Search Results (15)

Superdeep diamonds and their syngenetic inclusions are crucial for understanding Earth’s deep carbon cycle and slab–mantle redox dynamics. The origins of these diamonds, especially their links to iron (Fe) carbides and ferropericlase with varying Mg# [=Mg/(Mg+Fe)_at], however, remain elusive. In this study, we performed high pressure–temperature (P-T) experiments (10–16 GPa and 1200–1700 K) across cold-to-warm subduction zones using a multi-anvil press. The results reveal a stepwise Fe-mediated carbonate reduction process for the formation of superdeep diamonds: MgCO₃ → Fe-carbides (Fe₃C/Fe₇C₃) → graphite/diamond. This mechanism explains two phenomena regarding superdeep diamonds: (1) anomalous ¹³C depletion results from kinetic isotope fractionation during ¹²C enrichment into the intermediate Fe-carbides; (2) nitrogen scarcity is due to Fe-carbides acting as nitrogen sinks. Ferropericlase [(Mg,Fe)O] formed during the reactions in our experiments shows Mg# variations (0.2–0.9), similar to those found in natural samples. High Mg# (>0.7) variants from lower temperature experiments indicate diamond crystallization from carbonatitic melts in the shallow lower mantle, while the broad Mg# range (0.2–0.9) from experiments at higher temperatures suggests multi-depth formation processes as found in Brazilian diamonds. These findings suggest that slab–mantle interactions produce superdeep diamonds with distinctive Fe-carbides and ferropericlase assemblages as inclusions, coupled with their ¹³C- and nitrogen-depleted signatures, which underscore thermochemical carbon cycling as a key factor in deep carbon storage and mantle mineralogy. Full article

Compressional (V_P) and shear (V_S) wave velocities of polycrystalline vanadium were measured simultaneously up to 11.5 GPa at room temperature using ultrasonic interferometry in a multi-anvil press. Complex softening behavior in V_S and resulting shear moduli are discovered, possibly revealing a precursor to the reported phase transition within 30–60 GPa. The current data enables a comprehensive assessment of the elastic and mechanical properties of vanadium at high pressures, including bulk and shear moduli, Young’s modulus, Poisson’s ratio, and Pugh’s ratio. Through fitting to the 3rd-order finite strain equations, the elastic moduli and their pressure derivatives were determined to be K_S0 = 151 (2) GPa, G₀ = 46.9 (8) GPa, K’_S0 = 3.47 (5), and G’₀ = 0.62 (1). These experimental results allow us to compare with and benchmark the existing Steinberg–Guinan models for extrapolations to extreme pressure and temperature conditions. Full article

Melting of carbonated rocks in the mantle influences the Earth’s deep carbon cycle and the long-term evolution of the atmosphere. Previous studies of the high-pressure melting curve of K₂CO₃ have yielded inconsistent results, with discrepancies of nearly 200 °C at 3 GPa and more than 400 °C at 12 GPa. Here, we report constraints on the melting curve of K₂CO₃ at pressures up to 20 GPa from in situ ionic conduction experiments and Pt sphere experiments. To help resolve the large discrepancies, we tested the ionic conduction method against the well-established differential thermal analysis (DTA) method and conventional Pt sphere method at the ambient pressure of 1 bar. Furthermore, ionic conduction experiments were conducted on sodium chloride (NaCl) to reduce uncertainties in pressure calibration of the multi-anvil press. We also modified the configuration of the in situ ionic conduction experiments to minimize the influence of thermal gradient on melting point determination. Finally, we inspected the effect of water by varying the initial sample state and container wall thickness in the Pt sphere experiments and applied X-ray radiography as a reliable and efficient method to examine the products. Compared with the results from the ionic conduction experiments, the melting point of K₂CO₃ from the Pt sphere experiments was found to be 200~400 °C lower, likely due to a small amount of water trapped by hygroscopic K₂CO₃ in closed platinum (Pt) capsules. We find that anhydrous K₂CO₃ remains more refractory than Na₂CO₃ at elevated pressures. Full article

Akimotoite, ilmenite-type MgSiO₃ high-pressure polymorph can be stable in the lower-mantle transition zone along average mantle and subducting slab geotherms. Significant amounts of Al₂O₃ can be incorporated into the structure, having the pyrope (Mg₃Al₂Si₃O₁₂) composition. Previous studies have investigated the effect of Al₂O₃ on its crystal structure at nearly endmember compositions. In this study, we synthesized high-quality ilmenite-type Mg₃Al₂Si₃O₁₂ phase at 27 GPa and 1073 K by means of a Kawai-type multi-anvil press and refined the crystal structure at ambient conditions using a synchrotron X-ray diffraction data via the Rietveld method to examine the effect of Al₂O₃. The unit-cell lattice parameters were determined to be a = 4.7553(7) Å, c = 13.310(2) Å, and V = 260.66(6) ų, with Z = 6 (hexagonal, R$\overline{3}$). The volume of the present phase was placed on the akimotoite-corundum endmember join. However, the refined structure showed a strong nonlinear behavior of the a- and c-axes, which can be explained by Al incorporation into the MgO₆ and SiO₆ octahedral sites, which are distinctly different each other. Ilmenite-type Mg₃Al₂Si₃O₁₂ phase may be found in shocked meteorites and can be a good indicator for shock conditions at relatively low temperatures of 1027–1127 K. Full article

Inclusions in mantle minerals and xenoliths from kimberlites worldwide derived from depths exceeding 100 km vary in composition from alkali-rich saline to carbonatitic. Despite the wide distribution of these melts and their geochemical importance as metasomatic agents that altered the mineralogy and geochemistry of mantle rocks, the P-T range of stability of these melts remains largely undefined. Here we report new experimental data on phase relations in the system KCl–CaCO₃–MgCO₃ at 3 GPa obtained using a multianvil press. We found that the KCl–CaCO₃ and KCl–MgCO₃ binaries have the eutectic type of T-X diagrams. The KCl-calcite eutectic is situated at K2# 56 and 1000 °C, while the KCl-magnesite eutectic is located at K2# 79 and 1100 °C, where K2# = 2KCl/(2KCl + CaCO₃ + MgCO₃) × 100 mol%. Just below solidus, the KCl–CaCO₃–MgCO₃ system is divided into two partial ternaries: KCl + magnesite + dolomite and KCl + calcite–dolomite solid solutions. Both ternaries start to melt near 1000 °C. The minimum on the liquidus/solidus surface corresponds to the KCl + Ca_0.73Mg_0.27CO₃ dolomite eutectic situated at K2#/Ca# 39/73, where Ca# = 100∙Ca/(Ca + Mg) × 100 mol%. At bulk Ca# ≤ 68, the melting is controlled by a ternary peritectic: KCl + dolomite = magnesite + liquid with K2#/Ca# 40/68. Based on our present and previous data, the KCl + dolomite melting reaction, expected to control solidus of KCl-bearing carbonated eclogite, passes through 1000 °C at 3 GPa and 1200 °C at 6 GPa and crossovers a 43-mW/m² geotherm at a depth of 120 km and 37-mW/m² geotherm at a depth of 190 km. Full article

High-Pressure (HP) technology allows new possibilities of processing by Spark Plasma Synthesis (SPS). This process is mainly involved in the sintering process and for bonding, growing and reaction. High-Pressure tools combined with SPS is applied for processing polycrystalline diamond without binder (binderless PCD) in this current work. Our described innovative Ultra High Pressure Spark Plasma Sintering (UHP-SPS) equipment shows the combination of our high-pressure apparatus (Belt-type) with conventional pulse electric current generator (Fuji). Our UHP-SPS equipment allows the processing up to 6 GPa, higher pressure than HP-SPS equipment, based on a conventional SPS equipment in which a non-graphite mold (metals, ceramics, composite and hybrid) with better mechanical properties (capable of 1 GPa) than graphite. The equipment of UHP-SPS and HP-SPS elements (pistons + die) conductivity of the non-graphite mold define a Hot-Pressing process. This study presents the results showing the ability of sintering diamond powder without additives at 4–5 GPa and 1300–1400 °C for duration between 5 and 30 min. Our described UHP-SPS innovative cell design allows the consolidation of diamond particles validated by the formation of grain boundaries on two different grain size powders, i.e., 0.75–1.25 μm and 8–12 μm. The phenomena explanation is proposed by comparison with the High Pressure High Temperature (HP-HT) (Belt, toroidal-Bridgman, multi-anvils (cubic)) process conventionally used for processing binderless polycrystalline diamond (binderless PCD). It is shown that using UHP-SPS, binderless diamond can be sintered at very unexpected P-T conditions, typically ~10 GPa and 500–1000 °C lower in typical HP-HT setups. This makes UHP-SPS a promising tool for the sintering of other high-pressure materials at non-equilibrium conditions and a potential industrial transfer with low environmental fingerprints could be considered. Full article

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

Electrical conductivities of the dry hot-pressed sintering gabbro with various mineralogical proportions (Cpx_XPl_100−X, X = 0, 10, 20, 30, 40, 50, 60, 70, 80, 90 and 100 vol% (the signals of Cpx and Pl denote clinopyroxene and plagioclase, respectively) were measured in the YJ-3000t multi-anvil pressure and Solartron-1260 impedance spectroscopy analyzer at temperatures of 773–1073 K and pressures of 1.0–3.0 GPa. At the given pressure conditions, the electrical conductivity and temperature conformed to an Arrhenius relation. For the fixed mineralogical composition of Cpx₅₀Pl₅₀, the electrical conductivities of the samples significantly increased with the rise of temperature, but slightly decreased with increasing pressure. Furthermore, the activation energy and activation volume were determined as 1.06 ± 0.12 eV and 6.00 ± 2.00 cm³/mole, respectively. As for the various mineralogical compositions of dry gabbro, the electrical conductivities of the samples increased with the rise of volume percentage of clinopyroxene (Cpx) at 1.0 GPa. It is proposed that the main conduction mechanism is the small polaron, owing to the positive relation between the electrical conductivity and the iron content in samples. On the basis of these obtained conductivity results, laboratory-based electrical conductivity–depth profiles for the hot-pressed sintering gabbro with various mineralogical proportions and temperature gradients were successfully established. In conclusion, although the present acquired electrical conductivity results on the dry hot-pressed sintering gabbro with various mineralogical proportions cannot explain the high conductivity anomaly in the oceanic crust and West African craton, it can provide one reasonable constraint on the mineralogical composition in these representative gabbro-rich regions. Full article

As a dominant water carrier, hydrous silicate minerals and rocks are widespread throughout the representative regions of the mid-lower crust, upper mantle, and subduction zone of the deep Earth interior. Owing to the high sensitivity of electrical conductivity on the variation of water content, high-pressure laboratory-based electrical characterizations for hydrous silicate minerals and rocks have been paid more attention to by many researchers. With the improvement and development of experimental technique and measurement method for electrical conductivity, there are many related results to be reported on the electrical conductivity of hydrous silicate minerals and rocks at high-temperature and high-pressure conditions in the last several years. In this review paper, we concentrated on some recently reported electrical conductivity results for four typical hydrous silicate minerals (e.g., hydrous Ti-bearing olivine, epidote, amphibole, and kaolinite) investigated by the multi-anvil press and diamond anvil cell under conditions of high temperatures and pressures. Particularly, four potential influence factors including titanium-bearing content, dehydration effect, oxidation−dehydrogenation effect, and structural phase transition on the high-pressure electrical conductivity of these hydrous silicate minerals are deeply explored. Finally, some comprehensive remarks on the possible future research aspects are discussed in detail. Full article

The first high-pressure scandium tellurate HP-Sc₂TeO₆ was synthesized from an NP-Sc₂TeO₆ normal-pressure precursor at 12 GPa and 1173 K using a multianvil apparatus (1000 t press, Walker-type module). The compound crystallizes in the monoclinic space group P2/c (no. 13) with a = 729.43(3), b = 512.52(2), c = 1095.02(4) pm and β = 103.88(1)°. The structure was refined from X-ray single-crystal diffractometer data: R₁ = 0.0261, wR₂ = 0.0344, 568 F² values and 84 variables. HP-Sc₂TeO₆ is isostructural to Yb₂WO₆ and is built up from TeO₆ octahedra, typical for tellurate(VI) compounds. During synthesis, a reconstructive transition from P321 (normal-pressure modification) to P2/c (high-pressure modification) takes place and the scandium–oxygen distances as well as the coordination number of scandium increase. However, the coordination sphere around the Te⁶⁺ cations gets only slightly distorted. High-temperature powder XRD investigations revealed a back-transformation of HP-Sc₂TeO₆ to the ambient-pressure modification above 973 K. Full article

Although the general instability of the iron nitride γ′-Fe₄N with respect to other phases at high pressure is well established, the actual type of phase transitions and equilibrium conditions of their occurrence are, as of yet, poorly investigated. In the present study, samples of γ′-Fe₄N and mixtures of α Fe and γ′-Fe₄N powders have been heat-treated at temperatures between 250 and 1000 °C and pressures between 2 and 8 GPa in a multi-anvil press, in order to investigate phase equilibria involving the γ′ phase. Samples heat-treated at high-pressure conditions, were quenched, subsequently decompressed, and then analysed ex situ. Microstructure analysis is used to derive implications on the phase transformations during the heat treatments. Further, it is confirmed that the Fe–N phases in the target composition range are quenchable. Thus, phase proportions and chemical composition of the phases, determined from ex situ X-ray diffraction data, allowed conclusions about the phase equilibria at high-pressure conditions. Further, evidence for the low-temperature eutectoid decomposition ${\mathsf{\gamma }}^{\prime }\to \mathsf{\alpha }+{\mathsf{\epsilon }}^{\prime }$ is presented for the first time. From the observed equilibria, a P–T projection of the univariant equilibria in the Fe-rich portion of the Fe–N system is derived, which features a quadruple point at 5 GPa and 375 °C, above which γ′-Fe₄N is thermodynamically unstable. The experimental work is supplemented by ab initio calculations in order to discuss the relative phase stability and energy landscape in the Fe–N system, from the ground state to conditions accessible in the multi-anvil experiments. It is concluded that γ′-Fe₄N, which is unstable with respect to other phases at 0 K (at any pressure), has to be entropically stabilised in order to occur as stable phase in the system. In view of the frequently reported metastable retention of the γ′ phase during room temperature compression experiments, energetic and kinetic aspects of the polymorphic transition ${\mathsf{\gamma }}^{\prime }\rightleftharpoons {\mathsf{\epsilon }}^{\prime }$ are discussed. Full article

A new series of soda–lime glass naturally doped with Nd and doped with 0.2 wt% of Eu₂O₃ was densified in a multi-anvil press up to 21 GPa. The densities of the millimetric samples were precisely measured using a floatation method in a heavy liquid made with sodium polytungstate. The obtained densification curve is significantly different from the calibration previously reported, reaching a maximum densification saturation of 3.55 ± 0.14%. This difference could be due to better hydrostatic conditions realized in this new study. The densified samples were characterized using Raman and Brillouin spectroscopy, as well as the emission of both Eu³⁺ and Nd³⁺. The evolution of the spectra was evaluated using integration methods to reduce error bars. The relative precision of the calibration curves is discussed. The evolution of Nd³⁺ transition was found to be the most sensitive calibration. Linear dependence with the density was found for all observables, with exception for Brillouin spectroscopy showing a divergent behavior. The Brillouin shift shows an unreported minimum for a densification ~0.4%. Full article

Making consistent and precise octahedral pressure media is crucial for reproducible high-pressure experiments in the multi-anvil press. Here we report a new approach of casting octahedra using 3D-printed molds, and pressure calibrations for octahedra both with and without pre-existing gaskets (“fins”). The 3D-printed molds for casting octahedra from either Ceramacast 584-OF or 646 cement improve the reproducibility of the octahedra and allow for a pre-existing central hole (for the high-pressure cell assembly) in the final cast product. Pressure and temperature calibrations of the octahedra have been performed based on phase transitions in bismuth (Bi) and silica (SiO₂), respectively, in order to determine the efficiency and reproducibility of pressure generation and thermal insulation for cast octahedra designed for use with 18/12, 14/8, and 10/5 multi-anvil assemblies. The pressure-generating efficiency of the 14/8 and 10/5 octahedra with pre-existing gaskets, cast from the 584-OF cement, is similar to that of the corresponding COMPRES (Consortium for Materials Properties Research in Earth Sciences) octahedra, and more efficient than pre-cast octahedra made from the same material but lacking pre-existing gaskets. The efficiency of pre-gasketed 18/12 octahedra made of the 646 cement is markedly lower than those of the 584 cement. However, the 18/12 large-volume octahedra, cast (with fins) from the ZrO₂-based 646 cement, also provides efficient thermal insulation. Casting octahedral solid pressure media for multi-anvil experiments using 3D-printed “injection” molds is a low-cost and low failure-rate alternative for conducting reproducible experiments at high pressure in the multi-anvil apparatus. Full article

A Paris-Edinburgh press combined with a multi-channel collimator assembly has been commissioned at the GeoSoilEnviro Center for Advanced Radiation Sources (GSECARS) beamline for monochromatic X-ray scattering, with an emphasis on studying low-Z liquids, especially silicate liquids at high pressure. The Paris-Edinburgh press is mounted on a general-purpose diffractometer, with a pixel array detector mounted on the detector arm. The incident monochromatic undulator beam with energies up to 60 keV is focused both horizontally and vertically to a beam size about 30 × 30 µm. With this setup, background scattering from the surrounding pressure media is completely removed at 2θ angles above 10° for samples larger than 1.05 mm in diameter. Thirty minutes is typically sufficient to collect robust X-ray scattering signals from a 1.6 mm diameter amorphous silicate sample. Cell assemblies for the standard Paris-Edinburgh anvils have been developed and pressures and temperatures up to 7 GPa and 2300 K, respectively, have been maintained steadily over hours. We have also developed a cupped-toroidal Drickamer anvil to further increase pressure and temperature capabilities. The cupped-toroidal Drickamer anvil combines features of a modified Drickamer anvil and the traditional Paris-Edinburgh anvil. Pressures up to 12 GPa have been generated at temperatures up to 2100 K. Full article

Titanium aluminides find application in modern light-weight, high-temperature turbines, such as aircraft engines, but suffer from poor plasticity during manufacturing and processing. Huge forging presses enable materials processing in the 10-GPa range, and hence, it is necessary to investigate the phase diagrams of candidate materials under these extreme conditions. Here, we report on an in situ synchrotron X-ray diffraction study in a large-volume press of a modern (α₂ + γ) two-phase material, Ti-45Al-7.5Nb-0.25C, under pressures up to 9.6 GPa and temperatures up to 1686 K. At room temperature, the volume response to pressure is accommodated by the transformation γ → α₂, rather than volumetric strain, expressed by the apparently high bulk moduli of both constituent phases. Crystallographic aspects, specifically lattice strain and atomic order, are discussed in detail. It is interesting to note that this transformation takes place despite an increase in atomic volume, which is due to the high ordering energy of γ. Upon heating under high pressure, both the eutectoid and γ-solvus transition temperatures are elevated, and a third, cubic β-phase is stabilized above 1350 K. Earlier research has shown that this β-phase is very ductile during plastic deformation, essential in near-conventional forging processes. Here, we were able to identify an ideal processing window for near-conventional forging, while the presence of the detrimental β-phase is not present under operating conditions. Novel processing routes can be defined from these findings. Full article