Heterocyclic Bismuth(III) Dithiocarbamato Complexes as Single-Source Precursors for the Synthesis of Anisotropic Bi sub(2)S sub(3) Nanoparticles
New complexes catena-( mu sub(2)-nitrato-O,O')bis(piperidinedithiocar bamato)bismuth(III) (1) and tetrakis( mu -nitrato)tetrakis[bis(tetrahydroquinolinedithiocar bamato)bismuth(III)] (2) were synthesised and characterised by elemental analysis, FTIR spectroscopy and thermogravimetric analysis....
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Veröffentlicht in: | Chemistry : a European journal 2016-09, Vol.22 (37), p.13127-13135 |
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Zusammenfassung: | New complexes catena-( mu sub(2)-nitrato-O,O')bis(piperidinedithiocar bamato)bismuth(III) (1) and tetrakis( mu -nitrato)tetrakis[bis(tetrahydroquinolinedithiocar bamato)bismuth(III)] (2) were synthesised and characterised by elemental analysis, FTIR spectroscopy and thermogravimetric analysis. The single-crystal X-ray structures of 1 and 2 were determined. The coordination numbers of the Bi super(III) ion are 8 for 1 and greater than or equal to 6 for 2 when the experimental electron density for the nominal 6s super(2) lone pair of electrons is included. Both complexes were used as single-source precursors for the synthesis of dodecylamine-, hexadecylamine-, oleylamine and tri-n-octylphosphine oxide-capped Bi sub(2)S sub(3) nanoparticles at different temperatures. UV/Vis spectra showed a blueshift in the absorbance band edge characteristic of a quantum size effect. High-quality, crystalline, long and short Bi sub(2)S sub(3) nanorods were obtained depending on the thermolysis temperature, which was varied from 190 to 270 degree C. A general trend of increasing particle breadth with increasing reaction temperature and increasing length of the carbon chain of the amine (capping agent) was observed. Powder XRD patterns revealed the orthorhombic crystal structure of Bi sub(2)S sub(3). Bismuth sulfide nanorods: Two bismuth(III) dithiocarbamato complexes were synthesised and characterised by elemental analysis, FTIR spectroscopy, thermogravimetric analysis and single-crystal XRD. Both complexes were used as single-source precursors for the synthesis of capped Bi sub(2)S sub(3) nanoparticles at different temperatures. High-quality, crystalline, long and short Bi sub(2)S sub(3) nanorods were obtained (see figure) depending on the thermolysis temperature, which was varied from 190 to 270 degree C. |
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ISSN: | 0947-6539 1521-3765 |
DOI: | 10.1002/chem.201602106 |