Synthesis of tetragonal mackinawite-type FeS nanosheets by solvothermal crystallization

Ian T. Sines; Dimitri D. Vaughn; Rajiv Misra; Eric J. Popczun; Raymond E. Schaak

doi:10.1016/j.jssc.2012.07.056

Synthesis of tetragonal mackinawite-type FeS nanosheets by solvothermal crystallization

Ian T. Sines, Dimitri D. Vaughn, Rajiv Misra, Eric J. Popczun, Raymond E. Schaak

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Abstract

Mackinawite, a metastable 1:1 compound of iron and sulfur that adopts an anti-PbO-type structure, is of interest because of its relationship to known iron chalcogenide superconductors, as well as its biogeochemical relevance. Colloidal nanosheets of mackinawite-type FeS were synthesized by first generating an amorphous Fe-S precursor via the aqueous room-temperature co-precipitation of Fe ² and S ^2-, then solvothermally crystallizing it in ethylene glycol at 200 °C in an autoclave. The product is highly crystalline, with lattice constants of a=3.674(3) Å and c=5.0354(3) Å. The nanosheets, with their surface normal oriented along the [0 0 1] direction, are irregularly faceted with edge lengths that range from 100 nm to over 1 μm and average thicknesses of approx. 30 nm. The samples showed a ferromagnetic background signal with no evidence of superconductivity.

Original language	English (US)
Pages (from-to)	17-20
Number of pages	4
Journal	Journal of Solid State Chemistry
Volume	196
DOIs	https://doi.org/10.1016/j.jssc.2012.07.056
State	Published - Dec 2012

All Science Journal Classification (ASJC) codes

Electronic, Optical and Magnetic Materials
Ceramics and Composites
Condensed Matter Physics
Physical and Theoretical Chemistry
Inorganic Chemistry
Materials Chemistry

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10.1016/j.jssc.2012.07.056

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title = "Synthesis of tetragonal mackinawite-type FeS nanosheets by solvothermal crystallization",

abstract = "Mackinawite, a metastable 1:1 compound of iron and sulfur that adopts an anti-PbO-type structure, is of interest because of its relationship to known iron chalcogenide superconductors, as well as its biogeochemical relevance. Colloidal nanosheets of mackinawite-type FeS were synthesized by first generating an amorphous Fe-S precursor via the aqueous room-temperature co-precipitation of Fe 2 and S 2-, then solvothermally crystallizing it in ethylene glycol at 200 °C in an autoclave. The product is highly crystalline, with lattice constants of a=3.674(3) {\AA} and c=5.0354(3) {\AA}. The nanosheets, with their surface normal oriented along the [0 0 1] direction, are irregularly faceted with edge lengths that range from 100 nm to over 1 μm and average thicknesses of approx. 30 nm. The samples showed a ferromagnetic background signal with no evidence of superconductivity.",

author = "Sines, {Ian T.} and Vaughn, {Dimitri D.} and Rajiv Misra and Popczun, {Eric J.} and Schaak, {Raymond E.}",

note = "Funding Information: This work was supported primarily by the U.S. Department of Energy, Office of Basic Energy Sciences, Division of Materials Sciences and Engineering , under Award No. DE-FG02–08ER46483 (I.T.S., E.J.P., R.E.S., materials synthesis and characterization). D.D.V. acknowledges support from an NSF Graduate Research Fellowship. R.M. (magnetic measurements) acknowledges support from the Penn State MRSEC (NSF DMR-0820404). TEM imaging was performed in the Electron Microscopy Facility of the Huck Institutes of the Life Sciences and HRTEM and AFM imaging were performed at the Materials Characterization Lab of the Penn State Materials Research Institute. The authors thank Prof. Peter Schiffer for helpful discussions about the magnetic measurements.",

year = "2012",

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doi = "10.1016/j.jssc.2012.07.056",

language = "English (US)",

volume = "196",

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journal = "Journal of Solid State Chemistry",

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publisher = "Academic Press Inc.",

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T1 - Synthesis of tetragonal mackinawite-type FeS nanosheets by solvothermal crystallization

AU - Sines, Ian T.

AU - Vaughn, Dimitri D.

AU - Misra, Rajiv

AU - Popczun, Eric J.

AU - Schaak, Raymond E.

N1 - Funding Information: This work was supported primarily by the U.S. Department of Energy, Office of Basic Energy Sciences, Division of Materials Sciences and Engineering , under Award No. DE-FG02–08ER46483 (I.T.S., E.J.P., R.E.S., materials synthesis and characterization). D.D.V. acknowledges support from an NSF Graduate Research Fellowship. R.M. (magnetic measurements) acknowledges support from the Penn State MRSEC (NSF DMR-0820404). TEM imaging was performed in the Electron Microscopy Facility of the Huck Institutes of the Life Sciences and HRTEM and AFM imaging were performed at the Materials Characterization Lab of the Penn State Materials Research Institute. The authors thank Prof. Peter Schiffer for helpful discussions about the magnetic measurements.

PY - 2012/12

Y1 - 2012/12

N2 - Mackinawite, a metastable 1:1 compound of iron and sulfur that adopts an anti-PbO-type structure, is of interest because of its relationship to known iron chalcogenide superconductors, as well as its biogeochemical relevance. Colloidal nanosheets of mackinawite-type FeS were synthesized by first generating an amorphous Fe-S precursor via the aqueous room-temperature co-precipitation of Fe 2 and S 2-, then solvothermally crystallizing it in ethylene glycol at 200 °C in an autoclave. The product is highly crystalline, with lattice constants of a=3.674(3) Å and c=5.0354(3) Å. The nanosheets, with their surface normal oriented along the [0 0 1] direction, are irregularly faceted with edge lengths that range from 100 nm to over 1 μm and average thicknesses of approx. 30 nm. The samples showed a ferromagnetic background signal with no evidence of superconductivity.

AB - Mackinawite, a metastable 1:1 compound of iron and sulfur that adopts an anti-PbO-type structure, is of interest because of its relationship to known iron chalcogenide superconductors, as well as its biogeochemical relevance. Colloidal nanosheets of mackinawite-type FeS were synthesized by first generating an amorphous Fe-S precursor via the aqueous room-temperature co-precipitation of Fe 2 and S 2-, then solvothermally crystallizing it in ethylene glycol at 200 °C in an autoclave. The product is highly crystalline, with lattice constants of a=3.674(3) Å and c=5.0354(3) Å. The nanosheets, with their surface normal oriented along the [0 0 1] direction, are irregularly faceted with edge lengths that range from 100 nm to over 1 μm and average thicknesses of approx. 30 nm. The samples showed a ferromagnetic background signal with no evidence of superconductivity.

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Synthesis of tetragonal mackinawite-type FeS nanosheets by solvothermal crystallization

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