Viscosity measurements in the diamond anvil pressure cell

The viscosity of liquids can be measured in the diamond-anvil pressure cell utilizing a falling-solid sphere method and the ruby technique for pressure measurement. The pressure dependence of the viscosity of a 4:1 mixture (by volume) of methanol-ethanol was determined to 70 kilobars. The accuracy of the method is estimated from measurements made on a fluid of known viscosity.     

Manometer extension for high pressure measurement: nuclear quadrupole resonance study of Cu2O with a modified Bridgman anvil cell up to 10 GPa

We report (63)Cu nuclear quadrupole resonance (NQR) measurement of Cu(2)O under pressure up to about 10 GPa at low temperatures. Because the lattice parameter of Cu(2)O changes with increasing pressure, the electric field gradient at the Cu site also changes correspondingly with pressure. This enables us to use the Cu(2)O as an in situ manometer for high pressure nuclear magnetic resonance/NQR up to about 9 GPa.     

Simple adaptation of the Bridgman high pressure technique for use with liquid media

We present a simple novel technique to adapt a standard Bridgman cell for the use of a liquid pressure transmitting medium. The technique has been implemented in a compact cell, able to fit in a commercial Quantum Design PPMS system, and would also be easily adaptable to extreme conditions of very low temperatures or high magnetic fields. Several media have been tested and a mix of fluorinert FC84:FC87 has been shown to produce a considerable improvement over the pressure conditions in the standard steatite solid medium, while allowing a relatively easy setup procedure. For optimized hydrostatic conditions, the success rate is about 80% and the maximum pressure achieved so far is 7.1 GPa. Results are shown for the heavy fermion system YbAl(3) and for NaV(6)O(15), an insulator showing charge order.     

Density measurements of noncrystalline materials at high pressure with diamond anvil cell

We describe an x-ray absorption method for in situ density measurement of non-crystalline materials in the diamond anvil cell using a monochromatic synchrotron x-ray microbeam. Sample thickness, which is indispensable in the absorption method, can be determined precisely by extrapolating the thickness profile of the gasket obtained by x-ray absorption and diffraction measurements. Diamond deformation across the sample chamber becomes noticeable at high pressures above 10 GPa, which can be monitored with a precision better than 1%, as demonstrated by measurements on crystalline Ag. We have applied the developed method to measure densities of the classic network-forming GeO(2) glass in octahedral form at pressures up to 56 GPa. The fit to the pressure-volume data with the Birch-Murnaghan equation from 13 to 56 GPa gives parameters of V(0)=23.2+/-0.4 cm(3)mol and K=35.8+/-3.0 GPa, assuming that K(')=4. This method could be applicable for in situ determination of the density of liquids and other noncrystalline materials using a diamond anvil cell up to ultrahigh pressures.     

In situ Hall effect measurement on diamond anvil cell under high pressure

A method for in situ Hall effect measurement under high pressure was developed on a diamond anvil cell. The electrode was accurately integrated on one diamond anvil with regular shape. A uniform and strong magnetic field was introduced into the sample zone. The voltage errors brought by some negative effects during the measurement were well eliminated. The correction factor of the Hall coefficient, brought by the nonpoint contact between the electrode and the sample, was 4.51%. The measurement error of the magnetic field did not exceed 1%. The carrier character of ZnTe powders was studied up to 23 GPa. The evolution of conductivity with pressure was explained based on the variation of the carrier behavior.     

An induction heating diamond anvil cell for high pressure and temperature micro-Raman spectroscopic measurements

A new external heating configuration is presented for high-temperature diamond anvil cell instruments. The supporting rockers are thermally excited by induction from an externally mounted copper coil passing a 30 kHz alternating current. The inductive heating configuration therefore avoids the use of breakable wires, yet is capable of cell temperatures of 1100 K or higher. The diamond anvil cell has no resistive heaters, but uses a single-turn induction coil for elevating the temperature. The induction coil is placed near the diamonds and directly heats the tungsten carbide rockers that support the diamond. The temperature in the cell is determined from a temperature-power curve calibrated by the ratio between the intensities of the Stokes and anti-Stokes Raman lines of silicon. The high-pressure transformation of quartz to coesite is successfully observed by micro-Raman spectroscopy using this apparatus. The induction heating diamond anvil cell is thus a useful alternative to resistively heated diamond anvil cells.     

Preparation of W-Ta thin-film thermocouple on diamond anvil cell for in-situ temperature measurement under high pressure

In this paper, a W-Ta thin-film thermocouple has been integrated on a diamond anvil cell by thin-film deposition and photolithography methods. The thermocouple was calibrated and its thermal electromotive force was studied under high pressure. The results indicate that the thermal electromotive force of the thermocouple exhibits a linear relationship with temperature and is not associated with pressure. The resistivity measurement of ZnS powders under high pressure at different temperatures shows that the phase transition pressure decreases as the temperature increases.     

Thickness measurement of sample in diamond anvil cell

We report on an original method that measures sample thickness in a diamond anvil cell under high pressures. The method is based on two hypotheses: completely plastic deformation on the gasket and completely elastic deformation of the diamonds. This method can further eliminate the effect of diamond deformation on the thickness measurement of a sample, which permits us to measure the thickness of alumina up to 41.4 GPa.     

X-ray diffraction in the pulsed laser heated diamond anvil cell

We have developed in situ x-ray synchrotron diffraction measurements of samples heated by a pulsed laser in the diamond anvil cell at pressure up to 60 GPa. We used an electronically modulated 2-10 kHz repetition rate, 1064-1075 nm fiber laser with 1-100 μs pulse width synchronized with a gated x-ray detector (Pilatus) and time-resolved radiometric temperature measurements. This enables the time domain measurements as a function of temperature in a microsecond time scale (averaged over many events, typically more than 10,000). X-ray diffraction data, temperature measurements, and finite element calculations with realistic geometric and thermochemical parameters show that in the present experimental configuration, samples 4 μm thick can be continuously temperature monitored (up to 3000 K in our experiments) with the same level of axial and radial temperature uniformities as with continuous heating. We find that this novel technique offers a new and convenient way of fine tuning the maximum sample temperature by changing the pulse width of the laser. This delicate control, which may also prevent chemical reactivity and diffusion, enables accurate measurement of melting curves, phase changes, and thermal equations of state.     

Uniform stress conditions in the diamond anvil cell at 200 kilobars

Pressure gradients in a diamond anvil cell have been measured with a 4:1 methanol:ethanol mixture as a pressure medium up to 350 kilobars. When pressure is applied rapidly, stress gradients are shown to be negligible up to 200 kilobars and probably above. With this procedure it is possible to significantly increase the precision of pressure measurements above 100 kilobars.     

Adaption of a diamond anvil cell to an automatic four-circle diffractometer for x-ray diffraction

A diamond anvil high-pressure device for x-ray diffraction on single crystals under hydrostatic pressures up to about 100 kilobars has been adapted to the automatic four-circle x-ray diffractometer Philips PW 1100. The mechanical adaption, the centering procedure, and quick pressure calibration on the diffractometer are described. Hints to improve the peak-to-background ratio of the intensity measurements are given.     

An in situ approach to study trace element partitioning in the laser heated diamond anvil cell

Data on partitioning behavior of elements between different phases at in situ conditions are crucial for the understanding of element mobility especially for geochemical studies. Here, we present results of in situ partitioning of trace elements (Zr, Pd, and Ru) between silicate and iron melts, up to 50 GPa and 4200 K, using a modified laser heated diamond anvil cell (DAC). This new experimental set up allows simultaneous collection of x-ray fluorescence (XRF) and x-ray diffraction (XRD) data as a function of time using the high pressure beamline ID27 (ESRF, France). The technique enables the simultaneous detection of sample melting based to the appearance of diffuse scattering in the XRD pattern, characteristic of the structure factor of liquids, and measurements of elemental partitioning of the sample using XRF, before, during and after laser heating in the DAC. We were able to detect elements concentrations as low as a few ppm level (2-5 ppm) on standard solutions. In situ measurements are complimented by mapping of the chemical partitions of the trace elements after laser heating on the quenched samples to constrain the partitioning data. Our first results indicate a strong partitioning of Pd and Ru into the metallic phase, while Zr remains clearly incompatible with iron. This novel approach extends the pressure and temperature range of partitioning experiments derived from quenched samples from the large volume presses and could bring new insight to the early history of Earth.     

Determination of the thickness of a gasket in a diamond anvil high-pressure cell

A method for determining the thickness of a gasket in a diamond anvil high-pressure cell is described. This method is based on measuring the relative position of the anvils. The gasket thickness is determined by measuring the distance between two marks, viz., virtual points “locked” to side surfaces of the anvils. The distance between the marks is determined by digital processing of microphotographs. The error of measuring the gasket thickness disregarding the deformations of the anvils is ∼1 μm. The results of measuring the gasket thickness, the aperture area, and the optical length between the working planes of the anvils for a helium-filled cell are presented. The pressure dependences of the refractive index and the volume of helium, which is compressed to a pressure of 16 GPa, that are calculated using these data are in good agreement with the published data.     

Adaptation of spherical and cylindrical vessels to variable internal pressure and temperature

The kinematic theorem is applied to solve some problems of shakedown of spherical and cylindrical vessels subjected to variable internal pressure and temperature, taking into account the temperature dependence of the yield stress.     

New method for measuring electrical conductivities of solids in a diamond anvil cell

A new method of measuring electrical conductivities of solids in a diamond anvil cell (DAC) has been developed. The dc method involves a four-point probe measurement. The method is suitable for measuring the electrical conductance of bulk (polycrystalline) solids or single crystals, as a function of temperature and/or pressure.     

Dynamic diamond anvil cell (dDAC): a novel device for studying the dynamic-pressure properties of materials

We have developed a unique device, a dynamic diamond anvil cell (dDAC), which repetitively applies a time-dependent load/pressure profile to a sample. This capability allows studies of the kinetics of phase transitions and metastable phases at compression (strain) rates of up to 500 GPa/s (approximately 0.16 s(-1) for a metal). Our approach adapts electromechanical piezoelectric actuators to a conventional diamond anvil cell design, which enables precise specification and control of a time-dependent applied load/pressure. Existing DAC instrumentation and experimental techniques are easily adapted to the dDAC to measure the properties of a sample under the varying load/pressure conditions. This capability addresses the sparsely studied regime of dynamic phenomena between static research (diamond anvil cells and large volume presses) and dynamic shock-driven experiments (gas guns, explosive, and laser shock). We present an overview of a variety of experimental measurements that can be made with this device.     

Adaptation of a low-power stereomicroscope to scan cell colonies labelled with fluorescein isothiocyanate

A stereomicroscope was modified for use in visualizing fluorescence-labelled cell-colonies at low magnifications. A xenon lamp and an FITC filter (Zeiss) were used to obtain exciting radiation to illuminate fluorescent-labelled specimens. The system is precise enough to distinguish between normal and cancer cell-colonies after specific interaction with FITC-conjugated antiserum.     

A high pressure cell for small angle neutron scattering up to 500 MPa in combination with light scattering to investigate liquid samples

We report on a high pressure cell to use with small angle neutron scattering (SANS) in a pressure range up to 500 MPa. The cell offers the new possibility to investigate liquid samples by a specially designed sample chamber, which allows changing of samples relatively easily. Since the cell construction uses sapphire as window material, also light scattering investigations can be performed simultaneously to the SANS measurements. In this article we describe the construction of a high pressure cell and we demonstrate the applicability of the construction for SANS in combination with dynamic light scattering showing data on the biological molecule lysozyme.     

High pressure ellipsometry: a novel method for measuring the optical properties and electronic structure of materials in diamond anvil cells

High pressure ellipsometry (HPE) method was developed for determining the index of refraction of opaque materials in a diamond anvil cell (DAC). A main difficulty in DAC-based HPE, namely, the pressure-induced birefringence developed in the diamond, was overcome enabling the extraction of the ellipsometric parameters of the sample. The method used was based on the fact that an unpolarized light is unaffected by a retarding optical element and thus reduces the number of unknown parameters in the problem. Because of technical difficulties in using unpolarized light, a linear combination of orthogonal polarizations was applied. In the experimental procedure, multiangle measurements of the ellipsometric parameter ψ are collected at each pressure and the data is fitted together with a measurement of the near normal reflectivity, in order to extract the complex index of refraction. As a test case, this procedure was used to measure the high pressure index of refraction of iron up to 30 GPa for light with wavelengths of 532 and 633 nm. From the index of refraction as a function of pressure the diamond-iron interface emissivity for different pressures was derived and from which the phase transition α → ε could be identified and characterized. The emissivity increases with pressure both at the α (0-9 GPa) and the ε phase (21-30 GPa) however decreases at the mixed α - ε (9-21 GPa) range. From the imaginary part of the index of refraction the pressure dependence of the energy skin depth of iron was extracted. It was found that the energy skin depth increases by an order of magnitude at 30 GPa relative to ambient conditions.     

A design of backing seat and gasket assembly in diamond anvil cell for accurate single crystal x-ray diffraction to 5 GPa

We designed a new cell assembly of diamond anvil cells for single crystal x-ray diffraction under pressure and demonstrate the application of the cell to the crystallographic studies for ice VI and ethanol high-pressure (HP) phase at 0.95(5) GPa and 1.95(2) GPa, respectively. The features of the assembly are: (1) the platy anvil and unique-shaped backing seat (called as "Wing seat") allowing the extremely wide opening angle up to ±65°, (2) the PFA-bulk metallic glass composite gasket allowing the easy attenuation correction and less background. Thanks to the designed assembly, the R(int) values after attenuation corrections are fairly good (0.0125 and 0.0460 for ice VI and ethanol HP phase, respectively), and the errors of the refined parameters are satisfactory small even for hydrogen positions, those are comparable to the results which obtained at ambient conditions. The result for ice VI is in excellent agreement with the previous study, and that for ethanol HP phase has remarkable contributions to the revision to its structure; the H12 site, which makes gauche molecules with O1, C2, and C3 sites, may not exist so that only trans conformers are present at least at 1.95(2) GPa. The accurate intensities using the cell assembly allow us to extract the electron density for ethanol HP phase by the maximum entropy method.