Two-stage electrochemical synthesis of double carbides

The temperature was measured with a Termodat-17E3 temperature controller. Molybdenum plates located on current leads were immersed in a molten electrolyte through special holes in the retort. We used a bulk 

During investigations, we chose the following two regimes of preparing molybdenum and nickel alloys electrolysis at a cathodic current density of 5 mA-cm in the NaCl-KCl-NiCl2-Ni melt (anode is metallic nickel), at a temperature of 1123 K, process time of 1 hour, and currentless transfer in the NaCl-KCl-NiCl2-Ni melt at the same temperature and time. 

The cyclic voltammetric curves were measured at a potential sweep rate varied from 5-10 to 2.0 V-s in the temperature range 973-1123 K. Cyclic voltammograms were recorded on molybdenum and glassy carbon working electrodes 0.5-2.0mm in diameter with respect to a platinum wire, which was used as a quasi-reference electrode, and a reference electrode Ag/NaCl-KCl-AgCl (2 wt%). The glassy carbon crucible served as an auxiliary electrode. 

The prepared molybdenum and nickel alloys were carbonized under various conditions. Carbonization was performed by electrolysis in an equimolar mixture of sodium and potassium chlorides containing carbonate ions (5 wt% Li2C03) during cathodic polarization of a sample at a current density of 5 mA-cm . The other process parameters (namely, electrolysis time and temperature) are given in Table 4.11.1. 

After experiments the samples were washed in distilled water and alcohol. 

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