Iron (III) sulfide particles produced by a polyol method
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Iron (III) sulfide particles produced by a polyol method Ryo Shimizu · Ippei Kubono · Yoshio Kobayashi · Yasuhiro Yamada
Received: 18 September 2014 / Accepted: 6 November 2014 © Springer International Publishing Switzerland 2014
Abstract Iron(III) sulfide Fe2 S3 particles were produced using a polyol method. Although pyrrhotite Fe1−x S appeared together with Fe2 S3 , the relative yield of Fe2 S3 changed when the concentration of reagents in the oleylamine changed. M¨ossbauer spectra of the particles showed superparamagnetic doublets due to Fe2 S3 at 293 K, along with a hyperfine magnetic splitting of H = 24.7 T at 6 K. XRD patterns of the Fe2 S3 suggested a structure similar to that of greigite Fe3 S4 . Keywords Iron(III) sulfide · Polyol method · Nanoparticles · X-ray diffraction · Hyperfine magnetic field
1 Introduction The iron sulfides of pyrite FeS2 , marcasite FeS2 , and pyrrhotite Fe1−x S are commonly available iron(II) compounds. While Fe3 S4 has been well investigated, iron(III) sulfides are generally unstable under conventional conditions. The possible significance of Fe2 S3 as a catalyst for coal liquefaction has attracted considerable recent attention [1, 2]. Metastable iron(III) sulfide Fe2 S3 has been studied for a long time, but its detailed structure and
Proceedings of the 5th Joint International Conference on Hyperfine Interactions and International Symposium on Nuclear Quadrupole Interactions (HFI/NQI 2014) Canberra, Australia, 21-26 September 2014 R. Shimizu · I. Kubono · Y. Yamada () Tokyo University of Science, 1-3 Kagurazaka, Shinjuku-ku, Tokyo 162-8601, Japan e-mail: [email protected] Y. Kobayashi The University of Electro-Communications, 1-5-1 Chofugaoka, Chofu, Tokyo 182-8585, Japan Y. Kobayashi RIKEN, 2-1 Hirosawa, Wako, Saitama 351-0198, Japan
R. Shimizu et al.
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Fig. 1 SEM images of iron sulfide particles
magnetic nature remain unclear. XRD patterns of iron(III) sulfide synthesized in solution have suggested a tetragonal system [3]. Fe2 S3 formed by mixing ferric chloride and ammo˚ [4, 5]. A nium sulfide was found to have a spinel structure with a lattice size of 9.87 A M¨ossbauer spectrum of amorphous Fe2 S3 had hyperfine magnetic splitting of 25.3 (6) T at 4.2 K [6]. EXAFS of Fe2 S3 has also been measured [7]. The magnetic properties and structures of metastable Fe2 S3 embedded in pyrrhotite have been discussed [8], and it has been proposed that Fe2 S3 has a hexagonal structure with ferromagnetic properties. Recently, Lyubutin et al. prepared Fe1−x S nanoparticles by thermal decomposition of a mixture of iron-oleylamine and sulfur oleylamine [9], and Fe3 S4 nanoparticles were also synthesized by a polyol process [10]. It was further reported that small particles (
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