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Synthesis and Characterization of Tungsten Amide Complexes for the Deposition of Tungsten Disulfide Thin Films.

ABSTRACT: To substitute corrosive halogen ligands, we designed and synthesized novel tungsten complexes containing amido ligands, W(DMEDA)₃ (1) and W(DEEDA)₃ (2) (DMEDA = N,N'-dimethylethylenediamido; DEEDA = N,N'-diethylethylenediamido). Complexes 1 and 2 were characterized by ¹H NMR, ¹³C NMR, FT-IR, and elemental analysis. The pseudo-octahedral molecular structure of 1 was confirmed by single-crystal X-ray crystallography. The thermal properties of 1 and 2 were analyzed by thermogravimetric analysis (TGA), which confirmed that the precursors were volatile and exhibited adequate thermal stability. Additionally, the WS₂ deposition test was performed using 1 in thermal chemical vapor deposition (thermal CVD). Further analysis of the surface of the thin films was conducted using Raman spectroscopy, scanning electron microscopy (SEM), and X-ray photoelectron spectroscopy (XPS).

SUBMITTER: Son JY

PROVIDER: S-EPMC10249077 | biostudies-literature | 2023 Jun

REPOSITORIES: biostudies-literature

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Synthesis and Characterization of Tungsten Amide Complexes for the Deposition of Tungsten Disulfide Thin Films.

Son Ji Young JY Kim Su Han SH Seo Ji Min JM Lim Jongsun J Chung Taek-Mo TM Park Bo Keun BK

ACS omega 20230524 22

To substitute corrosive halogen ligands, we designed and synthesized novel tungsten complexes containing amido ligands, W(DMEDA)3 (1) and W(DEEDA)3 (2) (DMEDA = N,N'-dimethylethylenediamido; DEEDA = N,N'-diethylethylenediamido). Complexes 1 and 2 were characterized by 1H NMR, 13C NMR, FT-IR, and elemental analysis. The pseudo-octahedral molecular structure of 1 was confirmed by single-cryst ...[more]

PMID: 37305263

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Project description:This study aimed to investigate the structural, optical, and electronic properties of WO3 thin films modified by Ta-doping, considering their potential application in photoelectrochemical (PEC) water splitting. Due to its unique physical and chemical properties, WO3 films have been commonly suggested as a promising photoanode for hydrogen production. However, the wide bandgap and unsuitable band edge positions of WO3 limit its PEC efficiency. Doping have been extensively applied as an effective strategy for bandgap engineering. Here, post-annealed WO3 films with different concentrations of Ta dopant were synthesized via reactive magnetron co-sputtering, while DC and RF sputtering powers were varied with the aim of achieving the desired properties. EDX analysis showed that Ta atoms were doped into WO3 in the range of 0-3.93 at%. As evident from SEM and AFM images, the surface morphology was significantly affected by increasing Ta doping, the formation of a granular structure with well-defined boundaries and increasing surface roughness (1.79-47.94 nm). XRD patterns confirmed that the incorporation of Ta atoms into a monoclinic WO3 improved the crystallinity, especially in the (002) direction. Most importantly, a decrease in the average transparency (92.82-74.27%), an increase in visible absorption, a red shift of the fundamental absorption edge corresponding to a favorable drop in the optical bandgap energy (3.07-2.61 eV) were found with increasing Ta concentration. Notably, the substitution of W6+ ions with Ta dopant (0-3.93 at%) led to an upward shift in the valence band maximum (3.62-3.31 eV) and a downward shift in the conduction band minimum (0.55-0.70 eV). The WO3 photoanode doped with 3.93 at% Ta exhibited the maximum photocurrent density of 0.65 mA/cm2 (at 1 V vs. Ag/AgCl) under simulated sunlight. Furthermore, WO3 photoanode doped with 3.93 at% Ta showed excellent photoresponsivity and slow electron-hole recombination. The obtained results predict the potential of Ta-doping coupled with post-annealing to optimize the structural and optoelectronic properties of sputtered WO3 thin films as photoanode for use in efficient PEC water splitting.

Dataset Information

Synthesis and Characterization of Tungsten Amide Complexes for the Deposition of Tungsten Disulfide Thin Films.

Publications

Synthesis and Characterization of Tungsten Amide Complexes for the Deposition of Tungsten Disulfide Thin Films.

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