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Title: Microwave-assisted synthesis of iron sulfide motifs for electrochemical applications

Journal Article · · JPhys Materials
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  1. State Univ. of New York (SUNY) at Stony Brook, NY (United States)
  2. Brookhaven National Laboratory (BNL), Upton, NY (United States). Center for Functional Nanomaterials (CFN)
  3. State Univ. of New York (SUNY) at Stony Brook, NY (United States); Brookhaven National Laboratory (BNL), Upton, NY (United States)
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The syntheses of FeS2 and Fe3S4 nanomaterials were optimized using a novel facile, surfactant-free, and microwave-assisted, one-pot synthesis method, run under ambient and reasonably mild reaction conditions. Synthetic parameters, such as metal precursor salt identity, reaction time, reaction temperature, metal:sulfur molar ratios, and solvent combinations, were all systematically investigated and optimized. A series of FeS2 (pyrite) samples was initially fabricated using thioacetamide (TAA) as the sulfur precursor to generate a distinctive, uniform octahedra-based morphology. Switching the sulfur precursor from TAA to L-cysteine resulted in a corresponding transformation in not only chemical composition from FeS2 to an iron thiospinel structure, Fe3S4 (otherwise known as greigite), but also an associated morphological evolution from octahedra to nanosheet aggregates. The study of these materials has enabled crucial insights into the formation mechanisms of these materials under a relatively non-conventional microwave-assisted setting. Furthermore, in separate experiments, multi-walled carbon nanotubes (MWNTs) and graphene were added in with underlying metal sulfide species to create conductive Fe–S/MWNT composites and Fe–S/graphene composites, respectively. The method of addition of either MWNTs or graphene was also explored, wherein an 'ex-situ' synthetic procedure was found to be the least disruptive means of attachment and immobilization onto iron sulfide co-reagents as a means of preserving the latter's inherent composition and morphology. The redox acidity for the parent material and associated composites demonstrates the utility of our as-developed synthetic methods for creating motifs relevant for electrochemical applications, such as energy storage.

Research Organization:
Brookhaven National Laboratory (BNL), Upton, NY (United States); Energy Frontier Research Centers (EFRC) (United States). Center for Mesoscale Transport Properties (m2M)
Sponsoring Organization:
USDOE Office of Science (SC), Basic Energy Sciences (BES); USDOE
Grant/Contract Number:
SC0012704; SC0012673
OSTI ID:
1971710
Alternate ID(s):
OSTI ID: 2382638
Report Number(s):
BNL-225758-2024-JAAM
Journal Information:
JPhys Materials, Vol. 6, Issue 2; ISSN 2515-7639
Publisher:
IOP PublishingCopyright Statement
Country of Publication:
United States
Language:
English

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25 ENERGY STORAGE
microwave synthesis
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metal sulfide
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