Synthesis and characterization of ruthenium and rhodium sulfide thin films and nanoparticles

Abstract
The reaction of the metal salt (MClynH20) with the solution mixture of carbon disulfide (CS2), dialkylamine (R2NH) and sodium hydroxide (NaOH) yields a dithiocarbamate complex of formulation [M(S2CNR2)n], (M = Ru and Rh; R = alkyl group; n = 2 or 3). In this work, these complexes were synthesized and characterized, using such techniques as thermogravimetric analysis (TGA), infrared (IR), nuclear magnetic resonance (NMR), mass spectroscopy (MS) and elemental analysis. The complexes were then used as single-source molecular precursors for the synthesis of metal chalcogenide thin films and nanoparticles. The deposition of RI12S3 and RuS2 thin films was achieved by the decomposition of [Rh(S2CNEt2)2] and [Ru(S2CNEt2)3] dissolved in toluene using aerosol assisted chemical vapour deposition (AACVD) technique. The precursors gave good yields of high quality materials and pyrolyze cleanly to give the required films at reasonably high growth rates. Shiny, adherent thin films were deposited on glass substrates at 350-450 °C. The thin films were characterized using X-ray diffraction (XRD), UV-Vis absorption, ellipsometry, scanning electron microscopy (SEM) and energy dispersive X-ray analysis (EDAX). Metal chalcogenide nanoparticles were also synthesized using complexes [Ru(S2CNEt2)3] and [Rh(S2CNEt2}2] as single source molecular precursors. Both TOPO and HDA were used as capping agents for the nanoparticles. Materials of sizes up to 20 run were synthesized from the precursors. Characterization of the nanoparticles was done using UV-Vis absorption spectroscopy, TEM and photoluminescence (PL).
Description
Submitted to the Faculty of Science and Agriculture In fulfilment of the requirement for the award of the degree of Master of Science in the Department of Chemistry University of Zululand, South Africa, 2004.
Keywords
Platinum group, Nanoparticles, Ruthenium and rhodium
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