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

H Hélène Ginestet (Univ. Lille, CNRS, INRAE, Centrale Lille, UMR 8207—UMET—Unité Matériaux et Transformations 1 , F-59000 Lille,) R Rachel J. Husband (Deutsches Elektronen‐Synchrotron DESY Notkestr. 85 22607 Hamburg Germany) N Nicolas Jaisle (Centre for Science at Extreme Conditions and School of Physics and Astronomy University of Edinburgh King's Buildings Edinburgh EH9 3FD UK) E Eric Edmund (Earth and Planets Laboratory Carnegie Institution for Science 5241 Broad Branch Rd., NW Washington DC 20015 USA) Z Zuzana Konôpková (European XFEL, Holzkoppel 4, 22869 Schenefeld, Germany) C Cornelius Strohm (Deutsches Elektronen-Synchrotron DESY, Notkestr. 85, 22607 Hamburg, Germany) M Madden S. Anae (Department of Geosciences, Stony Brook University 7 , Stony Brook, New York 11794-2100,) D Daniele Antonangeli (Sorbonne Université, Muséum National d’Histoire Naturelle, UMR CNRS 7590, Institut de Minéralogie, de Physique des Matériaux et de Cosmochimie (IMPMC) 8 , Paris,) K Karen Appel O Orianna B. Ball (SUPA, School of Physics and Astronomy, and Centre for Science at Extreme Conditions (CSEC), The University of Edinburgh 4 , Peter Guthrie Tait Road, Edinburgh EH9 3FD,) M Marzena Baron (Sorbonne Université, CNRS, Laboratoire Chimie de la Matière Condensée de Paris (LCMCP) 9 , 4 place Jussieu, 75005 Paris,) S Silvia Boccato (Sorbonne Université, Muséum National d’Histoire Naturelle, UMR CNRS 7590, Institut de Minéralogie, de Physique des Matériaux et de Cosmochimie (IMPMC) 8 , Paris,) K Khachiwan Buakor (European XFEL, Holzkoppel 4, 22869 Schenefeld, Germany) J Julien Chantel H Hyunchae Cynn (Lawrence Livermore National Laboratory, Physical and Life Science Directorate 10 , Livermore, California 94550,) A Anand P. Dwivedi (Earth and Planets Laboratory, Carnegie Institution for Science 5 , 5251 Broad Branch Rd., Washington, DC 20015,) H Heinz Graafsma (Deutsches Elektronen-Synchrotron DESY, Notkestr. 85, 22607 Hamburg, Germany) E Egor Koemets (Department of Earth Sciences, University of Oxford 11 , 3 South Parks Road, OX1 3AN Oxford,) T Torsten Laurus (Deutsches Elektronen-Synchrotron DESY, Notkestr. 85, 22607 Hamburg, Germany) H Hauke Marquardt (Department of Earth Sciences, University of Oxford 11 , 3 South Parks Road, OX1 3AN Oxford,) B Bernhard Massani (University of Edinburgh , , ,) J James D. McHardy (SUPA, School of Physics and Astronomy, and Centre for Science at Extreme Conditions (CSEC), The University of Edinburgh 4 , Peter Guthrie Tait Road, Edinburgh EH9 3FD,) M Malcolm I. McMahon (SUPA, School of Physics and Astronomy, and Centre for Science at Extreme Conditions (CSEC), The University of Edinburgh 4 , Peter Guthrie Tait Road, Edinburgh EH9 3FD,) V Vitali Prakapenka (University of Chicago , , 5640 South Ellis Avenue , , ,) J Jolanta Sztuk-Dambietz (European XFEL, Holzkoppel 4, 22869 Schenefeld, Germany) M Minxue Tang (European XFEL, Holzkoppel 4, 22869 Schenefeld, Germany) T Tianqi Xie (Department of Geosciences, Stony Brook University 7 , Stony Brook, New York 11794-2100,) Z Zena Younes (Centre for Science at Extreme Conditions and School of Physics and Astronomy University of Edinburgh King's Buildings Edinburgh EH9 3FD UK) U Ulf Zastrau A Alexander F. Goncharov (The Earth and Planets Laboratory, Carnegie Institution for Science 2 , Washington, District of Columbia 20015,) C Clemens Prescher (Institute of Earth and Environmental Sciences—Geomaterials and Crystalline Materials, Albert-Ludwigs Universität Freiburg 15 , Hermann-Herder Str. 5, 79104 Freiburg,) A Agnès Dewaele (CEA, DAM, DIF 16 , 91297 Arpajon,) R R. Stewart McWilliams (The School of Physics and Astronomy and Centre for Science at Extreme Conditions) G Guillaume Morard S Sébastien Merkel (Univ. Lille, CNRS, INRAE, Centrale Lille, UMR8207—UMET—Unité Matériaux et Transformations 2 , 59000 Lille,)

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.

Article Details

Volume / Issue Vol. 139, Issue 4
Published January 28, 2026
ISSN 0021-8979
Publisher American Institute of Physics

Journal Info

Journal of Applied Physics

American Institute of Physics

ISSN: 0021-8979 Physical Sciences

Authors (35)

H

Hélène Ginestet

Univ. Lille, CNRS, INRAE, Centrale Lille, UMR 8207—UMET—Unité Matériaux et Transformations 1 , F-59000 Lille,

R

Rachel J. Husband

Deutsches Elektronen‐Synchrotron DESY Notkestr. 85 22607 Hamburg Germany

N

Nicolas Jaisle

Centre for Science at Extreme Conditions and School of Physics and Astronomy University of Edinburgh King's Buildings Edinburgh EH9 3FD UK

E

Eric Edmund

Earth and Planets Laboratory Carnegie Institution for Science 5241 Broad Branch Rd., NW Washington DC 20015 USA

Z

Zuzana Konôpková

European XFEL, Holzkoppel 4, 22869 Schenefeld, Germany

C

Cornelius Strohm

Deutsches Elektronen-Synchrotron DESY, Notkestr. 85, 22607 Hamburg, Germany

M

Madden S. Anae

Department of Geosciences, Stony Brook University 7 , Stony Brook, New York 11794-2100,

D

Daniele Antonangeli

Sorbonne Université, Muséum National d’Histoire Naturelle, UMR CNRS 7590, Institut de Minéralogie, de Physique des Matériaux et de Cosmochimie (IMPMC) 8 , Paris,

K

Karen Appel

O

Orianna B. Ball

SUPA, School of Physics and Astronomy, and Centre for Science at Extreme Conditions (CSEC), The University of Edinburgh 4 , Peter Guthrie Tait Road, Edinburgh EH9 3FD,

M

Marzena Baron

Sorbonne Université, CNRS, Laboratoire Chimie de la Matière Condensée de Paris (LCMCP) 9 , 4 place Jussieu, 75005 Paris,

S

Silvia Boccato

Sorbonne Université, Muséum National d’Histoire Naturelle, UMR CNRS 7590, Institut de Minéralogie, de Physique des Matériaux et de Cosmochimie (IMPMC) 8 , Paris,

K

Khachiwan Buakor

European XFEL, Holzkoppel 4, 22869 Schenefeld, Germany

J

Julien Chantel

H

Hyunchae Cynn

Lawrence Livermore National Laboratory, Physical and Life Science Directorate 10 , Livermore, California 94550,

A

Anand P. Dwivedi

Earth and Planets Laboratory, Carnegie Institution for Science 5 , 5251 Broad Branch Rd., Washington, DC 20015,

H

Heinz Graafsma

Deutsches Elektronen-Synchrotron DESY, Notkestr. 85, 22607 Hamburg, Germany

E

Egor Koemets

Department of Earth Sciences, University of Oxford 11 , 3 South Parks Road, OX1 3AN Oxford,

T

Torsten Laurus

Deutsches Elektronen-Synchrotron DESY, Notkestr. 85, 22607 Hamburg, Germany

H

Hauke Marquardt

Department of Earth Sciences, University of Oxford 11 , 3 South Parks Road, OX1 3AN Oxford,

B

Bernhard Massani

University of Edinburgh , , ,

J

James D. McHardy

SUPA, School of Physics and Astronomy, and Centre for Science at Extreme Conditions (CSEC), The University of Edinburgh 4 , Peter Guthrie Tait Road, Edinburgh EH9 3FD,

M

Malcolm I. McMahon

SUPA, School of Physics and Astronomy, and Centre for Science at Extreme Conditions (CSEC), The University of Edinburgh 4 , Peter Guthrie Tait Road, Edinburgh EH9 3FD,

V

Vitali Prakapenka

University of Chicago , , 5640 South Ellis Avenue , , ,

J

Jolanta Sztuk-Dambietz

European XFEL, Holzkoppel 4, 22869 Schenefeld, Germany

M

Minxue Tang

European XFEL, Holzkoppel 4, 22869 Schenefeld, Germany

T

Tianqi Xie

Department of Geosciences, Stony Brook University 7 , Stony Brook, New York 11794-2100,

Z

Zena Younes

Centre for Science at Extreme Conditions and School of Physics and Astronomy University of Edinburgh King's Buildings Edinburgh EH9 3FD UK

U

Ulf Zastrau

A

Alexander F. Goncharov

The Earth and Planets Laboratory, Carnegie Institution for Science 2 , Washington, District of Columbia 20015,

C

Clemens Prescher

Institute of Earth and Environmental Sciences—Geomaterials and Crystalline Materials, Albert-Ludwigs Universität Freiburg 15 , Hermann-Herder Str. 5, 79104 Freiburg,

A

Agnès Dewaele

CEA, DAM, DIF 16 , 91297 Arpajon,

R

R. Stewart McWilliams

The School of Physics and Astronomy and Centre for Science at Extreme Conditions

G

Guillaume Morard

S

Sébastien Merkel

Univ. Lille, CNRS, INRAE, Centrale Lille, UMR8207—UMET—Unité Matériaux et Transformations 2 , 59000 Lille,