Sonochemical preparation of SnS and SnS2 nano- and micropowders and their characterization

Sonochemical production of tin(II) and tin(IV) sulfides is investigated. Different conditions of syntheses are examined: used solvent (ethanol or ethylenediamine), source of tin (SnCl2 or SnCl4), the molar ratio of thioacetamide to the tin source, and time of sonication. The obtained powders are cha...

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Main Authors: Grzegorz Matyszczak, Paweł Jóźwik, Emilia Polesiak, Małgorzata Sobieska, Krzysztof Krawczyk, Cezariusz Jastrzębski, Tomasz Płociński
Format: Article
Language:English
Published: Elsevier 2021-07-01
Series:Ultrasonics Sonochemistry
Subjects:
Online Access:http://www.sciencedirect.com/science/article/pii/S135041772100136X
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author Grzegorz Matyszczak
Paweł Jóźwik
Emilia Polesiak
Małgorzata Sobieska
Krzysztof Krawczyk
Cezariusz Jastrzębski
Tomasz Płociński
author_facet Grzegorz Matyszczak
Paweł Jóźwik
Emilia Polesiak
Małgorzata Sobieska
Krzysztof Krawczyk
Cezariusz Jastrzębski
Tomasz Płociński
author_sort Grzegorz Matyszczak
collection DOAJ
description Sonochemical production of tin(II) and tin(IV) sulfides is investigated. Different conditions of syntheses are examined: used solvent (ethanol or ethylenediamine), source of tin (SnCl2 or SnCl4), the molar ratio of thioacetamide to the tin source, and time of sonication. The obtained powders are characterized by the X-ray diffraction method (PXRD), scanning electron microscopy (SEM), scanning transmission electron microscopy (STEM), energy-dispersive X-ray spectroscopy (EDX), and the Tauc method. Raman and FT-IR measurements were performed for the obtained samples, which additionally confirmed the crystallinity and phase composition of the samples. The influence of experimental conditions on composition (is it SnS or SnS2), morphology, and on the bandgap of obtained products is elucidated. It was found that longer sonication times favor more crystalline product. Each of bandgaps is direct and most of them show typical values – c.a. 1.3 eV for SnS and 2.4 eV for SnS2. However, there are some exceptions. Synthesized powders show a variety of forms such as needles, flower-like, rods, random agglomerates (SnS2) and balls (SnS). Using ethanol as a solvent led to powders of SnS2 independently of which tin chloride is used. Sonochemistry in ethylenediamine is more diverse: this solvent protects Sn2+ cations from oxidation so mostly SnS is obtained, while SnCl4 does not produce powder of SnS2 but Sn(SO4)2 instead or, at a higher ratio of thioacetamide to SnCl4, green clear mixture.
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spelling doaj.art-939f972f24e44954a936cacf51974add2022-12-21T18:50:55ZengElsevierUltrasonics Sonochemistry1350-41772021-07-0175105594Sonochemical preparation of SnS and SnS2 nano- and micropowders and their characterizationGrzegorz Matyszczak0Paweł Jóźwik1Emilia Polesiak2Małgorzata Sobieska3Krzysztof Krawczyk4Cezariusz Jastrzębski5Tomasz Płociński6Department of Chemical Technology, Faculty of Chemistry, Warsaw University of Technology, Noakowskiego Street 3, 00-664 Warsaw, Poland; Corresponding author.Faculty of Advanced Technologies and Chemistry, Military University of Technology, ul. gen. Sylwestra Kaliskiego 2, 00-908 Warsaw, PolandDepartment of Chemical Technology, Faculty of Chemistry, Warsaw University of Technology, Noakowskiego Street 3, 00-664 Warsaw, PolandDepartment of Chemical Technology, Faculty of Chemistry, Warsaw University of Technology, Noakowskiego Street 3, 00-664 Warsaw, PolandDepartment of Chemical Technology, Faculty of Chemistry, Warsaw University of Technology, Noakowskiego Street 3, 00-664 Warsaw, PolandFaculty of Physics, Warsaw University of Technology, Koszykowa street 75, 00-662 Warsaw, PolandFaculty of Materials Science and Engineering, Warsaw University of Technology, Wołoska Street 141A, 02-507 Warsaw, PolandSonochemical production of tin(II) and tin(IV) sulfides is investigated. Different conditions of syntheses are examined: used solvent (ethanol or ethylenediamine), source of tin (SnCl2 or SnCl4), the molar ratio of thioacetamide to the tin source, and time of sonication. The obtained powders are characterized by the X-ray diffraction method (PXRD), scanning electron microscopy (SEM), scanning transmission electron microscopy (STEM), energy-dispersive X-ray spectroscopy (EDX), and the Tauc method. Raman and FT-IR measurements were performed for the obtained samples, which additionally confirmed the crystallinity and phase composition of the samples. The influence of experimental conditions on composition (is it SnS or SnS2), morphology, and on the bandgap of obtained products is elucidated. It was found that longer sonication times favor more crystalline product. Each of bandgaps is direct and most of them show typical values – c.a. 1.3 eV for SnS and 2.4 eV for SnS2. However, there are some exceptions. Synthesized powders show a variety of forms such as needles, flower-like, rods, random agglomerates (SnS2) and balls (SnS). Using ethanol as a solvent led to powders of SnS2 independently of which tin chloride is used. Sonochemistry in ethylenediamine is more diverse: this solvent protects Sn2+ cations from oxidation so mostly SnS is obtained, while SnCl4 does not produce powder of SnS2 but Sn(SO4)2 instead or, at a higher ratio of thioacetamide to SnCl4, green clear mixture.http://www.sciencedirect.com/science/article/pii/S135041772100136XTin(II) sulfideTin(IV) sulfideNanopowderMicropowderSonochemistry
spellingShingle Grzegorz Matyszczak
Paweł Jóźwik
Emilia Polesiak
Małgorzata Sobieska
Krzysztof Krawczyk
Cezariusz Jastrzębski
Tomasz Płociński
Sonochemical preparation of SnS and SnS2 nano- and micropowders and their characterization
Ultrasonics Sonochemistry
Tin(II) sulfide
Tin(IV) sulfide
Nanopowder
Micropowder
Sonochemistry
title Sonochemical preparation of SnS and SnS2 nano- and micropowders and their characterization
title_full Sonochemical preparation of SnS and SnS2 nano- and micropowders and their characterization
title_fullStr Sonochemical preparation of SnS and SnS2 nano- and micropowders and their characterization
title_full_unstemmed Sonochemical preparation of SnS and SnS2 nano- and micropowders and their characterization
title_short Sonochemical preparation of SnS and SnS2 nano- and micropowders and their characterization
title_sort sonochemical preparation of sns and sns2 nano and micropowders and their characterization
topic Tin(II) sulfide
Tin(IV) sulfide
Nanopowder
Micropowder
Sonochemistry
url http://www.sciencedirect.com/science/article/pii/S135041772100136X
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AT emiliapolesiak sonochemicalpreparationofsnsandsns2nanoandmicropowdersandtheircharacterization
AT małgorzatasobieska sonochemicalpreparationofsnsandsns2nanoandmicropowdersandtheircharacterization
AT krzysztofkrawczyk sonochemicalpreparationofsnsandsns2nanoandmicropowdersandtheircharacterization
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