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NASA NTRS2003

Examination of the Atomic Pair Distribution Function (PDF) of SiC Nanocrystals by In-situ High Pressure Diffraction

Key properties of nanocrystals are determined by their real atomic structure, therefore a reasonable understanding and meaningful interpretation of their properties requires a realistic model of the structure. In this paper we present an evidence of a complex response of the lattice distances to external pressure indicating a presence of a complex structure of Sic nanopowders. The experiments were performed on nanocrystalline Sic subjected to hydrostatic or isostatic pressure using synchrotron and neutron powder diffraction. Elastic properties of the samples were examined based on X-ray diffraction data using a Diamond Anvil Cell (DAC) in HASYLAB at DESY. The dependence'of the lattice parameters and of the Bragg reflections width with pressure exhibits a ha1 nature of the properties (compressibilities) of the powders and indicates a complex structure of the grains. We interpreted tws behaviour as originating from different elastic properties of the grain interior and surface. Analysis of the dependence of individual interatomic distances on pressure was based on in-situ neutron diffraction measurements done with HbD diffractometer at LANSCE in Los Alamos National Laboratory with the Paris-Edinburgh cell under pressures up to 8 GPa (Qmax = 26/A). Interatomic distances were obtained by PDF analysis using the PDFgetN program. We have found that the interatomic distances undergo a complex, non-monotonic changes. Even under substantial pressures a considerable relaxation of the lattice may take place: some interatomic distances increase with an increase in pressure. We relate this phenomenon to: (1), changes of the microstructure of the densified material, in particular breaking of its fractal chain structure and, (2), its complex structure resembling that of a material composed of two phases, each with its distinct elastic properties.

Grzanka, E.↗

NASA NTRS2004

High Pressure X-Ray Diffraction Studies of Nanocrystalline Materials

Experimental evidence obtained for a variety of nanocrystalline materials suggest that the crystallographic structure of a very small size particle deviates from that in the bulk crystals. In this paper we show the effect of the surface of nanocrystals on their structure by the analysis of generation and distribution of macro- and micro-strains at high pressures and their dependence on the grain size in nanocrystalline powders of Sic. We studied the structure of Sic nanocrystals by in-situ high-pressure powder diffraction technique using synchrotron and neutron sources and hydrostatic or isostatic pressure conditions. The diffraction measurements were done in HASYLAB at DESY using a Diamond Anvil Cell (DAC) in the energy dispersive geometry in the diffraction vector range up to 3.5 - 4/A and under pressures up to 50 GPa at room temperature. In-situ high pressure neutron diffraction measurements were done at LANSCE in Los Alamos National Laboratory using the HIPD and HIPPO diffractometers with the Paris-Edinburgh and TAP-98 cells, respectively, in the diffraction vector range up to 26 Examination of the response of the material to external stresses requires nonstandard methodology of the materials characterization and description. Although every diffraction pattern contains a complete information on macro- and micro-strains, a high pressure experiment can reveal only those factors which contribute to the characteristic diffraction patterns of the crystalline phases present in the sample. The elastic properties of powders with the grain size from several nm to micrometers were examined using three methodologies: (l), the analysis of positions and widths of individual Bragg reflections (used for calculating macro- and micro-strains generated during densification) [I], (2). the analysis of the dependence of the experimental apparent lattice parameter, alp, on the diffraction vector Q [2], and (3), the atomic Pair Distribution Function (PDF) technique [3]. The results of our studies show, that Sic nanocrystals have the features of two phases, each with its distinct elastic properties. and under pressures up to 8 GPa.

Palosz, B.↗

NASA NTRS2008

Exploring Cosmic X-ray Source Polarization

Cosmic X-ray sources are expected to be polarized, either because of their asymmetry and the role of scattering in their emission or the role of magnetic fields. Polarization at other wavelengths has been useful. X-ray polarization will provide a new handle on black hole parameters, in particular the spin, on accretion flows and outflows, on neutron star spin orientations and emission mechanisms, on the quantum mechanical effects of super-strong magnetic fields of magnetars, and on the structure of supernovae shocks. The proposed Gravity and Extreme Magnetism SMEX (GEMS) will use high efficiency polarimeters behind thin foil mirrors. The statistical sensitivity and control of systematics will allow measurement of polarization fractions as small as 1% from many galactic and extragalactic sources. Targets which should be polarized at the level that GEMS can easily measure include stellar black holes, Seyfert galaxies and quasars, blazars, rotation-powered and accretion-powered pulsars, magnetars, shell supernova remnants and pulsar wind nebulae. The polarimeters are Time Projection Chambers that allow reconstruction of images of photoelectron tracks for 2-10 keV Xrays. They can be deep without sacrificing modulation. These polarimeters do not image the sky, but the telescope point spread function and detector collimation allow structure to be resolved at the 10 arcmin level. Rotation of the spacecraft is not needed for the signal measurement in the Time Projection Chambers, but provides for measurement and correction of systematic errors. It also allows a small Bragg reflection soft X-ray experiment to be included that can be used for isolated neutron stars and blazars.

Swank, Jean Hebb↗

NASA NTRS2011

The Gravity and Extreme Magnetism Small Explorer (GEMS)

The Gravity and Extreme Magnetism Small Explorer (GEMS) was selected by NASA for flight in 2014 to make a sensitive search for X-ray polarization from a wide set of source classes, including stellar black holes, Seyfert galaxies and quasars, blazars, rotation and accretion-powered pulsars, magnetars, shell supernova remnants and pulsar wind nebulae. Among the primary scientific objectives are determining the effects of the spin of black holes and the geometry of supermassive black hole accretion, determining the configurations of the magnetic fields and the X-ray emission of magnetars, and determining the magnetic structure of the supernova shocks in which cosmic rays are accelerated. GEMS will observe 23 targets during a 16 month prime mission, in observations that will be able to reach predicted levels of polarization. The mission can be extended to provide a guest observer phase. The GEMS instrument has time projection chamber polarimeters with high 2-10 keV efficiency at the focus of thin foil mirrors. The 4.5 m focal length mirrors will be deployed on an extended boom. The spacecraft with the instrument is rotated with a period of about 10 minutes to enable measurement and correction of systematic errors. A small Bragg reflection soft X-ray experiment takes advantage of this rotation to obtain a measurement at 0.5 keV. The design of the GEMS instrument and the mission, the expected performance and the planned science program will be discussed.

Kallman, T. R.↗

DOE OSTI2014

Performance of a beam-multiplexing diamond crystal monochromator at the Linac Coherent Light Source

A double-crystal diamond monochromator was recently implemented at the Linac Coherent Light Source. It enables splitting pulses generated by the free electron laser in the hard x-ray regime and thus allows the simultaneous operations of two instruments. Both monochromator crystals are High-Pressure High-Temperature grown type-IIa diamond crystal plates with the (111) orientation. The first crystal has a thickness of ∼100 μm to allow high reflectivity within the Bragg bandwidth and good transmission for the other wavelengths for downstream use. The second crystal is about 300 μm thick and makes the exit beam of the monochromator parallel to the incoming beam with an offset of 600 mm. Here we present details on the monochromator design and its performance.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

DOE OSTI2014

SrFe{sub 0.9}Ti{sub 0.1}O{sub 3−δ}: A cluster spin glass

Graphical abstract: - Highlights: • Prepared SrFe{sub 0.9}Ti{sub 0.1}O{sub 3−δ} is in nanocrystalline form. • Arrott plot shows absence of spontaneous magnetization which rules out the possibility of long range ferromagnetic order. • AC susceptibility data is evidence of cluster spin glass. • There is no magnetic Bragg's reflection. • By substituting Ti{sup 4+}, helical antiferromagetic SrFeO{sub 3} is transformed to a cluster spin glass. - Abstract: The magnetic ground state of nanocrystalline SrFe{sub 0.9}Ti{sub 0.1}O{sub 3−δ} system has been investigated from 2 K to 300 K using AC Susceptibilty (ACS), magnetization and neutron diffraction measurements. The cusp in the temperature dependent magnetization and dispersion below T{sub max} (the temperature at which the maximum susceptibility is observed) in real part of ac susceptibility with frequency is observed. Arrott plot shows the lack of M{sub S} (spontaneous magnetization) down to 2 K, and the non-occurrence of magnetic Bragg reflections below the T{sub max} in neutron diffraction measurements, indicates the absence of long range ferro and antiferromagnetic order. The frequency dependence of T{sub max} obeys Vögel–Fulcher model establishing the cluster spin glass behavior in this system.

36 MATERIALS SCIENCE↗

DOE OSTI2016

Optical spectroscopy of a resonant Bragg structure with InGaN/GaN quantum wells

The optical reflectance and transmittance spectra of a periodic InGaN/GaN semiconductor heterostructure with 60 quantum wells are studied at room temperature. The period of the structure was chosen such that, at some angles of incidence of light, the energy of a photon resonantly reflected from the Bragg structure coincides with the excitation energy for quantum-well excitons in quantum wells. The parameters of these excitons are determined by fitting the spectra measured at two different angles of incidence, 30° and 60°. We take into account the resonant exciton transitions in quantum wells as well as the transitions into the continuous spectrum. The radiative decay parameter is determined to be (0.20 ± 0.02) meV.

36 MATERIALS SCIENCE↗

DOE OSTI2014

Manipulating light propagation and emission using photonic crystals

We discuss the synthesis and characterization of self-assembled photonic crystals using polymer colloids having sub-micron diameters. The angle resolved optical reflectivity measurements indicate the hybridization between stop gaps in the multiple Bragg diffraction regimes. Each diffraction resonances in the multiple Bragg diffraction regimes are assigned to respective crystal planes. We also discuss laser-induced studies of spontaneous emission in self-assembled photonic crystals having Rhodamine-B dye doped colloids. Our experimental results reveal more than 51% inhibition in emission intensity within the stop gap as compared to a proper reference sample.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

DOE OSTI2014

Off-axis phonon and photon propagation in porous silicon superlattices studied by Brillouin spectroscopy and optical reflectance

Brillouin light scattering experiments and optical reflectance measurements were performed on a pair of porous silicon-based optical Bragg mirrors which had constituent layer porosity ratios close to unity. For off-axis propagation, the phononic and photonic band structures of the samples were modeled as a series of intersecting linear dispersion curves. Zone-folding was observed for the longitudinal bulk acoustic phonon and the frequency of the probed zone-folded longitudinal phonon was shown to be dependent on the propagation direction as well as the folding order of the mode branch. There was no conclusive evidence of coupling between the transverse and the folded longitudinal modes. Two additional observed Brillouin peaks were attributed to the Rayleigh surface mode and a possible pseudo-surface mode. Both of these modes were dispersive, with the velocity increasing as the wavevector decreased.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

NASA NTRS2006

In Search of Multi-Peaked Reflective Spectrum with Optic Fiber Bragg Grating Sensor for Dynamic Strain Measurement

In a typical optic fiber Bragg grating (FBG) strain measurement, unless in an ideal static laboratory environment, the presence of vibration or often disturbance always exists, which often creates spurious multiple peaks in the reflected spectrum, resulting in a non-unique determination of strain value. In this report we attempt to investigate the origin of this phenomenon by physical arguments and simple numerical simulation. We postulate that the fiber gratings execute small amplitude transverse vibrations changing the optical path in which the reflected light traverses slightly and non-uniformly. Ultimately, this causes the multi-peak reflected spectrum.

Tai, Hsiang↗

NASA NTRS2003

Theory of Fiber Optical Bragg Grating: Revisited

The reflected signature of an optical fiber Bragg grating is analyzed using the transfer function method. This approach is capable to cast all relevant quantities into proper places and provides a better physical understanding. The relationship between reflected signal, number of periods, index of refraction, and reflected wave phase is elucidated. The condition for which the maximum reflectivity is achieved is fully examined. We also have derived an expression to predict the reflectivity minima accurately when the reflected wave is detuned. Furthermore, using the segmented potential approach, this model can handle arbitrary index of refraction profiles and compare the strength of optical reflectivity of different profiles. The condition of a non-uniform grating is also addressed.

Tai, H.↗

NASA NTRS2001

Ultra Narrowband Optical Filters for Water Vapor Differential Absorption Lidar (DIAL) Atmospheric Measurements

Differential absorption lidar (DIAL) systems are being deployed to make vertical profile measurements of atmospheric water vapor from ground and airborne platforms. One goal of this work is to improve the technology of such DIAL systems that they could be deployed on space-based platforms. Since background radiation reduces system performance, it is important to reduce it. One way to reduce it is to narrow the bandwidth of the optical receiver system. However, since the DIAL technique uses two or more wavelengths, in this case separated by 0.1 nm, a fixed-wavelength narrowband filter that would encompass both wavelengths would be broader than required for each line, approximately 0.02 nm. The approach employed in this project is to use a pair of tunable narrowband reflective fiber Bragg gratings. The Bragg gratings are germanium-doped silica core fiber that is exposed to ultraviolet radiation to produce index-of-refraction changes along the length of the fiber. The gratings can be tuned by stretching. The backscattered laser radiation is transmitted through an optical circulator to the gratings, reflected back to the optical circulator by one of the gratings, and then sent to a photodiode. The filter reflectivities were >90 percent, and the overall system efficiency was 30 percent.

Stenholm, Ingrid↗

DOE OSTI2018

Cathodic Corrosion at the Bismuth-Ionic Liquid Electrolyte Interface under Conditions for CO 2 Reduction

Bismuth electrodes undergo distinctive electrochemically induced structural changes in nonaqueous imidazolium ([Im])(+))-based ionic liquid solutions under cathodic polarization. In situ X-ray reflectivity (XR) studies have been undertaken to probe well-ordered Bi (001) films which originally contain a native Bi 2 O 3 layer. This oxide layer gets reduced to Bi(0)during the first cyclic voltammetry (CV) scan in acetonitrile solutions containing 1-butyl-3-methylimidazolium ([BMIM](+)) electrolytes. Approximately 60% of the Bi (001) Bragg peak reflectivity is lost during a potential sweep between -1.5 and -1.9 V vs Ag/AgCI due to a similar to 4-10% thinning and a similar to 40% decrease in lateral size of Bi (001) domains, which are mostly reversed during the anodic scan. Repeated potential cycling enhances the thinning and roughening of the films, suggesting that partial dissolution of Bi ensues during negative polarization. The mechanism of this behavior is understood through molecular dynamics simulations using ReaxFF and density functional theory (DFT) calculations. Both approaches indicate that [Im] + cations bind to the metal surface more strongly than tetrabutylammonium (TBA + ) as the potential and the charge on the Bi surface become more negative. ReaxFF simulations predict a higher degree of disorder for a negatively charged Bi (001) slab in the presence of the [Im](+)cations and substantial migration of Bi atoms from the surface. DFT simulations show the formation of Bi center dot center dot center dot[Im] + complexes that lead to the dissolution of Bi atoms from step edges on the Bi (001) surface at potentials between -1.65 and -1.95 V. Bi desorption from a flat terrace requires a potential of approximately -2.25 V. Together, these results suggest the formation of a Bi center dot center dot center dot[Im] + complex through partial cathodic corrosion of the Bi film under conditions (potential and electrolyte composition) that favor the catalytic reduction of CO 2 .

36 MATERIALS SCIENCE↗

DOE OSTI2020

Cubic crystals in an x-ray polarization-splitting geometry

Hexagonal and cubic crystals contain paired sets of internal planes that reflect the linearly polarized components of certain x rays into two separate, perpendicular directions. For the cubic crystals, two distinct crystal orientations provide the same polarization-splitting geometry. One of the orientations may have advantages for plasma spectroscopy by suppressing unwanted reflections. This paper demonstrates the two orientations with a germanium crystal and K characteristic lines from copper and zirconium.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

DOE OSTI2013

Anomalous X-ray scattering study of quantum dots embedded in MBE grown silicon/germanium multilayers

Anomalous X-ray scattering is a unique technique to determine the composition profile of quantum dots embedded in buried interfaces of multilayer-structures. Here we present the results of MBE grown Si/Ge multilayer structures on Si(001) substrates having self-assembled Ge quantum dots in its buried interfaces. We performed grazing incidence diffraction measurements of (400) reflections along with (004) diffraction profiles exhibiting super-lattice reflections at and away from the germanium K-edge. Systematic analysis of the acquired data enabled us to extract average composition and strain profiles of the quantum dots.

36 MATERIALS SCIENCE↗

DOE OSTI2015

Grazing-incidence X-ray diffraction from a crystal with subsurface defects

The diffraction of X rays incident on a crystal surface under grazing angles under conditions of total external reflection has been investigated. An approach is proposed in which exact solutions to the dynamic problem of grazing-incidence diffraction in an ideal crystal are used as initial functions to calculate the diffuse component of diffraction in a crystal with defects. The diffuse component of diffraction is calculated for a crystal with surface defects of a dilatation-center type. Exact formulas of the continuum theory which take into account the mirror-image forces are used for defect-induced atomic displacements. Scattering intensity maps near Bragg peaks are constructed for different scan modes, and the conditions for detecting primarily the diffuse component are determined. The results of dynamic calculations of grazing-incidence diffraction in defect-containing crystals are compared with calculations in the kinematic approximation.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2016

Defect modes of one-dimensional photonic-crystal structure with a resonance nanocomposite layer

We have studied the defect modes of a structure of Fabry – Perot interferometer type, in which the layer separating Bragg mirrors is made of a heterogeneous composite material with metallic nanoscale inclusions. Effective optical characteristics of the nanocomposite material have resonance singularities in the visible region of the spectrum, which are conditioned by the surface plasmon resonance of metallic nanoparticles. It is shown that the spectral profile of the energy bandgap of the photonic structure can be modified by varying the volume fraction and size of nanoparticles. The interrelation of splitting and shift of defect modes with structural parameters of a nanocomposite layer is studied by means of a numerical – graphical method with allowance for the frequency dependences of phases and amplitudes of reflectances in Bragg mirrors. (photonic crystal structures)

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗

NASA NTRS2005

Processing of Signals from Fiber Bragg Gratings Using Unbalanced Interferometers

Fiber Bragg gratings (FBG) have become preferred sensory structures in fiber optic sensing system. High sensitivity, embedability, and multiplexing capabilities make FBGs superior to other sensor configurations. The main feature of FBGs is that they respond in the wavelength domain with the wavelength of the returned signal as the indicator of the measured parameter. The wavelength is then converted to optical intensity by a photodetector to detect corresponding changes in intensity. This wavelength-to-intensity conversion is a crucial part in any FBG-based sensing system. Among the various types of wavelength-to-intensity converters, unbalanced interferometers are especially attractive because of their small weight and volume, lack of moving parts, easy integration, and good stability. In this paper we investigate the applicability of unbalanced interferometers to analyze signals reflected from Bragg gratings. Analytical and experimental data are presented.

Adamovsky, Grigory↗