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Surprising Coordination Geometry Differences in Ce(IV)- and Pu(IV)-Maltol Complexes

Description: As part of a study to characterize the detailed coordination behavior of Pu(IV), single crystal X-ray diffraction structures have been determined for Pu(IV) and Ce(IV) complexes with the naturally-occurring ligand maltol (3-hydroxy-2-methyl-pyran-4-one) and its derivative bromomaltol (5-bromo-3-hydroxy-2-methyl-pyran-4-one). Although Ce(IV) is generally accepted as a structural analog for Pu(IV), and the maltol complexes of these two metals are isostructural, the corresponding bromomaltol complexes are strikingly different with respect to ligand orientation about the metal ion: All complexes exhibit trigonal dodecahedral coordination geometry but the Ce(IV)-bromomaltol complex displays an uncommon ligand arrangement not mirrored in the Pu(IV) complex, although the two metal species are generally accepted to be structural analogs.
Date: February 12, 2008
Creator: Laboratory, Lawrence Berkeley National; Raymond, Kenneth; Szigethy, Geza; Xu, Jide; Gorden, Anne E.V.; Teat, Simon J. et al.
Partner: UNT Libraries Government Documents Department

Incorporating Electrochemistry and X-ray Diffraction Experiments Into an Undergraduate Instrumental Analysis Course

Description: Experiments were designed for an undergraduate instrumental analysis laboratory course, two in X-ray diffraction and two in electrochemistry. Those techniques were chosen due their underrepresentation in the Journal of Chemical Education. Paint samples (experiment 1) and pennies (experiment 2) were characterized using x-ray diffraction to teach students how to identify different metals and compounds in a sample. in the third experiment, copper from a penny was used to perform stripping analyses at different deposition times. As the deposition time increases, the current of the stripping peak also increases. the area under the stripping peak gives the number of coulombs passed, which allows students to calculate the mass of copper deposited on the electrode surface. the fourth experiment was on the effects of variable scan rates on a chemical system. This type of experiment gives valuable mechanistic information about the chemical system being studied.
Date: May 2012
Creator: Molina, Cathy
Partner: UNT Libraries

X-ray diffraction characterization of suspended structures forMEMS applications

Description: Mechanical stress control is becoming one of the major challenges for the future of micro and nanotechnologies. Micro scanning X-ray diffraction is one of the promising techniques that allows stress characterization in such complex structures at sub micron scales. Two types of MEMS structure have been studied: a bilayer cantilever composed of a gold film deposited on poly-silicon and a boron doped silicon bridge. X-ray diffraction results are discussed in view of numerical simulation experiments.
Date: September 15, 2005
Creator: Goudeau, P.; Tamura, N.; Lavelle, B.; Rigo, S.; Masri, T.; Bosseboeuf, A. et al.
Partner: UNT Libraries Government Documents Department

The Reactivity Patterns of Low-Coordinate Iron-Hydride Complexes

Description: This article discusses the reactivity patterns of low-coordinate iron-hydride complexes. The authors report a survey of the reactivity of the first isolable iron-hydride complexes with a coordiination number less than 5.
Date: April 30, 2008
Creator: Yu, Ying; Sadique, Azwana R.; Smith, Jeremy M.; Dugan, Thomas R.; Cowley, Ryan E.; Brennessel, William W. et al.
Partner: UNT College of Arts and Sciences

THREE-DIMENSIONAL IMAGING OF NANOSCALE MATERIALS BY UISNG COHERENT X-RAYS

Description: X-ray crystallography is currently the primary methodology used to determine the 3D structure of materials and macromolecules. However, many nanostructures, disordered materials, biomaterials, hybrid materials and biological specimens are noncrystalline and, hence, their structures are not accessible by X-ray crystallography. Probing these structures therefore requires the employment of different approaches. A very promising technique currently under rapid development is X-ray diffraction microscopy (or lensless imaging), in which the coherent X-ray diffraction pattern of a noncrystalline specimen is measured and then directly phased to obtain a high-resolution image. Through the DOE support over the past three years, we have applied X-ray diffraction microscopy to quantitative imaging of GaN quantum dot particles, and revealed the internal GaN-Ga2O3 core shell structure in three dimensions. By exploiting the abrupt change in the scattering cross-section near electronic resonances, we carried out the first experimental demonstration of resonant X-ray diffraction microscopy for element specific imaging. We performed nondestructive and quantitative imaging of buried Bi structures inside a Si crystal by directly phasing coherent X-ray diffraction patterns acquired below and above the Bi M5 edge. We have also applied X-ray diffraction microscopy to nondestructive imaging of mineral crystals inside biological composite materials - intramuscular fish bone - at the nanometer scale resolution. We identified mineral crystals in collagen fibrils at different stages of mineralization and proposed a dynamic mechanism to account for the nucleation and growth of mineral crystals in the collagen matrix. In addition, we have also discovered a novel 3D imaging modality, denoted ankylography, which allows for complete 3D structure determination without the necessity of sample titling or scanning. We showed that when the diffraction pattern of a finite object is sampled at a sufficiently fine scale on the Ewald sphere, the 3D structure of the object is determined by the 2D spherical pattern. We ...
Date: April 18, 2011
Creator: Miao, Jianwei
Partner: UNT Libraries Government Documents Department

Crystal Splitting in the Growth of Bi2S3

Description: Novel Bi{sub 2}S{sub 3} nanostructures with a sheaf-like morphology are obtained via reaction of bismuth acetate-oleic acid complex with elemental sulfur in 1-octadecence. We propose these structures form by the splitting crystal growth mechanism, which is known to account for the morphology some mineral crystals assume in nature. By controlling the synthetic parameters, different forms of splitting, analogous to observed in minerals, are obtained in our case of Bi{sub 2}S{sub 3}. These new and complex Bi{sub 2}S{sub 3} nanostructures are characterized by TEM, SEM, XRD and ED.
Date: June 15, 2006
Creator: Tang, Jing & Alivisatos, A. Paul
Partner: UNT Libraries Government Documents Department

Determination of mineral abundances in samples from the Exploratory Studies Facility, Yucca Mountain, Nevada, using x-ray diffraction

Description: Tuff samples collected from the Exploratory Studies Facility (ESF) were X-rayed to estimate relative mineral abundances. X-ray analysis was performed on sub-samples of specimens collected from both the Single Heater Test (SHT) and Drift Scale Heater Test (MT) that were used for thermomechanical measurements, as well as samples collected from cores retrieved from boreholes in the Drift Scale Test Area. The abundance of minerals that could affect the behavior of the host rock at repository relevant temperatures is of particular interest. These minerals include cristobalite, which undergoes a phase transition and volume change at elevated temperature (-250 {degree}C), and smectite and clinoptilolite that can dehydrate at elevated temperature with accompanying volume reduction. In addition, the spatial distribution of Si02 polymorphs and secondary minerals may provide evidence for deducing past fluid pathways. The mineral abundances tabulated here include data reported previously in three milestone reports but reanalyzed, as well as previously unreported data.
Date: January 13, 1998
Creator: Roberts, S. & Viani, B.
Partner: UNT Libraries Government Documents Department

Multitechnique Analysis of the Lattice Structures of Highly Siliceous Zeolites

Description: The combined use of high-resolution solid state NMR techniques (both 1D and 2D) with synchrotron-based powder x-ray diffraction studies yields detailed information on the lattice structures of highly siliceous zeolites. The two methods are complementary, the former probing short range ordering and structures while the latter is sensitive to long range orderings and periodicities.
Date: August 26, 1999
Creator: Fyfe, C. A.; Gies, H.; Kokotailo, G. T.; Feng, Y.; Strobl, H.; Marler, B. et al.
Partner: UNT Libraries Government Documents Department

Effects of Fe spin transition on the elasticity of (Mg,Fe)O magnesiow�ustites and implications for the seismological properties of the Earth's lower mantle

Description: High-pressure x-ray diffraction of (Mg{sub 0.8}Fe{sub 0.2})O at room temperature reveals a discontinuity in the bulk modulus at 40 ({+-}5) GPa, similar pressure at which an electronic spin-pairing transition of Fe{sup 2+} is also observed. In the x-ray diffraction experiments the transition is completed only at 80 GPa, possibly reflecting lack of equilibration. Combining recent measurements, we document anomalies in the compression curve of Mg-rich magnesiowuestites that are manifestations of the spin transition. The best fit to a third order Birch-Murnaghan equation for the low-spin phase of magnesiowuestite with 17-20 mol% FeO yields bulk modulus K{sub T0} = 190 ({+-}150) GPa, pressure derivative ({partial_derivative}K{sub T}/{partial_derivative}){sub T0} = 4.6 ({+-}2.7) and unit-cell volume V{sub 0} = 71 ({+-}5) {angstrom}{sup 3}, consistent with past estimates of the ionic radius of octahedrally-coordinated low-spin Fe{sup 2+} in oxides. A sharp spin transition at lower-mantle depths between 1100 and 1900 km (40-80 GPa) would cause a unit-cell volume decrease ({Delta}{nu}{sub {phi}}) of 3.7 ({+-}0.8) to 2.0 ({+-}0.2) percent and bulk sound velocity increase ({Delta}{nu}{sub {phi}}) of 8.1 ({+-}6-1.7) percent ({nu}{sub {phi}} = {radical}K{sub s}/{rho}). Even in the absence of a visible seismic discontinuity, we expect the Fe-spin transition to imply a correction to current compositional models of the lower mantle, with up to 10 mol percent increase of magnesiowuestite being required to match the seismological data.
Date: August 29, 2006
Creator: Speziale, S; Lee, V E; Clark, S M; Lin, J F; Pasternak, M P & Jeanloz, R
Partner: UNT Libraries Government Documents Department

Phase Identification of Seismic Borehole Samples

Description: This report documents the phase identification results obtained by x-ray diffraction (XRD) analysis of samples taken from borehole C4998 drilled at the Waste Treatment Plant (WTP) on the Hanford Site (REF). XRD samples were taken from fractures and vesicles or are minerals of interest at areas of interest within the basalt formations cored. The samples were powder mounted and analyzed. Search-match software was used to select the best match from the ICDD mineral database based on peak locations and intensities.
Date: November 1, 2006
Creator: Crum, Jarrod V. & Riley, Brian J.
Partner: UNT Libraries Government Documents Department

Amorphous clusters in Co implanted ZnO induced by boron pre-implantation

Description: We demonstrate the formation of superparamagnetic/ferromagnetic regions within ZnO(0001) single crystals sequently implanted with B and Co. While the pre-implantation with B plays a minor role for the electrical transport properties, its presence leads to the formation of amorphous phases. Moreover, B acts strongly reducing on the implanted Co. Thus, the origin of the ferromagnetic ordering in local clusters with large Co concentration is itinerant d-electrons as in the case of metallic Co. The metallic amorphous phases are non-detectable by common X-ray diffraction.
Date: February 9, 2009
Creator: Potzger, K.; Shalimov, A.; Zhou, S.; Schmidt, H.; Mucklich, A.; Helm, M. et al.
Partner: UNT Libraries Government Documents Department

Direct Observation of the alpha-epsilon Transition in Shock-compressed Iron via Nanosecond X-ray Diffraction

Description: In-situ x-ray diffraction studies of iron under shock conditions confirm unambiguously a phase change from the bcc ({alpha}) to hcp ({var_epsilon}) structure. Previous identification of this transition in shock-loaded iron has been inferred from the correlation between shock wave-profile analyses and static high-pressure x-ray measurements. This correlation is intrinsically limited because dynamic loading can markedly affect the structural modifications of solids. The in-situ measurements are consistent with a uniaxial collapse along the [001] direction and shuffling of alternate (110) planes of atoms, and in good agreement with large-scale non-equilibrium molecular dynamics simulations.
Date: March 21, 2005
Creator: Kalantar, D. H.; Belak, J. F.; Collins, G. W.; Colvin, J. D.; Davies, H. M.; Eggert, J. H. et al.
Partner: UNT Libraries Government Documents Department

Real-time Studies of Shocked Polycrystalline Materials with Single-Pulse X-ray Diffraction

Description: Characteristic K-α x-rays used for single-pulse XRD are conventionally produced by a 37-stage high-voltage Marx pulse generator coupled to a vacuum needle-and-washer x-ray diode via coaxial transmission line. A large field-of-view x-ray image plate detection system typically enables observation of several Debye-Scherrer rings. Recently, we have developed a fiber-optic reducer, coupled to a CCD camera, to obtain low-noise, large field-of-view images. The direct beam spot is produced by bremsstrahlung radiation attenuated by a twomillimeter tungsten beam stop. Determination of the direct beam position is necessary to perform the ring integration.
Date: May 25, 2011
Creator: Morgan, Dane V.
Partner: UNT Libraries Government Documents Department

In situ laser heating and radial synchrotron X-ray diffraction ina diamond anvil cell

Description: We report a first combination of diamond anvil cell radialx-ray diffraction with in situ laser heating. The laser-heating setup ofALS beamline 12.2.2 was modified to allow one-sided heating of a samplein a diamond anvil cell with an 80 W yttrium lithium fluoride laser whileprobing the sample with radial x-ray diffraction. The diamond anvil cellis placed with its compressional axis vertical, and perpendicular to thebeam. The laser beam is focused onto the sample from the top while thesample is probed with hard x-rays through an x-ray transparentboron-epoxy gasket. The temperature response of preferred orientation of(Fe,Mg)O is probed as a test experiment. Recrystallization was observedabove 1500 K, accompanied by a decrease in stress.
Date: June 29, 2007
Creator: Kunz, Martin; Caldwell, Wendel A.; Miyagi, Lowell & Wenk,Hans-Rudolf
Partner: UNT Libraries Government Documents Department

Can Ionic Liquids Be Used As Templating Agents For Controlled Design of Uranium-Containing Nanomaterials?

Description: Nanostructured uranium oxides have been prepared in ionic liquids as templating agents. Using the ionic liquids as reaction media for inorganic nanomaterials takes advantage of the pre-organized structure of the ionic liquids which in turn controls the morphology of the inorganic nanomaterials. Variation of ionic liquid cation structure was investigated to determine the impact on the uranium oxide morphologies. For two ionic liquid cations, increasing the alkyl chain length increases the aspect ratio of the resulting nanostructured oxides. Understanding the resulting metal oxide morphologies could enhance fuel stability and design.
Date: April 9, 2013
Creator: Visser, A.; Bridges, N. & Tosten, M.
Partner: UNT Libraries Government Documents Department

Flash X-Ray Diffraction System for Fast, Single-PulseTemperature and Phase Transition Measurements (Pre-print)

Description: A new, fast, single-pulse diagnostic for determining phase transitions and measuring the bulk temperature of polycrystalline metal objects has been developed. The diagnostic consists of a 37-stage Marx bank with a cable-coupled X-ray diode that produces a 35-ns pulse of mostly 0.71-{angstrom} monochromatic X rays and a P-43 fluor coupled to a cooled, charge-coupled device camera by a coherent fiber-optic bundle for detection of scattered X rays. The X-ray beam is collimated to a 1{sup o} divergence in the scattering plane with the combination of a 1.5-mm tungsten pinhole and a 1.5-mm-diameter molybdenum anode. X rays are produced by a high-energy electron beam transiting inward from the cathode to the anode in a needle-and-washer configuration. The anode's characteristic K-{alpha} X-ray emission lines are utilized for this diffraction system. The X-ray anode is heavily shielded in all directions other than the collimated beam. The X-ray diode has a sealed reentrant system, allowing X rays to be produced inside a vacuum containment vessel, close to the sample under study.
Date: June 12, 2007
Creator: Madlener, Michael J. & Morgan, Dane V.
Partner: UNT Libraries Government Documents Department

Flash X-Ray Diffraction System for Ultrafast Temperature and Phase Transition Measurements

Description: A novel ultrafast diagnostic for determining bulk temperature and phase transitions for polycrystalline metal objects has been developed. The diagnostic consists of a 38-stage Marx bank with a cable-coupled X-ray diode that produces a 35-ns pulse of mostly 0.71 Å monochromatic X rays, and a P-43 fluor coupled to a cooled charge-coupled device camera by a coherent fiber-optic bundle for detection of scattered X rays. The X-ray beam is collimated to a 1° divergence in the scattering plane with the combination of a 1.5-mm tungsten pinhole and a 1.5-mm diameter molybdenum anode. The X-ray diode, in a needle-and-washer configuration, is heavily shielded in all directions other than the collimated beam. The X-ray diode has a sealed reentrant system, which allows the X rays to be produced inside a vacuum containment vessel, close to the sample under study. The direct correlation between the solid-state structure and the coherent X-ray diffraction pattern from a metal surface allows an unequivocal determination of a phase transition. This correlation has been tested in the laboratory with samples of indium and tin. For both metals, diffraction lines were observed at temperatures just below the melt temperature, along with background consisting of Compton scattering and sample fluorescence. Upon melt, the diffraction lines were observed to disappear; however, the background from Compton scattering and sample fluorescence remained. Flash X-ray diffraction also enables direct ultrafast measurements of the bulk temperature of the sample under study. According to the Debye-Waller theory, the diffracted line intensity reduces as the temperature of the sample increases. The amplitude of the reduced diffracted signal also depends on the Debye temperature of the sample, the scattering angle of the diffracted X rays, and the X-ray wavelength. The feasibility of using the Debye-Waller theory for flash X-ray diffraction measurements of the bulk temperature is currently being ...
Date: June 1, 2007
Creator: Dane Morgan, Don Macy, Michael Madlener, Jaiming Morgan
Partner: UNT Libraries Government Documents Department

Final report [FASEB Summer Research Conference ''Virus Assembly''--agenda and attendee list]

Description: The conference brought together researchers working on virus structure and virus assembly in diverse systems. Information was integrated from many viral systems, including plant bacterial and eukaryotic viruses, and many techniques such as biophysical approaches of x-ray diffraction, electron microscopy and spectroscopy, along with molecular biological and molecular genetic analysis.
Date: January 31, 2001
Creator: Feiss, Michael
Partner: UNT Libraries Government Documents Department

Anticlastic curvature measurements on unribbed crystal optics for synchrotron radiation

Description: Various methods have been proposed for measuring the distortion in perfect crystals using double-crystal methods. The majority of these methods rely on making comparisons between double-crystal rocking curve measurements under the spatial extent of an extended x-ray beam. Unless the beam is large and parallel (such as at a synchrotron bending magnet), these methods are not easily scalable to large crystals (e.g., crystal focusing elements for synchrotron beamlines) due to the mechanical inaccuracies inherent in moving the various optical components. We present a method based on a scanning source which simplifies the problems in scaling double-crystal methods to large optics. In addition, results using this method are presented on a ribless sagittal focusing Si(111) crystal demonstrating that the anticlastic deviation can be made to be less than {plus_minus}1 s of arc over a 1-cm-long section parallel to the sagittal axis.
Date: January 1, 1996
Creator: Quintana, J.P.; Dolin, Yu. & Georgopoulos, P.
Partner: UNT Libraries Government Documents Department