Synthesis and characterization of organotin(IV) semicarbazones: potential precursors for nanosized tin oxide

A series of organotin(IV) semicarbazone adducts of the type R 2 SnCl 2 ·nLH ( 1 – 6 ) were synthesized by the reactions of R 2 SnCl 2 with newly synthesized carvone semicarbazone (LH) in anhydrous ethanol [where R = CH 3 , n  = 1 ( 1 ), 2 ( 2 ); R = C 4 H 9 , n  = 1 ( 3 ), 2 ( 4 ); and R = C 6 H 5 ,...

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Veröffentlicht in:Journal of sol-gel science and technology 2016-07, Vol.79 (1), p.114-121
Hauptverfasser: Atal, Mukesh Kumar, Sharma, Renu, Saini, Ajay, Dhayal, Veena, Nagar, Meena
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Sprache:eng
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Zusammenfassung:A series of organotin(IV) semicarbazone adducts of the type R 2 SnCl 2 ·nLH ( 1 – 6 ) were synthesized by the reactions of R 2 SnCl 2 with newly synthesized carvone semicarbazone (LH) in anhydrous ethanol [where R = CH 3 , n  = 1 ( 1 ), 2 ( 2 ); R = C 4 H 9 , n  = 1 ( 3 ), 2 ( 4 ); and R = C 6 H 5 , n  = 1 ( 5 ), 2 ( 6 )]. All the compounds have been characterized by elemental analyses, FT-IR, NMR ( 1 H, 13 C, 119 Sn) and FAB mass spectral studies. 119 Sn NMR studies suggest monodentate mode of attachment of the ligand with central tin atom in the solution state. Thermogravimetric study of ( 6 ) shows large thermal events. Transformations of ( 4 ) and ( 6 ) to pure tin oxides ( i and ii , respectively) have been carried out using sol–gel technique. Powder XRD patterns of the formed tin oxides indicate the formation of tetragonal cassiterite structure. SEM images of ( i ) and ( ii ) show wire- and grain-like morphologies of the crystallites, respectively. Graphical Abstract A series of organotin(IV) semicarbazone adducts were synthesized by the reactions of diorganotin dichloride with newly synthesized carvone semicarbazone. Transformations of some of the newly synthesized adducts to pure tin oxides have been carried out using sol–gel technique. Powder XRD patterns of the formed tin oxides indicate the formation of tetragonal cassiterite structure, while SEM images show wire- and grain-like morphologies.
ISSN:0928-0707
1573-4846
DOI:10.1007/s10971-016-4013-4