An investigation was conducted to explore the applicability of magnetic and microwave techniques to characterize grains size variation during mechanical alloying. A series of Nano crystalline Fe65Co35samples have been prepared, these structures are prepared using mechanical alloying based on planetary ball mill under several milling conditions. Mechanical alloying is a non-equilibrium process for materials synthesis. The structural effects of mechanical alloying of powders were investigated by X-Ray diffraction analysis, microwaves and VSM magnetic technique. Consequently, alloy powder with an average grain size about of 8 nm was obtained. Experimental results show that fine Nano crystalline alloy powders prepared by mechanical milling are very promising for microwave applications.