Microscopic imaging and characterization of semiconductor devices and material properties often begin with a sample preparation step. A variety of sample preparation methods such as mechanical lapping and broad ion beam (BIB) milling have been widely used in physical failure analysis (FPA) workflows, allowing internal defects to be analyzed with high-resolution scanning electron microscopy (SEM). However, these traditional methods become less effective for more complicated semiconductor devices, because the cross-sectioning accuracy and reliability do not satisfy the need to inspect nanometer scale structures. Recent trends on multi-chip stacking and heterogenous integration exacerbate the ineffectiveness. Additionally, the surface prepared by these methods are not sufficient for high-resolution imaging, often resulting in distorted sample information. In this work, we report a novel correlative workflow to improve the cross-sectioning accuracy and generate distortion-free surface for SEM analysis. Several semiconductor samples were imaged with 3D X-ray microscopy (XRM) in a non-destructive manner, yielding volumetric data for users to visualize and navigate at submicron accuracy in three dimensions. With the XRM data to serve as 3D maps of true package structures, the possibility to miss or destroy the fault regions is largely eliminated in PFA workflows. In addition to the correlative workflow, we will also demonstrate a proprietary micromachining process which is capable of preparing deformation-free surfaces for SEM analysis.