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The performance of many advanced materials is determined by the arrangement of their nanostructure which requires ever more precise characterization. In this respect, X-ray computed tomography (CT) is a powerful technique to investigate material properties as it provides non-destructive direct access to three-dimensional morphology with nanoscale resolution. However, challenges remain in clearly understanding physical mechanisms involved during their processing in real time and real conditions. So far, beam and sample stabilities, effective spatial resolution and tomography scan time have hindered the development of nanoscale in situ 4D imaging (3D plus time), and especially at high temperatures. Here, we report on the development of fast X-ray nanotomography at temperatures up to 700°C with an unprecedented combination of nanometer pixel size and acquisition times of a few tens of seconds. The great potential of the method is demonstrated by following the early stages of two thermally driven phenomena: neck curvature evolution in sintering and nucleation of liquid droplets in light alloys. The reported real time observations will benefit the fundamental understanding of the underlying physics and provide useful data to build new models. The novel aspects of this synchrotron based technique offer a powerful imaging tool for a wide variety of heterogeneous nanoscale dynamics in materials and open new perspectives for the investigation of advanced materials under realistic conditions.

Within the framework of the ESRF Phase I Upgrade Programme, a new state-of-the-art synchrotron beamline ID16B has been recently developed for hard X-ray nano-analysis. The construction of ID16B was driven by research areas with major scientific and societal impact such as nanotechnology, earth and environmental sciences, and bio-medical research. Based on a canted undulator source, this long beamline provides hard X-ray nanobeams optimized mainly for spectroscopic applications, including the combination of X-ray fluorescence, X-ray diffraction, X-ray excited optical luminescence, X-ray absorption spectroscopy and 2D/3D X-ray imaging techniques. Its end-station re-uses part of the apparatus of the earlier ID22 beamline, while improving and enlarging the spectroscopic capabilities: for example, the experimental arrangement offers improved lateral spatial resolution (∼50 nm), a larger and more flexible capability for in situ experiments, and monochromatic nanobeams tunable over a wider energy range which now includes the hard X-ray regime (5–70 keV). This paper describes the characteristics of this new facility, short-term technical developments and the first scientific results.