Behavior of thermocouples under high pressure in a multi-anvil apparatus

We have conducted experiments to study the behavior of W5%Re–W26%Re (type C) and Pt10%Rh–Pt (type S) thermocouples under high pressure in a multi-anvil apparatus. The electromotive force (emf) between four different or three identical thermocouple wires was measured up to 15?GPa and 2100?°C. Mechanical and chemical stability of the thermocouples was examined during and after the experiments. Due to the effect of pressure on the emf/temperature relation, the temperature reading of the type C minus that of the type S thermocouple rises to +5?°C then falls to ?15?°C between room temperature and 1500?°C at 5?GPa, and to +25?°C and then ?35?°C between room temperature and 1800?°C at 15?GPa. In addition, we observed variations in the emf/temperature relation caused by uncertainties in the position and geometry of hot junctions in a steep temperature gradient, and by variable distribution of pressure gradient and non-hydrostatic stress on the thermocouple wires. These errors are estimated at 1.6% for the type S thermocouple up to 1700?°C, and 0.8% for the type C thermocouple up to 2100?°C. Self-diffusion and chemical contamination of the thermocouples by high-purity insulating ceramics appear negligible for the type S thermocouple at 1700?°C for one hour, and for the type C thermocouple at 2100?°C for half an hour. In contrast, large-scale displacement of the hot junction due to dislocation of the type C thermocouple wires and plastic deformation of the type S thermocouple wires may lead to large errors in temperature measurement (±200?°C).     

TiC-MgO composite: an X-ray transparent and machinable heating element in a multi-anvil high pressure apparatus

ABSTRACT

TiC-MgO composite was developed as a heating element for X-ray study in the multi-anvil high pressure apparatus. We synthesized TiC-MgO blocks (50–70 wt.% of TiC) by compression in a cold isostatic press followed by baking in a gas flow furnace. Heaters of tubular shape were manufactured from the synthesized blocks either by lathe or numerically controlled milling machine. The so-produced heating elements have been proved to generate temperatures up to 2250?K at 10?GPa, condition where classical graphite heaters are not suitable anymore due to graphite-diamond transition. These new heaters have been successfully used for in situ X-ray radiography and diffraction measurements on liquid Fe alloys, exploiting excellent X-ray transparency.     

A nearly zero temperature gradient furnace system for high pressure multi-anvil experiments

A new furnace system with an almost zero temperature gradient throughout the sample area was designed for multi-anvil high pressure experiments. Test experiments of the new design were performed using 18/11 and 25/15 cell assemblies at 4?GPa, 1400°C and 1500°C, respectively. The temperature field within the sample capsules appeared to be very homogenous as indicated by Mg₂Si₂O₆–MgCaSi₂O₆ two-pyroxene thermometry, by direct temperature measurements using two thermocouples within the same assembly, and by distribution of solid and liquid phases in the sample capsule. The temperature gradient is estimated to be <2.4°C/mm over an area of 4?×?5?mm² within the furnace. It is significantly lower than standard multi-anvil experiments with straight or stepped furnace systems, which are at the levels of 20–200°C/mm.     

High-temperature calibration of a multi-anvil high pressure apparatus

Fusion and solidification of Al and Ag samples, as well as Fe₉₃–Al₃–C₄, Fe₅₆–Co₃₇–Al₃–C₄, and Fe_57.5–Co₃₈–Al₁–Pb_0.5–C₃ alloys (in wt%), have been investigated at 6.3?GPa. Heater power jumps due to heat consumption and release on metal fusion and solidification, respectively, were used to calibrate the thermal electromotive force of the thermocouple against the melting points (mp) for Ag and Al. Thus, obtained corrections are +100°C (for sample periphery) and +65°C (center) within the 1070–1320°C range. For small samples positioned randomly in the low-gradient zone of a high pressure cell, the corrections should be +80°C and +84°C at the temperatures 1070°C and 1320°C, respectively. The temperature contrast recorded in the low-gradient cell zone gives an error about ±17°C. The method has been applied to identify the mp of the systems, which is especially important for temperature-gradient growth of large type IIa synthetic diamonds.     

Boron-doped diamond synthesized by chemical vapor deposition as a heating element in a multi-anvil apparatus

ABSTRACT

We tested boron-doped diamond (BDD) synthesized by chemical vapor deposition (CVD) as a heating element in a multi-anvil apparatus. We succeeded in manufacturing BDD into a tubular shape by laser cutting and electric discharging machining. The BDD tube shaped by the electric discharging machining was contaminated by discharging electrode materials (Mo and W), which affected the heating performance. The laser-cut BDD tube has a clean surface and, therefore, had a good heating performance. We succeeded in generating temperature as high as 2670?K at a pressure around 30?GPa with laser-cut heater. Heating reproducibility was confirmed through repeated heating and cooling cycles. The recovered sample shows that a higher temperature generation above 2670?K was prevented by eutectic melting of ZrO₂ thermal insulator and Al₂O₃ sample. Owing to the commercial availability with a reasonable price, CVD–BDD heaters are more practical than a high-pressure synthesized BDD heaters for wide applications.     

A low-temperature high-pressure apparatus with a temperature control system

Abstract

A low-temperature high-pressure apparatus was designed using commercial cryogenic equipment. Pressures up to 1 GPa and temperatures down to 40 K can be obtained in a volume of up to 30 cm³. The apparatus is of the piston-cylinder type with a piston diameter of 45 mm, and the pressure can be varied at all temperatures, An adaptive temperature control system keeps the temperature inside the pressure cylinder constant to within ±0.1 K.     

滑块式六含八超高压实验装置及其压力温度标定

报道了一种新型六含八超高压实验装置.三柱式的机体框架与滑块式上三下三模具同为三次对称结构,在力学上较为合理.该装置加压时具有自动校准位置能力,同步性和重复性好.模具推动八块硬质合金压砧在叶腊石八面体中产生高压.分别采用Bi丝和ZnTe晶体的压致相变点255,77,96,12 GPa,对截角边长8 mm压砧和125 mm边长叶腊石块组合的实验体系进行了室温下的压力标定,结果表明压力可达12 GPa以上.在10 GPa压力下,用WRe3-WRe25热电偶将温度标定到1560 ℃,并结合铁碳二元相图和钢 关键词： 压力标定 温度标定 六含八多压砧模具 高压装置     

Hybrid-toroidal anvil: a replacement for the conventional WC anvil used for the large volume cubic high pressure apparatus

We propose a design and operation of a hybrid-toroidal anvil used for the large volume cubic high pressure apparatus (LV-CHPA), such that it is possible to obtain a higher sintered quality, less weight and cost of tungsten carbide (WC) anvil than the conventional anvil. We use the finite element simulations to show the distributions of the stress on the surface and in the bulk of the WC anvils, and conclude that, for a given load on the hybrid-toroidal anvil, the volume of the compressed press medium has increased by 4.88%, and the rate of the transmitted pressure has increased by 6.72% compared with the conventional anvil. Furthermore, the advantages of the hybrid-toroidal anvil are that the movement of anvils increases by 37.14% and the growth rate of the fatigue crack decreases by 40%. This has been proved by the high pressure experiments. This work gives an approach to optimize the WC anvils used for the LV-CHPA and presents a simple method to achieve the higher sample pressure and the larger sample volume.     

Measurement problem in quantum mechanics: Characteristics of an apparatus

The problem of measurement in Quantum Mechanics will be briefly reviewed. Since the measurement process involves a macroscopic apparatus, the attention is focussed on the dynamics of a pointer-like variable of the apparatus when it interacts with a quantum system. It is argued that since the measurement process requires an apparent collapse of the wave function in a certain basis, and collapse is an irreversible process, understanding of irreversibility in a quantum macroscopic system is crucial. The chief characteristics of an apparatus that are important in understanding measurement process are (a) its closely spaced energy levels and (b) its interaction with environment. The coupling with the environment drives the density matrix of the apparatus to diagonal form, but to have persistent correlations between system and apparatus states, it seems necessary to have a pointer variable that has a classical limit     

光学薄膜样品的温度场和形变场分析

通过积分变换理论上求解了光学薄膜样品在脉冲或方波调制激励光作用下的热传导方程和热弹方程,从而获得了样品在瞬态和稳态情况下对应的温度场和形变场.为验证所求解,将理论解析解的计算机模拟结果与有限元的分析结果在时域和空间域进行了比较,两结果获得了较好的一致性;同时讨论了温度,热变形随激励光的调制频率、光斑半径等参数的变化.讨论了此模型在测量光学薄膜样品吸收损耗和表面热变形中的应用. 关键词： 温度场 形变场 表面热透镜 有限元     

MOFs材料低温储氢性能测试装置用温控系统设计

设计了一套温控系统,用在金属有机骨架(MOFs)材料低温储氢性能测试装置上.测试装置以循环液氮作为冷源.根据测试装置内的温度信号,温控系统利用PID温控仪,并结合继电器对加热丝的加热量进行调节,满足测试装置所需的温度范围,并能恒定在某一测试温度下.所设计的温控系统可以实现低温宽温区范围内的连续调节,且系统简单、操作方便...     

Dynamic compensation temperature in the mixed spin-1 and spin-2 Ising model in an oscillating field on alternate layers of a hexagonal lattice

The dynamic behavior of a mixed spin-1 and spin-2 Ising system with a crystal-field interaction in the presence of a time-dependent oscillating external magnetic field on a hexagonal lattice is studied by using the Glauber-type stochastic dynamics. The lattice is formed by alternate layers of spins σ=1$\sigma =1$ and S=2. The Hamiltonian model includes intersublattice, intrasublattice and crystal-field interactions. The set of mean-field dynamic equations is obtained by employing the Glauber transition rates. Firstly, we study time variations of the average sublattice magnetizations in order to find the phases in the system, and the thermal behavior of the average sublattice magnetizations in a period or the dynamic sublattice magnetizations to obtain the dynamic phase transition points as well as to characterize the nature (continuous and discontinuous) of transitions. Then, the behavior of the dynamic total magnetization as a function of the temperature is investigated to find the dynamic compensation points as well as determine the type of behavior. We also present the dynamic phase diagrams for both presence and absence of the dynamic compensation temperatures in the nine different planes. According to the values of Hamiltonian parameters, besides the paramagnetic (p), antiferromagnetic (af), ferrimagnetic (i) and non-magnetic (nm) fundamental phases, eight different mixed phases and the compensation temperature or L- and N-types behavior in the Néel classification nomenclature exist in the system.     

Graphite–boron composite heater in a Kawai-type apparatus: the inhibitory effect of boron oxide and countermeasures

We have investigated the performance of a graphite–boron composite (GBC) with 3?wt % boron as a precursor for a boron-doped diamond heater in a Kawai-type apparatus at 15?GPa. We first tested a machinable cylinder of GBC sintered at 1000°C in Ar/H₂ gas (99:1 molar ratio). Boron oxide (B₂O₃) formed during sintering frequently hindered the GBC heater from stable operation at temperatures higher than 1400°C by producing melt throughout the heater together with oxide and/or silicates. We then rinsed the GBC heater in hydrochloric acid to remove B₂O₃. After rinsing, we succeeded in stably generating temperatures higher than 2000°C. We also improved a molding process of different-sized GBC tubes for convenient use and tested the molded GBC heater. It was free from the B₂O₃ problem. The electromotive force of the W/Re thermocouple was successfully monitored up to 2400°C.     

Effective temperature scaled dynamics of a flexible polymer in an active bath

Langevin dynamics simulations are employed to study the dynamical properties of a flexible polymer in an active bath. The diffusion of the centre of mass and end-to-end distance fluctuation are particularly analysed. We modulate both active force and active particle size to probe the activity-induced facilitation of polymer dynamics. Results indicate diffusivity and chain relaxation time can be well scaled by the effective temperature of the active bath. In addition, diffusion dynamics demonstrates an anomalous superdiffusive behaviour in short time scales, which becomes more prominent with increasing active particle size. Lastly, we extract the effective viscosity experienced by the probed chain, showing a sharp decrease with increment of effective temperature. The attenuation of effective viscosity due to activity might be responsible for the facilitated polymer dynamics.     

Method for determining the chemically active zones in a high-frequency ultrasonic reactor

In order to determine the optimal geometry of the high-frequency sonoreactors to be used for degradation of organic compounds in aqueous solutions, a method based on the chemiluminescence of luminol (which reacts specifically with OH radicals) is applied to visualize the zones where the sonochemical reactions are the most active. The spatial distribution of the light intensity emitted by these reactions is measured inside the reactor with an optical fibre fitted on a photomultiplier. To determine the relative ultrasonic energy distribution, the temperature is measured at different points of the reactor with a thermocouple probe embedded in an absorbing material. The zones where the energy density is the highest were shown not to correspond with those where chemiluminescence reactions are the most efficient.     

An optical probe for local ion temperature measurements in a plasma

Local measurements of the ion temperature and the spectral emissivity have been performed in the magnetized plasma of the PSI‐2 device using an optical probe. The proper operation of the probe could be demonstrated. The probe collects the light emission from a small separated plasma volume thus enabling to determine the ion temperature from Doppler‐broadening of suited spectral lines. In addition to the technical features stray light and finite Larmor radii effects ‐ limiting the spatial resolution ‐ are discussed. (© 2003 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Dynamic compensation temperature in the kinetic spin-1 Ising model in an oscillating external magnetic field on alternate layers of a hexagonal lattice

The dynamic behavior of a two-sublattice spin-1 Ising model with a crystal-field interaction (D) in the presence of a time-varying magnetic field on a hexagonal lattice is studied by using the Glauber-type stochastic dynamics. The lattice is formed by alternate layers of spins σ=1 and S=1. For this spin arrangement, any spin at one lattice site has two nearest-neighbor spins on the same sublattice, and four on the other sublattice. The intersublattice interaction is antiferromagnetic. We employ the Glauber transition rates to construct the mean-field dynamical equations. Firstly, we study time variations of the average magnetizations in order to find the phases in the system, and the temperature dependence of the average magnetizations in a period, which is also called the dynamic magnetizations, to obtain the dynamic phase transition (DPT) points as well as to characterize the nature (continuous and discontinuous) of transitions. Then, the behavior of the total dynamic magnetization as a function of the temperature is investigated to find the types of the compensation behavior. Dynamic phase diagrams are calculated for both DPT points and dynamic compensation effect. Phase diagrams contain the paramagnetic (p) and antiferromagnetic (af) phases, the p+af and nm+p mixed phases, nm is the non-magnetic phase, and the compensation temperature or the L-type behavior that strongly depend on the interaction parameters. For D<2.835 and H₀>3.8275, H₀ is the magnetic field amplitude, the compensation effect does not appear in the system.     

A new technique for determination of melting temperature of poly(ethylene glycol) by ultrasonic velocimetry

Ultrasonic velocity and density of poly(ethylene glycol) (PEG) (mol. wt. 2000 and 8000) solutions in water and benzene have been studied as a function of temperature from which respective isentropic compressibility has also been calculated. The velocity (as well as isentropic compressibility) undergoes a sudden change near melting temperature, T _m, of the solute polymer. Normally, we expect only one peak in viscoelastic properties at the T _m of PEG. However, we see two peaks (T _m1 and T _m2) in the case of the aqueous solution of PEG while there is only one peak for the case of benzene solution. This has been interpreted on the basis that one of the peaks (T _m1) is for unsolvated PEG and the other peak (T _m2) is that of PEG with water solvation shell. Such solvation shell is not formed with the aprotic solvent (benzene).     

Deformation of single crystal sample using D-DIA apparatus coupled with synchrotron X-rays: In situ stress and strain measurements at high pressure and temperature

We present a technique for high pressure and high temperature deformation experiment on single crystals, using the Deformation-DIA apparatus at the X17B2 beamline of the NSLS. While deformation experiments on polycrystalline samples using D-DIA in conjunction with synchrotrons have been previously reported, this technical paper focuses on single crystal application of the technique. Our single crystals are specifically oriented such that only [1 0 0] slip or [0 0 1] slip in (0 1 0) plane is allowed. Constant applied stress (sigma <300 MPa) and specimen strain rates were monitored using in situ time-resolved X-ray diffraction and radiography imaging, respectively. Rheological properties of each activated slip system in the crystals can be revealed using this technique. In this paper, we describe the principle of sample preparation (e.g. [1 1 0]_c and [0 1 1]_c orientations) to activate specific slip systems (i.e. [1 0 0](0 1 0) and [0 0 1](0 1 0), respectively), stress measurement and procedures of the deformation experiments.