Abstract: Mechanically alloyed Al-4.9Ni-4.9Ti powders were prepared by milling mixed aluminium, titanium and nickel powders, and then consolidated by hot hydrostatic extrusion. The microstructures of milled powders and extruded bars were characterized by X-ray diffraction and transmission eIectron microscopy observation. The results show that mechanical alloying and consolidating processes have great effects on the microstructures and mechanical properties of extruded materials. Polycrystalline materials having an ultrafine grain size may be prepared by mechanical alloying. The strength and thermal stability are improved with the increasing of processing time of mechanical alloying, since grain size decreases and volume fraction of dispersoids increases as milling time increased