Watching solids crystallise using in situ powder diffraction

The sections in this article are


Introduction
Pressure-Driven Phase Transitions
Framework Flexion
Increase in Coordination Number
Pressure-Induced Ordering


Generating High Pressure
Dynamic Pressure Generation
Static Pressure Devices
Large-Volume Presses
Diamond Anvil Cells




Probing Phase Transformations in Materials at High Pressure
Volumetric Techniques
Spectroscopic Techniques
Microscopy
Raman and Infrared Spectroscopy
Mossbauer Spectroscopy
X-Ray Absorption Spectroscopy
NMR


Ultrasonic Sound Velocity
Diffraction Techniques
X-Ray Diffraction
Neutron Diffraction




Examples
Zincblende-Type Semiconductors
Si and Ge
GaAs
InSb


Materials in the B–C–N System
C
BN
CN
BC
BCN


H2O
Ice Ih, XI and Ic
Ice II
Ice III and Ice IX
Ice V, Ice IV and Ice XII
Ice VI, Ice VII, Ice VIII, Ice X
Amorphous Ice at High Pressure




Acknowledgements

High Pressure Phase Transformations

Among binary compounds, there is a high potential for discovery of novel members (polymorphic phases or compounds) of the nitrides of transition metals group due to a pronounced dependence of the oxidation state of the metals (M) on pressure. The power of high pressure–high temperature (HP-HT) route for synthesis of binary nitrides has already been demonstrated by the discovery of cubic nitrides of the group 4 and 14 elements, of crystalline polymorphs of P3N5, and by reports on formation of four noble metal nitrides. It is anticipated that such HP products exhibit, in addition to enhanced elastic and mechanical behavior, other functional properties making them interesting for industrial applications. Here, HP–HT synthesis research is extended to nitrides of group 5 elements, resulting in the discovery of a novel hard tantalum nitride, exhibiting U2S3 structure: η-Ta2N3 (Pbnm, a = 8.1911(17) A, b = 8.1830(17) A, c = 2.9823(3) A). The stoichiometry is supported by two independent means, verifying that η-Ta2N3 is the first thermodynamically stable transition metal nitride with a N:M ratio exceeding 4:3. Due to its high hardness and peculiar texture (needle-like and granular crystallites), η-Ta2N3 may find practical applications as a hard fracture resistant material.

High-Pressure Synthesis of Tantalum Nitride Having Orthorhombic U2S3 Structure

The combination of synchrotron x-ray facilities with high-pressure methods provides new experimental tools for addressing geophysical problems relevant to understanding the interior of the Earth and other planets. Among the important geophysical questions related to the Earth’s silicate mantle are the origin of seismic discontinuities in the upper mantle, the rheological properties of mantle minerals and their influence on dynamic flow in the Earth, and the nature of the core–mantle boundary region. In the case of the Earth’s core, key questions are centred on the identity of the light elements of the core and their effect on energetics and thermodynamic properties, the melting curve of iron and its alloys and the origin of seismic anisotropy in the inner core. Both new and established high-pressure synchrotron methods applied to the diamond anvil cell and large-volume apparatus are surveyed. Advances in synchrotron capabilities have been accompanied by new innovations in high-pressure technology. X-ray diffraction techniques are mature but continued improvements are leading to expanded pressure–temperature coverage and better ability to recover crystallographic details. Diffraction and absorption studies of the properties of liquids of silicate and iron alloy composition have expanded in response to new capabilities. Recently, methods for inelastic scattering and nuclear resonance probes have been developed at high pressures and these provide constraints on vibrational, electronic and magnetic properties, which were previously unattainable. (Some figures in this article are in colour only in the electronic version)

http://iopscience.iop.org/article/10.1088/0034-4885/68/8/R03/pdf

Synchrotron facilities and the study of the Earth's deep interior

Elasticity of Polycrystalline Pyrope (Mg3Al2Si3O12) to 9 GPa and 1000°C

▪ Abstract Increased access to multi-anvil high-pressure devices interfaced to synchrotron X-ray radiation sources has led to a new class of experiments. These new capabilities include (a) high-precision crystal structure determination and refinement from powder X-ray diffraction data; (b) the determination of kinetic parameters and structure from time-resolved diffraction data; (c) the determination of absolute pressures by the combined use of ultrasonic techniques at high pressures and temperatures with simultaneous monitoring of X-ray diffraction; and (d) the determination of the strength and rheological properties of materials through the monitoring of the relaxation of broadened diffraction peak widths in the presence of a well-characterized deviatoric stress field generated in the multi-anvil high-pressure apparatus.

In situ studies of the properties of materials under high-pressure and temperature conditions using multi-anvil apparatus and synchrotron x-rays

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In situ studies of the properties of materials under high-pressure and temperature conditions using multi-anvil apparatus and synchrotron x-rays