Iron (III) sulfide particles produced by a polyol method

Shimizu, Ryo; Kubono, Ippei; Kobayashi, Yoshio; Yamada, Yasuhiro

doi:10.1007/s10751-014-1095-7

Cited by 11 publications

(7 citation statements)

References 15 publications

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“…While the detailed assignment of the doublet species cannot be unambiguously made with only Mossbauer parameters due to the diversity of species that are present, the observed parameters are in the range expected for mononuclear Fe− nitrogen species commonly present in iron ORR catalysts such as low-spin and high-spin FeN 4 type sites, as well as previously proposed Fe 2 N 5 binuclear sites. 11,12,15,38 For the sextet species, Sext 1 has parameters consistent with a bulk Fe−sulfide species (such as pyrrhotite 40,41 ) while Sext 2 is attributed to a bulk Fe− carbide species, similar to the previous observation of bulk sulfide and carbide species in PANI−Fe−C. 11 The minor singlet species is consistent with superparamagnetic Fe nanoparticles as previously assigned.…”

Section: ■ Results and Discussionsupporting

confidence: 85%

A Combined Probe-Molecule, Mössbauer, Nuclear Resonance Vibrational Spectroscopy, and Density Functional Theory Approach for Evaluation of Potential Iron Active Sites in an Oxygen Reduction Reaction Catalyst

et al. 2017

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Nonprecious metal M−N−C (M = Fe or Co) catalysts that are effective for the oxygen-reduction reaction in polymerelectrolyte fuel cells have been developed, but no consensus has yet been reached regarding the nature of the M sites in these heterogeneous catalysts that are responsible for the reaction with dioxygen (O 2 ). While multiple studies have developed correlations between Fe distributions in as-prepared catalysts and ORR activity, the direct identification of sites reactive toward O 2 or O 2 -analogue molecules remains a significant challenge. In the present study, we demonstrate a new approach to identifying and characterizing potential Fe active sites in complex ORR catalysts that combines an effective probe molecule (NO (g) ), Mossbauer spectroscopy, and nuclear resonance vibrational spectroscopy (NRVS) with density functional theory (DFT) calculations. Mossbauer spectroscopic studies demonstrate that NO (g) treatment of electrochemically reduced PANI− 57 Fe−C leads to a selective reaction with only a subset of the Fe species present. Nuclear resonance vibrational spectroscopic studies identified new Fe−ligand vibrations associated with the site reactive toward NO (g) . DFT calculations of the vibrational properties of a selection of previously proposed active-site structures suggest that graphene zigzag edge-hosted Fe−N structures may be responsible for the observed vibrational behavior with NO (g) probe molecules. Furthermore, such sites are likely also reactive to O 2 , possibly serving as the ORR active sites in the synthesized materials.

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Section: ■ Results and Discussionsupporting

confidence: 85%

A Combined Probe-Molecule, Mössbauer, Nuclear Resonance Vibrational Spectroscopy, and Density Functional Theory Approach for Evaluation of Potential Iron Active Sites in an Oxygen Reduction Reaction Catalyst

et al. 2017

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“…Mössbauer measurements revealed that surprisingly the sulfidation time has no significant impact on the amount of metallic iron remaining in the core‐shell particles (∼55% in 4 A – C ). The shell likely exhibits the Fe 2 S 2 and Fe 7 S 8 phases (as present in nanoflakes 2 and 3 ), and a further phase, which presumably can be attributed to the non‐stoichiometric iron sulfide Fe 1−X S (for details see ESI).…”

Section: Resultsmentioning

confidence: 99%

“…WAXS analyses of samples 5 A and 5 B confirm the presence of α‐iron, while Mössbauer studies strongly suggest the formation of a Fe 1−X S phase in the shell (ESI). Interestingly, the shell composition evolves with time: a relatively sulfur‐rich phase (Fe 2 S 3 ) was detected at the very beginning of the sulfidation process ( 5 B ) before disappearing at longer reaction time ( 5 A ). In the mean time, the amount of Fe(0) remains fairly constant (∼65%).…”

Section: Resultsmentioning

confidence: 99%

Controlling the Sulfidation Process of Iron Nanoparticles: Accessing Iron−Iron Sulfide Core‐Shell Structures

et al. 2018

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Iron sulfide nanocomposites have been prepared through reactions of bis[bis(trimethylsilyl)amido]iron(II) or zerovalent iron nanoparticles (NPs) with hydrogen sulfide gas. The chemical composition of these materials was analyzed by TEM, XRD, WAXS and Mö ssbauer measurements. Decomposition of bis[bis(trimethylsilyl)amido]iron(II) under an H 2 S atmosphere in the presence of palmitic acid produces thin iron sulfide nanoflakes, which seemingly consist of Fe 2 S 2 and Fe 7 S 8 . The sulfidation of 9 nm zerovalent iron NPs with H 2 S yields thin nano flakes exhibiting the same iron sulfide phases and residual iron. Remarkably, treatment of slightly larger iron NPs (13 nm) with H 2 S (or alternatively benzylthiol) yields wellshaped iron-iron sulfide core-shell particles. These particles exhibit a crystalline iron core and an amorphous iron sulfide shell, which likely consists of Fe 2 S 2 , Fe 7 S 8 and Fe 1ÀX S. Magnetic measurements on these core-shell particles show a decrease of the total magnetization (compared to bulk iron) coming along with the sulfidation process. Owing to the partially preserved ferromagnetic character these iron-iron sulfide core-shell particles were found to have magnetic heating properties.[a] Dr.

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“…The analysis of the gaseous stream containing H 2 S, O 2 , CH 4 , CO 2 , COS, CS 2 , SO 2 , H 2 , and N 2 (diluent) is performed with the mass spectrometer quadrupole (Hiden HPR-20). The CO measurement is not performed because the analysis is affected by interference due to N 2 having the same m/z ratio (28).…”

Section: Methodsmentioning

confidence: 99%

H₂S Oxidative Decomposition Reaction in the Presence of CH₄ over Metal-Sulfide-Based Catalysts: A Preliminary Investigation

Barba

Vaiano

Palma

et al. 2021

Ind. Eng. Chem. Res.

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Different alumina-supported metal sulfides catalysts were studied for the H 2 S oxidative decomposition reaction to simultaneously obtain sulfur and hydrogen in the presence of CH 4 . Mono and bimetallic catalysts were prepared, characterized, and tested at 1273 K by varying the contact time. X-ray diffraction and Raman evidenced a good dispersion of the Mo, Fe, and Co sulfide species on the Al 2 O 3 support. From the experimental results, it was argued that Mo sulfide species are the active phases able to inhibit the formation of SO 2 , while the Fe sulfide species promote the selective abatement of COS and CS 2 obtained because of the presence of CH 4 in the gaseous feed stream. The bimetallic sample containing both Mo and Fe sulfide species (5Fe-10Mo/Al 2 O 3 ) exhibited very interesting catalytic performances since it allowed us to achieve a H 2 yield, CH 4 , and H 2 S conversion very close to the equilibrium values and the complete removal of sulfur compounds at low contact times.

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Iron (III) sulfide particles produced by a polyol method

Cited by 11 publications

References 15 publications

A Combined Probe-Molecule, Mössbauer, Nuclear Resonance Vibrational Spectroscopy, and Density Functional Theory Approach for Evaluation of Potential Iron Active Sites in an Oxygen Reduction Reaction Catalyst

A Combined Probe-Molecule, Mössbauer, Nuclear Resonance Vibrational Spectroscopy, and Density Functional Theory Approach for Evaluation of Potential Iron Active Sites in an Oxygen Reduction Reaction Catalyst

Controlling the Sulfidation Process of Iron Nanoparticles: Accessing Iron−Iron Sulfide Core‐Shell Structures

H₂S Oxidative Decomposition Reaction in the Presence of CH₄ over Metal-Sulfide-Based Catalysts: A Preliminary Investigation

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Iron (III) sulfide particles produced by a polyol method

Cited by 11 publications

References 15 publications

A Combined Probe-Molecule, Mössbauer, Nuclear Resonance Vibrational Spectroscopy, and Density Functional Theory Approach for Evaluation of Potential Iron Active Sites in an Oxygen Reduction Reaction Catalyst

A Combined Probe-Molecule, Mössbauer, Nuclear Resonance Vibrational Spectroscopy, and Density Functional Theory Approach for Evaluation of Potential Iron Active Sites in an Oxygen Reduction Reaction Catalyst

Controlling the Sulfidation Process of Iron Nanoparticles: Accessing Iron−Iron Sulfide Core‐Shell Structures

H2S Oxidative Decomposition Reaction in the Presence of CH4 over Metal-Sulfide-Based Catalysts: A Preliminary Investigation

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H₂S Oxidative Decomposition Reaction in the Presence of CH₄ over Metal-Sulfide-Based Catalysts: A Preliminary Investigation