Simultaneous structure and elastic wave velocity measurement of SiO2 glass at high pressures and high temperatures in a Paris-Edinburgh cell

An integration of multi-angle energy-dispersive x-ray diffraction and ultrasonic elastic wave velocity measurements in a Paris-Edinburgh cell enabled us to simultaneously investigate the structures and elastic wave velocities of amorphous materials at high pressure and high temperature conditions. We report the first simultaneous structure and elastic wave velocity measurement for SiO(2) glass at pressures up to 6.8 GPa at around 500°C. The first sharp diffraction peak (FSDP) in the structure factor S(Q) evidently shifted to higher Q with increasing pressure, reflecting the shrinking of intermediate-range order, while the Si-O bond distance was almost unchanged up to 6.8 GPa. In correlation with the shift of FSDP position, compressional wave velocity (Vp) and Poisson's ratio increased markedly with increasing pressure. In contrast, shear wave velocity (Vs) changed only at pressures below 4 GPa, and then remained unchanged at ~4.0-6.8 GPa. These observations indicate a strong correlation between the intermediate range order variations and Vp or Poisson's ratio, but a complicated behavior for Vs. The result demonstrates a new capability of simultaneous measurement of structures and elastic wave velocities at high pressure and high temperature conditions to provide direct link between microscopic structure and macroscopic elastic properties of amorphous materials.     

A broadband spectroscopy method for ultrasonic wave velocity measurement under high pressure

A broadband spectroscopy method is proposed to measure the ultrasonic wave phase velocity of Z-cut quartz under high pressure up to 4.7 GPa. The sample is in a hydrostatic circumstance under high pressure, and we can get longitudinal wave and shear wave signals simultaneously in our work. By fast Fourier transform of received signals, the spectrum and phase of the received signals could be obtained. After unwrapping the phase of the received signals, the travel time of ultrasonic wave in the sample could be obtained, and the ultrasonic wave phase velocity could also be resolved after data processing. The elastic constant of measurement under high pressure is also compared with previous studies. This broadband spectroscopy method is a valid method to get ultrasonic wave travel parameters, and it could be applied for elasticity study of materials under high pressure.     

Laser-Doppler vibrating tube densimeter for measurements at high temperatures and pressures

A laser-Doppler vibrometer was used to measure the vibration of a vibrating tube densimeter for measuring P-V-T data at high temperatures and pressures. The apparatus developed allowed the control of the residence time of the sample so that decomposition at high temperatures could be minimized. A function generator and piezoelectric crystal was used to excite the U-shaped tube in one of its normal modes of vibration. Densities of methanol-water mixtures are reported for at 673 K and 40 MPa with an uncertainty of 0.009 g/cm3.     

Instrument for x-ray magnetic circular dichroism measurements at high pressures

An instrument has been developed for x-ray magnetic circular dichroism (XMCD) measurements at high pressures and low temperatures. This instrument couples a nonmagnetic copper-beryllium diamond anvil cell featuring perforated diamonds with a helium flow cryostat and an electromagnet. The applied pressure can be controlled in situ using a gas membrane and calibrated using Cu K-edge x-ray absorption fine structure measurements. The performance of this instrument was tested by measuring the XMCD spectra of the Gd(5)Si(2)Ge(2) giant magnetocaloric material.     

Optical cell for in situ vibrational spectroscopic measurements at high pressures and shear

An optical cell is described for performing simultaneous static high-pressure and shear experiments. This cell design is a modification of the previously designed megabar diamond anvil cell used by Mao and Bell that allows for controlled, remote shear. With this diamond anvil cell, it is possible to use a wide range of existing experimental techniques and pressure media. The cell was validated on a sample of calcite at 5 kbar. Raman measurements show the onset of the phase transformation from calcite to aragonite at 10° of rotation.     

Automatic and simultaneous measurements of ultrasonic velocity and attenuation changes

A method is described for measuring ultrasonic velocity and attenuation simultaneously by sampling echo pulses along with the repetition rate of velocity measurements. This is achieved by extending the pulse superposition method. This system enables us to measure the attenuation coefficient with a precision of 0.001 dB/cm, and the ultrasonic velocity with better precision than 1 part in 10(6). Velocity measurements can be made automatically up to five times the initial round trip time and can also track fast changes of 50 ms. Since the operation under the p=1 condition can be applied, the system can be used for the measurements of high-loss materials.     

Glass capillary for high resolution NMR measurements at pressures up to 400 MPa

A glass capillary for use in high resolution NMR spectroscopy at pressures up to 400 MPa is described together with the method of construction and use.     

Friction at high normal pressures

Friction conditions between tool and workpiece in metal working are of the greatest importance to a number of factors such as force and mode of deformation, properties of the finished specimen and resulting surface roughness.It is shown, theoretically and experimentally, that the Amonton friction law expressed by τ = μq does not apply when normal pressure is higher than approximately the yield stress of the specimen; in this case it is necessary to consider the frictional stress as a function of normal pressure, surface topography, length of sliding, viscosity, and compressibility of the lubricant.The theoretical work was carried out by means of upper bound and slipline field analysis based on experiments with model surfaces in wax and metal. The theoretical model applied is one of multihole extrusion, the material beneath the valleys of the workpiece surface being extruded up towards the tool when the real area of contact exceeds a certain value. The effect of the trapped lubricant is to build up a back-pressure on the extrusion process.The experimental work was carried out with newly developed equipment enabling direct determination of the abovementioned function; construction and calibration of the equipment are described. The equipment allows determination of frictional stress on a surface with well-defined values of normal pressure, sliding length, and sliding velocity. The normal pressure can attain about 8 times the yield stress for commercially pure aluminium.The results obtained show reasonably good agreement between theory and experiment, and a dependence of the frictional stress on the sliding length, this dependence being a function of normal pressure.     

Separation of the reservoir and wave pressure and velocity from measurements at an arbitrary location in arteries

Previous studies based on measurements made in the ascending aorta have demonstrated that it can be useful to separate the arterial pressure P into a reservoir pressure P* generated by the windkessel effect and a wave pressure p generated by the arterial waves: P = P*+p. The separation in these studies was relatively straightforward since the flow into the arterial system was measured. In this study the idea is extended to measurements of pressure and velocity at sites distal to the aortic root where flow into the arterial system is not known. P* is calculated from P at an arbitrary location in a large artery by fitting the pressure fall-off in diastole to an exponential function and assuming that p is proportional to the flow into the arterial system. A local reservoir velocity U* that is proportional to P* is also defined. The separation algorithm is applied to in vivo human and canine data and to numerical data generated using a one-dimensional model of pulse wave propagation in the larger conduit arteries. The results show that the proposed algorithm is reasonably robust, allowing for the separation of the measured pressure and velocity into reservoir and wave pressures and velocities. Application to data measured simultaneously in the aorta of the dog shows that the reservoir pressure is fairly uniform along the aorta, a test of self-consistency of the assumptions leading to the algorithm. Application to data generated with a validated numerical model indicates that the parameters derived by fitting the pressure data are close to the known values which were used to generate the numerical data. Finally, application to data measured in the human thoracic aorta indicates the potential usefulness of the separation.     

高温超声横波波速规律与影响因素研究

通过实验,得到了在-40℃-450℃范围变化内,超声波在16MnR钢内的横波传播速度值,按其趋势拟合了两种速度规律关系式,并对其进行了比较.讨论了由于热膨胀造成的试件半径的变化对速度测量误差的影响,给出了实际波速、量程修正和误差幅度关系式,修正了不同温度下波速实际值和缺陷的实际位置.分析了由于温度变化造成的弹性模量、泊松比和密度的变化对速度变化的影响,解决了目前在高温运行环境下压力容器与管道急需解决的问题.     

Yield strength of molybdenum at high pressures

In the diamond anvil cell technology, the pressure gradient approach is one of the three major methods in determining the yield strength for various materials at high pressures. In the present work, by in situ measuring the thickness of the sample foil, we have improved the traditional technique in this method. Based on this modification, the yield strength of molybdenum at pressures has been measured. Our main experimental conclusions are as follows: (1) The measured yield strength data for three samples with different initial thickness (100, 250, and 500 microm) are in good agreement above a peak pressure of 10 GPa. (2) The measured yield strength can be fitted into a linear formula Y=0.48(+/-0.19)+0.14(+/-0.01)P (Y and P denote the yield strength and local pressure, respectively, both of them are in gigapascals) in the local pressure range of 8-21 GPa. This result is in good agreement with both Y=0.46+0.13P determined in the pressure range of 5-24 GPa measured by the radial x-ray diffraction technique and the previous shock wave data below 10 GPa. (3) The zero-pressure yield strength of Mo is 0.5 GPa when we extrapolate our experimental data into the ambient pressure. It is close to the tensile strength of 0.7 GPa determined by Bridgman [Phys. Rev. 48, 825 (1934)] previously. The modified method described in this article therefore provides the confidence in determination of the yield strength at high pressures.     

Optical cell for combinatorial in situ Raman spectroscopic measurements of hydrogen storage materials at high pressures and temperatures

An optical cell is described for high-throughput backscattering Raman spectroscopic measurements of hydrogen storage materials at pressures up to 10 MPa and temperatures up to 823 K. High throughput is obtained by employing a 60 mm diameter × 9 mm thick sapphire window, with a corresponding 50 mm diameter unobstructed optical aperture. To reproducibly seal this relatively large window to the cell body at elevated temperatures and pressures, a gold o-ring is employed. The sample holder-to-window distance is adjustable, making this cell design compatible with optical measurement systems incorporating lenses of significantly different focal lengths, e.g., microscope objectives and single element lenses. For combinatorial investigations, up to 19 individual powder samples can be loaded into the optical cell at one time. This cell design is also compatible with thin-film samples. To demonstrate the capabilities of the cell, in situ measurements of the Ca(BH(4))(2) and nano-LiBH(4)-LiNH(2)-MgH(2) hydrogen storage systems at elevated temperatures and pressures are reported.     

Microwave cavity for EPR at high hydrostatic pressures

The design of a simple pressure locked cavity for use in X-band EPR studies at high hydrostatic pressures and temperatures down to liquid nitrogen is described. A coaxial coupling arrangement which avoids the use of sapphire is used.     

System for ESR measurements at hydrostatic pressures to 60 kilobars

A single-crystal sapphire serves both as a solid microwave cavity (X band) and an anvil in a Bridgman-anvil pressure geometry. A metal gasket is used in a manner similar to its use in the diamond-anvil pressure cell, and single-crystal samples are subject to purely hydrostatic pressures. The ruby-fluorescence pressure-measurement technique is utilized. Sample size is limited to a disk approximately 0.6 mm in diameter and 0.1 mm thick. ESR data on Cr(3+) in ruby to 60 kilobars are given as an illustration of the precision and data quality. Line widths and profiles, as well as line positions, are meaningful. Very little degradation of the data is experienced at the higher pressures. The first and second derivatives of the zero-field splitting (delta) of the states in ruby with pressure are measured as ddelta/dP= (6.70+/-0.08) x 10(-4) cm(-1) kilobar(-1) and d(2)delta/dP(2)= (-2.44+/-0.30) x10(-6) cm(-1) kilobar(-2) at P=0. The gyromagnetic ratio g(11) is shown to experience a fractional change less than 2 x 10(-4) to 60 kilobars.     

A speckle-interferometric setup for contactless measurements of the velocity of rayleigh ultrasonic waves

The velocity of a Rayleigh wave was determined by measuring its propagation time between two Iaser-illuminated small areas of a rough surface. It is sh own that, if a Rayleigh wave passes over these areas, a photodiode twice detects signals proportional to the surface displacement in the speckle overlap region. In contrast to the previous variant, signal-distorting reflections are eliminated in the instrument. A sample holder excluding adjustment of the interferometer upon a change in the object size has been manufactured. A new technique for determining the time interval between two signals is used. The instrument operates at a frequency of 5 MHz, and the distance between the areas is adjusted in the range 5–100 mm. The rms deviation of the velocity from the average value for ten measurements is 8 × 10–4.     

Comparative relationships of direct, indirect, and semi-direct ultrasonic pulse velocity measurements in concrete

An experimental study is conducted to compare direct, indirect and semi-direct ultrasonic pulse velocity (UPV) measurements on a total of 30 concrete blocks 30 × 30 × 25 cm³ in size that came from different mix batches and have cube compressive strength grades varying between 18.8 and 79.9 MPa. The correlations are established between the direct UPV and indirect UPV in the concrete casting direction as well as in the horizontal direction and semi-direct UPV measurements via statistical analysis. The statistical analysis reveals that the average value of direct UPV is 9%, 4%, and 4% higher than the average of indirect UPV in the casting direction, indirect UPV in the horizontal direction, and semi-direct UPV, respectively. The average value of indirect UPV in the horizontal direction is 5% higher than that in the casting direction. The text was submitted by the authors in English.     

Applicability of ultrasonic technique for evaluation of elastic plastic fracture toughness of high manganese steel at low temperatures

A study on the evaluation of elastic-plastic fracture toughness, J_IC, by ultrasonic technique is described for a newly developed high manganese steel at low temperature. In order to see the applicability of the ultrasonic technique based on pulse echo method at low temperature, special attention was paid to detect change point of ultrasonic echo due to the onset of stable crack growth. The J_IC values are evaluated by the ultrasonic method (which needs single specimen) and by stretched zone method (which needs several specimens) for compact tension (CT) specimens and three-point bend (3PB) specimens. The temperature dependence of these J_IC values of theCT specimens by the ultrasonic method show almost the same values to 3PB specimens over the temperature range tested. The J_IC values of 3PB specimens by the stretched zone method show slightly higher values than those of theCT specimens at low temperature. The J_IC values evaluated by the ultrasonic method give more conservative values than those evaluated by the stretched zone method for bothCT and 3PB specimens.     

Rolling resistance measurements at high loads

The theory of Collins for the rolling of a rigid cylinder on a rigid-perfectly plastic half-space has been investigated experimentally using a hard steel roller on a hard-drawn copper block. Two special cases were examined: (a) the roller propelled by a tangential force and (b) the roller propelled by a pure torque. In case (a) the measured rolling resistance and the mode of plastic deformation was observed to be in good agreement with Collins' theory, but in case (b) the observed mode of deformation and the measured resistance differed significantly from Collins' predictions and were found to be not very different from case (a).     

用于超声散斑跟踪血流测速的多角度平面波局部运动补偿

血流速度剖面用于计算壁面剪切率等血流动力学指标,与动脉粥样硬化病程发展密切相关。 超快超声散斑跟踪广泛用 于血流速度剖面估计,然而多角度平面波复合成像存在血流散射体的运动伪影,不利于流速估计。 提出了一种多角度平面波复 合成像的局部运动补偿法,对射频信号时间序列的相邻帧进行局部运动补偿来消除不同径向位置的运动伪影,从而提高流速测 量准确性。 相比直接相干复合,B-MoCo 法将仿真、仿体实验中流速测量结果的归一化均方根误差平均减小了 10. 37% 、 37. 82% ,说明了 B-MoCo 法的有效性。 基于兔骼动脉的实测实验进一步证明了 B-MoCo 法的临床可行性。 综上,B-MoCo 法能够 有效提高血流速度剖面的测量精度,有助于相关心血管疾病的早期诊断与病程监测。     

Small mass spectrometer with extended measurement capabilities at high pressures

For the in situ investigation of planetary atmospheres a small Mattauch-Herzog mass spectrometer has been developed. Its high-pressure performance has been improved by incorporating differential pumping between the ion source and the analyzing fields, shortening the path-length as well as increasing the extraction field in the ion source. In addition doubly ionized and dissociated ions are used for mass analysis. These measures make possible operation up to 10(-2) millibars. Results of laboratory tests related to linearity, dynamic range, and mass resolution are presented, in particular for CO(2).