The present invention relates to high-purity niobium monoxide powder (NbO) produced by a process of combining a mixture of higher niobium oxides and niobium metal powder or granules; heating and reacting the compacted mixture under controlled atmosphere to achieve temperature greater than about 1945.degree. C., at which temperature the NbO is liquid; solidifying the liquid NbO to form a body of material; and fragmenting the body to form NbO particles suitable for application as capacitor anodes. The NbO product is unusually pure in composition and crystallography, and can be used for capacitors and for other electronic applications. The method of production of the NbO is robust, does not require high-purity feedstock, and can reclaim value from waste streams associated with the processing of NbO electronic components. The method of production also can be used to make high-purity NbO.sub.2 and mixtures of niobium metal/niobium monoxide and niobium monoxide/niobium dioxide. The method further is ideal for doping of the product oxides to enhance particular characteristics of the materials. The method further allows the production of single crystal or directionally-solidified ingots. In contrast to the spongy, highly porous agglomerates produced by other techniques, the present invention produces solid, non-porous ingots that can be fragmented to fine, non-porous angular particles suitable for electronic applications.