Diamond Anvil Research Articles

Quantifying uncertainty in analysis of shockless dynamic compression experiments on platinum. I. Inverse Lagrangian analysis

Absolute measurements of solid-material compressibility by magnetically driven shockless dynamic compression experiments to multi-megabar pressures have the potential to greatly improve the accuracy and precision of pressure calibration standards for use in diamond anvil cell experiments. To this end, we apply characteristics-based inverse Lagrangian analysis (ILA) to 11 sets of ramp-compression data on pure platinum (Pt) metal and then reduce the resulting weighted-mean stress–strain curve to the principal isentrope and room-temperature isotherm using simple models for yield stress and Grüneisen parameter. We introduce several improvements to methods for ILA and quasi-isentrope reduction, the latter including calculation of corrections in wave speed instead of stress and pressure to render results largely independent of initial yield stress while enforcing thermodynamic consistency near zero pressure. More importantly, we quantify in detail the propagation of experimental uncertainty through ILA and model uncertainty through quasi-isentrope reduction, considering all potential sources of error except the electrode and window material models used in ILA. Compared to previous approaches, we find larger uncertainty in longitudinal stress. Monte Carlo analysis demonstrates that uncertainty in the yield-stress model constitutes by far the largest contribution to uncertainty in quasi-isentrope reduction corrections. We present a new room-temperature isotherm for Pt up to 444 GPa, with 1-sigma uncertainty at that pressure of just under ±1.2%; the latter is about a factor of three smaller than uncertainty previously reported for multi-megabar ramp-compression experiments on Pt. The result is well represented by a Vinet-form compression curve with (isothermal) bulk modulus K0=270.3±3.8 GPa, pressure derivative K0′=5.66±0.10, and correlation coefficient RK0,K0′=−0.843.

High-pressure single-crystal elasticity of corundum: Implication for multiple seismic structure of 660-km discontinuity

The complex multi-discontinuity structure at 660‐800 km depth is likely attributable to lateral mantle composition heterogeneities, which are closely related to the mid-ocean ridge basalts (MORB). To decipher the impact of varying composition on the seismic properties of MORB, detailed knowledge of the elasticity of candidate minerals is thus important. Here we employed Brillouin scattering coupled with diamond anvil cells to determine the single-crystal elasticity of corundum up to 14 GPa and 300 K. Using third-order finite strain equation of state, we calculate the pressure derivatives of adiabatic bulk modulus and shear modulus of corundum, which yields KS0’ = 3.8(1), G0’ = 1.8(1) with KS0 = 256(1) GPa and G0 = 163(1) GPa and ρ0 = 3.987(1) g/cm3. Combined with previous high-temperature data, the velocity and anisotropy of corundum have been calculated at 300 K or along normal geotherm. Our results are applied to model the density and velocity profiles of normal and alkali-depleted MORB. Our modeling demonstrates that varying the alkali content and temperature of MORB can significantly impact the discontinuity depth and velocity jump at 660–800 km depth. For normal MORB, reducing the temperature by 300 K from normal mantle geotherm results in a shift of the velocity jump from 670–710 to 650–710 km depth but hardly affects the magnitude of the velocity jump (5.8–6.8(3)% for VP and 10.0–10.8(5)% for VS). By contrast, in alkali-depleted MORB, the discontinuity will occur at a greater depth from 705–730 to 720–745 km depending on temperature with a VP jump of 3.8–4.6(2)% and VS jump of 6.3–7.4(4)%.

Synthesis of Ultra-Incompressible and Recoverable Carbon Nitrides Featuring CN4 Tetrahedra.

Carbon nitrides featuring three-dimensional frameworks of CN4 tetrahedra are one of the great aspirations of materials science, expected to have a hardness greater than or comparable to diamond. After more than three decades of efforts to synthesize them, no unambiguous evidence of their existence has been delivered. Here, the high-pressure high-temperature synthesis of three carbon-nitrogen compounds, tI14-C3 N4 , hP126-C3 N4 , and tI24-CN2 , in laser-heated diamond anvil cells, is reported. Their structures are solved and refined using synchrotron single-crystal X-ray diffraction. Physical properties investigations show that these strongly covalently bonded materials, ultra-incompressible and superhard, also possess high energy density, piezoelectric, and photoluminescence properties. The novel carbon nitrides are unique among high-pressure materials, as being produced above 100GPa they are recoverable in air at ambient conditions.

Combined First-Principles and Experimental Investigation into the Reactivity of Codeposited Chromium-Carbon under Pressure.

High-pressure synthesis in the diamond anvil cell suffers from the lack of a general approach for the control of precursor stoichiometry and homogeneity. Here, we present results from a new method we have developed that uses magnetron cosputtering to prepare stoichiometrically precise and atomically mixed amorphous films of Cr:C. Laser-heated diamond anvil cell experiments carried out on a flake of this sample at pressures between 13.5 and 24.3 GPa lead to the observation of Cr3C (Pnma) over the entire pressure range-in good agreement with our in-house theoretical predictions-but also reveal two other metastable phases that were not expected: a novel monoclinic chromium carbide phase and the NaCl-type CrC (Fm3̅m) phase. The unexpected stability of CrC is investigated by using first-principles methods, revealing a large stabilizing effect tied to substoichiometry at the carbon site. These results offer an important case study into the current limitations of crystal structure prediction methods with regard to phase complexity and bolster the growing need for advanced theoretical approaches that can more completely survey experimentally unexplored phase space.

Pressure-Induced Modulation of Tin Selenide Properties: A Review.

Tin selenide (SnSe) holds great potential for abundant future applications, due to its exceptional properties and distinctive layered structure, which can be modified using a variety of techniques. One of the many tuning techniques is pressure manipulating using the diamond anvil cell (DAC), which is a very efficient in situ and reversible approach for modulating the structure and physical properties of SnSe. We briefly summarize the advantages and challenges of experimental study using DAC in this review, then introduce the recent progress and achievements of the pressure-induced structure and performance of SnSe, especially including the influence of pressure on its crystal structure and optical, electronic, and thermoelectric properties. The overall goal of the review is to better understand the mechanics underlying pressure-induced phase transitions and to offer suggestions for properly designing a structural pattern to achieve or enhanced novel properties.

Sample heating above 1400 K in a diamond anvil cell

In high-pressure experimental methods, sample heating in the pressure chamber of a diamond anvil cell is an important topic, and numerous efforts have been made to improve and develop new technologies. In this paper, we propose a new type of internal resistance heating technique, the composite heating gasket, prepared by integrating an annular heater into the sample chamber for direct heating of the sample. As the effective heating area covers the entire pressure chamber wall, a relatively quasi-uniform temperature field is formed within the sample chamber. At the same time, the integration design reduces the risk of diamond oxidation and enables direct measurement of the spectroscopic properties of samples at high temperatures. The preparation of the composite heating gasket is simple and repeatable, and its heating performance is stable at temperatures above 1400 K. When the sample diameter is 210 μm and no thermal insulation is used, the diameter of the temperature zone in which the temperature difference is less than 10 and 20 K exceeds 120 and 170 μm, respectively. The composite heating gasket represents a significant advancement in providing a uniform temperature field for in situ measurements with diamond anvil cells at high pressure and temperature.

Optical full-field strain measurement within a diamond anvil cell.

Digital image correlation computations are run on optical images of iron samples within a diamond anvil cell to obtain in-plane strain components at the surface of the sample up to 17GPa. The α-Fe → ε-Fe transition onset pressure and phase coexistence pressure domain can be identified from the evolution of the surface average of strain components. Strain fields exhibit localizations for both direct and reverse transition; they coincide with the approximate boundary locations of reversion variants inside the microstructure of a single crystal sample. The so-called DICDAC (Digital Image Correlation within a Diamond Anvil Cell) setup is then a suitable tool for the investigation of phase transformations strains under pressure. In addition, specific volumes that are deduced from strain out of the transition pressure domains agree within ΔV/V = 0.4% with the equation of state data from the literature.

Externally Heated Diamond ANvil Cell Experimentation (EH-DANCE) for studying materials and processes under extreme conditions.

Externally heated diamond anvil cells provide a stable and uniform thermal environment, making them a versatile device to simultaneously generatehigh-pressure and high-temperature conditions in various fields of research, such as condensed matter physics, materials science, chemistry, and geosciences. The present study features the Externally Heated Diamond ANvil Cell Experimentation (EH-DANCE) system, a versatile configuration consisting of a diamond anvil cell with a customized microheater for stable resistive heating, bidirectional pressure control facilitated by compression and decompression membranes, and a water-cooled enclosure suitable for vacuum and controlled atmospheres. This integrated system excels with its precise control of both pressure and temperature for mineral and materials science research under extreme conditions. We showcase the capabilities of the system through its successful application in the investigation of the melting temperature and thermal equation of state of high-pressure ice-VII at temperatures up to 1400K. The system was also used to measure the elastic properties of solid ice-VII and liquid H2O using Brillouin scattering and Raman spectra of carbonates using Raman spectroscopy, highlighting the potential of the EH-DANCE system in high-pressure research.

Metallic hydrogen: Study of metastability

Metallic hydrogen (MH) has been predicted to be metastable, a high temperature superconductor, and a powerful rocket propellant. If true, MH could have an enormous impact on society. We have produced MH in a diamond anvil cell and studied its metastability. At a temperature of 5 K, the load on the metallic hydrogen was stepwise reduced until the pressure was essentially zero. While turning the load or pressure down, the sample evidently transformed to the molecular phase and escaped; the hole in the gasket containing the MH closed. We were unable to determine this value of the metastability pressure. Metallic hydrogen was not observed to be metastable at zero pressure, with no uncertainty.

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.

Superconductivity discovered in niobium polyhydride at high pressures

Niobium polyhydride was synthesized at high pressure and high temperature conditions by using diamond anvil cell combined with in situ high pressure laser heating techniques. High pressure electric transport experiments demonstrate that superconducting transition occurs with critical temperature(Tc) 42 K at 187 GPa. The shift of Tc as function of external applied magnetic field is in consistent to the nature of superconductivity while the upper critical field at zero temperature μ0Hc2(0) is estimated to ∼16.8 T while the GL coherent length ∼57 Å is estimated. The structure investigation using synchrotron radiation implies that the observed superconductivity may come from Fm-3m phase of NbH3.

An in-situ experimental HP/HT study on bromine release from a natural basalt

We present the first in-situ partitioning data for bromine between a natural basaltic melt and a coexisting fluid. For this study hydrothermal diamond anvil cell experiments at pressures up to 1.7 GPa were conducted. We combined laser heating to melt the basalt glass with external heating to lower the temperature gradient in the cell and to initiate circulation for the aqueous fluid. Bromine concentrations were measured in-situ with X-ray fluorescence in the basaltic melts, glasses, and in the fluid. From the results we calculated partition coefficients of DBrfluid/melt = 1.19 to 3.92 in the range of 0.4 to 1 GPa for aqueous fluids. Experiments with neon as the surrounding fluid (DBrfluid/melt = 0.38 ± 0.01 at 1.1 GPa) suggest that Br-release from a basalt into volatiles that have no bonding affinity with Br is weak. This should be the case for dry intra-plate volcanic eruptions. From the experimentally gained partition coefficients and from global Br concentration values in melt inclusions of arc magmas, we calculated an annual global Br flux of 23.5–72.9 × 109 g/y.

Pressure-dependent deformation in brittle diamond

Distinguished from ductile metals, in brittle covalent materials like diamond, hydrostatic pressure is a prerequisite for triggering the plastic deformation. Consequently, the theoretical framework rooted in equilibrium lattice proves inadequate in describing the behavior of brittle covalent materials, making it essential to include extrinsic hydrostatic pressure effects. Here, we take diamond as a model and introduce hydrostatic pressure in the calculation of generalized stacking fault energies (GSFE). A deformation mechanism transition from perfect dislocation slipping on {200} plane to the partial dislocation slipping on {111} plane when the hydrostatic pressure exceeds 100 GPa is revealed by the pressure-coupled GSFE and further authenticated by nanocompression and diamond anvil cell experiments. Such pressure-dependent deformation mechanism is attributed to the different pressure sensitivities of lattice volume expansion during different slip systems operating. Our works provide insights into the activation of slip systems in diamond at the atomic scale and a route to study the plastic deformation behavior of brittle covalent materials.

Spectroscopic pressure investigation of a novel high energy system

AbstractThis work combines a novel multimodal spectroscopic technique, O‐PTIR and Raman spectroscopy, which allows for the simultaneous collection of infrared and Raman spectra, with traditional diamond anvil cell techniques to explore pressure induced phase transitions in a high energy material. Two phase transitions are revealed, with the first transition emerging below 0.23 GPa, to a higher order phase, followed by a broad transition to a lower order phase. Aside from the pressure studies, hyperspectral imaging was performed, confirming the homogeneous nature of the system.

Melting line and thermal equation of state of fcc-cobalt: A combined experimental and computational approach

The melting line of cobalt has been investigated both experimentally, using synchrotron X-ray diffraction coupled with laser-heated diamond anvil cells, and theoretically, using ab initio simulations. Over the investigated pressure and temperature range – between 30 and 100 GPa and from ambient temperature up to 4000 K – the hexagonal close-packed structure, stable at ambient conditions, is replaced at high temperature by the face-centered cubic structure, observed stable till melting. The melting temperatures obtained by the two methods are in remarkable agreement and the melting line can be well described by a Simon–Glatzel equation of the form Tm= 1768(K)(P(GPa)/35.62+1)0.64. Finally, from the obtained results it was possible to determine a thermal equation of state for the cubic face-centered phase of Co.

Development of 0.5 mm gauge size radial collimators for high-pressure neutron diffraction experiments at PLANET in J-PARC

Radial collimators with a 0.5 mm gauge size (GS) were specially designed for high-pressure neutron diffraction experiments. The performance and efficacy of these collimators, along with the 1.5 mm and 3.0 mm GS radial collimators, were investigated. The radial collimators with nominal GS of 0.75 mm, 1.5 mm, and 3.0 mm effectively exhibited GS of 0.50 mm, 1.07 mm, and 2.78 mm, respectively. The transmissions of all three radial collimators were deemed equivalent. The assessment using a Paris–Edinburgh (PE) press equipped with double-toroidal anvils and a diamond anvil cell (DAC) tailored for neutron diffraction revealed that the scattering intensity from the anvils was considerably minimized using the radial collimators and the sample-to-anvil signal ratio, as defined by the Bragg peak intensity ratio (IMgO220/IDiamond220), reached values of 0.5 and 2.0 for the PE press and DAC, respectively, when using the 0.5 mm GS radial collimators. These results indicate that the 0.5 mm GS radial collimators have been fabricated as intended and exhibit efficacy for the high-pressure-neutron diffraction experiments, specifically those exceeding 30 GPa, which cannot be reached with a PE press equipped with the standard double-toroidal anvils of a 1.5 mm cup diameter. Among those ever manufactured for neutron scattering experiments, the radial collimators display the smallest GS.

Study of the electrophysical and magnetic properties of a Dirac 3D semimetal Cd3As2 with nanogranules of MnAs

We report on the main results of studying the electrical and magnetoresistance (MR) of a composite material consisting of 70 % mol. Dirac semi-metal Cd3As2 and 30 % mol. ferromagnet MnAs at pressures up to 50 GPa in a diamond anvil cell with a «rounded cone-flat» type anvils, as well as magnetization at hydrostatic pressures up to 6 GPa in a toroid-shaped high-pressure cell, both at room temperature and in the temperature range of 180 – 350 K at atmospheric pressure. A mixture of methanol and ethanol in a ratio of 4:1 was used as a pressure transmitting medium. Elemental analysis of Cd3As2 + 30 % mol MnAs composites showed that much of the volume is occupied by the Cd3As2 phase. The proportion of MnAs phase inclusions is less than 5 %. The feature of Cd3As2 + MnAs is the presence of a significant region of non-mixing of the Cd3As2 and MnAs phase melts. A negative MR was revealed with increasing pressure in the entire studied baric zone. The maximum negative MR is observed in the baric zone of 22 – 26 GPa. Further increase in the pressure up to the maximum level result in the appearance of several extrema on the ΔR/R0(P) curve, with negative MR not exceeding 4 %. Upon pressure release from 50 GPa, the baric dependence of ΔR/R0(P) is characterized by an inversion of the MR sign: at pressures around 40 GPa, a negative MR is replaced by a positive MR, and at around 20 GPa, the maximum value of positive MR of ~5.3 % is observed. Signs of the instability of the monoclinic structure of Cd3As2 resulted from its partial decomposition upon decompression were revealed. The results obtained can be used in spintronics when using appropriate composite materials.

Partitioning of silicon and sulfur between solid and liquid iron under core pressures: Constraints on Earth's core composition

Not only the Earth's outer core but also the inner core contains light elements, which causes reductions in density and velocity with respect to those of pure solid iron. Silicon, sulfur, and possibly hydrogen are believed to be important inner core light elements, because their partition coefficients between solid Fe and liquid, D (solid/liquid), are high (>0.7) under inner core pressures unlike other possible light elements such as oxygen and carbon. Recent experiments demonstrated that DSi is remarkably enhanced with increasing sulfur concentration in liquid at 15–21 GPa. Here we conducted solid/liquid partitioning experiments on the Fe-Si-S(-C) system up to the Earth's core pressure range of 189 GPa in a laser-heated diamond-anvil cell (DAC) and examined the effect of silicon-sulfur interaction on both DSi and DS. The results show that DS significantly diminishes with increasing the silicon content in liquid, while DSi increases with higher sulfur concentration. Based on these partitioning data, we explored the pairs of possible liquid outer core and solid inner core compositions in the Fe-Si-S±H±O system, which account for their respective seismological observations of the density and velocities. For the temperature at the inner core boundary of 5400 K, we obtained Fe + Ni + 2.7–3.0 wt% Si + 1.7 wt% S (fixed) + 0.32–0.59 wt% H + 0.05–2.5 wt% O for the outer core and Fe + Ni + 2.5–2.8 wt% Si + 0.69–0.70 wt% S + 0.23–0.43 wt% H for the inner core.

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.

Robustness of Trion State in Gated Monolayer MoSe2 under Pressure.

Quasiparticles consisting of correlated electron(s) and hole(s), such as excitons and trions, play important roles in the optical phenomena of van der Waals semiconductors and serve as unique platforms for studies of many-body physics. Herein, we report a gate-tunable exciton-to-trion transition in pressurized monolayer MoSe2, in which the electronic band structures are modulated continuously within a diamond anvil cell. The emission energies of both the exciton and trion undergo large blueshifts over 90 meV with increasing pressure. Surprisingly, the trion binding energy remains constant at 30 meV, regardless of the applied pressure. Combining ab initio density functional theory calculations and quantum Monte Carlo simulations, we find that the remarkable robustness of the trion binding energy originates from the spatially diffused nature of the trion wave function and the weak correlation between its constituent electron-hole pairs. Our findings shed light on the optical properties of correlated excitonic quasiparticles in low-dimensional materials.