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Surfactant-controlled composition and crystal structure of manganese(II) sulfide nanocrystals prepared by solvothermal synthesis.

ABSTRACT: We investigated how the outcome of the solvothermal synthesis of manganese(II) sulfide (MnS) nanocrystals (NCs) is affected by the type and amount of long chain surfactant present in the reaction mixture. Prompted by a previous observation that a larger than stoichiometric amount of sulfur is required [Puglisi, A.; Mondini, S.; Cenedese, S.; Ferretti, A. M.; Santo, N.; Ponti A. Chem. Mater. 2010, 22, 2804-2813], we carried out a wide set of reactions using Mn(II) carboxylates and Mn2(CO)10 as precursors with varying amounts of sulfur and carboxylic acid. MnS NCs were obtained provided that the S/Mn ratio was larger than the L/Mn ratio, otherwise MnO NCs were produced. Since MnS can crystallize in three distinct phases (rock salt ?-MnS, zincblende ?-MnS, and wurtzite ?-MnS), we also investigated whether the surfactant affected the NC polymorphism. We found that MnS polymorphism can be controlled by appropriate selection of the surfactant. ?-MnS nanocrystals formed when a 1:2 mixture of long chain carboxylic acid and amine was used, irrespective of the presence of carboxylic acid as a free surfactant or ligand in the metal precursor. When we used a single surfactant (carboxylic acid, alcohol, thiol, amine), ?-MnS nanocrystals were obtained. The peculiar role of the amine seems to be related to its basicity. The nanocrystals were characterized by TEM and electron diffraction; ATR-FTIR spectroscopy provided information about the surfactants adsorbed on the NCs.

SUBMITTER: Capetti E

PROVIDER: S-EPMC4685872 | biostudies-literature | 2015

REPOSITORIES: biostudies-literature

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Project description:We report the preparation and crystal structures of bis(diallydithiocarbamato)zinc(II) and silver(I) complexes. The compounds were used as single-source precursors to prepare zinc sulfide and silver sulfide nanophotocatalysts. The molecular structure of bis(diallydithiocarbamato)zinc(II) consists of a dimeric complex in which each zinc(II) ion asymmetrically coordinates with two diallydithiocarbamato anions in a bidentate chelating mode, and the centrosymmetrically related molecule is bridged through the S-atom that is chelated to the adjacent zinc(II) ion to form a distorted trigonal bipyramidal geometry around the zinc(II) ions. The molecular structure of bis(diallydithiocarbamato)silver(I) formed a cluster complex consisting of a trimetric Ag3S3 molecule in which the diallydithiocarbamato ligand is coordinated to all the Ag(I) ions. The complexes were thermolyzed in dodecylamine, hexadecylamine, and octadecylamine (ODA) to prepare zinc sulfide and silver sulfide nanoparticles. The powder X-ray diffraction patterns of the zinc sulfide nanoparticles correspond to the hexagonal wurtzite while silver sulfide is in the acanthite crystalline phase. The high-resolution transmission electron microscopy images show that quantum dot zinc sulfide nanoparticles are obtained with particle sizes ranging between 1.98 and 5.49 nm, whereas slightly bigger silver sulfide nanoparticles are obtained with particle sizes of 2.70-13.69 nm. The surface morphologies of the ZnS and AgS nanoparticles capped with the same capping agent are very similar. Optical studies revealed that the absorption band edges of the as-prepared zinc sulfide and silver sulfide nanoparticles were blue-shifted with respect to their bulk materials with some surface defects. The zinc sulfide and silver sulfide nanoparticles were used as nanophotocatalysts for the degradation of bromothymol blue (BTB) and bromophenol blue (BPB). ODA-capped zinc sulfide is the most efficient photocatalyst and degraded 87% of BTB and 91% of BPB.

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Surfactant-controlled composition and crystal structure of manganese(II) sulfide nanocrystals prepared by solvothermal synthesis.

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