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

✍ Scribed by Joy Heising; François Bonhomme; Mercouri G. Kanatzidis

• Publisher: Elsevier Science
• Year: 1998
• Tongue: English
• Weight: 295 KB
• Volume: 139
• Category: Article
• ISSN: 0022-4596
• DOI: 10.1006/jssc.1998.7783

✦ Synopsis

The synthesis of [Al 13 O 4 (OH) 24 (H 2 O) 12 ] x MS 2 (x ‫؍‬ 0.02-0.05, M ‫؍‬ Mo; x ‫؍‬ 0.02-0.055, M ‫؍‬ W) was accomplished by a precipitative encapsulation technique using single layers of MS 2 . The products were characterized by powder X-ray diffraction, energy dispersive spectroscopy (EDS), thermal gravimetric analysis (TGA), 27 Al MAS-NMR, room temperature electrical conductivity measurements, and surface area measurements. Powder X-ray diffraction patterns show an expansion of approximately 9.9 A s . 27 Al MAS-NMR indicates that the cluster is intact between the MS 2 layers. One-dimensional electron density mapping and Rietveld refinement performed on the powder diffraction data show that the cluster is oriented with its C 3 symmetry 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.