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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]

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]