Microwave-assisted synthesis of iron sulfide motifs for electrochemical applications

IF 2.9 4区 物理与天体物理 Q2 OPTICS Journal of Nonlinear Optical Physics & Materials Pub Date : 2023-04-01 DOI:10.1088/2515-7639/accc56
Kenna L. Salvatore, Christopher R. Tang, Edelmy Marin Bernardez, Weiqiao Wesley, Justin Fang, Katherine Lee, Ariadna Paltis, Chloe Nevers, S. Mcguire, Nathaniel Hurley, Xiao Tong, E. Takeuchi, K. Takeuchi, A. Marschilok, Stanislaus S. Wong
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Abstract

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.
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微波辅助合成硫化铁基序的电化学应用
采用一种简单、无表面活性剂、微波辅助的一锅合成方法,在环境和合理温和的反应条件下,优化了FeS2和Fe3S4纳米材料的合成。对金属前驱体盐特性、反应时间、反应温度、金属硫摩尔比、溶剂组合等合成参数进行了系统的研究和优化。采用硫乙酰胺(TAA)作为硫前驱体制备了一系列FeS2(黄铁矿)样品,以产生独特、均匀的八面体形态。将硫前体从TAA转换为l -半胱氨酸,不仅导致了化学成分从FeS2到铁硫尖晶石结构Fe3S4(也称为灰色长晶石)的相应转变,而且导致了从八面体到纳米片聚集体的相关形态演变。对这些材料的研究使人们能够在相对非常规的微波辅助环境下对这些材料的形成机制有重要的了解。此外,在单独的实验中,将多壁碳纳米管(MWNTs)和石墨烯与底层金属硫化物物质一起添加,分别制备了导电的Fe-S /MWNT复合材料和Fe-S /石墨烯复合材料。研究人员还探索了添加MWNTs或石墨烯的方法,其中发现“非原位”合成程序是最不具破坏性的附着和固定在硫化铁共试剂上的方法,可以保留后者的固有组成和形态。母体材料和相关复合材料的氧化还原酸度证明了我们开发的合成方法在创建与电化学应用相关的基序(如能量存储)方面的实用性。
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来源期刊
CiteScore
3.00
自引率
48.10%
发文量
53
审稿时长
3 months
期刊介绍: This journal is devoted to the rapidly advancing research and development in the field of nonlinear interactions of light with matter. Topics of interest include, but are not limited to, nonlinear optical materials, metamaterials and plasmonics, nano-photonic structures, stimulated scatterings, harmonic generations, wave mixing, real time holography, guided waves and solitons, bistabilities, instabilities and nonlinear dynamics, and their applications in laser and coherent lightwave amplification, guiding, switching, modulation, communication and information processing. Original papers, comprehensive reviews and rapid communications reporting original theories and observations are sought for in these and related areas. This journal will also publish proceedings of important international meetings and workshops. It is intended for graduate students, scientists and researchers in academic, industrial and government research institutions.
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