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Synthesis of Mixed-Valent Lanthanide Sulfide Nanoparticles.

ABSTRACT: In targeting reduced valent lanthanide chalcogenides, we report the first nanoparticle synthesis of the mixed-valent ferromagnets Eu₃ S₄ and EuSm₂ S₄ . Using divalent lanthanide halides with bis(trimethylsilyl)sulfide and oleylamine, we prepared nanoparticles of EuS, Eu₃ S₄ , EuSm₂ S₄ , SmS_1.9 , and Sm₃ S₄ . All nanoparticle phases were identified using powder X-ray diffraction, transmission electron microscopy was used to confirm morphology and nanoparticle size, and magnetic susceptibility measurements for determining the ordering temperatures and valence. The UV/Vis, Raman and X-ray photoelectron spectroscopies for each phase were compared. Surprisingly, the phase is influenced by the halide and the reaction temperature, where EuCl₂ formed EuS while EuI₂ formed Eu₃ S₄ , highlighting the role of kinetics in phase stabilization. Interestingly, at lower temperatures EuI₂ initially forms EuS, and converts over time to Eu₃ S₄ .

SUBMITTER: Glaser P

PROVIDER: S-EPMC10387447 | biostudies-literature | 2021 Oct

REPOSITORIES: biostudies-literature

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Synthesis of Mixed-Valent Lanthanide Sulfide Nanoparticles.

Glaser Priscilla P Stewart Orlando O Atif Rida R Asuigui Dane Romar C DRC Swanson Joel J Biacchi Adam J AJ Hight Walker Angela R AR Morrison Gregory G Zur Loye Hans-Conrad HC Stoll Sarah L SL

Angewandte Chemie (International ed. in English) 20210917 43

In targeting reduced valent lanthanide chalcogenides, we report the first nanoparticle synthesis of the mixed-valent ferromagnets Eu3 S4 and EuSm2 S4 . Using divalent lanthanide halides with bis(trimethylsilyl)sulfide and oleylamine, we prepared nanoparticles of EuS, Eu3 S4 , EuSm2 S4 , SmS1.9 , and Sm3 S4 . All nanoparticle phases were identified using powder X-ray diffractio ...[more]

PMID: 34424583

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Project description:Studies on cerium oxo clusters (CeOCs) are not only significant for understanding the redox and hydrolysis behaviors of Ce(III/IV) ions but also crucial for the rational synthesis of novel clusters and nanoceria with specific Ce(III)/Ce(IV) ratios. Here, two sets of reactions were conducted using cerium nitrate and H2O2-oxidized cerium nitrate, resulting in the formation of two distinct mixed-valent CeOCs [CeIII 4CeIV 10O14(OH)2(PhCO2)22(DMF)6] (Ce14) and [CeIII 2CeIV 22O28(OH)8(PhCO2)30(DMF)4] (Ce24C). These two clusters exhibit different structures and Ce(III)/Ce(IV) ratios, demonstrating the critical role of cerium oxidation states and the occurrence of redox reactions in cluster formation. Ce14 is the first tetradecanuclear CeOC with a novel structure, whereas Ce24C differed in its Ce(III)/Ce(IV) ratio, protonation levels of O atoms, and ligands from previously reported 24-nuclear CeOCs. Furthermore, various techniques were employed to investigate the formation process of these two clusters. X-ray photoelectron spectra (XPS) revealed that the white precipitates formed during the preparation of Ce14 contain Ce(III) ions, while the reddish-brown precipitates formed during the preparation of Ce24C contain a mixture of Ce(III) and Ce(IV) ions. These two precipitations were individually dissolved in N,N-Dimethylformamide (DMF). The evolution of solution color and ultraviolet-visible (UV-Vis) spectra over time revealed the gradual oxidation of partial Ce(III) ions by oxygen in the solution of the white precipitation. As Ce(IV) ions increased in this solution, time-resolved small angle X-ray scattering (SAXS) data demonstrated the self-assembly of the Ce14 clusters after 4 days. In contrast, SAXS data and UV-Vis spectra revealed the rapid assembly of Ce24C clusters within 2 h due to the initial coexistence of Ce(IV) and Ce(III) ions in the DMF solution of the reddish-brown precipitation. The continued reduction of partial Ce(IV) ions in this solution does not affect Ce24C clusters' formation and stability. Our studies expand the family of CeOCs and enhance our understanding of the effects of cerium's oxidation states on cluster formation.

Dataset Information

Synthesis of Mixed-Valent Lanthanide Sulfide Nanoparticles.

Publications

Synthesis of Mixed-Valent Lanthanide Sulfide Nanoparticles.

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