Numerous phenomenological descriptions of the mechanical behavior of composite materials have been developed. There is now an urgent need to study and interpret deformation behavior, load transfer, and strain distribution, in terms of micromechanisms at the atomic level. One approach is to characterize dislocation substructure resulting from specific test conditions by the various techniques of transmission electron microscopy. The present paper describes a technique for the preparation of electron transparent composites of aluminum-stainless steel, such that examination of the matrix-fiber (wire), or interfacial region is possible. Dislocation substructures are currently under examination following tensile, compressive, and creep loading. The technique complements and extends the one other study in this area by Hancock.The composite examined was hot-pressed (argon atmosphere) 99.99% aluminum reinforced with 15% volume fraction stainless steel wire (0.006″ dia.).Foils were prepared so that the stainless steel wires run longitudinally in the plane of the specimen i.e. the electron beam is perpendicular to the axes of the wires. The initial step involves cutting slices ∼0.040″ in thickness on a diamond slitting wheel.