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Results for “High resolution X-ray diffraction”

Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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NASA NTRS1987

Phase purity of NiCo2O4, a catalyst candidate for electrolysis of water

NiCo2O4 is shown to be difficult to obtain as a pure phase, and may never have been so obtained. High resolution x-ray diffractometry is required for its precise characterization. Film XRD is not likely to show the asymmetry in the spinel diffraction lines, caused by poorly crystallized NiO, as seen in diffractometer traces. The Co3O4 which is expected to accompany NiO as an impurity in NiCo2O4 syntheses has the same diffraction pattern as the binary oxide. Firings of the co-precipitated hydroxides at 300, 350, and 400 C, including one in pure O2, failed to produce single phase cobaltate. Scanning electron microscopy showed all the sintered products to range over several orders of magnitude in agglomerate/particle size. Surface areas by BET were all in the range 40 to 110 m sq/g, equivalent to particles of 200 to 100 Angstrom diameter. The spinel diffraction line breadths were compatible with those approximate dimensions.

Singer, J.↗
NASA NTRS1989

Center for the development of commercial crystal growth in space

The second year of operation of the Center for Commercial Crystal Growth in Space is described. This center is a consortium of businesses, universities and national laboratories. The primary goal of the Center's research is the development of commercial crystal growth in space. A secondary goal is to develop scientific understanding and technology which will improve commercial crystal growth on earth. In order to achieve these goals the Center's research is organized into teams by growth technique; melt growth, solution growth, and vapor growth. The melt growth team is working on solidification and characterization of bulk crystals of gallium arsenide and cadmium telluride. They used high resolution X-ray topography performed at the National Synchrotron Light Source at Brookhaven National Laboratory. Streak-like features were found in the diffraction images of semi-insulating undoped LEC GaAs. These were shown to be (110) antiphase boundaries, which have not been reported before but appear to be pervasive and responsible for features seen via less-sensitive characterization methods. The results on CdTe were not as definitive, but indicate that antiphase boundaries may also be responsible for the double peaks often seen in X-ray rocking curves of this material. A liquid encapsulated melt zone system for GaAs has been assembled and techniques for casting feed rods developed. It was found that scratching the inside of the quartz ampoules with silicon carbide abrasive minimized sticking of the GaAs to the quartz. Twelve floating zone experiments were done.

Wilcox, William R.↗
NASA NTRS1985

Construction of a multilayered X-ray telescope for solar coronal studies from space

The construction and testing of soft x-ray Ritchey-Chretien aplanatic telescope which is to be flown on a NASA sounding rocket in 1986 for very high resolution studies of the solar corona are discussed. Goals include figuring, polishing and measuring the mirror surfaces to tolerances exceding the 5000 A wavelength diffraction limit while achieving a superpolished surface finish, and the development of a structural design to withstand the rigors of the launch. Multilayer coatings are used to achieve usable reflectivity in the soft X-ray regime, and the design goal is for spatial resolution of 1/4 sec. Future applications are discussed.

Golub, L.↗
NASA NTRS1988

Soft X-ray images of the solar corona using normal incidence optics

A solar coronal loop system has been photographed in soft X-rays using a normal incidence telescope based on multilayer mirror technology. The telescope consisted of a spherical objective mirror of 4 cm aperture and 1 m focal length, a film cassette, and a focal plane shutter. A metallized thin plastic film filter was used to exclude visible light. The objective mirror was covered with a multilayer coating consisting of alternating layers of tungsten and carbon whose combined thicknesses satisfied the Bragg diffraction condition for 44 A radiation. The image was recorded during a rocket flight on October 25, 1985 and was dominated by emission lines arising from the Si XII spectrum. The rocket also carried a high resolution soft X-ray spectrograph that confirmed the presence of Si XII line radiation in the source. This image represents the first successful use of multilayer technology for astrophysical observations.

Bruner, M. E.↗
NASA NTRS1971

Electron microscopy and diffraction of layered, superconducting intercalation complexes.

Several layered, transition metal dichalcogenide intercalation complexes with unique superconducting properties have been examined by high-resolution electron microscopy and electron diffraction. Details of the crystalline lattice and of the lattice imperfections have been directly resolved. The results can be correlated with the available X-ray diffraction and chemical data, and they confirm and extend the postulated models.

Fernandez-Moran, H.↗
NASA NTRS1989

Dynamical diffraction imaging (topography) with X-ray synchrotron radiation

By contrast to electron microscopy, which yields information on the location of features in small regions of materials, X-ray diffraction imaging can portray minute deviations from perfect crystalline order over larger areas. Synchrotron radiation-based X-ray optics technology uses a highly parallel incident beam to eliminate ambiguities in the interpretation of image details; scattering phenomena previously unobserved are now readily detected. Synchrotron diffraction imaging renders high-resolution, real-time, in situ observations of materials under pertinent environmental conditions possible.

Kuriyama, M.↗
NASA NTRS1989

Three-dimensional structure of human serum albumin

The three-dimensional structure of human serum albumin has been solved at 6.0 A resolution by the method of multiple isomorphous replacement. Crystals were grown from solutions of polyethylene glycol in the infrequently observed space group P42(1)2 and diffracted X-rays to lattice d-spacings of less than 2.9 A. The electron density maps are of high quality and revealed the structure as a predominantly alpha-helical globin protein in which the course of the polypeptide can be traced. The binding loci of several organic compounds have been determined.

Carter, Daniel C.↗
NASA NTRS1994

Optical Analysis of an Ultra-High resolution Two-Mirror Soft X-Ray Microscope

This work has summarized for a Schwarzschild microscope some relationships between numerical aperture (NA), magnification, diameter of the primary mirror, radius of curvature of the secondary mirror, and the total length of the microscope. To achieve resolutions better than a spherical Schwarzschild microscope of 3.3 Lambda for a perfectly aligned and fabricated system. it is necessary to use aspherical surfaces to control higher-order aberrations. For an NA of 0.35, the aspherical Head microscope provides diffraction limited resolution of 1.4 Lambda where the aspherical surfaces differ from the best fit spherical surface by approximately 1 micrometer. However, the angle of incidence varies significantly over the primary and the secondary mirrors, which will require graded multilayer coatings to operate near peak reflectivities. For higher numerical apertures, the variation of the angle of incidence over the secondary mirror surface becomes a serious problem which must be solved before multilayer coatings can be used for this application. Tolerance analysis of the spherical Schwarzschild microscope has shown that water window operations will require 2-3 times tighter tolerances to achieve a similar performance for operations with 130 A radiation. Surface contour errors have been shown to have a significant impact on the MTF and must be controlled to a peak-to-valley variation of 50-100 A and a frequency of 8 periods over the surface of a mirror.

Shealy, David L.↗
NASA NTRS1994

Protein crystal growth in microgravity: Temperature induced large scale crystallization of insulin

One of the major stumbling blocks that prevents rapid structure determination using x-ray crystallography is macro-molecular crystal growth. There are many examples where crystallization takes longer than structure determination. In some cases, it is impossible to grow useful crystals on earth. Recent experiments conducted in conjuction with NASA on various Space Shuttle missions have demonstrated that protein crystals often grow larger and display better internal molecular order than their earth-grown counterparts. This paper reports results from three Shuttle flights using the Protein Crystallization Facility (PCF). The PCF hardware produced large, high-quality insulin crystals by using a temperature change as the sole means to affect protein solubility and thus, crystallization. The facility consists of cylinders/containers with volumes of 500, 200, 100, and 50 ml. Data from the three Shuttle flights demonstrated that larger, higher resolution crystals (as evidenced by x-ray diffraction data) were obtained from the microgravity experiments when compared to earth-grown crystals.

Long, Marianna M.↗
NASA NTRS1995

Transmission electron microscope studies of extraterrestrial materials

Transmission Electron Microscopy, X-Ray spectrometry and electron-energy-loss spectroscopy are used to analyse carbon in interplanetary dust particles. Optical micrographs are shown depicting cross sections of the dust particles embedded in sulphur. Selected-area electron diffraction patterns are shown. Transmission Electron Microscope specimens of lunar soil were prepared using two methods: ion-milling and ultramicrotomy. A combination of high resolution TEM imaging and electron diffraction is used to characterize the opaque assemblages. The opaque assemblages analyzed in this study are dominated by ilmenite with lesser rutile and spinel exsolutions, and traces of Fe metal.

Keller, Lindsay P.↗
NASA NTRS1991

Instrument design and test results of the new all-reflection spatial heterodyne spectrometer

An all-reflection spatial heterodyne spectrometer (SHS) has been recently developed. The advantages over conventional high-resolution grating spectrometers are that the SHS requires no mechanical scanning, a self-compensating optical design permits easy alignment, and it is much smaller than other spectrometers of comparable resolution. Since all beam-splits and recombinations occur by reflection off of a diffraction grating, the interferometer is capable of operating well into the extreme ultraviolet (EUV) and possibly into the soft X-ray region. A description of the design and the characteristics of the instrument is presented. Also, test results, including sample interferograms as well as their Fourier-transformed spectra, at both visible and UV wavelengths are shown. Finally, we report on future developments and possible applications.

Bush, Brett C.↗
NASA NTRS1987

X-ray optics - A technique for high resolution imaging

Both scattering and figure errors in grazing incidence optics are larger in the plane of incidence than out-of-plane by a factor equal to 1/sin theta, where theta is the graze angle. When the full annular aperture of a grazing incidence telescope is stopped down, the point spread function becomes highly elliptical with a width as much as sin theta times narrower than the full image. In practice, this means that improvements in resolution of up to 100 times can be achieved, and effective resolution can approach the diffraction limit. Laboratory data demonstrating the effect are presented.

Cash, Webster↗
NASA NTRS1990

Nature and origin of interstellar diamond from the Allende CV3 meteorite

Data and experimental evidence which support the contention that the C delta diamonds may result from grain-grain collisions in supernova shocks in the interstellar medium are presented. Fragments of the Allende CV3 chondrite were acid-treated. A whitish powder was obtained. For the Analytical Electron Microscopy (AEM) a small drop of ethanol suspension was transferred onto holey carbon support films on 3 mm EM grids. The AEM was performed on transmission-thin fragments of the material which overlay holes in the film, to eliminate interference from the substrate. Electron Spectroscopy for Chemical Analysis (ESCA) was performed on a large aliquot of C. Diamond was identified by selected area electron diffraction. Scanning Transmission Electron Microscope / Energy Dispersive X-ray (STEM-EDS) microanalyses of the C delta diamond, using a light-element detector, show that oxygen and possibly nitrogen are the only impurities consistently present. ESCA spectra from bulk C delta material confirm the presence of N at a level of 0.35 percent or less. Under UV irradiation a yellow-red fluorescence is observed, consistent with that of natural diamonds containing substitutional N. Electron Energy Loss Spectra (EELS) were recorded at 2 eV resolution from the C delta diamond, high pressure synthetic diamond, a diamond film produced in a low pressure plasma by chemical vapor deposition (CVD) on a heated silicon substrate (Roy, 1987), graphite, and amorphous arc sputtered carbon. Comparison of the carbon K edge shape and fine structure shows the Allende C delta phase to be largely diamond, but with a significant pre-edge absorption feature indicative of transitions of C 1s electrons into pi asterisk orbitals which are absent in the purely sp(3)-bonded diamond but present in graphite and amorphous carbon.

Blake, David↗
NASA NTRS1994

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↗
NASA NTRS1992

Large scale crystallization of protein pharmaceuticals in microgravity via temperature change

The major objective of this research effort is the temperature driven growth of protein crystals in large batches in the microgravity environment of space. Pharmaceutical houses are developing protein products for patient care, for example, human insulin, human growth hormone, interferons, and tissue plasminogen activator or TPA, the clot buster for heart attack victims. Except for insulin, these are very high value products; they are extremely potent in small quantities and have a great value per gram of material. It is feasible that microgravity crystallization can be a cost recoverable, economically sound final processing step in their manufacture. Large scale protein crystal growth in microgravity has significant advantages from the basic science and the applied science standpoints. Crystal growth can proceed unhindered due to lack of surface effects. Dynamic control is possible and relatively easy. The method has the potential to yield large quantities of pure crystalline product. Crystallization is a time honored procedure for purifying organic materials and microgravity crystallization could be the final step to remove trace impurities from high value protein pharmaceuticals. In addition, microgravity grown crystals could be the final formulation for those medicines that need to be administered in a timed release fashion. Long lasting insulin, insulin lente, is such a product. Also crystalline protein pharmaceuticals are more stable for long-term storage. Temperature, as the initiation step, has certain advantages. Again, dynamic control of the crystallization process is possible and easy. A temperature step is non-invasive and is the most subtle way to control protein solubility and therefore crystallization. Seeding is not necessary. Changes in protein and precipitant concentrations and pH are not necessary. Finally, this method represents a new way to crystallize proteins in space that takes advantage of the unique microgravity environment. The results from two flights showed that the hardware performed perfectly, many crystals were produced, and they were much larger than their ground grown controls. Morphometric analysis was done on over 4,000 crystals to establish crystal size, size distribution, and relative size. Space grown crystals were remarkably larger than their earth grown counterparts and crystal size was a function of PCF volume. That size distribution for the space grown crystals was a function of PCF volume may indicate that ultimate size was a function of temperature gradient. Since the insulin protein concentration was very low, 0.4 mg/ml, the size distribution could also be following the total amount of protein in each of the PCF's. X-ray analysis showed that the bigger space grown insulin crystals diffracted to higher resolution than their ground grown controls. When the data were normalized for size, they still indicated that the space crystals were better than the ground crystals.

Long, Marianna M.↗
NASA NTRS1972

A liquid radiation detector with high spatial resolution

Detector, using point anode, minimizes problem of oblique tracks by permitting construction of very thin counter. Detector is useful in cosmic ray and high energy physics research and X-ray and neutron diffraction technology.

Alvarez, L.↗
NASA NTRS1982

Echelle spectrographs at grazing incidence

It is shown that by using the conical diffraction mount, existing echelle gratings can be used at grazing incidence to achieve high spectral resolution in the extreme UV and soft X rays. Design considerations for grazing incidence echelle spectrographs are examined, and two sample designs are discussed. The first, for use in the extreme UV, has a primary mirror and an entrance slit to the spectrograph. The system has a resolution of 10,000, operates at any wavelength longward of 100 A, and covers 30% of the spectrum at a single setting. The X-ray spectrograph uses objective gratings to obtain spectral resolution of 28,000 over any factor of 2 in. wavelength. It operates to wavelengths as short as 4 A.

Cash, W.↗
NASA NTRS1983

High efficiency spectrographs for the EUV and soft X-rays

The use of grazing incidence optics and reflection grating designs is shown to be a method that improves the performance of spectrographs at wavelengths shorter than 1200 A. Emphasis is laid on spectroscopic designs for X ray and EUV astronomy, with sample designs for an objective reflection grating spectrograph (ORGS) and an echelle spectrograph for wavelengths longer than 100 A. Conical diffraction allows operations at grazing incidence in the echelle spectrograph. In ORGS, the extreme distance of X ray objects aids in collimating the source radiation, which encounters conical diffraction within the instrument, proceeds parallel to the optical axis, and arrives at the detector. A series of gratings is used to achieve the effect. A grazing echelle is employed for EUV observations, and offers a resolution of 20,000 over a 300 A bandpass.

Cash, W.↗