Powders of tantalum, niobium and an alloy thereof have been prepared by the electro-deoxidation of their oxide precursors in a eutectic melt of CaCl2-NaCl at 1098 K. The reduced products were characterised by X-ray diffraction analysis, scanning electron microscopy, energy dispersive X-ray analysis, and quantitative oxygen analysis. All metallic materials were of high purity and had porous nodular microstructures. The alloy powders were single phase, with a relatively wide particle size distribution and some variation in the local Ta-to-Nb ratio. The oxygen contents of the products were below 5000 ppm by mass.