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Title: Synthesis and characterization of K(In{sub 6.5}Ag{sub 6.5})

Abstract

The pseudo-ternary compound K(In{sub 6.5}Ag{sub 6.5}) has been synthesized from the elements and either excess indium or excess indium and silver. Single-crystal X-ray diffraction shows that K(In{sub 6.5}Ag{sub 6.5}) crystallizes in the cubic space group Fm3-bar c, a=13.5101(6)A(Z=8), and adopts the NaZn{sub 13} structure type (R{sub 1}=0.0338). Four probe resistivity measurements show K(In{sub 6.5}Ag{sub 6.5}) to be a metal with a room temperature resistivity of 81{mu}{omega}cm and a weak temperature dependence.

Authors:
 [1];  [2];  [3]
  1. Department of Chemistry and Chemical Biology, Cornell University, Ithaca, NY 14853 (United States)
  2. Department of Physics, Cornell University, Ithaca, NY 14853 (United States)
  3. Department of Chemistry and Chemical Biology, Cornell University, Ithaca, NY 14853 (United States). E-mail: fjd3@cornell.edu
Publication Date:
OSTI Identifier:
20784789
Resource Type:
Journal Article
Resource Relation:
Journal Name: Journal of Solid State Chemistry; Journal Volume: 178; Journal Issue: 11; Other Information: DOI: 10.1016/j.jssc.2005.09.004; PII: S0022-4596(05)00405-6; Copyright (c) 2005 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:
37 INORGANIC, ORGANIC, PHYSICAL AND ANALYTICAL CHEMISTRY; CUBIC LATTICES; ELECTRIC CONDUCTIVITY; INDIUM; INDIUM COMPOUNDS; MONOCRYSTALS; POTASSIUM COMPOUNDS; SILVER; SILVER COMPOUNDS; SPACE GROUPS; SYNTHESIS; TEMPERATURE DEPENDENCE; TEMPERATURE RANGE 0273-0400 K; X-RAY DIFFRACTION

Citation Formats

Bailey, Mark S., McGuire, Michael A., and DiSalvo, Francis J. Synthesis and characterization of K(In{sub 6.5}Ag{sub 6.5}). United States: N. p., 2005. Web. doi:10.1016/j.jssc.2005.09.004.
Bailey, Mark S., McGuire, Michael A., & DiSalvo, Francis J. Synthesis and characterization of K(In{sub 6.5}Ag{sub 6.5}). United States. doi:10.1016/j.jssc.2005.09.004.
Bailey, Mark S., McGuire, Michael A., and DiSalvo, Francis J. Tue . "Synthesis and characterization of K(In{sub 6.5}Ag{sub 6.5})". United States. doi:10.1016/j.jssc.2005.09.004.
@article{osti_20784789,
title = {Synthesis and characterization of K(In{sub 6.5}Ag{sub 6.5})},
author = {Bailey, Mark S. and McGuire, Michael A. and DiSalvo, Francis J.},
abstractNote = {The pseudo-ternary compound K(In{sub 6.5}Ag{sub 6.5}) has been synthesized from the elements and either excess indium or excess indium and silver. Single-crystal X-ray diffraction shows that K(In{sub 6.5}Ag{sub 6.5}) crystallizes in the cubic space group Fm3-bar c, a=13.5101(6)A(Z=8), and adopts the NaZn{sub 13} structure type (R{sub 1}=0.0338). Four probe resistivity measurements show K(In{sub 6.5}Ag{sub 6.5}) to be a metal with a room temperature resistivity of 81{mu}{omega}cm and a weak temperature dependence.},
doi = {10.1016/j.jssc.2005.09.004},
journal = {Journal of Solid State Chemistry},
number = 11,
volume = 178,
place = {United States},
year = {Tue Nov 15 00:00:00 EST 2005},
month = {Tue Nov 15 00:00:00 EST 2005}
}
  • Chemical preparation and reactions of silver salts of M(OTeF{sub 5}){sub 6}{sup {minus}} (M = Nb, Sb), and M{prime}(OTeF{sub 5}){sub 6}{sup {minus}} (M{prime} = Ti, Zr, Hf) were reported. The silver salts were converted to CPh{sub 3}{sup +} or N(n-Bu){sub 4}{sup +} salts. Ag{sub 2}Ti(OTeF{sub 5}){sub 6}, AgNb(OTeF{sub 5}){sub 6}, and AgSb(OTeF{sub 5}){sub 6} were recrystallized in dihaloalkane solvents yielding crystals containing solvent molecules which were subsequently characterized by X-ray crystallography. Reactivity of the anions toward other compounds was investigated.
  • Highlights: • The plasmatic Ag@AgCl surface-sensitized K{sub 2}Ti{sub 4}O{sub 9} composite photocatalysts. • Ag@AgCl greatly increased visible light absorption for K{sub 2}Ti{sub 4}O{sub 9}. • The photocatalysts exhibited enhanced photocatalytic dye degradation. - Abstract: Nano-sized plasmonic Ag@AgCl surface-sensitized K{sub 2}Ti{sub 4}O{sub 9} composite photocatalysts (hereafter designated as Ag@AgCl/K{sub 2}Ti{sub 4}O{sub 9}) was synthesized via a facile oil-in-water self-assembly method. The photocatalytic activity of the prepared materials for RhB (Rhodamine B) degradation was examined under visible light irradiation. The results reveal that the size of Ag@AgCl, which evenly dispersed on the surface of K{sub 2}Ti{sub 4}O{sub 9}, distributes about 20–50 nm.more » The UV–vis diffuse reflectance spectra indicate that Ag@AgCl/K{sub 2}Ti{sub 4}O{sub 9} samples have a significantly enhanced optical absorption in 380–700 nm. The photocatalytic activities of the Ag@AgCl/K{sub 2}Ti{sub 4}O{sub 9} samples increase first and then decrease with increasing amount of loading Ag@AgCl and the Ag@AgCl(20 wt.%)/K{sub 2}Ti{sub 4}O{sub 9} sample exhibits the best photocatalytic activity and 94.47% RhB was degraded after irradiation for 2 h. Additionally, studies performed using radical scavengers indicated that O{sub 2}·{sup −} and Cl{sup 0} acted as the main reactive species. The electronic interaction was systematically studied and confirmed by the photo-electrochemical measurements.« less
  • Silver complexes of the anionic forms of 2-(diphenylphosphino)benzenethiol [2-(Ph{sub 2}P)C{sub 6}H{sub 4}SH] (1) 2-(diphenylphosphino)-6-(trimethylsilyl)benzenethiol [2-(Ph{sub 2}P)-6-(Me{sub 3}Si)C{sub 6}H{sub 3}SH] (2), and 2-(diphenylphosphinyl)-6-(trimethylsilyl)benzenethiol [2-(Ph{sub 2}PO)-6-(Me{sub 3}Si)C{sub 6}H{sub 3}SH] (3) have been prepared by an electrochemical procedure and characterized by spectroscopic (IR, {sup 1}H, {sup 13}C, and {sup 31}P NMR) methods, and ligand 3 and [Ag{sub 4}{l_brace}2-(Ph{sub 2}P)-6-(Me{sub 3}Si)C{sub 6}H{sub 3}S{r_brace}{sub 4}] (5) and [Ag{sub 4}{l_brace}2-(Ph{sub 2}PO)-6-(Me{sub 3}Si)C{sub 6}H{sub 3}S{r_brace}{sub 4}] (6) complexes were characterized by X-ray crystallographic techniques. The (5) compound is tetranuclear with an array of four silver atoms bridged by four sulfur atoms. Each silver atom has a distortedmore » trigonal [AgS{sub 2}P] environment with each ligand acting as P,S bidentate S-bridging ligand. The (6) complex is also tetranuclear, but in this case two of the silver atoms are [AgO{sub 2}S{sub 2}] tetracoordinated and the other two Ag atoms are [AgS{sub 2}] two coordinated.« less
  • K{sub 3}InF{sub 6} is synthesized by a sol-gel route starting from indium and potassium acetates dissolved in isopropanol in the stoichiometry 1:3, with trifluoroacetic acid as fluorinating agent. The crystal structures of the organic precursors were solved by X-ray diffraction methods on single crystals. Three organic compounds were isolated and identified: K{sub 2}InC{sub 10}O{sub 10}H{sub 6}F{sub 9}, K{sub 3}InC{sub 12}O{sub 14}H{sub 4}F{sub 18} and K{sub 3}InC{sub 12}O{sub 12}F{sub 18}. The first one, deficient in potassium in comparison with the initial stoichiometry, is unstable. In its crystal structure, acetate as well as trifluoroacetate anions are coordinated to the indium atom. Themore » two other precursors are obtained, respectively, by quick and slow evaporation of the solution. They correspond to the final organic compounds, which give K{sub 3}InF{sub 6} by decomposition at high temperature. The crystal structure of K{sub 3}InC{sub 12}O{sub 14}H{sub 4}F{sub 18} is characterized by complex anions [In(CF{sub 3}COO){sub 4}(OH{sub x}){sub 2}]{sup (5-2x)-} and isolated [CF{sub 3}COOH{sub 2-x}]{sup (x-1)-} molecules with x=2 or 1, surrounded by K{sup +} cations. The crystal structure of K{sub 3}InC{sub 12}O{sub 12}F{sub 18} is only constituted by complex anions [In(CF{sub 3}COO){sub 6}]{sup 3-} and K{sup +} cations. For all these compounds, potassium cations ensure only the electroneutrality of the structure. IR spectra of K{sub 2}InC{sub 10}O{sub 10}H{sub 6}F{sub 9} and K{sub 3}InC{sub 12}O{sub 12}F{sub 18} were also performed at room temperature on pulverized crystals.« less
  • The phase relations in the cross-section of the K{sub 2}W{sub 2}O{sub 7}-K{sub 2}WO{sub 4}-KPO{sub 3} containing 15 mol% Bi{sub 2}O{sub 3} were undertaken using flux method. Crystallization fields of K{sub 6.5}Bi{sub 2.5}W{sub 4}P{sub 6}O{sub 34}, K{sub 2}Bi(PO{sub 4})(WO{sub 4}), Bi{sub 2}WO{sub 6}, KBi(WO{sub 4}){sub 2} and their cocrystallization areas were identified. Novel phase K{sub 6.5}Bi{sub 2.5}W{sub 4}P{sub 6}O{sub 34} was characterized by single-crystal X-ray diffraction: sp. gr. P-1, a=9.4170(5), b=9.7166(4), c=17.6050(7) A, {alpha}=90.052(5){sup o}, {beta}=103.880(5){sup o} and {gamma}=90.125(5){sup o}. It has a layered structure, which contains {l_brace}K{sub 7}Bi{sub 5}W{sub 8}P{sub 12}O{sub 68}{r_brace}{sub {infinity}} layers stacked parallel to ab plane andmore » sheets composed by potassium atoms separating these layers. Sandwich-like {l_brace}K{sub 7}Bi{sub 5}W{sub 8}P{sub 12}O{sub 68}{r_brace}{sub {infinity}} layers are assembled from [W{sub 2}P{sub 2}O{sub 13}]{sub {infinity}} and [BiPO{sub 4}]{sub {infinity}} building units, and are penetrated by tunnels with K/Bi atoms inside. FTIR-spectra of K{sub 2}Bi(PO{sub 4})(WO{sub 4}) and K{sub 6.5}Bi{sub 2.5}W{sub 4}P{sub 6}O{sub 34} were discussed on the basis of factor group theory. - Graphical abstract: Sandwich-like architecture of K{sub 6.5}Bi{sub 2.5}W{sub 4}P{sub 6}O{sub 34} prepared during high-temperature investigation of K{sub 2}W{sub 2}O{sub 7}-K{sub 2}WO{sub 4}-KPO{sub 3} system. It is organized from {l_brace}K{sub 7}Bi{sub 5}W{sub 8}P{sub 12}O{sub 68}{r_brace}{sub {infinity}} layers and potassium atom sheets.« less