Nanoelectronics is changing the world with the technology that enables global progress and enriches people’s lives. Continuing Moore’s law propels the research and the development of devices with better functionality and performance while controlling power, cost, and size. As the architectural complexity increases and functional nanomaterials advance into nano- and even atomic-scale regimes, three-dimensional (3D) metrologies become essential in validating the structure and chemistry of materials that govern the device properties. We cover recent advances of 3D metrologies in semiconductor industry research and development. It addresses the techniques from the device level, such as transmission electron microscopy and atom probe tomography to array level, such as compositional microscope and nondestructive optical-based metrologies, including 3D structural, 3D compositional analysis, and 3D property characterization.