Mechanical ball milling is a useful technique for systems with positive enthalpy of mixing. With this technique solubility of a solute in a solid solution can be enhanced. Al-Zn system has positive heat of mixing. High energy ball milling has been employed to produce four alloys of Al with 2.5 to 10 wt% Zn. Powders of Al (1-125 mum) and Zn (0.7-5.0 mum) were mixed together in the desired proportion and milled with a powder to ball weight ratio of 1:20. The size and shape of the particles of as-received and alloy powders were examined in a scanning electron microscope (SEM) while their microanalysis was performed by energy dispersive system (EDS) attached with SEM. It has been observed that 120 h of milling of the powders produced homogeneous alloys. X-ray diffraction (XRD) patterns confirm complete solubility up to 10 wt% Zn in Al. Using the quasi-chemical theory of binary solid solutions, the enthalpy of mixing of 10 wt% Zn in Al has been determined to be 276 cals/mol. It is shown that stress exerted by very high density of dislocations, generated by mechanical milling, plays a major role in the enhancement of solubility. Hardness has been measured and it increases with increasing solute content. (C) 2004 Kluwer Academic Publishers.