Simultaneous imaging and diffraction in the dynamic diamond anvil cell.

The ability to visualize a sample undergoing a pressure-induced phase transition allows for the determination of kinetic parameters, such as the nucleation and growth rates of the high-pressure phase. For samples that are opaque to visible light (such as metallic systems), it is necessary to rely on x-ray imaging methods for sample visualization. Here, we present an experimental platform developed at beamline P02.2 at the PETRA III synchrotron radiation source, which is capable of performing simultaneous x-ray imaging and diffraction of samples that are dynamically compressed in piezo-driven diamond anvil cells. This setup utilizes a partially coherent monochromatic x-ray beam to perform lensless phase contrast imaging, which can be carried out using either a parallel- or focused-beam configuration. The capabilities of this platform are illustrated by experiments on dynamically compressed Ga and Ar. Melting and solidification were identified based on the observation of solid/liquid phase boundaries in the x-ray images and corresponding changes in the x-ray diffraction patterns collected during the transition, with significant edge enhancement observed in the x-ray images collected using the focused-beam. These results highlight the suitability of this technique for a variety of purposes, including melt curve determination.

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).

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.

New dynamic diamond anvil cells for tera-pascal per second fast compression x-ray diffraction experiments.

Fast compression experiments performed using dynamic diamond anvil cells (dDACs) employing piezoactuators offer the opportunity to study compression-rate dependent phenomena. In this paper, we describe an experimental setup which allows us to perform time-resolved x-ray diffraction during the fast compression of materials using improved dDACs. The combination of the high flux available using a 25.6 keV x-ray beam focused with a linear array of compound refractive lenses and the two fast GaAs LAMBDA detectors available at the Extreme Conditions Beamline (P02.2) at PETRA III enables the collection of x-ray diffraction patterns at an effective repetition rate of up to 4 kHz. Compression rates of up to 160 TPa/s have been achieved during the compression of gold in a 2.5 ms fast compression using improved dDAC configurations with more powerful piezoactuators. The application of this setup to low-Z compounds at lower compression rates is described, and the high temporal resolution of the setup is demonstrated. The possibility of applying finely tuned pressure profiles opens opportunities for future research, such as using oscillations of the piezoactuator to mimic propagation of seismic waves in the Earth.

Single crystal toroidal diamond anvils for high pressure experiments beyond 5 megabar.

Static compression experiments over 4 Mbar are rare, yet critical for developing accurate fundamental physics and chemistry models, relevant to a range of topics including modeling planetary interiors. Here we show that focused ion beam crafted toroidal single-crystal diamond anvils with ~9.0 µm culets are capable of producing pressures over 5 Mbar. The toroidal surface prevents gasket outflow and provides a means to stabilize the central culet. We have reached a maximum pressure of ~6.15 Mbar using Re as in situ pressure marker, a pressure regime typically accessed only by double-stage diamond anvils and dynamic compression platforms. Optimizing single-crystal diamond anvil design is key for extending the pressure range over which studies can be performed in the diamond anvil cell.

A simple and portable multi-channel pyrometer allowing temperature measurements down to 800 K on the microsecond scale.

The measurement of transient temperatures less than 1000 K for samples in laser-heated diamond anvil cells remains a challenge. Here we present the design and performance characteristics of a multi-channel pyrometer that works in the near-infrared from 1200 to 2000 nm. It has a relatively small footprint, is portable, requires only low voltage power supplies, and can report temperatures down to 800 K on the millisecond scale or faster. A single data point without averaging can be acquired in 14 µs (sampling rate of 7 kilosamples per second). In conjunction with a diamond anvil cell, the system delivers accurate and rapid measurements down to ∼830 K. The pyrometer has been successfully interfaced several times with the combined x-ray diffraction and laser heating system at the High Pressure Collaborative Access Team at the Advanced Photon Source at Argonne National Laboratories.

Anomalous elastic properties across the γ to α volume collapse in cerium.

The behavior of the f-electrons in the lanthanides and actinides governs important macroscopic properties but their pressure and temperature dependence is not fully explored. Cerium with nominally just one 4f electron offers a case study with its iso-structural volume collapse from the γ-phase to the α-phase ending in a critical point (p C, V C, T C), unique among the elements, whose mechanism remains controversial. Here, we present longitudinal (c L) and transverse sound speeds (c T) versus pressure from higher than room temperature to T C for the first time. While c L experiences a non-linear dip at the volume collapse, c T shows a step-like change. This produces very peculiar macroscopic properties: the minimum in the bulk modulus becomes more pronounced, the step-like increase of the shear modulus diminishes and the Poisson's ratio becomes negative-meaning that cerium becomes auxetic. At the critical point itself cerium lacks any compressive strength but offers resistance to shear.

Strength and Debye temperature measurements of cerium across the γ → α volume collapse: the lattice contribution.

The longitudinal and transverse sound speeds, cL and cT, of polycrystalline cerium were measured under pressure across the iso-structural γ-α phase transition at 0.75 GPa to beyond 3 GPa. In contrast to previous methods all quantities were directly obtained and no assumptions were made about the size of the volume collapse. Up to the transition our values for cL are in excellent agreement with previous ones, while our values for cT are significantly lower. We deduce values for the adiabatic bulk modulus BS, the shear modulus [Formula: see text], and the pressure dependent Debye temperature, ΘD(p). ΘD(p) is in good agreement with recent results derived from phonon dispersion measurements on single crystals. The ratio of the Debye temperature values bracketing the transition indicates a lattice contribution to the entropy change across the volume collapse, ΔSvib(γ â†’ α) ≈ (0.68 ± 0.06)kB, consistent with previous results obtained by neutron scattering, but significantly larger than other previously determined values.