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DOI: 10.1039/A804066D (Paper) Reference Section for: J. Mater. Chem., 1999, 9, 519-523

Thermal decomposition of [M3(CO)12] (M=Ru, Os) physisorbed onto porous Vycor glass: a route to a glass/RuO2 nanocomposite

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Aldo J. G. Zarbin, Maria D. Vargas and Oswaldo L. Alves

Abstract

This paper reports the preparation and characterization of oxide/glass nanocomposites, obtained by the impregnation and thermal decomposition of the trinuclear metal carbonyl clusters [M3(CO)12] (M=Ru, Os) inside the pores of porous Vycor glass (PVG). The intermediate species formed during the thermal treatment of the [M3(CO)12] adsorbed PVG materials were studied by UV-VIS-NIR and diffuse reflectance infrared (DR-IR) spectroscopy. At 65[thin space (1/6-em)]°C (M=Ru) and 110[thin space (1/6-em)]°C (M=Os), formation of surface bound [HM3(CO)10(µ-OSi}}n3)] species occurs, as a result of oxidative addition of a PVG surface silanol group to a cluster M-M bond. At T>130[thin space (1/6-em)]°C (M=Ru) and T[thin space (1/6-em)]>200[thin space (1/6-em)]°C (M=Os) cluster breakdown is observed, with formation of [M(CO)n(OSi}}n3)2] (n=2 and/or 3) species. When [Ru3(CO)12] incorporated PVG is heated in air at T[thin space (1/6-em)]>250[thin space (1/6-em)]°C, decomposition of the cluster and formation of RuO2 nanoparticles are observed. At 1200[thin space (1/6-em)]°C, collapse of the glass pores leads to the formation of a transparent silica glass/RuO2 nanocomposite of particle average size 45 Å.

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