The development of cost-effective and easily accessible bifunctional materials, which can be effectively used for energy storage and energy generation, is highly desirable. Herein, a new molecular precursor [tris(morpholinodithiocarbamato)Co (III)] has been synthesized and the X-ray crystal structure of the complex determined. The precursor was used to prepare oleylamine (OLA)-capped cobalt sulfide nanoplatelets, using a facile hot injection method at two different temperatures (200°C and 260°C). The characterization of the samples shows that CoS synthesized at 200°C is slightly sulfur rich, whereas CoS synthesized at 260°C is slightly cobalt rich. The effect of off-stoichiometry of CoS nanoplatelets on the energy gener-ation and storage applications was studied. The oxygen evolution reaction catalytic performance of both samples indicate overpotentials of 307 and 276 mV as well as Tafel slopes of 96 and 82 mV/dec, respectively. Similarly, overpotentials of 132 and 153 mV were observed for the hydrogen evolution reaction, with Tafel slopes of 159 and 154 mV/dec, respectively. The capacitive behavior of the samples was also examined, and specific capacitance values of 298 and 440 F/g were obtained with cycling stabilities of 73 and 97 %, after 5000 cycles, respectively. The results indicate that sulfur-deficient CoS can show superior performance for efficient energy generation and storage devices.[a] C.
The synthesis and single-crystal X-ray structure of bis(piperidinedithiocarbamato)pyridinecadmium(II), [Cd(S 2 C(NC 5 H 10 )) 2 (NC 5 H 5 )] are reported and its use as a precursor for the synthesis of hexagonal CdS nanoparticles and CdS thin films is presented. Thermogravimetric analysis (TGA) of this complex showed clean decomposition in two steps to give CdS. Thermolysis of the complex in hexadecylamine at different temperatures in the range 190-270 1C gave CdS nanostructures including nanorods and oval shaped particles.The band gap of the as-synthesized CdS nanoparticles varied as the temperature was increased. CdS thin films with optical direct band gaps of ca. 2.4 eV were deposited by aerosol-assisted chemical vapour deposition (AACVD) in the temperature range 350 to 450 1C using the same precursor. Powder X-ray diffraction (p-XRD) patterns of CdS nanoparticles and thin films confirmed the hexagonal phase of CdS.
Tris-(piperidinedithiocarbamato)iron(III) (1) and tris-(tetrahydroquinolinedithiocarbamato)iron(iii) (2) complexes have been synthesized and their single-crystal X-ray structures were determined. Thermogravimetric analysis (TGA) of the complexes showed decomposition to iron sulfide. Both complexes were then used as single-source precursors for the deposition of iron sulfide thin films by aerosol-assisted chemical vapour deposition (AACVD). Energy-dispersive X-ray (EDX) spectroscopy confirmed the formation of iron sulfide films. The addition of tert-butyl thiol almost doubled the sulfur content in the deposited films. Scanning electron microscopy (SEM) images of the iron sulfide films from both complexes showed flakes/leaves/sheets, spherical granules and nanofibres. The sizes and shapes of these crystallites depended on the nature of the precursor, temperature, solvent and the amount of tert-butyl thiol used. The observed optical properties are dependent upon the variation of reaction parameters such as temperature and solvent. Powder X-ray diffraction (p-XRD) studies revealed that pyrrhotite, hexagonal (Fe0.975S), marcasite and smythite (Fe3S4) phases were differently deposited.
New complexes catena-(μ2 -nitrato-O,O')bis(piperidinedithiocarbamato)bismuth(III) (1) and tetrakis(μ-nitrato)tetrakis[bis(tetrahydroquinolinedithiocarbamato)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(III) ion are 8 for 1 and ≥6 for 2 when the experimental electron density for the nominal 6s(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 Bi2 S3 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 Bi2 S3 nanorods were obtained depending on the thermolysis temperature, which was varied from 190 to 270 °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 Bi2 S3 .
Cadmium(II) thiosemicarbazone complexes were prepared and characterized by elemental analysis and IR and NMR spectroscopy. The complexes were then investigated as potential single‐source precursors for the synthesis of oleylamine‐capped cadmium sulfide nanoparticles by solvothermal decomposition. The resulting nanomaterials were characterized by powder XRD, TEM, HRTEM, energy‐dispersive X‐ray analysis, and UV/Vis spectroscopy. Peak broadening in the XRD patterns confirmed the presence of relatively small hexagonal CdS nanocrystals. The TEM studies evidenced that the chlorido precursors produced CdS nanostructures whose morphologies differed from those obtained from the iodido precursors. CdS nanoparticles in the form of cubes/spheres/rods and nanodendrite structures were obtained from CdCl2 and CdI2 thiosemicarbazone complexes, respectively. The UV/Vis spectra revealed that the as‐synthesized CdS nanoparticles exhibited a quantum effect due to their sharp band edges, which are blueshifted relative to those of bulk CdS. The size, morphology and shape of the nanoparticles were also shown to depend on the temperature of formation.
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