The continuous and aggressive scaling in semiconductor technology results in the integration of increasingly complex 3D architectures and new materials. The realization of these downscaled 3D structures requires also further improvement in 3D characterization techniques. In this work, a potential route to improve the accuracy and reliability of the quantitative analysis of 3D nano‐devices is investigated. 3D organic and inorganic reference nanostructures with dimensions and structural ordering resembling those utilized in industrial applications are fabricated and characterized in detail. The 3D organic nanostructures are fabricated exploiting the self‐assembly capability of di‐block copolymers. Subsequent deposition of a thin Al film lead to the formation and realization of nanostructured Al. In addition, different inorganic nanostructures are fabricated using …