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The Critical Role of Thioacetamide Concentration in the Formation of ZnO/ZnS Heterostructures by Sol-Gel Process

1
Department of Drugs and Medicines, School of Pharmaceutical Sciences, São Paulo State University (UNESP), Araraquara, São Paulo 14800-903, Brazil
2
Institut Galien, University Paris-Sud, The National Center for Scientific Research (CNRS), UMR 8612, 92296 Châtenay-Malabry, France
3
Department of Chemistry, Sergipe Federal University—Campus Itabaiana, Av. Vereador Olimpio Grande, s/n—Itabaiana, SE 49506-036, Brazil
4
Chemistry Institute of São Paulo State University—UNESP, Prof. Francisco Degni Street, 55, Araraquara, São Paulo 14800-060, Brazil
5
Brazilian Synchrotron Light Laboratory (LNLS), Brazilian Center for Research in Energy and Materials (CNPEM), São Paulo 13083-970, Brazil
6
Synchrotron Optimized Light Source of Intermediate Energy to LURE (SOLEIL), L’Orme des Merisiers, BP48, Saint Aubin, 91192 Gif-sur Yvette, France
*
Authors to whom correspondence should be addressed.
Nanomaterials 2018, 8(2), 55; https://doi.org/10.3390/nano8020055
Received: 30 September 2017 / Revised: 3 November 2017 / Accepted: 6 November 2017 / Published: 23 January 2018
(This article belongs to the Special Issue ZnO and TiO2 Based Nanostructures)
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Abstract

ZnO/ZnS heterostructures have emerged as an attractive approach for tailoring the properties of particles comprising these semiconductors. They can be synthesized using low temperature sol-gel routes. The present work yields insight into the mechanisms involved in the formation of ZnO/ZnS nanostructures. ZnO colloidal suspensions, prepared by hydrolysis and condensation of a Zn acetate precursor solution, were allowed to react with an ethanolic thioacetamide solution (TAA) as sulfur source. The reactions were monitored in situ by Small Angle X-ray Scattering (SAXS) and UV-vis spectroscopy, and the final colloidal suspensions were characterized by High Resolution Transmission Electron Microscopy (HRTEM). The powders extracted at the end of the reactions were analyzed by X-ray Absorption spectroscopy (XAS) and X-ray diffraction (XRD). Depending on TAA concentration, different nanostructures were revealed. ZnO and ZnS phases were mainly obtained at low and high TAA concentrations, respectively. At intermediate TAA concentrations, we evidenced the formation of ZnO/ZnS heterostructures. ZnS formation could take place via direct crystal growth involving Zn ions remaining in solution and S ions provided by TAA and/or chemical conversion of ZnO to ZnS. The combination of all the characterization techniques was crucial to elucidate the reaction steps and the nature of the final products. View Full-Text
Keywords: ZnO; ZnS; quantum dots; heterostructure; sol-gel; Small Angle X-ray Scattering; X-ray Absorption Spectroscopy; UV-vis spectroscopy ZnO; ZnS; quantum dots; heterostructure; sol-gel; Small Angle X-ray Scattering; X-ray Absorption Spectroscopy; UV-vis spectroscopy
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This is an open access article distributed under the Creative Commons Attribution License which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited (CC BY 4.0).

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Berbel Manaia, E.; Kiatkoski Kaminski, R.C.; Caetano, B.L.; Magnani, M.; Meneau, F.; Rochet, A.; Santilli, C.V.; Briois, V.; Bourgaux, C.; Chiavacci, L.A. The Critical Role of Thioacetamide Concentration in the Formation of ZnO/ZnS Heterostructures by Sol-Gel Process. Nanomaterials 2018, 8, 55.

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