Abstract: A process of preparing aligned, in-situ, two-phase single crystal alloys of titanium, aluminum and niobium which comprises growing the alloys at rates of about 3.0 mm. to about 6.0 mm. per hour by rotating a seed rod alloy consisting essentially of Ti-43 to 45 Al-10 to 12 Nb+0.5 Si, in atomic percent, at about 7.75 to 8.25 RPM while in contact with a rotating feed rod alloy consisting essentially of Ti-43 to 45 Al-10 to 12 Nb, in atomic-percent, rotating at about 5.75 to 6.25 RPM in an atmosphere of substantially pure argon at melt temperatures ranging from about 1650° C. to 1750° C. to obtain two-phase single crystal alloys of Ti-43 to 45Al-10 to 12 Nb characterized as having improved ductility, excellent oxidation resistance, and high-temperature creep strength. These alloys are particularly useful for manufacturing high-temperature material components for internal combustion engines, gas turbines, and advanced aircraft engines.