Electrochemical synthesis of tantalum monoxide nanoneedles in molten salts

Abstract

us to avoid contact of oxides used in classical reference electrodes with the chloride–oxyfluoride melt. The electrolytic processes with accumulation of products electrodeposited on the cathode were per� formed in a sealed electrolyzer in the galvanostatic mode. The cell, as a platinum crucible (30 mm in diameter, 40 mm in height), was placed inside a cylin� der vessel made of stainless steel. The vessel was filled with pure argon. Heating of the vessel was carried out in a shaft furnace; the temperature was maintained with the accuracy of ±2°С. The anode (a tantalum plate 3 mm thick) was placed at the bottom of the plat� inum crucible. Molybdenum rods (5mm in diameter) were used as cathodes. Each portion of an electrolyte (about 40 g) served for a single cathodic deposition cycle only. Cathodic products, after cooling to room temperature in an argon atmosphere, were leached with 10% hydrochloric acid, then washed with dis� tilled water and ethanol, and dried in air at 40°C.