In situ conductivity measurement of matter under extreme conditions by film fabrication on diamond anvil cell

The film-fabricating technology has been used to prepare the microcircuit on diamond anvil for resistivity measurement under extreme conditions. We chose molybdenum as the electrode material and alumina as the insulator and protective material. The sample thickness measurement was conducted and then the resistivity correction was performed under different thickness. The experimental error was proved to be less than 10%. By mounting alumina film between diamond anvil and microcircuit, high-temperature performance of a laser heating diamond anvil cell was improved obviously, which is available for in situ resistivity measurement under high pressure and high temperature. Meanwhile, the impedance spectroscopy of a powdered semiconductor sample was detected. Through the impedance arcs obtained, the grain boundary contribution to the resistivity can be well distinguished.     

In situ electrical resistance and activation energy of solid C_(60) under high pressure

The in situ electrical resistance and transport activation energies of solid C60 fullerene have been measured under high pressure up to 25 GPa in the temperature range of 300-423 K by using a designed diamond anvil cell. In the experiment, four parts of boron-doped diamond films fabricated on one anvil were used as electrical measurement probes and a W-Ta thin film thermocouple which was integrated on the other diamond anvil was used to measure the temperature. The current results indicate that the measured high-pressure resistances are bigger than those reported before at the same pressure and there is no pressure-independent resistance increase before 8 GPa. From the temperature dependence of the resistivity, the C60 behaviors as a semiconductor and the activation energies of the cubic C60 fullerene are 0.49, 0.43, and 0.36 eV at 13, 15, and 19 GPa, respectively.     

An internally heated composite gasket for diamond-anvil cells using the pressure-chamber wall as the heating element

The implementation of a heating element to a composite gasket for high-temperature applications in the diamond-anvil cell was developed based on a double-gasket assemblage. The heating element is a thin platinum wall that covers the central borehole of the metal–ceramic–metal composite gasket and interconnects the two metal component parts of the gasket. Applying electric powers up to 35 W to the two gasket metal components result in ring-like heating around the sample inside the pressure chamber with temperatures exceeding ～2000 K in individual cases. The ring-like distribution of the maximum temperature located at the pressure-chamber wall facilitates a homogeneous temperature distribution at the sample position. As a consequence of the concentration of the heating power to the pressure chamber region, gradients of surface temperatures, both at the gasket and the diamond anvil, appear to be more pronounced compared with those known for classical external electrical heating. Apart from the tests of the mechanical stability on high-pressure operation in the diamond anvil cell at room temperature, the influence of the anvils in contact with the gasket on the characteristic power–temperature curves, temperature gradients and thermal equilibration resulting from changes in electrical power settings have been evaluated within the scope of a series of experimental investigations.     

High pressure X-ray diffraction and Raman spectroscopic studies of the phase change of D2O ice VII at approximately 11 GPa

High pressure experiments were performed on D₂O ice VII using a diamond anvil cell in a pressure range of 2.0–60 GPa at room temperature. In situ X-ray diffractometry revealed that the structure changed from cubic to a low symmetry phase at approximately 11 GPa, based on the observed splitting of the cubic structure's diffraction lines. Heating treatments were added for the samples to reduce the effect of non-hydrostatic stress. After heating, splitting diffraction lines became sharp and the splitting was clearly retained. Although symmetry and structure of the transformed phase have not been determined, change in volumes vs. pressure was calculated, assuming that the low-symmetry phase had a tetragonal structure. The bulk modulus calculated for the low-symmetry phase was slightly larger than that for the cubic structure. In Raman spectroscopy, the squared vibrational frequencies of ν₁ (A_1g), as a function of pressure, showed a clear change in the slope at 11–13 GPa. The full width at half maxima of the O-D modes decreased with increasing pressure, reaching a minimum at approximately 11 GPa, and increased again above 11 GPa. These results evidently support the existence of phase change at approximately 11 GPa for D₂O ice VII.     

Measurement of improved pressure dependence of superconducting transition temperature

We describe a technique for making electrical transport measurements in a diamond anvil cell at liquid helium temperature having in situ pressure measurement option, permitting accurate pressure determination at any low temperature during the resistance measurement scan. In general, for four-probe resistivity measurements on a polycrystalline sample, four fine gold wires are kept in contact with the sample with the help of the compression from the soft solid (usually alkali halides such as NaCl, KCl, etc.) acting as a pressure-transmitting medium. The actual pressure on the sample is underestimated if not measured from a ruby sphere placed adjacent to the sample and at that very low temperature. Here, we demonstrate the technique with a quasi-four-probe resistance measurement on an Fe-based superconductor in the temperature range 1.2–300 K and pressures up to 8 GPa to find an improved pressure dependence of the superconducting transition temperature.     

Electrical property and phase transition of CdSe under high pressure

In situ electrical resistivity measurement of CdSe was performed under high pressure and moderate temperature using a diamond anvil cell equipped with a microcircuit. With the pressure increasing, a sharp drop in resistivity of over two orders of magnitude was observed at about 2.6 GPa, it was caused by the transition to the rock-salt CdSe. After that, the resistivity decreased linearly with pressure. However, in different pressure range, the decreasing degree was obviously different. This attributed to the different electron structures. By fitting to the curve of pressure dependence of resistivity in different pressure range, the relationship of the band gap to pressure was given and the metallization pressure was speculated to be in the range of 70-100 GPa. The temperature dependence of resistivity showed that in the experimental temperature and pressure range the resistivity had a positive temperature coefficient.     

Electron Transport Property of CdTe under High Pressure and Moderate Temperature by In-Situ Resistivity Measurement in Diamond Anvil Cell

In situ resistivity measurement has been performed to investigate the electron transport property of powered CdTe under high pressure and moderate temperature in a designed diamond anvil cell. Several abnormal resistivity changes can be found at room temperature when the pressure increases from ambient to 33 GPa. The abnormal resistivity changes at about 3.8 GPa and 10 GPa are caused by the structural phase transitions to the rock-salt phase and to the Cmcm phase, respectively. The other abnormal resistivity changes at about 6.5 GPa, 15.5 GPa, 22.2 GPa and about 30 GPa never observed before are due to the electronic phase transitions of CdTe. The origin of the abnormal change occurred at about 6.5 GPa is discussed. The temperature dependence of the resistivity of CdTe shows its semiconducting behaviour at least before 11.3 GPa.     

Diamond anvil Raman gauge in multimegabar pressure range

The first-order Raman band of diamond anvils has been investigated at pressure up to 380 GPa in order to develop an optical pressure determination method. The high frequency edge of the band was calibrated by the pressure scale of the equation of state of Pt. The universality of the relationship between the sample pressure and the edge-frequency was confirmed up to 370 GPa and the usefulness of the diamond anvil Raman gauge was demonstrated. Using the diamond anvil Raman spectroscopy, the stress-state of the anvil culet was directly observed in the multimegabar pressure range. Obtained pressure dependence of the shear stress suggested further extension of feasible pressure beyond 400 GPa.     

Crystal structure and compressibility of FePt nanoparticles under high pressures and high temperatures

FePt nanoparticles with an average grain size of 4 nm and equiatomic composition of Fe and Pt was studied under high pressures in a diamond anvil cell to investigate its structural stability and compressibility under high compression. The ambient pressure disordered face-centered-cubic (fcc) phase was found to be stable to the highest pressure of 61 GPa (compression of 15%) at room temperature. The compression of Fe₅₀Pt₅₀ nanoparticles is closer to the compression curve for pure Pt and shows lower compressibility than what would be expected for a bulk Fe₅₀Pt₅₀ alloy. The nanoparticle character of Fe₅₀Pt₅₀ sample is maintained to the highest pressure without any observable grain coarsening effects at ambient temperature. Laser heating of disordered fcc phase at 32 GPa to a temperature of 2000 K resulted in a phase transformation to a microcrystalline phase with the distorted fcc structure.     

人造聚晶翡翠宝石

 综述了翡翠宝石的人工合成的进程及各种实验结果，给出了6×8MN六面顶高压装置的压力和温度工作曲线，对比了两面顶高压装置及六面顶高压装置上合成翡翠宝石的优缺点及解决办法，并做了合成高品级翡翠宝石的尝试。     

Thermal conductivity of hcp iron at high pressure and temperature

Results of steady-state heat transfer experiments on iron in laser-heated diamond anvil cell, combined with numerical simulation using finite-element method are reported. Thermal boundary conditions, dimensions of sample assemblage, heating-laser beam characteristics and relevant optical properties have been well defined in the course of experiments. The thermal conductivity of the polycrystalline hexagonal-iron foil has been determined up to pressure 70 GPa and temperature 2000 K. At these conditions, the conductivity value of 32±7 W/m K was found. Sources of errors arising from uncertainties in input parameters and applied experimental procedures are discussed. Considering results of earlier preferred-orientation studies in diamond anvil cell, an averaging effect of polycrystalline texture on the intrinsic anisotropy is assumed. The obtained conductivity is interpreted as an effective value, falling in between the upper and lower bounds on the average conductivity of a random aggregate of uniaxial crystals.     

Simultaneous electrical and X-ray diffraction studies on neodymium metal to 152 GPa

Using designer diamond anvils and angle dispersive X-ray diffraction technique at a synchrotron source, we have performed simultaneous electrical and structural studies on neodymium metal to 152 GPa in a diamond anvil cell. Four-probe electrical resistance measurement shows a 38% decrease in the electrical resistivity, associated with the delocalization of the 4f-shell electrons, starting at 100 GPa up to a final pressure of 152 GPa. The continuous decrease in electrical resistivity is consistent with the observation of a gradual phase transition to α-U structure in this pressure range. The (1 1 1) diffraction peak of α-U structure first appears at 100 GPa and increases in intensity with increasing pressure to 152 GPa. This increase in intensity is attributed to an increasing volume fraction of α-U phase and an increase in structural y-parameter from 0.07 at 118 GPa to 0.095 at 152 GPa. In contrast to the abrupt pressure-induced f-electron transition seen in cerium and praseodymium, the continuous evolution of α-U structure and electrical resistivity in neodymium confirms the gradual nature of 4f delocalization process in this element.     

Synthesis and characterization of p-type boron-doped IIb diamond large single crystals

High-quality p-type boron-doped IIb diamond large single crystals are successfully synthesized by the temperature gradient method in a china-type cubic anvil high-pressure apparatus at about 5.5 GPa and 1600 K.The morphologies and surface textures of the synthetic diamond crystals with different boron additive quantities are characterized by using an optical microscope and a scanning electron microscope respectively.The impurities of nitrogen and boron in diamonds are detected by micro Fourier transform infrared technique.The electrical properties including resistivities,Hall coefficients,Hall mobilities and carrier densities of the synthesized samples are measured by a four-point probe and the Hall effect method.The results show that large p-type boron-doped diamond single crystals with few nitrogen impurities have been synthesized.With the increase of quantity of additive boron,some high-index crystal faces such as {113} gradually disappear,and some stripes and triangle pits occur on the crystal surface.This work is helpful for the further research and application of boron-doped semiconductor diamond.     

Sulphur electric properties at superhigh pressure around the polymerization temperatures

Abstract

The electrical resistivity temperature dependence of S has been studied in the diamond anvil cell (DAC) of the “rounded cone-plane” type. The pressure is about 50 GPa. The experimental data analysis shows the polymerization between 380–410 K. The electrical resistivity temperature dependence is distorted by a number of maxima, some of them being shifted along the temperature axis towards the lower temperature and disappear with increasing transport current.     

A XANES study of the Cu K-edge in A2CuCl4 perovskite layers under pressure. Influence of antiferrodistortive structure

Abstract

The temperature dependence of ice resistivity R has been investigated in the diamond anvil cell (DAC) of “rounded cone-plane” type. Mean pressure is about 20 GPa, temperature interval is 4,2–273 K. Measuring R it has been detected that ice changes to metallic conductivity type state between 220–260 K. At 25 K the temperature dependence of R shows the transport current dependence.     

Hybrid Bridgman anvil design: an optical window for in situ spectroscopy in large volume presses

The absence of in situ optical probes for large volume presses (LVPs) often limits their application to high-pressure materials research. In this article, we present a unique anvil/optical window design for use in LVPs, which consists of an inverted diamond anvil seated in a Bridgman-type anvil. A small cylindrical aperture through the Bridgman anvil ending at the back of diamond anvil allows optical access to the sample chamber and permits direct optical spectroscopy measurements, such as ruby fluorescence (in situ pressure) or Raman spectroscopy. The performance of this anvil design has been demonstrated by loading KBr to a pressure of 14.5 GPa.     

Phase transition of ZnS at high pressures and temperatures

The high-pressure behaviour of zinc sulphide, ZnS, has been investigated, using an in situ X-ray powder diffraction technique in a diamond anvil cell, at pressures and temperatures up to 35 GPa and 1000 K, respectively. The pressure-induced phase transition from a zincblende (B3) to a rocksalt (B1) structure was observed. This transition occurred at 13.4 GPa and at room temperature, and a negative dependence on temperature for this transition was confirmed. The transition boundary was determined to be P (GPa) = 14.4 ? 0.0033 × T (K).     

Method of low-temperature optical measurements with diamond anvil cells

Abstract

Constructions of a cryogenic diamond anvil system with mechanical clamping press and helium pressure medium for microscopic optical studies are described. Low temperature nonmagnetic cells ø40 and ø20 mm have been developed. GaP samples doped with S, Te and isoelectronic impurities N, NN have been investigated up to 20 GPa at 1.5-300K.     

Influence of boron carbide on properties of CVD-diamond thin films at various deposition pressures

Microcrystalline boron-doped diamond (BDD) films are synthesized on the silicon substrate by the hot-filament chemical vapor deposition method under the gas mixture of hydrogen and methane in the presence of boron carbide (B₄C) placed in front of filaments. The observed results of scanning electron microscopy, Raman spectroscopy and X-ray diffraction show the morphologies. Microstructures for various deposition pressures of as-grown diamond films are found to be dependent on the change of deposition pressure. These results reveal that with the increase of deposition pressure, resistivity decreases and increase in the grain size is noted in the presence of B₄C. Resistivity shows a sudden fall of about three orders of magnitude by the addition of boron in the diamond films. This is due to the crystal integrity induced by B-atoms in the structure of diamond in the presence of B₄C. These results are also significant for the conventional applications of BDD materials. The effects of deposition pressure on the overall films morphology and the doping level dependence of the diamond films have also been discussed.