Abstract: The Ti-Al series non-equilibrium materials are prepared by the method of hot-plasticity extrusion alloying and the microstructure of materials was studied.It is found that materials prepared by hot-plasticity extrusion alloying are poly-crystalline material,including TiAl₃、Ti₂Al₃、Ti₃Al、TiAl and Ti₅Al₃ phase.The hot-plasticity extrusion alloying can markedly reduce the size of grains of Ti-Al alloying.In the direction of extrusion and deformation,the extraction materials have non-uniform components.The Ti/Al atoms in the front and back are lower than those in the middle.The Ti phase by the heat treatment at the 500℃/6 h can completely be transformed into the Ti-Al alloying phase.