A method is described which combines optical microscopy with x-ray microscopy and diffraction analysis. The topographical relationship of the grains of a fine-grained material and the fine-structural details of their surface texture are disclosed by a special technique of reflection x-ray microscopy. The experimental observations made by this technique are being correlated to those made by optical microscopy. The individual grains are subsequently analyzed for their substructure characteristics by a photographic tracer technique and a method based on the principle of the double-crystal diffractometer. Quantitaive information is obtained concerning the lattice misalignment of the grains, the size of subgrains, disorientation angle between subgrains, lattice misalignment existing within the subgrains and the nature of low-angle boundaries. Application of the method to the analysis of inclusions and precipitates dispersed in a polycrystalline matrix is discussed.