We report the synthesis and morphological studies of lead sulphide nanoparticles prepared from lead(II) complexes of morpholine dithiocarbamate (PbS1), thiomorpholine dithiocarbamate (PbS2), and N-(2-hydroxyethyl)phenyl dithiocarbamate (PbS3). Powder X-ray diffraction patterns (p-XRD) of the PbS nanoparticles are indexed to face-centered cubic phase of PbS. High-resolution transmission electron microscopy (HRTEM) micrograph revealed quasi-spherical PbS nanoparticles with particle size in the range 13.86-36.06 nm while scanning electron microscopy (SEM) revealed flaky/spherical/rough surface morphology. Photocatalytic degradation of methylene blue dye by the PbS nanoparticles showed degradation efficiency of 72.6 % for PbS1, 75.9 % for PbS2, and 47.4 % for PbS3. The photodegradation efficiency shows a correlation between efficiency and morphological properties. Total organic content removal by PbS2 is 69.5 % while that of PbS1 is 64.2 % and PbS3 is 40.1 %. The as-prepared PbS nanoparticles exhibited remarkable photostability in the recyclability studies.

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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.

Bis(4-methylpiperidine-1-carbodithioato)-lead(II) and bis(4-benzylpiperidine-1-carbodithioato)-lead(II) were prepared and their molecular structures elucidated using single crystal X-ray crystallography and spectroscopic techniques. The compounds were used as precursors for the preparation of lead sulphide nano photocatalysts for the degradation of rhodamine B. The single crystal structures of the lead(II) dithiocarbamate complexes show mononuclear lead(II) compounds in which each lead(II) ion coordinates two dithiocarbamato anions in a distorted tetrahedral geometry. The compounds were thermolyzed at 180 ℃ in hexadecylamine (HDA), octadecylamine (ODA), and trioctylphosphine oxide (TOPO) to prepare HDA, ODA, and TOPO capped lead sulphide (PbS) nanoparticles. Powder X-ray diffraction (pXRD) patterns of the lead sulphide nanoparticles were indexed to the rock cubic salt crystalline phase of lead sulphide. The lead sulphide nanoparticles were used as photocatalysts for the degradation of rhodamine B with ODA-PbS1 achieving photodegradation efficiency of 45.28% after 360 min. The photostability and reusability studies of the as-prepared PbS nanoparticles were studied in four consecutive cycles, showing that the percentage degradation efficiency decreased slightly by about 0.51–1.93%. The results show that the as-prepared PbS nanoparticles are relatively photostable with a slight loss of photodegradation activities as the reusability cycles progress.

Octylamine (OTA), 1-dodecanethiol (DDT), and tri-n-octylphosphine (TOP) capped magnetite nanoparticles were prepared by co-precipitation method. Powder X-ray diffraction patterns confirmed inverse spinel crystalline phases for the as-prepared iron oxide nanoparticles. Transmission electron microscopic micrographs showed iron oxide nanoparticles with mean particle sizes of 2.1 nm for Fe3O4-OTA, 5.0 nm for Fe3O4-DDT, and 4.4 nm for Fe3O4-TOP. The energy bandgap of the iron oxide nanoparticles ranges from 2.25 eV to 2.76 eV. The iron oxide nanoparticles were used as photocatalysts for the degradation of methylene blue with an efficiency of 55.5%, 58.3%, and 66.7% for Fe3O4-OTA, Fe3O4-DDT, and Fe3O4-TOP, respectively, while for methyl orange the degradation efficiencies were 63.8%, 47.7%, and 74.1%, respectively. The results showed that tri-n-octylphosphine capped iron oxide nanoparticles are the most efficient iron oxide nano-photocatalysts for the degradation of both dyes. Scavenger studies show that electrons (e−) and hydroxy radicals (•OH) contribute significantly to the photocatalytic degradation reaction of both methylene blue and methyl orange using Fe3O4-TOP nanoparticles. The influence of the dye solution’s pH on the photocatalytic reaction reveals that a pH of 10 is the optimum for methylene blue degradation, whereas a pH of 2 is best for methyl orange photocatalytic degradation using the as-prepared iron oxide nano-photocatalyst. Recyclability studies revealed that the iron oxide photocatalysts can be recycled three times without losing their photocatalytic activity.