Rod-like Al3Ni intermetallic structures have been widely studied by Bridgman techniques of solidification. However, there is a lack of experiments conducted under unsteady-state solidification conditions. Such conditions are very close to the industrial reality since the thermal solidification variables (tip cooling rate, tip growth rate and thermal gradient) are freely changing as solidification progresses. In this research, Al3Ni structures found in hypoeutectic Al-Ni alloys were characterized under transient solidification conditions. Two Al-Ni alloys (1.0 and 5.0 wt%Ni) were directionally solidified. SEM (Scanning Electron Microscope) micrographs were obtained along the casting length (P). It was possible to observe with adequate magnifications the distribution of rod-like Al3Ni particles along the interdendritic regions. In order to emphasize the examination of morphology and distribution of such particles, the aluminum-rich matrix was dissolved by immersion of the sample in a fluoride acid solution (0.5%HF + 99.5% H2O). The effects of nickel content, dendritic arrangement and Al3Ni distribution on mechanical properties were investigated by tensile tests.