Conventional Diamond Anvil Cells Research Articles

Improving equations of state calibrations in the toroidal DAC—The case study of molybdenum

We report an updated isothermal equation of state (EoS) of molybdenum (Mo) obtained by compression in beveled and toroidal diamond-anvil cells (DACs). For an improved compression environment, we developed a copper (Cu) pressure-transmitting medium (PTM) for the toroidal diamond-anvil cell samples, as it is a soft metal compared to Mo with a well calibrated EoS. A Ne PTM was used for the conventional beveled DAC samples. The unit-cell volumes of Mo were measured to 336(1) GPa in the Cu PTM and 231.2(6) GPa in the Ne PTM at room temperature. We additionally calculated elastic stiffness and compliance constants and evaluated the uniaxial stress of Mo and Cu with pressure. A new EoS for Mo is presented from data collected in all sample environments and compared to our theoretical predictions as well as previous compression studies of Mo. The (200) lattice plane of Mo produced the lowest volumes across the pressure range of this study for all compression environments, suggesting that it is less affected by nonhydrostatic stresses in the DAC compared to the other observed diffraction planes. The presented Mo EoS is compatible with extrapolations of EoS fits of Mo in helium (He) within ∼1% at 330 GPa. Results from this work demonstrate that compressing a sample in a softer metal in the toroidal DAC can improve the compression environment and result in measured sample volumes comparable to those collected in noble-gas media at multi-megabar conditions.

Viscosity of Earth’s inner core constrained by Fe–Ni interdiffusion in Fe–Si alloy in an internal-resistive-heated diamond anvil cell

Abstract Diffusivity in iron (Fe) alloys at high pressures and temperatures imposes constraints on the transport properties of the inner core, such as viscosity. Because silicon (Si) is among the most likely candidates for light elements in the inner core, the presence of Si must be considered when studying diffusivity in the Earth’s inner core. In this study, we conducted diffusion experiments under pressures up to about 50 GPa using an internal-resistive-heated diamond-anvil cell (DAC) that ensures stable and homogeneous heating compared with a conventional laser-heated DAC and thus allows us to conduct more reliable diffusion experiments under high pressure. We determined the coefficients of Fe–nickel (Ni) interdiffusion in the Fe–Si 2 wt% alloy. The obtained diffusion coefficients follow a homologous temperature relationship derived from previous studies without considering Si. This indicates that the effect of Si on Fe–Ni interdiffusion is not significant. The upper limit of the viscosity of the inner core inferred from our results is low, indicating that the Lorentz force is a plausible mechanism to deform the inner core.

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.

Electrical transport measurements for superconducting sulfur hydrides using boron-doped diamond electrodes on beveled diamond anvil

A diamond anvil cell (DAC) has become an effective tool for investigating physical phenomena that occur at extremely high pressure, such as high-transition temperature superconductivity. Electrical transport measurements, which are used to characterize one of the most important properties of superconducting materials, are difficult to perform using conventional DACs. The available sample space in conventional DACs is very small and there is an added risk of electrode deformation under extreme operating conditions. To overcome these limitations, we herein report the fabrication of a boron-doped diamond microelectrode and undoped diamond insulation on a beveled culet surface of a diamond anvil. Using the newly developed DAC, we have performed in-situ electrical transport measurements on sulfur hydride H2S, which is a well-known precursor of the pressure-induced, high-transition temperature superconducting sulfur hydride, H3S. These measurements conducted under high pressures up to 192 GPa, indicated the presence of a multi-step superconducting transition, which we have attributed to elemental sulfur and possibly HS2.

Review: high pressure generation techniques beyond the limit of conventional diamond anvils

ABSTRACTCurrent anvil designs and problems associated with various efforts to generate static high pressures beyond the limit of conventional diamond anvil cells (DACs) (∼400 GPa) are reviewed. Pressures of up to 1 TPa have been reported by one research group using the double-stage DAC (ds-DAC) technique, but no other research group has successfully reproduced this high pressure result. Some research groups have used toroidal anvils, achieving pressures of >400 GPa. We have conducted numerous ds-DAC experiments and investigated the problems associated with such experiments. They include problems associated with various pressure scales in the multi-megabar region, difficulties in obtaining reliable X-ray diffraction patterns from micron-sized samples, and physical property measurements of tiny materials that may be harder than diamond. Each of these problems is discussed, following the summary of various experiments.

Toroidal diamond anvil cell for detailed measurements under extreme static pressures

Over the past 60 years, the diamond anvil cell (DAC) has been developed into a widespread high static pressure device. The adaptation of laboratory and synchrotron analytical techniques to DAC enables a detailed exploration in the 100 GPa range. The strain of the anvils under high load explains the 400 GPa limit of the conventional DAC. Here we show a toroidal shape for a diamond anvil tip that enables to extend the DAC use toward the terapascal pressure range. The toroidal-DAC keeps the assets for a complete, reproducible, and accurate characterization of materials, from solids to gases. Raman signal from the diamond anvil or X-ray signal from the rhenium gasket allow measurement of pressure. Here, the equations of state of gold, aluminum, and argon are measured with X-ray diffraction. The data are compared with recent measurements under similar conditions by two other approaches, the double-stage DAC and the dynamic ramp compression.

Diamond anvil cell behavior up to 4 Mbar

The diamond anvil cell (DAC) is considered one of the dominant devices to generate ultrahigh static pressure. The development of the DAC technique has enabled researchers to explore rich high-pressure science in the multimegabar pressure range. Here, we investigated the behavior of the DAC up to 400 GPa, which is the accepted pressure limit of a conventional DAC. By using a submicrometer synchrotron X-ray beam, double cuppings of the beveled diamond anvils were observed experimentally. Details of pressure loading, distribution, gasket-thickness variation, and diamond anvil deformation were studied to understand the generation of ultrahigh pressures, which may improve the conventional DAC techniques.

Phase transitions in the system CaCO3 at high P and T determined by in situ vibrational spectroscopy in diamond anvil cells and first-principles simulations

The stability of the high-pressure CaCO3 calcite (cc)-related polymorphs was studied in experiments that were performed in conventional diamond anvil cells (DAC) at room temperature as a function of pressure up to 30 GPa as well as in internally heated diamond anvil cells (DAC-HT) at pressures and temperatures up to 20 GPa and 800 K. To probe structural changes, we used Raman and FTIR spectroscopy. For the latter, we applied conventional and synchrotron mid-infrared as well as synchrotron far-infrared radiation. Within the cc-III stability field (2.2–15 GPa at room temperature, e.g., Catalli and Williams in Phys Chem Miner 32(5–6):412–417, 2005), we observed in the Raman spectra consistently three different spectral patterns: Two patterns at pressures below and above 3.3 GPa were already described in Pippinger et al. (Phys Chem Miner 42(1):29–43, 2015) and assigned to the phase transition of cc-IIIb to cc-III at 3.3 GPa. In addition, we observed a clear change between 5 and 6 GPa that is independent of the starting material and the pressure path and time path of the experiments. This apparent change in the spectral pattern is only visible in the low-frequency range of the Raman spectra—not in the infrared spectra. Complementary electronic structure calculations confirm the existence of three distinct stability regions of cc-III-type phases at pressures up to about 15 GPa. By combining experimental and simulation data, we interpret the transition at 5–6 GPa as a re-appearance of the cc-IIIb phase. In all types of experiments, we confirmed the transition from cc-IIIb to cc-VI at about 15 GPa at room temperature. We found that temperature stabilizes cc-VI to lower pressure. The reaction cc-IIIb to cc-VI has a negative slope of −7.0 × 10−3 GPa K−1. Finally, we discuss the possibility of the dense cc-VI phase being more stable than aragonite at certain pressure and temperature conditions relevant to the Earth’s mantle.

Pressure, stress, and strain distribution in the double-stage diamond anvil cell

Double stage diamond anvil cells (DACs) of two designs have been assembled and tested. We used a standard symmetric DAC with flat or beveled culets as a primary stage and CVD microanvils machined by a focused ion beam as a second. We evaluated pressure, stress, and strain distributions in gold and a mixture of gold and iron as well as in secondary anvils using synchrotron x-ray diffraction with a micro-focused beam. A maximum pressure of 240 GPa was reached independent of the first stage anvil culet size. We found that the stress field generated by the second stage anvils is typical of conventional DAC experiments. The maximum pressures reached are limited by strains developing in the secondary anvil and by cupping of the first stage diamond anvil in the presented experimental designs. Also, our experiments show that pressures of several megabars may be reached without sacrificing the first stage diamond anvils.

Implementation of micro-ball nanodiamond anvils for high-pressure studies above 6 Mbar

Since invention of the diamond anvil cell technique in the late 1950s for studying materials at extreme conditions, the maximum static pressure generated so far at room temperature was reported to be about 400 GPa. Here we show that use of micro-semi-balls made of nanodiamond as second-stage anvils in conventional diamond anvil cells drastically extends the achievable pressure range in static compression experiments to above 600 GPa. Micro-anvils (10–50 μm in diameter) of superhard nanodiamond (with a grain size below ∼50 nm) were synthesized in a large volume press using a newly developed technique. In our pilot experiments on rhenium and gold we have studied the equation of state of rhenium at pressures up to 640 GPa and demonstrated the feasibility and crucial necessity of the in situ ultra high-pressure measurements for accurate determination of material properties at extreme conditions.

Dynamic diamond anvil cell (dDAC): A novel device for studying the dynamic-pressure properties of materials

We have developed a unique device, a dynamic diamond anvil cell (dDAC), which repetitively applies a time-dependent load/pressure profile to a sample. This capability allows studies of the kinetics of phase transitions and metastable phases at compression (strain) rates of up to 500 GPa/s (approximately 0.16 s(-1) for a metal). Our approach adapts electromechanical piezoelectric actuators to a conventional diamond anvil cell design, which enables precise specification and control of a time-dependent applied load/pressure. Existing DAC instrumentation and experimental techniques are easily adapted to the dDAC to measure the properties of a sample under the varying load/pressure conditions. This capability addresses the sparsely studied regime of dynamic phenomena between static research (diamond anvil cells and large volume presses) and dynamic shock-driven experiments (gas guns, explosive, and laser shock). We present an overview of a variety of experimental measurements that can be made with this device.

The c-DAC: A novel cubic diamond anvil cell with large sample volume/area and multidirectional optics

We report on a new high-pressure instrument that has important advantages over the conventional diamond anvil cell (DAC). Our design is basically a miniaturized cubic press, i.e., six trimmed pyramidal diamond anvils compressing a central sample in three orthogonal directions rather than uniaxially. This geometry has three advantages over the DAC: first, it provides a high quality of uniform pressure due to the six-sided load, with improved support of the diamonds; second, samples can have volumes several hundred times larger and areas an order of magnitude greater; and third, it allows multidirectional optical access to the sample, with important advantages for spectroscopic studies such as Raman and Brillouin scatterings. The c-DAC is about the size and weight of a DAC and its pressure can be varied remotely, for example, while in a cryostat. The highest pressure achieved in our ongoing research is currently 22.4GPa, but limitations were not fundamental and we believe that pressures in the megabar range can be achieved.

Large volume high-pressure cell with supported moissanite anvils

The recently developed moissanite anvil cell (MAC) has become a useful device for achieving both high-pressure and large sample volume in an anvil cell. We describe two improvements in the basic design of the MAC. First, the loading environment has been optimized by centering the load. Second, a variety of supported systems have been examined to provide anvil stability at high loads with large anvils. Sample volumes that are nearly three orders magnitude greater than allowed by conventional diamond anvil cells can be pressurized and characterized at ∼50 GPa.

The double-diamond anvil cell, the poor-man’s megabar pressure cell

We present a new configuration for diamond anvils used in high pressure research. We show how to make a gasketed diamond indentor cell (DIC) in a conventional diamond anvil cell (DAC). Moreover, diamond anvils an order of magnitude smaller than those currently used can easily be mounted, with minor modification. These configurations are called DIC-DACs and double DACs (D-DACs). D-DACs have been tested to a megabar and appear to have the same range as a conventional DAC. D-DACs can lower the cost of diamonds for high pressure research by more than an order of magnitude.