In situ X-ray diffraction analysis of electrochemical Dy–Ni alloying in molten LiCl–KCl

Katasho, Yumi; Oishi, Tadashi

doi:10.1016/j.elecom.2022.107287

Cited by 5 publications

(8 citation statements)

References 28 publications

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“…In addition to the diffraction peaks, Dy fluorescence peaks were observed, which were similar to those observed in previous measurements. 17 Fluorescence peaks of Pb, Ta, and W were also detected, which were attributed to the materials used in the X-ray beamline.…”

Section: The Overview Results Of Edxrdmentioning

confidence: 92%

“…The in situ experiment was conducted in a similar manner as in the previous study. 17 Figure 1a shows the experimental equipment. Before the experiment, 35.0 g of LiCl-KCl (44 : 56 wt% eutectic melt, >99 % purity, Fujifilm Wako Pure Chemical Corp.) was placed in a 99 % graphite crucible shaped like an oval cylinder with an outer diameter (o.d.)…”

Section: In Situ Edxrdmentioning

confidence: 99%

“…The authors previously used in situ energy-dispersive X-ray diffraction (EDXRD) to investigate the formation of Dy-Ni alloys in molten LiCl-KCl. 17 EDXRD enables us to obtain the crystal structure of products in the thickness direction of plate every a few minutes in this study. The in situ analysis successfully obtained the diffraction pattern of DyNi 2 while eliminating the effects of water and air exposure and cooling on the working electrode.…”

Section: Introductionmentioning

confidence: 99%

“…The gauge volume was increased to improve the data quality and eliminate the issues encountered in the previous study. 17 To confirm the rapid formation of Dy-Ni at the grain boundaries, not only polycrystalline Ni plates but also single-crystal and annealed Ni plates were alloyed in molten salt, and the relationship between the crystal orientations of the Ni plate and formed alloys was examined. The crystal orientation of porous Ni formed by sequential alloying and de-alloying in molten salt was investigated.…”

Section: Introductionmentioning

confidence: 99%

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In Situ X-ray Diffraction and Crystal Orientation Analysis for Dy–Ni Electrochemical Alloying and De-alloying in Molten LiCl–KCl–DyCl<sub>3</sub>

KATASHO,

OISHI

2024

Electrochemistry

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In situ white X-ray diffraction was used to investigate the electrochemical alloying and de-alloying processes of Dy-Ni alloys in molten LiCl-KCl-DyCl 3 at 723 K. X-ray diffraction peaks of Ni and DyNi 2 and fluorescence peaks of Dy were obtained. DyNi 2 was the only identified Dy-Ni alloy, although previous ex situ studies have reported the formation of several Dy-Ni alloys. During the dealloying process, the apparent lattice constant of DyNi 2 decreased to a small value. Also, the area of Dy fluorescence peaks increased, which can be attributed to the formation of a Dy compound layer on the electrode surface. Electron backscatter diffraction was performed to clarify the relationship between the crystal orientations of Ni and DyNi 2 after electrochemical alloying or sequential alloying and de-alloying. The results confirmed that Dy-Ni alloying was faster at the Ni grain boundaries. In addition, DyNi 2 or porous Ni grains in reacted regions had similar crystal orientations as adjacent Ni grains in unreacted regions. These results help clarify the rapid electrochemical formation mechanism of Dy-Ni alloys in molten LiCl-KCl, which can help facilitate the separation and recovery of rare-earth elements, such as Dy, from spent magnets.

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Section: The Overview Results Of Edxrdmentioning

confidence: 92%

Section: In Situ Edxrdmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

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In Situ X-ray Diffraction and Crystal Orientation Analysis for Dy–Ni Electrochemical Alloying and De-alloying in Molten LiCl–KCl–DyCl<sub>3</sub>

KATASHO,

OISHI

2024

Electrochemistry

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“…At the same time, despite the advanced studies concerning the valence state, coordination form, and reduction process of tungsten ions, the fundamental physical properties of tungsten ion complexes are still under debate. Such situations have spurred the development of in situ characterization technologies that can track the dynamic reduction processes, capture short-lived intermediates, and reveal reaction mechanism, including in situ ultraviolet absorption spectroscopy (UV–vis), infrared spectroscopy (IR), and Raman spectroscopy (Ram). − …”

mentioning

confidence: 99%

In Situ Spectroscopic Identification and DFT-Assisted Prediction of the Valence and Structure of Tungsten Ions in a Cationic/Anionic Molten Salt System

Feng

Zhang

et al. 2023

J. Phys. Chem. C

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Understanding the reduction mechanism and coordination of tungsten ions in molten salt is one of the key factors to improve the electrolysis efficiency of tungsten carbide. In situ spectroscopy combined with simulation calculation is a strong analytical technique for characterizing chemical species and their behaviors in molten salts. The tungsten ion group was investigated by in situ high-temperature and room-temperature spectroscopy combined with density functional theory (DFT) calculations. For the described in situ spectroscopic studies, a new setup was used, which allowed the registration of UV−vis spectra of tungsten ions in cationic and anionic molten salt systems. The DFT calculation results proved useful for estimating the trend of experimental spectra. Through experimental and theoretical studies, the tungsten ion groups in various molten salt systems were identified, and the effect of cations and anions in molten salt systems onto tungsten ion group formation could be elucidated.

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In situ characterization techniques and methodologies for high-temperature electrochemistry

Yuan,

Jiao,

Zhu

et al. 2023

Chem

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In situ X-ray diffraction analysis of electrochemical Dy–Ni alloying in molten LiCl–KCl

Cited by 5 publications

References 28 publications

In Situ X-ray Diffraction and Crystal Orientation Analysis for Dy–Ni Electrochemical Alloying and De-alloying in Molten LiCl–KCl–DyCl<sub>3</sub>

In Situ X-ray Diffraction and Crystal Orientation Analysis for Dy–Ni Electrochemical Alloying and De-alloying in Molten LiCl–KCl–DyCl<sub>3</sub>

In Situ Spectroscopic Identification and DFT-Assisted Prediction of the Valence and Structure of Tungsten Ions in a Cationic/Anionic Molten Salt System

In situ characterization techniques and methodologies for high-temperature electrochemistry

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