DOE Office of Scientific and Technical Information (OSTI.GOV)

Dalal, M.; Mallick, A.; Mahapatra, A.S.

Highlights: • Cation distribution in tetrahedral and octahedral sites of spinel Ni{sub 0.4}Zn{sub 0.4}Co{sub 0.2}Fe{sub 2}O{sub 4}. • Structural analysis of observed X-ray diffraction pattern using Rietveld method. • Study of hyperfine behaviour using Mössbauer spectroscopy. • Static and dynamic magnetic measurements. • Correlation of cation distributions obtained from Rietveld analysis with the results of magnetic and Mössbauer effect measurements. - Abstract: Nanoparticles of Ni{sub 0.4}Zn{sub 0.4}Co{sub 0.2}Fe{sub 2}O{sub 4} are prepared by a simple co-precipitation method. The as dried sample is heat treated at 400, 500, 600, 700 and 800 °C to obtain different sizes of nanoparticles. The crystallographicmore » phase of the samples is confirmed analyzing observed X-ray diffraction (XRD) by Rietveld method. Hyperfine parameters of the samples are derived from room temperature (RT) Mössbauer spectra of the samples. Magnetic properties of the samples are investigated by static and dynamic hysteresis loops. Different magneto-crystalline parameters are calculated from the variation of magnetization with temperature (M–T curve) under zero field cooled (ZFC) and field cooled (FC) conditions of the as dried sample. The cation distribution estimated from Rietveld analysis are correlated with the results of magnetic and Mössbauer effect measurements. The observed high value of saturation magnetization (72.7 emu/g at RT) of the sample annealed at 800 °C would be interesting for applications in different electromagnetic devices.« less

Ba0.06(Na,Bi)0.94Ti1-x(Ni1/3Nb2/3)xO3 ceramics: X-ray diffraction and infrared spectroscopy studies

NASA Astrophysics Data System (ADS)

Mishra, R. K.; Prasad, Ashutosh; Chandra, K. P.; Prasad, K.

2018-05-01

Non-lead ceramic samples of Ba0.06(Na0.5Bi0.5)0.94Ti1-x(Ni1/3Nb2/3)xO3; 0 ≤ x ≤ 1.0 were prepared by standard high temperature ceramic synthesis method. Rietveld refinements of X-ray diffraction data of these ceramics were carried out using FullProf software and determined their crystal symmetry, space group and unit cell dimensions. Rietveld refinement revealed that Ba0.06(Na0.5Bi0.5)0.94TiO3 has a monoclinic structure with space group P4/m while B0.06(Na0.5Bi0.5)0.94(Ni1/3Nb2/3)O3 has tetragonal (pseudo-cubic) structure with space group P4/mmm. Partial replacement of Ti4+ ion by pseudo-cation (Ni1/33 +Nb2/3 5 +) 4 + resulted in the change of unit cell structure from monoclinic to tetragonal. SEM studies were carried out in order to access the quality of the prepared ceramics which showed a change in grain sizes with the increase of (Ni1/33 +Nb2/3 5 +) 4 + content. FTIR spectra confirmed the formation of perovskite type solid solutions.

Structural properties of barium stannate

NASA Astrophysics Data System (ADS)

Phelan, D.; Han, F.; Lopez-Bezanilla, A.; Krogstad, M. J.; Gim, Y.; Rong, Y.; Zhang, Junjie; Parshall, D.; Zheng, H.; Cooper, S. L.; Feygenson, M.; Yang, Wenge; Chen, Yu-Sheng

2018-06-01

BaSnO3 has attracted attention as a transparent conducting oxide with high room temperature carrier mobility. We report a series of measurements that were carried out to assess the structure of BaSnO3 over a variety of length scales. Measurements included single crystal neutron and x-ray diffraction, Rietveld and pair distribution analysis of neutron powder diffraction, Raman scattering, and high-pressure x-ray diffraction. Results from the various diffraction probes indicate that both the long-range and local structures are consistent with the cubic symmetry. The diffraction data under pressure was consistent with a robustly cubic phase up to 48.9 GPa, which is supported by density functional calculations. Additionally, transverse phonon velocities were determined from measured dispersion of the transverse acoustic phonon branches, the results of which are in good agreement with previous theoretical estimates and ultrasound measurements.

Time-resolved in situ powder X-ray diffraction reveals the mechanisms of molten salt synthesis.

PubMed

Moorhouse, Saul J; Wu, Yue; Buckley, Hannah C; O'Hare, Dermot

2016-11-24

We report the first use of high-energy monochromatic in situ X-ray powder diffraction to gain unprecedented insights into the chemical processes occurring during high temperature, lab-scale metal oxide syntheses. During the flux synthesis of the n = 4 Aurivillius phase, Bi 5 Ti 3 Fe 0.5 Cr 0.5 O 15 at 950 °C in molten Na 2 SO 4 we observe the progression of numerous metastable phases. Using sequential multiphase Rietveld refinement of the time-dependent in situ XRD data, we are able to obtain mechanistic understanding of this reaction under a range of conditions.

X-ray diffraction analysis of LiCu{sub 2}O{sub 2} crystals with additives of silver atoms

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sirotinkin, V. P., E-mail: irotinkin.vladimir@mail.ru; Bush, A. A.; Kamentsev, K. E.

2015-09-15

Silver-containing LiCu{sub 2}O{sub 2} crystals up to 4 × 8 × 8 mm in size were grown by the crystallization of 80(1-x)CuO · 20{sub x}AgNO{sub 3} · 20Li{sub 2}CO{sub 3} (0 ≤ x ≤ 0.5) mixture melt. According to the X-ray spectral and Rietveld X-ray diffraction data, the maximum amount of silver incorporated in the LiCu{sub 2}O{sub 2} structure is about 4 at % relative to the copper content. It was established that silver atoms occupy statistically crystallographic positions of lithium atoms. The incorporation of silver atoms is accompanied by a noticeable increase in parameter c of the LiCu{sub 2}O{submore » 2} rhombic unit cell, a slight increase in parameter a, and a slight decrease in parameter b.« less

Phase Compositions of Self Reinforcement Al2O3/CaAl12O19 Composite using X-ray Diffraction Data and Rietveld Technique

NASA Astrophysics Data System (ADS)

Asmi, D.; Low, I. M.; O'Connor, B.

2008-03-01

The analysis of x-ray diffraction (XRD) patterns by the Rietveld technique was tested to the quantitatively phase compositions of self reinforcement Al2O3/CaAl12O19 composite. Room-temperature XRD patterns revealed that α-Al2O3 was the only phase presence in the CA0 sample, whereas the α-Al2O3 and CaAl12O19 phases were found for CA5, CA15, CA30, and CA50 samples. The peak intensity of CA6 in the self reinforcement Al2O3/CaAl12O19 composites increased in proportion with increase in CaAl12O19 content in contrast to α-Al2O3. The diffraction patterns for CA100 sample shows minor traces of α-Al2O3 even in relatively low peak intensity. It is suggesting that the in-situ reaction sintering of raw materials were not react completely to form 100 wt% CaAl12O19 at temperature 1650 °C. Quantitative phase compositions of self reinforcement Al2O3/CaAl12O19 composites by Rietveld analysis with XRD data has been well demonstrated. The results showed that the GOF values are relatively low and the fluctuation in the difference plots shows a reasonable fit between the observed and the calculated plot.

The first X-ray diffraction measurements on Mars.

PubMed

Bish, David; Blake, David; Vaniman, David; Sarrazin, Philippe; Bristow, Thomas; Achilles, Cherie; Dera, Przemyslaw; Chipera, Steve; Crisp, Joy; Downs, R T; Farmer, Jack; Gailhanou, Marc; Ming, Doug; Morookian, John Michael; Morris, Richard; Morrison, Shaunna; Rampe, Elizabeth; Treiman, Allan; Yen, Albert

2014-11-01

The Mars Science Laboratory landed in Gale crater on Mars in August 2012, and the Curiosity rover then began field studies on its drive toward Mount Sharp, a central peak made of ancient sediments. CheMin is one of ten instruments on or inside the rover, all designed to provide detailed information on the rocks, soils and atmosphere in this region. CheMin is a miniaturized X-ray diffraction/X-ray fluorescence (XRD/XRF) instrument that uses transmission geometry with an energy-discriminating CCD detector. CheMin uses onboard standards for XRD and XRF calibration, and beryl:quartz mixtures constitute the primary XRD standards. Four samples have been analysed by CheMin, namely a soil sample, two samples drilled from mudstones and a sample drilled from a sandstone. Rietveld and full-pattern analysis of the XRD data reveal a complex mineralogy, with contributions from parent igneous rocks, amorphous components and several minerals relating to aqueous alteration. In particular, the mudstone samples all contain one or more phyllosilicates consistent with alteration in liquid water. In addition to quantitative mineralogy, Rietveld refinements also provide unit-cell parameters for the major phases, which can be used to infer the chemical compositions of individual minerals and, by difference, the composition of the amorphous component.

Structural Properties of Barium Stannate.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Phelan, D.; Han, F.; Lopez-Bezanilla, A.

2018-06-01

BaSnO3 has attracted attention as a transparent conducting oxide with high room temperature carrier mobility. We report a series of measurements that were carried out to assess the structure of BaSnO3 over a variety of length scales. Measurements included single crystal neutron and x-ray diffraction, Rietveld and pair distribution analysis of neutron powder diffraction, Raman scattering, and high-pressure x-ray diffraction. Results from the various diffraction probes indicate that both the long-range and local structures are consistent with the cubic symmetry. The diffraction data under pressure was consistent with a robustly cubic phase up to 48.9 GPa, which is supported bymore » density functional calculations. Additionally, transverse phonon velocities were determined from measured dispersion of the transverse acoustic phonon branches, the results of which are in good agreement with previous theoretical estimates and ultrasound measurements.« less

Crystalline phases involved in the hydration of calcium silicate-based cements: Semi-quantitative Rietveld X-ray diffraction analysis.

PubMed

Grazziotin-Soares, Renata; Nekoofar, Mohammad H; Davies, Thomas; Hübler, Roberto; Meraji, Naghmeh; Dummer, Paul M H

2017-08-30

Chemical comparisons of powder and hydrated forms of calcium silicate cements (CSCs) and calculation of alterations in tricalcium silicate (Ca 3 SiO 5 ) calcium hydroxide (Ca(OH) 2 ) are essential for understanding their hydration processes. This study aimed to evaluate and compare these changes in ProRoot MTA, Biodentine and CEM cement. Powder and hydrated forms of tooth coloured ProRoot MTA, Biodentine and CEM cement were subjected to X-ray diffraction (XRD) analysis with Rietveld refinement to semi-quantitatively identify and quantify the main phases involved in their hydration process. Data were reported descriptively. Reduction in Ca 3 SiO 5 and formation of Ca(OH) 2 were seen after the hydration of ProRoot MTA and Biodentine; however, in the case of CEM cement, no reduction of Ca 3 SiO 5 and no formation of Ca(OH) 2 were detected. The highest percentages of amorphous phases were seen in Biodentine samples. Ettringite was detected in the hydrated forms of ProRoot MTA and CEM cement but not in Biodentine. © 2017 Australian Society of Endodontology Inc.

Direct Observations of a Dynamically Driven Phase Transition with in situ X-Ray Diffraction in a Simple Ionic Crystal

NASA Astrophysics Data System (ADS)

Kalita, Patricia; Specht, Paul; Root, Seth; Sinclair, Nicholas; Schuman, Adam; White, Melanie; Cornelius, Andrew L.; Smith, Jesse; Sinogeikin, Stanislav

2017-12-01

We report real-time observations of a phase transition in the ionic solid CaF2 , a model A B2 structure in high-pressure physics. Synchrotron x-ray diffraction coupled with dynamic loading to 27.7 GPa, and separately with static compression, follows, in situ, the fluorite to cotunnite structural phase transition, both on nanosecond and on minute time scales. Using Rietveld refinement techniques, we examine the kinetics and hysteresis of the transition. Our results give insight into the kinetic time scale of the fluorite-cotunnite phase transition under shock compression, which is relevant to a number of isomorphic compounds.

Direct Observations of a Dynamically Driven Phase Transition with in situ X-Ray Diffraction in a Simple Ionic Crystal

DOE PAGES

Kalita, Patricia E.; Specht, Paul Elliot; Root, Seth; ...

2017-12-21

Here, we report real-time observations of a phase transition in the ionic solid CaF 2, a model AB 2 structure in high-pressure physics. Synchrotron x-ray diffraction coupled with dynamic loading to 27.7 GPa, and separately with static compression, follows, in situ, the fluorite to cotunnite structural phase transition, both on nanosecond and on minute time scales. Using Rietveld refinement techniques, we examine the kinetics and hysteresis of the transition. Our results give insight into the kinetic time scale of the fluorite-cotunnite phase transition under shock compression, which is relevant to a number of isomorphic compounds.

Simultaneous X-ray and neutron diffraction Rietveld refinements of nanophase iron substituted hydroxyapatite

NASA Astrophysics Data System (ADS)

Kyriacou, Andreas

The effect of Fe substitution on the crystal structure of hydroxyapatite (HAp) is studied by applying simultaneous Rietveld refinements of powder x-ray and neutron diffraction patterns. Fe is one of the trace elements replacing Ca in HAp, which is the major mineral phase in bones and teeth. The morphology and magnetic properties of the Fe-HAp system are also studied by transmission electron microscopy and magnetization measurements. Samples of Ca(5-x)Fex(PO4)3OH with 0 ≤ x ≤ 0.3 were prepared. Single phase HAp was identified in x-ray diffraction patterns (XRD) of samples with x < 0.1 inferring that the solubility limits are less than 0.1. Hematite (alpha-Fe2O3) is identified as a secondary phase for higher Fe content. The refined parameters show that Fe is incorporated in the HAp structure by replacing Ca in the two crystallographic sites with a preference at the Ca2 site. This preference explains the small effect of the Fe substitution on the lattice constants of HAp. The overall decrease of the lattice constants is explained by the ionic size difference of Ca and Fe. The increasing trend of the a-lattice constant with x in the Fe substituted samples is attributed to a lattice relaxation caused by the substitution of the 4- and 6-fold Fe at the 7- and 9-fold Ca1 and Ca2 sites. This Ca local geometry reduction is indicated by a slight increase of the Ca1-O3 and Ca2-O1 bond lengths. Above the solubility limit x = 0.05, the Fe is partitioned in and out of the HAp structure with increasing nominal Fe content x. The excess Fe is oxidized to hematite. The TEM analysis and magnetic measurements support the results of the simultaneous Rietveld refinements. The TEM images show no significant effect on the morphology and size of the HAp particles upon Fe incorporation. The particles are either spheres or short rods of dimensions 20--60 nm. Hematite particles are imaged in the samples with x exceeding the solubility limit. These particles are spheres, about 15 nm in diameter and are more resistant to electron beam damage. Magnetic measurements reveal a transition of the diamagnetic pure HAp to paramagnetic Fe substituted HAp.

Synthesis and characterization of Ca-doped LaMnAsO

NASA Astrophysics Data System (ADS)

Liu, Yong; Straszheim, Warren E.; Das, Pinaki; Islam, Farhan; Heitmann, Thomas W.; McQueeney, Robert J.; Vaknin, David

2018-05-01

We report on our attempt to hole-dope the antiferromagnetic semiconductor LaMnAsO by substitution of the La3 + site by Ca2 +. We use neutron and x-ray diffraction, magnetic susceptibility, and transport techniques to characterize polycrystalline (La1 -xCax)MnAsO samples prepared by solid-state reaction and find that the parent compound is highly resistant to substitution with an upper limit x ≤0.01 . Magnetic susceptibility of the parent and the x =0.002 (xnom=0.04 ) compounds indicate a negligible presence of magnetic impurities (i.e., MnO or MnAs). Rietveld analysis of neutron and x-ray diffraction data shows the preservation of both the tetragonal (P 4 /n m m ) structure upon doping and the antiferromagnetic ordering temperature, TN=355 ±5 K.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Frølich, S.; Leemreize, H.; Jakus, A.

A model sample consisting of two different hydroxyapatite (hAp) powders was used as a bone phantom to investigate the extent to which X-ray diffraction tomography could map differences in hAp lattice constants and crystallite size. The diffraction data were collected at beamline 1-ID, the Advanced Photon Source, using monochromatic 65 keV X-radiation, a 25 × 25 µm pinhole beam and translation/rotation data collection. The diffraction pattern was reconstructed for each volume element (voxel) in the sample, and Rietveld refinement was used to determine the hAp lattice constants. The crystallite size for each voxel was also determined from the 00.2 hApmore » diffraction peak width. The results clearly show that differences between hAp powders could be measured with diffraction tomography.« less

Synthesis and characterization of Ca-doped LaMnAsO

DOE Office of Scientific and Technical Information (OSTI.GOV)

Liu, Yong; Straszheim, Warren E.; Das, Pinaki

Here, we report on our attempt to hole-dope the antiferromagnetic semiconductor LaMnAsO by substitution of the La 3+ site by Ca 2+. We use neutron and x-ray diffraction, magnetic susceptibility, and transport techniques to characterize polycrystalline (La 1–xCa x)MnAsO samples prepared by solid-state reaction and find that the parent compound is highly resistant to substitution with an upper limit x ≤ 0.01. Magnetic susceptibility of the parent and the x = 0.002(x nom = 0.04) compounds indicate a negligible presence of magnetic impurities (i.e., MnO or MnAs). Rietveld analysis of neutron and x-ray diffraction data shows the preservation of bothmore » the tetragonal (P4/nmm) structure upon doping and the antiferromagnetic ordering temperature, T N = 355 ± 5 K.« less

Synthesis and characterization of Ca-doped LaMnAsO

DOE PAGES

Liu, Yong; Straszheim, Warren E.; Das, Pinaki; ...

2018-05-18

Here, we report on our attempt to hole-dope the antiferromagnetic semiconductor LaMnAsO by substitution of the La 3+ site by Ca 2+. We use neutron and x-ray diffraction, magnetic susceptibility, and transport techniques to characterize polycrystalline (La 1–xCa x)MnAsO samples prepared by solid-state reaction and find that the parent compound is highly resistant to substitution with an upper limit x ≤ 0.01. Magnetic susceptibility of the parent and the x = 0.002(x nom = 0.04) compounds indicate a negligible presence of magnetic impurities (i.e., MnO or MnAs). Rietveld analysis of neutron and x-ray diffraction data shows the preservation of bothmore » the tetragonal (P4/nmm) structure upon doping and the antiferromagnetic ordering temperature, T N = 355 ± 5 K.« less

Multidataset Refinement Resonant Diffraction, and Magnetic Structures

PubMed Central

Attfield, J. Paul

2004-01-01

The scope of Rietveld and other powder diffraction refinements continues to expand, driven by improvements in instrumentation, methodology and software. This will be illustrated by examples from our research in recent years. Multidataset refinement is now commonplace; the datasets may be from different detectors, e.g., in a time-of-flight experiment, or from separate experiments, such as at several x-ray energies giving resonant information. The complementary use of x rays and neutrons is exemplified by a recent combined refinement of the monoclinic superstructure of magnetite, Fe3O4, below the 122 K Verwey transition, which reveals evidence for Fe2+/Fe3+ charge ordering. Powder neutron diffraction data continue to be used for the solution and Rietveld refinement of magnetic structures. Time-of-flight instruments on cold neutron sources can produce data that have a high intensity and good resolution at high d-spacings. Such profiles have been used to study incommensurate magnetic structures such as FeAsO4 and β–CrPO4. A multiphase, multidataset refinement of the phase-separated perovskite (Pr0.35Y0.07Th0.04Ca0.04Sr0.5)MnO3 has been used to fit three components with different crystal and magnetic structures at low temperatures. PMID:27366599

Rietveld refinement of the crystal structures of Rb2 XSi5O12 (X = Ni, Mn).

PubMed

Bell, Anthony M T; Henderson, C Michael B

2016-02-01

The synthetic leucite silicate framework mineral analogues Rb2 XSi5O12 {X = Ni [dirubidium nickel(II) penta-silicate] and Mn [dirubidium manganese(II) penta-silicate]} have been prepared by high-temperature solid-state synthesis. The results of Rietveld refinements, using X-ray powder diffraction data collected using Cu Kα X-rays, show that the title compounds crystallize in the space group Pbca and adopt the cation-ordered structure of Cs2CdSi5O12 and other leucites. The structures consist of tetra-hedral SiO4 and XO4 units sharing corners to form a partially substituted silicate framework. Extraframework Rb(+) cations sit in channels in the framework. All atoms occupy the 8c general position for this space group. In these refined structures, silicon and X atoms are ordered onto separate tetra-hedrally coordinated sites (T-sites). However, the Ni displacement parameter and the Ni-O bond lengths suggest that for the X = Ni sample, there may actually be some T-site cation disorder.

Rietveld refinement of the crystal structures of Rb2 XSi5O12 (X = Ni, Mn)

PubMed Central

Bell, Anthony M. T.; Henderson, C. Michael B.

2016-01-01

The synthetic leucite silicate framework mineral analogues Rb2 XSi5O12 {X = Ni [dirubidium nickel(II) penta­silicate] and Mn [dirubidium manganese(II) penta­silicate]} have been prepared by high-temperature solid-state synthesis. The results of Rietveld refinements, using X-ray powder diffraction data collected using Cu Kα X-rays, show that the title compounds crystallize in the space group Pbca and adopt the cation-ordered structure of Cs2CdSi5O12 and other leucites. The structures consist of tetra­hedral SiO4 and XO4 units sharing corners to form a partially substituted silicate framework. Extraframework Rb+ cations sit in channels in the framework. All atoms occupy the 8c general position for this space group. In these refined structures, silicon and X atoms are ordered onto separate tetra­hedrally coordinated sites (T-sites). However, the Ni displacement parameter and the Ni—O bond lengths suggest that for the X = Ni sample, there may actually be some T-site cation disorder. PMID:26958399

Synchrotron X-ray diffraction study of the Ba{sub 1−x}SrSnO{sub 3} solid solution

DOE Office of Scientific and Technical Information (OSTI.GOV)

Prodjosantoso, Anti K., E-mail: Prodjosantoso@yahoo.com; Zhou, Qingdi; Kennedy, Brendan J.

At room temperature the sequence of phases with increasing amounts of strontium in the stannate perovskite system Ba{sub 1−x}SrSnO{sub 3} has been established from high resolution synchrotron X-ray powder diffraction. The observed sequence orthorhombic (Pbnm), orthorhombic (Ibmm), tetragonal (I4/mcm), and cubic (Pm3-bar m) is a consequence of the sequential introduction of cooperative tilting of the corner sharing SnO{sub 6} octahedra. The cell volume changes smoothly across the series with no obvious discontinuities associated with the phase transitions. - Graphical abstract: Portions of the synchrotron X-ray diffraction profiles (λ=0.82453 Å) from selected Ba{sub 1−x}Sr{sub x}SnO{sub 3} samples together with the resultsmore » of fitting by the Rietveld method. Highlights: ► Structures of the stannate perovskites Ba{sub 1−x}SrSnO{sub 3} refined from synchrotron XRD. ► The sequence Pm3-bar m→I4/mcm→Ibmm→Pbnm results from tilting of the octahedra. ► The tilting maintains optimal bonding of the cations seen from the BVS analysis.« less

Rietveld analysis of the effect of annealing atmosphere on phase evolution of nanocrystalline TiO2 powders.

PubMed

Salari, M; Rezaee, M; Chidembo, A T; Konstantinov, K; Liu, H K

2012-06-01

The structural evolution of nanocrystalline TiO2 was studied by X-ray diffraction (XRD) and the Rietveld refinement method (RRM). TiO2 powders were prepared by the sol-gel technique. Post annealing of as-synthesized powders in the temperature range from 500 degrees C to 800 degrees C under air and argon atmospheres led to the formation of TiO2 nanoparticles with mean crystallite size in the range of 37-165 nm, based on the Rietveld refinement results. It was found that the phase structure, composition, and crystallite size of the resulting particles were dependent on not only the annealing temperature, but also the annealing atmosphere. Rietveld refinement of the XRD data showed that annealing the powders under argon atmosphere promoted the polymorphic phase transformation from anatase to rutile. Field emission scanning electron microscopy (FESEM) was employed to investigate the morphology and size of the annealed powders.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Aldridge, James D.; Womick, Jordan M.; Rosmus, Kimberly A.

Novel quaternary lanthanide-substituted oxides of stoichiometry LnxY2-xTi2O7 (where Ln is lanthanum, neodymium, samarium, gadolinium, or ytterbium) were prepared by traditional high-temperature, solid-state techniques and characterized by X-ray powder diffraction. Samples with nominal values of x up to 1.0 were attempted. The well-studied ternary cubic pyrochlore compound yttrium titanium oxide (Y2Ti2O7, space group Fd-3m, Z = 8), served as a parent structural framework in which Ln3+ cations were substituted on the Y3+ site. Laboratory-grade X-ray powder diffraction data revealed pure quaternary pyrochlore phases for LnxY2-xTi2O7 with x ≤ 0.2. Pyrochlore phase purity was verified by Rietveld analysis using high-resolution synchrotron X-raymore » powder diffraction data when x ≤ 0.2, however, for La3+ substitution specifically, pure quaternary pyrochlore formed at x<0.1. Band gap energies on selected samples were determined using optical diffuse reflectance spectroscopy and showed that these materials can be classified as electrical insulators with indirect band gap energies around 3.7 eV.« less

Effect of laser welding parameters on the austenite and martensite phase fractions of NiTi

DOE Office of Scientific and Technical Information (OSTI.GOV)

Oliveira, J.P., E-mail: jp.oliveira@campus.fct.unl

Although laser welding is probably the most used joining technique for NiTi shape memory alloys there is still a lack of understanding about the effects of laser welding parameters on the microstructural induced changes: in both the heat affected and fusion zones martensite may be present, while the base material is fully austenitic. Synchrotron X-ray diffraction was used for fine probing laser welded NiTi joints. Through Rietveld refinement the martensite and austenite phase fractions were determined and it was observed that the martensite content increases towards the weld centreline. This is related to a change of the local transformation temperaturesmore » on these regions, which occurs due to compositional variation in those regions. The martensite phase fraction in the thermally affected regions may have significant implications on functional properties on these joints. - Highlights: •Synchrotron X-ray diffraction was used for fine probing of the microstructure in laser welded NiTi joints. •Rietveld refinement allowed to determine the content of martensite along the heat affected and fusion zones. •The martensite content increases from the base material towards the weld centreline.« less

Tin-Platinum catalysts interactions on titania and silica

NASA Astrophysics Data System (ADS)

Nava, N.; Del Angel, P.; Salmones, J.; Baggio-Saitovitch, E.; Santiago, P.

2007-09-01

Pt-Sn was supported on titania and silica, and the resulting interactions between the components in prepared samples and the resulting interactions between the components before and after treatment with hydrogen were characterized by Mössbauer spectroscopy, X-ray diffraction, Rietveld refinement, high-resolution transmission electron microscopy (HRTEM) and catalytic tests data. Results show the presence of Pt and SnO 2 after calcinations, and Pt 3Sn, PtSn and PtSn 3 after reduction. Rietveld analysis shows that some Ti 4+ are replaced by Sn 4+ atoms in the titania structure. Finally, HRTEM and the practically absence of activity observed confirms that metallic platinum is encapsulated.

Grain size dependent phase stabilities and presence of a monoclinic (Pm) phase in the morphotropic phase boundary region of (1-x)Bi(Mg1/2Ti1/2)O3-xPbTiO3 piezoceramics

NASA Astrophysics Data System (ADS)

Upadhyay, Ashutosh; Singh, Akhilesh Kumar

2015-04-01

Results of the room temperature structural studies on (1-x)Bi(Mg1/2Ti1/2)O3-xPbTiO3 ceramics using Rietveld analysis of the powder x-ray diffraction data in the composition range 0.28 ≤ x ≤ 0.45 are presented. The morphotropic phase boundary region exhibits coexistence of monoclinic (space group Pm) and tetragonal (space group P4 mm) phases in the composition range 0.33 ≤ x ≤ 0.40. The structure is nearly single phase monoclinic (space group Pm) in the composition range 0.28 ≤ x ≤ 0.32. The structure for the compositions with x ≥ 0.45 is found to be predominantly tetragonal with space group P4 mm. Rietveld refinement of the structure rules out the coexistence of rhombohedral and tetragonal phases in the morphotropic phase boundary region reported by earlier authors. The Rietveld structure analysis for the sample x = .35 calcined at various temperatures reveals that phase fraction of the coexisting phases in the morphotropic phase boundary region varies with grain size. The structural parameters of the two coexisting phases also change slightly with changing grain size.

Synchrotron-based XAS on structure investigation of La0.99-xSrx(Na, K, Ba)0.01MnO3 nanoparticles: Evidence of magnetic properties

NASA Astrophysics Data System (ADS)

Daengsakul, Sujittra; Saengplot, Saowalak; Kidkhunthod, Pinit; Pimsawat, Adulphan; Maensiri, Santi

2018-04-01

This work presents the structural study of La0.99-xSrx(Na, K, Ba)0.01MnO3 or LSAM nanoparticles synthesized using thermal-hydro decomposition method where A denotes Na, K, Sr and Ba, respectively. The effect of ionic radii size of A dopants or rA from the substitution of A for La and Sr on the MnO6 octrahedral structure, where the average size of the cations occupying in A-site or 〈rA〉 is fixed at ∼ 1.24 Å, is focused. The LSAM nanoparticles are carefully studied using X-ray diffraction (XRD) including Rietveld refinement and X-ray Absorption Spectroscopy (XAS) including X-ray Absorption Near edge Structure (XANES) and X-ray Absorption Fine Structure (EXAFS). The Rietveld refinement shows all nano-powder samples have rhombohedral structure. By XANES technique we found that the effect of A substitutions at A-site causes a slight change of mean oxidation state of Mn between 3.54 and 3.60. Furthermore, the structural distortion of MnO6 octrahedral in samples is analysed and obtained from EXAFS. The observed trend of ferromagnetism for all LSAM samples can be clearly explained by evidences of A-site doping, structural distortion around Mn atoms and mixing Mn3+/Mn4+ valence states.

Structural properties of a family of hydrogen-bonded co-crystals formed between gemfibrozil and hydroxy derivatives of t-butylamine, determined directly from powder X-ray diffraction data

NASA Astrophysics Data System (ADS)

Cheung, Eugene Y.; David, Sarah E.; Harris, Kenneth D. M.; Conway, Barbara R.; Timmins, Peter

2007-03-01

We report the formation and structural properties of co-crystals containing gemfibrozil and hydroxy derivatives of t-butylamine H 2NC(CH 3) 3-n(CH 2OH) n, with n=0, 1, 2 and 3. In each case, a 1:1 co-crystal is formed, with transfer of a proton from the carboxylic acid group of gemfibrozil to the amino group of the t-butylamine derivative. All of the co-crystal materials prepared are polycrystalline powders, and do not contain single crystals of suitable size and/or quality for single crystal X-ray diffraction studies. Structure determination of these materials has been carried out directly from powder X-ray diffraction data, using the direct-space Genetic Algorithm technique for structure solution followed by Rietveld refinement. The structural chemistry of this series of co-crystal materials reveals well-defined structural trends within the first three members of the family ( n=0, 1, 2), but significantly contrasting structural properties for the member with n=3.

An Improved X-ray Diffraction Method For Cellulose Crystallinity Measurement

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ju, Xiaohui; Bowden, Mark E.; Brown, Elvie E.

2015-06-01

We show in this work a modified X-ray diffraction method to determine cellulose crystallinity index (CrI). Nanocrystalline cellulose (NCC) dervided from bleached wood pulp was used as a model substrate. Rietveld refinement was applied with consideration of March-Dollase preferred orientation at the (001) plane. In contrast to most previous methods, three distinct amorphous peaks identified from new model samples which are used to calculate CrI. A 2 theta range from 10° to 75° was found to be more suitable to determine CrI and crystallite structural parameters such as d-spacing and crystallite size. This method enables a more reliable measurement ofmore » CrI of cellulose and may be applicable to other types of cellulose polymorphs.« less

Crystal phase analysis of SnO{sub 2}-based varistor ceramic using the Rietveld method

DOE Office of Scientific and Technical Information (OSTI.GOV)

Moreira, M.L.; Pianaro, S.A.; Andrade, A.V.C.

2006-09-15

A second addition of l mol% of CoO to a pre calcined SnO{sub 2}-based ceramic doped with 1.0 mol% of CoO, 0.05 mol% of Nb{sub 2}O{sub 5} and 0.05 mol% of Cr{sub 2}O{sub 3} promotes the appearance of a secondary phase, Co{sub 2}SnO{sub 4}, besides the SnO{sub 2} cassiterite phase, when the ceramic was sintered at 1350 deg. C/2 h. This was observed using X-ray powder diffraction, scanning electron microscopy and energy dispersive X-ray techniques. Rietveld refinement was carried out to quantify the phases present in the ceramic system. The results of the quantitative analysis were 97 wt.% SnO{sub 2}more » and 3 wt.% Co{sub 2}SnO{sub 4}. The microstructural analysis showed that a certain amount of cobalt ion remains into cassiterite grains.« less

Presence of a monoclinic (Pm) phase in the morphotropic phase boundary region of multiferroic (1 − x)Bi(Ni{sub 1/2}Ti{sub 1/2})O{sub 3}-xPbTiO{sub 3} solid solution: A Rietveld study

DOE Office of Scientific and Technical Information (OSTI.GOV)

Pandey, Rishikesh, E-mail: akhilesh-bhu@yahoo.com, E-mail: aksingh.mst@itbhu.ac.in; Singh, Akhilesh Kumar, E-mail: akhilesh-bhu@yahoo.com, E-mail: aksingh.mst@itbhu.ac.in

2014-07-28

We present here the results of structural studies on multiferroic (1 − x)Bi(Ni{sub 1/2}Ti{sub 1/2})O{sub 3}-xPbTiO{sub 3} solid solution using Rietveld analysis on powder x-ray diffraction data in the composition range 0.35 ≤ x ≤ 0.55. The stability region of various crystallographic phases at room temperature for (1 − x)Bi(Ni{sub 1/2}Ti{sub 1/2})O{sub 3}-xPbTiO{sub 3} is determined precisely. Structural transformation from pseudo-cubic (x ≤ 0.40) to tetragonal (x ≥ 0.50) phase is observed via phase coexistence region demarcating the morphotropic phase boundary. The morphotropic phase boundary region consists of coexisting tetragonal and monoclinic structures with space group P4mm and Pm, respectively, stable in composition range 0.41 ≤ x ≤ 0.49 as confirmed by Rietveld analysis. The resultsmore » of Rietveld analysis completely rule out the coexistence of rhombohedral and tetragonal phases in the morphotropic phase boundary region reported by earlier workers. A comparison between the bond lengths for “B-site cations-oxygen anions” obtained after Rietveld refinement, with the bond length calculated using Shannon-Prewitt ionic radii, reveals the ionic nature of B-O (Ni/Ti-O) bonds for the cubic phase and partial covalent character for the other crystallographic phases.« less

Extended investigation of intermartensitic transitions in Ni-Mn-Ga magnetic shape memory alloys: A detailed phase diagram determination

NASA Astrophysics Data System (ADS)

Ćakιr, Aslι; Righi, Lara; Albertini, Franca; Acet, Mehmet; Farle, Michael; Aktürk, Selçuk

2013-11-01

Martensitic transitions in shape memory Ni-Mn-Ga Heusler alloys take place between a high temperature austenite and a low temperature martensite phase. However, intermartensitic transformations have also been encountered that occur from one martensite phase to another. To examine intermartensitic transitions in magnetic shape memory alloys in detail, we carried out temperature dependent magnetization, resistivity, and x-ray diffraction measurements to investigate the intermartensitic transition in Ni50Mn50-xGax in the composition range 12≤x≤25 at. %. Rietveld refined x-ray diffraction results are found to be consistent with magnetization and resistivity data. Depending on composition, we observe that intermartensitic transitions occur in the sequences 7M→L10, 5M →7M, and 5M→7M→L10 with decreasing temperature. The L10 non-modulated structure is most stable at low temperature.

Application of micro X-ray diffraction to investigate the reaction products formed by the alkali silica reaction in concrete structures

DOE Office of Scientific and Technical Information (OSTI.GOV)

Dähn, R.; Arakcheeva, A.; Schaub, Ph.

Alkali–silica reaction (ASR) is one of the most important deterioration mechanisms in concrete leading to substantial damages of structures worldwide. Synchrotron-based micro-X-ray diffraction (micro-XRD) was employed to characterize the mineral phases formed in micro-cracks of concrete aggregates as a consequence of ASR. This particular high spatial resolution technique enables to directly gain structural information on ASR products formed in a 40-year old motorway bridge damaged due to ASR. Micro-X-ray-fluorescence was applied on thin sections to locate the reaction products formed in veins within concrete aggregates. Micro-XRD pattern were collected at selected points of interest along a vein by rotating themore » sample. Rietveld refinement determined the structure of the ASR product consisting of a new layered framework similar to mountainite and rhodesite. Furthermore, it is conceivable that understanding the structure of the ASR product may help developing new technical treatments inhibiting ASR.« less

Application of micro X-ray diffraction to investigate the reaction products formed by the alkali–silica reaction in concrete structures

DOE Office of Scientific and Technical Information (OSTI.GOV)

Dähn, R., E-mail: rainer.daehn@psi.ch; Arakcheeva, A.; Schaub, Ph.

Alkali–silica reaction (ASR) is one of the most important deterioration mechanisms in concrete leading to substantial damages of structures worldwide. Synchrotron-based micro-X-ray diffraction (micro-XRD) was employed to characterize the mineral phases formed in micro-cracks of concrete aggregates as a consequence of ASR. This high spatial resolution technique enables to directly gain structural information on ASR products formed in a 40-year old motorway bridge damaged due to ASR. Micro-X-ray-fluorescence was applied on thin sections to locate the reaction products formed in veins within concrete aggregates. Micro-XRD pattern were collected at selected points of interest along a vein by rotating the sample.more » Rietveld refinement determined the structure of the ASR product consisting of a new layered framework similar to mountainite and rhodesite. It is conceivable that understanding the structure of the ASR product may help developing new technical treatments inhibiting ASR.« less

In Situ XRD Studies of the Process Dynamics During Annealing in Cold-Rolled Copper

NASA Astrophysics Data System (ADS)

Dey, Santu; Gayathri, N.; Bhattacharya, M.; Mukherjee, P.

2016-12-01

The dynamics of the release of stored energy during annealing along two different crystallographic planes, i.e., {111} and {220}, in deformed copper have been investigated using in situ X-ray diffraction measurements at 458 K and 473 K (185 °C and 200 °C). The study has been carried out on 50 and 80 pct cold-rolled Cu sheets. The microstructures of the rolled samples have been characterized using optical microscopy and electron backscattered diffraction measurements. The microstructural parameters were evaluated from the X-ray diffractogram using the Scherrer equation and the modified Rietveld method. The stored energy along different planes was determined using the modified Stibitz formula from the X-ray peak broadening, and the bulk stored energy was evaluated using differential scanning calorimetry. The process dynamics of recovery and recrystallization as observed through the release of stored energy have been modeled as the second-order and first-order processes, respectively.

Ferroelectric performances and crystal structures of (Pb, La)(Zr, Ti, Nb)O{sub 3}

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kitamura, Naoto; Division of Ecosystem Research, Research Institute for Science and Technology, Tokyo University of Science, 2641 Yamazaki, Noda, Chiba 278-8510; Mizoguchi, Takuma

2014-02-15

In this study, we focused on Nb and La substituted Pb(Zr, Ti)O{sub 3}: i.e., (Pb, La)(Zr, Ti, Nb)O{sub 3}. As for the samples, dependences of ferroelectric properties on La and Nb compositions were examined. In addition, the crystal structures were analyzed by the Rietveld method, and then a relationship between the metal compositions and the crystal structures were discussed. From P–E hysteresis loop measurements, it was found that the remanant polarization of Pb(Zr, Ti)O{sub 3} was increased by both the La and Nb substitutions although the heavy substitution of La had an undesirable effect. It was also indicated that themore » Curie temperature decreased with increasing La content. The Rietveld analysis using synchrotron X-ray diffraction patterns demonstrated that the structure distortion was relaxed by the La and Nb substitutions. Such a change in the crystals was well consistent with the harmful effects on the Curie temperature and the remanent polarization by the heavy La substitution. - Graphical abstract: Rietveld refinement pattern of 2 mol% PbSiO{sub 3}-added Pb{sub 0.95}La{sub 0.05}Zr{sub 0.50}Ti{sub 0.45}Nb{sub 0.05}O{sub 3} (synchrotron X-ray diffraction). Display Omitted - Highlights: • (Pb,La)(Zr,Ti,Nb)O{sub 3} were successfully synthesized. • Remanant polarization of Pb(Zr,Ti)O{sub 3} was improved by substitutions of La and Nb. • Crystal structures of (Pb,La)(Zr,Ti,Nb)O{sub 3} were refined and the distortions were estimated.« less

Polymorphism of Alprazolam (Xanax): a review of its crystalline phases and identification, crystallographic characterization, and crystal structure of a new polymorph (form III).

PubMed

de Armas, Héctor Novoa; Peeters, Oswald M; Van den Mooter, Guy; Blaton, Norbert

2007-05-01

A new polymorphic form of Alprazolam (Xanax), 8-chloro-1-methyl-6-phenyl-4H-[1,2,4]triazolo-[4,3-alpha][1,4]benzodiazepine, C(17)H(13)ClN(4), has been investigated by means of X-ray powder diffraction (XRPD), single crystal X-ray diffraction, and differential scanning calorimetry (DSC). This polymorphic form (form III) was obtained during DSC experiments after the exothermic recrystallization of the melt of form I. The crystal unit cell dimensions for form III were determined from diffractometer methods. The monoclinic unit cell found for this polymorph using XRPD after indexing the powder diffractogram was confirmed by the cell parameters obtained from single crystal X-ray diffractometry on a crystal isolated from the DSC pans. The single crystal unit cell parameters are: a = 28.929(9), b = 13.844(8), c = 7.361(3) angstroms, beta = 92.82(3) degrees , V = 2944(2) angstroms(3), Z = 8, space group P2(1) (No.4), Dx = 1.393 Mg/m(3). The structure obtained from single crystal X-ray diffraction was used as initial model for Rietveld refinement on the powder diffraction data of form III. The temperature phase transformations of alprazolam were also studied using high temperature XRPD. A review of the different phases available in the Powder Diffraction File (PDF) database for this drug is described bringing some clarification and corrections. (c) 2007 Wiley-Liss, Inc. and the American Pharmacists Association.

Trithallium hydrogen bis(sulfate), Tl(3)H(SO(4))(2), in the super-ionic phase by X-ray powder diffraction.

PubMed

Matsuo, Yasumitsu; Kawachi, Shinya; Shimizu, Yuya; Ikehata, Seiichiro

2002-07-01

The structure of trithallium hydrogen bis(sulfate), Tl(3)H(SO(4))(2), in the super-ionic phase has been analyzed by Rietveld analysis of the X-ray powder diffraction pattern. Atomic parameters based on the isotypic Rb(3)H(SeO(4))(2) crystal in space group R3m in the super-ionic phase were used as the starting model, because it has been shown from the comparison of thermal and electric properties in Tl(3)H(SO(4))(2) and M(3)H(SO(4))(2) type crystals (M = Rb, Cs or NH(4)) that the room-temperature Tl(3)H(SO(4))(2) phase is isostructural with the high-temperature R3m-symmetry M(3)H(SO(4))(2) crystals. The structure was determined in the trigonal space group R3m and the Rietveld refinement shows that an hydrogen-bond O-H...O separation is slightly shortened compared with O-H...O separations in isotypic M(3)H(SeO(4))(2) crystals. In addition, it was found that the distortion of the SO(4) tetrahedra in Tl(3)H(SO(4))(2) is less than that in isotypic crystals.

Structure resolution by electron diffraction tomography of the complex layered iron-rich Fe-2234-type Sr{sub 5}Fe{sub 6}O{sub 15.4}

DOE Office of Scientific and Technical Information (OSTI.GOV)

Lepoittevin, Christophe, E-mail: christophe.lepoittevin@neel.cnrs.fr

2016-10-15

The crystal structure of the strontium ferrite Sr{sub 5}Fe{sub 6}O{sub 15.4}, was solved by direct methods on electron diffraction tomography data acquired on a transmission electron microscope. The refined cell parameters are a=27.4047(3) Å, b=5.48590(7) Å and c=42.7442(4) Å in Fm2m symmetry. Its structure is built up from the intergrowth sequence between a quadruple perovskite-type layer with a complex rock-salt (RS)-type block. In the latter iron atoms are found in two different environments : tetragonal pyramid and tetrahedron. The structural model was refined by Rietveld method based on the powder X-ray diffraction pattern. - Highlights: • Complex structure of Sr{submore » 5}Fe{sub 6}O{sub 15.4} solved by electron diffraction tomography. • Observed Fourier maps allow determining missing oxygen atoms in the structure. • Structural model refined from powder X-ray diffraction data. • Intergrowth between quadruple perovskite layer with double rock-salt-type layer.« less

Extended investigation of intermartensitic transitions in Ni-Mn-Ga magnetic shape memory alloys: A detailed phase diagram determination

DOE Office of Scientific and Technical Information (OSTI.GOV)

Çakir, Asli; Aktürk, Selçuk; Righi, Lara

2013-11-14

Martensitic transitions in shape memory Ni-Mn-Ga Heusler alloys take place between a high temperature austenite and a low temperature martensite phase. However, intermartensitic transformations have also been encountered that occur from one martensite phase to another. To examine intermartensitic transitions in magnetic shape memory alloys in detail, we carried out temperature dependent magnetization, resistivity, and x-ray diffraction measurements to investigate the intermartensitic transition in Ni{sub 50}Mn{sub 50–x}Ga{sub x} in the composition range 12≤x≤25 at. %. Rietveld refined x-ray diffraction results are found to be consistent with magnetization and resistivity data. Depending on composition, we observe that intermartensitic transitions occur inmore » the sequences 7M→L1{sub 0}, 5M→7M, and 5M→7M→L1{sub 0} with decreasing temperature. The L1{sub 0} non-modulated structure is most stable at low temperature.« less

Combined Approach for the Structural Characterization of Alkali Fluoroscandates: Solid-State NMR, Powder X-ray Diffraction, and Density Functional Theory Calculations.

PubMed

Rakhmatullin, Aydar; Polovov, Ilya B; Maltsev, Dmitry; Allix, Mathieu; Volkovich, Vladimir; Chukin, Andrey V; Boča, Miroslav; Bessada, Catherine

2018-02-05

The structures of several fluoroscandate compounds are presented here using a characterization approach combining powder X-ray diffraction and solid-state NMR. The structure of K 5 Sc 3 F 14 was fully determined from Rietveld refinement performed on powder X-ray diffraction data. Moreover, the local structures of NaScF 4 , Li 3 ScF 6 , KSc 2 F 7 , and Na 3 ScF 6 compounds were studied in detail from solid-state 19 F and 45 Sc NMR experiments. The 45 Sc chemical shift ranges for six- and seven-coordinated scandium environments were defined. The 19 F chemical shift ranges for bridging and terminal fluorine atoms were also determined. First-principles calculations of the 19 F and 45 Sc NMR parameters were carried out using plane-wave basis sets and periodic boundary conditions (CASTEP), and the results were compared with the experimental data. A good agreement between the calculated shielding constants and experimental chemical shifts was obtained. This demonstrates the good potential of computational methods in spectroscopic assignments of solid-state 45 Sc NMR spectroscopy.

On the measurement of austenite in supermartensitic stainless steel by X-ray diffraction

DOE Office of Scientific and Technical Information (OSTI.GOV)

Tolchard, Julian Richard, E-mail: tolchard@material.ntnu.no; Sømme, Astri; Solberg, Jan Ketil

2015-01-15

Sections of a 13Cr supermartensitic stainless steel were investigated to determine the optimum sample preparation for measurement of the austenite content by X-ray diffraction. The surface of several samples was mechanically ground or polished using media of grit sizes in the range 1–120 μm. The strained surface layer was afterwards removed stepwise by electropolishing, and the austenite content measured at each step. It was found that any level of mechanical grinding or polishing results in a reduction of the measured austenite fraction relative to the true bulk value, and that coarser grinding media impart greater damage and greater reduction inmore » the measured austenite content. The results thus highlight the importance of the electropolishing step in preparation of such samples, but suggest that the American Society for Testing and Materials standard E975-03 substantially overestimates the amount of material which needs to be removed to recover the true “bulk” content. - Highlights: • Quantitative Rietveld analysis of austenite/martensite ratio in supermartensitic stainless steels • Critical evaluation of sample preparation for residual austenite measurements by X-ray diffraction • Highlighting of the importance of electropolishing as a final preparation step.« less

Quantifying point defects in Cu 2 ZnSn(S,Se) 4 thin films using resonant x-ray diffraction

DOE PAGES

Stone, Kevin H.; Christensen, Steven T.; Harvey, Steven P.; ...

2016-10-17

Cu 2ZnSn(S,Se)4 is an interesting, earth abundant photovoltaic material, but has suffered from low open circuit voltage. To better understand the film structure, we have measured resonant x-ray diffraction across the Cu and Zn K-edges for the device quality thin films of Cu 2ZnSnS4 (8.6% efficiency) and Cu 2ZnSn(S,Se)4 (3.5% efficiency). This approach allows for the confirmation of the underlying kesterite structure and quantification of the concentration of point defects and vacancies on the Cu, Zn, and Sn sublattices. Rietveld refinement of powder diffraction data collected at multiple energies is used to determine that there exists a high level ofmore » Cu Zn and Zn Cu defects on the 2c and 2d Wyckoff positions. We observe a significantly lower concentration of Zn Sn defects and Cu or Zn vacancies.« less

Low-temperature synthesis of homogeneous solid solutions of scheelite-structured Ca 1-xSr xWO 4 and Sr 1-xBa xWO 4 nanocrystals

DOE PAGES

Culver, Sean P.; Greaney, Matthew J.; Tinoco, Antonio; ...

2015-07-24

Here, a series of compositionally complex scheelite-structured nanocrystals of the formula A 1-xA’ xWO 4 (A = Ca, Sr, Ba) have been prepared under benign synthesis conditions using the vapor diffusion sol–gel method. Discrete nanocrystals with sub-20 nm mean diameters were obtained after kinetically controlled hydro- lysis and polycondensation at room temperature, followed by composition-dependent thermal aging at or below 60 °C. Rietveld analysis of X-ray diffraction data and Raman spectroscopy verified the synthesis of continuous and phase-pure nanocrystal solid solutions across the entire composition space for A 1-xA’ xWO 4, where 0 ≤ x ≤ 1. Elemental analysis bymore » X-ray photoelectron and inductively coupled plasma- atomic emission spectroscopies demonstrated excellent agreement between the nominal and experi- mentally determined elemental stoichiometries, while energy dispersive X-ray spectroscopy illustrated good spatial elemental homogeneity within these nanocrystals synthesized under benign conditions.« less

Neutron and X-ray powder diffraction study of skutterudite thermoelectrics

DOE PAGES

Wang, H.; Kirkham, M. J.; Watkins, T. R.; ...

2016-02-17

N- and p-type filled-skutterudite materials prepared for thermoelectric power generation modules were analyzed by neutron diffraction at the POWGEN beam line of the Spallation Neutron Source (SNS) and X-ray diffraction (XRD). The skutterudite powders were processed by melt spinning, followed by ball milling and annealing. The n-type material consists of Ba–Yb–Co–Sb and the p-type material consists of Di–Fe–Ni–Sb or Di–Fe–Co–Sb (Di = didymium, an alloy of Pr and Nd). Powders for prototype module fabrication from General Motors and Marlow Industries were analyzed in this study. XRD and neutron diffraction studies confirm that both the n- and p-type materials have cubicmore » symmetry. Structural Rietveld refinements determined the lattice parameters and atomic parameters of the framework and filler atoms. The cage filling fraction was found to depend linearly on the lattice parameter, which in turn depends on the average framework atom size. Ultimately, this knowledge may allow the filling fraction of these skutterudite materials to be purposefully adjusted, thereby tuning the thermoelectric properties.« less

Boron monosulfide: Equation of state and pressure-induced phase transition

NASA Astrophysics Data System (ADS)

Cherednichenko, K. A.; Kruglov, I. A.; Oganov, A. R.; Le Godec, Y.; Mezouar, M.; Solozhenko, V. L.

2018-04-01

Quasi-hydrostatic compression of rhombohedral boron monosulfide (r-BS) has been studied up to 50 GPa at room temperature using diamond-anvil cells and angle-dispersive synchrotron X-ray diffraction. A fit of the experimental P-V data to the Vinet equation of state yields the bulk modulus B0 of 42.2(1.4) GPa and its first pressure derivative B0' of 7.6(2) that are in excellent agreement with our ab initio calculations. Formation of a new high-pressure phase of boron monosulfide (hp-BS) has been observed above 35 GPa. According to ab initio evolutionary crystal structure predictions combined with Rietveld refinement of high-pressure X-ray diffraction data, the structure of hp-BS has trigonal symmetry and belongs to the space group P-3m1. As it follows from the electron density of state calculations, the phase transformation is accompanied by an insulator-metal transition.

Study of the mechanical behavior of the hydride blister/rim structure in Zircaloy-4 using in-situ synchrotron X-ray diffraction

DOE Office of Scientific and Technical Information (OSTI.GOV)

Lin, Jun-li; Han, Xiaochun; Heuser, Brent J.

2016-04-01

High-energy synchrotron X-ray diffraction was utilized to study the mechanical response of the f.c.c delta hydride phase, the intermetallic precipitation with hexagonal C14 lave phase and the alpha-Zr phase in the Zircaloy-4 materials with a hydride rim/blister structure near one surface of the material during in-situ uniaxial tension experiment at 200 degrees C. The f.c.c delta was the only hydride phase observed in the rim/blister structure. The conventional Rietveld refinement was applied to measure the macro-strain equivalent response of the three phases. Two regions were delineated in the applied load versus lattice strain measurement: a linear elastic strain region andmore » region that exhibited load partitioning. Load partitioning was quantified by von Mises analysis. The three phases were observed to have similar elastic modulus at 200 degrees C.« less

Magnetism in La{sub 0.7}Sr{sub 0.3}Mn{sub 1-x}Co{sub x}O{sub 3} (0 ≤ x ≤ 1)

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kumar, Ashutosh, E-mail: ashutosh.pph13@iitp.ac.in; Sharma, Himanshu; Tomy, C. V.

2016-05-23

We study the structural and magnetic properties of La{sub 0.7}Sr{sub 0.3}Mn{sub 1-x}Co{sub x}O{sub 3} (0 ≤ x ≤ 1). Rietveld refinement of X-ray Diffraction (XRD) pattern suggests phase purity of the polycrystalline samples with R-3c space group. Interplay of Ferromagnetic (FM) and Antiferromagnetic (AFM) interaction upon Co substitution at Mn site in La{sub 0.7}Sr{sub 0.3}MnO{sub 3} is evident from magnetic measurements. There is an optimal cobalt substitution at which the coercive field is maximum.

Microstructural characterisation of proton irradiated niobium using X-ray diffraction technique

NASA Astrophysics Data System (ADS)

Dutta, Argha; Gayathri, N.; Neogy, S.; Mukherjee, P.

2018-04-01

The microstructural parameters in pure Nb, irradiated with 5 MeV proton beam have been evaluated as a function of dose using X-ray diffraction line profile analysis. In order to assess the microstructural changes in the homogeneous region and in the peak damage region of the damage energy deposition profile, X-ray diffraction patterns have been collected using two different geometries (Bragg-Brentano and parallel beam geometries). Different X-ray line profile analysis like Williamson-Hall (W-H) analysis, modified W-H analysis, double-Voigt analysis, modified Rietveld technique and convolutional multiple whole profile fitting have been employed to extract the microstructural parameters like coherent domain size, microstrain within the domain, dislocation density and arrangement of dislocations. The coherent domain size decreases drastically along with increase in microstrain and dislocation density in the first dose for both the geometries. With increasing dose, a decreasing trend in microstrain associated with decrease in dislocation density is observed for both the geometries. This is attributed to the formation of defect clusters due to irradiation which with increasing dose collapse to dislocation loops to minimise the strain in the matrix. This is corroborated with the observation of black dots and loops in the TEM images. No significant difference is observed in the trend of microstructural parameters between the homogeneous and peak damage region of the damage profile.

Incorporation of Cadmium and Nickel into Ferrite Spinel Solid Solution: X-ray Diffraction and X-ray Absorption Fine Structure Analyses.

PubMed

Su, Minhua; Liao, Changzhong; Chan, Tingshan; Shih, Kaimin; Xiao, Tangfu; Chen, Diyun; Kong, Lingjun; Song, Gang

2018-01-16

The feasibility of incorporating Cd and Ni in hematite was studied by investigating the interaction mechanism for the formation of Cd x Ni 1-x Fe 2 O 4 solid solutions (CNFs) from CdO, NiO, and α-Fe 2 O 3 . X-ray diffraction results showed that the CNFs crystallized into spinel structures with increasing lattice parameters as the Cd content in the precursors was increased. Cd 2+ ions were found to occupy the tetrahedral sites, as evidenced by Rietveld refinement and extended X-ray absorption fine structure analyses. The incorporation of Cd and Ni into ferrite spinel solid solution strongly relied on the processing parameters. The incorporation of Cd and Ni into the CNFs was greater at high x values (0.7 < x ≤ 1.0) than at low x values (0.0 ≤ x ≤ 0.7). A feasible treatment technique based on the investigated mechanism of CNF formation was developed, involving thermal treatment of waste sludge containing Cd and Ni. Both of these metals in the waste sludge were successfully incorporated into a ferrite spinel solid solution, and the concentrations of leached Cd and Ni from this solid solution were substantially reduced, stabilizing at low levels. This research offers a highly promising approach for treating the Cd and Ni content frequently encountered in electronic waste and its treatment residues.

Investigation on the structural, magnetic and magnetocaloric properties of nanocrystalline Pr-deficient Pr1-xSrxMnO3-δ manganites

NASA Astrophysics Data System (ADS)

Arun, B.; Athira, M.; Akshay, V. R.; Sudakshina, B.; Mutta, Geeta R.; Vasundhara, M.

2018-02-01

We have investigated the structural, magnetic and magnetocaloric properties of nanocrystalline Pr-deficient Pr1-xSrxMnO3-δ Perovskite manganites. Rietveld refinement of the X-ray powder diffraction patterns confirms that all the studied compounds have crystallized into an orthorhombic structure with Pbnm space group. Transmission electron microscopy analysis reveals nanocrystalline compounds with crystallite size less than 50 nm. The selected area electron diffraction patterns reveal the highly crystalline nature of the compounds and energy dispersive X-ray spectroscopic analysis shows that the obtained compositions are nearly identical with the nominal one. The oxygen stoichiometry is estimated by iodometric titration method and stoichiometric compositions are confirmed by X-ray Fluorescence Spectrometry analysis. A large bifurcation is observed in the ZFC/FC curves and Arrott plots not show a linear relation but have a convex curvature nature. The temperature dependence of inverse magnetic susceptibility at higher temperature confirms the existence of ferromagnetic clusters. The experimental results reveal that the reduction of crystallite size to nano metric scale in Pr-deficient manganites adversely influences structural, magnetic and magnetocaloric properties as compared to its bulk counterparts reported earlier.

Nano-Crystalline Thermally Evaporated Bi2Se3 Thin Films Synthesized from Mechanically Milled Powder

NASA Astrophysics Data System (ADS)

Amara, A.; Abdennouri, N.; Drici, A.; Abdelkader, D.; Bououdina, M.; Chaffar Akkari, F.; Khemiri, N.; Kanzari, M.; Bernède, J. C.

2017-08-01

Bi2Se3 powder has been successfully synthesized via mechanical ball milling of bismuth and selenium as starting materials. X-ray diffraction characterization revealed the formation of the rhombohedral and orthorhombic phases of Bi2Se3 material belonging to systems with space groups R\\bar{3}m and Pbnm, respectively. The advantageous last finding is confirmed by the Rietveld refinement of the x-ray diffraction data. Furthermore, the analysis of the x-ray data of thermally deposited thin films revealed that both orthorhombic and rhombohedral phases are coexisting in the layer. The morphology of the ball milled powder was studied by scanning electron microscopy. The phase formation of the material is confirmed by Raman spectroscopy. M-H (Magnetization versus Magnetic field) curve indicates that Bi2Se3 powder has a ferromagnetic behavior. Additionally, absorbance and transmittance measurements were carried out on the obtained thermally evaporated thin films and yielded a band gap of 1.33 eV supporting the potential application of the heterogeneous rhombohedral/orthorhombic Bi2Se3 material in photovoltaics.

X-ray diffraction, Raman, and photoacoustic studies of ZnTe nanocrystals

NASA Astrophysics Data System (ADS)

Ersching, K.; Campos, C. E. M.; de Lima, J. C.; Grandi, T. A.; Souza, S. M.; da Silva, D. L.; Pizani, P. S.

2009-06-01

Nanocrystalline ZnTe was prepared by mechanical alloying. X-ray diffraction (XRD), energy dispersive spectroscopy, Raman spectroscopy, and photoacoustic absorption spectroscopy techniques were used to study the structural, chemical, optical, and thermal properties of the as-milled powder. An annealing of the mechanical alloyed sample at 590 °C for 6 h was done to investigate the optical properties in a defect-free sample (close to bulk form). The main crystalline phase formed was the zinc-blende ZnTe, but residual trigonal tellurium and hexagonal ZnO phases were also observed for both as-milled and annealed samples. The structural parameters, phase fractions, average crystallite sizes, and microstrains of all crystalline phases were obtained from Rietveld analyses of the X-ray patterns. Raman results corroborate the XRD results, showing the longitudinal optical phonons of ZnTe (even at third order) and those modes of trigonal Te. Nonradiative surface recombination and thermal bending heat transfer mechanisms were proposed from photoacoustic analysis. An increase in effective thermal diffusivity coefficient was observed after annealing and the carrier diffusion coefficient, the surface recombination velocity, and the recombination time parameters remained the same.

Cation distribution of Ni-Zn-Mn ferrite nanoparticles

NASA Astrophysics Data System (ADS)

Parvatheeswara Rao, B.; Dhanalakshmi, B.; Ramesh, S.; Subba Rao, P. S. V.

2018-06-01

Mn substituted Ni-Zn ferrite nanoparticles, Ni0.4Zn0.6-xMnxFe2O4 (x = 0.00-0.25 in steps of 0.05), using metal nitrates were prepared by sol-gel autocombustion in citric acid matrix. The samples were examined by X-ray diffraction and vibrating sample magnetometer techniques. Rietveld structural refinements using the XRD data were performed on the samples to consolidate various structural parameters like phase (spinel), crystallite size (24.86-37.43 nm), lattice constant (8.3764-8.4089 Å) etc and also to determine cation distributions based on profile matching and integrated intensity ratios. Saturation magnetization values (37.18-68.40 emu/g) were extracted from the measured M-H loops of these nanoparticles to estimate their magnetic moments. Experimental and calculated magnetic moments and lattice constants were used to confirm the derived cation distributions from Rietveld analysis. The results of these ferrite nanoparticles are discussed in terms of the compositional modifications, particle sizes and the corresponding cation distributions as a result of Mn substitutions.

The Use of Rietveld Technique to Study Phase Composition and Developments of Calcium Aluminate

NASA Astrophysics Data System (ADS)

Ridwan, I.; Asmi, D.

2008-03-01

The phase composition and development of calcium aluminates (CA, CA2, and CA6) processed by in-situ reaction sintering of Al2O3 and CaCO3 have been studied by Rietveld refinement technique. The formation of calcium aluminates is temperature-dependent. X-ray diffraction result revealed that the CA, CA2, and CA6 phases starts to develop at approximately 1000 °C, 1100 °C and 1375 °C, respectively. The relative phase compositions obtained from x-ray diffraction patterns for the α-Al2O3 phase decreased markedly with increasing temperature, i.e. from 86.0(1.1) wt% at 1000 °C to 34.7(0.4) wt% at 1400 °C. The wt% of CA decreased from 10.9(0.3)-1.9(0.2) wt% at 1100-1200 °C but disappeared at 1300 °C. The wt% of CA2 reached 36.0(0.7) wt% at 1300 °C and decreased to 18.5 (0.5) wt% at 1400 °C. The wt% CA6 increased markedly from 1375 to 1400 °C, i.e. 12.80(0.6)-47.3(0.9) wt%. The goodness of fit values is relatively low and the fluctuation in the difference plots shows a reasonable fit between the observed and the calculated plot.

Synchrotron powder X-ray diffraction and structural analysis of Eu0.5La0.5FBiS2-x Se x

NASA Astrophysics Data System (ADS)

Nagasaka, K.; Jinno, G.; Miura, O.; Miura, A.; Moriyoshi, C.; Kuroiwa, Y.; Mizuguchi, Y.

2017-07-01

Eu0.5La0.5FBiS2-x Se x is a new BiS2-based superconductor system. In Eu0.5La0.5FBiS2-x Se x , electron carriers are doped to the BiS2 layer by the substitution of Eu by La. Bulk superconductivity in this system is induced by increasing the in-plane chemical pressure, which is controlled by the Se concentration (x). In this study, we have analysed the crystal structure of Eu0.5La0.5FBiS2-x Se x using synchrotron powder diffraction and the Rietveld refinement. The precise determination of the structural parameters and thermal factors suggest that the emergence of bulk superconductivity in Eu0.5La0.5FBiS2-x Se x is achieved by the enhanced in-plane chemical pressure and the decrease in in-plane disorder.

Effect of sintering on structure and magnetic properties of Mn-doped Zn ferrite

NASA Astrophysics Data System (ADS)

Farheen, Atiya; Singh, Rajender

2018-05-01

The Mn-doped zinc ferrites, MnxZn1-xFe2O4 (x= 0 and 0.1) were prepared using co-precipitation method. The as-prepared samples were sintered at different temperatures. The x-ray diffraction pattern for all the samples confirms single phase spinel structure with Fd-3m space group. The lattice parameters have been estimated using Rietveld fitting. The magnetic moment is found to increase with Mn-doping. The magnetization increases as the sintering temperature increases up to 1200°C. The as-prepared samples are super paramagnetic, while the sintered samples are ferrimagnetic in nature.

Fatigue of LiNi0.8Co0.15Al0.05O2 in commercial Li ion batteries

NASA Astrophysics Data System (ADS)

Kleiner, Karin; Dixon, Ditty; Jakes, Peter; Melke, Julia; Yavuz, Murat; Roth, Christina; Nikolowski, Kristian; Liebau, Verena; Ehrenberg, Helmut

2015-01-01

The degradation of LiNi0.8Co0.15Al0.05O2 (LNCAO), a cathode material in lithium-ion-batteries, was studied using in situ powder diffraction and in situ Ni K edge X-ray absorption spectroscopy (XAS). The fatigued material was taken from a 7 Ah battery which was cycled for 34 weeks under defined durability conditions. Meanwhile, a cell was stored, as reference, under controlled conditions without electrochemical treatment. The fatigued LNCAO used in this study showed a capacity loss of 26% ± 9% compared to the non-cycled material. During charge and discharge the local and the overall structure of LNCAO was investigated by X-ray near edge structure (XANES) analysis, the extended X-ray absorption fine structure (EXAFS) analysis and by using Rietveld refinement of in situ powder diffraction patterns. Both powder diffraction and XAS revealed additional, rhombohedral phases which do not change with electrochemical cycling. Moreover, a phase with the lattice parameters of fully lithiated LNCAO was still present in the fatigued material at high potentials, while it was absent in the non-fatigued reference material. The coexistence of these phases is described by domains within the LNCAO particles, in correlation with the observed fatigue.

Structure, microstructure and infrared studies of Ba{sub 0.06}(Na{sub 1/2}Bi{sub 1/2}){sub 0.94}TiO{sub 3}-NaNbO{sub 3} ceramics

DOE Office of Scientific and Technical Information (OSTI.GOV)

Roy, Sumit K., E-mail: sumit.sxc13@gmail.com; Singh, S. N., E-mail: snsphyru@gmail.com; Prasad, K., E-mail: k.prasad65@gmail.com

2016-05-06

Lead-free solid solutions (1-x)Ba{sub 0.06}(Na{sub 1/2}Bi{sub 1/2}){sub 0.94}TiO{sub 3}-xNaNbO{sub 3} (0 ≤ x ≤ 1.0) were prepared by conventional ceramic fabrication technique. X-ray diffraction and Rietveld refinement analyses of these ceramics were carried out using X’Pert HighScore Plus software to determine the crystal symmetry, space group and unit cell dimensions. Rietveld refinement revealed that NaNbO{sub 3} with orthorhombic structure was completely diffused into Ba{sub 0.06}(Na{sub 1/2}Bi{sub 1/2}){sub 0.94}TiO{sub 3} lattice having the rhombohedral-tetragonal symmetry. EDS and SEM studies were carried out in order to evaluate the quality and purity of the compounds. SEM images showed a change in grain shapemore » with the increase of NaNbO{sub 3} content. FTIR spectra confirmed the formation of solid solution.« less

Rietveld refinement and dielectric properties of (Na{sub 0.5}Bi{sub 0.5}TiO{sub 3})-(Bi{sub 0.8}Ba{sub 0.2}FeO{sub 3}) ceramics

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kaswan, Kavita, E-mail: kaswan.kavita@gmail.com; Agarwal, Ashish; Sanghi, Sujata

2015-06-24

(1-x)(Na{sub 0.5}Bi{sub 0.5}TiO{sub 3})-x(Bi{sub 0.8}Ba{sub 0.2}FeO{sub 3}) lead free ceramics (NBT, NBT-BBFO; x = 0.0, 0.1 respectively) have been synthesized by conventional solid state reaction method. Crystalline phase of sintered ceramics was investigated at room temperature using X-ray diffraction. Rietveld refinement of XRD data performed by FullProf revealed that both the samples exhibited rhombohedral structure with R3c space group. Dielectric properties of these ceramics were studied at different temperatures in a wide frequency range using impedance analyzer. Dielectric constant and dielectric loss were found to be increase with increase of BBFO content. The prepared ceramics exhibit a broad maximum inmore » dielectric permittivity at 593K and dispersive permittivity at high temperatures. The NBT-BBFO sample shows a relaxor ferroelectric behavior at different frequencies.« less

Electronic structure modifications and band gap narrowing in Zn0.95V0.05O

NASA Astrophysics Data System (ADS)

Ahad, Abdul; Majid, S. S.; Rahman, F.; Shukla, D. K.; Phase, D. M.

2018-04-01

We present here, structural, optical and electronic structure studies on Zn0.95V0.05O, synthesized using solid state method. Rietveld refinement of x-ray diffraction pattern indicates no considerable change in the lattice of doped ZnO. The band gap of doped sample, as calculated by Kubelka-Munk transformed reflectance spectra, has been found reduced compared to pure ZnO. Considerable changes in absorbance in UV-Vis range is observed in doped sample. V doping induced decrease in band gap is supported by x-ray absorption spectroscopy measurements. It is experimentally confirmed that conduction band edge in Zn0.95V0.05O has shifted towards Fermi level than in pure ZnO.

Optical and magnetic properties of Co-doped CuO flower/plates/particles-like nanostructures.

PubMed

Basith, N Mohamed; Vijaya, J Judith; Kennedy, L John; Bououdina, M; Hussain, Shamima

2014-03-01

In this study, pure and Co-doped CuO nanostructures (0.5, 1.0, 1.5, and 2.0 at wt% of Co) were synthesized by microwave combustion method. The prepared samples were characterized by X-ray diffraction (XRD), high resolution scanning electron microscopy (HR-SEM), energy dispersive X-ray analysis (EDX), diffuse reflectance spectroscopy (DRS), photoluminescence (PL) spectroscopy and vibrating sample magnetometry (VSM). Powder X-ray diffraction patterns refined by the Rietveld method indicated the formation of single-phase monoclinic structure. The surface morphology and elemental analysis of Co-doped CuO nanostructures were studied by using HR-SEM and EDX. Interestingly, the morphology was found to change considerably from nanoflowers to nanoplates then to nanoparticles with the variation of Co concentration. The optical band gap calculated using DRS was found to be 2.1 eV for pure CuO and increases up to 3.4 eV with increasing cobalt content. Photoluminescence measurements also confirm these results. The magnetic measurements indicated that the obtained nanostructures were ferromagnetic at room temperature with an optimum value of saturation magnetization at 1.0 wt.% of Co-doped CuO, i.e., 970 micro emu/g.

Structural and Electronic Properties Study of Colombian Aurifer Soils by Mössbauer Spectroscopy and X-ray Diffraction

NASA Astrophysics Data System (ADS)

Bustos Rodríguez, H.; Rojas Martínez, Y.; Oyola Lozano, D.; Pérez Alcázar, G. A.; Fajardo, M.; Mojica, J.; Molano, Y. J. C.

2005-02-01

In this work a study on gold mineral samples is reported, using optical microscopy, X-ray diffraction (XRD) and Mössbauer spectroscopy (MS). The auriferous samples are from the El Diamante mine, located in Guachavez-Nariño (Colombia) and were prepared by means of polished thin sections. The petrography analysis registered the presence, in different percentages that depend on the sample, of pyrite, quartz, arsenopyirite, sphalerite, chalcopyrite and galena. The XRD analysis confirmed these findings through the calculated cell parameters. One typical Rietveld analysis showed the following weight percent of phases: 85.0% quartz, 14.5% pyrite and 0.5% sphalerite. In this sample, MS demonstrated the presence of two types of pyrite whose hyperfine parameters are δ 1 = 0.280 ± 0.002 mm/s and Δ 1 = 0.642 ± 0.002 mm/s, δ 2 = 0.379 ± 0.002 mm/s and Δ 2 = 0.613 ± 0.002 mm/s.

Investigation of La and Al substitution on the spontaneous polarization and lattice dynamics of the Pb(1-x)LaxTi(1-x)AlxO3 ceramics

NASA Astrophysics Data System (ADS)

Yadav, Arun Kumar; Verma, Anita; Kumar, Sunil; Srihari, Velaga; Sinha, A. K.; Reddy, V. Raghavendra; Liu, Shun Wei; Biring, Sajal; Sen, Somaditya

2018-03-01

The phase purity and crystal structure of Pb(1-x)LaxTi(1-x)AlxO3 (0 ≤ x ≤ 0.25) samples (synthesized via the sol-gel process) were confirmed using synchrotron x-ray powder diffraction (XRD) (wavelength, λ = 0.44573 Å). Rietveld analyses of powder x-ray diffraction data confirmed the tetragonal structure for compositions with x ≤ 0.18 and cubic structure for the sample with x = 0.25. Temperature-dependent XRD was performed to investigate the structural change from tetragonal to cubic structure phase transition. Raman spectroscopy at room temperature also confirmed this phase transition with compositions. Field emission scanning electron microscopy (FESEM) provided information about the surface morphology while an energy dispersive x-ray spectrometer attached with FESEM confirmed the chemical compositions of samples. Temperature and frequency dependent dielectric studies showed that the tetragonal to cubic phase transition decreased from 680 K to 175 K with an increase in the x from 0.03 to 0.25, respectively. This is correlated with the structural studies. Electric field dependent spontaneous polarization showed a proper ferroelectric loop for 0.06 ≤ x ≤ 0.18 belonging to a tetragonal phase, while for x ≥ 0.25, the spontaneous polarization vanishes. Bipolar strain versus electric field revealed a butterfly loop for 0.06 ≤ x ≤ 0.18 compositions. Energy storage efficiency initially increases nominally with substitution but beyond x = 0.18 enhances considerably.

Grain size dependent phase stabilities and presence of a monoclinic (Pm) phase in the morphotropic phase boundary region of (1−x)Bi(Mg{sub 1/2}Ti{sub 1/2})O{sub 3}-xPbTiO{sub 3} piezoceramics

DOE Office of Scientific and Technical Information (OSTI.GOV)

Upadhyay, Ashutosh; Singh, Akhilesh Kumar, E-mail: akhilesh-bhu@yahoo.com, E-mail: aksingh.mst@itbhu.ac.in

2015-04-14

Results of the room temperature structural studies on (1−x)Bi(Mg{sub 1/2}Ti{sub 1/2})O{sub 3}-xPbTiO{sub 3} ceramics using Rietveld analysis of the powder x-ray diffraction data in the composition range 0.28 ≤ x ≤ 0.45 are presented. The morphotropic phase boundary region exhibits coexistence of monoclinic (space group Pm) and tetragonal (space group P4 mm) phases in the composition range 0.33 ≤ x ≤ 0.40. The structure is nearly single phase monoclinic (space group Pm) in the composition range 0.28 ≤ x ≤ 0.32. The structure for the compositions with x ≥ 0.45 is found to be predominantly tetragonal with space group P4 mm. Rietveld refinement of the structure rules out the coexistence of rhombohedral and tetragonal phases inmore » the morphotropic phase boundary region reported by earlier authors. The Rietveld structure analysis for the sample x = .35 calcined at various temperatures reveals that phase fraction of the coexisting phases in the morphotropic phase boundary region varies with grain size. The structural parameters of the two coexisting phases also change slightly with changing grain size.« less

Static and Dynamical Structural Investigations of Metal-Oxide Nanocrystals by Powder X-ray Diffraction: Colloidal Tungsten Oxide as a Case Study

DOE PAGES

Caliandro, Rocco; Sibillano, Teresa; Belviso, B. Danilo; ...

2016-02-02

In this study, we have developed a general X-ray powder diffraction (XPD) methodology for the simultaneous structural and compositional characterization of inorganic nanomaterials. The approach is validated on colloidal tungsten oxide nanocrystals (WO 3-x NCs), as a model polymorphic nanoscale material system. Rod-shaped WO 3-x NCs with different crystal structure and stoichiometry are comparatively investigated under an inert atmosphere and after prolonged air exposure. An initial structural model for the as-synthesized NCs is preliminarily identified by means of Rietveld analysis against several reference crystal phases, followed by atomic pair distribution function (PDF) refinement of the best-matching candidates (static analysis). Subtlemore » stoichiometry deviations from the corresponding bulk standards are revealed. NCs exposed to air at room temperature are monitored by XPD measurements at scheduled time intervals. The static PDF analysis is complemented with an investigation into the evolution of the WO 3-x NC structure, performed by applying the modulation enhanced diffraction technique to the whole time series of XPD profiles (dynamical analysis). Prolonged contact with ambient air is found to cause an appreciable increase in the static disorder of the O atoms in the WO 3-x NC lattice, rather than a variation in stoichiometry. Finally, the time behavior of such structural change is identified on the basis of multivariate analysis.« less

Synthesis and characterization of spinel type high-power cathode materials Li MxMn2-x O4 (M=Ni, Co, Cr)

NASA Astrophysics Data System (ADS)

Yoon, Y. K.; Park, C. W.; Ahn, H. Y.; Kim, D. H.; Lee, Y. S.; Kim, J.

2007-05-01

The transition metal-doped spinel cathode materials, LiM0.5Mn1.5O4 (M=Ni. Co, Cr) were prepared by solid-state reaction. The structure and morphology of the samples were investigated by X-ray diffraction, Rietveld refinement and scanning electron microscopy (SEM). The diffraction peaks of all the samples corresponded to a single phase of cubic spinel structure with a space group Fd3m. Field-emission SEM shows octahedron like shapes and the primary particles size was between 500 nm and 2 μm. Oxidation states of Ni, Co and Cr were found to be 2+, 2+ and 3+ as revealed by X-ray photoelectron spectroscopy. During discharging, LiNi0.5Mn1.5O4 and LiCo0.5Mn1.5O4 sample shows more than 130 mAh/g between 3.5 and 5.2 V at a current density of 0.65 mA/cm2 and well developed plateau around 5 V, respectively.

Effect of cobalt doping on structural and optical properties of nanocrystalline La0.8Pb0.2CrO3 orthochromite

NASA Astrophysics Data System (ADS)

Zarrin, Naima; Shahidhusain

2018-04-01

We have synthesized nanocrystalline La0.8Pb0.2Cr1-xCoxO3 (0≤x≤0.3) through sol-gel process and studied their structural and optical properties. X-ray diffraction patterns reveal that the samples conform in the orthorhombic crystal symmetry with Pnma space group. Structural parameters are refined by Rietveld Refinement using Fullprof software. Lattice parameters and unit cell volume of doped samples are found to decrease with increase in Co doping. The optical energy band gapdecreases whereas Urbach energy increases with the increase in Co content.

Impedance spectroscopy studies on lead free Ba1-xMgx(Ti0.9Zr0.1)O3 ceramics

NASA Astrophysics Data System (ADS)

Ben Moumen, S.; Neqali, A.; Asbani, B.; Mezzane, D.; Amjoud, M.; Choukri, E.; Gagou, Y.; El Marssi, M.; Luk'yanchuk, Igor A.

2018-06-01

Ba1-xMgx(Ti0.9Zr0.1)O3 (x = 0.01 and 0.02) ceramics were prepared using the conventional solid state reaction. Rietveld refinement performed on X-ray diffraction patterns indicates that the samples are tetragonal crystal structure with P4mm space group. By increasing Mg content from 1 to 2% the unit cell volume decreased. Likewise, the grains size is greatly reduced from 10 μm to 4 μm. The temperature dependence of dielectric constants at different frequencies exhibited typical relaxor ferroelectric characteristic, with sensitive dependence in frequency and temperature for ac conductivity. The obtained activation energy values were correlated to the proposed conduction mechanisms.

Structural, vibrational and dielectric studies of (0.95)Pb(Zr{sub x}Ti{sub 1−x})O{sub 3}-(0.05)BiFeO{sub 3} nanoceramics

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sharma, Subhash, E-mail: rk.dwivedi@jiit.ac.in; Singh, Vikash, E-mail: rk.dwivedi@jiit.ac.in; Dwivedi, R. K., E-mail: rk.dwivedi@jiit.ac.in

2014-04-24

(0.95)Pb(Zr{sub x}Ti{sub 1−x})O{sub 3}-(0.05)BiFeO{sub 3} nanoceramics with x=0.51, 0.53 and 0.55 were synthesized by sol-gel route. Rietveld refined X-ray powder diffraction pattern of the samples confirm the single phase formation of compounds with tetragonal structure (P4mm). FT-IR studies revealed that slight shift of phonon modes towards the lower wave number and increase in the bond length with increasing Zr{sup 4+} concentration. Room temperature dielectric properties of system revealed that relaxor characteristics of these samples. Ferroelectric hysteresis curve shows the decrease in polarization values with Zr concentration.

Understanding microstrain anisotropy in yttrium oxide synthesized by sol-gel route

NASA Astrophysics Data System (ADS)

Murugesan, S.; Thirumurugesan, R.; Parameswaran, P.

2018-04-01

Yttrium oxide was synthesized by wet chemical route and calcined at various temperatures. On x-ray diffraction analysis of the material using Williamson-Hall analysis followed by Rietveld analysis indicates that the powder exists in nano crystallite size with lattice strain. The spherical harmonics analysis model of microstrain indicates the presence of strain anisotropy. The change in crystal structure lattice parameter, atomic coordinates of Y, O in yttria and the bond length analysis of the calcined powder reveals the presence of oxygen vacancies in the system.

Synthesis of MAX Phases in the Hf-Al-C System.

PubMed

Lapauw, Thomas; Tunca, Bensu; Cabioc'h, Thierry; Lu, Jun; Persson, Per O Å; Lambrinou, Konstantina; Vleugels, Jozef

2016-11-07

For the first time, MAX phases in the Hf-Al-C system were experimentally synthesized using reactive hot pressing. HfC was observed as the main competing phase. The lattice parameters of Hf 2 AlC and Hf 3 AlC 2 were determined by Rietveld refinement based on the X-ray diffraction data. The atomic stacking sequence was revealed by high-resolution scanning transmission electron microscopy. Mixtures of 211 and 312 stacking were observed within the same grain, including 523 layers. This transition in atomic structure is discussed.

Evolution of structural and transport properties in Y-doped double perovskite Sr2FeIrO6

NASA Astrophysics Data System (ADS)

Kharkwal, K. C.; Pramanik, A. K.

2018-05-01

The structural and transport properties of Yttrium doped double perovskite Sr2FeIrO6 have been investigated. Structural properties have been investigated by means of x-ray diffraction measurement and Rietveld analysis. Structural transition has not been observed although lattice parameters evolve with the Yttrium doping. All samples have been found to be insulating over the whole temperature range where the resistivity increases with doping. This increase in resistivity with doping may be due to the change in charge state of transition metal.

Infrared and Raman spectroscopy and DFT calculations of DL amino acids: Valine and lysine hydrochloride

NASA Astrophysics Data System (ADS)

Paiva, F. M.; Batista, J. C.; Rêgo, F. S. C.; Lima, J. A.; Freire, P. T. C.; Melo, F. E. A.; Mendes Filho, J.; de Menezes, A. S.; Nogueira, C. E. S.

2017-01-01

Single crystals of DL-valine and DL-lysine hydrochloride were grown by slow evaporation method and the crystallographic structure were confirmed by X-ray diffraction experiment and Rietveld method. These two crystals have been studied by Raman spectroscopy in the 25-3600 cm-1 spectral range and by infrared spectroscopy through the interval 375-4000 cm-1 at room temperature. Experimental and theoretical vibrational spectra were compared and a complete analysis of the modes was done in terms of the Potential Energy Distribution (PED).

Study the oxidation kinetics of uranium using XRD and Rietveld method

NASA Astrophysics Data System (ADS)

Zhang, Yanzhi; Guan, Weijun; Wang, Qinguo; Wang, Xiaolin; Lai, Xinchun; Shuai, Maobing

2010-03-01

The surface oxidation of uranium metal has been studied by X-ray diffraction (XRD) and Rietveld method in the range of 50~300°C in air. The oxidation processes are analyzed by XRD to determine the extent of surface oxidation and the oxide structure. The dynamics expression for the formation of UO2 was derived. At the beginning, the dynamic expression was nonlinear, but switched to linear subsequently for uranium in air and humid oxygen. That is, the growth kinetics of UO2 can be divided into two stages: nonlinear portion and linear portion. Using the kinetic data of linear portion, the activation energy of reaction between uranium and air was calculated about 46.0 kJ/mol. However the content of oxide as a function of time was linear in humid helium ambience. Contrast the dynamics results, it prove that the absence of oxygen would accelerate the corrosion rate of uranium in the humid gas. We can find that the XRD and Rietveld method are a useful convenient method to estimate the kinetics and thermodynamics of solid-gas reaction.

Structure Evolution of BaTiO3 on Co Doping: X-ray diffraction and Raman study

NASA Astrophysics Data System (ADS)

Mansuri, Amantulla; Mishra, Ashutosh

2016-10-01

In the present study, we have synthesize polycrystalline samples of BaTi1-xCoxO3 (x = 0, 0.05 and 0.1) with standard solid state reaction technique. The obtained samples are characterized by X-ray diffraction (XRD) and Raman spectroscopy. The detail structural analysis has been performed by Rietveld refinement using Fullprof program. The structural analysis reveal the samples are chemical pure and crystallize in tetragonal phase with space group Pm3m. We observe an increase in lattice parameters which results due to substitution of Co2+ with large ionic radii (0.9) for smaller ionic radii (0.6) Ti4+. Moreover peak at 45.5° shift to 45° on Co doping, which is due to structure phase transition from tetragonal to cubic. Raman study infers that the intensity of characteristic peaks decreases and linewidth increases with Co doping. The bands linked with the tetragonal structure (307 cm1) decreased due to the tetragonal-towards-cubic phase transition with Co doping. Our structural study reveals the expansion of BTO unit cell and tetragonal-to-cubic phase transformation takes place, results from different characterization techniques are conclusive and show structural evolution with Co doping.

Structure refinement for tantalum nitrides nanocrystals with various morphologies

DOE Office of Scientific and Technical Information (OSTI.GOV)

Liu, Lianyun; School of Science, Beijing Jiaotong University, 3 Shang Yuan Cun, Haidian District, Beijing 100044; Huang, Kai

2012-07-15

Graphical abstract: Tantalum nitrides nanocrystals with various phases and morphologies for the first time have been synthesized through homogenous sodium reduction under low temperature with the subsequent annealing process under high vacuum. Highlights: ► The spherical TaN, cuboidal TaN{sub 0.83} and TaN{sub 0.5} nanocrystals have been synthesized through homogenous sodium reduction under low temperature with the subsequent annealing process under high vacuum. ► The crystal structures of different tantalum nitrides were determined by Rietveld refinement on the X-ray diffraction data and the examinations of electron microcopies. ► The specific surface area of the tantalum nitrides powders was around 10 m{supmore » 2} g{sup −1}. ► Tantalum nitrides powders could be suitable for capacitor with high specific capacitance. -- Abstract: Tantalum nitrides (TaN{sub x}) nanocrystals with different phase and morphology have been synthesized through homogenous sodium reduction under low temperature with the subsequent annealing process under high vacuum. The crystal structures of tantalum nitrides were determined by Rietveld refinement based on the X-ray diffraction data. The morphologies of various tantalum nitrides nanocrystals in high quality were analyzed through the electron microcopies examinations. The spherical TaN nanoparticles, cuboidal TaN{sub 0.83} and TaN{sub 0.5} nanocrystals have been selectively prepared at different annealing temperatures. In addition, the specific surface areas of the tantalum nitrides nanocrystals measured by BET method were around 9.87–11.64 m{sup 2} g{sup −1}, indicating that such nano-sized tantalum nitrides could be suitable for capacitor with high specific capacitance.« less

Thermally induced phase transformation in multi-phase iron oxide nanoparticles on vacuum annealing

NASA Astrophysics Data System (ADS)

Anupama, A. V.; Keune, W.; Sahoo, B.

2017-10-01

The evolution of magnetic phases in multi-phase iron oxide nanoparticles, synthesized via the transferred arc plasma induced gas phase condensation method, was investigated by X-ray diffraction, vibrating sample magnetometry and 57Fe Mössbauer spectroscopy. The particles are proposed to be consisting of three different iron oxide phases: α-Fe2O3, γ-Fe2O3 and Fe3O4. These nanoparticles were exposed to high temperature (∼935 K) under vacuum (10-3 mbar He pressure), and the thermally induced phase transformations were investigated. The Rietveld refinement of the X-ray diffraction data corroborates the least-squares fitting of the transmission Mössbauer spectra in confirming the presence of Fe3O4, γ-Fe2O3 and α-Fe2O3 phases before the thermal treatment, while only Fe3O4 and α-Fe2O3 phases exist after thermal treatment. On thermal annealing in vacuum, conversion from γ-Fe2O3 to Fe3O4 and α-Fe2O3 was observed. Interestingly, we have observed a phase transformation occurring in the temperature range ∼498 K-538 K, which is strikingly lower than the phase transformation temperature of γ-Fe2O3 to α-Fe2O3 (573-623 K) in air. Combining the results of Rietveld refinement of X-ray diffraction patterns and Mössbauer spectroscopy, we have attributed this phase transformation to the phase conversion of a metastable "defected and strained" d-Fe3O4 phase, present in the as-prepared sample, to the α-Fe2O3 phase. Stabilization of the phases by controlling the phase transformations during the use of different iron-oxide nanoparticles is the key factor to select them for a particular application. Our investigation provides insight into the effect of temperature and chemical nature of the environment, which are the primary factors governing the phase stability, suitability and longevity of the iron oxide nanomaterials prepared by the gas-phase condensation method for various applications.

Crystal structure and X-ray photoemission spectroscopic study of A{sub 2}LaMO{sub 6} [A=Ba, Ca; M=Nb, Ta

DOE Office of Scientific and Technical Information (OSTI.GOV)

Dutta, Alo, E-mail: alo_dutta@yahoo.com; Saha, Sujoy; Kumari, Premlata

2015-09-15

The X-ray photoemission spectroscopic (XPS) study of the double perovskite oxides A{sub 2}LaMO{sub 6} [A=Ba, Ca; M=Nb, Ta] synthesized by the solid-state reaction technique has been carried out to investigate the nature of the chemical state of the constituent ions and the bonding between them. The Rietveld refinement of the X-ray diffraction patterns suggests the monoclinic crystal structure of all the materials at room temperature. The negative and positive chemical shifts of the core level XPS spectrum of O-1s and Nb-3d{sub 3/2}/Ta-4f{sub 5/2} respectively suggest the covalent bonding between Nb/Ta cations and O ion. The change of the bonding strengthmore » between the anion and the cations from one material to another has been analyzed. The vibrational property of the materials is investigated using the room temperature Raman spectra. A large covalency of Ta-based compound than Nb compound is confirmed from the relative shifting of the Raman modes of the materials. - Graphical abstract: Crystal structure of two perovskite oxides CLN and CLT is investigated. XPS study confirms the two different co-ordination environments of Ca and covalent bonding between B-site cations and O-ion. - Highlights: • Ordered perovskite structure obtained by Rietveld refinement of XRD patterns. • Study of nature of chemical bonding by X-ray photoemission spectroscopy. • Opposite chemical shift of d-states of Nb/Ta with respect to O. • Covalent bonding between d-states of Nb/Ta and O. • Relative Raman shifts of CLN and CLT substantiate the more covalent character of Ta than Nb.« less

Applying the X-ray diffraction analysis for estimating the height and width of nanorods in low symmetry crystal multiphase materials

NASA Astrophysics Data System (ADS)

Mokhtari, Ali; Soleimanian, Vishtasb; Dehkordi, Hamed Aleebrahim; Dastafkan, Kamran

2017-11-01

In this work the potential of Rietveld refinement procedure is used to study the shape and size of non-spherical nanocrystallites. The main advantages of this approach are that not only it can successfully extend to all nanomaterials with different crystal symmetries but also it can evaluate the various phases of multiple materials comparing to electron microscopy methods. Therefore, between seven crystal systems, the formulation of monoclinic and hexagonal crystals is developed. This procedure is applied for the mixture of sodium carbonate and zinc oxide nanocrystallites at different fractions of doped gadolinium oxide. It is found that the crystallites of sodium carbonate and zinc oxide have the rod and ellipsoidal shapes, respectively. The microstructure results are compared with the results of scanning electron microscopy imaging. Good agreement is achieved between the results of scanning electron microscopy and Rietveld methods.

Rietveld refinement, dielectric and magnetic properties of Nb modified Bi0.80Ba0.20FeO3 ceramic

NASA Astrophysics Data System (ADS)

Jangra, Sandhaya; Sanghi, Sujata; Agarwal, Ashish; Rangi, Manisha

2018-05-01

Bi0.80Ba0.20Fe0.95Nb0.05O3 ceramic has been prepared via conventional solid state reaction method. Structure analysis was carried out by X-ray diffraction (XRD) technique at room temperature. XRD pattern confirmed the crystalline nature of prepared sample. Rietveld analysis used for further structural investigations and confirmed the existence of rhombohedral symmetry (R3c space group). The dielectric response shows dispersion at lower frequency range and becomes frequency independent at high frequency. The approximation of conduction mechanism is determined by the temperature dependent behavior of frequency exponent `s'. Fitting results suggests the applicability of small polaron conduction mechanism at lower temperatures and CBH model at higher temperature. Room temperature magnetic measurements give the evidence of significant enhancement in magnetic properties with remanent magnetization (Mr = 0.1218 emu/g) and coercive field (Hc = 3.5342 kOe).

Combined PDF and Rietveld studies of ADORable zeolites and the disordered intermediate IPC-1P.

PubMed

Morris, Samuel A; Wheatley, Paul S; Položij, Miroslav; Nachtigall, Petr; Eliášová, Pavla; Čejka, Jiří; Lucas, Tim C; Hriljac, Joseph A; Pinar, Ana B; Morris, Russell E

2016-09-28

The disordered intermediate of the ADORable zeolite UTL has been structurally confirmed using the pair distribution function (PDF) technique. The intermediate, IPC-1P, is a disordered layered compound formed by the hydrolysis of UTL in 0.1 M hydrochloric acid solution. Its structure is unsolvable by traditional X-ray diffraction techniques. The PDF technique was first benchmarked against high-quality synchrotron Rietveld refinements of IPC-2 (OKO) and IPC-4 (PCR) - two end products of IPC-1P condensation that share very similar structural features. An IPC-1P starting model derived from density functional theory was used for the PDF refinement, which yielded a final fit of Rw = 18% and a geometrically reasonable structure. This confirms the layers do stay intact throughout the ADOR process and shows PDF is a viable technique for layered zeolite structure determination.

Raman effect, structural and dielectric properties of sol-gel synthesized polycrystalline GaFe{sub 1-x}Zr{sub x}O{sub 3} (0≤x≤0.15)

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kumar, Rajeev, E-mail: rajeevgiitk@gmail.com; Mall, Ashish Kumar; Gupta, Rajeev

2016-05-23

Polycrystalline ceramic samples of Zirconium (Zr)-doped GaFeO{sub 3} (GaFe{sub 1-x}Zr{sub x}O{sub 3}) were studied using powder X-ray diffraction, complex impedance spectroscopy and Raman spectroscopic measurements to understand the effect of Zr doping on the structural and dielectric properties. The samples with varying Zr content were prepared by Sol-Gel method. X-ray data analysis confirmed the formation of single phase material without formation of any secondary phases and all are crystallized in Pc2{sub 1}n orthorhombic symmetry. Rietveld refinement of the X-ray data suggested an increase in the lattice constants due to size effect and decreases on x = 0.15 due to themore » effect of change in interplanner spacing. Impedance studies on the samples showed that the dielectric constant increases while loss tangent decrease as the Zr content increases. Raman scattering on GaFe{sub 1-x}Zr{sub x}O{sub 3} (x = 0, 0.05, 0.10, & 0.15) used to understand the composition dependence on phonon modes at room temperature. On Zr doping, Raman modes frequencies shifts to lower energies consistent with the X-ray data.« less

Application of x-ray absorption fine structure (XAFS) to local-order analysis in Fe-Cr maghemite-like materials

DOE Office of Scientific and Technical Information (OSTI.GOV)

Montero-Cabrera, M. E., E-mail: elena.montero@cimav.edu.mx; Fuentes-Cobas, L. E.; Macías-Ríos, E.

2015-07-23

The maghemite-like oxide system γ-Fe{sub 2-x}Cr{sub x}O{sub 3} (x=0.75, 1 and 1.25) was studied by X-ray absorption fine structure (XAFS) and by synchrotron radiation X-ray diffraction (XRD). Measurements were performed at the Stanford Synchrotron Radiation Lightsource at room temperature, at beamlines 2-1, 2-3 and 4-3. High-resolution XRD patterns were processed by means of the Rietveld method. In cases of atoms being neighbors in the Periodic Table, the order/disorder degree of the considered solutions is indiscernible by “normal” (absence of “anomalous scattering”) diffraction experiments. Thus, maghemite-like materials were investigated by XAFS in both Fe and Cr K-edges to clarify, via short-rangemore » structure characterization, the local ordering of the investigated system. Athena and Artemis graphic user interfaces for IFEFFIT and FEFF8.4 codes were employed for XAFS spectra interpretation. Pre-edge decomposition and theoretical modeling of X-ray absorption near edge structure (XANES) transitions were performed. By analysis of the Cr K-edge XANES, it has been confirmed that Cr is located in an octahedral environment. Fitting of the extended X-ray absorption fine structure (EXAFS) spectra was performed under the consideration that the central atom of Fe is allowed to occupy octa- and tetrahedral positions, while Cr occupies only octahedral ones. Coordination number of neighboring atoms, interatomic distances and their quadratic deviation average were determined for x=1, by fitting simultaneously the EXAFS spectra of both Fe and Cr K-edges. The results of fitting the experimental spectra with theoretical standards showed that the cation vacancies tend to follow a regular pattern within the structure of the iron-chromium maghemite (FeCrO{sub 3})« less

Ferri-magnetic order in Mn induced spinel Co3-xMnxO4 (0.1≤x≤1.0) ceramic compositions

NASA Astrophysics Data System (ADS)

Meena, P. L.; Sreenivas, K.; Singh, M. R.; Kumar, Ashok; Singh, S. P.; Kumar, Ravi

2016-04-01

We report structural and magnetic properties of spinel Co3-xMnxO4 (x=0.1-1.0) synthesized by solid state reaction technique. Rietveld refinement analysis of X-ray diffraction (XRD) data, revealed the formation of polycrystalline single phase Co3-xMnxO4 without any significant structural change in cubic crystal symmetry with Mn substitution, except change in lattice parameter. Temperature dependent magnetization data show changes in magnetic ordering temperature, indicating formation of antiferromagnetic (AFM) and ferrimagnetic (FM) phase at low Mn concentration (x≤0.3) and well-defined FM phase at high Mn concentration (x≥0.5). The isothermal magnetization records established an AFM/FM mixed phase for composition ranging 0.10.5.

Detecting Nanophase Weathering Products with CheMin: Reference Intensity Ratios of Allophane, Aluminosilicate Gel, and Ferrihydrite

NASA Technical Reports Server (NTRS)

Rampe, E. B.; Bish, D. L.; Chipera, S. J.; Morris, R. V.; Achilles, C. N.; Ming, D W.; Blake, D. F.; Anderson, R. C.; Bristow, T. F.; Crisp, A.;

Crystal structure of carnidazole form II from synchrotron X-ray powder diffraction: structural comparison with form I, the hydrated form and the low energy conformations in vacuo.

PubMed

de Armas, Héctor Novoa; Peeters, Oswald M; Blaton, Norbert; Van den Mooter, Guy; De Ridder, Dirk J A; Schenk, Henk

2006-10-01

The crystal structure of carnidazole form II, O-methyl [2-(2-methyl-5-nitro-1H-imidazole-1-yl)ethyl]thiocarbamate, has been determined using synchrotron X-ray powder diffraction in combination with simulated annealing and whole profile pattern matching, and refined by the Rietveld method. For structure solution, 12 degrees of freedom were defined: one motion group and six torsions. Form II crystallizes in space group P2(1)/n, Z=4, with unit cell parameters after Rietveld refinement: a=13.915(4), b=8.095(2), c=10.649(3) A, beta=110.83(1) degrees, and V=1121.1(5) A3. The two polymorphic forms, as well as the hydrate, crystallize in the monoclinic space group P2(1)/n having four molecules in the cell. In form II, the molecules are held together by forming two infinite zig-zag chains via hydrogen bonds of the type N--H...N, the same pattern as in form I. A conformational study of carnidazole, at semiempirical PM3 level, was performed using stochastic approaches based on modification of the flexible torsion angles. The values of the torsion angles for the molecules of the two polymorphic forms and the hydrate of carnidazole are compared to those obtained from the conformational search. Form I and form II are enantiotropic polymorphic pairs this agrees with the fact that the two forms are conformational polymorphs. Copyright (c) 2006 Wiley-Liss, Inc. and the American Pharmacists Association

Influence of Mn doping on structural, dielectric and optical properties of neodymium orthoferrite

NASA Astrophysics Data System (ADS)

Somvanshi, Anand; Manzoor, Samiya; Husain, Shahid

2018-05-01

We report the study of structural, dielectric and optical properties of nanocrystalline samples of NdFe1-xMnxO3 (x=0, 0.1 and 0.2) synthesized using solid state reaction route. X-ray diffraction (XRD) patterns are recorded to confirm phase purity. These samples conform in orthorhombic crystal symmetry with Pbnm space group. The lattice parameters are determined using Rietveld refinement. The crystallite size is calculated using Scherrer formula and that is found to lie in the range of 40-50 nm. The dielectric constant (ɛ') decreases with the increase in frequency as well as Mn doping concentration. Energy bandgap (Eg) as determined using UV-Vis. absorption spectra, is found to decrease with the increase in Mn doping.

Analysis and interpretation of diffraction data from complex, anisotropic materials

NASA Astrophysics Data System (ADS)

Tutuncu, Goknur

Most materials are elastically anisotropic and exhibit additional anisotropy beyond elastic deformation. For instance, in ferroelectric materials the main inelastic deformation mode is via domains, which are highly anisotropic crystallographic features. To quantify this anisotropy of ferroelectrics, advanced X-ray and neutron diffraction methods were employed. Extensive sets of data were collected from tetragonal BaTiO3, PZT and other ferroelectric ceramics. Data analysis was challenging due to the complex constitutive behavior of these materials. To quantify the elastic strain and texture evolution in ferroelectrics under loading, a number of data analysis techniques such as the single peak and Rietveld methods were used and their advantages and disadvantages compared. It was observed that the single peak analysis fails at low peak intensities especially after domain switching while the Rietveld method does not account for lattice strain anisotropy although it overcomes the low intensity problem via whole pattern analysis. To better account for strain anisotropy the constant stress (Reuss) approximation was employed within the Rietveld method and new formulations to estimate lattice strain were proposed. Along the way, new approaches for handling highly anisotropic lattice strain data were also developed and applied. All of the ceramics studied exhibited significant changes in their crystallographic texture after loading indicating non-180° domain switching. For a full interpretation of domain switching the spherical harmonics method was employed in Rietveld. A procedure for simultaneous refinement of multiple data sets was established for a complete texture analysis. To further interpret diffraction data, a solid mechanics model based on the self-consistent approach was used in calculating lattice strain and texture evolution during the loading of a polycrystalline ferroelectric. The model estimates both the macroscopic average response of a specimen and its hkl-dependent lattice strains for different reflections. It also tracks the number of grains (or domains) contributing to each reflection and allows for domain switching. The agreement between the model and experimental data was found to be satisfactory.

Studies on densification, mechanical, micro-structural and structure–properties relationship of magnesium aluminate spinel refractory aggregates prepared from Indian magnesite

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ghosh, Chandrima; Ghosh, Arup; Haldar, Manas Kamal, E-mail: manashaldar@cgcri.res.in

The present work intends to study the development of magnesium aluminate spinel aggregates from Indian magnesite in a single firing stage. The raw magnesite has been evaluated in terms of chemical analysis, differential thermal analysis, thermogravimetric analysis, infrared spectroscopy, and X-ray diffraction. The experimental batch containing Indian magnesite and calcined alumina has been sintered in the temperature range of 1550 °C–1700 °C. The sintered material has been characterized in terms of physico-chemical properties like bulk density, apparent porosity, true density, relative density and thermo-mechanical/mechanical properties like hot modulus of rupture, thermal shock resistance, cold modulus of rupture and structural propertiesmore » by X-ray diffraction in terms of phase identification and evaluation of crystal structure parameters of corresponding phases by Rietveld analysis. The microstructures developed at different temperatures have been analyzed by field emission scanning electron microscope study and compositional analysis of the developed phase has been carried out by energy dispersive X-ray study. - Highlights: • The studies have been done to characterize the developed magnesium aluminate spinel. • The studies reveal correlation between refractory behavior of spinel and developed microstructures. • The studies show the values of lattice parameters of developed phases.« less

Defect Chemistry of " BaCuO2" I. Oxygen Non -Stoichiometry, Cation Molecularity and X-ray Diffraction Determinations

NASA Astrophysics Data System (ADS)

Spinolo, G.; Anselmi-Tamburini, U.; Arimondi, M.; Ghigna, P.; Flor, G.

1995-11-01

"BaCuO2" is the key intermediate in the synthesis of the Ba2YCu3O7-δ superconductor. Its very complex crystal structure is able to accommodate a large change in oxygen content. Oxygen non-stoichiometry of "BaCuO2" materials with 1:1 and 88:90 (Ba :Cu) molecularity has been investigated by polythermal X-ray powder diffraction coupled with isobaric-isothermal gravimetry determinations under different temperature and oxygen partial pressure conditions [300≤ T≤ 820 °C, 1 ≥ P(O2) ≥ 3 • 10-3 atm]. The 1:1 composition does not give well reproducible results, thus suggesting its polyphasic nature, at least in part of the investigated range. The results for the 88:90 ≅ 0.98 (Ba :Cu) composi­ tion are well reproducible and show that the material is single phase. Ba0.98CuO1.98 + δ is oxygen over-stoichiometric in the whole investigated [T, P(O2)] range, with a maximum value δ˜0.21. A Rietveld X-ray profile fitting is in agreement with previous single-crystal data. The trend of δ vs. P(O2) is consistent with the presence of oxygen interstitial defects on (possibly different) crystallographic sites.

Low-temperature synthesis and structural properties of ferroelectric K 3WO 3F 3 elpasolite

NASA Astrophysics Data System (ADS)

Atuchin, V. V.; Gavrilova, T. A.; Kesler, V. G.; Molokeev, M. S.; Aleksandrov, K. S.

2010-06-01

Low-temperature ferroelectric G2 polymorph of K 3WO 3F 3 has been prepared by chemical synthesis. Structural and chemical properties of the final product have been evaluated with X-ray powder diffraction (XRD), scanning electron microscopy (SEM) and X-ray photoelectron spectroscopy (XPS). Structure parameters of G2-K 3WO 3F 3 are refined by the Rietveld method from XRD data measured at room temperature (space group Cm, Z = 2, a = 8.7350(3) Å, b = 8.6808(5) Å, c = 6.1581(3) Å, β = 135.124(3) Å, V = 329.46(3) Å 3; RB = 2.47%). Partial ordering of oxygen and fluorine atoms has been found over anion positions. Mechanism of ferroelectric phase transition in A 2BMO 3F 3 oxyfluorides is discussed.

Quantitative Phase Analysis of Plasma-Treated High-Silica Materials

NASA Astrophysics Data System (ADS)

Kosmachev, P. V.; Abzaev, Yu. A.; Vlasov, V. A.

2018-06-01

The paper presents the X-ray diffraction (XRD) analysis of the crystal structure of SiO2 in two modifications, namely quartzite and quartz sand before and after plasma treatment. Plasma treatment enables the raw material to melt and evaporate after which the material quenches and condenses to form nanoparticles. The Rietveld refinement method is used to identify the lattice parameters of SiO2 phases. It is found that after plasma treatment SiO2 oxides are in the amorphous state, which are modeled within the microcanonical ensemble. Experiments show that amorphous phases are stable, and model X-ray reflection intensities approximate the experimental XRD patterns with fine precision. Within the modeling, full information is obtained for SiO2 crystalline and amorphous phases, which includes atom arrangement, structural parameters, atomic population of silicon and oxygen atoms in lattice sites.

First-principles prediction of low-energy structures for AlH3

NASA Astrophysics Data System (ADS)

Sun, Shoutian; Ke, Xuezhi; Chen, Changfeng; Tanaka, Isao

2009-01-01

We report density-functional calculations that predict ten different low-energy structures for aluminum hydride AlH3 with space groups Pnma , P6/mmm , I4/mcm , P4/mbm , P4/nmm , Pm3¯m , P21/m , P21/c , Pbcm , and P4/n . Phonon calculations within harmonic approximation reveal unstable modes in the P6/mmm , I4/mcm , P4/mbm , P4/nmm , Pm3¯m , P21/m , and P21/c structures, indicating that they are unstable at low temperatures. The calculations show that the thermodynamic stabilities for AlH3 with space groups Pnma , Pbcm , and P4/n are overall close to the existing α - and γ-AlH3 . From x-ray powder-diffraction patterns, the simulated main-peak positions for AlH3 (P4/n) are in good agreement with experimental δ-AlH3 . A full Rietveld analysis reveals that the fitting space groups R3¯c , Pbcm , and Pnma to the experimental x-ray powder-diffraction pattern of α-AlH3 gives almost the same satisfactory result.

Structural, vibrational and luminescence properties of the (1−x)CaWO{sub 4}−xCdWO{sub 4} system

DOE Office of Scientific and Technical Information (OSTI.GOV)

Taoufyq, A.; Laboratoire Matériaux et Environnement LME, Faculté des Sciences, Université Ibn Zohr, BP 8106, Cité Dakhla, Agadir, Maroc; CEA/DEN, Département d’Études des Réacteurs, Laboratoire Dosimétrie Capteurs Instrumentation, CEA Cadarache, 13108, Saint-Paul-lez-Durance

2014-11-15

In the present work, we investigate the structural, microstructural, vibrational and luminescence properties of the system (1−x)CaWO{sub 4}−xCdWO{sub 4} with x ranging between 0 and 1. Polycrystalline samples were elaborated using a coprecipitation technique followed by thermal treatment at 1000 °C. The samples were then characterized using X-ray diffraction, scanning electron microscopy, Raman spectroscopy and luminescence analyses. X-ray diffraction profile analyses using Rietveld method showed that two kinds of solid solutions Ca{sub 1−x}Cd{sub x}WO{sub 4} having scheelite and wolframite structures, with respectively tetragonal and monoclinic crystal cells, were observed, with a biphasic system for compositions x=0.6 and 0.7. The scanningmore » electron microscopy experiments showed a complex evolution of morphologies and crystallite sizes as x increased. The vibration modes of Raman spectra were characteristic of composition-dependent disordered solid solutions with decreasing wavenumbers as x increased. Luminescence experiments were performed under UV-laser light irradiation. The energies of emission bands increased linearly with cadmium composition x. The integrated intensity of luminescence reached a maximum value for the substituted wolframite phase with composition x=0.8. - Graphical abstract: Luminescence on UV excitation (364.5 nm) of (1−x)CaWO{sub 4−x}CdWO{sub 4} system, elaborated from coprecipitation technique at 1000 °C, with 0« less

Synthesis, structure and magnetic properties of Sr{sub 2}Fe{sub 1-x}Ga{sub x}MoO{sub 6} (0 {<=} x {<=} 0.6) double perovskites

DOE Office of Scientific and Technical Information (OSTI.GOV)

Azad, Abul K., E-mail: aka7@st-andrews.ac.uk; Khan, Abdullah; Eriksson, Sten-G.

2009-12-15

Polycrystalline Sr{sub 2}Fe{sub 1-x}Ga{sub x}MoO{sub 6} (0 {<=} x {<=} 0.6) materials have been synthesized by solid state reaction method and studied by neutron powder diffraction (NPD) and magnetization measurements. Rietveld analysis of the temperature dependent NPD data shows that the compounds crystallize in the tetragonal symmetry in the space group I4/m. The anti-site (AS) defects concentration increases with Ga doping, giving rise to highly B-site disordered materials. Ga doping at the Fe-site decreases the cell volume. The evolution of bond lengths and the cation oxidation states was determined from the Rietveld refinement data. The saturation magnetization and Curie temperaturemore » decreased with the increasing Ga content in the samples. Low temperature neutron diffraction data analysis and magnetization measurements confirm the magnetic interaction as ferrimagnetic in the sample.« less

Structure refinement of Zn and Pr-doped Y-Ba-Cu-oxides

NASA Astrophysics Data System (ADS)

Naik, M. S.; Sarode, P. R.; Priolkar, K. R.; Prabhu, R. B.

2018-05-01

Superconducting compounds of composition Y0.9 Pr0.1Ba2 [Cu1-yZny]3O7-δ (0 ≤ y ≤ 0.10) have been synthesized. The structure of these materials has been studied using powder X-ray diffraction technique and refinement has been carried out by using Rietveld refinement procedure. It has been shown that all these compounds crystallize in orthorhombic structure with slight change in c parameter. Increase of parameter O(2) and decrease of parameter O(3)suggest the changes in the Cu-O2 plane of these orthorhombic materials on Zn substitution.

Applied Crystallography - Proceedings of the XVth Conference

NASA Astrophysics Data System (ADS)

Morawiec, H.; Ströż, D.

1993-06-01

The Table of Contents for the full book PDF is as follows: * Foreword * The International Centre for Diffraction Data and Its Future Developments * The Rietveld Method - A Historical Perspective * Real Structure in Quantitative Powder Diffraction Phase Analysis * Neutron Focusing Optics in Applied Crystallography * The Crystal Structures of Oxygen Deficient Rare Earth Oxides * Short-Range Order in Layer-Structured Ba1-xSrxBi2Nb2O9 Ferroelectrics * Radial Distribution Function as a Tool of Structural Studies on Noncrystalline Materials * Determination of Radial Distribution Function (RDF) of Electrodeposited Cu-Cd Alloys After Annealing * Spheres Packing as a Factor Describing the Local Environment and Structure Stability * X-Ray Stress Measurement of Samples Combined with Diffraction Line Analysis * Phase Stability and Martensitic Transformation in Cu-Zn and Cu-Zn-Al Single Crystals * Order, Defects, Precipitates and the Martensitic Transformation in β Cu-Zn-Al * Effect of γ Precipitates on the Martensitic Transformation in Cu-Zn-Al Alloys * Phase Transitions and Shape Memory Effect in a Thermomechanically Treated NiTi Alloy * Structure of Martensite and Bainite in CuAlMn Alloys * Glass-Ceramics * Mechanism of Texture Formation at the Rolling of Low Stacking Fault Energy Metals and Alloys * Shear Texture of Zinc and the Conditions of Its Occuring * The Development of Texture of ZnAlMg Sheets Depending on Deformation Geometry * Texture Stability of the D.S. NiAlMoCrTi Alloy After Heat Treatment * X-Ray Diffraction Method for Controlling of Texture Evolution in Layers * Texture and Lattice Imperfections Study of Some Low Alloyed Copper Alloys * Selected Examples of the Calculation of the Orientation Distribution Function for Low Crystal and Sample Symmetries * Automatical X-Ray Quantitative Phase Analysis * Application of a PC Computer for Crystallographic Calculations * Electron Diffraction Analysis using a Personal Computer * CA.R.INE Crystallography Version 2.1-1992 * PC-MINREF: The Computer Program Package for Neutron Refinement of Incommensurate Multiphase Crystal and Magnetic Structures on IBM PC Computers * Possibilities of Deflections from Stoichiometry Investigation for Phases of b1-b37 Structure by X-Ray Method * A Computer Program: “Measurement of Elastic Constants of Phases in Nontextured Polycrystalline Materials by X-Ray Method” * Crystallite Sizes and Lattice Strains of Hydrogenatid Tungsten Carbid Powder * The Bragg-Case Images of Dislocations at Different Absorption * Extended X-Ray Bremsstrahlung Isochromat of Molybdenum * Size Distribution Determination of Heterogeneity Regions in Electrodeposited Metals by Saxs Method * The Possibility of the Application of the CH2I2 - Paraffin Oil Mixture as a Masking Liquid for Metal/Carrier Systems in Saxs Investigations * Investigation on Mechanical Alloying and Amorphisation Processes by the Rietveld Method * Growth of β' Phase Single Crystals of Sn-Sb Alloy * Effect of Oxygen Agglomeration on Structure of Annealed Cz-Si Single Crystal * X-Ray Investigation of Non-Uniform Stress Fields * Problem of Polytype Structures Series for Martensitic Phases of Metals and Alloys * Structure of Strain-Induced Martensite in β-CuZnAl Alloy * The Effect of Heat Treatment on the Phase Transitions in NiTiCo Shape Memory Alloy * 9R → 18R Phase Transformation in Cu-13Zn-8Al Alloy * Effect of Austenite Thermal Instability on Characteristics of Martensitic Transformation in Fe-Ni Alloys * Vacuum Annealing Study of Thin Ti Layers on High Carbon Steel Substrates * Vacuum Annealing Study of Thin Ta Layers on High Carbon Steel Substrates * Investigation of Speed of Ionic Sputtering of NiTi Alloys in Sea 02 Auger Spectrometer * Effect of Precipitation Hardening on Thermal Stability of Austenite in Fe-Ni Alloys * Structure of 18Cr-25Ni-Nb L Steel After Two Years Operation in Catalytic Tubes * Influence of Magnetic Field on Mechanical Barkhausen Effect Stress Dependence in Steel * Precipitation Structure in High Strength Aluminium Alloys * Morphology of Laser Treated Al-Zn and Al-Fe Alloys * Structure of Rapidly Solidified AlFe and AlFeNi Ribbons After Continuous Heating * X-Ray Diffractometric Investigations of Anatase—Rutile Titanium Dioxide Forms Transformation in the Presence of Some Additives * Investigations on Phase Transformation of Coprecipitated Iron-Magnesium Hydroxides * Determination of the Crystallinity of Polymer Blends by X-Ray Diffraction Method * XPD Study of the Selected Magnesium Compounds with the Expected Pharmacological Activity * Supermolecular Structure of the Nylon 6.10 Crystallized from the Melt and Its Changes During Heating * The Analysis of Substructural Parameters of PZT-Type Ferroelectric Ceramics

HPHT synthesis, structure and electrical properties of type-I clathrates Ba{sub 8}Al{sub x}Si{sub 46−x}

DOE Office of Scientific and Technical Information (OSTI.GOV)

Liu, Binwu; Jia, Xiaopeng; Sun, Hairui

2016-01-15

Clathrate compounds Ba{sub 8}Al{sub x}Si{sub 46−x} were successfully synthesized using the method of high-pressure and high-temperature (HPHT). In this process, we used BaSi{sub 2} as one of the starting materials in place of Ba metals, which reduces the complexity of the program caused by the extremely high chemical reactivity. By using this method, the processing time was reduced from few days to an hour. X-ray diffraction and structural refinement indicated this composition crystallized in type-I clathrate phase. Bond length analysis showed the Ba atoms in small dodecahedron had spherical thermal ellipsoids while those in large tetrakaidecahedron displayed anisotropic thermal ellipsoids.more » The negative Seebeck coefficient indicated transport processes were dominated by electrons as carriers, and increased with the increasing temperature. The electrical properties, including Seebeck coefficient and Power factor, were greatly enhanced by Al substitution. - Graphical abstract: Left: The cavity structure diagram of a China-type large volume cubic high-pressure apparatus, and the Type-I clathrate structure of sample synthesized using HPHT. Middle: X-ray Rietveld refinement profile for Ba{sub 8}Si{sub 46} and element mapping for Ba{sub 8}Al{sub 16}Si{sub 30}. Right: Temperature dependence of Seebeck coefficient for Ba{sub 8}Al{sub x}Si{sub 46−x} prepared by HPHT. - Highlights: • HPHT is a simple and rapid synthetic approach. • We use BaSi{sub 2} as one of the starting materials replacing Ba metals. • The processing time reduces from few days to an hour. • Structure determination is refined by Rietveld analysis of XRD data. • Variable temperature electrical properties are characterized.« less

In-situ high-pressure powder X-ray diffraction study of α-zirconium phosphate.

PubMed

Readman, Jennifer E; Lennie, Alistair; Hriljac, Joseph A

2014-06-01

The high-pressure structural chemistry of α-zirconium phosphate, α-Zr(HPO4)2·H2O, was studied using in-situ high-pressure diffraction and synchrotron radiation. The layered phosphate was studied under both hydrostatic and non-hydrostatic conditions and Rietveld refinement carried out on the resulting diffraction patterns. It was found that under hydrostatic conditions no uptake of additional water molecules from the pressure-transmitting medium occurred, contrary to what had previously been observed with some zeolite materials and a layered titanium phosphate. Under hydrostatic conditions the sample remained crystalline up to 10 GPa, but under non-hydrostatic conditions the sample amorphized between 7.3 and 9.5 GPa. The calculated bulk modulus, K0 = 15.2 GPa, showed the material to be very compressible with the weak linkages in the structure of the type Zr-O-P.

Unravelling the low thermal expansion coefficient of cation-substituted YBaCo 4O 7+δ

DOE PAGES

Manthiram, Arumugam; Huq, Ashfia; Kan, Wang Hay; ...

2016-01-12

With an aim to understand the origin of the low thermal expansion coefficients (TECs), cation substituted YBaCo 4O 7-type oxides have been investigated by in-situ neutron diffraction, bond valence sum (BVS), thermogravimetric analysis, and dilatometry. The compositions YBaCo 4O 7+δ, Y 0.9ln 0.1BaCo 3ZnO 7+δ, and Y 0.9ln 0.1BaCo 3Zn 0.6Fe 0.4O 7+δ) were synthesized by solid-state reaction at 1200 °C. Here, Rietveld refinement of the joint synchrotron X-ray and neutron diffraction data shows that the Zn and Fe dopants have different preferences to substitute the Co ions in the 6c and 2a sites.

Superparamagnetic behavior in Sn0.95Mg0.05O2 nanoparticles

NASA Astrophysics Data System (ADS)

Ahmed, Ateeq; Siddique, M. Naseem; Ali, Tinku; Tripathi, P.

2018-04-01

We have studied structural, optical and magnetic properties of Sn0.95Mg0.05O2 nanoparticles synthesized by sol-gel process. Single phase tetragonal structure of Mg doped SnO2 nanoparticles (NPs) have been inferred by X-ray diffraction, which involves Rietveld refinement analysis and average crystallite size is found to be 20.4 nm. Energy dispersive X -ray analysis confirmed the presence of Mg into host SnO2 lattice. The energy band gap is found to be wider (Eg = 3.73 eV) compared to the bulk (3.6 eV) which is due to the quantum confinement effect. The observed defects due to oxygen vacancies are studied by the photoluminescence study. The SQUID magnetometer measurements shows superparamagnetic behavior of Mg-doped SnO2 NPs at room temperature and they are single domain NPs. Our results suggest that it is possible to control the superparamagnetic properties through chemical composition.

A New Look at the Structural and Magnetic Properties of Potassium Neptunate K2NpO4 Combining XRD, XANES Spectroscopy, and Low-Temperature Heat Capacity.

PubMed

Smith, Anna L; Colineau, Eric; Griveau, Jean-Christophe; Popa, Karin; Kauric, Guilhem; Martin, Philippe; Scheinost, Andreas C; Cheetham, Anthony K; Konings, Rudy J M

2017-05-15

The physicochemical properties of the potassium neptunate K 2 NpO 4 have been investigated in this work using X-ray diffraction, X-ray absorption near edge structure (XANES) spectroscopy at the Np-L 3 edge, and low-temperature heat capacity measurements. A Rietveld refinement of the crystal structure is reported for the first time. The Np(VI) valence state has been confirmed by the XANES data, and the absorption edge threshold of the XANES spectrum has been correlated to the Mössbauer isomer shift value reported in the literature. The standard entropy and heat capacity of K 2 NpO 4 have been derived at 298.15 K from the low-temperature heat capacity data. The latter suggest the existence of a magnetic ordering transition around 25.9 K, most probably of the ferromagnetic type.

Neutron and X-ray total scattering study of hydrogen disorder in fully hydrated hydrogrossular, Ca3Al2(O4H4)3

NASA Astrophysics Data System (ADS)

Keen, David A.; Keeble, Dean S.; Bennett, Thomas D.

2018-04-01

The structure of fully hydrated grossular, or katoite, contains an unusual arrangement of four O-H bonds within each O4 tetrahedra. Neutron and X-ray total scattering from a powdered deuterated sample have been measured to investigate the local arrangement of this O4D4 cluster. The O-D bond length determined directly from the pair distribution function is 0.954 Å, although the Rietveld-refined distance between average O and D positions was slightly smaller. Reverse Monte Carlo refinement of supercell models to the total scattering data show that other than the consequences of this correctly determined O-D bond length, there is little to suggest that the O4D4 structure is locally significantly different from that expected based on the average structure determined solely from Bragg diffraction.

Structural and magnetic behavior of (Ni, Cu) substituted Nd0.67Sr0.33MnO3 perovskite compounds

NASA Astrophysics Data System (ADS)

Arun, B.; Sudakshina, B.; Akshay, V. R.; Chandrasekhar, K. Devi; Yang, H. D.; Vasundhara, M.

2018-05-01

Structural and magnetic phase transition of Ni and Cu substituted Nd0.67Sr0.33MnO3 perovskite compounds have been investigated. The Rietveld refinement of X-ray powder diffraction patterns confirms that both compounds have crystallized into an orthorhombic structure with Pbnm space group same as that of Nd0.67Sr0.33MnO3 compound. X-ray absorption spectra studies completely ruled out the possibility of existence of any impurities. Both compounds do not obey the Curie-Weiss law indicates the presence of some ferromagnetic clusters within the paramagnetic matrix. Ni substituted compound shows a lower value of TC and Cu substituted compound shows a higher value of TC than that of the parent. Non-saturating tendency of magnetization is more prominently seen in the case of Cu substituted compound, indicating an increase in the AFM component.

Study of structural and magnetic characterization of polycrystalline Y0.5Ho0.5CrO3

NASA Astrophysics Data System (ADS)

Mall, Ashish Kumar; Garg, Ashish; Gupta, Rajeev

2018-05-01

A polycrystalline ceramic sample of Y0.5Ho0.5CrO3 was studied using powder X-ray diffraction, Raman spectroscopic and dc magnetometry measurement to understand the structural and magnetic properties. The Rietveld refinement of X-ray data suggests sample crystallized in Pnma orthorhombic structure without formation of any secondary phases confirming their phase-pure nature. However, Raman study shows a prominent effect of Ho doping in low wavenumber Raman active phonon modes. Further, M-T measurement shows magnetic phase transition (TN) at 141 K and a negative value of Curie-Weiss temperature suggesting an antiferromagnetic system. Subsequent, the appearance of the clear opening in the M-H loop below TN is an evidence of the appearance of a weak ferromagnetic component in the low- temperature regime while the magnetization increases linearly in the high magnetic field regime suggest antiferromagnetic component.

Drastic effect of the Mn-substitution in the strongly correlated semiconductor FeSb2.

NASA Astrophysics Data System (ADS)

Kassem, Mohamed A.; Tabata, Yoshikazu; Waki, Takeshi; Nakamura, Hiroyuki

2017-06-01

We report the effects of Mn substitution, corresponding to hole doping, on the electronic properties of the narrow gap semiconductor, FeSb2, using single crystals of Fe1- x Mn x Sb2 grown by the Sb flux method. The orthorhombic Pnnm structure was confirmed by powder X-ray diffraction (XRD) for the pure and Mn-substituted samples. Their crystal structure parameters were refined using the Rietveld method. The chemical composition was investigated by wavelength-dispersive X-ray spectroscopy (WDX). The solubility limit of Mn in FeSb2 is x max ˜ 0.05 and the lattice constants change monotonically with increasing the actual Mn concentration. A drastic change from semiconducting to metallic electronic transports was found at very low Mn concentration at x ˜ 0.01. Our experimental results and analysis indicate that the substitution of a small amount of Mn changes drastically the electronic state in FeSb2 as well as the Co-substitution does: closing of the narrow gap and emergence of the density of states (DOS) at the Fermi level.

New process of preparation, X-ray characterisation, structure and vibrational studies of a solid solution LiTiOAs 1-xP xO 4 (0⩽ x⩽1)

NASA Astrophysics Data System (ADS)

Chakir, M.; El Jazouli, A.; Chaminade, J. P.; Bouree, F.; de Waal, D.

2006-01-01

LiTiOAs 1-xP xO 4 (0⩽ x⩽1) compounds have been prepared using solutions of Li, Ti, As and P elements as starting products. Selected compositions have been investigated by powder X-ray or neutrons diffraction analysis, Raman and infrared spectroscopy. The structure of LiTiOAs 1-xP xO 4 ( x=0, 0.5 and 1) samples determined by Rietveld analysis is orthorhombic with Pnma space group. It is formed by a 3D network of TiO 6 octahedra and XO 4 ( X=As 1-xP x) tetrahedra where octahedral cavities are occupied by lithium atoms. TiO 6 octahedra are linked together by corners and form infinite chains along a-axis. Ti atoms are displaced from the centre of octahedral units in alternating short (1.700-1.709 Å) and long (2.301-2.275 Å) Ti-O bonds. Raman and infrared studies confirm the existence of Ti-O-Ti chains. Thermal stability of LiTiOAsO 4 has been reported.

Facile one-pot synthesis of hexagons of NaSrB5O9:Tb3+ phosphor for solid-state lighting

NASA Astrophysics Data System (ADS)

Ramesh, B.; Dillip, G. R.; Deva Prasad Raju, B.; Somasundaram, K.; Prasad Peddi, Siva; de Carvalho dos Anjos, Virgilio; Joo, S. W.

2017-04-01

NaSrB5O9:Tb3+ hexagons were synthesized by a facile solid-state reaction method. The synthesized powders were structurally examined by x-ray diffraction analysis (XRD), and Rietveld refinement was performed using the XRD data and Fullprof software. Hexagon-like morphology was observed using field emission scanning electron microscopy (FESEM) and transmission electron microscopy (TEM). The elemental composition of the phosphors was investigated qualitatively by energy dispersive x-ray analysis (EDS) and quantitatively by x-ray photoelectron spectroscopy (XPS). The phosphor has a strong green emission at 545 nm under excitation of 379 nm, which is due to the 5{{\\text{D}}4}{{\\to}7}{{\\text{F}}5} transition of the Tb3+ ion. A lifetime of 3.48 ms was obtained for the phosphor. The important parameters of the light source were determined, such as the thermal quenching, critical distance, the nature of the dopant ion interaction, color coordinates, and quantum yield values. Other reported properties include the site occupancy of the dopant, surface properties, morphological properties, and optical properties.

Mesozoic clay diagenesis in the Appalachian Plateau

NASA Astrophysics Data System (ADS)

Boles, A.; Mulch, A.; van der Pluijm, B.

2017-12-01

Integrated investigation of authigenic clays in the Appalachian Plateau of the northeastern US Midcontinent using X-ray goniometry, Rietveld-method based illite polytype analysis, and 40Ar/39Ar geochronology yields novel insights about the structural diagenetic history of the North American sedimentary cover sequence. Texture analysis by High Resolution X-ray Texture Goniometry records the presence of a bedding-parallel diagenetic fabric, corresponding to a burial depth of 2-5 km. New development of polytype modeling using BGMN®, a quantitative X-ray powder diffraction forward modeling and whole-pattern matching program matches mineralic characteristic of illite at those depths and reduces uncertainty estimates in age analysis. Based on dating size fractions, the diagenetic age is constrained to 225-250 Ma (Triassic) by four authigenic illite samples, reflecting protracted, regional diagenesis in the area. Preliminary H isotopic analysis points to a surface-derived diagenetic fluid with δD values ranging from -48 to -72‰ (in the range of predicted Pangea meteoric fluid), with a dependence on proximity to the Appalachian Mountains that may reflect a rain shadow effect.

Effects of structural distortion induced by Sc substitution in LuFe2O4

NASA Astrophysics Data System (ADS)

Jeong, Jinwon; Noh, Han-Jin; Kim, Sung Baek

2014-06-01

We have studied the correlation between the structural distortion and the electronic/magnetic properties in single-crystalline (Lu,Sc)Fe2O4 (Sc = 0.05 and 0.3) by using X-ray diffraction (XRD), magnetic susceptibility, and X-ray absorption spectroscopy (XAS)/X-ray magnetic circular dichroism (XMCD) measurements. The Rietveld structure analysis of the XRD patterns revealed that the Sc substitution induced an elongation of the FeO5 bipyramidal cages in LuFe2O4 and increased the Fe2O4 bilayer thickness. A non-negligible decrease in the ferrimagnetic transition temperature T C is observed in the magnetic susceptibility curve of the Sc = 0.3 sample, but the XAS/XMCD spectra do not show any difference except for a small reduction of dichroism signals at the Fe3+absorption edge. We interpret this suppression of TC to be the result of a decreased spin-orbit coupling effect in the Fe2+ e 1 g doublet under D 3 h symmetry, which is induced by the weakened structural asymmetry of the FeO5 bipyramids.

Synthesis, surface chemistry and pseudocapacitance mechanisms of VN nanocrystals derived by a simple two-step halide approach

DOE Office of Scientific and Technical Information (OSTI.GOV)

Choi, Daiwon; Jampani, Prashanth H.; Jayakody, J. R. P.

Chloroamide precursors generated via a simple two-step ammonolysis reaction of transition metal chloride in the liquid phase at room temperature were heat treated in ammonia at moderate temperature to yield nano-sized VN crystallites. Grain growth inhibited by lowering the synthesis temperature (≈400°C) yielded agglomerated powders of spherical crystallites of cubic phase of VN with particle sizes as small as 6nm in diameter. X-ray diffraction, FTIR, mass spectroscopy (MS), and nuclear magnetic resonance (NMR) spectroscopy assessed the ammonolysis and nitridation reaction of the VCl 4-NH 3 system. X-ray Rietveld refinement, the BET technique and high-resolution transmission microscopy (HRTEM), energy dispersive x-raymore » (EDX) and thermogravimetric analysis (TGA) helped assess the crystallographic and microstructural nature of the VN nanocrystals. The surface chemistry and redox reaction leading to the gravimetric pseudo-capacitance value of (≈855 F/g) measured for the VN nanocrystals was determined and validated using FTIR, XPS and cyclic voltammetry analyses.« less

Structure and magnetic properties of flux grown single crystals of Co3-xFexSn2S2 shandites

NASA Astrophysics Data System (ADS)

Kassem, Mohamed A.; Tabata, Yoshikazu; Waki, Takeshi; Nakamura, Hiroyuki

2016-01-01

We report a successful single crystal growth of the shandite-type half-metallic ferromagnet Co3Sn2S2, and its Fe-substituted compounds, Co3-xFexSn2S2, by employing the flux method. Although Fe3Sn2S2 is unstable phase, we found that using the self Sn flux enables us to obtain single phase crystals up to x=0.53. The chemical composition of the grown plate-shaped single crystals was examined using wavelength-dispersive X-ray spectroscopy. The shandite structure with R 3 ̅m symmetry was confirmed by powder X-ray diffraction and the crystal structure parameters were refined using the Rietveld method. Magnetization measurements show suppression of the ferromagnetic order upon Fe-substitution , as well as in other substituted systems such as In- and Ni-substituted Co3Sn2S2. The almost identical magnetic phase diagrams of the Fe- and In-substituted compounds indicate that the electron number is dominantly significant to the magnetism in the Co-based shandite.

Solid state characterization and crystal structure from X-ray powder diffraction of two polymorphic forms of ranitidine base.

PubMed

de Armas, Héctor Novoa; Peeters, Oswald M; Blaton, Norbert; Van Gyseghem, Elke; Martens, Johan; Van Haele, Gerrit; Van Den Mooter, Guy

2009-01-01

Ranitidine hydrochloride (RAN-HCl), a known anti-ulcer drug, is the product of reaction between HCl and ranitidine base (RAN-B). RAN-HCl has been extensively studied; however this is not the case of the RAN-B. The solid state characterization of RAN-B polymorphs has been carried out using different analytical techniques (microscopy, thermal analysis, Fourier transform infrared spectrometry in the attenuated total reflection mode, (13)C-CPMAS-NMR spectroscopy and X-ray powder diffraction). The crystal structures of RAN-B form I and form II have been determined using conventional X-ray powder diffraction in combination with simulated annealing and whole profile pattern matching, and refined using rigid-body Rietveld refinement. RAN-B form I is a monoclinic polymorph with cell parameters: a = 7.317(2), b = 9.021(2), c = 25.098(6) A, beta = 95.690(1) degrees and space group P2(1)/c. The form II is orthorhombic: a = 31.252(4), b = 13.052(2), c = 8.0892(11) A with space group Pbca. In RAN-B polymorphs, the nitro group is involved in a strong intramolecular hydrogen bond responsible for the existence of a Z configuration in the enamine portion of the molecules. A tail to tail packing motif can be denoted via intermolecular hydrogen bonds. The crystal structures of RAN-B forms are compared to those of RAN-HCl polymorphs. RAN-B polymorphs are monotropic polymorphic pairs. (c) 2008 Wiley-Liss, Inc. and the American Pharmacists Association

Crystal-Chemical Analysis of Soil at Rocknest, Gale Crater

NASA Technical Reports Server (NTRS)

Morrison, S. M.; Downs, R. T.; Blake, D. F.; Bish, D. L.; Ming, D. W.; Morris, R. V.; Yen, A. S.; Chipera, S. J.; Treiman, A. H.; Vaniman, D. T.;

Novel high pressure hexagonal OsB2 by mechanochemistry

NASA Astrophysics Data System (ADS)

Xie, Zhilin; Graule, Moritz; Orlovskaya, Nina; Andrew Payzant, E.; Cullen, David A.; Blair, Richard G.

2014-07-01

Hexagonal OsB2, a theoretically predicted high-pressure phase, has been synthesized for the first time by a mechanochemical method, i.e., high energy ball milling. X-ray diffraction indicated that formation of hexagonal OsB2 begins after 2.5 h of milling, and the reaction reaches equilibrium after 18 h of milling. Rietveld refinement of the powder data indicated that hexagonal OsB2 crystallizes in the P63/mmc space group (No. 194) with lattice parameters of a=2.916 Å and c=7.376 Å. Transmission electron microscopy confirmed the appearance of the hexagonal OsB2 phase after high energy ball milling. in situ X-ray diffraction experiments showed that the phase is stable from -225 °C to 1050 °C. The hexagonal OsB2 powder was annealed at 1050 °C for 6 days in vacuo to improve crystallinity and remove strain induced during the mechanochemical synthesis. The structure partially converted to the orthorhombic phase (20 wt%) after fast current assisted sintering of hexagonal OsB2 at 1500 °C for 5 min. Mechanochemical approaches to the synthesis of hard boride materials allow new phases to be produced that cannot be prepared using conventional methods.

Influence of Annealing on the Depth Microstructure of the Shot Peened Duplex Stainless Steel at Elevated Temperature

NASA Astrophysics Data System (ADS)

Feng, Qiang; She, Jia; Xiang, Yong; Wu, Xianyun; Wang, Chengxi; Jiang, Chuanhai

The depth profiles of residual stresses and lattice parameters in the surface layers of shot peened duplex stainless steel at elevated temperature were investigated utilizing X-ray diffraction analysis. At each deformation depth, residual stress distributions in both ferrite and austenite were studied by X-ray diffraction stress analysis which is performed on the basis of the sin2ψ method and the lattice parameters were explored by Rietveld method. The results reveal that difference changes of depth residual compressive stress profiles between ferrite and austenite under the same annealing condition are resulted from the diverse coefficient of thermal expansion, dislocation density, etc. for different phases in duplex stainless steel. The relaxations of depth residual stresses in austenite are more obvious than those in ferrite. The lattice parameters decrease in the surface layer with the extending of annealing time, however, they increase along the depth after annealing for 16min. The change of the depth lattice parameters can be ascribed to both thermal expansion and the relaxation of residual stress. The different changes of microstructure at elevated temperature between ferrite and austenite are discussed.

Sr 2Fe 1.5Mo 0.5O 6- δ as a regenerative anode for solid oxide fuel cells

NASA Astrophysics Data System (ADS)

Liu, Qiang; Bugaris, Daniel E.; Xiao, Guoliang; Chmara, Maxwell; Ma, Shuguo; zur Loye, Hans-Conrad; Amiridis, Michael D.; Chen, Fanglin

Sr 2Fe 1.5Mo 0.5O 6- δ (SFM) was prepared using a microwave-assisted combustion synthesis method. Rietveld refinement of powder X-ray diffraction data reveals that SFM crystallizes in the simple cubic perovskite structure with iron and molybdenum disordered on the B-site. No structure transition was observed by variable temperature powder X-ray diffraction measurements in the temperature range of 25-800 °C. XPS results show that the iron and molybdenum valences change with an increase in temperature, where the mixed oxidation states of both iron and molybdenum are believed to be responsible for the increase in the electrical conductivity with increasing temperature. SFM exhibits excellent redox stability and has been used as both anode and cathode for solid oxide fuel cells. Presence of sulfur species in the fuel or direct utilization of hydrocarbon fuel can result in loss of activity, however, as shown in this paper, the anode performance can be regenerated from sulfur poisoning or coking by treating the anode in an oxidizing atmosphere. Thus, SFM can be used as a regenerating anode for direct oxidation of sulfur-containing hydrocarbon fuels.

X-ray powder diffraction, spectroscopic study, dielectric properties and thermal analysis of new doped compound TiGa0.67Te2.33O8

NASA Astrophysics Data System (ADS)

Smaoui, S.; Ben Aribia, W.; Kabadou, A.; Abdelmouleh, M.

2017-04-01

A novel mixed valence tellurium oxide, TiGa0.67Te2.33O8, was synthesized and its crystal structure determined using the X-ray powder diffraction technique. The obtained oxide was found to crystallize in a cubic unit-cell, Ia 3 bar space group, with the lattice parameter a = 10.9557(1) Å. Rietveld refinement of the structure led to ultimate confidence factors Rp = 7.63 and Rwp = 6.71. This structure was based on slabs containing groups of (Te/Ga)O4 joined by the metal cations Ti4+. The structure analysis showed a cation ordering of Te4+ and Te6+ yielding a TiGa2/3Te7/3O8 formula. The IR and RAMAN spectra confirmed the presence of the TiO6 and (Te/Ga)O4 groups. The dielectric anomalies observed at 500 K were attributed to the mixed valence structure, arising from the mixed-valence Te6+/Te4+. We detected only one peak in thermal behavior by the DTA/TG analysis; which implied a melting reaction.

Ensemble modeling of very small ZnO nanoparticles.

PubMed

Niederdraenk, Franziska; Seufert, Knud; Stahl, Andreas; Bhalerao-Panajkar, Rohini S; Marathe, Sonali; Kulkarni, Sulabha K; Neder, Reinhard B; Kumpf, Christian

2011-01-14

The detailed structural characterization of nanoparticles is a very important issue since it enables a precise understanding of their electronic, optical and magnetic properties. Here we introduce a new method for modeling the structure of very small particles by means of powder X-ray diffraction. Using thioglycerol-capped ZnO nanoparticles with a diameter of less than 3 nm as an example we demonstrate that our ensemble modeling method is superior to standard XRD methods like, e.g., Rietveld refinement. Besides fundamental properties (size, anisotropic shape and atomic structure) more sophisticated properties like imperfections in the lattice, a size distribution as well as strain and relaxation effects in the particles and-in particular-at their surface (surface relaxation effects) can be obtained. Ensemble properties, i.e., distributions of the particle size and other properties, can also be investigated which makes this method superior to imaging techniques like (high resolution) transmission electron microscopy or atomic force microscopy, in particular for very small nanoparticles. For the particles under study an excellent agreement of calculated and experimental X-ray diffraction patterns could be obtained with an ensemble of anisotropic polyhedral particles of three dominant sizes, wurtzite structure and a significant relaxation of Zn atoms close to the surface.

Structural and microstructural description of the glacial state in triphenyl phosphite from powder synchrotron X-ray diffraction data and Raman scattering investigations

NASA Astrophysics Data System (ADS)

Derollez, P.; Hernandez, O.; Hédoux, A.; Guinet, Y.; Masson, O.; Lefebvre, J.; Descamps, M.

2004-06-01

The structure and microstructure (refinement of the isotropic size and microstrain parameters) of the glacial state in triphenyl phosphite (TPP, P(OC 6H 5) 3) transformed at 222K have been determined from powder synchrotron X-ray diffraction data through a Rietveld and a Le Bail refinement, respectively. It is shown that the glacial state is composed of crystallites of the stable crystal phase coexisting with non-transformed supercooled liquid, the apparent size of the crystallites—depending on the aging temperature at which the glacial state is isothermally formed, [Phys. Rev. B 60 (1999) 9390]—being equal to 329.2(2) Å at 222K. The molecular conformation is slightly less mirror-symmetric than the one in the crystal state, and correlatively only one of the two unusual weak intermolecular C-H⋯O hydrogen bonds already observed in the latter state is encountered in the glacial one. Additional Raman scattering investigations confirm the previous result and reveal in addition that no hydrogen bonding interaction is observed neither in the glass nor in the liquid states.

A structural diagnostics diagram for metallofullerenes encapsulating metal carbides and nitrides.

PubMed

Maki, Sachiko; Nishibori, Eiji; Terauchi, Ikuya; Ishihara, Masayuki; Aoyagi, Shinobu; Sakata, Makoto; Takata, Masaki; Umemoto, Hisashi; Inoue, Takashi; Shinohara, Hisanori

2013-01-16

Systematic structural studies of 24 different kinds of endohedral metallofullerenes, M(x)C(2n) (M = La, Y, Sc, Lu, Ti, Eu, Er, Hf, Sc(3)N; 34 ≤ n ≤ 43), as 1:1 cocrystals with solvent toluene molecules have been carried out using synchrotron radiation powder diffraction. Thirteen of the 24 molecular structures, including five metal carbides, one metal nitride endohedral fullerene, and one hollow fullerene, have been determined by a combination of the maximum entropy method and Rietveld refinement of the X-ray diffraction data obtained. We have found that the volume for one fullerene and one toluene molecule depends linearly on the number of carbon atoms in the fullerene cage. Fifteen different kinds of metal carbide endohedral fullerenes have been identified, which can be structurally characterized from the obtained lattice constants using only this linear dependence. The linear dependence found in the present study provides a metallofullerene diagnostics diagram that may have universal importance for structural characterization of the so-called cluster endohedral fullerenes.

Abinitio powder x-ray diffraction and PIXEL energy calculations on thiophene derived 1,4 dihydropyridine

DOE Office of Scientific and Technical Information (OSTI.GOV)

Karthikeyan, N., E-mail: karthin10@gmail.com; Sivakumar, K.; Pachamuthu, M. P.

We focus on the application of powder diffraction data to get abinitio crystal structure determination of thiophene derived 1,4 DHP prepared by cyclocondensation method using solid catalyst. Crystal structure of the compound has been solved by direct-space approach on Monte Carlo search in parallel tempering mode using FOX program. Initial atomic coordinates were derived using Gaussian 09W quantum chemistry software in semi-empirical approach and Rietveld refinement was carried out using GSAS program. The crystal structure of the compound is stabilized by one N-H…O and three C-H…O hydrogen bonds. PIXEL lattice energy calculation was carried out to understand the physical naturemore » of intermolecular interactions in the crystal packing, on which the total lattice energy is contributed into Columbic, polarization, dispersion, and repulsion energies.« less

Crystal structure and thermal expansion of CsCaI3:Eu and CsSrBr3:Eu scintillators

NASA Astrophysics Data System (ADS)

Loyd, Matthew; Lindsey, Adam; Patel, Maulik; Koschan, Merry; Melcher, Charles L.; Zhuravleva, Mariya

2018-01-01

The distorted-perovskite scintillator materials CsCaI3:Eu and CsSrBr3:Eu prepared as single crystals have shown promising potential for use in radiation detection applications requiring a high light yield and excellent energy resolution. We present a study using high temperature powder X-ray diffraction experiments to examine a deleterious high temperature phase transition. High temperature phases were identified through sequential diffraction pattern Rietveld refinement in GSAS II. We report the linear coefficients of thermal expansion for both high and low temperature phases of each compound. Thermal expansion for both compositions is greatest in the [0 0 1] direction. As a result, Bridgman growth utilizing a seed oriented with the [0 0 1] along the growth direction should be used to mitigate thermal stress.

Synthesis, magnetic and electrical properties of R3AlCx (R = Ce, Pr and Nd)

NASA Astrophysics Data System (ADS)

Ghule, S. S.; Garde, C. S.; Ramakrishnan, S.; Singh, S.; Rajarajan, A. K.; Laad, Meena; Karmakar, Koushik

2017-09-01

R3AlCx (R = Ce, Pr and Nd; x = 0-1) series has been synthesized by arc melting. Rietveld analysis of x-ray powder diffraction reveals cubic (Pm-3m) structure. A Kondo temperature TK 1 K is estimated for Ce3AlC0.65 from the susceptibility and resistivity data. Magnetic susceptibility measurements indicate antiferromagnetic (AFM) order for R = Pr (x = 0.8 and 1) and Nd (x = 0.6, 0.8 and 1) and ferromagnetic (FM) for Nd3Al. Metamagnetic behaviour in the magnetization curve indicates complex magnetic structure. Band structure calculations indicate growth of a pseudo-gap in the density of states (DOS) from Ce3AlC to Pr3AlC to Nd3AlC. The DOS calculations predict a metallic behaviour which is consistent with the resistivity measurements.

Analysis of Short and Long Range Atomic Order in Nanocrystalline Diamonds with Application of Powder Diffractometry

NASA Technical Reports Server (NTRS)

Palosz, B.; Grzanka, E.; Stelmakh, S.; Pielaszek, R.; Bismayer, U.; Neuefiend, J.; Weber, H.-P.; Proffen, T.; VonDreele, R.; Palosz, W.;

Tuning the surface anisotropy in Fe-doped NiO nanoparticles.

PubMed

Moura, K O; Lima, R J S; Coelho, A A; Souza-Junior, E A; Duque, J G S; Meneses, C T

2014-01-07

Ni(1-x)FexO nanoparticles have been obtained by the co-precipitation chemical route. X-ray diffraction analyses using Rietveld refinement have shown a slight decrease in the microstrain and mean particle size as a function of the Fe content. The zero-field-cooling (ZFC) and field-cooling (FC) magnetization curves show superparamagnetic behavior at high temperatures and a low temperature peak (at T = 11 K), which is enhanced with increasing Fe concentration. Unusual behavior of the coercive field in the low temperature region and an exchange bias behavior were also observed. A decrease in the Fe concentration induces an increase in the exchange bias field. We argue that these behaviors can be linked with the strengthening of surface anisotropy caused by the incorporation of Fe ions.

Evidence for weak ferromagnetism, isostructural phase transition, and linear magnetoelectric coupling in the multiferroic Bi0.8Pb0.2Fe0.9Nb0.1O3 solid solution

NASA Astrophysics Data System (ADS)

Patel, Jay Prakash; Senyshyn, Anatoliy; Fuess, Hartmut; Pandey, Dhananjai

2013-09-01

Magnetization, dielectric, and calorimetric studies on Bi0.8 Pb0.2 Fe0.9 Nb0.1O3 (BF-0.2PFN) reveal very weak ferromagnetism but strong dielectric anomaly at the antiferromagnetic transition temperature (TN) characteristic of magnetoelectric coupling. We correlate these results with nuclear and magnetic structure studies using x-ray and neutron powder diffraction techniques, respectively. Rietveld refinements using x-ray powder diffraction data in the temperature range 300 to 673 K reveal pronounced anomalies in the unit cell parameters at TN, indicating strong magnetoelastic coupling. The nuclear and magnetic structures of BF-0.2PFN were determined from neutron powder diffraction data using a representation theory approach. They show the occurrence of a first-order isostructural phase transition (IPT) accompanying the magnetic ordering below TN˜566 K, leading to significant discontinuous change in the ionic polarization (ΔPz˜1.6(3) μC/cm2) and octahedral tilt angle (˜0.3°) at TN. The ionic polarization obtained from refined positional coordinates of the nuclear structure and Born effective charges is shown to scale linearly with sublattice magnetization, confirming the presence of linear magnetoelectric coupling in BF-0.2PFN at the atomic level, despite the very low value of remanent magnetization (Mr).

Magnetic and neutron diffraction study on quaternary oxides MTeMoO6 (M = Mn and Zn)

NASA Astrophysics Data System (ADS)

Doi, Yoshihiro; Suzuki, Ryo; Hinatsu, Yukio; Ohoyama, Kenji

2009-01-01

Crystal structures and magnetic properties of quaternary oxides MTeMoO6 (M = Mn and Zn) were investigated. From the Rietveld analyses for the powder x-ray and neutron diffraction measurements, their detailed structures have been determined. Both compounds have orthorhombic structure with space group P 21212 and a charge configuration of M2+Te4+Mo6+O6. ZnTeMoO6 shows diamagnetic behavior. In this structure, M ions are arranged in a square-planar manner. The temperature dependence of the magnetic susceptibility for MnTeMoO6 shows a broad peak at ~33 K, which is due to a two-dimensional characteristic of the magnetic interaction. In addition, this compound shows an antiferromagnetic transition at 20 K. The magnetic structure was determined by the powder neutron diffraction measurement at 3.3 K. The magnetic moments of Mn2+ ions (4.45 μB) order in a collinear antiferromagnetic arrangement along the b axis.

Structure, microstructure, and size dependent catalytic properties of nanostructured ruthenium dioxide

NASA Astrophysics Data System (ADS)

Nowakowski, Pawel; Dallas, Jean-Pierre; Villain, Sylvie; Kopia, Agnieszka; Gavarri, Jean-Raymond

2008-05-01

Nanostructured powders of ruthenium dioxide RuO 2 were synthesized via a sol gel route involving acidic solutions with pH varying between 0.4 and 4.5. The RuO 2 nanopowders were characterized by X-ray diffraction, scanning and transmission electron microscopy (SEM and TEM). Rietveld refinement of mean crystal structure was performed on RuO 2 nanopowders and crystallized standard RuO 2 sample. Crystallite sizes measured from X-ray diffraction profiles and TEM analysis varied in the range of 4-10 nm, with a minimum of crystallite dimension for pH=1.5. A good agreement between crystallite sizes calculated from Williamson Hall approach of X-ray data and from direct TEM observations was obtained. The tetragonal crystal cell parameter (a) and cell volumes of nanostructured samples were characterized by values greater than the values of standard RuO 2 sample. In addition, the [Ru-O 6] oxygen octahedrons of rutile structure also depended on crystal size. Catalytic conversion of methane by these RuO 2 nanostructured catalysts was studied as a function of pH, catalytic interaction time, air methane composition, and catalysis temperature, by the way of Fourier transform infrared (FTIR) spectroscopy coupled to homemade catalytic cell. The catalytic efficiency defined as FTIR absorption band intensities I(CO 2) was maximum for sample prepared at pH=1.5, and mainly correlated to crystallite dimensions. No significant catalytic effect was observed from sintered RuO 2 samples.

Three NiAs-Ni 2In Type Structures in the Mn-Sn System

NASA Astrophysics Data System (ADS)

Elding-Pontén, Margareta; Stenberg, Lars; Larsson, Ann-Kristin; Lidin, Sven; Ståhl, Kenny

1997-03-01

TheB8-type structure field of the Mn-Sn system has been investigated. Two high temperature phases (HTP1 and HTP2) and one low temperature phase (Mn3Sn2) were found. They all crystallize with the NiAs structure type with part of the trigonal bipyramidal interstices filled by manganese atoms in an ordered manner. The ordering as well as the manganese content is different for the three phases, giving rise to three different orthorhombic superstructures. Mn3Sn2seems to have the lowest manganese content, since the corresponding basal unit cell is smaller than for HTP1-2. Structural models of the phases are based on selected area electron diffraction, X-ray powder diffraction, and preliminary single crystal X-ray measurements. The ideal cell parameters found are (a=7ahex,b=3ahex,c=chex), (a=5ahex,b=3ahex,c=chex), and (a=2ahex,b=3ahex,c=chex) for HTP1, HTP2, and Mn3Sn2, respectively. The crystal structure of Mn3Sn2has been refined by means of the Rietveld method from X-ray powder diffraction data. Mn3Sn2is orthorhombic,Pnma,a=7.5547(2),b=5.4994(2),c=8.5842(2) Å,Z=4. (Pbnmin the setting above.) The compound is isostructural with Ni3Sn2andγ‧-Co3Sn2(H. Fjellvåg and A. Kjekshus,Acta Chem. Scand.A40, 23-30 (1986)). FinalRp=8.97%,Rwp=11.44%, GOF=2.86, andRBragg=4.11% using 43 parameters and 5701 observations and 330 Bragg reflections.

Crystal structures of the new ternary stannides La3Mg4-xSn2+x and LaMg3-xSn2

NASA Astrophysics Data System (ADS)

Solokha, P.; De Negri, S.; Minetti, R.; Proserpio, D. M.; Saccone, A.

2016-01-01

Synthesis and structural characterization of the two new lanthanum-magnesium-stannides La3Mg4-xSn2+x (0.12≤x≤0.40) and LaMg3-xSn2 (0.33≤x≤0.78) are reported. The crystal structures of these intermetallics were determined by single crystal X-ray diffraction analysis and confirmed by Rietveld refinement of powder X-ray diffraction patterns of the corresponding samples. The La3Mg4-xSn2+x phase crystallizes in the hexagonal Zr3Cu4Si2 structure type (P6bar2m, hP9, Z=3, x=0.12(1), a=7.7974(7), c=4.8384(4) Å), which represents an ordered derivative of the hP9-ZrNiAl prototype, ubiquitous among equiatomic intermetallics. The LaMg3-xSn2 phase is the second representative of the trigonal LaMg3-xGe2 type, which is a superstructure of the LaLi3Sb2 structure type (P3bar1c, hP34-0.12, Z=6, x=0.35(1), a=8.3222(9), c=14.9546(16) Å). The scheme describing the symmetry reduction/coloring with respect to the parent type is reported here with the purpose to discuss the LaMg3-xSn2 off-stoichiometry from the geometrical point of view. Structural relationships between the La-Mg-Sn ternary phases, including the already known equiatomic LaMgSn compound (oP12-TiNiSi), are presented in the framework of the AlB2-related compounds family and discussed with the aid of group-subgroup relations in the Bärnighausen formalism.

The low temperature synthesis, characterization and properties of ferroelectrics

NASA Astrophysics Data System (ADS)

Xu, Jie

2000-10-01

PZT 50:50 xerogels prepared by two different sol-gel routes crystallized in a similar fashion to give a mixture of tetragonal and rhombohedral at high temperature (1000°C). Both the diffraction and EXAFS data suggest that the compositional inhomogeneity of the samples prepared by the two routes is similar. The crystallization of CZT gels is complicated. Crystalline CaCO 3 was always detected in the dry gels regardless of the sample composition and preparation methods. At intermediate temperatures a fluorite related phase was always formed and it transformed to perovskite at higher temperatures. The EXAFS data suggest that perovskite CZT samples prepared using alkoxide sol-gel chemistry may not be random solid solutions. All the solution processed ZrTiO4 materials crystallized in the range 600--700°C. The KTN samples prepared using a conventional alkoxide sol-gel route crystallized completely to perovskite at lower temperatures than those prepared using prehydrolyzed precursors. The EXAFS data for the KTN samples prepared using a conventional alkoxide sol-gel route are consistent with a random distribution of tantalum and niobium in the solid solution. However, materials prepared using the inhomogeneous sol-gel route and by the direct reaction of mixed oxides were shown to be compositionally inhomogeneous. The heterogeneity could not be removed by regrinding and heating the mixed oxide samples several times. K2Ta4-xNbxO11 (x = 0, 2, 4) samples were prepared using alkoxide sol-gel chemistry and their crystallization was examined by powder X-ray diffraction. A Rietveld structure analysis of the pyrochlore formed from a gel with bulk composition K2Ta 2Nb2O11 indicated that it was rich in potassium relative to the bulk sample. On heating to high temperatures tetragonal tungsten bronzes were formed. A Rietveld analysis was also performed for K2Ta 2Nb2O11 with tetragonal tungsten bronze structure. The defect pyrochlores "AgTaO3" and GaTaO 3 were synthesized by ion-exchange using pyrochlore KTaO3 as a starting material. The structures of the pyrochlores were examined using the Rietveld method. The pyrochlore-to-perovskite transformations were also explored.

Multifunctionality of nanocrystalline lanthanum ferrite

DOE Office of Scientific and Technical Information (OSTI.GOV)

Rai, Atma, E-mail: atma@iitp.ac.in; Thakur, Awalendra K.; Centre for Energy and Environment, Indian Institute of Technology Patna 800013 India

2016-05-06

Nanocrystalline lanthanum ferrite has been synthesized by adopting modified Pechini route. No evidence of impurity or secondary phase has been detected up to the detection of error limit of X-ray diffractometer (XRD). Rietveld refinement of X-ray diffraction pattern reveals orthorhombic crystal system with space group Pnma (62).Crystallite size and lattice strain was found to be ∼42.8nm and 0.306% respectively. Optical band gap was found to be 2.109 eV, by UV-Visible diffused reflectance spectrum (DRS). Brunauer-Emmet-Teller (BET) surface area was found to be ∼3.45 m{sup 2}/g. Magnetization-hysteresis (M-H) loop was recorded at room temperature (300K) reveals weak ferromagnetism in Nanocrystalline lanthanummore » ferrite. The weak ferromagnetism in lanthanum ferrite is due to the uncompensated antiferromagnetic spin ordering. Ferroelectric loop hysteresis observed at room temperature at 100Hz depicts the presence of ferroelectric ordering in LaFeO{sub 3}.Simultanious presence of magnetic and ferroelectric ordering at room temperature makes it suitable candidate of Multiferroic family.« less

Multifunctionality of nanocrystalline lanthanum ferrite

NASA Astrophysics Data System (ADS)

Rai, Atma; Thakur, Awalendra K.

2016-05-01

Nanocrystalline lanthanum ferrite has been synthesized by adopting modified Pechini route. No evidence of impurity or secondary phase has been detected up to the detection of error limit of X-ray diffractometer (XRD). Rietveld refinement of X-ray diffraction pattern reveals orthorhombic crystal system with space group Pnma (62).Crystallite size and lattice strain was found to be ˜42.8nm and 0.306% respectively. Optical band gap was found to be 2.109 eV, by UV-Visible diffused reflectance spectrum (DRS). Brunauer-Emmet-Teller (BET) surface area was found to be ˜3.45 m2/g. Magnetization-hysteresis (M-H) loop was recorded at room temperature (300K) reveals weak ferromagnetism in Nanocrystalline lanthanum ferrite. The weak ferromagnetism in lanthanum ferrite is due to the uncompensated antiferromagnetic spin ordering. Ferroelectric loop hysteresis observed at room temperature at 100Hz depicts the presence of ferroelectric ordering in LaFeO3.Simultanious presence of magnetic and ferroelectric ordering at room temperature makes it suitable candidate of Multiferroic family.

In situ X-ray diffraction study of reduction processes of Fe{sub 3}O{sub 4}- and Fe{sub 1-x}O-based ammonia-synthesis catalysts

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zheng Yifan, E-mail: zhengyifan@zjut.edu.c; Catalysis Institute, Zhejiang University of Technology, Hangzhou 310014; Liu Huazhang

2009-09-15

The temperature-programmed reduction process of two types of industrial ammonia-synthesis catalysts, A110 and ZA-5, which are, respectively, based on Fe{sub 3}O{sub 4} and Fe{sub 1-x}O precursors, were studied by in situ X-ray power diffraction (XRD). It has been found that the ZA-5 has lower reduction temperature and faster reduction rate, and its active phase alpha-Fe possesses a higher value of lattice microstrain than A110. The simulation based on Rietveld refinement has also shown that the shape of alpha-Fe grain of ZA-5 has a mixed shape of cube and sphere with more exposing (111) and (211) planes, while that of A110more » looks like a concave cube with more exposing (110) planes. Based on the results obtained, a growth model of alpha-Fe during the reduction of Fe{sub 3}O{sub 4}- and Fe{sub 1-x}O-based ammonia-synthesis catalysts is proposed, and the origins for the activity difference has been also discussed. - Graphical Abstract: A proposed growth model of active phase alpha-Fe during reduction. Due to H{sub 2} diffusing easily into the pores, reduction starts on outside and inside surface simultaneously to form 'microcrystalline film', and the particles shrink during reduction which results in breaking of the aggregated oxide particle.« less

Synthesis, structural and optical properties of (ALa)(FeMn)O6 (A = Ba and Sr) double perovskites

NASA Astrophysics Data System (ADS)

Kumar, Dinesh; Sudarshan, V.; Singh, Akhilesh Kumar

2018-05-01

Here, we report structural and optical properties of ALaFeMnO6 (A = Ba and Sr) double perovskite synthesized via auto-combustion followed by calcinations process. Rietveld refinement of structure using x-ray diffraction data reveals that BaLaFeMnO6 crystallizes into cubic crystal structure with space group Pm-3m while SrLaFeMnO6 crystallizes into rhombohedral crystal structure having space group R-3c. The absorption spectrum measurement using UV-Vis spectroscopy reveals that these samples are prefect insulator having energy band gap between conduction and valence band of the order of 6 eV.

Nano sized La2Co2O6 double perovskite synthesized by sol gel method

NASA Astrophysics Data System (ADS)

Solanki, Neha; Lodhi, Pavitra Devi; Choudhary, K. K.; Kaurav, Netram

2018-05-01

We report here the synthesis of double perovskite La2Co2O6 (LCO) compound by a sol gel route method. The double perovskite structure of LCO system was confirmed via X-ray diffraction (XRD) analysis. Further, the lattice parameter, unit cell volume and bond length were refined by means of rietveld analysis using the full proof software. Debye Scherer formula was used to determine the particle size. The compound crystallized in triclinic structure with space group P-1 in ambient condition. We also obtained Raman modes from XRD spectra of poly-crystalline LCO sample. These results were interpreted for the observation of phonon excitations in this compound.

Solution combustion method for synthesis of nanostructured hydroxyapatite, fluorapatite and chlorapatite

NASA Astrophysics Data System (ADS)

Zhao, Junjie; Dong, Xiaochen; Bian, Mengmeng; Zhao, Junfeng; Zhang, Yao; Sun, Yue; Chen, JianHua; Wang, XuHong

2014-09-01

Hydroxyapatite (HAP), fluorapatite (Fap) and chlorapatite (Clap) were prepared by solution combustion method with further annealing at 800 °C. The characterization and structural features of the synthesized powders were evaluated by the powder X-ray diffraction (XRD, Fourier transform infrared spectroscopy (FT-IR), scanning electron microscope (SEM) and transmission electron microscopy (TEM) techniques. Characterization results from XRD and Rietveld analysis revealed that OH- in the HAP lattice were gradually substituted with the increase of F- and Cl- content and totally substituted at the molar concentration of 0.28 and 0.6, respectively. The results from FI-IR have also confirmed the incorporation of substituted anions in the apatite structure.

Phase equilibria and crystal structure of the complex oxides in the Sr Fe Co O system

NASA Astrophysics Data System (ADS)

Aksenova, T. V.; Gavrilova, L. Ya.; Cherepanov, V. A.

2008-06-01

Phase relations in the Sr-Fe-Co-O system have been investigated at 1100 °C in air by X-ray powder diffraction on quenched samples. Solid solutions of the form SrFe 1-xCo xO 3-δ (0⩽ x⩽0.7), Sr 3Fe 2-yCo yO 7-δ (0⩽ y⩽0.4) and Sr 4Fe 6-zCo zO 13±δ (0⩽ z⩽1.6) were prepared by solid-state reaction and by the sol-gel method. The structural parameters of single-phase samples were refined by the Rietveld profile method. The variation of the lattice parameters with composition has been determined for each solid solution and a cross-section of the phase diagram at 1100 °C in air for the entire Sr-Fe-Co-O system has been constructed.

Enhancement in electrical and magnetic properties with Ti-doping in Bi0.5La0.5Fe0.5Mn0.5O3

NASA Astrophysics Data System (ADS)

Singh, Rahul; Gupta, Prince Kumar; Kumar, Shiv; Joshi, Amish G.; Ghosh, A. K.; Patil, S.; Chatterjee, Sandip

2017-04-01

In this investigation, we have synthesized Bi0.5La0.5Fe0.5Mn0.5-xTixO3 (where x = 0 and 0.05) samples. The Rietveld refinement of X-ray diffraction (XRD) patterns shows that the systems crystallize in the orthorhombic phase with the Pnma space group. The observed Raman modes support the XRD results. The appearance of prominent A1-3 and weak E-2 modes in Bi0.5La0.5Fe0.5Mn0.45Ti0.05O3 indicates the presence of chemically more active Bi-O covalent bonds. Ferromagnetism of Bi0.5La0.5Fe0.5Mn0.5O3 is enhanced by Ti doping at the Mn-site, indicating that these particular samples might be interesting for device applications.

Long- and Short-Range Structure of Ferrimagnetic Iron-Chromium Maghemites.

PubMed

García-Guaderrama, Marco; Montero-Cabrera, María E; Morán, Emilio; Alario-Franco, Miguel A; Fuentes-Cobas, Luis E; Macías-Ríos, Edgar; Esparza-Ponce, Hilda E; Fuentes-Montero, María E

2015-12-07

Maghemite-like materials containing Fe(3+) and Cr(3+) in comparable amounts have been prepared by solution-combustion synthesis. The conditions of synthesis and the magnetic properties are described. These materials are ferrimagnetic and are much more stable than pure iron maghemite since their maghemite-hematite transformation takes place at about ∼ 700 °C instead of ∼ 300 °C, as usually reported. These materials were studied by synchrotron radiation X-ray diffraction (XRD) and by X-ray absorption fine structure (XAFS) of the K-absorption edge of two elements. High-resolution XRD patterns were processed by means of the Rietveld method. Thus, maghemites were studied by XAFS in both Fe and Cr K-edges to clarify the short-range structure of the investigated systems. Pre-edge decomposition and theoretical modeling of X-ray absorption near edge structure transitions were performed. The extended X-ray absorption fine structure (EXAFS) spectra were fitted considering the facts that the central atom of Fe is able to occupy octahedral and tetrahedral sites, each with a weight adjustment, while Cr occupies only octahedral sites. Interatomic distances were determined for x = 1, by fitting simultaneously both Fe and Cr K-edges average EXAFS spectra. The results showed that the cation vacancies tend to follow a regular pattern within the structure of the iron-chromium maghemite (FeCrO3).

Structural analysis and martensitic transformation in equiatomic HfPd alloy

NASA Astrophysics Data System (ADS)

Hisada, S.; Matsuda, M.; Takashima, K.; Yamabe-Mitarai, Y.

2018-02-01

We investigated the crystal structure and the martensitic transformation in equiatomic HfPd alloy. The analysis of the crystal structure by electron diffraction and Rietveld refinement using X-ray diffraction data indicates that the space group of the martensitic phase is Cmcm, and the lattice parameters are a = 0.329 nm, b = 1.021 nm, and c = 0.438 nm. Martensitic variants are composed of the plate-like morphology of several hundred nm, and the boundaries between the variants have (021)Cmcm twin relations. This (021)Cmcm twin boundary seems to be sharp without ledge and steps. Differential scanning calorimetry measurement indicates that each martensitic transformation temperature is determined to be Ms = 819 K, Mf = 794 K, As = 928 K, and Af = 954 K. Based on the dimension change using a thermo-mechanical analyzer, the expansion and shrinkage of the sample occurred with the forward and reverse martensitic transformation, respectively.

Average and local crystal structures of (Ga 1–xZn x)(N 1–xO x) solid solution nanoparticles

DOE PAGES

Feygenson, Mikhail; Neuefeind, Joerg C.; Tyson, Trevor A.; ...

2015-11-06

We report the comprehensive study of the crystal structure of (Ga 1–xZn x)(N 1–xO x) solid solution nanoparticles by means of neutron and synchrotron x-ray scattering. In our study we used four different types of (Ga 1–xZn x)(N 1–xO x) nanoparticles, with diameters of 10–27 nm and x = 0.075–0.51, which show the narrow energy-band gaps from 2.21 to 2.61 eV. The Rietveld analysis of the neutron diffraction data revealed that the average crystal structure is the hexagonal wurtzite (space group P6 3mc), in agreement with previous reports on similar bulk materials. The pair-distribution function (PDF) analysis of the samemore » data found that the local structure is more disordered than the average one. It is best described by the model with a lower symmetry space group P1, where atoms are quasirandomly distorted from their nominal positions in the hexagonal wurtzite lattice.« less

Structural, spectroscopic, and magnetic properties of Eu3+-doped GdVO4 nanocrystals synthesized by a hydrothermal method.

PubMed

Szczeszak, Agata; Grzyb, Tomasz; Śniadecki, Zbigniew; Andrzejewska, Nina; Lis, Stefan; Matczak, Michał; Nowaczyk, Grzegorz; Jurga, Stefan; Idzikowski, Bogdan

2014-12-01

New interesting aspects of the spectroscopic properties, magnetism, and method of synthesis of gadolinium orthovanadates doped with Eu(3+) ions are discussed. Gd(1-x)Eu(x)VO4 (x = 0, 0.05, 0.2) bifunctional luminescent materials with complex magnetic properties were synthesized by a microwave-assisted hydrothermal method. Products were formed in situ without previous precipitation. The crystal structures and morphologies of the obtained nanomaterials were analyzed by X-ray diffraction and transmission and scanning electron microscopy. Crystallographic data were analyzed using Rietveld refinement. The products obtained were nanocrystalline with average grain sizes of 70-80 nm. The qualitative and quantitative elemental composition as well as mapping of the nanocrystals was proved using energy-dispersive X-ray spectroscopy. The spectroscopic properties of red-emitting nanophosphors were characterized by their excitation and emission spectra and luminescence decays. Magnetic measurements were performed by means of vibrating sample magnetometry. GdVO4 and Gd0.8Eu0.2VO4 exhibited paramagnetic behavior with a weak influence of antiferromagnetic couplings between rare-earth ions. In the substituted sample, an additional magnetic contribution connected with the population of low-lying excited states of europium was observed.

The structure of denisovite, a fibrous nanocrystalline polytypic disordered ‘very complex’ silicate, studied by a synergistic multi-disciplinary approach employing methods of electron crystallography and X-ray powder diffraction

PubMed Central

Schowalter, Marco; Schmidt, Martin U.; Czank, Michael; Depmeier, Wulf; Rosenauer, Andreas

2017-01-01

Denisovite is a rare mineral occurring as aggregates of fibres typically 200–500 nm diameter. It was confirmed as a new mineral in 1984, but important facts about its chemical formula, lattice parameters, symmetry and structure have remained incompletely known since then. Recently obtained results from studies using microprobe analysis, X-ray powder diffraction (XRPD), electron crystallography, modelling and Rietveld refinement will be reported. The electron crystallography methods include transmission electron microscopy (TEM), selected-area electron diffraction (SAED), high-angle annular dark-field imaging (HAADF), high-resolution transmission electron microscopy (HRTEM), precession electron diffraction (PED) and electron diffraction tomography (EDT). A structural model of denisovite was developed from HAADF images and later completed on the basis of quasi-kinematic EDT data by ab initio structure solution using direct methods and least-squares refinement. The model was confirmed by Rietveld refinement. The lattice parameters are a = 31.024 (1), b = 19.554 (1) and c = 7.1441 (5) Å, β = 95.99 (3)°, V = 4310.1 (5) Å3 and space group P12/a1. The structure consists of three topologically distinct dreier silicate chains, viz. two xonotlite-like dreier double chains, [Si6O17]10−, and a tubular loop-branched dreier triple chain, [Si12O30]12−. The silicate chains occur between three walls of edge-sharing (Ca,Na) octahedra. The chains of silicate tetrahedra and the octahedra walls extend parallel to the z axis and form a layer parallel to (100). Water molecules and K+ cations are located at the centre of the tubular silicate chain. The latter also occupy positions close to the centres of eight-membered rings in the silicate chains. The silicate chains are geometrically constrained by neighbouring octahedra walls and present an ambiguity with respect to their z position along these walls, with displacements between neighbouring layers being either Δz = c/4 or −c/4. Such behaviour is typical for polytypic sequences and leads to disorder along [100]. In fact, the diffraction pattern does not show any sharp reflections with l odd, but continuous diffuse streaks parallel to a* instead. Only reflections with l even are sharp. The diffuse scattering is caused by (100) nano­lamellae separated by stacking faults and twin boundaries. The structure can be described according to the order–disorder (OD) theory as a stacking of layers parallel to (100). PMID:28512570

Effect of Fe doping on structural and impedance properties of PZTFN ceramics

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kumar, Arvind, E-mail: arvindmse07311209.in@gmail.com; Pal, Vijayeta; Mishra, S. K.

2016-05-06

An attempts have been made to synthesis the ceramics Pb{sub 1-3x/2} Fe{sub x}(Zr{sub 0.52}Ti{sub 0.48}){sub 1-5y/4} NbyO{sub 3} abbreviated as (PFZTN) for x = 1-6 mol% and y = 5.5 mol% by a semi-wet route. In the present paper, we have investigated the effect of Fe doping on structural and electrical properties of the PFZTN ceramics. X-ray diffraction (XRD) patterns reveal that PFZTN ceramics are single phase in nature. However, for x = 0.05 and 0.06, a secondary phase appears as discernible from the XRD profiles. Rietveld analysis of the powder diffraction data shows the presence of coexistence of tetragonal (P4mm spacemore » group) and rhombohedral phases (R3c space group) occurs near the morphotropic phase boundary (MPB) at x ≥ = 0.05. The log-log plots show that the conductivity increases with increase of temperature. The ac conductivity becomes sensitive at high frequency region and shifted towards higher frequency side with increasing temperature. It is observed that the activation energy (Ea) decreases with increasing frequency. This complex perovskite structure can be used as a multilayer ceramic capacitors and electromechanical transducers.« less

Structural evolution in three and four-layer Aurivillius solid solutions: A comparative study versus relaxor properties

NASA Astrophysics Data System (ADS)

Tellier, Jenny; Boullay, Philippe; Ben Jennet, Dorra; Mercurio, Daniele

2008-02-01

Two solid solutions of three-layer Ba xBi 4- xNb xTi 3- xO 12 (0 ≤ x ≤ 1.2) and four-layer Aurivillius compounds (Na 0.5Bi 0.5) 1- xBa xBi 4Ti 4O 15 (0 ≤ x ≤ 1), which both present a ferroelectric to relaxor-like transition with increasing x, were synthesized by solid state reaction. The evolution of their crystal structures, as a function of x, was performed using Rietveld refinements from X-ray powder diffraction data. As x increases, the average crystal structures become less distorted with respect to the archetypal high temperature tetragonal one and the coordination number of Bi 3+ in M 2O 2 layers continuously changes from {4 + 2} to {4}. The relaxor behaviour which appears in samples for a tolerance factor t > 0.96 is associated with a general static disorder in A and M sites together with the presence of some Ba 2+ cations in M 2O 2 layers (less than 10%).

Structural, magnetic and magnetoreactance studies in NiFe2-xRxO4 (x = 0, 0.05; R = Y, Yb and Lu)

NASA Astrophysics Data System (ADS)

Ugendar, Kodam; Chunchu, Venkatrao; Rani, G. Neeraja; Markaneyulu, G.

2018-04-01

Structural, magnetic and magnetoreactance (mr) properties of NiFe2-xRxO4 (x = 0, 0.05; R = Y, Yb and Lu) compounds were investigated and the results are discussed and presented in this paper. Rietveld refined X-ray diffraction (XRD) patterns and Raman spectroscopy revealed the cubic inverse spinel phase for all the compounds investigated. The former also identified small amounts of RFeO3 as the secondary phase. Lattice constant values were increased upon partial substitution of Fe3+ by R3+ (R = Y, Yb and Lu). Magnetization measurements revealed that the magnetic moment of R3+ (R = Y, Yb and Lu) substituted compounds decreased compared with NiFe2O4. mr was measured at 3 kHz and 3 MHz both longitudinal (LT) and transverse (TR) configuration. A maximum mr of 54 % was observed in Y3+ substituted NiFe2O4 in TR mode.

Parametric Rietveld refinement and magnetic characterization of superparamagnetic iron oxide nanoparticles

NASA Astrophysics Data System (ADS)

Pereira, Guilherme Ferreira Lemos; Costa, Fanny Nascimento; Souza, José Antonio; Haddad, Paula Silvia; Ferreira, Fabio Furlan

2018-06-01

This article describes the synthesis of two superparamagnetic iron oxide nanoparticles (SPIONs) covered with different ligands - hydrophobic (oleic acid (OA)) and hydrophilic (tetraethyl ammonium (TEA)) - and the investigation of the effects of thermal treatments on the crystal structure of TEA-SPIONs or OA-SPIONs using X-ray powder diffraction data and parametric Rietveld refinements; we stablished non-crystallographic models to describe how the oxidation processes take place with increasing temperatures for the different systems. The morphological and magnetic properties revealed the nanoparticles have a mean diameter of ∼10 nm in the solid state and are superparamagnetic at room temperature. Magnetization measurements confirmed the superparamagnetic state for both systems and revealed smaller particle sizes and narrower size distribution for OA-SPIONs than for TEA-SPIONs. The thermomagnetic analyses show only the ferrimagnetic phase transition of magnetite for OA-SPIONs while in the TEA-SPIONs, besides the ferrimagnetic phase transition there is the appearance of an antiferromagnetic one disclosing the evolution of hematite phase probably on the surface of magnetite due to thermal cycles.

X-ray diffraction investigations of structural modifications in In-doped tin pyrophosphates

DOE Office of Scientific and Technical Information (OSTI.GOV)

Botez, Cristian E.; Martinez, Heber; Morris, Joshua L.

2017-08-01

Laboratory and synchrotron x-ray powder diffraction were used to investigate the structural modifications that occur upon indium doping of tin pyrophosphate. The data collected under air, vacuum, and inert gas sample environments at temperatures (T) from 50 °C to 300 °C show that regardless of the In-doping level (0 ≤ x ≤ 0.18) all InxSn1-xP2O7 samples are isomorphic (have the same P a -3 cubic crystal structure) at all temperatures and under all the conditions investigated. The cubic lattice parameter (a) increases linearly with T at all doping levels, but the “a vs. x|T“ isotherms exhibit a robust peak atmore » x = 0.1 when data are collected on samples measured in air. On the other hand, Rietveld refinements against data collected on InxSn1-xP2O7 samples yield values of OO bond lengths and POP bond angles that show no major changes at x = 0.1 at any temperature. This is significant, as the Sn0.9In0.1P2O7 (x = 0.1) compound is known to exhibit the highest proton conductivity within the series, but the microscopic details responsible for the increased proton conductivity are not understood. Finally, the peak observed in the “a vs. x|T“ curves vanishes if the measurements are taken on samples kept either under vacuum or in an inert gas environment. This is a remarkable behavior as it lends further support to our hypothesis that a key microscopic feature responsible for the large proton conductivity of the Sn0.9In0.1P2O7 compound is the enlargement of the lattice constant at x = 0.1.« less

Phase composition and morphological characterization of human kidney stones using IR spectroscopy, scanning electron microscopy and X-ray Rietveld analysis.

PubMed

Chatterjee, Paramita; Chakraborty, Arup; Mukherjee, Alok K

2018-07-05

Pathological calcification in human urinary tract (kidney stones) is a common problem affecting an increasing number of people around the world. Analysis of such minerals or compounds is of fundamental importance for understanding their etiology and for the development of prophylactic measures. In the present study, structural characterization, phase quantification and morphological behaviour of thirty three (33) human kidney stones from eastern India have been carried out using IR spectroscopy (FT-IR), powder X-ray diffraction (PXRD) and scanning electron microscopy (SEM). Quantitative phase composition of kidney stones has been analyzed following the Rietveld method. Based on the quantitative estimates of constituent phases, the calculi samples have been classified into oxalate (OX), uric acid (UA), phosphate (PH) and mixed (MX) groups. Rietveld analysis of PXRD patterns showed that twelve (36%) of the renal calculi were composed exclusively of whewellite (calcium oxalate monohydrate, COM). The remaining twenty one (64%) stones were mixture of phases with oxalate as the major constituent in fourteen (67%) of these stones. The average crystallite size of whewellite in oxalate stones, as determined from the PXRD analysis, varies between 93 (1) nm and 202 (3) nm, whereas the corresponding sizes for the uric acid and struvite crystallites in UA and PH stones are 79 (1)-155 (4) nm and 69 (1)-123(1) nm, respectively. The size of hydroxyapatite crystallites, 10 (1)-21 (1) nm, is smaller by about one order of magnitude compared to other minerals in the kidney stones. A statistical analysis using fifty (50) kidney stones (33 calculi from the present study and 17 calculi reported earlier from our laboratory) revealed that the oxalate group (whewellite, weddellite or mixture of whewellite and weddellite as the major constituent) is the most prevalent (82%) kidney stone type in eastern India. Copyright © 2018 Elsevier B.V. All rights reserved.

Local and average structures of BaTiO 3-Bi(Zn 1/2Ti 1/2)O 3

DOE Office of Scientific and Technical Information (OSTI.GOV)

Usher, Tedi-Marie; Iamsasri, Thanakorn; Forrester, Jennifer S.

The complex crystallographic structures of (1-x)BaTiO 3-xBi(Zn 1/2Ti 1/2)O 3 (BT-xBZT) are examined using high resolution synchrotron X-ray diffraction, neutron diffraction, and neutron pair distribution function (PDF) analyses. The short-range structures are characterized from the PDFs, and a combined analysis of the X-ray and neutron diffraction patterns is used to determine the long-range structures. Our results demonstrate that the structure appears different when averaged over different length scales. In all compositions, the local structures determined from the PDFs show local tetragonal distortions (i.e., c/a > 1). But, a box-car fitting analysis of the PDFs reveals variations at different length scales.more » For 0.80BT-0.20BZT and 0.90BT-0.10BZT, the tetragonal distortions decrease at longer atom-atom distances (e.g., 30 vs. 5 ). When the longest distances are evaluated (r > 40 ), the lattice parameters approach cubic. Neutron and X-ray diffraction yield further information about the long-range structure. Compositions 0.80BT-0.20BZT and 0.90BT-0.10BZT appear cubic by Bragg diffraction (no peak splitting), consistent with the PDFs at long distances. However, these patterns cannot be adequately fit using a cubic lattice model; modeling their structures with the P4mm space group allows for a better fit to the patterns because the space group allows for c-axis atomic displacements that occur at the local scale. Furthermore, for the compositions 0.92BT-0.08BZT and 0.94BT-0.06BZT, strong tetragonal distortions are observed at the local scale and a less-distorted tetragonal structure is observed at longer length scales. In Rietveld refinements, the latter is modeled using a tetragonal phase. Since the peak overlap in these two-phase compositions limits the ability to model the local-scale structures as tetragonal, it is approximated in the refinements as a cubic phase. These results demonstrate that alloying BT with BZT results in increased disorder and disrupts the long-range ferroelectric symmetry present in BT, while the large tetragonal distortion present in BZT persists at the local scale.« less

Local and average structures of BaTiO 3-Bi(Zn 1/2Ti 1/2)O 3

DOE PAGES

Usher, Tedi-Marie; Iamsasri, Thanakorn; Forrester, Jennifer S.; ...

2016-11-11

The complex crystallographic structures of (1-x)BaTiO 3-xBi(Zn 1/2Ti 1/2)O 3 (BT-xBZT) are examined using high resolution synchrotron X-ray diffraction, neutron diffraction, and neutron pair distribution function (PDF) analyses. The short-range structures are characterized from the PDFs, and a combined analysis of the X-ray and neutron diffraction patterns is used to determine the long-range structures. Our results demonstrate that the structure appears different when averaged over different length scales. In all compositions, the local structures determined from the PDFs show local tetragonal distortions (i.e., c/a > 1). But, a box-car fitting analysis of the PDFs reveals variations at different length scales.more » For 0.80BT-0.20BZT and 0.90BT-0.10BZT, the tetragonal distortions decrease at longer atom-atom distances (e.g., 30 vs. 5 ). When the longest distances are evaluated (r > 40 ), the lattice parameters approach cubic. Neutron and X-ray diffraction yield further information about the long-range structure. Compositions 0.80BT-0.20BZT and 0.90BT-0.10BZT appear cubic by Bragg diffraction (no peak splitting), consistent with the PDFs at long distances. However, these patterns cannot be adequately fit using a cubic lattice model; modeling their structures with the P4mm space group allows for a better fit to the patterns because the space group allows for c-axis atomic displacements that occur at the local scale. Furthermore, for the compositions 0.92BT-0.08BZT and 0.94BT-0.06BZT, strong tetragonal distortions are observed at the local scale and a less-distorted tetragonal structure is observed at longer length scales. In Rietveld refinements, the latter is modeled using a tetragonal phase. Since the peak overlap in these two-phase compositions limits the ability to model the local-scale structures as tetragonal, it is approximated in the refinements as a cubic phase. These results demonstrate that alloying BT with BZT results in increased disorder and disrupts the long-range ferroelectric symmetry present in BT, while the large tetragonal distortion present in BZT persists at the local scale.« less

High-pressure structural parameters and equation of state of osmium to 207 GPa

DOE PAGES

Perreault, Christopher S.; Velisavljevic, Nenad; Vohra, Yogesh K.; ...

2017-09-08

We studied the most incompressible transition metal osmium (Os) under high pressure. There is significant interest in Os because of the structural anomalies attributed to topological transitions in the Fermi surface for valence electrons in the hexagonal close-packed phase. We report on measurements of structural parameters and equation of state on Os metal to a pressure of 207 GPa at ambient temperature using platinum as a pressure standard. We also obtained angle-dispersive X-ray diffraction data at a synchrotron source with closely spaced pressure intervals to observe any discontinuities or anomalies in the axial c/a ratio at high pressures. Rietveld refinementsmore » of X-ray diffraction data show a slowly varying axial ratio (c/a) with a broad minimum at 75 GPa. Our data do not provide any evidence of anomalous behavior in the c/a ratio in Os at 25 or 150 GPa as have been reported in previous studies. These experimental results are in agreement with theoretical calculations that do not predict any anomalous behavior in c/a ratio in Os under extreme conditions. We present an equation of state for Os to 207 GPa (V/V 0 = 0.761) at ambient temperature and compare our results with the previously published data.« less

High-pressure structural parameters and equation of state of osmium to 207 GPa

DOE Office of Scientific and Technical Information (OSTI.GOV)

Perreault, Christopher S.; Velisavljevic, Nenad; Vohra, Yogesh K.

We studied the most incompressible transition metal osmium (Os) under high pressure. There is significant interest in Os because of the structural anomalies attributed to topological transitions in the Fermi surface for valence electrons in the hexagonal close-packed phase. We report on measurements of structural parameters and equation of state on Os metal to a pressure of 207 GPa at ambient temperature using platinum as a pressure standard. We also obtained angle-dispersive X-ray diffraction data at a synchrotron source with closely spaced pressure intervals to observe any discontinuities or anomalies in the axial c/a ratio at high pressures. Rietveld refinementsmore » of X-ray diffraction data show a slowly varying axial ratio (c/a) with a broad minimum at 75 GPa. Our data do not provide any evidence of anomalous behavior in the c/a ratio in Os at 25 or 150 GPa as have been reported in previous studies. These experimental results are in agreement with theoretical calculations that do not predict any anomalous behavior in c/a ratio in Os under extreme conditions. We present an equation of state for Os to 207 GPa (V/V 0 = 0.761) at ambient temperature and compare our results with the previously published data.« less

Unraveling the Hydrogenation of TiO 2 and Graphene Oxide/TiO 2 Composites in Real Time by in Situ Synchrotron X-ray Powder Diffraction and Pair Distribution Function Analysis

DOE PAGES

Nguyen-Phan, Thuy-Duong; Liu, Zongyuan; Luo, Si; ...

2016-02-18

The functionalization of graphene oxide (GO) and graphene by TiO 2 and other metal oxides has attracted considerable attention due to numerous promising applications in catalysis, energy conversion, and storage. We propose hydrogenation of this class of materials as a promising way to tune catalytic properties by altering the structural and chemical transformations that occur upon H incorporation. We also investigate the structural changes that occur during the hydrogenation process using in situ powder X-ray diffraction and pair distribution function analysis of GO–TiO 2 and TiO 2 under H 2 reduction. Sequential Rietveld refinement was employed to gain insight intomore » the evolution of crystal growth of TiO 2 nanoparticles in the presence of two-dimensional (2D) GO nanosheets. GO sheets not only significantly retarded the nucleation and growth of rutile impurities, stabilizing the anatase structure, but was also partially reduced to hydrogenated graphene by the introduction of atomic hydrogen into the honeycomb lattice. We discuss the hydrogenation processes and the resulting composite structure that occurs during the incorporation of atomic H and the dynamic structural transformations that leads to a highly active photocatalyst.« less

Metrological characterization of X-ray diffraction methods at different acquisition geometries for determination of crystallite size in nano-scale materials

DOE Office of Scientific and Technical Information (OSTI.GOV)

Uvarov, Vladimir, E-mail: vladimiru@savion.huji.ac.il; Popov, Inna

2013-11-15

Crystallite size values were determined by X-ray diffraction methods for 183 powder samples. The tested size range was from a few to about several hundred nanometers. Crystallite size was calculated with direct use of the Scherrer equation, the Williamson–Hall method and the Rietveld procedure via the application of a series of commercial and free software. The results were statistically treated to estimate the significance of the difference in size resulting from these methods. We also estimated effect of acquisition conditions (Bragg–Brentano, parallel-beam geometry, step size, counting time) and data processing on the calculated crystallite size values. On the basis ofmore » the obtained results it is possible to conclude that direct use of the Scherrer equation, Williamson–Hall method and the Rietveld refinement employed by a series of software (EVA, PCW and TOPAS respectively) yield very close results for crystallite sizes less than 60 nm for parallel beam geometry and less than 100 nm for Bragg–Brentano geometry. However, we found that despite the fact that the differences between the crystallite sizes, which were calculated by various methods, are small by absolute values, they are statistically significant in some cases. The values of crystallite size determined from XRD were compared with those obtained by imaging in a transmission (TEM) and scanning electron microscopes (SEM). It was found that there was a good correlation in size only for crystallites smaller than 50 – 60 nm. Highlights: • The crystallite sizes for 183 nanopowders were calculated using different XRD methods • Obtained results were subject to statistical treatment • Results obtained with Bragg-Brentano and parallel beam geometries were compared • Influence of conditions of XRD pattern acquisition on results was estimated • Calculated by XRD crystallite sizes were compared with same obtained by TEM and SEM.« less

Phase coexistence and magnetic behavior in the low-dimensional hexagonal cobaltites BaxA1-xCoO3-δ (A = Mg or Ca and 0 ⩽ x ⩽ 0.20)

NASA Astrophysics Data System (ADS)

Oliveira, M. P.; Mercena, S. G.; Meneses, C. T.; Jesus, C. B. R.; Pagliuso, P. G.; Duque, J. G. S.

2018-04-01

In this work, we report on X-ray diffraction and magnetization measurements carried out in the low-dimensional hexagonal cobaltites BaxA1-xCoO3-δ (A = Mg or Ca, 0 ⩽ x ⩽ 0.20 and δ = 0 or 0.4). Polycrystalline samples have been synthesized by solid-state reaction. The Rietveld refinements of the X-ray diffraction patterns show clearly a phase coexistence of both BaCoO2.6 and BaCoO3 hexagonal polytype structures (space group: P63/mmc), which is dependent on both the dopant ion and doping level. At low temperatures (T < 50K), the ZFC-FC data recorded at H = 1 kOe for Ca-doped (x < 0.15) and Ba0.80Mg0.20CoO3-δ samples present a broad peak and strong thermal hysteresis. Besides, a second anomaly around room temperature is also observed in susceptibility curves for all samples. Further increasing in the Ca-doping produces a continuous decreasing of magnetization and for the samples with x > 0.10 the low temperature hysteresis is not observed anymore. The field-dependence of ZFC-FC curves taken for the sample grown with x = 0 show a displacement of the peak position into low temperature region. Except for the sample grown with x = 0.20, the MvsH loops taken at T = 2 K show multiple steps in the field region ranging - 15 ⩽ H ⩽ 15 kOe . Finally, the saturation magnetization values are consistent with a low-spin state for the Co2+ or Co4+ ions.

Nanostructured Co1-xNix(Sb1-yTey)3 skutterudites: Theoretical modeling, synthesis and thermoelectric properties

NASA Astrophysics Data System (ADS)

Stiewe, Christian; Bertini, Luca; Toprak, Muhammet; Christensen, Mogens; Platzek, Dieter; Williams, Simon; Gatti, Carlo; Müller, Eckhard; Iversen, Bo B.; Muhammed, Mamoun; Rowe, Michael

2005-02-01

The properties of Te-doped Co(Sb1-yTey)3 and Te-Ni double-doped Co1-xNix(Sb1-yTey)3 nanostructured skutterudites were evaluated by means of x-ray powder diffraction, and transport properties measured on the synthesized samples have been compared with ab initio theoretical modeling. Theoretical optimal dopant contents have been evaluated according to the maximum value of the power factor, calculating the electronic transport properties from the ab initio material band structure using semiclassical Boltzmann transport theory. The samples have been synthesized by chemical alloying with Te substitution for Sb up to 2.5at.% and Ni substitution for Co up to 2.0at.%. X-ray powder diffraction has been performed on all samples to reveal information about phase purity and Rietveld refinement was performed for the phase composition and cell parameter. The thermoelectric properties of the resulting consolidates were investigated in a temperature range from 300to723K using various measurement facilities. A standardization and round robin program was started among the participating evaluation laboratories in order to ensure reliability of the data obtained. The significant reduction in thermal conductivity, when compared to highly annealed CoSb3, could be proved which is caused by the nanostructuring, resulting in a high concentration of grain boundaries. A combination of substitution levels for Ni and Te has been found resulting in the largest ZT value of 0.65 at 680K among unfilled skutterudite materials.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Caliandro, Rocco; Sibillano, Teresa; Belviso, B. Danilo

In this study, we have developed a general X-ray powder diffraction (XPD) methodology for the simultaneous structural and compositional characterization of inorganic nanomaterials. The approach is validated on colloidal tungsten oxide nanocrystals (WO 3-x NCs), as a model polymorphic nanoscale material system. Rod-shaped WO 3-x NCs with different crystal structure and stoichiometry are comparatively investigated under an inert atmosphere and after prolonged air exposure. An initial structural model for the as-synthesized NCs is preliminarily identified by means of Rietveld analysis against several reference crystal phases, followed by atomic pair distribution function (PDF) refinement of the best-matching candidates (static analysis). Subtlemore » stoichiometry deviations from the corresponding bulk standards are revealed. NCs exposed to air at room temperature are monitored by XPD measurements at scheduled time intervals. The static PDF analysis is complemented with an investigation into the evolution of the WO 3-x NC structure, performed by applying the modulation enhanced diffraction technique to the whole time series of XPD profiles (dynamical analysis). Prolonged contact with ambient air is found to cause an appreciable increase in the static disorder of the O atoms in the WO 3-x NC lattice, rather than a variation in stoichiometry. Finally, the time behavior of such structural change is identified on the basis of multivariate analysis.« less

Synthesis of nanocrystalline zirconia by amorphous citrate route: structural and thermal (HTXRD) studies

DOE Office of Scientific and Technical Information (OSTI.GOV)

Bhagwat, Mahesh; Ramaswamy, Veda

Nanocrystalline zirconia powder with a fairly narrow particle size distribution has been synthesized by the amorphous citrate route. The sample obtained has a high BET surface area of 89 m{sup 2} g{sup -1}. Rietveld refinement of the powder X-ray diffraction (XRD) profile of the zirconia sample confirms stabilization of zirconia in the tetragonal phase with around 8% monoclinic impurity. The data show the presence of both anionic as well as cationic vacancies in the lattice. Crystallite size determined from XRD is 8 nm and is in close agreement with the particle size determined by TEM. The in situ high temperature-X-raymore » diffraction (HTXRD) study revealed high thermal stability of the mixture till around 1023 K after which the transformation of tetragonal phase into the monoclinic phase has been seen as a function of temperature till 1473 K. This transformation is accompanied by an increase in the crystallite size of the sample from 8 to 55 nm. The thermal expansion coefficients are 9.14 x 10{sup -6} K{sup -1} along 'a'- and 15.8 x 10{sup -6} K{sup -1} along 'c'-axis. The lattice thermal expansion coefficient in the temperature range 298-1623 K is 34.6 x 10{sup -6} K{sup -1}.« less

Solid-state evaluation and polymorphic quantification of venlafaxine hydrochloride raw materials using the Rietveld method.

PubMed

Bernardi, Larissa S; Ferreira, Fábio F; Cuffini, Silvia L; Campos, Carlos E M; Monti, Gustavo A; Kuminek, Gislaine; Oliveira, Paulo R; Cardoso, Simone G

2013-12-15

Venlafaxine hydrochloride (VEN) is an antidepressant drug widely used for the treatment of depression. The purpose of this study was to carry out the preparation and solid state characterization of the pure polymorphs (Forms 1 and 2) and the polymorphic identification and quantification of four commercially-available VEN raw materials. These two polymorphic forms were obtained from different crystallization methods and characterized by X-ray Powder Diffraction (XRPD), Diffuse Reflectance Infrared Fourier Transform (DRIFT), Raman Spectroscopy (RS), liquid and solid state Nuclear Magnetic Resonance (NMR and ssNMR) spectroscopies, Differential Scanning Calorimetry (DSC), and Scanning Electron Microscopy (SEM) techniques. The main differences were observed by DSC and XRPD and the latter was chosen as the standard technique for the identification and quantification studies in combination with the Rietveld method for the commercial raw materials (VEN1-VEN4) acquired from different manufacturers. Additionally Form 1 and Form 2 can be clearly distinguished from their (13)C ssNMR spectra. Through the analysis, it was possible to conclude that VEN1 and VEN2 were composed only of Form 1, while VEN3 and VEN4 were a mixture of Forms 1 and 2. Additionally, the Rietveld refinement was successfully applied to quantify the polymorphic ratio for VEN3 and VEN4. Copyright © 2013 Elsevier B.V. All rights reserved.

Single crystal growth and characterization of kagomé-lattice shandites Co3Sn2-xInxS2

NASA Astrophysics Data System (ADS)

Kassem, Mohamed A.; Tabata, Yoshikazu; Waki, Takeshi; Nakamura, Hiroyuki

2015-09-01

Single crystals of the shandite-type half metallic ferromagnet Co3Sn2S2, and its In-substituted compounds, Co3Sn2-xInxS2 (0

Local structure and oxide-ion conduction mechanism in apatite-type lanthanum silicates.

PubMed

Masson, Olivier; Berghout, Abid; Béchade, Emilie; Jouin, Jenny; Thomas, Philippe; Asaka, Toru; Fukuda, Koichiro

2017-01-01

The local structure of apatite-type lanthanum silicates of general formula La 9.33+x (SiO 4 ) 6 O 2+3x/2 has been investigated by combining the atomic pair distribution function (PDF) method, conventional X-ray and neutron powder diffraction (NPD) data and density functional theory (DFT) calculations. DFT was used to build structure models with stable positions of excess oxide ions within the conduction channel. Two stable interstitial positions were obtained in accordance with literature, the first one located at the very periphery of the conduction channel, neighbouring the SiO 4 tetrahedral units, and the second one closer to the channel axis. The corresponding PDFs and average structures were then calculated and tested against experimental PDFs obtained by X-ray total scattering and NPD Rietveld refinements results gathered from literature. It was shown that of the two stable interstitial positions obtained with DFT only the second one located within the channel is consistent with experimental data. This result consolidates one of the two main conduction mechanisms along the c-axis reported in the literature, namely the one involving cooperative movement of O4 and Oi ions.

Local structure and oxide-ion conduction mechanism in apatite-type lanthanum silicates

PubMed Central

Masson, Olivier; Berghout, Abid; Béchade, Emilie; Jouin, Jenny; Thomas, Philippe; Asaka, Toru; Fukuda, Koichiro

2017-01-01

Abstract The local structure of apatite-type lanthanum silicates of general formula La9.33+x(SiO4)6O2+3x/2 has been investigated by combining the atomic pair distribution function (PDF) method, conventional X-ray and neutron powder diffraction (NPD) data and density functional theory (DFT) calculations. DFT was used to build structure models with stable positions of excess oxide ions within the conduction channel. Two stable interstitial positions were obtained in accordance with literature, the first one located at the very periphery of the conduction channel, neighbouring the SiO4 tetrahedral units, and the second one closer to the channel axis. The corresponding PDFs and average structures were then calculated and tested against experimental PDFs obtained by X-ray total scattering and NPD Rietveld refinements results gathered from literature. It was shown that of the two stable interstitial positions obtained with DFT only the second one located within the channel is consistent with experimental data. This result consolidates one of the two main conduction mechanisms along the c-axis reported in the literature, namely the one involving cooperative movement of O4 and Oi ions. PMID:28970872

Local structure and oxide-ion conduction mechanism in apatite-type lanthanum silicates

NASA Astrophysics Data System (ADS)

Masson, Olivier; Berghout, Abid; Béchade, Emilie; Jouin, Jenny; Thomas, Philippe; Asaka, Toru; Fukuda, Koichiro

2017-12-01

The local structure of apatite-type lanthanum silicates of general formula La9.33+x(SiO4)6O2+3x/2 has been investigated by combining the atomic pair distribution function (PDF) method, conventional X-ray and neutron powder diffraction (NPD) data and density functional theory (DFT) calculations. DFT was used to build structure models with stable positions of excess oxide ions within the conduction channel. Two stable interstitial positions were obtained in accordance with literature, the first one located at the very periphery of the conduction channel, neighbouring the SiO4 tetrahedral units, and the second one closer to the channel axis. The corresponding PDFs and average structures were then calculated and tested against experimental PDFs obtained by X-ray total scattering and NPD Rietveld refinements results gathered from literature. It was shown that of the two stable interstitial positions obtained with DFT only the second one located within the channel is consistent with experimental data. This result consolidates one of the two main conduction mechanisms along the c-axis reported in the literature, namely the one involving cooperative movement of O4 and Oi ions.

Structural analysis and ferroelectric properties of Fe doped BaTiO{sub 3}

DOE Office of Scientific and Technical Information (OSTI.GOV)

Mishra, Ashutosh, E-mail: a.mansuri14@gmail.com, E-mail: amishra1960@yahoo.co.in; Mansuri, Amantulla, E-mail: a.mansuri14@gmail.com, E-mail: amishra1960@yahoo.co.in; Dwivedi, J. P.

2016-05-23

The polycrystalline samples of Fe doped BaTiO{sub 3} (BTO) with compositional formula BaTi{sub 1-x}Fe{sub x}O{sub 3} (x = 0, 0.03, 0.04 and 0.05) were prepared by solid-state reaction route. The influence of the Fe content on the structural, vibrational and electric properties of BaTiO{sub 3} was investigated using X-ray powder diffraction (XRD), Raman spectroscopy and Polarization techniques. XRD analysis indicates the formation of single-phase tetragonal structure for all the prepared samples. Tetragonal cubic structure with space group P4mm of all samples is further approved by Rietveld refinement. Room temperature Raman spectra of pure BaTiO{sub 3} show four active modes ofmore » vibration whose intensity decreases with increasing Fe doping. Small shift in Raman modes and increment in the line width has been observed with the doping ions. The hysteresis loop is very well performed with regular sharp characteristic of ferroelectric materials.« less

Doping effect on the structural properties of Cu1-x(Ni, Zn, Al and Fe)xO samples (0

NASA Astrophysics Data System (ADS)

Amaral, J. B.; Araujo, R. M.; Pedra, P. P.; Meneses, C. T.; Duque, J. G. S.; dos S. Rezende, M. V.

2016-09-01

In this work, the effect of insertion of transition metal, TM (=Ni, Zn, Al and Fe), ions in Cu1-xTMxO samples (0

Synthesis, crystal structure and spectroscopy properties of Na 3AZr(PO 4) 3 ( A=Mg, Ni) and Li 2.6Na 0.4NiZr(PO 4) 3 phosphates

NASA Astrophysics Data System (ADS)

Chakir, M.; El Jazouli, A.; de Waal, D.

2006-06-01

Na 3AZr(PO 4) 3 ( A=Mg, Ni) phosphates were prepared at 750 °C by coprecipitation route. Their crystal structures have been refined at room temperature from X-ray powder diffraction data using Rietveld method. Li 2.6Na 0.4NiZr(PO 4) 3 was synthesized through ion exchange from the sodium analog. These materials belong to the Nasicon-type structure. Raman spectra of Na 3AZr(PO 4) 3 ( A=Mg, Ni) phosphates present broad peaks in favor of the statistical distribution in the sites around PO 4 tetrahedra. Diffuse reflectance spectra indicate the presence of octahedrally coordinated Ni 2+ ions.

Magnetic and transport properties of Ce 6MnSb 15

NASA Astrophysics Data System (ADS)

Godart, Claude; Rogl, Peter; Alleno, Eric; Gonçalves, António P.; Rouleau, Olivier

2006-05-01

In our effort to look for new Ce/Yb-based compounds with large unit cell, we studied Ce 6MnSb 15. Rietveld refinements of X-ray powder diffraction confirm that the material crystallizes in orthorhombic structure La 6MnSb 15-type, Imm2 space group, with 2 Ce sites (8e and 4d) and lattice parameters a=15.1643 Å, b=19.3875 Å and c=4.2794 Å, which closely agree with those already published. Magnetic susceptibility results show a paramagnetic behavior and no magnetic order down to 2 K in contrast to antiferromagnetic order previously reported at 7 K. Resistivity shows a metallic behavior and the Seebeck coefficient is very low, typically -2 μV/K.

SrFe 12O 19 prepared by the proteic sol-gel process

NASA Astrophysics Data System (ADS)

Brito, P. C. A.; Gomes, R. F.; Duque, J. G. S.; Macêdo, M. A.

2006-10-01

Powders of strontium hexaferrite (SrFe 12O 19) were prepared by the proteic sol-gel process using coconut water as a precursor. X-ray diffraction (XRD) measurement showed the formation of SrFe 12O 19 with a small amount of the hematite for the sample calcined at 1000 °C with Fe/Sr=12. Rietveld refinement disclosed that this sample had 87.56% of the SrFe 12O 19 and 12.44% of Fe 2O 3 and the values for Rp, Rwp and χ2 were 4.28%, 5.93% and 1.71, respectively. The magnetic properties were Ms=64 emu/g, Mr/ Ms=0.55 and Hc=1.4 kOe for a crystallite size of 57 nm.

Study of conduction behavior in Pr0.67Sr0.03Ag0.30MnO3

NASA Astrophysics Data System (ADS)

Bhat, Masroor Ahmad; Modi, Anchit; Pandey, Devendra K.; Gaur, N. K.

2018-05-01

In this paper, we report the conduction mechanism in Pr0.67Sr0.03Ag0.30MnO3 system synthesized via conventional solid state reaction route. The structural information was carried by X - Ray diffraction using Rietveld refinement which confirms the secondary phase of the sample. The SEM image shows the formation of double phase composite because of limited reaction of silver with parent compound. The resistivity behavior indicates the semiconducting behavior. The electronic nature can be estimated by means of variable range hopping (VRH) and small polaron hopping (SPH) model showing that the enhancement of double exchange interaction suppress the band gap and boost the carrier delocalization of charge carriers.

Structure and electrochemical behaviour of metastable Mg 50Ti 50 alloy prepared by ball milling

NASA Astrophysics Data System (ADS)

Rousselot, S.; Bichat, M.-P.; Guay, D.; Roué, L.

A 50-50 mixture of Mg and Ti was milled for different times, and the cycling discharge capacities of the resulting compounds were evaluated in KOH media. From Rietveld refinement analysis of the X-ray diffraction patterns, it is shown that a metastable hcp Mg 50Ti 50 compound is formed after 20 h of milling. This material has a very low-electrochemical hydriding activity. However, in the presence of 10 wt.% Pd (added before milling), it displays a maximum discharge capacity of ca. 400 mAh g -1 after three charge/discharge cycles. The irreversible structural evolution of the Mg 50Ti 50 alloy from a hcp phase to a fcc phase upon cycling is demonstrated.

Aging-Induced Transformations of Maraging-400 Alloys

NASA Astrophysics Data System (ADS)

Alves, T. J. B.; Nunes, G. C. S.; Tupan, L. F. S.; Sarvezuk, P. W. C.; Ivashita, F. F.; de Oliveira, C. A. S.; Paesano, A.

2018-06-01

Solubilized maraging-400 alloys were aged at 480 °C, 580 °C, and 650 °C, for 3, 6, and 12 hours and characterized by X-ray diffraction (Rietveld refinement), Mössbauer spectroscopy, and microhardness tests. The results revealed that the aging treatments induced an atomic rearrangement in the martensite phase, involving a change in the composition and lattice parameters, reversion of austenite, and, in some samples, the formation of the μ phase. The amounts of reverted and precipitated phases were dependent on the aging time and temperature. The tetragonal distortion from cubic symmetry, usually presented by martensite in solution-annealed maraging steels, was not eliminated after aging. The results obtained for these maraging-400 alloys are compared with those obtained for maraging-350 steel samples.

Ammonium–cobalt–nickel phosphates, NH{sub 4}[Co{sub 1−x}Ni{sub x}PO{sub 4}]·H{sub 2}O

DOE Office of Scientific and Technical Information (OSTI.GOV)

Torre-Fernández, Laura; Trobajo, Camino; Pedro, Imanol de

The ammonium–cobalt–nickel phosphates, NH{sub 4}[Co{sub 1−x}Ni{sub x}PO{sub 4}]·H{sub 2}O (x=0.00, 0.34, 0.59, 0.70, 1.00), and the deuterated forms, ND{sub 4}[Co{sub 1−x}Ni{sub x}PO{sub 4}]·D{sub 2}O (x=0.00, 0.38, 0.48, 0.69, 0.85), have been synthesized under mild hydrothermal conditions and characterised using X-ray and neutron diffraction, chemical and thermal analysis, and magnetic measurements. Their crystal structures, including hydrogen positions, were determined by Rietveld refinement using single-crystal X-ray and neutron powder diffraction data. The space group of these orthorhombic crystals modifies as a function of their composition. The magnetic susceptibility and magnetization measurements of these ammonium–cobalt–nickel phosphates show antiferromagnetic behaviour, and the Neel temperaturemore » evolves from 5.5 K (x=0.00) up to 13.2 K (x=1.00). - Graphical abstract: We obtained single crystals for all the members of the family. In this series, although all crystals are orthorhombic, the space group changes as a function of the composition, showing how the single-crystal diffraction data is capable to manifest structural subtleties that had not been described before for this group of materials. All the investigated materials behave antiferromagnetically with ordering temperatures from 5.5 K up to 13.2 K. Display Omitted - Highlights: • The ammonium–cobalt–nickel phosphates, NH{sub 4}[Co{sub 1−x}Ni{sub x}PO{sub 4}]·H{sub 2}O (x=0.00, 0.34, 0.59, 0.70, 1.00) and the deuterated forms ND4[Co1-xNixPO4]·D{sub 2}O (x=0.00, 0.38, 0.49, 0.68, 0.85) have synthesized by hydrothermal synthesis. • The structural studies of these compounds are introduced as a function of the composition. • The magnetic studies show an antiferromagnetically behavior with ordering temperatures from 5.5 K to 13.2 K.« less

Evolution of ferroelectric SrBi2Nb2O9 phase embedded in tellurite glass

NASA Astrophysics Data System (ADS)

Mohamed, E. A.

2017-12-01

Glasses with the composition, [(100-x)TeO2- x(SrO-Bi2O3-Nb2O5)] with x = 20, 30 and 40 (in mol %) were prepared. The X-ray diffraction (XRD) pattern and differential thermal analysis (DTA) for the as-prepared samples confirmed the amorphous and glassy characteristics, respectively. The SrBi2Nb2O9 phase in tellurite glass for HT773 sample at x = 40 mol % is formed and confirmed by the Rietveld refinement. DTA curves for all glass samples exhibit two endothermic dips while the two broad exothermic peaks at lower x reduced to one at higher x. Infrared (IR) results revealed that the glassy matrix are composed of TeO3, TeO3+1, TeO4, BiO6 and NbO6 structural units. The changes in the density (ρ), molar volume (Vm), oxygen molar volume (V0) and oxygen packing fraction (OPD) have correlated with structural changes in the glass network. The optical studies show an absorption bands below the absorption edge in the glass samples.

Crystal-structure analysis of four mineral samples of anhydrite, CaSO[subscript 4], using synchrotron high-resolution powder X-ray diffraction data

DOE Office of Scientific and Technical Information (OSTI.GOV)

Antao, Sytle M.

2014-05-28

The crystal structures of four samples of anhydrite, CaSO{sub 4}, were obtained by Rietveld refinements using synchrotron high-resolution powder X-ray diffraction (HRPXRD) data and space group Amma. As an example, for one sample of anhydrite from Hants County, Nova Scotia, the unit-cell parameters are a = 7.00032(2), b = 6.99234(1), c = 6.24097(1) {angstrom}, and V = 305.487(1) {angstrom}{sup 3} with a > b. The eight-coordinated Ca atom has an average distance of 2.4667(4) {angstrom}. The tetrahedral SO{sub 4} group has two independent S-O distances of 1.484(1) to O1 and 1.478(1) {angstrom} to O2 and an average distancemore » of 1.4810(5) {angstrom}. The three independent O-S-O angles [108.99(8) x 1, 110.38(3) x 4, 106.34(9){sup o} x 1; average [6] = 109.47(2){sup o}] and S-O distances indicate that the geometry of the SO{sub 4} group is quite distorted in anhydrite. The four anhydrite samples have structural trends where the a, b, and c unit-cell parameters increase linearly with increasing unit-cell volume, V, and their average and distances are nearly constant. The grand mean = 2.4660(2) {angstrom}, and grand mean = 1.4848(3) {angstrom}, the latter is longer than 1.480(1) {angstrom} in celestite, SrSO{sub 4}, as expected.« less

Tunable-color luminescence via energy transfer in NaCa13/18Mg5/18PO4:A (A = Eu2+/Tb3+/Mn2+, Dy3+) phosphors for solid state lighting.

PubMed

Li, Kai; Fan, Jian; Mi, Xiaoyun; Zhang, Yang; Lian, Hongzhou; Shang, Mengmeng; Lin, Jun

2014-11-17

A series of NaCa13/18Mg5/18PO4(NCMPO):A (A = Eu(2+)/Tb(3+)/Mn(2+), Dy(3+)) phosphors have been prepared by the high-temperature solid-state reaction method. The X-ray diffraction (XRD) and Rietveld refinement, X-ray photoelectron spectroscopy (XPS), photoluminescence (PL), cathodoluminescence (CL), decay lifetimes, and PL quantum yields (QYs) were utilized to characterize the phosphors. The pure crystalline phase of as-prepared samples has been demonstrated via XRD measurement and Rietveld refinements. XPS reveals that the Eu(2+)/Tb(3+)/Mn(2+) can be efficiently doped into the crystal lattice. NCMPO:Eu(2+)/Tb(3+)/Mn(2+) phosphors can be effectively excited under UV radiation, which show tunable color from purple-blue to red including white emission based on energy transfer from Eu(2+) to Tb(3+)/Mn(2+) ions. Under low-voltage electron beam bombardment, the NCMPO:A (A = Eu(2+)/Tb(3+)/Mn(2+), Dy(3+)) display their, respectively, characteristic emissions with different colors, and the CL spectrum of NCMPO:0.04Tb(3+) has the comparable intensity to the ZnO:Zn commercial product. In addition, the calculated CIE coordinate of NCMPO:0.04Tb(3+) (0.252, 0.432) is more saturated than it (0.195, 0.417). These results reveal that NCMPO:A (A = Eu(2+)/Tb(3+)/Mn(2+), Dy(3+)) may be potential candidate phosphors for WLEDs and FEDs.

Reversal magnetization dependence with the Cr and Fe oxidation states in YFe1-xCrxO3 (0≤x≤1) perovskites

NASA Astrophysics Data System (ADS)

Fabian, F. A.; Pedra, P. P.; Moura, K. O.; Duque, J. G. S.; Meneses, C. T.

2016-06-01

In this work, we have carried out a detailed study of the magnetic and structural properties of YFe1-xCrxO3 (0≤x≤1) samples with orthorhombic structure obtained by co-precipitation method. Analysis of X-ray diffraction data using Rietveld refinement show that all samples present an orthorhombic crystal system with space group Pnma. Besides, we have observed a reduction of unit cell volume with increasing of the Cr concentration. SEM images show the formation of grains of micrometer order. X-ray Absorption near edge spectroscopy (XANES) measurements show a shift of absorption edge which can be indicate there is (i) different oxidation states to Fe and Cr ions and/or (ii) a changing in the point symmetry of Fe and Cr ions to the compounds. The magnetization measurements indicate a continuous decreasing of the magnetic transition temperature as function of chromium doping. The reversal magnetization effect was observed to concentrations around x=0.5. Besides, the deviation of the Curie-Weiss law and a weak ferromagnetic behavior observed at room temperature in the M vs H curves can be attributed to the strong magnetic interactions between the transition metals with different oxidation states.

Structure and colossal dielectric permittivity of Ca2TiCrO6 ceramics

NASA Astrophysics Data System (ADS)

Yan-Qing, Tan; Meng, Yan; Yong-Mei, Hao

2013-01-01

A colossal permittivity ceramic material, Ca2TiCrO6, was successfully synthesized by the conventional solid-state reaction, and was characterized by scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), x-ray photoemission spectroscopy (XPS) and x-ray diffraction (XRD). Rietveld refinement of XRD data indicated that the material crystallized in orthorhombic structure with space group pbnm. SEM displayed Ca2TiCrO6 ceramic grains packed uniformly with the size range 5-20 µm. XPS analyses indicated that elemental chromium and titanium of the material were in mixed valence. The corresponding dielectric property was tested in the frequency range 1 kHz-1 MHz and the temperature range 213-453 K, and the ceramics exhibited a relaxation-like dielectric behaviour. Importantly, the permittivity of Ca2TiCrO6 could reach 80 000 at 298 K (100 Hz) and was maintained at 40 000 up to 398 K at 1 MHz, which could be attributed to the ion disorder and mixed valence of Cr3+/Cr6+ and Ti3+/Ti4+.

Structural and magnetic properties of Nd0.67Ba0.33MnO3 manganites with partial replacement of Fe and Cu at Mn-site

NASA Astrophysics Data System (ADS)

Sudakshina, B.; Arun, B.; Chandrasekhar, K. Devi; Yang, H. D.; Vasundhara, M.

2018-06-01

We have investigated the structural and magnetic properties of Nd0.67Ba0.33MnO3 manganite and partial replacement of Mn with Fe and Cu compounds followed by X-ray diffraction (XRD), X-ray absorption spectroscopy (XAS) and vibrating sample magnetometer (VSM). The Rietveld refinement of XRD indicates orthorhombic crystal structure with I-mma space group for all the compounds and thus obtained lattice parameters confirm the presence of co-operative Jahn-Teller effect. XRD and XAS spectra results suggests the existence of Fe3+ in Fe-substituted compound where as a mixed state of Cu2+ and Cu3+ ions in the Cu-substituted compound. The ferromagnetic (FM) to paramagnetic (PM) transition and magnetic moment is found to decrease upon the substitution of Fe and Cu atoms because of the suppression of double exchange interaction. The theoretically obtained and experimentally determined values of effective PM moment and saturation magnetic moment confirms the presence of inhomogeneous magnetic states containing FM and antiferromagnetic clusters in all the studied compounds.

Temperature Dependence of the Structural Parameters in the Transformation of Aragonite to Calcite, as Determined from In Situ Synchrotron Powder X-ray-Diffratction Data

DOE Office of Scientific and Technical Information (OSTI.GOV)

Antao, Sytle M.; Hassan, Ishmael; West Indies)

The temperature dependency of the crystal structure and the polymorphic transition of CaCO{sub 3} from aragonite to calcite were studied using Rietveld structure refinement and high-temperature in situ synchrotron powder X-ray-diffraction data at ambient pressure, P. The orthorhombic metastable aragonite at room P, space group Pmcn, transforms to trigonal calcite, space group R{bar 3}c, at about T{sub c} = 468 C. This transformation occurs rapidly; it starts at about 420 C and is completed by 500 C, an 80 C interval that took about 10 minutes using a heating rate of 8 C/min. Structurally, from aragonite to calcite, the distributionmore » of the Ca atom changes from approximately hexagonal to cubic close-packing. A 5.76% discontinuous increase in volume accompanies the reconstructive first-order transition. Besides the change in coordination of the Ca atom from nine to six from aragonite to calcite, the CO{sub 3} groups change by a 30{sup o} rotation across the transition.« less

Nano-sized ZnO powders prepared by co-precipitation method with various pH

DOE Office of Scientific and Technical Information (OSTI.GOV)

Purwaningsih, S. Y., E-mail: sriyanisaputri@gmail.com; Pratapa, S.; Triwikantoro,

2016-04-19

In this work, nano-sized ZnO powders have been synthesized by the co-precipitation method with Zn(CH3COOH)2.2H2O, HCl, and NH3.H2O as raw materials in various pH ranging from 8 to 10. The purity, microstructure, chemical group analysis, morphology of the prepared ZnO powders were studied by X-ray diffraction (XRD), Fourier transform infrared spectrometer (FTIR), energy dispersive X-ray spectrometry (EDX), and scanning electron microscope (SEM), respectively. Rietveld refinement of XRD data showed that ZnO crystallizes in the wurtzite structure with high purity. The obtained powders were nano-sized particles with the average crystallite size about 17.9 ± 2.1 nm synthesized with pH of 9.5, atmore » 85°C, and stirring time of 6 h. The SEM results have visualied the morphology of ZnO nanoparticles with spherical-like shape. The effect of processing conditions on morphology of ZnO was also discussed.« less

Characterization of tetraethylene glycol passivated iron nanoparticles

NASA Astrophysics Data System (ADS)

Nunes, Eloiza da Silva; Viali, Wesley Renato; da Silva, Sebastião William; Coaquira, José Antonio Huamaní; Garg, Vijayendra Kumar; de Oliveira, Aderbal Carlos; Morais, Paulo César; Jafelicci Júnior, Miguel

2014-10-01

The present study describes the synthesis and characterization of iron@iron oxide nanoparticles produced by passivation of metallic iron in tetraethylene glycol media. Structural and chemical characterizations were performed using transmission electron microscopy (TEM), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), and Mössbauer spectroscopy. Pomegranate-like core@shell nanoparticulate material in the size range of 90-120 nm was obtained. According to quantitative phase analysis using Rietveld structure refinement the synthesized iron oxide was identified as magnetite (Fe3O4) whereas the iron to magnetite mass fractions was found to be 47:53. These findings are in good agreement with the data obtained from Mössbauer and thermal gravimetric analysis (TGA). The XPS data revealed the presence of a surface organic layer with higher hydrocarbon content, possibly due to the tetraethylene glycol thermal degradation correlated with iron oxidation. The room-temperature (300 K) saturation magnetization measured for the as-synthesized iron and for the iron-iron oxide were 145 emu g-1 and 131 emu g-1, respectively. The measured saturation magnetizations are in good agreement with data obtained from TEM, XRD and Mössbauer spectroscopy.

Structure Evolution and Reactivity of the Sc(2- x)V xO3+δ (0 ≤ x ≤ 2.0) System.

PubMed

Lussier, Joey A; Simon, Fabian J; Whitfield, Pamela S; Singh, Kalpana; Thangadurai, Venkataraman; Bieringer, Mario

2018-05-07

Solid oxide fuel cells (SOFCs) are solid-state electrochemical devices that directly convert chemical energy of fuels into electricity with high efficiency. Because of their fuel flexibility, low emissions, high conversion efficiency, no moving parts, and quiet operation, they are considered as a promising energy conversion technology for low carbon future needs. Solid-state oxide and proton conducting electrolytes play a crucial role in improving the performance and market acceptability of SOFCs. Defect fluorite phases are some of the most promising fast oxide ion conductors for use as electrolytes in SOFCs. We report the synthesis, structure, phase diagram, and high-temperature reactivity of the Sc (2- x) V x O 3+δ (0 ≤ x ≤ 2.00) oxide defect model system. For all Sc (2- x) V x O 3.0 phases with x ≤ 1.08 phase-pure bixbyite-type structures are found, whereas for x ≥ 1.68 phase-pure corundum structures are reported, with a miscibility gap found for 1.08 < x < 1.68. Structural details obtained from the simultaneous Rietveld refinements using powder neutron and X-ray diffraction data are reported for the bixbyite phases, demonstrating a slight V 3+ preference toward the 8b site. In situ X-ray diffraction experiments were used to explore the oxidation of the Sc (2- x) V x O 3.0 phases. In all cases ScVO 4 was found as a final product, accompanied by Sc 2 O 3 for x < 1.0 and V 2 O 5 when x > 1.0; however, the oxidative pathway varied greatly throughout the series. Comments are made on different synthesis strategies, including the effect on crystallinity, reaction times, rate-limiting steps, and reaction pathways. This work provides insight into the mechanisms of solid-state reactions and strategic guidelines for targeted materials synthesis.

Titanium doped LSCM anode for hydrocarbon fuelled SOFCs

DOE Office of Scientific and Technical Information (OSTI.GOV)

Azad, Abul K.; Hakem, Afizul; Petra, Pg. M. Iskandar

2015-05-15

La{sub 0.75}Sr{sub 0.25}Cr{sub 0.5-x}Mn{sub 0.5}Ti{sub x}O{sub 3} (x = 0.1, 0.2) has been synthesized in solid state reaction method and tested as a potential anode material for solid oxide fuel cells. Rietveld refinement of X-ray powder diffraction data using Fullprof software shows that the materials crystallize in the rhombohedral symmetry in the R-3C space group. The cell parameters are: a = b = 5.5286 (4) Å, c = 13.408(1) Å, α = β = 90°, γ = 120°. Particle size distribution measurements show that the average particle size for x = 0.1 and 0.2 was 232.66 nm and 176.63 nm, respectively. Themore » potential on particles were found to be −22.86 mV and −27.73 mV, for x = 0.1 and x = 0.2, respectively. Thermal expansion measurement using thermo-mechanical analyzer shows that the thermal expansion coefficient is 13.96 × 10{sup −6}/°C which is close to the thermal expansion of the state-of–the art YSZ electrolyte. Microstructure has been observed from scanning electron microscopy which shows a porous structure. Energy dispersive X-ray shows that the percentage of the different cations and anions in the structure are close to the chemical occupancies.« less

Structure-substitution limit correlation study on Cr{sup 3+} substituted polycrystalline yttrium iron garnet

DOE Office of Scientific and Technical Information (OSTI.GOV)

Modi, K. B.; Saija, K. G.; Sharma, P. U.

2016-05-06

Polycrystalline samples of Cr{sup 3+} - substituted yttrium iron garnet (Y{sub 3}Fe{sub 5}O{sub 12}) system with general chemical formula, Y{sub 3}Fe{sub 5-x}Cr{sub x}O{sub 12}, x = 0.0, 0.2, 0.4 and 0.6 were synthesized by double sintering ceramic technique and characterized by X-ray powder diffractometry. The Rietveld fitted X-ray diffraction patterns analysis revealed mono phase formation for x = 0.0 - 0.4 compositions while x = 0.6 composition possesses mixed phase character. The observed substitution limit has been discussed in the light of ionic size of substituent, electrostatic energy, electronic configuration and synthesis parameters. These observations strongly suggest that the electronicmore » configuration of Cr{sup 3+}, which is favorable to the formation of d2sp3 (octahedral) type bonds, must be important. In the case of Cr{sup 3+}, the substitution does not appear to proceed well for x much greater than 0.5, this limitation probably is a consequence of the strong preference of a smaller ion Cr{sup 3+}, for a larger octahedral site which quickly leads to a condition not comparable with the requirement of the structure. The distribution of cations, mean ionic radii and theoretical lattice constant values have been determined.« less

Dielectric properties of A- and B-site doped BaTiO 3: Effect of La and Ga

NASA Astrophysics Data System (ADS)

Gulwade, Devidas; Gopalan, Prakash

2009-06-01

Extremely small amounts of La and Ga doping on the A- and B-site of BaTiO 3, respectively, resulting in a solid solution of the type Ba 1-3xLa 2xTi 1-3yGa 4yO 3 have been investigated. The present work dwells on the influence of the individual dopants, namely La and Ga, on the dielectric properties of BaTiO 3. The compositions have been prepared by solid-state reaction. X-ray diffraction (XRD) reveals the presence of tetragonal (P4/mmm) phase. The XRD data has been analyzed using FULLPROF, a Rietveld refinement package. The microstructure have been studied by orientation imaging microscopy (OIM). The compositions have been characterized by dielectric spectroscopy between room temperature and 250 °C. Further, the nature of phase transition has been studied using high temperature XRD. The resulting compounds exhibit high dielectric constant, enhanced diffuseness and low temperature coefficient of capacitance.

Synthesis of ZnSnO{sub 3} nanostructure by sol gel method

DOE Office of Scientific and Technical Information (OSTI.GOV)

Para, Touseef Ahmad; Reshi, Hilal Ahmad; Shelke, Vilas, E-mail: drshelke@gmail.com

2016-05-23

Zinc Stannate (ZST) with composition ZnSnO{sub 3} is known for high electron mobility, optical, piezoelectric and charge storage properties. ZST crystalizes in different lattice structures, which allows a wide range of tunablity. We demonstrate successful synthesis of ZnSnO{sub 3} nanomaterial by sol-gel method. ZnSnO{sub 3} nanomaterials were calcined and sintered at different temperatures. Powder X-ray diffraction confirmed the single phase of the nanomaterial with rhombohedral R-3 space group. The Rietveld refinement of diffraction pattern yielded lattice parameter values a=5.26Å, c=14.09Å. Raman spectroscopy revealed higher activity towards higher wavenumbers. Raman shift around 530cm{sup −1} was found to be highly structure dependent,more » most probably due to anharmonic atomic vibrations in ZnO{sub 6}/SnO{sub 6} octahedra around center of mass. Sharp Peak around 650cm{sup −1} is characteristic of ZnSnO{sub 3} molecule.« less

The Ni-rich part of the Al–Ge–Ni phase diagram

PubMed Central

Jandl, Isabella; Reichmann, Thomas L.; Richter, Klaus W.

2013-01-01

The Ni-rich part of the ternary system Al–Ge–Ni (xNi > 50 at.%) was investigated by means of optical microscopy, powder X-ray diffraction (XRD), differential thermal analysis (DTA) and scanning electron microscopy (SEM). The two isothermal sections at 550 °C and 700 °C were determined. Within these two sections a new ternary phase, designated as τ4, AlyGe9−yNi13±x (hP66, Ga3Ge6Ni13-type) was detected and investigated by single crystal X-ray diffraction. Another ternary low temperature phase, τ5, was found only in the isothermal section at 550 °C around the composition AlGeNi4. This compound was found to crystallise in the Co2Si type structure (oP12, Pnma). The structure was identified by Rietveld refinement of powder data. The NiAs type (B8) phase based on binary Ge3Ni5 revealed an extended solid solubility of Al and the two isotypic compounds AlNi3 and GeNi3 form a complete solid solution. Based on DTA results, six vertical sections at 55, 60, 70, 75 and 80 at.% Ni and at a constant Al:Ni ratio of 1:3 were constructed. Furthermore, the liquidus surface projection and the reaction scheme (Scheil diagram) were completed by combining our results with previous results from the Ni-poor part of the phase diagram. Six invariant ternary reactions were identified in the Ni-rich part of the system. PMID:27087754

Structural, magnetic and Mossbauer studies of TI doped Gd2Fe17-xTix and Gd2Fe16Ga1-xTix (0≤x≤1)

NASA Astrophysics Data System (ADS)

Pokharel, G.; Syed Ali, K. S.; Mishra, S. R.

2015-05-01

Magnetic compounds of the type Gd2Fe17-xTix and Gd2Fe16Ga1-xTix (x=0.0-1.0) were prepared by arc melting and their structural and magnetic properties were studied by X-ray diffraction (XRD), magnetometery and Mossbauer spectroscopy. The Rietveld analysis of X-ray data shows that these α-Fe free solid-solutions crystallize with Th2Ni17-type structure as main phase along with GdFe2 and TiFe2 as additional phases at higher, x≥0.5 contents. The unit cell volume expands with Ga and Ti content. The Rietveld analysis indicate that both Ti and Ga atoms prefer 12j and 12k sites in both compounds. The effect of Ti and co-substituted Ga-Ti on the bond length are quite different. The saturation magnetization Ms, at 300 K for Gd2Fe17-xTix and Gd2Fe16Ga1-xTix was found to decrease linearly with increasing Ti content. The Ms in both compounds at x=1 reduced by 9% as compared to their parent compounds at x=0. The Curie temperature, Tc, for Gd2Fe17-xTix increased from 513 K (x=0) to 544 K (x=1) while Tc for Gd2Fe16Ga1-xTix reduced from 560 (x=0) to 544 K (x=1) with increase in Ti content. Thus the observed variation in Tc follows Gd2Fe17

Preparation of niobium based oxynitride nanosheets by exfoliation of Ruddlesden-Popper phase precursor

NASA Astrophysics Data System (ADS)

da Silva Maia, Ary; Cheviré, François; Demange, Valérie; Bouquet, Valérie; Pasturel, Mathieu; Députier, Stéphanie; Lebullenger, Ronan; Guilloux-Viry, Marylline; Tessier, Franck

2016-04-01

A new oxynitride Ruddlesden-Popper phase K1.6Ca2Nb3O9.4N0.6.1.1H2O was synthesized by the topochemical ammonolysis reaction at 700 °C from the oxide Dion-Jacobson phase KCa2Nb3O10 in the presence of K2CO3. The oxynitride showed good stability with a little loss of nitrogen, even after a few months of exposure to air. Its crystal structure was solved by Rietveld refinement of X-ray powder diffraction data in space group P4/mmm and considering a two-phase mixture, due to the difference in the degree of hydration, with a = 3.894(2) Å and c = 17.90(8) Å for the most hydrated phase and a = 3.927(6) Å and c = 17.09(2) Å for the less one. Optical band gaps were measured by diffuse reflectance in the UV-Visible range indicating a red shift of Eg to the visible region. The oxynitride layered perovskite was then protonated and exfoliated into nanosheets. TEM images and SAED patterns of the nanosheets proved that exfoliation was successful, showing lattice parameters quite compatible with the Rietveld refinement.

Synthesis, Crystal Structure, and Physical Properties of New Layered Oxychalcogenide La2O2Bi3AgS6

NASA Astrophysics Data System (ADS)

Hijikata, Yudai; Abe, Tomohiro; Moriyoshi, Chikako; Kuroiwa, Yoshihiro; Goto, Yosuke; Miura, Akira; Tadanaga, Kiyoharu; Wang, Yongming; Miura, Osuke; Mizuguchi, Yoshikazu

2017-12-01

We have synthesized a new layered oxychalcogenide La2O2Bi3AgS6. From synchrotron X-ray diffraction and Rietveld refinement, the crystal structure of La2O2Bi3AgS6 was refined using a model of the P4/nmm space group with a = 4.0644(1) Å and c = 19.412(1) Å, which is similar to the related compound LaOBiPbS3, while the interlayer bonds (M2-S1 bonds) are apparently shorter in La2O2Bi3AgS6. The tunneling electron microscopy (TEM) image confirmed the lattice constant derived from Rietveld refinement (c ˜ 20 Å). The electrical resistivity and Seebeck coefficient suggested that the electronic states of La2O2Bi3AgS6 are more metallic than those of LaOBiS2 and LaOBiPbS3. The insertion of a rock-salt-type chalcogenide into the van der Waals gap of BiS2-based layered compounds, such as LaOBiS2, will be a useful strategy for designing new layered functional materials in the layered chalcogenide family.

Synthesis, Rietveld refinements, Infrared and Raman spectroscopy studies of the sodium diphosphate NaCryFe1-yP2O7 (0 ≤ y ≤ 1)

NASA Astrophysics Data System (ADS)

Bih, H.; Saadoune, I.; Bih, L.; Mansori, M.; ToufiK, H.; Fuess, H.; Ehrenberg, H.

2016-01-01

In the present study we report on the synthesis and crystal structure studies of NaCryFe1-yP2O7 sodium diphosphate solid solution (0 ≤ y ≤ 1). The X-ray diffraction shows that these compounds are isostructural with NaFeP2O7 and NaCrP2O7 (space group P21/c (C2h5) Z = 4). The Rietveld refinements based on the XRD patterns show the existence of a continuous solid solution over the whole composition range (0 ≤ y ≤ 1). A continuous evolution of the monoclinic unit cell parameters was obtained. The transition metal ions (Cr3+ and/or Fe3+) connect the diphosphate anions forming a three-dimensional network with cages filled by Na+ cations. IR and Raman spectra have been interpreted using factor group analysis. A small shift of the band frequencies is observed when Fe is substituted by Cr. The POP bridge angles are determined from Lazarev's relation and agree well with those deduced from the crystal structure refinement.

Investigation of the Microstructure Evolution in a Fe-17Mn-1.5Al-0.3C Steel via In Situ Synchrotron X-ray Diffraction during a Tensile Test

PubMed Central

Song, Wenwen; Bleck, Wolfgang

2017-01-01

The quantitative characterization of the microstructure evolution in high-Mn steel during deformation is of great importance to understanding its strain-hardening behavior. In the current study, in situ high-energy synchrotron X-ray diffraction was employed to characterize the microstructure evolution in a Fe-17Mn-1.5Al-0.3C steel during a tensile test. The microstructure at different engineering strain levels—in terms of ε-martensite and α’-martensite volume fractions, the stacking fault probability, and the twin fault probability—was analyzed by the Rietveld refinement method. The Fe-17Mn-1.5Al-0.3C steel exhibits a high ultimate tensile strength with a superior uniform elongation and a high strain-hardening rate. The remaining high strain-hardening rate at the strain level about 0.025 to 0.35 results from ε-martensite dominant transformation-induced-plasticity (TRIP) effect. The increase in the strain-hardening rate at the strain level around 0.35 to 0.43 is attributed to the synergetic α’-martensite dominant TRIP and twinning-induced-plasticity (TWIP) effects. An evaluation of the stacking fault energy (SFE) of the Fe-17Mn-1.5Al-0.3C steel by the synchrotron measurements shows good agreement with the thermodynamic calculation of the SFE. PMID:28946692

Investigation of the Microstructure Evolution in a Fe-17Mn-1.5Al-0.3C Steel via In Situ Synchrotron X-ray Diffraction during a Tensile Test.

PubMed

Ma, Yan; Song, Wenwen; Bleck, Wolfgang

2017-09-25

The quantitative characterization of the microstructure evolution in high-Mn steel during deformation is of great importance to understanding its strain-hardening behavior. In the current study, in situ high-energy synchrotron X-ray diffraction was employed to characterize the microstructure evolution in a Fe-17Mn-1.5Al-0.3C steel during a tensile test. The microstructure at different engineering strain levels-in terms of ε-martensite and α'-martensite volume fractions, the stacking fault probability, and the twin fault probability-was analyzed by the Rietveld refinement method. The Fe-17Mn-1.5Al-0.3C steel exhibits a high ultimate tensile strength with a superior uniform elongation and a high strain-hardening rate. The remaining high strain-hardening rate at the strain level about 0.025 to 0.35 results from ε-martensite dominant transformation-induced-plasticity (TRIP) effect. The increase in the strain-hardening rate at the strain level around 0.35 to 0.43 is attributed to the synergetic α'-martensite dominant TRIP and twinning-induced-plasticity (TWIP) effects. An evaluation of the stacking fault energy (SFE) of the Fe-17Mn-1.5Al-0.3C steel by the synchrotron measurements shows good agreement with the thermodynamic calculation of the SFE.

Phase transitions of sodium niobate powder and ceramics, prepared by solid state synthesis

NASA Astrophysics Data System (ADS)

Koruza, J.; Tellier, J.; Malič, B.; Bobnar, V.; Kosec, M.

2010-12-01

Phase transitions of sodium niobate, prepared by the solid state synthesis method, were examined using dielectric measurements, differential scanning calorimetry, and high temperature x-ray diffraction, in order to contribute to the clarification of its structural behavior below 400 °C. Four phase transitions were detected in the ceramic sample using dielectric measurements and differential scanning calorimetry and the obtained temperatures were in a good agreement with previous reports for the transitions of the P polymorph. The anomaly observed by dielectric measurements in the vicinity of 150 °C was frequency dependent and could be related to the dynamics of the ferroelectric nanoregions. The phase transitions of the as-synthesized NaNbO3 powder were investigated using differential scanning calorimetry and high temperature x-ray diffraction. The results show the existence of the Q polymorph at room temperature, not previously reported for the powder, which undergoes a transition to the R polymorph upon heating through a temperature region between 265 and 326.5 °C. This transition is mainly related to the displacement of Na into a more symmetric position and a minor change in the tilting system. The structures at room temperature, 250, 300, and 420 °C were refined by the Rietveld method and the evolution of the tilting system of the octahedral network and cationic displacement are reported.

Structure elucidation of 3-[1-(6-methoxy-2-naphtyl)ethyl]-6-(2,4-dichlorophenyl)-7H-1,2,4-triazolo[3,4-b]-1,3,4-thiadiazine, C 23H 18Cl 2N 4OS from synchrotron X-ray powder diffraction

DOE Office of Scientific and Technical Information (OSTI.GOV)

Gündoğdu, Gülsüm; Aytaç, Sevim Peri; Müller, Melanie

The 3-[1-(6-methoxy-2-naphtyl)ethyl]-6-(2,4-dichlorophenyl)-7H-1,2,4-triazolo[3,4-b]-1,3,4-thiadiazine, C 23H 18Cl 2N 4OS compound was synthesized, as a member of the family of novel potential anticancer agents. The structure of the title compound was characterized by IR, 1H-NMR, mass spectroscopy, and elemental analysis, previously. In this study, the crystal structure of this compound has been determined from synchrotron X-ray powder diffraction data. The crystal structure was solved by simulated annealing and the final structure was achieved by Rietveld refinement method using soft restrains on all interatomic bond lengths and angles. This compound crystallizes in space groupP21,Z= 2, with the unit-cell parametersa= 15.55645(11) Å,b= 8.61693(6) Å,c= 8.56702(6)more » Å,β= 104.3270(4)°, andV= 1112.68(1) Å 3. In the crystal structure, strong C-H∙∙∙πand weak intermolecular hydrogen-bonding interactions link the molecules into a three-dimensional network. The molecules are in a head-to-head arrangement in the unit cell.« less

Tuning Thermoelectric Properties of Type I Clathrate K 8–x Ba x Al 8+x Si 38–x through Barium Substitution

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sui, Fan; Kauzlarich, Susan M.

2016-05-10

The thermal stability and thermoelectric properties of type I clathrate K8Al8Si38 up to 873 K are reported. K8Al8Si38 possesses a high absolute Seebeck coefficient value and high electrical resistivity in the temperature range of 323 to 873 K, which is consistent with previously reported low temperature thermoelectric properties. Samples with Ba partial substitution at the K guest atom sites were synthesized from metal hydride precursors. The samples with the nominal chemical formula of K8–xBaxAl8+xSi38–x (x = 1, 1.5, 2) possess type I clathrate structure (cubic, Pm3n), confirmed by X-ray diffraction. The guest atom site occupancies and thermal motions were investigatedmore » with Rietveld refinement of synchrotron powder X-ray diffraction. Transport properties of Ba-containing samples were characterized from 2 to 300 K. The K–Ba alloy phases showed low thermal conductivity and improved electrical conductivity compared to K8Al8Si38. Electrical resistivity and Seebeck coefficients were measured over the temperature range of 323 to 873 K. Thermal conductivity from 323 to 873 K was estimated from the Wiedemann–Franz relation and lattice thermal conductivity extrapolation from 300 to 873 K. K8–xBaxAl8+xSi38–x (x = 1, 1.5) synthesized with Al deficiency showed enhanced electrical conductivity, and the absolute Seebeck coefficients decrease with the increased carrier concentration. When x = 2, the Al content increases toward the electron balanced composition, and the electrical resistivity increases with the decreasing charge carrier concentration. Overall, K6.5Ba1.5Al9Si37 achieves an enhanced zT of 0.4 at 873 K.« less

In-situ early-age hydration study of sulfobelite cements by synchrotron powder diffraction

DOE Office of Scientific and Technical Information (OSTI.GOV)

Álvarez-Pinazo, G.; Cuesta, A.; García-Maté, M.

Eco-friendly belite calcium sulfoaluminate (BCSA) cement hydration behavior is not yet well understood. Here, we report an in-situ synchrotron X-ray powder diffraction study for the first hours of hydration of BCSA cements. Rietveld quantitative phase analysis has been used to establish the degree of reaction (α). The hydration of a mixture of ye'elimite and gypsum revealed that ettringite formation (α ∼ 70% at 50 h) is limited by ye'elimite dissolution. Two laboratory-prepared BCSA cements were also studied: non-active-BCSA and active-BCSA cements, with β- and α′{sub H}-belite as main phases, respectively. Ye'elimite, in the non-active-BCSA system, dissolves at higher pace (αmore » ∼ 25% at 1 h) than in the active-BCSA one (α ∼ 10% at 1 h), with differences in the crystallization of ettringite (α ∼ 30% and α ∼ 5%, respectively). This behavior has strongly affected subsequent belite and ferrite reactivities, yielding stratlingite and other layered phases in non-active-BCSA. The dissolution and crystallization processes are reported and discussed in detail. -- Highlights: •Belite calcium sulfoaluminate cements early hydration mechanism has been determined. •Belite hydration strongly depends on availability of aluminum hydroxide. •Orthorhombic ye’elimite dissolved at a higher pace than cubic one. •Ye’elimite larger reaction degree yields stratlingite formation by belite reaction. •Rietveld method quantified gypsum, anhydrite and bassanite dissolution rates.« less

Synthesis and characterization of FeSe1-xTex (x=0, 0.5, 1) superconductors

NASA Astrophysics Data System (ADS)

Zargar, Rayees A.; Hafiz, A. K.; Awana, V. P. S.

2015-08-01

In this study, FeTe1-xSex (x=0,0.5,1) samples were prepared by conventional solid state reaction method and investigated by powder XRD, SEM, Raman and resistivity measurement techniques to reveal the effect of tellurium (Te) substitution in FeSe matrix. Rietveld analysis was performed on room temperature recorded, X-ray diffraction (XRD) patterns of pure FeSe, FeTe and FeSe0.5Te0.5 which shows that all the compounds are crystallized in a tetragonal structure. SEM images show the dense surface morphology. Raman spectra recorded in the range from 100 to 700 cm-1 at ambient temperature has been interpreted by P4/nmm space group of the lattice. The variation in intensity and shift in peak positions of some phonon modes has been discussed on the basis of variation in crystalline field effect by substituting Te in FeSe lattice. The resistivity versus temperature curves reveals that FeSe becomes superconductor at 7 K and FeSe0.5Te0.5 shows superconductivity below 14 K while FeTe is non-superconducting compound.

Structure determination of two structural analogs, named 3-[1-(2-fluoro-4-biphenyl)ethyl]-6-(4-fluorophenyl)-1,2,4-triazolo[3,4-b]-1,3,4-thiadiazole (C23H16F2N4S) and 3-[1-(2-fluoro-4-biphenyl)ethyl]-6-(4-chlorophenyl)-1,2,4-triazolo[3,4-b]-1,3,4-thiadiazole (C23H16ClFN4S) by synchrotron X-ray powder diffraction

DOE Office of Scientific and Technical Information (OSTI.GOV)

Gündoğdu, Gülsüm; Aytaç, Sevim Peri; Müller, Melanie

Two novel compounds, 3-[1-(2-fluoro-4-biphenyl)ethyl]-6-(4-fluorophenyl)-1,2,4-triazolo[3,4-b]-1,3,4-thiadiazole (C 23H 16F 2N 4S) (1) and 3-[1-(2-fluoro-4-biphenyl)ethyl]-6-(4-chlorophenyl)-1,2,4-triazolo[3,4-b]-1,3,4-thiadiazole (C 23H 16ClFN 4S) (2), have been designed and synthesized as cytotoxic agents. The compounds were characterized by infrared, proton nuclear magnetic resonance, mass spectral data, elemental analysis and X-ray powder diffraction. The present study comprises spectral data and crystal structures of these novel compounds determined from synchrotron X-ray powder diffraction data. The structure solutions were obtained by simulated annealing. The final structures were achieved by Rietveld refinement using soft restraints for all bond lengths, bond angles, and planar groups. Both compounds crystallize in space groupmore » $$P\\bar 1$$,Z= 2, with the unit-cell parametersa= 6.37433(9),b= 11.3641(2),c= 14.09115(19) Å,α= 80.1740(8)°,β= 85.1164(8)°,γ= 80.9831(10)°,V= 991.55(3) Å 3of compound (1) anda= 6.53736(6),b= 11.55725(15),c= 14.01373(13) Å,α= 80.3323(7)°,β= 84.8939(6)°,γ= 79.3954(8)°,V= 1024.08(2) Å 3of compound (2). Structural analyses reveal that the title compounds are isostructural.« less

Brillouin function characteristics for La-Co substituted barium hexaferrites

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wu, Chuanjian, E-mail: wcjuestc2005@gmail.com, E-mail: ksun@uestc.edu.cn; Yu, Zhong; Sun, Ke, E-mail: wcjuestc2005@gmail.com, E-mail: ksun@uestc.edu.cn

2015-09-14

La-Co substituted barium hexaferrites with the chemical formula of Ba{sub 1−x}La{sub x}Fe{sub 12−x}Co{sub x}O{sub 19} (x = 0.0, 0.1, 0.3, and 0.5), prepared by a conventional ceramic method, were systematically investigated by Raman spectra, X-ray photoelectron spectroscopy, Rietveld refinement of X-ray diffraction patterns, and vibrating sample magnetometer. The result manifests that all the compounds are crystallized in magnetoplumbite hexagonal structure. Trivalent cobalt ions prevailingly occupy the 2a, 4f{sub 1}, and 12k sites. According to Néel model of collinear-spin ferrimagnetism, the molecular-field coefficients ω{sub bf2}, ω{sub kf1}, ω{sub af1}, ω{sub kf2}, and ω{sub bk} of La-Co substituted barium hexaferrites have been calculated usingmore » the nonlinear fitting method, and the magnetic moment of five sublattices (2a, 2b, 4f{sub 1}, 4f{sub 2}, and 12k) versus temperature T has been also investigated. The fitting results are coincided well with the experimental data. Moreover, with the increase of La-Co substitution amount x, the molecular-field coefficients ω{sub bf2} and ω{sub af1} decrease constantly, while the molecular-field coefficients ω{sub kf1}, ω{sub kf2}, and ω{sub bk} show a slight change.« less

Diffraction leveraged modulation of X-ray pulses using MEMS-based X-ray optics

DOEpatents

Lopez, Daniel; Shenoy, Gopal; Wang, Jin; Walko, Donald A.; Jung, Il-Woong; Mukhopadhyay, Deepkishore

2016-08-09

A method and apparatus are provided for implementing Bragg-diffraction leveraged modulation of X-ray pulses using MicroElectroMechanical systems (MEMS) based diffractive optics. An oscillating crystalline MEMS device generates a controllable time-window for diffraction of the incident X-ray radiation. The Bragg-diffraction leveraged modulation of X-ray pulses includes isolating a particular pulse, spatially separating individual pulses, and spreading a single pulse from an X-ray pulse-train.

Crystallite size strain analysis of nanocrystalline La0.7Sr0.3MnO3 perovskite by Williamson-Hall plot method

NASA Astrophysics Data System (ADS)

Kumar, Dinesh; Verma, Narendra Kumar; Singh, Chandra Bhal; Singh, Akhilesh Kumar

2018-04-01

The nanocrystalline Sr-doped LaMnO3 (La0.7Sr0.3MnO3 = LSMO) perovskite manganites having different crystallite size were synthesized using the nitrate-glycine auto-combustion method. The phase purity of the manganites was checked by X-ray diffraction (XRD) measurement. The XRD patterns of the sample reveal that La0.7S0.3MnO3 crystallizes into rhombohedral crystal structure with space group R-3c. The size-dependence of structural lattice parameters have been investigated with the help of Rietveld refinement. The structural parameters increase as a function of crystallite size. The crystallite-size and internal strain as a function of crystallite-size have been calculated using Williamson-Hall plot.

Giant dielectric permittivity and weak ferromagnetic behavior in Bi{sub 0.5}La{sub 0.5}Fe{sub 0.5}Cr{sub 0.5}O{sub 3} ceramic

DOE Office of Scientific and Technical Information (OSTI.GOV)

Tirupathi, Patri; Raju, K.; Peetla, Naresh

A pervoskite (Bi{sub 0.5}La{sub 0.5})(Fe{sub 0.5}Cr{sub 0.5})O{sub 3} (BLFC) nanoparticles were synthesized by high energy ball milling. Rietveld refined X-ray diffraction studies revealed that this compound shows orthorhombic structure with Pbnm space group. The dielectric studies were investigated in wide frequency (10{sup 2}-10{sup 6}) range indicating giant dielectric permittivity behavior similar to LaFeO{sub 3} ceramic. The noted dielectric loss relaxation frequency dependent is as following the Arrhenius law can be ascribed as polaronic conduction. Further, magnetic transition at around 337 K and coexistence of weak ferromagnetic and antiferromagnetic behavior is observed below magnetic transition.

Structural analysis of zeolite NaA synthesized by a cost-effective hydrothermal method using kaolin and its use as water softener.

PubMed

Loiola, A R; Andrade, J C R A; Sasaki, J M; da Silva, L R D

2012-02-01

Zeolite 4A (LTA) has been successfully synthesized by a hydrothermal method, where kaolin was used as silica and alumina source. The synthesized zeolite was characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), laser granulometry, and FTIR spectroscopy. XRD data from the Rietveld refinement method confirmed only one crystallographic phase. Zeolite A morphology was observed by SEM analysis, and it showed well-defined crystals with slightly different sizes but with the same cubic shape. Particle size distribution of the crystals was confirmed by laser granulometry, whereas FTIR spectroscopy revealed significant structural differences between the starting material and the final zeolite product used as water softener. Copyright © 2010 Elsevier Inc. All rights reserved.

Structural and optical properties of Nd- and Tb-doped BaY 2F 8

NASA Astrophysics Data System (ADS)

Valerio, Mário E. G.; Ribeiro, Viviane G.; de Mello, Ana C. S.; dos Santos, Marcos A. C.; Baldochi, Sonia L.; Mazzocchi, Vera L.; Parente, Carlos B. R.; Jackson, Robert A.; Amaral, Jomar B.

2007-09-01

In the present work, we report the optical properties of rare-earth doped BaY2F8 and its potential use as a scintillator in radiation detection. The samples were synthesized and grown by the zone melting method under a HF flow. X-ray powder diffraction was performed and quantitative phase analysis was done using the Rietveld method. Emission and excitation spectra of the doped samples were measured at room temperature. The identification of the transitions was done comparing the excitation and emission peaks with the results obtained from computer modelling. The scintillator properties of the pure and doped samples were checked by measuring the radioluminescence of the sample when excited with different types of radiation, revealing that these materials are promising radiation detectors.

Thermochemistry of Rare Earth Silicates for Environmental Barrier Coatings

NASA Technical Reports Server (NTRS)

Costa, Gustavo; Jacobson, Nathan

2015-01-01

Rare earth silicates are promising candidates as environmental protective coatings (EBCs) for silica-forming ceramics and composites in combustion environments since they are predicted to have lower reactivity with the water vapor combustion products. The reactivity of rare earth silicates is assessed by the thermodynamic activity of the silica component which is best measured by Knudsen effusion mass spectrometry (KEMS). Here, we discuss a novel method based on a reducing agent to increase the partial pressure of SiO(g) which is then used to calculate thermodynamic activity of silica in Y2O3-SiO2 and Yb2O3-SiO2 systems. After the KEMS measurements, samples were probed by X-ray diffraction and their phase content was calculated from Rietveld refinement.

Experimental and first principle study of the structure, electronic, optical and luminescence properties of M-type GdNbO4 phosphor

NASA Astrophysics Data System (ADS)

Ding, Shoujun; Zhang, Haotian; Zhang, Qingli; Chen, Yuanzhi; Dou, Renqin; Peng, Fang; Liu, Wenpeng; Sun, Dunlu

2018-06-01

In this work, GdNbO4 polycrystalline with monoclinic phase was prepared by traditional high-temperature solid-state reaction. Its structure was determined by X-ray diffraction and its unit cell parameters were obtained with Rietveld refinement method. Its luminescence properties (including absorbance, emission and luminescence lifetime) were investigated with experiment method and the CIE chromaticity coordinate was presented. Furthermore, a systematic theoretical calculation (including band gap, density of states and optical properties) based on the density function theory methods was performed on GdNbO4. Lastly, a comparison between experiment and calculated results was conducted. The calculated and experiment results obtained in this work can provide an essential understanding of GdNbO4 material.

Mineralogy, Provenance, and Diagenesis of a Potassic Basaltic Sandstone on Mars: CheMin X-Ray Diffraction of the Windjana Sample (Kimberley Area, Gale Crater)

NASA Technical Reports Server (NTRS)

Treiman, Allan H.; Bish, David L.; Vaniman, David T.; Chipera, Steve J.; Blake, David F.; Ming, Doug W.; Morris, Richard V.; Bristow, Thomas F.; Morrison, Shaunna M.; Baker, Michael B.;

Mineralogy, provenance, and diagenesis of a potassic basaltic sandstone on Mars: CheMin X-ray diffraction of the Windjana sample (Kimberley area, Gale Crater)

DOE Office of Scientific and Technical Information (OSTI.GOV)

Treiman, Allan H.; Bish, David L.; Vaniman, David T.

The Windjana drill sample, a sandstone of the Dillinger member (Kimberley formation, Gale Crater, Mars), was analyzed by CheMin X-ray diffraction (XRD) in the MSL Curiosity rover. From Rietveld refinements of its XRD pattern, Windjana contains the following: sanidine (21% weight, ~Or 95); augite (20%); magnetite (12%); pigeonite; olivine; plagioclase; amorphous and smectitic material (~25%); and percent levels of others including ilmenite, fluorapatite, and bassanite. From mass balance on the Alpha Proton X-ray Spectrometer (APXS) chemical analysis, the amorphous material is Fe rich with nearly no other cations—like ferrihydrite. The Windjana sample shows little alteration and was likely cemented bymore » its magnetite and ferrihydrite. From ChemCam Laser-Induced Breakdown Spectrometer (LIBS) chemical analyses, Windjana is representative of the Dillinger and Mount Remarkable members of the Kimberley formation. LIBS data suggest that the Kimberley sediments include at least three chemical components. The most K-rich targets have 5.6% K 2O, ~1.8 times that of Windjana, implying a sediment component with >40% sanidine, e.g., a trachyte. A second component is rich in mafic minerals, with little feldspar (like a shergottite). A third component is richer in plagioclase and in Na 2O, and is likely to be basaltic. The K-rich sediment component is consistent with APXS and ChemCam observations of K-rich rocks elsewhere in Gale Crater. The source of this sediment component was likely volcanic. Finally, the presence of sediment from many igneous sources, in concert with Curiosity's identifications of other igneous materials (e.g., mugearite), implies that the northern rim of Gale Crater exposes a diverse igneous complex, at least as diverse as that found in similar-age terranes on Earth.« less

Mineralogy, provenance, and diagenesis of a potassic basaltic sandstone on Mars: CheMin X-ray diffraction of the Windjana sample (Kimberley area, Gale Crater)

DOE PAGES

Treiman, Allan H.; Bish, David L.; Vaniman, David T.; ...

2015-12-27

The Windjana drill sample, a sandstone of the Dillinger member (Kimberley formation, Gale Crater, Mars), was analyzed by CheMin X-ray diffraction (XRD) in the MSL Curiosity rover. From Rietveld refinements of its XRD pattern, Windjana contains the following: sanidine (21% weight, ~Or 95); augite (20%); magnetite (12%); pigeonite; olivine; plagioclase; amorphous and smectitic material (~25%); and percent levels of others including ilmenite, fluorapatite, and bassanite. From mass balance on the Alpha Proton X-ray Spectrometer (APXS) chemical analysis, the amorphous material is Fe rich with nearly no other cations—like ferrihydrite. The Windjana sample shows little alteration and was likely cemented bymore » its magnetite and ferrihydrite. From ChemCam Laser-Induced Breakdown Spectrometer (LIBS) chemical analyses, Windjana is representative of the Dillinger and Mount Remarkable members of the Kimberley formation. LIBS data suggest that the Kimberley sediments include at least three chemical components. The most K-rich targets have 5.6% K 2O, ~1.8 times that of Windjana, implying a sediment component with >40% sanidine, e.g., a trachyte. A second component is rich in mafic minerals, with little feldspar (like a shergottite). A third component is richer in plagioclase and in Na 2O, and is likely to be basaltic. The K-rich sediment component is consistent with APXS and ChemCam observations of K-rich rocks elsewhere in Gale Crater. The source of this sediment component was likely volcanic. Finally, the presence of sediment from many igneous sources, in concert with Curiosity's identifications of other igneous materials (e.g., mugearite), implies that the northern rim of Gale Crater exposes a diverse igneous complex, at least as diverse as that found in similar-age terranes on Earth.« less

Magnetization reversal in orthorhombic Sr-doped LaFe0.5Cr0.5O3–δ

NASA Astrophysics Data System (ADS)

Coutinho, P. V.; Moreno, N. O.; Ochoa, E. A.; da Costa, M. E. H. Maia; Barrozo, Petrucio

2018-06-01

In this paper we studied the reversal magnetization of La1‑x Sr x Fe0.5Cr0.5O3‑δ (x  =  0, 0.1 and 0.2) samples produced by combustion synthesis. The structural analysis was carried out by x-ray diffraction with Rietveld analysis. These analyses revealed that all samples have an orthorhombic structure with space group Pbnm (62) and that the Sr-doping induces a decrease of the lattice parameter. The x-ray photoelectron spectroscopy analysis indicates that the Sr-doping favor the change of the valence states of the Fe3+ to Fe4+. The magnetization as a function of the temperature reveals an unusual magnetic behavior with a reversal of magnetization. The increase of the Sr content induces a decrease of the temperature where occurs an inversion of the magnetization and do the value of the magnetization at 5 K more negative. This effect is attributed to the increase of the concentration of Fe4+ with increasing of the Sr content. The Fe and Cr with a valence of 4+  act as paramagnetic impurities in the antiferromagnetic lattice and are responsible for the changes in the magnetic behavior.

Accurate solid solution range of BiMnxFe3-xO6 and low temperature magnetism

NASA Astrophysics Data System (ADS)

Jiang, Pengfei; Yue, Mufei; Cong, Rihong; Gao, Wenliang; Yang, Tao

2017-11-01

BiMnxFe3-xO6 (x = 1) represents a new type of oxide structure containing Bi3+ and competing magnetic super-exchanges. In literature, multiple magnetic states were realized at low temperatures in BiMnFe2O6, and the hypothetical parent compounds (BiMn3O6, BiFe3O6) were predicted to be different in magnetism. Herein, we performed a careful study on the syntheses of BiMnxFe3-xO6 at ambient pressure, and the solid solution range was determined to be 0.9 ≤ x ≤ 1.3 by Rietveld refinements on high-quality powder X-ray diffraction data. Due to the very similar cationic size of Mn3+ and Fe3+, and possibly the structural rigidity, there was no significant structure change in the whole range of solid solution. The magnetic behavior of BiMnxFe3-xO6 (x = 1.2, 1.22, 1.26, 1.28 and 1.3) was generally similar to BiMnFe2O6, while the relative higher concentration of Mn3+ led to the decreasing of the antiferromagnetic ordering temperature.

Iron insertion and hematite segregation on Fe-doped TiO2 nanoparticles obtained from sol-gel and hydrothermal methods.

PubMed

Santos, Reginaldo da S; Faria, Guilherme A; Giles, Carlos; Leite, Carlos A P; Barbosa, Herbert de S; Arruda, Marco A Z; Longo, Claudia

2012-10-24

Iron-doped TiO(2) (Fe:TiO(2)) nanoparticles were synthesized by the sol-gel method (with Fe/Ti molar ratio corresponding to 1, 3, and 5%), followed by hydrothermal treatment, drying, and annealing. A similar methodology was used to synthesize TiO(2) and α-Fe(2)O(3) nanoparticles. For comparison, a mixture hematite/titania, with Fe/Ti = 4% was also investigated. Characterization of the samples using Rietveld refinement of X-ray diffraction data revealed that TiO(2) consisted of 82% anatase and 18% brookite; for Fe:TiO(2), brookite increased to 30% and hematite was also identified (0.5, 1.0, and 1.2 wt % for samples prepared with 1, 3, and 5% of Fe/Ti). For hematite/titania mixture, Fe/Ti was estimated as 4.4%, indicating the Rietveld method reliability for estimation of phase composition. Because the band gap energy, estimated as 3.2 eV for TiO(2), gradually ranged from 3.0 to 2.7 eV with increasing Fe content at Fe:TiO(2), it can be assumed that a Fe fraction was also inserted as dopant in the TiO(2) lattice. Extended X-ray absorption fine structure spectra obtained for the Ti K-edge and Fe K-edge indicated that absorbing Fe occupied a Ti site in the TiO(2) lattice, but hematite features were not observed. Hematite particles also could not be identified in the images obtained by transmission electron microscopy, in spite of iron identification by elemental mapping, suggesting that hematite can be segregated at the grain boundaries of Fe:TiO(2).

Electrical Properties and Dipole Relaxation Behavior of Zinc-Substituted Cobalt Ferrite

NASA Astrophysics Data System (ADS)

Supriya, Sweety; Kumar, Sunil; Kar, Manoranjan

2017-12-01

Co1- x Zn x Fe2O4 ceramics with x = 0.00, 0.05, 0.10, 0.15 and 0.20 were synthesized by a modified citric acid sol-gel method. The crystalline phase of the samples was characterized by the powder x-ray diffraction technique (XRD) and the Rietveld analysis of the XRD patterns. The morphology and particle size were studied using field emission scanning electron microscopy. Fourier transform infrared spectroscopy studies were consistent with the XRD results. The impedance measurements were carried out from 100 Hz to 10 MHz at different temperatures from 40°C to 300°C. The frequency dispersion of dielectric was analyzed with a modified Debye equation. The activation energy derived from the dielectric constant and the impedance follows the Arrhenius law and are comparable with each other. The dielectric relaxation and impedance relaxation are correlated in terms of activation energy, show a good temperature stability of the dielectrics and are useful for their applications in microelectronic devices such as filters, capacitors, resonators, etc.

Spin canting and magnetic transition in NixZn1-xFe2O4 (x=0.0, 0.5 and 1.0) nanoparticles

NASA Astrophysics Data System (ADS)

Rani, Stuti; Raghav, Dharmendra Singh; Yadav, Prashant; Varma, G. D.

2018-04-01

Nanoparticles of NixZn1-xFe2O4(x=0.0, 0.5 and 1.0) have been synthesized via co-precipitation method and studied thestructural and magnetic properties. Rietveld refinement of X ray diffraction data of as synthesized samples revealthat the samples have mixed spinel structure with space group Fd-3m. The lattice parameter of the samples decreases as doping concentration of Ni ions increases. Magnetic measurements show paramagnetic to ferrimagnetic transition at room temperature on Ni doping in ZnFe2O4 nanoparticles. The magnetic measurements also show spin canting in samples possibly due to their nanocrystalline nature. The spin canting angles have been calculated with the help of Yafet-Kittel (Y-K) model. Furthermore, the Law of approach (LA) fitting of M-H curves indicates that the samples are highly anisotropicin nature. The Arrot plots of as synthesized samples also indicate the paramagnetic to ferrimagnetic transition. The correlation between the structural and observed magnetic properties of NixZn1-xFe2O4(x=0.0, 0.5 and 1.0) nanocrystals will be described and discussed in this paper.

Structural and magnetic characterizations of Co2FeGa/SiO2 nanoparticles prepared via chemical route

NASA Astrophysics Data System (ADS)

Priyanka, Dhaka, Rajendra S.

2018-04-01

We report the synthesis of Co2FeGa/SiO2 nanoparticles by sol-gel method and characterization usingx-ray diffraction (XRD), transmission electron microscopy (TEM) and magnetic measurements. The Rietveld refinementsof XRD data with space group Fm-3m clearly show the formation of A2 disordersingle phase and the lattice constant isfound to be 5.738 Å. The energy-dispersive x-ray spectroscopy (EDX) confirm the elemental composition close the desired values. The value of coercivity is found to be around 283 Oe and 126 Oe, measured at 10 K and 300 K, respectively. We observed the saturation magnetization significantly lower than expected from Slater-Pauling rule. This decrease in the magnetic moment might be due to the presence of amorphous SiO2 during the synthesis process. A large content of small size SiO2 particles along with Co2FeGa nanoparticles are also found in TEM study.

Single phase Pb0.7Bi0.3Fe0.65Nb0.35O3 multiferroic: Neutron diffraction, impedance and modulus studies

NASA Astrophysics Data System (ADS)

Dadami, Sunanda T.; Matteppanvar, Shidaling; Shivaraja, I.; Rayaprol, Sudhindra; Deshpande, S. K.; Angadi, Basavaraj

2018-04-01

The Pb0.7Bi0.3Fe0.65Nb0.35O3 (PBFNO) multiferroic solid solution was synthesized by using single step solid state reaction method. Single phase formation was confirmed through room temperature (RT) X Ray Diffraction (XRD) and Neutron Diffraction (ND). Rietveld refinement was used to perform the structural analysis using FullProf Suite program. RT XRD and ND patterns well fitted with monoclinic structure (Cm space group) and cell parameters from the ND data are found to be a = 5.6474(4) Å, b = 5.6415(3) Å, c = 3.9992(3) Å and β = 89.95(2)°. ND data at RT exhibits G-type antiferromagnetic structure. The electrical properties (impedance and modulus) of PBFNO were studied as a function of frequency (100 Hz - 5 MHz) and temperature (133 K - 293 K) by Impedance spectroscopy technique. Impedance and modulus spectroscopy studies confirm the contribution to the conductivity is from grains only and the relaxation is of non-Debye type. The PBFNO sample exhibits negative temperature coefficient of resistance (NTCR) behaviour. PBFNO is found be a potential candidate for RT applications.

Crystallographic site swapping of La3+ ion in BaA'LaTeO6 (A' = Na, K, Rb) double perovskite type compounds: diffraction and photoluminescence evidence for the site swapping.

PubMed

Phatak, R; Gupta, S K; Krishnan, K; Sali, S K; Godbole, S V; Das, A

2014-02-28

Double perovskite type compounds of the formula BaA'LaTeO6 (A' = Na, K, Rb) were synthesized by solid state route and their crystal structures were determined by Rietveld analysis using powder X-ray diffraction and neutron diffraction data. Na compound crystallizes in the monoclinic system with P2₁/n space group whereas, K and Rb compounds crystallize in Fm3m space group. All the three compounds show rock salt type ordering at B site. Crystal structure analysis shows that La ion occupies A site in Na compound whereas, it occupies B site in K and Rb compounds according to the general formula of AA'BB'O6 for a double perovskite type compound. Effect of this crystallographic site swapping of the La ion was also observed in the photoluminescence study by doping Eu(3+) in La(3+) site. The large decrease in the intensity of the electric dipole ((5)D0-(7)F2) transition in the Rb compound compared to the Na compound indicates that Eu(3+) ion resides in the centrosymmetric octahedral environment in the Rb compound.

X-Ray Amorphous Phases in Antarctica Dry Valley Soils: Insight into Aqueous Alteration Processes on Mars?

NASA Technical Reports Server (NTRS)

Ming, D. W.; Morris, R. V.; Rampe, E. B.; Golden, D. C.; Quinn, J. E.

2015-01-01

The Chemistry and Mineralogy (CheMin) instrument onboard the Mars Curiosity rover has detected abundant amounts (approx. 25-30 weight percentage) of X-ray amorphous materials in a windblown deposit (Rocknest) and in a sedimentary mudstone (Cumberland and John Klein) in Gale crater, Mars. On Earth, X-ray amorphous components are common in soils and sediments, but usually not as abundant as detected in Gale crater. One hypothesis for the abundant X-ray amorphous materials on Mars is limited interaction of liquid water with surface materials, kinetically inhibiting maturation to more crystalline phases. The objective of this study was to characterize the chemistry and mineralogy of soils formed in the Antarctica Dry Valleys, one of the driest locations on Earth. Two soils were characterized from different elevations, including a low elevation, coastal, subxerous soil in Taylor Valley and a high elevation, ultraxerous soil in University Valley. A variety of techniques were used to characterize materials from each soil horizon, including Rietveld analysis of X-ray diffraction data. For Taylor Valley soil, the X-ray amorphous component ranged from about 4 weight percentage in the upper horizon to as high as 15 weight percentage in the lowest horizon just above the permafrost layer. Transmission electron microscopy indicated that the presence of short-range ordered (SRO) smectite was the most likely candidate for the X-ray amorphous materials in the Taylor Valley soils. The SRO smectite is likely an aqueous alteration product of mica inherited from granitic materials during glaciation of Taylor Valley. The drier University Valley soils had lower X-ray amorphous contents of about 5 weight percentage in the lowest horizon. The X-ray amorphous materials in University Valley are attributed to nanoparticles of TiO2 and possibly amorphous SiO2. The high abundance of X-ray amorphous materials in Taylor Valley is surprising for one of the driest places on Earth. These materials may have been physically and chemical altered during soil formation, however, the limited interaction with water and low temperatures may result in the formation of "immature" X-ray amorphous or SRO materials. Perhaps, a similar process contributes to the formation of the high content of X-ray amorphous materials detected on Mars.

Structural, Optical, and Electronic Characterization of Fe-Doped Alumina Nanoparticles

NASA Astrophysics Data System (ADS)

Heiba, Zein K.; Mohamed, Mohamed Bakr; Wahba, Adel Maher; Imam, N. G.

2018-01-01

The effects of iron doping on the structural, optical, and electronic properties of doped alumina have been studied. Single-phase iron-doped alumina Al2- x Fe x O3 ( x = 0.00 to 0.30) nanoparticles were synthesized via citrate-precursor method. Formation of single-phase hexagonal corundum structure with no other separate phases was demonstrated by x-ray diffraction (XRD) analysis and Fourier-transform infrared spectroscopy. The effects of iron doping on the α-Al2O3 structural parameters, viz. atomic coordinates, lattice parameters, crystallite size, and microstrain, were estimated from XRD data by applying the Rietveld profile fitting method. Transmission electron microscopy further confirmed the nanosize nature of the prepared samples with size ranging from 12 nm to 83 nm. The electronic band structure was investigated using density functional theory calculations to explain the decrease in the energy gap of Al2- x Fe x O3 as the amount of Fe was increased. The colored emission peaks in the visible region (blue, red, violet) of the electromagnetic spectrum obtained for the Fe-doped α-Al2O3 nanoparticles suggest their potential application as ceramic nanopigments.

Micro X-ray diffraction analysis of thin films using grazing-exit conditions.

PubMed

Noma, T; Iida, A

1998-05-01

An X-ray diffraction technique using a hard X-ray microbeam for thin-film analysis has been developed. To optimize the spatial resolution and the surface sensitivity, the X-ray microbeam strikes the sample surface at a large glancing angle while the diffracted X-ray signal is detected with a small (grazing) exit angle. Kirkpatrick-Baez optics developed at the Photon Factory were used, in combination with a multilayer monochromator, for focusing X-rays. The focused beam size was about 10 x 10 micro m. X-ray diffraction patterns of Pd, Pt and their layered structure were measured. Using a small exit angle, the signal-to-background ratio was improved due to a shallow escape depth. Under the grazing-exit condition, the refraction effect of diffracted X-rays was observed, indicating the possibility of surface sensitivity.

Chemical Reduction of Nd 1.85 Ce 0.15 CuO 4− δ Powders in Supercritical Sodium Ammonia Solutions

DOE PAGES

Dias, Yasmin; Wang, Hui; Zhou, Haiqing; ...

2015-01-01

Nd 1.85 Ce 0.15 CuO 4− δ powders are chemically reduced in supercritical sodium ammonia solutions from room temperature to 350°C. The crystallographic structure of the reduced powders is investigated from Rietveld refinement of X-ray powder diffraction. The atomic positions are maintained constant within experimental errors while temperature factors of all atoms increase significantly after the chemical treatments, especially of Nd/Ce atoms. The ammonothermally reduced Nd 1.85 Ce 0.15 CuO 4− δ powders show diamagnetic below 24 K which is contributed to the lower oxygen content and higher temperature factors of atoms in the treated compound. Themore » ammonothermal method paves a new way to reduce oxides in supercritical solutions near room temperature.« less

Fabrication of Far Red Emission Phosphors Y3Al5O12:Eu(YAG:Eu) by Co-precipitation Method

NASA Astrophysics Data System (ADS)

Thu, L. D.; Trung, D. Q.; Lam, T. D.; Anh, T. X.

2016-05-01

Phosphors YAG:Eu (with seven molar percent of Eu to YAG) was synthesized by the co-precipitation method using NH3 solution as a precipitating agent. X-ray diffraction (XRD) patterns show that the samples are single phase, and the crystallinity starts forming at a sintering temperature of 1000°C. The crystallinity increases with the increasing sintered temperature. XRD studies followed by Rietveld refinement confirmed the body center cubic structure of the host lattice. The crystalline YAG:Eu showed four emission bands of europium ion with the force dipole transition ascribed to 5D0-7F4 located at 710 nm as the most dominating group (far-red emission—FR). The ratio of FR/OR (far-red/orange—red) is about 1.24 in all samples.

Cubic to tetragonal phase transition of Tm{sup 3+} doped nanocrystals in oxyfluoride glass ceramics

DOE Office of Scientific and Technical Information (OSTI.GOV)

Li, Yiming; Fu, Yuting; Shi, Yahui

2016-02-15

Tm{sup 3+} ions doped β-PbF{sub 2} nanocrystals in oxyfluoride glass ceramics with different doping concentrations and thermal temperatures are prepared by a traditional melt-quenching and thermal treatment method to investigate the structure and the phase transition of Tm{sup 3+} doped nanocrystals. The structures are characterized by X-ray diffraction Rietveld analysis and confirmed with numerical simulation. The phase transitions are proved further by the emission spectra. Both of the doping concentration and thermal temperature can induce an O{sub h} to D{sub 4h} site symmetry distortion and a cubic to tetragonal phase transition. The luminescence of Tm{sup 3+} doped nanocrystals at 800more » nm was modulated by the phase transition of the surrounding crystal field.« less

Studies of ferroelectric and dielectric properties of pure and doped barium titanate prepared by sol-gel method

NASA Astrophysics Data System (ADS)

Bisen, Supriya; Mishra, Ashutosh; Jarabana, Kanaka M.

2016-05-01

In this work, Barium Titanate (BaTiO3) powders were synthesized via Sol-Gel auto combustion method using citric acid as a chelating agent. We study the behavior of ferroelectric and dielectric properties of pure and doped BaTiO3 on different concentration. To understand the phase and structure of the powder calcined at 900°C were characterized by X-ray Diffraction shows that tetragonal phase is dominant for pure and doped BTO and data fitted by Rietveld Refinement. Electric and Dielectric properties were characterized by P-E Hysteresis and Dielectric measurement. In P-E measurement ferroelectric loop tracer applied for different voltage. The temperature dependant dielectric constant behavior was observed as a function of frequency recorded on hp-Hewlett Packard 4192A, LF impedance, 5Hz-13Hz analyzer.

Pressure-Stabilized Cubic Perovskite Oxyhydride BaScO2H.

PubMed

Goto, Yoshihiro; Tassel, Cédric; Noda, Yasuto; Hernandez, Olivier; Pickard, Chris J; Green, Mark A; Sakaebe, Hikari; Taguchi, Noboru; Uchimoto, Yoshiharu; Kobayashi, Yoji; Kageyama, Hiroshi

2017-05-01

We report a scandium oxyhydride BaScO 2 H prepared by solid state reaction under high pressure. Rietveld refinements against powder synchrotron X-ray and neutron diffraction data revealed that BaScO 2 H adopts the ideal cubic perovskite structure (Pm3̅m), where oxide (O 2- ) and hydride (H - ) anions are disordered. 1 H nuclear magnetic resonance (NMR) spectroscopy provides a positive chemical shift of about +4.4 ppm, which can be understood by the distance to the nearest (and possibly the next nearest) cation from the H nucleus. A further analysis of the NMR data and calculations based on ab initio random structure searches suggest a partial cis preference in ScO 4 H 2 octahedra. The present oxyhydride, if compositionally or structurally tuned, may become a candidate for H - conductors.

Co nanoparticle effects on the thermoluminescent signal induced by UV and gamma radiation in ZrO2 powders

NASA Astrophysics Data System (ADS)

Villa-Sánchez, G.; Mendoza-Anaya, D.; Eufemia Fernández-García, M.; Escobar-Alarcón, L.; Olea-Mejía, O.; González-Martínez, P. R.

2014-05-01

Zirconia powders, both pure and doped with Co nanoparticles were prepared by the sol-gel method followed by thermal treatment at 1000 °C. The morphological and crystallographic characteristics were studied by scanning and transmission electron microscopy, X-ray diffraction and the Rietveld refinements method. Analysis of the thermoluminescent (TL) signal induced by UV and gamma radiation was also conducted. According to the results, Co nanoparticles have a strong influence on the growth of ZrO2 particles and favor the formation of monoclinic zirconia. Moreover, an important influence of the added Co nanoparticles was observed on the position of the TL peaks of ZrO2, inducing a shift in the luminescence towards higher temperatures as well as the presence of more TL peaks at higher temperatures.

Study on photocatalytic activity of nanosized Co0.3Zn0.7Fe2O4 synthesized by hydrothermal method

NASA Astrophysics Data System (ADS)

Mondal, R.; Sarkar, K.; Dey, S.; Bhattacharjee, S.; Ghosh, C. K.; Kumar, S.

2018-04-01

We have reported the photocatalytic activity of nanosized Co0.3Zn0.7Fe2O4 (CZM) synthesized by hydrothermal method. Powder x-ray diffraction (PXRD), field emission and transmission electron microscopic techniques have been employed for structural and microstructural characterization of the sample. The Rietveld refinement of the PXRD pattern of CZM reveals that the sample is a single phase spinel ferrite of F d 3 ¯m symmetry having crystallite size ˜ 20 nm. The average particle size is ˜ 23 nm. The photocatalytic study suggests that CZM can be suitably used as an efficient (rate constant and % degradation are 7.4×10-2 min-1, 95.76 % at 40 min, respectively), magnetically separable, recyclable photocatalyst for removal of Congo Red from its aqueous solution.

Improvement of thermoelectric properties and their correlations with electron effective mass in Cu1.98SxSe1-x.

PubMed

Zhao, Lanling; Fei, Frank Yun; Wang, Jun; Wang, Funing; Wang, Chunlei; Li, Jichao; Wang, Jiyang; Cheng, Zhenxiang; Dou, Shixue; Wang, Xiaolin

2017-01-16

Sulphur doping effects on the crystal structures, thermoelectric properties, density-of-states, and effective mass in Cu 1.98 S x Se 1-x were studied based on the electrical and thermal transport property measurements, and first-principles calculations. The X-ray diffraction patterns and Rietveld refinements indicate that room temperature Cu 1.98 S x Se 1-x (x = 0, 0.02, 0.08, 0.16) and Cu 1.98 S x Se 1-x (x = 0.8, 0.9, 1.0) have the same crystal structure as monoclinic-Cu 2 Se and orthorhombic-Cu 2 S, respectively. Sulphur doping can greatly enhance zT values when x is in the range of 0.8≤ × ≤1.0. Furthermore, all doped samples show stable thermoelectric compatibility factors over a broad temperature range from 700 to 1000 K, which could greatly benefit their practical applications. First-principles calculations indicate that both the electron density-of-sates and the effective mass for all the compounds exhibit non-monotonic sulphur doping dependence. It is concluded that the overall thermoelectric performance of the Cu 1.98 S x Se 1-x system is mainly correlated with the electron effective mass and the density-of-states.

Mg-doped Li2FeSiO4/C as high-performance cathode material for lithium-ion battery

NASA Astrophysics Data System (ADS)

Qu, Long; Luo, Dong; Fang, Shaohua; Liu, Yi; Yang, Li; Hirano, Shin-ichi; Yang, Chun-Chen

2016-03-01

Mg-doped Li2FeSiO4/C is synthesized by using Fe2O3 nanoparticle as iron source. Through Rietveld refinement of X-ray diffraction data, it is confirmed that Mg-doped Li2FeSiO4 owns monoclinic P21/n structure and Mg occupies in Fe site in the lattice. Through energy dispersive X-ray measurement, it is detected that Mg element is distributed homogenously in the resulting product. The results of transmission electron microscopy measurement reveal that the effect of Mg-doping on Li2FeSiO4 crystallite size is not obvious. As a cathode material for lithium-ion battery, this Mg-doped Li2FeSiO4/C delivers high discharge capacity of 190 mAh g-1 (the capacity was with respect to the mass of Li2FeSiO4) at 0.1C and its capacity retention of 100 charge-discharge cycles reaches 96% at 0.1C. By the analysis of electrochemical impedance spectroscopy, it is concluded that Mg-doping can help to decrease the charge-transfer resistance and increase the Li+ diffusion capability.

X-ray diffraction and Mössbauer spectroscopy studies of LiFe 0.5Ti 1.5O 4 - A new primitive cubic ordered spinel

NASA Astrophysics Data System (ADS)

Avdeev, Georgi; Petrov, Kostadin; Mitov, Ivan

2007-12-01

LiFe 0.5Ti 1.5O 4 was synthesized by solid-state reaction carried out at 900 °C in flowing argon atmosphere, followed by rapid quenching of the reaction product to room temperature. The compound has been characterized by X-ray powder diffraction (XRD) and 57Fe Mössbauer effect spectroscopy (MES). It crystallizes in the space group P4 332, a = 8.4048(1) Å. Results from Rietveld structural refinement indicated 1:3 cation ordering on the octahedral sites: Li occupies the octahedral (4 b) sites, Ti occupies the octahedral (12 d) sites, while the tetrahedral (8 c) sites have mixed (Fe/Li) occupancy. A small, about 5%, inversion of Fe on the (4 b) sites has been detected. The MES data is consistent with cation distribution and oxidation state of Fe, determined from the structural data. The title compound is thermally unstable in air atmosphere. At 800 °C it transforms to a mixture of two Fe 3+ containing phases - a face centred cubic spinel Li (1+ y)/2 Fe (5-3 y)/2 Ti yO 4 and a Li ( z-1)/2 Fe (7-3 z)/2 Ti zO 5 - pseudobrookite. The major product of thermal treatment at 1000 °C is a ramsdellite type lithium titanium iron(III) oxide, accompanied by traces of rutile and pseudobrookite.

Homologous compounds of type ARO3(ZnO)m in the system Ga-Sn-Zn-O

NASA Astrophysics Data System (ADS)

Eichhorn, Simon; Schmid, Herbert; Assenmacher, Wilfried; Mader, Werner

2017-02-01

Several members of hitherto unknown homologous compounds [Sn0.5Zn0.5]GaO3(ZnO)m (m=3-7) of the general formula ARO3(ZnO)m were prepared by solid state methods from the binary oxides in sealed Pt-tubes. UV-vis measurements confirm these compounds to be transparent oxides with an optical band gap in the UV region with Eg≈3 eV. Rietveld refinements on powder samples of [Sn0.5Zn0.5]GaO3(ZnO)m proved the compounds to be isostructural with InGaO3(ZnO)m, where In3+ on octahedral sites is replaced statistically by Sn4+ and Zn2+ in equal amounts preserving an average charge of 3+. Additionally, the structure of [Sn0.5Zn0.5]GaO3(ZnO)3 has been determined from flux-grown single crystals by X-ray diffraction (R 3 ̅ m , Z=3, a=3.2387(7) Å, c=41.78(1) Å, 19 parameters, 201 independent reflections, R1=0.047, wR2=0.074). The compound [Sn0.5Zn0.5]GaO3(ZnO)3 is isostructural with InGaO3(ZnO)3. [Sn0.5Zn0.5]GaO3(ZnO)3 was furthermore analyzed by High Angle Annular Dark Field (HAADF) scanning TEM and EELS spectroscopic imaging, supporting the structure model derived from X-ray diffraction data.

Crystal structure and low-energy Einstein mode in ErV{sub 2}Al{sub 20} intermetallic cage compound

DOE Office of Scientific and Technical Information (OSTI.GOV)

Winiarski, Michał J., E-mail: mwiniarski@mif.pg.gda.pl; Klimczuk, Tomasz

Single crystals of a new ternary aluminide ErV{sub 2}Al{sub 20} were grown using a self-flux method. The crystal structure was determined by powder X-ray diffraction measurements and Rietveld refinement, and physical properties were studied by means of electrical resistivity, magnetic susceptibility and specific heat measurements. These measurements reveal that ErV{sub 2}Al{sub 20} is a Curie-Weiss paramagnet down to 1.95 K with an effective magnetic moment μ{sub eff} =9.27(1) μ{sub B} and Curie-Weiss temperature Θ{sub CW} =−0.55(4) K. The heat capacity measurements show a broad anomaly at low temperatures that is attributed to the presence of a low-energy Einstein mode withmore » characteristic temperature Θ{sub E} =44 K, approximately twice as high as in the isostructural ‘Einstein solid’ VAl{sub 10.1}. - Graphical abstract: A low-energy Einstein mode is observed in a novel intermetallic cage compound ErV{sub 2}Al{sub 20} by specific heat and resistivity measurements. - Highlights: • Single crystals of a new compound ErV{sub 2}Al{sub 20} were grown by self-flux method. • Crystal structure is reported, based on powder x-ray diffraction. • ErV{sub 2}Al{sub 20} is a Curie-Weiss paramagnet. • Low-energy ‘rattling’ phonon mode (Θ{sub E}=44 K) is found in specific heat measurements.« less

Application of Mythen detector: In-situ XRD study on the thermal expansion behavior of metal indium

NASA Astrophysics Data System (ADS)

Du, Rong; Chen, ZhongJun; Cai, Quan; Fu, JianLong; Gong, Yu; Wu, ZhongHua

2016-07-01

A Mythen detector has been equipped at the beamline 4B9A of Beijing Synchrotron Radiation Facility (BSRF), which is expected to enable BSRF to perform time-resolved measurement of X-ray diffraction (XRD) full-profiles. In this paper, the thermal expansion behavior of metal indium has been studied by using the in-situ XRD technique with the Mythen detector. The indium was heated from 303 to 433 K with a heating rate of 2 K/min. The in-situ XRD full-profiles were collected with a rate of one profile per 10 seconds. Rietveld refinement was used to extract the structural parameters. The results demonstrate that these collected quasi-real-time XRD profiles can be well used for structural analysis. The metal indium was found to have a nonlinear thermal expansion behavior from room temperature to the melting point (429.65 K). The a-axis of the tetragonal unit cell expands with a biquadratic dependency on temperature, while the c-axis contracts with a cubic dependency on temperature. By the time-resolved XRD measurements, it was observed that the [200] preferred orientation can maintain to about 403.15 K. While (110) is the last and detectable crystal plane just before melting of the polycrystalline indium foil. This study is not only beneficial to the application of metal indium, but also exhibits the capacity of in-situ time-resolved XRD measurements at the X-ray diffraction station of BSRF.

A comprehensive study on the structural evolution of HfO 2 thin films doped with various dopants

DOE PAGES

Park, Min Hyuk; Schenk, Tony; Fancher, Christopher M.; ...

2017-04-19

The origin of the unexpected ferroelectricity in doped HfO 2 thin films is now considered to be the formation of a non-centrosymmetric Pca2 1 orthorhombic phase. Due to the polycrystalline nature of the films as well as their extremely small thickness (~10 nm) and mixed orientation and phase composition, structural analysis of doped HfO 2 thin films remains a challenging task. As a further complication, the structural similarities of the orthorhombic and tetragonal phase are difficult to distinguish by typical structural analysis techniques such as X-ray diffraction. To resolve this issue, the changes in the grazing incidence X-ray diffraction (GIXRD)more » patterns of HfO 2 films doped with Si, Al, and Gd are systematically examined. For all dopants, the shift of o111/ t101 diffraction peak is observed with increasing atomic layer deposition (ALD) cycle ratio, and this shift is thought to originate from the orthorhombic to P4 2/ nmc tetragonal phase transition with decreasing aspect ratio (2 a/(b + c) for orthorhombic and c/a for the tetragonal phase). For quantitative phase analysis, Rietveld refinement is applied to the GIXRD patterns. A progressive phase transition from P2 1/c monoclinic to orthorhombic to tetragonal is confirmed for all dopants, and a strong relationship between orthorhombic phase fraction and remanent polarization value is uniquely demonstrated. The concentration range for the ferroelectric properties was the narrowest for the Si-doped HfO 2 films. As a result, the dopant size is believed to strongly affect the concentration range for the ferroelectric phase stabilization, since small dopants can strongly decrease the free energy of the tetragonal phase due to their shorter metal–oxygen bonds.« less

A comprehensive study on the structural evolution of HfO 2 thin films doped with various dopants

DOE Office of Scientific and Technical Information (OSTI.GOV)

Park, Min Hyuk; Schenk, Tony; Fancher, Christopher M.

The origin of the unexpected ferroelectricity in doped HfO 2 thin films is now considered to be the formation of a non-centrosymmetric Pca2 1 orthorhombic phase. Due to the polycrystalline nature of the films as well as their extremely small thickness (~10 nm) and mixed orientation and phase composition, structural analysis of doped HfO 2 thin films remains a challenging task. As a further complication, the structural similarities of the orthorhombic and tetragonal phase are difficult to distinguish by typical structural analysis techniques such as X-ray diffraction. To resolve this issue, the changes in the grazing incidence X-ray diffraction (GIXRD)more » patterns of HfO 2 films doped with Si, Al, and Gd are systematically examined. For all dopants, the shift of o111/ t101 diffraction peak is observed with increasing atomic layer deposition (ALD) cycle ratio, and this shift is thought to originate from the orthorhombic to P4 2/ nmc tetragonal phase transition with decreasing aspect ratio (2 a/(b + c) for orthorhombic and c/a for the tetragonal phase). For quantitative phase analysis, Rietveld refinement is applied to the GIXRD patterns. A progressive phase transition from P2 1/c monoclinic to orthorhombic to tetragonal is confirmed for all dopants, and a strong relationship between orthorhombic phase fraction and remanent polarization value is uniquely demonstrated. The concentration range for the ferroelectric properties was the narrowest for the Si-doped HfO 2 films. As a result, the dopant size is believed to strongly affect the concentration range for the ferroelectric phase stabilization, since small dopants can strongly decrease the free energy of the tetragonal phase due to their shorter metal–oxygen bonds.« less

Landed XRD/XRF analysis of prime targets in the search for past or present Martian life.

PubMed

Vaniman, D; Bish, D; Blake, D; Elliott, S T; Sarrazin, P; Collins, S A; Chipera, S

1998-12-25

Mars landers seeking evidence for past or present life will be guided by information from orbital mapping and from previous surface exploration. Several target options have been proposed, including sites that may harbor extant life and sites most likely to preserve evidence of past life These sites have specific mineralogic characteristics. Extant life might be gathered around the sinters and associated mineral deposits of rare active fumaroles, or held within brine pockets and inclusions in a few evaporite-mineral deposits. Possibilities for fossilization include deltaic and lake-bottom sediments of once-flooded craters, sinters formed by ancient hot-spring deposits, and the carbonate deposits associated with some evaporite systems. However, the highly varied mineralogy of fossil occurrences on Earth leads to the inference that Mars, an equally complex planet, could host a broad variety of potential fossilizing deposits. The abundance of volcanic systems on Mars and evidence for close associations between volcanism and water release suggest possibilities of organism entrapment and mineralization in volcaniclastic deposits, as found in some instances on Earth. Thus the targets being considered for exploration include a wide variety of unique deposits that would be characterized by silica or various nonsilicate minerals. Beyond these "special" deposits and in the most general case, an ability to distinguish mineralized from uncemented volcanic detritus may be the key to success in finding possible fossil-bearing authigenic mineralogies. A prototype miniaturized X ray diffraction/X ray fluorescence (XRD/XRF) instrument has been evaluated with silica, carbonate, and sulfate minerals and with a basalt, to examine the capabilities of this tool in mineralogic and petrologic exploration for exobiological goals. This instrument. CHEMIN (chemical and mineralogical analyzer), is based on an innovative low-power X ray tube, transmission geometry, and CCD collection and discrimination of diffracted and fluoresced X rays. The ability to accumulate and integrate the entire circumference of each complete Debye diffraction ring compensates for poor powder preparations, as might be produced by robotic sampling systems. With CHEMIN, a wide range of minerals can be uniquely identified. Using Rietveld analysis of the XRD results, mineral quantification is also possible. Expanded capabilities in phase analysis and constrained data solutions using quantitative XRD and XRF are within reach.

Transport of oxygen ions in Er doped La2Mo2O9 oxide ion conductors: Correlation with microscopic length scales

NASA Astrophysics Data System (ADS)

Paul, T.; Ghosh, A.

2018-01-01

We report oxygen ion transport in La2-xErxMo2O9 (0.05 ≤ x ≤ 0.25) oxide ion conductors. We have measured conductivity and dielectric spectra at different temperatures in a wide frequency range. The mean square displacement and spatial extent of non-random sub-diffusive regions are estimated from the conductivity spectra and dielectric spectra, respectively, using linear response theory. The composition dependence of the conductivity is observed to be similar to that of the spatial extent of non-random sub-diffusive regions. The behavior of the composition dependence of the mean square displacement of oxygen ions is opposite to that of the conductivity. The attempt frequency estimated from the analysis of the electric modulus agrees well with that obtained from the Raman spectra analysis. The full Rietveld refinement of X-ray diffraction data of the samples is performed to estimate the distance between different oxygen lattice sites. The results obtained from such analysis confirm the ion hopping within the spatial extent of non-random sub-diffusive regions.

Structural investigation of Y1-xNixBa2Cu3O7-δ superconductor

NASA Astrophysics Data System (ADS)

Hadi-Sichani, Behnaz; Shakeripour, Hamideh; Salamati, Hadi

2018-07-01

Y1-xNixBa2Cu3O7-δ superconducting samples with 0 ≤ x ≤ 0.02 were synthesized by standard solid-state reaction and characterized by the X-ray powder diffraction technique. The Rietveld fitted XRD refinements show that all samples are crystallized in single phase, having orthorhombic structure with Pmmm space group. We investigated the effect of adding a magnetic element on the structure of this superconductor. The c cell parameter increases by doping of Ni until to an optimal value of Ni content, x ∼ 0.004, and then starts to decrease by higher value of Ni substitution. Moreover, it is seen that Cu(2)sbnd O(2) bond length decreases with increasing Ni up to the optimal concentration of Ni, too. The CuO2 planes become more distorted and hence charge carriers may have better chances of transportation to the CuO2 planes. By further increasing of Ni content than the optimal value, the Cu(2)sbnd O(2) bond lengths start to increase, and cause CuO2 planes to be flatten. We suggest, besides affecting the magnetic characteristic of Ni impurity, the Ni substitution leads to interesting crystallographic changes.

X-ray diffraction from shock-loaded polycrystals.

PubMed

Swift, Damian C

2008-01-01

X-ray diffraction was demonstrated from shock-compressed polycrystalline metals on nanosecond time scales. Laser ablation was used to induce shock waves in polycrystalline foils of Be, 25-125 microm thick. A second laser pulse was used to generate a plasma x-ray source by irradiation of a Ti foil. The x-ray source was collimated to produce a beam of controllable diameter, which was directed at the Be sample. X-rays were diffracted from the sample, and detected using films and x-ray streak cameras. The diffraction angle was observed to change with shock pressure. The diffraction angles were consistent with the uniaxial (elastic) and isotropic (plastic) compressions expected for the loading conditions used. Polycrystalline diffraction will be used to measure the response of the crystal lattice to high shock pressures and through phase changes.

Ferroelectric properties of oxalate and phenanthroline based 1-D single chain molecular magnet [{FeII(Δ)FeII(Λ)}0.5{CrII(Δ)CrII(Λ)}0.5(ox)2(phen)2

NASA Astrophysics Data System (ADS)

Bhatt, Pramod; Mukadam, M. D.; Mandal, B. P.; Yusuf, S. M.

2018-04-01

The one-dimensional (1-D) single chain molecular magnet [{FeII(Δ)FeII(Λ)}0.5{CrII(Δ)CrII(Λ)}0.5(ox)2(phen)2] is hydrothermally synthesized using oxalate (ox) and phenanthroline (phen) ligands with transition metal ions (Fe and Cr). The compound is characterized using x-ray diffraction, dc magnetization measurements and P-E ferroelectric loop measurements. The diffraction analysis using Rietveld refinement confirms a single phase formation of the compound in monoclinic structure with space group of P21. The compound crystallizes in 1-D chain like structure containing two different crystallographic sites of metal ions (Δ- and Λ-), which are bridged by the ox ligand and Phen ligand. These two metals site are different in bond length and bond angles results lattice distortions. The lattice distortion induces ferroelectric behavior in the compound which is discussed in terms of lattice distortion induced dipole moments.

Refinement of atomic and magnetic structures using neutron diffraction for synthesized bulk and nano-nickel zinc gallate ferrite

NASA Astrophysics Data System (ADS)

Ata-Allah, S. S.; Balagurov, A. M.; Hashhash, A.; Bobrikov, I. A.; Hamdy, Sh.

2016-01-01

The parent NiFe2O4 and Zn/Ga substituted spinel ferrite powders have been prepared by solid state reaction technique. As a typical example, the Ni0.7Zn0.3Fe1.5Ga0.5O4 sample has been prepared by sol-gel auto combustion method with the nano-scale crystallites size. X-ray and Mössbauer studies were carried out for the prepared samples. Structure and microstructure properties were investigated using the time-of-flight HRFD instrument at the IBR-2 pulsed reactor, at a temperatures range 15-473 K. The Rietveld refinement of the neutron diffraction data revealed that all samples possess cubic symmetry corresponding to the space group Fd3m. Cations distribution show that Ni2+ is a complete inverse spinel ion, while Ga3+ equally distributed between the two A and B-sublattices. The level of microstrains in bulk samples was estimated as very small while the size of coherently scattered domains is quite large. For nano-structured sample the domain size is around 120 Å.

Hydration studies of calcium sulfoaluminate cements blended with fly ash

DOE Office of Scientific and Technical Information (OSTI.GOV)

García-Maté, M.; De la Torre, A.G.; León-Reina, L.

The main objective of this work is to study the hydration and properties of calcium sulfoaluminate cement pastes blended with fly ash (FA) and the corresponding mortars at different hydration ages. Laboratory X-ray powder diffraction, rheological studies, thermal analysis, porosimetry and compressive strength measurements were performed. The analysis of the diffraction data by Rietveld method allowed quantifying crystalline phases and overall amorphous contents. The studied parameters were: i) FA content, 0, 15 and 30 wt.%; and ii) water addition, water-to-CSA mass ratio (w/CSA = 0.50 and 0.65), and water-to-binder mass ratio (w/b = 0.50). Finally, compressive strengths after 6 monthsmore » of 0 and 15 wt.% FA [w/CSA = 0.50] mortars were similar: 73 ± 2 and 72 ± 3 MPa, respectively. This is justified by the filler effect of the FA as no strong evidences of reactivity of FA with CSA were observed. These results support the partial substitution of CSA cements with FA with the economic and environmental benefits.« less

From average to local structure: a Rietveld and an atomic pair distribution function (PDF) study of selenium clusters in zeolite-NdY.

PubMed

Abeykoon, A M Milinda; Donner, Wolfgang; Brunelli, Michela; Castro-Colin, Miguel; Jacobson, Allan J; Moss, Simon C

2009-09-23

The structure of Se particles in the approximately 13 A diameter alpha-cages of zeolite NdY has been determined by Rietveld refinement and pair distribution function (PDF) analysis of X-ray data. With the diffuse scattering subtracted an average structure comprised of an undistorted framework containing nanoclusters of 20 Se atoms is observed. The intracluster correlations and the cluster-framework correlations which give rise to diffuse scattering were modeled by using PDF analysis.

Single-pulse x-ray diffraction using polycapillary optics for in situ dynamic diffraction

DOE Office of Scientific and Technical Information (OSTI.GOV)

Maddox, B. R., E-mail: maddox3@llnl.gov; Akin, M. C., E-mail: akin1@llnl.gov; Teruya, A.

2016-08-15

Diagnostic use of single-pulse x-ray diffraction (XRD) at pulsed power facilities can be challenging due to factors such as the high flux and brightness requirements for diffraction and the geometric constraints of experimental platforms. By necessity, the x-ray source is usually positioned very close, within a few inches of the sample. On dynamic compression platforms, this puts the x-ray source in the debris field. We coupled x-ray polycapillary optics to a single-shot needle-and-washer x-ray diode source using a laser-based alignment scheme to obtain high-quality x-ray diffraction using a single 16 ns x-ray pulse with the source >1 m from themore » sample. The system was tested on a Mo sample in reflection geometry using 17 keV x-rays from a Mo anode. We also identified an anode conditioning effect that increased the x-ray intensity by 180%. Quantitative measurements of the x-ray focal spot produced by the polycapillary yielded a total x-ray flux on the sample of 3.3 ± 0.5 × 10{sup 7} molybdenum Kα photons.« less

DOE Office of Scientific and Technical Information (OSTI.GOV)

He, Guang; Huq, Ashfia; Manthiram, Arumugam

Vanadyl phosphates (VOPO 4) represent a class of attractive cathodes in lithium-ion batteries. However, the exploration of this type of materials in sodium-ion batteries is rare. Here, we report for the first time the synthesis of orthorhombic β-NaVOPO 4 by first chemically extracting lithium from beta-LiVOPO 4 and then inserting sodium into the obtained β-VOPO 4 by a microwave-assisted solvothermal process with NaI, which serves both as a reducing agent and sodium source. Intermediate Na xVOPO 4 compositions with x = 0.3, 0.5, and 0.8 have also been obtained by controlling the amount of NaI in the reaction mixture. Jointmore » Rietveld refinement of synchrotron X-ray diffraction (XRD) and neutron diffraction confirms that the fully sodiated β-NaVOPO 4 is isostructural with the lithium counterpart β-LiVOPO 4. Bond valence sum maps suggest that sodium ions possibly diffuse along the [010] direction in the lattice, similar to the ionic conduction pathway in β-LiVOPO 4. Although the initial discharge capacity is low due to the protons in the structure, it steadily increases with cycling with a long plateau at 3.3 V. As a result, ex situ XRD data of cycled β-VOPO 4 and β-NaVOPO 4 electrodes confirm the reversible reaction in sodium cells involving the V 4+/V 5+ redox couple.« less

Rietveld refinement and ionic conductivity of Ca{sub 8.4}Bi{sub 1.6}(PO{sub 4}){sub 6}O{sub 1.8}

DOE Office of Scientific and Technical Information (OSTI.GOV)

Tmar Trabelsi, I., E-mail: ilhem_tmar@yahoo.fr; Madani, A.; Mercier, A.M.

2013-01-15

The structure of Ca{sub 8.4}Bi{sub 1.6}(PO{sub 4}){sub 6}O{sub 1.8}, isostructural with Fluoroapatite, was determined by X-ray powder diffraction methods. The results of Rietveld refinement revealed that the formula of this compound is [Ca{sub 4}]{sup 4f}[Ca{sub 4.4}Bi{sub 1.6}]{sup 6h}(PO{sub 4}){sub 6}[O{sub 1.8}]{sup 2a}, space group P63/m (a=9.468 (3) A, c=6.957 (3) A). A total substitution of Bi{sup 3+} ions in the (6h) sites was related particularly to the high polarizability of the Bi{sup 3+} ion compared to Ca{sup 2+}. The observed frequencies in the Raman and infrared spectra were explained and discussed on the basis of unit-cell group analyses and inmore » comparison with Fluoroapatite and other oxyapatites. The ionic conductivity over a wide range of temperature was investigated according to the complex impedance method. The highest overall conductivity values were found at {sigma}{sub 700 Degree-Sign C} =5.03 Multiplication-Sign 10{sup -7} S cm{sup -1} and E{sub a}=0.50 eV. - Graphical abstract: The final Rietveld refinement plot of the Ca{sub 8.4}Bi{sub 1.6} (PO{sub 4}){sub 6}O{sub 1.8}. Highlights: Black-Right-Pointing-Pointer The Rietveld refinement revealed that the formula of this compound is Ca{sub 8.4}Bi{sub 1.6}(PO{sub 4}){sub 6}O{sub 1.8}. Black-Right-Pointing-Pointer Vibrational spectroscopy supports the high symmetry P63/m space group for this apatite. Black-Right-Pointing-Pointer This apatite contained channels where oxygen ions were located in 2a sites. Black-Right-Pointing-Pointer The possibility of anionic conduction along these channels was considered.« less

Domain wall and interphase boundary motion in (1-x)Bi(Mg 0.5 Ti 0.5 )O 3 –xPbTiO 3 near the morphotropic phase boundary

DOE Office of Scientific and Technical Information (OSTI.GOV)

Tutuncu, Goknur; Chen, Jun; Fan, Longlong

Electric field-induced changes in the domain wall motion of (1-x)Bi(Mg 0.5Ti 0.5)O 3–xPbTiO 3 (BMT-xPT) near the morphotropic phase boundary (MPB) where x = 0.37 (BMT-37PT) and x =0.38 (BMT-38PT), are studied by means of synchrotron x-ray diffraction. Through Rietveld analysis and profile fitting, a mixture of coexisting monoclinic (Cm) and tetragonal (P4mm) phases is identified at room temperature. Extrinsic contributions to the property coefficients are evident from electric-field-induced domain wall motion in both the tetragonal and monoclinic phases, as well as through the interphase boundary motion between the two phases. Domain wall motion in the tetragonal and monoclinic phasesmore » for BMT-37PT is larger than that of BMT-38PT, possibly due to this composition's closer proximity to the MPB. Increased interphase boundary motion was also observed in BMT-37PT. Lattice strain, which is a function of both intrinsic piezoelectric strain and elastic interactions of the grains (the latter originating from domain wall and interphase boundary motion), is similar for the respective tetragonal and monoclinic phases.« less

Magnetic and fluorescence properties of cerium-doped yttrium gadolinium aluminum iron garnet crystals

NASA Astrophysics Data System (ADS)

Aoki, Daichi; Shima, Mutsuhiro

2014-11-01

Magnetic and fluorescence properties of chemically synthesized Ce:Gd-YAIG (Ce0.05GdxY2.95-xAl5-yFeyO12) nanocrystals have been investigated. The structural characterization by X-ray diffraction (XRD) shows that a garnet phase has been identified in samples with 0 ≤ x ≤ 2.95 and 0 ≤ y ≤ 3.0. When y = 0, only garnet peaks are observed for 0 ≤ x ≤ 2.5, while both garnet and perovskite phases are present for x > 2.5. It is found from XRD Rietveld analyses that the site occupancy of Fe3+ at the tetrahedral and octahedral sites in the garnet is independent of the amount of Y3+ substituted by Ce3+ and Gd3+ at the dodecahedral sites. The saturation magnetization for the sample with x = 0 and y = 3.0 is 4.35 emu/g, while that with x = 2.5 and y = 3.0 is 87.5 emu/g. When the Fe3+ composition y is varied from 0 to 3.0 at x = 2.5, the intensity of fluorescence at the emission wavelength ˜570 nm significantly decreases presumably due to absorption by Fe3+ that is increased in the crystal.

X-Ray Diffraction Apparatus

NASA Technical Reports Server (NTRS)

Blake, David F. (Inventor); Bryson, Charles (Inventor); Freund, Friedmann (Inventor)

1996-01-01

An x-ray diffraction apparatus for use in analyzing the x-ray diffraction pattern of a sample is introduced. The apparatus includes a beam source for generating a collimated x-ray beam having one or more discrete x-ray energies, a holder for holding the sample to be analyzed in the path of the beam, and a charge-coupled device having an array of pixels for detecting, in one or more selected photon energy ranges, x-ray diffraction photons produced by irradiating such a sample with said beam. The CCD is coupled to an output unit which receives input information relating to the energies of photons striking each pixel in the CCD, and constructs the diffraction pattern of photons within a selected energy range striking the CCD.

Real-time X-ray Diffraction: Applications to Materials Characterization

NASA Technical Reports Server (NTRS)

Rosemeier, R. G.

1984-01-01

With the high speed growth of materials it becomes necessary to develop measuring systems which also have the capabilities of characterizing these materials at high speeds. One of the conventional techniques of characterizing materials was X-ray diffraction. Film, which is the oldest method of recording the X-ray diffraction phenomenon, is not quite adequate in most circumstances to record fast changing events. Even though conventional proportional counters and scintillation counters can provide the speed necessary to record these changing events, they lack the ability to provide image information which may be important in some types of experiment or production arrangements. A selected number of novel applications of using X-ray diffraction to characterize materials in real-time are discussed. Also, device characteristics of some X-ray intensifiers useful in instantaneous X-ray diffraction applications briefly presented. Real-time X-ray diffraction experiments with the incorporation of image X-ray intensification add a new dimension in the characterization of materials. The uses of real-time image intensification in laboratory and production arrangements are quite unlimited and their application depends more upon the ingenuity of the scientist or engineer.

Combined resistive and laser heating technique for in situ radial X-ray diffraction in the diamond anvil cell at high pressure and temperature

DOE Office of Scientific and Technical Information (OSTI.GOV)

Miyagi, Lowell; Department of Earth Sciences, Montana State University, Bozeman, Montana 59717; Kanitpanyacharoen, Waruntorn

2013-02-15

To extend the range of high-temperature, high-pressure studies within the diamond anvil cell, a Liermann-type diamond anvil cell with radial diffraction geometry (rDAC) was redesigned and developed for synchrotron X-ray diffraction experiments at beamline 12.2.2 of the Advanced Light Source. The rDAC, equipped with graphite heating arrays, allows simultaneous resistive and laser heating while the material is subjected to high pressure. The goals are both to extend the temperature range of external (resistive) heating and to produce environments with lower temperature gradients in a simultaneously resistive- and laser-heated rDAC. Three different geomaterials were used as pilot samples to calibrate andmore » optimize conditions for combined resistive and laser heating. For example, in Run1, FeO was loaded in a boron-mica gasket and compressed to 11 GPa then gradually resistively heated to 1007 K (1073 K at the diamond side). The laser heating was further applied to FeO to raise temperature to 2273 K. In Run2, Fe-Ni alloy was compressed to 18 GPa and resistively heated to 1785 K (1973 K at the diamond side). The combined resistive and laser heating was successfully performed again on (Mg{sub 0.9}Fe{sub 0.1})O in Run3. In this instance, the sample was loaded in a boron-kapton gasket, compressed to 29 GPa, resistive-heated up to 1007 K (1073 K at the diamond side), and further simultaneously laser-heated to achieve a temperature in excess of 2273 K at the sample position. Diffraction patterns obtained from the experiments were deconvoluted using the Rietveld method and quantified for lattice preferred orientation of each material under extreme conditions and during phase transformation.« less

Radiation damage free ghost diffraction with atomic resolution

DOE PAGES

Li, Zheng; Medvedev, Nikita; Chapman, Henry N.; ...

2017-12-21

The x-ray free electron lasers can enable diffractive structural determination of protein nanocrystals and single molecules that are too small and radiation-sensitive for conventional x-ray diffraction. However the electronic form factor may be modified during the ultrashort x-ray pulse due to photoionization and electron cascade caused by the intense x-ray pulse. For general x-ray imaging techniques, the minimization of the effects of radiation damage is of major concern to ensure reliable reconstruction of molecular structure. Here in this paper, we show that radiation damage free diffraction can be achieved with atomic spatial resolution by using x-ray parametric down-conversion and ghostmore » diffraction with entangled photons of x-ray and optical frequencies. We show that the formation of the diffraction patterns satisfies a condition analogous to the Bragg equation, with a resolution that can be as fine as the crystal lattice length scale of several Ångstrom. Since the samples are illuminated by low energy optical photons, they can be free of radiation damage.« less

Radiation damage free ghost diffraction with atomic resolution

DOE Office of Scientific and Technical Information (OSTI.GOV)

Li, Zheng; Medvedev, Nikita; Chapman, Henry N.

The x-ray free electron lasers can enable diffractive structural determination of protein nanocrystals and single molecules that are too small and radiation-sensitive for conventional x-ray diffraction. However the electronic form factor may be modified during the ultrashort x-ray pulse due to photoionization and electron cascade caused by the intense x-ray pulse. For general x-ray imaging techniques, the minimization of the effects of radiation damage is of major concern to ensure reliable reconstruction of molecular structure. Here in this paper, we show that radiation damage free diffraction can be achieved with atomic spatial resolution by using x-ray parametric down-conversion and ghostmore » diffraction with entangled photons of x-ray and optical frequencies. We show that the formation of the diffraction patterns satisfies a condition analogous to the Bragg equation, with a resolution that can be as fine as the crystal lattice length scale of several Ångstrom. Since the samples are illuminated by low energy optical photons, they can be free of radiation damage.« less

Synchrotron Radiation X-ray Diffraction Techniques Applied to Insect Flight Muscle.

PubMed

Iwamoto, Hiroyuki

2018-06-13

X-ray fiber diffraction is a powerful tool used for investigating the molecular structure of muscle and its dynamics during contraction. This technique has been successfully applied not only to skeletal and cardiac muscles of vertebrates but also to insect flight muscle. Generally, insect flight muscle has a highly ordered structure and is often capable of high-frequency oscillations. The X-ray diffraction studies on muscle have been accelerated by the advent of 3rd-generation synchrotron radiation facilities, which can generate brilliant and highly oriented X-ray beams. This review focuses on some of the novel experiments done on insect flight muscle by using synchrotron radiation X-rays. These include diffraction recordings from single myofibrils within a flight muscle fiber by using X-ray microbeams and high-speed diffraction recordings from the flight muscle during the wing-beat of live insects. These experiments have provided information about the molecular structure and dynamic function of flight muscle in unprecedented detail. Future directions of X-ray diffraction studies on muscle are also discussed.

Improvement of thermoelectric properties and their correlations with electron effective mass in Cu1.98SxSe1−x

PubMed Central

Zhao, Lanling; Fei, Frank Yun; Wang, Jun; Wang, Funing; Wang, Chunlei; Li, Jichao; Wang, Jiyang; Cheng, Zhenxiang; Dou, Shixue; Wang, Xiaolin

2017-01-01

Sulphur doping effects on the crystal structures, thermoelectric properties, density-of-states, and effective mass in Cu1.98SxSe1−x were studied based on the electrical and thermal transport property measurements, and first-principles calculations. The X-ray diffraction patterns and Rietveld refinements indicate that room temperature Cu1.98SxSe1−x (x = 0, 0.02, 0.08, 0.16) and Cu1.98SxSe1−x (x = 0.8, 0.9, 1.0) have the same crystal structure as monoclinic-Cu2Se and orthorhombic-Cu2S, respectively. Sulphur doping can greatly enhance zT values when x is in the range of 0.8≤ × ≤1.0. Furthermore, all doped samples show stable thermoelectric compatibility factors over a broad temperature range from 700 to 1000 K, which could greatly benefit their practical applications. First-principles calculations indicate that both the electron density-of-sates and the effective mass for all the compounds exhibit non-monotonic sulphur doping dependence. It is concluded that the overall thermoelectric performance of the Cu1.98SxSe1−x system is mainly correlated with the electron effective mass and the density-of-states. PMID:28091545

Synthesis, second-harmonic generation (SHG), and photoluminescence (PL) properties of noncentrosymmetric bismuth selenite solid solutions, Bi2-xLnxSeO5 (Ln = La and Eu; x = 0-0.3)

NASA Astrophysics Data System (ADS)

Qi, Hai-Xin; Jo, Hongil; Oh, Seung-Jin; Ok, Kang Min

2018-02-01

A series of La3+ or Eu3+-doped noncentrosymmetric (NCS) bismuth selenite solid solutions, Bi2-xLnxSeO5 (x = 0.1, 0.2, and 0.3), have been successfully synthesized via standard solid-state reactions under vacuum with Bi2O3, La2O3 (or Eu2O3), and SeO2 as starting materials. Crystal structures and phase purities of the resultant materials were thoroughly characterized by powder X-ray diffraction using the Rietveld method. The results clearly show that the reported materials crystallize in the orthorhombic space group, Abm2 (No. 39), and exhibit pseudo-three-dimensional frameworks consisting of BiO3, BiO5, and SeO3 polyhedra that share edges and corners. Detailed diffraction studies indicate that the cell volume of Bi2-xLnxSeO5 decreases with an increasing amount of Ln3+ on the Bi3+ sites. However, no ordering between Ln3+ and Bi3+ was observed in the Bi2-xLnxSeO5 solid solutions. Powder second-harmonic generation (SHG) measurements, using 1064 nm radiation, reveal that SHG efficiencies of Bi2-xLnxSeO5 solid solutions continuously decrease as more Ln3+ cations are added to the sites of polarizable Bi3+ cations. Photoluminescence (PL) measurements on Bi2-xEuxSeO5 exhibit three specific emission peaks at 592, 613, and 702 nm (5D0 → 7F1, 2, 4) owing to the 4f-4f intrashell transitions of Eu3+ ions.

Combining experiment and optical simulation in coherent X-ray nanobeam characterization of Si/SiGe semiconductor heterostructures

DOE PAGES

Tilka, J. A.; Park, J.; Ahn, Y.; ...

2016-07-06

Here, the highly coherent and tightly focused x-ray beams produced by hard x-ray light sources enable the nanoscale characterization of the structure of electronic materials but are accompanied by significant challenges in the interpretation of diffraction and scattering patterns. X-ray nanobeams exhibit optical coherence combined with a large angular divergence introduced by the x-ray focusing optics. The scattering of nanofocused x-ray beams from intricate semiconductor heterostructures produces a complex distribution of scattered intensity. We report here an extension of coherent xray optical simulations of convergent x-ray beam diffraction patterns to arbitrary x-ray incident angles to allow the nanobeam diffraction patternsmore » of complex heterostructures to be simulated faithfully. These methods are used to extract the misorientation of lattice planes and the strain of individual layers from synchrotron x-ray nanobeam diffraction patterns of Si/SiGe heterostructures relevant to applications in quantum electronic devices. The systematic interpretation of nanobeam diffraction patterns from semiconductor heterostructures presents a new opportunity in characterizing and ultimately designing electronic materials.« less

Shear Deformation of Fe Polycrystals in the Rotational Diamond Anvil Cell

NASA Astrophysics Data System (ADS)

Merkel, S.; Lincot, A.; Nisr, C.; Hanfland, M.; Zerr, A.

2014-12-01

For many years, experiments are being developed for performing deformation experiments under lower mantle conditions. They include methods such as the Deformation-DIA (Wang et al, 2003) or radial x-ray diffraction in the diamond anvil cell (Merkel et al, 2002). However, the strain applied to the sample is typically limited to about 40%. This can be an issue for studying effects of large deformation or, for the case of diamond anvil cells, applying actual plastic strain at megabar pressures. The issue can be solved using apparatus such as the Rotational-Drickamer (RDA) (e.g. Yamazaki and Karato, 2001). However, the RDA offers limited diffraction access to the sample and operating pressures do not reach those of the lower mantle.In this abstract, we investigate the potential applications of the rotational diamond anvil cell (Rot-DAC) for such studies. 300 K experiments in the Rot-DAC have been performed up to pressures exceeding 50 GPa (e.g. Serebryanaya et al, 1995) with studies focusing on the effect of shear on solid-solid phase transformation pressures. The authors did not investigate the possibility of using the Rot-DAC for studying rheological properties.Here, a sample of polycrystalline Fe is submitted to shear deformation in the Rot-DAC at pressures up to 20 GPa. Synchrotron X-ray diffraction and Rietveld refinements are then used to study the texture and stress state at multiple locations in the sample. The study shows that the Rot-DAC is efficient at producing deformation textures in a polycrystalline aggregate but that care should be taken in ensuring that the sample is actually undergoing plastic deformation and not solid rotation. Stresses, on the other hand, are difficult to extract from the x-ray diffraction data because of lack of understanding of stress distributions in the deforming aggregate.S. Merkel, H. R. Wenk, J. Shu, G. Shen, P. Gillet, H. K. Mao and R. J. Hemley, J. Geophys. Res., 107, 2271 (2002)N. Serebryanaya, V. Blank and V. Ivdenko, Phys. Lett. A, 197, 63-66 (1995)Y. Wang, W. B. Duhram, I. C. Getting and D. J. Weidner, Rev. Sci. Instrum., 74, 3002-3011 (2003)D. Yamazaki and S.-I. Karato, Rev. Sci. Instrum., 72, 4207-4211 (2001)

Controlled Synthesis and Magnetic Properties of Uniform Hierarchical Polyhedral α-Fe2O3 Particles

NASA Astrophysics Data System (ADS)

Long, Nguyen Viet; Yang, Yong; Thi, Cao Minh; Phuc, Le Hong; Nogami, Masayuki

2017-06-01

The controlled synthesis of uniform hierarchical polyhedral iron (Fe) micro-/nanoscale oxide particles with the α-Fe2O3 structure is presented. The hierarchical polyhedral iron oxide particles were synthesized by modified polyol methods with sodium borohydride as a powerful and efficient reducing agent. A critical heat treatment process used during the synthesis allowed for the interesting formation of α-Fe2O3 hematite with a micro-/nanoscale structure. The structure and weak ferromagnetism of the α-Fe2O3 particles were investigated by x-ray diffraction with whole pattern fitting and Rietveld refinement, scanning electron microscopy, and by vibrating sample magnetometry. The as-prepared α-Fe2O3 particles and the three dimensional models presented have promising practical applications for energy storage and conversion in batteries, capacitors, and fuel cells, and related spintronic devices and technologies.

Studies of ferroelectric and dielectric properties of pure and doped barium titanate prepared by sol-gel method

DOE Office of Scientific and Technical Information (OSTI.GOV)

Bisen, Supriya; Mishra, Ashutosh; Jarabana, Kanaka M.

2016-05-23

In this work, Barium Titanate (BaTiO{sub 3}) powders were synthesized via Sol-Gel auto combustion method using citric acid as a chelating agent. We study the behavior of ferroelectric and dielectric properties of pure and doped BaTiO{sub 3} on different concentration. To understand the phase and structure of the powder calcined at 900°C were characterized by X-ray Diffraction shows that tetragonal phase is dominant for pure and doped BTO and data fitted by Rietveld Refinement. Electric and Dielectric properties were characterized by P-E Hysteresis and Dielectric measurement. In P-E measurement ferroelectric loop tracer applied for different voltage. The temperature dependant dielectricmore » constant behavior was observed as a function of frequency recorded on hp-Hewlett Packard 4192A, LF impedance, 5Hz-13Hz analyzer.« less

An Ultrahigh CO2-Loaded Silicalite-1 Zeolite: Structural Stability and Physical Properties at High Pressures and Temperatures.

PubMed

Marqueño, Tomas; Santamaria-Perez, David; Ruiz-Fuertes, Javier; Chuliá-Jordán, Raquel; Jordá, Jose L; Rey, Fernando; McGuire, Chris; Kavner, Abby; MacLeod, Simon; Daisenberger, Dominik; Popescu, Catalin; Rodriguez-Hernandez, Placida; Muñoz, Alfonso

2018-06-04

We report the formation of an ultrahigh CO 2 -loaded pure-SiO 2 silicalite-1 structure at high pressure (0.7 GPa) from the interaction of empty zeolite and fluid CO 2 medium. The CO 2 -filled structure was characterized in situ by means of synchrotron powder X-ray diffraction. Rietveld refinements and Fourier recycling allowed the location of 16 guest carbon dioxide molecules per unit cell within the straight and sinusoidal channels of the porous framework to be analyzed. The complete filling of pores by CO 2 molecules favors structural stability under compression, avoiding pressure-induced amorphization below 20 GPa, and significantly reduces the compressibility of the system compared to that of the parental empty one. The structure of CO 2 -loaded silicalite-1 was also monitored at high pressures and temperatures, and its thermal expansivity was estimated.

Magnetic properties of M0.3Fe2.7O4 (M = Fe, Zn and Mn) ferrites nanoparticles

NASA Astrophysics Data System (ADS)

Modaresi, Nahid; Afzalzadeh, Reza; Aslibeiki, Bagher; Kameli, Parviz

2018-06-01

In the present article a comparative study on the structural and magnetic properties of nano-sized M0.3Fe0.7Fe2O4 (M = Fe, Zn and Mn) ferrites have been reported. The X-ray diffraction (XRD) patterns show that the crystallite size depends on the cation distribution. The Rietveld refinement of XRD patterns using MAUD software determines the distribution of cations and unit cell dimensions. The magnetic measurements show that the maximum and minimum value of saturation magnetization is obtained for Zn and Mn doped samples, respectively. The peak temperature of AC magnetic susceptibility of Zn and Fe doped samples below 300 K shows the superparamagnetic behavior in these samples at room temperature. the AC susceptibility results confirm the presence of strong interactions between the nanoparticles which leads to a superspin glass state in the samples at low temperatures.

Structural and magnetic properties of new uniaxial nanocrystalline Pr5Co19 compound

NASA Astrophysics Data System (ADS)

Bouzidi, W.; Mliki, N.; Bessais, L.

2017-11-01

Highly-coercive nanocrystalline Pr5Co19 powders have been synthesized by mechanical milling for the first time. The structural properties are studied by X-ray diffraction and refined with Rietveld method. This analysis revealed that whatever annealing temperature, samples crystallize in the rhombohedral (3R) of Ce5Co19-type structure (space group R 3 bar m). The magnetization curve as a function of temperature shows a magnetic transition state at the Curie temperature TC = 690 K. The optimum hard magnetic properties have been obtained for Pr5Co19 milled for 5 h and annealed at 1048 K for 30 min. These alloys exhibit a coercivity of 15 kOe at room temperature. This high coercivity is attributed to the high uniaxial magnetocrystalline anisotropy, nanoscale grain size, and to the homogeneous nanostructure developed by mechanical milling process and subsequent annealing.

Study of multi-functionality of lanthanum ferrite (LaFeO{sub 3})

DOE Office of Scientific and Technical Information (OSTI.GOV)

Gaikwad, Vishwajit M.; Uikey, Pankaj; Acharya, Smita A., E-mail: saha275@yahoo.com

2015-06-24

In the present work, multifunctional behaviors of LaFeO{sub 3} (LFO) are investigated by studying its dielectric and photocatalytic properties, respectively. LFO is synthesized by microwave-assisted co-precipitation route. Orthorhombic structure is confirmed by X-ray diffraction (XRD) and data is well fitted using Rietveld refinement by Full-Prof suite. Frequency and Temperature dependence dielectric behavior are systematically studied. The dielectric constant of LFO was found to be 2500 – 3000 with dissipation factor less than 5%. Photodegradation of toxic dye (Methylene Blue) using as-prepared LFO is also investigated. UV-visible absorption spectra are used to study the photodegradation behaviour. Photodegradation of methylene blue (MB)more » taken from textile industries by LFO are reported. The colossal value of dielectric constant of LFO exhibits high potential to use as room temperature capacitive component for device miniaturization in microelectronics as well as photodegradation ability shows good photocatalyst.« less

Structural, dielectric and magnetic studies of magnetoelectric trirutile Fe{sub 2}TeO{sub 6}

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kaushik, S. D., E-mail: sdkaushik@csr.res.in; Sahu, B.; Mohapatra, S. R.

2016-05-23

We have investigated structural, magnetic and dielectric properties of Fe{sub 2}TeO{sub 6} which is a magnetoelectric antiferromagnet with the trirutile lattice. Rietveld analysis of room temperature X-ray diffraction data shows the phase purity of the sample with tetragonal trirutile structure (space group P4{sub 2}/mnm). The DC susceptibility measurement performed on polycrystalline powders exhibits antiferromagnetic ordering below transition temperature ~ 210K. The employment of Curie-Weiss law to inverse magnetic susceptibility only in the temperature range 350-260 K indicates the magnetic ordering starts developing before the transition temperature. The temperature dependent dielectric measurements show an intrinsic behavior of dielectric constant below 150more » K while a continuous increase in dielectric constant with temperature above 150 K may be attributed to a small increase in electrical conduction, known commonly in the literatures.« less

Mineralogical characterization of strata of the Meade Peak phosphatic shale member of the Permian Phosphoria Formation: channel and individual rock samples of measured section J and their relationship to measured sections A and B, central part of Rasmussen Ridge, Caribou County, Idaho

USGS Publications Warehouse

Knudsen, A.C.; Gunter, M.E.; Herring, J.R.; Grauch, R.I.

2002-01-01

The Permian Phosphoria Formation of southeastern Idaho hosts one of the largest phosphate deposits in the world. Despite the economic significance of this Formation, the fine-grained nature of the phosphorite has discouraged detailed mineralogical characterization and quantification studies. Recently, selenium and other potentially toxic trace elements in mine wastes have drawn increased attention to this formation, and motivated additional study. This study uses powder X-ray diffraction (XRD), with Rietveld quantification software, to quantify and characterize the mineralogy of composite channel samples and individual samples collected from the stratigraphic sections measured by the U.S. Geological Survey in the Meade Peak Member of the Permian Phosphoria Formation at the Enoch Valley mine on Rasmussen Ridge, approximately 15 miles northeast of Soda Springs, Idaho.

Effect of synthesis methods with different annealing temperatures on micro structure, cations distribution and magnetic properties of nano-nickel ferrite

NASA Astrophysics Data System (ADS)

El-Sayed, Karimat; Mohamed, Mohamed Bakr; Hamdy, Sh.; Ata-Allah, S. S.

2017-02-01

Nano-crystalline NiFe2O4 was synthesized by citrate and sol-gel methods at different annealing temperatures and the results were compared with a bulk sample prepared by ceramic method. The effect of methods of preparation and different annealing temperatures on the crystallize size, strain, bond lengths, bond angles, cations distribution and degree of inversions were investigated by X-ray powder diffraction, high resolution transmission electron microscope, Mössbauer effect spectrometer and vibrating sample magnetometer. The cations distributions were determined at both octahedral and tetrahedral sites using both Mössbauer effect spectroscopy and a modified Bertaut method using Rietveld method. The Mössbauer effect spectra showed a regular decrease in the hyperfine field with decreasing particle size. Saturation magnetization and coercivity are found to be affected by the particle size and the cations distribution.

Dynamic Modification of Pore Opening of SAPO-34 by Adsorbed Surface Methoxy Species during Induction of Catalytic Methanol-to-Olefins Reactions

DOE Office of Scientific and Technical Information (OSTI.GOV)

Lo, Benedict T W.; Ye, Lin; Change, G.G. Z.

Here, we report that the pore opening of SAPO-34 can be significantly modified by an adsorbed surface methoxy species during induction of the catalytic methanol-to-olefins process, which offers molecular sieving properties due to physical obstacle of the methoxy group and its adsorption modification to other hydrocarbons. X-ray powder diffraction and Rietveld refinement clearly reveal that the adsorbed single carbon atom as the methoxy group is dynamically created from methanol dehydration on a Brønsted acid site in close proximity to the pore windows. As a result, industrial desirable smaller olefins such as ethylene and propylene can be favourably made at themore » expenses of higher olefins. The structures and fundamental understanding in alteration in the olefins selectivity during induction may allow rational optimisation in catalytic performance under the complex fluidisation conditions.« less

Synthesis and structural studies on cerium substituted La0.4Ca0.6MnO3 as solid oxide fuel cell electrode material

NASA Astrophysics Data System (ADS)

Singh, Monika; Kumar, Dinesh; Singh, Akhilesh Kumar

2018-04-01

For solid oxide fuel cell electrode material, calcium doped lanthanum manganite La0.4Ca0.6MnO3 (LCMO) and cerium-incorporated on Ca-site with composition La0.40Ca0.55Ce0.05MnO3 (LCCMO) were synthesized using most feasible and efficient glycine-nitrate method. The formation of crystalline single phase was confirmed by x-ray diffraction (XRD). The Rietveld analysis reveals that both systems crystallize into orthorhombic crystal structure with Pnma space group. Additionally, 8 mole % Y2O3 stabilized ZrO2 (8YSZ) solid electrolyte was also synthesized using high energy ball mill to check the reaction with electrode materials. It was found that the substitution of Ce+4 cations in LCMO perovskite suppressed formation of undesired insulating CaZrO3 phase.

Characterization of the Phase Composition of Nanosized Lithium Titanates Synthesized by Inductive Thermal Plasma

NASA Astrophysics Data System (ADS)

Quesnel, François; Soucy, Gervais; Veilleux, Jocelyn; Hovington, Pierre; Zhu, Wen; Zaghib, Karim

The properties of lithium titanates anodes in Li-ion batteries are highly dependent on their secondary constituents. While their main phase is usually constituted of Li4Ti5O12, significant quantity of lithium titanates compounds of various stoichiometry are often present, due to either the processing, usage or aging of the material. These may go underreported, as many of these spectrums overlap or display low signal in X-ray diffraction (XRD). Samples of nanosized lithium titanates synthetized by inductive plasma were characterized by XRD and scanning electron microscopy (SEM), as they provide a regular yet typical crystallite size and shape including multiple phases. A Rietveld refinement was developed to extract the composition of these samples. Mass balance through further annealing and differential scanning calorimetry (DSC) enthalpy measurements from phase transformations were also used as identification and validation techniques.

The crystal structure and crystal chemistry of fernandinite and corvusite

USGS Publications Warehouse

Evans, H.T.; Post, J.E.; Ross, D.R.; Nelen, J.A.

1994-01-01

Using type material of fernandinite from Minasragra, Peru, and corvusite from the Jack Claim, La Sal Mountains, Utah, the properties and crystal chemistry of these minerals have been determined by Rietveld analysis of the powder X-ray-diffraction patterns. The crystal structure of both species is isotypic with the V2O5 -type layer first found for ??-Ag0.68V2O5; it consists of chains of VO6 octahedra linked by opposite corners (parallel to b) condensed by edge-sharing to form the layer. The vanadium has average valence 4.8, and the resulting layer-charge is balanced by varying amounts of Ca, Na, and K in the interlayer region accompanied by labile water. This study has confirmed the validity of fernandinite as a unique mineral species. It is closely related to corvusite, from which it is distinguished on the basis of the dominant interlayer cation: Ca for fernandinite, Na for curvusite. -Authors

Intrinsic dependence of the magnetic properties of CoFe2O4 nanoparticles prepared via chemical methods with addition of chelating agents

NASA Astrophysics Data System (ADS)

Mendonça, E. C.; Tenório, Mayara A.; Mecena, S. G.; Zucolotto, B.; Silva, L. S.; Jesus, C. B. R.; Meneses, C. T.; Duque, J. G. S.

2015-12-01

In this work, the effect of addition of different chelating agents on the magnetic properties of cobalt ferrite nanoparticles produced by the combining of both co-precipitation and hydrothermal methods is reported. The Rietveld analyses of X-ray diffraction patterns reveal that our samples are single phase (space group: Fd-3m) with small average sizes. The weight losses observed in the thermogravimetric measurements together with the M×H curves show that the organic contamination coming from chelating agent decomposition can give rise to misinterpretation of the magnetization measurements. Besides, analyses of the zero-field-cooled (ZFC) and field-cooled (FC) magnetization measurements and the M×H curves measured at room temperature allows us to state that both the average blocking temperature and particles size distribution are sensitive to the kind of chelating agent.

Room temperature antiferroelectric-phase stability in BNT-BT lead-free ceramics

NASA Astrophysics Data System (ADS)

Guerra, J. D. S.; Peláiz-Barranco, A.; Calderón-Piñar, F.; Mendez-González, Y.

2017-11-01

In this work the electric field dependence of electrical polarization (hysteresis loop) has been investigated as a function of the frequency in the (Bi0.500Na0.500)0.920Ba0.065La0.010TiO3 ceramic system. Results, not previously reported in the current literature, revealed that the magnitude of the electric field, necessary to obtain true domain switching, is strongly dependent of the frequency of the applied electric field. The structural properties, studied from x-ray diffraction and Rietveld's refinement, showed the coexistence of both antiferroelectric (AFE) and ferroelectric (FE) phases at room temperature, confirming the major contribution for the AFE phase. A strong contribution of the AFE phase on the electric field dependence of the polarization has been also evaluated, even at higher frequencies, considering a non-power-law dependence for the coercive field.

Structural study in ceramic multiferroic Co{sub 3}TeO{sub 6} and analysis of possible Co-Co networks

DOE Office of Scientific and Technical Information (OSTI.GOV)

Singh, Harishchandra; Sinha, A. K., E-mail: anil@rrcat.gov.in; Ghosh, Haranath

2015-06-24

We show that there exist four networks (Co1-Co4, Co2-Co3-Co5, Co1-Co5 and Co2-Co3-Co4) in contrast to earlier observations of two networks (Co1-Co4 and Co2-Co3-Co5) in Co{sub 3}TeO{sub 6} (CTO) multiferroic [Phys. Rev. B 88, 184427 (2013)]. Due to five crystallographically different sites of Co ions coordinated by [IV], [V] and [VI] oxygen atoms, the coordination polyhedra exhibit strong distortions from their respective ideal polyhedra, and thus potentially allow to resolve low-symmetry crystal field splittings of d-d electronic transitions. Our structural analysis using Rietveld refinements on the room temperature Synchrotron X-ray Diffraction data indicates possible magnetic order, and may provide a basismore » for the complex and multiple magnetic transitions of CTO at low temperature.« less

Fabrication and testing of a newly designed slit system for depth-resolved X-ray diffraction measurements

DOE PAGES

Sinsheimer, John; Bouet, Nathalie; Ghose, Sanjit; ...

2016-10-06

A new system of slits called `spiderweb slits' have been developed for depth-resolved powder or polycrystalline X-ray diffraction measurements. The slits act on diffracted X-rays to select a particular gauge volume of sample, while absorbing diffracted X-rays from outside of this volume. Although the slit geometry is to some extent similar to that of previously developed conical slits or spiral slits, this new design has advantages over the previous ones in use for complex heterogeneous materials and in situ and operando diffraction measurements. For example, the slits can measure a majority of any diffraction cone for any polycrystalline material, overmore » a continuous range of diffraction angles, and work for X-ray energies of tens to hundreds of kiloelectronvolts. In addition, the design is generated and optimized using ray-tracing simulations, and fabricated through laser micromachining. The first prototype was successfully tested at the X17A beamline at the National Synchrotron Light Source, and shows similar performance to simulations, demonstrating gauge volume selection for standard powders, for all diffraction peaks over angles of 2–10°. A similar, but improved, design will be implemented at the X-ray Powder Diffraction beamline at the National Synchrotron Light Source II.« less

In-Filled La0.5Co4Sb12 Skutterudite System with High Thermoelectric Figure of Merit

NASA Astrophysics Data System (ADS)

Bashir, Mohamed Bashir Ali; Said, Suhana Mohd; Sabri, Mohd Faizul Mohd; Miyazaki, Yuzuru; Shnawah, Dhafer Abdulameer; Shimada, Masanori; Salleh, Mohd Faiz Mohd; Mahmood, Mohamad Syafie; Salih, Ethar Yahya; Fitriani, Fitriani; Elsheikh, Mohamed Hamid

2018-04-01

The contribution of In addition to the La0.5Co4Sb12 skutterudite structure to improve its thermoelectric properties has been demonstrated. In x La0.5Co4Sb12 (0 ≤ x ≤ 0.3) samples were prepared through mechanical alloying followed by spark plasma sintering. Characterization of the phase structure and morphology of the sintered In x La0.5Co4Sb12 bulk samples was carried out using x-ray diffraction (XRD) analysis, scanning electron microscopy, and energy-dispersive x-ray spectroscopy. Rietveld analysis of the XRD spectra indicated that double filling at the 2a (000) interstitial site with La and In was successfully achieved, significantly improving the thermoelectric performance of the La0.5Co4Sb12 compound through simultaneous increase in the electrical conductivity and Seebeck coefficient. A maximum power factor of 3.39 × 10-3 W/ m-K2 was recorded at 644 K for the In0.3La0.5Co4Sb12 sample, more than 96% of that of the La0.5Co4Sb12 sample. Double filling also effectively reduced the lattice thermal conductivity by about 46%, thus demonstrating that the overall improvement in ZT was primarily due to the reduced thermal conductivity. A maximum ZT value of 1.15 was achieved at 692 K for In0.3La0.5Co4Sb12.

Dynamical scattering in coherent hard x-ray nanobeam Bragg diffraction

NASA Astrophysics Data System (ADS)

Pateras, A.; Park, J.; Ahn, Y.; Tilka, J. A.; Holt, M. V.; Kim, H.; Mawst, L. J.; Evans, P. G.

2018-06-01

Unique intensity features arising from dynamical diffraction arise in coherent x-ray nanobeam diffraction patterns of crystals having thicknesses larger than the x-ray extinction depth or exhibiting combinations of nanoscale and mesoscale features. We demonstrate that dynamical scattering effects can be accurately predicted using an optical model combined with the Darwin theory of dynamical x-ray diffraction. The model includes the highly divergent coherent x-ray nanobeams produced by Fresnel zone plate focusing optics and accounts for primary extinction, multiple scattering, and absorption. The simulation accurately reproduces the dynamical scattering features of experimental diffraction patterns acquired from a GaAs/AlGaAs epitaxial heterostructure on a GaAs (001) substrate.

Coherent x-ray diffraction imaging with nanofocused illumination.

PubMed

Schroer, C G; Boye, P; Feldkamp, J M; Patommel, J; Schropp, A; Schwab, A; Stephan, S; Burghammer, M; Schöder, S; Riekel, C

2008-08-29

Coherent x-ray diffraction imaging is an x-ray microscopy technique with the potential of reaching spatial resolutions well beyond the diffraction limits of x-ray microscopes based on optics. However, the available coherent dose at modern x-ray sources is limited, setting practical bounds on the spatial resolution of the technique. By focusing the available coherent flux onto the sample, the spatial resolution can be improved for radiation-hard specimens. A small gold particle (size <100 nm) was illuminated with a hard x-ray nanobeam (E=15.25 keV, beam dimensions approximately 100 x 100 nm2) and is reconstructed from its coherent diffraction pattern. A resolution of about 5 nm is achieved in 600 s exposure time.

DynAMITe: a prototype large area CMOS APS for breast cancer diagnosis using x-ray diffraction measurements

NASA Astrophysics Data System (ADS)

Konstantinidis, A.; Anaxagoras, T.; Esposito, M.; Allinson, N.; Speller, R.

2012-03-01

X-ray diffraction studies are used to identify specific materials. Several laboratory-based x-ray diffraction studies were made for breast cancer diagnosis. Ideally a large area, low noise, linear and wide dynamic range digital x-ray detector is required to perform x-ray diffraction measurements. Recently, digital detectors based on Complementary Metal-Oxide- Semiconductor (CMOS) Active Pixel Sensor (APS) technology have been used in x-ray diffraction studies. Two APS detectors, namely Vanilla and Large Area Sensor (LAS), were developed by the Multidimensional Integrated Intelligent Imaging (MI-3) consortium to cover a range of scientific applications including x-ray diffraction. The MI-3 Plus consortium developed a novel large area APS, named as Dynamically Adjustable Medical Imaging Technology (DynAMITe), to combine the key characteristics of Vanilla and LAS with a number of extra features. The active area (12.8 × 13.1 cm2) of DynaMITe offers the ability of angle dispersive x-ray diffraction (ADXRD). The current study demonstrates the feasibility of using DynaMITe for breast cancer diagnosis by identifying six breast-equivalent plastics. Further work will be done to optimize the system in order to perform ADXRD for identification of suspicious areas of breast tissue following a conventional mammogram taken with the same sensor.

Combining 27Al Solid-State NMR and First-Principles Simulations To Explore Crystal Structure in Disordered Aluminum Oxynitride.

PubMed

Tu, Bingtian; Liu, Xin; Wang, Hao; Wang, Weimin; Zhai, Pengcheng; Fu, Zhengyi

2016-12-19

The nuclear magnetic resonance (NMR) technique gives insight into the local information in a crystal structure, while Rietveld refinement of powder X-ray diffraction (PXRD) sketches out the framework of a crystal lattice. In this work, first-principles calculations were combined with the solid-state NMR technique and Rietveld refinement to explore the crystal structure of a disordered aluminum oxynitride (γ-alon). The theoretical NMR parameters (chemical shift, δ iso , quadrupolar coupling constants, C Q , and asymmetry parameter, η) of Al 22.5 O 28.5 N 3.5 , predicted by the gauge-including projector augmented wave (GIPAW) algorithm, were used to facilitate the analytical investigation of the 27 Al magic-angle spinning (MAS) NMR spectra of the as-prepared sample, whose formula was confirmed to be Al 2.811 O 3.565 N 0.435 by quantitative analysis. The experimental δ iso , C Q , and η of 27 Al showed a small discrepancy compared with theoretical models. The ratio of aluminum located at the 8a to 16d sites was calculated to be 0.531 from the relative integration of peaks in the 27 Al NMR spectra. The occupancies of aluminum at the 8a and 16d positions were determined through NMR investigations to be 0.9755 and 0.9178, respectively, and were used in the Rietveld refinement to obtain the lattice parameter and anion parameter of Al 2.811 O 3.565 N 0.435 . The results from 27 Al NMR investigations and PXRD structural refinement complemented each other. This work provides a powerful and accessible strategy to precisely understand the crystal structure of novel oxynitride materials with multiple disorder.

Resolution enhancement in coherent x-ray diffraction imaging by overcoming instrumental noise.

PubMed

Kim, Chan; Kim, Yoonhee; Song, Changyong; Kim, Sang Soo; Kim, Sunam; Kang, Hyon Chol; Hwu, Yeukuang; Tsuei, Ku-Ding; Liang, Keng San; Noh, Do Young

2014-11-17

We report that reference objects, strong scatterers neighboring weak phase objects, enhance the phase retrieval and spatial resolution in coherent x-ray diffraction imaging (CDI). A CDI experiment with Au nano-particles exhibited that the reference objects amplified the signal-to-noise ratio in the diffraction intensity at large diffraction angles, which significantly enhanced the image resolution. The interference between the diffracted x-ray from reference objects and a specimen also improved the retrieval of the phase of the diffraction signal. The enhancement was applied to image NiO nano-particles and a mitochondrion and confirmed in a simulation with a bacteria phantom. We expect that the proposed method will be of great help in imaging weakly scattering soft matters using coherent x-ray sources including x-ray free electron lasers.

Temperature driven structural-memory-effects in carbon nanotubes filled with Fe3C nano crystals

NASA Astrophysics Data System (ADS)

Boi, Filippo S.; Zhang, Xiaotian; Corrias, Anna

2018-02-01

We report the observation of novel temperature-driven structural-memory-effects in carbon nanotubes (CNTs) filled with Fe3C nano-crystals. These structural-transitions were measured by means of temperature (T) dependent x-ray diffraction (XRD) in the T-range from 298 K to 12 K. A clear reversible 2θ-shift in the 002-peak of the graphitic-CNTs-walls is found with the decrease of the temperature. As determined by Rietveld refinement, such 2θ-shift translates in a not previously reported decrease in the value of the CNT graphitic c-axis with the decrease of the temperature (from 298 K to 12 K). Also, a clear reversible 2θ-shift in the 031 and 131 diffraction-peaks of Fe3C is observed within the same T-range. Rietveld refinements confirm the existence of such memory-effect and also reveal a gradual decrease of the 010-axis of Fe3C with the decrease of the temperature. These observations imply that the observed structural-memory-effect is a characteristic of CNTs when Fe3C is the encapsulated ferromagnet. The generality of such memory-effects was further confirmed by additional measurements performed on other types of CNTs characterized by continuous Fe3C-filling. XRD measurements in the T-range from 298 K to 673 K revealed also an unusual reversible decrease of the Fe3C-peak intensities with the increase of the temperature. These observations can have important implications on the magnetic data recording applications of these nanostructures by helping in better understanding the unusual temperature-dependent magnetic instabilities of iron-based nano-crystals which have been recently reported in literature.

Determination of Debye temperatures and Lamb-Mössbauer factors for LnFeO3 orthoferrite perovskites (Ln  =  La, Nd, Sm, Eu, Gd)

NASA Astrophysics Data System (ADS)

Scrimshire, A.; Lobera, A.; Bell, A. M. T.; Jones, A. H.; Sterianou, I.; Forder, S. D.; Bingham, P. A.

2018-03-01

Lanthanide orthoferrites have wide-ranging industrial uses including solar, catalytic and electronic applications. Here a series of lanthanide orthoferrite perovskites, LnFeO3 (Ln  =  La Nd; Sm; Eu; Gd), prepared through a standard stoichiometric wet ball milling route using oxide precursors, has been studied. Characterisation through x-ray diffraction and x-ray fluorescence confirmed the synthesis of phase-pure or near-pure LnFeO3 compounds. 57Fe Mössbauer spectroscopy was performed over a temperature range of 10 K-293 K to observe hyperfine structure and to enable calculation of the recoil-free fraction and Debye temperature (θ D) of each orthoferrite. Debye temperatures (Ln  =  La 474 K Nd 459 K Sm 457 K Eu 452 K Gd 473 K) and recoil-free fractions (Ln  =  La 0.827; Nd 0.817; Sm 0.816; Eu 0.812; Gd 0.826) were approximated through minimising the difference in the temperature dependent experimental centre shift and theoretical isomer shift, by allowing the Debye temperature and isomer shift values to vary. This method of minimising the difference between theoretical and actual values yields Debye temperatures consistent with results from other studies determined through thermal analysis methods. This displays the ability of variable-temperature Mössbauer spectroscopy to approximate Debye temperatures and recoil-free fractions, whilst observing temperature induced transitions over the temperature range observed. X-ray diffraction and Rietveld refinement show an inverse relationship between FeO6 octahedral volume and approximated Debye temperatures. Raman spectroscopy show an increase in the band positions attributed to soft modes of Ag symmetry, Ag(3) and Ag(5) from La to GdFeO3 corresponding to octahedral rotations and tilts in the [0 1 0] and [1 0 1] planes respectively.

Phase transformation, improved ferroelectric and magnetic properties of (1 − x) BiFeO{sub 3}–xPb(Zr{sub 0.52}Ti{sub 0.48})O{sub 3} solid solutions

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sharma, Subhash, E-mail: rk.dwivedi@jiit.ac.in, E-mail: subhash1jiit@gmail.com; Singh, Vikash; Dwivedi, R. K., E-mail: rk.dwivedi@jiit.ac.in, E-mail: subhash1jiit@gmail.com

2014-06-14

The authors prepared (1 − x)BiFeO{sub 3} – (x)Pb(Zr{sub 0.52}Ti{sub 0.48})O{sub 3} for x ≤ 0.30 by sol-gel method and investigated the material's structures, magnetic and electrical properties. Detailed Rietveld analysis of X-ray diffraction data revealed that the system retains distorted rhombohedral R3c structure for x ≤ 0.10 but transforms to monoclinic (Cc) structure for x > 0.10. Disappearance of some Raman modes corresponding to A1 modes and the decrease in the intensities of the remaining A1 modes with increasing x in the Raman spectra, which is a clear indication of structural modification and symmetry changes brought about by PZT doping. Enhanced magnetization with PZT doping content maymore » be attributed to the gradual change and destruction in the spin cycloid structure of BiFeO{sub 3.} The leakage current density at 3.5 kV/cm was reduced by approximately three orders of magnitude by doping PZT (x = 0.30), compared with BFO ceramics.« less

Structural, magnetic, and electrical properties of (1-x)Bi0.85La0.15FeO3-(x)CoFe2O4 multiferroic composites

NASA Astrophysics Data System (ADS)

Pandey, Rabichandra; Pradhan, Lagen Kumar; Kar, Manoranjan

2018-04-01

In this study, the tartaric acid modified sol-gel method was used to synthesize (1-x)Bi0.85La0.15FeO3-(x)CoFe2O4 (BLFO-CFO) composites where x = 0.00, 0.10, 0.20, 0.30, 0.40, and 0.50. The X-ray diffraction (XRD) patterns indicated the formation of composites with both BLFO and CFO crystal symmetry, i.e., perovskite and spinel structures, respectively. Rietveld refinement of the XRD patterns was performed for all of the samples in order to analyze the crystal phases and obtain the structural parameters. There were decreases in the lattice parameters of the perovskite phase as the CFO spinel phase increased in the composites, which may be explained by the strain at the interface of the BLFO and CFO phases. Electrical polarization and dielectric constant enhancements were observed in the BLFO-CFO composites compared with BLFO. The saturation magnetization increased as the CFO phase increased in the composites. The theoretical saturation magnetization (calculated using Vegard's law) was less than the experimentally observed value, possibly due to the spin interaction at the interface of BLFO and CFO.

Amorphization of Ta2O5 under swift heavy ion irradiation

NASA Astrophysics Data System (ADS)

Cusick, Alex B.; Lang, Maik; Zhang, Fuxiang; Sun, Kai; Li, Weixing; Kluth, Patrick; Trautmann, Christina; Ewing, Rodney C.

2017-09-01

Crystalline Ta2O5 powder is shown to amorphize under 2.2 GeV 197Au ion irradiation. Synchrotron X-ray diffraction (XRD), Raman spectroscopy, small-angle X-ray scattering (SAXS), and transmission electron microscopy (TEM) were used to characterize the structural transition from crystalline to fully-amorphous. Based on Rietveld refinement of XRD data, the initial structure is orthorhombic (P2mm) with a very large unit cell (a = 6.20, b = 40.29, c = 3.89 Å; V = 971.7 Å3), ideally containing 22 Ta and 55 O atoms. At a fluence of approximately 3 × 1011 ions/cm2, a diffuse amorphous background becomes evident, increasing in intensity relative to diffraction maxima until full amorphization is achieved at approximately 3 × 1012 ions/cm2. An anisotropic distortion of the orthorhombic structure occurred during the amorphization process, with an approximately constant unit cell volume. The amorphous phase fraction as a function of fluence was determined, yielding a trend that is consistent with a direct-impact model for amorphization. SAXS and TEM data indicate that ion tracks exhibit a core-shell morphology. Raman data show that the amorphous phase is comprised of TaO6 and TaO5 coordination-polyhedra in contrast to the TaO6 and TaO7 units that exist in crystalline Ta2O5. Analysis of Raman data shows that oxygen-deficiency increases with fluence, indicating a loss of oxygen that leads to an estimated final stoichiometry of Ta2O4.2 at a fluence of 1 × 1013 ions/cm2.

Fabrication and testing of a newly designed slit system for depth-resolved X-ray diffraction measurements

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sinsheimer, John; Bouet, Nathalie; Ghose, Sanjit

2016-10-06

A new system of slits called `spiderweb slits' have been developed for depth-resolved powder or polycrystalline X-ray diffraction measurements. The slits act on diffracted X-rays to select a particular gauge volume of sample, while absorbing diffracted X-rays from outside of this volume. Although the slit geometry is to some extent similar to that of previously developed conical slits or spiral slits, this new design has advantages over the previous ones in use for complex heterogeneous materials andin situandoperandodiffraction measurements. For example, the slits can measure a majority of any diffraction cone for any polycrystalline material, over a continuous range ofmore » diffraction angles, and work for X-ray energies of tens to hundreds of kiloelectronvolts. The design is generated and optimized using ray-tracing simulations, and fabricated through laser micromachining. The first prototype was successfully tested at the X17A beamline at the National Synchrotron Light Source, and shows similar performance to simulations, demonstrating gauge volume selection for standard powders, for all diffraction peaks over angles of 2–10°. A similar, but improved, design will be implemented at the X-ray Powder Diffraction beamline at the National Synchrotron Light Source II.« less

Local terahertz field enhancement for time-resolved x-ray diffraction

DOE PAGES

Kozina, M.; Pancaldi, M.; Bernhard, C.; ...

2017-02-20

We report local field strength enhancement of single-cycle terahertz (THz) pulses in an ultrafast time-resolved x-ray diffraction experiment. We show that patterning the sample with gold microstructures increases the THz field without changing the THz pulse shape or drastically affecting the quality of the x-ray diffraction pattern. Lastly, we find a five-fold increase in THz-induced x-ray diffraction intensity change in the presence of microstructures on a SrTiO 3 thin-film sample.

Local terahertz field enhancement for time-resolved x-ray diffraction

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kozina, M.; Pancaldi, M.; Bernhard, C.

We report local field strength enhancement of single-cycle terahertz (THz) pulses in an ultrafast time-resolved x-ray diffraction experiment. We show that patterning the sample with gold microstructures increases the THz field without changing the THz pulse shape or drastically affecting the quality of the x-ray diffraction pattern. Lastly, we find a five-fold increase in THz-induced x-ray diffraction intensity change in the presence of microstructures on a SrTiO 3 thin-film sample.

Thermal x-ray diffraction and near-field phase contrast imaging

NASA Astrophysics Data System (ADS)

Li, Zheng; Classen, Anton; Peng, Tao; Medvedev, Nikita; Wang, Fenglin; Chapman, Henry N.; Shih, Yanhua

2017-10-01

Using higher-order coherence of thermal light sources, the resolution power of standard x-ray imaging techniques can be enhanced. In this work, we applied the higher-order measurement to far-field x-ray diffraction and near-field phase contrast imaging (PCI), in order to achieve superresolution in x-ray diffraction and obtain enhanced intensity contrast in PCI. The cost of implementing such schemes is minimal compared to the methods that achieve similar effects by using entangled x-ray photon pairs.

Thermal x-ray diffraction and near-field phase contrast imaging

DOE PAGES

Li, Zheng; Classen, Anton; Peng, Tao; ...

2017-12-27

Using higher-order coherence of thermal light sources, the resolution power of standard x-ray imaging techniques can be enhanced. Here in this work, we applied the higher-order measurement to far-field x-ray diffraction and near-field phase contrast imaging (PCI), in order to achieve superresolution in x-ray diffraction and obtain enhanced intensity contrast in PCI. The cost of implementing such schemes is minimal compared to the methods that achieve similar effects by using entangled x-ray photon pairs.

An image focusing means by using an opaque object to diffract x-rays

DOEpatents

Sommargren, Gary E.; Weaver, H. Joseph

1991-01-01

The invention provides a method and apparatus for focusing and imaging x-rays. An opaque sphere is used as a diffractive imaging element to diffract x-rays from an object so that the divergent x-ray wavefronts are transformed into convergent wavefronts and are brought to focus to form an image of the object with a large depth of field.

Soft X-Ray Diffraction Microscopy of a Frozen Hydrated Yeast Cell

DOE PAGES

Huang, Xiaojing; Nelson, Johanna; Kirz, Janos; ...

2009-11-01

We report the first image of an intact, frozen hydrated eukaryotic cell using x-ray diffraction microscopy, or coherent x-ray diffraction imaging. By plunge freezing the specimen in liquid ethane and maintaining it below -170 °C, artifacts due to dehydration, ice crystallization, and radiation damage are greatly reduced. In this example, coherent diffraction data using 520 eV x rays were recorded and reconstructed to reveal a budding yeast cell at a resolution better than 25 nm. This demonstration represents an important step towards high resolution imaging of cells in their natural, hydrated state, without limitations imposed by x-ray optics.

Fabrication and characterization of cerium-doped barium titanate inverse opal by sol-gel method

DOE Office of Scientific and Technical Information (OSTI.GOV)

Jin Yi; Zhu Yihua; Yang Xiaoling

Cerium-doped barium titanate inverted opal was synthesized from barium acetate contained cerous acetate and tetrabutyl titanate in the interstitial spaces of a polystyrene (PS) opal. This procedure involves infiltration of precursors into the interstices of the PS opal template followed by hydrolytic polycondensation of the precursors to amorphous barium titanate and removal of the PS opal by calcination. The morphologies of opal and inverse opal were characterized by scanning electron microscope (SEM). The pores were characterized by mercury intrusion porosimetry (MIP). X-ray photoelectron spectroscopy (XPS) investigation showed the doping structure of cerium, barium and titanium. And powder X-ray diffraction allowsmore » one to observe the influence of doping degree on the grain size. The lattice parameters, crystal size and lattice strain were calculated by the Rietveld refinement method. The synthesis of cerium-doped barium titanate inverted opals provides an opportunity to electrically and optically engineer the photonic band structure and the possibility of developing tunable three-dimensional photonic crystal devices. - Graphical abstract: Cerium-doped barium titanate inverted opal was synthesized from barium acetate acid contained cerous acetate and tetrabutyl titanate in the interstitial spaces of a PS opal, which involves infiltration of precursors into the interstices of the PS opal template and removal of the PS opal by calcination.« less

Anomalous structural disorder and distortion in metal-to-insulator-transition Ti{sub 2}O{sub 3}

DOE Office of Scientific and Technical Information (OSTI.GOV)

Hwang, In-Hui; Jin, Zhenlan; Park, Chang-In

2016-01-07

Mott proposed that impurity bands in corundum-symmetry Ti{sub 2}O{sub 3} at high temperatures caused a collapse in the bandgap. However, the origin of the impurity bands has not yet been clarified. We examine the local structural properties of metal-to-insulator-transition Ti{sub 2}O{sub 3} using in-situ x-ray absorption fine structure (XAFS) measurements at the Ti K edge in the temperature range from 288 to 739 K. The Ti{sub 2}O{sub 3} powder is synthesized by using a chemical reaction method. X-ray diffraction (XRD) measurements from Ti{sub 2}O{sub 3} with a Rietveld refinement demonstrate a single-phased R-3c symmetry without additional distortion. Extended-XAFS combined with XRDmore » reveals a zigzag patterned Ti position and an anomalous structural disorder in Ti-Ti pairs, accompanied by a bond length expansion of the Ti-Ti pairs along the c-axis for T > 450 K. The local structural distortion and disorder of the Ti atoms would induce impurity levels in the band gap between the Ti 3d a{sub 1g} and e{sub g}{sup π} bands, resulting in a collapse of the band gap for T > 450 K.« less

Optical and Structural Properties of Zn2TiO4:Mn2+

NASA Astrophysics Data System (ADS)

Sosman, L. P.; López, A.; Camara, A. R.; Pedro, S. S.; Carvalho, I. C. S.; Cella, N.

2017-12-01

Polycrystalline Zn2TiO4 samples with Mn2+ doping level of 0%, 0.1%, 1.0%, and 5.0% have been produced by conventional solid-state method and their optical and structural properties investigated. Rietveld refinement of x-ray diffraction patterns revealed the formed phases and the crystallographic parameters. The chemical composition was obtained by x-ray fluorescence measurements. The optical properties were studied by photoluminescence, excitation, reflectance, and photoacoustic spectroscopy. All measurements were performed at room temperature. The photoluminescence spectrum of the pure sample (0% Mn2+) showed a band in the red region associated with Zn2TiO4, while the sample with 0.1% Mn2+ exhibited two bands, in the green and red spectral regions, assigned to Mn2+ ions at tetrahedral and octahedral sites. No emission was observed for the samples with 1.0% or 5.0% Mn2+. The excitation results for the sample with 0.1% Mn2+ ions showed characteristic peaks of Mn2+ transitions. Tanabe-Sugano theory was used to obtain the crystal field Dq, B, and C Racah parameters from the energy peak positions in the excitation spectrum of the sample with 0.1% Mn2+. Photoacoustic measurements revealed a broad band, characteristic of semiconductor materials, hiding the Mn2+ transitions.

Observation of high-spin mixed oxidation state of cobalt in ceramic Co3TeO6

NASA Astrophysics Data System (ADS)

Singh, Harishchandra; Ghosh, Haranath; Chandrasekhar Rao, T. V.; Sinha, A. K.; Rajput, Parasmani

2014-12-01

We report coexistence of high spin Co3+ and Co2+ in ceramic Co3TeO6 using X-ray Absorption Near Edge Structure (XANES), DC magnetization, and first principles ab-initio calculations. The main absorption line of cobalt Co K-edge XANES spectra, along with a linear combination fit, led us to estimate relative concentration of Co2+ and Co3+as 60:40. The pre edge feature of XANES spectrum shows crystal field splitting of ˜1.26 eV between eg and t2g states, suggesting a mixture of high spin states of both Co2+ and Co3+. Temperature dependent high field DC magnetization measurements reveal dominant antiferromagnetic order with two Neel temperatures (TN1 ˜ 29 K and TN2 ˜ 18 K), consistent with single crystal study. A larger effective magnetic moment is observed in comparison to that reported for single crystal (which contains only Co2+), supports our inference that Co3+ exists in high spin state. Furthermore, we show that both Co2+ and Co3+ being in high spin states constitute a favorable ground state through first principles ab-initio calculations, where Rietveld refined synchrotron X-ray diffraction data are used as input.

Influences of Sr dose on the crystal structure parameters and Sr distributions of Sr-incorporated hydroxyapatite.

PubMed

Guo, D G; Hao, Y Z; Li, H Y; Fang, C Q; Sun, L J; Zhu, H; Wang, J; Huang, X F; Ni, P F; Xu, K W

2013-10-01

Stoichiometric strontium-incorporated hydroxyapatite (Sr-HA) with different Sr concentrations [Sr/(Sr+Ca)] were synthesized using a wet chemical approach and characterized by X-ray diffraction, Fourier-transformed infrared absorption, X-ray photoelectron spectroscopy, and Rietveld Structure Refinement. The crystal lattice parameter, Sr distribution, chemical state of Sr, and also the relationships between their variations and the Sr concentrations have been intensively studied. The results show that both the crystal lattice parameters and crystal plane space of Sr-HA remarkably increase with the Sr concentration increasing. Whether Sr preferably occupies the Ca(I) site or Ca(II) site after incorporated into apatite lattice depends on the Sr number incorporated into apatite. All the Sr ions completely occupy the Ca(II) sites when the Sr concentration is below 5%. With the exception of partial Sr ions occupying the Ca(II) sites, the other Sr ions start to occupy the Ca(I) sites when the Sr concentration doped in HA is beyond 10%. The ratio of Sr ions occupying the Ca(I) sites increases with the further raising Sr concentration up to 20%. The Sr ions inherit the chemical state and environment of the original Ca(I) or Ca(II) site after incorporated into apatite. Copyright © 2013 Wiley Periodicals, Inc.

Electronic and Crystalline Structure, Magnetic Response, and Optical Characterization of Rare-Earth Ruthenate Sr2HoRuO6

NASA Astrophysics Data System (ADS)

Velásquez Moya, X. A.; Cardona, R.; Villa Hernández, J. I.; Landínez Téllez, D. A.; Roa-Rojas, J.

2018-03-01

Sr2HoRuO6 ceramic has been synthesized and its structural, morphological, magnetic, optical, and electronic properties studied. Rietveld refinement of x-ray diffraction patterns revealed that this oxide material crystallizes in monoclinic perovskite structure in space group P2 1 /n (no. 14). Scanning electron microscopy revealed polycrystalline surface morphology. x-Ray dispersive spectroscopy suggested that Sr2HoRuO6 was obtained with expected stoichiometry. Magnetic susceptibility curves as a function of temperature revealed ferrimagnetic feature of this material below the Néel temperature T N of 14 K. Evidence of magnetic disorder was provided by the irreversibility observed in the zero-field-cooled and field-cooled responses of the susceptibility below T irr = 169 K. Analysis of the diffuse reflectance spectrum suggested that this material behaves as a semiconductor with energy gap E g of 1.38 eV. Results of band structure and density-of-states calculations are in agreement with the interpretation of Sr2HoRuO6 as a semiconductor. The ferrimagnetic behavior is interpreted as due to exchange mechanisms of d-f (Ru-O-Ho) electrons. The effective magnetic moment calculated from density functional theory was 93.5% of the experimental value obtained from Curie-Weiss fitting of the susceptibility curve.

Effect of copper concentration in the electrolyte on the surface morphology and the microstructure of CuInSe2 films

NASA Astrophysics Data System (ADS)

Hung, Pin-Kun; Kuo, Ting-Wei; Huang, Kuo-Chan; Wang, Na-Fu; Hsieh, Po-Tsung; Houng, Mau-Phon

2012-07-01

The surface morphology and the microstructure of CuInSe2 precursor films have been investigated by co-electrodeposition with different [Cu2+] concentrations from 2 mM to 4 mM. The characteristic of the precursor films was examined using field-emission scanning electron microscopy (FE-SEM), energy dispersive X-ray spectroscopy (EDS), glancing incidence angle X-ray diffraction (GIXRD) and micro-Raman spectrometer, respectively. The surface morphology of the precursor films become more smoother and compact with choice of appropriate [Cu2+] concentration (3-3.5 mM) in the electrolyte. The relation between surface morphology and [Cu2+] concentration is also considered in terms of electrodeposition nucleation mechanisms using the mathematical models of Scharifker and Hills. It is suggested that the higher [Cu2+] concentrations can provide more numbers of nucleation sites on the surface of the electrode. Results simulated from the Rietveld refinement method suggest that decreasing dCusbnd Se is related to charge transfer from interstitial copper atoms and can affect the film microstructure. Micro-Raman spectrum also shows that the excess Cu atoms in the precursor films does not contribute significantly to large amounts of secondary phases but rather exists in the crystallite structure as other defect types.

Four new polymorphic forms of suplatast tosilate.

PubMed

Nagai, Keiko; Ushio, Takanori; Miura, Hidenori; Nakamura, Takashi; Moribe, Kunikazu; Yamamoto, Keiji

2014-01-02

We found four new polymorphic forms (γ-, ε-, ζ-, and η-forms) of suplatast tosilate (ST) by recrystallization and seeding with ST-analogous compounds; three polymorphic forms (α-, β-, and δ-forms) of ST have been previously reported. The physicochemical properties of these new forms were investigated using infrared (IR) spectroscopy, solid-state nuclear magnetic resonance (NMR) spectroscopy, differential scanning calorimetry, and powder X-ray diffractometry. The presence of hydrogen bonds in the new forms was assessed from the IR and solid-state NMR spectra. The crystal structures of the ε- and η-forms were determined from their powder X-ray diffraction data using the direct space approach and the Monte Carlo method, followed by Rietveld refinement. The structures determined for the ε- and η-forms supported the presence of hydrogen bonds between the ST molecules, as the IR and solid-state NMR spectra indicated. The thermodynamic characteristics of the seven polymorphic forms were evaluated by determining the solubility of each form. The α-form was the most insoluble in 2-propanol at 35°C, and was thus concluded to be the most stable form. The ε-form was the most soluble, and a polymorphic transition from the ε- to the α-form was observed during solubility testing. Copyright © 2013 Elsevier B.V. All rights reserved.

Low-temperature x-ray crystal structure analysis of the cage-structured compounds M Be13 (M =La,Sm, and U)

NASA Astrophysics Data System (ADS)

Hidaka, Hiroyuki; Nagata, Ryoma; Tabata, Chihiro; Shimizu, Yusei; Miura, Naoyuki; Yanagisawa, Tatsuya; Amitsuka, Hiroshi

2018-05-01

The beryllides M Be13 (M = rare earths and actinides) crystallize in a NaZn13-type cubic structure, which can be categorized as a cage-structured compound. In this study, powder x-ray diffraction measurements have been performed on LaBe13,SmBe13, and UBe13 in the temperature range between 7 and 300 K in order to investigate their crystallographic characteristics systematically. They keep the NaZn13-type cubic structure down to the lowest temperature. We estimated their Debye temperature to be 600-750 K from analyses of the temperature dependence of a lattice parameter, being in good agreement with the values reported previously. Rietveld refinements on the obtained powder patterns revealed that the M atom in the 8 a site is located in an almost ideal snub cube formed by 24 BeII atoms in the 96 i site, whose caged structure is unchanged even at the low temperatures. In addition, it is argued from the temperature variation of an isotropic mean-square displacement parameter that the M Be13 compounds commonly have a low-energy phonon mode, which can be described by a model assuming an Einstein oscillation of the M atom with a characteristic temperature of ˜160 K.

Application of focused-beam flat-sample method to synchrotron powder X-ray diffraction with anomalous scattering effect

NASA Astrophysics Data System (ADS)

Tanaka, M.; Katsuya, Y.; Matsushita, Y.

2013-03-01

The focused-beam flat-sample method (FFM), which is a method for high-resolution and rapid synchrotron X-ray powder diffraction measurements by combination of beam focusing optics, a flat shape sample and an area detector, was applied for diffraction experiments with anomalous scattering effect. The advantages of FFM for anomalous diffraction were absorption correction without approximation, rapid data collection by an area detector and good signal-to-noise ratio data by focusing optics. In the X-ray diffraction experiments of CoFe2O4 and Fe3O4 (By FFM) using X-rays near the Fe K absorption edge, the anomalous scattering effect between Fe/Co or Fe2+/Fe3+ can be clearly detected, due to the change of diffraction intensity. The change of observed diffraction intensity as the incident X-ray energy was consistent with the calculation. The FFM is expected to be a method for anomalous powder diffraction.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Viani, Alberto, E-mail: viani@itam.cas.cz; Sotiriadis, Konstantinos; Len, Adél

Full characterization of fired-clay bricks is crucial for the improvement of process variables in manufacturing and, in case of old bricks, for restoration/replacement purposes. To this aim, five bricks produced in a plant in Czech Republic in the past have been investigated with a combination of analytical techniques in order to derive information on the firing process. An additional old brick from another brickyard was also used to study the influence of different raw materials on sample microstructure. The potential of X-ray diffraction with the Rietveld method and small angle neutron scattering technique has been exploited to describe the phasemore » transformations taking place during firing and characterize the brick microstructure. Unit-cell parameter of spinel and amount of hematite are proposed as indicators of the maximum firing temperature, although for the latter, limited to bricks produced from the same raw material. The fractal quality of the surface area of pores obtained from small angle neutron scattering is also suggested as a method to distinguish between bricks produced from different raw clays. - Highlights: • Rietveld method helps in describing microstructure and physical properties of bricks. • XRPD derived cell parameter of spinel is proposed as an indicator of firing temperature. • SANS effectively describes brick micro and nanostructure, including closed porosity. • Fractal quality of pore surface is proposed as ‘fingerprint’ of brick manufacturing.« less

Synthesis and crystal structure of LiCuFe{sub 2}(VO{sub 4}){sub 3} by Rietveld method

DOE Office of Scientific and Technical Information (OSTI.GOV)

Belik, A.A.

1999-10-01

A new triple vanadate LiCuFe{sub 2}(VO{sub 4}){sub 3} was synthesized by a solid-state method. The compound is isotypic with mineral howardevansite, NaCuFe{sub 2}(VO{sub 4}){sub 3}, and crystallizes in a triclinic system (space group P{bar 1} (No. 2); a = 8.1484(5), b = 9.8024(7), c = 6.6355(4) {angstrom}, {alpha} = 103.832(3), {beta} = 102.353(3), {gamma} = 106.975(3), V = 468.68 {angstrom}{sup 3}, Z = 2). Crystal structure of LiCuFe{sub 2}(VO{sub 4}){sub 3} was refined by Rietveld method with R{sub WP} = 2.32%, R{sub P} = 1.76%, R{sub I} = 2.82%, S = 1.55, using X-ray diffraction. The crystal structure has fivemore » independent cation sites. Lithium cations are located in the cavities M(1)O{sub 6} and M(5)O{sub 10}, which form infinite chains in the [001] direction and are linked through a common face. The lithium cation in the M(1)O{sub 6} cavity has a square planar coordination. The lithium cation in the M(5)O{sub 10} cavity is strongly displaced up to 1.2 {angstrom} from the special position (0, 0, 0.5) to a half-occupied general position (0.037, 0.087, 0.40).« less

Effect of laser irradiation on Ag4In12Sb56Te28

NASA Astrophysics Data System (ADS)

Chinnusamy, Rangasami

2018-04-01

Ag4In12Sb56Te28 has been synthesized by melt-quench method. Phase homogeneity, crystal structure and effect of laser irradiation have been investigated using X-ray diffraction (XRD) and Raman spectroscopy. Rietveld refinement of crystal structure revealed that Ag4In12Sb56Te28 is a multiphase system with AgIn3Te5, Sb8Te3 and Sb phases. Combined optical microscopy and Raman spectroscopy have been used to understand the distribution of different phases on the surface of the samples, which substantiated the results of Rietveld analysis. Interaction of 20 mW laser beam with samples has been investigated using Raman measurements. The results have shown that regions with large phase fraction of AgIn3Te5 become amorphous during laser-sample interaction, but the starting phase remains nearly same after the interaction. Regions with AgIn3Te5 and nearly equal or larger amount of Sb8Te3 have shown significant growth of α-Sb2O3 during and after laser-sample interaction. Regions rich in Sb have shown formation of AgIn3Te5 and growth of α-Sb2O3 during and after interaction. These observations have been explained based on the maximum temperature rise at different regions during laser-sample interaction.

Design of Functional Layered Oxide Materials Through Understanding Structure-Property Relationships

NASA Astrophysics Data System (ADS)

Strayer, Megan E.

A fundamental understanding of structure-property relationships is imperative in the rational design of new materials for tailored applications. In this dissertation, structureproperty relationships are exploited in layered oxides and their composite materials. Recent advances in characterization techniques have allowed for more in-depth investigations into both the atomic level structure and properties of these materials. This dissertation focuses on understanding the structure-property relationships in supported catalytic systems and ferroelectric materials to aid in the rational design of functional materials. In Chapter 2, a correlation between the enthalpy of nanoparticle adsorption to oxide supports and the subsequent growth of these nanoparticles as a function of temperature is investigated. When deposited onto layered niobium oxide and tantalum oxide supports, rhodium hydroxide nanoparticles remain small and evenly dispersed upon heating to 750 °C. Using isothermal titration calorimetry, the bonding enthalpy of rhodium hydroxide nanoparticles to oxide supports is quantified for the first time under the wet synthetic conditions of catalyst preparation. Rh(OH)3 is concluded to have a strong, covalent interaction with the early transition metal oxide supports, and the interfacial bonding is hypothesized to occur through Rh - O - Nb bonding. Chapter 3 extends the studies in Chapter 2 to include supported metal, metal oxide, and metal hydroxide nanoparticles in the cobalt, nickel and copper triads. The data confirms a strong correlation between the heats of interaction and stability of the supported nanoparticles. Both experimental data and density functional theory calculations demonstrate that the support and nanoparticle compositions impact the heat of interaction and that the qualitative periodic trends of the metal bonding interaction are independent of the metal oxidation state. A strong bond is shown computationally to arise from the formation of mixed d-states between an adsorbed metal atom and a metal atom in the support. A preliminary investigation into the synthesis and stability of catalytically relevant ligand-free metal nanoparticles is presented in Chapter 4. The nanoparticles are synthesized via base hydrolysis and reduction with methanol. When deposited onto a niobium oxide support, the nanoparticles are thermally stable at temperatures up to 900 °C. The mechanism of platinum nanoparticle formation is still largely unknown, and a synthesis of rhodium and iridium ligand-free nanoparticles is reported. In Chapter 5, the n = 2 Dion Jacobson family A'LaB2O 7 (A': Rb, Cs; B: Nb, Ta) is reported as non-centrosymmetric and piezoelectric at room temperature for the first time. This non-centrosymmetry is predicted to arise from two nonpolar oxygen octahedral rotational modes condensing via the hybrid improper ferroelectricity mechanism. Rietveld refinement of synchrotron X-ray diffraction data is unable to confirm an acentric crystal structure as peak splitting is evident, revealing that multiple phases are likely present in these materials. Chapter 6 presents temperature-dependent synchrotron X-ray diffraction and neutron diffraction Rietveld refinement analysis of CsLaNb2O 7 to investigate the crystal structure and mechanism of non-centrosymmetry. The crystal structure is found to be in the centrosymmetric P4/mmm phase at 600 K and above. From 550 K to 350 K, the space group is assigned to the non-centrosymmetric Amm2 phase, as SHG signal is steadily increasing over this temperature range. Unfortunately, the 300 K and below crystal structure(s) have yet to be solved. Currently, both single-phase and dual-phase models are being refined in the synchrotron X-ray and neutron diffraction data.

Preparation and structure of BiCrTeO{sub 6}: A new compound in Bi–Cr–Te–O system. Thermal expansion studies of Cr{sub 2}TeO{sub 6}, Bi{sub 2}TeO{sub 6} and BiCrTeO{sub 6}

DOE Office of Scientific and Technical Information (OSTI.GOV)

Vats, Bal Govind; Phatak, Rohan; Krishnan, K.

Graphical abstract: A new compound BiCrTeO{sub 6} in the Bi–Cr–Te–O system was prepared by solid state route and characterized by X-ray diffraction method. The crystal structure of BiCrTeO{sub 6} shows that there is one distinct site for bismuth (Bi) atom (pink color), one chromium rich (Cr/Te = 68/32) (blue/green color), one tellurium rich (Te/Cr = 68/32) sites (green/blue color), and one distinct site for oxygen (O) atom (red color) in the unit cell. All cations in this structure show an octahedral coordination with oxygen atoms at the corners. The thermogram (TG) of the compound in air shows that it ismore » stable up to 1103 K and decomposes thereafter. The thermal expansion behaviour of BiCrTeO{sub 6} was studied using high temperature X-ray diffraction method from room temperature to 923 K under vacuum of 10{sup −8} atmosphere and showed positive thermal expansion with the average volume thermal expansion coefficients of 16.0 × 10{sup −6}/K. - Highlights: • A new compound BiCrTeO{sub 6} in Bi–Cr–Te–O system was prepared and characterized. • The crystal structure of BiCrTeO{sub 6} was determined by Rietveld refinement method. • The structure of BiCrTeO{sub 6} shows an octahedral coordination for all the metal ions. • The thermal expansion behavior of BiCrTeO{sub 6} from room temperature to 923 K showed a positive thermal expansion. • The average volume thermal expansion coefficient for BiCrTeO{sub 6} is 16.0 × 10{sup −6}/K. - Abstract: A new compound BiCrTeO{sub 6} in Bi–Cr–Te–O system was prepared by solid state reaction of Bi{sub 2}O{sub 3}, Cr{sub 2}O{sub 3} and H{sub 6}TeO{sub 6} in oxygen and characterized by X-ray diffraction (XRD) method. It could be indexed on a trigonal lattice, with the space group P-31c, unit cell parameters a = 5.16268(7) Å and c = 9.91861(17) Å. The crystal structure of BiCrTeO{sub 6} was determined by Rietveld refinement method using the powder XRD data. Structure shows that there is one distinct site for bismuth (Bi) atom, one chromium rich (Cr/Te = 68/32), and one tellurium rich (Te/Cr = 68/32) sites, and one distinct site for oxygen (O) atom in the unit cell. All cations in this structure show an octahedral coordination with oxygen atoms at the corners. The thermogravimetric analysis (TGA) of the compound in air shows that it is stable up to 1103 K and decomposes thereafter. The thermal expansion behavior of Cr{sub 2}TeO{sub 6}, Bi{sub 2}TeO{sub 6} and BiCrTeO{sub 6} was studied using High Temperature X-ray diffraction (HTXRD) method from room temperature to 973, 873 and 923 K respectively under vacuum of 10{sup −8} atmospheres. All the compounds showed positive thermal expansion with the average volume thermal expansion coefficients of 14.38 × 10{sup −6}/K, 22.0 × 10{sup −6}/K and 16.0 × 10{sup −6}/K respectively.« less

DOE Office of Scientific and Technical Information (OSTI.GOV)

Taran, Subhrangsu, E-mail: ami.subhra@gmail.com; Sun, C. P.; Yang, H. D.

A detail study of transport and magnetic properties of La{sub 1-x}Li{sub x}MnO{sub 3+δ} (0.05 ≤ x ≤ 0.3) system synthesized by wet-chemical mixing route has been done. The room temperature x-ray powder diffraction (XRD) data show single phase behavior of all samples except x = 0.3. Rietveld refinement of XRD data shows structural transition from rhombohedral (R3-C) to orthorhombic (Pnma) symmetry occurs at the Li-doping level x > 0.2 with both the lattice parameter and unit-cell volume decrease with increase of ‘x’. All the samples show ferromagnetic (FM) behavior while metallic behavior are shown by the samples up to Li-concentrationmore » x = 0.2. With further Li doping i.e. for x = 0.25, the sample shows insulating behavior accompanied by charge-order transition around T ~ 225 K. Metallic part of the resistivity data of the samples is best fitted with an expression ρ(T) = ρ{sub 0} + ρ{sub 4.5}T{sup 4.5} + C/ sinh{sup 2}(hv{sub s}/2k{sub B}T) containing small-polaron contribution (last term). Most interesting finding in the present study is the observation of large anomalous decrease in thermoelectric power (S) below 100 K shown by the sample with x = 0.25. Probable mechanisms responsible for the observed colossal thermoelectric power have been discussed.« less

Structural stability, enhanced magnetic, piezoelectric, and transport properties in (1-x)BiFeO3-(x)Ba0.70Sr0.30TiO3 nanoparticles

NASA Astrophysics Data System (ADS)

Sharma, Subhash; Singh, Vikash; Anshul, Avneesh; Siqueiros, J. M.; Dwivedi, R. K.

2018-05-01

Multiferroic samples with composition (1-x)BiFeO3-(x)(Ba0.70Sr0.30)TiO3 (BFO-BST) were synthesized using a sol-gel route to study the effect of BST doping on structural, transport, and magnetic properties in BiFeO3 (BFO). X-ray diffraction studies with Rietveld analysis revealed that a phase transition occurred from rhombohedral (R3c) (0.0 ≤ × ≤ 0.15) to tetragonal (P4 mm) for x = 0.20 and nanocrystalline nature confirmed by transmission electron microscopy measurements. Piezoelectric properties improved as x increased from x = 0.0 (58 pC/N) to x = 0.20 (112 pC/N) increasing distortion in the crystal structure as evinced by Williamson-Hall analysis. Ferromagnetism was observed in doped BFO, different from the antiferromagnetic ordering in bulk BFO, indicating the noteworthy size effects and Fe-O-Fe bond angle variations in the magnetic ordering of BFO. An improvement in ferroelectric properties is observed with doping of BST compared to pristine BFO. Thermally activated conduction behavior occurred at low and high temperature regions as revealed by temperature dependent dc resistivity measurement. Effective improvements in dielectric response, meaning high dielectric constant with a low dielectric loss, were found in the doped samples.

Synthesis temperature effect on the structural features and optical absorption of Zn(1-x)Co(x)Al2O4 oxides.

PubMed

Gaudon, M; Apheceixborde, A; Ménétrier, M; Le Nestour, A; Demourgues, A

2009-10-05

Zinc/cobalt aluminates with spinel-type structure were prepared by a polymeric route, leading to a pure phase with controlled grain size. The prepared pigments were characterized by powder X-ray diffraction Rietveld analyses in order to determine structural features, scanning electron microscopy for morphological investigation, helium pycnometry and (27)Al MAS NMR in order to highlight the occurrence of defects inside the structure, and UV-visible-near-IR spectroscopy to identify electronic transitions responsible for the compounds' color. The green-blue coloration of these pigments is known to be dependent on the sample thermal history. Here, for the first time, the Zn(1-x)Co(x)Al(2)O(4) color is newly interpreted. The pigment is green once synthesized at low temperature (i.e., with diminution of the pigment grain size); this variation was attributed to the appearance of a new absorption band located at about 500 nm, linked to a complex network feature involving Co ions in octahedral sites as well as oxygen and cationic vacancies. Hence, this work shows the possibility of easily getting a nonstoichiometric network with an abnormal cationic distribution from "chimie douce" processes with moderate synthesis temperature, and so various colorations for the same composition.

Effect of cobalt doping on structural and dielectric properties of nanocrystalline LaCrO3

NASA Astrophysics Data System (ADS)

Zarrin, Naima; Husain, Shahid

2018-05-01

Pure and Co doped Lanthanum chromite (LaCrO3) nanoparticles, LaCr1-xCoxO3 (0≤x≤0.3), have been synthesized through sol-gel process and their structural, morphological and dielectric properties have been studied. X ray diffraction patterns reveal that the samples are in single phase having orthorhombic structure with Pnma space group. Structural parameters are refined by Rietveld refinement using Fullprof software. Lattice parameters and unit cell volume are found to decrease with increase in Co doping. Crystallite size is calculated using Scherrer equation and is also found to decrease with increase in Co concentration. Surface morphology is examined using SEM-EDX analysis, which confirms the formation of regular and homogeneous samples without any impurities. The value of dielectric constant (ɛ') decreases with the increase in frequency while it enhances with the increase in Co concentration. The log (ɛ'×f) versus log (f) graphs have been plotted to verify the universal dielectric response (UDR) model. All the samples follow UDR model in the low frequency range.

High-throughput continuous hydrothermal synthesis of an entire nanoceramic phase diagram.

PubMed

Weng, Xiaole; Cockcroft, Jeremy K; Hyett, Geoffrey; Vickers, Martin; Boldrin, Paul; Tang, Chiu C; Thompson, Stephen P; Parker, Julia E; Knowles, Jonathan C; Rehman, Ihtesham; Parkin, Ivan; Evans, Julian R G; Darr, Jawwad A

2009-01-01

A novel High-Throughput Continuous Hydrothermal (HiTCH) flow synthesis reactor was used to make directly and rapidly a 66-sample nanoparticle library (entire phase diagram) of nanocrystalline Ce(x)Zr(y)Y(z)O(2-delta) in less than 12 h. High resolution PXRD data were obtained for the entire heat-treated library (at 1000 degrees C/1 h) in less than a day using the new robotic beamline I11, located at Diamond Light Source (DLS). This allowed Rietveld-quality powder X-ray diffraction (PXRD) data collection of the entire 66-sample library in <1 day. Consequently, the authors rapidly mapped out phase behavior and sintering behaviors for the entire library. Out of the entire 66-sample heat-treated library, the PXRD data suggests that 43 possess the fluorite structure, of which 30 (out of 36) are ternary compositions. The speed, quantity and quality of data obtained by our new approach, offers an exciting new development which will allow structure-property relationships to be accessed for nanoceramics in much shorter time periods.

β-NaVOPO 4 obtained by a low-temperature synthesis process: A new 3.3 V cathode for sodium-ion batteries

DOE PAGES

He, Guang; Huq, Ashfia; Manthiram, Arumugam; ...

2016-02-02

Vanadyl phosphates (VOPO 4) represent a class of attractive cathodes in lithium-ion batteries. However, the exploration of this type of materials in sodium-ion batteries is rare. Here, we report for the first time the synthesis of orthorhombic β-NaVOPO 4 by first chemically extracting lithium from beta-LiVOPO 4 and then inserting sodium into the obtained β-VOPO 4 by a microwave-assisted solvothermal process with NaI, which serves both as a reducing agent and sodium source. Intermediate Na xVOPO 4 compositions with x = 0.3, 0.5, and 0.8 have also been obtained by controlling the amount of NaI in the reaction mixture. Jointmore » Rietveld refinement of synchrotron X-ray diffraction (XRD) and neutron diffraction confirms that the fully sodiated β-NaVOPO 4 is isostructural with the lithium counterpart β-LiVOPO 4. Bond valence sum maps suggest that sodium ions possibly diffuse along the [010] direction in the lattice, similar to the ionic conduction pathway in β-LiVOPO 4. Although the initial discharge capacity is low due to the protons in the structure, it steadily increases with cycling with a long plateau at 3.3 V. As a result, ex situ XRD data of cycled β-VOPO 4 and β-NaVOPO 4 electrodes confirm the reversible reaction in sodium cells involving the V 4+/V 5+ redox couple.« less

Dynamical effects in Bragg coherent x-ray diffraction imaging of finite crystals

NASA Astrophysics Data System (ADS)

Shabalin, A. G.; Yefanov, O. M.; Nosik, V. L.; Bushuev, V. A.; Vartanyants, I. A.

2017-08-01

We present simulations of Bragg coherent x-ray diffractive imaging (CXDI) data from finite crystals in the frame of the dynamical theory of x-ray diffraction. The developed approach is based on a numerical solution of modified Takagi-Taupin equations and can be applied for modeling of a broad range of x-ray diffraction experiments with finite three-dimensional crystals of arbitrary shape also in the presence of strain. We performed simulations for nanocrystals of a cubic and hemispherical shape of different sizes and provided a detailed analysis of artifacts in the Bragg CXDI reconstructions introduced by the dynamical diffraction. Based on our theoretical analysis we developed an analytical procedure to treat effects of refraction and absorption in the reconstruction. Our results elucidate limitations for the kinematical approach in the Bragg CXDI and suggest a natural criterion to distinguish between kinematical and dynamical cases in coherent x-ray diffraction on a finite crystal.

Structural and optical properties of co-precipitated copper doped zinc oxide

NASA Astrophysics Data System (ADS)

Pandey, Devendra K.; Modi, Anchit; Pandey, Padmini; Gaur, N. K.

2018-05-01

We have synthesized pure and copper doped zinc oxide Zn1-xO:Cux (x = 0, 0.03) powder by wet chemical co-precipitation method followed by sintering of the co-precipitated amorphous phase powder at 450°C for 4 hours. The experiment is performed to recognize the effect of nominal doping of transition metal over the structural, morphological and optical properties. The structural parameters are observed by using Rietveld refinement of X-ray diffraction data which clearly represents that Cu ion is perfectly incorporated at the Zn site with minimal distortions within the lattice. The crystallite size is estimated by Debye-Scherrer and Hall-Williamson formulation. The particle morphology and size is determined with scanning electron microscopic (SEM) technique. The band gap and optical measurements are carried out with UV-visible absorption and photoluminescence (PL) spectroscopic technique, respectively. Enhanced PL spectral response is observed for ZnO:Cu along with non-radiative transitions from conduction band to valence band. The energy levels near the conduction band that are commonly involved in the optoelectronic transitions in the UV-region are traced by using absorption and luminescence spectral graphs.

Room temperature ferromagnetism in Mn-doped NiO nanoparticles

NASA Astrophysics Data System (ADS)

Layek, Samar; Verma, H. C.

2016-01-01

Mn-doped NiO nanoparticles of the series Ni1-xMnxO (x=0.00, 0.02, 0.04 and 0.06) are successfully synthesized using a low temperature hydrothermal method. Samples up to 6% Mn-doping are single phase in nature as observed from powder x-ray diffraction (XRD) studies. Rietveld refinement of the XRD data shows that all the single phase samples crystallize in the NaCl like fcc structure with space group Fm-3m. Unit cell volume decreases with increasing Mn-doping. Pure NiO nanoparticles show weak ferromagnetism, may be due to nanosize nature. Introduction of Mn within NiO lattice improves the magnetic properties significantly. Room temperature ferromagnetism is found in all the doped samples whereas the magnetization is highest for 2% Mn-doping and then decreases with further doping. The ZFC and FC branches in the temperature dependent magnetization separate well above 350 K indicating transition temperature well above room temperature for 2% Mn-doped NiO Nanoparticle. The ferromagnetic Curie temperature is found to be 653 K for the same sample as measured by temperature dependent magnetization study using vibrating sample magnetometer (VSM) in high vacuum.

Instrument and method for X-ray diffraction, fluorescence, and crystal texture analysis without sample preparation

NASA Technical Reports Server (NTRS)

Gendreau, Keith (Inventor); Martins, Jose Vanderlei (Inventor); Arzoumanian, Zaven (Inventor)

2010-01-01

An X-ray diffraction and X-ray fluorescence instrument for analyzing samples having no sample preparation includes a X-ray source configured to output a collimated X-ray beam comprising a continuum spectrum of X-rays to a predetermined coordinate and a photon-counting X-ray imaging spectrometer disposed to receive X-rays output from an unprepared sample disposed at the predetermined coordinate upon exposure of the unprepared sample to the collimated X-ray beam. The X-ray source and the photon-counting X-ray imaging spectrometer are arranged in a reflection geometry relative to the predetermined coordinate.

Influence of Fe-substitution on structural, magnetic and magnetocaloric properties of Nd2Fe17-xCox solid solutions

NASA Astrophysics Data System (ADS)

Bouchaala, N.; Jemmali, M.; Bartoli, T.; Nouri, K.; Hentech, I.; Walha, S.; Bessais, L.; Salah, A. Ben

2018-02-01

Nd2Fe17-xCox (x = 0 , 1 , 2 , 3 , 4) intermetallic compounds, obtained under arc-melting conditions, have been investigated by means of X-ray diffraction analysis (XRD), Mössbauer spectrometry and magnetic measurements. The Rietveld refinement revealed that the sample is a pure compound with rhombohedral Th2Zn17-type structure (R 3 bar m space group) with the following lattice parameters: a = 8.5792 (2) Å, c = 12.4615 (2) Å. Using Mössbauer spectrometry analysis coupled with structural consideration we have unambiguously determined the cobalt atoms preferred inequivalent crystallographic site. Nd2Fe17 show an increase of 3.5 T in their weighted average hyperfine fields upon cobalt substitution. Whatever the cobalt content, the hyperfine field of these compounds follow this sequence Hhf { 6 c } >Hhf { 9 d } >Hhf { 18 f } >Hhf { 18 h }. The magnetic measurements showed that the Curie temperature increases with the Co content. The magnetic entropy change (ΔSM) was estimated from isothermal magnetization curves and it increases from 3.35 J/Kg K for x = 0 to 5.83 J/Kg K for x = 2 at μ0 H = 1.6 T . The relative cooling power (RCP) is in the range of 11.6 J/kg (x = 0) and 16 J/kg (x = 2).

Philip A. Parilla | NREL

Science.gov Websites

atomic layer deposition for applications. He also manages the majority of X-ray characterization equipment at NREL, specifically X-ray diffraction and X-ray fluorescence instrumentation. Additionally, he for EERE's Hydrogen Storage program. He is also an expert in X-ray diffraction and X-ray fluorescence

Correlation between structural and transport properties of electron beam irradiated PrMnO3 compounds

NASA Astrophysics Data System (ADS)

Christopher, Benedict; Rao, Ashok; Nagaraja, B. S.; Shyam Prasad, K.; Okram, G. S.; Sanjeev, Ganesh; Petwal, Vikash Chandra; Verma, Vijay Pal; Dwivedi, Jishnu; Poornesh, P.

2018-02-01

The structural, electrical, magnetic, and thermal properties of electron beam (EB) irradiated PrMnO3 manganites were investigated in the present communication. X-ray diffraction data reveals that all samples are single phased with orthorhombic distorted structure (Pbnm). Furthermore, the diffracted data are analyzed in detail using Rietveld refinement technique. It is observed that the EB dosage feebly disturbs the MnO6 octahedra. The electrical resistivity of all the samples exhibits semiconducting behavior. Small polaron hopping model is conveniently employed to investigate the semiconducting nature of the pristine as well as EB irradiated samples. The Seebeck coefficient (S) of the pristine as well as the irradiated samples exhibit large positive values at lower temperatures, signifying holes as the dominant charge carriers. The analysis of Seebeck coefficient data confirms that the small polaron hopping mechanism assists the thermoelectric transport property in the high temperature region. The magnetic measurements confirm the existence of paramagnetic (PM) to ferromagnetic (FM) behavior for the pristine and irradiated samples. In the lower temperature regime, coexistence of FM clusters and AFM matrix is dominating. Thus, the complex magnetic behavior of the compound has been explained in terms of rearrangement of antiferromagnetically coupled ionic moments.

Contents and occurrence of cadmium in the coals from Guizhou province, China.

PubMed

Song, Dangyu; Wang, Mingshi; Zhang, Junying; Zheng, Chuguang

2008-10-01

Eleven raw coal samples were collected from Liuzhi, Suicheng, Zunyi, Xingren, Xingyi, and Anlong districts in Guizhou Province, Southwest China. The content of cadmium (Cd) in coal was determined using inductively coupled plasma mass-spectrometry (ICP-MS). Cd contents ranged from 0.146 to 2.74 ppm (whole coal basis), with an average of 1.09 ppm. In comparison with the arithmetic means of Cd in Chinese coal (0.25 ppm), this is much higher. In order to find its occurrence in coal, float-sink analysis and a coal flotation test by progressive release were conducted on two raw coal samples. The content of the Cd and ash yield of the flotation products were determined. The organic matter was removed by low-temperature ashing (LTA). X-ray diffraction (XRD) was used to differentiate the main, minor, and trace minerals in the LTA from different flotation subproducts. Quartz, kaolinite, pyrite, and calcite were found to dominate the mineral matters, with a proportion of anatase, muscovite, and illite. Then quantitative analysis of minerals in LTA was conducted using material analysis using diffraction (MAUD) based on the Rietveld refinement method. Results show that Cd has a strong association with kaolinite.

Electrical analysis of inter-growth structured Bi4Ti3O12-Na0.5Bi4.5Ti4O15 ceramics

NASA Astrophysics Data System (ADS)

Jiang, Xiangping; Jiang, Yalin; Jiang, Xingan; Chen, Chao; Tu, Na; Chen, Yunjing

2017-06-01

Inter-growth bismuth layer-structured ferroelectrics (BLSFs), Bi4Ti3O12-Na0.5Bi4.5Ti4O15 (BIT-NBT), were successfully synthesized using the traditional solid-state reaction method. X-ray diffraction (XRD) Rietveld refinements were conducted using GSAS software. Good agreement and low residual are obtained. The XRD diffraction peaks can be well indexed into I2cm space group. The inter-growth structure was further observed in the high-resolution TEM image. Dielectric and impedance properties were measured and systematically analyzed. At the temperature range 763-923 K (below {T}{{c}}), doubly ionized oxygen vacancies (OVs) are localized and the short-range hopping leads to the relaxation processes with an activation energy of 0.79-1.01 eV. Above {T}{{c}}, the doubly charged OVs are delocalized and become free ones, which contribute to the long-range dc conduction. The reduction in relaxation species gives rise to a higher relaxation activation energy ˜1.6  eV. Project supported by the National Natural Science Foundation of China (Grant Nos. 51562014, 51262009, and 51602135).

Phase progression of γ-Al2O3 nanoparticles synthesized in a solvent-deficient environment.

PubMed

Smith, Stacey J; Amin, Samrat; Woodfield, Brian F; Boerio-Goates, Juliana; Campbell, Branton J

2013-04-15

Our simple and uniquely cost-effective solvent-deficient synthetic method produces 3-5 nm Al2O3 nanoparticles which show promise as improved industrial catalyst-supports. While catalytic applications are sensitive to the details of the atomic structure, a diffraction analysis of alumina nanoparticles is challenging because of extreme size/microstrain-related peak broadening and the similarity of the diffraction patterns of various transitional Al2O3 phases. Here, we employ a combination of X-ray pair-distribution function (PDF) and Rietveld methods, together with solid-state NMR and thermogravimetry/differential thermal analysis-mass spectrometry (TG/DTA-MS), to characterize the alumina phase-progression in our nanoparticles as a function of calcination temperature between 300 and 1200 °C. In the solvent-deficient synthetic environment, a boehmite precursor phase forms which transitions to γ-Al2O3 at an extraordinarily low temperature (below 300 °C), but this γ-Al2O3 is initially riddled with boehmite-like stacking-fault defects that steadily disappear during calcination in the range from 300 to 950 °C. The healing of these defects accounts for many of the most interesting and widely reported properties of the γ-phase.

Simulations of X-ray diffraction of shock-compressed single-crystal tantalum with synchrotron undulator sources.

PubMed

Tang, M X; Zhang, Y Y; E, J C; Luo, S N

2018-05-01

Polychromatic synchrotron undulator X-ray sources are useful for ultrafast single-crystal diffraction under shock compression. Here, simulations of X-ray diffraction of shock-compressed single-crystal tantalum with realistic undulator sources are reported, based on large-scale molecular dynamics simulations. Purely elastic deformation, elastic-plastic two-wave structure, and severe plastic deformation under different impact velocities are explored, as well as an edge release case. Transmission-mode diffraction simulations consider crystallographic orientation, loading direction, incident beam direction, X-ray spectrum bandwidth and realistic detector size. Diffraction patterns and reciprocal space nodes are obtained from atomic configurations for different loading (elastic and plastic) and detection conditions, and interpretation of the diffraction patterns is discussed.

Simulations of X-ray diffraction of shock-compressed single-crystal tantalum with synchrotron undulator sources

DOE Office of Scientific and Technical Information (OSTI.GOV)

Tang, M. X.; Zhang, Y. Y.; E, J. C.

Polychromatic synchrotron undulator X-ray sources are useful for ultrafast single-crystal diffraction under shock compression. Here, simulations of X-ray diffraction of shock-compressed single-crystal tantalum with realistic undulator sources are reported, based on large-scale molecular dynamics simulations. Purely elastic deformation, elastic–plastic two-wave structure, and severe plastic deformation under different impact velocities are explored, as well as an edge release case. Transmission-mode diffraction simulations consider crystallographic orientation, loading direction, incident beam direction, X-ray spectrum bandwidth and realistic detector size. Diffraction patterns and reciprocal space nodes are obtained from atomic configurations for different loading (elastic and plastic) and detection conditions, and interpretation of themore » diffraction patterns is discussed.« less

The CheMin XRD on the Mars Science Laboratory Rover Curiosity: Construction, Operation, and Quantitative Mineralogical Results from the Surface of Mars

NASA Technical Reports Server (NTRS)

Blake, David F.

2015-01-01

The Mars Science Laboratory mission was launched from Cape Canaveral, Florida on Nov. 26, 2011 and landed in Gale crater, Mars on Aug. 6, 2012. MSL's mission is to identify and characterize ancient "habitable" environments on Mars. MSL's precision landing system placed the Curiosity rover within 2 km of the center of its 20 X 6 km landing ellipse, next to Gale's central mound, a 5,000 meter high pile of laminated sediment which may contain 1 billion years of Mars history. Curiosity carries with it a full suite of analytical instruments, including the CheMin X-ray diffractometer, the first XRD flown in space. CheMin is essentially a transmission X-ray pinhole camera. A fine-focus Co source and collimator transmits a 50µm beam through a powdered sample held between X-ray transparent plastic windows. The sample holder is shaken by a piezoelectric actuator such that the powder flows like a liquid, each grain passing in random orientation through the beam over time. Forward-diffracted and fluoresced X-ray photons from the sample are detected by an X-ray sensitive Charge Coupled Device (CCD) operated in single photon counting mode. When operated in this way, both the x,y position and the energy of each photon are detected. The resulting energy-selected Co Kalpha Debye-Scherrer pattern is used to determine the identities and amounts of minerals present via Rietveld refinement, and a histogram of all X-ray events constitutes an X-ray fluorescence analysis of the sample.The key role that definitive mineralogy plays in understanding the Martian surface is a consequence of the fact that minerals are thermodynamic phases, having known and specific ranges of temperature, pressure and composition within which they are stable. More than simple compositional analysis, definitive mineralogical analysis can provide information about pressure/temperature conditions of formation, past climate, water activity and the like. Definitive mineralogical analyses are necessary to establish the origin or provenance of a sample. The search for evidence of extant or extinct life on Mars will initially be a search for evidence of present or past conditions supportive of life (e.g., evidence of water), not for life itself.Results of the first 1,000 sols (Mars days) will be discussed, including the discovery of the first habitable environment on Mars.

Coherent X-ray diffraction imaging of nanoengineered polymeric capsules

NASA Astrophysics Data System (ADS)

Erokhina, S.; Pastorino, L.; Di Lisa, D.; Kiiamov, A. G.; Faizullina, A. R.; Tayurskii, D. A.; Iannotta, S.; Erokhin, V.

2017-10-01

For the first time, nanoengineered polymeric capsules and their architecture have been studied with coherent X-ray diffraction imaging technique. The use of coherent X-ray diffraction imaging technique allowed us to analyze the samples immersed in a liquid. We report about the significant difference between polymeric capsule architectures under dry and liquid conditions.

A high-transparency, micro-patternable chip for X-ray diffraction analysis of microcrystals under native growth conditions

DOE Office of Scientific and Technical Information (OSTI.GOV)

Murray, Thomas D.; Johns Hopkins University School of Medicine, Baltimore, MD 21205; Lyubimov, Artem Y.

A highly X-ray-transparent, silicon nitride-based device has been designed and fabricated to harvest protein microcrystals for high-resolution X-ray diffraction data collection using microfocus beamlines and XFELs. Microcrystals present a significant impediment to the determination of macromolecular structures by X-ray diffraction methods. Although microfocus synchrotron beamlines and X-ray free-electron lasers (XFELs) can enable the collection of interpretable diffraction data from microcrystals, there is a need for efficient methods of harvesting small volumes (<2 µl) of microcrystals grown under common laboratory formats and delivering them to an X-ray beam source under native growth conditions. One approach that shows promise in overcoming themore » challenges intrinsic to microcrystal analysis is to pair so-called ‘fixed-target’ sample-delivery devices with microbeam-based X-ray diffraction methods. However, to record weak diffraction patterns it is necessary to fabricate devices from X-ray-transparent materials that minimize background scattering. Presented here is the design of a new micro-diffraction device consisting of three layers fabricated from silicon nitride, photoresist and polyimide film. The chip features low X-ray scattering and X-ray absorption properties, and uses a customizable blend of hydrophobic and hydrophilic surface patterns to help localize microcrystals to defined regions. Microcrystals in their native growth conditions can be loaded into the chips with a standard pipette, allowing data collection at room temperature. Diffraction data collected from hen egg-white lysozyme microcrystals (10–15 µm) loaded into the chips yielded a complete, high-resolution (<1.6 Å) data set sufficient to determine a high-quality structure by molecular replacement. The features of the chip allow the rapid and user-friendly analysis of microcrystals grown under virtually any laboratory format at microfocus synchrotron beamlines and XFELs.« less

Synthesis and optical properties of Pr and Ti doped BiFeO{sub 3} ceramics

DOE Office of Scientific and Technical Information (OSTI.GOV)

Singh, Vikash, E-mail: vikash.singh@abes.ac.in; Applied Science and Humanities, ABES EC, Ghaziabad; Sharma, Subhash

2016-05-23

Bi{sub 1-x}Pr{sub x}Fe{sub 1-x}Ti{sub x}O{sub 3} ceramics with x = 0.00, 0.10 and 0.20 were synthesized by solid state reaction method. Rietveld fitting of diffraction data reveals structural transition from rhombohedral phase (R{sub 3C}) for x ≤ 0.10 to orthorhombic phase (P{sub nma}) for x = 0.20. FTIR spectra exhibit broad absorption bands, which may be due to the overlapping of Fe-O and Bi-O vibrations in these ceramics. UV-visible spectroscopy results show strong absorption of light in the spectral range of 400-600 nm, indicating optical band gap in the visible region for these samples.

Effects of Al(3+) doping on the structure and properties of goethite and its adsorption behavior towards phosphate.

PubMed

Li, Wei; Wang, Longjun; Liu, Fan; Liang, Xiaoliang; Feng, Xionghan; Tan, Wenfeng; Zheng, Lirong; Yin, Hui

2016-07-01

Al substitution in goethite is common in soils, and has strong influence on the structure and physicochemical properties of goethite. In this research, a series of Al-doped goethites were synthesized, and characterized by powder X-ray diffraction (XRD), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), Fourier transform infrared spectroscopy (FT-IR) and extended X-ray absorption fine structure (EXAFS) spectroscopy. The adsorption behavior of these samples towards PO4(3-) was also investigated. Characterization results demonstrated that increasing Al content in goethite led to a reduction in crystallinity, increase in specific surface area (SSA), and morphology change from needle-like to granular. Rietveld structure refinement revealed that the lattice parameter a remained almost constant and b slightly decreased, but c was significantly reduced, and the calculated crystal density increased. EXAFS analysis demonstrated that the Fe(Al)-O distance in the structure of the doped goethites was almost the same, but the Fe-Fe(Al) distance decreased with increasing Al content. Surface analysis showed that, with increasing Al content, the content of OH groups on the mineral surface increased. The adsorption of phosphate per unit mass of Al-doped goethite increased, while adsorption per unit area decreased owing to the decrease of the relative proportion of (110) facets in the total surface area of the minerals. The results of this research facilitate better understanding of the effect of Al substitution on the structure and properties of goethite and the cycling of phosphate in the environment. Copyright © 2016. Published by Elsevier B.V.

X-Ray Structure determination of the Glycine Cleavage System Protein H of Mycobacterium tuberculosis Using An Inverse Compton Synchrotron X-Ray Source

PubMed Central

Abendroth, Jan; McCormick, Michael S.; Edwards, Thomas E.; Staker, Bart; Loewen, Roderick; Gifford, Martin; Rifkin, Jeff; Mayer, Chad; Guo, Wenjin; Zhang, Yang; Myler, Peter; Kelley, Angela; Analau, Erwin; Hewitt, Stephen Nakazawa; Napuli, Alberto J.; Kuhn, Peter; Ruth, Ronald D.; Stewart, Lance J.

2010-01-01

Structural genomics discovery projects require ready access to both X-ray and NMR instrumentation which support the collection of experimental data needed to solve large numbers of novel protein structures. The most productive X-ray crystal structure determination laboratories make extensive frequent use of tunable synchrotron X-ray light to solve novel structures by anomalous diffraction methods. This requires that frozen cryo-protected crystals be shipped to large government-run synchrotron facilities for data collection. In an effort to eliminate the need to ship crystals for data collection, we have developed the first laboratory-scale synchrotron light source capable of performing many of the state-of-the-art synchrotron applications in X-ray science. This Compact Light Source is a first-in-class device that uses inverse Compton scattering to generate X-rays of sufficient flux, tunable wavelength and beam size to allow high-resolution X-ray diffraction data collection from protein crystals. We report on benchmarking tests of X-ray diffraction data collection with hen egg white lysozyme, and the successful high-resolution X-ray structure determination of the Glycine cleavage system protein H from Mycobacterium tuberculosis using diffraction data collected with the Compact Light Source X-ray beam. PMID:20364333

Anti-contamination device for cryogenic soft X-ray diffraction microscopy

DOE PAGES

Huang, Xiaojing; Miao, Huijie; Nelson, Johanna; ...

2011-05-01

Cryogenic microscopy allows one to view frozen hydrated biological and soft matter specimens with good structural preservation and a high degree of stability against radiation damage. We describe a liquid nitrogen-cooled anti-contamination device for cryogenic X-ray diffraction microscopy. The anti-contaminator greatly reduces the buildup of ice layers on the specimen due to condensation of residual water vapor in the experimental vacuum chamber. We show by coherent X-ray diffraction measurements that this leads to fivefold reduction of background scattering, which is important for far-field X-ray diffraction microscopy of biological specimens.

Observation of electromigration in a Cu thin line by in situ coherent x-ray diffraction microscopy

NASA Astrophysics Data System (ADS)

Takahashi, Yukio; Nishino, Yoshinori; Furukawa, Hayato; Kubo, Hideto; Yamauchi, Kazuto; Ishikawa, Tetsuya; Matsubara, Eiichiro

2009-06-01

Electromigration (EM) in a 1-μm-thick Cu thin line was investigated by in situ coherent x-ray diffraction microscopy (CXDM). Characteristic x-ray speckle patterns due to both EM-induced voids and thermal deformation in the thin line were observed in the coherent x-ray diffraction patterns. Both parts of the voids and the deformation were successfully visualized in the images reconstructed from the diffraction patterns. This result not only represents the first demonstration of the visualization of structural changes in metallic materials by in situ CXDM but is also an important step toward studying the structural dynamics of nanomaterials using x-ray free-electron lasers in the near future.

Note: application of a pixel-array area detector to simultaneous single crystal X-ray diffraction and X-ray absorption spectroscopy measurements.

PubMed

Sun, Cheng-Jun; Zhang, Bangmin; Brewe, Dale L; Chen, Jing-Sheng; Chow, G M; Venkatesan, T; Heald, Steve M

2014-04-01

X-ray diffraction (XRD) and X-ray absorption spectroscopy (XAS) are two main x-ray techniques in synchrotron radiation facilities. In this Note, we present an experimental setup capable of performing simultaneous XRD and XAS measurements by the application of a pixel-array area detector. For XRD, the momentum transfer in specular diffraction was measured by scanning the X-ray energy with fixed incoming and outgoing x-ray angles. By selecting a small fixed region of the detector to collect the XRD signal, the rest of the area was available for collecting the x-ray fluorescence for XAS measurements. The simultaneous measurement of XRD and X-ray absorption near edge structure for Pr0.67Sr0.33MnO3 film was demonstrated as a proof of principle for future time-resolved pump-probe measurements. A static sample makes it easy to maintain an accurate overlap of the X-ray spot and laser pump beam.

X-Ray Diffraction Wafer Mapping Method for Rhombohedral Super-Hetero-Epitaxy

NASA Technical Reports Server (NTRS)

Park, Yoonjoon; Choi, Sang Hyouk; King, Glen C.; Elliott, James R.; Dimarcantonio, Albert L.

2010-01-01

A new X-ray diffraction (XRD) method is provided to acquire XY mapping of the distribution of single crystals, poly-crystals, and twin defects across an entire wafer of rhombohedral super-hetero-epitaxial semiconductor material. In one embodiment, the method is performed with a point or line X-ray source with an X-ray incidence angle approximating a normal angle close to 90 deg, and in which the beam mask is preferably replaced with a crossed slit. While the wafer moves in the X and Y direction, a narrowly defined X-ray source illuminates the sample and the diffracted X-ray beam is monitored by the detector at a predefined angle. Preferably, the untilted, asymmetric scans are of {440} peaks, for twin defect characterization.

Diffraction based method to reconstruct the spectrum of the Thomson scattering x-ray source

NASA Astrophysics Data System (ADS)

Chi, Zhijun; Yan, Lixin; Zhang, Zhen; Zhou, Zheng; Zheng, Lianmin; Wang, Dong; Tian, Qili; Wang, Wei; Nie, Zan; Zhang, Jie; Du, Yingchao; Hua, Jianfei; Shi, Jiaru; Pai, Chihao; Lu, Wei; Huang, Wenhui; Chen, Huaibi; Tang, Chuanxiang

2017-04-01

As Thomson scattering x-ray sources based on the collision of intense laser and relativistic electrons have drawn much attention in various scientific fields, there is an increasing demand for the effective methods to reconstruct the spectrum information of the ultra-short and high-intensity x-ray pulses. In this paper, a precise spectrum measurement method for the Thomson scattering x-ray sources was proposed with the diffraction of a Highly Oriented Pyrolytic Graphite (HOPG) crystal and was demonstrated at the Tsinghua Thomson scattering X-ray source. The x-ray pulse is diffracted by a 15 mm (L) ×15 mm (H)× 1 mm (D) HOPG crystal with 1° mosaic spread. By analyzing the diffraction pattern, both x-ray peak energies and energy spectral bandwidths at different polar angles can be reconstructed, which agree well with the theoretical value and simulation. The higher integral reflectivity of the HOPG crystal makes this method possible for single-shot measurement.

Diffraction based method to reconstruct the spectrum of the Thomson scattering x-ray source.

PubMed

Chi, Zhijun; Yan, Lixin; Zhang, Zhen; Zhou, Zheng; Zheng, Lianmin; Wang, Dong; Tian, Qili; Wang, Wei; Nie, Zan; Zhang, Jie; Du, Yingchao; Hua, Jianfei; Shi, Jiaru; Pai, Chihao; Lu, Wei; Huang, Wenhui; Chen, Huaibi; Tang, Chuanxiang

2017-04-01

As Thomson scattering x-ray sources based on the collision of intense laser and relativistic electrons have drawn much attention in various scientific fields, there is an increasing demand for the effective methods to reconstruct the spectrum information of the ultra-short and high-intensity x-ray pulses. In this paper, a precise spectrum measurement method for the Thomson scattering x-ray sources was proposed with the diffraction of a Highly Oriented Pyrolytic Graphite (HOPG) crystal and was demonstrated at the Tsinghua Thomson scattering X-ray source. The x-ray pulse is diffracted by a 15 mm (L) ×15 mm (H)× 1 mm (D) HOPG crystal with 1° mosaic spread. By analyzing the diffraction pattern, both x-ray peak energies and energy spectral bandwidths at different polar angles can be reconstructed, which agree well with the theoretical value and simulation. The higher integral reflectivity of the HOPG crystal makes this method possible for single-shot measurement.

Gas gun shock experiments with single-pulse x-ray phase contrast imaging and diffraction at the Advanced Photon Source

NASA Astrophysics Data System (ADS)

Luo, S. N.; Jensen, B. J.; Hooks, D. E.; Fezzaa, K.; Ramos, K. J.; Yeager, J. D.; Kwiatkowski, K.; Shimada, T.

2012-07-01

The highly transient nature of shock loading and pronounced microstructure effects on dynamic materials response call for in situ, temporally and spatially resolved, x-ray-based diagnostics. Third-generation synchrotron x-ray sources are advantageous for x-ray phase contrast imaging (PCI) and diffraction under dynamic loading, due to their high photon fluxes, high coherency, and high pulse repetition rates. The feasibility of bulk-scale gas gun shock experiments with dynamic x-ray PCI and diffraction measurements was investigated at the beamline 32ID-B of the Advanced Photon Source. The x-ray beam characteristics, experimental setup, x-ray diagnostics, and static and dynamic test results are described. We demonstrate ultrafast, multiframe, single-pulse PCI measurements with unprecedented temporal (<100 ps) and spatial (˜2 μm) resolutions for bulk-scale shock experiments, as well as single-pulse dynamic Laue diffraction. The results not only substantiate the potential of synchrotron-based experiments for addressing a variety of shock physics problems, but also allow us to identify the technical challenges related to image detection, x-ray source, and dynamic loading.

X-ray and neutron diffraction studies of crystallinity in hydroxyapatite coatings.

PubMed

Girardin, E; Millet, P; Lodini, A

2000-02-01

To standardize industrial implant production and make comparisons between different experimental results, we have to be able to quantify the crystallinity of hydroxyapatite. Methods of measuring crystallinity ratio were developed for various HA samples before and after plasma spraying. The first series of methods uses X-ray diffraction. The advantage of these methods is that X-ray diffraction equipment is used widely in science and industry. In the second series, a neutron diffraction method is developed and the results recorded are similar to those obtained by the modified X-ray diffraction methods. The advantage of neutron diffraction is the ability to obtain measurements deep inside a component. It is a nondestructive method, owing to the very low absorption of neutrons in most materials. Copyright 2000 John Wiley & Sons, Inc.

X-ray Diffraction Gratings for Astrophysics

NASA Astrophysics Data System (ADS)

Paerels, Frits

2010-12-01

Over the past year, we have celebrated the tenth anniversary of the Chandra and XMM-Newton X-ray observatories. Both carry powerful, novel diffraction grating spectrometers, which have opened true X-ray spectroscopy for astrophysics. I will describe the design and operation of these instruments, as the background to some of the beautiful results they have produced. But these designs do not exhaust the versatility and essential simplicity of diffraction grating spectrometers, and I will discuss applications for the International X-ray Observatory IXO.

Structural, microstructural and vibrational analyses of the monoclinic tungstate BiLuWO{sub 6}

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ait Ahsaine, H.; Taoufyq, A.; Institut Matériaux Microélectronique et Nanosciences de Provence, IM2NP, UMR CNRS 7334, Université de Toulon, BP 20132, 83957 La Garde Cedex

2014-10-15

The bismuth lutetium tungstate phase BiLuWO{sub 6} has been prepared using a solid state route with stoichiometric mixtures of oxide precursors. The obtained polycrystalline phase has been characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and Raman spectroscopy. In the first step, the crystal structure has been refined using Rietveld method: the crystal cell was resolved using monoclinic system (parameters a, b, c, β) with space group A2/m. SEM images showed the presence of large crystallites with a constant local nominal composition (BiLuW). TEM analyses showed that the actual local structure could be better representedmore » by a superlattice (a, 2b, c, β) associated with space groups P2 or P2/m. The Raman spectroscopy showed the presence of vibrational bands similar to those observed in the compounds BiREWO{sub 6} with RE=Y, Gd, Nd. However, these vibrational bands were characterized by large full width at half maximum, probably resulting from the long range Bi/Lu disorder and local WO{sub 6} octahedron distortions in the structure. - Graphical abstract: The average structure of BiLuWO{sub 6} determined from X-ray diffraction data can be represented by A2/m space group. Experimental Electron Diffraction patterns along the [0vw] zone axes of the monoclinic structure and associated simulated patterns show the existence of a monoclinic superstructure with space group P2 or P2/m. - Highlights: • A new monoclinic BiLuWO{sub 6} phase has been elaborated from solid-state reaction. • The space group of the monoclinic disordered average structure should be A2/m. • Transmission electron microscopy leads to a superlattice with P2/m space group. • Raman spectroscopy suggests existence of local disorder.« less

Lattice strain induced multiferroicity in PZT-CFO particulate composite

NASA Astrophysics Data System (ADS)

Pradhan, Lagen Kumar; Pandey, Rabichandra; Kumar, Rajnish; Kar, Manoranjan

2018-02-01

Lead Zirconate Titanate [Pb(Zr0.52Ti0.48)O3/PZT] and Cobalt Ferrite [CoFe2O4/CFO] based multiferroic composites [(1-x)PZT-(x)CFO] with (x = 0.10-0.40) have been prepared to study its magnetoelectric (ME) and multiferroic properties. X-ray diffraction method along with the Rietveld refinement technique reveals that the crystal symmetries corresponding to PZT and CFO exist independently in the composites. The effect of interfacial strain on lattice distortion in PZT has been observed. It is well correlated with the magnetoelectric coupling of the composites. Dispersion behavior of dielectric constant with frequency can be explained by the modified Debye model. Different relaxation phenomena have been observed in PZT-CFO particulate composites. The ferroelectric properties of composites decrease with the increase in percentage of CFO in the composite. Both saturation (Ms) and remanent (Mr) magnetization increase with the increase in CFO content in the composite. The maximum ME coupling was found to be 1.339 pC/cm2 Oe for the composition (0.80) PZT-(0.20) CFO at the application of maximum magnetic field of 50 Oe. The multiferroic properties in CFO-PZT can be explained by the lattice strain at the CFO-PZT interfaces.

Amorphous boron gasket in diamond anvil cell research

NASA Astrophysics Data System (ADS)

Lin, Jung-Fu; Shu, Jinfu; Mao, Ho-kwang; Hemley, Russell J.; Shen, Guoyin

2003-11-01

Recent advances in high-pressure diamond anvil cell experiments include high-energy synchrotron x-ray techniques as well as new cell designs and gasketing procedures. The success of high-pressure experiments usually depends on a well-prepared sample, in which the gasket plays an important role. Various gasket materials such as diamond, beryllium, rhenium, and stainless steel have been used. Here we introduce amorphous boron as another gasket material in high-pressure diamond anvil cell experiments. We have applied the boron gasket for laser-heating x-ray diffraction, radial x-ray diffraction, nuclear resonant inelastic x-ray scattering, and inelastic x-ray scattering. The high shear strength of the amorphous boron maximizes the thickness of the sample chamber and increases the pressure homogeneity, improving the quality of high-pressure data. Use of amorphous boron avoids unwanted x-ray diffraction peaks and reduces the absorption of incident and x rays exiting the gasket material. The high quality of the diffraction patterns makes it possible to refine the cell parameters with powder x-ray diffraction data under high pressure and high temperature. The reactivity of boron prevents its use at high temperatures, however. When heated, boron may also react with the specimen to produce unwanted phases. The relatively porous boron starting material at ambient conditions also poses some challenges for sample preparation.

X-Ray Sum Frequency Diffraction for Direct Imaging of Ultrafast Electron Dynamics

NASA Astrophysics Data System (ADS)

Rouxel, Jérémy R.; Kowalewski, Markus; Bennett, Kochise; Mukamel, Shaul

2018-06-01

X-ray diffraction from molecules in the ground state produces an image of their charge density, and time-resolved x-ray diffraction can thus monitor the motion of the nuclei. However, the density change of excited valence electrons upon optical excitation can barely be monitored with regular diffraction techniques due to the overwhelming background contribution of the core electrons. We present a nonlinear x-ray technique made possible by novel free electron laser sources, which provides a spatial electron density image of valence electron excitations. The technique, sum frequency generation carried out with a visible pump and a broadband x-ray diffraction pulse, yields snapshots of the transition charge densities, which represent the electron density variations upon optical excitation. The technique is illustrated by ab initio simulations of transition charge density imaging for the optically induced electronic dynamics in a donor or acceptor substituted stilbene.

Addressing the amorphous content issue in quantitative phase analysis: the certification of NIST standard reference material 676a.

PubMed

Cline, James P; Von Dreele, Robert B; Winburn, Ryan; Stephens, Peter W; Filliben, James J

2011-07-01

A non-diffracting surface layer exists at any boundary of a crystal and can comprise a mass fraction of several percent in a finely divided solid. This has led to the long-standing issue of amorphous content in standards for quantitative phase analysis (QPA). NIST standard reference material (SRM) 676a is a corundum (α-Al(2)O(3)) powder, certified with respect to phase purity for use as an internal standard in powder diffraction QPA. The amorphous content of SRM 676a is determined by comparing diffraction data from mixtures with samples of silicon powders that were engineered to vary their specific surface area. Under the (supported) assumption that the thickness of an amorphous surface layer on Si was invariant, this provided a method to control the crystalline/amorphous ratio of the silicon components of 50/50 weight mixtures of SRM 676a with silicon. Powder diffraction experiments utilizing neutron time-of-flight and 25 keV and 67 keV X-ray energies quantified the crystalline phase fractions from a series of specimens. Results from Rietveld analyses, which included a model for extinction effects in the silicon, of these data were extrapolated to the limit of zero amorphous content of the Si powder. The certified phase purity of SRM 676a is 99.02% ± 1.11% (95% confidence interval). This novel certification method permits quantification of amorphous content for any sample of interest, by spiking with SRM 676a.

High energy X-ray diffraction study of a dental ceramics–titanium functional gradient material prepared by field assisted sintering technique

DOE Office of Scientific and Technical Information (OSTI.GOV)

Witte, K., E-mail: kerstin.witte@uni-rostock.de; Bodnar, W.; Schell, N.

A functional gradient material with eleven layers composed of a dental ceramics and titanium was successfully consolidated using field assisted sintering technique in a two-step sintering process. High energy X-ray diffraction studies on the gradient were performed at High Energy Material Science beamline at Desy in Hamburg. Phase composition, crystal unit edges and lattice mismatch along the gradient were determined applying Rietveld refinement procedure. Phase analysis revealed that the main crystalline phase present in the gradient is α-Ti. Crystallinity increases stepwisely along the gradient with a decreasing increment between every next layer, following rather the weight fraction of titanium. Themore » crystal unit edge a of titanium remains approximately constant with a value of 2.9686(1) Å, while c is reduced with increasing amount of titanium. In the layer with pure titanium the crystal unit edge c is constant with a value of 4.7174(2) Å. The lattice mismatch leading to an internal stress was calculated over the whole gradient. It was found that the maximal internal stress in titanium embedded in the studied gradient is significantly smaller than its yield strength, which implies that the structure of titanium along the whole gradient is mechanically stable. - Highlights: • High energy XRD studies of dental ceramics–Ti gradient material consolidated by FAST. • Phase composition, crystallinity and lattice parameters are determined. • Crystallinity increases stepwisely along the gradient following weight fraction of Ti. • Lattice mismatch leading to internal stress is calculated over the whole gradient. • Internal stress in α-Ti embedded in the gradient is smaller than its yield strength.« less

Synthesis and ab initioStructure Determination from Powder X-Ray Diffraction Data of a New Metallic Mixed-Valence Platinum-Lead Oxide PbPt 2O 4

NASA Astrophysics Data System (ADS)

Tancret, N.; Obbade, S.; Bettahar, N.; Abraham, F.

1996-07-01

The mixed-valence PbPt2O4compound was synthesized both by solid state reaction between stoichiometric amounts of PbO and Pt heated at 650-750°C for 1 week and by chemical attack of Pb2PtO4. It decomposes to PbO and Pt at 750°C. The crystal structure was completely solved from direct methods and difference Fourier maps from powder X-ray diffraction data. The unit cell is triclinic (space groupP1,Z= 2) witha= 6.1161(2) Å,b= 6.6504(2) Å,c= 5.5502(2) Å, α = 97.178(2)°, β = 108.803(2)°, and γ = 115.241(2)°. The structural model was refined using the Rietveld profile technique and led to the reliability factorsRwp= 0.118,Rp= 0.086,RBragg= 0.029,RF= 0.018, and χ2= 1.51. The structure of PbPt2O4appears to be a unique one involving both Pt4+in octahedral coordination and Pt2+or partially oxidized platinum in square-planar coordination. The PbPt2O4structure consists of columnar-stacked PtO4groups extending along thecaxis of the unit cell. These columnar stacks are held by other planar PtO4groups to constitute Pt3O8sheets. These sheets are linked together by PtO6octahedra to form a three-dimensional framework. Lead atoms are surrounded by six oxygens forming a distorted octahedron. Metallic conductivity in PbPt2O4is consistent with short Pt-Pt bonds in the columnar stacks of PtO4groups along thecaxis direction (dPt-Pt= 2.78 Å).

Development of an adaptable coherent x-ray diffraction microscope with the emphasis on imaging hydrated specimens.

PubMed

Nam, Daewoong; Park, Jaehyun; Gallagher-Jones, Marcus; Shimada, Hiroki; Kim, Sangsoo; Kim, Sunam; Kohmura, Yoshiki; Ishikawa, Tetsuya; Song, Changyong

2013-11-01

This paper describes the development of a versatile coherent x-ray diffraction microscope capable of imaging biological specimens in solution. The microscope is a flexible platform accommodating various conditions, from low vacuum (10(-2) Pa) to helium gas filled ambient pressure. This flexibility greatly expands the application area, from in situ materials science to biology systems in their native state, by significantly relaxing restrictions to the sample environment. The coherent diffraction microscope has been used successfully to image a yeast cell immersed in buffer solution. We believe that the design of this coherent diffraction microscope can be directly adapted to various platforms such as table top soft x-ray laser, synchrotron x-ray sources, and x-ray free electron laser with minor relevant adjustments.

Development of an adaptable coherent x-ray diffraction microscope with the emphasis on imaging hydrated specimens

NASA Astrophysics Data System (ADS)

Nam, Daewoong; Park, Jaehyun; Gallagher-Jones, Marcus; Shimada, Hiroki; Kim, Sangsoo; Kim, Sunam; Kohmura, Yoshiki; Ishikawa, Tetsuya; Song, Changyong

2013-11-01

This paper describes the development of a versatile coherent x-ray diffraction microscope capable of imaging biological specimens in solution. The microscope is a flexible platform accommodating various conditions, from low vacuum (10-2 Pa) to helium gas filled ambient pressure. This flexibility greatly expands the application area, from in situ materials science to biology systems in their native state, by significantly relaxing restrictions to the sample environment. The coherent diffraction microscope has been used successfully to image a yeast cell immersed in buffer solution. We believe that the design of this coherent diffraction microscope can be directly adapted to various platforms such as table top soft x-ray laser, synchrotron x-ray sources, and x-ray free electron laser with minor relevant adjustments.

Thin Film Research. Volume 1

DTIC Science & Technology

1985-05-30

Order (FECO) ......... 23 3. X -Ray Diffraction ............................... 26 4. Transmission Electron Microscopy (TEM) ............... 26 5...remained amorphous after bombardment, as evidenced by X - ray diffraction, and showed no other changes. 0 (2) For Sb203, the crystallite size was reduced...main effect on MgF2 was the reduction in crystallite size. The films were too thir. for meaningful x - ray diffraction analysis. Durability and

X-Ray Diffraction and the Discovery of the Structure of DNA

ERIC Educational Resources Information Center

Crouse, David T.

2007-01-01

A method is described for teaching the analysis of X-ray diffraction of DNA through a series of steps utilizing the original methods used by James Watson, Francis Crick, Maurice Wilkins and Rosalind Franklin. The X-ray diffraction pattern led to the conclusion of the basic helical structure of DNA and its dimensions while basic chemical principles…

High Resolution X-Ray Diffraction of Macromolecules with Synchrotron Radiation

NASA Technical Reports Server (NTRS)

Stojanoff, Vivian; Boggon, Titus; Helliwell, John R.; Judge, Russell; Olczak, Alex; Snell, Edward H.; Siddons, D. Peter; Rose, M. Franklin (Technical Monitor)

2000-01-01

We recently combined synchrotron-based monochromatic X-ray diffraction topography methods with triple axis diffractometry and rocking curve measurements: high resolution X-ray diffraction imaging techniques, to better understand the quality of protein crystals. We discuss these methods in the light of results obtained on crystals grown under different conditions. These non destructive techniques are powerful tools in the characterization of the protein crystals and ultimately will allow to improve, develop, and understand protein crystal growth. High resolution X-ray diffraction imaging methods will be discussed in detail in light of recent results obtained on Hen Egg White Lysozyme crystals and other proteins.

Hard X-ray polarizer to enable simultaneous three-dimensional nanoscale imaging of magnetic structure and lattice strain

DOE PAGES

Logan, Jonathan; Harder, Ross; Li, Luxi; ...

2016-01-01

Recent progress in the development of dichroic Bragg coherent diffractive imaging, a new technique for simultaneous three-dimensional imaging of strain and magnetization at the nanoscale, is reported. This progress includes the installation of a diamond X-ray phase retarder at beamline 34-ID-C of the Advanced Photon Source. Here, the performance of the phase retarder for tuning X-ray polarization is demonstrated with temperature-dependent X-ray magnetic circular dichroism measurements on a gadolinium foil in transmission and on a Gd 5Si 2Ge 2crystal in diffraction geometry with a partially coherent, focused X-ray beam. Feasibility tests for dichroic Bragg coherent diffractive imaging are presented. Thesemore » tests include (1) using conventional Bragg coherent diffractive imaging to determine whether the phase retarder introduces aberrations using a nonmagnetic gold nanocrystal as a control sample, and (2) collecting coherent diffraction patterns of a magnetic Gd 5Si 2Ge 2nanocrystal with left- and right-circularly polarized X-rays. Future applications of dichroic Bragg coherent diffractive imaging for the correlation of strain and lattice defects with magnetic ordering and inhomogeneities are considered.« less

Anomalous magnetic and spin glass behavior in Nb-substituted LaCo1 -xNbxO3

NASA Astrophysics Data System (ADS)

Shukla, Rishabh; Dhaka, R. S.

2018-01-01

We report the structural, magnetic, transport, and electronic properties of Nb-substituted LaCo1 -xNbxO3 (x =0 -0.2 ). The Rietveld refinement of x-ray diffraction data demonstrate structural phase transitions from rhombohedral to orthorhombic and further to monoclinic with increasing the Nb concentration up to x ≥0.2 . Interestingly, we observed dramatic changes in the magnetization (M ) with increasing the Nb concentration, as the M sharply increases below 10 K even at 2.5% substitution. Furthermore, ac susceptibility data show the spin glass behavior in x =0.1 sample. We find that the density of states near the Fermi level decreases and the activation energy increases, which results in the decreasing conductivity with higher Nb concentration. A significant shift in the peak position of A2 g phonon mode has been observed using Raman spectroscopy, which indicates the change in the coupling due to the structural distortion with Nb substitution. The core-level photoemission study confirms that the Nb is present in 5 + valence state. Our study reveals that the nonmagnetic Nb5 + (d0) substitution converts Co3 + ions to Co2 + and stabilizes both in the high-spin state. Our results suggest that structural and spin-state transitions as well as the difference in the ionic radii between Nb5 + and Co3 + are playing an important role in tuning the physical properties.

The importance of proper crystal-chemical and geometrical reasoning demonstrated using layered single and double hydroxides

PubMed Central

Richardson, Ian G.

2013-01-01

Atomistic modelling techniques and Rietveld refinement of X-ray powder diffraction data are widely used but often result in crystal structures that are not realistic, presumably because the authors neglect to check the crystal-chemical plausibility of their structure. The purpose of this paper is to reinforce the importance and utility of proper crystal-chemical and geometrical reasoning in structural studies. It is achieved by using such reasoning to generate new yet fundamental information about layered double hydroxides (LDH), a large, much-studied family of compounds. LDH phases are derived from layered single hydroxides by the substitution of a fraction (x) of the divalent cations by trivalent. Equations are derived that enable calculation of x from the a parameter of the unit cell and vice versa, which can be expected to be of widespread utility as a sanity test for extant and future structure determinations and computer simulation studies. The phase at x = 0 is shown to be an α form of divalent metal hydroxide rather than the β polymorph. Crystal-chemically sensible model structures are provided for β-Zn(OH)2 and Ni- and Mg-based carbonate LDH phases that have any trivalent cation and any value of x, including x = 0 [i.e. for α-M(OH)2·mH2O phases]. PMID:23719702

Domain wall and interphase boundary motion in (1−x)Bi(Mg{sub 0.5}Ti{sub 0.5})O{sub 3}–xPbTiO{sub 3} near the morphotropic phase boundary

DOE Office of Scientific and Technical Information (OSTI.GOV)

Tutuncu, Goknur; Chen, Jun; Fan, Longlong

Electric field-induced changes in the domain wall motion of (1−x)Bi(Mg{sub 0.5}Ti{sub 0.5})O{sub 3}–xPbTiO{sub 3} (BMT-xPT) near the morphotropic phase boundary (MPB) where x = 0.37 (BMT-37PT) and x = 0.38 (BMT-38PT), are studied by means of synchrotron x-ray diffraction. Through Rietveld analysis and profile fitting, a mixture of coexisting monoclinic (Cm) and tetragonal (P4mm) phases is identified at room temperature. Extrinsic contributions to the property coefficients are evident from electric-field-induced domain wall motion in both the tetragonal and monoclinic phases, as well as through the interphase boundary motion between the two phases. Domain wall motion in the tetragonal and monoclinic phases for BMT-37PT ismore » larger than that of BMT-38PT, possibly due to this composition's closer proximity to the MPB. Increased interphase boundary motion was also observed in BMT-37PT. Lattice strain, which is a function of both intrinsic piezoelectric strain and elastic interactions of the grains (the latter originating from domain wall and interphase boundary motion), is similar for the respective tetragonal and monoclinic phases.« less

Mg doped Li2FeSiO4/C nanocomposites synthesized by the solvothermal method for lithium ion batteries.

PubMed

Kumar, Ajay; Jayakumar, O D; Jagannath; Bashiri, Parisa; Nazri, G A; Naik, Vaman M; Naik, Ratna

2017-10-14

A series of porous Li 2 Fe 1-x Mg x SiO 4 /C (x = 0, 0.01, 0.02, 0.04) nanocomposites (LFS/C, 1Mg-LFS/C, 2Mg-LFS and 4Mg-LFS/C) have been synthesized via a solvo-thermal method using the Pluronic P123 polymer as an in situ carbon source. Rietveld refinement of the X-ray diffraction data of Li 2 Fe 1-x Mg x SiO 4 /C composites confirms the formation of the monoclinic P2 1 structure of Li 2 FeSiO 4 . The addition of Mg facilitates the growth of impurity-free Li 2 FeSiO 4 with increased crystallinity and particle size. Despite having the same percentage of carbon content (∼15 wt%) in all the samples, the 1Mg-LFS/C nanocomposite delivered the highest initial discharge capacity of 278 mA h g -1 (∼84% of the theoretical capacity) at the C/30 rate and also exhibited the best rate capability and cycle stability (94% retention after 100 charge-discharge cycles at 1C). This is attributed to its large surface area with a narrow pore size distribution and a lower charge transfer resistance with enhanced Li-ion diffusion coefficient compared to other nanocomposites.

Three Dimensional Variable-Wavelength X-Ray Bragg Coherent Diffraction Imaging

DOE PAGES

Cha, W.; Ulvestad, A.; Allain, M.; ...

2016-11-23

Here, we present and demonstrate a formalism by which three-dimensional (3D) Bragg x-ray coherent diffraction imaging (BCDI) can be implemented without moving the sample by scanning the energy of the incident x-ray beam. This capability is made possible by introducing a 3D Fourier transform that accounts for x-ray wavelength variability. We also demonstrate the approach by inverting coherent Bragg diffraction patterns from a gold nanocrystal measured with an x-ray energy scan. Furthermore, variable-wavelength BCDI will expand the breadth of feasible in situ 3D strain imaging experiments towards more diverse materials environments, especially where sample manipulation is difficult.

Synchrotron X-Ray Diffraction Analysis of Meteorites in Thin Section: Preliminary Results

NASA Technical Reports Server (NTRS)

Treiman, A. H.; Lanzirotti, A.; Xirouchakis, D.

2004-01-01

X-ray diffraction is the pre-eminent technique for mineral identification and structure determination, but is difficult to apply to grains in thin section, the standard meteorite preparation. Bright focused X-ray beams from synchrotrons have been used extensively in mineralogy and have been applied to extraterrestrial particles. The intensity and small spot size achievable in synchrotron X-ray beams makes them useful for study of materials in thin sections. Here, we describe Synchrotron X-ray Diffraction (SXRD) in thin section as done at the National Synchrotron Light Source, and cite examples of its value for studies of meteorites in thin section.

Three Dimensional Variable-Wavelength X-Ray Bragg Coherent Diffraction Imaging

NASA Astrophysics Data System (ADS)

Cha, W.; Ulvestad, A.; Allain, M.; Chamard, V.; Harder, R.; Leake, S. J.; Maser, J.; Fuoss, P. H.; Hruszkewycz, S. O.

2016-11-01

We present and demonstrate a formalism by which three-dimensional (3D) Bragg x-ray coherent diffraction imaging (BCDI) can be implemented without moving the sample by scanning the energy of the incident x-ray beam. This capability is made possible by introducing a 3D Fourier transform that accounts for x-ray wavelength variability. We demonstrate the approach by inverting coherent Bragg diffraction patterns from a gold nanocrystal measured with an x-ray energy scan. Variable-wavelength BCDI will expand the breadth of feasible in situ 3D strain imaging experiments towards more diverse materials environments, especially where sample manipulation is difficult.

Three Dimensional Variable-Wavelength X-Ray Bragg Coherent Diffraction Imaging.

PubMed

Cha, W; Ulvestad, A; Allain, M; Chamard, V; Harder, R; Leake, S J; Maser, J; Fuoss, P H; Hruszkewycz, S O

2016-11-25

We present and demonstrate a formalism by which three-dimensional (3D) Bragg x-ray coherent diffraction imaging (BCDI) can be implemented without moving the sample by scanning the energy of the incident x-ray beam. This capability is made possible by introducing a 3D Fourier transform that accounts for x-ray wavelength variability. We demonstrate the approach by inverting coherent Bragg diffraction patterns from a gold nanocrystal measured with an x-ray energy scan. Variable-wavelength BCDI will expand the breadth of feasible in situ 3D strain imaging experiments towards more diverse materials environments, especially where sample manipulation is difficult.

In-situ X-ray diffraction system using sources and detectors at fixed angular positions

DOEpatents

Gibson, David M [Voorheesville, NY; Gibson, Walter M [Voorheesville, NY; Huang, Huapeng [Latham, NY

2007-06-26

An x-ray diffraction technique for measuring a known characteristic of a sample of a material in an in-situ state. The technique includes using an x-ray source for emitting substantially divergent x-ray radiation--with a collimating optic disposed with respect to the fixed source for producing a substantially parallel beam of x-ray radiation by receiving and redirecting the divergent paths of the divergent x-ray radiation. A first x-ray detector collects radiation diffracted from the sample; wherein the source and detector are fixed, during operation thereof, in position relative to each other and in at least one dimension relative to the sample according to a-priori knowledge about the known characteristic of the sample. A second x-ray detector may be fixed relative to the first x-ray detector according to the a-priori knowledge about the known characteristic of the sample, especially in a phase monitoring embodiment of the present invention.

The effect of exit beam phase aberrations on parallel beam coherent x-ray reconstructions

NASA Astrophysics Data System (ADS)

Hruszkewycz, S. O.; Harder, R.; Xiao, X.; Fuoss, P. H.

2010-12-01

Diffraction artifacts from imperfect x-ray windows near the sample are an important consideration in the design of coherent x-ray diffraction measurements. In this study, we used simulated and experimental diffraction patterns in two and three dimensions to explore the effect of phase imperfections in a beryllium window (such as a void or inclusion) on the convergence behavior of phasing algorithms and on the ultimate reconstruction. A predictive relationship between beam wavelength, sample size, and window position was derived to explain the dependence of reconstruction quality on beryllium defect size. Defects corresponding to this prediction cause the most damage to the sample exit wave and induce signature error oscillations during phasing that can be used as a fingerprint of experimental x-ray window artifacts. The relationship between x-ray window imperfection size and coherent x-ray diffractive imaging reconstruction quality explored in this work can play an important role in designing high-resolution in situ coherent imaging instrumentation and will help interpret the phasing behavior of coherent diffraction measured in these in situ environments.

The effect of exit beam phase aberrations on parallel beam coherent x-ray reconstructions.

PubMed

Hruszkewycz, S O; Harder, R; Xiao, X; Fuoss, P H

2010-12-01

Diffraction artifacts from imperfect x-ray windows near the sample are an important consideration in the design of coherent x-ray diffraction measurements. In this study, we used simulated and experimental diffraction patterns in two and three dimensions to explore the effect of phase imperfections in a beryllium window (such as a void or inclusion) on the convergence behavior of phasing algorithms and on the ultimate reconstruction. A predictive relationship between beam wavelength, sample size, and window position was derived to explain the dependence of reconstruction quality on beryllium defect size. Defects corresponding to this prediction cause the most damage to the sample exit wave and induce signature error oscillations during phasing that can be used as a fingerprint of experimental x-ray window artifacts. The relationship between x-ray window imperfection size and coherent x-ray diffractive imaging reconstruction quality explored in this work can play an important role in designing high-resolution in situ coherent imaging instrumentation and will help interpret the phasing behavior of coherent diffraction measured in these in situ environments.

Calcium aluminates hydration in presence of amorphous SiO{sub 2} at temperatures below 90 deg. C

DOE Office of Scientific and Technical Information (OSTI.GOV)

Rivas Mercury, J.M.; Turrillas, X.; Aza, A.H. de

2006-10-15

The hydration behaviour of Ca{sub 3}Al{sub 2}O{sub 6}, Ca{sub 12}Al{sub 14}O{sub 33} and CaAl{sub 2}O{sub 4} with added amorphous silica at 40, 65 and 90 deg. C has been studied for periods ranging from 1 to 31 days. In hydrated samples crystalline phases like katoite (Ca{sub 3}Al{sub 2}(SiO{sub 4}){sub 3-} {sub x} (OH){sub 4} {sub x} ) and gibbsite, Al(OH){sub 3}, were identified, likewise amorphous phases like Al(OH) {sub x} , calcium silicate hydrates, C-S-H, and calcium aluminosilicate hydrates, C-S-A-H, were identified. The stoichiometry of Ca{sub 3}Al{sub 2}(SiO{sub 4}){sub 3-} {sub x} (OH){sub 4} {sub x} (0{<=}3-x{<=}0.334), which was themore » main crystalline product, was established by Rietveld refinement of X-ray and neutron diffraction data and by transmission electron microscopy. - Graphical abstract: Katoite, Ca{sub 3}Al{sub 2}(SiO{sub 4}){sub 3-} {sub x} (OH){sub 4} {sub x} (0{<=}3-x{<=}0.334), was identified besides gibbsite, Al(OH){sub 3}, as a crystalline stable hydration products in Ca{sub 3}Al{sub 2}O{sub 6}, Ca{sub 12}Al{sub 14}O{sub 33} and CaAl{sub 2}O{sub 4} hydrated with added amorphous silica between 40 and 90 deg. C.« less

Femtosecond X-ray Diffraction From Two-Dimensional Protein Crystals

DOE Office of Scientific and Technical Information (OSTI.GOV)

Frank, Matthias; Carlson, David B.; Hunter, Mark

2014-02-28

Here we present femtosecond x-ray diffraction patterns from two-dimensional (2-D) protein crystals using an x-ray free electron laser (XFEL). To date it has not been possible to acquire x-ray diffraction from individual 2-D protein crystals due to radiation damage. However, the intense and ultrafast pulses generated by an XFEL permits a new method of collecting diffraction data before the sample is destroyed. Utilizing a diffract-before-destroy methodology at the Linac Coherent Light Source, we observed Bragg diffraction to better than 8.5 Å resolution for two different 2-D protein crystal samples that were maintained at room temperature. These proof-of-principle results show promisemore » for structural analysis of both soluble and membrane proteins arranged as 2-D crystals without requiring cryogenic conditions or the formation of three-dimensional crystals.« less

Influence of gamma ray irradiation on stoichiometry of hydrothermally synthesized bismuth telluride nanoparticles

NASA Astrophysics Data System (ADS)

Abishek, N. S.; Naik, K. Gopalakrishna

2018-05-01

Bismuth telluride (Bi2Te3) nanoparticles were synthesized by the hydrothermal method at 200 °C for 24 h. The synthesized Bi2Te3 nanoparticles were irradiated with gamma rays at doses of 50 kGy and 100 kGy. The structural characterization of the pre-irradiated and post-irradiated samples was carried out by X-ray diffraction technique and was found to have rhombohedral phase having R3 ¯m (166) space group. The X-ray diffraction peaks were found to shift towards lower diffraction angle with gamma ray irradiation. The morphologies and compositions of the grown Bi2Te3 nanoparticles were studied using Field Emission Scanning Electron Microscope and X-ray energy dispersive analysis, respectively. The possible cause for the shift in the X-ray diffraction peaks with gamma ray irradiation has been discussed in the present work.

High Power Optical Coatings by Atomic Layer Deposition and Signatures of Laser-Induced Damage

DTIC Science & Technology

2012-08-28

diffraction angle 0 into crystal lattice spacing d by the Bragg condition, mX = 2d sin 0. Here X is the x - ray wavelength... angle x - ray diffraction (GAXRD) measurements, which were made at a fixed shallow incidence angle of 0.5°. Detector scans were done to measure the...was finished with 200 hafnia cycles m the fmal half period rather than 400. Crystallinity was measured by x - ray diffraction (XRD) with

Materials identification using a small-scale pixellated x-ray diffraction system

NASA Astrophysics Data System (ADS)

O'Flynn, D.; Crews, C.; Drakos, I.; Christodoulou, C.; Wilson, M. D.; Veale, M. C.; Seller, P.; Speller, R. D.

2016-05-01

A transmission x-ray diffraction system has been developed using a pixellated, energy-resolving detector (HEXITEC) and a small-scale, mains operated x-ray source (Amptek Mini-X). HEXITEC enables diffraction to be measured without the requirement of incident spectrum filtration, or collimation of the scatter from the sample, preserving a large proportion of the useful signal compared with other diffraction techniques. Due to this efficiency, sufficient molecular information for material identification can be obtained within 5 s despite the relatively low x-ray source power. Diffraction data are presented from caffeine, hexamine, paracetamol, plastic explosives and narcotics. The capability to determine molecular information from aspirin tablets inside their packaging is demonstrated. Material selectivity and the potential for a sample classification model is shown with principal component analysis, through which each different material can be clearly resolved.

Dynamic X-ray diffraction sampling for protein crystal positioning

DOE Office of Scientific and Technical Information (OSTI.GOV)

Scarborough, Nicole M.; Godaliyadda, G. M. Dilshan P.; Ye, Dong Hye

A sparse supervised learning approach for dynamic sampling (SLADS) is described for dose reduction in diffraction-based protein crystal positioning. Crystal centering is typically a prerequisite for macromolecular diffraction at synchrotron facilities, with X-ray diffraction mapping growing in popularity as a mechanism for localization. In X-ray raster scanning, diffraction is used to identify the crystal positions based on the detection of Bragg-like peaks in the scattering patterns; however, this additional X-ray exposure may result in detectable damage to the crystal prior to data collection. Dynamic sampling, in which preceding measurements inform the next most information-rich location to probe for image reconstruction,more » significantly reduced the X-ray dose experienced by protein crystals during positioning by diffraction raster scanning. The SLADS algorithm implemented herein is designed for single-pixel measurements and can select a new location to measure. In each step of SLADS, the algorithm selects the pixel, which, when measured, maximizes the expected reduction in distortion given previous measurements. Ground-truth diffraction data were obtained for a 5 µm-diameter beam and SLADS reconstructed the image sampling 31% of the total volume and only 9% of the interior of the crystal greatly reducing the X-ray dosage on the crystal. Furthermore, by usingin situtwo-photon-excited fluorescence microscopy measurements as a surrogate for diffraction imaging with a 1 µm-diameter beam, the SLADS algorithm enabled image reconstruction from a 7% sampling of the total volume and 12% sampling of the interior of the crystal. When implemented into the beamline at Argonne National Laboratory, without ground-truth images, an acceptable reconstruction was obtained with 3% of the image sampled and approximately 5% of the crystal. The incorporation of SLADS into X-ray diffraction acquisitions has the potential to significantly minimize the impact of X-ray exposure on the crystal by limiting the dose and area exposed for image reconstruction and crystal positioning using data collection hardware present in most macromolecular crystallography end-stations.« less

Dynamic X-ray diffraction sampling for protein crystal positioning

DOE PAGES

Scarborough, Nicole M.; Godaliyadda, G. M. Dilshan P.; Ye, Dong Hye; ...

2017-01-01

A sparse supervised learning approach for dynamic sampling (SLADS) is described for dose reduction in diffraction-based protein crystal positioning. Crystal centering is typically a prerequisite for macromolecular diffraction at synchrotron facilities, with X-ray diffraction mapping growing in popularity as a mechanism for localization. In X-ray raster scanning, diffraction is used to identify the crystal positions based on the detection of Bragg-like peaks in the scattering patterns; however, this additional X-ray exposure may result in detectable damage to the crystal prior to data collection. Dynamic sampling, in which preceding measurements inform the next most information-rich location to probe for image reconstruction,more » significantly reduced the X-ray dose experienced by protein crystals during positioning by diffraction raster scanning. The SLADS algorithm implemented herein is designed for single-pixel measurements and can select a new location to measure. In each step of SLADS, the algorithm selects the pixel, which, when measured, maximizes the expected reduction in distortion given previous measurements. Ground-truth diffraction data were obtained for a 5 µm-diameter beam and SLADS reconstructed the image sampling 31% of the total volume and only 9% of the interior of the crystal greatly reducing the X-ray dosage on the crystal. Furthermore, by usingin situtwo-photon-excited fluorescence microscopy measurements as a surrogate for diffraction imaging with a 1 µm-diameter beam, the SLADS algorithm enabled image reconstruction from a 7% sampling of the total volume and 12% sampling of the interior of the crystal. When implemented into the beamline at Argonne National Laboratory, without ground-truth images, an acceptable reconstruction was obtained with 3% of the image sampled and approximately 5% of the crystal. The incorporation of SLADS into X-ray diffraction acquisitions has the potential to significantly minimize the impact of X-ray exposure on the crystal by limiting the dose and area exposed for image reconstruction and crystal positioning using data collection hardware present in most macromolecular crystallography end-stations.« less

Dynamic X-ray diffraction sampling for protein crystal positioning

PubMed Central

Scarborough, Nicole M.; Godaliyadda, G. M. Dilshan P.; Ye, Dong Hye; Kissick, David J.; Zhang, Shijie; Newman, Justin A.; Sheedlo, Michael J.; Chowdhury, Azhad U.; Fischetti, Robert F.; Das, Chittaranjan; Buzzard, Gregery T.; Bouman, Charles A.; Simpson, Garth J.

2017-01-01

A sparse supervised learning approach for dynamic sampling (SLADS) is described for dose reduction in diffraction-based protein crystal positioning. Crystal centering is typically a prerequisite for macromolecular diffraction at synchrotron facilities, with X-ray diffraction mapping growing in popularity as a mechanism for localization. In X-ray raster scanning, diffraction is used to identify the crystal positions based on the detection of Bragg-like peaks in the scattering patterns; however, this additional X-ray exposure may result in detectable damage to the crystal prior to data collection. Dynamic sampling, in which preceding measurements inform the next most information-rich location to probe for image reconstruction, significantly reduced the X-ray dose experienced by protein crystals during positioning by diffraction raster scanning. The SLADS algorithm implemented herein is designed for single-pixel measurements and can select a new location to measure. In each step of SLADS, the algorithm selects the pixel, which, when measured, maximizes the expected reduction in distortion given previous measurements. Ground-truth diffraction data were obtained for a 5 µm-diameter beam and SLADS reconstructed the image sampling 31% of the total volume and only 9% of the interior of the crystal greatly reducing the X-ray dosage on the crystal. Using in situ two-photon-excited fluorescence microscopy measurements as a surrogate for diffraction imaging with a 1 µm-diameter beam, the SLADS algorithm enabled image reconstruction from a 7% sampling of the total volume and 12% sampling of the interior of the crystal. When implemented into the beamline at Argonne National Laboratory, without ground-truth images, an acceptable reconstruction was obtained with 3% of the image sampled and approximately 5% of the crystal. The incorporation of SLADS into X-ray diffraction acquisitions has the potential to significantly minimize the impact of X-ray exposure on the crystal by limiting the dose and area exposed for image reconstruction and crystal positioning using data collection hardware present in most macromolecular crystallography end-stations. PMID:28009558

Dynamic X-ray diffraction sampling for protein crystal positioning.

PubMed

Scarborough, Nicole M; Godaliyadda, G M Dilshan P; Ye, Dong Hye; Kissick, David J; Zhang, Shijie; Newman, Justin A; Sheedlo, Michael J; Chowdhury, Azhad U; Fischetti, Robert F; Das, Chittaranjan; Buzzard, Gregery T; Bouman, Charles A; Simpson, Garth J

2017-01-01

A sparse supervised learning approach for dynamic sampling (SLADS) is described for dose reduction in diffraction-based protein crystal positioning. Crystal centering is typically a prerequisite for macromolecular diffraction at synchrotron facilities, with X-ray diffraction mapping growing in popularity as a mechanism for localization. In X-ray raster scanning, diffraction is used to identify the crystal positions based on the detection of Bragg-like peaks in the scattering patterns; however, this additional X-ray exposure may result in detectable damage to the crystal prior to data collection. Dynamic sampling, in which preceding measurements inform the next most information-rich location to probe for image reconstruction, significantly reduced the X-ray dose experienced by protein crystals during positioning by diffraction raster scanning. The SLADS algorithm implemented herein is designed for single-pixel measurements and can select a new location to measure. In each step of SLADS, the algorithm selects the pixel, which, when measured, maximizes the expected reduction in distortion given previous measurements. Ground-truth diffraction data were obtained for a 5 µm-diameter beam and SLADS reconstructed the image sampling 31% of the total volume and only 9% of the interior of the crystal greatly reducing the X-ray dosage on the crystal. Using in situ two-photon-excited fluorescence microscopy measurements as a surrogate for diffraction imaging with a 1 µm-diameter beam, the SLADS algorithm enabled image reconstruction from a 7% sampling of the total volume and 12% sampling of the interior of the crystal. When implemented into the beamline at Argonne National Laboratory, without ground-truth images, an acceptable reconstruction was obtained with 3% of the image sampled and approximately 5% of the crystal. The incorporation of SLADS into X-ray diffraction acquisitions has the potential to significantly minimize the impact of X-ray exposure on the crystal by limiting the dose and area exposed for image reconstruction and crystal positioning using data collection hardware present in most macromolecular crystallography end-stations.

Fixture for supporting and aligning a sample to be analyzed in an x-ray diffraction apparatus

DOEpatents

Green, L.A.; Heck, J.L. Jr.

1985-04-23

A fixture is provided for supporting and aligning small samples of material on a goniometer for x-ray diffraction analysis. A sample-containing capillary is accurately positioned for rotation in the x-ray beam by selectively adjusting the fixture to position the capillary relative to the x and y axes thereof to prevent wobble and position the sample along the z axis or the axis of rotation. By employing the subject fixture relatively small samples of materials can be analyzed in an x-ray diffraction apparatus previously limited to the analysis of much larger samples.

Fixture for supporting and aligning a sample to be analyzed in an X-ray diffraction apparatus

DOEpatents

Green, Lanny A.; Heck, Jr., Joaquim L.

1987-01-01

A fixture is provided for supporting and aligning small samples of material on a goniometer for X-ray diffraction analysis. A sample-containing capillary is accurately positioned for rotation in the X-ray beam by selectively adjusting the fixture to position the capillary relative to the x and y axes thereof to prevent wobble and position the sample along the z axis or the axis of rotation. By employing the subject fixture relatively small samples of materials can be analyzed in an X-ray diffraction apparatus previously limited to the analysis of much larger samples.

JMFA2—a graphically interactive Java program that fits microfibril angle X-ray diffraction data

Treesearch

Steve P. Verrill; David E. Kretschmann; Victoria L. Herian

2006-01-01

X-ray diffraction techniques have the potential to decrease the time required to determine microfibril angles dramatically. In this paper, we discuss the latest version of a curve-fitting toll that permits us to reduce the time required to evaluate MFA X-ray diffraction patterns. Further, because this tool reflects the underlying physics more accurately than existing...

Rietveld refinement, electronic structure and ionic conductivity of Sr{sub 4}La{sub 6}(SiO{sub 4}){sub 6}F{sub 2} and Sr{sub 4}La{sub 6}(SiO{sub 4}){sub 6}O ceramics

DOE Office of Scientific and Technical Information (OSTI.GOV)

Boughzala, Khaled, E-mail: khaledboughzala@gmail.com; Preparatory Institute for Engineering Studies, 5000 Monastir; Debbichi, Mourad

In this paper, we report the effect of the tunnel anions on the ionic conductivity of Strontium-Lanthanum silicate apatites. The Sr{sub 4}La{sub 6}(SiO{sub 4}){sub 6}F{sub 2} and Sr{sub 4}La{sub 6}(SiO{sub 4}){sub 6}O ceramics were prepared by the solid state reaction method. X-ray diffraction, NMR spectroscopy and Raman measurements were performed to investigate the crystal structure and vibrational active modes. Moreover, the electronic structures of the crystals were evaluated by the first-principles quantum mechanical calculation based on the density functional theory. Finally, the ionic conductivity was studied according to the complex impedance method. - Graphical abstract: The relaxed primitive unit cellmore » for Sr{sub 4}La{sub 6}Fap. Display Omitted.« less

Synthesis and Structure of A New Perovskite, SrCuO 2.5

NASA Astrophysics Data System (ADS)

Chen, Bai-Hao; Walker, Dave; Scott, Bruce A.; Mitzi, David B.

1996-02-01

A new oxygen-deficient perovskite, SrCuO2.5, was prepared at 950°C and 100 kbar pressure in a multianvil apparatus. Rietveld profile analysis, using X-ray powder diffraction data, was employed for the structural determination. SrCuO2.5is orthorhombic,Pbam(No. 55),Z= 4,a= 5.424(2) Â,b= 10.837(4) Â, andc= 3.731(1) Â, which is related to the perovskite subcell by root{2}ap× 2root{2}ap×ap, whereapis the simple cubic perovskite lattice parameter. It consists of corner-shared CuO5square pyramids with oxygen vacancy ordering in the CuO2layers. The ordered oxygen vacancies create parallel pseudo-hexagonal tunnels where the Sr atoms reside, forming SrO10polyhedra. Structural features with respect to oxygen vacancies, superstructures, and distortions are analogous to the type of ordering observed in Sr2CuO3+δ. Superconductivity was not observed in SrCuO2.5down to 5 K.

Rattling induced superconductivity in RV2Al20 (R = Sc, Lu, Y) aluminides - an experimental and theoretical study

NASA Astrophysics Data System (ADS)

Winiarski, Michal; Wiendlocha, Bartlomiej; Sternik, Malgorzata; Wisniewski, Piotr; Kaczorowski, Dariusz; Klimczuk, Tomasz

Polycrystalline samples of four ternary intermetallics RV2Al20 (R = Sc, Y, La, and Lu) were synthesized. Structural studies carried out using powder x-ray diffraction and Rietveld analysis show that all compounds crystallize in CeCr2Al20-type structure composed of icosahedral Al-R cages. Results of physical properties measurements reveal that ScV2Al20, YV2Al20, and LuV2Al20 are weakly-coupled BCS superconductors with critical temperatures Tc = 1.0, 0.57, and 0.60 K, respectively. Electronic and phonon structure calculations reveal the key role of low-frequency anharmonic vibrations of R atoms (rattling effect) for the appearance of superconductivity. A correlation between phonon and crystal structures was observed, allowing to search for new RV2Al20 superconductors. Project was financially supported by the National Science Centre (Poland) Grant (DEC-2012/07/E/ST3/00584).

Study of structural, electrical, magnetic and optical properties of BaFe12O19 and its modified systems with Ni and Ti

NASA Astrophysics Data System (ADS)

Nayak, Debabrata; Pattanayak, Ranjit; Raut, Subhajit; Panigrahi, Simanchalo

2018-02-01

In this work, BaFe12O19 (BaM) and its modified systems (by substitution of Ni and Ti) have been synthesized by solid-state reaction method. From Rietveld refinement of X-ray diffraction pattern, it is found that volume of unit cell increased slightly in case of modified systems. SEM images provided the information about the microstructure of BaM and its modified systems. The electric, magnetic and optical properties have been carried out with the help of complex impedance spectroscopy, VSM and UV spectrum, respectively. From electrical analysis, it is perceived that Ni-substitution system has shown co-contribution of grain and grain boundary effect due to increases of grain size. The M- H loops are explored that, with substitution of Ni and Ti both M s and H c are decreased. From the variation of band gap ( E g), it is observed that E g has been significantly decreased with substitution (least for Ni-substitution).

Structural transformation study of TiO2 nanoparticles annealing at different temperatures and the photodegradation process of eosin-Y

NASA Astrophysics Data System (ADS)

Pandi, P.; Gopinathan, C.

2018-04-01

Hydrothermal method was used to prepare TiO2 nanoparticles with annealing temperature at 500 °C-700 °C. The mixture of anatase-rutile phase was investigated by powerful tool of X-ray diffraction (XRD). The structural parameters of anatase and rutile mixture phaseTiO2 nanoparticles were calculated from the Rietveld refinement. The transformation rate of rutile was increased linearly with an annealing temperature of 500 °C-700 °C. The spherical morphology of the anatase and rutile mixed phase were obtained by scanning electron microscope and transmission electron microscope. The spherical particle of the anatase and rutile TiO2 shows with great aggregation with different size and within the range of few tens nm. The EDAX study revealed the presence of titanium and oxygen. The best photocatalytic activity was identified as the 87.04% of anatase and 12.96% of rutile mixer phase of TiO2. Various factors could be involved for a better photocatalytic activity.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Deus, R.C.; Cortés, J.A., E-mail: leandrosrr89@gmail.com; Ramirez, M.A.

Highlights: • CeO{sub 2} nanoparticles were obtained by microwave-hydrothermal method. • Rietveld refinement reveals a cubic structure. • KOH mineralizer agent exhibit weak agglomeration at low temperature and shorter time. - Abstract: The structural and photoluminescent properties at room temperature of CeO{sub 2} and La-doped CeO{sub 2} particles were undertaken. The obtained particles were synthesized by a microwave-assisted hydrothermal method (MAH) under different lanthanum contents. X-ray diffraction (XRD), Fourier transform infrared (FT-IR), Fourier transform Raman (FT-Raman), Ultra-violet spectroscopy (UV–vis) and photoluminescence (PL) measurements were carried out. XRD revealed that the powders are free of secondary phases and crystallize in themore » cubic structure. Raman data show that increasing La doping content increase oxygen vacancies due to lattice expansion. The UV/vis absorption spectroscopy suggested the presence of intermediate energy levels in the band gap of structurally ordered powders. Lanthanum addition creates oxygen vacancies and shifts the photoluminescence in the low energy range leading to intense PL emission.« less

A new LiNbO{sub 3}-type polar oxide with closed-shell cations: ZnPbO{sub 3}

DOE Office of Scientific and Technical Information (OSTI.GOV)

Yu, Runze, E-mail: yu.r.aa@m.titech.ac.jp, E-mail: mazuma@msl.titech.ac.jp; Hojo, Hajime; Azuma, Masaki, E-mail: yu.r.aa@m.titech.ac.jp, E-mail: mazuma@msl.titech.ac.jp

2015-09-07

A new lithium-niobate (LiNbO{sub 3})-type polar compound, namely, ZnPbO{sub 3} (a = 5.41605(7) Å and c = 14.33151(3) Å), with closed-shell ions only was synthesized under high pressure and high temperature (8 GPa and 1273 K). A point-charge-model calculation based on atomic positions refined by Rietveld analysis of synchrotron X-ray diffraction data gave an electrical ionic polarization of 77 μC/cm{sup 2} along the hexagonal c-axis. Detailed structural analysis indicated that the contribution of Pb{sup 4+} in ZnPbO{sub 3} to the polarization was almost twice as large as that of Sn{sup 4+} in ZnSnO{sub 3}. Transport measurement showed metallic behavior of ZnPbO{sub 3} from room temperature to lowmore » temperature despite the fact that both cations are closed-shell ions.« less

Quantitative Mineralogical Analysis of Mars Analogues Using CHEMIN Data and Rietveld Refinement

NASA Technical Reports Server (NTRS)

Bish, D. L.; Sarrazin, P.; Chipera, S. J.; Vaniman, D. T.; Blake, D.

2004-01-01

Mineralogical analysis is a critical component of planetary surface exploration. Chemical data alone leave serious gaps in our understanding of the surfaces of planets where complex minerals may form in combination with H, S, and halogens. On such planets (e.g., Mars) a single chemical composition may represent a range of mineral assemblages. For example, Viking chemical analyses of excavated duricrust indicate that Mg and S are correlated and 10% MgSO4 (anhydrous weight) is a likely cementing agent. Pathfinder chemical data support a similar abundance of MgSO4 in the most altered materials. However, there are many possible Mg-sulfates with widely varying hydration states (including dehydrated and 1-, 2-, 3-, 4-, 5-, 6-, and 7-hydrates). In addition, other sulfate minerals such as gypsum (CaSO4 .2H2O) and other salts containing Cl may also exist. X-ray diffraction (XRD) has the ability to decipher mixtures of these phases that would be difficult, if not impossible to unravel using only chemical or spectral data.

Crystallographic, hyperfine and magnetic characterization of a maraging-400 alloy

NASA Astrophysics Data System (ADS)

Alves, T. J. B.; Nunes, G. C. S.; Sarvezuk, P. W. C.; Ivashita, F. F.; de Andrade, A. M. H.; Viegas, A.; Paesano, A.

2017-11-01

Maraging400-like alloys were made by arc-melting iron with the alloy elements (i.e., Ni, Co, Ti and Mo), followed by a high temperature heat-treatment for solubilization. The solubilized alloys were further heat-treated (480 °C and 580 °C, by 3 h), for aging. The samples were finely characterized by X-ray diffraction (Rietveld refinement), Mössbauer spectroscopy and magnetization techniques. The results revealed that the as-solubilized sample is martensitic and ferromagnetic. Its residual induction and coercive field increase monotonically with the maximum applied field of a magnetization minor loop and both curves presented very similar shapes. The area of the minor loops varies parabolically with this maximum applied field. The aging induced an atomic rearrangement in the martensite phase, involving change in the composition and lattice parameters, reversion of austenite and the formation of the Fe 3 Mo 2 intermetallic compound. Comparisons are presented between the results obtained by us for these alloys and those obtained for Maraging-350 steel samples.

Crystal-Chemical Analysis Martian Minerals in Gale Crater

NASA Technical Reports Server (NTRS)

Morrison, S. M.; Downs, R. T.; Blake, D. F.; Bish, D. L.; Ming, D. W.; Morris, R. V.; Yen, A. S.; Chipera, S. J.; Treiman, A. H.; Vaniman, D. T.;

Preparation, crystal structure and enhanced bipolar response of 0.90BLNT-0.10BCT lead-free piezoceramics

DOE Office of Scientific and Technical Information (OSTI.GOV)

Pal, Vijayeta, E-mail: vijayetapal@yahoo.in; Dwivedi, R. K.; Kumar, A.

2016-05-06

In the present work, a solid solution of lead free 0.90[(Bi{sub 0.96}La{sub 0.04}){sub 0.5}Na{sub 0.5}TiO{sub 3}]-0.10(Ba{sub 0.90}Ca{sub 0.10}TiO{sub 3}] (abbreviated as 0.90BLNT-0.10BCT) piezoceramics has been synthesized by semi-wet technique. X-ray diffraction pattern confirms the phase formation. Rietveld refinement of XRD data demonstrates the coexistence of rhombhohedral (R3c) + tetragonal (P4mm) phase at room temperature. Raman spectrum is also support the above analysis. A large enhancement in bipolar strain of 0.12 % and calculated normalized strain, d*{sub 33} (defined as S{sub max}/E{sub max}) ~ 265 pm/V at 40kV/cm has been observed for this composition as compared to pure BLNT specimen, whichmore » make possible it as a potential lead-free candidates for piezoelectric applications.« less

Probing the limit of magnesium uptake by β-tricalcium phosphate in biphasic mixtures formed from calcium deficient apatites

NASA Astrophysics Data System (ADS)

Kumar, P. Nandha; Mishra, Sandeep K.; Kannan, S.

2015-11-01

A series of magnesium doped non-stoichiometric calcium deficient apatites were synthesized through an aqueous precipitation route. The resultant structural changes during heat treatment were investigated by X-ray diffraction, Raman and FT-IR spectroscopy and Rietveld refinement. The results confirmed the formation of biphasic mixtures comprising Ca10(PO4)6(OH)2 and β-Ca3(PO4)2 after heat treatment at 1000 °C with the preferential occupancy of Mg2+ at the crystal lattice of β-Ca3(PO4)2. The concentration of Mg2+ uptake in β-Ca3(PO4)2 is limited till reaching the stoichiometric ratio of (Ca+Mg)/P=1.67 and beyond this stoichiometric value [(Ca+Mg)/P>1.67], Mg2+ precipitates as Mg(OH)2 and thereafter gets converted to MgO during heat treatment. Any kind of Mg2+ uptake in the crystal lattice of Ca10(PO4)6(OH)2 is discarded from the investigation.

Enhancement of thermoelectric figure of merit in β-Zn{sub 4}Sb{sub 3} by indium doping control

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wei, Pai-Chun, E-mail: pcwei68@gmail.com, E-mail: cheny2@phys.sinica.edu.tw; Hsu, Chia-Hao; Chang, Chung-Chieh

2015-09-21

We demonstrate the control of phase composition in Bridgman-grown β-Zn{sub 4}Sb{sub 3} crystals by indium doping, an effective way to overcome the difficulty of growing very pure β-Zn{sub 4}Sb{sub 3} thermoelectric material. The crystal structures are characterized by Rietveld refinement with synchrotron X-ray diffraction data. The results show an anisotropic lattice expansion in In-doped β-Zn{sub 4}Sb{sub 3} wherein the zinc atoms are partially substituted by indium ones at 36f site of R-3c symmetry. Through the elimination of ZnSb phase, all the three individual thermoelectric properties are simultaneously improved, i.e., increasing electrical conductivity and Seebeck coefficient while reducing thermal conductivity. Undermore » an optimal In concentration (x = 0.05), pure phase β-Zn{sub 4}Sb{sub 3} crystal can be obtained, which possesses a high figure of merit (ZT) of 1.4 at 700 K.« less

Temperature dependence of lower critical field of YBCO superconductor

NASA Astrophysics Data System (ADS)

Rani, Poonam; Hafiz, A. K.; Awana, V. P. S.

2018-05-01

We report the detailed study of the temperature dependence of the lower critical field (Hc1) of the YBa2Cu3O7 superconductor by magnetization measurements. The curve shows the multiband gap behavior of the sample. It is found that the sample is not a single BCS type superconductor. Hc1 is measured as the point at which the curve deviates from a Meissner-like linear M(H) curve to a nonlinear path. The Hc1 for YBCO at different temperatures from 10K to 85K has been determined by magnetization measurements M(H) with applied field parallel to the c-axis. The sample phase purity has been confirmed by Rietveld fitted X-ray diffraction data. The amplitude (1-17Oe) dependent AC susceptibility confirms the granular nature of superconducting compound. Using Bean model we calculated the temperature dependency of inter-grain critical current density and Jc(0) is found as 699.14kAcm-2.

A sol-powder coating technique for fabrication of yttria stabilised zirconia

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wattanasiriwech, Darunee; Wattanasiriwech, Suthee; Stevens, Ron

Yttria stabilised zirconia has been prepared using a simple sol-powder coating technique. The polymeric yttria sol, which was prepared using 1,3 propanediol as a network modifier, was homogeneously mixed with nanocrystalline zirconia powder and it showed a dual function: as a binder which promoted densification and a phase modifier which stabilised zirconia in the tetragonal and cubic phases. Thermal analysis and X-ray diffraction revealed that the polymeric yttria sol which decomposed at low temperature into yttrium oxide could change the m {sup {yields}} t phase transformation behaviour of the zirconia, possibly due to the small particle size and very highmore » surface area of both yttria and zirconia particles allowing rapid alloying. The sintered samples exhibited three crystalline phases: monoclinic, tetragonal and cubic, in which cubic and tetragonal are the major phases. The weight fractions of the individual phases present in the selected specimens were determined using quantitative Rietveld analysis.« less

Reciprocal-space and real-space neutron investigation of nanostructured Mo 2C and WC

NASA Astrophysics Data System (ADS)

Page, Katharine; Li, Jun; Savinelli, Robert; Szumila, Holly N.; Zhang, Jinping; Stalick, Judith K.; Proffen, Thomas; Scott, Susannah L.; Seshadri, Ram

2008-11-01

As possible substitute materials for platinum group metal heterogeneous catalysts, high surface area carbides of the early transition metals Mo and W are of great interest. Here we report nanostructured, high surface area Mo 2C and WC prepared by decomposing and carburizing ammonium paramolybdate [(NH 4) 6Mo 7O 24·4H 2O] and ammonium paratungstate [(NH 4) 10W 12O 41·5H 2O] in flowing 50%CH 4/50%H 2. Surface areas as high as 52 m 2/g for Mo 2C and 24 m 2/g for WC were obtained, with both structures crystallizing in structures appropriate for catalytic activity. We have studied these materials using a combination of neutron diffraction Rietveld refinement, X-ray photoelectron spectroscopy, surface area measurements, and scanning transmission electron microscopy. In addition, we have used pair-distribution function (PDF) analysis of the neutron total scattering data as a means of establishing the presence of graphitic carbon in the as-prepared materials.

Hot Corrosion of Yttrium Stabilized Zirconia Coatings Deposited by Air Plasma Spray on a Nickel-Based Superalloy

NASA Astrophysics Data System (ADS)

Vallejo, N. Diaz; Sanchez, O.; Caicedo, J. C.; Aperador, W.; Zambrano, G.

In this research, the electrochemical impedance spectroscopy (EIS) and Tafel analysis were utilized to study the hot corrosion performance at 700∘C of air plasma-sprayed (APS) yttria-stabilized zirconia (YSZ) coatings with a NiCrAlY bond coat grown by high velocity oxygen fuel spraying (HVOF), deposited on an INCONEL 625 substrate, in contact with corrosive solids salts as vanadium pentoxide V2O5 and sodium sulfate Na2SO4. The EIS data were interpreted based on proposed equivalent electrical circuits using a suitable fitting procedure performed with Echem AnalystTM Software. Phase transformations and microstructural development were examined using X-ray diffraction (XRD), with Rietveld refinement for quantitative phase analysis, scanning electron microscopy (SEM) was used to determinate the coating morphology and corrosion products. The XRD analysis indicated that the reaction between sodium vanadate (NaVO3) and yttrium oxide (Y2O3) produces yttrium vanadate (YVO4) and leads to the transformation from tetragonal to monoclinic zirconia phase.

Titanium dioxide nanoparticles: Impact of increasing ionic strength during synthesis, reflux, and hydrothermal aging

DOE Office of Scientific and Technical Information (OSTI.GOV)

Isley, Sara L.; Jordan, David S.; Penn, R. Lee

2009-01-08

This work investigates the role of ionic strength during synthesis, reflux, and hydrothermal aging of sol-gel synthesized titanium dioxide. Research presented here uses X-ray diffraction data and Rietveld refinements to quantify anatase, brookite, and rutile phases as functions of synthetic and aging variables. In addition, the Scherrer equation is used to obtain average crystallite sizes for each phase quantified. Results presented in this work demonstrate that the most control over the sol-gel products can be obtained by modifying the pH during hydrolysis. In addition, while varying the ionic strength during reflux and hydrothermal aging can result in enhanced control overmore » the crystalline phase and crystallite size, the most control can be achieved by varying the ionic strength during synthesis. Finally, sol-gel synthesis at low pH (-0.6) and high-chloride concentration (3 M NaCl) produced a heterogeneous sample composed of nanocrystalline anatase (3.8 nm) and rutile (2.9 nm)« less

Cu3Mo2O9: An Ultralow-Firing Microwave Dielectric Ceramic with Good Temperature Stability and Chemical Compatibility with Aluminum

NASA Astrophysics Data System (ADS)

Wen, Wangxi; Li, Chunchun; Sun, Yihua; Tang, Ying; Fang, Liang

2018-02-01

An ultralow-firing microwave dielectric ceramic Cu3Mo2O9 with orthorhombic structure has been fabricated via a solid-state reaction method. X-ray diffraction analysis, Rietveld refinement, Raman spectroscopy, energy-dispersive spectrometry, and scanning electron microscopy were employed to explore the phase purity, crystal structure, and microstructure. Pure and dense Cu3Mo2O9 ceramics could be obtained in the sintering temperature range from 580°C to 680°C. The sample sintered at 660°C for 4 h exhibited the highest relative density (˜ 97.2%) and best microwave dielectric properties with ɛ r = 7.2, Q × f = 19,300 GHz, and τ f = - 7.8 ppm/°C. Chemical compatibility with aluminum electrodes was also confirmed. All the results suggest that Cu3Mo2O9 ceramic is a promising candidate for use in ultralow-temperature cofired ceramic applications.

A high-transparency, micro-patternable chip for X-ray diffraction analysis of microcrystals under native growth conditions

DOE PAGES

Murray, Thomas D.; Lyubimov, Artem Y.; Ogata, Craig M.; ...

2015-08-11

Microcrystals present a significant impediment to the determination of macromolecular structures by X-ray diffraction methods. Although microfocus synchrotron beamlines and X-ray free-electron lasers (XFELs) can enable the collection of interpretable diffraction data from microcrystals, there is a need for efficient methods of harvesting small volumes (<2 µl) of microcrystals grown under common laboratory formats and delivering them to an X-ray beam source under native growth conditions. One approach that shows promise in overcoming the challenges intrinsic to microcrystal analysis is to pair so-called `fixed-target' sample-delivery devices with microbeam-based X-ray diffraction methods. However, to record weak diffraction patterns it is necessarymore » to fabricate devices from X-ray-transparent materials that minimize background scattering. Presented here is the design of a new micro-diffraction device consisting of three layers fabricated from silicon nitride, photoresist and polyimide film. The chip features low X-ray scattering and X-ray absorption properties, and uses a customizable blend of hydrophobic and hydrophilic surface patterns to help localize microcrystals to defined regions. Microcrystals in their native growth conditions can be loaded into the chips with a standard pipette, allowing data collection at room temperature. Diffraction data collected from hen egg-white lysozyme microcrystals (10–15 µm) loaded into the chips yielded a complete, high-resolution (<1.6 Å) data set sufficient to determine a high-quality structure by molecular replacement. In addition, the features of the chip allow the rapid and user-friendly analysis of microcrystals grown under virtually any laboratory format at microfocus synchrotron beamlines and XFELs.« less

A high-transparency, micro-patternable chip for X-ray diffraction analysis of microcrystals under native growth conditions

DOE Office of Scientific and Technical Information (OSTI.GOV)

Murray, Thomas D.; Lyubimov, Artem Y.; Ogata, Craig M.

Microcrystals present a significant impediment to the determination of macromolecular structures by X-ray diffraction methods. Although microfocus synchrotron beamlines and X-ray free-electron lasers (XFELs) can enable the collection of interpretable diffraction data from microcrystals, there is a need for efficient methods of harvesting small volumes (<2 µl) of microcrystals grown under common laboratory formats and delivering them to an X-ray beam source under native growth conditions. One approach that shows promise in overcoming the challenges intrinsic to microcrystal analysis is to pair so-called `fixed-target' sample-delivery devices with microbeam-based X-ray diffraction methods. However, to record weak diffraction patterns it is necessarymore » to fabricate devices from X-ray-transparent materials that minimize background scattering. Presented here is the design of a new micro-diffraction device consisting of three layers fabricated from silicon nitride, photoresist and polyimide film. The chip features low X-ray scattering and X-ray absorption properties, and uses a customizable blend of hydrophobic and hydrophilic surface patterns to help localize microcrystals to defined regions. Microcrystals in their native growth conditions can be loaded into the chips with a standard pipette, allowing data collection at room temperature. Diffraction data collected from hen egg-white lysozyme microcrystals (10–15 µm) loaded into the chips yielded a complete, high-resolution (<1.6 Å) data set sufficient to determine a high-quality structure by molecular replacement. In addition, the features of the chip allow the rapid and user-friendly analysis of microcrystals grown under virtually any laboratory format at microfocus synchrotron beamlines and XFELs.« less

A high-transparency, micro-patternable chip for X-ray diffraction analysis of microcrystals under native growth conditions

DOE Office of Scientific and Technical Information (OSTI.GOV)

Murray, Thomas D.; Lyubimov, Artem Y.; Ogata, Craig M.

Microcrystals present a significant impediment to the determination of macromolecular structures by X-ray diffraction methods. Although microfocus synchrotron beamlines and X-ray free-electron lasers (XFELs) can enable the collection of interpretable diffraction data from microcrystals, there is a need for efficient methods of harvesting small volumes (<2µl) of microcrystals grown under common laboratory formats and delivering them to an X-ray beam source under native growth conditions. One approach that shows promise in overcoming the challenges intrinsic to microcrystal analysis is to pair so-called `fixed-target' sample-delivery devices with microbeam-based X-ray diffraction methods. However, to record weak diffraction patterns it is necessary tomore » fabricate devices from X-ray-transparent materials that minimize background scattering. Presented here is the design of a new micro-diffraction device consisting of three layers fabricated from silicon nitride, photoresist and polyimide film. The chip features low X-ray scattering and X-ray absorption properties, and uses a customizable blend of hydrophobic and hydrophilic surface patterns to help localize microcrystals to defined regions. Microcrystals in their native growth conditions can be loaded into the chips with a standard pipette, allowing data collection at room temperature. Diffraction data collected from hen egg-white lysozyme microcrystals (10–15µm) loaded into the chips yielded a complete, high-resolution (<1.6Å) data set sufficient to determine a high-quality structure by molecular replacement. The features of the chip allow the rapid and user-friendly analysis of microcrystals grown under virtually any laboratory format at microfocus synchrotron beamlines and XFELs.« less

A high-transparency, micro-patternable chip for X-ray diffraction analysis of microcrystals under native growth conditions

PubMed Central

Murray, Thomas D.; Lyubimov, Artem Y.; Ogata, Craig M.; Vo, Huy; Uervirojnangkoorn, Monarin; Brunger, Axel T.; Berger, James M.

2015-01-01

Microcrystals present a significant impediment to the determination of macromolecular structures by X-ray diffraction methods. Although microfocus synchrotron beamlines and X-ray free-electron lasers (XFELs) can enable the collection of interpretable diffraction data from microcrystals, there is a need for efficient methods of harvesting small volumes (<2 µl) of microcrystals grown under common laboratory formats and delivering them to an X-ray beam source under native growth conditions. One approach that shows promise in overcoming the challenges intrinsic to microcrystal analysis is to pair so-called ‘fixed-target’ sample-delivery devices with microbeam-based X-ray diffraction methods. However, to record weak diffraction patterns it is necessary to fabricate devices from X-ray-transparent materials that minimize background scattering. Presented here is the design of a new micro-diffraction device consisting of three layers fabricated from silicon nitride, photoresist and polyimide film. The chip features low X-ray scattering and X-ray absorption properties, and uses a customizable blend of hydrophobic and hydrophilic surface patterns to help localize microcrystals to defined regions. Microcrystals in their native growth conditions can be loaded into the chips with a standard pipette, allowing data collection at room temperature. Diffraction data collected from hen egg-white lysozyme microcrystals (10–15 µm) loaded into the chips yielded a complete, high-resolution (<1.6 Å) data set sufficient to determine a high-quality structure by molecular replacement. The features of the chip allow the rapid and user-friendly analysis of microcrystals grown under virtually any laboratory format at microfocus synchrotron beamlines and XFELs. PMID:26457423

High-resolution x-ray diffraction microscopy of specifically labeled yeast cells

PubMed Central

Nelson, Johanna; Huang, Xiaojing; Steinbrener, Jan; Shapiro, David; Kirz, Janos; Marchesini, Stefano; Neiman, Aaron M.; Turner, Joshua J.; Jacobsen, Chris

2010-01-01

X-ray diffraction microscopy complements other x-ray microscopy methods by being free of lens-imposed radiation dose and resolution limits, and it allows for high-resolution imaging of biological specimens too thick to be viewed by electron microscopy. We report here the highest resolution (11–13 nm) x-ray diffraction micrograph of biological specimens, and a demonstration of molecular-specific gold labeling at different depths within cells via through-focus propagation of the reconstructed wavefield. The lectin concanavalin A conjugated to colloidal gold particles was used to label the α-mannan sugar in the cell wall of the yeast Saccharomyces cerevisiae. Cells were plunge-frozen in liquid ethane and freeze-dried, after which they were imaged whole using x-ray diffraction microscopy at 750 eV photon energy. PMID:20368463

High-resolution x-ray diffraction microscopy of specifically labeled yeast cells

DOE PAGES

Nelson, Johanna; Huang, Xiaojing; Steinbrener, Jan; ...

2010-04-20

X-ray diffraction microscopy complements other x-ray microscopy methods by being free of lens-imposed radiation dose and resolution limits, and it allows for high-resolution imaging of biological specimens too thick to be viewed by electron microscopy. We report here the highest resolution (11-13 nm) x-ray diffraction micrograph of biological specimens, and a demonstration of molecular-specific gold labeling at different depths within cells via through-focus propagation of the reconstructed wavefield. The lectin concanavalin A conjugated to colloidal gold particles was used to label the α-mannan sugar in the cell wall of the yeast Saccharomyces cerevisiae. Cells were plunge-frozen in liquid ethane andmore » freeze-dried, after which they were imaged whole using x-ray diffraction microscopy at 750 eV photon energy.« less

Crystal structures of (Mg1-x,Fe(x))SiO3 postperovskite at high pressures.

PubMed

Yamanaka, Takamitsu; Hirose, Kei; Mao, Wendy L; Meng, Yue; Ganesh, P; Shulenburger, Luke; Shen, Guoyin; Hemley, Russell J

2012-01-24

X-ray diffraction experiments on postperovskite (ppv) with compositions (Mg(0.9)Fe(0.1))SiO(3) and (Mg(0.6)Fe(0.4))SiO(3) at Earth core-mantle boundary pressures reveal different crystal structures. The former adopts the CaIrO(3)-type structure with space group Cmcm, whereas the latter crystallizes in a structure with the Pmcm (Pmma) space group. The latter has a significantly higher density (ρ = 6.119(1) g/cm(3)) than the former (ρ = 5.694(8) g/cm(3)) due to both the larger amount of iron and the smaller ionic radius of Fe(2+) as a result of an electronic spin transition observed by X-ray emission spectroscopy (XES). The smaller ionic radius for low-spin compared to high-spin Fe(2+) also leads to an ordered cation distribution in the M1 and M2 crystallographic sites of the higher density ppv structure. Rietveld structure refinement indicates that approximately 70% of the total Fe(2+) in that phase occupies the M2 site. XES results indicate a loss of 70% of the unpaired electronic spins consistent with a low spin M2 site and high spin M1 site. First-principles calculations of the magnetic ordering confirm that Pmcm with a two-site model is energetically more favorable at high pressure, and predict that the ordered structure is anisotropic in its electrical and elastic properties. These results suggest that interpretations of seismic structure in the deep mantle need to treat a broader range of mineral structures than previously considered.

Coherent x-ray zoom condenser lens for diffractive and scanning microscopy.

PubMed

Kimura, Takashi; Matsuyama, Satoshi; Yamauchi, Kazuto; Nishino, Yoshinori

2013-04-22

We propose a coherent x-ray zoom condenser lens composed of two-stage deformable Kirkpatrick-Baez mirrors. The lens delivers coherent x-rays with a controllable beam size, from one micrometer to a few tens of nanometers, at a fixed focal position. The lens is suitable for diffractive and scanning microscopy. We also propose non-scanning coherent diffraction microscopy for extended objects by using an apodized focused beam produced by the lens with a spatial filter. The proposed apodized-illumination method will be useful in highly efficient imaging with ultimate storage ring sources, and will also open the way to single-shot coherent diffraction microscopy of extended objects with x-ray free-electron lasers.

Scanning force microscope for in situ nanofocused X-ray diffraction studies

PubMed Central

Ren, Zhe; Mastropietro, Francesca; Davydok, Anton; Langlais, Simon; Richard, Marie-Ingrid; Furter, Jean-Jacques; Thomas, Olivier; Dupraz, Maxime; Verdier, Marc; Beutier, Guillaume; Boesecke, Peter; Cornelius, Thomas W.

2014-01-01

A compact scanning force microscope has been developed for in situ combination with nanofocused X-ray diffraction techniques at third-generation synchrotron beamlines. Its capabilities are demonstrated on Au nano-islands grown on a sapphire substrate. The new in situ device allows for in situ imaging the sample topography and the crystallinity by recording simultaneously an atomic force microscope (AFM) image and a scanning X-ray diffraction map of the same area. Moreover, a selected Au island can be mechanically deformed using the AFM tip while monitoring the deformation of the atomic lattice by nanofocused X-ray diffraction. This in situ approach gives access to the mechanical behavior of nanomaterials. PMID:25178002

Study of magnetic and electrical properties of nanocrystalline Mn doped NiO.

PubMed

Raja, S Philip; Venkateswaran, C

2011-03-01

Diluted Magnetic Semiconductors (DMS) are intensively explored in recent years for its applications in spintronics, which is expected to revolutionize the present day information technology. Nanocrystalline Mn doped NiO samples were prepared using chemical co-precipitation method with an aim to realize room temperature ferromagnetism. Phase formation of the samples was studied using X-ray diffraction-Rietveld analysis. Scanning electron microscopy and Energy dispersive X-ray analysis results reveal the nanocrystalline nature of the samples, agglomeration of the particles, considerable particle size distribution and the near stoichiometry. Thermomagnetic curves confirm the single-phase formation of the samples up to 1% doping of Mn. Vibrating Sample Magnetometer measurements indicate the absence of ferromagnetism at room temperature. This may be due to the low concentration of Mn2+ ions having weak indirect coupling with Ni2+ ions. The lack of free carriers is also expected to be the reason for the absence of ferromagnetism, which is in agreement with the results of resistivity measurements using impedance spectroscopy. Arrhenius plot shows the presence of two thermally activated regions and the activation energy for the nanocrystalline Mn doped sample was found to be greater than that of undoped NiO. This is attributed to the doping effect of Mn. However, the dielectric constant of the samples was found to be of the same order of magnitude very much comparable with that of undoped NiO.

Investigating the effect of moisture protection on solid-state stability and dissolution of fenofibrate and ketoconazole solid dispersions using PXRD, HSDSC and Raman microscopy.

PubMed

Kanaujia, Parijat; Lau, Grace; Ng, Wai Kiong; Widjaja, Effendi; Schreyer, Martin; Hanefeld, Andrea; Fischbach, Matthias; Saal, Christoph; Maio, Mario; Tan, Reginald B H

2011-09-01

Enhanced dissolution of poorly soluble active pharmaceutical ingredients (APIs) in amorphous solid dispersions often diminishes during storage due to moisture-induced re-crystallization. This study aims to investigate the influence of moisture protection on solid-state stability and dissolution profiles of melt-extruded fenofibrate (FF) and ketoconazole (KC) solid dispersions. Samples were kept in open, closed and Activ-vials(®) to control the moisture uptake under accelerated conditions. During 13-week storage, changes in API crystallinity were quantified using powder X-ray diffraction (PXRD) (Rietveld analysis) and high sensitivity differential scanning calorimetry (HSDSC) and compared with any change in dissolution profiles. Trace crystallinity was observed by Raman microscopy, which otherwise was undetected by PXRD and HSDSC. Results showed that while moisture protection was ineffective in preventing the re-crystallization of amorphous FF, KC remained X-ray amorphous despite 5% moisture uptake. Regardless of the degree of crystallinity increase in FF, the enhanced dissolution properties were similarly diminished. Moisture uptake above 10% in KC samples also led to re-crystallization and significant decrease in dissolution rates. In conclusion, eliminating moisture sorption may not be sufficient in ensuring the stability of solid dispersions. Analytical quantification of API crystallinity is crucial in detecting subtle increase in crystallinity that can diminish the enhanced dissolution properties of solid dispersions.

Effect of preparation methods and doping on the structural and tunable emissions of CdS

NASA Astrophysics Data System (ADS)

Mohamed, Mohamed Bakr; Abdel-Kader, M. H.; Alhazime, Ali A.; Almarashi, Jamal Q. M.

2018-03-01

Fe, Mn and Mg doped CdS samples were prepared by thermolysis method in air and under flow of nitrogen. Structural, compositional and optical properties of the prepared samples were investigated using x-ray powder diffraction (XRD), scanning electron microscope (SEM/EDS mapping), Fourier transform infrared red (FTIR), UV-vis absorption and photoluminescence (PL) spectroscopes. Rietveld refinement of x-ray data showed that all the undoped and doped CdS samples prepared in air and under flow of nitrogen have both cubic and hexagonal structures. The percentages of hexagonal and cubic phases for all prepared samples were determined. The crystallite size increased for CdS prepared under flow of N2 compared with the sample prepared in air. The energy gap of all the samples was calculated using UV data. The intensity of PL emission changed according to the method of preparation and the kind of doping elements. PL emission revealed a blue shift for CdS prepared in air compared with CdS prepared under flow of nitrogen; also all doped samples showed a red shift of PL spectra compared with undoped samples. Undoped and doped CdS with Fe and Mg samples emitted violet and blue sub-spectra. Mn doped CdS prepared in air revealed violet, blue and yellow sub-spectra, while the sample prepared under flow of N2 emitted violet, blue and green sub-spectra.

Mineralogical and chemical characterization of iron-, manganese-, and copper-containing synthetic hydroxyapatites.

PubMed

Sutter, B; Ming, D W; Clearfield, A; Hossner, L R

2003-01-01

The National Aeronautics and Space Administration's (NASA) Advanced Life Support (ALS) Program is evaluating the use of Fe-, Mn-, and Cu-containing synthetic hydroxyapatite (SHA) as a slow release fertilizer for crops that might be grown on the International Space Station or at Lunar and Martian outposts. Separate Fe-, Mn-, and Cu-containing SHA materials along with a transition-metal free SHA (pure-SHA) were synthesized using a precipitation method. Chemical and mineralogical analyses determined if and how Fe, Mn, and Cu were incorporated into the SHA structure. X-ray diffraction (XRD), Rietveld refinement, and transmission electron microscopy (TEM) confirmed that SHA materials with the apatite structure were produced. Chemical analyses indicated that the metal containing SHA materials were deficient in Ca relative to pure-SHA. The shift in the infrared PO4-mu 3 vibrations, smaller unit cell parameters, smaller particle size, and greater structural strain for Fe-, Mn-, and Cu-containing SHA compared with pure-SHA suggested that Fe, Mn, and Cu were incorporated into SHA structure. Rietveld analyses revealed that Fe, Mn, and Cu substituted into the Ca2 site of SHA. An Fe-rich phase was detected by TEM analyses and backscattered electron microscopy in the Fe-containing SHA material with the greatest Fe content. The substitution of metals into SHA suggests that metal-SHA materials are potential slow-release sources of micronutrients for plant uptake in addition to Ca and P.

Mineralogical and chemical characterization of iron-, manganese-, and copper-containing synthetic hydroxyapatites

NASA Technical Reports Server (NTRS)

Sutter, B.; Ming, D. W.; Clearfield, A.; Hossner, L. R.

2003-01-01

The National Aeronautics and Space Administration's (NASA) Advanced Life Support (ALS) Program is evaluating the use of Fe-, Mn-, and Cu-containing synthetic hydroxyapatite (SHA) as a slow release fertilizer for crops that might be grown on the International Space Station or at Lunar and Martian outposts. Separate Fe-, Mn-, and Cu-containing SHA materials along with a transition-metal free SHA (pure-SHA) were synthesized using a precipitation method. Chemical and mineralogical analyses determined if and how Fe, Mn, and Cu were incorporated into the SHA structure. X-ray diffraction (XRD), Rietveld refinement, and transmission electron microscopy (TEM) confirmed that SHA materials with the apatite structure were produced. Chemical analyses indicated that the metal containing SHA materials were deficient in Ca relative to pure-SHA. The shift in the infrared PO4-mu 3 vibrations, smaller unit cell parameters, smaller particle size, and greater structural strain for Fe-, Mn-, and Cu-containing SHA compared with pure-SHA suggested that Fe, Mn, and Cu were incorporated into SHA structure. Rietveld analyses revealed that Fe, Mn, and Cu substituted into the Ca2 site of SHA. An Fe-rich phase was detected by TEM analyses and backscattered electron microscopy in the Fe-containing SHA material with the greatest Fe content. The substitution of metals into SHA suggests that metal-SHA materials are potential slow-release sources of micronutrients for plant uptake in addition to Ca and P.

Structural, magnetic, magneto-caloric and Mössbauer spectral study of Tb{sub 2}Fe{sub 17} compound synthesized by arc melting

DOE Office of Scientific and Technical Information (OSTI.GOV)

Charfeddine, S.; LVMU, Centre National de Recherches en Sciences des Matériaux, Technopole de Borj-Cédria, BP 73 Soliman 8027; Zehani, K.

We have synthesized the intermetallic Tb{sub 2}Fe{sub 17} compound in hexagonal crystal structure by arc-melting without annealing. X-ray diffraction pattern has been refined by Rietveld method. The crystal structure is hexagonal with P6{sub 3}/mmc space group (Th{sub 2}Ni{sub 17}-type). The Mössbauer spectrum of Tb{sub 2}Fe{sub 17} compound has been analyzed with seven magnetic sextets assigned to the inequivalent crystallographic sites. The temperature dependence of magnetization data revealed that Tb{sub 2}Fe{sub 17} exhibits a second-order ferromagnetic to paramagnetic phase transition in the vicinity of Curie temperature (T{sub C}=412 K). The relative cooling power around the magnetic transition and the Arrott plotsmore » are also reported. - Graphical abstract: A 3D surface showing the temperature and applied magnetic field dependencies of the magnetization for Tb{sub 2}Fe{sub 17} compound (left). Rietveld analysis of the XRD pattern (right). Crystal structure for the hexagonal P6{sub 3}/mmc Tb{sub 2}Fe{sub 17} (bottom). Display Omitted - Highlights: • Tb{sub 2}Fe{sub 17} single-phase synthesized by simple arc-melting without any heat treatment. • The crystal structure is hexagonal with P6{sub 3}/mmc space group. • The magnetic entropy change of the sample was determined by Maxwell relation. • Hyperfine parameters, magnetic and magnetocaloric properties were studied.« less

Understanding the formation and growth of Ag nanoparticles on silver chromate induced by electron irradiation in electron microscope: A combined experimental and theoretical study

DOE Office of Scientific and Technical Information (OSTI.GOV)

Fabbro, Maria T.; Department of Inorganic and Organic Chemistry, Universitat Jaume I, Campus del Riu Sec, E-12071 Castellón; Gracia, Lourdes

Ag{sub 2}CrO{sub 4} microcrystals were synthesized using the co-precipitation method. These microcrystals were characterized through X-ray diffraction (XRD) with Rietveld analysis, field-emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM) with energy-dispersive spectroscopy (EDS), micro-Raman (MR). XRD patterns and Rietveld refinement data showed that the material exhibits an orthorhombic structure without any deleterious phases. FE-SEM and TEM micrographs revealed the morphology and the growth of Ag nanoparticles on Ag{sub 2}CrO{sub 4} microcrystals during electron beam irradiation. These events were directly monitored in real-time. Their optical properties were investigated using ultraviolet-visible (UV–vis) diffuse reflectance spectroscopy that allowed the calculation of themore » optical band gap energy. Theoretical analyses based on the density functional theory level indicate that the incorporation of electrons is responsible for structural modifications and formation of defects on the [AgO{sub 6}] and [AgO{sub 4}] clusters, generating ideal conditions for the growth of Ag nanoparticles. - Graphical abstract: Theoretical representation of the Ag{sub 2}CrO{sub 4} orthorhombic structure. Display Omitted - Highlights: • The Ag{sub 2}CrO{sub 4} microcrystals indicate an orthorhombic structure. • The formation of Ag{sup 0} promotes Ag-nanoparticle growth on the surface of the Ag{sub 2}CrO{sub 4}. • Electron irradiation of the material induces the formation of Ag vacancies.« less

X-ray topography using the forward transmitted beam under multiple-beam diffraction conditions

DOE Office of Scientific and Technical Information (OSTI.GOV)

Tsusaka, Y., E-mail: tsusaka@sci.u-hyogo.ac.jp; Takano, H.; Takeda, S.

2016-02-15

X-ray topographs are taken for a sapphire wafer with the [0001] surface normal, as an example, by forward transmitted synchrotron x-ray beams combined with two-dimensional electronic arrays in the x-ray detector having a spatial resolution of 1 μm. They exhibit no shape deformation and no position shift of the dislocation lines on the topographs. Since the topography is performed under multiple-beam diffraction conditions, the topographic images of a single diffraction (two-wave approximation condition) or plural diffractions (six-wave approximation condition) can be recorded without large specimen position changes. As usual Lang topographs, it is possible to determine the Burgers vector ofmore » each dislocation line. Because of high parallelism of the incoming x-rays and linear sensitivity of the electronic arrays to the incident x-rays, the present technique can be used to visualize individual dislocations in single crystals of the dislocation density as high as 1 × 10{sup 5} cm{sup −2}.« less

Multiple defocused coherent diffraction imaging: method for simultaneously reconstructing objects and probe using X-ray free-electron lasers.

PubMed

Hirose, Makoto; Shimomura, Kei; Suzuki, Akihiro; Burdet, Nicolas; Takahashi, Yukio

2016-05-30

The sample size must be less than the diffraction-limited focal spot size of the incident beam in single-shot coherent X-ray diffraction imaging (CXDI) based on a diffract-before-destruction scheme using X-ray free electron lasers (XFELs). This is currently a major limitation preventing its wider applications. We here propose multiple defocused CXDI, in which isolated objects are sequentially illuminated with a divergent beam larger than the objects and the coherent diffraction pattern of each object is recorded. This method can simultaneously reconstruct both objects and a probe from the coherent X-ray diffraction patterns without any a priori knowledge. We performed a computer simulation of the prposed method and then successfully demonstrated it in a proof-of-principle experiment at SPring-8. The prposed method allows us to not only observe broad samples but also characterize focused XFEL beams.

Angular rheology study of colloidal nanocrystals using Coherent X-ray Diffraction

NASA Astrophysics Data System (ADS)

Liang, Mengning; Harder, Ross; Robinson, Ian

2007-03-01

A new method using coherent x-ray diffraction provides a way to investigate the rotational motion of a colloidal suspension of crystals in real time. Coherent x-ray diffraction uses the long coherence lengths of synchrotron sources to illuminate a nanoscale particle coherently over its spatial dimensions. The penetration of high energy x-rays into various media allows for in-situ measurements making it ideal for suspensions. This technique has been used to image the structure of nanocrystals for some time but also has the capability of providing information about the orientation and dynamics of crystals. The particles are imaged in a specific diffraction condition allowing us to determine their orientation and observe how they rotate in real time with exceptional resolution. Such sensitivity allows for the study of rotational Brownian motion of nanocrystals in various suspensions and conditions. We present a study of the angular rheology of alumina and TiO2 colloidal nanocrystals in media using coherent x-ray diffraction.

Characterization of polycrystalline materials using synchrotron X-ray imaging and diffraction techniques

NASA Astrophysics Data System (ADS)

Ludwig, W.; King, A.; Herbig, M.; Reischig, P.; Marrow, J.; Babout, L.; Lauridsen, E. M.; Proudhon, H.; Buffière, J. Y.

2010-12-01

The combination of synchrotron radiation x-ray imaging and diffraction techniques offers new possibilities for in-situ observation of deformation and damage mechanisms in the bulk of polycrystalline materials. Minute changes in electron density (i.e., cracks, porosities) can be detected using propagation based phase contrast imaging, a 3-D imaging mode exploiting the coherence properties of third generation synchrotron beams. Furthermore, for some classes of polycrystalline materials, one may use a 3-D variant of x-ray diffraction imaging, termed x-ray diffraction contrast tomography. X-ray diffraction contrast tomography provides access to the 3-D shape, orientation, and elastic strain state of the individual grains from polycrystalline sample volumes containing up to thousand grains. Combining both imaging modalities, one obtains a comprehensive description of the materials microstructure at the micrometer length scale. Repeated observation during (interrupted) mechanical tests provide unprecedented insight into crystallographic and grain microstructure related aspects of polycrystalline deformation and degradation mechanisms.

Selenium single-wavelength anomalous diffraction de novo phasing using an X-ray-free electron laser

DOE PAGES

Hunter, Mark S.; Yoon, Chun Hong; DeMirci, Hasan; ...

2016-11-04

Structural information about biological macromolecules near the atomic scale provides important insight into the functions of these molecules. To date, X-ray crystallography has been the predominant method used for macromolecular structure determination. However, challenges exist when solving structures with X-rays, including the phase problem and radiation damage. X-ray-free electron lasers (X-ray FELs) have enabled collection of diffraction information before the onset of radiation damage, yet the majority of structures solved at X-ray FELs have been phased using external information via molecular replacement. De novo phasing at X-ray FELs has proven challenging due in part to per-pulse variations in intensity andmore » wavelength. Here we report the solution of a selenobiotinyl-streptavidin structure using phases obtained by the anomalous diffraction of selenium measured at a single wavelength (Se-SAD) at the Linac Coherent Light Source. Finally, our results demonstrate Se-SAD, routinely employed at synchrotrons for novel structure determination, is now possible at X-ray FELs.« less

Macromolecular structures probed by combining single-shot free-electron laser diffraction with synchrotron coherent X-ray imaging.

PubMed

Gallagher-Jones, Marcus; Bessho, Yoshitaka; Kim, Sunam; Park, Jaehyun; Kim, Sangsoo; Nam, Daewoong; Kim, Chan; Kim, Yoonhee; Noh, Do Young; Miyashita, Osamu; Tama, Florence; Joti, Yasumasa; Kameshima, Takashi; Hatsui, Takaki; Tono, Kensuke; Kohmura, Yoshiki; Yabashi, Makina; Hasnain, S Samar; Ishikawa, Tetsuya; Song, Changyong

2014-05-02

Nanostructures formed from biological macromolecular complexes utilizing the self-assembly properties of smaller building blocks such as DNA and RNA hold promise for many applications, including sensing and drug delivery. New tools are required for their structural characterization. Intense, femtosecond X-ray pulses from X-ray free-electron lasers enable single-shot imaging allowing for instantaneous views of nanostructures at ambient temperatures. When combined judiciously with synchrotron X-rays of a complimentary nature, suitable for observing steady-state features, it is possible to perform ab initio structural investigation. Here we demonstrate a successful combination of femtosecond X-ray single-shot diffraction with an X-ray free-electron laser and coherent diffraction imaging with synchrotron X-rays to provide an insight into the nanostructure formation of a biological macromolecular complex: RNA interference microsponges. This newly introduced multimodal analysis with coherent X-rays can be applied to unveil nano-scale structural motifs from functional nanomaterials or biological nanocomplexes, without requiring a priori knowledge.

Experimental and Theoretical Investigations on Intermediate Band in Doped Nano-SnS2

NASA Astrophysics Data System (ADS)

Heiba, Zein K.; Mohamed, Mohamed Bakr; Abdel Kader, M. H.

2018-03-01

Nano-SnS2 and Sn0.75 X 0.25S2 (X = Cr, Fe, Y) have been prepared by thermolysis method. Phase analysis of x-ray diffraction data confirmed the single-phase nature of all prepared samples, with some residual carbon contributing to the background. Rietveld refinement revealed high anisotropy in crystallite size, signifying a cylindrical structure for the particle shape, as confirmed by transmission electron microscopy. The refined occupancies obtained for the doped cations were found to be smaller than the nominal target doping ratio (25%). Fourier-transform infrared spectra showed presence of Sn-S bond in all samples. The energy was found to be 3.42 eV, 3.33 eV, 2.1 eV and 3.14 eV, and 3.62 eV for undoped SnS2 and when doped with Cr, Fe, and Y, respectively. Density functional theory calculations illustrated that Fe-doped SnS2 has two bandgaps [normal and intermediate (IB) bands]. Meanwhile, Sn0.75Fe0.25S2 sample showed anti-Stokes and an extra photoluminescence peak related to the newly created intermediate band (IB) inside the energy gap. On the other hand, pure SnS2 and Sn0.75 X 0.25S2 (X = Cr, Y) samples emitted four photoluminescence subspectra in ultraviolet, violet, and blue regions.

Structure and magnetic behaviors of melt-spun SmFeSiB ribbons and their nitrides

NASA Astrophysics Data System (ADS)

Luo, Y.; Zhang, K.; Li, K. S.; Yu, D. B.; Ling, J. J.; Men, K.; Dou, Q. Y.; Yan, W. L.; Xie, J. J.; Yang, Y. F.

2016-05-01

SmFe9.3+xSi0.2B0.1 (x=0, 0.5, 1.0) ribbons and their nitrides were prepared by melt-spinning, followed by annealing and subsequent nitriding. The structure and magnetic properties have been investigated by means of powder X-ray diffraction, vibrating sample magnetometer and Mossbauer spectroscopy. Rietveld analysis shows that the augment of Fe content gives rise to an increase of the c/a ratio and cell volume. The increasing amount of Fe atoms occupying the 2e sites results in the change of initial structure. It is indicated that the isomer shift of 3g and 6l atom remains quasi-constant while the 2e atom shows a noticeable increase with the increase of iron content, which further conforms the preferential occupation of excessive Fe atoms at this site. Consistent with Tc, the mean hyperfine field 〈Bhf〉 has the highest value of 25.7 T when x=0.5. The hyperfine fields at different Fe sites follow the order H2e>H3g>H6l. The highest curie temperature of 477.68 K and the hyperfine field of 25.7 T in the as-quenched ribbons were obtained when x=0.5. Meanwhile, the highest magnetic properties of Hcj=4.31 kOe, (BH)m=3.5 MGOe in the nitride powders were found.

Exploration of New Principles in Spintronics Based on Topological Insulators (Option 1)

DTIC Science & Technology

2012-05-14

on the surface and found that our crystals are exceedingly homogeneous (Supplementary Information). The persistently narrow X - ray diffraction peaks...modified Bridgman method (see Supplementary Information for details). X - ray diffraction measurements indicated the monotonic shrinkage of a and c axis...and annealing at that temperature for 4 days. X - ray diffraction analyses confirmed that all the samples have the same crystal structure (R 3m

Efficient modeling of Bragg coherent x-ray nanobeam diffraction

DOE PAGES

Hruszkewycz, S. O.; Holt, M. V.; Allain, M.; ...

2015-07-02

X-ray Bragg diffraction experiments that utilize tightly focused coherent beams produce complicated Bragg diffraction patterns that depend on scattering geometry, characteristics of the sample, and properties of the x-ray focusing optic. In this paper, we use a Fourier-transform-based method of modeling the 2D intensity distribution of a Bragg peak and apply it to the case of thin films illuminated with a Fresnel zone plate in three different Bragg scattering geometries. Finally, the calculations agree well with experimental coherent diffraction patterns, demonstrating that nanodiffraction patterns can be modeled at nonsymmetric Bragg conditions with this approach—a capability critical for advancing nanofocused x-raymore » diffraction microscopy.« less

Structural analysis and characterization of layer perovskite oxynitrides made from Dion Jacobson oxide precursors

NASA Astrophysics Data System (ADS)

Schottenfeld, Joshua A.; Benesi, Alan J.; Stephens, Peter W.; Chen, Gugang; Eklund, Peter C.; Mallouk, Thomas E.

2005-07-01

A three-layer oxynitride Ruddlesden-Popper phase Rb 1+xCa 2Nb 3O 10-xN x· yH 2O ( x=0.7-0.8, y=0.4-0.6) was synthesized by ammonialysis at 800 °C from the Dion-Jacobson phase RbCa 2Nb 3O 10 in the presence of Rb 2CO 3. Incorporation of nitrogen into the layer perovskite structure was confirmed by XPS, combustion analysis, and MAS NMR. The water content was determined by thermal gravimetric analysis and the rubidium content by ICP-MS. A similar layered perovskite interconversion occurred in the two-layer Dion-Jacobson oxide RbLaNb 2O 7 to yield Rb 1+xLaNb 2O 7-xN x· yH 2O ( x=0.7-0.8, y=0.5-1.0). Both compounds were air- and moisture-sensitive, with rapid loss of nitrogen by oxidation and hydrolysis reactions. The structure of the three-layer oxynitride Rb 1.7Ca 2Nb 3O 9.3N 0.7·0.5H 2O was solved in space group P4 /mmm with a=3.887(3) and c=18.65(1) Å, by Rietveld refinement of X-ray powder diffraction data. The two-layer oxynitride structure Rb 1.8LaNb 2O 6.3N 0.7·1.0H 2O was also determined in space group P4 /mmm with a=3.934(2) and c=14.697(2) Å. GSAS refinement of synchrotron X-ray powder diffraction data showed that the water molecules were intercalated between a double layer of Rb+ ions in both the two- and three-layer Ruddlesden-Popper structures. Optical band gaps were measured by diffuse reflectance UV-vis for both materials. An indirect band gap of 2.51 eV and a direct band gap of 2.99 eV were found for the three-layer compound, while an indirect band gap of 2.29 eV and a direct band gap of 2.84 eV were measured for the two-layer compound. Photocatalytic activity tests of the three-layer compound under 380 nm pass filtered light with AgNO 3 as a sacrificial electron acceptor gave a quantum yield of 0.025% for oxygen evolution.

Influence of Zn doping on structural, optical and dielectric properties of LaFeO3

NASA Astrophysics Data System (ADS)

Manzoor, Samiya; Husain, Shahid

2018-05-01

The effect of Zn doping on structural, optical and dielectric properties of nano-crystalline LaFe1‑xZnxO3 (0.0 ≤ x ≤ 0.3) samples have been investigated. These samples are synthesized using conventional solid state reaction route. X-ray diffraction patterns with Rietveld analysis confirm the single phase nature of samples. Further, the sample formation has been confirmed by FTIR spectroscopy. All the samples are formed in orthorhombic crystal symmetry with Pbnm space group. The average crystallite sizes, calculated from the Scherer’s formula, lie in the range below 50 nm. Rietveld refinement technique is used to determine lattice parameters, bond lengths and unit cell volume. Williamson-Hall analysis has been performed to calculate the crystallite size and lattice strain. Crystallite sizes are found to be of nanometer range while the strain is of the order of 10‑3. Zn doping leads to the expansion of volume due to the tensile strain. Optical bandgap has been determined from Kubelka-Munk function using Tauc’s relation. Zinc doping in LaFeO3 leads to decrease in optical bandgap. Dielectric constant as a function of frequency is measured in the frequency range of 75 kHz–5 MHz. The dielectric behavior has been investigated by analyzing ‘universal dielectric response’ (UDR) model. The dielectric constant (ε‧) shows colossal value with Zn doping in the whole frequency range. However, the imaginary part (ε″) shows relaxational behavior which may be attributed to the strong correlation that exists between conduction mechanism and dielectric behavior in ferrites. Cole-Cole analysis has been done that confirms the dielectric material does not follow the ideal Debye theory but shows distribution of relaxation times. The a.c conductivity increases with frequency and with Zn doping due to the increased polaron hopping.

HiSPoD: a program for high-speed polychromatic X-ray diffraction experiments and data analysis on polycrystalline samples

DOE PAGES

Sun, Tao; Fezzaa, Kamel

2016-06-17

Here, a high-speed X-ray diffraction technique was recently developed at the 32-ID-B beamline of the Advanced Photon Source for studying highly dynamic, yet non-repeatable and irreversible, materials processes. In experiments, the microstructure evolution in a single material event is probed by recording a series of diffraction patterns with extremely short exposure time and high frame rate. Owing to the limited flux in a short pulse and the polychromatic nature of the incident X-rays, analysis of the diffraction data is challenging. Here, HiSPoD, a stand-alone Matlab-based software for analyzing the polychromatic X-ray diffraction data from polycrystalline samples, is described. With HiSPoD,more » researchers are able to perform diffraction peak indexing, extraction of one-dimensional intensity profiles by integrating a two-dimensional diffraction pattern, and, more importantly, quantitative numerical simulations to obtain precise sample structure information.« less

X-ray diffraction and X-ray standing-wave study of the lead stearate film structure

DOE Office of Scientific and Technical Information (OSTI.GOV)

Blagov, A. E.; Dyakova, Yu. A.; Kovalchuk, M. V.

2016-05-15

A new approach to the study of the structural quality of crystals is proposed. It is based on the use of X-ray standing-wave method without measuring secondary processes and considers the multiwave interaction of diffraction reflections corresponding to different harmonics of the same crystallographic reflection. A theory of multiwave X-ray diffraction is developed to calculate the rocking curves in the X-ray diffraction scheme under consideration for a long-period quasi-one-dimensional crystal. This phase-sensitive method is used to study the structure of a multilayer lead stearate film on a silicon substrate. Some specific structural features are revealed for the surface layer ofmore » the thin film, which are most likely due to the tilt of the upper layer molecules with respect to the external normal to the film surface.« less

Molybdenum cell for x-ray diffraction measurements of fluid alkali metals at high temperatures and high pressures

NASA Astrophysics Data System (ADS)

Matsuda, Kazuhiro; Tamura, Kozaburo; Katoh, Masahiro; Inui, Masanori

2004-03-01

We have developed a sample cell for x-ray diffraction measurements of fluid alkali metals at high temperatures and high pressures. All parts of the cell are made of molybdenum which is resistant to the chemical corrosion of alkali metals. Single crystalline molybdenum disks electrolytically thinned down to 40 μm were used as the walls of the cell through which x rays pass. The crystal orientation of the disks was controlled in order to reduce the background from the cell. All parts of the cell were assembled and brazed together using a high-temperature Ru-Mo alloy. Energy dispersive x-ray diffraction measurements have been successfully carried out for fluid rubidium up to 1973 K and 16.2 MPa. The obtained S(Q) demonstrates the applicability of the molybdenum cell to x-ray diffraction measurements of fluid alkali metals at high temperatures and high pressures.

High-resolution ab initio three-dimensional x-ray diffraction microscopy

DOE PAGES

Chapman, Henry N.; Barty, Anton; Marchesini, Stefano; ...

2006-01-01

Coherent x-ray diffraction microscopy is a method of imaging nonperiodic isolated objects at resolutions limited, in principle, by only the wavelength and largest scattering angles recorded. We demonstrate x-ray diffraction imaging with high resolution in all three dimensions, as determined by a quantitative analysis of the reconstructed volume images. These images are retrieved from the three-dimensional diffraction data using no a priori knowledge about the shape or composition of the object, which has never before been demonstrated on a nonperiodic object. We also construct two-dimensional images of thick objects with greatly increased depth of focus (without loss of transverse spatialmore » resolution). These methods can be used to image biological and materials science samples at high resolution with x-ray undulator radiation and establishes the techniques to be used in atomic-resolution ultrafast imaging at x-ray free-electron laser sources.« less

Enhancing resolution in coherent x-ray diffraction imaging.

PubMed

Noh, Do Young; Kim, Chan; Kim, Yoonhee; Song, Changyong

2016-12-14

Achieving a resolution near 1 nm is a critical issue in coherent x-ray diffraction imaging (CDI) for applications in materials and biology. Albeit with various advantages of CDI based on synchrotrons and newly developed x-ray free electron lasers, its applications would be limited without improving resolution well below 10 nm. Here, we review the issues and efforts in improving CDI resolution including various methods for resolution determination. Enhancing diffraction signal at large diffraction angles, with the aid of interference between neighboring strong scatterers or templates, is reviewed and discussed in terms of increasing signal-to-noise ratio. In addition, we discuss errors in image reconstruction algorithms-caused by the discreteness of the Fourier transformations involved-which degrade the spatial resolution, and suggest ways to correct them. We expect this review to be useful for applications of CDI in imaging weakly scattering soft matters using coherent x-ray sources including x-ray free electron lasers.

A portable X-ray diffraction apparatus for in situ analyses of masters' paintings

NASA Astrophysics Data System (ADS)

Eveno, Myriam; Duran, Adrian; Castaing, Jacques

2010-09-01

It is rare that the analyses of materials in paintings can be carried out by taking micro-samples. Valuable works of art are best studied in situ by non-invasive techniques. For that purpose, a portable X-ray diffraction and fluorescence apparatus has been designed and constructed at the C2RMF. This apparatus has been used for paintings of Rembrandt, Leonardo da Vinci, Van Gogh, Mantegna, etc. Results are given to illustrate the performance of X-ray diffraction, especially when X-ray fluorescence does not bring sufficient information to conclude.

Microstructural characterization of dental zinc phosphate cements using combined small angle neutron scattering and microfocus X-ray computed tomography.

PubMed

Viani, Alberto; Sotiriadis, Konstantinos; Kumpová, Ivana; Mancini, Lucia; Appavou, Marie-Sousai

2017-04-01

To characterize the microstructure of two zinc phosphate cement formulations in order to investigate the role of liquid/solid ratio and composition of powder component, on the developed porosity and, consequently, on compressive strength. X-ray powder diffraction with the Rietveld method was used to study the phase composition of zinc oxide powder and cements. Powder component and cement microstructure were investigated with scanning electron microscopy. Small angle neutron scattering (SANS) and microfocus X-ray computed tomography (XmCT) were together employed to characterize porosity and microstructure of dental cements. Compressive strength tests were performed to evaluate their mechanical performance. The beneficial effects obtained by the addition of Al, Mg and B to modulate powder reactivity were mitigated by the crystallization of a Zn aluminate phase not involved in the cement setting reaction. Both cements showed spherical pores with a bimodal distribution at the micro/nano-scale. Pores, containing a low density gel-like phase, developed through segregation of liquid during setting. Increasing liquid/solid ratio from 0.378 to 0.571, increased both SANS and XmCT-derived specific surface area (by 56% and 22%, respectively), porosity (XmCT-derived porosity increased from 3.8% to 5.2%), the relative fraction of large pores ≥50μm, decreased compressive strength from 50±3MPa to 39±3MPa, and favored microstructural and compositional inhomogeneities. Explain aspects of powder design affecting the setting reaction and, in turn, cement performance, to help in optimizing cement formulation. The mechanism behind development of porosity and specific surface area explains mechanical performance, and processes such as erosion and fluoride release/uptake. Copyright © 2017 The Authors. Published by Elsevier Ltd.. All rights reserved.

X-ray fractography on fatigue fractured surface of austenitic stainless steel

DOE Office of Scientific and Technical Information (OSTI.GOV)

Yajima, Zenjiro; Tokuyama, Hideki; Kibayashi, Yasuo

1995-12-31

X-ray diffraction observation of the material internal structure beneath fracture surfaces provide fracture analysis with useful information to investigate the conditions and mechanisms of fracture. X-ray fractography is a generic name given to this technique. In the present study, X-ray fractography was applied to fatigue fracture surfaces of austenitic stainless steel (AISI 304) which consisted of solution treatment. The fatigue tests were carried out on compact tension (CT) specimens. The plastic strain on the fracture surface was estimated from measuring the line broadening of X-ray diffraction profiles. The line broadening of X-ray diffraction profiles was measured on and beneath fatiguemore » fracture surfaces. The depth of the plastic zone left on fracture surfaces was evaluated from the line broadening. The results are discussed on the basis of fracture mechanics.« less

Toward in situ x-ray diffraction imaging at the nanometer scale

NASA Astrophysics Data System (ADS)

Zatsepin, Nadia A.; Dilanian, Ruben A.; Nikulin, Andrei Y.; Gable, Brian M.; Muddle, Barry C.; Sakata, Osami

2008-08-01

We present the results of preliminary investigations determining the sensitivity and applicability of a novel x-ray diffraction based nanoscale imaging technique, including simulations and experiments. The ultimate aim of this nascent technique is non-destructive, bulk-material characterization on the nanometer scale, involving three dimensional image reconstructions of embedded nanoparticles and in situ sample characterization. The approach is insensitive to x-ray coherence, making it applicable to synchrotron and laboratory hard x-ray sources, opening the possibility of unprecedented nanometer resolution with the latter. The technique is being developed with a focus on analyzing a technologically important light metal alloy, Al-xCu (where x is 2.0-5.0 %wt). The mono- and polycrystalline samples contain crystallographically oriented, weakly diffracting Al2Cu nanoprecipitates in a sparse, spatially random dispersion within the Al matrix. By employing a triple-axis diffractometer in the non-dispersive setup we collected two-dimensional reciprocal space maps of synchrotron x-rays diffracted from the Al2Cu nanoparticles. The intensity profiles of the diffraction peaks confirmed the sensitivity of the technique to the presence and orientation of the nanoparticles. This is a fundamental step towards in situ observation of such extremely sparse, weakly diffracting nanoprecipitates embedded in light metal alloys at early stages of their growth.

Diffraction and Imaging Study of Imperfections of Protein Crystals with Coherent X-rays

NASA Technical Reports Server (NTRS)

Hu, Z. W.; Thomas, B. R.; Chernov, A. A.; Chu, Y. S.; Lai, B.

2004-01-01

High angular-resolution x-ray diffraction and phase contrast x-ray imaging were combined to study defects and perfection of protein crystals. Imperfections including line defects, inclusions and other microdefects were observed in the diffraction images of a uniformly grown lysozyme crystal. The observed line defects carry distinct dislocation features running approximately along the <110> growth front and have been found to originate mostly in a central growth area and occasionally in outer growth regions. Slow dehydration led to the broadening of a fairly symmetric 4 4 0 rocking curve by a factor of approximately 2.6, which was primarily attributed to the dehydration-induced microscopic effects that are clearly shown in diffraction images. X-ray imaging and diffraction characterization of the quality of apoferritin crystals will also be discussed in the presentation.

Profex: a graphical user interface for the Rietveld refinement program BGMN.

PubMed

Doebelin, Nicola; Kleeberg, Reinhard

2015-10-01

Profex is a graphical user interface for the Rietveld refinement program BGMN . Its interface focuses on preserving BGMN 's powerful and flexible scripting features by giving direct access to BGMN input files. Very efficient workflows for single or batch refinements are achieved by managing refinement control files and structure files, by providing dialogues and shortcuts for many operations, by performing operations in the background, and by providing import filters for CIF and XML crystal structure files. Refinement results can be easily exported for further processing. State-of-the-art graphical export of diffraction patterns to pixel and vector graphics formats allows the creation of publication-quality graphs with minimum effort. Profex reads and converts a variety of proprietary raw data formats and is thus largely instrument independent. Profex and BGMN are available under an open-source license for Windows, Linux and OS X operating systems.

Profex: a graphical user interface for the Rietveld refinement program BGMN

PubMed Central

Doebelin, Nicola; Kleeberg, Reinhard

2015-01-01

Profex is a graphical user interface for the Rietveld refinement program BGMN. Its interface focuses on preserving BGMN’s powerful and flexible scripting features by giving direct access to BGMN input files. Very efficient workflows for single or batch refinements are achieved by managing refinement control files and structure files, by providing dialogues and shortcuts for many operations, by performing operations in the background, and by providing import filters for CIF and XML crystal structure files. Refinement results can be easily exported for further processing. State-of-the-art graphical export of diffraction patterns to pixel and vector graphics formats allows the creation of publication-quality graphs with minimum effort. Profex reads and converts a variety of proprietary raw data formats and is thus largely instrument independent. Profex and BGMN are available under an open-source license for Windows, Linux and OS X operating systems. PMID:26500466

THE EFFECT OF SATELLITE LINES FROM THE X-RAY SOURCE ON X-RAY DIFFRACTION PEAKS

EPA Science Inventory

The article discusses the development of a method for relating reactivity to crystallite size and strain parameters obtained by the Warren-Averbach technique. EPA has been using crystallite size and strain data obtained from x-ray diffraction (XRD) peak profile analysis to predic...

History and Solution of the Phase Problem in theTheory of Structure Determination of Crystals from X-ray Diffraction Experiments

ScienceCinema

Wolf, Emil [University of Rochester, Rochester, New York, United States

2017-12-09

Since the pioneering work of Max von Laue on interference and diffraction of x-rays, carried out almost 100 years ago, numerous attempts have been made to determine structures of crystalline media from x-ray diffraction experiments. The usefulness of all of them has been limited by the inability of measuring phases of the diffracted beams. In this talk, the most important research carried out in this field will be reviewed and a recently obtained solution of the phase problem will be presented.

Facile transformation of FeO/Fe3O4 core-shell nanocubes to Fe3O4 via magnetic stimulation

NASA Astrophysics Data System (ADS)

Lak, Aidin; Niculaes, Dina; Anyfantis, George C.; Bertoni, Giovanni; Barthel, Markus J.; Marras, Sergio; Cassani, Marco; Nitti, Simone; Athanassiou, Athanassia; Giannini, Cinzia; Pellegrino, Teresa

2016-09-01

Here, we propose the use of magnetic hyperthermia as a means to trigger the oxidation of Fe1-xO/Fe3-δO4 core-shell nanocubes to Fe3-δO4 phase. As a first relevant consequence, the specific absorption rate (SAR) of the initial core-shell nanocubes doubles after exposure to 25 cycles of alternating magnetic field stimulation. The improved SAR value was attributed to a gradual transformation of the Fe1-xO core to Fe3-δO4, as evidenced by structural analysis including high resolution electron microscopy and Rietveld analysis of X-ray diffraction patterns. The magnetically oxidized nanocubes, having large and coherent Fe3-δO4 domains, reveal high saturation magnetization and behave superparamagnetically at room temperature. In comparison, the treatment of the same starting core-shell nanocubes by commonly used thermal annealing process renders a transformation to γ-Fe2O3. In contrast to other thermal annealing processes, the method here presented has the advantage of promoting the oxidation at a macroscopic temperature below 37 °C. Using this soft oxidation process, we demonstrate that biotin-functionalized core-shell nanocubes can undergo a mild self-oxidation transformation without losing their functional molecular binding activity.

The study of ultrasonic irradiation effects on solid state powders of HTc superconductor YBa2Cu3O7-x

NASA Astrophysics Data System (ADS)

Kargar, Mahboubeh; Khoshnevisan, Bahram

2016-03-01

In this paper, an ultrasound assisted solid state synthesis method for high-temperature (HTc) YBa2Cu3O7-x (YBCO) superconductor nanostructures with different morphologies is presented. Here, the routine heat treatment of the powder mixture of as-prepared precursors is followed by the ultrasound irradiation inside various alcoholic solutions. Not only the influence of the ultrasound irradiation intensity and duration but also the influence of different solvents such as ethanol, methanol and 1-butanol with various vapor pressures and so various destruction powers were also studied on the morphology and particle size of the products. The various morphologies were studied by scanning electron microscope (SEM) which not only have been affected by intensity and type of alcoholic solvent but also sonication time and ultrasound power have significant role as well. Formation of the YBCO superconducting phase was examined by using Rietveld refinement of X-ray diffraction (XRD) which indicates the crystalline preferred growth in c-axis orientation in crystal. Magnetic susceptibility measurements showed the ultrasound waves had no important effect on the onset critical temperature of the prepared nanorods (about 91.64 K) which is compared with the bulk samples (Tc ˜ 92K).

Structural, transport and thermoelectric properties of Nb-doped CaLaMnO perovskite

NASA Astrophysics Data System (ADS)

Villa, J. I.; Rodríguez, J. E.

2014-12-01

Poly-crystalline perovskite-type (CaLaMnO) Ca0.95La0.05Mn1-xNbxO3 (0.0 ≤ x ≤ 0.10) was synthesized using the conventional solid-state reaction method. Structural and morphological properties were studied by X-ray diffraction analysis (XRD) and scanning electron microscopy (SEM), respectively. Their transport and thermoelectric properties were studied from electrical resistivity ρ(T) and Seebeck coefficient S(T) measurements as a function of temperature and niobium content. The Rietveld analysis revealed a compound with orthorhombic structure, where their lattice parameters increase with the niobium content which is given by a distortion in octahedra MnO6. Electrical resistivity exhibits a semiconducting-like behavior, for low niobium contents (Nb ≤ 0.03) the magnitude of the electrical resistivity decreases, reaching minimum values close to 0.1 Ω - cm. Seebeck coefficient is negative in all studied temperature range. The temperature behavior of S(T) is interpreted in terms of variable range hopping (VRH) and Heikes model. From ρ(T) and S(T) measurements it was possible to calculate the thermoelectric power factor (PF), which reaches maximum values around 0.4 μW /K2 -cm. These values make these ceramics promising electronic thermoelectric materials.

Modifications of the structure and magnetic properties of ceramic YCrO3 with Fe/Ni doping

NASA Astrophysics Data System (ADS)

Mall, Ashish Kumar; Garg, Ashish; Gupta, Rajeev

2017-07-01

In this manuscript, we have investigated the effect of Fe and Ni doping on the structure and magnetic properties of YCr1-x M x O3 ceramics (M  =  Fe, Ni and x  =  0, 0.1). X-ray diffraction analysis of the samples accompanied with, Rietveld refinement suggested no change in the structure upon doping, with structure of the samples being orthorhombic (space group: Pnma). Raman spectroscopic analysis of the samples revealed that doping induced disorder leads to broadening of the certain Raman modes of the system. While, both B 3g(5) and B 1g(3) modes are broadened in Ni and Fe doped samples, in addition Fe doped samples also show broadening of B 1g(4) mode. In doped samples a new mode, A 1g(3) appears due to the induced lattice disorder. Temperature dependent magnetic measurements suggested a negative value of Curie-Weiss temperature (θ cw) indicating that all the samples are antiferromagnetic. However, the Neel temperature (T N) increased for Fe doping and decreased with Ni doping. These changes in the Neel temperature upon doping can be correlated to the changes in the nearest neighbor and next nearest neighbor exchange interactions.

XRayView: a teaching aid for X-ray crystallography.

PubMed

Phillips, G N

1995-10-01

A software package, XRayView, has been developed that uses interactive computer graphics to introduce basic concepts of x-ray diffraction by crystals, including the reciprocal lattice, the Ewald sphere construction, Laue cones, the wavelength dependence of the reciprocal lattice, primitive and centered lattices and systematic extinctions, rotation photography. Laue photography, space group determination and Laue group symmetry, and the alignment of crystals by examination of reciprocal space. XRayView is designed with "user-friendliness" in mind, using pull-down menus to control the program. Many of the experiences of using real x-ray diffraction equipment to examine crystalline diffraction can be simulated. Exercises are available on-line to guide the users through many typical x-ray diffraction experiments.

Structure of β-AgGaO{sub 2}; ternary I–III–VI{sub 2} oxide semiconductor with a wurtzite-derived structure

DOE Office of Scientific and Technical Information (OSTI.GOV)

Nagatani, Hiraku; Suzuki, Issei; Kita, Masao

2015-02-15

The structure of the wurtzite-derived β-AgGaO{sub 2} was refined by Rietveld analysis of high-resolution powder diffraction data obtained using synchrotron X-ray radiation. The space group of the crystal is Pna2{sub 1} with lattice parameters of a{sub 0}=5.56175 Å, b{sub 0}=7.14749 Å, and c{sub 0}=5.46875 Å. The deviation of O–Ag–O and M–O–M bond angles from the regular tetrahedral angle of 109.5° was very large at ∼8° and ∼11°, respectively. The electronic structure of β-AgGaO{sub 2} is discussed based on its structure, and the indirect band gap of β-AgGaO{sub 2} was related to significant tetrahedral distortion. Although β-AgGaO{sub 2} decomposes into metallicmore » silver and Ga{sub 2}O{sub 3} at a high temperature in any atmosphere, β-AgGaO{sub 2} is stable up to 690 °C under an O{sub 2} atmosphere. No direct transformation from the wurtzite-derived phase to a delafossite phase occurs in β-AgGaO{sub 2}. - Graphical abstract: Crystal structure of β-AgGaO{sub 2} was refined by Rietveld analysis. AgO{sub 4} and O(Ag,Ga){sub 4} tetrahedra are significantly distorted from ideal tetrahedron. - Highlights: • Orthorhombic β-AgGaO{sub 2} with a wurtzite-derived β-NaFeO{sub 2} structure was synthesized. • Its structure was refined by Rietveld analysis of high-resolution XRD data. • Silver and oxygen tetrahedra are significantly distorted from an ideal tetrahedron. • The extent of this tetrahedral distortion is related to the band gap nature. • β-AgGaO{sub 2} is a metastable phase but is stable up to 690 °C in an O{sub 2} atmosphere.« less

Application of MEMS-based x-ray optics as tuneable nanosecond choppers

NASA Astrophysics Data System (ADS)

Chen, Pice; Walko, Donald A.; Jung, Il Woong; Li, Zhilong; Gao, Ya; Shenoy, Gopal K.; Lopez, Daniel; Wang, Jin

2017-08-01

Time-resolved synchrotron x-ray measurements often rely on using a mechanical chopper to isolate a set of x-ray pulses. We have started the development of micro electromechanical systems (MEMS)-based x-ray optics, as an alternate method to manipulate x-ray beams. In the application of x-ray pulse isolation, we recently achieved a pulse-picking time window of half a nanosecond, which is more than 100 times faster than mechanical choppers can achieve. The MEMS device consists of a comb-drive silicon micromirror, designed for efficiently diffracting an x-ray beam during oscillation. The MEMS devices were operated in Bragg geometry and their oscillation was synchronized to x-ray pulses, with a frequency matching subharmonics of the cycling frequency of x-ray pulses. The microscale structure of the silicon mirror in terms of the curvature and the quality of crystallinity ensures a narrow angular spread of the Bragg reflection. With the discussion of factors determining the diffractive time window, this report showed our approaches to narrow down the time window to half a nanosecond. The short diffractive time window will allow us to select single x-ray pulse out of a train of pulses from synchrotron radiation facilities.

Structural change in lead fluorapatite at high pressure

NASA Astrophysics Data System (ADS)

Fleet, Michael E.; Liu, Xi; Shieh, Sean R.

2010-01-01

The structure of lead fluorapatite [PbFAP; Pb10(PO4)6F2], crystallized from the melt in a platinum capsule at 1,000°C and 1 atm, has been investigated by single-crystal X-ray diffraction. Crystal data are a = 9.7638 (6), c = 7.2866 (4) Å, space group P63/ m, R = 0.043, R w = 0.034. We have also studied the compressional behaviour of the c-axis channel of PbFAP up to 9 GPa at 25°C, using a diamond-anvil cell, synchrotron X-radiation, and Rietveld powder structure refinement. Pressure-volume data for the channel polyhedron of PbFAP fitted to the third-order Birch-Murnaghan equation resulted in K T = 33.2 ± 1.2 GPa when K T ' is fixed at 4. The c-axis channel of PbFAP is about twice as compressible as the unit-cell volume of PbFAP and the channel of calcium apatites. This is attributed to the anomalous narrowing of the channel of PbFAP with increase in confining pressure. Flexibility of the apatite channel is a key factor in the scavenging of toxic heavy metals by calcium apatites.

Fabrication of high-resolution x-ray diffractive optics at King's College London

NASA Astrophysics Data System (ADS)

Charalambous, Pambos S.; Anastasi, Peter A. F.; Burge, Ronald E.; Popova, Katia

1995-09-01

The fabrication of high resolution x-ray diffractive optics, and Fresnel zone plates (ZPs) in particular, is a very demanding multifaceted technological task. The commissioning of more (and brighter) synchrotron radiation sources, has increased the number of x-ray imaging beam lines world wide. The availability of cheaper and more effective laboratory x-ray sources, has further increased the number of laboratories involved in x-ray imaging. The result is an ever increasing demand for x-ray optics with a very wide range of specifications, reflecting the particular type of x-ray imaging performed at different laboratories. We have been involved in all aspects of high resolution nanofabrication for a number of years, and we have explored many different methods of lithography, which, although unorthodox, open up possibilities, and increase our flexibility for the fabrication of different diffractive optical elements, as well as other types of nanostructures. The availability of brighter x-ray sources, means that the diffraction efficiency of the ZPs is becoming of secondary importance, a trend which will continue in the future. Resolution, however, is important and will always remain so. Resolution is directly related to the accuracy af pattern generation, as well as the ability to draw fine lines. This is the area towards which we have directed most of our efforts so far.

High-pressure structural behavior of hydrogarnet, katoite Ca3Al2(O4H4)3

NASA Astrophysics Data System (ADS)

Kyono, A.; Kato, M.; Sano-Furukawa, A.; Machida, S. I.; Hattori, T.

2016-12-01

High-pressure structural behavior of hydrogarnet, katoite Ca3Al2(O4H4)3, was investigated using single-crystal synchrotron x-ray diffraction, Raman spectroscopic, and neutron diffraction analyses. The high-pressure single-crystal synchrotron x-ray diffraction was performed at BL10A, Photon Factory, KEK, Japan. With compression, the a lattice parameter decreased continuously from 12.565 (1) Å to 12.226 (3) Å up to 7.1 GPa. A fit to the Birch-Murnaghan equation of state (EoS) based on the P-V data gives K0 = 56.0 (6) GPa, K' = 4.3 (1), and V0 = 1984.2 (5) Å3, which were consistent with the previous study by Lager et al. (2002). Weak reflections forbidden by the systematic absence of hk0 with k, l = 2n were observed at 5.5 GPa and their intensities became stronger as increasing pressure. The pattern change of systematic absence implies phase transformation from space group Ia-3d to its non-centrosymmetric space group I-43d. High-pressure Raman spectroscopic study was performed up to 8.3 GPa at room temperature. The pressure dependence of lattice modes showed a positive pressure shifts, whereas that of OH stretching vibration mode was changed negative above 5.1 GPa. The change indicates that the strength of hydrogen bonding turns to increase above 5.1 GPa. High-pressure and high-temperature neutron diffraction study was performed with six-axis large volume press, ATSUHIME, at BL11 (PLANET), J-PARC, Japan. At a pressure of approximately 8 GPa, the a lattice parameter increased with temperature, but neither thermal decomposition nor dehydroxylation process occurred up to 1123 K. The crystal structure of katoite was determined by Rietveld method using neutron diffraction data with the space group I-43d. The volume of dodecahedral site containing Ca cations and that of octahedral site occupied by Al cations remained almost constant with temperature, but two crystallographically inequivalent tetrahedral sites which were caused by phase transformation behaved differently from each other. The volume of T2 site was continuously increased, but that of T1 site was constantly decreased, resulting from anisotropic expansion of the dodecahedral site. Consequently, these anisotropic modifications of coordination polyhedra seem to induce the thermal decomposition of katoite at 1123 K and 8 GPa.

Curiosity Rover's CheMin Instrument Investigates Mineralogy of Gale Crater and Implications for Diagenesis

NASA Astrophysics Data System (ADS)

Fendrich, Kim; Rampe, Elizabeth; Vaniman, David; Bish, David; Blake, David; Treiman, Allan; Ming, Doug; Morris, Richard; Bristow, Tom; Cavanagh, Patrick; Downs, Robert; Morrison, Shaunna; Chipera, Steve; Achilles, Cherie; Farmer, Jack; Sarrazin, Philippe; Crisp, Joy; Morookian, John Michael; Yen, Albert; Gellert, Ralf

2015-04-01

The Mars Science Laboratory rover Curiosity employs a suite of instruments to investigate past or present habitability of Mars, as observed at Gale crater and particularly in the lower strata of the crater's central mound, informally named Mount Sharp. The X-ray diffractometer on board, CheMin, is used to assess the quantitative mineralogy of scooped soil samples and drilled rock powders. Methods of modeling diffraction peak positions and intensities to evaluate the abundances of minerals include Rietveld refinement and FULLPAT (full-pattern fitting). Each of the samples analyzed by CheMin contains X-ray amorphous material. The amorphous component chemistry is resolved by subtracting the chemistry of the crystalline composition, as determined by X-ray diffraction data, from the bulk sample chemistry, as determined by the Alpha Particle X-ray Spectrometer (APXS). Diffraction results have been obtained on five samples thus far to include Rocknest, John Klein, Cumberland, Windjana and Confidence Hills. Soil samples collected at Rocknest, an aeolian bedform in Gale crater, were the first to be analyzed in situ by CheMin. The Rocknest mineral assemblage is basaltic (plagioclase, Fe-forsterite, augite, pigeonite) and contains amorphous material that is compositionally similar to palagonitic volcanic soils found on Earth, with the addition of sulfur and chlorine. The four drill analyses are characteristic of deposition in a variety of fluvio-lacustrine environments and exhibit evidence of low-temperature diagenesis. Both John Klein and Cumberland are part of the Sheepbed mudstone at Yellowknife Bay, where the first drilled samples were acquired as well as the first evidence of a habitable environment on Mars. Drilled three meters apart from each other, the two samples reveal basaltic minerals similar to those at Rocknest, as well as phyllosilicates, Fe-oxides/hydroxides, Ca-sulfates, Fe-sulfides, and amorphous materials. The nature and hydration of interlayer cations within the phyllosilicates differs between the two samples, which implies localized diagenesis. The Windjana sandstone at the Kimberley location differs from the Sheepbed mudstone in that it contains more pyroxene and magnetite and abundant K-feldspar, as well as phyllosilicates and amorphous material. These phases may represent potassium-rich basaltic provenance or aqueous alteration by potassium-bearing fluids. While the Confidence Hills sample is still in the preliminary stages of evaluation, major crystalline phases observed in this fine-grained sedimentary rock include plagioclase, pyroxene, K-feldspar and phyllosilicates; hematite, rare in all previous samples, is notably abundant and jarosite is present. The findings suggest localized mobilization of iron-bearing fluids and acidic conditions. The more oxidized assemblage of Confidence Hills marks the transition into the lower strata of Mount Sharp.

Two-photon x-ray diffraction

DOE Office of Scientific and Technical Information (OSTI.GOV)

Stohr, J.

The interference pattern of a circular photon source has long been used to define the optical diffraction limit. Here we show the breakdown of conventional x-ray diffraction theory for the fundamental case of a “source”, consisting of a back-illuminated thin film in a circular aperture. When the conventional spontaneous x-ray scattering by atoms in the film is replaced at high incident intensity by stimulated resonant scattering, the film becomes the source of cloned photon twins and the diffraction pattern becomes self-focused beyond the diffraction limit. Furthermore, the case of cloned photon pairs is compared to and distinguished from entangled photonmore » pairs or biphotons.« less

Two-photon x-ray diffraction

DOE PAGES

Stohr, J.

2017-01-11

The interference pattern of a circular photon source has long been used to define the optical diffraction limit. Here we show the breakdown of conventional x-ray diffraction theory for the fundamental case of a “source”, consisting of a back-illuminated thin film in a circular aperture. When the conventional spontaneous x-ray scattering by atoms in the film is replaced at high incident intensity by stimulated resonant scattering, the film becomes the source of cloned photon twins and the diffraction pattern becomes self-focused beyond the diffraction limit. Furthermore, the case of cloned photon pairs is compared to and distinguished from entangled photonmore » pairs or biphotons.« less

Characterization of X80 and X100 Microalloyed Pipeline Steel Using Quantitative X-ray Diffraction

NASA Astrophysics Data System (ADS)

Wiskel, J. B.; Li, X.; Ivey, D. G.; Henein, H.

2018-06-01

Quantitative X-ray diffraction characterization of four (4) X80 and three (3) X100 microalloyed steels was undertaken. The effect of through-thickness position, processing parameters, and composition on the measured crystallite size, microstrain, and J index (relative magnitude of crystallographic texture) was determined. Microstructure analysis using optical microscopy, scanning electron microscopy, transmission electron microscopy, and electron-backscattered diffraction was also undertaken. The measured value of microstrain increased with increasing alloy content and decreasing cooling interrupt temperature. Microstructural features corresponding to crystallite size in the X80 steels were both above and below the detection limit for quantitative X-ray diffraction. The X100 steels consistently exhibited microstructure features below the crystallite size detection limit. The yield stress of each steel increased with increasing microstrain. The increase in microstrain from X80 to X100 is also associated with a change in microstructure from predominantly polygonal ferrite to bainitic ferrite.

Synthesis and structure of a stuffed derivative of α-quartz, Mg 0.5AlSiO 4

DOE PAGES

Xu, Hongwu; Heaney, Peter J.; Yu, Ping; ...

2015-10-01

A structural derivative of quartz with the composition Mg 0.5AlSiO 4 has been grown from glass and characterized using synchrotron X-ray diffraction (XRD), transmission electron microscopy (TEM), and 29Si nuclear magnetic resonance (NMR) spectroscopy. Rietveld analysis of the XRD data indicates that the framework of Mg 0.5AlSiO 4 is isostructural with α-quartz, rather than β-quartz, as is consistent with previous theoretical modeling (Sternitzke and Müller 1991). Al and Si exhibit long-range disorder over the framework tetrahedral sites, indicated by the absence of the superlattice reflections corresponding to the doubling of c relative to that of quartz. Nevertheless, 29Si NMR measurementsmore » show that Al and Si exhibit partial short-range order with an ordering degree of 56%. Electron diffraction reveals superlattice reflections indicative of doubled periodicities along the a-axes. In conclusion, Fourier electron density maps show that Mg occupies channel sites that each are bonded to six O atoms, in contrast to the tetrahedral coordination of Li in the β-quartz-type framework for β-eucryptite, LiAlSiO 4. Furthermore, the concentrations of Mg in adjacent channels are different, resulting in framework distortions that generate the superstructures along a.« less

Electric-field-induced structural changes in multilayer piezoelectric actuators during electrical and mechanical loading

DOE Office of Scientific and Technical Information (OSTI.GOV)

Esteves, Giovanni; Fancher, Chris M.; Röhrig, Sören

The effects of electrical and mechanical loading on the behavior of domains and phases in Multilayer Piezoelectric Actuators (MAs) is studied using in situ high-energy X-ray diffraction (XRD) and macroscopic property measurements. Rietveld refinement is carried out on measured diffraction patterns using a two-phase tetragonal (P4mm) and rhombohedral (R3m) model. Applying an electric field promotes the rhombohedral phase, while increasing compressive uniaxial pre-stress prior to electric field application favors the tetragonal phase. The competition between electrical and mechanical energy leads to a maximal difference between electric-field-induced phase fractions at 70 MPa pre-stress. Additionally, the available volume fraction of non-180° domainmore » reorientation that can be accessed during electric field application increases with compressive pre-stress up to 70 MPa. The origin for enhanced strain and polarization with applied pre-stress is attributed to a combination of enhanced non-180° domain reorientation and electric-field-induced phase transitions. The suppression of both the electric-field-induced phase transitions and domain reorientation at high pre-stresses (>70 MPa) is attributed to a large mechanical energy barrier, and alludes to the competition of the electrical and mechanical energy within the MA during applied stimuli.« less

Electric-field-induced structural changes in multilayer piezoelectric actuators during electrical and mechanical loading

DOE PAGES

Esteves, Giovanni; Fancher, Chris M.; Röhrig, Sören; ...

2017-04-08

The effects of electrical and mechanical loading on the behavior of domains and phases in Multilayer Piezoelectric Actuators (MAs) is studied using in situ high-energy X-ray diffraction (XRD) and macroscopic property measurements. Rietveld refinement is carried out on measured diffraction patterns using a two-phase tetragonal (P4mm) and rhombohedral (R3m) model. Applying an electric field promotes the rhombohedral phase, while increasing compressive uniaxial pre-stress prior to electric field application favors the tetragonal phase. The competition between electrical and mechanical energy leads to a maximal difference between electric-field-induced phase fractions at 70 MPa pre-stress. Additionally, the available volume fraction of non-180° domainmore » reorientation that can be accessed during electric field application increases with compressive pre-stress up to 70 MPa. The origin for enhanced strain and polarization with applied pre-stress is attributed to a combination of enhanced non-180° domain reorientation and electric-field-induced phase transitions. The suppression of both the electric-field-induced phase transitions and domain reorientation at high pre-stresses (>70 MPa) is attributed to a large mechanical energy barrier, and alludes to the competition of the electrical and mechanical energy within the MA during applied stimuli.« less

Diffractive-refractive optics: (+,-,-,+) X-ray crystal monochromator with harmonics separation.

PubMed

Hrdý, Jaromír; Mikulík, Petr; Oberta, Peter

2011-03-01

A new kind of two channel-cut crystals X-ray monochromator in dispersive (+,-,-,+) position which spatially separates harmonics is proposed. The diffracting surfaces are oriented so that the diffraction is inclined. Owing to refraction the diffracted beam is sagittally deviated. The deviation depends on wavelength and is much higher for the first harmonics than for higher harmonics. This leads to spatial harmonics separation. The idea is supported by ray-tracing simulation.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kondo, Shinichiro

The format of this dissertation is as follows. In the remainder of Chapter 1, brief introductions and reviews are given to the topics of frustration, heavy fermions and spinels including the precedent work of LiV 2O 4. In Chapter 2, as a general overview of this work the important publication in Physical Review Letters by the author of this dissertation and collaborators regarding the discovery of the heavy fermion behavior in LiV 2O 4 is introduced [removed for separate processing]. The preparation methods employed by the author for nine LiV 2O 4 and two Li 1+xTi 2-xO 4 (x =more » 0 and 1/3) polycrystalline samples are introduced in Chapter 3. The subsequent structural characterization of the LiV 2O 4 and Li 1+xT 2-xO 4 samples was done by the author using thermogravimetric analysis (TGA), x-ray diffraction measurements and their structural refinements by the Rietveld analysis. The results of the characterization are detailed in Chapter 3. In Chapter 4 magnetization measurements carried out by the author are detailed. In Chapter 5, after briefly discussing the resistivity measurement results including the single-crystal work by Rogers et al., for the purpose of clear characterization of LiV 2O 4 it is of great importance to introduce in the following chapters the experiments and subsequent data analyses done by his collaborators. Heat capacity measurements (Chapter 6) were carried out and analyzed by Dr. C.A. Swenson, and modeled theoretically by Dr. D.C. Johnston. In Chapter 7 a thermal expansion study using neutron diffraction by Dr. O. Chmaissem et al. and capacitance dilatometry measurements by Dr. C.A. Swenson are introduced. The data analyses for the thermal expansion study were mainly done by Dr. O. Chmaissem (for neutron diffraction) and Dr. C.A. Swendon (for dilatometry), with assistances by Dr. J.D. Jorgensen, Dr. D.C. Johnston, and S. Kondo the author of this dissertation. Chapter 8 describes nuclear magnetic resonance (NMR) measurements and analyses by Dr. A.V. Mahajan, R. Sala, E. Lee and Dr. F. Borsa. In the final chapter, a summary and discussion are given.« less

Room Temperature Elastic Moduli and Vickers Hardness of Hot-Pressed LLZO Cubic Garnet

DTIC Science & Technology

2012-01-01

polishing compounds, Leco, St. Joseph, MI). X - ray diffraction and scanning electron microscopy (SEM) The microstructure of the hot-pressed specimens...was examined on uncoated fracture surfaces by SEM with an accelerating voltage of 1 and 3 kV. Phase purity was evaluated from X - ray diffraction data...the micro- structure appeared to be homogenous for the two hot- pressed LLZO specimens included in this study (Fig. 1). X - ray diffraction confirmed that

Local symmetry breaking in SnO2 nanocrystals with cobalt doping and its effect on optical properties.

PubMed

Roy, S; Joshi, Amish G; Chatterjee, S; Ghosh, Anup K

2018-06-07

X-ray photoemission spectroscopy (XPS), X-ray diffraction (XRD) and transmission electron microscopy (TEM) have been used to study the structural and morphological characteristics of cobalt doped tin(iv) oxide (Sn1-xCoxO2; 0 ≤ x ≤ 0.04) nanocrystals synthesized by a chemical co-precipitation technique. Electronic structure analysis using X-ray photoemission spectroscopy (XPS) shows the formation of tin interstitials (Sni) and reduction of oxygen vacancies (VO) in the host lattice on Co doping and that the doped Co exists in mixed valence states of +2 and +3. Using XRD, the preferential position of the Sni and doped Co in the unit cell of the nanocrystals have been estimated. Rietveld refinement of XRD data shows that samples are of single phase and variation of lattice constants follows Vegard's law. XRD and TEM measurements show that the crystallite size of the nanocrystals decrease with increase in Co doping concentration. SAED patterns confirm the monocrystalline nature of the samples. The study of the lattice dynamics using Raman spectroscopy and Fourier transform infrared (FTIR) spectroscopy shows the existence of many disorder activated forbidden optical phonon modes, along with the corresponding classical modes, signifying Co induced local symmetry breaking in the nanocrystals. UV-Vis spectroscopy shows that the optical band gap has red shifted with increase in doping concentration. The study of Urbach energy confirms the increase in disorder in the nanocrystals with Co doping. Local symmetry breaking induced UV emission along with violet, blue and green luminescence has been observed from the PL study. The spectral contribution of UV emission decreases and green luminescence increases with increase in doping. Using PL, in conjunction with Raman spectroscopy, the type of oxygen vacancy induced in the nanocrystals on Co doping has been confirmed and the position of the defect levels in the forbidden zone (w.r.t. the optical band gap) has been studied.

Method for improve x-ray diffraction determinations of residual stress in nickel-base alloys

DOEpatents

Berman, Robert M.; Cohen, Isadore

1990-01-01

A process for improving the technique of measuring residual stress by x-ray diffraction in pieces of nickel-base alloys which comprises covering part of a predetermined area of the surface of a nickel-base alloy with a dispersion, exposing the covered and uncovered portions of the surface of the alloy to x-rays by way of an x-ray diffractometry apparatus, making x-ray diffraction determinations of the exposed surface, and measuring the residual stress in the alloy based on these determinations. The dispersion is opaque to x-rays and serves a dual purpose since it masks off unsatisfactory signals such that only a small portion of the surface is measured, and it supplies an internal standard by providing diffractogram peaks comparable to the peaks of the nickel alloy so that the alloy peaks can be very accurately located regardless of any sources of error external to the sample.

Crystal structure and density of helium to 232 kbar

NASA Technical Reports Server (NTRS)

Mao, H. K.; Wu, Y.; Jephcoat, A. P.; Hemley, R. J.; Bell, P. M.; Bassett, W. A.

1988-01-01

The properties of helium and hydrogen at high pressure are topics of great interest to the understanding of planetary interiors. These materials constitute 95 percent of the entire solar system. A technique was presented for the measurement of X-ray diffraction from single-crystals of low-Z condenses gases in a diamond-anvil cell at high pressure. The first such single-crystal X-ray diffraction measurements on solid hydrogen to 26.5 GPa were presented. The application of this technique to the problem of the crystal structure, equation of state, and phase diagram of solid helium is reported. Crucial for X-ray diffraction studies of these materials is the use of a synchrotron radiation source which provides high brillance, narrow collimation of the incident and diffracted X-ray beams to reduce the background noise, and energy-dispersive diffraction techniques with polychromatic (white) radiation, which provides high detection efficiency.

Addressing the amorphous content issue in quantitative phase analysis : the certification of NIST SRM 676a.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Cline, J. P.; Von Dreele, R. B.; Winburn, R.

2011-07-01

A non-diffracting surface layer exists at any boundary of a crystal and can comprise a mass fraction of several percent in a finely divided solid. This has led to the long-standing issue of amorphous content in standards for quantitative phase analysis (QPA). NIST standard reference material (SRM) 676a is a corundum ({alpha}-Al{sub 2}O{sub 3}) powder, certified with respect to phase purity for use as an internal standard in powder diffraction QPA. The amorphous content of SRM 676a is determined by comparing diffraction data from mixtures with samples of silicon powders that were engineered to vary their specific surface area. Undermore » the (supported) assumption that the thickness of an amorphous surface layer on Si was invariant, this provided a method to control the crystalline/amorphous ratio of the silicon components of 50/50 weight mixtures of SRM 676a with silicon. Powder diffraction experiments utilizing neutron time-of-flight and 25 keV and 67 keV X-ray energies quantified the crystalline phase fractions from a series of specimens. Results from Rietveld analyses, which included a model for extinction effects in the silicon, of these data were extrapolated to the limit of zero amorphous content of the Si powder. The certified phase purity of SRM 676a is 99.02% {+-} 1.11% (95% confidence interval). This novel certification method permits quantification of amorphous content for any sample of interest, by spiking with SRM 676a.« less

Addressing the Amorphous Content Issue in Quantitative Phase Analysis: The Certification of NIST Standard Reference Material 676a

DOE Office of Scientific and Technical Information (OSTI.GOV)

J Cline; R Von Dreele; R Winburn

2011-12-31

A non-diffracting surface layer exists at any boundary of a crystal and can comprise a mass fraction of several percent in a finely divided solid. This has led to the long-standing issue of amorphous content in standards for quantitative phase analysis (QPA). NIST standard reference material (SRM) 676a is a corundum ({alpha}-Al{sub 2}O{sub 3}) powder, certified with respect to phase purity for use as an internal standard in powder diffraction QPA. The amorphous content of SRM 676a is determined by comparing diffraction data from mixtures with samples of silicon powders that were engineered to vary their specific surface area. Undermore » the (supported) assumption that the thickness of an amorphous surface layer on Si was invariant, this provided a method to control the crystalline/amorphous ratio of the silicon components of 50/50 weight mixtures of SRM 676a with silicon. Powder diffraction experiments utilizing neutron time-of-flight and 25 keV and 67 keV X-ray energies quantified the crystalline phase fractions from a series of specimens. Results from Rietveld analyses, which included a model for extinction effects in the silicon, of these data were extrapolated to the limit of zero amorphous content of the Si powder. The certified phase purity of SRM 676a is 99.02% {+-} 1.11% (95% confidence interval). This novel certification method permits quantification of amorphous content for any sample of interest, by spiking with SRM 676a.« less

Structural investigation of porcine stomach mucin by X-ray fiber diffraction and homology modeling

DOE Office of Scientific and Technical Information (OSTI.GOV)

Veluraja, K., E-mail: veluraja@msuniv.ac.in; Vennila, K.N.; Umamakeshvari, K.

Research highlights: {yields} Techniques to get oriented mucin fibre. {yields} X-ray fibre diffraction pattern for mucin. {yields} Molecular modeling of mucin based on X-ray fibre diffraction pattern. -- Abstract: The basic understanding of the three dimensional structure of mucin is essential to understand its physiological function. Technology has been developed to achieve orientated porcine stomach mucin molecules. X-ray fiber diffraction of partially orientated porcine stomach mucin molecules show d-spacing signals at 2.99, 4.06, 4.22, 4.7, 5.37 and 6.5 A. The high intense d-spacing signal at 4.22 A is attributed to the antiparallel {beta}-sheet structure identified in the fraction of themore » homology modeled mucin molecule (amino acid residues 800-980) using Nidogen-Laminin complex structure as a template. The X-ray fiber diffraction signal at 6.5 A reveals partial organization of oligosaccharides in porcine stomach mucin. This partial structure of mucin will be helpful in establishing a three dimensional structure for the whole mucin molecule.« less

A nearly on-axis spectroscopic system for simultaneously measuring UV-visible absorption and X-ray diffraction in the SPring-8 structural genomics beamline.

PubMed

Sakaguchi, Miyuki; Kimura, Tetsunari; Nishida, Takuma; Tosha, Takehiko; Sugimoto, Hiroshi; Yamaguchi, Yoshihiro; Yanagisawa, Sachiko; Ueno, Go; Murakami, Hironori; Ago, Hideo; Yamamoto, Masaki; Ogura, Takashi; Shiro, Yoshitsugu; Kubo, Minoru

2016-01-01

UV-visible absorption spectroscopy is useful for probing the electronic and structural changes of protein active sites, and thus the on-line combination of X-ray diffraction and spectroscopic analysis is increasingly being applied. Herein, a novel absorption spectrometer was developed at SPring-8 BL26B2 with a nearly on-axis geometry between the X-ray and optical axes. A small prism mirror was placed near the X-ray beamstop to pass the light only 2° off the X-ray beam, enabling spectroscopic analysis of the X-ray-exposed volume of a crystal during X-ray diffraction data collection. The spectrometer was applied to NO reductase, a heme enzyme that catalyzes NO reduction to N2O. Radiation damage to the heme was monitored in real time during X-ray irradiation by evaluating the absorption spectral changes. Moreover, NO binding to the heme was probed via caged NO photolysis with UV light, demonstrating the extended capability of the spectrometer for intermediate analysis.

Investigating the Effects of Low Temperature Annealing of Amorphous Corrosion Resistant Alloys.

DTIC Science & Technology

1980-11-01

Ray Diffraction.................................................... 6 Differential Scanning Calorimetry....................................... 9...17 LIST OF FIGURES Figure 1. X- Ray Diffraction Results From Fe32Ni 36Cr 4P 2 B Annealed for One Hour at...Various Temperatures (Cr Ka Radiation) ................................. 7 Figure 2. X- Ray Diffraction Results From FeU2NiaeCr14SieB Annealed for One

Evidence from x-ray and neutron powder diffraction patterns that the so-called icosahedral and decagonal quasicrystals of MnAl(6) and other alloys are twinned cubic crystals.

PubMed

Pauling, L

1987-06-01

It is shown that the x-ray powder diffraction patterns of rapidly quenched MnAl(6) and Mg(32)(Al,Zn)(49) and the neutron powder diffraction pattern of MnAl(6) are compatible with the proposed 820-atom primitive cubic structure [Pauling, L. (1987) Phys. Rev. Lett. 58, 365-368]. The values found for the edge of the unit cube are 23.365 A (x-ray) and 23.416 A (neutron) for MnAl(6) and 24.313 A (x-ray) for Mg(32)(Al,Zn)(49).

Evidence from x-ray and neutron powder diffraction patterns that the so-called icosahedral and decagonal quasicrystals of MnAl6 and other alloys are twinned cubic crystals

PubMed Central

Pauling, Linus

1987-01-01

It is shown that the x-ray powder diffraction patterns of rapidly quenched MnAl6 and Mg32(Al,Zn)49 and the neutron powder diffraction pattern of MnAl6 are compatible with the proposed 820-atom primitive cubic structure [Pauling, L. (1987) Phys. Rev. Lett. 58, 365-368]. The values found for the edge of the unit cube are 23.365 Å (x-ray) and 23.416 Å (neutron) for MnAl6 and 24.313 Å (x-ray) for Mg32(Al,Zn)49. PMID:16593841

High-energy X-ray diffraction using the Pixium 4700 flat-panel detector.

PubMed

Daniels, J E; Drakopoulos, M

2009-07-01

The Pixium 4700 detector represents a significant step forward in detector technology for high-energy X-ray diffraction. The detector design is based on digital flat-panel technology, combining an amorphous Si panel with a CsI scintillator. The detector has a useful pixel array of 1910 x 2480 pixels with a pixel size of 154 microm x 154 microm, and thus it covers an effective area of 294 mm x 379 mm. Designed for medical imaging, the detector has good efficiency at high X-ray energies. Furthermore, it is capable of acquiring sequences of images at 7.5 frames per second in full image mode, and up to 60 frames per second in binned region of interest modes. Here, the basic properties of this detector applied to high-energy X-ray diffraction are presented. Quantitative comparisons with a widespread high-energy detector, the MAR345 image plate scanner, are shown. Other properties of the Pixium 4700 detector, including a narrow point-spread function and distortion-free image, allows for the acquisition of high-quality diffraction data at high X-ray energies. In addition, high frame rates and shutterless operation open new experimental possibilities. Also provided are the necessary data for the correction of images collected using the Pixium 4700 for diffraction purposes.

On the Use of Dynamical Diffraction Theory To Refine Crystal Structure from Electron Diffraction Data: Application to KLa5O5(VO4)2, a Material with Promising Luminescent Properties.

PubMed

Colmont, Marie; Palatinus, Lukas; Huvé, Marielle; Kabbour, Houria; Saitzek, Sébastien; Djelal, Nora; Roussel, Pascal

2016-03-07

A new lanthanum oxide, KLa5O5(VO4)2, was synthesized using a flux growth technique that involved solid-state reaction under an air atmosphere at 900 °C. The crystal structure was solved and refined using an innovative approach recently established and based on three-dimensional (3D) electron diffraction data, using precession of the electron beam and then validated against Rietveld refinement and denisty functional theory (DFT) calculations. It crystallizes in a monoclinic unit cell with space group C2/m and has unit cell parameters of a = 20.2282(14) Å, b = 5.8639(4) Å, c = 12.6060(9) Å, and β = 117.64(1)°. Its structure is built on Cresnel-like two-dimensional (2D) units (La5O5) of 4*3 (OLa4) tetrahedra, which run parallel to (001) plane, being surrounded by isolated VO4 tetrahedra. Four isolated vanadate groups create channels that host K(+) ions. Substitution of K(+) cations by another alkali metal is possible, going from lithium to rubidium. Li substitution led to a similar phase with a primitive monoclinic unit cell. A complementary selected area electron diffraction (SAED) study highlighted diffuse streaks associated with stacking faults observed on high-resolution electron microscopy (HREM) images of the lithium compound. Finally, preliminary catalytic tests for ethanol oxidation are reported, as well as luminescence evidence. This paper also describes how solid-state chemists can take advantages of recent progresses in electron crystallography, assisted by DFT calculations and powder X-ray diffraction (PXRD) refinements, to propose new structural types with potential applications to the physicist community.

Crystallization and preliminary X-ray diffraction analysis of a chitin-binding domain of hyperthermophilic chitinase from Pyrococcus furiosus

DOE Office of Scientific and Technical Information (OSTI.GOV)

Nakamura, Tsutomu; Ishikawa, Kazuhiko; Hagihara, Yoshihisa

The expression, purification and preliminary X-ray diffraction studies of a chitin-binding domain of the chitinase from P. furiosus are reported. The crystallization and preliminary X-ray diffraction analysis of the chitin-binding domain of chitinase from a hyperthermophilic archaeon, Pyrococcus furiosus, are reported. The recombinant protein was prepared using an Escherichia coli overexpression system and was crystallized by the hanging-drop vapour-diffusion method. An X-ray diffraction data set was collected to 1.70 Å resolution. The crystal belonged to space group P4{sub 3}2{sub 1}2 or P4{sub 1}2{sub 1}2. The unit-cell parameters were determined to be a = b = 48.8, c = 85.0 Å.

Long-Wavelength X-Ray Diffraction and Its Applications in Macromolecular Crystallography.

PubMed

Weiss, Manfred S

2017-01-01

For many years, diffraction experiments in macromolecular crystallography at X-ray wavelengths longer than that of Cu-K α (1.54 Å) have been largely underappreciated. Effects caused by increased X-ray absorption result in the fact that these experiments are more difficult than the standard diffraction experiments at short wavelengths. However, due to the also increased anomalous scattering of many biologically relevant atoms, important additional structural information can be obtained. This information, in turn, can be used for phase determination, for substructure identification, in molecular replacement approaches, as well as in structure refinement. This chapter reviews the possibilities and the difficulties associated with such experiments, and it provides a short description of two macromolecular crystallography synchrotron beam lines dedicated to long-wavelength X-ray diffraction experiments.

Data processing software suite SITENNO for coherent X-ray diffraction imaging using the X-ray free-electron laser SACLA.

PubMed

Sekiguchi, Yuki; Oroguchi, Tomotaka; Takayama, Yuki; Nakasako, Masayoshi

2014-05-01

Coherent X-ray diffraction imaging is a promising technique for visualizing the structures of non-crystalline particles with dimensions of micrometers to sub-micrometers. Recently, X-ray free-electron laser sources have enabled efficient experiments in the `diffraction before destruction' scheme. Diffraction experiments have been conducted at SPring-8 Angstrom Compact free-electron LAser (SACLA) using the custom-made diffraction apparatus KOTOBUKI-1 and two multiport CCD detectors. In the experiments, ten thousands of single-shot diffraction patterns can be collected within several hours. Then, diffraction patterns with significant levels of intensity suitable for structural analysis must be found, direct-beam positions in diffraction patterns determined, diffraction patterns from the two CCD detectors merged, and phase-retrieval calculations for structural analyses performed. A software suite named SITENNO has been developed to semi-automatically apply the four-step processing to a huge number of diffraction data. Here, details of the algorithm used in the suite are described and the performance for approximately 9000 diffraction patterns collected from cuboid-shaped copper oxide particles reported. Using the SITENNO suite, it is possible to conduct experiments with data processing immediately after the data collection, and to characterize the size distribution and internal structures of the non-crystalline particles.

Data processing software suite SITENNO for coherent X-ray diffraction imaging using the X-ray free-electron laser SACLA

PubMed Central

Sekiguchi, Yuki; Oroguchi, Tomotaka; Takayama, Yuki; Nakasako, Masayoshi

2014-01-01

Coherent X-ray diffraction imaging is a promising technique for visualizing the structures of non-crystalline particles with dimensions of micrometers to sub-micrometers. Recently, X-ray free-electron laser sources have enabled efficient experiments in the ‘diffraction before destruction’ scheme. Diffraction experiments have been conducted at SPring-8 Angstrom Compact free-electron LAser (SACLA) using the custom-made diffraction apparatus KOTOBUKI-1 and two multiport CCD detectors. In the experiments, ten thousands of single-shot diffraction patterns can be collected within several hours. Then, diffraction patterns with significant levels of intensity suitable for structural analysis must be found, direct-beam positions in diffraction patterns determined, diffraction patterns from the two CCD detectors merged, and phase-retrieval calculations for structural analyses performed. A software suite named SITENNO has been developed to semi-automatically apply the four-step processing to a huge number of diffraction data. Here, details of the algorithm used in the suite are described and the performance for approximately 9000 diffraction patterns collected from cuboid-shaped copper oxide particles reported. Using the SITENNO suite, it is possible to conduct experiments with data processing immediately after the data collection, and to characterize the size distribution and internal structures of the non-crystalline particles. PMID:24763651

Fast synthesis of La-substituted apatite by the dry mechanochemical method and analysis of its structure

NASA Astrophysics Data System (ADS)

Bulina, Natalia V.; Chaikina, Marina V.; Prosanov, Igor Yu.; Dudina, Dina V.; Solovyov, Leonid A.

2017-08-01

Compared to pure apatite, La-substituted apatites have improved thermal, mechanical and biological characteristics. In this article, a fast synthesis of La-substituted apatites by a dry mechanochemical method is presented. Structural studies by X-ray diffraction and Fourier transform infrared spectroscopy indicated the formation of a single-phase nanosized product after 30 min of high-energy ball milling of the reaction mixtures. The dry mechanochemical method is technologically attractive for the preparation of La-substituted apatites, as it allows reducing the processing time down to half an hour and does not require prolonged high-temperature annealing normally used in the synthesis practice of the substituted apatite. As the mechanochemically synthesized samples are nanosized, it is difficult to determine the details of their crystal structure by the Rietveld refinement method. Therefore, a series of the mechanochemically synthesized samples with different concentrations of lanthanum were annealed at 1000°C for 5 h. It was found that the annealed powders are microcrystalline La-substituted apatites Ca10-xLax(PO4)6Ox(OH)2-x, where 0 ≤ x ≤2. In their structure, the Ca2+ ions are replaced by the La3+ ions localized near the Ca2 sites, and the OH- groups are replaced by the O2- ions in the hexagonal channels.

Study on Dy0.45Ba0.05Sr0.5Co0.8Fe0.2O3-δ-Ce0.85Gd0.15O1.95 composite cathode material for intermediate temperature solid oxide fuel cell

NASA Astrophysics Data System (ADS)

Kautkar, Pranay R.; Acharya, Smita A.

2018-05-01

xDy0.45Ba0.05Sr0.5Co0.8Fe0.2O3-δ - xCe0.85Gd0.15O1.95 (x = 50 %) composite cathode supported on Ce0.85Gd0.15O1.95 (GDC15) electrolyte are studied for applications in IT-SOFCs. Results attribute that Dy0.45Ba0.05Sr0.5Co0.8Fe0.2O3-δ material is chemically compatible with Ce0.85Gd0.15O1.95 (GDC15). Rietveld refined X-ray diffraction patterns notify orthorhombic (space group:Pbnm) symmetry for Dy0.45 Ba0.05Sr0.5Co0.8Fe0.2O3-δ and fluorite type structure (space group: Fm-3m) symmetry for GDC15. The polarization resistance (Rp) of composite cathode reduces to the minimum value of 1.35 Ω cm2 at 650 °C in air. Area specific resistance (ASR) of composite cathode has found 0.67 Ω.cm2 at 650°C respectively. Result shows that the surface diffusion of the dissociative adsorbed oxygen at electrode/electrolyte interface on the composite cathode.