Recently there have been many investigations on the synthesis and properties of transition metal trialuminides based on Ti, Zr, V, Nb and Ta for use aircraft structure materials in an elevated environment. The effect of Zr additions on the formation behaviour of Al-Nb alloy was investigated. Al-1.3at.%(Nb+Zr) alloys with different Nb to Zr atomic 1:3, 1:1 and 3:1 were prepared by mechanical alloying(MA). The morphological changes and microstructural evolution of Al-Nb-Zr powders during MA were investigated by SEM, XRD and TEM. The intermetallic compound phase of $Nb_2Al; and; Al_3Zr_4$ was identified by X-ray diffraction. The intemetallic compound of $Al_3Zr,; Al_3Nb$ and $Al_3Zr_4$ were formed by heat treatment for 1 hour at $500^{circ}C$. The size of intermetallic compounds observed by TEM were approximately below 100nm, when they were heat treated after mechanically alloying for 30 hours.