Preparation of Mg-Zr alloys through direct electro-deoxidation of MgO-ZrO2 in CaCl2-NaCl molten salt

Li, Na; Peng, Yaru; Xiong, Wentao; Sun, Jiaqi; Chen, Yiming; Zhang, Putao; Liu, Meiyue; Li, Shengjun

doi:10.1016/j.electacta.2021.137816

Cited by 13 publications

(15 citation statements)

References 28 publications

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“…Recently, Li et al studied the CV of ZrO 2 in CaCl 2 -NaCl melt using MCE at 600 o C and reported two cathodic peaks prior to Ca deposition. 41 Based on literature data, the reduction peak currents at c 1 and c 2 could be attributed to the reduction of ZrO 2 to Zr x O and Zr x O (x ⩾2) to Zr, respectively. Equations 1 and 2 represent the cathodic reactions of ZrO 2 prior to calcium deposition.…”

Section: Resultsmentioning

confidence: 92%

Electrochemical Preparation of ZrFe₂ and ZrFe_1.8Ni_0.2 Intermetallic Compounds by FFC Cambridge Process

Khan,

Mukherjee,

Shakila

et al. 2023

J. Electrochem. Soc.

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The aim of the present study was to prepare ZrFe2 and ZrFe1.8Ni0.2 intermetallic compounds by FFC Cambridge process. The intermetallic compounds were prepared directly from the mixed oxide precursors, namely ZrO2-Fe2O3 and ZrO2-Fe2O3-NiO, respectively. Electrochemical de-oxidation experiments were carried out with mixed oxide pellet cathode and HD graphite anode by applying a constant cell voltage of 3.1 V in CaCl2 melt at 900 oC. The electrochemical behaviour of oxides was studied by cyclic voltammetry using metallic cavity electrodes (MCEs). The electrolysis was carried out for different durations of time to understand the mechanistic pathway of reduction of ZrO2-Fe2O3. The electro-reduced products were characterized by X-ray diffraction (XRD) technique, scanning electron microscope (SEM) and energy dispersive X-ray spectroscopy (EDS). The reduction intermediates involved Fe, CaZrO3, calcia stabilised zirconia (CSZ), Fe23Zr6, Zr6Fe3O and Zr2Fe. Single cubic C15 phase of ZrFe2 was obtained in 48 h electrolysis product. ZrFe1.8Ni0.2 was also electrochemically synthesized from its oxide precursors viz. ZrO2, Fe2O3 and NiO. Apart from ZrFe1.8Ni0.2 phase, the electro-reduced products had a Zr2Ni phase even after 72 h of electrolysis.

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Section: Resultsmentioning

confidence: 92%

Electrochemical Preparation of ZrFe₂ and ZrFe_1.8Ni_0.2 Intermetallic Compounds by FFC Cambridge Process

Khan,

Mukherjee,

Shakila

et al. 2023

J. Electrochem. Soc.

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“…Since Na is volatile, the peak D' is smaller than the reduced peak D. Since CaCl2 also has a certain degree of water absorption in molten salt, the formation of CaO causes the peak F to be relatively gentle. The formation of the peak F' is mainly due to the oxidation of the elemental Ca [22]. Peak E' corresponds to the oxidation of Cl − .…”

Section: Experimental Methodsmentioning

confidence: 99%

Electrochemical Mechanism of Recovery of Nickel Metal from Waste Lithium Ion Batteries by Molten Salt Electrolysis

Liang

et al. 2021

Materials

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With the widespread use of lithium-ion batteries, the cumulative amount of used lithium-ion batteries is also increasing year by year. Since waste lithium-ion batteries contain a large amount of valuable metals, the recovery of valuable metals has become one of the current research hotspots. The research uses electrometallurgical technology, and the main methods used are cyclic voltammetry, square wave voltammetry, chronoamperometry and open circuit potential. The electrochemical reduction behavior of Ni3+ in NaCl-CaCl2 molten salt was studied, and the electrochemical reduction behavior was further verified by using a Mo cavity electrode. It is determined that the reduction process of Ni3+ in LiNiO2 is mainly divided into two steps: LiNiO2 → NiO → Ni. Through the analysis of electrolysis products under different conditions, when the current value of LiNiO2 is not less than 0.03 A, the electrolysis product after 10 h is metallic Ni. When the current reaches 0.07 A, the current efficiency is 77.9%, while the Li+ in LiNiO2 is enriched in NaCl-CaCl2 molten salt. The method realizes the separation and extraction of the valuable metal Ni in the waste lithium-ion battery.

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“…cm − , and its reduction by the FFC Cambridge process is reported to be very difficult. 42 Incorporation of a thermodynamically less stable metal oxide, e.g., NiO, in the MgO matrix accelerated the reduction kinetics of MgO. 43 NiO, which has a lower reduction potential than MgO, was reduced first to metallic Ni and thereby improved the electrical conductivity of the oxide matrix.…”

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confidence: 99%

“…Subsequently, the electro-reduction of MgO occurred in the presence of pre-formed Ni to form a stable intermetallic compound, MgNi 2, which is thermodynamically more feasible than the reduction of MgO to Mg. Li et al conducted direct electro-deoxidation experiments with MgO-ZrO 2 mixture in CaCl 2 -NaCl melt to form Mg-Zr alloy and reported that the initial reduction of ZrO 2 to Zr promoted the reduction of MgO. 42 Electro-reduction of SiO 2 , an electrical insulator, was facilitated in presence of Ni and NiO additives because of the improvement of electrical conductivity of the oxide matrix and formation of NiSi 2 intermetallic. 44 Similarly, electroreduction of very stable rare Earth metal oxides, e.g., Tb 2 O 3 , Dy 2 O 3 , La 2 O 3 , and Nd 2 O 3 is reported to become more feasible when NiO, z E-mail: rkum@igcar.gov.in Fe 2 O 3 , Co 3 O 4 etc., is added to the matrix and various intermetallic compounds, e.g., TbNi 5 , TbFe 2 , DyFe 2 , LaNi 5 , NdCo 5 , etc are prepared in CaCl 2 based melts.…”

mentioning

confidence: 99%

Studies on Preparation of Thorium-Based Intermetallics in CaCl₂ Melt by Electrochemical De-Oxidation Process

Mukherjee,

Khan,

Kumaresan

2023

J. Electrochem. Soc.

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Thorium and its alloys find immense applications in nuclear technology. In the present study, the feasibility of direct electrochemical de-oxidation of mixed ThO2-NiO (7:3 molar ratio) and ThO2-Fe2O3 (7:1.5 molar ratio) to Th7Ni3 and Th7Fe3 intermetallics was investigated for the first time in CaCl2 melt at 900oC using FFC Cambridge process. Electro-reduction mechanisms of the mixed metal oxides were elucidated by conducting constant voltage electrolysis at 3.1 V cell potential with sintered mixed metal oxides pellet cathode and HD graphite anode in molten CaCl2 for different time intervals. The electrolysed products were characterized by X-ray diffraction, scanning electron microscopy, and energy dispersive X-ray analysis techniques. Reduction of the less stable metal oxide, e.g. NiO or Fe2O3 occurred at the initial phase of electrolysis and de-oxidation of more stable ThO2 took place in presence of newly formed metallic Ni or Fe in the later stage leading to the formation of Th7Ni3 or Th7Fe3. Electro-reduction mechanism of ThO2 was evaluated using cyclic voltammetry technique with ThO2 filled Mo cavity electrode and single-step reduction of ThO2 to Th was perceived.

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Preparation of Mg-Zr alloys through direct electro-deoxidation of MgO-ZrO2 in CaCl2-NaCl molten salt

Cited by 13 publications

References 28 publications

Electrochemical Preparation of ZrFe₂ and ZrFe_1.8Ni_0.2 Intermetallic Compounds by FFC Cambridge Process

Electrochemical Preparation of ZrFe₂ and ZrFe_1.8Ni_0.2 Intermetallic Compounds by FFC Cambridge Process

Electrochemical Mechanism of Recovery of Nickel Metal from Waste Lithium Ion Batteries by Molten Salt Electrolysis

Studies on Preparation of Thorium-Based Intermetallics in CaCl₂ Melt by Electrochemical De-Oxidation Process

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Preparation of Mg-Zr alloys through direct electro-deoxidation of MgO-ZrO2 in CaCl2-NaCl molten salt

Cited by 13 publications

References 28 publications

Electrochemical Preparation of ZrFe2 and ZrFe1.8Ni0.2 Intermetallic Compounds by FFC Cambridge Process

Electrochemical Preparation of ZrFe2 and ZrFe1.8Ni0.2 Intermetallic Compounds by FFC Cambridge Process

Electrochemical Mechanism of Recovery of Nickel Metal from Waste Lithium Ion Batteries by Molten Salt Electrolysis

Studies on Preparation of Thorium-Based Intermetallics in CaCl2 Melt by Electrochemical De-Oxidation Process

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Electrochemical Preparation of ZrFe₂ and ZrFe_1.8Ni_0.2 Intermetallic Compounds by FFC Cambridge Process

Electrochemical Preparation of ZrFe₂ and ZrFe_1.8Ni_0.2 Intermetallic Compounds by FFC Cambridge Process

Studies on Preparation of Thorium-Based Intermetallics in CaCl₂ Melt by Electrochemical De-Oxidation Process