摘要:
A facile one-pot procedure, or so-called "direct synthesis," was used to prepare the novel heterometallic complexes [M(2)Mn(OAc)(6)(bpy)(2)], where M=Cu (1), Co (2), Zn (3), bpy=2,2'-bipyridyl, with high yields via oxidative dissolution of pure metals in a liquid phase. The complexes were characterized by an elemental analysis, single crystal X-ray diffraction method and FTIR. These complexes are proposed as precursors, whose thermal degradation may lead to the formation of solids possessing nano- to microsize levels of dispersity. The thermal behavior of the complexes obtained was studied by thermal analysis (TG/DTA/DTG) in both air and N(2) and also by TPD mass-spectrometry in vacua. The FTIR, X-ray powder diffraction (PXRD) and thermoanalytical data were used for the identification of the solid products of thermal degradation. The morphology and microstructure of the solid residues were analyzed, using scanning electron microscopy with energy dispersive X-ray microanalysis (SEM/EDX) at mkm and sub-micro levels. (C) 2010 Elsevier Inc. All rights reserved.