In order to study the relationship between residual stress (RS) and the microstructure of friction stir weld (FSW), RS profiles through thickness in the un-welded aluminum alloy 7075 plate and in middle layer of its FSW joint were determined nondestructively by the short-wavelength X-ray diffraction (SWXRD) and neutron diffraction. Microstructure and mechanical properties of the FSW joint were also studied by optical microscopic analysis, and microhardness and tensile strength measurements. RS profiles measured by the two methods had the same distribution trend. The maximum tensile RS tested by SWXRD and neutron diffraction in transverse and longitudinal direction occurred in the weld nugget. Microhardness in the direction perpendicular to the weld line showed a "W" shape distribution. Position of the local maximal extremum of RS in thermo-mechanically affected zone corresponded to that of minimal microhardness. The grain-refined strengthening caused by the recrystallization in the weld nugget kept the joint from fracturing at this region notwithstanding the maximum tensile RS. And the tensile fracture occurred near the boundary of welding zone and thermo-mechanically affected zone where minimum of hardness and maximum of RS appear at the same position.