Spectrofluorimetric Characterization of an Ionic Conductor: Sodium Sulfate High-Temperature Phases Doped with Europium(III)

1994 ◽  
Vol 369 ◽  
Author(s):  
Lowell R. Matithews ◽  
Edward T. Knobbe ◽  
Gamini Dharmasena ◽  
Renée Cole ◽  
Roger Frech

AbstractThe highest-temperature polymorph of sodium sulfate, (I), has significant orientational disorder in its structure which allows it to readily accept substitution by di- and trivalent cations. Although Na2SO4 (I) exhibits reasonable ionic conductivity, it cannot be quenched to room temperature without changing phase. However, aliovalent solid solutions of (I) can be quenched to RT and resultant cation vacancies promote conduction via Na+ migration. The closely related but more ordered phase Na2SO4 (III) can also form aliovalent solid solutions which can be quenched to RT.The europium(III) ion is an extremely sensitive and useful probe of its immediate local environment. The presence, location, and intensity of its fluorescence transitions (particularly the 5D0→7F0-2 emissions) can provide detailed information about the symmetry, nature, and multiplicity of the individual Eu3+ site which cannot be gained from X-ray or neutron diffraction techniques.Our research (supported by the National Science Foundation and the State of Oklahoma) involves the structural characterization of two europium-doped sodium sulfate phases via fluorescence spectroscopy.

Materials ◽  
2021 ◽  
Vol 14 (13) ◽  
pp. 3502
Author(s):  
Fangzhou Song ◽  
Masayoshi Uematsu ◽  
Takeshi Yabutsuka ◽  
Takeshi Yao ◽  
Shigeomi Takai

LATP-based composite electrolytes were prepared by sintering the mixtures of LATP precursor and La2O3 nano-powder. Powder X-ray diffraction and scanning electron microscopy suggest that La2O3 can react with LATP during sintering to form fine LaPO4 particles that are dispersed in the LATP matrix. The room temperature conductivity initially increases with La2O3 nano-powder addition showing the maximum of 0.69 mS∙cm−1 at 6 wt.%, above which, conductivity decreases with the introduction of La2O3. The activation energy of conductivity is not largely varied with the La2O3 content, suggesting that the conduction mechanism is essentially preserved despite LaPO4 dispersion. In comparison with the previously reported LATP-LLTO system, although some unidentified impurity slightly reduces the conductivity maximum, the fine dispersion of LaPO4 particles can be achieved in the LATP–La2O3 system.


2000 ◽  
Vol 5 (S1) ◽  
pp. 412-424
Author(s):  
Jung Han ◽  
Jeffrey J. Figiel ◽  
Gary A. Petersen ◽  
Samuel M. Myers ◽  
Mary H. Crawford ◽  
...  

We report the growth and characterization of quaternary AlGaInN. A combination of photoluminescence (PL), high-resolution x-ray diffraction (XRD), and Rutherford backscattering spectrometry (RBS) characterizations enables us to explore the contours of constant- PL peak energy and lattice parameter as functions of the quaternary compositions. The observation of room temperature PL emission at 351nm (with 20% Al and 5% In) renders initial evidence that the quaternary could be used to provide confinement for GaInN (and possibly GaN). AlGaInN/GaInN MQW heterostructures have been grown; both XRD and PL measurements suggest the possibility of incorporating this quaternary into optoelectronic devices.


2020 ◽  
Vol 1000 ◽  
pp. 436-446
Author(s):  
Bambang Suharno ◽  
Nolzha Primadha Ilman ◽  
Achmad Shofi ◽  
Deni Ferdian ◽  
Fajar Nurjaman

This study was conducted to investigate the effect of palm shell charcoal reductant in the selective reduction of nickel ore with the addition of additive at various temperatures and times. In this present work, 10 wt. % of sodium sulfate as additive and 5, 10, 15 wt. % of palm shell charcoal as reductants were used. The reduction of nickel ore was performed at 950oC, 1050oC, and 1150oC for 60, 90, and 120 minutes. A wet magnetic separation method was then carried out to separate the concentrates and tailings. Characterization of reduced ore was performed by X-Ray Diffraction (XRD) and Scanning Electron Microscope (SEM) with Energy Dispersive X-ray Spectroscopy (EDS), while the composition of ferronickel in concentrate was identified by X-Ray Fluorescence (XRF). The result showed that the higher temperature reduction, the higher of nickel grade, and its recovery at the concentrate. Nevertheless, the longer reduction time and the more reductant in nickel ore lowering the nickel grade and its recovery in the concentrate. The optimum condition in this selective reduction process was obtained with the addition of 5 wt. % of reductant and 10 wt. % of sodium sulfate in nickel ore, which was reduced at 1150oC for 60 minutes. It resulted in 4.60% and 73.23% for nickel grade and its recovery, respectively.


2003 ◽  
Vol 18 (2) ◽  
pp. 128-134 ◽  
Author(s):  
A. Le Bail ◽  
A.-M. Mercier

The crystal structures of the chiolite-related room temperature phases α-Na5M3F14 (MIII=Cr,Fe,Ga) are determined. For all of them, the space group is P21/n, Z=2; a=10.5096(3) Å, b=7.2253(2) Å, c=7.2713(2) Å, β=90.6753(7)° (M=Cr); a=10.4342(7) Å, b=7.3418(6) Å, c=7.4023(6) Å, β=90.799(5)° (M=Fe), and a=10.4052(1) Å, b=7.2251(1) Å, c=7.2689(1), β=90.6640(4)° (M=Ga). Rietveld refinements produce final RF factors 0.036, 0.033, and 0.035, and RWP factors, 0.125, 0.116, and 0.096, for MIII=Cr, Fe, and Ga, respectively. The MF6 polyhedra in the defective isolated perovskite-like layers deviate very few from perfect octahedra. Subtle octahedra tiltings lead to the symmetry decrease from the P4/mnc space group adopted by the Na5Al3F14 chiolite aristotype to the P21/n space group adopted by the title series. Facile twinning precluded till now the precise characterization of these compounds.


2006 ◽  
Vol 21 (3) ◽  
pp. 214-219 ◽  
Author(s):  
Abderrahim Aatiq ◽  
Btissame Haggouch ◽  
Rachid Bakri ◽  
Youssef Lakhdar ◽  
Ismael Saadoune

Structures of two K2SnX(PO4)3(X=Fe,Yb) phosphates, obtained by conventional solid state reaction techniques at 950 °C, were determined at room temperature by X-ray powder diffraction using Rietveld analysis. The two materials exhibit the langbeinite-type structure (P213 space group, Z=4). Cubic unit cell parameter values are: a=9.9217(4) Å and a=10.1583(4) Å for K2SnFe(PO4)3 and K2SnYb(PO4)3, respectively. Structural refinements show that the two crystallographically independent octahedral sites (of symmetry 3) have a mixed Sn∕X (X=Fe,Yb) population although ordering is stronger in the Yb phase than in the Fe phase.


2012 ◽  
Vol 194 ◽  
pp. 187-193 ◽  
Author(s):  
J.M. Loureiro ◽  
Benilde F.O. Costa ◽  
Gerard Le Caër ◽  
Bernard Malaman

Ternary alloys, (Fe50−x/2Co50−x/2)Snx(x ≤ 33 at.%), are prepared by mechanical alloying from powder mixtures of the three elements. As-milled alloys are studied by X-ray diffraction and 57Fe and 119Sn Mössbauer spectroscopy. The solubility of Sn in near-equiatomic bcc FeCo is increased from ~0.5 at. % at equilibrium to ~20 at.% in the used milling conditions. The average 119Sn hyperfine magnetic field at room temperature is larger, for any x, than the corresponding fields in mechanically alloyed Fe-Sn solid solutions.


Inorganics ◽  
2021 ◽  
Vol 9 (4) ◽  
pp. 28
Author(s):  
Kriti Pathak ◽  
Chandan Nandi ◽  
Jean-François Halet ◽  
Sundargopal Ghosh

Synthesis, isolation, and structural characterization of unique metal rich diamagnetic cobaltaborane clusters are reported. They were obtained from reactions of monoborane as well as modified borohydride reagents with cobalt sources. For example, the reaction of [Cp*CoCl]2 with [LiBH4·THF] and subsequent photolysis with excess [BH3·THF] (THF = tetrahydrofuran) at room temperature afforded the 11-vertex tricobaltaborane nido-[(Cp*Co)3B8H10] (1, Cp* = η5-C5Me5). The reaction of Li[BH2S3] with the dicobaltaoctaborane(12) [(Cp*Co)2B6H10] yielded the 10-vertex nido-2,4-[(Cp*Co)2B8H12] cluster (2), extending the library of dicobaltadecaborane(14) analogues. Although cluster 1 adopts a classical 11-vertex-nido-geometry with one cobalt center and four boron atoms forming the open pentagonal face, it disobeys the Polyhedral Skeletal Electron Pair Theory (PSEPT). Compound 2 adopts a perfectly symmetrical 10-vertex-nido framework with a plane of symmetry bisecting the basal boron plane resulting in two {CoB3} units bridged at the base by two boron atoms and possesses the expected electron count. Both compounds were characterized in solution by multinuclear NMR and IR spectroscopies and by mass spectrometry. Single-crystal X-ray diffraction analyses confirmed the structures of the compounds. Additionally, density functional theory (DFT) calculations were performed in order to study and interpret the nature of bonding and electronic structures of these complexes.


2014 ◽  
Vol 625 ◽  
pp. 661-664
Author(s):  
Chen Chuang Lok ◽  
Yin Fong Yeong

In the present work, ZIF-8/6FDA-durene mixed matrix membranes (MMMs) were synthesized and characterized. ZIF-8 nanocrystals, which were used as the inorganic filler, were synthesized using rapid room-temperature synthesis method whereas 6FDA-durene polyimide was synthesized by polycondensation method followed by chemical imidization. Pure and 6FDA-durene membranes loaded with 5 wt%, 10 wt% and 15 wt% of ZIF-8 were fabricated. The structural properties and morphology of the resultant membranes were characterized by using X-ray Diffraction (XRD) and Field emission scanning electron microscope (FESEM) . The EDX images showed that ZIF-8 particles agglomerated in the polymer matrix. However, no phase separation was observed for all resultant MMMs.


2009 ◽  
Vol 63 (6) ◽  
Author(s):  
Yan Li ◽  
Chuan-Sheng Liu ◽  
Yun-Ling Zou

AbstractZnO nano-tubes (ZNTs) have been successfully synthesized via a simple hydrothermal-etching method, and characterized by X-ray diffraction, field emission scanning electron microscopy and room temperature photoluminescence measurement. The as-synthesized ZNTs have a diameter of 500 nm, wall thickness of 20–30 nm, and length of 5 µm. Intensity of the plane (0002) diffraction peak, compared with that of plane (10$$ \bar 1 $$0) of ZNTs, is obviously lower than that of ZnO nano-rods. This phenomenon can be caused by the smaller cross section of plane (0002) of the nano-tubes compared with that of other morphologies. On basis of the morphological analysis, the formation process of nano-tubes can be proposed in two stages: hydrothermal growth and reaction etching process.


1994 ◽  
Vol 47 (2) ◽  
pp. 391 ◽  
Author(s):  
CJ Kepert ◽  
BW Skeleton ◽  
AH White

The room-temperature single-crystal X-ray structural characterization of the title compound (tpyH2)2[Tb(OH2)8]Cl7.~2⅓H2O is recorded. Crystals are triclinic, Pī , a 17.063(5), b 16.243(3), c 7.878(3) Ǻ, α 84.78(2), β 84.39(3), γ 87.81(2)°, Z = 2 formula units; 3167 'observed' diffractometer reflections were refined by full-matrix least-squares procedures to a residual of 0.057. Notable features of interest of the compound are the 'chelation' of chloride ions by the terpyridinium cations , and the existence of a free [Tb(OH2)8]2+ cation in the presence of an abundance of chloride ions.


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