Lee et al. reported that a mixture of Cu and Ta, the combination of which is characterized by a positive heat of mixing, ${Delta}H_{mix}$ of +2 kJ/㏖, can be amorphized by mechanical alloying(MA). It is our aim to investigate to what extent the MA is capable of producing a non-equilibrium phase with increasing the heat of mixing. The system chosen is the binary $Cu_{30}Mo_{70}$ with ${Delta}H_{mix}$=+19 kJ/㏖. The mechanical alloying was carried out using a Fritsch P-5 planetary mill under Ar gas atmosphere. The vial and balls are made of Cu containing 1.8-2.0 wt.%Be to avoid contaminations arising mainly from Fe when steel balls and vial are used. The MA powders were characterized by the X-ray diffraction, EXAFS and thermal analysis. We conclude that two phase mixture of nanocrystalline fcc-Cu and bcc-Mo with grain size of 10 nm is formed by the ball-milling for a 3:7 mixture of pure Cu and Mo, the evidence for which has been deduced from the thermodynamic and structural analysis based on the DSC, X-ray diffraction and EXAFS spectra.