Search

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]

Hydrogen and helium are the most abundant elements in the universe, and they constitute the interiors of gas giant planets. Thus, their equations of states, phase, chemical state, and chemical reactivity at extreme conditions are of great interest. Applying Raman spectroscopy, visual observation, and synchrotron X-ray diffraction in diamond anvil cells, we performed experiments on H2–He 1:1 and D2–He 1:10 compressed gas mixtures up to 100 GPa at 300 K. By comparing with the available data on pure bulk materials, we find no sign of miscibility, chemical reactivity, and new compound formation. This result establishes a new baseline for future investigations of miscibility in the He–H2 system at extreme P-T conditions. [ABSTRACT FROM AUTHOR]

If successfully developed, calorimetry at tens of GPa of pressure could help characterize phase transitions in materials such as high-pressure minerals, metals, and molecular solids. Here, we extend alternating-current calorimetry to 9 GPa and 300 K in a diamond anvil cell and use it to study phase transitions in H2O. In particular, water is loaded into the sample chambers of diamond-cells, along with thin metal heaters (1 µm-thick platinum or 20 nm-thick gold on a glass substrate) that drive high-frequency temperature oscillations (20 Hz to 600 kHz; 1 to 10 K). The heaters also act as thermometers via the third-harmonic technique, yielding calorimetric data on (1) heat conduction to the diamonds and (2) heat transport into substrate and sample. Using this method during temperature cycles from 300 to 200 K, we document melting, freezing, and proton ordering and disordering transitions of H2O at 0 to 9 GPa, and characterize changes in thermal conductivity and heat capacity across these transitions. The technique and analysis pave the way for calorimetry experiments on any non-metal at pressures up to ~100 GPa, provided a thin layer (several µm-thick) of thermal insulation supports a metallic thin-film (tens of nm thick) Joule-heater attached to low contact resistance leads inside the sample chamber of a diamond-cell. [ABSTRACT FROM AUTHOR]

Part I shows that quantitative measurements of heat capacity are theoretically possible inside diamond anvil cells via high-frequency Joule heating (100 kHz-10MHz), opening up the possibility of new methods to detect and characterize transformations at high-pressure such as the glass transitions, melting, magnetic orderings, and the onset of superconductivity. Here, we test the possibility outlined in Part I, using prototypes and detailed numerical models. First, a coupled electrical-thermal numerical model shows that specific heat of metals inside diamond cells can be measured directly using ~1MHz frequency, with <10% accuracy. Second, we test physical models of high-pressure experiments, i.e., diamond-cell mock-ups. Metal foils of 2-6 μm-thickness are clamped between glass insulation inside diamond anvil cells. Fitting data from 10 Hz to ~30 kHz, we infer the specific heat capacities of Fe, Pt, and Ni with ±20%-30% accuracy. The electrical test equipment generates -80 dBc spurious harmonics, which overwhelm the thermally induced harmonics at higher frequencies, disallowing the high precision expected from numerical models. An alternative Joule-heating calorimetry experiment, on the other hand, does allow absolute measurements with <10% accuracy, despite the -80 dBc spurious harmonics: the measurement of thermal effusivity, √ρck (ρ, c, and k being density, specific heat, and thermal conductivity), of the insulation surrounding a thin-film heater. Using a ~50 nm-thick Pt heater surrounded by glass and 10 Hz-300 kHz frequency, we measure thermal effusivity with ±6% accuracy inside the sample chamber of a diamond anvil cell. [ABSTRACT FROM AUTHOR]

Numerical simulations of heat transport in diamond anvil cells reveal a possibility for absolute measurements of specific heat via high-frequency modulation calorimetry. Such experiments could reveal and help characterize temperature-driven phase transitions at high-pressure, such as melting, the glass transition, magnetic and electric orderings, or superconducting transitions. Specifically, we show that calorimetric information of a sample cannot be directly extracted from measurements at frequencies slower than the timescale of conduction to the diamond anvils (10 s-100 s of kHz) since the experiment is far from adiabatic. At higher frequencies, laser-heating experiments allow relative calorimetric measurements, where changes in specific heat of the sample are discriminated from changes in other material properties by scanning the heating frequency from ~1 MHz to 1 GHz. But laser-heating generates large temperature gradients in metal samples, preventing absolute heat capacities to be inferred. High-frequency Joule heating, on the other hand, allows accurate, absolute specific heat measurements if it can be performed at high-enough frequency: assuming a thin layer of KBr insulation, the specific heat of a 5 μm-thick metal sample heated at 100 kHz, 1MHz, or 10MHz frequency would be measured with 30%, 8%, or 2% accuracy, respectively. [ABSTRACT FROM AUTHOR]

Many high-pressure high-temperature studies using laser-heated diamond cells have documented plateaus in the increase of temperature with increasing laser power or with time. By modeling heat transfer in typical laser-heated diamond anvil cell experiments, we demonstrate that latent heat due to melting or other phase transformation is unlikely to be the source of observed plateaus in any previously published studies, regardless of whether pulsed or continuous lasers were used. Rather, large increases (∼10-fold) in thermal conductivity can explain some of the plateaus, and modest increases in reflectivity (tens of percent) can explain any or all of them. Modeling also shows that the sub-microsecond timescale of heating employed in recent pulsed heating experiments is fast enough compared to heat transport into and through typical insulations, but too slow compared to heat transport into metallic laser absorbers themselves to allow the detection of a large plateau due to latent heat of fusion. Four new designs are suggested for future experiments that could use the simple observation of a latent heat-induced plateau to provide reliable high-pressure melting data. [ABSTRACT FROM AUTHOR]

We performed optical absorption and photoluminescence experiments under high pressure up to 10 GPa on two good quality InGaN epilayers with ∼40% indium. The pressure coefficient of about 30 meV/GPa for the absorption edge is close to the bandgap pressure coefficients of InN and GaN, indicating similar pressure dependence of the fundamental band gap in the whole composition range. In contrast, the pressure coefficient of the photoluminescence peak energy shows much weaker pressure dependence which we attribute to an increasing role of highly localized defects when the conduction band approaches the Fermi level stabilization energy at higher indium contents. [ABSTRACT FROM AUTHOR]