A hybrid pressure cell of pyrophyllite and magnesium oxide to extend the pressure range for large volume cubic presses

A hybrid pressure cell of pyrophyllite and magnesium oxide (HPCPM) used in large volume cubic presses is presented. In the HPCPM, a cubic frame which is made of pyrophyllite with face-centered square holes works as gaskets, and a heteromorphosis magnesium oxide works as the pressure-transmitting medium. Our experimental results indicated that the pressure-generation efficiency using the HPCPM was improved by about 40% than that using the traditional pyrophyllite pressure cell without decreasing the anvil truncation size (without sacrificing the sample volume). The HPCPM could pressurize samples of 1000 mm³ volume up to about 8 GPa, which is significantly higher than that available using the traditional pressure cell, which reports a highest pressure of about 6 GPa.     

Finite-element analysis on pressure transfer mechanism in large-volume cubic press

Pressure transmission inside a large-volume cubic press was examined using finite-element (FE) simulations. Calculations were carried out for the pyrophyllite P-transmitting mediums (32.5?×?32.5?×?32.5?mm³). The cell pressures of the simulations were chosen as representative values, including 3.75 and 5.5?GPa. A modified constitutive model for pyrophyllite and more realistic modelling were proposed. The global pressure fields were displayed using the contour plots. The results reveal that (1) at the centre of the pyrophyllite cube exists a region of constant quasi-hydrostatic pressure (RoCQHyP) where the pressure drop is less than 50?MPa; (2) how mechanical property (e.g. bulk modulus) of the P-transmitting medium affects cubic press P-transmitting performance. The simulated results were corroborated by high pressure experiments.     

六面顶压机立方压腔内压强的定量测量及受力分析

将六面顶压机立方压腔内置入电路,采用原位电阻测量确定Bi,Tl,Ba相变的方法,标定了压腔内不同位置的压力(强).通过标定立方压腔顶锤表面的压力并结合计算,分别得到了外部加载与压腔密封边受力以及合成腔体受力的对应关系.实验分析结果表明,随着外部加载的增加,当腔体压力达到5 GPa时,消耗在压腔密封边上的加载急剧上升,消耗在合成腔体的加载趋于不变,从而导致立方压腔压力达到上限.利用实验结果,分析了立方压腔在高压下的受力状态,解释了立方压腔的压力难以超过7 GPa的原因.结合立方压腔的几何结构,通过理论分析,提出了采用高体弹模量的物质作为传压介质,同时采用低体弹模量的物质作为密封边提高立方压腔压力上限的可行方案.通过定量标定叶腊石压腔轴向的压力梯度,给出了压腔内沿对称轴不同位置压力值的计算方法,此方法可为高压实验提供更精确的压力数据.     

Cobalt-doped magnesium oxide pressure-transmitting medium for high pressure and high-temperature apparatus

ABSTRACT

Magnesium oxide (MgO) doped with cobalt (Co) semi-sintered pressure-transmitting medium (MCOPM) was prepared at 1200°C in air, starting with a pre-compressed mixture of MgO and cobalt oxide (CoO). The samples were characterized using powder X-ray diffraction, scanning electron microscopy, and thermal conductivity measurements. The results demonstrate that during the sintering process, the exchange of metal ions between the mixture powders introduced lattice defects into the MgO lattice structure, and an MgO–CoO solid solution was formed. Compared to commercial semi-sintered MgO pressure-transmitting medium (SSMPM), the temperature-generation efficiency of MCOPM-17 (MgO?+?17?mol% CoO) improved by about 220% at the high pressure of 12?GPa with a cell assembly in a two-stage multi-anvil large volume press. Moreover, the thermal conductivity of CoO-doped MgO decreased with increasing CoO doping.     

基于铰链式六面顶压机的二级6-8型大腔体静高压装置

报道了一种新型二级6-8型大腔体静高压装置.该装置是以国产DS6×800T铰链式六面顶压机为构架,在其六面体压腔中直接放入二级6-8模(球分割)增压装置以产生10GPa以上的压力,还实验了不同规格的预密封边和不同密度的叶蜡石对压力产生效率的影响,在室温下用BiⅠ-Ⅱ(2.55GPa),Ⅲ-Ⅴ(7.7GPa)和SnⅠ-Ⅱ(9.4GPa)在高压下的相变对14／8(8面体传压介质边长／8面体压腔边长)规格压腔进行了压力标定.实验结果表明,该系统可以在加载压力(油压)约为3×10⁶N(～42 关键词： 铰链式六面顶压机 6-8型球分割大腔体静高压装置 压力标定     

Simulation of pressure distribution in a pyrophyllite high-pressure cell by finite-element analysis

The pressure-transmitting behavior and pressure distribution of a pyrophyllite cell in a cubic-anvil large volume high-pressure apparatus is investigated by finite-element analysis (FEA). The mechanical equations describing pyrophyllite under high pressure are given, which are composed of the Drucker–Prager criterion and a linear equation of state. The related material parameters such as cohesive strength, angle of internal friction etc. are experimentally measured. The FEA simulation includes the non-uniformity deviatoric stress caused by plastic deformation and the isotropy hydrostatic pressure of the pyrophyllite cell caused by volume compression. The results demonstrate that, in such a pyrophyllite cell, almost 90{%} of the pressure is isotropy hydrostatic pressure, and the pressure gradient mainly arise from non-uniform deviatoric stresses. Simulated data are displayed using the contour and the path plots.     

A large volume cubic press with a pressure-generating capability up to about 10 GPa

A massive cubic press, with a maximum load of 1400 tons on every WC anvil, has been installed at the High Pressure Laboratory of Peking University. High-P experiments have been conducted to examine the performance of the conventional experimental setup and some newly developed assemblies adopting the anvil-preformed gasket system. The experimental results suggest that (1) the conventional experimental setup (assembly BJC2-0) can reach pressures up to about 6 GPa with a large cell volume of 34.33 cm³; (2) the anvil-preformed gasket system, despite decreasing the P-generating efficiency, extends the P-generating capability up to about 8 GPa at the expense of reducing the cell volume down to 8.62 cm³ (assembly BJC2-6); (3) due to the large cell volume, it is possible to make further modifications to extend the pressure range, as readily demonstrated, to about 10 GPa (assembly BJC5-7); (4) the effect of high temperature on the pressure generation of the press is not significant. It follows that this cubic press can be very useful in synthesizing materials of large volume at high pressures and to the studies such as high-P phase equilibrium, trace element partitioning and isotope fractionation in the research fields of Earth and planetary sciences.     

Pressurizing conditions in helium-pressure-transmitting medium

We present quantitative measurements of the macroscopic non-hydrostatic stress and of the microscopic stress in samples compressed in a diamond anvil cell, using helium as a pressure-transmitting medium. These are based on the analysis of X-ray diffraction line shifts and widths. The macroscopic non-hydrostatic stress reaches 0.3–0.5 GPa at 150 GPa when the sample remains embedded in the pressure medium. The effect of this non-hydrostatic stress on the measured equations of state is estimated in the cases of gold, silver, molybdenum and copper. It is found to be negligible, except in the case of gold. We show that the analysis of the X-ray diffraction line shifts is a more sensitive way of detecting non-hydrostatic compression than the monitoring of the ruby luminescence signal. It can be used to detect when the sample is directly compressed between the diamond anvils. The sample geometry, in particular its thickness, has to be carefully chosen to prevent that situation.     

FEM study on a double-beveled anvil and its application to synthetic diamonds

A new double-beveled anvil for the synthesis of high-quality diamonds has been described, which is used in a China-type large-volume, cubic-anvil, high-pressure apparatus (LV-CHPA, SPD-6X2000). Our results indicate that the pressure generation of a double-beveled anvil is more efficient than that of a single-beveled anvil. To gain the same cell pressure (5.5 GPa), the oil pressure of LV-CHPA using double-beveled anvils decreased by about 10%, compared to using single-beveled anvils. Furthermore, a double-beveled anvil can pressurize a cubic cell of 36 mm³ up to about 6.0 GPa, and simultaneously can increase the temperature up to 1360°C for routine operation. This provides considerable advantages to the synthesis of high-quality diamonds under ultra-high-pressure conditions with the same hydraulic rams.     

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.     

Compact multianvil device for in situ studies at high pressures and temperatures

We describe a recently developed device for in situ studies at pressures up to 25 GPa and temperatures up to 2300 K. The system consists of a 450 ton V7 Paris-Edinburgh press combined with a Stony Brook ‘T-cup’ multianvil stage. Such a compact large-volume set-up has a total mass of 100 kg only and can be readily used on most synchrotron radiation facilities. The optimization of the set-up by off-line tests is detailed, and we present some X-ray diffraction results which demonstrate the potential of the technique.     

The SrB4O7:Sm2+ optical sensor and the pressure homogeneization through thermal cycles in diamond anvil cells

Abstract

Preliminary results, up to 550 kbar, on a thermal-cycling relaxation process of the 4.Methanol-1.Ethanol pressure-transmitting medium, are presented. The homogeneization is monitored by linewidth measurements of the ⁵D₀-⁷F₀ emission line of SrB₄O₇:Sm²⁺, recently proposed as an “almost ideal” high pressure calibrant. Above 100 kbar at 20°C, the line broadens linearly with increaisng pressure. Upon heating, at a fixed pressure, the linewidth is reduced to a minimum (“hydrostatic”) value provided a sufficient temperature is reached and this narrowing is irreversible upon cooling. For T=300°C this relaxation is observed for P (250 kbar, incomplete at 340 kbar and not observed at 550 kbar.     

A new multi-anvil press employing six independently acting 8 MN hydraulic rams

A new large volume multi-anvil system which employs six independently acting hydraulic rams with independent oil pressurization systems has been developed for high pressure and temperature experiments. The six 8 MN hydraulic rams approach at right angles inside a composite steel plate frame and can each advance a square faceted anvil of either hardened steel or tungsten carbide. The position of each anvil can be measured relative to the frame of the press to a precision of 0.1 μ m. The press is designed to perform both deformation experiments using cubic ceramic pressure media and experiments employing eight inner cubic anvils to compress an octahedral pressure medium. During compression, the position of each anvil relative to the press frame can be precisely measured and controlled independently, thus ensuring a high level of symmetry in the compressive stress environment. The highly cubic compressive regime provides an optimal environment for the use of inner sintered diamond cubic anvils, which can potentially obtain pressures above 50 GPa. The large loading capacity (24 MN) allows larger cubic pressure media to be used at higher pressures than conventional systems.     

Modified Bridgman anvils for high pressure synthesis and neutron scattering

ABSTRACT

A simple modified Bridgman design for large volume pressure anvils usable in the Paris-Edinburgh (PE) press has been demonstrated at Oak Ridge National Laboratory Spallation Neutron Source. The design shows advantages over the toroidal anvils typically used in the PE press, mainly rapid compression/decompression rates, complete absence of blow-outs upon drastic phase transitions, simplified cooling, high reliability, and relative low loads (～40 tons) corresponding to relatively high pressures (～20?GPa). It also shows advantages over existing large-volume diamond cells as sample volumes of ～2–3?mm³ can be easily and rapidly synthesized. The anvils thus allow sample sizes sufficient for in situ neutron diffraction as well as rapid synthesis of adequate amounts of new materials for ex situ analysis via total neutron scattering and neutron spectroscopy.     

Practical effects of pressure-transmitting media on neutron diffraction experiments using Paris–Edinburgh presses

ABSTRACT

To understand the practical effects of pressure-transmitting media (PTM) on neutron diffraction using Paris–Edinburgh presses, diffraction patterns of MgO were collected to approximately 20?GPa using PTMs of Pb, AgCl, 4:1 methanol–ethanol (ME) mixture with and without heating, N₂, and Ar. Hydrostaticity in the sample chamber estimated from the MgO 220 peak width improves in the order of Pb, AgCl, Ar, ME mixture, N₂, and the heated ME mixture. Unlike previous results using diamond anvil cells, the unheated ME mixture is superior to Ar even after freezing, probably due to the cup on the anvil face. Considering these results and the sizable coherent scattering of Ne, which would show good hydrostaticity, we conclude that the ME mixture (preferably the heated one) is the best PTM in neutron experiments up to 20?GPa, while Ar can be substituted when a sample is reactive to alcohols.     

Structure refinement of sub-cubic-mm volume sample at high pressures by pulsed neutron powder diffraction: application to brucite in an opposed anvil cell

Neutron powder diffraction measurements of 0.9 mm³ of mixture of deuterated brucite and pressure medium were conducted at pressures to 2.8 GPa, using an opposed anvil cell and a medium-resolution diffractometer at Japan Proton Accelerator Research Complex pulsed neutron source. Spurious-free diffraction patterns were successfully obtained and refined to provide all structural parameters including Debye–Waller factors. Tilting of hydroxyl dipoles of brucite toward one of the three nearest-neighbor oxygen anions was confirmed to be substantial at pressure as low as 1.5 GPa. By this application, technical feasibility to analyze such a small sample has been newly established, which would be useful to extend the applications of neutron diffraction at high pressures.     

Laser machined macro and micro structures on glass for enhanced light trapping in solar cells

In order to increase the efficiency of solar cell modules it is necessary to make the optimum use of light incident upon them. Much research has been done on improving light absorption through front surface texturisation and light trapping schemes. Laser light is commonly used in industry for various applications including marking and texturisation. By controlling laser parameters, it is possible to tailor macro and micro structures in most materials. The CO₂ laser used in this investigation emits radiation at 10.6 μm with the ability to pulse in the micro-second range. The laser was used to ablate grooved textures in the fused quartz material, used in this study as the light trapping medium, following which an analysis of the effects of the laser parameters on the texture geometry and surface morphology was performed through a combination of cross sectioning and scanning electron microscopy. Transmission through the textured glass was improved for most samples after acid etching. The light trapping effects of the best performing textures were analysed by investigating the effects on a silicon solar cell’s performance at varying angles of incidence. Results indicated a significant increase in light trapping when light was incident at acute angles. For an angle of incidence of 10^° a relative increase in efficiency of up to 51 % was observed.     

高压低温条件下固态氩和4∶1甲醇-乙醇混合物传压介质的传压特性

 在高压低温（77 K）条件下，利用红宝石荧光测压方法，系统地研究了金刚石对顶砧装置中固态氩和4∶1甲醇-乙醇混合物的传压特性。通过测量不同位置上红宝石荧光R₁线的频移，确定了样品室内的压力分布。实验结果表明：在0~16 GPa的压力范围内，固态氩介质中反映介质非均匀性程度的|Δp/p|<3%、σ_p/p<2%，均在室温静水压条件下所允许的范围之内。红宝石荧光R线除随压力变宽外，与常压的很相似，表明固态氩在高压低温条件下是良好的传压介质。与之相比，4∶1甲醇-乙醇介质在77 K低温下的传压特性明显差于固态氩，已不适合作传压介质。     

Effects of pressure on the two polymorphs of [Co(NH3)5NO2]I2: The anisotropy of lattice distortion and a phase transition

Abstract

The effect of pressure on the two polymorphs of [CO(NH₃)₅NO₂]I₂ (phase I-orthorhombic, S.G. Pnma; phase II-monoclinic, S.G. C2/m) was studied by X-ray powder diffraction in a diamond anvil cell (DAC). In the presence of the ethanol-methanol-water mixture used as a pressure-transmitting liquid polymorph I was shown to undergo a phase transition at pressures between 0.45 GPa and 0.65 GPa. The diffraction pattern of the high-pressure phase (phase III) could be indexed as tetragonal with lattice parameters similar to those, which were previously reported for polymorph II in a 'pseudotetragonal setting'. The lattice distortions of phases II and III were studied at pressures up to 3.2 GPa and 3.7 GPa, correspondingly, and were shown to be very similar. Phases II and III were supposed to be very closely related. If poly(chlortrifluorethylen)-oil was used as a pressure-transmitting medium, no phase transitions were observed in phase I of [CO(NH₃)₅NO₂I₂ at least up to 1.8 GPa (the point when poly(chlortrifluorethylen)-oil becomes solid), and the anisotropy of lattice distortion could be measured.