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Title: Understanding the role of zinc dithiocarbamate complexes as single source precursors to ZnS nanomaterials

Abstract

Zinc sulfide is an important wide-band gap semi-conductor and dithiocarbamate complexes [Zn(S2CNR2)2] find widespread use as single-source precursors for the controlled synthesis of ZnS nanoparticulate modifications. Decomposition of [Zn(S2CNiBu2)2] in oleylamine gives high aspect ratio wurtzite nanowires, the average length of which was increased upon addition of thiuram disulfide to the decomposition mixture. To provide further insight into the decomposition process, X-ray absorption spectroscopy (XAS) of [Zn(S2CNMe2)2] was performed in the solid-state, in non-coordinating xylene and in oleylamine. In the solid-state, dimeric [Zn(S2CNMe2)2]2 was characterised in accord with the single crystal X-ray structure, while in xylene this breaks down into tetrahedral monomers. In situ XAS in oleylamine (RNH2) shows that the coordination sphere is further modified, amine binding to give five-coordinate [Zn(S2CNMe2)2(RNH2)]. This species is stable to ca. 70 °C, above which amine dissociates and at ca. 90 °C decomposition occurs to generate ZnS. The relatively low temperature onset of nanoparticle formation is associated with amine-exchange leading to the in situ formation of [Zn(S2CNMe2)(S2CNHR)] which has a low temperature decomposition pathway. Combining these observations with the previous work of others allows us to propose a detailed mechanistic scheme for the overall process.

Authors:
 [1];  [2];  [2]; ORCiD logo [3];  [2]; ORCiD logo [4]; ORCiD logo [5]
  1. Department of Chemistry, University College London, London WC1H OAJ, UK, Netherlands Organisation for Scientific Research DUBBLE@ESRF
  2. Department of Chemistry, University College London, London WC1H OAJ, UK
  3. Netherlands Organisation for Scientific Research DUBBLE@ESRF, 38043 Grenoble, France, Chemical Sciences Division, Oak Ridge National Laboratory
  4. School of Chemistry, Cardiff University, Cardiff, UK
  5. Department of Chemistry, King's College London, London SE1 1DB, UK
Publication Date:
Research Org.:
Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States)
Sponsoring Org.:
USDOE
OSTI Identifier:
1591949
Alternate Identifier(s):
OSTI ID: 1761675
Grant/Contract Number:  
AC05-00OR22725
Resource Type:
Published Article
Journal Name:
Nanoscale Advances
Additional Journal Information:
Journal Name: Nanoscale Advances Journal Volume: 2 Journal Issue: 2; Journal ID: ISSN 2516-0230
Publisher:
Royal Society of Chemistry
Country of Publication:
United Kingdom
Language:
English
Subject:
36 MATERIALS SCIENCE

Citation Formats

Islam, Husn-Ubayda, Roffey, Anna, Hollingsworth, Nathan, Bras, Wim, Sankar, Gopinathan, De Leeuw, Nora H., and Hogarth, Graeme. Understanding the role of zinc dithiocarbamate complexes as single source precursors to ZnS nanomaterials. United Kingdom: N. p., 2020. Web. doi:10.1039/C9NA00665F.
Islam, Husn-Ubayda, Roffey, Anna, Hollingsworth, Nathan, Bras, Wim, Sankar, Gopinathan, De Leeuw, Nora H., & Hogarth, Graeme. Understanding the role of zinc dithiocarbamate complexes as single source precursors to ZnS nanomaterials. United Kingdom. doi:10.1039/C9NA00665F.
Islam, Husn-Ubayda, Roffey, Anna, Hollingsworth, Nathan, Bras, Wim, Sankar, Gopinathan, De Leeuw, Nora H., and Hogarth, Graeme. Tue . "Understanding the role of zinc dithiocarbamate complexes as single source precursors to ZnS nanomaterials". United Kingdom. doi:10.1039/C9NA00665F.
@article{osti_1591949,
title = {Understanding the role of zinc dithiocarbamate complexes as single source precursors to ZnS nanomaterials},
author = {Islam, Husn-Ubayda and Roffey, Anna and Hollingsworth, Nathan and Bras, Wim and Sankar, Gopinathan and De Leeuw, Nora H. and Hogarth, Graeme},
abstractNote = {Zinc sulfide is an important wide-band gap semi-conductor and dithiocarbamate complexes [Zn(S2CNR2)2] find widespread use as single-source precursors for the controlled synthesis of ZnS nanoparticulate modifications. Decomposition of [Zn(S2CNiBu2)2] in oleylamine gives high aspect ratio wurtzite nanowires, the average length of which was increased upon addition of thiuram disulfide to the decomposition mixture. To provide further insight into the decomposition process, X-ray absorption spectroscopy (XAS) of [Zn(S2CNMe2)2] was performed in the solid-state, in non-coordinating xylene and in oleylamine. In the solid-state, dimeric [Zn(S2CNMe2)2]2 was characterised in accord with the single crystal X-ray structure, while in xylene this breaks down into tetrahedral monomers. In situ XAS in oleylamine (RNH2) shows that the coordination sphere is further modified, amine binding to give five-coordinate [Zn(S2CNMe2)2(RNH2)]. This species is stable to ca. 70 °C, above which amine dissociates and at ca. 90 °C decomposition occurs to generate ZnS. The relatively low temperature onset of nanoparticle formation is associated with amine-exchange leading to the in situ formation of [Zn(S2CNMe2)(S2CNHR)] which has a low temperature decomposition pathway. Combining these observations with the previous work of others allows us to propose a detailed mechanistic scheme for the overall process.},
doi = {10.1039/C9NA00665F},
journal = {Nanoscale Advances},
number = 2,
volume = 2,
place = {United Kingdom},
year = {2020},
month = {2}
}

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DOI: 10.1039/C9NA00665F

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