The main goal of the study presented in this thesis was to perform in-situ investigations on deformation structures in plastically deformed polycrystalline copper at low degrees of tensile deformation (<5%). Copper is taken as a model system for cell forming pure fcc metals. Anovel synchrotron-radiation based technique High Angular Resolution 3DXRD has been developed at the 1-ID beam-line at the Advanced Photon Source. The technique extents the 3DXRD approach, to 3D reciprocal space mapping with a resolution of ≈ 1 · 10−3Å−1 and allows for in-situmapping of reflections from deeply-embedded individual grains in polycrystalline samples during tensile deformation. We have shown that the resulting 3D reciprocal space maps from tensile deformed copper comprise a pronounced structure, consisting of bright sharp peaks superimposed on a cloud of enhanced intensity. Based on the integrated intensity, the width of the peaks, and spatial scanning experiments it is concluded that the individual peaks arise from individual dislocation-free regions (the subgrains) in the dislocation structure. The cloud is attributed to the dislocation rich walls. Samples deformed to 2% tensile strain were investigated under load, focusing on grains that have the tensile direction close to the h100i direction. It was found that the individual subgrains, on average, are subjected to a reduction of the elastic strain with respect to the mean elastic strain of the grain. The walls are equivalently subjected to an increased elastic strain. The distribution of the elastic strains between the individual subgrains is found to be wider than the distribution of strains within the individual subgrains. The average properties are consistent with a composite type ofmodel. The details, however, show that present understanding of asymmetrical line broadening have to be reconsidered. Based on continuous deformation experiments, it is found that the dislocation patterning takes place during the deformation, and that a subgrain structure appears from the moment where plastic deformation is detected. By investigating samples under stress relaxation conditions, and unloading, it is found that the overall dislocation structure only depends on the maximum obtained flow stress. However, some changes in orientation and internal strain distribution between the subgrains were observed after the unloading. An in-situ stepwise straining experiment of a pre-deformed sample was performed, allowing for investigation of individual subgrains during straining. The result indicates that the cell refinement process generally does not take place through simple subgrain breakups. Surprisingly, the dislocation structure shows intermittent behavior, with subgrains appearing and disappearing with increasing strain, suggesting a dynamical development of the structure.