Neodymium was electrochemically deposited from NdF3–LiF–Nd2O3 molten salt electrolyte onto the Mo electrode at temperatures close to 1273 K. Cyclic voltammetry and chronoamperometry measurements were the applied electrochemical methods. Metallic neodymium is obtained by potentiostatic deposition. The optical microscopy and XRD were used to analyze the electrolyte, the working electrode surface, and the deposit on the electrode. It was established that Nd(III) ions were reduced to Nd metals in two steps: Nd(III) + e− → Nd(II) at potential ≈−0.55 V vs. W and Nd(II) + 2e− → Nd(0) at ≈−0.83 V vs. W. Both of these processes are reversible and under mass transfer control. Upon deposition under the regime of relatively small deposition overpotential of −0.10 V to −0.20 V, and after the electrolyte was cooled off, Nd metal was observed at the surface of the Mo electrode. CO and CF4 were gases registered as being evolved at the anode. CO and CF4 evolution were observed in quantities below 600 ppm and 10 ppm, respectively.

The processes of electrochemical deposition of magnesium oxide/hydroxide on glassy carbon (GC) electrode from magnesium nitrate hexahydrate melt have been investigated. A novel procedure predicting a possibility of direct formation of magnesium oxide during electrodeposition from the nitrate melt used is reported. XRD analysis of the obtained deposits showed the formation of magnesium oxide along with magnesium hydroxide. The electrodeposition of magnesium oxide/hydroxide commences in magnesium underpotential (UPD) and continues through the magnesium overpotential (OPD) region. Network of individual or intertwined very thin needles as well as those grouped in flower-like aggregates or honeycomb-like structures were formed in both magnesium UPD and OPD regions.Formation of the long needles was explained through theories of mechanisms of dendrite

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Electrodeposition processes of neodymium and praseodymium in molten NdF3 + PrF3 + LiF + 1 wt.%Pr6O11 + 1 wt.%Nd2O3 and NdF3 + PrF3 + LiF + 2 wt.%Pr6O11 + 2 wt.%Nd2O3 electrolytes at 1323 K were investigated. Cyclic voltammetry, square wave voltammetry, and open circuit potentiometry were applied to study the electrochemical reduction of Nd(III) and Pr(III) ions on Mo and W cathodes. It was established that a critical condition for Nd and Pr co-deposition in oxyfluoride electrolytes was a constant praseodymium deposition overpotential of ≈−0.100 V, which was shown to result in co-deposition current densities approaching 6 mAcm−2. Analysis of the results obtained by applied electrochemical techniques showed that praseodymium deposition proceeds as a one-step process involving exchange of three electrons (Pr(III)→Pr(0)) and that neodymium deposition is a two-step process: the first involves one electron exchange (Nd(III)→Nd(II)), and the second involves an exchange of two electrons (Nd(II)→Nd(0)). X-ray diffraction analyses confirmed the formation of metallic Nd and Pr on the working substrate. Keeping the anodic potential to the glassy carbon working anode low results in very low levels of carbon oxides, fluorine and fluorocarbon gas emissions, which should qualify the studied system as an environmentally friendly option for rare earth metal deposition. The newly reported data for Nd and Pr metals co-deposition provide valuable information for the recycling of neodymium-iron-boron magnets.

Magnesium underpotential deposition on gold electrodes from magnesium nitrate-ammonium nitrate melts has been investigated. Linear sweep voltammetry and potential step were used as electrochemical techniques. Scanning electron microscopy (SEM), energy dispersive spectrometry (EDS) and X-ray diffraction (XRD) were used for characterization of obtained electrode surfaces. It was observed that reduction processes of nitrate, nitrite and traces of water (when present), in the Mg underpotential range studied, proceeded simultaneously with magnesium underpotential deposition. There was no clear evidence of Mg/Au alloy formation induced by Mg UPD from the melt made from eutectic mixture [Mg(NO 3 ) 2 ·6H 2 O + NH 4 NO 3 ·XH 2 O]. However, EDS and XRD analysis showed magnesium present in the gold substrate and four different Mg/Au alloys being formed as a result of magnesium underpotential deposition and interdiffusion between Mg deposit and Au substrate from the melt made of a nonaqueous [Mg(NO 3 ) 2 + NH 4 NO 3 ] eutectic mixture at 460 K.