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Tin(IV) Chalcogenide Complexes: Single Source Precursors for SnS, SnSe and SnTe Nanoparticle Synthesis
Author(s) -
Thompson Joseph R.,
Ahmet Ibbi Y.,
Johnson Andrew L.,
KociokKöhn Gabriele
Publication year - 2016
Publication title -
european journal of inorganic chemistry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.667
H-Index - 136
eISSN - 1099-0682
pISSN - 1434-1948
DOI - 10.1002/ejic.201600790
Subject(s) - tin , chemistry , thermogravimetric analysis , chalcogenide , crystallography , nanoparticle , single crystal , powder diffraction , scanning electron microscope , spectroscopy , x ray crystallography , elemental analysis , diffraction , inorganic chemistry , nanotechnology , organic chemistry , materials science , physics , quantum mechanics , optics , composite material
A family of tin(IV) bis(hexamethylsilylamide) complexes 2 – 9 have been synthesized by reaction of [Sn{N(SiMe 3 ) 2 } 2 ] ( 1 ) with the diphenyl dichalcogenanes Ph 2 E 2 (E = S, Se, Te), the radical species TEMPO, or the group 16 elements to form the complexes [(PhE) 2 Sn{N(SiMe 3 ) 2 } 2 ] ( 2 – 4 ) and [(TEMPO) 2 Sn{N(SiMe 3 ) 2 } 2 ] ( 5 ), and [{(Me 3 Si) 2 N} 2 Sn(µ 2 ‐E)] 2 ( 6 – 9 ) (E = S, 2 & 6 ; E = Se 3 & 7 ; E = Te, 4 & 9 , E = O 2 , 9 ). The isolated tin complexes were characterized by elemental analysis, NMR spectroscopy, and the molecular structures of the complexes were determined by single crystal X‐ray diffraction. Thermogravimetric analysis showed complexes 2 – 4 and 6 – 8 all to have residual masses close to those expected for the formation of the corresponding “SnE” systems. Complexes 2 – 4 and 6 – 8 were also assessed for their utility in the formation of nanoparticles. The materials obtained were characterized by powder X‐ray diffraction (XRD), field emission scanning electron microscopy (FE‐SEM) and energy‐dispersive X‐ray analysis (EDX). Analysis showed formation of SnSe and SnTe from complexes 3 – 4 and 6 – 7 , respectively.