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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{sup 2+} and S{sup 2-}, then solvothermally crystallizing it in ethylene glycol at 200 Degree-Sign C in an autoclave. The product is highly crystalline, with lattice constants of a=3.674(3) A and c=5.0354(3) A. 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 {mu}m and average thicknesses of approx. 30 nm. The samples showed a ferromagnetic background signal with no evidence of superconductivity. - Grahpical abstract: Single-crystal colloidal nanosheets of mackinawite-type FeS were synthesized by the solvothermal crystallization of an amorphous Fe-S precursor. Highlights: Black-Right-Pointing-Pointer Aqueous co-precipitation yields an amorphous Fe-S precursor. Black-Right-Pointing-Pointer The amorphous precursor solvothermally crystallizes to form metastable mackinawite. Black-Right-Pointing-Pointer Mackinawite-type FeS forms as single crystal colloidal nanosheets. Black-Right-Pointing-Pointer Samples are ferromagnetic with no evidence of superconductivity.

Authors:
;  [1];  [2];  [1]
  1. Pennsylvania State University, Department of Chemistry, 104 Chemistry Building, University Park, PA 16802 (United States)
  2. Pennsylvania State University, Department of Physics, University Park, PA 16802 (United States)
Publication Date:
OSTI Identifier:
22149905
Resource Type:
Journal Article
Journal Name:
Journal of Solid State Chemistry
Additional Journal Information:
Journal Volume: 196; Other Information: Copyright (c) 2012 Elsevier Science B.V., Amsterdam, The Netherlands, All rights reserved.; Country of input: International Atomic Energy Agency (IAEA); Journal ID: ISSN 0022-4596
Country of Publication:
United States
Language:
English
Subject:
37 INORGANIC, ORGANIC, PHYSICAL AND ANALYTICAL CHEMISTRY; 77 NANOSCIENCE AND NANOTECHNOLOGY; CHEMICAL PREPARATION; COPRECIPITATION; CRYSTALLIZATION; IRON SULFIDES; MONOCRYSTALS; NANOSTRUCTURES; SUPERCONDUCTIVITY

Citation Formats

Sines, Ian T., Vaughn, II, Dimitri D., Misra, Rajiv, Materials Research Institute, The Pennsylvania State University, University Park, PA 16802, Popczun, Eric J., Schaak, Raymond E., E-mail: schaak@chem.psu.edu, and Materials Research Institute, The Pennsylvania State University, University Park, PA 16802. Synthesis of tetragonal mackinawite-type FeS nanosheets by solvothermal crystallization. United States: N. p., 2012. Web. doi:10.1016/J.JSSC.2012.07.056.
Sines, Ian T., Vaughn, II, Dimitri D., Misra, Rajiv, Materials Research Institute, The Pennsylvania State University, University Park, PA 16802, Popczun, Eric J., Schaak, Raymond E., E-mail: schaak@chem.psu.edu, & Materials Research Institute, The Pennsylvania State University, University Park, PA 16802. Synthesis of tetragonal mackinawite-type FeS nanosheets by solvothermal crystallization. United States. doi:10.1016/J.JSSC.2012.07.056.
Sines, Ian T., Vaughn, II, Dimitri D., Misra, Rajiv, Materials Research Institute, The Pennsylvania State University, University Park, PA 16802, Popczun, Eric J., Schaak, Raymond E., E-mail: schaak@chem.psu.edu, and Materials Research Institute, The Pennsylvania State University, University Park, PA 16802. Sat . "Synthesis of tetragonal mackinawite-type FeS nanosheets by solvothermal crystallization". United States. doi:10.1016/J.JSSC.2012.07.056.
@article{osti_22149905,
title = {Synthesis of tetragonal mackinawite-type FeS nanosheets by solvothermal crystallization},
author = {Sines, Ian T. and Vaughn, II, Dimitri D. and Misra, Rajiv and Materials Research Institute, The Pennsylvania State University, University Park, PA 16802 and Popczun, Eric J. and Schaak, Raymond E., E-mail: schaak@chem.psu.edu and Materials Research Institute, The Pennsylvania State University, University Park, PA 16802},
abstractNote = {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{sup 2+} and S{sup 2-}, then solvothermally crystallizing it in ethylene glycol at 200 Degree-Sign C in an autoclave. The product is highly crystalline, with lattice constants of a=3.674(3) A and c=5.0354(3) A. 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 {mu}m and average thicknesses of approx. 30 nm. The samples showed a ferromagnetic background signal with no evidence of superconductivity. - Grahpical abstract: Single-crystal colloidal nanosheets of mackinawite-type FeS were synthesized by the solvothermal crystallization of an amorphous Fe-S precursor. Highlights: Black-Right-Pointing-Pointer Aqueous co-precipitation yields an amorphous Fe-S precursor. Black-Right-Pointing-Pointer The amorphous precursor solvothermally crystallizes to form metastable mackinawite. Black-Right-Pointing-Pointer Mackinawite-type FeS forms as single crystal colloidal nanosheets. Black-Right-Pointing-Pointer Samples are ferromagnetic with no evidence of superconductivity.},
doi = {10.1016/J.JSSC.2012.07.056},
journal = {Journal of Solid State Chemistry},
issn = {0022-4596},
number = ,
volume = 196,
place = {United States},
year = {2012},
month = {12}
}