Anvil Apparatus Research Articles

Pressure-Induced Superconductivity In Polycrystalline La3Ni2O7−δ

We synthesized polycrystalline La3Ni2O7−δ (δ≈0.07) samples by using the sol-gel method without postannealing under high oxygen pressure, and then measured temperature-dependent resistivity under various hydrostatic pressures up to 18 GPa by using the cubic anvil and two-stage multianvil apparatus. We find that the density-wave-like anomaly in resistivity is progressively suppressed with increasing pressure and the resistivity drop corresponding to the onset of superconductivity emerges at pressure as low as ∼6 GPa. Zero resistivity is achieved at 9 GPa below Tczero≈6.6 K, which increases quickly with pressure to 41 K at 18 GPa. However, the diamagnetic response was not detected in the ac magnetic susceptibility measurements up to 15 GPa, indicating a filamentary nature of the observed superconductivity in the studied pressure range. The constructed T−P phase diagram reveals an intimate relationship between superconductivity, density-wave-like order, and the strange-metal-like behaviors. The observation of zero-resistance state in the polycrystalline La3Ni2O7−δ samples under high pressures not only corroborates the recent report of superconductivity in the pressurized La3Ni2O7 crystals but also facilitates further studies on this emerging family of nickelate high-Tc superconductors. Published by the American Physical Society 2024

Equation-of-state-constrained pressure dependence of x-ray elastic constants of gold for stress components calculation in a high-pressure anvil apparatus

In the resolution of the large divergence between pressure calculated by way of axial stress components from elastic constants and pressure determined by an equation of state, a 2nd order pressure dependency of elastic constants is introduced. Incorporating results from the equation of state and ultrasonic measurements in the literature, we determined the pressure dependency of x-ray elastic constants of gold and established functions for the calculation of macro-stress components from its macro-strain counterparts. The precision of stress components through these functions is estimated to be at 1% level. The determination of stress components, including crucial shear components, through analysis of an x-ray diffraction image, is demonstrated.

Macro strain-stress determination in a high pressure rotational anvil apparatus

With the increasing development of techniques that utilize high-pressure shear in multiple fields, constructing a proper interpretation of strain and stress in rotational anvil apparatuses is becoming more and more urgent. A macro strain analysis in a rotational anvil apparatus that generates high pressure and shear was performed based on a polycrystal strain spatial distribution. Based on the strain, macro stress components were retrieved. Three analytical methods suitable for various application purposes are presented that can be used to conduct stress/strain analysis of a sample under pressure and shear: a sample center fitting method that obtains macro strain components from the refinement of d-spacing azimuth angle distribution, a six-point graphical method that calculates macro strain components from graphical strain distribution, and a four-point graphical method that determines the components directly from a diffraction image. This study also discusses and verifies the validity of and comparison between the methods through experimental data. The present work is expected to provide a foundation for further experimental studies of shear at pressures and expand the field of high-pressure sciences.

Disappearance and Survival of Superconductivity in FeSe under High Pressure

Superconductivity in FeSe was investigated under high pressure through the measurements of DC magnetization by using a diamond anvil cell. We successfully observed that the disappearance of the superconductivity as a results of the appearance of the non-superconducting ortho I\hspace{-1pt}I phase above $\sim$7 GPa ($\sim$5 GPa), when Ar (glycerin) is used as the pressure transmitting media. Contrary to this, it has been found that the superconductivity even survives under pressure above 7 GPa, when the thickness ($t$) of a platelet-single crystal specimen is reduced. The survival of the superconductivity above 7 GPa is consistent with a previous observation under hydrostatic pressure by using a cubic anvil apparatus, suggesting that the hydrostaticity of the pressure is improved by reducing $t$. It is also inferred that the appearance of the ortho I\hspace{-1pt}I phase is due to uniaxial stress along the [001] direction.

Thermal properties of harzburgite and dunite at 0.8–3 ​GPa and 300–823 ​K and implications for the thermal evolution of Tibet

Thermal diffusivity (D) and thermal conductivity (κ) of harzburgite and dunite from Luobusha ophiolite were simultaneously measured up to 3 ​GPa and 823 ​K using the transient plane-source method in a multi anvil apparatus. The results show that the values of D and κ of both samples systematically decrease with increasing temperature and increase with increasing pressure. By combination of the thermal physical data of rocks and minerals and geophysical constraints, we performed numerical simulation on the thermal evolution of Tibet vary over depth, distance and geologic ages. The present results provide new constraints on occurrence of partial melting and its geophysical significance beneath Tibetan crust.

Preservation conditions of CLIPPIR diamonds in the earth’s mantle in a heterogeneous metal–sulphide–silicate medium (experimental modeling)

The genesis of CLIPPIR diamonds (Cullinan–like, large, inclusion–poor, pure, irregular, and resorbed) have attracted much interest due to their possible crystallization from metal melt in deep horizons of the earth’s mantle. These diamonds usually show a pronounced resorption and irregular morphology. The present paper reports new experimental data on the dissolution of diamond crystals at high P–T parameters in Fe–S melt containing large amounts of silicate components (5–20 wt%). The experiments were performed using a split–sphere multi–anvil apparatus (BARS) at a pressure of 4 GPa and a temperature of 1450 °C. The samples consisted of natural diamond crystals placed in mixtures of Fe, S, and kimberlite. Wide variations in dissolution rates of diamond crystals were obtained. The absence of diamond dissolution in a heterogeneous medium indicates that the amount of solid silicate phases present in metal melt plays a role in the preservation of diamonds. This study demonstrated how diamonds can be stored in natural environments due to the heterogeneity of the medium composition which could insulate diamonds from the metal–sulphide melt. The obtained results improve our understanding of processes that lead to preservation of CLIPPIR diamonds in the deep mantle.

Conical support for double-stage diamond anvil apparatus

ABSTRACTBoth micro-paired and conical support type double-stage diamond anvil cells (ds-DAC) were tested using a newly synthesized ultra-fine nano-polycrystalline diamond (NPD). Well-focused X-ray sub-micron beam and the conically supported 2nd stage anvils (micro-anvils) with 10 μm culet enable us to obtain good quality X-ray diffraction peaks from the sample at around 400 GPa. The relationship between confining pressure and sample pressure depends heavily on the initial height (thickness) of micro-anvils, the difference of a few micrometers leads to a quite different compression path. The conical support type is a solution to retain both enough thickness and strength of micro-anvils at higher confining pressure conditions. All conical support ds-DAC experiments terminated by the failure of the 1st stage anvil instead of 2nd one. The combination of ultra-fine NPD 2nd stage anvil and NPD 1st stage anvil opens a new frontier for measurement of the X-ray absorption spectrum above 300 GPa.

The effect of fluorine on the stability of wadsleyite: Implications for the nature and depths of the transition zone in the Earth's mantle

The Earth's mantle contains significant amounts of volatile elements, such as hydrogen (H), carbon (C) and the halogens fluorine (F), chlorine (Cl) and bromine (Br) and iodine (I). There is a wealth of knowledge about the global cycling of H and C, but there is only scant data on the concentrations of halogens in different Earth reservoirs and on the behavior of halogens during recycling in subduction zones. Here we focus on the storage potential of F in deeper parts of the Earth's mantle. The transition zone is a region in the Earth's mantle (410–660 km) known for its high water storage capacity, as the high pressure polymorphs of olivine, wadsleyite and ringwoodite are known to be able to incorporate several per-cent of water. In order to assess potential fractionation between water and F in the transition zone of the Earth's mantle, we set out to investigate the storage capacity of the halogen F in wadsleyite and olivine at transition zone conditions. Experiments were performed in a simplified mantle composition at temperatures from 1400 °C to 1900 °C and pressures from 17 up to 21 GPa in a multi anvil apparatus. The results show that F can shift the olivine–wadsleyite transition towards higher pressure. We find that F has an opposing effect to water, the latter of which extends the transition zone towards lower pressure. Moreover, the F storage capacity of wadsleyite is significantly lower than previously anticipated. F concentrations in wadsleyite range from 1470±60 μg/g to 2110±600 μg/g independent of temperature or pressure. The F storage capacity in wadsleyite is even lower than the F storage capacity of forsterite under transition zone conditions, and the latter can incorporate 3930±140 μg/g F under these conditions. Based on our data we find that the transition zone cannot be a reservoir for F as it is assumed to be for water. Furthermore, we argue that during subduction of a volatile-bearing slab, fractionation of water from F will occur, where water enters preferentially the transition zone and F remains in the peridotite of the lowermost upper mantle.

Shift of Glass Transition Temperature under High Pressure for Ge<sub>20</sub>Te<sub>80 </sub>Glass

Amorphous solids prepared from their melt state exhibit glass transition phenomena upon heating. Derivatives of volume like viscosity, specific heat and thermal expansion coefficient show rapid changes at the glass transition temperature (Tg). In general, application f high pressure increases the Tg (a positive dTg/dP). This positive dTg/dP has been well understood with the Free Volume and Entropy models. However, there are few exceptions where a negative dTg/dP has been observed. It has been proposed that the glasses which undergo negative thermal expansion can exhibit a negative dTg/dP. In this study, electrical resistivity of semiconducting Ge20Te80 glass at high pressures as a function of temperature has been measured in a Bridgman anvil apparatus. Electrical resistivity showed a pronounced change at Tg. The pressure dependence of Tg (dTg/dP) shows a decreasing trend (-dTg/dP). Chalcogenide glasses like Se, As2Se3 and As30Se30Te40 show a positive dTg/dP in contradiction to the present observation of negative dTg/dP. A model proposed by deNeufville and Rockstad finds a linear relationship between Tg and the optical band gap (Eg) when they are grouped according to their connectivity (Zav).Application of high pressure decreases the interatomic distance which in turn decreases the separation between the valence and conduction bands (optical band gap). This reduction in optical band gap shifts the glass transition to lower values. It is also suggested that the sign of the pressure derivative of Tg can be negative (-dTg/dP) if the thermal expansion coefficient is negative. Inelastic neutron diffraction studies show a negative thermal expansion coefficient for most of the Te based chalcogenide glasses. Hence, Ge20Te80 glass is uniquethat its pressure dependence of Tgobeys both thermodynamic and the Tg-Eg-Zav models.

ChemInform Abstract: Pressure‐Induced Phase Transitions of Hexagonal Perovskite‐Like Oxides.

AbstractTwo new cubic (3C structured) A2B′B′′O6‐type double‐perovskite phases, Ba2CoSbO6 (I) and Ba2ZnTeO6 (II) are prepared and stabilized by high pressure heat treatment of the corresponding hexagonal (6H and 12R structured, resp.) non‐perovskite phases (Au capsule in cubic anvil apparatus, 4 GPa, 1000 °C, 1 h).

マルチアンビル装置とMg<sub>2</sub>Si熱電材料の高圧合成

High-pressure X-ray diffraction study by using synchrotron radiation source was carried out to determine the synthetic condition of high-pressure synthesis. We also open our cell assembly of multi anvil apparatus which is readily available for beginners of high-pressure experiment. The synthetic condition of Mg2Si, which is expected to be inexpensive thermoelectric material, was explored by means of X-ray diffraction study. High-pressure synthesis of Mg2Si was performed by piston cylinder equipment. Thermoelectric properties of Mg2Si including Seebeck coefficient and electrical conductivity were measured at room pressure and high temperatures. A simple measurement system we develop enables us to measure the thermoelectric properties of small-sized synthesized sample under pressure.

A strip anvil apparatus with linear uniform pressure distribution

Bridgman anvil is a useful and effective tool in high-pressure research. However, in this apparatus, the pressure distribution is essentially centrosymmetric. Thus, considerable pressure gradients exist in the gasket and in the sample chamber respectively, and the uniform pressure area is limited. To improve the pressure uniformity in flat face supported anvils, we design a strip face anvil instead of conventional round face anvil and adopt an assortive strip gasket. Principle analysis and a series of pressure calibration experiments are also presented in this paper.The construction of the strip anvil and relevant parts of the apparatus are shown in the diagrams and photos. The relationship between pressure and shearing stress in the strip gasket is investigated by using the model of M. Wakatsuki, which indicates that the pressure distribution should be uniform along the central line of the strip gasket.Pressure calibration experiments are conducted by using strip anvils made of tungsten carbide with a length of 20 mm and width of 5 mm and by using the assortive strip gasket of pyrophyllite. Pressures at different places of the central line are calibrated according to the known phase transitions of bismuth in the same loading process, and the samples are assembled with symmetrical, unsymmerical, and separated local collocations, respectively.Experimental results exhibit that the pressure reaches up to 10 GPa in the central line of the strip gasket, and the pressures are almost equal at least within the range of 12 mm on the central line. The bias errores of oil pressures measured at different places of the central line are all less than 2.0% at 2.55 GPa and 3.6% at 7.7 GPa, indicating only a small pressure gradient along the central line. The main reason for the measuring bias errors lies in the difficulty of the assembly technique. Specifically, the bismuth wire is difficult to adhere to the central line of the anvil during compression. Hence, further improvement of the process is expected in the future.In conclusion, the strip anvil is a unique high-pressure apparatus. The principle analysis and pressure calibration experiments confirm that the pressure is uniform in one-dimensional direction along the central line of the strip anvil. This feature is propitious to the accurate investigation of linear samples under high pressure.

Pressure dependence of glass transition in As2Te3 glass.

Amorphous solids prepared from their melt state exhibit glass transition phenomenon upon heating. Viscosity, specific heat, and thermal expansion coefficient of the amorphous solids show rapid changes at the glass transition temperature (Tg). Generally, application of high pressure increases the Tg and this increase (a positive dT(g)/dP) has been understood adequately with free volume and entropy models which are purely thermodynamic in origin. In this study, the electrical resistivity of semiconducting As(2)Te(3) glass at high pressures as a function of temperature has been measured in a Bridgman anvil apparatus. Electrical resistivity showed a pronounced change at Tg. The Tg estimated from the slope change in the resistivity-temperature plot shows a decreasing trend (negative dT(g)/dP). The dT(g)/dP was found to be -2.36 °C/kbar for a linear fit and -2.99 °C/kbar for a polynomial fit in the pressure range 1 bar to 9 kbar. Chalcogenide glasses like Se, As(2)Se(3), and As(30)Se(30)Te(40) show a positive dT(g)/dP which is very well understood in terms of the thermodynamic models. The negative dT(g)/dP (which is generally uncommon in liquids) observed for As(2)Te(3) glass is against the predictions of the thermodynamic models. The Adam-Gibbs model of viscosity suggests a direct relationship between the isothermal pressure derivative of viscosity and the relaxational expansion coefficient. When the sign of the thermal expansion coefficient is negative, dT(g)/dP = Δk/Δα will be less than zero, which can result in a negative dT(g)/dP. In general, chalcogenides rich in tellurium show a negative thermal expansion coefficient (NTE) in the supercooled and stable liquid states. Hence, the negative dT(g)/dP observed in this study can be understood on the basis of the Adams-Gibbs model. An electronic model proposed by deNeufville and Rockstad finds a linear relation between Tg and the optical band gap (Eg) for covalent semiconducting glasses when they are grouped according to their average coordination number. The electrical band gap (ΔE) of As(2)Te(3) glass decreases with pressure. The optical and electrical band gaps are related as Eg = 2ΔE; thus, a negative dT(g)/dP is expected when As(2)Te(3) glass is subjected to high pressures. In this sense, As(2)Te(3) is a unique glass where its variation of Tg with pressure can be understood by both electronic and thermodynamic models.

Electrical conductivity anisotropy in alkali feldspar at high temperature and pressure

The electrical conductivity of alkali feldspar along different orientations was determined at 1.0 GPa and at temperatures of 823–1286 K in a cubic anvil apparatus using alternating current impedance spectroscopy. Impedance arcs representing crystal conductivity occur in the frequency range of ∼103–106 Hz. The electrical conductivity of alkali feldspar increases with increasing temperature. The highest electrical conductivities in alkali feldspars were measured along the a-axis, with somewhat lower conductivities along the b-axis, and the lowest conductivities along the c-axis, suggesting minor anisotropy. The activation enthalpies ranged from 100 to 110 kJ/mol. The anisotropic results were combined to yield an isotropic model with an activation enthalpy of 102 kJ/mol. By comparing these results with previous results, we suggest that the dominating charge carriers for alkali feldspars are alkali ions. The minor anisotropy in conductivity for alkali feldspar may not account for the anisotropy of the crust.

Pressure Effect on the Structure and Superconducting Transition Temperature of Filled Skutterudites LaT4P12 (T=Fe, Ru)

We studied the effect of pressure on the superconducting transition temperature \(T_{\text{SC}}\) of La\(T_{4}\)P12 (\(T=\text{Fe}\), Ru) up to 8 GPa through electrical resistivity measurements in a cubic anvil apparatus. The \(T_{\text{SC}}\) of LaFe4P12 was also determined through magnetization measurements up to 3.4 GPa with an opposed-anvil pressure cell. In LaFe4P12, \(T_{\text{SC}}\) increases with pressure at a rate of 0.71 K/GPa from 0 GPa reaching its maximum at approximately 7 GPa. In contrast, the \(T_{\text{SC}}\) of LaRu4P12 monotonically decreases with pressure. The decrease rate gradually increases from \(-0.07\) to \(-0.29\) K/GPa. The distinct pressure dependences of both \(T_{\text{SC}}\)'s cannot be explained solely from a structural point of view. We propose that the difference between the pressure dependence of \(T_{\text{SC}}\) for LaFe4P12 and that for LaRu4P12 can be attributed to the difference in the electronic density of states at the Fermi energy between these two compounds.

Pressure dependence of the superconducting transition temperature of the filled skutterudite YFe4P12

We have studied the pressure dependence of the superconducting transition temperature T-c of the filled skutterudite YFe4P12 under various quasihydrostatic pressures up to 8 GPa. DC magnetization measurements up to 1.2 GPa in a piston-cylinder cell yields a linear increase of T-c with a positive coefficient dT(c)/dP = 1 K/GPa. Resistivity measurements up to 8 GPa in a cubic anvil apparatus show that Tc increases to 9.3 K at 8 GPa, but the slope decreases gradually with increasing pressure. Besides the previously reported LaFe4P12, YFe4P12 becomes the second filled skutterudite superconductor that exhibits a positive pressure coefficient dT(c)/dP in a broad pressure range. The observed large dT(c)/dP > 0 of YFe4P12 can be rationalized by our band-structure calculations that show an enhancement of density of states at Fermi energy and the Hopfield parameter under pressure at least up to 8 GPa. On the other hand, similar calculations predict a dT(c)/dP < 0 for YRu4P12.

Growth, Structural and High Pressure Study of GeS&lt;sub&gt;0.25&lt;/sub&gt;Se&lt;sub&gt;0.75&lt;/sub&gt; and GeS&lt;sub&gt;0.75&lt;/sub&gt;Se&lt;sub&gt;0.25&lt;/sub&gt; Single Crystals

The orthorhombic semi-conducting compound GeS0.25Se0.75 and GeS0.75Se0.25 possess interesting electrical properties and can been the subject of numerous investigations. The changes in solids under high pressure can reveal several new features of interatomic forces, which are responsible for their diverse physical properties. Authors have carried out growth of GeS0.25Se0.75 and GeS0.75Se0.25 crystals by Direct Vapor Transport (DVT) technique. For compositional confirmation energy dispersive analysis of X-ray (EDAX) has been used. EDAX results show that the grown crystals are nearly stoichiometrycally perfect. The grown crystals have been characterized by X-ray diffraction technique (using Philips X Pert MPD diffractometer) for structural characterization. These crystals are crystallized in orthorhombic structure. The values of lattice parameters, unit cell volume and X-ray density are calculated and presented. It is observed from lattice parameters, unit cell volume and X-ray density, that as the content of sulfur increases the value of all the lattice parameters decreases. High pressure study is also of great importance to visualize the mechanism governing the structural changes and to reveal solid state properties associated with different structure. For the room temperature measurement of resistance as a function of pressure, up to 7 GPa, the sample was set at the centre of the talc disc on the lower anvil. The pressure was generated by a hydraulic press on the Bridgman type tungsten carbide opposed anvil apparatus with in-situ Bismuth pressure calibration. The resistance was measured in several independent runs on these crystals as a function of pressure and was found to be reproducible. The results of variation of electrical resistance do not show presence of any phase transition up to 7 GPa. We investigate in GeS0.25Se0.75 and GeS0.75Se0.25 single crystals that as sulfur content increases, resistance of this compound increases.

High pressure characterization and modelling of CaCO3 powder mix in the Bridgman anvil apparatus

For investigating high pressure sintering processes, numerical models can be used. This will demand material models which give realistic mechanical response throughout the whole parameter space of the actual process. As the pressures become higher, the material density approaches its full theoretical value and the elastic part of the material properties becomes increasingly important. In this investigation, Poisson's ratio was determined using ultrasonic pulse-echo measurements. A new elastic model and an improved plasticity model were implemented into a user-defined material subroutine in a finite element (FE) code. To experimentally investigate the load displacement response and pressure distribution in powder compacts during pressing, a pressure instrumented Bridgman anvil apparatus was used. Validation of the FE model was conducted against experimental data from pressing experiments using two different start densities. The results show that the simulation model is indeed capable of reproducing load–thickness curves and pressure profiles reasonable close to the experimental curves.

High pressure synthesis at 10 GPa and 1400 K using a small cubic anvil apparatus with a multi-anvil 6-6 system

In the present study, high pressure synthesis up to 10 GPa was done using a small cubic anvil apparatus (W45×D52×H92 cm3, load capacity of 1.80 MN) with a multi-anvil 6-6 system. Its performance was demonstrated by synthesizing a ferromagnetic perovskite oxide, CaCu3Fe4O12, at pressure–temperature conditions of 10 GPa and 1400 K. The synthesized CaCu3Fe4O12 perovskite was ∼1 mm in diameter and ∼2 mm in height and its size was large enough for performing magnetic susceptibility measurements at 5–300 K using a superconducting quantum interference device magnetometer and phase identification by X-ray diffraction. The experimental system developed in the present study has many advantages when used in high pressure synthesis experiments, and the technical development of a small cubic anvil apparatus will greatly contribute to the advancement of high pressure synthesis of novel materials.

A miniature cubic anvil apparatus for optical measurement under high pressure

A miniature cubic anvil apparatus was developed for optical measurement on materials in a high-pressure space of 8-10 mm(3) under high pressure, and preliminary experiments were conducted to 3.6 GPa at room temperature with optical visual observation and ruby fluorescence measurement. In the apparatus, a cubic pressure medium was squeezed with six tungsten carbide anvils, which are driven with a pair of guide blocks by tightening four loading screws. Optical access on the sample was made through holes in axial anvils and the guide blocks as well as optical windows made of Al(2)O(3) single crystals embedded in the pressure medium. The apparatus is compact and light, ~53 mm in diameter and height and ~530 g in weight, and the features of the apparatus benefit easy application of the apparatus to various types of standard optical measurement systems. The optical measurement on the sample in the high-pressure space of 8-10 mm(3) should greatly contribute to advancements of studies relevant to high-pressure behaviors of materials.