In the past couple of decades, the laser-heated diamond anvil cell (combined with in situ techniques) has become an extensively used tool for studying pressure-temperature-induced evolution of various physical (and chemical) properties of materials. In this review, the general challenges associated with the use of the laser-heated diamond anvil cells are discussed together with the recent progress in the use of this tool combined with synchrotron X-ray diffraction and absorption spectroscopy.

As the main constituent of planetary cores, pure iron phase diagram under high pressure and temperature is of fundamental importance in geophysics and planetary science. However, previously reported iron‐melting curves show large discrepancies (up to 1000 K at the Earth's core–mantle boundary, 136 GPa), resulting in persisting high uncertainties on the solid‐liquid phase boundary. Here we unambiguously show that the observed differences commonly attributed to the nature of the used melting diagnostic are due to a carbon contamination of the sample as well as pressure overestimation at high temperature. The high melting temperature of pure iron under core‐mantle boundary (4250 ± 250 K), here determined by X‐ray absorption experiments at the Fe K‐edge, indicates that volatile light elements such as sulfur, carbon, or hydrogen are required to lower the crystallization temperature of the Earth's liquid outer core in order to prevent extended melting of the surrounding silicate mantle.

Nickel is the second most abundant element in the Earth's core. However, the properties of Fe‐Ni alloys are still poorly constrained under planetary cores conditions, in particular concerning the effect of Ni on the melting curve of Fe. Here we show that Ni alloying up to 36 wt% does not affect the melting curve of Fe up to 100 GPa. However, Ni strongly modifies the hexagonal‐closed‐packed/face‐centered‐cubic (hcp/fcc) phase boundary, pushing the hcp/fcc/liquid triple point of Fe‐20wt%Ni to higher pressures and temperatures. Our results allow constraining the triple point for Fe‐10wt%Ni, a composition relevant for the Earth interior, and point out a decrease of the melting temperature at core‐mantle boundary by 400 K with respect to pure Fe. A lower amount of light elements than previously predicted is thus required to reduce the crystallization temperature of core materials below that of a peridotitic lower mantle, in better agreement with geochemical observations.

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.

Recent experiments have demonstrated the existence of previously unknown iron oxides at high pressure and temperature including newly discovered pyrite‐type FeO₂ and FeO₂H_x phases stable at deep terrestrial lower mantle pressures and temperatures. In the present study, we probed the iron oxidation state in high‐pressure transformation products of Fe³⁺OOH goethite by in situ X‐ray absorption spectroscopy in laser‐heated diamond‐anvil cell. At pressures and temperatures of ~91 GPa and 1,500–2,350 K, respectively, that is, in the previously reported stability field of FeO₂H_x, a measured shift of −3.3 ± 0.1 eV of the Fe K‐edge demonstrates that iron has turned from Fe³⁺ to Fe²⁺. We interpret this reductive valence change of iron by a concomitant oxidation of oxygen atoms from O²⁻ to O⁻, in agreement with previous suggestions based on the structures of pyrite‐type FeO₂ and FeO₂H_x phases. Such peculiar chemistry could drastically change our view of crystal chemistry in deep planetary interiors.