Copper tellurolate clusters in trimethylsilylated MCM-41 — Preparation and condensation

Abstract

The copper tellurolate cluster [(Cu6(TePh)6(PEtPh2)5] (1) has been loaded into the pores of a trimethylsilylated MCM-41 (TMS–MCM-41) framework. Solutions of 1 in tetrahydrofuran lead to good impregnation weight % (~10 wt%, 1). The resulting material was analysed by powder X-ray diffraction (PXRD), nitrogen sorption isotherms, thermogravimetric analysis (TGA), energy dispersive X-ray (EDX) analysis, 31P CP MAS NMR spectroscopy, and transmission electron microscopy (TEM). It was observed that the loading process proceeds with the intact cluster 1 being present within the hexagonal architecture. The intact nature of 1 makes it an ideal candidate for condensation by photochemical or thermal means. Both of these condensation treatments increase the Cu:Te ratio of 1 to approach that observed in binary semiconductor Cu2Te. The condensation process was analysed by GC–MS spectrometry and characterization of the condensed, isolated composites was performed by TGA, EDX analysis, 31P CP MAS NMR spectroscopy, nitrogen adsorption, and TEM measurements. Thermal condensation results in the formation of Cu2Te particles, whereas photochemical condensation yields larger copper-tellurolate nanoclusters.Key words: copper, tellurium, cluster, MCM-41, trimethylsilylated, photolysis, thermolysis, Cu2Te, composite, mesoporous material.