Abstract

The structures of the subnanometer clusters of CdS that form in zeolite Y (FAU), prepared as follows, have been determined. A single crystal of Cd2+-exchanged zeolite Y was prepared by the exchange of Na75–Y (|Na75|[Si117Al75O384]–Y with aqueous Cd(NO3)2 at 294 K, followed by vacuum dehydration at 723 K (crystal 1). A second crystal, similarly prepared, was exposed to 6.7 × 104 Pa of dry H2S(g) for 6 h at 294 K and evacuated (crystal 2). Their structures were determined crystallographically using synchrotron X-rays and were refined using all data to the final error indices (calculated using only Fo > 4σ(Fo)) of R1/wR2 = 0.040/0.156 and 0.049/0.186, respectively. In crystal 1, Cd2+ ions primarily occupy sites I and II. In crystal 2, |Cd27(Cd4S6+)0.6(Cd(SHCd)46+)0.9H12|[Si117Al75O384]–FAU, tetrahedral Cd4S6+ ions center about 7.5% of the sodalite cavities and tetrahedral Cd(SHCd)46+ ions center about 11% of the supercages. In Cd(SHCd)46+, a Cd2+ ion at the center of a supercage bonds tetrahedrally to four S...

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