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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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At least 19 records
All sourcesNASA NTRSDOE OSTI
NASA NTRS1994

Volatiles in the deep Earth: An experimental study using the laser-heated diamond cell

Experiments with the laser-heated diamond cell show that H2O and CO2 can be stabilized within crystalline mineral structures of the lower-mantle, and hence can be present at relatively non-volatile components of the Earth's deep interior. Samples quenched from high pressures and temperatures document that the MgCO3-FeCO3 magnesite-siderite solid-solution is stable and coexists with (Mg,Fe)SiO3 perovskite at 30-40 GPa and approximately 1500-2000 K. In contrast, H2O combines with the silicate to form (Mg,Fe)SiH2O4 phase D, coexisting with (Mg,Fe)SiO3 perovskite at these conditions. If enough water is present, phase D can become the predominant phase in the MgSiO3-H2O system at lower-mantle conditions. Our work extends previous studies to Fe-bearing compositions and to the pressures of the mid-lower mantle. Thus, the results of high-pressure experiments suggest that both H2O and CO2 can be abundant in the Earth's lower mantle, being present in stable hydroxisilicate and carbonate phases.

Li, Xiaoyuan↗
DOE OSTI2026

A simple wire-coil resistive heater for high temperature radial x-ray diffraction in a diamond anvil cell

Diamond anvil cells are commonly used at synchrotron x-ray diffraction beamlines to study structural and thermoelastic properties of materials at high pressures. In a radial geometry, where the x-ray probe is oriented perpendicular to the axis of force, the deformation and strength of materials can be measured in situ. Because the anelastic and failure properties of materials depend strongly on temperature, many applications would benefit from the ability to measure high pressure radial diffraction in elevated and accurately controlled thermal environments. Previous work to introduce high temperature to radial diamond anvil cells has been largely limited to laser heating, with relatively scant efforts to resistively heat the sample. Here, we report a relatively straightforward adaptation of a simple wire coil heater, with in situ high-temperature radial diffraction performed on tungsten carbide up to 573 K at beamline 12.2.2 of the Advanced Light Source. In conclusion, the results demonstrate that the differential stress supported by WC decreases with increasing temperature: the differential stress on the basal (001) and pyramidal (101) planes decreased 6.6% and 5.5%, respectively, while the (100) plane only saw a 2.7% decrease, in agreement with previous studies.

Diamond anvil cells↗
NASA NTRS1984

Experiments at high temperature and pressure - Laser heating through the diamond cell

CW laser heating through a diamond anvil cell by means of a focused Nd:YAG laser has resulted in the achievement of temperatures in the 1500-5000 K range for pressures of 10-100 GPa. Temperatures are determined radiometrically, with an accuracy of about 200 K, and temperature variation across the laser-heated spot is derived by means of spatial filtering with a slit that can be scanned. Melting temperatures are thus determined either on the basis of observed temperature at the liquid-solid interface or on that of the peak temperature at which glass is first produced with increasing laser power.

Jeanloz, R.↗
DOE OSTI2022

Melting diamond in the diamond cell by laser-flash heating

The phase behavior of carbon at high pressure and the search for carbon structures denser than diamond has been explored for decades showing large discrepancies, with many fundamental questions remaining unresolved. Here we show evidence of melting above the graphite-diamond-liquid (GDL) triple point (~13 GPa, 4000 K) up to 50 GPa on samples recovered from single flash-heating events using spectroscopic and electron microscopic methods. The results show that for all pressures, diamond melts below the triple point temperature contradicting previous studies, most of which predict a positive slope of the melting curve.

36 MATERIALS SCIENCE↗
NASA NTRS1987

Melting of troilite at high pressure in a diamond cell by laser heating

A system for measuring melting temperatures at high pressures is described. The sample is heated with radiation from a YAG laser. The beam is reflected downward through a microscope objective, through the upper diamond anvil, and focused onto the sample. Hense, intense heating is produced only at the sample and not within the diamond anvils. A vidicon system is used to observe the sample during heating. Incandescent light from the heated sample passes back through the objective lens into a grating spectrometer. The spectrum of the incandescent light is received by the photodiode array and stored in the multichannel analyzer. These data can then be transferred to floppy disk for analysis. A curve fitting program is used to compare the spectra with standard blackbody curves and to determine the temperature. Pressure is measured by the ruby fluorescence method. The system was used to study the melting behavior of natural troilite (FeS).

Bassett, William A.↗
DOE OSTI2024

A miniature multi-anvil apparatus using diamond as anvils—MDAC: Multi-axis diamond anvil cell

The diamond anvil cell (DAC) has been widely used in high-pressure research. Despite significant progress over the past five decades, the opposed anvil geometry in the DAC inevitably leads to a disk-shaped sample configuration at high pressure. This intrinsic limitation is largely responsible for the large pressure and temperature gradients in the DAC, which often compromise precise experiments and their characterizations. Here, we designed and fabricated a multi-axis diamond anvil cell (MDAC) by adopting the concept of a multi-anvil apparatus but using single crystal diamonds as the anvil material. Preliminary data show that the MDAC can generate extreme pressure conditions above 100 GPa. The advantages of the MDAC over a traditional opposed anvil DAC include thicker, voluminous samples, quasi-hydrostatic, or designed deviatoric stress conditions, and multidirectional access windows for optical applications and x-ray probes. In this article, we present the design and performance of a prototype MDAC, as well as the application prospects in high-pressure research.

47 OTHER INSTRUMENTATION↗
DOE OSTI2023

Development of Large-Volume-Diamond Anvil Cell for Neutron Diffraction: The Neutron Diamond Anvil Cell Project at ORNL

10 years ago, Dave Mao, director of EFree (energy frontier research in extreme environments), a DOE energy frontier recognized the importance of neutron science for energy research. The subsequent establishment of a neutron group within EFree lead to the establishment of an “Instrument Development Team” for SNAP, the High-Pressure beamline at the Spallation Neutron Source at Oak Ridge National Laboratory in Tennessee. The idea was to develop novel high pressure techniques to expand the pressure range for neutron diffraction. A goal was set to reach half megabar levels (50 GPa), which at the time was considered as extremely challenging. Here we will give a brief overview of the developments during the last decade in this novel area of research. Fortunately, during this period multi carat diamond anvils have become available mainly by the chemical vapor deposition process (CVD), making research in this pressure range and beyond rather routine. This paper shows the latest developments in large anvil designs, compact multiple ton diamond cells and some examples of high-quality neutron diffraction patterns of sample sizes far below conventional levels.

Boehler, Reinhard↗
DOE OSTI2023

MHz free electron laser x-ray diffraction and modeling of pulsed laser heated diamond anvil cell

A new diamond anvil cell experimental approach has been implemented at the European x-ray Free Electron Laser, combining pulsed laser heating with MHz x-ray diffraction. In this report we use this setup to determine liquidus temperatures under extreme conditions, based on the determination of time-resolved crystallization. The focus is on a Fe-Si-O ternary system, relevant for planetary cores. This time-resolved diagnostic is complemented by a finite-element model, reproducing temporal temperature profiles measured experimentally using streaked optical pyrometry. This model calculates the temperature and strain fields by including (i) pressure and temperature dependencies of material properties, and (ii) the heat-induced thermal stress, including feedback effect on material parameter variations. Making our model more realistic, these improvements are critical as they give 7000 K temperature differences compared to previous models. Laser intensities are determined by seeking minimal deviation between measured and modeled temperatures. Combining models and streak optical pyrometry data extends temperature determination below detection limit. The presented approach can be used to infer the liquidus temperature by the appearance of SiO 2 diffraction spots. In addition, temperatures obtained by the model agree with crystallization temperatures reported for Fe–Si alloys. Our model reproduces the planetary relevant experimental conditions, providing temperature, pressure, and volume conditions. Those predictions are then used to determine liquidus temperatures at experimental timescales where chemical migration is limited. This synergy of novel time-resolved experiments and finite-element modeling pushes further the interpretation capabilities in diamond anvil cell experiments.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Cinema:Snap: Real-time tools for analysis of dynamic diamond anvil cell experiment data

We report we developed tools and a workflow for real-time analysis of data from dynamic diamond anvil cell experiments performed at user light sources. These tools allow users to determine the phases of matter observed during the compression of materials in order to make decisions during an experiment to improve the quality of experimental results and maximize the use of scarce experimental facility time. The tools fill a gap in dynamic compression data analysis tools that are real-time, are flexible to the needs of high-pressure scientists, connect to automated processing of results, can be easily incorporated into workflows with existing tools and data formats, and support remote experimental data analysis workflows. Specific analytics developed include novel automated two-peak analysis for overlapping peaks and multiple phases, coordinated views of pressure and temperature values, full-compression contour plots, and configurable views of integrated x-ray diffraction. We present an experimental use case to show how the tools produce real-time analytics that help the scientists revise parameters for the next compression

47 OTHER INSTRUMENTATION↗
DOE OSTI2021

Phase transformations, microstructural refinement and defect evolution mechanisms in Al-Si alloys under non-hydrostatic diamond anvil cell compression

Non-hydrostatic compression of materials using a diamond anvil cell (DAC) can transform equilibrium microstructure of an alloy to novel, potentially metastable states. In this study, in situ synchrotron X-ray diffraction (XRD) during compression up to 24 GPa and subsequent ex situ, high resolution analytical electron microscopy (AEM) after decompression of an Al-Si alloy provided insight into the crystallographic changes during the compression as well as microstructural refinement, and defect structures caused by such a high pressure compression-decompression process. Pressure resolved in-situ synchrotron XRD was used to detail the phase transformation pathway of the eutectic Si phase in Al-Si alloy, from Si-I → Si-XI → Si-V during compression, and a final transformation predominantly to Si-III after decompression. Using scanning and transmission electron microscopy (S/TEM), site specific analysis of the alloy immediately underneath the anvil contact surface demonstrated a highly complex microstructure. A narrow region of thick amorphous Al oxide interspersed with nanocrystalline grains was found at the top surface. Underneath this Al oxide, while the majority the eutectic Si was transformed into highly-deformed, polycrystalline (PC) Si-III, a complex intermediate layer was discovered at the interface between Al and Si, comprised of a small fraction of Al nanocrystals and a majority of nanocrystalline Si-I. This combination of pressure resolved in-situ synchrotron XRD coupled with subsequent high resolution, electron microscopy resolved the phase transformation as well as non-equilibrium microstructures in a metallic alloy induced by a non-hydrostatic high pressure compression followed by decompression.

36 MATERIALS SCIENCE↗
DOE OSTI2026

Design of a double-sided laser heating compatible piezoelectrically driven dynamic diamond anvil cell

Piezoelectrically driven dynamic diamond anvil cells are generally limited to use at room temperature due to spatial conflicts with the optical components necessary for double-sided laser heating. Here, this work describes the design of a double-sided laser-heating-compatible, piezoelectrically driven dynamic diamond anvil cell (LH-dDAC) that expands the range of experimentally accessible compression rate/temperature space. By developing a spatially in-parallel design, in which the diamond anvils and the piezo actuators lie alongside each other, the total length of the apparatus is reduced to 66.5 mm. The new LH-dDAC is capable of probing both overpressure and compression-rate effects on the kinetics of phase transitions. We illustrate the capability of the new LH-dDAC using the following cases: (1) a simultaneous pressure and temperature jump from 19.5 GPa and room temperature to 40 GPa and ≈1550 K and (2) a controlled compression ramp at ≈1850 K and ≈100 GPa/s. By pairing rapid compression with laser heating, the new LH-dDAC opens the door to studies of diffusionally controlled transformations at high pressures and temperatures.

Copley, J. A. [Princeton Univ., NJ (United States)↗
DOE OSTI2026

Hyperspectral radiance mapping and chromatic correction for temperature measurement in laser-heated diamond anvil cells

In laser-heated diamond anvil cell (DAC) experiments, the effective heated region typically decreases in size with increasing pressure, leading to steeper thermal gradients. Under these conditions, chromatic aberration in the optical path from sample to detector can significantly create bias in spectro-radiometric temperature measurement. We present a radiance-mapping approach using a hyperspectral camera that records 25 spectral channels spanning 605–875 nm at each pixel in a single exposure, providing spatially and spectrally resolved radiance in each frame. This enables chromatic effects to be recorded and corrected in data processing. We developed a procedure for hyperspectral mapping, involving per-camera calibration, crosstalk removal, measured spectral throughput functions, and optional sub-pixel co-registration to minimize chromatic distortion. The calibrated radiance maps are then used to derive temperature maps of the laser-heated hotspots. For smaller heating spots, the radiance mapping approach reveals chromatic shifts that conventional spectro-radiometric methods cannot quantify. Ambient-pressure heating experiments confirm accurate temperature retrieval. At high pressure, application of the hyperspectral system to a platinum-heating experiment at 12 GPa demonstrates stable temperature reconstruction under steep thermal gradients. Beyond mitigating chromatic aberrations, the ability to diagnose optical artifacts separately from emissivity variations during controlled test experiments or in situ suggests a path toward more rigorous spectral emissivity analysis and improved modeling of thermal transport in laser-heated DAC experiments.

47 OTHER INSTRUMENTATION↗
NASA NTRS1986

Resistance heating of Fe and W in diamond-anvil cells

A new method for internally heating a diamond-anvil cell is described. Fine wires of iron or tungsten are resistively heated in a gasketed cell, thus providing a uniformly distributed pressure that can be measured in situ by employing the ruby scale. Temperatures of several thousand degrees have been measured by fitting a black body radiation function to the spectrum of the hot wire taken with an optical multichannel analyzer. Temperatures as high as the melting temperature of tungsten have been achieved. The alpha-gamma and alpha-epsilon phase transitions of iron have been studied, and the results show excellent agreement with previous data obtained with piston-cylinder or externally-heated diamond cells.

Boehler, R.↗
DOE OSTI2023

A MHz X-ray diffraction set-up for dynamic compression experiments in the diamond anvil cell

An experimental platform for dynamic diamond anvil cell (dDAC) research has been developed at the High Energy Density (HED) Instrument at the European X-ray Free Electron Laser (European XFEL). Advantage was taken of the high repetition rate of the European XFEL (up to 4.5 MHz) to collect pulse-resolved MHz X-ray diffraction data from samples as they are dynamically compressed at intermediate strain rates (≤10 3 s −1 ), where up to 352 diffraction images can be collected from a single pulse train. The set-up employs piezo-driven dDACs capable of compressing samples in ≥340 µs, compatible with the maximum length of the pulse train (550 µs). Results from rapid compression experiments on a wide range of sample systems with different X-ray scattering powers are presented. A maximum compression rate of 87 TPa s −1 was observed during the fast compression of Au, while a strain rate of ∼1100 s −1 was achieved during the rapid compression of N 2 at 23 TPa s −1 .

73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗
DOE OSTI2024

Phase transition kinetics revealed by in situ x-ray diffraction in laser-heated dynamic diamond anvil cells

We report successful coupling of dynamic loading in a diamond anvil cell and stable laser heating, which enables compression rates up to 500 GPa/s along high-temperature isotherms. Dynamic loading in a diamond-anvil cell allows exploration of a wider range of pathways in the pressure-temperature space compared to conventional dynamic compression techniques. By x-ray diffraction, we are able to characterize and monitor the structural transitions with the appropriate time resolution i.e., millisecond timescales. Using this method, we investigate the γ − ε phase transition of iron under dynamic compression, reaching compression rates of hundreds of GPa/s and temperatures of 2000 K. Our results demonstrate a distinct response of the γ − ε and α − ε transitions to the high compression rates achieved, possibly due to the different transition mechanisms. These findings open up new avenues to study tailored dynamic compression pathways in the pressure-temperature space and highlight the potential of this platform to capture kinetic effects (over ms time scales) in a diamond anvil cell. Published by the American Physical Society 2024

Ricks, Matthew (ORCID:000000015315612X)↗