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Presented and discussed here is the implementation of a software solution that provides prompt X‐ray diffraction data analysis during fast dynamic compression experiments conducted within the dynamic diamond anvil cell technique. It includes efficient data collection, streaming of data and metadata to a high‐performance cluster (HPC), fast azimuthal data integration on the cluster, and tools for controlling the data processing steps and visualizing the data using the DIOPTAS software package. This data processing pipeline is invaluable for a great number of studies. The potential of the pipeline is illustrated with two examples of data collected on ammonia–water mixtures and multiphase mineral assemblies under high pressure. The pipeline is designed to be generic in nature and could be readily adapted to provide rapid feedback for many other X‐ray diffraction techniques, e.g. large‐volume press studies, in situ stress/strain studies, phase transformation studies, chemical reactions studied with high‐resolution diffraction etc. [ABSTRACT FROM AUTHOR]

In this study, we conduct extensive high‐pressure experiments to investigate phase stability in the cobalt‐nitrogen system. Through a combination of synthesis in a laser‐heated diamond anvil cell, first‐principles calculations, Raman spectroscopy, and single‐crystal X‐ray diffraction, we establish the stability fields of known high‐pressure phases, hexagonal NiAs‐type CoN, and marcasite‐type CoN2 within the pressure range of 50–90 GPa. We synthesize and characterize previously unknown nitrides, Co3N2, Pnma‐CoN and two polynitrides, CoN3 and CoN5, within the pressure range of 90–120 GPa. Both polynitrides exhibit novel types of polymeric nitrogen chains and networks. CoN3 feature branched‐type nitrogen trimers (N3) and CoN5 show π‐bonded nitrogen chain. As the nitrogen content in the cobalt nitride increases, the CoN6 polyhedral frameworks transit from face‐sharing (in CoN) to edge‐sharing (in CoN2 and CoN3), and finally to isolated (in CoN5). Our study provides insights into the intricate interplay between structure evolution, bonding arrangements, and high‐pressure synthesis in polynitrides, expanding the knowledge for the development of advanced energy materials [ABSTRACT FROM AUTHOR]

A natural intermediate member of the scapolite solid solution {Me47; chemical formula: (Na1.86Ca1.86K0.23Fe0.01)(Al4.36Si7.64)O24[Cl0.48(CO3)0.48(SO4)0.01]}, with the unusual I4/m space group, has been studied at various temperatures and combined high-T and high-P by means of in situ single-crystal and powder X-ray diffraction, using both conventional and synchrotron X-ray sources. In addition, single-crystal neutron diffraction data were collected at ambient-T and 685 °C. A fit of the experimental V-T data with a thermal equation of state yielded a thermal expansion coeficient at ambient conditions: αV25°C = 1/V0·(∂V/∂T)P,25°C = 1.74(3)·10–5 K–1. A comparative analysis of the elastic behavior of scapolite based on this study and previous high-T XRD data suggests that a thorough re-investigation of the diferent members of the marialite-meionite solid solution is needed to fully understand the role of crystal chemistry on the thermal behavior of these complex nonbinary solid solutions. The experimental data obtained within the full temperature range of analysis at ambient pressure confirm that the investigated sample always preserves the I4/m space group, and possible implications on the metastability of I4/m intermediate scapolite are discussed. Neutron difraction data show that no significant Si and Al rearrangement among the T sites occurs between 25 and 685 °C. The combined high-T and high-P data show that at 650 °C and between 10.30(5) and 10.71(5) GPa a phase transition toward a triclinic polymorph occurs, with a positive Clapeyron slope (i.e., dP/dT > 0). A comprehensive description of the atomic-scale structure deformation mechanisms induced by temperature and/or pressure, including those leading to structural instability, is provided based on single-crystal structure refinements. [ABSTRACT FROM AUTHOR]

The inorganic pyrocarbonate salt Na2[C2O5] crystallizes in the acentric, monoclinic space group P21 with Z = 2. It contains monovalent alkali metal cations together with isolated pyrocarbonate anions. The [C2O5]2−-groups consist of two planar [CO3]2−-groups which are slightly tilted with respect to each other around the bridging oxygen atom. Na2[C2O5] was synthesized in a laser-heated diamond anvil cell at 20(2) GPa by heating a mixture of Na2[CO3] + CO2 to ≈800(200) K. Its crystal structure was obtained by single crystal synchrotron X-ray diffraction and confirmed by density functional theory-based calculations in combination with Raman spectroscopy. Second harmonic generation measurements verified the acentric space group symmetry. The crystal structure is characterized by alternating layers of Na+-cations and [C2O5]2−-complex anions. [ABSTRACT FROM AUTHOR]

Shock‐induced transformations of quartz to high‐pressure polymorphs and diaplectic glass are decisive in identifying impact cratering events. Under shock compression, quartz can melt in local hot spots and crystallization of these silica melts under pressure can yield the high‐pressure mineral stishovite. A solid‐state transition to stishovite in relation to the formation of amorphous lamellae was already suggested in the late 1960s, but this idea was never comprehensively proven. Therefore, the mechanism responsible for such an intracrystalline stishovite formation is unknown to date. Herein, crystallographically oriented single crystals of quartz were compressed and decompressed in a membrane‐driven diamond anvil cell. These experiments aim at simulating the pressure paths of natural impacts on the timescale of seconds using compression rates between 0.2 and 0.6 GPa/s and peak pressures between 20 and 37 GPa. During the compression of quartz, the time‐resolved synchrotron X‐ray diffraction patterns reveal the almost simultaneous formation of two high‐pressure polymorphs, the recently identified rosiaite‐structured silica and stishovite. Transmission electron microscopic observations of recovered samples show that stishovite occurs as arrays of uniformly oriented nanometer‐sized crystals in amorphous intracrystalline lamellae. These observations indicate that the numerous stishovite crystals likely nucleated from the structurally similar rosiaite phase and thus inherited their uniform orientation during compression. During decompression, the metastable and non‐quenchable rosiaite‐structured phase collapsed to the amorphous stishovite‐containing lamellae. These findings attest to a novel mechanism of the formation of stishovite in the solid state and provide an explanation for similar microstructural occurrences of stishovite in impact‐metamorphic rocks and shocked meteorites. Plain Language Summary: The extreme pressures and temperatures of asteroid impacts on planetary surfaces result in irreversible changes in the affected rocks. The mineral quartz can then display characteristic amorphous lamellae and crystals of the high‐pressure mineral stishovite. While stishovite usually crystallizes from locally molten silica under pressure, its formation in the solid state free of silica melts has remained enigmatic to date. Here, we simulated asteroid impacts on the time scale of seconds and at ambient temperature through experiments of rapid compression and decompression of quartz. The crystallographic changes during the experiments and the microstructural observations of the recovered samples provide evidence that stishovite is indeed formed in the solid state during compression of quartz. In particular, a large number of stishovite crystals form in an identical crystallographic orientation through nucleation from the structurally similar rosiaite‐structured silica phase. The latter is formed metastably during compression. The final microstructure consists of the numerous stishovite crystals located in amorphous lamellae, because the metastable rosiaite‐structured phase transforms into amorphous silica during decompression. The discoveries describe a novel mechanism for rapid stishovite formation in the solid state, explaining very similar stishovite occurrences in meteorites and rock samples recovered from impact sites. Key Points: Stishovite can form in the solid state from compressed quartz through nucleation from a transient rosiaite‐structured silica phaseThe solid state transition from quartz to finally stishovite results in a uniform orientation relationshipShock‐metamorphic features in quartz can be mimicked by compression in the diamond anvil cell [ABSTRACT FROM AUTHOR]

This article discusses the discovery of cobalt polynitrides through high-pressure synthesis using laser-heated diamond anvil cells. The researchers found that the degree of nitrogen polymerization increased with increasing pressure. By utilizing single-crystal synchrotron X-ray diffraction and micro-Raman imaging spectroscopy, the crystal structures of these nitrides were elucidated. The study also suggests the possibility of recovering these materials under ambient conditions. The full research article provides more detailed information on the topic. [Extracted from the article]

The inorganic pyrocarbonate salt Na2[C2O5] crystallizes in the acentric, monoclinic space group P21 with Z = 2. It contains monovalent alkali metal cations together with isolated pyrocarbonate anions. The [C2O5]2−-groups consist of two planar [CO3]2−-groups which are slightly tilted with respect to each other around the bridging oxygen atom. Na2[C2O5] was synthesized in a laser-heated diamond anvil cell at 20(2) GPa by heating a mixture of Na2[CO3] + CO2 to ≈800(200) K. Its crystal structure was obtained by single crystal synchrotron X-ray diffraction and confirmed by density functional theory-based calculations in combination with Raman spectroscopy. Second harmonic generation measurements verified the acentric space group symmetry. The crystal structure is characterized by alternating layers of Na+-cations and [C2O5]2−-complex anions. [ABSTRACT FROM AUTHOR]

We have synthesized the first hydrous sp 3 -carbonate by laser-heating Ba[CO 3 ], CO 2 and H 2 O in a diamond anvil cell at 40(3) GPa. The crystal structure of Ba[H 4 C 4 O 10 ][H 3 C 4 O 10 ][H 2 CO 3 ][HCO 3 ] was determined by synchrotron single crystal X-ray diffraction. The experiments were complemented by DFT-based calculations. This compound is the first example of a carbonate containing both trigonally-coordinated carbon in [CO 3 ] 2- -groups and tetrahedrally coordinated carbon in [CO 4 ] 4- -groups. The [CO 4 ] 4- -groups polymerize by corner-sharing to form pyramidal [C 4 O 10 ] 4- -groups, which can bind three or four hydrogen atoms. As the pyramidal [C 4 O 10 ] 4- -groups are a constituent of several anhydrous sp 3 -carbonates, we now expect that further high-pressure hydrous carbonates can be obtained.

In this study, we conduct extensive high-pressure experiments to investigate phase stability in the cobalt-nitrogen system. Through a combination of synthesis in a laser-heated diamond anvil cell, first-principles calculations, Raman spectroscopy, and single-crystal X-ray diffraction, we establish the stability fields of known high-pressure phases, hexagonal NiAs-type CoN, and marcasite-type CoN 2 within the pressure range of 50-90 GPa. We synthesize and characterize previously unknown nitrides, Co 3 N 2 , Pnma-CoN and two polynitrides, CoN 3 and CoN 5 , within the pressure range of 90-120 GPa. Both polynitrides exhibit novel types of polymeric nitrogen chains and networks. CoN 3 feature branched-type nitrogen trimers (N 3 ) and CoN 5 show π-bonded nitrogen chain. As the nitrogen content in the cobalt nitride increases, the CoN 6 polyhedral frameworks transit from face-sharing (in CoN) to edge-sharing (in CoN 2 and CoN 3 ), and finally to isolated (in CoN 5 ). Our study provides insights into the intricate interplay between structure evolution, bonding arrangements, and high-pressure synthesis in polynitrides, expanding the knowledge for the development of advanced energy materials., (© 2024 Wiley-VCH GmbH.)