Development of synchrotron X‐ray micro‐tomography under extreme conditions of pressure and temperature

X‐ray tomography is a non‐destructive three‐dimensional imaging/microanalysis technique selective to a wide range of properties such as density, chemical composition, chemical states and crystallographic structure with extremely high sensitivity and spatial resolution. Here the development of in situ high‐pressure high‐temperature micro‐tomography using a rotating module for the Paris–Edinburgh cell combined with synchrotron radiation is described. By rotating the sample chamber by 360°, the limited angular aperture of ordinary high‐pressure cells is surmounted. Such a non‐destructive high‐resolution probe provides three‐dimensional insight on the morphological and structural evolution of crystalline as well as amorphous phases during high pressure and temperature treatment. To demonstrate the potentials of this new experimental technique the compression behavior of a basalt glass is investigated by X‐ray absorption tomography, and diffraction/scattering tomography imaging of the structural changes during the polymerization of C 60 molecules under pressure is performed. Small size and weight of the loading frame and rotating module means that this apparatus is portable, and can be readily installed on most synchrotron facilities to take advantage of the diversity of three‐dimensional imaging techniques available at beamlines. This experimental breakthrough should open new ways for in situ imaging of materials under extreme pressure–temperature–stress conditions, impacting diverse areas in physics, chemistry, geology or materials sciences.