Toward Pillared Metal Sulfides

Encapsulation and Rietveld Structural Characterization of the Al13O4(OH)24(H2O)7+ 12Cluster into MoS2and WS2

Joy Heising, François Bonhomme, Mercouri G Kanatzidis

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27 Citations (Scopus)

Abstract

The synthesis of [Al13O4(OH)24(H2O) 12]xMS2(x=0.02-0.05,M=Mo;x=0.02-0.055,M=W) was accomplished by a precipitative encapsulation technique using single layers ofMS2. The products were characterized by powder X-ray diffraction, energy dispersive spectroscopy (EDS), thermal gravimetric analysis (TGA),27Al MAS-NMR, room temperature electrical conductivity measurements, and surface area measurements. Powder X-ray diffraction patterns show an expansion of approximately 9.9 Å.27Al MAS-NMR indicates that the cluster is intact between theMS2layers. One-dimensional electron density mapping and Rietveld refinement performed on the powder diffraction data show that the cluster is oriented with its C3symmetry axis perpendicular to the layers. The samples exhibit conductivity values from 3 to 14 S/cm. TGA shows that the cluster is completely stable to 100°C, and largely stable to 330°C. Surface area measurements suggest that the space between the clusters is not accessible.

Original languageEnglish
Pages (from-to)22-26
Number of pages5
JournalJournal of Solid State Chemistry
Volume139
Issue number1
DOIs
Publication statusPublished - Aug 1998

Fingerprint

Sulfides
Encapsulation
sulfides
Gravimetric analysis
Metals
Nuclear magnetic resonance
metals
thermal analysis
Rietveld refinement
X ray powder diffraction
Diffraction patterns
nuclear magnetic resonance
Carrier concentration
Energy dispersive spectroscopy
diffraction
Powders
X rays
x rays
diffraction patterns
conductivity

ASJC Scopus subject areas

  • Inorganic Chemistry
  • Physical and Theoretical Chemistry
  • Materials Chemistry

Cite this

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title = "Toward Pillared Metal Sulfides: Encapsulation and Rietveld Structural Characterization of the Al13O4(OH)24(H2O)7+ 12Cluster into MoS2and WS2",
abstract = "The synthesis of [Al13O4(OH)24(H2O) 12]xMS2(x=0.02-0.05,M=Mo;x=0.02-0.055,M=W) was accomplished by a precipitative encapsulation technique using single layers ofMS2. The products were characterized by powder X-ray diffraction, energy dispersive spectroscopy (EDS), thermal gravimetric analysis (TGA),27Al MAS-NMR, room temperature electrical conductivity measurements, and surface area measurements. Powder X-ray diffraction patterns show an expansion of approximately 9.9 {\AA}.27Al MAS-NMR indicates that the cluster is intact between theMS2layers. One-dimensional electron density mapping and Rietveld refinement performed on the powder diffraction data show that the cluster is oriented with its C3symmetry axis perpendicular to the layers. The samples exhibit conductivity values from 3 to 14 S/cm. TGA shows that the cluster is completely stable to 100°C, and largely stable to 330°C. Surface area measurements suggest that the space between the clusters is not accessible.",
author = "Joy Heising and Fran{\cc}ois Bonhomme and Kanatzidis, {Mercouri G}",
year = "1998",
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journal = "Journal of Solid State Chemistry",
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T2 - Encapsulation and Rietveld Structural Characterization of the Al13O4(OH)24(H2O)7+ 12Cluster into MoS2and WS2

AU - Heising, Joy

AU - Bonhomme, François

AU - Kanatzidis, Mercouri G

PY - 1998/8

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N2 - The synthesis of [Al13O4(OH)24(H2O) 12]xMS2(x=0.02-0.05,M=Mo;x=0.02-0.055,M=W) was accomplished by a precipitative encapsulation technique using single layers ofMS2. The products were characterized by powder X-ray diffraction, energy dispersive spectroscopy (EDS), thermal gravimetric analysis (TGA),27Al MAS-NMR, room temperature electrical conductivity measurements, and surface area measurements. Powder X-ray diffraction patterns show an expansion of approximately 9.9 Å.27Al MAS-NMR indicates that the cluster is intact between theMS2layers. One-dimensional electron density mapping and Rietveld refinement performed on the powder diffraction data show that the cluster is oriented with its C3symmetry axis perpendicular to the layers. The samples exhibit conductivity values from 3 to 14 S/cm. TGA shows that the cluster is completely stable to 100°C, and largely stable to 330°C. Surface area measurements suggest that the space between the clusters is not accessible.

AB - The synthesis of [Al13O4(OH)24(H2O) 12]xMS2(x=0.02-0.05,M=Mo;x=0.02-0.055,M=W) was accomplished by a precipitative encapsulation technique using single layers ofMS2. The products were characterized by powder X-ray diffraction, energy dispersive spectroscopy (EDS), thermal gravimetric analysis (TGA),27Al MAS-NMR, room temperature electrical conductivity measurements, and surface area measurements. Powder X-ray diffraction patterns show an expansion of approximately 9.9 Å.27Al MAS-NMR indicates that the cluster is intact between theMS2layers. One-dimensional electron density mapping and Rietveld refinement performed on the powder diffraction data show that the cluster is oriented with its C3symmetry axis perpendicular to the layers. The samples exhibit conductivity values from 3 to 14 S/cm. TGA shows that the cluster is completely stable to 100°C, and largely stable to 330°C. Surface area measurements suggest that the space between the clusters is not accessible.

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