Fig. 3: X-ray diffraction collected during XFEL irradiation of H2O at 69.3 GPa.

Data were collected using an Ag doughnut coupler (DAC 8) and an X-ray beam diameter of <8 µm FWHM. a, b Integrated XRD patterns and (c–h) unwrapped (2θ-φ) XRD images collected during irradiation with 300 XFEL pulses at 29% transmission (run 505). In (a), darker shades correspond to higher intensity. In (c–h), lighter shades correspond to higher intensity. Heating results in a splitting of the ice (110), Ag (111), and Ag (200) reflections, which is indicative of two distinct temperatures in the probed volume, predominantly originating from the lack of thermal insulation between the H2O and the diamond anvils. Panel (a) illustrates how heating occurs during the first ~20 pulses, after which the diffracted signal from H2O remains essentially constant. In (d), the diameters of the orange circles are unrelated to individual spot sizes. Source data are provided as a Source Data file.