In order to understand the deformation behavior and to improve the ductility, single crystals of [gamma]-TiAl and pseudo-single crystal with oriented lamellar structure of [alpha][sub 2]/[gamma] have been used to investigate the deformation mode of the intermetallics. However, little work has been published solely on the preparation and microstructural characterization of [gamma]-TiAl single crystals or single oriented lamellar crystals. In this work, the directionally solidified microstructure of TiAl alloys has been investigated by optical, scanning (SEM) and transmission electron microscopy (TEM) in order to study the solidification process of two phase peritectic alloys. EDX compositional analysis has been carried out in order to understand the segregation behavior during peritectic solidification. Master alloys of Ti-48, Ti-52, Ti-54, Ti-56Al were used.