Intense Reactivity in Sulfur–Hydrogen Mixtures at High Pressure under X-ray Irradiation

Pace, Edward J.; Coleman, Amy L.; Husband, R. J.; Hwang, Ho Kyoung; Choi, Jae Chan; Kim, Tae Hyun; Hwang, Gil Chan; Chun, Sae Hwan; Nam, Daewoong; Kim, Sang Soo; Ball, Orianna B.; Liermann, Hanns‐Peter; McMahon, M. I.; Lee, Yong Jae; McWilliams, R. S.

doi:10.1021/acs.jpclett.9b03797

Cited by 13 publications

(10 citation statements)

References 37 publications

(118 reference statements)

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“…At this repetition rate, XFEL pulses were so close in time (443 ns) that they may be used to pump and probe in-situ chemical reactions. 13,29 A DAC with 500 μm culets was used as a pre-compression chamber. A small piece of a 4 μm thick Fe foil (< 250 μm × 250 μm, 99.99% purity) was loaded into a cylindrical chamber of 310 μm diameter and 50 μm height made by electro-spark erosion in a pre-indented rhenium gasket (Figure 1).…”

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confidence: 99%

“…Diamond-anvil cell (DAC) experiments are suitable for such studies because the contained gas can function simultaneously as a pressure-transmitting medium (PTM) and a reactant. To trigger a chemical reaction, the energy of intense electromagnetic radiation pulses can be used . Time-resolved diffraction and spectroscopic studies in a DAC at XFEL facilities have the potential to elucidate the formation and dynamics of new materials under extreme conditions.…”

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confidence: 99%

“…The fluence incident on the DAC at 100% transmission was 187(48) μJ/pulse over a spot size of 14 ± 1 μm fwhm, focused by the compound refractive lens (CRL), as measured using damage imprinting in freestanding Ta foil. At this repetition rate, XFEL pulses were so close in time (443 ns) that they may be used to pump and probe in situ chemical reactions. , …”

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confidence: 99%

“…To trigger a chemical reaction, the energy of intense electromagnetic radiation pulses can be used. 13 Time-resolved diffraction and spectroscopic studies in a DAC at XFEL facilities have the potential to elucidate the formation and dynamics of new materials under extreme conditions.…”

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confidence: 99%

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X-ray Free Electron Laser-Induced Synthesis of ε-Iron Nitride at High Pressures

Hwang

Kim

Cynn

et al. 2021

J. Phys. Chem. Lett.

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The ultrafast synthesis of ε-Fe 3 N 1+x in a diamond-anvil cell (DAC) from Fe and N 2 under pressure was observed using serial exposures of an X-ray free electron laser (XFEL). When the sample at 5 GPa was irradiated by a pulse train separated by 443 ns, the estimated sample temperature at the delay time was above 1400 K, confirmed by in situ transformation of αto γ-iron. Ultimately, the Fe and N 2 reacted uniformly throughout the beam path to form Fe 3 N 1.33 , as deduced from its established equation of state (EOS). We thus demonstrate that the activation energy provided by intense X-ray exposures in an XFEL can be coupled with the source time structure to enable exploration of the time-dependence of reactions under high-pressure conditions.

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X-ray Free Electron Laser-Induced Synthesis of ε-Iron Nitride at High Pressures

Hwang

Kim

Cynn

et al. 2021

J. Phys. Chem. Lett.

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“…Current explorations of how best to integrate DAC techniques with XFEL sources focus on probing conditions of rapidly varying pressure and temperature states using piezoelectrically driven pressure cells (dynamic DAC or dDAC) and pulsed optical laser heating (e.g. Liermann, 2014;Liermann et al, 2016), or the use of the X-ray source itself for dynamic excitation (Meza-Galvez et al, 2020;Pace et al, 2020).…”

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confidence: 99%

Novel experimental setup for megahertz X-ray diffraction in a diamond anvil cell at the High Energy Density (HED) instrument of the European X-ray Free-Electron Laser (EuXFEL)

Liermann¹,

Konôpková²,

Appel³

et al. 2021

J Synchrotron Rad

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The high-precision X-ray diffraction setup for work with diamond anvil cells (DACs) in interaction chamber 2 (IC2) of the High Energy Density instrument of the European X-ray Free-Electron Laser is described. This includes beamline optics, sample positioning and detector systems located in the multipurpose vacuum chamber. Concepts for pump–probe X-ray diffraction experiments in the DAC are described and their implementation demonstrated during the First User Community Assisted Commissioning experiment. X-ray heating and diffraction of Bi under pressure, obtained using 20 fs X-ray pulses at 17.8 keV and 2.2 MHz repetition, is illustrated through splitting of diffraction peaks, and interpreted employing finite element modeling of the sample chamber in the DAC.

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Ultrafast Yttrium Hydride Chemistry at High Pressures via Non-equilibrium States Induced by an X-ray Free Electron Laser

Siska,

Smith,

Villa-Cortes

et al. 2024

J. Phys. Chem. Lett.

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Controlling the formation and stoichiometric content of the desired phases of materials has become of central interest for a variety of fields. The possibility of accessing metastable states by initiating reactions by X-ray-triggered mechanisms over ultrashort time scales has been enabled by the development of X-ray free electron lasers (XFELs). Utilizing the exceptionally highbrilliance X-ray pulses from the EuXFEL, we report the synthesis of a previously unobserved yttrium hydride under high pressure, along with nonstoichiometric changes in hydrogen content as probed at a repetition rate of 4.5 MHz using time-resolved X-ray diffraction. Exploiting non-equilibrium pathways, we synthesize and characterize a hydride in a Weaire−Phelan structure type at pressures as low as 125 GPa, predicted using a crystal structure search, with a hydrogen content of 4.0−5.75 hydrogens per cation, that is enthalpically metastable on the convex hull.Letter pubs.acs.org/JPCL

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Intense Reactivity in Sulfur–Hydrogen Mixtures at High Pressure under X-ray Irradiation

Cited by 13 publications

References 37 publications

X-ray Free Electron Laser-Induced Synthesis of ε-Iron Nitride at High Pressures

X-ray Free Electron Laser-Induced Synthesis of ε-Iron Nitride at High Pressures

Novel experimental setup for megahertz X-ray diffraction in a diamond anvil cell at the High Energy Density (HED) instrument of the European X-ray Free-Electron Laser (EuXFEL)

Ultrafast Yttrium Hydride Chemistry at High Pressures via Non-equilibrium States Induced by an X-ray Free Electron Laser

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