Selective morphological analysis of cerium metal in electrodeposit recovered from molten LiCl-KCl eutectic by radiography and computed tomography

Jee, Young Taek; Park, Mi-Ran; Cho, Seungryong; Yun, Jong-Il

doi:10.1038/s41598-018-38022-3

Cited by 9 publications

(4 citation statements)

References 27 publications

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“…Interestingly, a gradual increase in current density is observed only in the chronoamperogram of the OTF À -based electrolyte (Figure 2D), whereas a current plateau is recorded for the Cl À -based electrolyte. The increase in current densities during chronoamperometry experiments has been attributed to an increase in the electroactive surface area, [79,80] which in this case could be associated with the increase in the concentration of free H À at the interfaces that occurs as a result of continuous Al plating.…”

Section: Plating and Characterization Of Aluminum Depositsmentioning

confidence: 98%

Hydride‐Enhanced Plating and Stripping of Aluminum from Triflate‐based Organic Electrolytes**

Slim

Menke

2023

Batteries & Supercaps

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In the quest for developing rechargeable aluminum (Al) batteries, reversible Al plating in the absence of active‐halide components is considered an immense challenge. For this reason, the choice of electrolyte has been primarily limited to the highly corrosive chloroaluminate systems based on aluminum trichloride (AlCl3). In this work, we demonstrate reversible room‐temperature Al plating from an active‐halide‐free (AHF) organic electrolyte based on aluminum trifluoromethanesulfonate (Al(OTF)3) and lithium aluminum hydride (LiAlH4) in tetrahydrofuran (THF), as well as its AlCl3 counterpart. From insights obtained by Density Functional Theory (DFT) and Fourier‐Transform Infrared (FTIR) spectroscopy, ionic speciation in the electrolyte is explored, and mechanisms for the underlying electrochemical processes in the trifluoromethanesulfonate (OTF−)‐based electrolytes are proposed. Al plating and stripping were confirmed by optical microscopy, scanning electron microscopy (SEM) and X‐ray diffraction (XRD). Characterizing the Al deposits from either the OTF−‐ or the chloride (Cl−)‐based electrolytes via depth‐profile X‐ray Photoelectron Spectroscopy (XPS) analyses, we find that these deposits consist of metallic Al, aluminum oxide (Al2O3), and either aluminum trifluoride (AlF3) or aluminum chloride (AlxCly) contaminants arising from a reaction with the electrolyte components which occurs during the plating process.

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Section: Plating and Characterization Of Aluminum Depositsmentioning

confidence: 98%

Hydride‐Enhanced Plating and Stripping of Aluminum from Triflate‐based Organic Electrolytes**

Slim

Menke

2023

Batteries & Supercaps

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“…Recently, Chen-Wiegart and co-workers ( 15 ) used in situ 3D x-ray m-CT to study dealloying by settling the sample in heated molten salt. Nevertheless, there is still a lack of in situ or operando techniques for investigating electrode kinetics in high-temperature electrochemical systems due to the extremely harsh operating environment; thus, parameter optimization of high-temperature electrochemical processes is unfortunately still based on empirical work ( 16 , 17 ).…”

Section: Introductionmentioning

confidence: 99%

A 4D x-ray computer microtomography for high-temperature electrochemistry

Jiao

et al. 2022

Sci. Adv.

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High-temperature electrochemistry is widely used in many fields. However, real-time observations and an in-depth understanding of the inside evolution of this system from an experimental perspective remain limited because of harsh reaction conditions and multiphysics fields. Here, we tackled this challenge with a high-temperature electrolysis facility developed in-house. This facility permits in situ x-ray computer microtomography (μ-CT) for nondestructive and quantitative three-dimensional (3D) imaging. In an electrorefining system, the μ-CT probed the dynamic evolution of 3D morphology and components of electrodes (4D). Subsequently, this 4D process was visually presented via reconstructed images. The results monitor the efficiency of the process, explore the dynamic mechanisms, and even offer real-time optimization. This 4D analysis platform is notable for in-depth combinations of traditional electrochemistry with digital twin technologies owing to its multiscale visualization and high efficiency of data extraction.

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“…[ 17 , 18 ] Subsequently, various studies based on ex situ and in situ X‐ray techniques were employed in the electrochemistry. For instance, Young Taek Jeek and coworkers [ 18 ] investigated microstructure evolution of the electrodeposits during electroreduction processes by using ex situ X‐ray computed tomography. On the other hand, other researchers recently used in situ X‐ray techniques to demonstrate the dynamic processes of electrodes in the energy industry.…”

Section: Introductionmentioning

confidence: 99%

“…On the other hand, other researchers recently used in situ X-ray techniques to demonstrate the dynamic processes of electrodes in the energy industry. [19][20][21] Aiming to operando monitoring and analyzing the electrodeposition process, in the present contribution, we employ an Xray tomography technique to open the "black box" via establishing the four-dimensional (4D) visualization methodology (in situ evolution of three-dimensional (3D) spatial imaging with time), aiming to operando monitor and analyze the electrodeposition process. With the unique advantages on sufficient penetration capacity [22][23][24] and non-destructive and non-contact features, the X-ray tomography allows for reconstructing the growth process of the deposited metal dendrites timely.…”

Section: Introductionmentioning

confidence: 99%

Quantificational 4D Visualization of Industrial Electrodeposition

Jiao

et al. 2021

Advanced Science

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Electrodeposition is a fundamental technology in modern society and has been widely used in metal plating and extraction, etc. However, extreme reaction conditions, including wide operation temperature ranges and corrosive media (molten salt/oxide systems as a particular example), inhibit direct in situ observation of the electrodeposition process. To visualize the electrode kinetics in such "black box," X-ray tomography is employed to monitor the electrochemical processes and three-dimensional (3D) evolution of morphology. Benefiting from the excellent penetration of X-ray, a non-destructive and non-contact in situ four-dimensional (4D) visualization of Ti deposition is realized. Real-time 3D reconstructed images reveal that the counterintuitive nucleation and growth process of a mesoscale Ti dendrite at both solid and liquid cathodes. According to 3D morphology evolution, unusual mechanism based on synergetic effect of the diffusion of metallic Ti and local field enhancement is achieved utilizing a simulation method based on a finite element method. This approach allows for timely and accurately regulating the electrodeposition process upon in situ monitored parameters. More importantly, the 4D technique upon operando X-ray tomography and numerical simulation can be easily applied to other electrodeposition systems, which will help deeply understand the internal kinetics and the precise optimization of the electrodeposition conditions.

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Selective morphological analysis of cerium metal in electrodeposit recovered from molten LiCl-KCl eutectic by radiography and computed tomography

Cited by 9 publications

References 27 publications

Hydride‐Enhanced Plating and Stripping of Aluminum from Triflate‐based Organic Electrolytes**

Hydride‐Enhanced Plating and Stripping of Aluminum from Triflate‐based Organic Electrolytes**

A 4D x-ray computer microtomography for high-temperature electrochemistry

Quantificational 4D Visualization of Industrial Electrodeposition

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