Abstract
Thermal decomposition of diorganotin(IV) derivatives of macrocycles of general formula, R2Sn(L1) and R2Sn(L2) (where R = n-butyl (1/4), methyl (2/5), and phenyl (3/6); H2L1 = 5,12-dioxa-7,14-dimethyl-1,4,8,11-tetraazacyclotetradeca-1,8-diene and H2L2 = 6,14-dioxa-8,16-dimethyl-1,5,9,13-tetraazacyclotetradeca-1,9-diene), provides a simple route to prepare nanometric SnO2 particles. X-ray line broadening shows that the particle size varies in the range of 36–57 nm. The particle size of SnO2 obtained by pyrolysis of 3 and 5 is in the range of 5–20 nm as determined by transmission electron microscope (TEM). The surface morphology of SnO2 particles was determined by scanning electron microscopy (SEM). Mathematical analysis of thermogravimetric analysis (TGA) data shows that the first step of decomposition of compound 4 follows first-order kinetics. The energy of activation (), preexponential factor (A), entropy of activation (), free energy of activation (), and enthalpy of activation () of the first step of decomposition have also been calculated. Me2Sn(L2) and Ph2Sn(L1) are the best precursors among the studied diorganotin(IV) derivatives of macrocycles for the production of nanometric SnO2.
Highlights
In recent years nanometric SnO2 is of current interest because of its semiconducting, optical, and electronic properties
A considerable attention has been given to the thermal decomposition of organometallic compounds in the last few years because they decompose at low temperature producing metallic oxides/sulfides and metallic particles
We report a simple route to prepare SnO2 semiconducting nanoparticles by the thermal decomposition of diorganotin(IV) derivatives of 5,12-dioxa7,14-dimethyl-1,4,8,11-tetraazacyclotetradeca-1,8-diene and
Summary
In recent years nanometric SnO2 is of current interest because of its semiconducting, optical, and electronic properties. It is important to mention that there is only a single reference recently reported by us in which some organotin-macrocyclic complexes are used as single source precursors for preparation of nanometric SnO2 through their pyrolysis route [21]. It is, worth investigating to explore the best precursors which would produce pure phase, nanosized SnO2 on thermal decomposition. The residues (SnO2) obtained were characterized by infrared (IR), X-ray diffraction analysis (XRD), scanning electron microscopy (SEM), field emission scanning electron microscopy in combination with energy-dispersive X-ray spectrometry (FESEM-EDX), and transmission electron microscopy with electron diffraction analysis (TEMED)
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