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.

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).

Molten Salt Synthesis and Structural Characterization of BaTiO3 Nanocrystal Ceramics

NASA Astrophysics Data System (ADS)

Ahda, S.; Misfadhila, S.; Parikin, P.; Putra, T. Y. S. P.

2017-02-01

A new synthesis route to obtain high-purity barium titanate powder, BaTiO3, using the molten salt method by reacting the raw materials (BaCO3 and TiO2) in an atmosphere of molten NaCl and KCl, has been developed. The synthesized BaTiO3 ceramic particles have been successfully carried out at the sintering temperature 950°C for 4 hours. The Rietveld refinement of the XRD diffraction patterns was employed to characterize the structural information of the nanocrystalline BaTiO3 ceramics. The lattice parameters (a=4.0043 Å, b=4.0308Å with space group P4mm) of tetragonal perovskite structure, as an indication of piezoelectric characteristics, have been successfully determined by the Rietveld refinement. While the crystallitte particle size and strains have been obtained for the values of 110.6 nm and 0.74 % respectively

The embodied brain: towards a radical embodied cognitive neuroscience

PubMed Central

Kiverstein, Julian; Miller, Mark

2015-01-01

In this programmatic paper we explain why a radical embodied cognitive neuroscience is needed. We argue for such a claim based on problems that have arisen in cognitive neuroscience for the project of localizing function to specific brain structures. The problems come from research concerned with functional and structural connectivity that strongly suggests that the function a brain region serves is dynamic, and changes over time. We argue that in order to determine the function of a specific brain area, neuroscientists need to zoom out and look at the larger organism-environment system. We therefore argue that instead of looking to cognitive psychology for an analysis of psychological functions, cognitive neuroscience should look to an ecological dynamical psychology. A second aim of our paper is to develop an account of embodied cognition based on the inseparability of cognitive and emotional processing in the brain. We argue that emotions are best understood in terms of action readiness (Frijda, 1986, 2007) in the context of the organism’s ongoing skillful engagement with the environment (Rietveld, 2008; Bruineberg and Rietveld, 2014; Kiverstein and Rietveld, 2015, forthcoming). States of action readiness involve the whole living body of the organism, and are elicited by possibilities for action in the environment that matter to the organism. Since emotion and cognition are inseparable processes in the brain it follows that what is true of emotion is also true of cognition. Cognitive processes are likewise processes taking place in the whole living body of an organism as it engages with relevant possibilities for action. PMID:25999836

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.

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.

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

X-ray Diffraction and Rietveld Refinement in Deferrified Clays for Forensic Science.

PubMed

Prandel, Luis V; Melo, Vander de F; Brinatti, André M; Saab, Sérgio da C; Salvador, Fábio A S

2018-01-01

Soil vestiges might provide information about a crime scene. The Rietveld method with X-ray diffraction data (RM-XRD) is a nondestructive technique that makes it possible to characterize minerals present in the soils. Soil clays from the metropolitan region of Curitiba (Brazil) were submitted to DCB treatment and analyzed using XRD with CuK α radiation in the step-scan mode (0.02° 2θ/5 s). The GSAS+EXPGUI software was used for RM refinement. The RM-XRD results, together with the principal component analysis (PCA) (52.6% total variance), showed the kaolinite predominance in most analyzed samples and the highest quartz contents in "site 1." Higher anatase, and gibbsite and muscovite contents influenced discrimination, mainly in "site 3" and "site 1," respectively. These results were enough to discriminate clays of four sites and two horizons using a reduced amount of sample showing that the technique can be applied to the investigation into soil vestiges. © 2017 American Academy of Forensic Sciences.

ZrO2:Sm3+ nanophosphor: synthesis, Rietveld refinement, optical and thermoluminescent properties

NASA Astrophysics Data System (ADS)

Ponkumar, S.; Janaki, K.; Prakashbabu, D.; Ramalingam, H. B.; Munirathnam, K.; Sreekanth, T. V. M.; Dhoble, S. J.

2018-02-01

We have synthesized undoped and Sm3+ ions doped ZrO2 nanophosphors by solution combustion method. These nanophosphors crystallized in cubic structure. Rietveld refinement of the samples was performed to estimate lattice parameters. Spherical particles with the sizes of 10-25 nm were observed by transmission electron microscopy. Photoluminescence and thermoluminescence (TL) properties of samples were investigated. Under 400 nm excitation, the nanophosphors have intense red emission at 600 nm. The color coordinates (0.67, 0.33) were located in the red region of CIE diagram. TL properties of nanophosphors were studied by exposing the samples to γ-rays. 5 mol% Sm3+ doped ZrO2 nanophosphor has shown maximum TL intensity after γ-irradiation. To test suitability of the nanophosphors for practical application in dosimetry, the 5 mol% Sm3+ doped ZrO2 sample was irradiated by 14 MeV electron beam in various electron fluence ranging from 100 to 900 Gy and their TL response was recorded.

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

Synchrotron Powder X-ray Diffraction Study of the Structure and Dehydration Behavior of Sepiolite

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

Post,J.; Bish, D.; Heaney, P.

2007-01-01

Rietveld refinements using synchrotron powder X-ray diffraction data were used to study the crystal structure and dehydration behavior of sepiolite from Durango, Mexico. The room-temperature (RT) sepiolite structure in air compares well with previous models but reveals an additional zeolitic H{sub 2}O site. The RT structure under vacuum retained only {approx}1/8 of the zeolitic H{sub 2}O and the volume decreased by 1.3%. Real-time, temperature-resolved synchrotron powder X-ray diffraction data and Rietveld refinements were used to investigate the behavior of the sepiolite structure from 300 to 925 K. Rietveld refinements revealed that most of the zeolitic H{sub 2}O is lost bymore » {approx}390 K, accompanied by a decrease in the a and c unit-cell parameters. Above {approx}600 K the sepiolite structure folds as one-half of the crystallographically bound H{sub 2}O is lost. Rietveld refinements of the 'anhydrous' sepiolite structure reveal that, in general, unit-cell parameters a and b and volume steadily decrease with increasing temperature; there is an obvious change in slope at {approx}820 K suggesting a phase transformation coinciding with the loss of the remaining bound H{sub 2}O molecule.« less

On the possibility of using polycrystalline material in the development of structure-based generic assays

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

Allaire, Marc, E-mail: allaire@bnl.gov; Moiseeva, Natalia; Botez, Cristian E.

The correlation coefficients calculated between raw powder diffraction profiles can be used to identify ligand-bound/unbound states of lysozyme. The discovery of ligands that bind specifically to a targeted protein benefits from the development of generic assays for high-throughput screening of a library of chemicals. Protein powder diffraction (PPD) has been proposed as a potential method for use as a structure-based assay for high-throughput screening applications. Building on this effort, powder samples of bound/unbound states of soluble hen-egg white lysozyme precipitated with sodium chloride were compared. The correlation coefficients calculated between the raw diffraction profiles were consistent with the known bindingmore » properties of the ligands and suggested that the PPD approach can be used even prior to a full description using stereochemically restrained Rietveld refinement.« less

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

Accuracy in Rietveld quantitative phase analysis: a comparative study of strictly monochromatic Mo and Cu radiations.

PubMed

León-Reina, L; García-Maté, M; Álvarez-Pinazo, G; Santacruz, I; Vallcorba, O; De la Torre, A G; Aranda, M A G

2016-06-01

This study reports 78 Rietveld quantitative phase analyses using Cu  K α 1 , Mo  K α 1 and synchrotron radiations. Synchrotron powder diffraction has been used to validate the most challenging analyses. From the results for three series with increasing contents of an analyte (an inorganic crystalline phase, an organic crystalline phase and a glass), it is inferred that Rietveld analyses from high-energy Mo  K α 1 radiation have slightly better accuracies than those obtained from Cu  K α 1 radiation. This behaviour has been established from the results of the calibration graphics obtained through the spiking method and also from Kullback-Leibler distance statistic studies. This outcome is explained, in spite of the lower diffraction power for Mo radiation when compared to Cu radiation, as arising because of the larger volume tested with Mo and also because higher energy allows one to record patterns with fewer systematic errors. The limit of detection (LoD) and limit of quantification (LoQ) have also been established for the studied series. For similar recording times, the LoDs in Cu patterns, ∼0.2 wt%, are slightly lower than those derived from Mo patterns, ∼0.3 wt%. The LoQ for a well crystallized inorganic phase using laboratory powder diffraction was established to be close to 0.10 wt% in stable fits with good precision. However, the accuracy of these analyses was poor with relative errors near to 100%. Only contents higher than 1.0 wt% yielded analyses with relative errors lower than 20%.

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

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.;

Rietveld analysis of X-ray powder diffraction patterns as a potential tool for the identification of impact-deformed carbonate rocks

NASA Astrophysics Data System (ADS)

Huson, S. A.; Foit, F. F.; Watkinson, A. J.; Pope, M. C.

2009-12-01

Previous X-ray powder diffraction (XRD) studies revealed that shock deformed carbonates and quartz have broader XRD patterns than those of unshocked samples. Entire XRD patterns, single peak profiles and Rietveld refined parameters of carbonate samples from the Sierra Madera impact crater, west Texas, unshocked equivalent samples from 95 miles north of the crater and the Mission Canyon Formation of southwest Montana and western Wyoming were used to evaluate the use of X-ray powder diffraction as a potential tool for distinguishing impact deformed rocks from unshocked and tectonically deformed rocks. At Sierra Madera dolostone and limestone samples were collected from the crater rim (lower shock intensity) and the central uplift (higher shock intensity). Unshocked equivalent dolostone samples were collected from well cores drilled outside of the impact crater. Carbonate rocks of the Mission Canyon Formation were sampled along a transect across the tectonic front of the Sevier and Laramide orogenic belts. Whereas calcite subjected to significant shock intensities at the Sierra Madera impact crater can be differentiated from tectonically deformed calcite from the Mission Canyon Formation using Rietveld refined peak profiles, weakly shocked calcite from the crater rim appears to be indistinguishable from the tectonically deformed calcite. In contrast, Rietveld analysis readily distinguishes shocked Sierra Madera dolomite from unshocked equivalent dolostone samples from outside the crater and tectonically deformed Mission Canyon Formation dolomite.

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

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.

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

Rietveld analysis of the cubic crystal structure of Na-stabilized zirconia

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

Fagherazzi, G.; Canton, P.; Benedetti, A.

Using x-ray Rietveld analysis the fcc (fluorite-type) structure of a Na-containing nanocrystalline zirconia powder (9.5 nm estimated of crystallite size) obtained by precipitation and subsequent calcination has been confirmed. The result shows that using conventional x-ray diffraction techniques the cubic crystallographic form of ZrO{sub 2} from the tetragonal one in nanosized powders. These conclusions are supported by the findings of independent Raman scattering experiments. {copyright} {ital 1997 Materials Research Society.}

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

Probing the Crystal Structure and Formation Mechanism of Lanthanide-Doped Upconverting Nanocrystals

DOE PAGES

Hudry, Damien; Abeykoon, A. M. M.; Dooryhee, E.; ...

2016-11-23

Lanthanide (Ln)-doped upconverting nanocrystals (UCNCs), such as NaLnF 4 (with Ln = lanthanide), constitute an important class of nanoscale materials due to their capacity to convert near-infrared photons into near-ultraviolet or visible light. Although under intense investigation for more than a decade, UCNCs have been relatively underexplored especially regarding their crystal structure and mechanisms of formation in organic media. The former is needed to explain the relationship between atomic scale structure and upconversion (UC) properties of UCNCs (i.e., local symmetry for 4f–4f transition probability, Ln 3+ distances for energy migration), while the latter is essential to finely tune the size, morphology, chemical composition, and architecture of well-defined upconverting nanostructures, which constitute the experimental levers to modify the optical properties. In this contribution, we use synchrotron-based diffraction experiments coupled to Rietveld and pair distribution function (PDF) analyses to understand the formation of NaGdF 4:Yb:Er UCNCs in organic media and to investigate their crystal structure. Our results reveal a complex mechanism of the formation of NaGdF 4:Yb:Er UCNCs based on chemical reactions involving molecular clusters and in situ-generated, crystalline sodium fluoride at high temperature. Additionally, a detailed crystallographic investigation of NaGdF 4:Yb:Er UCNCs is presented. Our Rietveld and PDF analyses show that the space group Pmore » $$\\bar{6}$$ is the one that best describes the crystal structure of NaGdF 4:Yb:Er UCNCs contrary to what has been recently proposed. Further, our Rietveld and PDF data reveal the formation of bulk-like crystal structure down to 10 nm with limited distortions. Finally, the results presented in this paper constitute an important step toward the comprehensive understanding of the underlying picture that governs UC properties of lanthanide-doped nanostructures.« less

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).

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.

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.

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

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.

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, structure refinement and chromate sorption characteristics of an Al-rich bayerite-based layered double hydroxide

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

Britto, Sylvia, E-mail: sylviabritto11@gmail.com; Kamath, P. Vishnu

2014-07-01

“Imbibition” of Zn{sup 2+} ions into the cation vacancies of bayerite–Al(OH){sub 3} and NO{sub 3}{sup −} ions into the interlayer gallery yields an Al-rich layered double hydroxide with Al/Zn ratio ∼3. NO{sub 3}{sup −} ions are intercalated with their molecular planes inclined at an angle to the plane of the metal hydroxide slab and bonded to it by hydrogen bonds. Rietveld refinement of the structure shows that the monoclinic symmetry of the precursor bayerite is preserved in the product, showing that the imbibition is topochemical in nature. The nitrate ion is labile and is quantitatively replaced by CrO{sub 4}{sup 2−}more » ions from solution. The uptake of CrO{sub 4}{sup 2−} ions follows a Langmuir adsorption isotherm, thus showing that the hydroxide is a candidate material for green chemistry applications for the removal of CrO{sub 4}{sup 2−} ions from waste water. Rietveld refinement of the structure of the hydroxide after CrO{sub 4}{sup 2−} inclusion reveals that the CrO{sub 4}{sup 2−} ion is intercalated with one of its 2-fold axes parallel to the b-crystallographic axis of the crystal, also the principal 2 axis of the monoclinic cell. - Graphical abstract: The structure of the [Zn–Al4-nitrate] LDH viewed along the a-axis. - Highlights: • Synthesis of Al-rich layered double hydroxide with Al/Zn ratio ∼3. • Rietveld refinement indicates that the imbibition of Zn into Al(OH){sub 3} is topochemical in nature. • The uptake of CrO{sub 4}{sup 2−} ions follows a Langmuir adsorption isotherm.« less

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.

Microstructure characterization and phase transformation kinetic study of ball-milled m-ZrO 2-30 mol% a-TiO 2 mixture by Rietveld method

NASA Astrophysics Data System (ADS)

Pradhan, S. K.; Dutta, H.

2005-05-01

High-energy ball milling of monoclinic ZrO 2-30 mol% anatase TiO 2 mixture at different durations results in the formation of m-ZrO 2-a-TiO 2 solid solution from which the nucleation of nanocrystalline cubic (c) ZrO 2 polymorphic phase sets in. Post-annealing of 12 h ball-milled sample at different elevated temperatures for 1 h results in almost complete formation of c-ZrO 2 phase. Microstructure of the unmilled, all the ball milled and annealed samples has been characterized by Rietveld's X-ray powder structure refinement method. Particle size, rms lattice strain, change in lattice parameters and phase content of individual phases have been estimated from Rietveld analysis, and are utilized to interpret the results. In course of milling, (1 1 1) of cubic lattice became parallel to ( 1bar 1 1) plane of monoclinic lattice due to the orientation effect and cubic phase may have been formed on the (0 0 1) of the m-ZrO 2-a-TiO 2 solid solution lattice. A comparative study of microstructure and phase transformation kinetics of ZrO 2-10, 20 and 30 mol% a-TiO 2 ball-milled and post-annealed samples reveals that rate of phase transformation m→c-ZrO 2 increases with increasing a-TiO 2 concentration and ∼30 mol% of nanocrystalline c-ZrO 2 phase can be obtained within 4 h of milling time in the presence of 30 mol% of a-TiO 2. The post-annealing treatment at 773, 873 and 973 K for 1 h duration each reveals that rate of c-ZrO 2 formation with increasing temperature is retarded with increasing a-TiO 2 concentration but the amount of c-ZrO 2 becomes almost equal (∼95 mol%) at 973 K. It suggests that almost fully stabilized nanocrystalline c-ZrO 2 can be formed by adding a tetravalent solute to m-ZrO 2.

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.

Neutron powder diffraction and molecular simulation study of the structural evolution of ammonia borane from 15 to 340 K.

PubMed

Hess, Nancy J; Schenter, Gregory K; Hartman, Michael R; Daemen, Luc L; Proffen, Thomas; Kathmann, Shawn M; Mundy, Christopher J; Hartl, Monika; Heldebrant, David J; Stowe, Ashley C; Autrey, Tom

2009-05-14

The structural behavior of (11)B-, (2)H-enriched ammonia borane, ND(3)(11)BD(3), over the temperature range from 15 to 340 K was investigated using a combination of neutron powder diffraction and ab initio molecular dynamics simulations. In the low temperature orthorhombic phase, the progressive displacement of the borane group under the amine group was observed leading to the alignment of the B-N bond near parallel to the c-axis. The orthorhombic to tetragonal structural phase transition at 225 K is marked by dramatic change in the dynamics of both the amine and borane group. The resulting hydrogen disorder is problematic to extract from the metrics provided by Rietveld refinement but is readily apparent in molecular dynamics simulation and in difference Fourier transform maps. At the phase transition, Rietveld refinement does indicate a disruption of one of two dihydrogen bonds that link adjacent ammonia borane molecules. Metrics determined by Rietveld refinement are in excellent agreement with those determined from molecular simulation. This study highlights the valuable insights added by coupled experimental and computational studies.

Effect of vanadium doping on structural and magnetic properties of defective nano-nickel ferrite

NASA Astrophysics Data System (ADS)

Heiba, Zein K.; Mohamed, Mohamed Bakr; Wahba, Adel Maher; Almalowi, M. I.

2018-04-01

Nano-nickel ferrites defected by vanadium doping (NiV x Fe2-1.67 x O4, 0 ≤ x ≤ 0.25) were prepared using a simple sol gel method. Rietveld analysis revealed a nonmonotonic change in lattice parameter, oxygen parameter and magnetization upon doping with vanadium. Cation distributions suggested from either Rietveld analysis or from experimental magnetic moments were in a good agreement. For low doping values ( x = 0.05), vanadium was residing mainly in octahedral sites, while for samples with vanadium content ( x ≥ 0.1) a significant part of vanadium ions resided at tetrahedral sites; a result which has been confirmed by the analysis of Fourier-transform infrared (FTIR) spectrums obtained for the samples. The transmission electron microscope (TEM) image showed fine spherical particles with size of ˜ 11 nm. All samples showed a superparamagnetic nature with a nonmonotonic change of either magnetization ( M S) or coercivity (H C) with the content of nonmagnetic V5+. The cation occupancies indicated presence of an enormous number of vacancies through doping with high valence cation V5+, making present samples potential electrodes for Li- or Na-ion batteries.

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

Thermal expansion coefficient prediction of fuel-cell seal materials from silica sand

NASA Astrophysics Data System (ADS)

Hidayat, Nurul; Triwikantoro, Baqiya, Malik A.; Pratapa, Suminar

2013-09-01

This study is focused on the prediction of coefficient of thermal expansion (CTE) of silica-sand-based fuel-cell seal materials (FcSMs) which in principle require a CTE value in the range of 9.5-12 ppm/°C. A semi-quantitative theoretical method to predict the CTE value is proposed by applying the analyzed phase compositions from XRD data and characterized density-porosity behavior. A typical silica sand was milled at 150 rpm for 1 hour followed by heating at 1000 °C for another hour. The sand and heated samples were characterized by means of XRD to perceive the phase composition correlation between them. Rietveld refinement was executed to investigate the weight fraction of the phase contained in the samples, and then converted to volume fraction for composite CTE calculations. The result was applied to predict their potential physical properties for FcSM. Porosity was taken into account in the calculation after which it was directly measured by the Archimedes method.

Synchrotron Powder X-ray Diffraction Study of the Structure and Dehydration Behavior of Sepiolite

NASA Astrophysics Data System (ADS)

Post, J. E.; Bish, D. L.; Heaney, P. J.

2006-05-01

Sepiolite is a hydrous Mg-silicate clay mineral with fibrous morphology that typically occurs as fine-grained, poorly crystalline masses. It occurs in a wide variety of geological environments and has been mined for centuries because of its many uses, e.g. in the pharmaceutical, fertilizer, and pesticide industries. Its versatile functionality derives from the large surface area and microporosity that are characteristic of the material. In recent years, sepiolite has received considerable attention with regard to the adsorption of organics, for use as a support for catalysts, as a molecular sieve, and as an inorganic membrane for ultrafiltration. Because of its fine-grained and poorly crystalline nature, it has not been possible to study sepiolite's crystal structure using single-crystal X-ray diffraction methods, and consequently many details of the structure are still not well known. In this study, Rietveld refinements using synchrotron powder X-ray diffraction data were used to investigate the crystal structure and dehydration behavior of sepiolite from Durango, Mexico. The room- temperature (RT) sepiolite structure in air compares well with previous models but reveals an additional zeolitic water site. The RT structure under vacuum retained only ~1/8 of the zeolitic water and the volume decreased 1.3%. Real-time, temperature-resolved synchrotron powder X-ray diffraction data and Rietveld refinements were used to investigate the behavior of the sepiolite structure from 300 to 925 K. Rietveld refinements revealed that most of the zeolitic water is lost by ~390 K, accompanied by a decrease in the a and c unit-cell parameters. Above ~600 K the sepiolite structure folds as one-half of the crystallographically bound water is lost. Rietveld refinements of the "anhydrous" sepiolite structure reveal that, in general, unit-cell parameters a, b, â and volume steadily decrease with increasing temperature; there is an obvious change in slope at ~820 K suggesting a phase transformation coinciding with the loss of the remaining bound water molecule. These temperature-resolved real-time powder X-ray diffraction studies provide the first comprehensive description of the sepiolite structure and the complex changes it undergoes as it dehydrates. Additional heating and cooling in situ powder X-ray diffraction experiments are underway in order to investigate the relative stabilities and rehydration behaviors of the partially-hydrated sepiolite phases. The results of these studies should provide a more robust model for predicting and modifying the properties and applications of this critical industrial material and environmentally important mineral.

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

In situ high-pressure measurement of crystal solubility by using neutron diffraction

NASA Astrophysics Data System (ADS)

Chen, Ji; Hu, Qiwei; Fang, Leiming; He, Duanwei; Chen, Xiping; Xie, Lei; Chen, Bo; Li, Xin; Ni, Xiaolin; Fan, Cong; Liang, Akun

2018-05-01

Crystal solubility is one of the most important thermo-physical properties and plays a key role in industrial applications, fundamental science, and geoscientific research. However, high-pressure in situ measurements of crystal solubility remain very challenging. Here, we present a method involving high-pressure neutron diffraction for making high-precision in situ measurements of crystal solubility as a function of pressure over a wide range of pressures. For these experiments, we designed a piston-cylinder cell with a large chamber volume for high-pressure neutron diffraction. The solution pressures are continuously monitored in situ based on the equation of state of the sample crystal. The solubility at a high pressure can be obtained by applying a Rietveld quantitative multiphase analysis. To evaluate the proposed method, we measured the high-pressure solubility of NaCl in water up to 610 MPa. At a low pressure, the results are consistent with the previous results measured ex situ. At a higher pressure, more reliable data could be provided by using an in situ high-pressure neutron diffraction method.

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

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.

Rietveld-refinement and optical study of the Fe doped ZnO thin film by RF magnetron sputtering

NASA Astrophysics Data System (ADS)

Kumar, Arun; Dhiman, Pooja; Singh, M.

2017-05-01

Fe Doped ZnO Dilute Magnetic Semiconductor thin film prepared by RF magnetron sputtering on glass substrate and Influence of 3% Fe-doping on structural and Optical properties has been studied. The Rietveld-refinement analysis shows that Fe doping has a significant effect on crystalline structure, grain size and strain in the thin film. Two dimensional and three-dimensional atom probe tomography of the thin film shows that Fe ions are randomly distributed which is supported by Xray Diffraction (XRD). Fe-doping is found to effectively modify the band gap energy up to 3.5 eV.

Micro-structural study and Rietveld analysis of fast reactor fuels: U-Mo fuels

NASA Astrophysics Data System (ADS)

Chakraborty, S.; Choudhuri, G.; Banerjee, J.; Agarwal, Renu; Khan, K. B.; Kumar, Arun

2015-12-01

U-Mo alloys are the candidate fuels for both research reactors and fast breeder reactors. In-reactor performance of the fuel depends on the microstructural stability and thermal properties of the fuel. To improve the fuel performance, alloying elements viz. Zr, Mo, Nb, Ti and fissium are added in the fuel. The first reactor fuels are normally prepared by injection casting. The objective of this work is to compare microstructure, phase-fields and hardness of as-cast four different U-Mo alloy (2, 5, 10 and 33 at.% Mo) fuels with the equilibrium microstructure of the alloys. Scanning electron microscope with energy dispersive spectrometer and optical microscope have been used to characterize the morphology of the as-cast and annealed alloys. The monoclinic α'' phase in as-cast U-10 at.% Mo alloy has been characterized through Rietveld analysis. A comparison of metallographic and Rietveld analysis of as-cast (dendritic microstructure) and annealed U-33 at.% Mo alloy, corresponding to intermetallic compound, has been reported here for the first time. This study will provide in depth understanding of microstructural and phase evolution of U-Mo alloys as fast reactor fuel.

Solvothermal growth of a ruthenium metal-organic framework featuring HKUST-1 structure type as thin films on oxide surfaces.

PubMed

Kozachuk, Olesia; Yusenko, Kirill; Noei, Heshmat; Wang, Yuemin; Walleck, Stephan; Glaser, Thorsten; Fischer, Roland A

2011-08-14

Phase-pure crystalline thin films of a mixed-valence Ru(2)(II,III) metal-organic framework with 1,3,5-benzenetricarboxylate (btc) as a linker were solvothermally grown on amorphous alumina and silica surfaces. Based on the Rietveld refinement, the structure of Ru-MOF was assigned to be analogous to [Cu(3)(btc)(2)] (HKUST-1). This journal is © The Royal Society of Chemistry 2011

Synthesis and structural investigation of new Co1-xNixTeO4 (x = 0, 0.2, 0.5, 0.8 and 1) compounds

NASA Astrophysics Data System (ADS)

Patel, Akhilesh K.; Singh, Harishchandra; Suresh, K. G.

2018-05-01

The new polycrystalline compounds Co1-xNixTeO4 (x = 0, 0.2, 0.5, 0.8 and 1) were prepared by sol-gel method and their structural properties have been studied. Structural investigation through Rietveld method shows monoclinic structure with space group P21/c for all compounds. All compounds polyhedral structure found to be in octahedral form with cations (M) at the center and six oxygen atoms at corner of octahedral structure. The lattice parameters variation with Ni substitution are found to be decreasing with Ni substitution.

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.

Arsenic uptake by gypsum and calcite: Modelling and probing by neutron and X-ray scattering

NASA Astrophysics Data System (ADS)

Fernández-Martínez, A.; Román-Ross, G.; Cuello, G. J.; Turrillas, X.; Charlet, L.; Johnson, M. R.; Bardelli, F.

2006-11-01

Uptaking of contaminants by solid phases is relevant to many issues in environmental science as this process can remove them from solutions and retard their transport into the hydrosphere. Here we report on two structural studies performed on As-doped gypsum (CaSO 4 2H 2O) and calcite (CaCO 3), using neutron (D20-ILL) and X-ray (ID11-ESRF) diffraction data and EXAFS (BM8-ESRF). The aim of this study is to determine whether As gets into the bulk of gypsum and calcite structures or is simply adsorbed on the surface. Different mechanisms of substitution are used as hypotheses. The combined Rietveld analysis of neutron and X-ray diffraction data shows an expansion of the unit cell volume proportional to the As concentration within the samples. DFT-based simulations confirm the increase of the unit cell volume proportional to the amount of carbonate or sulphate groups substituted. Interpolation of the experimental Rietveld data allows us to distinguish As substituted within the structure from that adsorbed on the surface of both minerals. Results obtained by EXAFS analysis from calcite samples show good agreement with the hypothesis of replacement of As into the C crystallographic site.

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.

Revisiting elastic anisotropy of biotite gneiss from the Outokumpu scientific drill hole based on new texture measurements and texture-based velocity calculations

NASA Astrophysics Data System (ADS)

Wenk, H.-R.; Vasin, R. N.; Kern, H.; Matthies, S.; Vogel, S. C.; Ivankina, T. I.

2012-10-01

A sample of biotite gneiss from the Outokumpu deep drilling project in Finland was investigated by Kern et al. (2008) for crystal preferred orientation and elastic anisotropy. Considerable differences between measured acoustic velocities and velocities calculated on the basis of texture patterns were observed. Measured P-wave anisotropy was 15.1% versus a Voigt average yielding 7.9%. Here we investigate the same sample with different methods and using different averaging techniques. Analyzing time-of-flight neutron diffraction data from Dubna-SKAT and LANSCE-HIPPO diffractometers with the Rietveld technique, much stronger preferred orientation for biotite is determined, compared to conventional pole-figure analysis reported previously. The comparison reveals important differences: HIPPO has much better counting statistics but pole figure coverage is poor. SKAT has better angular resolution. Using the new preferred orientation data and applying a self-consistent averaging method that takes grain shapes into account, close agreement of calculated and measured P-wave velocities is observed (12.6%). This is further improved by adding 0.1 vol.% flat micropores parallel to the biotite platelets in the simulation (14.9%).

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

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.

Crystal structure of human tooth enamel studied by neutron diffraction

NASA Astrophysics Data System (ADS)

Ouladdiaf, Bachir; Rodriguez-Carvajal, Juan; Goutaudier, Christelle; Ouladdiaf, Selma; Grosgogeat, Brigitte; Pradelle, Nelly; Colon, Pierre

2015-02-01

Crystal structure of human tooth enamel was investigated using high-resolution neutron powder diffraction. Excellent agreement between observed and refined patterns is obtained, using the hexagonal hydroxyapatite model for the tooth enamel, where a large hydroxyl deficiency ˜70% is found in the 4e site. Rietveld refinements method combined with the difference Fourier maps have revealed, however, that the hydroxyl ions are not only disordered along the c-axis but also within the basal plane. Additional H ions located at the 6h site and forming HPO42- anions were found.

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).

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.

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

Structural studies of TiC{sub 1−x}O{sub x} solid solution by Rietveld refinement and first-principles calculations

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

Jiang, Bo, E-mail: youqin5912@yahoo.com.cn; Hou, Na; Huang, Shanyan

2013-08-15

The lattice parameters, structural stability and electronic structure of titanium oxycarbides (TiC{sub 1−x}O{sub x}, 0≤x≤1) solid solution were investigated by Rietveld refinement and first-principles calculations. Series of TiC{sub 1−x}O{sub x} were precisely synthesized by sintering process under the vacuum. Rietveld refinement results of XRD patterns show the properties of continuous solid solution in TiC{sub 1−x}O{sub x} over the whole composition range. The lattice parameters vary from 0.4324 nm to 0.4194 nm decreasing with increasing oxygen concentration. Results of first-principles calculations reveal that the disorder C/O structure is stable than the order C/O structure. Further investigations of the vacancy in Ti{submore » 1−Va}(C{sub 1−x}O{sub x}){sub 1−Va} solid solution present that the structure of vacancy segregated in TiO-part is more stable than the disorder C/O structure, which can be ascribed to the Ti–Ti bond across O-vacancy and the charge redistributed around Ti-vacancy via the analysis of the electron density difference plots and PDOS. - Graphical abstract: XRD of series of titanium oxycarbides (TiC{sub 1−x}O{sub x}, 0≤x≤1) solid solution prepared by adjusting the proportion of TiO in the starting material. Highlights: • Titanium oxycarbides were obtained by sintering TiO and TiC under carefully controlled conditions. • Rietveld refinement results show continuous solid solution with FCC structure in TiC{sub 1−x}O{sub x}. • The disorder C/O structure is stable than the order C/O structure. • Introduction of vacancy segregated in TiO-part is more stable than disorder C/O structure. • Ti–Ti bond across O-vacancy and the charge redistributed around Ti-vacancy enhance structural stability.« less

The magnetic structure of Co(NCNH)₂ as determined by (spin-polarized) neutron diffraction

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

Jacobs, Philipp; Houben, Andreas; Senyshyn, Anatoliy

The magnetic structure of Co(NCNH)₂ has been studied by neutron diffraction data below 10 K using the SPODI and DNS instruments at FRM II, Munich. There is an intensity change in the (1 1 0) and (0 2 0) reflections around 4 K, to be attributed to the onset of a magnetic ordering of the Co²⁺ spins. Four different spin orientations have been evaluated on the basis of Rietveld refinements, comprising antiferromagnetic as well as ferromagnetic ordering along all three crystallographic axes. Both residual values and supplementary susceptibility measurements evidence that only a ferromagnetic ordering with all Co²⁺ spins parallelmore » to the c axis is a suitable description of the low-temperature magnetic ground state of Co(NCNH)₂. The deviation of the magnetic moment derived by the Rietveld refinement from the expectancy value may be explained either by an incomplete saturation of the moment at temperatures slightly below the Curie temperature or by a small Jahn–Teller distortion. - Graphical abstract: The magnetic ground state of Co(NCNH)₂ has been clarified by (spin-polarized) neutron diffraction data at low temperatures. Intensity changes below 4 K arise due to the onset of ferromagnetic ordering of the Co²⁺ spins parallel to the c axis, corroborated by various (magnetic) Rietveld refinements. Highlights: • Powderous Co(NCNH)₂ has been subjected to (spin-polarized) neutron diffraction. • Magnetic susceptibility data of Co(NCNH)₂ have been collected. • Below 4 K, the magnetic moments align ferromagnetically with all Co²⁺ spins parallel to the c axis. • The magnetic susceptibility data yield an effective magnetic moment of 4.68 and a Weiss constant of -13(2) K. • The ferromagnetic Rietveld refinement leads to a magnetic moment of 2.6 which is close to the expectancy value of 3.« 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.

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

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.

Rietveld refinement and electrical properties of Ni-Zn spinel ferrites

NASA Astrophysics Data System (ADS)

Hooda, Ashima; Sanghi, Sujata; Agarwal, Ashish; Khasa, Satish; Hooda, Bhawana

2017-05-01

NiFe2O4, ZnFe2O4, Ni0.5Zn0.5Fe2O4 spinel samples have been synthesized by conventional solid state reaction technique. Powder X-ray diffraction and Rietveld refinement revealed that the samples were single Spinel phase with space group fd3m. The average crystalline size (D), lattice constant (a), X-ray density (ρx), measured density (ρm) and Porosity (P) of prepared samples were determined from XRD data. The dc electrical resistivity (p) was measured as a function of temperature. The variations of ρ were explained on the basis of Verwey and de Bohr mechanism. The value of DC resistivity found to increase with increase Zn concentration.

Sensitivity and Limitations of Structures from X-ray and Neutron-Based Diffraction Analyses of Transition Metal Oxide Lithium-Battery Electrodes

DOE PAGES

Liu, Hao; Liu, Haodong; Lapidus, Saul H.; ...

2017-06-21

Lithium transition metal oxides are an important class of electrode materials for lithium-ion batteries. Binary or ternary (transition) metal doping brings about new opportunities to improve the electrode’s performance and often leads to more complex stoichiometries and atomic structures than the archetypal LiCoO 2. Rietveld structural analyses of X-ray and neutron diffraction data is a widely-used approach for structural characterization of crystalline materials. But, different structural models and refinement approaches can lead to differing results, and some parameters can be difficult to quantify due to the inherent limitations of the data. Here, through the example of LiNi 0.8Co 0.15Al 0.05Omore » 2 (NCA), we demonstrated the sensitivity of various structural parameters in Rietveld structural analysis to different refinement approaches and structural models, and proposed an approach to reduce refinement uncertainties due to the inexact X-ray scattering factors of the constituent atoms within the lattice. Furthermore, this refinement approach was implemented for electrochemically-cycled NCA samples and yielded accurate structural parameters using only X-ray diffraction data. The present work provides the best practices for performing structural refinement of lithium transition metal oxides.« less

Sensitivity and Limitations of Structures from X-ray and Neutron-Based Diffraction Analyses of Transition Metal Oxide Lithium-Battery Electrodes

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

Liu, Hao; Liu, Haodong; Lapidus, Saul H.

Lithium transition metal oxides are an important class of electrode materials for lithium-ion batteries. Binary or ternary (transition) metal doping brings about new opportunities to improve the electrode’s performance and often leads to more complex stoichiometries and atomic structures than the archetypal LiCoO 2. Rietveld structural analyses of X-ray and neutron diffraction data is a widely-used approach for structural characterization of crystalline materials. But, different structural models and refinement approaches can lead to differing results, and some parameters can be difficult to quantify due to the inherent limitations of the data. Here, through the example of LiNi 0.8Co 0.15Al 0.05Omore » 2 (NCA), we demonstrated the sensitivity of various structural parameters in Rietveld structural analysis to different refinement approaches and structural models, and proposed an approach to reduce refinement uncertainties due to the inexact X-ray scattering factors of the constituent atoms within the lattice. Furthermore, this refinement approach was implemented for electrochemically-cycled NCA samples and yielded accurate structural parameters using only X-ray diffraction data. The present work provides the best practices for performing structural refinement of lithium transition metal oxides.« less

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.

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.

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.

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.

Quantitative analysis of thoria phase in Th-U alloys using diffraction studies

NASA Astrophysics Data System (ADS)

Thakur, Shital; Krishna, P. S. R.; Shinde, A. B.; Kumar, Raj; Roy, S. B.

2017-05-01

In the present study the quantitative phase analysis of Th-U alloys in bulk form namely Th-52 wt% U and Th-3wt%U has been performed over the data obtained from both X ray diffraction and neutron diffraction technique using Rietveld method of FULLPROF software. Quantifying thoria (ThO2) phase present in bulk of the sample is limited due to surface oxidation and low penetration of x rays in high Z material. Neutron diffraction study probing bulk of the samples has been presented in comparison with x-ray diffraction study.

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.

Analysis of macromolecules, ligands and macromolecule-ligand complexes

DOEpatents

Von Dreele, Robert B [Los Alamos, NM

2008-12-23

A method for determining atomic level structures of macromolecule-ligand complexes through high-resolution powder diffraction analysis and a method for providing suitable microcrystalline powder for diffraction analysis are provided. In one embodiment, powder diffraction data is collected from samples of polycrystalline macromolecule and macromolecule-ligand complex and the refined structure of the macromolecule is used as an approximate model for a combined Rietveld and stereochemical restraint refinement of the macromolecule-ligand complex. A difference Fourier map is calculated and the ligand position and points of interaction between the atoms of the macromolecule and the atoms of the ligand can be deduced and visualized. A suitable polycrystalline sample of macromolecule-ligand complex can be produced by physically agitating a mixture of lyophilized macromolecule, ligand and a solvent.

Crystallographic changes in lead zirconate titanate due to neutron irradiation

DOE PAGES

Henriques, Alexandra; Graham, Joseph T.; Landsberger, Sheldon; ...

2014-11-17

Piezoelectric and ferroelectric materials are useful as the active element in non-destructive monitoring devices for high-radiation areas. Here, crystallographic structural refinement (i.e., the Rietveld method) is used to quantify the type and extent of structural changes in PbZr 0 .5Ti 0 .5O 3 after exposure to a 1 MeV equivalent neutron fluence of 1.7 × 10 15 neutrons/cm 2. The results show a measurable decrease in the occupancy of Pb and O due to irradiation, with O vacancies in the tetragonal phase being created preferentially on one of the two O sites. The results demonstrate a method by which themore » effects of radiation on crystallographic structure may be investigated.« less

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

Volcanic glass in Cretaceous dacites and rhyolites of the Paraná Magmatic Province, southern Brazil: Characterization and quantification by XRD-Rietveld

NASA Astrophysics Data System (ADS)

Andrade, Fábio Ramos Dias de; Polo, Liza Angélica; Janasi, Valdecir de Assis; Carvalho, Flávio Machado de Souza

2018-04-01

Acidic rocks are a significant component of the Cretaceous Paraná Magmatic Province, occurring in different stratigraphic positions, and often forming deposits of complex and as yet poorly defined architecture. Vitrophyric varieties are surprisingly abundant for a volcanic sequence of this age, and are composed of predominant glass plus plagioclase (labradorite-andesine), pyroxenes (augite ± pigeonite and orthopyroxene), Ti-rich magnetite, and traces of apatite. Hypocrystalline rocks, largely derived from devitrification, additionally contain sanidine, cristobalite, and quartz. The negative correlation between the abundance of these minerals and the amount of glass suggests that these latter phases formed by devitrification. Modal analysis using a combined XRD Rietveld-RIR method detected glass contents between 0 and 85 wt% % in a set of representative samples of Palmas-type acidic rocks from southern Brazil with dacite to rhyolite composition. Modal compositions determined by XRD and by scanning electron microscope are in good agreement with each other, and were checked against whole-rock XRF chemical data. Water contents up to 4 wt% show a positive linear correlation with the amount of glass, and are inferred to be mostly secondary, as original (pre-eruptive) H2O dissolved in melts is inferred to have been < 1.5 wt% in all rocks. Glass is the only water bearing phase in the studied samples, which lack low temperature hydrated phases. Water loss during devitrification appears to have occurred along fractures, and was accompanied by Na loss and, in some samples, also Ca, Rb and Sr loss. The rapid and inexpensive method of modal analyses of glassy rocks developed here may be a useful tool for mapping acidic volcanic rocks in southern Paraná Magmatic Province, and also to identify the architecture of these deposits.

Hydrothermal synthesis, characterization, and thermal properties of alumino silicate azide sodalite, Na8[AlSiO4]6(N3)2

NASA Astrophysics Data System (ADS)

Borhade, A. V.; Wakchaure, S. G.; Dholi, A. G.; Kshirsagar, T. A.

2017-07-01

First time we report the synthesis, structural characterization and thermal behavior of an unusual N3 - containing alumino-silicate sodalite mineral. Azide sodalite, Na8[AlSiO4]6(N3)2 has been synthesized under hydrothermal conditions at 433 K in steel lined Teflon autoclave. The structural and microstructural properties of azide sodalite mineral was characterized by various methods including FT-IR, XRD, SEM, TGA, and MAS NMR. Crystal structure have been refined by Rietveld method in P\\bar 43n space group, indicating that the N3 - sodalite has cubic in lattice. High temperature study was carried out to see the effect of thermal expansion on cell dimension ( a o) of azide sodalite. Thermal behavior of sodalite was also assessed by thermogravimetric method.

Investigation of phase segregation using Rietveld refinement in Mg doped BaTiO3 solid solutions and their ferroelectric properties

NASA Astrophysics Data System (ADS)

Aanchal, Kaur, Kiranpreet; Singh, Anupinder; Singh, Mandeep

2018-05-01

Ba(1-x) Mgx Ti O3 (BMT) samples were synthesised using solid state reaction route with `x' varying from 0.025 to 0.10. The structural and ferroelectric properties of the bulk samples were investigated. The XRD analysis shows the presence of two phases, the first phase being magnesium doped BT (space group P4mm) and the second phase being Ba2TiO4 (space group Pna21). The tetragonal phase was found to be the major phase in the samples. The double phase Rietveld refinement was done and the weight percentage of orthorhombic phase was found to vary from 3.43% to 6.96% for x varying from 0.025≤x≤0.10. The P - E measurements reveal that all the samples exhibit lossy behaviour.

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

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.

Crystal structure of Ca{sub 12}Al{sub 14}O{sub 32}Cl{sub 2} and luminescence properties of Ca{sub 12}Al{sub 14}O{sub 32}Cl{sub 2}:Eu{sup 2+}

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

Iwata, Tomoyuki; Haniuda, Masahide; Fukuda, Koichiro

2008-01-15

The crystal structure of Ca{sub 12}Al{sub 14}O{sub 32}Cl{sub 2} was determined from laboratory X-ray powder diffraction data (CuK{alpha}{sub 1}) using the Rietveld method, with the anisotropic displacement parameters being assigned for all atoms. The crystal structure is cubic (space group I4-bar 3d, Z=2) with lattice dimensions a=1.200950(5) nm and V=1.73211(1) nm{sup 3}. The reliability indices calculated from the Rietveld method were R{sub wp}=8.48% (S=1.21), R{sub p}=6.05%, R{sub B}=1.27% and R{sub F}=1.01%. The validity of the structural model was verified by the three-dimensional electron density distribution, the structural bias of which was reduced as much as possible using the maximum-entropy methods-basedmore » pattern fitting (MPF). The reliability indices calculated from the MPF were R{sub B}=0.75% and R{sub F}=0.56%. In the structural model there are one Ca site, two Al sites, two O sites and one Cl site. This compound is isomorphous with Ca{sub 12}Al{sub 10.6}Si{sub 3.4}O{sub 32}Cl{sub 5.4}. Europium-doped sample Ca{sub 12}Al{sub 14}O{sub 32}Cl{sub 2}:Eu{sup 2+} was prepared and the photoluminescence properties were presented. The excitation spectrum consisted of two wide bands, which were located at about 268 and 324 nm. The emission spectrum, when excited at 324 nm, resulted in indigo light with a peak at about 442 nm. - Graphical abstract: A portion of the crystal structure of Ca{sub 12}Al{sub 14}O{sub 32}Cl{sub 2} showing eight-membered AlO{sub 4} rings and Ca-Cl-Ca unit.« less

Superstructure ZrV2O7 nanofibres: thermal expansion, electronic and lithium storage properties.

PubMed

Li, Qidong; Zhao, Yanming; Kuang, Quan; Fan, Qinghua; Dong, Youzhong; Liu, Xudong

2016-11-30

ZrV 2 O 7 has attracted much attention as a negative thermal expansion (NTE) material due to its isotropic negative structure. However, rarely has investigation of the lithium storage behaviors been carried out except our first report on it. Meanwhile, the electrochemical behaviors and energy storage characteristics have not been studied in depth and will be explored in this article. Herein, we report on the synthesis, characterization and lithium intercalation mechanism of superstructure ZrV 2 O 7 nanofibres that were prepared through a facile solution-based method with a subsequent annealing process. The thermal in situ XRD technique combined with the Rietveld refinement method is adopted to analyze the change in the temperature-dependent crystal structure. Benefiting from the nanostructured morphology and relatively high electronic conductivity, it presents acceptable cyclic stability and rate capability. According to the operando evolution of the XRD patterns obtained from electrochemical in situ measurements, the Li intercalation mechanism of the solid solution process with a subsequent conversion reaction can be concluded. Finally, the amorphous state of the electrodes after the initial fully discharged state can effectively enhance the electrochemical performances.

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.

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.;

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.

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

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

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.

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.

Optical and Piezoelectric Study of KNN Solid Solutions Co-Doped with La-Mn and Eu-Fe.

PubMed

Peña-Jiménez, Jesús-Alejandro; González, Federico; López-Juárez, Rigoberto; Hernández-Alcántara, José-Manuel; Camarillo, Enrique; Murrieta-Sánchez, Héctor; Pardo, Lorena; Villafuerte-Castrejón, María-Elena

2016-09-28

The solid-state method was used to synthesize single phase potassium-sodium niobate (KNN) co-doped with the La 3+ -Mn 4+ and Eu 3+ -Fe 3+ ion pairs. Structural determination of all studied solid solutions was accomplished by XRD and Rietveld refinement method. Electron paramagnetic resonance (EPR) studies were performed to determine the oxidation state of paramagnetic centers. Optical spectroscopy measurements, excitation, emission and decay lifetime were carried out for each solid solution. The present study reveals that doping KNN with La 3+ -Mn 4+ and Eu 3+ -Fe 3+ at concentrations of 0.5 mol % and 1 mol %, respectively, improves the ferroelectric and piezoelectric behavior and induce the generation of optical properties in the material for potential applications.

Optical and Piezoelectric Study of KNN Solid Solutions Co-Doped with La-Mn and Eu-Fe

PubMed Central

Peña-Jiménez, Jesús-Alejandro; González, Federico; López-Juárez, Rigoberto; Hernández-Alcántara, José-Manuel; Camarillo, Enrique; Murrieta-Sánchez, Héctor; Pardo, Lorena; Villafuerte-Castrejón, María-Elena

2016-01-01

The solid-state method was used to synthesize single phase potassium-sodium niobate (KNN) co-doped with the La3+–Mn4+ and Eu3+–Fe3+ ion pairs. Structural determination of all studied solid solutions was accomplished by XRD and Rietveld refinement method. Electron paramagnetic resonance (EPR) studies were performed to determine the oxidation state of paramagnetic centers. Optical spectroscopy measurements, excitation, emission and decay lifetime were carried out for each solid solution. The present study reveals that doping KNN with La3+–Mn4+ and Eu3+–Fe3+ at concentrations of 0.5 mol % and 1 mol %, respectively, improves the ferroelectric and piezoelectric behavior and induce the generation of optical properties in the material for potential applications. PMID:28773925

Correlation between magnetocaloric and electrical properties based on phenomenological models in La0.47Pr0.2Pb0.33MnO3 perovskite

NASA Astrophysics Data System (ADS)

Mechi, Nesrine; Alzahrani, Bandar; Hcini, Sobhi; Bouazizi, Mohamed Lamjed; Dhahri, Abdessalem

2018-06-01

We have investigated the correlation between magnetocaloric and electrical properties of La0.47Pr0.2Pb0.33MnO3 perovskite prepared using the sol-gel method. Rietveld analysis of X-ray diffraction (XRD) pattern shows pure crystalline phase with rhombohedral ? structure. Magnetic entropy change, relative cooling power (RCP) and specific heat were predicted from M(T, μ0H) data at different magnetic fields with the help of the phenomenological model. The magnetic entropy change reaches a maximum value ? of about 3.96 J kg-1 K-1 for μ0H = 5 T corresponding to RCP of 183 J kg-1. These values are relatively higher, making our sample a promising candidate for the magnetic refrigeration. Electrical-resistivity measurements were well fitted with the phenomenological percolation model, which is based on the phase segregation of ferromagnetic-metallic clusters and paramagnetic-semiconductor regions. The temperature and magnetic field dependences of resistivity data, ρ(T, μ0H), allowed us to determine the magnetic entropy change ?. Results show that the as-obtained magnetic entropy change values are similar to those determined from the phenomenological model.

Thermal stability, optical and Photoluminescence properties of spherical Ce x Zr1‑x O2 (x = 0.05) crystalline blue-emitting nanophosphors synthesized by microwave method

NASA Astrophysics Data System (ADS)

Manjunatha, S.; Dharmaprakash, M. S.

2018-03-01

Nanocrystalline ZrO2 based material is an impressive candidate for the various functional applications owing to their ease of preparation and high thermal stability. This paper reports the synthesis, structural and optical characterization of thermally stable monodispersed CexZr1‑xO2 (x = 0.05) nanoparticles. This method is based on the fact that, microwave irradiation allows the formation of size controlled and single phase cubic ZrO2 nanoparticles containing Ce+4 as a dopant. The XRD and Rietveld analysis revealed the formation of the crystalline cubic fluorite phase. The formation of nanoparticles was confirmed by FTIR. The morphology of the nanophosphors was characterised by FESEM and TEM. The optical band gap was calculated from the UV–visible absorption spectra and was found to vary from 3.93 to 4.25 eV with calcination temperature. It shows the decrease in the optical band gap from the pristine ZrO2. The particle size was measured by using HRTEM, and the average particle size was found to be 22 nm. Under the 268 nm Ultra Violet irradiation excitation a blue emission at 443 nm was observed at room temperature. The possible luminescence mechanism of CexZr1‑xO2 nanophosphor under UV excitation is discussed.

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.

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

Precursor routes to quaternary intermetallics: Synthesis, crystal structure, and physical properties of clathrate-II Cs8Na16Al24Si112

NASA Astrophysics Data System (ADS)

Wei, Kaya; Dong, Yongkwan; Nolas, George S.

2016-05-01

A new quaternary clathrate-II composition, Cs8Na16Al24Si112, was synthesized by kinetically controlled thermal decomposition (KCTD) employing both NaSi and NaAlSi as the precursors and CsCl as a reactive flux. The crystal structure and composition of Cs8Na16Al24Si112 were investigated using both Rietveld refinement and elemental analysis, and the temperature dependent transport properties were investigated. Our results indicate that KCTD with multiple precursors is an effective method for the synthesis of multinary inorganic phases that are not easily accessible by traditional solid-state synthesis or crystal growth techniques.

Evaluation of structural vacancies for 1/1-Al-Re-Si approximant crystals by positron annihilation spectroscopy

NASA Astrophysics Data System (ADS)

Yamada, K.; Suzuki, H.; Kitahata, H.; Matsushita, Y.; Nozawa, K.; Komori, F.; Yu, R. S.; Kobayashi, Y.; Ohdaira, T.; Oshima, N.; Suzuki, R.; Takagiwa, Y.; Kimura, K.; Kanazawa, I.

2018-01-01

The size of structural vacancies and structural vacancy density of 1/1-Al-Re-Si approximant crystals with different Re compositions were evaluated by positron annihilation lifetime and Doppler broadening measurements. Incident positrons were found to be trapped at the monovacancy-size open space surrounded by Al atoms. From a previous analysis using the maximum entropy method and Rietveld method, such an open space is shown to correspond to the centre of Al icosahedral clusters, which locates at the vertex and body centre. The structural vacancy density of non-metallic Al73Re17Si10 was larger than that of metallic Al73Re15Si12. The observed difference in the structural vacancy density reflects that in bonding nature and may explain that in the physical properties of the two samples.

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.

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.

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.

Significant enhancement in photocatalytic performance of Ni doped BiFeO3 nanoparticles

NASA Astrophysics Data System (ADS)

Nadeem, M.; Khan, Wasi; Khan, Shakeel; Shoeb, Mohd; Husain, Shahid; Mobin, Mohammad

2018-06-01

In the present work, we have investigated the effect of Ni doping on the microstructure and photocatalytic properties of BiFeO3 samples. All the compositions of BiFe1‑xNixO3 (0 ≤ x ≤ 0.07) have been synthesized via cost effective ethylene glycol based sol-gel method. The Rietveld refinement of the XRD data revealed rhombohedral crystal structure with R3c space group. The FTIR spectroscopy confirms the formation of BiFeO3 compound. UV–visible DRS result affirmed that the band gap of the samples can be tuned towards visible range by the Ni substitution. The photoluminescence spectra indicate lower intensity with the Ni content, signify reduction in recombination rate of the electron-hole pairs. The photocatalytic response of the nanoparticles was examined for the degradation of methylene blue (MB) dye under visible light irradiation and the highest photocatalytic response was observed for 7% Ni doped sample. Therefore, the observed results suggest potential application of the synthesized nanoparticles for wastewater treatment purpose.

Instrumental resolution as a function of scattering angle and wavelength as exemplified for the POWGEN instrument

PubMed Central

Jacobs, Philipp; Houben, Andreas; Schweika, Werner; Tchougréeff, Andrei L.; Dronskowski, Richard

2017-01-01

The method of angular- and wavelength-dispersive (e.g. two-dimensional) Rietveld refinement is a new and emerging tool for the analysis of neutron diffraction data measured at time-of-flight instruments with large area detectors. Following the approach for one-dimensional refinements (using either scattering angle or time of flight), the first step at each beam time cycle is the calibration of the instrument including the determination of instrumental contributions to the peak shape variation to be expected for diffraction patterns measured by the users. The aim of this work is to provide the users with calibration files and – for the later Rietveld refinement of the measured data – with an instrumental resolution file (IRF). This article will elaborate on the necessary steps to generate such an IRF for the angular- and wavelength-dispersive case, exemplified for the POWGEN instrument. A dataset measured on a standard diamond sample is used to extract the profile function in the two-dimensional case. It is found that the variation of reflection width with 2θ and λ can be expressed by the standard equation used for evaluating the instrumental resolution, which yields a substantially more fundamental approach to the parameterization of the instrumental contribution to the peak shape. Geometrical considerations of the POWGEN instrument and sample effects lead to values for Δθ, Δt and ΔL that yield a very good match to the extracted FWHM values. In a final step the refinement results are compared with the one-dimensional, i.e. diffraction-focused, case. PMID:28656041

Agroforestry: mapping the way with GIS

Treesearch

Gary Bentrup; Tim Leininger

2002-01-01

Agroforestry combines agriculture and forestry technologies to create diverse, profitable, and sustainable land-use systems (Rietveld, 1995). Agroforestry practices include alley cropping, forest farming, riparian forest buffers, silvopasture, and windbreaks-each of which meets environmental, social, and economic needs (Gold et al., 2000). Environmentally, agroforestry...

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.

Local and average structure of Mn- and La-substituted BiFeO3

NASA Astrophysics Data System (ADS)

Jiang, Bo; Selbach, Sverre M.

2017-06-01

The local and average structure of solid solutions of the multiferroic perovskite BiFeO3 is investigated by synchrotron X-ray diffraction (XRD) and electron density functional theory (DFT) calculations. The average experimental structure is determined by Rietveld refinement and the local structure by total scattering data analyzed in real space with the pair distribution function (PDF) method. With equal concentrations of La on the Bi site or Mn on the Fe site, La causes larger structural distortions than Mn. Structural models based on DFT relaxed geometry give an improved fit to experimental PDFs compared to models constrained by the space group symmetry. Berry phase calculations predict a higher ferroelectric polarization than the experimental literature values, reflecting that structural disorder is not captured in either average structure space group models or DFT calculations with artificial long range order imposed by periodic boundary conditions. Only by including point defects in a supercell, here Bi vacancies, can DFT calculations reproduce the literature results on the structure and ferroelectric polarization of Mn-substituted BiFeO3. The combination of local and average structure sensitive experimental methods with DFT calculations is useful for illuminating the structure-property-composition relationships in complex functional oxides with local structural distortions.

Local and average structure of Mn- and La-substituted BiFeO 3

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

Jiang, Bo; Selbach, Sverre M.

2017-06-01

The local and average structure of solid solutions of the multiferroic perovskite BiFeO 3 is investigated by synchrotron X-ray diffraction (XRD) and electron density functional theory (DFT) calculations. The average experimental structure is determined by Rietveld refinement and the local structure by total scattering data analyzed in real space with the pair distribution function (PDF) method. With equal concentrations of La on the Bi site or Mn on the Fe site, La causes larger structural distortions than Mn. Structural models based on DFT relaxed geometry give an improved fit to experimental PDFs compared to models constrained by the space groupmore » symmetry. Berry phase calculations predict a higher ferroelectric polarization than the experimental literature values, reflecting that structural disorder is not captured in either average structure space group models or DFT calculations with artificial long range order imposed by periodic boundary conditions. Only by including point defects in a supercell, here Bi vacancies, can DFT calculations reproduce the literature results on the structure and ferroelectric polarization of Mn-substituted BiFeO 3. The combination of local and average structure sensitive experimental methods with DFT calculations is useful for illuminating the structure-property-composition relationships in complex functional oxides with local structural distortions.« less

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

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.

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.

Structural, dielectric and magnetic properties of ZnFe2O4-Na0.5Bi0.5TiO3 multiferroic composites

NASA Astrophysics Data System (ADS)

Bhasin, Tanvi; Agarwal, Ashish; Sanghi, Sujata; Yadav, Manisha; Tuteja, Muskaan; Singh, Jogender; Rani, Sonia

2018-04-01

Multiferroic xNa0.5Bi0.5TiO3-(1-x)ZnFe2O4 (x=0.10, 0.20) composites were prepared by conventional solid state reaction method. Rietveld analysis of XRD data shows that samples exhibit both cubic (Fd-3m) and rhombohedral (R3c) crystal structure. Structural parameters and unit cell volume of samples vary with composition. The dielectric constant and dielectric loss (tanδ) display dispersion at low frequency due to space charge polarization and inhomogeneity in the composites. Magnetic analysis depicts the antiferromagnetic behavior of composites and magnetization is enhanced with the introduction of ferrite (ZnFe2O4) phase.

Electrochemical sensing of modified ABO3 perovskite: LaFe0.8 R0.2O3(R= Cr, Co, Al)

NASA Astrophysics Data System (ADS)

Vidya Rajan, N.; Alexander, L. K.

2017-06-01

Perovskite LaFeO3 with orthorhombic structure has been synthesized by citric acid mediated solution method. The effectiveness of ionic radii and Oxidation state of the doping material on ionic conductivity of the host matrix was evaluated by B-site (Fe) doping on LaFeO3 with Cr, Co and Al, resulting LaFe0.8 R0.2O3 (R = Cr, Co, Al). XRD with Rietveld refinement and Raman spectroscopic analysis demonstrate successful synthesis. The effect of the 20% B site doping on electrochemical activity is reported. The doped materials exhibit a decrease in sensing activity towards the non enzymatic detection of H2O2.

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.

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.

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.

The Handling of Missing Binary Data in Language Research

ERIC Educational Resources Information Center

Pichette, François; Béland, Sébastien; Jolani, Shahab; Lesniewska, Justyna

2015-01-01

Researchers are frequently confronted with unanswered questions or items on their questionnaires and tests, due to factors such as item difficulty, lack of testing time, or participant distraction. This paper first presents results from a poll confirming previous claims (Rietveld & van Hout, 2006; Schafer & Graham, 2002) that data…

Sintering and crystallization behavior of CaMgSi{sub 2}O{sub 6}-NaFeSi{sub 2}O{sub 6} based glass-ceramics

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

Goel, Ashutosh; Kansal, Ishu; Dipartimento di Ingegneria dei Materiali e dell'Ambiente, Facolta di Ingegneria, Universita di Modena e Reggio Emilia, 41100 Modena

2009-11-01

We report on the synthesis, sintering, and crystallization behaviors of a glass with a composition corresponding to 90 mol % CaMgSi{sub 2}O{sub 6}-10 mol % NaFeSi{sub 2}O{sub 6}. The investigated glass composition crystallized superficially immediately after casting of the melt and needs a high cooling rate (rapid quenching) in order to produce an amorphous glass. Differential thermal analysis and hot-stage microscopy were employed to investigate the glass forming ability, sintering behavior, relative nucleation rate, and crystallization behavior of the glass composition. The crystalline phase assemblage in the glass-ceramics was studied under nonisothermal heating conditions in the temperature range of 850-950more » deg. C in both air and N{sub 2} atmosphere. X-ray diffraction studies adjoined with the Rietveld-reference intensity ratio method were employed to quantify the amount of crystalline phases, while electron microscopy was used to shed some light on the microstructure of the resultant glass-ceramics. Well sintered glass-ceramics with diopside as the primary crystalline phase were obtained where the amount of diopside varied with the heating conditions.« less

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.

Growth, Faraday and inverse Faraday characteristics of Tb₂Ti₂O₇ crystal.

PubMed

Guo, Feiyun; Sun, Yilin; Yang, Xiongsheng; Chen, Xin; Zhao, Bin; Zhuang, Naifeng; Chen, Jianzhong

2016-03-21

Tb₂Ti₂O₇ (TTO) single crystal with dimensions of 20 × 20 × 16 mm³ was grown by the Czochralski method. Rietveld structure refinement of X-ray diffraction (XRD) data confirms that the compound crystallizes in the cubic system with pyrochlore structure. Transmission spectra, Magnetic circular dichroism (MCD) spectra, Faraday and inverse Faraday characteristics of TTO crystal have been measured and analyzed in detail. The results demonstrate that TTO crystal has high transmittance at 700-1400 nm waveband and a larger Verdat constant than that of TGG reported. Magnetic circular dichroism (MCD) spectra showed that the 4f→4f transitions of Tb³⁺ have significant contributions to the magneto-optical activity (MOA). In the time-resolved pump-probe spectroscopy, the rotation signals of the probe beam based on the inverse Faraday effect in magneto-optical crystal were observed at zero time delay, the full width at half maximum of the rotation and ellipticity signals can be as fast as ~500 fs, which indicates that TTO crystal can be a promising material for ultrafast all-optical magnetic switching.

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

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

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.

Ultrathin inorganic molecular nanowire based on polyoxometalates

PubMed Central

Zhang, Zhenxin; Murayama, Toru; Sadakane, Masahiro; Ariga, Hiroko; Yasuda, Nobuhiro; Sakaguchi, Norihito; Asakura, Kiyotaka; Ueda, Wataru

2015-01-01

The development of metal oxide-based molecular wires is important for fundamental research and potential practical applications. However, examples of these materials are rare. Here we report an all-inorganic transition metal oxide molecular wire prepared by disassembly of larger crystals. The wires are comprised of molybdenum(VI) with either tellurium(IV) or selenium(IV): {(NH4)2[XMo6O21]}n (X=tellurium(IV) or selenium(IV)). The ultrathin molecular nanowires with widths of 1.2 nm grow to micrometre-scale crystals and are characterized by single-crystal X-ray analysis, Rietveld analysis, scanning electron microscopy, X-ray photoelectron spectroscopy, ultraviolet–visible spectroscopy, thermal analysis and elemental analysis. The crystals can be disassembled into individual molecular wires through cation exchange and subsequent ultrasound treatment, as visualized by atomic force microscopy and transmission electron microscopy. The ultrathin molecular wire-based material exhibits high activity as an acid catalyst, and the band gap of the molecular wire-based crystal is tunable by heat treatment. PMID:26139011

Mg(OH)2 nanoparticles produced at room temperature by an innovative, facile, and scalable synthesis route

NASA Astrophysics Data System (ADS)

Taglieri, Giuliana; Felice, Benito; Daniele, Valeria; Ferrante, Fabiola

2015-10-01

Nanoparticles form the fundamental building blocks for many exciting applications in various scientific disciplines. However, the problem of the large-scale synthesis of nanoparticles remains challenging. An original, eco-friendly, single step, and scalable method to produce magnesium hydroxide nanoparticles in aqueous suspensions is here presented. The method, based on an exchange ion process, is extremely simple and rapid (few minutes). It employs cheap or renewable reactants, operates at room temperature and does not require intermediate steps (washings/purifications) to eliminate undesired compounds. Moreover, it is possible to regenerate the exchange material and to reuse it for new operation of synthesis, according to a cyclic procedure, providing potential aptitudes of scalability of nanoparticles production. Some of the synthesis parameters are varied, and structural and morphological features of the produced nanoparticles, after few seconds from the beginning of the synthesis up to the ending time, are investigated by means of several techniques, such as X-ray diffraction (profile fitting and Rietveld refinement), transmission electron microscopy, infrared spectroscopy, thermal analyses, and surface area measurements. In any case, pure and stable suspensions are produced, characterized by crystalline and mesoporous Mg(OH)2 nanoparticles, with lamellar morphology. In particular, the nanolamellas appeared constituted by a superimposition of hexagonally plated and crystalline nanosized precursors (2-3 nm in dimensions), crystallographically oriented.

Neutron diffraction determination of the cell dimensions and thermal expansion of the fluoroperovskite KMgF3 from 293 to 3.6 K

NASA Astrophysics Data System (ADS)

Mitchell, Roger H.; Cranswick, Lachlan M. D.; Swainson, Ian

2006-11-01

The cell dimensions of the fluoroperovskite KMgF3 synthesized by solid state methods have been determined by powder neutron diffraction and Rietveld refinement over the temperature range 293 3.6 K using Pt metal as an internal standard for calibration of the neutron wavelength. These data demonstrate conclusively that cubic Pmoverline{3} m KMgF3 does not undergo any phase transitions to structures of lower symmetry with decreasing temperature. Cell dimensions range from 3.9924(2) Å at 293 K to 3.9800(2) Å at 3.6 K, and are essentially constant within experimental error from 50 to 3.6 K. The thermal expansion data are described using a fourth order polynomial function.

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.

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.

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

Confidence Hills Mineralogy and Chemin Results from Base of Mt. Sharp, Pahrump Hills, Gale Crater, Mars

NASA Technical Reports Server (NTRS)

Cavanagh, P. D.; Bish, D. L.; Blake, D. F.; Vaniman, D. T.; Morris, R. V.; Ming, D. W.; Rampe, E. B.; Achilles, C. N.; Chipera, S. J.; Treiman, A. H.;

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.

New approach for extraction of cellulose from tucumã's endocarp and its structural characterization

NASA Astrophysics Data System (ADS)

Manzato, L.; Rabelo, L. C. A.; de Souza, S. M.; da Silva, C. G.; Sanches, E. A.; Rabelo, D.; Mariuba, L. A. M.; Simonsen, J.

2017-09-01

The recycling of plant wasted materials into useful products represents a green alternative to prevent environmental problems. Tucumã palm fruit (Astrocaryum aculeatum Meyer) is widely used in Amazon region for food and crafts. Due to the large amount of wasted Tucumã's endocarp, this work proposes a new approach for extraction of cellulose and its structural characterization. X-ray Diffraction (XRD), Rietveld Refinement, Scanning Electron Microscopy (SEM), Infrared-transform Fourier Spectroscopy (FTIR) and Thermal Analysis (TG/DSC) have been used for characterization of the extracted cellulose. XRD patterns of the in natura tucumã's endocarp has showed a natural crystalline content embedded in a non-crystalline matrix. Nanocrystals of cellulose have been observed in the XRD pattern of the extracted cellulose, showing a good agreement with type II. Rietveld refinement allowed the cell parameters obtainment (a = 8.43(1) Å, b = 9.50(1) Å, c = 9.39(3) Å and γ = 118.43(4)°). Apparent average crystallite size and microstrain were, respectively, 20.0 Å and 0.1%. Two different methods were applied for estimative of crystallinity percentage. In the first method the height ratio between the intensity of the crystalline peak and the total intensity after the subtraction of the non-crystalline content was applied, leading to 48.5%. The second approach was performed using the amorphous area and the total area of the (1 1 0) peak from the experimental diffractogram, leading to 31.5%. The difference in crystallinity percentage concerning these two used approaches may be explained due to the first method does not consider the broad peaks resulted from nanocrystals diffraction. FTIR spectroscopy has evidenced a cellulose type II structure. SEM images showed micrometric sized fibers with ranged thicknesses. However, a new morphology of spherical nanostructures was observed on the type II matrix fibers. Thermal analysis suggests that the extracted cellulose have low thermal stability, which resulted from poor ordered, packed chains. A large exothermic band was found in DSC curve and associated to the release of energy from the amorphous phase degradation. Thus, this work successfully extracted cellulose from tucumã's endocarp and allowed its structural, morphological and thermal characterization.

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

Luminescent properties under X-ray excitation of Ba(1-x)PbxWO4 disordered solid solution

NASA Astrophysics Data System (ADS)

Bakiz, B.; Hallaoui, A.; Taoufyq, A.; Benlhachemi, A.; Guinneton, F.; Villain, S.; Ezahri, M.; Valmalette, J.-C.; Arab, M.; Gavarri, J.-R.

2018-02-01

A series of polycrystalline barium-lead tungstate Ba1-xPbxWO4 with 0 ≤ x ≤ 1 was synthesized using a classical solid-state method with thermal treatment at 1000 °C. These materials were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), Fourier Transform Raman (FT-Raman) spectroscopy. X-ray diffraction profile analyses were performed using Rietveld method. These materials crystallized in the scheelite tetragonal structure and behaved as quasi ideal solid solution. Raman spectroscopy confirmed the formation of the solid solution. Structural distortions were evidenced in X-ray diffraction profiles and in vibration Raman spectra. The scanning electron microscopy experiments showed large and rounded irregular grains. Luminescence experiments were performed under X-ray excitation. The luminescence emission profiles have been interpreted in terms of four Gaussian components, with a major contribution of blue emission. The integrated intensity of luminescence reached a maximum value in the composition range x = 0.3-0.6, in relation with distortions of crystal lattice.

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

Investigation of microstructural and optical properties of La0.8Ca0.2FeO3 nanostructure synthesized via gel combustion method

NASA Astrophysics Data System (ADS)

Naseem, Swaleha; Ali, S. Asad; Khan, Wasi; Khan, Shakeel

2018-05-01

Ca substituted LaFeO3 orthoferrite nanostructure perovskite has been synthesized by gel combustion method using citric acid as a fuel. The structural and optical properties were investigated by various tools. The structural analysis through Rietveld refinement of the XRD data revealed single phase of orthorhombic structure in R-3c space group of the sample without presence of any other impurity phase. Scanning electron microscopy (SEM) image exhibits non-uniform distribution of the nanoparticles in agglomerated form. The purity of the sample and stoichiometric ratio of the elements were established through energy dispersive x-ray spectroscopy (EDS). FTIR spectroscopy measurement predicts the presence of various band relation of the chemical species of Ca with LaFeO3. Optical properties were explored through UV-visible absorption spectroscopy that showed absorption edge at 347 nm and energy band gap was estimated as 3.47eV using Tauc's relation.

Synthesis and characterization of Y2O3 nano-material: An experimental and theoretical study

NASA Astrophysics Data System (ADS)

Ahmad, Sheeraz; Faizan, Mohd; Ahmad, Shabbir; Ikram, Mohd

2018-04-01

We made an attempt to synthesize pure Y2O3 nanomaterial by using the sol-gel method followed by annealing at 600°C and 900°C. The synthesized Y2O3 nanoparticle was characterized by using XRD, FTIR, and UV-Vis spectroscopy. The structural refinement was performed using FULLPROF software by the Rietveld method. The refinement parameters such as lattice constant, atomic position, occupancy, R-factor and goodness of fit (χ2) were calculated. The nanoparticle has a single phase cubic structure with Ia -3 space group. The main absorption band in FTIR spectra centered at 560 cm-1 is attributed to Y-O vibration while the broadband at 3450 cm-1 arises due to O-H vibration. The band gap was obtained from the reflectance spectra using the K-M function F(R∞). The optimized structural parameters and UV-Vis spectrum were calculated using DFT and TD-DFT/B3LYP methods in bulk phase of Y2O3 and compared with experimental UV-Vis spectra in nanophase.

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

Synthesis and effect of Sr substitution on fluorescence of new Ba 2-xSr xZnS 3: Eu 2+ red phosphor: Considerable enhancement of emission intensity

NASA Astrophysics Data System (ADS)

Lee, Chi-Woo; Petrykin, Valery; Kakihana, Masato

2009-01-01

A series of 0.5 mol% Eu 2+-activated Ba 2-xSr xZnS 3 phosphor materials were synthesized using precursors prepared by the polymerizable complex method and their fluorescent properties were studied for the first time. It was found that Sr substitution for Ba leads to the considerable improvement of internal quantum efficiency and emission intensity in these materials compared to Ba 2ZnS 3, while emission peak wavelength exhibits a blue shift from 680 to 660 nm. Rietveld refinement of crystal structure of sample with x=0.7 suggests that Sr ions preferentially occupy one of two Ba sites in this compound. Such a structural re-arrangement might be responsible for the observed quantum efficiency dependence on Sr concentration.

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

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.

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

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.

The Effect of Multiple Shot Peening on the Corrosion Behavior of Duplex Stainless Steel

NASA Astrophysics Data System (ADS)

Feng, Qiang; She, Jia; Wu, Xueyan; Wang, Chengxi; Jiang, Chuanhai

2018-03-01

Various types of shot peening treatments were applied to duplex stainless steel. The effects of shot peening intensity and working procedures on the microstructure were investigated. The domain size and microstrain evolution in the surface layer were characterized utilizing the Rietveld method. As the shot peening intensity increased, the surface roughness increased in the surface layer; however, it decreased after multiple (dual and triple) shot peening. The mole fraction of strain-induced martensite as a function of the intensity of shot peening was evaluated by XRD measurements. Both potentiodynamic polarization curves and salt spray tests of shot-peened samples in NaCl solution were investigated. The results indicate that traditional shot peening has negative effects on corrosion resistance with increasing shot peening intensity; however, the corrosion rate can be reduced by means of multiple shot peening.

Electron Gyro-Harmonic Effects on Ionospheric Stimulated Brillouin Scatter

DTIC Science & Technology

2014-08-21

27709-2211 Brillouin, SBS, emission lines, pump frequency stepping, cyclotron , EIC, airglow, upper hybrid REPORT DOCUMENTATION PAGE 11. SPONSOR...direction and the background magnetic field vector, the excited electrostatic wave could be either ion acoustic (IA) or electrostatic ion cyclotron (EIC...A. Hedberg, B. Lundborg, P. Stubbe, H. Kopka, and M. T. Rietveld (1989), Stimulated electromagnetic emission near electron cyclotron harmonics in

High-pressure Phase Relation In The MgAl2O4-Mg2SiO4 System

NASA Astrophysics Data System (ADS)

Kojitani, H.; Hisatomi, R.; Akaogi, M.

2005-12-01

High-pressure and high-temperature experiments indicate that high-pressure phases of oceanic basalts contain Al-rich phases. MgAl2O4 with calcium ferrite-type crystal structure is considered as a main component of such the Al-rich phases. Since the calcium ferrite-type MgAl2O4 can be synthesized at only the maximum pressure of a Kawai-type high-pressure apparatus with tungsten carbide (WC) anvils, the amount of a synthesized sample is very limited. Therefore, the crystal structure of the calcium ferrite-type MgAl2O4 has been hardly known in detail due to these difficulties in sample synthesis. In our high-pressure experiments in the MgO-Al2O3-SiO2 system, it was shown that Mg2SiO4 component could be dissolved in the MgAl2O4 calcium ferrite. In this study, we tried to synthesize a single phase MgAl2O4 calcium ferrite sample and to make the Rietveld refinement of the XRD pattern of the sample. The high-pressure phase relations in the MgAl2O4-Mg2SiO4 system were studied to know the stability field of the MgAl2O4-Mg2SiO4 calcium ferrite solid solutions. Lattice parameters-composition relation of the MgAl2O4-Mg2SiO4 calcium ferrite solid solutions was also determined. High-pressure and high-temperature experiments were performed by using a Kawai-type high-pressure apparatus at Gakushuin University. WC anvils with truncated edge length of 1.5 mm were used. Heating was made by a Re heater. Temperature was measured by a Pt/Pt-13%Rh thermocouple. Starting materials for the phase relation experiments were the mixture of MgO, Al2O3 and SiO2 with bulk compositions of MgAl2O4:Mg2SiO4 = 90:10, 78:22, 70:30 and 50:50. The starting materials were held at 21-27 GPa and 1600 °C for 3 hours and then were recovered by the quenching method. The MgAl2O4 calcium ferrite sample for the Rietveld analysis was prepared by heating MgAl2O4 spinel at 27 GPa and about 2200 °C for one hour. Powder X-ray diffraction (XRD) profiles of obtained samples were measured by using a X-ray diffractometer at Gakushuin University (RINT 2500V, Cr Kα, 45 kV, 250 mA). Composition analysis of the recovered samples was made using SEM-DES. The RIETAN-2000 program was used to perform the Rietveld refinement. The results of the high-pressure phase relation experiments show that stability field of single phase of MgAl2O4-Mg2SiO4 solid solutions spreads at lower pressure than that of pure MgAl2O4 calcium ferrite. The lowest pressure at which the calcium ferrite solid solution can be synthesized is about 23 GPa. The maximum solubility of Mg2SiO4 component is about 35%. Lattice parameters of pure MgAl2O4 calcium ferrite were determined as a = 9.9495(6) Å, b = 8.6466(5) Å, c = 2.7901(2) Å ( Pbnm space group) by the Rietveld refinement. Obtained atomic positions for calcium ferrite-type MgAl2O4 are very similar to those of CaFe2O4 calcium ferrite. Lattice parameters of MgAl2O4-Mg2SiO4 calcium ferrite solid solutions with various compositions indicate that c-axis does not change with the composition and that a- and b-axes have a linear increase and decrease trend with increasing Mg2SiO4 component, respectively.

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 transport properties of double perovskite Dy{sub 2}NiMnO{sub 6}

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

Chanda, Sadhan, E-mail: sadhan.physics@gmail.com; Saha, Sujoy; Dutta, Alo

2015-02-15

Highlights: • Sol–gel citrate method is used to prepare the double perovskite Dy{sub 2}NiMnO{sub 6}. • Structure and dielectric relaxation of the sample are studied for nano and bulk phases. • The relaxation mechanism of the sample is modeled by Cole–Cole equation. • With increasing sintering temperature conductivity increases. • Electronic structures and magnetic properties have been studied by DFT calculations. - Abstract: The double perovskite oxide Dy{sub 2}NiMnO{sub 6} (DNMO) is synthesized in nano and bulk phase by the sol–gel citrate method. The Rietveld refinement of X-ray diffraction pattern of the sample at room temperature shows the monoclinic P2{submore » 1}/n phase. Dielectric relaxation of the sample is investigated in the impedance and electric modulus formalisms in the frequency range from 50 Hz to 1 MHz and in the temperature range from 253 to 415 K. The Cole–Cole model is used to explain the relaxation mechanism in DNMO. The frequency-dependent maxima in the imaginary part of impedance are found to obey an Arrhenius law with activation energy of 0.346 and 0.344 eV for nano and bulk DNMO, respectively. A significant increase in conductivity of bulk DNMO has been observed than that of the nanoceramic. Electronic structures and magnetic properties of DNMO have been studied by performing first principles calculation based on density functional theory.« less

Synthesis of LiFePO4/C composites based on natural iron stone using a sol gel method

NASA Astrophysics Data System (ADS)

Angela, Riyan; Islam, Humaatul; Sari, Vamellia; Latif, Chaironi; Zainuri, Mochamad; Pratapa, Suminar

2017-01-01

Synthesis of LiFePO4/C composites has been carried out using a sol gel method. The Fe precursor was made from a natural iron stone of Tanah Laut, South Kalimantan, while the other raw materials were commercial Li2CO3 powder and NH4H2PO4 powder with HCl and water as solvents. Citric acid was used as the carbon source in the synthesis. This study used a molar ratio of 1:1:2 for Li:Fe:P with variation of added citric acid of 1.5 and 2.5 g. The solutions were dried in air at 100°C. The dried powders were characterized using DSC-TGA and then calcined at 600 and 700°C under argon environment for 10 hours. The calcined powders were characterized by X-ray diffractometry (XRD), scanning electron microscopy-energy dispersive x-ray (SEM-EDX), and LCR meter. It was found that the samples contained LiFePO4 as the dominant phase and LiFeP2O7 and Fe2O3 as secondary phases. The analysis showed that the addition of citric acid influenced the electronic conductivity of the composites. A Rietveld relative weight fraction of up to 94.7% was achieved in the synthesis at temperature 600°C. The LFP/C sample exhibited electronic conductivity of 4.56×10-3 Scm-1 which was six times of that of the pure LFP.

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

Tunable Luminescence in Sr2MgSi2O7:Tb3+, Eu3+Phosphors Based on Energy Transfer

PubMed Central

Li, Minhong; Wang, Lili; Ran, Weiguang; Deng, Zhihan; Shi, Jinsheng; Ren, Chunyan

2017-01-01

A series of Tb3+, Eu3+-doped Sr2MgSi2O7 (SMSO) phosphors were synthesized by high temperature solid-state reaction. X-ray diffraction (XRD) patterns, Rietveld refinement, photoluminescence spectra (PL), and luminescence decay curves were utilized to characterize each sample’s properties. Intense green emission due to Tb3+ 5D4→7F5 transition was observed in the Tb3+ single-doped SMSO sample, and the corresponding concentration quenching mechanism was demonstrated to be a diople-diople interaction. A wide overlap between Tb3+ emission and Eu3+ excitationspectraresults in energy transfer from Tb3+ to Eu3+. This has been demonstrated by the emission spectra and decay curves of Tb3+ in SMSO:Tb3+, Eu3+ phosphors. Energy transfer mechanism was determined to be a quadrupole-quadrupole interaction. And critical distance of energy transfer from Tb3+ to Eu3+ ions is calculated to be 6.7 Å on the basis of concentration quenching method. Moreover, white light emission was generated via adjusting concentration ratio of Tb3+ and Eu3+ in SMSO:Tb3+, Eu3+ phosphors. All the results indicate that SMSO:Tb3+, Eu3+ is a promising single-component white light emitting phosphor. PMID:28772587

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.

X-ray and dielectric characterization of Co doped tetragonal BaTiO3 ceramics

NASA Astrophysics Data System (ADS)

Bujakiewicz-Koronska, R.; Vasylechko, L.; Markiewicz, E.; Nalecz, D. M.; Kalvane, A.

2017-01-01

The crystal structure modifications of BaTiO3 induced by cobalt doping were studied. The polycrystalline (1 - x)BaTiO3 + xCo2O3 samples, with x ≤ 10 wt.%, were prepared by high temperature sintering conventional method. According to X-ray phase and structural characterization, performed by full-profile Rietveld refinement technique, all synthesized samples showed tetragonal symmetry perovskite structure with minor amount of parasitic phases. Pure single-phase composition has been detected only in the low level of doping BaTiO3. It was indicated that substitution of Co for the Ti sites in the (1 - x)BaTiO3 + xCo2O3 series led to decrease of tetragonality (c/a) of the BaTiO3 perovskite structure. This effect almost vanished in the (1 - x)BaTiO3 + xCo2O3 samples with nominal Co content higher than ∼1 wt.%, in which precipitation of parasitic Co-containing phases CoO and Co2TiO4 has been observed. Based on the results, the solubility limit of Co in Ti sub-lattice in the (1 - x)BaTiO3 + xCo2O3 series is estimated as x = 0.75 wt.%.

Novel ultra-low temperature co-fired microwave dielectric ceramic at 400 degrees and its chemical compatibility with base metal

PubMed Central

Di, Zhou; Li-Xia, Pang; Ze-Ming, Qi; Biao-Bing, Jin; Xi, Yao

2014-01-01

A novel NaAgMoO4 material with spinel-like structure was synthesized by using the solid state reaction method and the ceramic sample was well densified at an extreme low sintering temperature about 400°C. Rietveld refinement of the crystal structure was performed using FULLPROF program and the cell parameters are a = b = c = 9.22039 Å with a space group F D −3 M (227). High performance microwave dielectric properties, with a permittivity ~7.9, a Qf value ~33,000 GHz and a temperature coefficient of resonant frequency ~−120 ppm/°C, were obtained. From X-ray diffraction (XRD) and Energy Dispersive Spectrometer (EDS) analysis of the co-fired sample, it was found that the NaAgMoO4 ceramic is chemically compatible with both silver and aluminum at the sintering temperature and this makes it a promising candidate for the ultra-low temperature co-fired ceramics technology. Analysis of infrared and THz spectra indicated that dielectric polarizability at microwave region of the NaAgMoO4 ceramic was equally contributed by ionic displasive and electronic polarizations. Its small microwave dielectric permittivity can also be explained well by the Shannon's additive rule. PMID:25099530

Cation distribution correlated with magnetic properties of cobalt ferrite nanoparticles defective by vanadium doping

NASA Astrophysics Data System (ADS)

Heiba, Zein K.; Mohamed, Mohamed Bakr; Ahmed, S. I.

2017-11-01

Nanoparticles cobalt ferrite, vacancies defective through vanadium substitution for iron, were synthesized by a sol-gel method. Two systems CoFe2-xVxO4 (0.0 ≤ x ≤ 0.25) and CoFe2-1.67xVxO4 (x = 0.1, 0.2) were prepared. The crystal structure, microstructure and magnetic properties were investigated using XRD, SEM and VSM magnetometer. The occupancy of tetrahedral and octahedral sites by different cations was determined by Rietveld analysis and correlated with magnetic measurements. Vanadium resides at octahedral sites up to x = 0.10, while for higher values it resides mainly at octahedral sites with a lesser amount at the tetrahedrons. Upon increasing the vanadium content, the cell parameter decreases and the bond lengths of the tetrahedral and octahedral sites change opposite to each other. The change in the coercivity and saturation magnetization is correlated with cation distribution. For the same amount of doping x, the iron deficient samples CoFe2-1.67xVxO4 have saturation magnetization obviously reduced than the corresponding samples in CoFe2-xVxO4. The spin canting between cations in A- and B- sites was discussed in details based on Yafet-Kittel triangular arrangement model.

Calcio-olivine γ-Ca2SiO4: I. Rietveld refinement of the crystal structure

NASA Astrophysics Data System (ADS)

Gobechiya, E. R.; Yamnova, N. A.; Zadov, A. E.; Gazeev, V. M.

2008-05-01

The structure of the natural mineral calcio-olivine (γ-Ca2SiO4) found in skarn xenoliths in the region of the Lakargi Mountain (North Caucasus, Kabardino-Balkaria, Russia) is refined by the Rietveld method [ a = 5.07389(7) Å, b = 11.21128(14) Å, c = 6.75340(9) Å, V = 384.170(5) Å3, Z = 4, ρcalcd = 2.98 g/cm3, space group Pbnm]. The X-ray diffraction pattern of a powdered sample is recorded on a STOE STADI MP diffractometer [λCu K α1; Ge(111) primary monochromator; 6.00° < 2θ < 100.88°; step width, 2.5° in 2θ; number of reflections, 224]. All calculations are performed with the WYRIET (version 3.3) software package. The structural model is refined in the anisotropic approximation to R p = 6.44, R wp = 8.52, R exp = 5.85, R B = 4.98, R F = 6.90, and s = 1.46. It is shown that the sample under investigation is a mixture of several mineral phases, among which calcio-olivine (the natural analogue of the γ-Ca2SiO4 compound) (83%), hillebrandite (13%), and wadalite (4%) are dominant. Only the scale factors and the unit cell parameters are refined for hillebrandite Ca2SiO3(OH)2 [ a = 3.63472(16) Å, b = 16.4140(10) Å, c = 11.7914(8) Å, space group Cmc21, Z = 6] and wadalite Ca6Al5Si2O16Cl3 ( a = 12.0088 Å, space group, I bar 4 3 d Z = 4). The results of the structure refinement of the main component of the sample confirm that the mineral calcio-olivine is isostructural to the synthetic compound γ-Ca2SiO4. The structure of this compound is formed by the heteropolyhedral framework composed of Ca octahedra joined together into olivine-like ribbons and isolated Si tetrahedra.

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

Pratapa, S.; Susanti, L.; Insany, Y. A. S.

Simple coprecipitation method has been used to produce nanoparticles of MgO (magnesia), MgO{center_dot}Al{sub 2}O{sub 3}(spinel), Y{sub 2}O{sub 3}(yttria) and Fe{sub 3}O{sub 4}(ferrite). The raw materials were, in respective, magnesium powder, magnesium and aluminium powders, ytrria powder, and natural sand. The coprecipitation included the use of suitable acid and base to dissolve the powders or sand and to produce precipitates, as well as the use of water to wash and purify the precipitates, and drying at relatively low temperatures, namely lower than 100 deg. C, followed by heating at 450 deg. C, 750 deg. C, 600 deg. C and 200 deg.more » C to produce magnesia, spinel, yttria and ferrite nanopowders, respectively. X-ray diffractometry was used to characterise the purity and nanocrystallinity of the final powders. It was found qualitatively that the powders were of high purity. Further line-broadening analysis using single-line and Rietveld-based softwares was performed to reveal the nanocrystallinity of the powders. Different line breadth values were found for the powders, indicating different crystallite sizes. It was also found that, particularly for spinel and yttria, the diffraction peaks exhibited 'longer' tails, indicating broader crystallite size distribution. The average crystallite size for the powders ranged from 3 to 70 nm. The results could then be used as 'fingerprints' for nanocrystallinity using x-ray diffractometry. The XRD crystallite sizes for yttria and ferrite nanocrystals are in fair agreement with their counterparts from electron microscopy observation.« less

Photoelectrochemical water splitting with mesoporous hematite prepared by a solution-based colloidal approach.

PubMed

Sivula, Kevin; Zboril, Radek; Le Formal, Florian; Robert, Rosa; Weidenkaff, Anke; Tucek, Jiri; Frydrych, Jiri; Grätzel, Michael

2010-06-02

Sustainable hydrogen production through photoelectrochemical water splitting using hematite (alpha-Fe(2)O(3)) is a promising approach for the chemical storage of solar energy, but is complicated by the material's nonoptimal optoelectronic properties. Nanostructuring approaches have been shown to increase the performance of hematite, but the ideal nanostructure giving high efficiencies for all absorbed light wavelengths remains elusive. Here, we report for the first time mesoporous hematite photoelectodes prepared by a solution-based colloidal method which yield water-splitting photocurrents of 0.56 mA cm(-2) under standard conditions (AM 1.5G 100 mW cm(-2), 1.23 V vs reversible hydrogen electrode, RHE) and over 1.0 mA cm(-2) before the dark current onset (1.55 V vs RHE). The sintering temperature is found to increase the average particle size, and have a drastic effect on the photoactivity. X-ray photoelectron spectroscopy and magnetic measurements using a SQUID magnetometer link this effect to the diffusion and incorporation of dopant atoms from the transparent conducting substrate. In addition, examining the optical properties of the films reveals a considerable change in the absorption coefficient and onset properties, critical aspects for hematite as a solar energy converter, as a function of the sintering temperature. A detailed investigation into hematite's crystal structure using powder X-ray diffraction with Rietveld refinement to account for these effects correlates an increase in a C(3v)-type crystal lattice distortion to the improved optical properties.

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.

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.

Structural, optical and dielectric properties of Sn0.97Ce0.03O2 nanostructures

NASA Astrophysics Data System (ADS)

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

2018-05-01

In present work, 3% cerium doped SnO2 (Sn0.97Ce0.03O2) nanoparticles (NPs) have been synthesized by sol-gel method. The prepared sample has been characterized by using various techniques such as XRD, UV-visible absorption spectroscopy and LCR meter measurements. Structural Rietveld refinement of XRD data reveals that (Sn0.97Ce0.03O2) sample has a pure single phase tetragonal structure with space group (P42/mnm) without creating any impurity phase such as cerium oxide. UV-visible spectroscopy determines band gap value 3.47 eV for (Sn0.97Ce0.03O2) NPs using Tauc's relation. Dielectric constant and loss decreased with increase in frequency while ac conductivity was found to increase with increase in frequency. The observed dielectric results has been explained in the light of Maxwell-Wagner model.

Advanced setup for high-pressure and low-temperature neutron diffraction at hydrostatic conditions

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

Lokshin, Konstantin A.; Zhao Yusheng

2005-06-15

We describe a design of the experimental setup for neutron diffraction studies at low temperatures and hydrostatic pressure. The significant benefit of the setup, compared to the previous methods, is that it makes possible the simultaneous collection of neutrons diffracted at the 30 deg. -150 deg. range with no contamination by the primary scattering from the sample surroundings and without cutting out the incident and diffracted beams. The suggested design is most useful for third-generation time-of-flight diffractometers and constant wavelength instruments. Application of the setup expands the capabilities of high-pressure neutron diffraction, allowing time-resolved kinetics and structural studies, multihistogram Rietveld,more » and pair distribution function and texture analyses. The high efficiency of the setup was proven for the HIPPO diffractometer at Los Alamos Neutron Science Center under pressures up to 10 kbar and temperatures from 4 to 300 K.« 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.

Hydrolysis of dilute acid-pretreated cellulose under mild hydrothermal conditions.

PubMed

Chimentão, R J; Lorente, E; Gispert-Guirado, F; Medina, F; López, F

2014-10-13

The hydrolysis of dilute acid-pretreated cellulose was investigated in a conventional oven and under microwave heating. Two acids--sulfuric and oxalic--were studied. For both hydrothermal conditions (oven and microwave) the resultant total organic carbon (TOC) values obtained by the hydrolysis of the cellulose pretreated with sulfuric acid were higher than those obtained by the hydrolysis of the cellulose pretreated with oxalic acid. However, the dicarboxylic acid exhibited higher hydrolytic efficiency towards glucose. The hydrolysis of cellulose was greatly promoted by microwave heating. The Rietveld method was applied to fit the X-ray patterns of the resultant cellulose after hydrolysis. Oxalic acid preferentially removed the amorphous region of the cellulose and left the crystalline region untouched. On the other hand, sulfuric acid treatment decreased the ordering of the cellulose by partially disrupting its crystalline structure. Copyright © 2014 Elsevier Ltd. All rights reserved.

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.

Quantitative analysis of carbides and the sigma phase in thermally exposed GTD-111

NASA Astrophysics Data System (ADS)

Lee, Han-sang; Kim, Doo-soo; Yoo, Keun-bong; Song, Kyu-so

2012-04-01

The effects of thermal exposure on γ', carbides and TCP-type phases, such as the sigma and eta phases, in the nickel-based superalloy GTD-111 were investigated in this study. The thermal exposure was performed at 871 °C and 982 °C for 1,000, 5,000 and 10,000 h, after which the thermally exposed specimens were compared in terms of their microstructure, weight fraction and growth rate of each precipitate. Electrolytic extraction and Rietveld refinement were successfully applied for a quantitative analysis of the carbides and the sigma phase in the thermally exposed GTD-111. The weight fractions of MC, Cr-rich M23C6 and the sigma phase for various thermal exposure times and temperatures were obtained to understand the formation and decomposition rate of each phase.

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.

Lithium ion insertion and extraction reactions with Hollandite-type manganese dioxide free from any stabilizing cations in its tunnel cavity

NASA Astrophysics Data System (ADS)

Kijima, Norihito; Takahashi, Yasuhiko; Akimoto, Junji; Awaka, Junji

2005-09-01

Lithium ion insertion and extraction reactions with a hollandite-type α-MnO 2 specimen free from any stabilizing cations in its tunnel cavity were investigated, and the crystal structure of a Li+-inserted α-MnO 2 specimen was analyzed by Rietveld refinement and whole-pattern fitting based on the maximum-entropy method (MEM). The pH titration curve of the α-MnO 2 specimen displayed a monobasic acid behavior toward Li+, and an ion-exchange capacity of 3.25 meq/g was achieved at pH>11. The Li/Mn molar ratio of the Li+-inserted α-MnO 2 specimen showed that about two Li+ ions can be chemically inserted into one unit cell of the hollandite-type structure. As the amount of Li content was increased, the lattice parameter a increased while c hardly changed. On the other hand, the mean oxidation number of Mn decreased slightly regardless of Li content whenever ions were exchanged. The Li+-inserted α-MnO 2 specimen reduced topotactically in one phase when it was used as an active cathode material in a liquid organic electrolyte (1:1 EC:DMC, 1 mol/dm 3 LiPF 6) lithium cell. An initial discharge with a capacity of approximately 230 mAh/g was achieved, and the reaction was reversible, whereas the capacity fell steadily upon cycling. About six Li+ ions could be electrochemically inserted into one unit cell of the hollandite-type structure. By contrast, the parent α-MnO 2 specimen showed a poor discharge property although no cationic residues or residual H 2O molecules remained in the tunnel space. Rietveld refinement from X-ray powder diffraction data for a Li+-inserted specimen of (Li 2O) 0.12MnO 2 showed it to have the hollandite-type structure (tetragonal; space group I4/m; a=9.993(11) and c=2.853(3) Å; Z=8; Rwp=6.12%, Rp=4.51%, RB=1.41%, and RF=0.79%; S=1.69). The electron-density distribution images in (Li 2O) 0.12MnO 2 showed that Li 2O molecules almost fill the tunnel space. These findings suggest that the presence of stabilizing atoms or molecules within the tunnel of a hollandite-type structure is necessary to facilitate the diffusion of Li+ ions during cycling.

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.

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

Structure and decomposition of the silver formate Ag(HCO{sub 2})

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

Puzan, Anna N., E-mail: anna_puzan@mail.ru; Baumer, Vyacheslav N.; Mateychenko, Pavel V.

Crystal structure of the silver formate Ag(HCO{sub 2}) has been determined (orthorhombic, sp.gr. Pccn, a=7.1199(5), b=10.3737(4), c=6.4701(3)Å, V=477.88(4) Å{sup 3}, Z=8). The structure contains isolated formate ions and the pairs Ag{sub 2}{sup 2+} which form the layers in (001) planes (the shortest Ag–Ag distances is 2.919 in the pair and 3.421 and 3.716 Å between the nearest Ag atoms of adjacent pairs). Silver formate is unstable compound which decompose spontaneously vs time. Decomposition was studied using Rietveld analysis of the powder diffraction patterns. It was concluded that the diffusion of Ag atoms leads to the formation of plate-like metal particlesmore » as nuclei in the (100) planes which settle parallel to (001) planes of the silver formate matrix. - Highlights: • Silver formate Ag(HCO{sub 2}) was synthesized and characterized. • Layered packing of Ag-Ag pairs in the structure was found. • Decomposition of Ag(HCO{sub 2}) and formation of metal phase were studied. • Rietveld-refined micro-structural characteristics during decomposition reveal the space relationship between the matrix structure and forming Ag phase REPLACE with: Space relationship between the matrix structure and forming Ag phase.« 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.

Synthesis and characterization of TiC nanopowders via sol-gel and subsequent carbothermal reduction process

NASA Astrophysics Data System (ADS)

Chen, Xu; Fan, Jinglian; Lu, Qiong

2018-06-01

TiC nanocrystalline powders were synthesized by in-situ carbothermic reduction of Ti-O-C precursor under vacuum atmosphere. And the Ti-O-C precursor was formed by sol-gel method from titanium butyrate (TBOT) and sucrose. To obtain stable sol, TBOT was directly added into mixed solution which contains water, sucrose, acetic acid (AcOH) and acetylacetone (ACAC). This procedure is more convenient and economical because it avoids the use of alcohol which is used as solvent in most reports of alkoxide hydrolysis sol-gel method. TG-DSC, XRD, FTIR and SEM/TEM were employed to analyze and characterize the product during the entire process. The phase composition and crystalline structure parameters of powders with different C/Ti molar ratio were investigated by Rietveld refinement method, and elemental quantitative analysis of the samples were performed. Furthermore, the optimal parameters of carbothermal reduction were obtained and the grain growth mechanism was demonstrated. The results show that TiC nanocrystalline powders (C/Ti molar ratio is 3.5 in the precursor) were synthesized at 1300 °C for 2 h, which have near standard lattice parameter, well crystallinity and fine average grain size ( 37.4 nm).

X-ray and neutron total scattering analysis of Hy·(Bi0.2Ca0.55Sr0.25)(Ag0.25Na0.75)Nb3O10·xH2O perovskite nanosheet booklets with stacking disorder

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

Metz, Peter; Koch, Robert; Cladek, Bernadette

Ion-exchanged Aurivillius materials form perovskite nanosheet booklets wherein well-defined bi-periodic sheets, with ~11.5 Å thickness, exhibit extensive stacking disorder. The perovskite layer contents were defined initially using combined synchrotron X-ray and neutron Rietveld refinement of the parent Aurivillius structure. The structure of the subsequently ion-exchanged material, which is disordered in its stacking sequence, is analyzed using both pair distribution function (PDF) analysis and recursive method simulations of the scattered intensity. Combined X-ray and neutron PDF refinement of supercell stacking models demonstrates sensitivity of the PDF to both perpendicular and transverse stacking vector components. Further, hierarchical ensembles of stacking models weightedmore » by a standard normal distribution are demonstrated to improve PDF fit over 1–25 Å. Recursive method simulations of the X-ray scattering profile demonstrate agreement between the real space stacking analysis and more conventional reciprocal space methods. The local structure of the perovskite sheet is demonstrated to relax only slightly from the Aurivillius structure after ion exchange.« less

Biosynthesised ZnO : Dy3+ nanoparticles: Biodiesel properties and reusable catalyst for N-formylation of aromatic amines with formic acid

NASA Astrophysics Data System (ADS)

Reddy Yadav, L. S.; Raghavendra, M.; Sudheer Kumar, K. H.; Dhananjaya, N.; Nagaraju, G.

2018-04-01

ZnO nanoparticles doped with trivalent dysprosium ions (Dy3+) were prepared through the green combustion technique using E. tirucalli plant latex as a fuel. The fundamental and optical properties of the samples are examined via the X-ray diffraction, FTIR, UV-visible analytical methods and morphology by scanning electron microscope and transmission electron microscope. Rietveld refinement results show that the ZnO : Dy3+ were crystallized in the wurtzite hexagonal structure with space group P63mc (No. 186). The average particle size of ZnO : Dy3+ prepared with the different concentration of latex was found to be in the range 30-38nm, which is also confirmed by TEM analysis. A rapid and convenient method for the one-pot preparation of N-formamide derivatives aromatic amines and amino acid esters has been developed using Dy3+ doped ZnO as a catalytic agent. This method provides an efficient and much improved modification over reported protocols regarding yield, clean and work-up procedure milder reaction conditions. In this work, Pongamiapinnata oil was recycled for the preparation of biodiesel via Dy3+ doped ZnO as a catalytic agent.

Zeta potential study of Sb2S3 nanoparticles synthesized by a facile polyol method in various surfactants

NASA Astrophysics Data System (ADS)

Saxena, Monika; Okram, Gunadhor Singh

2018-05-01

In the present work, we report the successful synthesis of stibnite Sb2S3 nanoparticles (NPs) by a facile polyol method using various surfactant. The structural and optical properties were investigated by X-ray diffraction (XRD), Raman spectroscopy and Zeta potential. Rietveld refinement of XRD data confirms the single phase orthorhombic crystal structure of stibnite Sb2S3. Presence of six obvious Raman modes further confirmed their stoichiometric formation. Effect of different surfactants on the surface charge of Sb2S3 NPs was studied using Zeta potential measurement in deionized water at different pH values. They reveal that these NPs are more stable when it was synthesized in presence of EDTA than that of CTAB or without surfactant samples with high zeta potential. The isoelectronic point was found at pH = 6.4 for pure sample, 3.5 and 7.2 for CTAB and not found for EDTA Sb2S3 samples. This information can be useful for many industrial applications like pharmaceuticals, ceramics, waste water treatment and medicines.

Magnetic transition in Y-site doped multiferroic YMnO3

NASA Astrophysics Data System (ADS)

Thakur, Rajesh K.; Thakur, Rasna; Gaur, N. K.

2016-05-01

We have synthesized polycrystalline hexagonal Y1-xSrxMnO3 (x=0.02, 0.1) compounds by using conventional solid state reaction method. The detailed structural investigations are carried out by using XRD studies which reveals the single phase formation of the reported compounds with hexagonal structure and space group P63cm (JCPDS: 25-1079). Further the XRD data of reported compounds were analyzed by RIETVELD (FULLPROFF) method which shows the decrease in the lattice parameter with increasing concentration of divalent strontium to Y-site. The observed pointed kinks in the specific heat study are indicative of the probable coupling in between the electric and magnetic orders in this class of materials. The reported systematic specific heat studies shows that the antiferromagnetic (AFM) transition temperature (TN) shifts to higher value with increasing concentration of Sr2+ ion in the YMnO3 compound which is attributed to the enhanced lattice contribution to the specific heat in the this compound. The present compound shows the independence of specific heat and magnetic transition temperature with applied magnetic field of 8T and 12T.

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.

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

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

Thermal expansion in UO 2 determined by high-energy X-ray diffraction

DOE PAGES

Guthrie, M.; Benmore, C. J.; Skinner, L. B.; ...

2016-06-24

In this study, we present crystallographic analyses of high-energy X-ray diffraction data on polycrystalline UO 2 up to the melting temperature. The Rietveld refinements of our X-ray data are in agreement with previous measurements, but are systematically located around the upper bound of their uncertainty, indicating a slightly steeper trend of thermal expansion compared to established values. This observation is consistent with recent first principles calculations.

Synthesis and magnetic properties of LiFePO4 substitution magnesium

NASA Astrophysics Data System (ADS)

Choi, Hyunkyung; Kim, Min Ji; Hahn, Eun Joo; Kim, Sam Jin; Kim, Chul Sung

2017-06-01

LiFe0.9Mg0.1PO4 sample was prepared by using a solid-state reaction method, and the temperature-dependent magnetic properties of the sample were studied. The X-ray diffraction (XRD) pattern showed an olivine-type orthorhombic structure with space group Pnma based on Rietveld refinement method. The effect of Mg substitution in antiferromagnetic LiFe0.9Mg0.1PO4 was investigated using a vibrating sample magnetometer (VSM) and Mössbauer spectroscopy. The temperature-dependence of the magnetization curves of LiFe0.9Mg0.1PO4 shows abnormal antiferromagnetic behavior with ordering temperature. Sudden changes in both the magnetic hyperfine field (Hhf) and its slope below 15 K suggest that magnetic phase transition associated to the abrupt occurrence of spin-reorientation. The Néel temperature (TN) and spin-reorientation temperature (TS) of LiFe0.9Mg0.1PO4 are lower than those of pure LiFePO4 (TN = 51 K, TS = 23 K). This is due to the Fe-O-Fe superexchange interaction being larger than that of the Fe-O-Mg link. Also, we have confirmed a change in the electric quadrupole splitting (ΔEQ) by the spin-orbit coupling effect and the shape of Mössbauer spectrum has provided the evidence for TS and a strong crystalline field. We have found that Mg ions in LiFe0.9Mg0.1PO4 induce an asymmetric charge density due to the presence of Mg2+ ions at the FeO6 octahedral sites.

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

Garlea, Elena; Steiner, M. A.; Calhoun, C. A.

The α-phase transformation kinetics of as-cast U - 8 wt% Mo below the eutectoid temperature have been established by in situ neutron diffraction. α-phase weight fraction data acquired through Rietveld refinement at five different isothermal hold temperatures can be modeled accurately utilizing a simple Johnson-Mehl-Avrami-Kolmogorov impingement-based theory, and the results are validated by a corresponding evolution in the γ-phase lattice parameter during transformation that follows Vegard’s law. Neutron diffraction data is used to produce a detailed Time-Temperature-Transformation diagram that improves upon inconsistencies in the current literature, exhibiting a minimum transformation start time of 40 min at temperatures between 500 °Cmore » and 510 °C. Lastly, the transformation kinetics of U – 8 wt% Mo can vary significantly from as-cast conditions after extensive heat treatments, due to homogenization of the typical dendritic microstructure which possesses non-negligible solute segregation.« less

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.

4d Electronic structure analysis of ruthenium in the perovskite oxides by Ru K- and L-edge XAS.

PubMed

Kim, J Y; Hwang, S H; Kim, S J; Demazeau, G; Choy, J H; Shimada, H

2001-03-01

The 4d electronic structure of ruthenium in the perovskite oxides, La2MRuIVO6 (M = Zn, Mg, and Li) and Ba2YRuVO6, has been investigated by the Ru K-and L-edge XANES and EXAFS analyses. Such X-ray absorption spectroscopic results clarify that the RuIV (d4) and RuV (d3) ions are stabilized in nearly regular Oh site. Comparing the Ru L-edge XANES spectra of perovskites containing isovalent ruthenium, it has been found that the t2g state is mainly influenced by A site cation, whereas the eg is mainly affected by neighboring B site cation. The experimental EXAFS spectra in the range of R < or = approximately 4.5 A are well reproduced by ab-initio calculation based on crystallographic data, which supports the long-range structure presented by Rietveld refinement.

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.

Large scale synthesis of nanostructured zirconia-based compounds from freeze-dried precursors

NASA Astrophysics Data System (ADS)

Gómez, A.; Villanueva, R.; Vie, D.; Murcia-Mascaros, S.; Martínez, E.; Beltrán, A.; Sapiña, F.; Vicent, M.; Sánchez, E.

2013-01-01

Nanocrystalline zirconia powders have been obtained at the multigram scale by thermal decomposition of precursors resulting from the freeze-drying of aqueous acetic solutions. This technique has equally made possible to synthesize a variety of nanostructured yttria or scandia doped zirconia compositions. SEM images, as well as the analysis of the XRD patterns, show the nanoparticulated character of those solids obtained at low temperature, with typical particle size in the 10-15 nm range when prepared at 673 K. The presence of the monoclinic, the tetragonal or both phases depends on the temperature of the thermal treatment, the doping concentration and the nature of the dopant. In addition, Rietveld refinement of the XRD profiles of selected samples allows detecting the coexistence of the tetragonal and the cubic phases for high doping concentration and high thermal treatment temperatures. Raman experiments suggest the presence of both phases also at relatively low treatment temperatures.

Effect of partial nitridation on the structure and luminescence properties of melilite-type Ca2Al2SiO7:Eu2+ phosphor

NASA Astrophysics Data System (ADS)

Luo, Yi; Xia, Zhiguo

2014-09-01

Ca1.97Al2-xSi1+xO7-xNx:0.03Eu2+ (x = 0-0.4) phosphors have been prepared by using the high temperature solid-state reaction. The effect of phase structures, photoluminescence (PL) properties and the thermal stabilities have been investigated based on the substitution of Al-O bond in Ca2Al2SiO7:Eu2+ phosphor with Si-N bond. The XRD Rietveld refinement and 29Si NMR analysis results verify the introduction of partial Si-N bonds. It is found that the PL spectra shift to the blue region abnormally from 530 to 515 nm, and the possible mechanism has been proposed. The activation energy becomes large along with the nitridation process, which coincides with the explanation of configuration coordinate diagram.

Na-doped La0.7Ca0.3MnO3 compounds exhibiting a large magnetocaloric effect near room temperature

NASA Astrophysics Data System (ADS)

Chi Linh, Dinh; Thi Ha, Nguyen; Huu Duc, Nguyen; Giang Nam, Le Huu; Bau, Le Viet; Manh An, Nguyen; Yu, Seong-Cho; Dang Thanh, Tran

2018-03-01

In this work, we have investigated the magnetic properties and the magnetocaloric effect of La0.7-xNaxCa0.3MnO3 compounds, which were prepared by a conventional solid-state reaction technique. The Rietveld refinement results suggested that the samples are single phase belonging to an orthorhombic structure (space group Pnma). Analyzing temperature dependence of magnetization M(T) revealed that the Curie temperature (TC) increases with increasing Na content (x). Their TC value is found to be 260-298 K for x=0.0-0.1, respectively. Base on M(T) data measured at different applied magnetic fields (H), temperature dependence of magnetic entropy change ΔSm(T) data for all the samples was calculated by using a phenomenological model. In the vicinity of TC, -ΔSm(T) curve reaches a maximum value (denoted as |ΔSmax|), which gradually increases with increasing H. Under 12 kOe, the value of |ΔSmax| is in a range of 1.47-5.19 J/kg K corresponding to the relative cooling power RCP=57.12-75.88 J/kg. Applied the universal master curve method for the magnetic entropy change, we concluded that Na-doped in La0.7-xNaxCa0.3MnO3 compounds leads to modification the nature of the magnetic phase transition from the first- to the second-order.

Formation of TbCu7-type CeFe10Zr0.8 by rapid solidification

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

Zhou, C; Pinkerton, FE; Herbst, JF

2013-08-25

We report the discovery of a new ternary compound prepared by melt spinning induction melted ingot of nominal composition CeFe11Zr. The sample melt spun at v(s) = 25 m/s exhibits the hexagonal TbCu7-type structure of space group P6/mmm. Through fitting the experimental X-ray diffraction pattern by Rietveld method, we have successfully derived the crystal structure of the new compound melt spun at v(s) = 25 m/s to be CeFe10Zr0.8. Subsequent density function theory calculation fully supports the chemical stability of the new ternary compound. Annealing test showed that the melt spun CeFe10Zr0.8 is stable up to 700 degrees C andmore » annealing at higher temperature would cause it to decompose into hexagonal Ce2Fe17-type structure and ZrFe2. The Curie temperature measurement found that CeFe10Zr0.8 boasts a T-c = 181 degrees C, which is higher than the Tc values of all known Ce-Fe binary compounds, and 30 degrees C higher than that of Ce2Fe14B. These interesting properties stimulate continued search for new Ce-based permanent magnets that could be a cost effective solution to engineering needs in the future. (c) 2013 Elsevier B.V. All rights reserved.« less

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.

Influence of Carbon Nanotubes on the Structure Formation of Cement Matrix

NASA Astrophysics Data System (ADS)

Petrunin, S.; Vaganov, V.; Reshetniak, V.; Zakrevskaya, L.

2015-11-01

The potential of application of CNTs as a reinforcing agent in cement composites is governed by their unique mechanical and electronic properties. The analysis of concrete strength changes under CNTs introduction shows non-uniformity and sometimes inconsistency of results. Due to the fact that CNTs influence the hydration kinetics, structure and phase composition of concrete, an idea concerning the importance of interaction between the surface of CNTs and hydrate ions formed by the dissolution of the clinker phases has been suggested. In this paper, the theoretical and experimental study of interaction between hydrate ions and CNTs surface is discussed. Reference nanotubes and nanotubes functionalized by carboxylic groups are used in this research. Phase composition was determined by X-Ray analysis according to the Rietveld method. It was found that the presence of oxygen-containing functional groups on CNTs surface leads to intensification of the hydration process and increase in concentration of C-S-H gel from 65.9% to 74.4%. Special attention is usually paid to interactions between Ca2+ ions and CNTs, because the hardening rate and structure of cement stone are determined by principle of Ca2+ localization in the solution. In this paper the possible binding mechanisms are discussed. Based on the experimental results, the hypothesis regarding the formation of cement composite structure for different CNTs surface functionalizations is considered. According to this hypothesis, the CNTs act as the centers of crystallization for hydration products contributing to the acceleration of hydration, increase of the concentration of C-S-H gel and strength improvement of CNTs based composites.

Metallic-covalent bonding conversion and thermoelectric properties of Al-based icosahedral quasicrystals and approximants.

PubMed

Takagiwa, Yoshiki; Kimura, Kaoru

2014-08-01

In this article, we review the characteristic features of icosahedral cluster solids, metallic-covalent bonding conversion (MCBC), and the thermoelectric properties of Al-based icosahedral quasicrystals and approximants. MCBC is clearly distinguishable from and closely related to the well-known metal-insulator transition. This unique bonding conversion has been experimentally verified in 1/1-AlReSi and 1/0-Al 12 Re approximants by the maximum entropy method and Rietveld refinement for powder x-ray diffraction data, and is caused by a central atom inside the icosahedral clusters. This helps to understand pseudogap formation in the vicinity of the Fermi energy and establish a guiding principle for tuning the thermoelectric properties. From the electron density distribution analysis, rigid heavy clusters weakly bonded with glue atoms are observed in the 1/1-AlReSi approximant crystal, whose physical properties are close to icosahedral Al-Pd-TM (TM: Re, Mn) quasicrystals. They are considered to be an intermediate state among the three typical solids: metals, covalently bonded networks (semiconductor), and molecular solids. Using the above picture and detailed effective mass analysis, we propose a guiding principle of weakly bonded rigid heavy clusters to increase the thermoelectric figure of merit ( ZT ) by optimizing the bond strengths of intra- and inter-icosahedral clusters. Through element substitutions that mainly weaken the inter-cluster bonds, a dramatic increase of ZT from less than 0.01 to 0.26 was achieved. To further increase ZT , materials should form a real gap to obtain a higher Seebeck coefficient.

Microstructure and Electrical Conductivity of ZnO Addition on the Properties of (Bi0.92Ho0.03Er0.05)2O3

NASA Astrophysics Data System (ADS)

Ermiş, İ.; Çorumlu, V.; Sertkol, M.; Öztürk, M.; Kaleli, M.; Çetin, A.; Turemiş, M.; Arı, M.

2016-11-01

The solid electrolyte is one of the most important components for a solid oxide fuel cell (SOFC). The various divalent or trivalent metal ion-doped bismuth-based materials exhibit good ionic conductivity. Therefore, these materials are used as electrolytes in the SOFC. In this paper, the samples of (Bi0.92- x Ho0.03Er0.05)2O3 + (ZnO) x solutions with a 0 ≤ x ≤ 0.2 molar ratio are synthesized by the solid state reaction method. The detailed structural and electrical characterizations are investigated by using x-ray diffraction (XRD), alternating current electrochemical impedance spectroscopy, and scanning electron microscopy (SEM). The XRD patterns of all samples are indexed on a monoclinic symmetry with a P21/c space group. In addition, the rietveld parameters are determined by using the FullProf software program. The impedance measurements of the samples are obtained at the 1 Hz to 20 MHz frequency range. The impedance value of the pellets increases with temperature. Based on the impedance results, it is found that the contribution of grain (bulk) is more than a grain boundary in terms of conductivity, which permits the attribution of a grain boundary. The ionic conductivity decreases with an increasing amount of Zn contribution. The value of highest electrical conductivity among all samples is calculated as 0.358 S cm-1 at 800°C for undoped (Bi0.92Ho0.03Er0.05)2O3.

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.

X-ray diffraction and infrared spectroscopy studies of Ba(Fe1/2Nb1/2)O3-(Na1/2Bi1/2)TiO3 ceramics

NASA Astrophysics Data System (ADS)

Chandra, K. P.; Yadav, Anjana; Prasad, K.

2018-05-01

Ceramics (1-x)Ba(Fe1/2Nb1/2)O3-x(Na1/2Bi1/2)TiO3; 0≤x≤1.0 were prepared by conventional ceramic synthesis technique. 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 Ba(Fe1/2Nb1/2)O3 has cubic structure with space group Pm 3 ¯ m and Na1/2Bi1/2)TiO3 has rhombohedral structure with space group R3c. Addition of (Na1/2Bi1/2)TiO3 to Ba(Fe1/2Nb1/2)O3 resulted in the change of unit cell structure from cubic to tetragonal (P4/mmm) for x = 0.75 and the X-Ray diffraction peaks slightly shift towards higher Bragg's angle, suggesting slight decrease in unit cell volume. SEM studies were carried out in order to access the quality of the prepared ceramics which showed a change in grain shapes with the increase of (Na1/2Bi1/2)TiO3 content. FTIR spectra confirmed the formation of perovskite type solid solutions.

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

Antao, Sytle M.; Cruickshank, Laura A.

The crystal structure of an optically anisotropic kimzeyite garnet from Magnet Cove, Arkansas, USA, where it was first discovered, was refined with the Rietveld method, cubic space group, Ia\\overline 3 d, and monochromatic [λ = 0.41422 (2) Å] synchrotron high-resolution powder X-ray diffraction (HRPXRD) data. The Rietveld refinement reduced χ 2and overallR(F 2) values are 1.840 and 0.0647, respectively. The sample, with the general garnet formula [8]X 3 [6]Y 2 [4]Z 3 [4]O 12, contains an intergrowth of two cubic phases that occur initially as oscillatory growth zoning, and patchy intergrowths arise later from fluid-enhanced dissolution and re-precipitation. The twomore » compositions obtained with electron-probe microanalyses (EPMA) are Ca 3.00(Zr 1.31Ti 4+ 0.46Fe 3+ 0.22Mn 3+ 0.01) Σ2[Al 0.76Fe 3+ 1.01Si 1.23] Σ3O 12for phase 1aand Ca 2.99(Zr 1.48Ti 4+ 0.37Fe 3+ 0.15) Σ2[Al 0.87Fe 3+ 0.98Si 1.15] Σ3O 12for phase 1b. The weight percentage, unit-cell parameter (Å), distances (Å), and site occupancy factors (s.o.f.s) for phase 1aare as follows: 42.6 (2)%,a= 12.46553 (3) Å, average = 2.482,Y—O = 2.059 (2),Z—O = 1.761 (2) Å, Ca (Xs.o.f.) = 0.960 (4), Zr (Ys.o.f.) = 0.809 (3), and Fe (Zs.o.f.) = 0.623 (2). The corresponding values for phase 1bare 57.4 (2)%,a= 12.47691 (2) Å, average = 2.482,Y—O = 2.062 (1),Z—O = 1.762 (1) Å, Ca (Xs.o.f.) = 0.957 (3), Zr (Ys.o.f.) = 0.828 (2) and Fe (Zs.o.f.) = 0.617 (2). The main structural differences between the two phases are in the unit-cell parameter, Δa= 0.01138 Å,Y(s.o.f.), andY—O distance. Structural mismatch between the two cubic phases in a crystal gives rise to strain-induced optical anisotropy.« less

Calcio-olivine {gamma}-Ca{sub 2}SiO{sub 4}: I. Rietveld refinement of the crystal structure

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

Gobechiya, E. R., E-mail: elgob@mail.ru; Yamnova, N. A.; Zadov, A. E.

2008-05-15

The structure of the natural mineral calcio-olivine ({gamma}-Ca{sub 2}SiO{sub 4}) found in skarn xenoliths in the region of the Lakargi Mountain (North Caucasus, Kabardino-Balkaria, Russia) is refined by the Rietveld method [a = 5.07389(7) A, b = 11.21128(14) A, c = 6.75340(9) A, V = 384.170(5) A{sup 3}, Z = 4, {rho}{sub calcd} = 2.98 g/cm{sup 3}, space group Pbnm]. The X-ray diffraction pattern of a powdered sample is recorded on a STOE STADI MP diffractometer [{lambda}CuK{sub {alpha}1}; Ge(111) primary monochromator; 6.00{sup o} < 2{theta} < 100.88{sup o}; step width, 2.5{sup o} in 2{theta}; number of reflections, 224]. All calculationsmore » are performed with the WYRIET (version 3.3) software package. The structural model is refined in the anisotropic approximation to R{sub p} = 6.44, R{sub wp} = 8.52, R{sub exp} = 5.85, R{sub B} = 4.98, R{sub F} = 6.90, and s = 1.46. It is shown that the sample under investigation is a mixture of several mineral phases, among which calcio-olivine (the natural analogue of the {gamma}-Ca{sub 2}SiO{sub 4} compound) (83%), hillebrandite (13%), and wadalite (4%) are dominant. Only the scale factors and the unit cell parameters are refined for hillebrandite Ca{sub 2}SiO{sub 3}(OH){sub 2} [a = 3.63472(16) A, b = 16.4140(10) A, c = 11.7914(8) A, space group Cmc2{sub 1}, Z = 6] and wadalite Ca{sub 6}Al{sub 5}Si{sub 2}O{sub 16}Cl{sub 3} (a = 12.0088 A, space group, I 4 bar 3d, Z = 4). The results of the structure refinement of the main component of the sample confirm that the mineral calcio-olivine is isostructural to the synthetic compound {gamma}-Ca{sub 2}SiO{sub 4}. The structure of this compound is formed by the heteropolyhedral framework composed of Ca octahedra joined together into olivine-like ribbons and isolated Si tetrahedra.« less

Crystal chemistry and oxidation state of Fe-rich prehnite from a hydrothermally altered dolerite

NASA Astrophysics Data System (ADS)

Nagashima, Mariko; Iwasa, Kiyoka; Akasaka, Masahide

2018-04-01

Fe-rich prehnite, Ca2(Al,Fe)(AlSi3)O10(OH)2, in a hydrothermally altered dolerite sill from Mitsu, Shimane Peninsula, Japan, was studied using 57Fe Mössbauer spectroscopy and X-ray Rietveld method to determine the oxidation state and distribution of Fe within the prehnite and to clarify its structural properties. Prehnite shows two modes of occurrence: a druse and vein mineral (prehnite I) associated with Fe-rich pumpellyite and laumontite and a replacement of primary plagioclase (prehnite II). The Fe contents of prehnite I and II are 0.33-0.44 and 0.01-0.46 Fe3+ atoms per formula unit, respectively. The Mössbauer spectrum of prehnite II consists of one doublet with isomer shift ( IS) = 0.364 mm/s and quadrupole splitting ( QS) = 0.284 mm/s assigned to Fe3+ at the octahedral M site. In contrast, the Mössbauer spectrum of prehnite I consists of two doublets assigned to Fe3+ at the M site ( IS = 0.369 mm/s and QS = 0.299 mm/s) and Fe2+ at the seven coordinated A site ( IS = 1.05 and QS = 2.78 mm/s). According to X-ray Rietveld refinements with Pmna and Pma2 space groups, the fitting with Pma2 gave more reduced reliability factors than those using Pmna for both specimens, implying ordering of Al and Si at the tetrahedral T2 sites. Determined T2-O bond lengths at the Al-rich and Si-rich T2 sites, 1.71-1.72 and 1.62-1.64 Å, respectively, also indicate the ordered arrangement of Al and Si at the T2 sites. Refined site occupancies at the A and M sites are represented as A (Ca0.993(9)Fe2 + 0.007) M (Al0.666(6)Fe3 + 0.334) for prehnite I, and A Ca1.0 M (Al0.865(5)Fe3 + 0.135) for prehnite II, respectively. The existence of Fe2+ in the A site filling Ca deficiency in prehnite I is consistent with the result from the Mössbauer analysis.

Electron density distribution and disordered crystal structure of 15R-SiAlON, SiAl{sub 4}O{sub 2}N{sub 4}

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

Banno, Hiroki; Hanai, Takaaki; Asaka, Toru

2014-03-15

The crystal structure of SiAl{sub 4}O{sub 2}N{sub 4} was characterized by laboratory X-ray powder diffraction (CuKα{sub 1}). The title compound is trigonal with space group R3-bar m. The hexagonal unit-cell dimensions (Z=3) are a=0.301332(3) nm, c=4.18616(4) nm and V=0.3291825(5) nm{sup 3}. The initial structural model was successfully derived by the charge-flipping method and further refined by the Rietveld method. The final structural model showed the positional disordering of one of the three (Si,Al) sites. The maximum-entropy method-based pattern fitting (MPF) method was used to confirm the validity of the split-atom model, in which conventional structure bias caused by assuming intensitymore » partitioning was minimized. The reliability indices calculated from the MPF were R{sub wp}=5.05%, S (=R{sub wp}/R{sub e})=1.21, R{sub p}=3.77%, R{sub B}=1.29% and R{sub F}=1.01%. The disordered crystal structure was successfully described by overlapping three types of domains with ordered atom arrangements. The distribution of atomic positions in one of the three types of domains can be achieved in the space group R3-bar m. The atom arrangements in the other two types of domains are noncentrosymmetrical with the space group R3m. These two structural configurations are related by the pseudo-symmetry inversion. -- Graphical abstract: A bird's eye view of electron densities up to 75.3% (0.133 nm{sup −3}) of the maximum on the plane parallel to (110) with the corresponding atomic arrangements of SiAl{sub 4}O{sub 2}N{sub 4}. Highlights: • Crystal structure of SiAl{sub 4}O{sub 2}N{sub 4} is determined by laboratory X-ray powder diffraction. • The atom arrangements are represented by the split-atom model. • The maximum-entropy method-based pattern fitting method is used to confirm the validity of the model. • The disordered structure is described by overlapping three types of domains with ordered atom arrangements.« less

Effect of synthesis route on the uptake of Ni and Cd by MgFe2O4 nanopowders

NASA Astrophysics Data System (ADS)

Al-Najar, B.; Khezami, L.; Judith Vijaya, J.; Lemine, O. M.; Bououdina, M.

2017-01-01

In this study, MgFe2O4 nanopowders were synthesized through two different methods, sol-gel method (SG) and modified sol-gel with Ammonia (MSG-A). The influence of synthesis route was investigated in terms of phase stability, pores size and surface area, magnetic properties and uptake of Ni and Cd metals from aqueous solution. Rietveld refinements of x-ray diffraction patterns confirmed the formation of single spinel phase for SG sample, while minor impurity was detected for SGM-A sample (few amount of MgO). The crystallite size was found to be sensitive to the preparation method; it ranges from 4 nm for SG to 15 nm for MSG-A. Magnetization experiment at room temperature showed ferromagnetic behavior with a saturation magnetization ( M s) ranging from 5.39 emu/g for SG to 9.93 emu/g for MSG-A. Preliminary results showed that SG and MSG-A samples are efficient adsorbent for Ni and Cd metal ions from aqueous solution. Maximum quantity of 62.67 and 61.2 mg of Ni(II) and 36.49 and 32.84 mg of Cd(II) was adsorbed per gram of MgFe2O4 synthesized by SG and MSG-A, respectively.

Calcium-deficient apatite synthesized by ammonia hydrolysis of dicalcium phosphate dihydrate: influence of temperature, time, and pressure.

PubMed

Obadia, Laetitia; Rouillon, Thierry; Bujoli, Bruno; Daculsi, Guy; Bouler, Jean Michel

2007-01-01

In this work, calcium-deficient apatites (CDA) were synthesized by ammonia hydrolysis reaction of dicalcium phosphate dihydrate (DCPD; CaHPO4 x 2 H2O) to obtain biphasic calcium phosphates (BCP) without any extraionic substitution. The influence of three parameters was studied: temperature of the reaction (70 and 100 degrees C), time of the reaction (4 and 18 h), and the pressure (open and closed system). Experiments were made according to a factorial design method (FDM) allowing optimization of the number of samples as well as statistical analysis of results. Moreover, the influence of temperature (until 200 degrees C) was investigated. The crystal size of CDA was determined according to the Scherrer's formula and from Rietveld refinements taking the CDA anisotropy into account. The last method seems to be a reliable method to determine crystallite sizes of CDA, since crystallite sizes of CDA along <00l> and directions were accessible. The results describe the hydroxyapatite % (HA%) in BCP by a first-order polynomial equation in the experimental area studied and the HA content was found to increase by raising time and temperature of the reaction. Moreover, the type of reaction system (open/closed vessel) appeared to have little influence on HA%. 2006 Wiley Periodicals, Inc.

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

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.

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.

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.

Application of SR Methods for the Study of Nanocomposite Materials for Hydrogen Energy

NASA Astrophysics Data System (ADS)

Sadykov, V. A.; Pavlova, S. N.; Vinokurov, Z. S.; Shmakov, A. N.; Eremeev, N. F.; Fedorova, Yu. E.; Yakimchuk, E. P.; Kriventsov, V. V.; Bolotov, V. A.; Tanashev, Yu. Yu.; Sadovskaya, E. M.; Cherepanova, S. V.; Zolotarev, K. V.

This work summarizes results of synchrotron radiation (SR) studies of the real/defect structure of nanocrystalline/nanocomposite oxide materials, which determines their functional properties in hydrogen energy field as catalysts and mixed ionic electronic conductors (cathodes and anodes of solid oxide fuel cells, oxygen separation membranes). For nanocrystalline ceria-zirconia mixed oxide prepared via modified Pechini route using ethanol solution of reagents, a high spatial uniformity of cations distribution between domains along with the oxygen sublattice deficiency revealed by full-profile Rietveld refinement of SR diffraction data provide structure disordering enhancing oxygen mobility. For PrNi0.5Co0.5O3-δ - Ce0.9Y0.1O2-δ nanocomposite extensive transfer of Pr cations into fluorite domains generates a new path of fast oxygen diffusion along chains of Pr3+ - Pr4+ cations as directly proved by analysis of the unit cell relaxation after changing pO2 in perfect agreement with data obtained by oxygen isotope heteroexchange.

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.;

Thermoelectric properties of PbTe with indium and bismuth secondary phase

NASA Astrophysics Data System (ADS)

Bali, A.; Chetty, R.; Mallik, R. C.

2016-06-01

Lead telluride (PbTe) with indium (In) and bismuth (Bi) as micrometer sized secondary phases dispersed throughout the bulk has been prepared by matrix encapsulation method. In and Bi are not found to substitute in PbTe as shown by Rietveld and room temperature Raman studies but are present as secondary phases. Increased values of temperature dependent electrical resistivity and Seebeck coefficient show the effect of interfaces on electronic transport. As expected, thermal conductivity is found to reduce on addition of secondary phases due to a reduced electronic contribution, further confirming that electron scattering at interfaces is more important than phonon scattering in such systems for thermoelectric properties. However, due to the reduction in the power factor of the In and Bi added samples from that of the parent PbTe, the overall thermoelectric figure of merit ( zT) does not increase beyond that of PbTe, for which the highest value of 0.7 is obtained at 778 K.

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.

High-resolution inelastic neutron scattering and neutron powder diffraction study of the adsorption of dihydrogen by the Cu(II) metal-organic framework material HKUST-1

NASA Astrophysics Data System (ADS)

Callear, Samantha K.; Ramirez-Cuesta, Anibal J.; David, William I. F.; Millange, Franck; Walton, Richard I.

2013-12-01

We present new high-resolution inelastic neutron scattering (INS) spectra (measured using the TOSCA and MARI instruments at ISIS) and powder neutron diffraction data (measured on the diffractometer WISH at ISIS) from the interaction of the prototypical metal-organic framework HKUST-1 with various dosages of dihydrogen gas. The INS spectra show direct evidence for the sequential occupation of various distinct sites for dihydrogen in the metal-organic framework, whose population is adjusted during increasing loading of the guest. The superior resolution of TOSCA reveals subtle features in the spectra, not previously reported, including evidence for split signals, while complementary spectra recorded on MARI present full information in energy and momentum transfer. The analysis of the powder neutron patterns using the Rietveld method shows a consistent picture, allowing the crystallographic indenisation of binding sites for dihydrogen, thus building a comprehensive picture of the interaction of the guest with the nanoporous host.

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.

Thermally activated rotational disorder in CaMoO 4 nanocrystals

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

Culver, Sean P.; Brutchey, Richard L.

2016-04-12

In this study, a dual-space approach, combining Rietveld and pair distribution function (PDF) analyses, has been applied to temperature-dependent synchrotron X-ray total scattering data collected on vapor diffusion sol–gel derived CaMoO 4 nanocrystals. A sharp transition in Ca–O bond distances in the range of 151–163 K was identified by PDF analysis, which is attributed to the thermal activation of rotational disorder associated with the rigid MoO 4 tetrahedra.

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.

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.

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.

Magnetic transition in Y-site doped multiferroic YMnO{sub 3}

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

Thakur, Rajesh K., E-mail: thakur.rajesh2009@gmail.com; Thakur, Rasna, E-mail: rasnathakur@yahoo.com; Gaur, N. K., E-mail: srl-nkgaur@yahoo.co.in

2016-05-06

We have synthesized polycrystalline hexagonal Y{sub 1-x}Sr{sub x}MnO{sub 3} (x=0.02, 0.1) compounds by using conventional solid state reaction method. The detailed structural investigations are carried out by using XRD studies which reveals the single phase formation of the reported compounds with hexagonal structure and space group P6{sub 3}cm (JCPDS: 25-1079). Further the XRD data of reported compounds were analyzed by RIETVELD (FULLPROFF) method which shows the decrease in the lattice parameter with increasing concentration of divalent strontium to Y-site. The observed pointed kinks in the specific heat study are indicative of the probable coupling in between the electric and magneticmore » orders in this class of materials. The reported systematic specific heat studies shows that the antiferromagnetic (AFM) transition temperature (T{sub N}) shifts to higher value with increasing concentration of Sr{sup 2+} ion in the YMnO{sub 3} compound which is attributed to the enhanced lattice contribution to the specific heat in the this compound. The present compound shows the independence of specific heat and magnetic transition temperature with applied magnetic field of 8T and 12T.« less

Synthesis and structural characterization of bulk Sb2Te3 single crystal

NASA Astrophysics Data System (ADS)

Sultana, Rabia; Gahtori, Bhasker; Meena, R. S.; Awana, V. P. S.

2018-05-01

We report the growth and characterization of bulk Sb2Te3 single crystal synthesized by the self flux method via solid state reaction route from high temperature melt (850˚C) and slow cooling (2˚C/hour) of constituent elements. The single crystal X-ray diffraction pattern showed the 00l alignment and the high crystalline nature of the resultant sample. The rietveld fitted room temperature powder XRD revealed the phase purity and rhombohedral structure of the synthesized crystal. The formation and analysis of unit cell structure further verified the rhombohedral structure composed of three quintuple layers stacked one over the other. The SEM image showed the layered directional growth of the synthesized crystal carried out using the ZEISS-EVOMA-10 scanning electron microscope The electrical resistivity measurement was carried out using the conventional four-probe method on a quantum design Physical Property Measurement System (PPMS). The temperature dependent electrical resistivity plot for studied Sb2Te3 single crystal depicts metallic behaviour in the absence of any applied magnetic field. The synthesis as well as the structural characterization of as grown Sb2Te3 single crystal is reported and discussed in the present letter.

Zeta potential and Raman studies of PVP capped Bi2S3 nanoparticles synthesized by polyol method

NASA Astrophysics Data System (ADS)

Tarachand, Sathe, Vasant G.; Okram, Gunadhor S.

2018-05-01

Here we report the synthesis and characterisation of polyvinylpyrrolidone (PVP) capped Bi2S3 nanoparticles via one step catalyst-free polyol method. Raman spectroscopy, dynamic light scattering and zeta potential analysis were performed on it. Rietveld refinement of powder XRD of PVP capped samples confirmed the formation of single phase orthorhombic Bi2S3 for all PVP capped samples. The presence of eight obvious Raman modes further confirmed the formation of stoichiometric Bi2S3. Dynamic light scattering (DLS) studies show a clear increase in hydrodynamic diameter for samples made with increasing PVP concentration. Particle size obtained from DLS and XRD (using Scherrer's formula) combine with change in full width half maxima of Raman modes collectively suggest overall improvement in crystallinity and quality of product on introducing PVP. In zeta potential (ζ) measurement, steric hindrance of carbon chains plays very crucial role and a systematic reduction of ζ value is observed for samples made with decreasing PVP concentration. An isoelectric point is obtained for sample made with low PVP (1g). Present results are likely to open a window for its medical and catalytic applications.

Characterization of a wollastonite glass-ceramic material prepared using sugar cane bagasse ash (SCBA) as one of the raw materials

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

Teixeira, Silvio R., E-mail: rainho@fct.unesp.br; Souza, Agda E.; Carvalho, Claudio L.

Glass-ceramic material prepared with sugar cane bagasse ash as one of the raw materials was characterized to determine some important properties for its application as a coating material. X-ray diffraction patterns showed that wollastonite-2M (CaSiO{sub 3}) was the major glass-ceramic phase. The Rietveld method was used to quantify the crystalline (60 wt.%) and vitreous (40 wt.%) phases in the glass-ceramic. The microstructure (determined by scanning electron microscopy) of this material had a marble appearance, showing a microporous network of elongated crystals with some areas with dendritic, feather-like ordering. Microhardness data gave a mean hardness value of 564.4 HV (Vickers-hardness), andmore » light microscopy disclosed a greenish brown colored material with a vitreous luster. - Highlights: • We studied the properties of a glass-ceramic material obtained from sugarcane ash. • This material has the appearance and hardness of natural stones. • A refining method gave information about its amorphous and crystalline phases. • This material has potential to be used as coating plates for buildings.« less

Room temperature ferromagnetism of nanocrystalline Nd1.90Ni0.10O3-δ

NASA Astrophysics Data System (ADS)

Sarkar, B. J.; Mandal, J.; Dalal, M.; Bandyopadhyay, A.; Chakrabarti, P. K.

2018-05-01

Nanocrystalline sample of Ni2+ doped neodymium oxide (Nd1.90Ni0.10O3-δ, NNO) is synthesized by co-precipitation method. Analysis of X-ray diffraction (XRD) pattern by Rietveld refinement method confirms the desired phase of NNO and complete substitution of Ni2+ ions in the Nd2O3 lattice. Analyses of transmission electron microscopy (TEM) and Raman spectroscopy of NNO recorded at room temperature (RT) also substantiate this fact. Besides, no traces of impurities are found in the analyses of XRD, TEM and Raman data. Room temperature hysteresis loop of NNO suggests the presence of weak ferromagnetism (FM) in low field region ( 600 mT), but in high field region paramagnetism of the host is more prominent. Magnetization vs. temperature ( M- T) curve in the entire temperature range (300-5 K) is analyzed successfully by a combined equation generated from three-dimensional (3D) spin wave model and Curie-Weiss law, which suggests the presence of mixed paramagnetic phase together with ferromagnetic phase in the doped sample. The onset of magnetic ordering is analyzed by oxygen vacancy mediated F-center exchange (FCE) coupling mechanism.

Room temperature magnetic ordering, enhanced magnetization and exchange bias of GdMnO3 nanoparticles in (GdMnO3)0.70(CoFe2O4)0.30

NASA Astrophysics Data System (ADS)

Mitra, A.; Mahapatra, A. S.; Mallick, A.; Chakrabarti, P. K.

2017-02-01

Nanoparticles of GdMnO3 (GMO) are prepared by sol-gel method. To enhance the magnetic property and also to obtain the magnetic ordering at room temperature (RT), nanoparticles of GMO are incorporated in the matrix of CoFe2O4 (CFO). Desired crystallographic phases of CFO, GMO and GMO-CFO are confirmed by analyzing X-ray diffractrograms (XRD) using Rietveld method. The average size of nanoparticles and their distribution, crystallographic phase, nanocrystallinity etc. are studied by high-resolution transmission electron microscope (HRTEM). Magnetic hysteresis loops (M-H) of GMO-CFO under zero field cooled (ZFC) and field cooled (FC) conditions are observed at different temperatures down to 5 K. Magnetization vs. temperature (M-T) under ZFC and FC conditions are also recorded. Interestingly, exchange bias (EB) is found at low temperature which suggests the encapsulation of the ferromagnetic (FM) nanoparticles of GMO by the ferrimagnetic nanoparticles of CFO below 100 K. Enhanced magnetization, EB effect and RT magnetic ordering of GMO-CFO would be interesting for both theoretical and experimental investigations.

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.

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.

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.

Improving Dielectric Properties of PVDF Composites by Employing Surface Modified Strong Polarized BaTiO₃ Particles Derived by Molten Salt Method.

PubMed

Fu, Jing; Hou, Yudong; Zheng, Mupeng; Wei, Qiaoyi; Zhu, Mankang; Yan, Hui

2015-11-11

BaTiO3/polyvinylidene fluoride (BT/PVDF) is the extensive reported composite material for application in modern electric devices. However, there still exists some obstacles prohibiting the further improvement of dielectric performance, such as poor interfacial compatibility and low dielectric constant. Therefore, in depth study of the size dependent polarization and surface modification of BT particle is of technological importance in developing high performance BT/PVDF composites. Here, a facile molten-salt synthetic method has been applied to prepare different grain sized BT particles through tailoring the calcination temperature. The size dependent spontaneous polarizationof BT particle was thoroughly investigated by theoretical calculation based on powder X-ray diffraction Rietveld refinement data. The results revealed that 600 nm sized BT particles possess the strong polarization, ascribing to the ferroelectric size effect. Furthermore, the surface of optimal BT particles has been modified by water-soluble polyvinylprrolidone (PVP) agent, and the coated particles exhibited fine core-shell structure and homogeneous dispersion in the PVDF matrix. The dielectric constant of the resulted composites increased significantly, especially, the prepared composite with 40 vol % BT loading exhibited the largest dielectric constant (65, 25 °C, 1 kHz) compared with the literature values of BT/PVDF at the same concentration of filler. Moreover, the energy storage density of the composites with tailored structure was largely enhanced at the low electric field, showing promising application as dielectric material in energy storage device. Our work suggested that introduction of strong polarized ferroelectric particles with optimal size and construction of core-shell structured coated fillers by PVP in the PVDF matrix are efficacious in improving dielectric performance of composites. The demonstrated approach can also be applied to the design and preparation of other polymers-based nanocomposites filled with ferroelectric particles to achieve desirable dielectric properties.

Local and average structure of Mn- and La-substituted BiFeO{sub 3}

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

Jiang, Bo; Selbach, Sverre M., E-mail: selbach@ntnu.no

2017-06-15

The local and average structure of solid solutions of the multiferroic perovskite BiFeO{sub 3} is investigated by synchrotron X-ray diffraction (XRD) and electron density functional theory (DFT) calculations. The average experimental structure is determined by Rietveld refinement and the local structure by total scattering data analyzed in real space with the pair distribution function (PDF) method. With equal concentrations of La on the Bi site or Mn on the Fe site, La causes larger structural distortions than Mn. Structural models based on DFT relaxed geometry give an improved fit to experimental PDFs compared to models constrained by the space groupmore » symmetry. Berry phase calculations predict a higher ferroelectric polarization than the experimental literature values, reflecting that structural disorder is not captured in either average structure space group models or DFT calculations with artificial long range order imposed by periodic boundary conditions. Only by including point defects in a supercell, here Bi vacancies, can DFT calculations reproduce the literature results on the structure and ferroelectric polarization of Mn-substituted BiFeO{sub 3}. The combination of local and average structure sensitive experimental methods with DFT calculations is useful for illuminating the structure-property-composition relationships in complex functional oxides with local structural distortions. - Graphical abstract: The experimental and simulated partial pair distribution functions (PDF) for BiFeO{sub 3}, BiFe{sub 0.875}Mn{sub 0.125}O{sub 3}, BiFe{sub 0.75}Mn{sub 0.25}O{sub 3} and Bi{sub 0.9}La{sub 0.1}FeO{sub 3}.« less

Structural, microstructural and electrical characterization of BaSnO3 and Ba0.90Y0.10SnO3 synthesized by solution combustion method

NASA Astrophysics Data System (ADS)

Kumar, Upendra; Yadav, Dharmendra; Upadhyay, Shail; Thakur, Anukul K.

2018-04-01

Powder of perovskite oxides BaSnO3 and Ba0.90Y0.10SnO3 have been synthesized by solution combustion method. Rietveld profile analysis shows that the phases crystallize with cubic unit cell in the space group pm3m. Further purity of the synthesized powders was checked by Fourier transform of infrared (FTIR) spectroscopy. The average grain size of the sintered samples was obtained using Scanning electron microscopy (SEM) and found to be 4.9 and 2.8 1m for BaSnO3 and Ba0.90Y0.10SnO3, respectively. The AC conductivity (σac) of synthesized samples was measured in the frequency range from 24Hz-1MHz and temperature range 100 - 600°C. Conductivity spectra of both the samples followed universal Johnscher's power law at different temperatures. The value of bulk or dc conductivity (σdc) at different temperatures has been extracted by fitting the Johnscher's power law to AC conductivity spectra. The activation energy for σc has been obtained from the least square linear fit of data points and found to be 0.53 eV and 0.43 eV, respectively for BaSnO3 and Ba0.90Y0.10SnO3. Based on the value of activation energy it is proposed that conduction in these samples is govern via hopping of (OH)•. The value of conductivity at temperature 550°C of Ba0.90Y0.10SnO3 is 0.00406 S-cm-1 higher than BaSnO3 (0.00173 S-cm-1) at the same temperature.

Effects of Bi doping on structural and magnetic properties of double perovskite oxides Sr2FeMoO6

NASA Astrophysics Data System (ADS)

Lan, Yaohai; Feng, Xiaomei; Zhang, Xin; Shen, Yifu; Wang, Ding

2016-08-01

A new series of double perovskite compounds Sr2 - δBixFeMoO6 have been synthesized by solid-state reaction. δ refers to the nominal doping content of Bi (δ = 0, 0.1, 0.2, 0.3, 0.4, 0.5), while the Bi content obtained by the Rietveld refinement is x = 0, 0.01, 0.05, 0.08, 0.10 and 0.12. Their crystal structure and magnetic properties are investigated. Rietveld analysis of the room temperature XRD data shows all the samples crystallize in the cubic crystal structure with the space group Fm 3 ‾ m and have no phase transition. SEM images show that substituted samples present a denser microstructure and bigger grains than Sr2FeMoO6, which is caused by a liquid sintering process due to the effumability of Bi. The unit cell volume increases with augment of Bi3+ concentration despite the smaller ionic radius Bi3+ compared with the Sr2+, which is attributed to the electronic effect. The degree of Fe/Mo order (η) increases first and then decreases to almost disappearance with augment of Bi doping, which is the result of contribution from electronic effect. Calculated saturation magnetization Ms(3) according to our phase separation likeness model matches well with the experimental ones. The observed variations of magnetoresistance (MR) are consistent with the Fe/Mo order (η) due to the internal connection with anti-site defect (ASD).

The new insight into the structure-activity relation of Pd/CeO2-ZrO2-Nd2O3 catalysts by Raman, in situ DRIFTS and XRD Rietveld analysis.

PubMed

Yang, X; Yang, L; Lin, J; Zhou, R

2016-01-28

Pd/CeO2-ZrO2-Nd2O3 (CZN) catalysts with different CeO2/ZrO2 molar ratios were synthesized and have been characterized by multiple techniques, e.g. XRD in combination with Rietveld refinement, UV-Raman, XPS and in situ DRIFTS. The XRD pattern of CZN with CeO2/ZrO2 molar ratios ≥1/2 can be indexed satisfactorily to the fluorite structure with a space group Fm3̄m, while the XRD patterns of CZ12 only display diffraction peaks of the tetragonal phase (S.G. P42/nmc). Nd addition can effectively stabilize the cubic structure of the CZN support and increase the enrichment of defect sites on the surface, which may be related to the better catalytic activity of Pd/CZN12 catalysts compared with Pd/CZ12. The presence of moderate ZrO2 can increase the concentration of O* active species, leading to accelerate the formation of nitrate species and thus enhance the catalytic activity of NOx and HC elimination. The Pd-dispersion decreases with the increasing Zr content, leading to the decreased CO catalytic activity, especially for the aged catalysts. The change regularity of the OSC value is almost the same with the in situ dynamic operational window, demonstrating that the in situ dynamic operational window is basically affected by the OSC value.

Triggering Incipient Ferroelectricity in Calcium Copper Titanate (CaCu3Ti4O12) ceramics through partial B-site substitution with Te4+ ion

NASA Astrophysics Data System (ADS)

Barman, Nabadyuti; Varma, K. B. R.

Double perovskite structured dielectric ceramic CaCu3Ti4- x TexO12 (CCTTO) (x = 0, 0.05, 0.1, 0.15, 0.2) was fabricated from the powder obtained by conventional solid state synthetic route. The room temperature XRD patterns for the x = 0, 0.05, 0.075 modified samples were confirmed to possess a single phase with cubic space group Im3by Rietveld refinement. But, the Rietveld refinement performed on XRD patterns recorded for the compositions corresponding to x = 0.1, 0.15, 0.2 shows the coexistence of the cubic phase (space group Im3; a = 7.4065Å) and tetragonal phase (space group I4/mcm; a = 7.369 Å and c = 6.967 Å). The dielectric properties of these ceramics were studied over a wide frequency (40Hz-2MHz) and temperature range (30-400K). The Te4+ doped samples (CCTTO) exhibited dielectric permittivity (?r) value of ~23-33X103 which is more than twice that of undoped CCTO (~11x103) at 1kHz. A decreasing trend in dielectric permittivity with increasing temperature, a signature of incipient ferroelectricity, was observed for all the samples. Barrett's formula was invoked to rationalize the dielectric permittivity variation as a function of temperature. The incipient ferroelectric behavior is correlated with soft phonon mode observed in temperature dependent Raman Spectroscopic studies. .

Nitrogen-modified nano-titania: True phase composition, microstructure and visible-light induced photocatalytic NOx abatement

NASA Astrophysics Data System (ADS)

Tobaldi, D. M.; Pullar, R. C.; Gualtieri, A. F.; Otero-Irurueta, G.; Singh, M. K.; Seabra, M. P.; Labrincha, J. A.

2015-11-01

Titanium dioxide (TiO2) is a popular photocatalyst used for many environmental and anti-pollution applications, but it normally operates under UV light, exploiting ∼5% of the solar spectrum. Nitrification of titania to form N-doped TiO2 has been explored as a way to increase its photocatalytic activity under visible light, and anionic doping is a promising method to enable TiO2 to harvest visible-light by changing its photo-absorption properties. In this paper, we explore the insertion of nitrogen into the TiO2 lattice using our green sol-gel nanosynthesis method, used to create 10 nm TiO2 NPs. Two parallel routes were studied to produce nitrogen-modified TiO2 nanoparticles (NPs), using HNO3+NH3 (acid-precipitated base-peptised) and NH4OH (totally base catalysed) as nitrogen sources. These NPs were thermally treated between 450 and 800 °C. Their true phase composition (crystalline and amorphous phases), as well as their micro-/nanostructure (crystalline domain shape, size and size distribution, edge and screw dislocation density) was fully characterised through advanced X-ray methods (Rietveld-reference intensity ratio, RIR, and whole powder pattern modelling, WPPM). As pollutants, nitrogen oxides (NOx) are of particular concern for human health, so the photocatalytic activity of the NPs was assessed by monitoring NOx abatement, using both solar and white-light (indoor artificial lighting), simulating outdoor and indoor environments, respectively. Results showed that the onset of the anatase-to-rutile phase transformation (ART) occurred at temperatures above 450 °C, and NPs heated to 450 °C possessed excellent photocatalytic activity (PCA) under visible white-light (indoor artificial lighting), with a PCA double than that of the standard P25 TiO2 NPs. However, higher thermal treatment temperatures were found to be detrimental for visible-light photocatalytic activity, due to the effects of four simultaneous occurrences: (i) loss of OH groups and water adsorbed on the photocatalyst surface; (ii) growth of crystalline domain sizes with decrease in specific surface area; (iii) onset and progress of the ART; (iv) the increasing instability of the nitrogen in the titania lattice.

Rare-earth free self-luminescent Ca2KZn2(VO4)3 phosphors for intense white light-emitting diodes

PubMed Central

Bharat, L. Krishna; Jeon, Soo-Kun; Krishna, Kurugundla Gopi; Yu, Jae Su

2017-01-01

The commercially available white-light-emitting diodes (WLEDs) are made with a combination of blue LEDs and yellow phosphors. These types of WLEDs lack certain properties which make them meagerly applicable for general illumination and flat panel displays. The solution for such problem is to use near-ultraviolet (NUV) chips as an excitation source because of their high excitation efficiency and good spectral distribution. Therefore, there is an active search for new phosphor materials which can be effectively excited within the NUV wavelength range (350–420 nm). In this work, novel rare-earth free self-luminescent Ca2KZn2(VO4)3 phosphors were synthesized by a citrate assisted sol-gel method at low calcination temperatures. Optical properties, internal quantum efficiency and thermal stability as well as morphology and crystal structure of Ca2KZn2(VO4)3 phosphors for their application to NUV-based WLEDs were studied. The crystal structure and phase formation were confirmed with XRD patterns and Rietveld refinement. The optical properties of these phosphor materials which can change the NUV excitation into visible yellow-green emissions were studied. The synthesized phosphors were then coated onto the surface of a NUV chip along with a blue phosphor (LiCaPO4:Eu2+) to get brighter WLEDs with a color rendering index of 94.8 and a correlated color temperature of 8549 K. PMID:28181549

Effects of composition modulation on the luminescence properties of Eu(3+) doped Li1-xAgxLu(MoO4)2 solid-solution phosphors.

PubMed

Cheng, Fangrui; Xia, Zhiguo; Molokeev, Maxim S; Jing, Xiping

2015-11-07

Double molybdate scheelite-type solid-solution phosphors Li1-xAgxLu1-y(MoO4)2:yEu(3+) were synthesized by the solid state reaction method, and their crystal structures and luminescence properties were investigated in detail. The composition modulation and structural evolution of this series of samples were studied and the selected AgEu(MoO4)2, AgLu(MoO4)2, LiLu(MoO4)2 and LiEu(MoO4)2 phases were analyzed based on the Rietveld refinement. Depending on the variation of the Li/Ag ratio in Li1-xAgxLu1-y(MoO4)2:yEu(3+) phosphors, the difference in the luminescence properties of Li1-xAgxLu1-y(MoO4)2:yEu(3+) phosphors was ascribed to two factors, one reason could be assigned to the coupling effect and the nonradiative transition between the energy levels of LixAg1-xLu(MoO4)2 matrices and the activator Eu(3+), another could be due to the near ultraviolet energy absorption and transmission efficiency between the charge-transfer (CT) band of O(2-)-Mo(6+) and the 4f → 4f emissive transitions of Eu(3+). The ultraviolet-visible diffuse reflection spectra (UV-vis DRS) and Raman spectra analysis were also used to verify the above mechanism.

Rare-earth free self-luminescent Ca2KZn2(VO4)3 phosphors for intense white light-emitting diodes.

PubMed

Bharat, L Krishna; Jeon, Soo-Kun; Krishna, Kurugundla Gopi; Yu, Jae Su

2017-02-09

The commercially available white-light-emitting diodes (WLEDs) are made with a combination of blue LEDs and yellow phosphors. These types of WLEDs lack certain properties which make them meagerly applicable for general illumination and flat panel displays. The solution for such problem is to use near-ultraviolet (NUV) chips as an excitation source because of their high excitation efficiency and good spectral distribution. Therefore, there is an active search for new phosphor materials which can be effectively excited within the NUV wavelength range (350-420 nm). In this work, novel rare-earth free self-luminescent Ca 2 KZn 2 (VO 4 ) 3 phosphors were synthesized by a citrate assisted sol-gel method at low calcination temperatures. Optical properties, internal quantum efficiency and thermal stability as well as morphology and crystal structure of Ca 2 KZn 2 (VO 4 ) 3 phosphors for their application to NUV-based WLEDs were studied. The crystal structure and phase formation were confirmed with XRD patterns and Rietveld refinement. The optical properties of these phosphor materials which can change the NUV excitation into visible yellow-green emissions were studied. The synthesized phosphors were then coated onto the surface of a NUV chip along with a blue phosphor (LiCaPO 4 :Eu 2+ ) to get brighter WLEDs with a color rendering index of 94.8 and a correlated color temperature of 8549 K.

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.

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

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

α-Phase transformation kinetics of U – 8 wt% Mo established by in situ neutron diffraction

DOE PAGES

Garlea, Elena; Steiner, M. A.; Calhoun, C. A.; ...

2016-05-08

The α-phase transformation kinetics of as-cast U - 8 wt% Mo below the eutectoid temperature have been established by in situ neutron diffraction. α-phase weight fraction data acquired through Rietveld refinement at five different isothermal hold temperatures can be modeled accurately utilizing a simple Johnson-Mehl-Avrami-Kolmogorov impingement-based theory, and the results are validated by a corresponding evolution in the γ-phase lattice parameter during transformation that follows Vegard’s law. Neutron diffraction data is used to produce a detailed Time-Temperature-Transformation diagram that improves upon inconsistencies in the current literature, exhibiting a minimum transformation start time of 40 min at temperatures between 500 °Cmore » and 510 °C. Lastly, the transformation kinetics of U – 8 wt% Mo can vary significantly from as-cast conditions after extensive heat treatments, due to homogenization of the typical dendritic microstructure which possesses non-negligible solute segregation.« less

Effect of Spark Plasma Sintering on the Structure and Properties of Ti1−xZrxNiSn Half-Heusler Alloys

PubMed Central

Downie, Ruth A.; Popuri, Srinivas R.; Ning, Huanpo; Reece, Mike J.; Bos, Jan-Willem G.

2014-01-01

XNiSn (X = Ti, Zr and Hf) half-Heusler alloys have promising thermoelectric properties and are attracting enormous interest for use in waste heat recovery. In particular, multiphase behaviour has been linked to reduced lattice thermal conductivities, which enables improved energy conversion efficiencies. This manuscript describes the impact of spark plasma sintering (SPS) on the phase distributions and thermoelectric properties of Ti0.5Zr0.5NiSn based half-Heuslers. Rietveld analysis reveals small changes in composition, while measurement of the Seebeck coefficient and electrical resistivities reveals that all SPS treated samples are electron doped compared to the as-prepared samples. The lattice thermal conductivities fall between 4 W·m−1·K−1 at 350 K and 3 W·m−1·K−1 at 740 K. A maximum ZT = 0.7 at 740 K is observed in a sample with nominal Ti0.5Zr0.5NiSn composition. PMID:28788234

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.

Local Atomic Structure Deviation from Average Structure of Na0.5Bi0.5TiO3: Combined X-ray and Neutron Total Scattering Study

DTIC Science & Technology

2013-03-27

part of a new generation of ferroelectric materials used in a multitude of piezoelectric applications. This work examines the short and long range...2211 15. SUBJECT TERMS Na0.5Bi0.5TiO3, ferroelectric , structure, Rietveld, local structure Elena Aksel, Jennifer S. Forrester, Juan C. Nino, Katharine...a new generation of ferroelectric materials used in a multitude of piezoelectric applications. This work examines the short and long range structure

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.

Electron tomography and fractal aspects of MoS2 and MoS2/Co spheres.

PubMed

Ramos, Manuel; Galindo-Hernández, Félix; Arslan, Ilke; Sanders, Toby; Domínguez, José Manuel

2017-09-26

A study was made by a combination of 3D electron tomography reconstruction methods and N 2 adsorption for determining the fractal dimension for nanometric MoS 2 and MoS 2 /Co catalyst particles. DFT methods including Neimarke-Kiselev's method allowed to determine the particle porosity and fractal arrays at the atomic scale for the S-Mo-S(Co) 2D- layers that conform the spherically shaped catalyst particles. A structural and textural correlation was sought by further characterization performed by x-ray Rietveld refinement and Radial Distribution Function (RDF) methods, electron density maps, computational density functional theory methods and nitrogen adsorption methods altogether, for studying the structural and textural features of spherical MoS 2 and MoS 2 /Co particles. Neimark-Kiselev's equations afforded the evaluation of a pore volume variation from 10 to 110 cm 3 /g by cobalt insertion in the MoS 2 crystallographic lattice, which induces the formation of cavities and throats in between of less than 29 nm, with a curvature radius r k  < 14.4 nm; typical large needle-like arrays having 20 2D layers units correspond to a model consisting of smooth surfaces within these cavities. Decreasing D P , D B , D I and D M values occur when Co atoms are present in the MoS 2 laminates, which promote the formation of smoother edges and denser surfaces that have an influence on the catalytic properties of the S-Mo-S(Co) system.

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.

Dependence of microwave dielectric properties on crystallization behaviour of CaMgSi{sub 2}O{sub 6} glass-ceramics

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

Choi, Bo Kyeong; Jang, Sung Wook; Kim, Eung Soo, E-mail: eskim@kyonggi.ac.kr

2015-07-15

The effects of the crystallization behaviour of CaMgSi{sub 2}O{sub 6} (diopside) glass-ceramics on their microwave dielectric properties were investigated as functions of the Cr{sub 2}O{sub 3} content and heat-treatment method used (one or two steps). The crystallization behaviours of the specimens were affected by the Cr{sub 2}O{sub 3} content as well as by the heat-treatment method employed, and were evaluated using X-ray diffraction and the combined Rietveld and reference intensity ratio (RIR) method. The dielectric constants (K) of the specimens did not change significantly with an increase in the Cr{sub 2}O{sub 3} content. The quality factor (Qf) of the specimensmore » increased for Cr{sub 2}O{sub 3} contents of up to 0.5 wt% Cr{sub 2}O{sub 3}, but then decreased for higher contents. These results could be attributed to the degree of crystallization. For the same Cr{sub 2}O{sub 3} content, the specimens that underwent a two-step heat treatment showed lower K values and higher Qf values than those heat-treated in one-step. These results could be attributed to the smaller crystallite size and higher degree of crystallization in the specimens obtained from the two-step heat treatment compared with those of the specimens heat-treated in one-step method.« less

Coupled transport-reaction pathways and distribution patterns between siliciclastic-carbonate sediments at the Ria de Vigo

NASA Astrophysics Data System (ADS)

García, T.; Velo, A.; Fernandez-Bastero, S.; Gago-Duport, L.; Santos, A.; Alejo, I.; Vilas, F.

2005-02-01

This paper examines the linkages between the space-distribution of grain sizes and the relative percentage of the amount of mineral species that result from the mixing process of siliciclastic and carbonate sediments at the Ria de Vigo (NW of Spain). The space-distribution of minerals was initially determined, starting from a detailed mineralogical study based on XRD-Rietveld analysis of the superficial sediments. Correlations between the maps obtained for grain sizes, average fractions of either siliciclastic or carbonates, as well as for individual-minerals, were further stabilised. From this analysis, spatially organized patterns were found between carbonates and several minerals involved in the siliciclastic fraction. In particular, a coupled behaviour is observed between plagioclases and carbonates, in terms of their relative percentage amounts and the grain size distribution. In order to explain these results a conceptual model is proposed, based on the interplay between chemical processes at the seawater-sediment interface and hydrodynamical factors. This model suggests the existence of chemical control mechanisms that, by selective processes of dissolution-crystallization, constrain the mixed environment's long-term evolution, inducing the formation of self-organized sedimentary patterns.

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

Carbon coated nano-LiTi2(PO4)3 electrodes for non-aqueous hybrid supercapacitors.

PubMed

Aravindan, V; Chuiling, W; Reddy, M V; Rao, G V Subba; Chowdari, B V R; Madhavi, S

2012-04-28

The Pechini type polymerizable complex decomposition method is employed to prepare LiTi(2)(PO(4))(3) at 1000 °C in air. High energy ball milling followed by carbon coating by the glucose-method yielded C-coated nano-LiTi(2)(PO(4))(3) (LTP) with a crystallite size of 80(±5) nm. The phase is characterized by X-ray diffraction, Rietveld refinement, thermogravimetry, SEM, HR-TEM and Raman spectra. Lithium cycling properties of LTP show that 1.75 moles of Li (~121 mA h g(-1) at 15 mA g(-1) current) per formula unit can be reversibly cycled between 2 and 3.4 V vs. Li with 83% capacity retention after 70 cycles. Cyclic voltammograms (CV) reveal the two-phase reaction mechanism during Li insertion/extraction. A hybrid electrochemical supercapacitor (HEC) with LTP as negative electrode and activated carbon (AC) as positive electrode in non-aqueous electrolyte is studied by CV at various scan rates and by galvanostatic cycling at various current rates up to 1000 cycles in the range 0-3 V. Results show that the HEC delivers a maximum energy density of 14 W h kg(-1) and a power density of 180 W kg(-1). This journal is © the Owner Societies 2012

Blue-green tunable color of Ce3+/Tb3+ coactivated NaBa3La3Si6O20 phosphor via energy transfer

PubMed Central

Jia, Zhen; Xia, Mingjun

2016-01-01

A series of color tunable phosphors NaBa3La3Si6O20:Ce3+, Tb3+ were synthesized via the high-temperature solid-state method. NaBa3La3Si6O20 crystallizes in noncentrosymmetric space group Ama2 with the cell parameters of a = 14.9226(4) Å, b = 24.5215(5) Å and c = 5.6241(2) Å by the Rietveld refinement method. The Ce3+ ions doped NaBa3La3Si6O20 phosphors have a strong absorption band from 260 to 360 nm and show near ultraviolet emission light centered at 378 nm. The Ce3+ and Tb3+ ions coactivated phosphors exhibit color tunable emission light from deep blue to green by adjusting the concentration of the Tb3+ ions. An energy transfer of Ce3+ → Tb3+ investigated by the photoluminescence properties and lifetime decay, is demonstrated to be dipole–quadrupole interaction. These results indicate the NaBa3La3Si6O20:Ce3+, Tb3+ phosphors can be considered as potential candidates for blue-green components for white light emitting diodes. PMID:27628111

Synthesis and Characterization of Yttria-Stabilized Zirconia Nanoparticles Doped with Ytterbium and Gadolinium: ZrO2 9.5Y2O3 5.6Yb2O3 5.2Gd2O3

NASA Astrophysics Data System (ADS)

Bahamirian, M.; Hadavi, S. M. M.; Rahimipour, M. R.; Farvizi, M.; Keyvani, A.

2018-06-01

Defect cluster thermal barrier coatings (TBCs) are attractive alternatives to Yttria-stabilized zirconia (YSZ) in advanced applications. In this study, YSZ nanoparticles doped with ytterbium and gadolinium (ZrO2 9.5Y2O3 5.6Yb2O3 5.2Gd2O3 (ZGYbY)) were synthesized through a chemical co-precipitation and calcination method, and characterized by in situ high-temperature X-ray diffraction analysis in the temperature range of 25 °C to 1000 °C (HTK-XRD), thermogravimetric analysis, differential thermal analysis, Fourier transform infrared spectroscopy, Raman spectroscopy, and field emission scanning electron microscopy (FE-SEM). Precise cell parameters of t-prime phase and the best zirconia phase for TBC applications were calculated by Cohen's and Rietveld refinement methods. Optimum crystallization temperature of the precursor powder was found to be 1000 °C. Furthermore, FE-SEM results for the calcined ZGYbY powders indicated orderly particles of uniform shape and size with a small tendency toward agglomeration. Average lattice thermal expansion coefficient in the temperature range of 25 °C to 1000 °C was determined to be 31.71 × 10-6 K-1.

Swift heavy ion induced structural and luminescence characterization of Y₂O₃:Eu³⁺ phosphor: a comparative study.

PubMed

Som, S; Sharma, S K; Lochab, S P

2014-08-01

We report a comparative study on structural and thermoluminescence modifications of Y2O3:Eu(3+) phosphor induced by 150 MeV Ni(7+), 120 MeV Ag(9+) and 110 MeV Au(8+) swift heavy ions (SHI) in the fluence range 1 × 10(11) to 1 × 10(13) ions/cm(2). X-Ray diffraction and transition electron microscopy studies confirm the loss of crystallinity of the phosphors after ion irradiation, which is greater in the case of Au ion irradiation. Structural refinement using the Rietveld method yields the various structural parameters of ion-irradiated phosphors. Thermoluminescence glow curves of ion-irradiated phosphors show a small shift in the position of the peaks, along with an increase in intensity with ion fluence. Stopping range of ions in Matter (SRIM) calculations were performed to correlate the change in thermoluminescence properties of various ion-irradiated phosphors. It shows that the defects created by 110 MeV Au(8+) ions are greater in number. Trapping parameters of ion-irradiated phosphors were calculated from thermoluminescence data using various glow curve analysis methods. Copyright © 2013 John Wiley & Sons, Ltd.

Synthesis and Characterization of Yttria-Stabilized Zirconia Nanoparticles Doped with Ytterbium and Gadolinium: ZrO2 9.5Y2O3 5.6Yb2O3 5.2Gd2O3

NASA Astrophysics Data System (ADS)

Bahamirian, M.; Hadavi, S. M. M.; Rahimipour, M. R.; Farvizi, M.; Keyvani, A.

2018-03-01

Defect cluster thermal barrier coatings (TBCs) are attractive alternatives to Yttria-stabilized zirconia (YSZ) in advanced applications. In this study, YSZ nanoparticles doped with ytterbium and gadolinium (ZrO2 9.5Y2O3 5.6Yb2O3 5.2Gd2O3 (ZGYbY)) were synthesized through a chemical co-precipitation and calcination method, and characterized by in situ high-temperature X-ray diffraction analysis in the temperature range of 25 °C to 1000 °C (HTK-XRD), thermogravimetric analysis, differential thermal analysis, Fourier transform infrared spectroscopy, Raman spectroscopy, and field emission scanning electron microscopy (FE-SEM). Precise cell parameters of t-prime phase and the best zirconia phase for TBC applications were calculated by Cohen's and Rietveld refinement methods. Optimum crystallization temperature of the precursor powder was found to be 1000 °C. Furthermore, FE-SEM results for the calcined ZGYbY powders indicated orderly particles of uniform shape and size with a small tendency toward agglomeration. Average lattice thermal expansion coefficient in the temperature range of 25 °C to 1000 °C was determined to be 31.71 × 10-6 K-1.

Unique coordination of pyrazine in T[Ni(CN){sub 4}].2pyz with T=Mn, Zn, Cd

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

Lemus-Santana, A.A.; Rodriguez-Hernandez, J.; Castillo, L.F. del, E-mail: lfelipe@servidor.unam.m

2009-04-15

The materials under study, T[Ni(CN){sub 4}].2pyz with T=Mn, Zn, Cd, were prepared by separation of T[Ni(CN){sub 4}] layers in citrate aqueous solution to allow the intercalation of the pyrazine molecules. The obtained solids were characterized from chemical analyses, X-ray diffraction, infrared, Raman, thermogravimetry, UV-Vis, magnetic and adsorption data. Their crystal structure was solved from ab initio using direct methods and then refined by the Rietveld method. A unique coordination for pyrazine to metal centers at neighboring layers was observed. The pyrazine molecule is found forming a bridge between Ni and T atoms, quite different from the proposed structures for T=Fe,more » Ni where it remains coordinated to two T atoms to form a vertical pillar between neighboring layers. The coordination of pyrazine to both Ni and T atoms minimizes the material free volume and leads to form a hydrophobic framework. On heating the solids remain stable up to 140 deg. C. No CO{sub 2} and H{sub 2} adsorption was observed in the small free spaces of their frameworks. - Graphical abstract: Framework for T[Ni(CN){sub 4}].2pyz with T=Mn, Zn, Cd.« less

Synthesis of nano-sized ZnO particles by co-precipitation method with variation of heating time

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

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

Zinc oxide powders have been synthesized by a co-precipitation method at low temperature (85 °C), using zinc acetate dihydrate, ammonia, hydrochloric acid solutions as the reactants. A number of process parameters such as reaction temperature, solution basicity or pH and heating time are the main factors affecting the morphology and physical properties of the ZnO nanostructures. In this work the effect of heating time on the morphology and particles size were studied. The as-synthesized ZnO powders were characterized using transmission electron microscopy (TEM) and X-ray diffraction (XRD) techniques. The samples were also analyzed using Fourier transform infrared (FTIR). Rietveld refinementmore » of XRD data confirms that ZnO crystallizes in the hexagonal wurtzite structure with high degree of purity and the (101) plane predominant. The XRD results show that the average crystallite sizes were about 66, 27 and 12 nm for 3, 4 and 5 h of heating times, respectively. The XRD analysis indicated that a fraction of nano-sized ZnO powders were in the form of aggregates, which was also verified by TEM image. The TEM photograph demonstrated that the nano-sized ZnO particles were a pseudo-spherical shape.« less

Application of Powder Diffraction Methods to the Analysis of the Atomic Structure of Nanocrystals: The Concept of the Apparent Lattice Parameter (ALP)

NASA Technical Reports Server (NTRS)

Palosz, B.; Grzanka, E.; Gierlotka, S.; Stelmakh, S.; Pielaszek, R.; Bismayer, U.; Weber, H.-P.; Palosz, W.; Curreri, Peter A. (Technical Monitor)

2002-01-01

The applicability of standard methods of elaboration of powder diffraction data for determination of the structure of nano-size crystallites is analysed. Based on our theoretical calculations of powder diffraction data we show, that the assumption of the infinite crystal lattice for nanocrystals smaller than 20 nm in size is not justified. Application of conventional tools developed for elaboration of powder diffraction data, like the Rietveld method, may lead to erroneous interpretation of the experimental results. An alternate evaluation of diffraction data of nanoparticles, based on the so-called 'apparent lattice parameter' (alp) is introduced. We assume a model of nanocrystal having a grain core with well-defined crystal structure, surrounded by a surface shell with the atomic structure similar to that of the core but being under a strain (compressive or tensile). The two structural components, the core and the shell, form essentially a composite crystal with interfering, inseparable diffraction properties. Because the structure of such a nanocrystal is not uniform, it defies the basic definitions of an unambiguous crystallographic phase. Consequently, a set of lattice parameters used for characterization of simple crystal phases is insufficient for a proper description of the complex structure of nanocrystals. We developed a method of evaluation of powder diffraction data of nanocrystals, which refers to a core-shell model and is based on the 'apparent lattice parameter' methodology. For a given diffraction pattem, the alp values are calculated for every individual Bragg reflection. For nanocrystals the alp values depend on the diffraction vector Q. By modeling different a0tomic structures of nanocrystals and calculating theoretically corresponding diffraction patterns using the Debye functions we showed, that alp-Q plots show characteristic shapes which can be used for evaluation of the atomic structure of the core-shell system. We show, that using a simple model of a nanocrystal with spherical shape and centro-symmetric strain at the surface shell we obtain theoretical alp-Q values which match very well the alp-Q plots determined experimentally for Sic, GaN, and diamond nanopowders. The theoretical models are defined by the lattice parameter of the grain core, thickness of the surface shell, and the magnitude and distribution of the strain field in the surface shell. According to our calculations, the part of the diffraction pattern measured at relatively low diffraction vectors Q (below 10/angstrom) provides information on the surface strain, whle determination of the lattice parameters in the grain core requires measurements at large Q-values (above 15 - 20/angstrom).

Elaboration, Rietveld refinements and vibrational spectroscopic study of Na₁-xKxCaPb₃(PO₄)₃ lacunar apatites (0 ⩽ x ⩽ 1).

PubMed

Lahrich, S; Elmhammedi, M A; Manoun, B; Tamraoui, Y; Mirinioui, F; Azrour, M; Lazor, P

2015-06-15

Synthesis of apatites, Na1-xKxCaPb3(PO4)3 0 ⩽ x ⩽ 1, with anion vacancy were carried out using solid state reactions. The solid solution of apatite-type structure crystallize in the hexagonal system, space group P63/m (No. 176). Rietveld refinements showed that around 90% of Pb(2+) cations are located in the (6h) sites, the left amount of Pb(2+) cations are located in the (4f) sites; 27-31% of Ca(2+) cations are located in the (6h) sites, the left amount of Ca(2+) cations are located in the (4f) sites. The ninefold coordination sites (4f) are also occupied by the K(+) and Na(+) monovalent ions. The structure can be described as built up from [PO4](3-) tetrahedra and Pb(2+)/Ca(2+) of sixfold coordination cavities (6h positions), which delimit void hexagonal tunnels running along [001]. These tunnels are connected by cations of mixed sites (4f) which are half occupied by Pb(2+)/Ca(2+) and half by Na(+)/K(+) mixed cations. The assignment of the observed frequencies in the Raman and infrared spectra is discussed on the basis of a unit cell group analysis and by comparison with other apatites. Vibrational spectra of all the compositions are similar and show some linear shifts of the frequencies as a function of the composition toward lower values due the substitutions of Na(+) by K(+) with a larger radius. Copyright © 2015 Elsevier B.V. All rights reserved.

Multislice frozen phonon high angle annular dark-field image simulation study of Mo-V-Nb-Te-O complex oxidation catalyst "M1".

PubMed

Blom, Douglas A

2012-01-01

Multislice frozen phonon calculations were performed on a model structure of a complex oxide which has potential use as an ammoxidation catalyst. The structure has 11 cation sites in the framework, several of which exhibit mixed Mo/V substitution. In this paper the sensitivity of high-angle annular dark-field (HAADF) imaging to partial substitution of V for Mo in this structure is reported. While the relationship between the average V content in an atom column and the HAADF image intensity is not independent of thickness, it is a fairly weak function of thickness suggesting that HAADF STEM imaging in certain cases can provide a useful starting point for Rietveld refinements of mixed occupancy in complex materials. The thermal parameters of the various cations and oxygen anions in the model affect the amount of thermal diffuse scattering and therefore the intensity in the HAADF images. For complex materials where the structure has been derived via powder Rietveld refinement, the uncertainty in the thermal parameters may limit the accuracy of HAADF image simulations. With the current interest in quantitative microscopy, simulations need to accurately describe the electron scattering to the very high angles often subtended by a HAADF detector. For this system approximately 15% of the scattering occurs above 200 mrad at 200 kV. To simulate scattering to such high angles, very fine sampling of the projected potential is necessary which increases the computational cost of the simulation. Copyright © 2011 Elsevier B.V. All rights reserved.

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.

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.

Precursor Routes to Complex Ternary Intermetallics: Single-Crystal and Microcrystalline Preparation of Clathrate-I Na8Al8Si38 from NaSi + NaAlSi.

PubMed

Dong, Yongkwan; Chai, Ping; Beekman, Matt; Zeng, Xiaoyu; Tritt, Terry M; Nolas, George S

2015-06-01

Single crystals of the ternary clathrate-I Na8Al8Si38 were synthesized by kinetically controlled thermal decomposition (KCTD), and microcrystalline Na8Al8Si38 was synthesized by spark plasma sintering (SPS) using a NaSi + NaAlSi mixture as the precursor. Na8AlxSi46-x compositions with x ≤ 8 were also synthesized by SPS from precursor mixtures of different ratios. The crystal structure of Na8Al8Si38 was investigated using both Rietveld and single-crystal refinements. Temperature-dependent transport and UV/vis measurements were employed in the characterization of Na8Al8Si38, with diffuse-reflectance measurement indicating an indirect optical gap of 0.64 eV. Our results indicate that, when more than one precursor is used, both SPS and KCTD are effective methods for the synthesis of multinary inorganic phases that are not easily accessible by traditional solid-state synthesis or crystal growth techniques.

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.

Effect of Zn-doping on structural and magnetic properties of copper ferrite nanoparticles

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

Gautam, Nisha; Thirupathi, Gadipelly; Singh, Rajender

2016-05-23

The nanoparticles of CuFe{sub 2}O{sub 4} (CF) and Cu{sub 0.8}Zn{sub 0.2}Fe{sub 2}O{sub 4} (CZF) were synthesized using co-precipitation method to study the effect of Zn doping in Cu-ferrite. The X-ray diffraction (XRD) patterns were well fitted with two-phase structure using Rietveld analysis as Fd-3 m space group (spinel system) and C12/c1 space group (monoclinic system CuO-phase). The average crystallite size of the CF and CZF nanoparticles for spinel structure are 6 and 7 nm respectively. The spinel phase fraction is increased from 56% to 71% with Zn-doping of 20% in CF. The transmission electron micrograph analysis showed the narrow size distribution formore » CZF nanoparticles. The magnetization plots as a function of magnetic field (M (H)) of CF and CZF nanoparticles indicate superparamagnetic behavior. The magnetization is increased with Zn-doping in CF. The stable spinel Cu-ferrite can be obtained with Zn-doping in CF.« less

Structural, microstructural and vibrational analyses of the monoclinic tungstate BiLuWO6

NASA Astrophysics Data System (ADS)

Ait Ahsaine, H.; Taoufyq, A.; Patout, L.; Ezahri, M.; Benlhachemi, A.; Bakiz, B.; Villain, S.; Guinneton, F.; Gavarri, J.-R.

2014-10-01

The bismuth lutetium tungstate phase BiLuWO6 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 represented 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 BiREWO6 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 WO6 octahedron distortions in the structure.

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

Atomic displacements in the charge ice pyrochlore Bi2Ti2O6O' studied by neutron total scattering

NASA Astrophysics Data System (ADS)

Shoemaker, Daniel P.; Seshadri, Ram; Hector, Andrew L.; Llobet, Anna; Proffen, Thomas; Fennie, Craig J.

2010-04-01

The oxide pyrochlore Bi2Ti2O6O' is known to be associated with large displacements of Bi and O' atoms from their ideal crystallographic positions. Neutron total scattering, analyzed in both reciprocal and real space, is employed here to understand the nature of these displacements. Rietveld analysis and maximum entropy methods are used to produce an average picture of the structural nonideality. Local structure is modeled via large-box reverse Monte Carlo simulations constrained simultaneously by the Bragg profile and real-space pair distribution function. Direct visualization and statistical analyses of these models show the precise nature of the static Bi and O' displacements. Correlations between neighboring Bi displacements are analyzed using coordinates from the large-box simulations. The framework of continuous symmetry measures has been applied to distributions of O'Bi4 tetrahedra to examine deviations from ideality. Bi displacements from ideal positions appear correlated over local length scales. The results are consistent with the idea that these nonmagnetic lone-pair containing pyrochlore compounds can be regarded as highly structurally frustrated systems.

Studies on structural, electrical, thermal and magnetic properties of YFeO3 ceramic

NASA Astrophysics Data System (ADS)

Suthar, Lokesh; Jha, V. K.; Bhadala, Falguni; Roy, M.; Sahu, S.; Barbar, S. K.

2017-10-01

The polycrystalline ceramic sample of YFeO3 has been synthesized by high-temperature solid-state reaction method using high-purity oxides. The formation of the compound has been confirmed by the room temperature (RT) X-ray diffraction analysis. The refined lattice parameters obtained by Rietveld analysis are: a = 5.5907 Å, b = 7.6082 Å and c = 5.2849 Å with orthorhombic symmetry in space group Pnma. The average grain size obtained from the SEM micrograph is around 2 µm. The three-dimensional surface morphology has been investigated using atomic force microscopy (AFM), and the average roughness measured in the sampling area of 100.07 µm2 is around 142 nm. The frequency- and temperature-dependent dielectric constant has been measured. The material shows high dielectric constant value (750) at RT. The activation energy obtained from dc conductivity using Arrhenius relation σ = σ oexp(-Ea/kT) is 2.12 eV. Thermal analysis shows phase change around 625 K with minimum weight loss (i.e. 1.27% of initial weight) from RT to 1273 K. The magnetization measurement indicates soft magnetic behaviour.

Electron doping effect on structural and magnetic phase transitions in Sr{sub 2-x}Nd{sub x}FeMoO{sub 6} double perovskites

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

Azad, A.K.; Eriksson, S.-G.; Khan, Abdullah

2006-05-15

Polycrystalline Sr{sub 2-x}Nd{sub x}FeMoO{sub 6} (x=0.0, 0.1, 0.2, 0.4) materials have been synthesized by a citrate co-precipitation method and studied by neutron powder diffraction (NPD) and magnetization measurements. Rietveld analysis of the temperature-dependent NPD data shows that the compounds (x=0.0, 0.1, 0.2) crystallize in the tetragonal symmetry in the range 10-400K and converts to cubic symmetry above 450K. The unit cell volume increases with increasing Nd{sup 3+} concentration, which is an electronic effect in order to change the valence state of the B-site cations. Antisite defects at the Fe-Mo sublattice increases with the Nd{sup 3+} doping. The Curie temperature wasmore » increased from 430K for x=0 to 443K for x=0.4. The magnetic moment of the Fe-site decreases while the Mo-site moment increases with electron doping. The antiferromagnetic arrangement causes the system to show a net ferrimagnetic moment.« less

WinPSSP : a revamp of the computer program PSSP and its performance solving the crystal structures of small organic compounds and solids of biological and pharmaceutical interest

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

Pagola, Silvina; Polymeros, Alekos; Kourkoumelis, Nikolaos

2017-02-01

The direct-space methods softwarePowder Structure Solution Program(PSSP) [Pagola & Stephens (2010).J. Appl. Cryst.43, 370–376] has been migrated to the Windows OS and the code has been optimized for fast runs.WinPSSPis a user-friendly graphical user interface that allows the input of preliminary crystal structure information, integrated intensities of the reflections and FWHM, the definition of structural parameters and a simulated annealing schedule, and the visualization of the calculated and experimental diffraction data overlaid for each individual solution. The solutions are reported as filename.cif files, which can be used to analyze packing motifs and chemical bonding, and to input the atomic coordinatesmore » into the Rietveld analysis softwareGSAS. WinPSSPperformance in straightforward crystal structure determinations has been evaluated using 18 molecular solids with 6–20 degrees of freedom. The free-distribution program as well as multimedia tutorials can be accessed at http://users.uoi.gr/nkourkou/winpssp/.« less

Structural and transport properties of Yb substituted YBaCo4O7

NASA Astrophysics Data System (ADS)

Singh, Bharat; Kumar, Naresh; Gaur, N. K.; Rayaprol, S.

2012-06-01

We investigate a series of compounds of the type, Y1-xYbxBaCo4O7, to study the effect of chemical pressure on the structural and electrical transport properties of a geometrically frustrated cobaltite, YBaCo4O7. Rietveld analysis of XRD data were carried out for all the samples studied. The four probe resistivity measurements were carried out to understand the transport mechanism in these compounds at temperatures below room temperatures. These results are presented and discussed in the context of ongoing efforts in studying geometrically frustrated magnetic compounds with novel physical properties.

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.

Multiple-step preparation and physicochemical characterization of crystalline α-germanium hydrogenphosphate

NASA Astrophysics Data System (ADS)

Romano, Ricardo; Ruiz, Ana I.; Alves, Oswaldo L.

2004-04-01

The reaction between germanium oxide and phosphoric acid has previously been described and led to impure germanium hydrogenphosphate samples with low crystallinity. A new multiple-step route involving the same reaction under refluxing and soft hydrothermal conditions is described for the preparation of pure and crystalline α-GeP. The physicochemical characterization of the samples allows accompaniment of the reaction evolution as well as determining short- and long-range structural organization. The phase purity of the α-GeP sample was confirmed by applying Rietveld's profile analysis, which also determined the cell parameters of its crystals.

Ferro- and antiferro-magnetism in (Np, Pu)BC

NASA Astrophysics Data System (ADS)

Klimczuk, T.; Shick, A. B.; Kozub, A. L.; Griveau, J.-C.; Colineau, E.; Falmbigl, M.; Wastin, F.; Rogl, P.

2015-04-01

Two new transuranium metal boron carbides, NpBC and PuBC, have been synthesized. Rietveld refinements of powder XRD patterns of {Np,Pu}BC confirmed in both cases isotypism with the structure type of UBC. Temperature dependent magnetic susceptibility data reveal antiferromagnetic ordering for PuBC below TN = 44 K, whereas ferromagnetic ordering was found for NpBC below TC = 61 K. Heat capacity measurements prove the bulk character of the observed magnetic transition for both compounds. The total energy electronic band structure calculations support formation of the ferromagnetic ground state for NpBC and the antiferromagnetic ground state for PuBC.

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

Cathodic Properties of Al-DOPED LiCoO2 Prepared by Molten Salt Method for Li-Ion Batteries

NASA Astrophysics Data System (ADS)

Reddy, M. V.; Rao, G. V. Subba; Chowdari, B. V. R.

2006-06-01

Layered Li(Co1-xAlx)O2, x=0.05-0.25 phases have been prepared by using the one-pot molten salt method at 850 °C in air and characterized by X-ray diffraction, Rietveld refinement, SEM-EDAX, chemical analysis, BET surface area and density methods. Cathodic properties were studied at ambient temperature in cells with Li-metal as the counter electrode by cyclic voltammetry (CV), galvanostatic charge-discharge cycling (up to 130 cycles) and Impedance spectroscopy. Single-phase compounds with hexagonal layer structure formed for all x. Results showed that for x≥0.05, the Li-de-intercalation potential during the first charge-cycle occurs at a value slightly higher than that shown by pure LiCoO2 and the structural transitions that occur at ˜4.1 V and ˜ 4.2 V are suppressed. However, the transition at ˜4.5 V is not suppressed. As a consequence, the long-term cyclability of Li(Co1-xAlx)O2 is greatly improved, when cycled in the potential ranges 2.5-4.3 V and 2.5-4.4 V at the current rate of 30 mA/g. Higher 10th cycle capacities were noted for x≥0.1-0.2 in the 2.5-4.5 V range but capacity-fading was noted, by 5-7 % at the end of 55 cycles. The observed CV and impedance data have been analyzed and interpreted.

Changing the characteristics and properties of zeolite Y and nano-anatase in the formation of a nano-anatase/Y composite with improved photocatalytic and adsorption properties

NASA Astrophysics Data System (ADS)

Domoroshchina, E. N.; Chernyshev, V. V.; Kuz'micheva, G. M.; Dorokhov, A. V.; Pirutko, L. V.; Kravchenko, G. V.; Chumakov, R. B.

2018-02-01

Zeolite Y and the NTD/Y nanocomposite, which were synthesized in situ (the addition of zeolite Y to the reaction mixture in the course of the synthesis of NTD by the sulfate method), were studied by a variety of methods. The decrease in the particle size (scanning electron microscopy) and the water content in pores (X-ray powder diffraction study, the full-profile Rietveld method, IR spectroscopy, differential scanning calorimetry), the increase in OH groups content and the decrease in the water content on the surface of zeolite (X-ray photoelectron spectroscopy) in the composition of NTD/Y compared to the initial zeolite Y were all established. A larger specific surface area of NTD/Y (Brunauer-Emmet-Teller method) compared to the initial zeolite Y is due to the fact that zeolite Y in the nanocomposite contains a smaller amount of water because of the synthesis conditions and the presence of nanocrystalline NTD on the surface of zeolite particles. It was found that NTD/Y nanocomposite exhibits a higher photocatalytic activity in the model decomposition reaction of methyl orange under UV and adsorption capacity for the extraction of P(V) and As(V) ions from aqueous media compared to the initial zeolite and pure NTD obtained under the same conditions, which differs from NTD/Y by the larger particle size, the smaller specific surface and the smaller content of OH groups and water on the surface. The role of Bronsted and Lewis centers in the realization of properties is discussed.

Nanostructured Na2Ti9O19 for Hybrid Sodium-Ion Capacitors with Excellent Rate Capability.

PubMed

Bhat, Swetha S M; Babu, Binson; Feygenson, Mikhail; Neuefeind, Joerg C; Shaijumon, M M

2018-01-10

Herein, we report a new Na-insertion electrode material, Na 2 Ti 9 O 19 , as a potential candidate for Na-ion hybrid capacitors. We study the structural properties of nanostructured Na 2 Ti 9 O 19 , synthesized by a hydrothermal technique, upon electrochemical cycling vs Na. Average and local structures of Na 2 Ti 9 O 19 are elucidated from neutron Rietveld refinement and pair distribution function (PDF), respectively, to investigate the initial discharge and charge events. Rietveld refinement reveals electrochemical cycling of Na 2 Ti 9 O 19 is driven by single-phase solid solution reaction during (de)sodiation without any major structural deterioration, keeping the average structure intact. Unit cell volume and lattice evolution on discharge process is inherently related to TiO 6 distortion and Na ion perturbations, while the PDF reveals the deviation in the local structure after sodiation. Raman spectroscopy and X-ray photoelectron spectroscopy studies further corroborate the average and local structural behavior derived from neutron diffraction measurements. Also, Na 2 Ti 9 O 19 shows excellent Na-ion kinetics with a capacitve nature of 86% at 1.0 mV s -1 , indicating that the material is a good anode candidate for a sodium-ion hybrid capacitor. A full cell hybrid Na-ion capacitor is fabricated by using Na 2 Ti 9 O 19 as anode and activated porous carbon as cathode, which exhibits excellent electrochemical properties, with a maximum energy density of 54 Wh kg -1 and a maximum power density of 5 kW kg -1 . Both structural insights and electrochemical investigation suggest that Na 2 Ti 9 O 19 is a promising negative electrode for sodium-ion batteries and hybrid capacitors.

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.

Lithium ion conduction in sol-gel synthesized LiZr2(PO4)3 polymorphs

NASA Astrophysics Data System (ADS)

Kumar, Milind; Yadav, Arun Kumar; Anita, Sen, Somaditya; Kumar, Sunil

2018-04-01

Safety issue associated with the high flammability and volatility of organic electrolytes used in commercial rechargeable lithium ion batteries has led to significant attention to ceramic-based solid electrolytes. In the present study, lithium ion conduction in two polymorphs of LiZr2(PO4)3 synthesized via the sol-gel route has been investigated. Rietveld refinement of room temperature X-ray diffraction data of LiZr2(PO4)3 powders calcined at 900 °C and 1300 °C confirmed these to be the monoclinic phase with P21/n structure and rhombohedral phase with R3¯c structure, respectively. Increase in calcination temperature and resultant phase transformation improved the room temperature conductivity from 2.27×10-6 ohm-1m-1 for the monoclinic phase to 1.41×10-4 ohm-1m-1 for rhombohedral phase. Temperature dependence of conductivity was modeled using Arrhenius law and activation energy of ˜ 0.59 eV (for monoclinic phase) and ˜0.50 eV (for rhombohedral phase) were obtained.

Photocatalytic ability of Bi6Ti3WO18 nanoparticles with a mix-layered Aurivillius structure

NASA Astrophysics Data System (ADS)

Mi, Longqing; Feng, Yongyi; Cao, Lei; Xue, Mingqiang; Qin, Chuanxiang; Huang, Yanlin; Qin, Lin; Seo, Hyo Jin

2018-01-01

Aurivillius phase layered perovskites Bi6Ti3WO18 was prepared by the sol-gel citrate-complexation synthesis. The sample developed into the plate-like nanoparticles with the exposed (001) facets. The phase formation and structure have been verified via X-ray polycrystalline powder diffraction (XRD) Rietveld refinements. The nanoparticles were investigated via the measurements such as FE-SEM, TEM, EDS, and the surface analyses. UV-Vis absorption data revealed that the Aurivillius compound has a direct band characteristic with the band energy of 2.214 eV. The band structure of Bi6Ti3WO18 nanoparticles was discussed on the base of the experiments and theoretical calculation. Bi3+-containing Aurivillius Bi6Ti3WO18 shows efficient photocatalytic degradation for rhodamine B dye (RhB) with the visible light irradiation ( λ > 420 nm). Dynamic characteristic of the light-created excitons was measured by the luminescence and decay lifetime. The multivalent properties of W and Ti ions in the Aurivillius-like lattices of Bi6Ti3WO18 photocatalyst were discussed.

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

Antao, S.M.

The crystal structure of a biogenic aragonite from the nacre of an ammonite shell was obtained using synchrotron high-resolution powder X-ray diffraction (HRPXRD) data and Rietveld structure refinement. The well-preserved ammonite sample is from Alberta, Canada, and is from the Cretaceous period. The aragonite structure was refined in space group Pmcn, Z = 4, and the cell parameters obtained are a = 4.96265(2), b = 7.97016(4), c = 5.74474(3) {angstrom}, and V = 227.222(2) {angstrom}{sup 3}. The chemical analyses indicate a formula of [Ca{sub 0.995}Sr{sub 0.004}Ba{sub 0.001}]{Sigma} = 1.0(CO{sub 3}). The average and distances are 2.5281(3) and 1.2871(6)more » {angstrom}, respectively, and the average angle is 119.94(8){sup o}. The CO{sub 3} groups are non-planar. Based on crystal-structure data for biogenic and non-biogenic aragonite samples, aragonite from ammonite nacre has minimal structural distortions and is very similar to non-biogenic aragonite, in particular, a sample from Spain.« less

Tunable blue-green emission and energy transfer properties in β-Ca3(PO4)2:Eu(2+), Tb(3+) phosphors with high quantum efficiencies for UV-LEDs.

PubMed

Li, Kai; Zhang, Yang; Li, Xuejiao; Shang, Mengmeng; Lian, Hongzhou; Lin, Jun

2015-03-14

A series of Eu(2+) and Tb(3+) singly-doped and co-doped β-Ca3(PO4)2 phosphors have been synthesized via the high-temperature solid-state reaction method. Thermogravimetric (TG) analysis, fourier transform infrared (FT-IR) spectra, X-ray diffraction (XRD) patterns and Rietveld refinements, photoluminescence (PL) spectra including temperature-dependent PL and quantum efficiency, and fluorescence decay lifetimes have been used to characterise the as-prepared samples. Under UV excitation, β-Ca3(PO4)2:Eu(2+) presents a broad emission band centered at 415 nm, which can be decomposed into five symmetrical bands peaking at 390, 408, 421, 435 and 511 nm based on the substitution of five kinds of Ca(2+) sites by Eu(2+) ions. β-Ca3(PO4)2:Tb(3+) shows characteristic emission lines under Tb(3+) 4f-5d transition excitation around 223 nm. In β-Ca3(PO4)2:Eu(2+), Tb(3+) phosphors, similar excitation spectra monitored at 415 and 547 nm have been observed, which illustrates the possibility of energy transfer from Eu(2+) to Tb(3+) ions. The variations in the emission spectra and decay lifetimes further demonstrate the existence of energy transfer from Eu(2+) to Tb(3+) ions under UV excitation. The energy transfer mechanism has been confirmed to be dipole-quadrupole, which can be validated via the agreement of critical distances obtained from the concentration quenching (12.11 Å) and spectrum overlap methods (9.9-13.2 Å). The best quantum efficiency can reach 90% for the β-Ca3(PO4)2:0.01Eu(2+), 0.15Tb(3+) sample under 280 nm excitation. These results show that the developed phosphors may possess potential applications in UV-pumped white light-emitting diodes.

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

Hamdi, S.; Ouni, S.; Chaker, H.

A new compound DySr{sub 5}Ni{sub 2.4}Cu{sub 0.6}O{sub 12-{delta}} has been prepared by sol gel method and annealed at 1473 K in 1 atm of Ar gas flow. The X-ray diffraction (XRD) is used for phase identification. The sample shows to adopt the K{sub 2}NiF{sub 4}-type structure based on tolerance factor calculation. XRD analysis using the Rietveld method was carried out and it was found that DySr{sub 5}Ni{sub 2.4}Cu{sub 0.6}O{sub 12-{delta}} (Dy{sub 0.33}Sr{sub 1.67}Ni{sub 0.8}Cu{sub 0.2}O{sub 4-{delta}}') compound crystallizes in tetragonal symmetry with space group I4/mmm (Z=2). The lattice parameters are found to be at room temperature a=3.7696(5) A and c=12.3747(2)more » A. The final reliability indices were: R{sub B}=5.219% and {chi}{sup 2}=3.47. Four probe electrical resistivity measurements were performed versus temperature in the range 294-579 K. A semiconducting behaviour over the whole range of temperature, with a conductivity maximum of 0.4 S cm{sup -1} is observed at 510 K. - Graphical abstract: DySr{sub 5}Ni{sub 2.4}Cu{sub 0.6}O{sub 12-{delta}} exhibits a semi-conducting behaviour over the whole temperature range 294-579 K with a conductivity maximum of 0.4 S cm{sup -1} at 510 K. Highlights: > We described our attempts to synthesize the pure compound DySr{sub 5}Ni{sub 2.4}Cu{sub 0.6}O{sub 12-{delta}}. > Product was characterized by XRD and electrical resistivity measurements. > Iodometric titration was used for the analysis of the oxygen nonstoichiometry. > Calculated tolerance factor was included in the tetragonal symmetry stability range. > Compound exhibits a semi-conducting behaviour over the whole temperature range 294-579 K.« less

Large scale synthesis of nanostructured zirconia-based compounds from freeze-dried precursors

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

Gomez, A.; Villanueva, R.; Vie, D.

2013-01-15

Nanocrystalline zirconia powders have been obtained at the multigram scale by thermal decomposition of precursors resulting from the freeze-drying of aqueous acetic solutions. This technique has equally made possible to synthesize a variety of nanostructured yttria or scandia doped zirconia compositions. SEM images, as well as the analysis of the XRD patterns, show the nanoparticulated character of those solids obtained at low temperature, with typical particle size in the 10-15 nm range when prepared at 673 K. The presence of the monoclinic, the tetragonal or both phases depends on the temperature of the thermal treatment, the doping concentration and themore » nature of the dopant. In addition, Rietveld refinement of the XRD profiles of selected samples allows detecting the coexistence of the tetragonal and the cubic phases for high doping concentration and high thermal treatment temperatures. Raman experiments suggest the presence of both phases also at relatively low treatment temperatures. - Graphical abstract: Zr{sub 1-x}A{sub x}O{sub 2-x/2} (A=Y, Sc; 0{<=}x{<=}0.12) solid solutions have been prepared as nanostructured powders by thermal decomposition of precursors obtained by freeze-drying, and this synthetic procedure has been scaled up to the 100 g scale. Highlights: Black-Right-Pointing-Pointer Zr{sub 1-x}A{sub x}O{sub 2-x/2} (A=Y, Sc; 0{<=}x{<=}0.12) solid solutions have been prepared as nanostructured powders. Black-Right-Pointing-Pointer The synthetic method involves the thermal decomposition of precursors obtained by freeze-drying. Black-Right-Pointing-Pointer The temperature of the thermal treatment controls particle sizes. Black-Right-Pointing-Pointer The preparation procedure has been scaled up to the 100 g scale. Black-Right-Pointing-Pointer This method is appropriate for the large-scale industrial preparation of multimetallic systems.« 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

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.

Sol concentration effect on ZnO nanofibers photocatalytic activity synthesized by sol-gel dip coating method

NASA Astrophysics Data System (ADS)

Toubane, M.; Tala-Ighil, R.; Bensouici, F.; Bououdina, M.; Souier, M.; Liu, S.; Cai, W.; Iratni, A.

2017-03-01

ZnO thin films were deposited onto glass substrate by sol-gel dip coating method. The initial sol concentrations were varied from 0.2 to 0.5 M. Zinc acetate dihydrate, ethanol and Diethanolamine (DEA) were used as staring material, solvent and stabilizer respectively. The evolution of structural, optical properties and methylene blue (MB) photodegradation of the as-deposited films on sol concentration was investigated. Rietveld refinements of x-ray patterns reveal that all the as-prepared thin films have a Zincite-type structure with grain orientation along to c-axis. The strongest sol concentration is favorable for the highest crystallization quality. However, the high preferred orientation factor (POF) occurs for 0.3 M sol concentration. The field emission scanning electron microscopy observations reveals nanofibrous morphology with different lengths. The nanofibers density increases with increasing sols concentrations until forming a flower-like morphology. The EDS analysis confirms the high purity of the as-deposited ZnO films. It is found that all films present good transparency greater than 95% in the visible range; the optical band gap is slightly reduced with the increase in sol concentration. The photocatalytic degradation is enhanced by 90% with the sol concentration. The K app rate reaction increased with increasing sol concentration. The films stability is found to slightly decrease after the third cycle, especially for 0.5 M sol concentration.

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.

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.

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.

Crystallographic phases in heavy rare earth metals under megabar pressures

NASA Astrophysics Data System (ADS)

Samudrala, G. K.; Vohra, Y. K.

2012-07-01

Experiments aimed at understanding the crystallographic phases of heavy rare earth metals were carried out in a diamond anvil cell at the Advanced Photon Source, Argonne National Laboratory. Heavy rare earth metals dysprosium (Dy), holmium (Ho), erbium (Er) and thulium (Tm) were compressed to multi-megabar pressures. The rare earth crystal sequence hcp→Sm-type→dhcp→distorted-fcc (dfcc) is observed in all four elements. Upon further compression, a structural transformation to a monoclinic C2/m phase has been observed. We summarize the results from these experiments and present Rietveld structural refinements on high pressure phases for the specific case of dysprosium.

Phase transformation of Ca{sub 4}[Al{sub 6}O{sub 12}]SO{sub 4} and its disordered crystal structure at 1073 K

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

Kurokawa, Daisuke; R and D Center, Taiheiyo Cement Corporation, Chiba 285-8655; Takeda, Seiya

The phase transformation of Ca{sub 4}[Al{sub 6}O{sub 12}]SO{sub 4} and the crystal structure of its high-temperature phase were investigated by differential thermal analysis, temperature-dependent Raman spectroscopy and high-temperature X-ray powder diffraction (CuKα{sub 1}). We determined the starting temperature of the orthorhombic-to-cubic transformation during heating (=711 K) and that of the reverse transformation during cooling (=742 K). The thermal hysteresis was negative (=−31 K), suggesting the thermoelasticity of the transformation. The space group of the high temperature phase is I4{sup ¯}3m with the unit-cell dimensions of a=0.92426(2) nm and V=0.78955(2) nm{sup 3} (Z=2) at 1073 K. The initial structural model wasmore » derived by the direct methods and further refined by the Rietveld method. The final structural model showed the orientational disordering of SO{sub 4} tetrahedra. The maximum-entropy method-based pattern fitting method was used to confirm the validity of the split-atom model, in which conventional structure bias caused by assuming intensity partitioning was minimized. At around the transformation temperature during heating, the vibrational spectra, corresponding to the Raman-active SO{sub 4} internal stretching mode, showed the continuous and gradual change in the slope of full width at half maximum versus temperature curve. This strongly suggests that the orthorhombic-to-cubic phase transformation would be principally accompanied by the statistical disordering in orientation of the SO{sub 4} tetrahedra, without distinct dynamical reorientation. - Graphical abstract: (Left) Three-dimensional electron-density distributions of the SO{sub 4} tetrahedron with the split-atom model, and (right) a bird's eye view of electron densities on the plane parallel to (111). - Highlights: • Crystal structure of Ca{sub 4}[Al{sub 6}O{sub 12}]SO{sub 4} at 1073 K is determined by powder XRD. • The atom arrangements are represented by the split-atom model. • The MPF method is used to confirm the validity of the model. • The phase transition is accompanied by orientational disordering of SO{sub 4} tetrahedra.« less

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.

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

Influence of pH and fuels on the combustion synthesis, structural, morphological, electrical and magnetic properties of CoFe{sub 2}O{sub 4} nanoparticles

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

Shanmugavani, A.; Selvan, R.Kalai, E-mail: selvankram@buc.edu.in; Layek, Samar

2015-11-15

Nanocrystalline spinel cobalt ferrite particles are synthesized by simple combustion method using aspartic acid and glycine as fuels. The single phase cubic structure of CoFe{sub 2}O{sub 4} is revealed through X-ray diffraction analysis (XRD). Further the Rietveld refinement confirms the formation of inverse spinel structure of CoFe{sub 2}O{sub 4}. The characteristic functional groups of Co–O and Fe–O are identified from Fourier Transform Infrared (FT-IR) analysis. Uniform distribution of of nearly spherical particles with the size range of 40–80 nm is identified through field emission scanning electron microscope (FESEM) images. The calculated DC conductivity is 1.469 × 10{sup −7} and 2.214more » × 10{sup −8} S cm{sup −1}, for CoFe{sub 2}O{sub 4} synthesized using aspartic acid and glycine, respectively. The dielectric behavior obeys the Maxwell–Wagner interfacial polarization. The ferromagnetic behavior of CoFe{sub 2}O{sub 4} is identified using VSM analysis and the calculated coercivity is 27 Oe and saturation magnetization is 68 emu/g.« less

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

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.

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.

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.

Size-dependent photocatalytic activity of La0.8Sr0.2MnO3 nanoparticles prepared by hydrothermal synthesis

NASA Astrophysics Data System (ADS)

Rahmani Afje, F.; Ehsani, M. H.

2018-04-01

Synthesize of La0.8Sr0.2MnO3 (LSMO) manganite were carried out in different particle sizes by hydrothermal method. Structural and optical properties of the prepared specimens were studied by x-ray diffraction (XRD), Fourier transform infra-red (FT-IR) spectroscopy, field emission scanning electron microscopy (FESEM), and UV–vis spectroscopy. The XRD study, coupled with the Rietveld refinement, exhibited rhombohedral structure with R-3C space group. Using the FT-IR and FESEM analyses, the perovskite structure of the samples with Nano-rod-like morphologies were inferred. Furthermore, the average sizes of 48.11, 70.99 and 111.45 nm were obtained for the ones sintered at 800, 900, and 1000 °C temperatures, respectively. The optical research showed that band gap energy is about 2.13 eV, being suitable in visible-light photocatalytic activity for water purification from dyes and toxic organic materials. The photo-degradation efficiency for decolorizing methyl orange solution (10 ppm) for various samples (100 ppm) were systematically probed and a strong relation is concluded between particle size and photocatalytic activity.

Effect of addition of nanoparticle TiO 2/SiO 2 on the superconducting properties of MgB 2

NASA Astrophysics Data System (ADS)

Zhang, Y.; Zhou, S. H.; Wang, X. L.; Dou, S. X.

2008-09-01

In this paper, bulk MgB 2 was prepared by doping with nanoparticle TiO 2 surface-modified by 5-10% SiO 2. The doping ratio of TiO 2/SiO 2 to MgB 2 was 0, 5, 10, and 15 wt%. The sintering temperature varied from 650 °C to 950 °C. Quantitative X-ray diffraction (XRD) analysis was performed to obtain the lattice constants and the weight fraction of impurities using the Rietveld method. It was found that the critical temperature ( Tc) increases with the lattice constants. The critical current density ( Jc) is affected by the doping ratio and the sintering temperature. The Jc exhibited the highest value at the doping ratio of 10 wt% for 5 K and 20 K and at the doping ratio of 5 wt% for 30 K, when the sintering temperature was fixed at 750 °C. When the doping ratio was fixed at 5 wt%, the samples with the sintering temperature of 750 °C had the best Jc for 5 K and 20 K, while the sample with the sintering temperature of 850 °C exhibited the highest Jc at 30 K.

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.

Low-Temperature Synthesis, Structural Characterization, and Electrochemistry of Ni-Rich Spinel-like LiNi 2–yMn yO 4 (0.4 ≤ y ≤ 1)

DOE PAGES

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

2015-10-28

The thermal conversion of chemically delithiated layered Li 0.5Ni 1–yMn yO 2 (0.2 ≤ y ≤ 0.5) into spinel-like LiNi 2–yMn yO 4 (0.4 ≤ y ≤ 1) has been systematically investigated in this paper. The formed spinel-like phases are metastable and cannot be accessed by a conventional high-temperature solid-state method. The layered-to-spinel transformation mechanism has been studied by the Rietveld refinement of in situ neutron diffraction as a function of temperature (25–300 °C). In particular, the ionic diffusion of Li and M ions is quantified at different temperatures. Electrochemistry of the metastable spinel-like phases obtained has been studied inmore » lithium-ion cells. A bond valence sum map has been performed to understand the ionic diffusion of lithium ions in the Ni-rich layered, spinel, and rock-salt structures. Finally, the study can aid the understanding of the possible phases that could be formed during the cycling of Ni-rich layered oxide cathodes.« less

Low-Temperature Synthesis, Structural Characterization, and Electrochemistry of Ni-Rich Spinel-like LiNi 2–yMn yO 4 (0.4 ≤ y ≤ 1)

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

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

The thermal conversion of chemically delithiated layered Li 0.5Ni 1–yMn yO 2 (0.2 ≤ y ≤ 0.5) into spinel-like LiNi 2–yMn yO 4 (0.4 ≤ y ≤ 1) has been systematically investigated in this paper. The formed spinel-like phases are metastable and cannot be accessed by a conventional high-temperature solid-state method. The layered-to-spinel transformation mechanism has been studied by the Rietveld refinement of in situ neutron diffraction as a function of temperature (25–300 °C). In particular, the ionic diffusion of Li and M ions is quantified at different temperatures. Electrochemistry of the metastable spinel-like phases obtained has been studied inmore » lithium-ion cells. A bond valence sum map has been performed to understand the ionic diffusion of lithium ions in the Ni-rich layered, spinel, and rock-salt structures. Finally, the study can aid the understanding of the possible phases that could be formed during the cycling of Ni-rich layered oxide cathodes.« less

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.

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).

Low-Temperature Synthesis, Structural Characterization, and Electrochemistry of Ni-Rich Spinel-like LiNi 2–y Mn y O 4 (0.4 ≤ y ≤ 1)

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

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

The thermal conversion of chemically delithiated layered Li 0.5Ni 1-yMn yO 2 (0.2 ≤ y ≤ 0.5) into spinel-like LiNi 2-yMn yO 4 (0.4 ≤ y ≤ 1) has been systematically investigated. The formed spinel-like phases are metastable and cannot be accessed by a conventional high-temperature solid-state method. The layered-to-spinel transformation mechanism has been studied by the Rietveld refinement of in situ neutron diffraction as a function of temperature (25–300 °C). In particular, the ionic diffusion of Li and M ions is quantified at different temperatures. Electrochemistry of the metastable spinel-like phases obtained has been studied in lithium-ion cells. Amore » bond valence sum map has been performed to understand the ionic diffusion of lithium ions in the Ni-rich layered, spinel, and rock-salt structures. The study can aid the understanding of the possible phases that could be formed during the cycling of Ni-rich layered oxide cathodes.« less

Further Improvement of the RITS Code for Pulsed Neutron Bragg-edge Transmission Imaging

NASA Astrophysics Data System (ADS)

Sato, H.; Watanabe, K.; Kiyokawa, K.; Kiyanagi, R.; Hara, K. Y.; Kamiyama, T.; Furusaka, M.; Shinohara, T.; Kiyanagi, Y.

The RITS code is a unique and powerful tool for a whole Bragg-edge transmission spectrum fitting analysis. However, it has had two major problems. Therefore, we have proposed methods to overcome these problems. The first issue is the difference in the crystallite size values between the diffraction and the Bragg-edge analyses. We found the reason was a different definition of the crystal structure factor. It affects the crystallite size because the crystallite size is deduced from the primary extinction effect which depends on the crystal structure factor. As a result of algorithm change, crystallite sizes obtained by RITS drastically approached to crystallite sizes obtained by Rietveld analyses of diffraction data; from 155% to 110%. The second issue is correction of the effect of background neutrons scattered from a specimen. Through neutron transport simulation studies, we found that the background components consist of forward Bragg scattering, double backward Bragg scattering, and thermal diffuse scattering. RITS with the background correction function which was developed through the simulation studies could well reconstruct various simulated and experimental transmission spectra, but refined crystalline microstructural parameters were often distorted. Finally, it was recommended to reduce the background by improving experimental conditions.

Low carrier semiconductor like behavior in Lu3Ir4Ge13 single crystal

NASA Astrophysics Data System (ADS)

Kumar, Anil; Matteppanavar, Shidaling; Thamizhavel, A.; Ramakrishnan, S.

2018-04-01

Single crystal of Lu3Ir4Ge13 crystallizing in the Yb3Rh4Sn13-type cubic crystal structure has been grown by Czochralski method in a tetra-arc furnace. In this paper we report on the crystal structure, magnetic and transport properties of Lu3Ir4Ge13. The analysis of the powder x-ray diffraction (XRD) studies revealed that Lu3Ir4Ge13 crystallizes in a cubic structure with the space group Pm-3n, no. 223. The lattice parameter was obtained from the Rietveld refinement of the room temperature XRD data which amounts to 8.904 (3) Å with low R factors. The temperature dependence of the resistivity exhibited semiconductor like behavior till 1.8 K, with a broad hump around 15 - 62 K. This hump was observed in both warming and cooling cycle with a very small hysteresis, it may be due to the existence of structural transition from high - low symmetry. The temperature dependent magnetization data shows the diamagnetic behavior with an anomaly around 70 K, which is well supported by the derivative of resistivity data.

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.

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.

An insight into the influence of crystallite size on the performances of microsized spherical Li(Ni0.5Co0.2Mn0.3)O2 cathode material composed of aggregated nanosized particles

NASA Astrophysics Data System (ADS)

Fan, Guangxin; Wen, Yin; Liu, Baozhong; Yang, Wenpeng

2018-02-01

Relationships between the performance and the crystallite size of the microsized spherical Li(Ni0.5Co0.2Mn0.3)O2 cathode material composed of aggregated nanosized primary particles have been comprehensively studied. The cathode material was synthesized by a high-temperature solid-state method. The results obtained by XRD, Rietveld refinement, SEM, HR-TEM, DSC, and galvanostatic test show that the crystallite size (XS) of Li(Ni0.5Co0.2Mn0.3)O2 is greatly affected by the temperature in the range of 750 to 820 °C. Most of all, the crystallite size plays a unique role in the performance of the material. That is, the electrochemical characteristics of Li(Ni0.5Co0.2Mn0.3)O2, such as discharge capacity, rate performance, and thermal stability, are closely related to the crystallite size. Furthermore, the retention of discharge capacity is determined by that of crystallite size in Li(Ni0.5Co0.2Mn0.3)O2 after 100 cycles.

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.

Discovery of a Red-Emitting Li3RbGe8O18:Mn4+ Phosphor in the Alkali-Germanate System: Structural Determination and Electronic Calculations.

PubMed

Singh, Satendra Pal; Kim, Minseuk; Park, Woon Bae; Lee, Jin-Woong; Sohn, Kee-Sun

2016-10-17

A solid-state combinatorial chemistry approach, which used the A-Ge-O (A = Li, K, Rb) system doped with a small amount of Mn 4+ as an activator, was adopted in a search for novel red-emitting phosphors. The A site may have been composed of either a single alkali metal ion or of a combination of them. This approach led to the discovery of a novel phosphor in the above system with the chemical formula Li 3 RbGe 8 O 18 :Mn 4+ . The crystal structure of this novel phosphor was solved via direct methods, and subsequent Rietveld refinement revealed a trigonal structure in the P3̅1m space group. The discovered phosphor is believed to be novel in the sense that neither the crystal structure nor the chemical formula matches any of the prototype structures available in the crystallographic information database (ICDD or ICSD). The measured photoluminescence intensity that peaked at a wavelength of 667 nm was found to be much higher than the best intensity obtained among all the existing A 2 Ge 4 O 9 (A = Li, K, Rb) compounds in the alkali-germanate system. An ab initio calculation based on density function theory (DFT) was conducted to verify the crystal structure model and compare the calculated value of the optical band gap with the experimental results. The optical band gap obtained from diffuse reflectance measurement (5.26 eV) and DFT calculation (4.64 eV) results were in very good agreement. The emission wavelength of this phosphor that exists in the deep red region of the electromagnetic spectrum may be very useful for increasing the color gamut of LED-based display devices such as ultrahigh-definition television (UHDTV) as per the ITU-R BT.2020-2 recommendations and also for down-converter phosphors that are used in solar-cell applications.

(Na,□)5[MnO2]13 nanorods: a new tunnel structure for electrode materials determined ab initio and refined through a combination of electron and synchrotron diffraction data

PubMed Central

Mugnaioli, Enrico; Gemmi, Mauro; Merlini, Marco; Gregorkiewitz, Michele

2016-01-01

(Nax□1 − x)5[MnO2]13 has been synthesized with x = 0.80 (4), corresponding to Na0.31[MnO2]. This well known material is usually cited as Na0.4[MnO2] and is believed to have a romanèchite-like framework. Here, its true structure is determined, ab initio, by single-crystal electron diffraction tomography (EDT) and refined both by EDT data applying dynamical scattering theory and by the Rietveld method based on synchrotron powder diffraction data (χ2 = 0.690, R wp = 0.051, R p = 0.037, R F2 = 0.035). The unit cell is monoclinic C2/m, a = 22.5199 (6), b = 2.83987 (6), c = 14.8815 (4) Å, β = 105.0925 (16)°, V = 918.90 (4) Å3, Z = 2. A hitherto unknown [MnO2] framework is found, which is mainly based on edge- and corner-sharing octahedra and comprises three types of tunnels: per unit cell, two are defined by S-shaped 10-rings, four by egg-shaped 8-rings, and two by slightly oval 6-rings of Mn polyhedra. Na occupies all tunnels. The so-determined structure excellently explains previous reports on the electrochemistry of (Na,□)5[MnO2]13. The trivalent Mn3+ ions concentrate at two of the seven Mn sites where larger Mn—O distances and Jahn–Teller distortion are observed. One of the Mn3+ sites is five-coordinated in a square pyramid which, on oxidation to Mn4+, may easily undergo topotactic transformation to an octahedron suggesting a possible pathway for the transition among different tunnel structures. PMID:27910840

Magnetism and Hyperfine Parameters in Iron Rich Gd_2Fe_{17-x}Si_x Intermetallics

NASA Astrophysics Data System (ADS)

Nouri, K.; Bartoli, T.; Chrobak, A.; Moscovici, J.; Bessais, L.

2018-04-01

Gd_2Fe_{17-x}Si_x (x = 0.25 , 0.5 and 1) samples were synthesized by arc melting and annealed at 1073 K for 1 week. X-ray diffraction analysis by the Rietveld method has shown that these materials crystallize in the rhombohedral Th_2Zn_{17} -type structure (space group R\\bar{3}m ). The Curie temperature increases with Si content x, whereas the unit-cell parameters decrease slightly. The temperature dependence of magnetization data revealed that Gd_2Fe_{17-x}Si_x exhibits a second-order ferromagnetic to paramagnetic phase transition in the vicinity of the Curie temperature. Exchange coupling parameters of R-R, M-M and R-M (R—rare earth, M—transition metal) have been determined from M(T) magnetization curves based on the mean field theory calculation. The magnetic entropy change Δ S_M and the relative cooling power were estimated from isothermal magnetization curves for all samples. In the proximity of {T}_C and in an applied field of 1.56 T, Δ S_M reached a maximum values of 1.38, 1.67 and 3.07 J/kg K for x = 0.25, 0.5 and 1, respectively. We have calculated the magnetic moment per Fe atom from magnetization measurements at 293 K up to 17 kOe, and it decreases with Si content. These results are verified by the Mössbauer spectrometry measurements obtained at the same temperature. The Mössbauer spectra analysis is based on the correlation between the Wigner-Seitz volume and the isomer-shift evolution of each specific site 6c, 9d, 18f, and 18h of the R\\bar{3} m structure. For all Si concentrations, the magnitude of the hyperfine fields are {H_HF}{6c} > {H_HF}{9d} > {H_HF}{18f} > {H_HF}{18h} . The mean hyperfine field decreases with the Si content.

Magnetism and Hyperfine Parameters in Iron Rich Gd_2Fe_{17-x}Si_x Intermetallics

NASA Astrophysics Data System (ADS)

Nouri, K.; Bartoli, T.; Chrobak, A.; Moscovici, J.; Bessais, L.

2018-07-01

Gd_2Fe_{17-x}Si_x (x = 0.25, 0.5 and 1) samples were synthesized by arc melting and annealed at 1073 K for 1 week. X-ray diffraction analysis by the Rietveld method has shown that these materials crystallize in the rhombohedral Th_2Zn_{17}-type structure (space group R\\bar{3}m). The Curie temperature increases with Si content x, whereas the unit-cell parameters decrease slightly. The temperature dependence of magnetization data revealed that Gd_2Fe_{17-x}Si_x exhibits a second-order ferromagnetic to paramagnetic phase transition in the vicinity of the Curie temperature. Exchange coupling parameters of R- R, M- M and R- M ( R—rare earth, M—transition metal) have been determined from M( T) magnetization curves based on the mean field theory calculation. The magnetic entropy change Δ S_M and the relative cooling power were estimated from isothermal magnetization curves for all samples. In the proximity of {T}_C and in an applied field of 1.56 T, Δ S_M reached a maximum values of 1.38, 1.67 and 3.07 J/kg K for x = 0.25, 0.5 and 1, respectively. We have calculated the magnetic moment per Fe atom from magnetization measurements at 293 K up to 17 kOe, and it decreases with Si content. These results are verified by the Mössbauer spectrometry measurements obtained at the same temperature. The Mössbauer spectra analysis is based on the correlation between the Wigner-Seitz volume and the isomer-shift evolution of each specific site 6 c, 9 d, 18 f, and 18 h of the R\\bar{3}m structure. For all Si concentrations, the magnitude of the hyperfine fields are {H_HF}{6c} > {H_HF}{9d} > {H_HF}{18f} > {H_HF}{18h}. The mean hyperfine field decreases with the Si content.

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.

Colossal change in thermopower with temperature-driven p-n-type conduction switching in La x Sr2-x TiFeO6 double perovskites

NASA Astrophysics Data System (ADS)

Roy, Pinku; Maiti, Tanmoy

2018-02-01

Double perovskite materials have been studied in detail by many researchers, as their magnetic and electronic properties can be controlled by the substitution of alkaline earth metals or lanthanides in the A site and transition metals in the B site. Here we report the temperature-driven, p-n-type conduction switching assisted, large change in thermopower in La3+-doped Sr2TiFeO6-based double perovskites. Stoichiometric compositions of La x Sr2-x TiFeO6 (LSTF) with 0  ⩽  x  ⩽  0.25 were synthesized by the solid-state reaction method. Rietveld refinement of room-temperature XRD data confirmed a single-phase solid solution with cubic crystal structure and Pm\\bar{3}m space group. From temperature-dependent electrical conductivity and Seebeck coefficient (S) studies it is evident that all the compositions underwent an intermediate semiconductor-to-metal transition before the semiconductor phase reappeared at higher temperature. In the process of semiconductor-metal-semiconductor transition, LSTF compositions demonstrated temperature-driven p-n-type conduction switching behavior. The electronic restructuring which occurs due to the intermediate metallic phase between semiconductor phases leads to the colossal change in S for LSTF oxides. The maximum drop in thermopower (ΔS ~ 2516 µV K-1) was observed for LSTF with x  =  0.1 composition. Owing to their enormous change in thermopower of the order of millivolts per kelvin, integrated with p-n-type resistance switching, these double perovskites can be used for various high-temperature multifunctional device applications such as diodes, sensors, switches, thermistors, thyristors, thermal runaway monitors etc. Furthermore, the conduction mechanisms of these oxides were explained by the small polaron hopping model.

Thermoelectric Properties of In-Doped Cu2ZnGeSe4

NASA Astrophysics Data System (ADS)

Chetty, R.; Bali, A.; Femi, O. E.; Chattopadhyay, K.; Mallik, R. C.

2016-03-01

Recently, much research has been focused on finding new thermoelectric materials. Cu-based quaternary chalcogenides that belong to A2BCD4 (A = Cu; B = Zn, Cd; C = Sn, Ge; D = S, Se, Te) are wide band gap materials and one of the potential thermoelectric materials due to their complex crystal structures. In this study, In-doped quaternary compounds Cu2ZnGe1- x In x Se4 ( x = 0, 0.025, 0.05, 0.075, 0.1) were prepared by a solid state synthesis method. Powder x-ray diffraction patterns of all the samples showed a tetragonal crystal structure (space group I- 42m) of the main phase with a trace amount of impurity phases, which was further confirmed by Rietveld analysis. The elemental composition of all the samples showed a slight deviation from the nominal composition with the presence of secondary phases. All the transport properties were measured in the temperature range 373-673 K. The electrical resistivity of all the samples initially decreased up to ˜470 K and then increased with increase in temperature upto 673 K, indicating the transition from semiconducting to metallic behavior. Positive Seebeck coefficients for all the samples revealed that holes are the majority carriers in the entire temperature range. The substitution of In3+ on Ge4+ introduces holes and results in the decrease of resistivity as well as the Seebeck coefficient, thereby leading to the optimization of the power factor. The lattice thermal conductivity of all the samples decreased with increasing temperature, indicating the presence of phonon-phonon scattering. As a result, the thermoelectric figure of merit ( zT) of the doped sample showed an increase as compared to the undoped compound.

Structural and Electrochemical Characterization of Zn1-xFexO-Effect of Aliovalent Doping on the Li⁺ Storage Mechanism.

PubMed

Giuli, Gabriele; Eisenmann, Tobias; Bresser, Dominic; Trapananti, Angela; Asenbauer, Jakob; Mueller, Franziska; Passerini, Stefano

2017-12-29

In order to further improve the energy and power density of state-of-the-art lithium-ion batteries (LIBs), new cell chemistries and, therefore, new active materials with alternative storage mechanisms are needed. Herein, we report on the structural and electrochemical characterization of Fe-doped ZnO samples with varying dopant concentrations, potentially serving as anode for LIBs (Rechargeable lithium-ion batteries). The wurtzite structure of the Zn 1-x Fe x O samples (with x ranging from 0 to 0.12) has been refined via the Rietveld method. Cell parameters change only slightly with the Fe content, whereas the crystallinity is strongly affected, presumably due to the presence of defects induced by the Fe 3+ substitution for Zn 2+ . XANES (X-ray absorption near edge structure) data recorded ex situ for Zn 0.9 Fe 0.1 O electrodes at different states of charge indicated that Fe, dominantly trivalent in the pristine anode, partially reduces to Fe 2+ upon discharge. This finding was supported by a detailed galvanostatic and potentiodynamic investigation of Zn 1-x Fe x O-based electrodes, confirming such an initial reduction of Fe 3+ to Fe 2+ at potentials higher than 1.2 V (vs. Li⁺/Li) upon the initial lithiation, i.e., discharge. Both structural and electrochemical data strongly suggest the presence of cationic vacancies at the tetrahedral sites, induced by the presence of Fe 3+ (i.e., one cationic vacancy for every two Fe 3+ present in the sample), allowing for the initial Li⁺ insertion into the ZnO lattice prior to the subsequent conversion and alloying reaction.

Formation, stability and crystal structure of mullite-type Al{sub 6−x}B{sub x}O{sub 9}

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

Hoffmann, K., E-mail: Kristin.Hoffmann@uni-bremen.de; Institut für Anorganische Chemie und Kristallographie, FB02, Leobener Straße/NW2, Universität Bremen, D-28359 Bremen; Hooper, T.J.N.

2016-11-15

Mullite-type Al{sub 6−x}B{sub x}O{sub 9} compounds were studied by means of powder diffraction and spectroscopic methods. The backbones of this structure are chains of edge-connected AlO{sub 6} octahedra crosslinked by AlO- and BO-polyhedra. Rietveld refinements show that the a and b lattice parameters can be well resolved, thus representing an orthorhombic metric. A continuous decrease of the lattice parameters most pronounced in c-direction indicates a solid solution for Al{sub 6−x}B{sub x}O{sub 9} with 1.09≤x≤2. A preference of boron in 3-fold coordination is confirmed by {sup 11}B MAS NMR spectroscopy and Fourier calculations based on neutron diffraction data collected at 4more » K. Distance Least Squares modeling was performed to simulate a local geometry avoiding long B-O distances linking two octahedral chains by planar BO{sub 3} groups yielding split positions for the oxygen atoms and a strong distortion in the octahedral chains. The lattice thermal expansion was calculated using the Grüneisen first-order equation of state Debye-Einstein-Anharmonicity model. - Graphical abstract: Local distortion induced by boron linking the octahedral chains. - Highlights: • Decreasing lattice parameters indicate a solid solution for Al{sub 6−x}B{sub x}O{sub 9} (1.09≤x≤2). • B-atoms induce a local distortion of neighboring AlO{sub 6} octahedra. • A preference of boron in BO{sub 3} coordination is confirmed by {sup 11}B MAS NMR spectroscopy. • An optimized structural model for Al{sub 6−x}B{sub x}O{sub 9} is presented.« less

Thermoelectric power factor of La0.9M0.1FeO3 (M = Ca and Ba) system: Structural, band gap and electrical transport evaluations

NASA Astrophysics Data System (ADS)

Karthikeyan, N.; Kumar, R. Ramesh; Jaiganesh, G.; Sivakumar, K.

2018-01-01

The search for thermoelectric materials has been incredibly increased due to the increase in global energy demand. Hence the present work focus on preparation and characterization of thermal transport phenomena of pure and Ba/Ca substituted perovskite LaFeO3 orthoferrite system. The conventional solid state reaction technique is utilized for the preparation of LaFeO3 and La0.9M0.1FeO3 (M = Ca and Ba) compounds. Crystal structure analyses of the prepared samples are analyses using Rietveld refinement process which confirms the orthoferrite crystal structure of all the prepared compounds with induced distortion in position of atoms by the incorporation of substituent atoms. The electronic structure calculations are performed by VASP. As the LaFeO3 compound is a strongly energy correlated system, the Density Functional Theory (DFT) calculations are performed by DFT + U (Hubbard function) method. The computed band gap values are compared with the energy gap values calculated from UV-Vis spectral analysis. Electrical conductivity measurement and Arrhenius behavior for the temperature range of room temperature to 650 K are analyzed and the drift increase in conductivity with respect to temperature is due to the thermally activated mobility of charge carriers. Temperature dependent thermopower analysis is also examined using homemade seebeck coefficient measurement system. The calculation of thermoelectric power factor reveals that the Ba substituted LaFeO3 compound show highest power factor value of 3.73 μW/K2 cm at higher temperature and the superior power factor values observed in the Ba substituted compound determine the material's capability in power generating devices based on thermoelectric effect.

Structural evaluations and temperature dependent photoluminescence characterizations of Eu3+-activated SrZrO3 hollow spheres for luminescence thermometry applications

PubMed Central

Das, Subrata; Som, Sudipta; Yang, Che-Yuan; Chavhan, Sudam; Lu, Chung-Hsin

2016-01-01

This research is focused on the temperature sensing ability of perovskite SrZrO3:Eu3+ hollow spheres synthesized via the sol-gel method followed by heating. The Rietveld refinement indicated that the precursors annealed at 1100 °C were crystallized to form orthorhombic SrZrO3. SrZrO3 particles exhibited non-agglomerated hollow spherical morphology with an average particle size of 300 nm. The UV-excited photoluminescence spectrum of SrZrO3:Eu3+ consisted of two regions. One region was associated with SrZrO3 trap emission, and the other one was related to the emission of Eu3+ ions. The intensity ratio of the emission of Eu3+ ions to the host emission (FIR) and the emission lifetime of Eu3+ ions were measured in the temperature range of 300–550 K. The sensitivity obtained via the lifetime method was 7.3× lower than that measured via the FIR. Within the optimum temperature range of 300–460 K, the as-estimated sensor sensitivity was increased from 0.0013 to 0.028 K−1. With a further increase in temperatures, the sensitivity started to decline. A maximum relative sensitivity was estimated to be 2.22%K−1 at 460 K. The resolutions in both methods were below 1K in the above temperature range. The results indicated the suitability of SrZrO3:Eu3+ for the distinct high temperature sensing applications. PMID:27189117

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.

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.

Characteristic length scale dependence on conductivity for La2-xErxMo2O9 (0.05 ≤ x ≤ 0.3) oxide ion conductors

NASA Astrophysics Data System (ADS)

Paul, T.; Ghosh, A.

2016-05-01

Structural property of polycrystalline La2-xErxMo2O9 has been investigated. Rietveld refinements at room temperature of the materials suggest a single phase nature with cubic symmetry (space group P213). The electron density contour plot confirms the nature of different cation-oxygen bonds. Time dependent mean square displacement (√) and the spatial extent of the sub-diffusive motion (√) are evaluated using the linear response theory. The localized hop at O2 and O3 sites is found to be favorable for oxygen ion migration for these systems.

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.

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.

Neutron Diffraction Study On Gamma To Alpha Phase Transition In Ce0.9th0.1 Alloy

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

Lashley, Jason C1; Heffner, Robert H; Llobet, A

2008-01-01

Comprehensive neutron diffraction measurements were performed to study the isostructural {gamma} {leftrightarrow} {alpha} phase transition in Ce{sub 0.9}Th{sub 0.1} alloy. Using Rietveld refinements, we obtained lattice and thermal parameters as a function of temperature. From the temperature slope of the thermal parameters, we determined Debye temperatures {Theta}{sup {gamma}}{sub D} = 133(1) K and {Theta}{sup {alpha}}{sub D} = 140(1) K for the {gamma} phase and the {alpha} phase, respectively. This result implies that the vibrational entropy change is not significant at the {gamma} {leftrightarrow} {alpha} transition, contrary to that from elemental Cerium [Phys. Rev. Lett. 92, 105702, 2004].

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

Strong enhancement in thermal conductivity of ethylene glycol-based nanofluids by amorphous and crystalline Al{sub 2}O{sub 3} nanoparticles

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

Gangwar, J.; Department of Physics, Panjab University, Chandigarh 160014; Srivastava, A. K., E-mail: aks@nplindia.org, E-mail: avanish.aks555@gmail.com

2014-08-11

In the present work, the temperature and concentration dependence of thermal conductivity (TC) enhancement in ethylene glycol (EG)-based amorphous and crystalline Al{sub 2}O{sub 3} nanofluids have been investigated at temperatures ranging from 0 to 100 °C. In our prior study, nanometer-sized particles of amorphous-, γ-, and α-Al{sub 2}O{sub 3} were prepared via a simple sol-gel process with annealing at different temperatures and characterized by various techniques. Building upon the earlier study, we probe here the crystallinity, microstructure, and morphology of the obtained α-Al{sub 2}O{sub 3} nanoparticles (NPs) by using X-ray powder diffraction with Rietveld full-profile refinement, scanning electron microscopy, and high-resolutionmore » transmission electron microscopy, respectively. In this study, we achieved a 74% enhancement in TC at higher temperature (100 °C) of base fluid EG by incorporating 1.0 vol. % of amorphous-Al{sub 2}O{sub 3}, whereas 52% and 37% enhancement is accomplished by adding γ- and α-Al{sub 2}O{sub 3} NPs, respectively. The amorphous phase of NPs appears to have good TC enhancement in nanofluids as compared to crystalline Al{sub 2}O{sub 3}. In a nutshell, these results are demonstrating the potential consequences of Al{sub 2}O{sub 3} NPs for applications of next-generation efficient energy transfer in nanofluids.« less

Detoxification and immobilization of chromite ore processing residue in spinel-based glass-ceramic.

PubMed

Liao, Chang-Zhong; Tang, Yuanyuan; Lee, Po-Heng; Liu, Chengshuai; Shih, Kaimin; Li, Fangbai

2017-01-05

A promising strategy for the detoxification and immobilization of chromite ore processing residue (COPR) in a spinel-based glass-ceramic matrix is reported in this study. In the search for a more chemically durable matrix for COPR, the most critical crystalline phase for Cr immobilization was found to be a spinel solid solution with a chemical composition of MgCr 1.32 Fe 0.19 Al 0.49 O 4 . Using Rietveld quantitative X-ray diffraction analysis, we identified this final product is with the phases of spinel (3.5wt.%), diopside (5.2wt.%), and some amorphous contents (91.2wt.%). The partitioning ratio of Cr reveals that about 77% of the Cr was incorporated into the more chemically durable spinel phase. The results of Cr K-edge X-ray absorption near-edge spectroscopy show that no Cr(VI) was observed after conversion of COPR into a glass-ceramic, which indicates successful detoxification of Cr(VI) into Cr(III) in the COPR-incorporated glass-ceramic. The leaching performances of Cr 2 O 3 and COPR-incorporated glass-ceramic were compared with a prolonged acid-leaching test, and the results demonstrate the superiority of the COPR-incorporated glass-ceramic matrix in the immobilization of Cr. The overall results suggest that the use of affordable additives has potential in more reliably immobilizing COPR with a spinel-based glass-ceramic for safer disposal of this hazardous waste. Copyright © 2016 Elsevier B.V. All rights reserved.

The formation, structure and physical properties of M(2)Pd(14+x)B(5-y) compounds, with M =  La, Ce, Pr, Nd, Sm, Eu, Gd, Lu and Th.

PubMed

Royanian, E; Bauer, E; Kaldarar, H; Galatanu, A; Khan, R T; Hilscher, G; Michor, H; Reissner, M; Rogl, P; Sologub, O; Giester, G; Gonçalves, A P

2009-07-29

Novel ternary compounds, M(2)Pd(14+x)B(5-y) (M =  La, Ce, Pr, Nd, Sm, Eu, Gd, Lu, Th; x∼0.9, y∼0.1), have been synthesized by arc melting. The crystal structures of Nd(2)Pd(14+x)B(5-y) and Th(2)Pd(14+x)B(5-y) were determined from x-ray single-crystal data and both are closely related to the structure type of Sc(4)Ni(29)B(10). All compounds were characterized by Rietveld analyses and found to be isotypic with the Nd(2)Pd(14+x)B(5-y) type. Measurements of the temperature dependent susceptibility and specific heat as well as the temperature and field dependent resistivity were employed to derive basic information on bulk properties of these compounds. The electrical resistivity of M(2)Pd(14+x)B(5-y), in general, is characterized by small RRR (residual resistance ratio) values originating from defects inherent to the crystal structure. Whereas the compounds based on Ce, Nd, Sm and Gd exhibit magnetic order, those based on Pr and Eu seem to be non-magnetic, at least down to 400 mK. While the non-magnetic ground state of the Pr based compound is a consequence of crystalline electric field effects in the context of the non-Kramers ion Pr, the lack of magnetic order in the case of the Eu based compound results from an intermediate valence state of the Eu ion.

Geochemical and mineralogical maps for soils of the conterminous United States

USGS Publications Warehouse

Smith, David B.; Cannon, William F.; Woodruff, Laurel G.; Solano, Federico; Ellefsen, Karl J.

2014-01-01

The U.S. Geological Survey began sampling in 2007 for a low-density (1 site per 1,600 square kilometers, 4,857 sites) geochemical and mineralogical survey of soils in the conterminous United States as part of the North American Soil Geochemical Landscapes Project. The sampling protocol for the national-scale survey included, at each site, a sample from a depth of 0 to 5 centimeters, a composite of the soil A horizon, and a deeper sample from the soil C horizon or, if the top of the C horizon was at a depth greater than 1 meter, a sample from a depth of approximately 80–100 centimeters. The <2-millimeter fraction of each sample was analyzed for a suite of 45 major and trace elements by methods that yield the total or near-total elemental content. The major mineralogical components in the samples from the soil A and C horizons were determined by a quantitative X-ray diffraction method using Rietveld refinement. Sampling in the conterminous United States was completed in 2010, with chemical and mineralogical analyses completed in May 2013. The resulting data set provides an estimate of the abundance and spatial distribution of chemical elements and minerals in soils of the conterminous United States and represents a baseline for soil geochemistry and mineralogy against which future changes may be recognized and quantified. This report releases geochemical and mineralogical maps along with a histogram, boxplot, and empirical cumulative distribution function plot for each element or mineral.

Microwave-assisted chemical insertion: a rapid technique for screening cathodes for Mg-ion batteries

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

Kaveevivitchai, Watchareeya; Huq, Ashfia; Manthiram, Arumugam

We report an ultrafast microwave-assisted solvothermal method for chemical insertion of Mg2+ ions into host materials using magnesium acetate [Mg(CH3COO)2] as a metal-ion source and diethylene glycol (DEG) as a reducing agent. For instance, up to 3 Mg ions per formula unit of a microporous host framework Mo2.5+yVO9+z could be inserted in as little as 30 min at 170–195 °C in air. This process is superior to the traditional method which involves the use of organometallic reagents, such as di-n-butylmagnesium [(C4H9)2Mg] and magnesium bis(2,6-di-tert-butylphenoxide) [Mg-(O-2,6-But2C6H3)2], and requires an inert atmosphere with extremely long reaction times. Considering the lack of robustmore » electrolytes for Mg-ion batteries, this facile approach can be readily used as a rapid screening technique to identify potential Mg-ion electrode hosts without the necessity of fabricating electrodes and assembling electrochemical cells. Due to the mild reaction conditions, the overall structure and morphology of the Mg-ion inserted products are maintained and the compounds can be used successfully as a cathode in Mg-ion batteries. The combined synchrotron X-ray and neutron diffraction Rietveld analysis reveals the structure of the Mg-inserted compounds and gives an insight into the interactions between the Mg ions and the open-tunnel host framework.« less

Experimental and theoretical study to explain the morphology of CaMoO4 crystals

NASA Astrophysics Data System (ADS)

Oliveira, F. K. F.; Oliveira, M. C.; Gracia, L.; Tranquilin, R. L.; Paskocimas, C. A.; Motta, F. V.; Longo, E.; Andrés, J.; Bomio, M. R. D.

2018-03-01

CaMoO4 crystals were prepared by a controlled co-precipitation method and processed in a domestic microwave-assisted hydrothermal system with two different surfactants (ethyl 4-dimethylaminobenzoate and 1,2,4,5-benzenetetracarboxylic dianhydride). The corresponding structures were characterized by X-ray diffraction and Rietveld refinement techniques, Fourier transform infrared spectroscopy, ultraviolet-visible absorption spectroscopy, and photoluminescence measurements. Field emission scanning electron microscopy was used to investigate the morphology of the as-synthesized aggregates. The structure, the surface stability of the (001), (112), (100), (110), (101), and (111) surfaces of CaMoO4, and their morphological transformations were investigated through systematic first-principles calculations within the density functional theory method at the B3LYP level. Analysis of the surface structures showed that the electronic properties were associated with the presence of undercoordinated [CaOx] (x = 5 and 6) and [MoOy] (y = 4 and 3) clusters. The relative surfaces energies were tuned to predict a complete map of the morphologies available through a Wulff construction approach. The results reveal that the experimental and theoretical morphologies obtained coincide when the surface energies of the (001) and (101) surfaces increase, while the surface energy of the (100) facet decreases simultaneously. The results provide a comprehensive catalog of the morphologies most likely to be present under realistic conditions, and will serve as a starting point for future studies on the surface chemistry of CaMoO4 crystals.

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.

In-situ TOF neutron diffraction studies of cyclic softening in superelasticity of a NiFeGaCo shape memory alloy

DOE PAGES

Yang, Hui; Yu, Dunji; Chen, Yan; ...

2016-10-24

Real-time in-situ neutron diffraction was conducted during uniaxial cycling compression of a Ni 49.3Fe 18Ga 27Co 5.7 shape memory alloy to explore the mechanism on its superelasticity at room temperature, which was manifested by the almost recoverable large strains and the apparent cyclic softening. Based on the Rietveld refinements, the real-time evolution of volume fraction of martensite was in-situ monitored, indicating the incremental amount of residual martensite with increasing load cycles. Real-time changes in intensities and lattice strains of { hkl} reflections for individual phase were obtained through fitting individual peaks, which reveal the quantitative information on phase transformation kineticsmore » as a function of grain orientation and stress/strain partitioning. Moreover, a large compressive residual stress was evidenced in the parent phase, which should be balanced by the residual martensite after the second unloading cycle. As a result, the large compressive residual stress found in the parent austenite phase may account for the cyclic effect on critical stress required for triggering the martensitic transformation in the subsequent loading.« less

Spatially-correlated Site Occupancy in the Nonstoichiometric Meta-stable ε -Al 60Sm 11 Phase during Devitrification of Al-10.2 at.% Sm Glasses

DOE PAGES

Yang, Lin; Zhang, Feng; Meng, Fan -Qiang; ...

2018-05-12

A metastable ε-Al 60Sm 11 phase appears during the initial devitrification of as-quenched Al-10.2 at.% Sm glasses. The ε phase is nonstoichiometric in nature since Al occupation is observed on the 16 f Sm lattice sites. Scanning transmission electron microscopic images reveal profound spatial correlation of Sm content on these sites, which cannot be explained by the “average crystal” description from Rietveld analysis of diffraction data. Thermodynamically favorable configurations, established by Monte Carlo (MC) simulations based on a cluster-expansion model, also give qualitatively different correlation functions from experimental observations. On the other hand, molecular dynamics simulations of the growth ofmore » ε-Al 60Sm 11 in undercooled liquid show that when the diffusion range of Sm is limited to ~4 Å, the correlation function of the as-grown crystal structure agrees well with that of the scanning transmission electronic microscopy (STEM) images. Furthermore, our results show that kinetic effects, especially the limited diffusivity of Sm atoms plays the fundamental role in determining the nonstoichiometric site occupancies of the ε-Al 60Sm 11 phase during the crystallization process.« less

Structural and dielectric properties of Ba{sub 2}LaSbO{sub 6} ceramics

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

Kumari, Premlata, E-mail: k.premlata1@gmail.com; Dutta, Alo; Sinha, T. P.

2014-04-24

The ceramic Ba{sub 2}LaSbO{sub 6} (BLS) is synthesized by the solid state reaction technique. The Rietveld refinement of X-ray diffraction pattern at room temperature shows Monoclinic P2{sub 1}/n space group symmetry with lattice parameter a = 6.0720 (0) Å, b = 6.1058 (3) Å, c = 8.6016 (6) Å and β =89.7091 ° (8). Dielectric study of sample has been performed in the temperature range from 30 °C to 300 °C in the frequency range 50 Hz to 1.1 MHz. Dielectric relaxation peaks are observed in the imaginary part of complex permittivity of the spectra. The frequency dependence of realmore » and imaginary parts of dielectric permittivity is analyzed using Cole-Cole model. The temperature dependent relaxation time is found to obey the Arrhenius law having activation energy 0.48 eV which indicates that the conduction mechanism in the materials may be due to polaron hopping based on electron carriers. The complex plane plots of BLS shows the presence of both grain and grain boundary effects. Conductivity spectra follow the power law.« less

Spatially-correlated Site Occupancy in the Nonstoichiometric Meta-stable ε -Al 60Sm 11 Phase during Devitrification of Al-10.2 at.% Sm Glasses

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

Yang, Lin; Zhang, Feng; Meng, Fan -Qiang

A metastable ε-Al 60Sm 11 phase appears during the initial devitrification of as-quenched Al-10.2 at.% Sm glasses. The ε phase is nonstoichiometric in nature since Al occupation is observed on the 16 f Sm lattice sites. Scanning transmission electron microscopic images reveal profound spatial correlation of Sm content on these sites, which cannot be explained by the “average crystal” description from Rietveld analysis of diffraction data. Thermodynamically favorable configurations, established by Monte Carlo (MC) simulations based on a cluster-expansion model, also give qualitatively different correlation functions from experimental observations. On the other hand, molecular dynamics simulations of the growth ofmore » ε-Al 60Sm 11 in undercooled liquid show that when the diffusion range of Sm is limited to ~4 Å, the correlation function of the as-grown crystal structure agrees well with that of the scanning transmission electronic microscopy (STEM) images. Furthermore, our results show that kinetic effects, especially the limited diffusivity of Sm atoms plays the fundamental role in determining the nonstoichiometric site occupancies of the ε-Al 60Sm 11 phase during the crystallization process.« less

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.

Efficient luminescent solar cells based on tailored mixed-cation perovskites

PubMed Central

Bi, Dongqin; Tress, Wolfgang; Dar, M. Ibrahim; Gao, Peng; Luo, Jingshan; Renevier, Clémentine; Schenk, Kurt; Abate, Antonio; Giordano, Fabrizio; Correa Baena, Juan-Pablo; Decoppet, Jean-David; Zakeeruddin, Shaik Mohammed; Nazeeruddin, Mohammad Khaja; Grätzel, Michael; Hagfeldt, Anders

2016-01-01

We report on a new metal halide perovskite photovoltaic cell that exhibits both very high solar-to-electric power-conversion efficiency and intense electroluminescence. We produce the perovskite films in a single step from a solution containing a mixture of FAI, PbI2, MABr, and PbBr2 (where FA stands for formamidinium cations and MA stands for methylammonium cations). Using mesoporous TiO2 and Spiro-OMeTAD as electron- and hole-specific contacts, respectively, we fabricate perovskite solar cells that achieve a maximum power-conversion efficiency of 20.8% for a PbI2/FAI molar ratio of 1.05 in the precursor solution. Rietveld analysis of x-ray diffraction data reveals that the excess PbI2 content incorporated into such a film is about 3 weight percent. Time-resolved photoluminescence decay measurements show that the small excess of PbI2 suppresses nonradiative charge carrier recombination. This in turn augments the external electroluminescence quantum efficiency to values of about 0.5%, a record for perovskite photovoltaics approaching that of the best silicon solar cells. Correspondingly, the open-circuit photovoltage reaches 1.18 V under AM 1.5 sunlight. PMID:26767196

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.

Structural differences in enamel and dentin in human, bovine, porcine, and ovine teeth.

PubMed

Ortiz-Ruiz, Antonio José; Teruel-Fernández, Juan de Dios; Alcolea-Rubio, Luis Alberto; Hernández-Fernández, Ana; Martínez-Beneyto, Yolanda; Gispert-Guirado, Francesc

2018-07-01

The aim was to study differences between crystalline nanostructures from the enamel and dentin of human, bovine, porcine, and ovine species. Dentine and enamel fragments extracted from sound human, bovine, porcine and ovine incisors and molars were mechanically ground up to a final particle size of <100μm. Samples were analyzed using X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), and differential scanning calorimetry (DSC). Human enamel (HE) and dentin (HD) showed a-axis and c-axis lengths of the carbonate apatite (CAP) crystal lattice nearer to synthetic hydroxyapatite (SHA), which had the smallest size. Enamel crystal sizes were always higher than those of dentin for all species. HE and HD had the largest crystal, followed by bovine samples. Hydroxyapatites (HAs) in enamel had a higher crystallinity index (CI), CI Rietveld and CI FTIR, than the corresponding dentin of the same species. HE and HD had the highest CIs, followed by ovine enamel (OE). The changes in heat capacity that were nearest to values in human teeth during the glass transition (ΔCp) were in porcine specimens. There was a significant direct correlation between the size of the a-axis and the substitution by both type A and B carbonates. The size of the nanocrystals and the crystallinity (CI Rietveld y CI FTIR ) were significantly and negatively correlated with the proteic phase of all the substrates. There was a strongly positive correlation between the caloric capacity, the CIs and the crystal size and a strongly negative correlation between carbonates type A and B and proteins. There are differences in the organic and inorganic content of human, bovine, porcine and ovine enamels and dentins which should be taken into account when interpreting the results of studies using animal substrates as substitutes for human material. Copyright © 2018 Elsevier GmbH. All rights reserved.

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

Determining the structure of tetragonal Y 2WO 6 and the site occupation of Eu 3+ dopant

NASA Astrophysics Data System (ADS)

Huang, Jinping; Xu, Jun; Li, Hexing; Luo, Hongshan; Yu, Xibin; Li, Yikang

2011-04-01

The compound Y 2WO 6 is prepared by solid state reaction at 750 °C using sodium chloride as mineralizer. Its structure is solved by ab-initio methods from X-ray powder diffraction data. This low temperature phase of yttrium tungstate crystallizes in tetragonal space group P4/ nmm (No. 129), Z=2, a=5.2596(2) Å, c=8.4158(4) Å. The tungsten atoms in the structure adopt an unusual [WO 6] distorted cubes coordination, connecting [YO 6] distorted cubes with oxygen vacancies at the O 2 layers while other yttrium ions Y 2 form [YO 8] cube coordination. Y 3+ ions occupy two crystallographic sites of 2 c ( C4v symmetry) and 2 a ( D2d symmetry) in the Y 2WO 6 host lattice. With Eu 3+ ions doped, the high resolution emission spectrum of Y 2WO 6:Eu 3+ suggests that Eu 3+ partly substituted for Y 3+ in these two sites. The result of the Rietveld structure refinement shows that the Eu 3+ dopants preferentially enter the 2 a site. The uniform cube coordination environment of Eu 3+ ions with the identical eight Eu-O bond lengths is proposed to be responsible for the intense excitation of long wavelength ultraviolet at 466-535 nm.

Exploring the Room-Temperature Ferromagnetism and Temperature-Dependent Dielectric Properties of Sr/Ni-Doped LaFeO3 Nanoparticles Synthesized by Reverse Micelle Method

NASA Astrophysics Data System (ADS)

Naseem, Swaleha; Khan, Shakeel; Husain, Shahid; Khan, Wasi

2018-03-01

This paper reports the thermal, microstructural, dielectric and magnetic properties of La0.75Sr0.25Fe0.65Ni0.35O3 nanoparticles (NPs) synthesized via reverse micelle technique. The thermogravimetric analysis of as-prepared NPs confirmed a good thermal stability of the sample. Powder x-ray diffraction data analyzed with a Rietveld refinement technique revealed single-phase and orthorhombic distorted perovskite crystal structure of the NPs having Pbnm space group. The transmission electron microscopy images show the crystalline nature and formation of nanostructures with a fairly uniform distribution of particles throughout the sample. Temperature-dependent dielectric properties of the NPs in accordance with the Kramers-Kronig transformation (KKT) model, universal dielectric response model and jump relaxation model have been discussed. Electrode or interface polarization is likely the cause of the observed dielectric behavior. Due to grain boundaries and Schottky barriers of the metallic electrodes of semiconductors, the depletion region is observed, which gives rise to Maxwell-Wagner relaxation and hence high dielectric constants. Magnetic studies revealed the ferromagnetic nature of the prepared NPs upon Sr and Ni doping in LaFeO3 perovskite at room temperature. Therefore, these NPs could be a potential candidate as electrode material in solid oxide fuel cells.

Structural and low temperature dielectric studies on Pb0.8Bi0.2Fe0.6Nb0.4O3 multiferroic solid solution

NASA Astrophysics Data System (ADS)

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

2018-05-01

In this paper the structural and low temperature dielectric properties of Pb0.8Bi0.2Fe0.6Nb0.4O3 (PBFNO) multiferroic solid solution were reported. PBFNO multiferroic was synthesized by single step solid state reaction method. Calcination was carried out at 700 °/2hr with different sintering temperature (800 °C, 850 °C, 900 °C, 950 °C, 1000 °C and 1050 °C for 1 hr) and time duration (800 °C for 1 to 5 hr). Single phase was confirmed through room temperature (RT) X-ray Diffraction (XRD). It was found that sintering carried out at 800°C/3 hr gives single phase. Rietveld refined lattice parameters using monoclinic structure are: a = 5.6663(1) Å, b = 5.6694(1) Å, c = 4.0112(1) Å and β = 90.038(1)° with the average grain size as 2.987 µm. The dielectric properties studied over a wide range of frequency (100 Hz - 5 MHz) and temperature (133 K - 293 K). Dielectric constant and loss tangent exhibits frequency dispersion nature at low frequency region. AC conductivity increases with increase in temperature corresponds to negative temperature coefficient of resistance (NTCR) behaviour.

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

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.

Structural analysis, optical and dielectric function of [Ba{sub 0.9}Ca{sub 0.1}](Ti{sub 0.9}Zr{sub 0.1})O{sub 3} nanocrystals

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

Herrera-Pérez, G., E-mail: guillermo.herrera@cimav.edu.mx, E-mail: damasio.morales@cimav.edu.mx; Physics of Materials Department, Centro de Investigación en Materiales Avanzados; Morales, D., E-mail: guillermo.herrera@cimav.edu.mx, E-mail: damasio.morales@cimav.edu.mx

2016-09-07

This work presents the identification of inter-band transitions in the imaginary part of the dielectric function (ε{sub 2}) derived from the Kramers–Kronig analysis for [Ba{sub 0.9}Ca{sub 0.1}](Ti{sub 0.9}Zr{sub 0.1})O{sub 3} (BCZT) nanocrystals synthesized by the modified Pechini method. The analysis started with the chemical identification of the atoms that conform BCZT in the valence loss energy region of a high energy-resolution of electron energy loss spectroscopy. The indirect band energy (E{sub g}) was determined in the dielectric response function. This result is in agreement with the UV-Vis technique, and it obtained an optical band gap of 3.16 eV. The surface andmore » volume plasmon peaks were observed at 13.1 eV and 26.2 eV, respectively. The X-ray diffraction pattern and the Rietveld refinement data of powders heat treated at 700 °C for 1 h suggest a tetragonal structure with a space group (P4 mm) with the average crystal size of 35 nm. The average particle size was determined by transmission electron microscopy.« less

Crystal structure and chemical bonding of the high-temperature phase of AgN3.

PubMed

Schmidt, Carsten L; Dinnebier, Robert; Wedig, Ulrich; Jansen, Martin

2007-02-05

The crystal structure of silver azide (AgN3) in its high-temperature (HT) modification was determined from X-ray powder diffraction data, recorded at T = 170 degrees C and was further refined by the Rietveld method. The structure is monoclinic (P21/c (No. 14), a = 6.0756(2) A, b = 6.1663(2) A, c = 6.5729(2) A, beta = 114.19(0) degrees, V = 224.62(14) A3, Z = 4) and consists of two-dimensional Ag and N containing layers in which the silver atoms are coordinated by four nitrogen atoms exhibiting a distorted square coordination environment. These sheets are linked together by weaker perpendicular Ag-N contacts, thus forming a 4 + 2 coordination geometry around the silver atoms. The phase transition has been characterized by DTA, DSC, and measurement of the density, as well as of the ionic conductivity. Both, the room-temperature and the HT phase are electrically insulating. This fact is getting support by DFT band structure calculations within the generalized gradient approximation, using the PBE functional. On the basis of the DFT band structure, the bonding characteristics of both phases are essentially the same. Finally, the implication of the existence of a low-symmetry HT-phase in a crystalline explosive concerning decomposition mechanisms is discussed.

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.

Synthesis, structural and electron paramagnetic resonance studies on Pb0.9Bi0.1Fe0.7W0.3O3 ceramic

NASA Astrophysics Data System (ADS)

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

2018-04-01

A single phase Pb0.9Bi0.1Fe0.7W0.3O3 (0.9Pb(Fe2/3W1/3)O3 - 0.1BiFeO3 or PBFW) polycrystalline ceramic was synthesized by the two step solid state reaction method, with low-temperature sintering at 800°C for 30 mins and slow cooling to room temperature (RT). Detailed studies of RT X-ray diffraction (XRD) and Raman spectroscopy measurements confirm the formation of high symmetry cubic structure with Pm-3m space group. The Rietveld refinement was carried out on RT XRD data and the obtained structural parameters are a = b = c = 3.97563(6) Å and unit cell volume = 62.837 (2) Å3. Scanning Electron Microscopy (SEM) images show the uniform distribution of grains with some agglomerated nature. RT Raman spectroscopy reveals the main broad peak at 770 cm-1, related to the A1g mode, which confirms the formation of cubic (ABO3 perovskite) structure. The single symmetric electron paramagnetic resonance (EPR) line shape with g = 2.13985 observed in PBFW was identified to be due to Fe3+ ions.

The crystal structure of synthetic simmonsite, Na 2LiAlF 6

NASA Astrophysics Data System (ADS)

Ross, Kirk C.; Mitchell, Roger H.; Chakhmouradian, Anton R.

2003-04-01

The structure of the synthetic fluoroperovskite, Na 2LiAlF 6 (simmonsite), has been determined by powder X-ray diffraction using the Rietveld method of structure refinement. The compound adopts space group P2 1/ n [#14; a=5.2842(1); b=5.3698(1); c=7.5063(2) Å; β=89.98(1)°; Z=4), and is a member of the cryolite (Na 2NaAlF 6) structural group characterized by ordering of the B-site cations (Li, Al) and tilting of the BF 6 octahedra according to the tilt scheme a-b-c+. Rotations of the B-site polyhedra are less ( ΦLi=14.9°; ΦAl=17.0°) than those found in cryolite ( ΦNa=18.6; ΦAl=23.5°) because of the larger difference in the ionic radii of the B-site cations in cryolite as compared to those in simmonsite. Na at the A-site is displaced from the special position resulting in 10- and 8-fold coordination in simmonsite and cryolite, respectively. By analogy with the synthetic compound, naturally occurring simmonsite is considered to adopt space group P2 1/ n (#14) and not the P2 1(#4) or P2 1/ m(#11) space groups.

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

Williamson-Hall analysis and optical properties of small sized ZnO nanocrystals

NASA Astrophysics Data System (ADS)

Kalita, Amarjyoti; Kalita, Manos P. C.

2017-08-01

We apply Williamson-Hall (WH) method of X-ray diffraction (XRD) line profile analysis for lattice strain estimation of small sized ZnO nanocrystals (crystallite size≈4 nm). The ZnO nanocrystals are synthesized by room temperature chemical co-precipitation followed by heating at 40 °C. Zinc acetate, sodium hydroxide and 2-mercaptoethanol (ME) are used for the synthesis of the nanocrystals. {100}, {002}, {101} and {200}, {112}, {201} line profiles in the XRD pattern are significantly merged, therefore determination of the full width at half maximum values and peak positions of the line profiles required for WH analysis has been carried out by executing Rietveld refinement of the XRD pattern. Lattice strain of the 4 nm sized ZnO nanocrystals is found to be 5.8×10-3 which is significantly higher as compared to the literature reported values for larger ones (crystallite size≈17-47 nm). Role of ME as capping agent is confirmed by Fourier transform infrared spectroscopy. The band gap of the nanocrystals is determined from the UV-Visible absorption spectrum and is found to be 3.68 eV. The photoluminescence spectrum exhibits emissions in the visible (408 nm-violet, 467 nm-blue and 538 nm-green) regions showing presence of zinc interstitial and oxygen vacancy in the ZnO nanocrystals.

Role of lattice distortion on diffuse phase transition temperatures in Bi0.5Na0.5TiO3-BaTiO3 [BNBTO] solid solutions

NASA Astrophysics Data System (ADS)

Pradhan, Lagen Kumar; Pandey, Rabichandra; Kumar, Sunil; Supriya, Sweety; Kar, Manoranjan

2018-04-01

Effect of lattice distortion on diffuse phase transition in BNBTO solid solutions near Morphotropic phase boundary (MPB) has been investigated. Solid solutions of (Bi0.5Na0.5)1-xBaxTiO3 (with mole % of x= 0.04, 0.05, 0.06, 0.07 and 0.08) were prepared by the planetary ball mill method in ethanol medium. Rietveld refinement technique with rhombohedral (R3c) and tetragonal (P4bm) crystal symmetry has been employed for structural as well as phase analysis of the solid solutions. Both rhombohedral and tetragonal lattice distortion (c/a) tends toward the pseudo-cubic crystal symmetry with the increase of mole fraction of Ba2+ near MPB (x= 6 mole %). Also, the average crystallite size and grain size decrease with increase of mole fraction of Ba2+ in BNT ceramic are due to larger ionic radius of Ba2+ and grain boundary pinning process in the solid solutions respectively. Additionally, depolarization temperature (Td) and maximum temperature (Tm) reduces due to the lattice distortion of both the phases in BNBTO solid solutions, which is explained extensively. Significant increase of dielectric constant has been observed near MPB composition (x=6%) in BNBTO solid solutions.

Partially collapsed cristobalite structure in the non molecular phase V in CO2

PubMed Central

Santoro, Mario; Gorelli, Federico A.; Bini, Roberto; Haines, Julien; Cambon, Olivier; Levelut, Claire; Montoya, Javier A.; Scandolo, Sandro

2012-01-01

Non molecular CO2 has been an important subject of study in high pressure physics and chemistry for the past decade opening up a unique area of carbon chemistry. The phase diagram of CO2 includes several non molecular phases above 30 GPa. Among these, the first discovered was CO2-V which appeared silica-like. Theoretical studies suggested that the structure of CO2-V is related to that of β-cristobalite with tetrahedral carbon coordination similar to silicon in SiO2, but reported experimental structural studies have been controversial. We have investigated CO2-V obtained from molecular CO2 at 40–50 GPa and T > 1500 K using synchrotron X-ray diffraction, optical spectroscopy, and computer simulations. The structure refined by the Rietveld method is a partially collapsed variant of SiO2 β-cristobalite, space group , in which the CO4 tetrahedra are tilted by 38.4° about the c-axis. The existence of CO4 tetrahedra (average O-C-O angle of 109.5°) is thus confirmed. The results add to the knowledge of carbon chemistry with mineral phases similar to SiO2 and potential implications for Earth and planetary interiors. PMID:22431594

Texture and elastic anisotropy of a mylonitic anorthosite from the Morin Shear Zone (Quebec, Canada)

NASA Astrophysics Data System (ADS)

Gómez Barreiro, Juan; Wenk, Hans-Rudolf; Vogel, Sven

2015-02-01

A sample of anorthosite from the granulite facies Morin Shear Zone (Quebec, Canada) was investigated for crystal preferred orientation and elastic anisotropy. Time-of-flight neutron diffraction data obtained with the HIPPO diffractometer at LANSCE were analyzed with the Rietveld method to obtain orientation distribution functions of the principal phases (plagioclase, clinopyroxene and orthopyroxene). Texture and microstructures are compatible with the plastic deformation of the aggregate under high-T conditions. All mineral phases depict a significant preferred orientation that could be related to the general top-to-the north shearing history of the Morin Shear Zone. Texture patterns suggest that (010)[001] in plagioclase and (110)[001] in clinopyroxene are likely dominant slip systems. Using preferred orientation data P- and S-waves velocities and elastic anisotropy were calculated and compared with previous studies to explore elastic properties of rocks with different pyroxene-plagioclase mixtures. P-wave velocity, S-wave splitting and anisotropy increase with clinopyroxene content. Seismic anisotropy is linked to the texture symmetry which can lead to large deviations between actual anisotropy and that measured along Cartesian XYZ sample directions (lineation/foliation reference frame). This is significant for the prediction and interpretation of seismic data, particularly for monoclinic or triclinic texture symmetries.

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.

Room Temperature Antiferromagnetic Ordering of Nanocrystalline Tb1.90Ni0.10O3

NASA Astrophysics Data System (ADS)

Mandal, J.; Dalal, M.; Sarkar, B. J.; Chakrabarti, P. K.

2017-02-01

Nanocrystalline Ni-doped terbium oxide (Tb1.90Ni0.10O3) has been synthesized by the co-precipitation method followed by annealing at 700°C for 6 h in vacuum. The crystallographic phase and the substitution of Ni2+ ions in the lattice of Tb2O3 are confirmed by Rietveld analysis of the x-ray diffraction pattern using the software MAUD. High-resolution transmission electron microscopy is also carried out to study the morphology of the sample. Magnetic measurements are carried out at different temperatures from 5 K to 300 K using a superconducting quantum interference device (SQUID) magnetometer. The dependence of the magnetization of Tb1.90Ni0.10O3 as a function of temperature ( M- T) and magnetic field ( M- H) suggests the presence of both paramagnetic and antiferromagnetic phase at room temperature, but antiferromagnetic phase dominates below ˜120 K. The lack of saturation in the M- H curve and good fitting of the M- T curve by the Johnston formula also indicate the presence of both paramagnetic and antiferromagnetic phase at room temperature. Interestingly, an antiferromagnetic to ferromagnetic phase transition is observed below ˜40 K. The result also shows a high value of magnetization at 5 K.

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).

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.

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.

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.

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.

Gas sensing behaviour of Cr{sub 2}O{sub 3} and W{sup 6+}: Cr{sub 2}O{sub 3} nanoparticles towards acetone

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

Kohli, Nipin, E-mail: nipinkohli82@yahoo.com; Hastir, Anita; Singh, Ravi Chand

2016-05-23

This paper reports the acetone gas sensing properties of Cr{sub 2}O{sub 3} and 2% W{sup 6+} doped Cr{sub 2}O{sub 3} nanoparticles. The simple cost-effective hydrolysis assisted co-precipitation method was adopted. Synthesized samples were characterized by X-ray diffraction (XRD) and field emission scanning electron microscopy (FESEM) techniques. XRD revealed that synthesized nanoparticles have corundum structure. The lattice parameters have been calculated by Rietveld refinement; and strain and crystallite size have been calculated by using the Williamson-Hall plots. For acetone gas sensing properties, the nanoparticles were applied as thick film onto alumina substrate and tested at different operating temperatures. The results showedmore » that the optimum operating temperature of both the gas sensors is 250°C. At optimum operating temperature, the response of Cr{sub 2}O{sub 3} and 2% W{sup 6+} doped Cr{sub 2}O{sub 3} gas sensor towards 100 ppm acetone was found to be 25.5 and 35.6 respectively. The investigations revealed that the addition of W{sup 6+} as a dopant enhanced the sensing response of Cr{sub 2}O{sub 3} nanoparticles appreciably.« less

Nitrogen-modified nano-titania: True phase composition, microstructure and visible-light induced photocatalytic NO{sub x} abatement

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

Tobaldi, D.M., E-mail: david.tobaldi@ua.pt; Pullar, R.C.; Gualtieri, A.F.

2015-11-15

Titanium dioxide (TiO{sub 2}) is a popular photocatalyst used for many environmental and anti-pollution applications, but it normally operates under UV light, exploiting ∼5% of the solar spectrum. Nitrification of titania to form N-doped TiO{sub 2} has been explored as a way to increase its photocatalytic activity under visible light, and anionic doping is a promising method to enable TiO{sub 2} to harvest visible-light by changing its photo-absorption properties. In this paper, we explore the insertion of nitrogen into the TiO{sub 2} lattice using our green sol–gel nanosynthesis method, used to create 10 nm TiO{sub 2} NPs. Two parallel routesmore » were studied to produce nitrogen-modified TiO{sub 2} nanoparticles (NPs), using HNO{sub 3}+NH{sub 3} (acid-precipitated base-peptised) and NH{sub 4}OH (totally base catalysed) as nitrogen sources. These NPs were thermally treated between 450 and 800 °C. Their true phase composition (crystalline and amorphous phases), as well as their micro-/nanostructure (crystalline domain shape, size and size distribution, edge and screw dislocation density) was fully characterised through advanced X-ray methods (Rietveld-reference intensity ratio, RIR, and whole powder pattern modelling, WPPM). As pollutants, nitrogen oxides (NO{sub x}) are of particular concern for human health, so the photocatalytic activity of the NPs was assessed by monitoring NO{sub x} abatement, using both solar and white-light (indoor artificial lighting), simulating outdoor and indoor environments, respectively. Results showed that the onset of the anatase-to-rutile phase transformation (ART) occurred at temperatures above 450 °C, and NPs heated to 450 °C possessed excellent photocatalytic activity (PCA) under visible white-light (indoor artificial lighting), with a PCA double than that of the standard P25 TiO{sub 2} NPs. However, higher thermal treatment temperatures were found to be detrimental for visible-light photocatalytic activity, due to the effects of four simultaneous occurrences: (i) loss of OH groups and water adsorbed on the photocatalyst surface; (ii) growth of crystalline domain sizes with decrease in specific surface area; (iii) onset and progress of the ART; (iv) the increasing instability of the nitrogen in the titania lattice. - Graphical abstract: Nitrogen modified TiO{sub 2} synthesised via a green aqueous sol–gel method showed to degrade nitrogen oxides (NO{sub x}) under visible white-light (indoor artificial lighting), with a photocatalytic activity double than that of the standard P25 TiO{sub 2} NPs. - Highlights: • N–TiO{sub 2} synthesised via a green aqueous sol–gel method. • Advanced X-ray methods used to detect both crystalline and amorphous contents. • Microstructure fully addressed via XRPD and whole powder pattern modelling. • Photocatalytic NO{sub x} removal assessed using both solar and visible-light lamps.« less

Geochemical and mineralogical data for soils of the conterminous United States

USGS Publications Warehouse

Smith, David B.; Cannon, William F.; Woodruff, Laurel G.; Solano, Federico; Kilburn, James E.; Fey, David L.

2013-01-01

In 2007, the U.S. Geological Survey initiated a low-density (1 site per 1,600 square kilometers, 4,857 sites) geochemical and mineralogical survey of soils of the conterminous United States as part of the North American Soil Geochemical Landscapes Project. Sampling and analytical protocols were developed at a workshop in 2003, and pilot studies were conducted from 2004 to 2007 to test and refine these recommended protocols. The final sampling protocol for the national-scale survey included, at each site, a sample from a depth of 0 to 5 centimeters, a composite of the soil A horizon, and a deeper sample from the soil C horizon or, if the top of the C horizon was at a depth greater than 1 meter, from a depth of approximately 80–100 centimeters. The <2-millimeter fraction of each sample was analyzed for a suite of 45 major and trace elements by methods that yield the total or near-total elemental content. The major mineralogical components in the samples from the soil A and C horizons were determined by a quantitative X-ray diffraction method using Rietveld refinement. Sampling in the conterminous United States was completed in 2010, with chemical and mineralogical analyses completed in May 2013. The resulting dataset provides an estimate of the abundance and spatial distribution of chemical elements and minerals in soils of the conterminous United States and represents a baseline for soil geochemistry and mineralogy against which future changes may be recognized and quantified. This report (1) describes the sampling, sample preparation, and analytical methods used; (2) gives details of the quality control protocols used to monitor the quality of chemical and mineralogical analyses over approximately six years; and (3) makes available the soil geochemical and mineralogical data in downloadable tables.

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

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

Kalsi, Deepti; Rayaprol, S.; Siruguri, V.

We report the crystallographic properties of RE{sub 2}NiGe{sub 3} (RE=La, Ce) synthesized by arc melting. Rietveld refinement on the powder neutron diffraction (ND) data suggest both compounds are isostructural and crystallize in the non-centrosymmetric Er{sub 2}RhSi{sub 3} type structure having hexagonal space group P6{sup ¯}2c. In the crystal structure of RE{sub 2}NiGe{sub 3}, two dimensional arrangements of nickel and germanium atoms lead to the formation of hexagonal layers with rare earth atoms sandwiched between them. Magnetic susceptibility measurements performed in low fields exhibit antiferromagnetic ordering in cerium compound around (T{sub o}=) 3.2 K. Neutron diffraction measurements at 2.8 K (i.e.,more » at T« less

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.

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.

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.

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.

The formation and structure of mechano-synthesized nanocrystalline Sr{sub 3}Fe{sub 2}O{sub 6.4}: XRD Rietveld, Mössabuer and XPS analyses

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

Al-Rawas, A.D., E-mail: arawas@squ.edu.om; Widatallah, H.M.; Al-Harthi, S.H.

2015-05-15

Highlights: • The formation of mechano-synthesized nanocrystalline Sr{sub 3}Fe{sub 2}O{sub 7−δ} is investigated. • Pre-milling the reactants substantially lowers the formation temperature. • The core and surface structures were studied. • XRD and {sup 57}Fe Mössbauer spectroscopic analyses indicate the δ-value to be 0.60. • XPS shows a complex surface structure for the mechanosynthesized Sr{sub 3}Fe{sub 2}O{sub 7−δ} nanoparticles. - Abstract: The influence of ball milling and subsequent sintering of a 3:1 molar mixture of SrCO{sub 3} and α-Fe{sub 2}O{sub 3} on the formation of Sr{sub 3}Fe{sub 2}O{sub 7−δ} double perovskite is investigated with different analytical techniques. Milling the mixturemore » for 110 h leads to the formation of SrCO{sub 3}-α-Fe{sub 2}O{sub 3} nanocomposites and the structural deformation of α-Fe{sub 2}O{sub 3} via the incorporation of Sr{sup 2+} ions. Subsequent sintering of the pre-milled reactants’ mixture has led to the partial formation of an SrFeO{sub 3} perovskite-related phase in the temperature range 400–600 °C. This was followed by the progressive development of an Sr{sub 3}Fe{sub 2}O{sub 7−δ} phase that continued to increase with increasing sintering temperature until a single-phased nanocrystalline Sr{sub 3}Fe{sub 2}O{sub 7−δ} phase was attained at 950 °C (12 h). This temperature is ∼350 °C lower than the temperature at which the material is prepared conventionally using the ceramic method. The evolution of different structural phases during the reaction process is discussed. Rietveld refinement of the X-ray diffraction data shows a value of 0.60 for the oxygen deficiency δ, in consistency with the Fe{sup 3+}/Fe{sup 4+} ratio derived from the {sup 57}Fe Mössbauer data recorded at both 300 K and 78 K. The Mössbauer data suggests that the Sr{sub 3}Fe{sub 2}O{sub 6.4} nanoparticles are superparamagnetic with blocking temperatures below 78 K. The surfaces of the Sr{sub 3}Fe{sub 2}O{sub 6.4} nanoparticles were shown to have a complex structure and composition relative to those of their cores with traces of SrCO{sub 3}, SrO and SrFeO{sub 3−δ} being detected.« less

Frictional properties of fault rocks along the shallow part of the Japan Trench décollement: insights from samples recovered during the Integrated Ocean Drilling Project Expedition 343 (the JFAST project)

NASA Astrophysics Data System (ADS)

Remitti, Francesca; Smith, Steven; Gualtieri, Alessandro; Di Toro, Giulio; Nielsen, Stefan

2014-05-01

The Japan Trench Fast Drilling Project (JFAST), Integrated Ocean Drilling Program (IODP) Expedition 343, successfully located and sampled the shallow slip zone of the Mw =9.0 Tohoku-Oki earthquake where the largest coseismic slip occurred (c. 50 m). Logging-while-drilling, core-sample observations and the analysis of temperature data recovered from a third borehole show that a thin (<5 m), smectite rich plate-boundary fault accommodated the large slip of the Tohoku-Oki Earthquake rupture, as well as most of the interplate motion at the drill site. Effective normal stress along the shallow plate-boundary fault is estimated to be c. 7 MPa. Single-velocity and velocity-stepping rotary-shear friction experiments on fault material were performed with the Slow to HIgh Velocity Apparatus (SHIVA) installed at INGV in Rome. Quantitative phase analysis using the combined Rietveld and R.I.R. method indicates that the starting material is mainly composed of smectite (56 wt%) and illite/mica (21 wt%) and minor quartz, kaolinite, plagioclase and K-feldspar. The amount of amorphous fraction has also been calculated and it is close to the detection limit. Each experiment used 3.5 g of loosely disaggregated gouge, following sieving to a particle size fraction <1 mm. Experiments were performed either 1) "room-dry" (40-60% humidity) at 8.5 MPa normal stress (one test at 12.5 MPa), or 2) "water-dampened" (0.5 ml distilled water added to the gouge layers) at 3.5 MPa normal stress. Slip velocities ranged over nearly seven orders of magnitude (10-5 - 3 m s-1). Total displacement is always less than 1 m. The peak and steady-state frictional strengths of the gouges are significantly lower under water-dampened conditions, with mean steady-state friction coefficients (μ, shear stress/normal stress) at all investigated velocities of 0.04<μ<0.1. This is consistent with the small measured frictional heat anomaly along the plate boundary fault ~1.5 years after the Tohoku-Oki earthquake. Under room-dry conditions the gouge material is velocity-strengthening at intermediate velocities (0.001 - 0.1 m s-1), but strongly velocity-weakening at > 0.1 m s-1. Instead, under water-dampened conditions, the gouge is velocity-neutral to velocity-weakening at all investigated velocities. In other words, the intermediate-velocity strengthening, which would probably act as a "barrier" to rupture propagation in the dry gouges, disappears in water-dampened gouges. This result is compatible with propagation of the Tohoku rupture to the trench, and also with large coseismic slip at shallow depths. Quantitative phase analysis using the combined Rietveld and R.I.R. method has been performed also on six post-experiment gouges for the determination of both the crystalline and amorphous fractions. Preliminary results show that the mineralogical assemblage is basically the same after the experiments, with both smectite and illite phases preserved, this suggests that the weakening mechanism operating in this material is active at low temperature.

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

Effect of the hydration temperature on the microstructure of Class G cement: C-S-H composition and density

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

Bahafid, Sara; Ghabezloo, Siavash; Duc, Myriam

Curing temperature has a significant influence on cement paste microstructure and the properties of its principal hydrate C-S-H. In this paper, the effect of the hydration temperature in the range of 7 °C to 90 °C on the microstructure of a class G oil-well cement is studied. This is done by combining various experimental methods, including X-ray diffraction associated with the Rietveld analysis, thermo-gravimetric analysis, mercury intrusion porosimetry and porosity evaluation by drying. The experimental results show an increase of the capillary porosity and a decrease of the gel porosity by increasing the hydration temperature. This is attributed to amore » decrease of the C-S-H intrinsic porosity and a corresponding increase of the C-S-H density for higher curing temperatures. The experimental results are used in a simple analysis method to evaluate the density of C-S-H, as well as its C/S ratio and H/S ratio in dry and saturated conditions. The evaluated C-S-H density varies from 1.88 g/cm{sup 3} at 7 °C to 2.10 g/cm{sup 3} at 90 °C. The results also show a decrease of molar C/S ratio with increasing hydration temperature from 1.93 at 7 °C to 1.71 at 90 °C and of the H/S ratio from 5.1 at 7 °C to 2.66 at 90 °C.« less

Crystal structure characteristics, dielectric loss, and vibrational spectra of Zn-rich non-stoichiometric Ba[(Zn1/3Nb2/3)1-x Zn x ]O3 ceramics

NASA Astrophysics Data System (ADS)

Li, Jianzhu; Xing, Chao; Qiao, Hengyang; Chen, Huiling; Yang, Jun; Dong, Helei; Shi, Feng

2017-07-01

Zn-Rich non-stoichiometric Ba(Zn1/3Nb2/3)1-x Zn x O3 (BZNZ) (x  =  0.01, 0.02, 0.03, 0.04) ceramics were prepared by the solid-state reaction method at 1500 °C for 2 h. The crystal structures and morphologies were analyzed by x-ray diffraction (XRD) and scanning electron microscopy. The vibration modes were obtained by Raman scattering spectroscopy and Fourier transform far-infrared (FTIR) reflectance spectroscopy. Rietveld refinement was performed for the XRD data. The relationship between crystal structures, dielectric properties, and phonon modes was analyzed in detail. XRD results show that the main phase is Ba(Zn1/3Nb2/3)O3. The Raman results displayed that the ordering structure of BZNZ transformed from 1:2 to 1:1 when x changed from 0.02 to 0.04, and the dielectric losses have a positive correlation with the full width at half maximum values of the A 1g(O) and E g(O) modes. The FTIR spectra were analyzed by the Kramers-Krönig method to obtain the real parts (ɛ‧) and the imaginary parts (ɛ″) of the dielectric constant. When x  =  0.02, the sample possesses uniform grains with clear boundaries and the lowest dielectric loss value (tanδ  =  5.5  ×  10‒4) due to the largest packing fraction.

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

Biasotto, G.; Simoes, A.Z., E-mail: alezipo@yahoo.com; Foschini, C.R.

Highlights: Black-Right-Pointing-Pointer BiFeO{sub 3} (BFO) nanoparticles were grown by hydrothermal microwave method (HTMW). Black-Right-Pointing-Pointer The soaking time is effective in improving phase formation. Black-Right-Pointing-Pointer Rietveld refinement reveals an orthorhombic structure. Black-Right-Pointing-Pointer The observed magnetism of the BFO crystallites is a consequence of particle size. Black-Right-Pointing-Pointer The HTMW is a genuine technique for low temperatures and short times of synthesis. -- Abstract: Hydrothermal microwave method (HTMW) was used to synthesize crystalline bismuth ferrite (BiFeO{sub 3}) nanoparticles (BFO) in the temperature of 180 Degree-Sign C with times ranging from 5 min to 1 h. BFO nanoparticles were characterized by means of X-raymore » analyses, FT-IR, Raman spectroscopy, TG-DTA and FE-SEM. X-ray diffraction results indicated that longer soaking time was benefit to refraining the formation of any impurity phases and growing BFO crystallites into almost single-phase perovskites. Typical FT-IR spectra for BFO nanoparticles presented well defined bands, indicating a substantial short-range order in the system. TG-DTA analyses confirmed the presence of lattice OH{sup -} groups, commonly found in materials obtained by HTMW process. Compared with the conventional solid-state reaction process, submicron BFO crystallites with better homogeneity could be produced at the temperature as low as 180 Degree-Sign C. These results show that the HTMW synthesis route is rapid, cost effective, and could be used as an alternative to obtain BFO nanoparticles in the temperature of 180 Degree-Sign C for 1 h.« 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

Fabrication and Performance of High Energy Li-Ion Battery Based on the Spherical Li[Li(0.2)Ni(0.16)Co(0.1)Mn(0.54)]O2 Cathode and Si Anode.

PubMed

Ye, Jing; Li, Yi-xuan; Zhang, Li; Zhang, Xue-ping; Han, Min; He, Ping; Zhou, Hao-shen

2016-01-13

The cathode materials of Li-ion batteries for electric vehicles require not only a large gravimetric capacity but also a high volumetric capacity. A new Li-rich layered oxide cathode with superior capacity, Li[Li0.20Ni0.16Co0.10Mn0.54]O2 (denoted as LNCM), is synthesized from precursor, a coprecipitated spherical metal hydroxide. The preparation technology of precursor such as stirring speed, concentration of metal solution, and reaction time are regulated elaborately. The final product LNCM shows a well-ordered, hexagonal-layer structure, as confirmed by Rietveld refinement of X-ray diffraction pattern. The particle size of the final product has an average diameter of about 10 μm, and the corresponding tap density is about 2.25 g cm(-3). Electrochemical measurements indicate that as-prepared LNCM has great initial columbic efficiency, reversible capacity, and cycling stability, with specific discharge capacities of 278 and 201 mAh g(-1) at 0.03 and 0.5 C rates, respectively. Cycling at 0.1 C, LNCM delivers a discharge capacity of 226 mAh g(-1) with 95% retention capacity after 50 cycles. Si/LNCM cell is fabricated using Si submicroparticle as anode against LNCM. The cell can exhibit a specific energy of 590 Wh kg(-1) based on the total weight of cathode and anode materials.

Hydrothermal synthesis of a photovoltaic material based on CuIn0.5Ga0.5Se2

NASA Astrophysics Data System (ADS)

Castellanos Báez, Y. T.; Fuquen Peña, D. A.; Gómez-Cuaspud, J. A.; Vera-López, E.; Pineda-Triana, Y.

2017-12-01

The present work report, the synthesis and characterization of the CuIn0.5Ga0.5Se2 system (abbreviated CIGS), by the implementation of a hydrothermal route, in order to obtain a solid with appropriate properties in terms of surface, morphological and texture properties for potential applications in the design of photovoltaic cells. The synthesis was carried out using the corresponding stoichiometric quantities (Cu:In:Ga:Se 1:0.5:0.5:2), which were mixed in a Teflon vessel under stirring conditions. The homogeneous solution was treated in a steel autoclave at 300°C for 72 hours at the end of which the resulting material was characterized by X-Ray Diffraction (XRD) and Rietveld refinement. The results of the structural characterization allowed to confirm the obtaining of a chalcopyrite type structure, with a I-42 d (122) structure and cell parameters a=0.570, b=0.570, c=1.140nm, α=90, β=90, γ=90° oriented along (1 0 4) facet, detecting the presence of a secondary phases, related with CuInSe and CuIn metallic selenides, derived from synthesis process. The structural refinement allowing to validate the obtaining of a nanometric crystalline material (10-20nm) for potential applications in field of photovoltaic technology.

Bluish-White Luminescence in Rare-Earth-Free Vanadate Garnet Phosphors: Structural Characterization of LiCa3MV3O12 (M = Zn and Mg).

PubMed

Hasegawa, Takuya; Abe, Yusuke; Koizumi, Atsuya; Ueda, Tadaharu; Toda, Kenji; Sato, Mineo

2018-01-16

Extensive attention has been focused toward studies on inexpensive and rare-earth-free garnet-structure vanadate phosphors, which do not have a low optical absorption due to the luminescence color being easily controlled by its high composition flexibility. However, bluish emission phosphors with a high quantum efficiency have not been found until now. In this study, we successfully discovered bluish-white emitting, garnet structure-based LiCa 3 MV 3 O 12 (M = Zn and Mg) phosphors with a high quantum efficiency, and the detailed crystal structure was refined by the Rietveld analysis technique. These phosphors exhibit a broad-band emission spectra peak at 481 nm under near UV-light excitation at 341 nm, indicating no clear difference in the emission and excitation spectra. A very compact tetrahedral [VO 4 ] unit is observed in the LiCa 3 MV 3 O 12 (M = Zn and Mg) phosphors, which is not seen in other conventional garnet compounds, and generates a bluish-white emission. In addition, these phosphors exhibit high quantum efficiencies of 40.1% (M = Zn) and 44.0% (M = Mg), respectively. Therefore, these vanadate garnet phosphors can provide a new blue color source for LED devices.

Compositionally driven giant strain and electrostrictive co-efficient in lead free NBT-BT-BFO system

NASA Astrophysics Data System (ADS)

Duraisamy, Dhayanithi; Venkatesan, Giridharan Nambi

2018-01-01

As lead free alternatives, bismuth based ferroelectric ceramics are currently under intense investigation. Here, the authors report on the development of a lead free (1-2x)Na0.5Bi0.5TiO3-xBaTiO3-xBiFeO3: NBT-BT-BFO [x = 0.01, 0.03, 0.05, 0.07, and 0.09] ceramic. Rietveld analysis of the powder diffraction data reveals the existence of compositionally driven single and two phase combinations. The compositions corresponding to x = 0.01 and 0.03 are found to be crystallized in a monoclinic (Cc) system, whereas the compositions corresponding to x =0.05, 0.07, and 0.09 are found to have the coexistence of [monoclinic (Cc) + Cubic (pm-3m)] and [Tetragonal (P4bm) + Cubic (pm-3m)] phases. A high electric field induced strain has been obtained for x = 0.07, which can be attributed to the polarization extension mechanism at the proximity of the phase boundary between polar and nonpolar phases. Further, the manufactured ceramic is characterized by Smax/Emax of 858 pm/V and an electrostrictive co-efficient (Q33) of 0.045 m4 C-2 much higher than the values of well-established Pb(Zr,Ti)O3 and other lead free ceramics.

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

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.

New in-situ neutron diffraction cell for electrode materials

NASA Astrophysics Data System (ADS)

Biendicho, Jordi Jacas; Roberts, Matthew; Offer, Colin; Noréus, Dag; Widenkvist, Erika; Smith, Ronald I.; Svensson, Gunnar; Edström, Kristina; Norberg, Stefan T.; Eriksson, Sten G.; Hull, Stephen

2014-02-01

A novel neutron diffraction cell has been constructed to allow in-situ studies of the structural changes in materials of relevance to battery applications during charge/discharge cycling. The new design is based on the coin cell geometry, but has larger dimensions compared to typical commercial batteries in order to maximize the amount of electrode material and thus, collect diffraction data of good statistical quality within the shortest possible time. An important aspect of the design is its modular nature, allowing flexibility in both the materials studied and the battery configuration. This paper reports electrochemical tests using a Nickel-metal-hydride battery (Ni-MH), which show that the cell is able to deliver 90% of its theoretical capacity when using deuterated components. Neutron diffraction studies performed on the Polaris diffractometer using nickel metal and a hydrogen-absorbing alloy (MH) clearly show observable changes in the neutron diffraction patterns as a function of the discharge state. Due to the high quality of the diffraction patterns collected in-situ (i.e. good peak-to-background ratio), phase analysis and peak indexing can be performed successfully using data collected in around 30 min. In addition to this, structural parameters for the β-phase (charged) MH electrode obtained by Rietveld refinement are presented.

Metal-like electrical conductivity in LaxSr2-xTiMoO6 oxides for high temperature thermoelectric power generation.

PubMed

Saxena, Mandvi; Maiti, Tanmoy

2017-05-09

Increasing electrical conductivity in oxides, which are inherently insulators, can be a potential route in developing oxide-based thermoelectric power generators with higher energy conversion efficiency. In the present work, environmentally friendly non-toxic double perovskite La x Sr 2-x TiMoO 6 (LSTM) ceramics were synthesized using a solid-state reaction route by optimizing the sintering temperature and atmosphere for high temperature thermoelectric applications. Rietveld refinement of XRD data confirmed a single-phase solid solution with a cubic structure in these double perovskites with the space-group Pm3[combining macron]m. SEM studies showed a highly dense microstructure in these ceramics. High electrical conductivity on the order of 10 5 S m -1 and large carrier concentration (∼10 22 cm -3 ) were obtained in these materials. The temperature-dependent electrical conductivity measurement showed that the LSTM ceramics exhibit a semiconductor to metal transition. Thermopower (S) measurements demonstrated the conductivity switching from a p-type to n-type behavior at higher temperature. A temperature dependent Seebeck coefficient was further explained using a model for coexistence of both types of charge carriers in these oxides. A conductivity mechanism of these double perovskites was found to be governed by a small polaron hopping model.

Tunable magnetic properties and magnetocaloric effect of off-stoichiometric LaMnO3 nanoparticles

NASA Astrophysics Data System (ADS)

Tola, P. S.; Kim, H. S.; Kim, D. H.; Phan, T. L.; Rhyee, J. S.; Shon, W. H.; Yang, D. S.; Manh, D. H.; Lee, B. W.

2017-12-01

The crystal and electronic structures and the magnetic and magnetocaloric properties of off-stoichiometric LaMnO3 nanoparticles (NPs) with various particle sizes D = 20-100 nm were studied. The Rietveld refinement revealed that all NPs were crystallized in the rhombohedral structure, with varied structural parameters dependent on D. Magnetization (M) measurements indicated a considerable difference between zero-field-cooled and field-cooled magnetizations at temperatures below ferromagnetic-paramagnetic (FM-PM) phase transition, particularly for the samples with D = 25-40 nm. These results are ascribed to spin-glass-like behaviors and magnetic inhomogeneity. We also found the possibility of tuning the FM-PM phase transition temperature (TC) from 77 to 262 K, which is dependent on both D and W (the eg-electron bandwidth). Under an applied field of H = 50 kOe, the absolute maximum magnetic entropy change that achieved around TC can be improved from 4.02 J kg-1 K-1 for D = 40 nm to 6.36 Jṡ kg-1ṡ K-1 for D = 100 nm, corresponding to the relative-cooling-power values of 241-245 Jṡ kg-1. We also analyzed the data of M and magnetic entropy change based on theoretical models to further understand the magnetic property and phase-transition type of the NP samples.

Texture development in naturally compacted and experimentally deformed silty clay sediments from the Nankai Trench and Forearc, Japan

NASA Astrophysics Data System (ADS)

Schumann, Kai; Stipp, Michael; Leiss, Bernd; Behrmann, Jan H.

2014-12-01

The petrophysical properties of fine-grained marine sediments to a large extent depend on the microstructure and crystallographic preferred orientations (CPOs). In this contribution we show that Rietveld-based synchrotron texture analysis is a new and valuable tool to quantify textures of water-saturated fine-grained phyllosilicate-rich sediments, and assess the effects of compaction and tectonic deformation. We studied the CPO of compositionally almost homogeneous silty clay drillcore samples from the Nankai Accretionary Prism slope and the incoming Philippine Sea plate, offshore SW Japan. Basal planes of phyllosilicates show bedding-parallel alignment increasing with drillhole depth, thus reflecting progressive burial and compaction. In some samples calcite and albite display a CPO due to crystallographically controlled non-isometric grain shapes, or nannofossil tests. Consolidated-undrained experimental deformation of a suite of thirteen samples from the prism slope shows that the CPOs of phyllosilicate and calcite basal planes develop normal to the experimental shortening axis. There is at least a qualitative relation between CPO intensity and strain magnitude. Scanning electron micrographs show concurrent evolution of preferred orientations of micropores and detrital illite flakes normal to axial shortening. This indicates that the microfabrics are sensitive strain gauges, and contribute to anisotropic physical properties along with the CPO.

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.

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, 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.

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.

Effect of Mg2+ on acidic calcium phosphate phases grown by electrodeposition

NASA Astrophysics Data System (ADS)

Correia, Matheus Bento; Júnior, José Pedro Gualberto; Macedo, Michelle Cardinale S. S.; Resende, Cristiane Xavier; dos Santos, Euler Araujo

2017-10-01

In this work, the effect of Mg2+ ions on the electrodeposition of dicalcium phosphate dihydrate (DCPD), octacalcium phosphate (OCP) and calcium-deficient hydroxyapatite (CDHA) crystals on a commercially pure titanium (cp-Ti) substrate was evaluated. We demonstrated that Mg2+ ions could change the morphology of the coatings by inhibiting the growth rate of the OCP and CDHA crystals and diminishing the crystallite size of DCPD. The inhibition effect on OCP and CDHA was most likely due to a surface adsorption mechanism since no evidence of a doping process was observed using Rietveld refinement and electron diffraction analyses. Conversely, the presence of Mg2+ ions generated a favorable condition for the nucleation of a new Mg2+-rich DCPD crystal population, presenting smaller crystallite sizes.

Suppression of the commensurate magnetic phase in nanosized hübnerite MnW O 4

DOE PAGES

Zajdel, P.; G?gor, A.; Pajerowski, D. M.; ...

2017-05-18

Magnetic structures of nanosized (20 to 70 nm) powders of MnWO 4 and MnWO 4:Mo were studied using neutron powder diffraction (NPD). Sizes and shapes of the crystallites calculated from anisotropic peak broadening of diffraction peaks were found to be orthogonal parallelepipedlike with the longest edge along the c axis and the shortest along the b axis. SQUID measurements indicate the presence of two magnetic transitions around 8 and 12 K. Rietveld refinement of the NPD data below the magnetic transition was consistent with the presence of an incommensurate spiral-like (ac-AF2) phase. Finally, a commensurate phase AF1 was not observedmore » down to 2.5 K for all of the samples.« less

Ultrasound synthesis of Y2O3: Dy3+ nanophosphor: Structural and photometric properties suitable for wLEDs

NASA Astrophysics Data System (ADS)

Marappa, B.; Rudresha, M. S.; Nagabhsuhana, H.; Basavaraj, R. B.; Prasad, B. Daruka

2017-05-01

The facile ultrasound synthesis of Y2O3:Dy3+ nanostructures by using bio-surfactant mimosa pudica leaves extract. The concentration of bio-surfactant was the key factor in controlling the morphology of Y2O3 nanostructures. The formation of different morphologies of Y2O3: Dy3+ was characterized by SEM, TEM and HRTEM. The PXRD data and Rietveld analysis evident the formation of single phase Y2O3 with cubic crystal structure. The influence of Dy3+ concentration on the structure morphology, UV absorption, and PL emission of Y2O3: Dy3+ nanostructures were investigated systematically. Y2O3: Dy3+ exhibits intense warm white emission with CIE chromaticity coordinates (0.32, 0.33) and CCT value is 5525 K which corresponds to vertical day light. SEM micrographs showed superstructure morphology influenced by both sonication time as well as surfactant concentration. Pl emission spectra shows three intense peaks observed at 480, 574 and 666 nm attributed to the Dy3+ transitions. The photometric properties were studied by evaluating the CIE, CCT diagrams and the results were very fruitful in making the white light emitting diodes. This method has been considered to be the cost effective and eco-friendly to synthesize nanomaterials with superior morphology suitable for display device applications.

Synthesis, structure, and photoluminescence properties of novel KBaSc2 (PO4 )3 :Ce(3+) /Eu(2+) /Tb(3+) phosphors for white-light-emitting diodes.

PubMed

Jiao, Mengmeng; Lü, Wei; Shao, Baiqi; Zhao, Lingfei; You, Hongpeng

2015-08-24

A series of novel KBaSc2 (PO4 )3 :Ce(3+) /Eu(2+) /Tb(3+) phosphors are prepared using a solid-state reaction. X-ray diffraction analysis and Rietveld structure refinement are used to check the phase purity and crystal structure of the prepared samples. Ce(3+) - and Eu(2+) -doped phosphors both have broad excitation and emission bands, owing to the spin- and orbital-allowed electron transition between the 4f and 5d energy levels. By co-doping the KBaSc2 (PO4 )3 :Eu(2+) and KBaSc2 (PO4 )3 :Ce(3+) phosphors with Tb(3+) ions, tunable colors from blue to green can be obtained. The critical distance between the Eu(2+) and Tb(3+) ions is calculated by a concentration quenching method and the energy-transfer mechanism for Eu(2+) →Tb(3+) is studied by utilizing the Inokuti-Hirayama model. In addition, the quantum efficiencies of the prepared samples are measured. The results indicate that KBaSc2 (PO4 )3 :Eu(2+) ,Tb(3+) and KBaSc2 (PO4 )3 :Ce(3+) ,Tb(3+) phosphors might have potential applications in UV-excited white-light-emitting diodes. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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.

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.

Precursor routes to quaternary intermetallics: Synthesis, crystal structure, and physical properties of clathrate-II Cs{sub 8}Na{sub 16}Al{sub 24}Si{sub 112}

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

Wei, Kaya; Dong, Yongkwan; Nolas, George S., E-mail: gnolas@usf.edu

A new quaternary clathrate–II composition, Cs{sub 8}Na{sub 16}Al{sub 24}Si{sub 112}, was synthesized by kinetically controlled thermal decomposition (KCTD) employing both NaSi and NaAlSi as the precursors and CsCl as a reactive flux. The crystal structure and composition of Cs{sub 8}Na{sub 16}Al{sub 24}Si{sub 112} were investigated using both Rietveld refinement and elemental analysis, and the temperature dependent transport properties were investigated. Our results indicate that KCTD with multiple precursors is an effective method for the synthesis of multinary inorganic phases that are not easily accessible by traditional solid-state synthesis or crystal growth techniques. - Graphical abstract: Quaternary Cs{sub 8}Na{sub 16}Al{sub 24}S{submore » 112} clathrate–II was synthesized for the first time by kinetically controlled thermal decomposition (KCTD) employing a NaSi+NaAlSi precursor mixture with CsCl as the reactive flux, and the structural and transport properties were investigated. Our approach demonstrates a new synthetic pathway for the synthesis of multinary inorganic compounds. This work reports the exploration of a new clathrate composition as this class of materials continues to be of interest for thermoelectrics and other energy-related applications.« less

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

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).

Flux free single crystal growth and characterization of FeTe1-xSx (x=0.00 and 0.10) crystals

NASA Astrophysics Data System (ADS)

Maheshwari, P. K.; Awana, V. P. S.

2018-05-01

We report synthesis of S doped FeTe1-xSx (x = 0.00 and 0.10) single crystals using flux free method via solid state reaction. Single crystal XRD patterns of FeTe1-xSx (x = 0.00 and 0.10) confirm the single crystalline property, as the crystals are grown in (00l) plane only. Powder XRD result of FeTe1-xSx (x = 0.00 and 0.10) crystals show that crystalline in tetragonal structure having P4/nmm space group. Rietveld refinement results show that both a and c lattice parameters decreases with S doping of 10% at Te site in FeTe1-xSx. Detailed scanning electron microscopy (SEM) image of FeTe0.90S0.10 shows that the growth of crystal is in slab-like morphology. Electrical resistivity measurement results onset confirm the superconductivity in S doped 10% sample at Te site and superconducting transition Tconset occurs at 9.5K and Tcoffset(ρ=0) occurs at 6.5K. ρ-T measurement has been performed under various magnetic field up to 12 Tesla down to 2K. Upper critical field Hc2(0), for x=0.10, which comes around 70Tesla, 60Tesla and 45Tesla of normal resistivity criterion ρn = 90%, 50% and 10% criterion respectively.

Effect of lattice strain on structural and magnetic properties of Ca substituted barium hexaferrite

NASA Astrophysics Data System (ADS)

Kumar, Sunil; Supriya, Sweety; Pandey, Rabichandra; Pradhan, Lagen Kumar; Singh, Rakesh Kumar; Kar, Manoranjan

2018-07-01

The calcium (Ca2+) substituted M-type barium hexaferrite (Ba1-xCaxFe12O19) for Ca2+ (x = 0.00, 0.025, 0.050, 0.075, 0.100, 0.150, and 0.200) have been synthesized by the citrate sol-gel method. The X-ray diffraction (XRD) patterns with Rietveld refinement reveal the formation of hexagonal crystal structure with P63/mmc space group. The lattice parameters a = b and c decrease, whereas lattice strain found to increase with the increase in Ca concentration in the samples. The analysis of Raman spectra well supports the XRD patterns analysis. The average particle size is obtained from the FE-SEM (Field Emission Scanning Electron Microscopy) micrographs and these are similar to that of crystallite size obtained from the XRD pattern analysis. The saturation magnetization and magnetocrystalline anisotropy have been obtained by employing the "Law of Approach (LA) to Saturation magnetization" technique at room temperature. The saturation magnetization and magnetocrystalline anisotropy constant are maximum for 5% Ca substitution in barium hexaferrite. It could be due to lattice strain mediated magnetism. However, these magnetic properties decrease for more than the 5% Ca substitution in barium hexaferrite. It could be due to decrease of magnetic exchange interaction (Fe-O-Fe) in the sample. A correlation between magnetic interaction and lattice strain has been observed in Ca2+ substituted M-type barium hexaferrite.

Room temperature ferromagnetism in Fe-doped CuO nanoparticles.

PubMed

Layek, Samar; Verma, H C

2013-03-01

The pure and Fe-doped CuO nanoparticles of the series Cu(1-x)Fe(x)O (x = 0.00, 0.02, 0.04, 0.06 and 0.08) were successfully prepared by a simple low temperature sol-gel method using metal nitrates and citric acid. Rietveld refinement of the X-ray diffraction data showed that all the samples were single phase crystallized in monoclinic structure of space group C2/c with average crystallite size of about 25 nm and unit cell volume decreases with increasing iron doping concentration. TEM micrograph showed nearly spherical shaped agglomerated particles of 4% Fe-doped CuO with average diameter 26 nm. Pure CuO showed weak ferromagnetic behavior at room temperature with coercive field of 67 Oe. The ferromagnetic properties were greatly enhanced with Fe-doping in the CuO matrix. All the doped samples showed ferromagnetism at room temperature with a noticeable coercive field. Saturation magnetization increases with increasing Fe-doping, becomes highest for 4% doping then decreases for further doping which confirms that the ferromagnetism in these nanoparticles are intrinsic and are not resulting from any impurity phases. The ZFC and FC branches of the temperature dependent magnetization (measured in the range of 10-350 K by SQUID magnetometer) look like typical ferromagnetic nanoparticles and indicates that the ferromagnetic Curie temperature is above 350 K.

Structural and electrochemical properties of Fe-doped Na2Mn3-xFex(P2O7)2 cathode material for sodium ion batteries

NASA Astrophysics Data System (ADS)

Liu, Huatao; Zhao, Yanming; Zhang, Hui; Lian, Xin; Dong, Youzhong; Kuang, Quan

2017-12-01

A series of Fe-doped Na2Mn3-xFex(P2O7)2 (x = 0.0, 0.5, 1.0, 1.5 and 2.0) compounds have been successfully prepared by using sol-gel method. Rietveld refinement results indicate that single phase Na2Mn3-xFex(P2O7)2 with triclinic structure can be obtained within 0 ≤ x ≤ 2 although no Na2Fe3(P2O7)2 existing under our experimental conditions, and the cell parameters (including a, b, c and V) are decreasing with the increasing of x. Our results reveal that Na2Mn3(P2O7)2 exhibits an electrochemical activity in the voltage range of 1.5 V-4.5 V vs. Na+/Na when using as the cathode material for SIBs although it gives a limited rate capability and poor capacity retention. However, the electrochemical performance of Fe-doped Na2Mn3-xFex(P2O7)2 (0 ≤ x ≤ 2) can be improved significantly where cycle performance and rate capability can be improved significantly than that of the pristine one. Sodium ion diffusion coefficient can be increased by about two orders of magnitude with the Fe-doping content higher than x = 0.5.

Structural, optical and dielectric properties of Ce0.9Nd0.1O1.95 nanocrystalline oxygen ion conductors: Effect of sintering temperature

NASA Astrophysics Data System (ADS)

Anirban, Sk.; Dutta, A.

2015-01-01

Neodymium doped nanocrystalline ceria [Ce0.9Nd0.1O1.95] was prepared through citrate auto-ignition method. The prepared samples were sintered at five different temperatures starting from 400 °C up to 1200 °C. Rietveld's powder structure refinement analysis of XRD data confirmed the single phase cubic fluorite structure of the prepared samples with space group Fm 3 barm and the obtained particle size and lattice parameter values were found to vary with sintering temperature from 6.68 nm to 39.51 nm and from 5.39077 Å to 5.42317 Å respectively. The optical properties were studied using FT-IR and UV-vis absorption spectra. The FT-IR spectra confirm the presence of functional groups and chemical bonding in the material. The optical band gap was calculated from UV-vis spectra and its value was found to decrease from 3.70 eV to 2.46 eV with increase in sintering temperature. The dc conductivity was found to be thermally activated and decreased with increase in sintering temperature. The nature of impedance spectra reveals the presence of both grain and grain boundary effect. The tangent loss exhibited the presence of relaxation peaks due to the presence of defect pair in the synthesized samples.

Improved dielectric and ferroelectric properties of Mn doped barium zirconium titanate (BZT) ceramics for energy storage applications

NASA Astrophysics Data System (ADS)

Sangwan, Kanta Maan; Ahlawat, Neetu; Kundu, R. S.; Rani, Suman; Rani, Sunita; Ahlawat, Navneet; Murugavel, Sevi

2018-06-01

Lead free Mn doped barium zirconium titanate ceramic of composition BaZr0.045 (MnxTi1-x)0.955O3 (x = 0.00, 0.01, 0.02) were prepared by solid state reaction method. Tetragonal perovskite structure was confirmed by Rietveld refinement of X-ray diffraction pattern. Analysis of Scanning electron microscope (SEM) micrographs revealed that addition of Mn up to a certain limit accelerates grain growth of BZT ceramic. Static dielectric constant was successfully extended up to high frequencies with an appreciable decrease in dielectric loss about 70% for Mn doped BZT ceramics. The experimental data fitted with Curie Weiss Law and Power Law confirmed first order transition and diffusive behavior of the investigated system. The shifting of Curie temperature (Tc) from 387 K to 402 K indicated tendency for sustained ferroelectricity in doped BZMT ceramics. High value of percentage temperature coefficient of capacitance TCC >10% near Tc was observed for all the compositions and increases with Mn content in pure BZT. At room temperature, BZT modified ceramic corresponding to x = 0.01 composition shows better values of remnant polarization (Pr = 5.718 μC/cm2), saturation polarization (Ps = 14.410 μC/cm2), low coercive field (Ec = 0.612 kV/cm), and highest value of Pr/Ps = 0.396.

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

Synthesis and characterization of sulfate and dodecylbenzenesulfonate intercalated zinc iron layered double hydroxides by one-step coprecipitation route

NASA Astrophysics Data System (ADS)

Zhang, Hui; Wen, Xing; Wang, Yingxia

2007-05-01

Inorganic sulfate- and organic dodecylbenzenesulfonate (DBS)-intercalated zinc-iron layered double hydroxides (LDHs) materials were prepared by one-step coprecipitation method from a mixed salt solutions containing Zn(II), Fe(II) and Fe(III) salts. The as-prepared samples have been characterized by X-ray powder diffraction (XRD), Fourier-transform infrared spectroscopy (FT-IR), low-temperature nitrogen adsorption, scanning electron microscopy (SEM), inductively coupled plasma emission spectroscopy (ICP), and Mössbauer spectroscopy (MS). The XRD analyses demonstrate the typical LDH-like layered structural characteristics of both products. The room temperature MS results reveal the characteristics of both the Fe(II) and Fe(III) species for SO 42--containing product, while only the Fe(III) characteristic for DBS-containing one. The combination characterization results and Rietveld analysis illustrate that the SO 42--containing product possesses the Green Rust two (GR2)-like crystal structure with an approximate chemical composition of [Zn 0.435·Fe II0.094·Fe III0.470·(OH) 2]·(SO 42-) 0.235·1.0H 2O, while the DBS-containing one exhibits the common LDH compound-like structure. The contact angle measurement indicates the evident hydrophobic properties of DBS-containing nanocomposite, compared with SO 42--containing product, due to the modification of the internal and external surface of LDHs by the organic hydrophobic chain of DBS.

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.

Hygroscopic La[B{sub 5}O{sub 8}(OH)]NO{sub 3}·2H{sub 2}O: Insight into the evolution of borate fundamental building blocks

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

Zhao, Biao-Chun, E-mail: zhaobiaochun@sohu.com; Sun, Wei, E-mail: 421221789@qq.com; Ren, Wei-Jian, E-mail: 935428502@qq.com

2013-10-15

Borates have exceptionally diverse fundamental building blocks (FBBs), but factors controlling the formation of borate FBBs are poorly understood. The title compound La[B{sub 5}O{sub 8}(OH)]NO{sub 3}·2H{sub 2}O crystallizes in the space group P2{sub 1}/n with a=6.5396(12) Å, b=15.550(3) Å, c=10.6719(19) Å, β=90.44(1)° and Z=4 at 173(2) K. Its structure has been refined from single-crystal X-ray diffraction data to R{sub 1}=0.049 (for 2465) and wR{sub 2}=0.173 (for 2459 I>2σ(I)). This structure analysis and first-principles calculations show that the change of the FBB from 3Δ2□ in the title compound to 2Δ3□ in La[B{sub 5}O{sub 8}(OH)(H{sub 2}O)]NO{sub 3}·2H{sub 2}O is accompanied by amore » rotation of the NO{sub 3} group. FTIR, Rietveld and thermal analysis results show that the hygroscopic title compound is partially changed to La[B{sub 5}O{sub 8}(OH)(H{sub 2}O)]NO{sub 3}·2H{sub 2}O, with the conversion of [BO{sub 3}] to [BO{sub 3}(H{sub 2}O)] by water absorption. - Graphical abstract: The change of fundamental building blocks from La[B{sub 5}O{sub 8}(OH)]NO{sub 3}·2H{sub 2}O to La[B{sub 5}O{sub 8}(OH)(H{sub 2}O)]NO{sub 3}·2H{sub 2}O is accompanied by a rotation of the NO{sub 3} group . Display Omitted - Highlights: • Synthesis of a new hydrous lanthanum polyborate nitrate. • Single-crystal XRD structure with the 3Δ2⎕ FBB and an oriented NO{sub 3} group. • DFT calculations locate the H positions in three lanthanide polyborate nitrates. • Rietveld, FTIR and DFT results show hygroscopicity changes the FBBs.« less

Improving the drug release of Naproxen Sodium tablets by preparing granules and tablets with a preferred mixing ratio of hydrates.

PubMed

Bär, David; Debus, Heiko; Grune, Christian; Tosch, Stephan; Fischer, Wolfgang; Mäder, Karsten; Imming, Peter

2017-12-01

Naproxen is a typical and well-known analgesic classified as non-steroidal anti-inflammatory drug (NSAID) and is commercialized as tablets or liquid-filled capsules. Naproxen is typically used asa sodium salt because of its better processability compared to Naproxen free acid. This entails hygroscopicity and gives rise to the existence of four different hydrates, which show polymorphic and pseudopolymorphic properties. Solid dosage forms containing Naproxen Sodium often have to be processed in an applicable dosage form by granulation and tablet compression. During granulation, Naproxen Sodium will be in contact with water and is exposed to the drop and rise in temperature and to mechanical stress. The result could be a mixture of different hydrates of Naproxen Sodium. This study showed that a modified designed fluid bed granulation was not affected by differences in the mixing ratio of hydrates when using different water contents after spraying and at the end with the finished granules. Here, X-ray diffraction combined with Rietveld refinement was used to analyze the ratio of the hydrates and its identity. All granulation batches showed a large amount of Naproxen Sodium Monohydrate (>87%) and no differences could be observed during tablet compression. Quantities of other hydrates were negligibly small. Furthermore, this study also demonstrated the influence of tablet compression by transforming the hydrates of the granules. In addition to Naproxen Sodium Monohydrate, a large quantity of amorphous structures has also been found. Rietveld evaluation combined with the preliminary studies of the raw hydrates provided conclusions on the drug release of the tablets containing hydrates of Naproxen Sodium which were influenced by tablet compression. Fast drug release was obtained when a maximum water content of about 21% was used after spraying during granulation, independently of the final water content of the finished granules. A maximum water content of less than 21% after spraying yielded a high quantity of amorphous components after tablet compression and thus worsened the drug release. Copyright © 2017 Elsevier B.V. All rights reserved.

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

Heterogeneous in-situ nanostructure contributes to the thermoelectric performance of Zn{sub 4}Sb{sub 3}

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

Lin, Jianping; Ma, Lingzhi; Yang, Baifeng

Single-phase Zn{sub 4}Sb{sub 3} and ZnSb-containing samples were prepared by Plasma Activated Sintering. An abrupt decrease of thermal conductivity was found at about 400 K, which is attributed to the microstructure change of Zn{sub 4}Sb{sub 3}. Nanoscale inclusions and compositional inhomogeneities were found in Zn{sub 4}Sb{sub 3} sample at 473 K by high-resolution transmission electron microscopy. The phonon scattering is enhanced by increasing grain boundaries and chaotic structure, which reduces the thermal conductivity and increases the thermoelectric performance of Zn{sub 4}Sb{sub 3} at elevated temperature. The Rietveld refinement results show that large ZnSb grains in ZnSb-containing samples will accommodate excessmore » Zn atoms, and then reduce thermoelectric performance.« less

X-ray diffraction analysis of LiCu2O2 crystals with additives of silver atoms

NASA Astrophysics Data System (ADS)

Sirotinkin, V. P.; Bush, A. A.; Kamentsev, K. E.; Dau, H. S.; Yakovlev, K. A.; Tishchenko, E. A.

2015-09-01

Silver-containing LiCu2O2 crystals up to 4 × 8 × 8 mm in size were grown by the crystallization of 80(1- x)CuO · 20 x AgNO3 · 20Li2CO3 (0 ≤ х ≤ 0.5) mixture melt. According to the X-ray spectral and Rietveld X-ray diffraction data, the maximum amount of silver incorporated in the LiCu2O2 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 с of the LiCu2O2 rhombic unit cell, a slight increase in parameter а, and a slight decrease in parameter b.

Absence of pressure-induced amorphization in LiKSO4.

PubMed

Machon, D; Pinheiro, C B; Bouvier, P; Dmitriev, V P; Crichton, W A

2010-08-11

Angle-resolved synchrotron radiation diffraction was used to investigate lithium potassium sulfate (LiKSO(4)) crystals under high pressure. We confirm that the title compound undergoes three phase transitions, α →β, β → γ and γ →δ, observed at around 0.8 GPa, 4.0 GPa and 7.0 GPa, respectively. Two competitive structures are proposed for the β-phase after powder diffraction data Rietveld refinements: an orthorhombic (space group Cmc 2(1)) or a monoclinic (space group Cc) structure. These structures correspond to the models of the low temperature phases. The γ-phase is indexed by a monoclinic structure. Finally, the δ-phase is found to be highly disordered. No evidence of any pressure-induced amorphous phase was observed up to 24 GPa, even under imposed highly non-hydrostatic conditions, contrary to previous propositions.

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.

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.

Leonardo da Vinci's drapery studies: characterization of lead white pigments by µ-XRD and 2D scanning XRF

NASA Astrophysics Data System (ADS)

Gonzalez, Victor; Calligaro, Thomas; Pichon, Laurent; Wallez, Gilles; Mottin, Bruno

2015-11-01

This work focuses on the composition and microstructure of the lead white pigment employed in a set of paintworks, using a combination of µ-XRD and 2D scanning XRF, directly applied on five drapery studies attributed to Leonardo da Vinci (1452-1519) and conserved in the Département des Arts Graphiques, Musée du Louvre and in the Musée des Beaux- Arts de Rennes. Trace elements present in the composition as well as in the lead white highlights were imaged by 2D scanning XRF. Mineral phases were determined in a fully noninvasive way using a special µ-XRD diffractometer. Phase proportions were estimated by Rietveld refinement. The analytical results obtained will contribute to differentiate lead white qualities and to highlight the artist's technique.

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.

Microstructural, optical and electrical properties of LaFe0.5Cr0.5O3 perovskite nanostructures

NASA Astrophysics Data System (ADS)

Ali, S. Asad; Naseem, Swaleha; Khan, Wasi; Sharma, A.; Naqvi, A. H.

2016-05-01

Perovskite nanocrystalline powder of LaFe0.5Cr0.5O3 was synthesized by sol-gel combustion route and characterized by x-ray diffractometer (XRD), scanning electron microscopy (SEM) equipped with EDS, UV-visible and LCR meter at room temperature Rietveld refinement of the XRD data confirms that the sample is in single phase-rhombohedral structure with space group R-3C. SEM micrograph shows clear nanostructure of the sample and EDS ensures the presence of all elements in good stoichiometric. The optical absorption indicates the maximum absorption at 315 nm and optical band gap of 2.94 eV was estimated using Tauc's relation. Dielectric constant (ɛ') and loss were found to decrease with increase in frequencies. The dielectric behavior was explained on the basis of Maxwell-Wagner's two layer model.

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.

Eu3+-doped Bi4Si3O12 red phosphor for solid state lighting: microwave synthesis, characterization, photoluminescence properties and thermal quenching mechanisms

PubMed Central

Zhang, Yan; Xu, Jiayue; Cui, Qingzhi; Yang, Bobo

2017-01-01

Europium-doped bismuth silicate (Bi4Si3O12) phosphor has been prepared by microwave irradiation method and its crystal structure is determined using Rietveld method. As-prepared phosphor consists of spherical, monodispersed particles with few agglomeration, high crystallinity, and narrow grain size distribution. The phosphor can be efficiently excited in the wavelength range of 260–400 nm, which matched well with the emission wavelengths of NUV LED chips. The photoluminescence spectra exhibit the highest emission peak at 703 nm originating from 5D0 → 7F4 transition of Eu3+ under NUV excitation. The luminescence lifetime for Bi4Si3O12: 2 at% Eu3+ phosphor decreases from 2.11 to 1.86 ms with increasing temperature from 10 to 498 K. This behavior of decays is discussed in terms of radiative and nonradiative decays dependence on temperature. The thermal quenching mechanism of 5D0 emission of Eu3+ in Bi4Si3O12 phosphor is a crossover process from the 5D0 level of Eu3+ to a ligand-to-europium (O2− → Eu3+) charge transfer state. The quantum efficiency of the phosphor under 393 nm excitation is found to be 14.5%, which is higher than that of the commercial red phosphors Y2O3: Eu3+, Y2O2S: Eu3+. The temperature effect on CIE coordinate was discussed in order to further investigate the potential applications. PMID:28198396

Synthesis and Structural, Electrical, and Magnetic Properties of New Iron-Aluminum Alluaudite Phases β-Na2Ni2M(PO4)3 (M = Fe and Al).

PubMed

Harbaoui, Douha; Sanad, Moustafa M S; Rossignol, Cécile; Hlil, El Kebir; Amdouni, Noureddine; Obbade, Saïd

2017-11-06

Herein we report the studies of different physical properties (structural, magnetic, thermal, morphologic, electrical, and electrochemical) of two new allotropic β-Na 2 Ni 2 M(PO 4 ) 3 (NNMP) phosphates, with M = Fe and Al. Pure orthorhombic single-phase powders were prepared under air, using an autocombustion synthesis method. They crystallize in the orthorhombic Imma space group with similar unit cell parameters [a = 10.1592(2), b = 13.0321(3), c = 6.4864(2) Å] and [a = 10.3993(1), b = 13.1966(1), c = 6.4955(1) Å] for β-Na 2 Ni 2 M(PO 4 ) 3 (NNAP) and β-Na 2 Ni 2 Fe(PO 4 ) 3 (NNFP), respectively. Crystal structures of both compounds were determined using X-ray powder diffraction and Rietveld method refinements, which indicate the occurrence of Ni 2+ in the 8g site, and of M 3+ in the 4a site of the structure. The structure consists of a three-dimensional anionic framework obtained by the association on MO 6 , NiO 6 , and PO 4 polyhedra, sharing edges and corners. The resulting three-dimensional structure creates monodimensional channels along the [100] and [010] directions formed by face-shared oxygen polyhedra and occupied by Na + cations. This nondisordered cationic distribution is confirmed by a significant change of magnetic properties. Thus, both NNAP and NNFP samples show paramagnetic to ferromagnetic transition at 14 and 19 K, respectively. For the two compounds, thermal stability, electrical conductivity, and electrochemical properties have been also investigated. The intercalation/desintercalation properties of NNMP compounds as positive electrode were tested in sodium-ion batteries. The first cycling curves exhibit a significant polarization for both prepared samples.

Effect of Ni and Ti substitutions on Li1.05Mn2O4-δ electrical conductivities at high temperature

NASA Astrophysics Data System (ADS)

Abe, Satoko; Iwasaki, Shoko; Shimonishi, Yuta; Komine, Shigeki; Munakata, Fumio

2016-10-01

Samples of Li1.05Mn2O4-δ, Li1.05Mn1.5Ni0.5O4-δ, and Li1.05Mn1.0Ni0.5Ti0.5O4-δ were prepared by a solid-state reaction technique and ultimately refined to a space group Fd-3m of spinel structure by the Rietveld method using synchrotron powder X-ray diffraction data. Comparison of lattice constants suggested that Ni-substitution increased the covalency in the bonding of MO6 (M: metal ion at 16d site) octahedrals, but Ni/Ti co-substitution decreased the covalency of M-O bonds and introduced structural distortion. Electrical conductivity measurements by a four-probe method resulted in the determination that electrical conduction (within all samples) exhibits a nonadiabatic hopping process at high temperatures. The activation energies of Li1.05Mn2O4-δ and Li1.05Mn1.5Ni0.5O4-δ were found to be of similar values. The Ni/Ti co-substituted sample of Li1.05Mn1.0Ni0.5Ti0.5O4-δ, on the other hand, showed the highest activation energy among all the measured samples. Substitution reduced the electrical conductivity relative to Li1.05Mn2O4-δ; furthermore, both the substituted samples (Li1.05Mn1.5Ni0.5O4-δ and Li1.05Mn1.0Ni0.5Ti0.5O4-δ) were found to exhibit functional independence from oxygen partial pressure (PO2).

Microstructural Investigation, Raman and Magnetic Studies on Chemically Synthesized Nanocrystalline Ni-Doped Gadolinium Oxide (Gd1.90Ni0.10O3- δ )

NASA Astrophysics Data System (ADS)

Sarkar, B. J.; Mandal, J.; Dalal, M.; Bandyopadhyay, A.; Satpati, B.; Chakrabarti, P. K.

2018-03-01

Nanocrystalline Ni-doped gadolinium oxide (Gd1.90Ni0.10O3- δ , GNO) is synthesized by co-precipitation method. The as-prepared sample is annealed in vacuum at 700°C for 6 h. Analyses of the x-ray diffractogram by Rietveld refinement method, transmission electron microscopy and Raman spectroscopy of GNO recorded at room temperature confirmed the pure crystallographic phase and complete substitution of Ni-ions in Gd2O3 lattice. Magnetization ( M) as a function of temperature ( T) and magnetic field ( H) is measured by a superconducting quantum interference device magnetometer, which suggests the presence of ferromagnetic/antiferromagnetic phases together with a paramagnetic phase. From the M-T curve it can be shown that the ferromagnetic phase dominates over para-/antiferromagnetic phases in the temperature range of 300-100 K, but from 100 K to 50 K, the antiferromagnetic phase dominates over ferro-/paramagnetic phases. Hysteresis loops recorded at different temperatures indicate the presence of weak ferro-/antiferromagnetism, which dominates in the low field region (˜ 4000 Oe), above which magnetization increases linearly. The sharp increase of magnetization in M-T curve observed in the temperature range of 50-5 K confirms the presence of dominating ferromagnetic plus paramagnetic phase over antiferromagnetic part. For the first time a combined formula generated from three-dimensional (3D) spin wave model and Johnston formula is proposed to analyze the coexistence of different magnetic phases in different temperature ranges. Interestingly, the combined formula successfully explains the co-existence of different magnetic phases along with their contribution at different temperatures. The onset of ferromagnetism in Gd1.90Ni0.10O3- δ is explained by oxygen vacancy mediated F-centre exchange (FCE) coupling mechanism.

Low temperature structural transformation in T[Ni(CN){sub 4}].xpyz with x=1,2; T=Mn,Co,Ni,Zn,Cd; pyz=pyrazine

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

Rodriguez-Hernandez, J.; Instituto de Ciencia y Tecnologia de Materiales, Universidad de La Habana; Lemus-Santana, A.A.

2010-01-15

The materials under study are pillared solids T[Ni(CN){sub 4}].xpyz with one and two (x=1,2) pyrazine (pyz) molecules and where T=Mn, Co, Ni, Zn, Cd. Stimulated by their structural features and potential role as prototype of porous solids for hydrogen storage, the structural stability under cryogenic conditions for this series of pillared solids was studied. At low temperature, in the 100-200 K range, the occurrence of a reversible structural transformation was found. For T=Mn, Co, Zn, Cd, with x=2, the structural transformation was observed to occur around 185 K, and the low temperature phase crystallizes with a monoclinic unit cell (spacemore » group Pc). This structure change results from certain charge redistribution on cooling within the involved ligands. For T=Ni with x=1, both the low and high temperature phases crystallize with unit cells of tetragonal symmetry, within the same space group but with a different unit cell volume. In this case the structure change is observed around 120 K. Above that temperature the rotational states for the pyrazine molecule are thermally excited and all the pyrazine molecules in the structure become equivalent. Under this condition the material structure is described using a smaller structural unit. The structural study using X-ray powder diffraction data was complemented with calorimetric and Raman spectroscopy measurements. For the low temperature phases the crystal structures were solved from Patterson methods and then refined using the Rietveld method. - Graphical abstract: Low temperature ordered structure for pyrazine in T[Ni(CN){sub 4}].pyz.« less

Improved photocatalytic activities of CuxCo0.5-xNi0.5Fe2O4 nanoparticles through co-precipitation method in degrading methylene blue

NASA Astrophysics Data System (ADS)

Lassoued, Abdelmajid; Lassoued, Mohamed Saber; Dkhil, Brahim; Ammar, Salah; Gadri, Abdellatif

2018-07-01

We report the synthesis of CuxCo0.5-xNi0.5Fe2O4 with x = (0.1, 0.2, 0.3, 0.4) nanoparticles using the co-precipitation method in the presence of oleic acid as a surfactant and coating material. The X-ray diffraction analysis with Rietveld refinement technique confirmed the formation of cubic phase with Fd-3m space group of all the prepared nano-ferrites. The average crystallite size varies in the range of 21-38 nm with varying concentration of copper. The lattice parameter was found to decrease with increase in copper substitution. This may be attributed to larger ionic radius of cobalt as compared to that of copper. TEM and SEM analysis showed the monodispersion and cubic-like nanostructure. Two prominent stretching bands were observed in FT-IR spectra around 400-600 cm-1. These two bands confirmed the spinel structure of the prepared nanoparticles. Raman spectroscopy is used to verify that we have synthesized ferrite spinels and determines their phonon modes. The thermal decomposition of CuxCo0.5-xNi0.5Fe2O4 was investigated by TGA∖DTA. The optical study UV-visible is used to calculate the optical band gap energies. The products exhibited the attractive magnetic properties with high saturation magnetization, which were examined by a vibrating sample magnetometer (VSM). On the other part, the photocatalytic activity of our compounds was studied using methylene blue (MB) as model organic pollutants, where the results showed that an appropriate amount of copper (Cu2+) could greatly increase the amount of hydroxyl radicals generated by the ferrite nanoparticles, which were responsible for the obvious increase in the photocatalytic activity.

Conventional and microwave combustion synthesis of optomagnetic CuFe2O4 nanoparticles for hyperthermia studies

NASA Astrophysics Data System (ADS)

Kombaiah, K.; Vijaya, J. Judith; Kennedy, L. John; Bououdina, M.; Al-Najar, Basma

2018-04-01

Nanosized copper ferrite (CuFe2O4) nanoparticles have been prepared by conventional (CCM) and microwave (MCM) combustion methods using Hibiscus rosa sinensis plant extract as a fuel. XRD and rietveld analysis confirmed the formation of single cubic phase and with crystallite size varying from 25 to 62 nm owing to grain growth after calcination. FT-IR analysis confirms the modes of the cubic CuFe2O4 phase, due to the stretching and bending vibrations. Spherical shaped particles are observed by scanning electron microscopy and the average particle size is found to be in the range of 50-200 nm. The chemical composition is confirmed by energy dispersive X-ray analysis. The optical band gap energy estimated using Kubelka-Munk function with the help of UV-Visible diffused reflectance spectroscopy, is found to be 2.34 and 2.22 eV for CCM and MCM respectively. Photoluminescence analysis indicates that both samples absorb light in the UV-visible region and exhibit emissions at 360, 376, and 412 nm. Magnetic measurements indicate a ferromagnetic behavior, where both magnetic properties very much influenced by the preparation method and calcination temperature: both saturation magnetization and coercivity are found higher when using CCM and MCM; from 29.40 to 34.09 emu/g while almost double from 224.4 to 432.2 Oe. The observed changes in physical properties are mainly associated with crystallinity, particle size, better chemical homogeneity, and cations distribution among tetrahedral/octahedral sites. The maximum specific absorption rate obtained was 14.63 W/g, which can be considered suitable and favorable for magnetic hyperthermia. This study highlighted the benefits of green synthesis of CuFe2O4 nanoparticles providing better magnetic properties for the platform of hyperthermia application.

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

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

Investigation of structural and electrical properties of La{sub 0.7}(Ba{sub 1-x}Ca{sub x}){sub 0.3}MnO{sub 3} compounds by sol-gel method

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

Winarsih, Suci; Kurniawan, Budhy, E-mail: bkuru07@gmail.com; Manaf, Azwar

2016-06-17

In this paper, we explored structural and electrical properties of La{sub 0.7}(Ba{sub 1-x}Ca{sub x}){sub 0.3}MnO{sub 3} (x = 0; 0.03; and 0.05) compounds. The general structure of perovskite manganites is AMnO{sub 3} (A= trivalent rare earth with divalent ion-doped). Average A-site cation size, external pressure, and the variance of the cation size σ{sup 2} are one of many factors that affected to magneto-transport properties of manganites as reported by others. In this work we focus only on the electrical properties in La{sub 0.7}Ba{sub 0.3}MnO{sub 3} Ca-doped compound which may influence crystal structure resulting resistivity phenomena under magnetic field influence. Allmore » samples were synthesized by sol-gel method from which fine powders were obtained. The X-ray powder diffraction pattern of powder materials shows that all samples are fully crystalline with a rhombohedral structure. Rietveld refinement shows that the presence of calcium has changed some crystal structural parameters such lattice parameter, Mn–O bond length, and Mn–O–Mn angles. The electrical resistivity of all synthesized materials investigated by four point probe method using Cryogenic Magnet in the temperature range of 50-300 K under influence a magnetic field shows resistivity temperature dependent. In fact presence of calcium has reduced the resistivity. It might occure because it has made an enhancement in the mobility of hopping electrons. The magnetic external field causes the resistivity decreased for all samples because host spin align by delocalizing the charge carries so electron itinerant through the lattice suggested by other authors. Both calcium dopant concentration and the applied external magnetic field shows strong correlation in reduction of resistivity.« less

Preparation and characterization of mechanically alloyed AB3-type based material LaMg2Ni5Al4 and its solid-gaz hydrogen storage reaction

NASA Astrophysics Data System (ADS)

Jaafar, Hassen; Aymard, Luc; Dachraoui, Walid; Demortière, Arnaud; Abdellaoui, Mohieddine

2018-04-01

We developed in the present paper the synthesis of a new AB3-type compound LaMg2Ni5Al4 by mechanical alloying (MA) process. ​​X-ray diffraction analysis (XRD) was used to determine the structural properties and the phase evolution of the powder mixtures. Two different synthesis pathways have been investigated. The first starting from elemental metals and the second from a mixture of two binary compounds LaNi5 (CaCu5-type structure, P6/mmm space group) and Al(Mg) solid solution (cubic Fm-3 m space group). The results show multiphase alloys which contain LaMg2Ni5Al4 main phase with hexagonal PuNi3-type structure (R-3 m space group). Rietveld analysis shows that using a planetary ball mill, we obtain a good yield of LaMg2Ni5Al4 compound after 5 h of mechanical alloying for both synthesis pathways. TEM analysis confirmed XRD results. SEM-EDX analysis of the final product was in agreement with the nominal chemical formula. A setup of possible solid-gaz hydrogenation reaction will be described so far at the end of this work. Electrochemical results demonstrate evidence on hydrogen absorption in the AB3 material and the discharge capacity was equal to 5.9 H/f.u.

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

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.

Burst nucleation by hot injection for size controlled synthesis of ε-cobalt nanoparticles.

PubMed

Zacharaki, Eirini; Kalyva, Maria; Fjellvåg, Helmer; Sjåstad, Anja Olafsen

2016-01-01

Reproducible growth of narrow size distributed ε-Co nanoparticles with a specific size requires full understanding and identification of the role of essential synthesis parameters for the applied synthesis method. For the hot injection methodology, a significant discrepancy with respect to obtained sizes and applied reaction conditions is reported. Currently, a systematic investigation controlling key synthesis parameters as injection-temperature and time, metal to surfactant ratio and reaction holding time in terms of their impact on mean ([Formula: see text]mean) and median ([Formula: see text]median) particle diameter using dichlorobenzene (DCB), Co2(CO)8 and oleic acid (OA) as the reactant matrix is lacking. A series of solution-based ε-Co nanoparticles were synthesized using the hot injection method. Suspensions and obtained particles were analyzed by DLS, ICP-OES, (synchrotron)XRD and TEM. Rietveld refinements were used for structural analysis. Mean ([Formula: see text]mean) and median ([Formula: see text]median) particle diameters were calculated with basis in measurements of 250-500 particles for each synthesis. 95 % bias corrected confidence intervals using bootstrapping were calculated for syntheses with three or four replicas. ε-Co NPs in the size range ~4-10 nm with a narrow size distribution are obtained via the hot injection method, using OA as the sole surfactant. Typically the synthesis yield is ~75 %, and the particles form stable colloidal solutions when redispersed in hexane. Reproducibility of the adopted synthesis procedure on replicate syntheses was confirmed. We describe in detail the effects of essential synthesis parameters, such as injection-temperature and time, metal to surfactant ratio and reaction holding time in terms of their impact on mean ([Formula: see text]mean) and median ([Formula: see text]median) particle diameter. The described synthesis procedure towards ε-Co nanoparticles (NPs) is concluded to be robust when controlling key synthesis parameters, giving targeted particle diameters with a narrow size distribution. We have identified two major synthesis parameters which control particle size, i.e., the metal to surfactant molar ratio and the injection temperature of the hot OA-DCB solution into which the cobalt precursor is injected. By increasing the metal to surfactant molar ratio, the mean particle diameter of the ε-Co NPs has been found to increase. Furthermore, an increase in the injection temperature of the hot OA-DCB solution into which the cobalt precursor is injected, results in a decrease in the mean particle diameter of the ε-Co NPs, when the metal to surfactant molar ratio [Formula: see text] is fixed at ~12.9.

Structural differences existing in bulk and nanoparticles of Y{sub 2}Sn{sub 2}O{sub 7}: Investigated by experimental and theoretical methods

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

Nigam, Sandeep, E-mail: snigam@barc.gov.in; Sudarsan, V., E-mail: vsudar@barc.gov.in; Majumder, C.

Present manuscript deals with the structural changes associated with transformation of bulk Y{sub 2}Sn{sub 2}O{sub 7} into nanoparticles of Y{sub 2}Sn{sub 2}O{sub 7}. Nanoparticles of Y{sub 2}Sn{sub 2}O{sub 7} both undoped and Eu{sup 3+} doped, were prepared at a relatively low temperature (700 °C) and investigated for their structural and luminescence properties and compared them with that of bulk Y{sub 2}Sn{sub 2}O{sub 7} sample prepared by the solid-state method at 1300 °C. Significant distortion in geometry and electron density distribution around Y{sup 3+}/Eu{sup 3+} ions in nanoparticles are confirmed from the Rietveld refinement of the powder X-ray diffraction patterns andmore » theoretical calculations based on the density functional theory (DFT). The SnO{sub 6} octahedron in Y{sub 2}Sn{sub 2}O{sub 7} is more expanded in nanoparticles compared to bulk. Iso-surface density distribution reveals that while bulk sample shows typical ionic feature in Y/Eu--O bonds, nanoparticle sample shows sharing of electron density along bond axis pertaining to covalent character. These inferences are further supported by the doped Eu{sup 3+} luminescence and calculated Ω{sub 2} and Ω{sub 4} parameters. - Graphical abstract: YO{sub 8} scalenohedron present in bulk and nanoparticles of Y{sub 2}Sn{sub 2}O{sub 7}.Variation of the electron density around Y{sup 3+} ions in YO{sub 8} polyhedron is also shown in bulk and nanoparticles of Y{sub 2}Sn{sub 2}O{sub 7}. The difference in the extent of ionic/covalent nature of the Y--O bond is clearly seen the contour plot of electron density. Highlights: ► YO{sub 8} scalenohedron is axially and equatorially distorted in Y{sub 2}Sn{sub 2}O{sub 7} nanoparticles. ► Enlargement of SnO{sub 6} octahedron in nanoparticles of Y{sub 2}Sn{sub 2}O{sub 7} compared to bulk. ► Less symmetric charge distribution around Y{sup 3+} ions in Y{sub 2}Sn{sub 2}O{sub 7} nanoparticles.« less

Real-time observations of lithium battery reactions-operando neutron diffraction analysis during practical operation.

PubMed

Taminato, Sou; Yonemura, Masao; Shiotani, Shinya; Kamiyama, Takashi; Torii, Shuki; Nagao, Miki; Ishikawa, Yoshihisa; Mori, Kazuhiro; Fukunaga, Toshiharu; Onodera, Yohei; Naka, Takahiro; Morishima, Makoto; Ukyo, Yoshio; Adipranoto, Dyah Sulistyanintyas; Arai, Hajime; Uchimoto, Yoshiharu; Ogumi, Zempachi; Suzuki, Kota; Hirayama, Masaaki; Kanno, Ryoji

2016-06-30

Among the energy storage devices for applications in electric vehicles and stationary uses, lithium batteries typically deliver high performance. However, there is still a missing link between the engineering developments for large-scale batteries and the fundamental science of each battery component. Elucidating reaction mechanisms under practical operation is crucial for future battery technology. Here, we report an operando diffraction technique that uses high-intensity neutrons to detect reactions in non-equilibrium states driven by high-current operation in commercial 18650 cells. The experimental system comprising a time-of-flight diffractometer with automated Rietveld analysis was developed to collect and analyse diffraction data produced by sequential charge and discharge processes. Furthermore, observations under high current drain revealed inhomogeneous reactions, a structural relaxation after discharge, and a shift in the lithium concentration ranges with cycling in the electrode matrix. The technique provides valuable information required for the development of advanced batteries.

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.

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

Reprobing the mechanism of negative thermal expansion in siliceous faujasite

DOE PAGES

Attfield, Martin P.; Feygenson, Mikhail; Neuefeind, Joerg C.; ...

2016-02-11

A combination of Rietveld refinement and PDF analysis of total neutron scattering data are used to provide further insight into the negative thermal expansion mechanism of siliceous faujasite. The negative thermal expansion mechanism of siliceous faujasite is attributed to the transverse vibrations of bridging oxygen atoms resulting in the coupled librations of the SiO 4 tetrahedra. The constituent SiO 4 tetrahedra are revealed to expand in size with temperature which is a behaviour that has not been determined directly previously and they are also shown to undergo some distortion as temperature is increased. However, these distortions are not distinct enoughmore » in any geometric manner for the average behaviour of the SiO 4 tetrahedra not to be considered as that of a rigid units. The work further displays the benefits of using total scattering experiments to unveil the finer details of dynamic thermomechanical processes within crystalline materials.« 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.

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.

Neutron and electron diffraction studies of La(Zn1/2Ti1/2)O3 perovskite.

PubMed

Ubic, Rick; Hu, Yi; Abrahams, Isaac

2006-08-01

The crystallography and microwave dielectric properties of La(Zn(1/2)Ti(1/2))O(3) (LZT) ceramics prepared via the mixed-oxide route were investigated in this study. While samples were largely single phase, small amounts of ZnO impurity were detected in sintered pellets. Observed reflections in electron and neutron diffraction patterns indicate that the symmetry of LZT is P2(1)/n. The B site is ordered on {110} or pseudocubic {111}, but the presence of the pseudocubic 1/2(111) reflection is in itself insufficient to indicate the existence of such order. Rietveld refinements of the neutron diffraction data yield an excellent fit for such a model. The structure is highly twinned, with variants related through common {211} composition planes and 90 degrees rotations about <011>. The microwave dielectric properties measured were epsilon(r) = 34, Qf = 36,090 and tau(f) = -70 MK(-1).

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

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

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.

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.

Novel trends in pair distribution function approaches on bulk systems with nanoscale heterogeneities

DOE PAGES

Emil S. Bozin; Billinge, Simon J. L.

2016-07-29

Novel materials for high performance applications increasingly exhibit structural order on the nanometer length scale; a domain where crystallography, the basis of Rietveld refinement, fails [1]. In such instances the total scattering approach, which treats Bragg and diffuse scattering on an equal basis, is a powerful approach. In recent years, the analysis of the total scattering data became an invaluable tool and the gold standard for studying nanocrystalline, nanoporous, and disordered crystalline materials. The data may be analyzed in reciprocal space directly, or Fourier transformed to the real-space atomic pair distribution function (PDF) and this intuitive function examined for localmore » structural information. Here we give a number of illustrative examples, for convenience picked from our own work, of recent developments and applications of total scattering and PDF analysis to novel complex materials. There are many other wonderful examples from the work of others.« less

Annealing effects on the structural and magnetic properties of off-stoichiometric Fe-Mn-Ga ferromagnetic shape memory alloys

DOE PAGES

Chen, Yan; Bei, Hongbin; Dela Cruz, Clarina R; ...

2016-05-07

Annealing plays an important role in modifying structures and properties of ferromagnetic shape memory alloys (FSMAs). The annealing effect on the structures and magnetic properties of off-stoichiometric Fe 45Mn 26Ga 29 FSMA has been investigated at different elevated temperatures. Rietveld refinements of neutron diffraction patterns display that the formation of the γ phase in Fe 45Mn 26Ga 29 annealed at 1073 K increases the martensitic transformation temperature and reduces the thermal hysteresis in comparison to the homogenized sample. The phase segregation of a Fe-rich cubic phase and a Ga-rich cubic phase occurs at the annealing temperature of 773 K. Themore » atomic occupancies of the alloys are determined thanks to the neutron's capability of differentiating transition metals. The annealing effects at different temperatures introduce a different magnetic characteristic that is associated with distinctive structural changes in the crystal.« 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.

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.

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

Real-time observations of lithium battery reactions—operando neutron diffraction analysis during practical operation

PubMed Central

Taminato, Sou; Yonemura, Masao; Shiotani, Shinya; Kamiyama, Takashi; Torii, Shuki; Nagao, Miki; Ishikawa, Yoshihisa; Mori, Kazuhiro; Fukunaga, Toshiharu; Onodera, Yohei; Naka, Takahiro; Morishima, Makoto; Ukyo, Yoshio; Adipranoto, Dyah Sulistyanintyas; Arai, Hajime; Uchimoto, Yoshiharu; Ogumi, Zempachi; Suzuki, Kota; Hirayama, Masaaki; Kanno, Ryoji

2016-01-01

Among the energy storage devices for applications in electric vehicles and stationary uses, lithium batteries typically deliver high performance. However, there is still a missing link between the engineering developments for large-scale batteries and the fundamental science of each battery component. Elucidating reaction mechanisms under practical operation is crucial for future battery technology. Here, we report an operando diffraction technique that uses high-intensity neutrons to detect reactions in non-equilibrium states driven by high-current operation in commercial 18650 cells. The experimental system comprising a time-of-flight diffractometer with automated Rietveld analysis was developed to collect and analyse diffraction data produced by sequential charge and discharge processes. Furthermore, observations under high current drain revealed inhomogeneous reactions, a structural relaxation after discharge, and a shift in the lithium concentration ranges with cycling in the electrode matrix. The technique provides valuable information required for the development of advanced batteries. PMID:27357605

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.

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

Rietveld refinement of AgCa10(PO4)7 from X-ray powder data

PubMed Central

Strutynska, Nataliya Yu.; Zatovsky, Igor V.; Ogorodnyk, Ivan V.; Slobodyanik, Nikolay S.

2013-01-01

Polycrystalline silver(I) deca­calcium heptakis(orthophos­phate), AgCa10(PO4)7, was obtained by solid-state reaction. It is isotopic with members of the series MCa10(PO4)7 (M = Li, Na, K and Cs), and is closely related to the structure of β-Ca3(PO4)2. The crystal structure of the title compound is built up from a framework of [CaO9] and two [CaO8] polyhedra, one [CaO6] octa­hedron (site symmetry 3.) and three PO4 tetra­hedra (one with site symmetry 3.). The Ag+ cation is likewise located on a threefold rotation axis and resides in the cavities of the rigid [Ca10(PO4)7]− framework. It is surrounded by three O atoms in an almost regular triangular environment. PMID:23723747

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

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

Structural evolution across the insulator-metal transition in oxygen-deficient BaTiO 3-δ studied using neutron total scattering and Rietveld analysis

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

Jeong, I.-K.; Lee, Seunghun; Jeong, Se-Young

2011-08-29

Oxygen-deficient BaTiO 3-δ exhibits an insulator-metal transition with increasing δ. We performed neutron total scattering measurements to study structural evolution across an insulator-metal transition in BaTiO 3-δ. Despite its significant impact on resistivity, slight oxygen reduction (δ=0.09) caused only a small disturbance on the local doublet splitting of Ti-O bond. This finding implies that local polarization is well preserved under marginal electric conduction. In the highly oxygen-deficient metallic state (δ=0.25), however, doublet splitting of the Ti-O bond became smeared. The smearing of the local Ti-O doublet is complemented with long-range structural analysis and demonstrates that the metallic conduction in themore » highly oxygen-reduced BaTiO 3-δ is due to the appearance of nonferroelectric cubic lattice.« less