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Synthesis, Optical, and Structural Studies of Iron Sulphide Nanoparticles and Iron Sulphide Hydroxyethyl Cellulose Nanocomposites from Bis-(Dithiocarbamato)Iron(II) Single-Source Precursors
In this study, Fe(II) complexes of phenyldithiocarbamate, dimethyldithiocarbamate and imidazolyldithiocarbamate were used as single-source precursors to prepare iron sulphide nanoparticles by thermolysis in oleic acid/octadecylamine (ODA) at 180 °C. The nanoparticles were dispersed into hydroxyethyl...
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Formato: | Online Artículo Texto |
Lenguaje: | English |
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MDPI
2018
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Materias: | |
Acceso en línea: | https://www.ncbi.nlm.nih.gov/pmc/articles/PMC5923517/ https://www.ncbi.nlm.nih.gov/pubmed/29570612 http://dx.doi.org/10.3390/nano8040187 |
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author | Paca, Athandwe M. Ajibade, Peter A. |
author_facet | Paca, Athandwe M. Ajibade, Peter A. |
author_sort | Paca, Athandwe M. |
collection | PubMed |
description | In this study, Fe(II) complexes of phenyldithiocarbamate, dimethyldithiocarbamate and imidazolyldithiocarbamate were used as single-source precursors to prepare iron sulphide nanoparticles by thermolysis in oleic acid/octadecylamine (ODA) at 180 °C. The nanoparticles were dispersed into hydroxyethyl cellulose (HEC) to prepare iron sulphide/HEC nanocomposites. Ultraviolet-Visible (UV-Vis), Photoluminescence (PL), Fourier Transform Infrared (FTIR), powder X-ray diffraction (pXRD), high-resolution transmission electron microscopy (HRTEM), Field emission scanning electron microscopy (FESEM), and energy dispersive X-ray spectroscopy (EDS) were used to characterize the iron sulphide nanoparticles and corresponding HEC nanocomposites. The absorption spectra studies revealed that the nanoparticles were blue shifted due to quantum confinement and the optical band gaps of the nanoparticles are 4.85 eV for FeS1, 4.36 eV for FeS2, and 4.77 eV for FeS3. The emission maxima are red-shifted and broader for the nanoparticles prepared from phenyldithiocarbamate. Rod-like and spherically shaped iron sulphide particles were observed from the HRTEM images. The crystallite sizes from the HRTEM images are 23.90–38.89 nm for FeS1, 4.50–10.50 nm for FeS2, and 6.05–6.19 nm for FeS3 iron sulphide nanoparticles, respectively. pXRD diffraction patterns confirmed that FeS1 is in the pyrrhotite-4M crystalline phase, FeS2 is in the pyrrhotite phase, and FeS3 is in the troilite phase of iron sulphide. The phases of the iron sulphide nanoparticles indicate that the nature of the precursor complex affects the obtained crystalline phase. FTIR spectra studies confirmed the incorporation of the nanoparticles in the HEC matrix by the slight shift of the O–H and C–O bonds and the intense peaks on the nanoparticles. FESEM images of the iron sulphide nanoparticles showed flake-like or leaf-like morphologies with some hollow spheres. The EDS confirmed the formation of iron sulphide nanoparticles by showing the peaks of Fe and S. |
format | Online Article Text |
id | pubmed-5923517 |
institution | National Center for Biotechnology Information |
language | English |
publishDate | 2018 |
publisher | MDPI |
record_format | MEDLINE/PubMed |
spelling | pubmed-59235172018-05-03 Synthesis, Optical, and Structural Studies of Iron Sulphide Nanoparticles and Iron Sulphide Hydroxyethyl Cellulose Nanocomposites from Bis-(Dithiocarbamato)Iron(II) Single-Source Precursors Paca, Athandwe M. Ajibade, Peter A. Nanomaterials (Basel) Article In this study, Fe(II) complexes of phenyldithiocarbamate, dimethyldithiocarbamate and imidazolyldithiocarbamate were used as single-source precursors to prepare iron sulphide nanoparticles by thermolysis in oleic acid/octadecylamine (ODA) at 180 °C. The nanoparticles were dispersed into hydroxyethyl cellulose (HEC) to prepare iron sulphide/HEC nanocomposites. Ultraviolet-Visible (UV-Vis), Photoluminescence (PL), Fourier Transform Infrared (FTIR), powder X-ray diffraction (pXRD), high-resolution transmission electron microscopy (HRTEM), Field emission scanning electron microscopy (FESEM), and energy dispersive X-ray spectroscopy (EDS) were used to characterize the iron sulphide nanoparticles and corresponding HEC nanocomposites. The absorption spectra studies revealed that the nanoparticles were blue shifted due to quantum confinement and the optical band gaps of the nanoparticles are 4.85 eV for FeS1, 4.36 eV for FeS2, and 4.77 eV for FeS3. The emission maxima are red-shifted and broader for the nanoparticles prepared from phenyldithiocarbamate. Rod-like and spherically shaped iron sulphide particles were observed from the HRTEM images. The crystallite sizes from the HRTEM images are 23.90–38.89 nm for FeS1, 4.50–10.50 nm for FeS2, and 6.05–6.19 nm for FeS3 iron sulphide nanoparticles, respectively. pXRD diffraction patterns confirmed that FeS1 is in the pyrrhotite-4M crystalline phase, FeS2 is in the pyrrhotite phase, and FeS3 is in the troilite phase of iron sulphide. The phases of the iron sulphide nanoparticles indicate that the nature of the precursor complex affects the obtained crystalline phase. FTIR spectra studies confirmed the incorporation of the nanoparticles in the HEC matrix by the slight shift of the O–H and C–O bonds and the intense peaks on the nanoparticles. FESEM images of the iron sulphide nanoparticles showed flake-like or leaf-like morphologies with some hollow spheres. The EDS confirmed the formation of iron sulphide nanoparticles by showing the peaks of Fe and S. MDPI 2018-03-23 /pmc/articles/PMC5923517/ /pubmed/29570612 http://dx.doi.org/10.3390/nano8040187 Text en © 2018 by the authors. Licensee MDPI, Basel, Switzerland. This article is an open access article distributed under the terms and conditions of the Creative Commons Attribution (CC BY) license (http://creativecommons.org/licenses/by/4.0/). |
spellingShingle | Article Paca, Athandwe M. Ajibade, Peter A. Synthesis, Optical, and Structural Studies of Iron Sulphide Nanoparticles and Iron Sulphide Hydroxyethyl Cellulose Nanocomposites from Bis-(Dithiocarbamato)Iron(II) Single-Source Precursors |
title | Synthesis, Optical, and Structural Studies of Iron Sulphide Nanoparticles and Iron Sulphide Hydroxyethyl Cellulose Nanocomposites from Bis-(Dithiocarbamato)Iron(II) Single-Source Precursors |
title_full | Synthesis, Optical, and Structural Studies of Iron Sulphide Nanoparticles and Iron Sulphide Hydroxyethyl Cellulose Nanocomposites from Bis-(Dithiocarbamato)Iron(II) Single-Source Precursors |
title_fullStr | Synthesis, Optical, and Structural Studies of Iron Sulphide Nanoparticles and Iron Sulphide Hydroxyethyl Cellulose Nanocomposites from Bis-(Dithiocarbamato)Iron(II) Single-Source Precursors |
title_full_unstemmed | Synthesis, Optical, and Structural Studies of Iron Sulphide Nanoparticles and Iron Sulphide Hydroxyethyl Cellulose Nanocomposites from Bis-(Dithiocarbamato)Iron(II) Single-Source Precursors |
title_short | Synthesis, Optical, and Structural Studies of Iron Sulphide Nanoparticles and Iron Sulphide Hydroxyethyl Cellulose Nanocomposites from Bis-(Dithiocarbamato)Iron(II) Single-Source Precursors |
title_sort | synthesis, optical, and structural studies of iron sulphide nanoparticles and iron sulphide hydroxyethyl cellulose nanocomposites from bis-(dithiocarbamato)iron(ii) single-source precursors |
topic | Article |
url | https://www.ncbi.nlm.nih.gov/pmc/articles/PMC5923517/ https://www.ncbi.nlm.nih.gov/pubmed/29570612 http://dx.doi.org/10.3390/nano8040187 |
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