Testing the Efficacy of the Synthesis of Iron Antimony Sulfide Powders from Single Source Precursors
The antimony-iron sulfide system in general does not produce alloys below 540 °C from traditional solid-state methods. However, single source precursors have been known to produce unexpected products that arise from kinetically trapped polymorphs. In this paper, we test the efficacy of this approach...
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MDPI AG
2021-08-01
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| Series: | Inorganics |
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| Online Access: | https://www.mdpi.com/2304-6740/9/8/61 |
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| author | Fadiyah Makin Dalal Alzahrani Firoz Alam Floriana Tuna David J. Lewis |
| author_facet | Fadiyah Makin Dalal Alzahrani Firoz Alam Floriana Tuna David J. Lewis |
| author_sort | Fadiyah Makin |
| collection | DOAJ |
| description | The antimony-iron sulfide system in general does not produce alloys below 540 °C from traditional solid-state methods. However, single source precursors have been known to produce unexpected products that arise from kinetically trapped polymorphs. In this paper, we test the efficacy of this approach toward the Fe-Sb-S system. Antimony and iron diethyldithiocarbamate complexes of the form Sb[S<sub>2</sub>CN(Et<sub>2</sub>)]<sub>3</sub> (<b>1</b>) and Fe[S<sub>2</sub>CN(Et<sub>2</sub>)]<sub>3</sub> (<b>2</b>) were synthesised, characterised, and used as single-source precursors for the preparation of Sb<sub>2</sub>S<sub>3</sub>, Fe<sub><i>x</i></sub>S<sub><i>y</i></sub>, and mixed iron antimony sulfide Sb<sub>2(1−<i>x</i>)</sub>Fe<sub>2<i>x</i></sub>S<sub>3</sub> (0 ≥ <i>x</i> ≥ 1) powders using the solvent-less thermolysis method at different temperatures ranging from 300 to 475 °C. The effect of different mole fractions of the iron precursor was evaluated on morphology, shape, and optical and magnetic properties of Sb<sub>2(1−<i>x</i>)</sub>Fe<sub>2<i>x</i></sub>S<sub>3</sub> (0 ≥ <i>x</i> ≥ 1). The obtained powders were characterized by X-ray diffraction (XRD), Raman spectroscopy scanning electron microscopy (SEM), energy dispersive X-ray (EDX) spectroscopy, magnetometer measurement, and UV/vis/NIR spectroscopy. The results demonstrated that the crystalline structure, morphology, and elemental composition of the samples changed with the mole fraction of the precursor. There was significant phase separation between Sb and Fe sulfides noted from EDX spectroscopic mapping, yet an optoelectronic study monitoring the direct band gap energy of antimony sulfide shows that the band gap energy increases as a function of Fe content, which suggests limited alloying is possible from the single source route. |
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| language | English |
| last_indexed | 2024-03-10T08:43:07Z |
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| spelling | doaj.art-9f212addfa7547b8a83273b3276b7ab12023-11-22T08:06:35ZengMDPI AGInorganics2304-67402021-08-01986110.3390/inorganics9080061Testing the Efficacy of the Synthesis of Iron Antimony Sulfide Powders from Single Source PrecursorsFadiyah Makin0Dalal Alzahrani1Firoz Alam2Floriana Tuna3David J. Lewis4Department of Materials, The University of Manchester, Oxford Road, Manchester M13 9PL, UKPhoton Science Institute, The University of Manchester, Oxford Road, Manchester M13 9PL, UKDepartment of Chemistry, The University of Manchester, Oxford Road, Manchester M13 9PL, UKPhoton Science Institute, The University of Manchester, Oxford Road, Manchester M13 9PL, UKDepartment of Materials, The University of Manchester, Oxford Road, Manchester M13 9PL, UKThe antimony-iron sulfide system in general does not produce alloys below 540 °C from traditional solid-state methods. However, single source precursors have been known to produce unexpected products that arise from kinetically trapped polymorphs. In this paper, we test the efficacy of this approach toward the Fe-Sb-S system. Antimony and iron diethyldithiocarbamate complexes of the form Sb[S<sub>2</sub>CN(Et<sub>2</sub>)]<sub>3</sub> (<b>1</b>) and Fe[S<sub>2</sub>CN(Et<sub>2</sub>)]<sub>3</sub> (<b>2</b>) were synthesised, characterised, and used as single-source precursors for the preparation of Sb<sub>2</sub>S<sub>3</sub>, Fe<sub><i>x</i></sub>S<sub><i>y</i></sub>, and mixed iron antimony sulfide Sb<sub>2(1−<i>x</i>)</sub>Fe<sub>2<i>x</i></sub>S<sub>3</sub> (0 ≥ <i>x</i> ≥ 1) powders using the solvent-less thermolysis method at different temperatures ranging from 300 to 475 °C. The effect of different mole fractions of the iron precursor was evaluated on morphology, shape, and optical and magnetic properties of Sb<sub>2(1−<i>x</i>)</sub>Fe<sub>2<i>x</i></sub>S<sub>3</sub> (0 ≥ <i>x</i> ≥ 1). The obtained powders were characterized by X-ray diffraction (XRD), Raman spectroscopy scanning electron microscopy (SEM), energy dispersive X-ray (EDX) spectroscopy, magnetometer measurement, and UV/vis/NIR spectroscopy. The results demonstrated that the crystalline structure, morphology, and elemental composition of the samples changed with the mole fraction of the precursor. There was significant phase separation between Sb and Fe sulfides noted from EDX spectroscopic mapping, yet an optoelectronic study monitoring the direct band gap energy of antimony sulfide shows that the band gap energy increases as a function of Fe content, which suggests limited alloying is possible from the single source route.https://www.mdpi.com/2304-6740/9/8/61metal chalcogenidessolvent-less thermolysisdiethyldithiocarbamate complexesoptical propertiesantimonyiron |
| spellingShingle | Fadiyah Makin Dalal Alzahrani Firoz Alam Floriana Tuna David J. Lewis Testing the Efficacy of the Synthesis of Iron Antimony Sulfide Powders from Single Source Precursors Inorganics metal chalcogenides solvent-less thermolysis diethyldithiocarbamate complexes optical properties antimony iron |
| title | Testing the Efficacy of the Synthesis of Iron Antimony Sulfide Powders from Single Source Precursors |
| title_full | Testing the Efficacy of the Synthesis of Iron Antimony Sulfide Powders from Single Source Precursors |
| title_fullStr | Testing the Efficacy of the Synthesis of Iron Antimony Sulfide Powders from Single Source Precursors |
| title_full_unstemmed | Testing the Efficacy of the Synthesis of Iron Antimony Sulfide Powders from Single Source Precursors |
| title_short | Testing the Efficacy of the Synthesis of Iron Antimony Sulfide Powders from Single Source Precursors |
| title_sort | testing the efficacy of the synthesis of iron antimony sulfide powders from single source precursors |
| topic | metal chalcogenides solvent-less thermolysis diethyldithiocarbamate complexes optical properties antimony iron |
| url | https://www.mdpi.com/2304-6740/9/8/61 |
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