Preparation, Characterization, and Condensation of Copper Tellurolate Clusters in the Pores of Periodic Mesoporous Silica MCM-41.
The Cu-tellurolate cluster [Cu6(TePh)6(PPh2Et)5] was loaded into the pores of MCM-41 by solid-state impregnation techniques. The best loading conditions are 110 Deg and 10-3 Torr static vacuum. The resulting material was analyzed by powder x-ray diffraction (PXRD), nitrogen adsorption isotherms, TGA, 31P CP MASNMR spectroscopy, and TEM. Loading is accompanied by loss of the phosphine shell, with retention of the Cu-Te core. Condensation of the impregnated material may proceed thermally or photochem. Thermal condensation gave Cu2Te nanoparticles as demonstrated by PXRD, and TEM data suggests that the process has taken place inside the pores of MCM-41. Photochem. condensation yields larger metal-chalcogen clusters in the pores as suggested by the result of UV-visible diffuse reflectance spectroscopy and TEM measurements.
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