Dynamic Diamond Anvil Cell Research Articles

Automated pipeline processing X-ray diffraction data from dynamic compression experiments on the Extreme Conditions Beamline of PETRAIII.

Presented and discussed here is the implementation of a software solution that provides prompt X-ray diffraction data analysis during fast dynamic compression experiments conducted within the dynamic diamond anvil cell technique. It includes efficient data collection, streaming of data and metadata to a high-performance cluster (HPC), fast azimuthal data integration on the cluster, and tools for controlling the data processing steps and visualizing the data using the DIOPTAS software package. This data processing pipeline is invaluable for a great number of studies. The potential of the pipeline is illustrated with two examples of data collected on ammonia-water mixtures and multiphase mineral assemblies under high pressure. The pipeline is designed to be generic in nature and could be readily adapted to provide rapid feedback for many other X-ray diffraction techniques, e.g. large-volume press studies, in situ stress/strain studies, phase transformation studies, chemical reactions studied with high-resolution diffraction etc.

Time‐resolved Raman spectroscopy study of rapid compressed silicon and its potential as a Raman pressure scale in a dynamic diamond anvil cell

AbstractThe nature of the nonequilibrium states of materials upon rapid compression/decompression processes in the intermediate regime, between static and shock compression, is an emerging field of high pressure research. Rapid compression experiments were performed to examine the structural response of silicon (Si) up to 11 GPa and over compression rates ranging from 0.011 to 0.325 GPa/s, using a piezo‐driven dynamic diamond anvil cell (dDAC) coupled with time‐resolved Raman spectroscopy. The observed structural stability and the remarkable consistency in the pressure‐dependent Raman shift of the diamond cubic Si (Si‐I) showed its high potential as a Raman pressure scale for compression rate below 0.325 GPa/s. The validity of the derived Si scale was verified by in situ continuously monitoring pressure of two rapid compressed samples, that is, gypsum and ZnO. Results indicated that pressures determined using Si were in good agreement with those estimated from the ruby scale. Success in pressure calibration with Si, during time‐resolved Raman spectroscopy measurements of material under rapid compression using a dDAC, will greatly simplify the required hardware system in home‐laboratory and may also help in reaching a higher signal‐to‐noise in Raman measurement on a short time scale.

New dynamic diamond anvil cell for time-resolved radial x-ray diffraction

New dynamic diamond anvil cell for time-resolved radial x-ray diffraction

Time-resolved Raman spectroscopy for monitoring the structural evolution of materials during rapid compression.

Rapid compression experiments performed using a dynamic diamond anvil cell (dDAC) offer the opportunity to study compression rate-dependent phenomena, which provide critical knowledge of the phase transition kinetics of materials. However, direct probing of the structure evolution of materials is scarce and so far limited to the synchrotron based x-ray diffraction technique. Here, we present a time-resolved Raman spectroscopy technique to monitor the structural evolutions in a subsecond time resolution. Instead of applying a shutter-based synchronization scheme in previous work, we directly coupled and synchronized the spectrometers with the dDAC, providing sequential Raman data over a broad pressure range. The capability and versatility of this technique are verified by in situ observation of the phase transition processes of three rapid compressed samples. Not only the phase transition pressures but also the transition pathways are reproduced with good accuracy. This approach has the potential to serve as an important complement to x-ray diffraction applied to study the kinetics of phase transitions occurring on time scales of seconds and above.

Simultaneous measurements of volume, pressure, optical images, and crystal structure with a dynamic diamond anvil cell: A real-time event monitoring system.

The dynamic diamond anvil cell (dDAC) technique has attracted great interest because it possibly provides a bridge between static and dynamic compression studies with fast, repeatable, and controllable compression rates. The dDAC can be a particularly useful tool to study the pathways and kinetics of phase transitions under dynamic pressurization if simultaneous measurements of physical quantities are possible as a function of time. We here report the development of a real-time event monitoring (RTEM) system with dDAC, which can simultaneously record the volume, pressure, optical image, and structure of materials during dynamic compression runs. In particular, the volume measurement using both Fabry-Pérot interferogram and optical images facilitates the construction of an equation of state (EoS) using the dDAC in a home-laboratory. We also developed an in-line ruby pressure measurement (IRPM) system to be deployed at a synchrotron x-ray facility. This system provides simultaneous measurements of pressure and x-ray diffraction in low and narrow pressure ranges. The EoSs of ice VI obtained from the RTEM and the x-ray diffraction data with the IRPM are consistent with each other. The complementarity of both RTEM and IRPM systems will provide a great opportunity to scrutinize the detailed kinetic pathways of phase transitions using dDAC.

Compressibility of ferropericlase at high-temperature: Evidence for the iron spin crossover in seismic tomography

The iron spin crossover in ferropericlase, the second most abundant mineral in Earth's lower mantle, causes changes in a range of physical properties, including seismic wave velocities. Understanding the effect of temperature on the spin crossover is essential to detect its signature in seismic observations and constrain its occurrence in the mantle. Here, we report the first experimental results on the spin crossover-induced bulk modulus softening at high temperatures, derived directly from time-resolved x-ray diffraction measurements during continuous compression of (Mg0.8Fe0.2)O in a resistive-heated dynamic diamond-anvil cell. We present new theoretical calculations of the spin crossover at mantle temperatures benchmarked by the experiments. Based on our results, we create synthetic seismic tomography models to investigate the signature of the spin crossover in global seismic tomography. A tomographic filter is applied to allow for meaningful comparisons between the synthetic models and data-based seismic tomography models, like SP12RTS. A negative anomaly in the correlation between Vs variations and Vc variations (S-C correlation) is found to be the most suitable measure to detect the presence of the spin crossover in tomographic models. When including the effects of the spin crossover, the misfit between the synthetic model and SP12RTS is reduced by 63%, providing strong evidence for the presence of the spin crossover, and hence ferropericlase, in the lower mantle. Future improvement of seismic resolution may facilitate a detailed mapping of spin state using the S-C correlation, providing constraints on mantle temperatures by taking advantage of the temperature sensitivity of the spin crossover.

A MHz X-ray diffraction set-up for dynamic compression experiments in the diamond anvil cell.

An experimental platform for dynamic diamond anvil cell (dDAC) research has been developed at the High Energy Density (HED) Instrument at the European X-ray Free Electron Laser (European XFEL). Advantage was taken of the high repetition rate of the European XFEL (up to 4.5 MHz) to collect pulse-resolved MHz X-ray diffraction data from samples as they are dynamically compressed at intermediate strain rates (≤103 s-1), where up to 352 diffraction images can be collected from a single pulse train. The set-up employs piezo-driven dDACs capable of compressing samples in ≥340 µs, compatible with the maximum length of the pulse train (550 µs). Results from rapid compression experiments on a wide range of sample systems with different X-ray scattering powers are presented. A maximum compression rate of 87 TPa s-1 was observed during the fast compression of Au, while a strain rate of ∼1100 s-1 was achieved during the rapid compression of N2 at 23 TPa s-1.

Pressure- and Rate-Dependent Mechanoluminescence with Maximized Efficiency and Tunable Wavelength in ZnS: Mn2+, Eu3.

Mechanoluminescence (ML) has received widespread attention because of potential application in stress sensors and imaging. However, pursuing highly efficient ML remains a challenge due to multifactorial limitations such as pressure and loading rate. Here, we systematically investigate pressure- and rate-dependent ML in Mn2+ and Eu3+ co-doped ZnS in a gigapascal pressure range by using a high-pressure dynamic diamond anvil cell and microsecond time-resolved fluorescent methods and demonstrate the giant tunability in both ML efficiency and wavelength. Compressed from ambient pressure to 11 GPa at different compression rates, ZnS: Mn2+, Eu3+ exhibits a volcano shape in ML emission efficiency with an optimum at ∼3.5 GPa and ∼211.1 GPa/s, at least 1000-fold higher than that measured in the MPa range. The pressure-dependent ML is accompanied with a tunable yellow-to-red emission color change. A combination of high-pressure X-ray diffraction and photoluminescence measurements reveals that the pressure- and rate-dependent ML behavior derives from pressure-induced strengthening of the crystal piezoelectric field and enhanced interaction between the host lattice and doped ions with a significant change of the energy level of the Mn ion. Significantly, the highly efficient ML of ZnS: Mn2+, Eu3+ at the GPa level is reproducible under a compression-decompression process and can be manipulated on a micron scale, implying great potential in mechanical-optical energy conversion and application in dynamic pressure imaging, stress sensors, and multicolor displays.

Evidence for a rosiaite-structured high-pressure silica phase and its relation to lamellar amorphization in quartz

When affected by impact, quartz (SiO2) undergoes an abrupt transformation to glass lamellae, the planar deformation features (PDFs). This shock effect is the most reliable indicator of impacts and is decisive in identifying catastrophic collisions in the Earth´s record such as the Chicxulub impact. Despite the significance of PDFs, there is still no consensus how they form. Here, we present time-resolved in-situ synchroton X-ray diffraction data of single-crystal quartz rapidly compressed in a dynamic diamond anvil cell. These experiments provide evidence for the transformation of quartz at pressures above 15 GPa to lamellae of a metastable rosiaite (PbSb2O6)-type high-pressure phase with octahedrally coordinated silicon. This phase collapses during decompression to amorphous lamellae, which closely resemble PDFs in naturally shocked quartz. The identification of rosiaite-structured silica provides thus an explanation for lamellar amorphization of quartz. Furthermore, it suggests that the mixed phase region of the Hugoniot curve may be related to the progressive formation of rosiaite-structured silica.

Broad Elastic Softening of (Mg,Fe)O Ferropericlase Across the Iron Spin Crossover and a Mixed‐Spin Lower Mantle

AbstractThe elastic bulk modulus softening of (Mg,Fe)O ferropericlase across the iron spin crossover induces dramatic changes in its physical properties, including seismic P‐velocities and viscosity. Here, we performed compression of powders of (Mg0.8‐0.9Fe0.2‐0.1)O in a piezo‐driven dynamic Diamond Anvil Cell (dDAC) and derive the bulk modulus by differentiation of pressure and volume data, providing first data on the broadness of the elastic softening for ferropericlase with mantle‐relevant compositions. We complement our experimental results with theoretical calculations that extend previous studies by considering multiple random configurations of iron, and going beyond treating high‐ and low‐spin iron as an ideal solution. Both experiments and computations show a broad and asymmetric softening of the bulk modulus, and suggest that the softening is sensitive to the distribution of iron in the ferropericlase structure. Our high‐temperature calculations show that mixed‐spin (Mg,Fe)O dominates the lower mantle at all depths below 1,000 km. In contrast to most previous works, we find that ferropericlase will not exist in pure low‐spin state along a typical mantle geotherm. Based on our model, the physical properties of ferropericlase will show significant lateral variation at depths below 1,400 km, with the strongest effects expected between 2,000 and 2,600 km.

Phase transitions in high-purity zirconium under dynamic compression

We present results from ramp compression experiments on high-purity Zr that show the $\ensuremath{\alpha}\ensuremath{\rightarrow}\ensuremath{\omega}, \ensuremath{\omega}\ensuremath{\rightarrow}\ensuremath{\beta}$, as well as reverse $\ensuremath{\beta}\ensuremath{\rightarrow}\ensuremath{\omega}$ phase transitions. Simulations with a multiphase equation of state and phenomenological kinetic model match the experimental wave profiles well. While the dynamic $\ensuremath{\alpha}\ensuremath{\rightarrow}\ensuremath{\omega}$ transition occurs $\ensuremath{\sim}9\phantom{\rule{0.16em}{0ex}}\mathrm{GPa}$ above the equilibrium phase boundary, the $\ensuremath{\omega}\ensuremath{\rightarrow}\ensuremath{\beta}$ transition occurs within 0.9 GPa of equilibrium. We estimate that the dynamic compression path intersects the equilibrium $\ensuremath{\omega}\text{\ensuremath{-}}\ensuremath{\beta}$ line at $P=29.2\phantom{\rule{0.16em}{0ex}}\mathrm{GPa}$, and $T=490\phantom{\rule{0.16em}{0ex}}\mathrm{K}$. The thermodynamic path in the interior of the sample lies $\ensuremath{\sim}100\phantom{\rule{0.16em}{0ex}}\mathrm{K}$ above the isentrope at the point of the $\ensuremath{\omega}\ensuremath{\rightarrow}\ensuremath{\beta}$ transition. Approximately half of this dissipative temperature rise is due to plastic work, and half is due to the nonequilibrium $\ensuremath{\alpha}\ensuremath{\rightarrow}\ensuremath{\omega}$ transition. The inferred rate of the $\ensuremath{\alpha}\ensuremath{\rightarrow}\ensuremath{\omega}$ transition is several orders of magnitude higher than that measured in dynamic diamond anvil cell (DDAC) experiments in an overlapping pressure range. We discuss a model for the influence of shear stress on the nucleation rate. We find that the shear stress ${s}_{ji}$ has the same effect on the nucleation rate as a pressure increase $\ensuremath{\delta}P=c{\ensuremath{\epsilon}}_{ij}{s}_{ji}/(\mathrm{\ensuremath{\Delta}}V/V),$ where $c$ is a geometric constant $\ensuremath{\sim}1$ and ${\ensuremath{\epsilon}}_{ij}$ are the transformation shear strains. The small fractional volume change $\mathrm{\ensuremath{\Delta}}V/V\ensuremath{\approx}0.1$ at the $\ensuremath{\alpha}\ensuremath{\rightarrow}\ensuremath{\omega}$ transition amplifies the effect of shear stress, and we estimate that for this case $\ensuremath{\delta}P$ is in the range of several GPa. Correcting our transition rate to a hydrostatic rate brings it approximately into line with the DDAC results, suggesting that shear stress plays a significant role in the transformation rate.

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.

In Situ Study on Dehydration and Phase Transformation of Antigorite

Antigorite is the main carrier of water in Earth’s subduction zones. The dehydration processes of antigorite were investigated by carrying out in situ phase transition experiments using a dynamic diamond anvil cell, with a time-resolved Raman scattering system, at 0.3–10 GPa and 396–1100 K. Three typical phase transformation reactions occurred within the P–T range of this study, corresponding to three reaction products. At low pressures (<0.7 GPa), antigorite transfers to talc and forsterite; as the temperature increases, the talc disappears and a combination of forsterite and clinoenstatite occurs. At moderate pressures (1.8–7.5 GPa), antigorite dehydrates into forsterite and clinoenstatite as temperatures increase; with the continuous increase in pressure, the dehydration products become clinoenstatite and phase A. At high pressures (>8.6 GPa), the products of the dehydration phase transition of antigorite are consistently clinoenstatite and phase A. Compared with the previous studies carried out by large-volume presses (such as a multi anvil press and a piston-cylinder press), the reaction to produce phase A occurs at higher P–T conditions, and the stable temperature region for talc as a dehydration product is narrower. Moreover, large quantities of pores with 5–10 μm in diameter formed in dehydration products, supporting the hypothesis that intermediate-depth earthquakes may result from dehydration embrittlement. The precise phase boundary determined by this in situ study provides a better understanding of the dehydration phase transition behavior and geological phenomena exhibited by antigorite under different pressure and temperature conditions.

In situ study of calcite-III dimorphism using dynamic diamond anvil cell

The phase transitions among the high-pressure polymorphic forms of CaCO3 (cc-I, cc-II, cc-III, and cc-IIIb) are investigated by dynamic diamond anvil cell (dDAC) and in situ Raman spectroscopy. Experiments are carried out at room temperature and high pressures up to 12.8 GPa with the pressurizing rate varying from 0.006 GPa/s to 0.056 GPa/s. In situ observation shows that with the increase of pressure, calcite transforms from cc-I to cc-II at ∼ 1.5 GPa and from cc-II to cc-III at ∼ 2.5 GPa, and transitions are independent of the pressurizing rate. Further, as the pressure continues to increase, the cc-IIIb begins to appear and coexists with cc-III within a pressure range that is inversely proportional to the pressurizing rate. At the pressurizing rates of 0.006, 0.012, 0.021, and 0.056 GPa/s, the coexistence pressure ranges of cc-III and cc-IIIb are 2.8 GPa–9.8 GPa, 3.1 GPa–6.9 GPa, 2.7 GPa–6.0 GPa, and 2.8 GPa–4.5 GPa, respectively. The dependence of the coexistence on the pressurizing rate may result from the influence of pressurizing rate on the activation process of transition by reducing the energy barrier. The higher the pressurizing rate, the lower the energy barrier is, and the easier it is to pull the system out of the coexistence state. The results of this in situ study provide new insights into the understanding of the phase transition of calcite.

In situx-ray diffraction study of dynamically compressedα-cristobalite using a dynamic diamond anvil cell

In this study we present results of the dynamic compression of $\ensuremath{\alpha}$-cristobalite up to a pressure of 106 GPa with the use of the dynamic diamond anvil cell. X-ray diffraction images were recorded at different ramp compression and decompression rates to investigate in situ the high-pressure phase transitions of $\ensuremath{\alpha}$-cristobalite. Our results suggest that the pressure onset of the phase transformation of $\ensuremath{\alpha}$-cristobalite to cristobalite II, cristobalite X-I, and ultimately to seifertite ($\ensuremath{\alpha}\text{\ensuremath{-}}{\mathrm{PbO}}_{2}$ type ${\mathrm{SiO}}_{2}$) is dependent on the applied compression rates and stress conditions of the experiment. Increasing compression rates in general shift the studied phase transitions to higher pressures. Furthermore, our results indicate for single crystals under hydrostatic conditions a suppression of a phase transition from cristobalite X-I to seifertite at pressures of up to 82 GPa.

Millisecond time-resolved synchrotron radiation X-ray diffraction and high-pressure rapid compression device and its application

Non-equilibrium transition dynamics under high pressure depends on temperature, pressure and (de)compression rate. The studies require combination of time-resolved probe and rapid compression device on different time scales. Here we report the time-resolved X-ray diffraction (XRD) and dynamic diamond anvil cell (dDAC) system, which were recently developed at the BL15U1 beamline of Shanghai Synchrotron Radiation Facility (SSRF). There are two rapid loading methods for dDAC. One uses membrane control and the other is piezoelectric actuator driven dDAC. Both methods can dynamically compress the DAC sample chamber up to 300 GPa on millisecond scale (20 μm culet is used), and the time-resolved XRD data are obtained correspondingly. A new type of piezoelectric ceramic dDAC is designed with single-side drive or double-side drive, which allows us to realize extremely high pressure (above 300 GPa) with a fast compression rate of 13 TPa/s. During the rapid compression process, the X-ray diffraction spectra are collected continuously and simultaneously. The XRD detector is Pilatus 3X 900K, which has 2-ms resolution with 500 kHz frame rate. The millisecond time-resolved XRD and high pressure rapid compression system developed at BL15U1 of SSRF enrich the high-pressure experimental methods and enable the beamline to carry out ultra-high pressure experiments, non-equilibrium phase transition and relevant scientific researches.

Static and dynamic diamond anvil cell (s-dDAC): A bidirectional remote controlled device for static and dynamic compression/decompression

A novel bidirectional remotely controlled device for static and dynamic compression/decompression using diamond anvil cells (DACs) has been developed that can control pressure in an accurate and consistent manner. Electromechanical piezoelectric actuators are applied to a conventional DAC, allowing applications under a variety of pressure conditions. Using this static and dynamic DAC (s-dDAC), it is possible to addresses the poorly studied experimental regime lying between purely static and purely dynamic studies. The s-dDAC, driven by three piezoelectric actuators, can be combined with a time-resolved spectral measurement system and high-speed imaging device to study the structural changes, chemical reactions, and properties of materials under extreme conditions. The maximum compression/decompression rate or pressure range highly depends on the culet size of the anvil, and a higher compression rate and wider pressure range can be realized in a DAC with smaller anvil culet. With our s-dDAC, we have been able to achieve the highest compression rate to date with a 300 μm culet anvil: 48 TPa/s. An overview of a variety of experimental measurements possible with our device is presented.

Cinema:Snap: Real-time tools for analysis of dynamic diamond anvil cell experiment data.

We developed tools and a workflow for real-time analysis of data from dynamic diamond anvil cell experiments performed at user light sources. These tools allow users to determine the phases of matter observed during the compression of materials in order to make decisions during an experiment to improve the quality of experimental results and maximize the use of scarce experimental facility time. The tools fill a gap in dynamic compression data analysis tools that are real-time, are flexible to the needs of high-pressure scientists, connect to automated processing of results, can be easily incorporated into workflows with existing tools and data formats, and support remote experimental data analysis workflows. Specific analytics developed include novel automated two-peak analysis for overlapping peaks and multiple phases, coordinated views of pressure and temperature values, full-compression contour plots, and configurable views of integrated x-ray diffraction. We present an experimental use case to show how the tools produce real-time analytics that help the scientists revise parameters for the next compression.

Compression-rate dependence of pressure-induced phase transitions in Bi

It is qualitatively well known that kinetics related to nucleation and growth can shift apparent phase boundaries from their equilibrium value. In this work, we have measured this effect in Bi using time-resolved X-ray diffraction with unprecedented 0.25 ms time resolution, accurately determining phase transition pressures at compression rates spanning five orders of magnitude (10–2–103 GPa/s) using the dynamic diamond anvil cell. An over-pressurization of the Bi-III/Bi-V phase boundary is observed at fast compression rates for different sample types and stress states, and the largest over-pressurization that is observed is ΔP = 2.5 GPa. The work presented here paves the way for future studies of transition kinetics at previously inaccessible compression rates.

Unraveling the anomalous mechanoluminescence intensity change and pressure-induced red-shift for manganese-doped zinc sulfide

Mechanoluminescence (ML) has promising applications such as stress sensors and many other fields, which raises intensive research attention and enthusiasms in the past few decades. However, accurate characterizations of the ML process with high temporal and spectral resolution remain a considerable challenge for the current scientific community. Here, an advanced ML characterization system based on the dynamic diamond anvil cell (dDAC) is developed to achieve flexible modulations of ML performances. Upon compression, the ML spectra of manganese-doped zinc sulfide (ZnS:Mn) show a large red-shift (~45 nm) and a volcano-trend of the ML intensity, where the cumulative ML intensity is solely dependent on the pressure change. DFT calculations identify the coupling of Mn-doping and surface vacancies is playing a crucial role in contributing to the improvement of ML through the band offset. The suppression of the vacancies formation on the surface by the applied pressure over 4 GPa leads to the decreases of the ML intensity. This work provides a brand new ML color and intensity tuning strategy and offers a promising method to explore the ML mechanism.