Electrochemical preparation method of superfine tantalum powder
An electrochemical and tantalum powder technology, which is applied in the field of preparation of ultrafine tantalum powder, can solve the problems of incompatibility with the electrochemical reduction of tantalum pentoxide solid cathode, low current efficiency and high energy consumption, and achieves reduction of electrolysis energy consumption and low energy consumption. The effect of consumption and optimization of supply
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Embodiment 1
[0037] Commercially available Ta with a purity of 99.99% 2 o 5 The powder is about 1.5g, pressed by mechanical pressure at 5-10MPa to about 20mm in diameter and 1.3-1.5mm in thickness, heated in air at 100-1600°C for 0.5-8 hours, and the porosity of the obtained sample is 20-80%. The sintered Ta 2 o 5 The test piece is combined with the conductive cathode current collector as the working electrode, the graphite rod is used as the counter electrode, and the molten CaCl 2 or CaCl 2 +NaCl is the electrolyte. In an argon environment, the temperature is 650, 750, 850 and 950°C. Use the high-temperature fully sealed Ag / AgCl reference electrode disclosed in the above-mentioned 200420017446.7 patent to control the potential for constant potential electrolysis. The potential is -0.7~-1.7V. After 30, 60, 120, 180, and 300 minutes of electrolysis, the products were washed with water, 0.1M HCl, water, and dried. The products were all ultrafine metal tantalum powders with a size of 10...
Embodiment 2
[0039] Commercially available Ta with a purity of 99.99% 2 o 5 The powder is about 5g, pressed into a disc with a diameter of about 20mm by mechanical pressure at 6MPa, and heated in air at 900°C for 2 hours. Will Ta 2 o 5 The test piece is combined with the conductive cathode current collector as the working electrode, the graphite rod is used as the counter electrode, and the molten CaCl 2 As an electrolyte, in an argon environment, the temperature is 850 °C, with the above-mentioned fully sealed Ag / AgCl reference electrode, the cathode potential is controlled at -1.0V, after 5 hours of electrolysis, the electrolysis products are passed through water in turn, 0.1M After washing with HCl and water, drying is performed to obtain superfine metal tantalum powder of 100-300 nanometers, the electrolysis efficiency is as high as 78%, and the energy consumption is lower than 2.4KWh / Kg-Ta.
Embodiment 3
[0041] Commercially available Ta with a purity of 99.99% 2 o 5 The powder is about 2g, heated in the air above 100°C for 3.5 hours, put into a basket made of molybdenum wire, and lead out a molybdenum wire with a diameter of 2mm as the working electrode, that is, the cathode, and use a graphite rod as the counter electrode to melt CaCl 2 As an electrolyte, in an argon environment, the temperature is 850 ° C, with the above-mentioned fully sealed Ag / AgCl reference electrode, the cathode potential is controlled at -1.3V, after electrolysis for 5 hours, the electrolysis products are passed through water in turn, 0.1M After washing with HCl and water and drying, superfine metal tantalum powder with a diameter of 100-300 nanometers is obtained, the electrolysis efficiency is higher than 80%, and the energy consumption is lower than 2.6KWh / Kg-Ta.
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