The present status of high-pressure research with the diamond anvil cell (DAC) is reviewed in this article, mainly from an experimental aspect. After a brief description of the different types of DAC's that are currently in vogue, the techniques used in conjunction with the DAC in modern high-pressure research are presented. These include techniques for low- and high-temperature studies, x-ray diffractometry, spectroscopy with the DAC, and other measurements. Results on selected materials, with a view to illustrating the physics behind high-pressure phenomena, are presented and discussed. These include metal-semiconductor transitions, electronic transitions, phonons and high-pressure lattice dynamics, and phase transitions. A whole section is devoted to the behavior of condensed gases, principally ${\mathrm{H}}_{2}$, ${\mathrm{D}}_{2}$, ${\mathrm{O}}_{2}$, ${\mathrm{N}}_{2}$, and rare-gas solids. The concluding section briefly deals with speculations on ultra-high-pressure research with the DAC in the future.

Diamond anvil cell and high-pressure physical investigations

We present a systematic and comparative study of the pressure-induced solidification of 11 frequently used pressure transmitting fluids using the ruby fluorescence technique in a diamond anvil cell. These fluids are 1 : 1 and 5 : 1 iso-n pentane, 4 : 1 deuterated methanol–ethanol, 16 : 3 : 1 deuterated methanol–ethanol-water, 1 : 1 FC84-FC87 Fluorinert, Daphne 7474, silicone oil, as well as nitrogen, neon, argon and helium. The data provide practical guidelines for the use of these fluids in high pressure experiments up to 50 GPa.

https://iopscience.iop.org/article/10.1088/0022-3727/42/7/075413/pdf

Hydrostatic limits of 11 pressure transmitting media

The behavior of a number of commonly used pressure media, including nitrogen, argon, 2-propanol, a 4:1 methanol–ethanol mixture, glycerol and various grades of silicone oil, has been examined by measuring the X-ray diffraction maxima from quartz single crystals loaded in a diamond-anvil cell with each of these pressure media in turn. In all cases, the onset of non-hydrostatic stresses within the medium is detectable as the broadening of the rocking curves of X-ray diffraction peaks from the single crystals. The onset of broadening of the rocking curves of quartz is detected at ∼9.8 GPa in a 4:1 mixture of methanol and ethanol and at ∼4.2 GPa in 2-propanol, essentially at the same pressures as the previously reported hydrostatic limits determined by other techniques. Gigahertz ultrasonic interferometry was also used to detect the onset of the glass transition in 4:1 methanol–ethanol and 16:3:1 methanol–ethanol–water, which were observed to support shear waves above ∼9.2 and ∼10.5 GPa, respectively, at 0.8–1.2 GHz. By contrast, peak broadening is first detected at ∼3 GPa in nitrogen, ∼1.9 GPa in argon, ∼1.4 GPa in glycerol and ∼0.9 GPa in various grades of silicone oil. These pressures, which are significantly lower than hydrostatic limits quoted in the literature, should be considered as the practical maximum limits to the hydrostatic behavior of these pressure media at room temperature.

Effective hydrostatic limits of pressure media for high-pressure crystallographic studies

The ruby luminescence method is widely used for pressure measurement in the diamond anvil cell and other optically transparent pressure cells. With this application in mind, we briefly review the ground-state physical properties of corundum (α-Al2O3) with some emphasis on its behavior under high pressure, survey the effects of temperature and stress on the R-line luminescence of ruby (Cr-doped corundum), and address the recent efforts towards an improved calibration of the R-line shift under hydrostatic pressures beyond the 50 GPa mark.

Ruby under pressure

Heterostructures can be assembled from atomically thin materials by combining a wide range of available van der Waals crystals, providing exciting possibilities for designer electronics1 In many cases, beyond simply realizing new material combinations, interlayer interactions lead to emergent electronic properties that are fundamentally distinct from those of the constituent layers2 A critical parameter in these structures is the interlayer coupling strength, but this is often not easy to determine and is typically considered to be a fixed property of the system Here we demonstrate that we can controllably tune the interlayer separation in van der Waals heterostructures using hydrostatic pressure, providing a dynamic way to modify their electronic properties In devices in which graphene is encapsulated in boron nitride and aligned with one of the encapsulating layers, we observe that increasing pressure produces a superlinear increase in the moire-superlattice-induced bandgap—nearly doubling within the studied range—together with an increase in the capacitive gate coupling to the active channel by as much as 25 per cent Comparison to theoretical modelling highlights the role of atomic-scale structural deformations and how this can be altered with pressure Our results demonstrate that combining hydrostatic pressure with controlled rotational order provides opportunities for dynamic band-structure engineering in van der Waals heterostructures For appropriately aligned layers of different two-dimensional materials, the separation between layers—and hence the interlayer coupling—is very sensitive to pressure, leading to pressure-induced changes in the electronic properties of the heterostructures

Dynamic band-structure tuning of graphene moiré superlattices with pressure

Recent work by Gupta and Shen [Appl. Phys Lett. 58, 583 (1991)] has shown that in a nonhydrostatic environment, the frequency of the ruby R2 line provides a reliable measure of the mean stress or pressure. When using the frequency of either the R1 or R2 line to measure pressure at nonambient temperature, it is necessary to know the temperature dependence of the line shift. Unfortunately, the shift of the R2 line with temperature has not been reported. The ruby R1 and R2 fluorescence shifts have been determined as a function of temperature from 15 to 600 K. Both can be fitted very well to the simple cubic forms R1(T) =14 423+4.49×10−2T−4.81×10−4T2+3.71×10−7T3 cm−1 and R2(T)=14 452 +3.00×10−2T−3.88×10−4T2+2.55×10−7T3 cm−1. From 300 to 600 K the shifts fit well to linear functions of temperature. In addition, it is found that the R1‐R2 splitting changes by about 3 cm−1 over the 600 K temperature range. Linewidths were found to vary both with temperature and from sample to sample.

Calibration of the ruby R1 and R2 fluorescence shifts as a function of temperature from 0 to 600 K

The pressure‐induced frequency shift of the Sm:YAG Y1 peak at elevated temperature is calibrated against the temperature‐corrected Raman shift of the nitrogen vibron and, at temperatures less than 673 K, the R1 shift of ruby. The results presented here indicate that pressure can be determined from the Y1 and Y2 peak frequencies, without temperature correction, from 6 to 820 K and from 1 bar to 25 GPa by using the equations: P(GPa) =−0.12204 (ωY1obs−16187.2) and P(GPa)=−0.15188 (ωY2obs−16232.2). However, pressure determinations based on Y2 are less accurate, especially at high temperature. At elevated temperature, the Sm:YAG Y1 and Y2 peak frequencies are most accurately determined by curve fitting a spectral window at least 400 cm−1 wide. The spectral range was chosen in order to include the decay of the intensity of the Lorentzian Y1 peak to a background value and incorporate a third peak at 16360 cm−1.

Comparison of the pressure‐induced frequency shift of Sm:YAG to the ruby and nitrogen vibron pressure scales from 6 to 820 K and 0 to 25 GPa and suggestions for use as a high‐temperature pressure calibrant

A single‐crystal gasketed diamond anvil cell of a new design for use on a diffractometer is described. It has achieved hydrostatic pressures of 50 kilobars as determined from the ruby fluorescence shift. The design combines several advantages. Nearly half the area of the Ewald sphere is available without having to remount the crystal. For reflecting planes nearly parallel to the diamond anvil faces, all reflections in the angular range ∼4°⩽ϑ⩽85° can be observed. Alignment of the diamonds, as well as loading and alignment of the sample crystals, is very simple and quick. The diffractometer geometry allows accurate measurements of weak reflections as well as accurate determinations of the x‐ray absorption corrections for the cell. The materials of construction are nontoxic except for one diamond mount, a small beryllium cylinder situated so that it is never touched, scraped, or rubbed. As a test problem, the z parameter of antimony has been found to increase linearly from z=0.23357 at 1 bar to z =0.2380±0.0...

50‐kilobar gasketed diamond anvil cell for single‐crystal x‐ray diffractometer use with the crystal structure of Sb up to 26 kilobars as a test problem

The usefulness of a silicone oil, Dow Corning 200, as a pressure medium in diamond anvil cells has been investigated. Common indicators of deviatoric stresses on ruby, such as changes in the R‐line widths and the R2‐R1 peak separation, show that this fluid does not deviate from hydrostaticity up to ∼15 GPa (150 kbar). The behavior of silicone is found to be very similar to the commonly used 4:1 methanol:ethanol mixture, while being much easier to use because of its higher viscosity. This ease of use and excellent performance makes silicone fluid a superior pressure medium.

Silicone fluid as a high-pressure medium in diamond anvil cells

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Calibration of the ruby R1 and R2 fluorescence shifts as a function of temperature from 0 to 600 K

Comparison of the pressure‐induced frequency shift of Sm:YAG to the ruby and nitrogen vibron pressure scales from 6 to 820 K and 0 to 25 GPa and suggestions for use as a high‐temperature pressure calibrant

50‐kilobar gasketed diamond anvil cell for single‐crystal x‐ray diffractometer use with the crystal structure of Sb up to 26 kilobars as a test problem

Silicone fluid as a high-pressure medium in diamond anvil cells