamma-ray bright quasars and BL Lacertae objects: EGRET data

The Compton Gamma-Ray Observatory (CGRO) Instruments, in particular, EGRET, have recently discovered new, gamma-ray bright active galactic nuclei (AGNs)(fluxes approximately 0.5-3 times as bright as 3C 273). Yet current sample sizes are modest (for example, EGRET as of 1993 January has detected 17 quasars and five BL Lac objects), and the sources probe only a small range in flux. Only by using a large, unbiased sample of AGNs can we answer key questions about source evolution, contributions to the gamma-ray background, and the different gamma-ray properties of quasars and BL Lac objects. Therefore, we need gamma-ray data on a much larger number of AGNs. We are currently pursuing two approaches toward remedying this situation: first, new (phase 2) OSSE, COMPTEL, and EGRET observations of X-ray selected AGNs predicted to be gamma-ray bright on simple assumptions; even an upper limit can set constraints on continuum models (e.g., pair production, synchrotron self-Compton); second, searches for radio-selected AGNs in wide-field EGRET data obtained during the pointings. For these AGN, we expect a large number of faint sources (i.e., mainly low signal-to-noise ratio detections and upper limits), a continuous progression down to the limiting EGRET sensitivity. Although special techniques must be employed to deal carefully with low-significance sources, the end product will be a much larger sample than currently available on which to base deductions about the gamma-ray properties of AGNs. Here we report the first results of this program. We find an upper limit for 3C 382 and demonstrate, using the 3C 382 field, how serendipitous blazars can systematically searched for in existing EGRET public (Phase 1) data. Preliminary results indicate that synchrotron self-Compton processes dominate.

Schachter, Jonathan↗