Future nanoelectronics manufacturing at extraordinary length scales, new device structures, and advanced materials will provide challenges to process development and engineering but also to process control and physical failure analysis. Advanced X‐ray techniques, using lab systems and synchrotron radiation sources, will play a key role for the characterization of thin films, nanostructures, surfaces, and interfaces. The development of advanced X‐ray techniques and tools will reduce risk and time for the introduction of new technologies. Eventually, time‐to‐market for new products will be reduced by the timely implementation of the best techniques for process development and process control. The development and use of advanced methods at synchrotron radiation sources will be increasingly important, particularly for research and development in the field of advanced processes and new materials but also for the development of new X‐ray components and procedures. The application of advanced X‐ray techniques, in‐line, in out‐of‐fab analytical labs and at synchrotron radiation sources, for research, development, and manufacturing in the nanoelectronics industry is reviewed. The focus of this paper is on the study of nanoscale device and on‐chip interconnect materials, and materials for 3D IC integration as well.