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Title: Fe( ii ) and Fe( iii ) dithiocarbamate complexes as single source precursors to nanoscale iron sulfides: a combined synthetic and in situ XAS approach

Abstract

Nanoparticulate iron sulfides have many possible applications and are also proposed to be prebiotic catalysts for the reduction of CO2 to biologically important molecules, thus the development of reliable routes to specific phases with controlled sizes and morphologies is important. In this work we focus on the use of iron dithiocarbamate complexes as single source precursors (SSPs) to generate greigite and pyrrhotite nanoparticles. Since these minerals contain both iron(III) and iron(II) centres, SSPs in both oxidation states, [Fe(S2CNR2)3] and cis-[Fe(CO)2(S2CNR2)2] respectively, have been utilised. Use of this Fe(II) precursor is novel and it readily loses both carbonyls in a single step (as shown by TGA measurements) providing an in situ source of the extremely air-sensitive Fe(II) dithiocarbamate complexes [Fe(S2CNR2)2]. Decomposition of [Fe(S2CNR2)3] alone in oleylamine affords primarily pyrrhotite, although by careful control of reaction conditions (ca. 230 °C, 40–50 nM SSP) a window exists in which pure greigite nanoparticles can be isolated. With cis-[Fe(CO)2(S2CNR2)2] we were unable to produce pure greigite, with pyrrhotite formation dominating, a similar situation being found with mixtures of Fe(II) and Fe(III) precursors. In situ X-ray absorption spectroscopy (XAS) studies showed that heating [Fe(S2CNiBu2)3] in oleylamine resulted in amine coordination and, at ca. 60 °C, reductionmore » of Fe(III) to Fe(II) with (proposed) elimination of thiuram disulfide (S2CNR2)2. We thus carried out a series of decomposition studies with added thiuram disulfide (R = iBu) and found that addition of 1–2 equivalents led to the formation of pure greigite nanoparticles between 230 and 280 °C with low SSP concentrations. Average particle size does not vary significantly with increasing concentration, thus providing a convenient route to ca. 40 nm greigite nanoparticles. In situ XAS studies have been carried out and allow a decomposition pathway for [Fe(S2CNiBu2)3] in oleylamine to be established; reduction of Fe(III) to Fe(II) reduction triggers substitution of the secondary amide backbone by oleylamine (RNH2) resulting in the in situ formation of a primary dithiocarbamate derivative [Fe(RNH2)2(S2CNHR)2]. This in turn extrudes RNCS to afford molecular precursors of the observed FeS nanomaterials. The precise role of thiuram disulfide in the decomposition process is unknown, but it likely plays a part in controlling the Fe(III)–Fe(II) equilibrium and may also act as a source of sulfur allowing control over the Fe:S ratio in the mineral products.« less

Authors:
ORCiD logo [1];  [2];  [3]; ORCiD logo [4];  [2]; ORCiD logo [5]; ORCiD logo [6]
+ Show Author Affiliations
  1. Department of Chemistry; King's College London; London SE1 1DB; UK; Department of Chemistry
  2. Department of Chemistry; University College London; London WC1H OAJ; UK
  3. Department of Chemistry; University College London; London WC1H OAJ; UK; Netherlands Organisation for Scientific Research DUBBLE@ESRF
  4. Netherlands Organisation for Scientific Research DUBBLE@ESRF; 38043 Grenoble; France; Chemistry Division; Oak Ridge National Laboratory
  5. School of Chemistry; Cardiff University; Cardiff; UK
  6. 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; Netherlands Organisation for Scientific Research (NWO)
OSTI Identifier:
1527056
Alternate Identifier(s):
OSTI ID: 1558538
Grant/Contract Number:  
AC05-00OR22725
Resource Type:
Published Article
Journal Name:
Nanoscale Advances
Additional Journal Information:
Journal Name: Nanoscale Advances Journal Volume: 1 Journal Issue: 8; Journal ID: ISSN 2516-0230
Publisher:
Royal Society of Chemistry
Country of Publication:
United Kingdom
Language:
English
Subject:
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY

Citation Formats

Roffey, Anna, Hollingsworth, Nathan, Islam, Husn-Ubayda, Bras, Wim, Sankar, Gopinathan, de Leeuw, Nora H., and Hogarth, Graeme. Fe( ii ) and Fe( iii ) dithiocarbamate complexes as single source precursors to nanoscale iron sulfides: a combined synthetic and in situ XAS approach. United Kingdom: N. p., 2019. Web. https://doi.org/10.1039/C9NA00262F.
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Roffey, Anna, Hollingsworth, Nathan, Islam, Husn-Ubayda, Bras, Wim, Sankar, Gopinathan, de Leeuw, Nora H., & Hogarth, Graeme. Fe( ii ) and Fe( iii ) dithiocarbamate complexes as single source precursors to nanoscale iron sulfides: a combined synthetic and in situ XAS approach. United Kingdom. https://doi.org/10.1039/C9NA00262F
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Roffey, Anna, Hollingsworth, Nathan, Islam, Husn-Ubayda, Bras, Wim, Sankar, Gopinathan, de Leeuw, Nora H., and Hogarth, Graeme. Tue . "Fe( ii ) and Fe( iii ) dithiocarbamate complexes as single source precursors to nanoscale iron sulfides: a combined synthetic and in situ XAS approach". United Kingdom. https://doi.org/10.1039/C9NA00262F.
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@article{osti_1527056,
title = {Fe( ii ) and Fe( iii ) dithiocarbamate complexes as single source precursors to nanoscale iron sulfides: a combined synthetic and in situ XAS approach},
author = {Roffey, Anna and Hollingsworth, Nathan and Islam, Husn-Ubayda and Bras, Wim and Sankar, Gopinathan and de Leeuw, Nora H. and Hogarth, Graeme},
abstractNote = {Nanoparticulate iron sulfides have many possible applications and are also proposed to be prebiotic catalysts for the reduction of CO2 to biologically important molecules, thus the development of reliable routes to specific phases with controlled sizes and morphologies is important. In this work we focus on the use of iron dithiocarbamate complexes as single source precursors (SSPs) to generate greigite and pyrrhotite nanoparticles. Since these minerals contain both iron(III) and iron(II) centres, SSPs in both oxidation states, [Fe(S2CNR2)3] and cis-[Fe(CO)2(S2CNR2)2] respectively, have been utilised. Use of this Fe(II) precursor is novel and it readily loses both carbonyls in a single step (as shown by TGA measurements) providing an in situ source of the extremely air-sensitive Fe(II) dithiocarbamate complexes [Fe(S2CNR2)2]. Decomposition of [Fe(S2CNR2)3] alone in oleylamine affords primarily pyrrhotite, although by careful control of reaction conditions (ca. 230 °C, 40–50 nM SSP) a window exists in which pure greigite nanoparticles can be isolated. With cis-[Fe(CO)2(S2CNR2)2] we were unable to produce pure greigite, with pyrrhotite formation dominating, a similar situation being found with mixtures of Fe(II) and Fe(III) precursors. In situ X-ray absorption spectroscopy (XAS) studies showed that heating [Fe(S2CNiBu2)3] in oleylamine resulted in amine coordination and, at ca. 60 °C, reduction of Fe(III) to Fe(II) with (proposed) elimination of thiuram disulfide (S2CNR2)2. We thus carried out a series of decomposition studies with added thiuram disulfide (R = iBu) and found that addition of 1–2 equivalents led to the formation of pure greigite nanoparticles between 230 and 280 °C with low SSP concentrations. Average particle size does not vary significantly with increasing concentration, thus providing a convenient route to ca. 40 nm greigite nanoparticles. In situ XAS studies have been carried out and allow a decomposition pathway for [Fe(S2CNiBu2)3] in oleylamine to be established; reduction of Fe(III) to Fe(II) reduction triggers substitution of the secondary amide backbone by oleylamine (RNH2) resulting in the in situ formation of a primary dithiocarbamate derivative [Fe(RNH2)2(S2CNHR)2]. This in turn extrudes RNCS to afford molecular precursors of the observed FeS nanomaterials. The precise role of thiuram disulfide in the decomposition process is unknown, but it likely plays a part in controlling the Fe(III)–Fe(II) equilibrium and may also act as a source of sulfur allowing control over the Fe:S ratio in the mineral products.},
doi = {10.1039/C9NA00262F},
journal = {Nanoscale Advances},
number = 8,
volume = 1,
place = {United Kingdom},
year = {2019},
month = {1}
}
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