DOE OSTI · 3388195
Metrology for femtosecond pulsed x-ray heating in diamond anvil cell experiments at the European XFEL: Revisiting the iron phase diagram up to 150 GPa
Abstract
The development of pulsed intense x-ray sources, such as free electron laser, offers new avenues for high pressure experiments. Here, we study the feasibility and metrology of x-ray heating in diamond anvil cells at the European x-ray free electron laser. This method enables one to volumetrically heat the sample while inhibiting chemical migration and probing the crystallographic structure of the sample throughout the heating with a high repetition rate. We focus our study on iron, whose phase diagram is well established up to 100 GPa, to explore the possibilities and limitations of this technique. We volumetrically heat iron samples at starting pressures ranging from 10 to 138 GPa, using the x-ray beam pulsed at 4.5 MHz in a serial pump-and-probe experimental design. Experimental challenges arise from temperature gradients within the sample, changes in temperature at the 100 ns timescale, the difficulty of direct temperature estimates, the effect of thermal pressure, and the presence of metastable crystallites due to rapid cycles of heating and cooling. Hence, we develop a multi-crystal-like data processing method that allows us to account for sample heterogeneity in probed conditions. We then calibrate our measurements using known physical properties of iron under pressure. Thermal pressure in our experiments increases from 4% of the isochoric prediction at 10 GPa to 23% at 138 GPa, and we show that our data are in agreement with most previous observations of iron in this pressure range. The method can now be implemented at higher pressures and temperatures and on materials with unknown phase diagrams.
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Ginestet, Hélène [Université de Lille (France); Centre National de la Recherche Scientifique (CNRS), Lille (France). Unité Matériaux et Transformations (UMET); French National Research Institute for Agriculture, Food and Environment (INRAE), Lille (France); École Centrale de Lille (France)] (ORCID:0000000269314062), Husband, Rachel J. [Deutsches Elektronen-Synchrotron (DESY), Hamburg (Germany)] (ORCID:000000027666401X), Jaisle, Nicolas [University of Grenoble Alpes, Grenoble (France); Centre National de la Recherche Scientifique (CNRS), Grenoble (France). Institut des Sciences de la Terre (ISTerre); University of Edinburgh, Scotland (United Kingdom)] (ORCID:0000000301295050), Edmund, Eric [Carnegie Institution of Science, Stanford, CA (United States)] (ORCID:0000000343637434), Konôpková, Zuzana [European XFEL, Schenefeld (Germany)] (ORCID:0000000189056307), Strohm, Cornelius [Deutsches Elektronen-Synchrotron (DESY), Hamburg (Germany)] (ORCID:0000000163840259), Anae, Madden S. [Stony Brook University, NY (United States)] (ORCID:0000000187543355), Antonangeli, Daniele [Sorbonne Université, Paris (France); Muséum National d'Histoire Naturelle (MNHN), Paris (France); Centre National de la Recherche Scientifique (CNRS), Paris (France). Institut de Minéralogie, de Physique des Matériaux et de Cosmochimie (IMPMC)] (ORCID:0000000249525700), Appel, Karen [European XFEL, Schenefeld (Germany)] (ORCID:0000000229022102), Ball, Orianna B. [University of Edinburgh, Scotland (United Kingdom)] (ORCID:0000000252150153), Baron, Marzena [Sorbonne Université, Paris (France); Centre National de la Recherche Scientifique (CNRS), Paris (France). Laboratoire Chimie de la Matière Condensée de Paris (LCMCP)] (ORCID:0000000256222177), Boccato, Silvia [Sorbonne Université, Paris (France); Muséum National d'Histoire Naturelle (MNHN), Paris (France); Centre National de la Recherche Scientifique (CNRS), Paris (France). Institut de Minéralogie, de Physique des Matériaux et de Cosmochimie (IMPMC)] (ORCID:0000000206138276), Buakor, Khachiwan [European XFEL, Schenefeld (Germany)] (ORCID:0000000302572822), Chantel, Julien [Université de Lille (France); Centre National de la Recherche Scientifique (CNRS), Lille (France). Unité Matériaux et Transformations (UMET); French National Research Institute for Agriculture, Food and Environment (INRAE), Lille (France); École Centrale de Lille (France)] (ORCID:0000000283329033), Cynn, Hyunchae [Lawrence Livermore National Laboratory (LLNL), Livermore, CA (United States)] (ORCID:0000000346585764), Dwivedi, Anand P. [Carnegie Institution of Science, Washington, DC (United States); European XFEL, Schenefeld (Germany)] (ORCID:0009000874970444), Graafsma, Heinz [Deutsches Elektronen-Synchrotron (DESY), Hamburg (Germany)] (ORCID:000000032304667X), Koemets, Egor [University of Oxford (United Kingdom); Harwell Science and Innovation Campus, Didcot (United Kingdom). Diamond Light Source, Ltd.] (ORCID:0000000310929406), Laurus, Torsten [Deutsches Elektronen-Synchrotron (DESY), Hamburg (Germany)], Marquardt, Hauke [University of Oxford (United Kingdom)] (ORCID:0000000317846515), Massani, Bernhard [University of Edinburgh, Scotland (United Kingdom)] (ORCID:0000000258171780), McHardy, James D. [University of Edinburgh, Scotland (United Kingdom)] (ORCID:0000000226308092), McMahon, Malcolm I. [University of Edinburgh, Scotland (United Kingdom)] (ORCID:000000034343344X), Prakapenka, Vitali [University of Chicago, IL (United States). Center for Advanced Radiation Sources (CARS)] (ORCID:0000000192702330), Sztuk-Dambietz, Jolanta [European XFEL, Schenefeld (Germany)], Tang, Minxue [Deutsches Elektronen-Synchrotron (DESY), Hamburg (Germany)] (ORCID:0000000239230677), Xie, Tianqi [Stony Brook University, NY (United States); University of Saskatchewan, Saskatoon, SK (Canada)] (ORCID:0000000337066583), Younes, Zena [University of Edinburgh, Scotland (United Kingdom)] (ORCID:0009000595842132), Zastrau, Ulf [European XFEL, Schenefeld (Germany)] (ORCID:0000000235754449), Goncharov, Alexander F. [Carnegie Institution of Science, Washington, DC (United States)] (ORCID:0000000264228819), Prescher, Clemens [Albert-Ludwigs Universität Freiburg (Germany)] (ORCID:0000000295561032), Dewaele, Agnès [CEA, DAM, DIF, Arpajon (France); Université Paris-Saclay, Bruyères-le-Châtel (France); Commissariat a l'Energie Atomique (CEA), Bruyères-le-Châtel (France). Laboratoire Matière en Conditions Extrêmes (LMCE)] (ORCID:0000000241944476), McWilliams, R. Stewart [University of Edinburgh, Scotland (United Kingdom)] (ORCID:0000000237308661), Morard, Guillaume [University of Grenoble Alpes, Grenoble (France); Centre National de la Recherche Scientifique (CNRS), Grenoble (France). Institut des Sciences de la Terre (ISTerre); Sorbonne Université, Paris (France); Muséum National d'Histoire Naturelle (MNHN), Paris (France); Centre National de la Recherche Scientifique (CNRS), Paris (France). Institut de Minéralogie, de Physique des Matériaux et de Cosmochimie (IMPMC)] (ORCID:0000000242250767), Merkel, Sébastien [Université de Lille (France); Centre National de la Recherche Scientifique (CNRS), Lille (France). Unité Matériaux et Transformations (UMET); French National Research Institute for Agriculture, Food and Environment (INRAE), Lille (France); École Centrale de Lille (France)] (ORCID:000000032767581X). 2026-01-23. Metrology for femtosecond pulsed x-ray heating in diamond anvil cell experiments at the European XFEL: Revisiting the iron phase diagram up to 150 GPa. https://doi.org/10.1063/5.0303953
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