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The correct description of the mechanical behaviour of metallic materials after deformation to large strains requires the quantitative determination of substructure characteristics on different length scales. Important tools for this purpose are transmission electron microscopy (TEM), electron backscattering diffraction (EBSD) and X-ray diffraction (XRD), which lead to quantities such as the mean total dislocation density, the density of excess dislocations stored in dislocation walls, the distributions and the averages of local lattice rotations and the size (chord length) of the lattice regions (cell blocks, fragments) of the mesoscale substructure. This present paper illustrates the application of EBSD and XRD for the analysis of the deformation substructure occurring in polycrystalline Al during uniaxial compression up to strains ε ≈ 2. [ABSTRACT FROM AUTHOR]