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When diamond anvil cell (DAC) sample chambers are outfitted with both thermal insulation and electrodes, two cutting-edge experimental methods are enabled: Joule heating with spectroradiometric temperature measurement and electrical resistance measurements of samples heated to thousands of kelvin. The accuracy of temperature and resistance measurements, however, often suffers from poor control of the shape and location of the sample, electrodes, and thermal insulation. Here, we present a recipe for the reproducible and precise fabrication of DAC sample, electrodes, and thermal insulation using a three-layer microassembly. The microassembly contains two potassium chloride thermal insulation layers, four electrical leads, a sample, and a buttressing layer made of polycrystalline alumina. The sample, innermost electrodes, and buttress layer are fabricated by focused-ion-beam milling. Three iron samples are presented as proof of concept. Each is successfully compressed and pulsed Joule heated while maintaining a four-point probe configuration. The highest pressure-temperature condition achieved is ∼ 150 GPa and 4000 K. [ABSTRACT FROM AUTHOR]

Decades of measurements of the thermophysical properties of hot metals show that pulsed Joule heating is an effective method to heat solid and liquid metals that are chemically reactive or difficult to contain. To extend such measurements to hundreds of GPa pressure, pulsed heating methods have recently been integrated with diamond anvil cells. The recent design used a low-side switch and active electrical sensing equipment that was prone to damage and measurement error. Here, we report the design and characterization of new electronics that use a high-side switch and robust, passive electrical sensing equipment. The new pulse amplifier can heat ∼ 5 to 50 μm diameter metal wires to thousands of kelvin at tens to hundreds of GPa using diamond anvil cells. Pulse durations and peak currents can each be varied over three orders of magnitude, from 5 µs to 10 ms and from 0.2 to 200 A. The pulse amplifier is integrated with a current probe. Two voltage probes attached to the body of a diamond anvil cell are used to measure voltage in a four-point probe geometry. The accuracy of four-point probe resistance measurements for a dummy sample with 0.1 Ω resistance is typically better than 5% at all times from 2 µs to 10 ms after the beginning of the pulse. [ABSTRACT FROM AUTHOR]

Accurate and precise measurements of spectroradiometric temperature are crucial for many high pressure experiments that use diamond anvil cells or shock waves. In experiments with sub-millisecond timescales, specialized detectors such as streak cameras or photomultiplier tubes are required to measure temperature. High accuracy and precision are difficult to attain, especially at temperatures below 3000 K. Here, we present a new spectroradiometry system based on multianode photomultiplier tube technology and passive readout circuitry that yields a 0.24 µs rise-time for each channel. Temperature is measured using five color spectroradiometry. During high pressure pulsed Joule heating experiments in a diamond anvil cell, we document measurement precision to be ±30 K at temperatures as low as 2000 K during single-shot heating experiments with 0.6 µs time-resolution. Ambient pressure melting tests using pulsed Joule heating indicate that the accuracy is ±80 K in the temperature range 1800–2700 K. [ABSTRACT FROM AUTHOR]

Stishovite is a key mineral for understanding the deep Earth water cycle because of its potential as a main carrier for water into the transition zone and lower mantle. During subduction-related metamorphism of basaltic oceanic crust, stishovite stabilizes at 8–9 GPa and comprises 10–25 vol% of the bulk mineralogy, with some experimental studies indicating that stishovite can accommodate 3.5 wt% H2O or more in the transition zone and upper lower mantle. This large water solubility has been explained by a hydrogarnet substitution mechanism (1Si4+ ↔ 4H+) and/or the incorporation of interstitial molecular water. To investigate water speciation and hydrogen isotope behavior, we synthesized partially deuterated hydrous stishovite at 9 GPa and 450 °C in a multi-anvil press (MA). The hydrous stishovite contains on average 1.69 ± 0.05 wt% water, which is consistent with earlier MA studies but is significantly lower than the 3.5 wt% reported from in situ diamond anvil cell (DAC) studies made at higher pressures and temperatures. 1H MAS NMR spinning sideband characteristics suggest a high abundance of interstitial molecular water in hydrous stishovite, while the presence of a hydrogarnet defect cannot be ruled out. Unit-cell volumes and deuterium enrichment in the quenched hydrous stishovite indicate that ~ 45% of the water is lost from the stishovite upon quenching and decompression of the experiment, consistent with a higher solubility. This implies that the pristine water contents of a P–T–fO2 equilibrated hydrous stishovite cannot be quenched to 1 atm and room temperature from classical MA experiments. We further present a capillary-based recovery method for fluid from experimental capsules, allowing direct determination of the D/H ratio of the experimental fluid and indirect determination of the hydrous stishovite. Using Rayleigh modeling to account for the quench-related water loss, we find that, at 450 °C and 9 GPa, deuterium is 3.5–4.5 times enriched in hydrous stishovite relative to coexisting aqueous fluid. This is opposite of what is commonly observed for mineral–fluid pairs above 300 °C, rendering hydrous stishovite a potential sink for deuterium and decreasing the D/H ratio of coexisting aqueous fluids. Partial decomposition (30–60%) of hydrous stishovite during mantle upwelling and production of primary basaltic melts could be accompanied by high-temperature D/H fractionation, decreasing the hydrogen isotope composition of such melts towards "mantle-like" δD values between −75 and −220‰. [ABSTRACT FROM AUTHOR]

High pressure–temperature experiments provide information on the phase diagrams and physical characteristics of matter at extreme conditions and offer a synthesis pathway for novel materials with useful properties. Experiments recreating the conditions of planetary interiors provide important constraints on the physical properties of constituent phases and are key to developing models of planetary processes and interpreting geophysical observations. The laser-heated diamond anvil cell (DAC) is currently the only technique capable of routinely accessing the Earth's lower-mantle geotherm for experiments on non-metallic samples, but large temperature uncertainties and poor temperature stability limit the accuracy of measured data and prohibits analyses requiring long acquisition times. We have developed a novel internal resistive heating (IRH) technique for the DAC and demonstrate stable heating of non-metallic samples up to 3000 K and 64 GPa, as confirmed by in situ synchrotron x-ray diffraction and simultaneous spectroradiometric temperature measurement. The temperature generated in our IRH-DAC can be precisely controlled and is extremely stable, with less than 20 K variation over several hours without any user intervention, resulting in temperature uncertainties an order of magnitude smaller than those in typical laser-heating experiments. Our IRH-DAC design, with its simple geometry, provides a new and highly accessible tool for investigating materials at extreme conditions. It is well suited for the rapid collection of high-resolution P–V–T data, precise demarcation of phase boundaries, and experiments requiring long acquisition times at high temperature. Our IRH technique is ideally placed to exploit the move toward coherent nano-focused x-ray beams at next-generation synchrotron sources. [ABSTRACT FROM AUTHOR]

Abstract We report on laser-heated diamond anvil cell (LHDAC) experiments in the FeO–MgO–SiO 2 –CO 2 (FMSC) and CaO–MgO–SiO 2 –CO 2 (CMSC) systems at lower mantle pressures designed to test for decarbonation and diamond forming reactions. Sub-solidus phase relations based on synthesis experiments are reported in the pressure range of ∼35 to 90 GPa at temperatures of ∼1600 to 2200 K. Ternary bulk compositions comprised of mixtures of carbonate and silica are constructed such that decarbonation reactions produce non-ternary phases (e.g. bridgmanite, Ca-perovskite, diamond, CO 2 –V), and synchrotron X-ray diffraction and micro-Raman spectroscopy are used to identify the appearance of reaction products. We find that carbonate phases in these two systems react with silica to form bridgmanite ±Ca-perovskite + CO 2 at pressures in the range of ∼40 to 70 GPa and 1600 to 1900 K in decarbonation reactions with negative Clapeyron slopes. Our results show that decarbonation reactions form an impenetrable barrier to subduction of carbonate in oceanic crust to depths in the mantle greater than ∼1500 km. We also identify carbonate and CO 2 –V dissociation reactions that form diamond plus oxygen. On the basis of the observed decarbonation reactions we predict that the ultimate fate of carbonate in oceanic crust subducted into the deep lower mantle is in the form of refractory diamond in the deepest lower mantle along a slab geotherm and throughout the lower mantle along a mantle geotherm. Diamond produced in oceanic crust by subsolidus decarbonation is refractory and immobile and can be stored at the base of the mantle over long timescales, potentially returning to the surface in OIB magmas associated with deep mantle plumes. Highlights • Experiments were made in the systems FMS-CO2 and CMS-CO2 at lower mantle pressures. • Carbonate in these systems react with silica in the lower mantle. • Decarbonation reactions with negative P–T slopes form CO 2 or diamond plus oxygen. • Carbonate in oceanic crust is limited to ∼1500 km depth along subduction geotherms. • Diamond is the stable form of carbon in oceanic crust at ambient mantle temperature. [ABSTRACT FROM AUTHOR]

In this article, the specification and application of the new double‐sided YAG laser‐heating system built on beamline I15 at Diamond Light Source are presented. This system, combined with diamond anvil cell and X‐ray diffraction techniques, allows in situ and ex situ characterization of material properties at extremes of pressure and temperature. In order to demonstrate the reliability and stability of this experimental setup over a wide range of pressure and temperature, a case study was performed and the phase diagram of lead was investigated up to 80 GPa and 3300 K. The obtained results agree with previously published experimental and theoretical data, underlining the quality and reliability of the installed setup. A double‐sided, off‐axis laser‐heating system for monochromatic X‐ray diffraction experiments using a diamond anvil cell has been installed at beamline I15 at Diamond Light Source. Measurements of the pressure–temperature phase diagram of Pb demonstrate the reliability of the setup and the high quality of the data. [ABSTRACT FROM AUTHOR]

We have developed numerical simulations of spectroradiometric temperature measurement for refractive optical systems used in laser-heated diamond anvil cell (LHDAC) experiments. Chromatic dispersion in refractive optics is quantified by the wavelength-dependent radial displacement function. Results show that a combination of high peak temperature, steep temperature gradient, high spatial resolution, and large radial displacement can cause extreme errors in temperature, on the order of hundreds to thousands of degrees of Kelvin. Increasing detector bin size can dampen the magnitude of the error in peak temperature, but the average temperature produced in this way is still likely to be erroneous. Accurate peak temperature can be measured if the radial displacement is less than the radius of a region of constant temperature. Errors in accuracy can be reduced by locating the wavelength range that produces a minimum and symmetrical radial displacement. The precision of the fitted blackbody function is correlated positively with accuracy so that the optimal wavelength range can be located by minimizing the error in the blackbody fit. Modern spectroradiometric systems that utilize refractive optics are capable of accurate temperature measurement if proper steps are taken to identify and mitigate the effects of chromatic dispersion. [Copyright &y& Elsevier]

Eutectic melting curves in the system MgO–SiO 2 have been experimentally determined at lower mantle pressures using laser-heated diamond anvil cell (LH-DAC) techniques. We investigated eutectic melting of bridgmanite plus periclase in the MgO–MgSiO 3 binary, and melting of bridgmanite plus stishovite in the MgSiO 3 –SiO 2 binary, as analogues for natural peridotite and basalt, respectively. The melting curve of model basalt occurs at lower temperatures, has a shallower d T / d P slope and slightly less curvature than the model peridotitic melting curve. Overall, melting temperatures detected in this study are in good agreement with previous experiments and ab initio simulations at ∼25 GPa ( Liebske and Frost, 2012 ; de Koker et al., 2013 ). However, at higher pressures the measured eutectic melting curves are systematically lower in temperature than curves extrapolated on the basis of thermodynamic modelling of low-pressure experimental data, and those calculated from atomistic simulations. We find that our data are inconsistent with previously computed melting temperatures and melt thermodynamic properties of the SiO 2 endmember, and indicate a maximum in short-range ordering in MgO–SiO 2 melts close to Mg 2 SiO 4 composition. The curvature of the model peridotite eutectic relative to an MgSiO 3 melt adiabat indicates that crystallization in a global magma ocean would begin at ∼100 GPa rather than at the bottom of the mantle, allowing for an early basal melt layer. The model peridotite melting curve lies ∼ 500 K above the mantle geotherm at the core–mantle boundary, indicating that it will not be molten unless the addition of other components reduces the solidus sufficiently. The model basalt melting curve intersects the geotherm at the base of the mantle, and partial melting of subducted oceanic crust is expected. [ABSTRACT FROM AUTHOR]