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Technologically viable principles have been developed for the preparation of titanium and zirconium powders via reduction of metal oxides. We have studied the effect of synthesis conditions (starting-mixture composition and relationships between reactants) on the composition, structure, and particle size of the powders. The results demonstrate that the addition of excess magnesium to the starting mixture leads to the complete reduction of the oxides and that reducing the combustion temperature of the starting mixture leads to an increase in the percentage of zirconium oxide in the final product. The titanium and zirconium powders prepared in the combustion regime with a reduction stage consist of agglomerates of particles ranging widely in size: from large (several microns) to ultrafine and nanoscale particles. The use of magnesium perchlorate as a heating additive leads to the formation of a titanium–zirconium solid solution. The composition of the powders has been determined by chemical analysis, microstructural analysis, and X-ray diffraction. [ABSTRACT FROM AUTHOR]