Abstract

High-pressure synthesis (which refers to pressure synthesis in the range of 1 to several GPa) adds a promising additional dimension for exploration of compounds that are inaccessible to traditional chemical methods and can lead to new industrially outstanding materials. It is nowadays a vast exciting field of industrial and academic research opening up new frontiers. In this context, an emerging and important methodology for the rapid exploration of composition-pressure-temperature-time space is the in situ method by synchrotron X-ray diffraction. This review introduces the latest advances of high-pressure devices that are adapted to X-ray diffraction in synchrotrons. It focuses particularly on the “large volume” presses (able to compress the volume above several mm3 to pressure higher than several GPa) designed for in situ exploration and that are suitable for discovering and scaling the stable or metastable compounds under “traditional” industrial pressure range (3–8 GPa). We illustrated the power of such methodology by (i) two classical examples of “reference” superhard high-pressure materials, diamond and cubic boron nitride c-BN; and (ii) recent successful in situ high-pressure syntheses of light-element compounds that allowed expanding the domain of possible application high-pressure materials toward solar optoelectronic and infra-red photonics. Finally, in the last section, we summarize some perspectives regarding the current challenges and future directions in which the field of in situ high-pressure synthesis in industrial pressure scale may have great breakthroughs in the next years.

Highlights

  • Achieving sustainable growth on a finite planet is a challenge of this century

  • That is why in this review, we aim to focus on recent examples of new light compounds synthesized recently under high pressure by the assistance of in situ X-ray diffraction with synchrotron radiation

  • If this principle is general, this type of device can fall into two main categories, according to the sample volume brought under high pressure: diamond anvil cells (DAC) and large volume devices

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Summary

Introduction

Achieving sustainable growth on a finite planet is a challenge of this century. The needs of societies are changing rapidly and the role of new smart materials in ensuring such transformations is paramount. One consists of exploring very high pressures beyond the industrial limits (P > 20 GPa) in order to reach significantly unusual solids (for example room temperature superconductor [21], or polymerization of CaC2 [22]) that would allow understanding the links between advanced properties and crystal structure/composition, which we will not consider in this paper Another methodological approach, more pragmatic but still promising, consists of the in situ exploration of “traditional” industrial pressure scale for the design of new stable or metastable compounds by playing with kinetics (e.g., for nanostructuring) and nucleation-growth mechanism for phase selection [23]. The materials syntheses described in our review principally concern (quasi-) hydrostatic synthesis conditions that allows producing well-crystallized powders and crystals (at high temperatures, melt or supercritical fluid form at each synthesis described)

Methods
Diamond Anvil Cell
Large Volume Devices
Multi-Anvil Devices
Adaptation of Multi-Anvil Devices to In Situ Synchrotron X-ray Diffraction
Paris–Edinburgh Press
Adaptation of Paris–Edinburgh Press to in Situ Synchrotron X-ray Diffraction
In Situ Large-Volume High-Pressure Syntheses
Diamond and c-BN
Boron-Rich
Magnesium Carbides
Silicon
Sodium Silicide Clathrates and Open-Framework Allotropes
10. Sequences
Findings
Current Challenges and Future Directions
Full Text
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