Diamond Anvil Cell Device Research Articles

In Situ Measurement Techniques Using Diamond Anvil Cell at High Pressure–Temperature Conditions: A Review

Diamond anvil cells have garnered significant attention in high‐pressure studies as a valuable tool for investigating material preparation, phase transition dynamics, and ultra‐high‐pressure physical chemistry. Its potential applications span fields such as materials science, condensed matter physics, chemistry, and geology. This study conducts a comprehensive review of the utilization of laser‐heated diamond anvil cell (LH‐DAC) devices in conjunction with in situ optical characterization techniques, such as X‐Ray and Raman scattering. Further, diverse in situ performance measurement methods encompassing electrical, thermal, magnetic, and acoustic analyses are examined. The development and role of the prevailing in situ measurement techniques have been described, along with the current progress in applied research for each technique. This study aims to facilitate the discovery of new structures and properties of materials under high pressure–temperature conditions.

Interlayer Coupling and Pressure Engineering in Bilayer MoS2

Controlling the interlayer coupling by tuning lattice parameters through pressure engineering is an important route for tailoring the optoelectronic properties of two-dimensional materials. In this work, we report a pressure-dependent study on the exciton transitions of bilayer MoS2 exfoliated on a diamond anvil surface. The applied hydrostatic pressure changes from ambient pressure up to 11.05 GPa using a diamond anvil cell device. Raman, photoluminescence, and reflectivity spectra at room temperature are analyzed to characterize the interlayer coupling of this bilayer system. With the increase of pressure, the indirect exciton emission disappears completely at about 5 GPa. Importantly, we clearly observed the interlayer exciton from the reflectivity spectra, which becomes invisible at a low pressure around 1.26 GPa. This indicates that the interlayer exciton is very sensitive to the hydrostatic pressure due to the oscillator strength transfer from the direct transition to the indirect one.

Effect of deformation of diamond anvil and sample in diamond anvil cell on the thermal conductivity measurement* *Project supported by the National Key Research and Development Program of China (Grant No. 2018YFA0702700) and the National Natural Science Foundation of China (Grant Nos. 11674404 and 11774126).

Studies show that the sample thickness is an important parameter in investigating the thermal transport properties of materials under high-temperature and high-pressure (HTHP) in the diamond anvil cell (DAC) device. However, it is an enormous challenge to measure the sample thickness accurately in the DAC under severe working conditions. In conventional methods, the influence of diamond anvil deformation on the measuring accuracy is ignored. For a high-temperature anvil, the mechanical state of the diamond anvil becomes complex and is different from that under the static condition. At high temperature, the deformation of anvil and sample would be aggravated. In the present study, the finite volume method is applied to simulate the heat transfer mechanism of stable heating DAC through coupling three radiative-conductive heat transfer mechanisms in a high-pressure environment. When the temperature field of the main components is known in DAC, the thermal stress field can be analyzed numerically by the finite element method. The obtained results show that the deformation of anvil will lead to the obvious radial gradient distribution of the sample thickness. If the top and bottom surfaces of the sample are approximated to be flat, it will be fatal to the study of the heat transport properties of the material. Therefore, we study the temperature distribution and thermal conductivity of the sample in the DAC by thermal-solid coupling method under high pressure and stable heating condition.

Evolution of hydrogen dissolution and superconductivity in Re-based solid solutions under pressure studied by ab initio calculations

The dissolving of hydrogen (H) into rhenium (Re) is non-negligible in high-pressure experiments involving dense hydrogen and hydrogenous materials, in which rhenium is often used as a gasket material in the high-pressure diamond-anvil cell devices. However, the evolution of hydrogen dissolution into Re and the pressure-induced effects of hydrogen coupling on the superconductivity of metal-based hydrides remain poorly understood experimentally, and theoretical investigations are currently lacking. The present work addresses these issues by applying ab initio calculations for systematically investigating the dissolution of H atoms in Re systems, as well as the electronic properties, lattice dynamics, and electron-phonon coupling (EPC) in the corresponding interstitial Re hydrides. A series of $\mathrm{Re}{\mathrm{H}}_{x}$ compounds with increasing $x$ in the range of 0 to 1 in increments of 0.125 are predicted to be stable at increasing pressures ranging from 1 to 50 GPa. It is found that H atoms generally play the role of impurities in the $\mathrm{Re}{\mathrm{H}}_{x}$ compounds except for $\mathrm{Re}{\mathrm{H}}_{0.5}$ and ReH, where H atoms are integrated into the crystal structure. Moreover, the atomic configuration of the Re host lattice is basically preserved with increasing $x$ and increasing pressure. Further analysis of the superconductive mechanism indicates that an increasing H concentration results in a decreased electronic density of states at the Fermi level and increasing phonon frequencies, which lead to a decrease of EPC \ensuremath{\lambda} and superconducting critical temperature. These findings quantitatively clarify the effects of hydrogen doping on superconductivity in metal-based hydrides, and thereby support the exploration of new types of superconductive hydrides.

Calibration of Manganin pressure gauge for diamond-anvil cells

Pressure calibration for most diamond-anvil cell (DAC) experiments is mainly based on the ruby scale, which is key to implementing this powerful tool for high-pressure study. However, the ruby scale can often hardly be used for programmably controlled DAC devices, especially the piezoelectric-driving cells, where a continuous pressure calibration is required. In this work, we present an effective pressure gauge for DACs made of Manganin metal based on the four-probe resistivity measurements. Pressure dependence of its resistivity is well established and shows excellent linear relations in the 0-30GPa pressure range with a slope of 23.4 (9) GPa for the first-cycle compression, in contrast to that of multiple-cycle compression and decompression having a nearly identical slope of 33.7 (4) GPa likely due to the strain effect. In addition, the such-established Manganin scale can be used for continuously monitoring the cell pressure of piezoelectric-driving DACs, and the reliability of this method is also verified by the fixed-point method with a Bi pressure standard. Realization of continuous pressure calibration for programmably controlled DACs would offer many opportunities for the study of dynamics, kinetics, and critical behaviors of pressure-induced phase transitions.

Pressure manipulation of exciton dynamics in few-layered MoS2

SynopsisTransition metal dichalcogenides have recently attracted great interest as an important class of two-dimensional semiconductors because of their distinctive electronic, optical and catalytic properties. Here we demonstrate the first experimental study on ultrafast excited state dynamics of few-layered molybdenum disulfide under high pressure by means of broadband transient absorption spectroscopy combined with diamond anvil cell devices.

Multimode scanning X-ray diffraction microscopy for diamond anvil cell experiments

We have designed and implemented a new experimental system for fast mapping of crystal structures and other structural features of materials under high pressure at the High Pressure Collaborative Access Team, Sector 16 of the Advanced Photon Source. The system utilizes scanning X-ray diffraction microscopy (SXDM) and is optimized for use with diamond anvil cell devices. In SXDM, the X-ray diffraction (XRD) is collected in a forward scattering geometry from points on a two-dimensional grid by fly-scanning the sample with respect to a micro-focused X-ray beam. The recording of XRD is made during the continuous motion of the sample using a fast (millisecond) X-ray area detector in synchrony with the sample positioners, resulting in a highly efficient data collection for SXDM. A new computer program, X-ray Diffractive Imaging (XDI), has been developed with the SXDM system. The XDI program provides a graphical interface for constructing and displaying the SXDM images in several modes: (1) phase mapping based on structural information, (2) pressure visualization based on the equation of state, (3) microstructural features mapping based on peak shape parameters, and (4) grain size and preferred-orientation based on peak shape parameters. The XDI is a standalone program and can be generally used for displaying SXDM images. Two examples of iron and zirconium samples under high pressure are presented to demonstrate the applications of SXDM.

Development of a high temperature diamond anvil cell for x ray absorption experiments under extreme conditions

X-ray absorption spectroscopy (XAS) is presently a powerful and established tool to investigate solid and liquid matter at high pressure and high temperature (HP-HT). HP-HT XAS experiments rely on high pressure technology whose continuous development has extended the achievable range up to 100 GPa and more. In high pressure devices, high temperature conditions are typically obtained by using internal and external resistive heaters or by laser heating. We have recently developed a novel design for an internally heated diamond anvil cell (DAC) allowing XAS measurements under controlled high temperature conditions (tested up to about 1300 K). The sample in the new device can be rapidly heated or cooled (seconds or less) so the cell is suitable for studying melting/crystallization dynamics when coupled with a time-resolved XAS setup (second and sub-second ranges). Here we describe the internally heated DAC device which has been realized and tested in experiments on pure selenium at the energy dispersive ODE beamline of Synchrotron SOLEIL. We also present results obtained in XAS experiments of elemental Se using a large volume Paris-Edinburgh press, as an example of the relevance of structural studies of matter under extreme conditions.

Anomalous Pressure Characteristics of Defects in Hexagonal Boron Nitride Flakes.

Research on hexagonal boron nitride (hBN) has been intensified recently due to the application of hBN as a promising system of single-photon emitters. To date, the single photon origin remains under debate even though many experiments and theoretical calculations have been performed. We have measured the pressure-dependent photoluminescence (PL) spectra of hBN flakes at low temperatures by using a diamond anvil cell device. The absolute values of the pressure coefficients of discrete PL emission lines are all below 15 meV/GPa, which is much lower than the pressure-induced 36 meV/GPa redshift rate of the hBN bandgap. These PL emission lines originate from atom-like localized defect levels confined within the bandgap of the hBN flakes. Interestingly, the experimental results of the pressure-dependent PL emission lines present three different types of pressure responses corresponding to a redshift (negative pressure coefficient), a blueshift (positive pressure coefficient), or even a sign change from negative to positive. Density functional theory calculations indicate the existence of competition between the intralayer and interlayer interaction contributions, which leads to the different pressure-dependent behaviors of the PL peak shift.

Development and application of piezoelectric driving diamond anvil cell device.

Diamond anvil cell (DAC) technique is widely employed for the high pressure measurements in the field of physics, chemistry, and material research. The new designs of DAC and new techniques for applying pressure have been gradually developed. This paper introduces a piezoelectric driving DAC device to achieve tunable high pressure at low temperature down to 20 K by in situ continuous pressure tuning. The tuning range is about 2-4 GPa depending on the applied electric voltage to piezoelectric lead zirconic titanate ceramic stack. The DAC device is well compatible with the cold chamber of a low temperature cryostat due to its small size and the convenient operation.

In situ tuning hydrostatic pressure at low temperature using electrically driven diamond anvil cell

Traditionally, a diamond anvil cell (DAC) operated at low temperature can be pressurized by using a helium-driven piston or remote control tightening mechanism. This approach of pressurizing DAC is not convenient for operating at low temperature. Here we develop a low-temperature pressurizing technique for in situ tuning pressure in DAC at 20 K by an electrically driven method. The improved DAC pressure apparatus is composed of traditional DAC device and a piezoelectric actuator (PZT). Here the PZT used in the experiment is the PSt 150/1010/40 supplied by the Piezomechanik. Both parts are assembled together in a red copper or stainless steel cylinder. The DAC part is thermally contacted with a low temperature holder for cooling the chamber of the DAC in the experiment. The wires of the PZT connect with the voltage source through the wiring terminals of the cryostat. As the DAC apparatus cools down, two electrodes of the PZT are connected together when a voltage difference between the electrodes is generated. When the temperature of the DAC chamber arrives at the presetting value, two electrodes of the PZT are connected with the voltage source for applying voltage to the PZT. In this paper, we find that the PZT stroke shows a linear increase with increasing voltage at 300 K, whereas it is approximately linear at 80 and 6 K. The maximum strokes are 40, 26 and 15 upm at 300, 80 and 6 K respectively when the applied voltage is 120 V. The experimental results show that the PZT-driven DAC apparatus can continuously generate pressure from 0.49 to 4.41 GPa at low temperature and applied voltage of 0-290 V, where at zero voltage an initial pressure of 0.49 GPa is generated by using driven screws of the DAC device at room temperature. The pressure in the DAC chamber is determined by the red shift of ruby florescence line. The calibrated chamber temperature in DAC is determined as a function of pressure (PZT voltage) by using the intensity ration (R2/R1) of ruby R2 and R1 fluorescence lines. We find that the chamber temperature only slightly increases with increasing pressure in a range of (19 1) K. The main difference between the present device and the other tuning DAC apparatus is that the force on the DAC can be conveniently applied by using PZT voltage. This guarantees a high pressure-tuned resolution in the experiment, e. g., we tune a single InAs quantum dot (QD) emission wavelength to match the cavity mode. Such a tuning technique is found to have applications in realizing a compact tunable single photon source or completing two-photon interference of Hong-Ou-Mandel experiments between the QD and nitrogen vacancy center in diamond or atom, respectively.

Conducting boron-doped single-crystal diamond films for high pressure research

Epitaxial boron-doped diamond films were grown by microwave plasma chemical vapor deposition for application as heating elements in high pressure diamond anvil cell devices. To a mixture of hydrogen, methane and oxygen, diborane concentrations of 240–1200 parts per million were added to prepare five diamond thin-film samples. Surface morphology has been observed to change depending on the amount of diborane added to the feed gas mixture. Single-crystal diamond film with a lowest room temperature resistivity of 18 mΩ cm was fabricated and temperature variation of resistivity was studied to a low temperature of 12 K. The observed minima in resistivity values with temperature for these samples have been attributed to a change in conduction mechanism from band conduction to hopping conduction. We also present a novel fabrication methodology for monocrystalline electrically conducting channels in diamond and present preliminary heating data with a boron-doped designer diamond anvil to 620 K at ambient pressure.

High pressure X-ray diffraction study of SrMnO3 perovskite

Using a diamond anvil cell device and synchrotron radiation, the in-situ high-pressure structure of SrMnO3 has been investigated. At pressure up to 28.6 GPa, no pressure-induced phase transition is observed. The lattice parameters as a function of pressure is reported, and the relationship of the axial compression coefficients is βa > βc. The isothermal bulk modulus K298=266(4) GPa is also obtained by fitting the pressure-volume data using the Murnaghan equation of state.

High pressure X-ray diffraction study of CaMnO3 perovskite

Using a diamond anvil cell device and synchrotron radiation, the in-situ high-pressure structure of CaMnO3 has been investigated. In the pressure up to 36.5 GPa, no pressure-induced phase transition is observed. The pressure dependence on the lattice parameters of CaMnO3 is reported, and the relationship of the axial compression coefficients is βa > βc > βb. The isothermal bulk modulus K298 = 224 (25) GPa is also obtained by fitting the pressure-volume data using the Murnaghan equation of state.

Structure and magnetic properties of stress-induced martensites in ferromagnetic shape memory alloy Mn2NiGa

In-situ high pressure X-ray diffraction experiments on Heusler-type ferromagnetic shape memory alloy Mn2NiGa under pressure up to 40 GPa have been carried out by using diamond anvil cell device with synchrotron radiation source， and magnetic measurements have also been performed on uninstalled samples by using vibration sample magnetometer. At ambient pressure Mn2NiGa has body centered cubic structure. Two phase transitions in Mn2NiGa were observed during high pressure experiments. The first at about 0.77 GPa is belong to martensitic transformation, and the second at about 20 GPa is isostructural transformation between two different martensites. Meanwhile, a lot of defects and distortion of lattice were generated in martensites due to pressurization. Consequently, coercive force of stress-induced martensites rises up to 204 kA/m and it is almost ten times larger than that of thermo-induced martensites. Pressure processes also make saturation magnetization of martensites decrease rapidly, which reveals the obvious defect effect.

Adhesion of nanostructured diamond film on a copper–beryllium alloy

Microwave plasma chemical vapor deposition (CVD) was used to coat nanostructured diamond onto a copper–beryllium alloy (∼1.7 wt% Be) commonly used as a nonmagnetic gasket material in diamond anvil cell devices. The coating is expected to be useful in preventing plastic flow of Cu–Be gaskets in diamond anvil cell devices, thus allowing for increased sample volume at high pressures and leading to improved sensitivity of magnetic measurements. The coatings were characterized by Raman spectroscopy, glancing-angle x-ray diffraction, microscopy (optical, scanning electron, and atomic force), Rockwell indentation, and nanoindentation. CVD diamond deposition on pure copper substrates has historically resulted in poor coating adhesion caused by the very large thermal expansion mismatch between the substrate and coating as well as the inability of copper to form a carbide phase at the interface. While an interfacial graphite layer formed on the pure copper substrates and resulted in complete film delamination, well-adhered 12.5 μm thick nanostructured diamond coatings were produced on the copper–beryllium (Cu–Be) alloy. The nanostructured diamond coatings on Cu–Be exhibit hardness of up to 84 GPa and can withstand strains from Rockwell indentation loads up to 150 kg without delamination.

Sound Velocity and Absorption Measurements under High Pressure Using Picosecond Ultrasonics in a Diamond Anvil Cell: Application to the Stability Study of AlPdMn

We report an innovative high pressure method combining the diamond anvil cell device with the technique of picosecond ultrasonics. Such an approach allows us to measure sound velocity and attenuation of solids and liquids under pressure of tens of GPa, overcoming all the drawbacks of traditional techniques. The power of this experimental technique is demonstrated in studies of lattice dynamics and relaxation processes in a metallic single grain of AlPdMn quasicrystal, and in rare gas solids neon and argon.

Finite-element modeling of stresses and strains in a diamond anvil cell device: case of a diamond-coated rhenium gasket

The stresses and strains in a diamond anvil cell device were investigated using a finite-element code NIKE2D for the case of an ultra-hard composite gasket material. The pressure distribution in a diamond-coated rhenium gasket was measured by the energy dispersive diffraction technique to 213 GPa and compared with the finite-element modeling results. We examine various models for the mechanical properties of diamond-coated rhenium gasket as well as for diamond failure for shear stresses exceeding 100 GPa. The elastic and plastic properties of gasket were varied such that a good agreement between the experimentally measured pressure distribution and the computational pressure profiles were obtained. As a result, we obtained the effective Young’s modulus, Poisson’s ratio, yield stress for indented gasket, linear hardening modulus, and hardening parameter value for this layered ultra-hard composite gasket material. Future diamond design strategies for attainment of extreme high pressures using ultra-hard gasket materials are also discussed.

Analysis of anisotropic compression of uranium under high pressures: a computational and experimental overview

We have investigated anisotropic compression effects observed in uranium metal under high pressures by analyzing data obtained with different X-ray diffraction techniques as well as data on samples obtained with different pressure media. Our analysis shows that the observed anisotropic compression effects are independent of the pressure transmitting medium or the experimental technique employed for studying uranium metal under high pressures. This suggests that the observed anisotropic compression effects are not related to non-hydrostatic stresses in the diamond anvil cell devices. First principle calculations using LMT-Art largely reproduce the experimentally measured axial ratios of the orthorhombic unit cell thereby confirming anisotropic effects in this f-band metal under compression.

Optical defect centers and surface morphology of isotopically enriched diamond layers in designer diamond anvils

We have studied optical defect centers and surface morphology of isotopically enriched layers grown on diamond anvils by microwave plasma chemical vapor deposition for applications as designer diamond anvils in high-pressure diamond anvil cell devices. Various mixtures of methane isotopes were used to grow homoepitaxial diamond with C13 molar fractions of 0.01, 0.41, 0.83, and 0.99 as determined from Raman spectroscopy. Defect centers were studied at temperatures between 80 and 320K using micro-photoluminescence (PL) spectroscopy with an argon ion and krypton laser excitation source. The defect spectra were dominated by zero phonon lines (ZPL) from nitrogen-related defect centers at nominal energies of 1.945eV (640nm defect) and 2.156eV (575nm defect), especially for the non-(100) surfaces. Polished (100) surfaces fluoresced weakly. ZPL’s at 1.77 and 1.68eV are observed, but not for all isotopically mixed samples. The 1.77eV ZPL appears to be associated from the original diamonds, while the 1.68eV ZPL is known to originate with silicon-based defects. Atomic force microscopy of as-grown isotopically enriched layers show rough growth steps in areas with surface roughness of hundred nanometers and smooth areas with surface roughness of few nanometers. Our studies indicate that (100) polished surfaces of isotopically enriched designer diamonds with low concentration of nitrogen defect centers can be fabricated for a variety of applications in high pressure research.