Uniform distribution of reinforcement particles in matrix is one of the most important parameters in composites fabrication. One way to obtain homougenous distribution is using mechanical milling for mixing powders. Therefore, it is worth identifying the optimum conditions for mechanical milling. The aim of this study is investigation of the optimum conditions for mechanical milling of Ni3Al reinforcement particles and Al powder in order to manufacture Al/5vol.% Ni3Al composite. In order to evaluate the effect of reinforcement particles on composite properties, two different kinds of reinforcement particles, i.e., oxide reinforcement particles (Al2O3) and intermetallic reinforcement particles (Ni3Al), were used. Since morphology and powder properties are affected by mecahanical milling conditions, dependency of composite properties on the mecahanical milling condition is expected. It was concluded that mechanical milling in optimum conditions causes decreasing density, increasing hardness and ultimate strength. Also, oxide reinforcement particles in compare to intermtallics cause lower increasing in hardness and considerable increase in strength and ducility.