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Title: Structural and conductivity studies of CsK(SO{sub 4}){sub 0.32}(SeO{sub 4}){sub 0.68}Te(OH){sub 6}

Abstract

The compound CsK(SO{sub 4}){sub 0.32}(SeO{sub 4}){sub 0.68}Te(OH){sub 6} crystallizes in the monoclinic P2{sub 1}/n space group. It was analyzed, at room temperature, using X-ray diffractometer data. The main feature of these atomic arrangements is the coexistence of three and different anions (SO{sub 4}{sup 2-}, SeO{sub 4}{sup 2-} and TeO{sub 6}{sup 6-}groups) in the unit cell, connected by hydrogen bonds which make the building of the crystal. The thermal analysis of the title compound shows three distinct endothermal peaks at 435, 460 and 475 K. Complex impedance measurements are performed on this material as a function of both temperature and frequency. The electric conduction has been studied. The temperature dependence on the conductivity indicates that the sample became an ionic conductor at high temperature. - Graphical abstract: Projection of crystal structure CsK(SO{sub 4}){sub 0.32}(SeO{sub 4}){sub 0.68}Te(OH){sub 6} on the ab plane. Highlights: Black-Right-Pointing-Pointer We have studied the results of the crystal structure of the new mixed compound. Black-Right-Pointing-Pointer We have characterized the phase transition observed in DSC curve. Black-Right-Pointing-Pointer The protonic conduction in our material is probably due to a hopping mechanism.

Authors:
 [1];  [1];  [2];  [3];  [1];  [1]
  1. Laboratoire de Chimie Inorganique, Universite de Sfax, Faculte des Sciences de Sfax, BP 1171, 3000 Sfax (Tunisia)
  2. (France)
  3. Laboratoire de l'Etat solide, Universite de Sfax, Faculte des Sciences de Sfax, BP 1171, 3000 Sfax (Tunisia)
Publication Date:
OSTI Identifier:
22149941
Resource Type:
Journal Article
Resource Relation:
Journal Name: Journal of Solid State Chemistry; Journal Volume: 196; Other Information: Copyright (c) 2012 Elsevier Science B.V., Amsterdam, The Netherlands, All rights reserved.; Country of input: International Atomic Energy Agency (IAEA)
Country of Publication:
United States
Language:
English
Subject:
36 MATERIALS SCIENCE; CALORIMETRY; CRYSTALS; DIELECTRIC PROPERTIES; MONOCLINIC LATTICES; PHASE TRANSFORMATIONS; POTASSIUM COMPLEXES; SELENATES; SPACE GROUPS; SULFATES; SUPERCONDUCTIVITY; TEMPERATURE DEPENDENCE; THERMAL ANALYSIS; X-RAY DIFFRACTION; X-RAY DIFFRACTOMETERS

Citation Formats

Djemel, M., E-mail: jmal_manel@yahoo.fr, Abdelhedi, M., E-mail: m_abdelhedi2002@yahoo.fr, Laboratoire Leon Brouillon, CE/Saclay, 91191 Gif-Sur-Yvette Cedex, Zouari, N., E-mail: bizrirl@yahoo.fr, Dammak, M., E-mail: meddammak@yahoo.fr, and Kolsi, A.W., E-mail: kolsi_abdelhwaheb@yahoo.fr. Structural and conductivity studies of CsK(SO{sub 4}){sub 0.32}(SeO{sub 4}){sub 0.68}Te(OH){sub 6}. United States: N. p., 2012. Web. doi:10.1016/J.JSSC.2012.06.040.
Djemel, M., E-mail: jmal_manel@yahoo.fr, Abdelhedi, M., E-mail: m_abdelhedi2002@yahoo.fr, Laboratoire Leon Brouillon, CE/Saclay, 91191 Gif-Sur-Yvette Cedex, Zouari, N., E-mail: bizrirl@yahoo.fr, Dammak, M., E-mail: meddammak@yahoo.fr, & Kolsi, A.W., E-mail: kolsi_abdelhwaheb@yahoo.fr. Structural and conductivity studies of CsK(SO{sub 4}){sub 0.32}(SeO{sub 4}){sub 0.68}Te(OH){sub 6}. United States. doi:10.1016/J.JSSC.2012.06.040.
Djemel, M., E-mail: jmal_manel@yahoo.fr, Abdelhedi, M., E-mail: m_abdelhedi2002@yahoo.fr, Laboratoire Leon Brouillon, CE/Saclay, 91191 Gif-Sur-Yvette Cedex, Zouari, N., E-mail: bizrirl@yahoo.fr, Dammak, M., E-mail: meddammak@yahoo.fr, and Kolsi, A.W., E-mail: kolsi_abdelhwaheb@yahoo.fr. Sat . "Structural and conductivity studies of CsK(SO{sub 4}){sub 0.32}(SeO{sub 4}){sub 0.68}Te(OH){sub 6}". United States. doi:10.1016/J.JSSC.2012.06.040.
@article{osti_22149941,
title = {Structural and conductivity studies of CsK(SO{sub 4}){sub 0.32}(SeO{sub 4}){sub 0.68}Te(OH){sub 6}},
author = {Djemel, M., E-mail: jmal_manel@yahoo.fr and Abdelhedi, M., E-mail: m_abdelhedi2002@yahoo.fr and Laboratoire Leon Brouillon, CE/Saclay, 91191 Gif-Sur-Yvette Cedex and Zouari, N., E-mail: bizrirl@yahoo.fr and Dammak, M., E-mail: meddammak@yahoo.fr and Kolsi, A.W., E-mail: kolsi_abdelhwaheb@yahoo.fr},
abstractNote = {The compound CsK(SO{sub 4}){sub 0.32}(SeO{sub 4}){sub 0.68}Te(OH){sub 6} crystallizes in the monoclinic P2{sub 1}/n space group. It was analyzed, at room temperature, using X-ray diffractometer data. The main feature of these atomic arrangements is the coexistence of three and different anions (SO{sub 4}{sup 2-}, SeO{sub 4}{sup 2-} and TeO{sub 6}{sup 6-}groups) in the unit cell, connected by hydrogen bonds which make the building of the crystal. The thermal analysis of the title compound shows three distinct endothermal peaks at 435, 460 and 475 K. Complex impedance measurements are performed on this material as a function of both temperature and frequency. The electric conduction has been studied. The temperature dependence on the conductivity indicates that the sample became an ionic conductor at high temperature. - Graphical abstract: Projection of crystal structure CsK(SO{sub 4}){sub 0.32}(SeO{sub 4}){sub 0.68}Te(OH){sub 6} on the ab plane. Highlights: Black-Right-Pointing-Pointer We have studied the results of the crystal structure of the new mixed compound. Black-Right-Pointing-Pointer We have characterized the phase transition observed in DSC curve. Black-Right-Pointing-Pointer The protonic conduction in our material is probably due to a hopping mechanism.},
doi = {10.1016/J.JSSC.2012.06.040},
journal = {Journal of Solid State Chemistry},
number = ,
volume = 196,
place = {United States},
year = {Sat Dec 15 00:00:00 EST 2012},
month = {Sat Dec 15 00:00:00 EST 2012}
}
  • The crystal structures of the title compounds were solved using the single-crystal X-ray diffraction technique. At room temperature CsKSO{sub 4}Te(OH){sub 6} was found to crystallize in the monoclinic system with Pn space group and lattice parameters: a=12.5463(6)A; b=6.5765(2)A; c=12.6916(7)A; {beta}=106.53(2){sup o}; V=1003.914(4)A{sup 3}; Z=4 and D{sub calc.}=3.29g/cm{sup 3}. The structural refinement has led to a reliability factor of R{sub 1}=0.0284 (wR{sub 2}=0.064) for 7577 independent reflections. Rb{sub 1.25}K{sub 0.75}SO{sub 4}Te(OH){sub 6} material possesses a monoclinic structure with space group P2{sub 1}/a and cell parameters: a=11.3411(6)A; b=6.5819(2)A; c=13.5730(8)A; {beta}=106.860(10){sup o}; V=969.62(10)A{sup 3}; Z=4 and D=3.16(3)g/cm{sup 3}. The residuals are R{sub 1}=0.0297more » and wR{sub 2}=0.0776 for 3336 independent reflections. The main interest of these structures is the presence of two different and independent anionic groups (TeO{sub 6}{sup 6-} and SO{sub 4}{sup 2-}) in the same crystal. Complex impedance measurements (Z*=Z{sup '}-iZ{sup '}') have been undertaken in the frequency and temperature ranges 20-10{sup 6}Hz and 400-600K, respectively. The dielectric relaxation is studied in the complex modulus formalism M*.« less
  • The crystal structure of Cs{sub 0.86}(NH{sub 4}){sub 1.14}SO{sub 4}.Te(OH){sub 6} is determined by X-ray diffraction analysis. The space group is P2{sub 1}/c with a=13.681(3)A, b=6.608(1)A, c=11.362(2)A, {beta}=106.65(3){sup o} and Z=4 at 293K. The structure is refined to R=2.9%. The distribution of atoms can be described as isolated TeO{sub 6} octahedra and SO{sub 4} tetrahedra. The Cs{sup +} and NH{sub 4}{sup +} cations, occupying the same positions, are located between these polyhedra. The main feature of this structure is the coexistence of two types of anions in the same crystal related by network hydrogen bonds. The mixed solid solution cesium ammoniummore » sulphate tellurate exhibits two phase transitions at 470 and 500K. These transitions, detected by differential scanning calorimetric, are analyzed by dielectric measurements using the impedance and modulus spectroscopy techniques.« less
  • The new compounds K{sub 3}V{sub 0.32}Ta{sub 0.68}S{sub 4} (1), K{sub 6}Nb{sub 1.07}Ta{sub 2.93}S{sub 22} (2), K{sub 6}Nb{sub 2.97}Ta{sub 1.03}S{sub 25} (3), K{sub 3}Cu{sub 3}Nb{sub 0.98}Ta{sub 1.02}S{sub 8} (4), and KCu{sub 2}Nb{sub 0.53}Ta{sub 0.47}S{sub 4} (5) have been synthesized by the reactive flux method. Their crystal structures were determined by single crystal X-ray diffraction. Crystal data: 1: space group Pnma, a=9.2354(7), b=10.6920(6), c=9.2991(5) A, Z=4; 2: space group P2{sub 1}/c, a=7.6412(4), b=8.7572(5), c=24.5772(14) A, {beta}=98.559(6){sup o}, Z=2; 3: space group P2{sub 1}/n, a=15.7147(10), b=12.9840(9), c=18.2363(12) A, {beta}=104.123(8){sup o}, Z=4; 4: space group C2/c, a=23.5934(19), b=5.5661(2), c=14.2373(12) A, {beta}=120.631(9){sup o}, Z=4; 5:more » space group Ama2, a=7.4615(4), b=18.2902(16), c=5.5320(6) A, Z=4. The structure of compound 1 is based on discrete tetrahedral MS{sub 4} (M=V/Ta) anions, which are separated by K{sup +} cations. The structure of 2 consists of K{sup +} cations and [M {sub 4}S{sub 22}]{sup 6-} (M=Nb/Ta) anions, in which two M {sub 2}S{sub 11} building blocks are linked via terminal sulfur ligands. In 3 the complex anion [M {sub 4}S{sub 25}]{sup 6-} (M=Nb/Ta) is observed which comprises two M {sub 2}S{sub 11} subunits bridged by a S{sub 3} chain. In 4 {sup 1} {sub {infinity}}[Cu{sub 3} M {sub 2}S{sub 8}]{sup 3-} (M=Nb/Ta) anionic chains are found which are formed by corner sharing of CuS{sub 4} tetrahedra and edge sharing between CuS{sub 4} and MS{sub 4} tetrahedra. The structure of 5 consists of [Cu{sub 2} MS{sub 4}]{sup -} (M=Nb/Ta) anionic layers separated by K{sup +} cations. The CuS{sub 4} and MS{sub 4} tetrahedra share edges and corners yielding layers. All compounds were characterized with Raman spectroscopy and the compound 2-5 with UV/vis diffuse reflectance spectroscopy. - Graphical abstract: The five compounds K{sub 3}V{sub 0.32}Ta{sub 0.68}S{sub 4}, K{sub 6}Nb{sub 1.07}Ta{sub 2.93}S{sub 22}, K{sub 6}Nb{sub 2.97}Ta{sub 1.03}S{sub 25}, K{sub 3}Cu{sub 3}Nb{sub 0.98}Ta{sub 1.02}S{sub 8}, and KCu{sub 2}Nb{sub 0.53}Ta{sub 0.47}S{sub 4} have been prepared in polychalcogenide melts. The structures of these compounds base on discrete tetrahedra [MS{sub 4}]{sup 3-} (M=V/Ta), complex [M {sub 4}S{sub 22}]{sup 6-} and [M {sub 4}S{sub 25}]{sup 6-} anions comprised of two M {sub 2}S{sub 11} subunits bridged by a S{sub 2} or S{sub 3} chain, {sup 1} {sub {infinity}}[Cu{sub 3} M {sub 2}S{sub 8}]{sup 3-} anionic chains, and {sup 2} {sub {infinity}}[Cu{sub 2} MS{sub 4}]{sup -} (M=Nb/Ta) anionic layers formed by corner sharing and edge sharing between CuS{sub 4} and MS{sub 4} tetrahedra.« less
  • Two uranyl sulfate hydrates, (H3O)2[(UO2)2(SO4)3(H2O)]·7H2O (NDUS) and (H3O)2[(UO2)2(SO4)3(H2O)]·4H2O (NDUS1), and one uranyl selenate-selenite [C5H6N][(UO2)(SeO4)(HSeO3)] (NDUSe), were obtained and their crystal structures solved. NDUS and NDUSe result from reactions in highly acidic media in the presence of L-cystine at 373 K. NDUS crystallized in a closed vial at 278 K after 5 days and NDUSe in an open beaker at 278 K after 2 weeks. NDUS1 was synthesized from aqueous solution at room temperature over the course of a month. NDUS, NDUS1, and NDUSe crystallize in the monoclinic space group P21/n, a = 15.0249(4) Å,b = 9.9320(2) Å, c = 15.6518(4)more » Å, β = 112.778(1)°, V = 2153.52(9) Å3,Z = 4, the tetragonal space group P43212, a = 10.6111(2) Å,c = 31.644(1) Å, V = 3563.0(2) Å3, Z = 8, and in the monoclinic space group P21/n, a = 8.993(3) Å, b = 13.399(5) Å, c = 10.640(4) Å,β = 108.230(4)°, V = 1217.7(8) Å3, Z = 4, respectively.The structural units of NDUS and NDUS1 are two-dimensional uranyl sulfate sheets with a U/S ratio of 2/3. The structural unit of NDUSe is a two-dimensional uranyl selenate-selenite sheets with a U/Se ratio of 1/2. In-situ reaction of the L-cystine ligands gives two distinct products for the different acids used here. Where sulfuric acid is used, only H3O+ cations are located in the interlayer space, where they balance the charge of the sheets, whereas where selenic acid is used, interlayer C5H6N+ cations result from the cyclization of the carboxyl groups of L-cystine, balancing the charge of the sheets.« less
  • An experimental and theoretical study has been carried out of the temperature dependent noise and responsivity performance of n-type x = 0.32 Hg{sub 1{minus}x}Cd{sub x}Te photoconductors. The fundamental noise sources that ultimately limit the specific detectivity, D*{sub {lambda}}, at the three main temperatures of interest are identified and correlated with the experimental material parameters of the device. A device model is presented for the responsivity and noise voltage which takes into account surface effects such as surface recombination and accumulation layer shunting. For a given set of device and material parameters this model is well able to account for themore » observed experimental values of responsivity and noise voltage over the full temperature range from 80--300 K. Using a theoretical model, it is shown that under ideal conditions it is possible to achieve background limited performance at temperatures up to 210 K. Experimental results are presented for responsivity, noise voltage, semiconductor surface charge density and D*{sub {lambda}} for a frontside-illuminated Hg{sub 1{minus}x} Cd{sub x} Te photoconductive detector, as a function of temperature in the range 80--300 K. The devices were fabricated on Liquid Phase Epitaxially (LPE) grown n-type Hg{sub 0.68}Cd{sub 0.32}Te, and were passivated with anodic oxide/ZnS on the front side.« less