<p>Titanium dioxide (TiO₂) nanomaterials with controlled morphology and crystalline phase are of significant interest for optoelectronic and photocatalytic applications. In this study, TiO₂ nanostructures were synthesized from a Ti-6Al-4V alloy target via a one-step, surfactant-free ultrasonic-assisted laser ablation in liquid (ULAL) process in deionized water. The effects of ultrasonic power (0, 30, and 50&#xa0;W) on nanoparticle morphology, size distribution, phase composition, and elemental characteristics were investigated. Electron microscopy revealed that ultrasonic irradiation markedly reduced particle size and suppressed agglomeration through cavitation-induced fragmentation. Nanorod-like structures were observed under the highest ultrasonic power condition (50&#xa0;W), suggesting that intense cavitation may influence crystal growth behavior during nanoparticle formation. X-ray diffraction, selected area electron diffraction, and Raman spectroscopy consistently confirmed the formation of mixed-phase TiO₂ composed primarily of anatase with the presence of brookite. The observed phase composition is attributed to the rapid cooling conditions associated with laser ablation in liquid. Energy-dispersive X-ray spectroscopy showed that Ti and O were the dominant elements in all samples, with minor amounts of Al originating from the alloy target, while vanadium remained below the detection limit. Raman spectroscopy further revealed phonon confinement and lattice strain associated with reduced crystallite size and oxygen vacancies. These results demonstrate that ultrasonic-assisted laser ablation provides an effective route for controlling the morphology and phase composition of TiO₂ nanostructures without the use of chemical additives.</p>