Phase Pure Pyrite FeS<inf>2</inf> Nanocubes Synthesized Using Oleylamine as Ligand, Solvent, and Reductant

Feng Jiang, Lauren T. Peckler, Anthony J Muscat

Research output: Contribution to journalArticle

26 Citations (Scopus)

Abstract

Pyrite (FeS<inf>2</inf>) nanocrystals with a narrow size distribution and optical absorption from 1600 to 380 nm were synthesized in a single stage by reacting ferrous chloride with elemental sulfur in oleylamine (OAm) without an additional ligand. X-ray diffraction, Raman, and scanning electron microscopy showed that pyrite cubes with dimensions of 88 ± 14 nm formed at 200 C, an S to Fe ratio of 6, and 1 h reaction time in OAm. The time required to form phase pure pyrite depended on the S to Fe ratio. Phase purity was obtained in less than 1 h at a ratio of 6, but times as long as 24 h were necessary at a ratio of 2.75. The rate of pyrite formation increased with higher sulfur concentrations, which shows that molecules containing sulfur are involved in the rate-determining step. Both H<inf>2</inf>S and polysulfides of the form S<inf>n</inf><sup>2-</sup> are known to form in oleylamine. The slow step is the reaction between FeS and these molecules. Fe<sup>2+</sup>S<sup>2-</sup> undergoes nucleophilic attack by H<inf>2</inf>S and S<inf>n</inf><sup>2-</sup>; S<sup>2-</sup> converts to S<sup>-</sup> and sulfur is transferred forming pyrite Fe<sup>2+</sup>S<inf>2</inf><sup>2-</sup>.

Original languageEnglish (US)
Pages (from-to)3565-3572
Number of pages8
JournalCrystal Growth and Design
Volume15
Issue number8
DOIs
StatePublished - Aug 5 2015

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Pyrites
Reducing Agents
pyrites
Sulfur
Ligands
sulfur
ligands
polysulfides
Polysulfides
Molecules
reaction time
Nanocrystals
Light absorption
attack
molecules
nanocrystals
purity
optical absorption
chlorides
oleylamine

ASJC Scopus subject areas

  • Chemistry(all)
  • Materials Science(all)
  • Condensed Matter Physics

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Phase Pure Pyrite FeS<inf>2</inf> Nanocubes Synthesized Using Oleylamine as Ligand, Solvent, and Reductant. / Jiang, Feng; Peckler, Lauren T.; Muscat, Anthony J.

In: Crystal Growth and Design, Vol. 15, No. 8, 05.08.2015, p. 3565-3572.

Research output: Contribution to journalArticle

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abstract = "Pyrite (FeS2) nanocrystals with a narrow size distribution and optical absorption from 1600 to 380 nm were synthesized in a single stage by reacting ferrous chloride with elemental sulfur in oleylamine (OAm) without an additional ligand. X-ray diffraction, Raman, and scanning electron microscopy showed that pyrite cubes with dimensions of 88 ± 14 nm formed at 200 C, an S to Fe ratio of 6, and 1 h reaction time in OAm. The time required to form phase pure pyrite depended on the S to Fe ratio. Phase purity was obtained in less than 1 h at a ratio of 6, but times as long as 24 h were necessary at a ratio of 2.75. The rate of pyrite formation increased with higher sulfur concentrations, which shows that molecules containing sulfur are involved in the rate-determining step. Both H2S and polysulfides of the form Sn2- are known to form in oleylamine. The slow step is the reaction between FeS and these molecules. Fe2+S2- undergoes nucleophilic attack by H2S and Sn2-; S2- converts to S- and sulfur is transferred forming pyrite Fe2+S22-.",
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N2 - Pyrite (FeS2) nanocrystals with a narrow size distribution and optical absorption from 1600 to 380 nm were synthesized in a single stage by reacting ferrous chloride with elemental sulfur in oleylamine (OAm) without an additional ligand. X-ray diffraction, Raman, and scanning electron microscopy showed that pyrite cubes with dimensions of 88 ± 14 nm formed at 200 C, an S to Fe ratio of 6, and 1 h reaction time in OAm. The time required to form phase pure pyrite depended on the S to Fe ratio. Phase purity was obtained in less than 1 h at a ratio of 6, but times as long as 24 h were necessary at a ratio of 2.75. The rate of pyrite formation increased with higher sulfur concentrations, which shows that molecules containing sulfur are involved in the rate-determining step. Both H2S and polysulfides of the form Sn2- are known to form in oleylamine. The slow step is the reaction between FeS and these molecules. Fe2+S2- undergoes nucleophilic attack by H2S and Sn2-; S2- converts to S- and sulfur is transferred forming pyrite Fe2+S22-.

AB - Pyrite (FeS2) nanocrystals with a narrow size distribution and optical absorption from 1600 to 380 nm were synthesized in a single stage by reacting ferrous chloride with elemental sulfur in oleylamine (OAm) without an additional ligand. X-ray diffraction, Raman, and scanning electron microscopy showed that pyrite cubes with dimensions of 88 ± 14 nm formed at 200 C, an S to Fe ratio of 6, and 1 h reaction time in OAm. The time required to form phase pure pyrite depended on the S to Fe ratio. Phase purity was obtained in less than 1 h at a ratio of 6, but times as long as 24 h were necessary at a ratio of 2.75. The rate of pyrite formation increased with higher sulfur concentrations, which shows that molecules containing sulfur are involved in the rate-determining step. Both H2S and polysulfides of the form Sn2- are known to form in oleylamine. The slow step is the reaction between FeS and these molecules. Fe2+S2- undergoes nucleophilic attack by H2S and Sn2-; S2- converts to S- and sulfur is transferred forming pyrite Fe2+S22-.

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