Heterometallic M/Mn (M=Cu, Co, Zn) acetate complexes as precursors for binary oxides

Journal Article · Mon Nov 15 00:00:00 EST 2010 · Journal of Solid State Chemistry

DOI:https://doi.org/10.1016/j.jssc.2010.08.040· OSTI ID:21504024

Khavryuchenko, Oleksiy V; Lisnyak, Vladyslav V; Kokozay, Vladimir N ^[1]; Dyakonenko, Viktoriya V ^[2]; Shishkin, Oleg V ^[2]; Skelton, Brian W ^[3]; Jezierska, Julia ^[4]

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1. Department of Inorganic Chemistry, Kyiv National Taras Shevchenko University, Volodymyrska street 64, Kyiv 01601 (Ukraine)
2. STC 'Institute for Single Crystals' National Academy of Sciences of Ukraine, 60 Lenina Avenue Kharkiv 61001 (Ukraine)
3. Chemistry M313, School of Biomedical, Biomolecular and Chemical Sciences, University of Western Australia, 6009 (Australia)
4. Faculty of Chemistry, University of Wroclaw, 14 F. Joliot-Curie, 50-383 Wroclaw (Poland)

A facile one-pot procedure, or so-called 'direct synthesis,' was used to prepare the novel heterometallic complexes [M{sub 2}Mn(OAc){sub 6}(bpy){sub 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{sub 2} and also by TPD mass-spectrometry in vacuo. 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. -- Graphical abstract: The novel heterometallic complexes [M{sub 2}Mn(OAc){sub 6}(bpy){sub 2}] (M=Cu, Co, Zn, bpy=2,2'-bipyridyl) were isolated and used as precursors for low-temperature synthesis of binary oxides. Single crystal X-ray diffraction, FTIR, TG/DTA/DTG, TPD-MS, PXRD, SEM/EDX analysis was performed on complexes and powders. Display Omitted

• OSTI ID: 21504024
• Journal Information: Journal of Solid State Chemistry, Vol. 183, Issue 11; Other Information: DOI: 10.1016/j.jssc.2010.08.040; PII: S0022-4596(10)00374-9; Copyright (c) 2010 Elsevier Science B.V., Amsterdam, The Netherlands, All rights reserved.; ISSN 0022-4596
• Country of Publication: United States
• Language: English

Related Subjects

37 INORGANIC
ORGANIC
PHYSICAL AND ANALYTICAL CHEMISTRY
ACETATES
CHROMIUM COMPLEXES
COBALT COMPLEXES
CRYSTALLOGRAPHY
DIFFERENTIAL THERMAL ANALYSIS
DISSOLUTION
FOURIER TRANSFORMATION
INFRARED SPECTRA
MANGANESE COMPLEXES
MASS SPECTROSCOPY
MICROANALYSIS
MICROSTRUCTURE
MONOCRYSTALS
MORPHOLOGY
OXIDATION
OXIDES
PRECURSOR
SCANNING ELECTRON MICROSCOPY
SYNTHESIS
THERMAL DEGRADATION
THERMAL GRAVIMETRIC ANALYSIS
X-RAY DIFFRACTION
ZINC COMPLEXES
CARBOXYLIC ACID SALTS
CHALCOGENIDES
CHEMICAL ANALYSIS
CHEMICAL REACTIONS
COHERENT SCATTERING
COMPLEXES
CRYSTALS
DIFFRACTION
ELECTRON MICROSCOPY
GRAVIMETRIC ANALYSIS
INTEGRAL TRANSFORMATIONS
MICROSCOPY
OXYGEN COMPOUNDS
QUANTITATIVE CHEMICAL ANALYSIS
SCATTERING
SPECTRA
SPECTROSCOPY
THERMAL ANALYSIS
TRANSFORMATIONS
TRANSITION ELEMENT COMPLEXES