Here we detail a study on light-weight structural alloys, which has benefitted from characterization of the same sample volume across multiple length scales. A new, efficient 3D correlative microscopy workflow is presented, that utilizes non-destructive 3D X-ray microscopy (XRM) to guide focused ion beam and scanning electron microscopy (FIB-SEM) tomography in order to reveal targeted sub-surface regions of interest. An aluminum 7075 alloy was investigated, exhibiting hierarchical structures that required characterization in 3D across multiple length scales, modalities and instruments. The alloy’s microstructure contains precipitates, constituent particles (inclusions), and pores associated with the inclusions. The size, shape, and distribution of these microstructural features in the alloy are known to affect the corrosion and mechanical behavior (fatigue, tensile, and stress corrosion cracking). Therefore, it is necessary to obtain combined information of the size, shape, and distribution of each feature in three dimensions (3D) and from the same volume of interest.