Metrology of high pressures to approximately 3.0 Gpa

Abstract

The pressure scale up to approximately 3. 0 GPa is considered in order to improve pressure measurement accuracy.

The main subjects presented are related to absolute and gage pressure measurements with gases to about few megapascal and gage pressure measurements in liquids to about 1. 5 GPa by means of piston gauges.

The use of a pressure scale based on fixed points is mentioned.     

Effect of viscosity of the pressure-transmitting fluid on the metrological characterization of the piston gauge up to 1 GPa

A systematic theoretical investigation has been carried out to study the effect of viscosity of the pressure-transmitting fluids on the measurement of pressure up to 1 GPa using piston gauges. The fluid flow equation is modified to determine the fall rate (v) with pressure (P), taking the pressure-dependent viscosityη(P) and clearance between piston and cylinder [H(P)] terms into account. Above 0.4 GPa, the fall rate curve shows the tendency to be pressure independent. The near-constancy ofv withP can be avoided with less viscous fluid or by increasingH(P). Finally. the initial clearance obtained from the experimental data of fall rate, shows a weak dependence of pressure, although theoretically it is assumed to be independent of pressure. This weak pressure dependence is attributed to the effect of viscosity of the pressure transmitting fluid.     

A laser pistonphone based on self-mixing interferometry for the absolute calibration of measurement microphones

A laser pistonphone for the absolute calibration of microphones at low frequencies has been developed at UME. The motion of an electro-dynamically driven piston in a small close cavity produces a sound pressure. Accurate measurement of the piston displacement, by self-mixing interferometry, enables this sound pressure to be calculated, and consequently the pressure sensitivity of a microphone, exposed to this sound pressure, to be determined. Absolute calibrations of type LS1P and WS1P microphones have been carried out with an uncertainty of less than 0.15 dB. The performance of the laser pistonphone has been validated by comparing the measured microphone sensitivities with those obtained by the closed coupler reciprocity method.     

High pressure measurement with simple piston gauge in static condition

This paper describes the characterization of the newly developed piston gauge pressure standard at the National Physical Laboratory (NPL), with particular reference to its fall rate, engagement length of the piston and the deceleration rate for the measurement of hydraulic hydrostatic pressure up to 60 MPa. The low pressure effective area of the gauge derived from its dimensional measurements when compared with the value obtained by its direct calibration against NPL transfer pressure standard agrees within 0.025%. The pressure gauge is quite stable, reproducible and has a sensitivity of 3 ppm. Though the theoretically calculated value of the pressure coefficient is low as compared to the experimentally observed one in its absolute terms, the pressure dependent effective area agrees within ± 0.025% over whole of the pressure range which is well within the uncertainty statement of the two independent techniques used.     

Elastic distortions in simple piston-cylinder units at pressures up to 100 MPa

Abstract

The study of elastic distortions in piston-cylinder units of primary standards piston gauges is of importance for the improvement of pressure measurement accuracy. Preliminary work (GF. Molinar et al., 1989) on distortion calculations was carried out on a tungsten carbide (t.c.) piston-cylinder of 0.2 cm² nominal effective area in the 100 MPa pressure range. The same calculations are now applied in the study of a similar piston-cylinder unit of hard steel (h.s.). The distortions on the outer surface of the cylinder are measured with strain gages and with a capacitance sensor. The calculated distortions, which can be also derived with other methods (G. Klingenberg 1989, R. Wisniewski et al. 1989), are compared with the experimental results obtained on the outer surface of the cylinder. The present two piston-cylinder units of h.s. and of t.c. were cross-floated up to 100 MPa and the ratio R = f(P) = Ae_h.s./Ae_t.c. obtained experimentally is compared with the calculated.     

Pressure calibration to 304 GPa on the basis of X-ray diffraction measurements of Pt,Fe and CsI

Abstract

X-ray diffraction measurements have been carried out above 300 GPa for the first time using Pt as a primary pressure standard. The equations of state of iron up to 304 GPa and of CsI up to 302 GPa have been obtained. These materials can therefore be used as secondary pressure calibrants.     

Experience in the design of free-cylinder pressure transducers to about 1 GPa

Abstract

Free-cylinder pressure transducers for pressure measurements to about 1.0 GPa have been developed; they use at present foil strain gauges bonded on the cylindrical surface in order to measure strains as a function of the applied hydrostatic pressure. All such transducers can be used with thin-or thick-film gauges; distortions of the active cylinder can be measured also by optical techniques. Pressure transducers of three types (different design as to pressure full scale and cylinder materials) are described and their metrological characteristics are given as well.     

Study of cerium phase transitions in shock wave experiments

Cerium has a complex phase diagram that is explained by the presence of structural phase transitions. Experiments to measure the sound velocities in cerium by two methods were carried out to determine the onset of cerium melting on the Hugoniot. In the pressure range 4–37 GPa, the sound velocity in cerium samples was measured by the counter release method using manganin-based piezoresistive gauges. In the pressure range 35–140 GPa, the sound velocity in cerium was measured by the overtaking release method using carbogal and tetrachloromethane indicator liquids. The samples were loaded with plane shock wave generators using powerful explosive charges. The onset of cerium melting on the Hugoniot at a pressure of about 13 GPa has been ascertained from the measured elastic longitudinal and bulk sound velocities.     

3 GPa熔融盐固体介质三轴高温压力容器的轴压摩擦力标定

 在温度标定和围压标定的基础上,采用轴压循环方法,对3 GPa固体介质三轴高温高压实验系统的轴压摩擦力进行了标定,分析了围压、温度、轴向位移速率、装样方式（盐套类型）等实验条件对轴压摩擦力的影响。结果表明：静摩擦力、挤压摩擦力和滑动摩擦力3种轴压摩擦力对轴向应力的影响不同,其中静摩擦力和挤压摩擦力对轴向应力的影响很小,影响应力精度的主要是滑动摩擦力。静摩擦力及滑动摩擦力与围压正相关;静摩擦力与轴向位移速率正相关,但受其影响较小,滑动摩擦力不受其影响;静摩擦力和滑动摩擦力与温度负相关,并且受其影响较显著;盐套类型对轴压摩擦力的影响较大,当实验条件接近盐套熔点时,轴压摩擦力显著降低,当样品周围的盐套处于熔融状态时,轴压摩擦力最小。基于此,确定了标定轴压摩擦力的具体步骤,并对角闪岩的应力-应变曲线进行了轴压摩擦力标定。对比轴压摩擦力校正前、后的应力-应变曲线发现,经过轴压摩擦力校正的应力-应变曲线能更好地反映样品的实际变形情况。     

阵列式薄膜锰铜计的动态压阻响应研究

 利用直流磁控溅射薄膜工艺制备阵列式薄膜锰铜压阻计,以氧化铝作为基片和绝缘封装材料。在结构上,4个具有相同阻值的薄膜锰铜计在同一氧化铝基片上呈对称分布。51.72 GPa压力下的动态加载实验表明,4个计的压阻一致性好,无高压旁路效应,验证了薄膜锰铜压阻计动态测试的准确性和可靠性。     

The kiel/berlin pressure cells for neutron powder diffraction

Abstract

Two piston/cylinder type pressure cells for neutron powder diffraction are presented. They provide a large sample volume and hence allow rapid data collection at moderate flux neutron sources. Structure refinements from the diffraction data are possible. The maximum attainable pressure is above 2 GPa for Ti/Zr zero-scattering pressure cylinders. Both cells may be equipped with a micro-furnace. This allows measurement up to 700 K, simultaneously to the application of pressure. The low temperature setup for the cell-I is presented which will allow experiments down to 1·5K.     

PVDF压电计的动态响应特性及其在橡胶材料SHPB实验中的应用

通过夹心式PVDF(Polyvinylide Fluoride)压电计的动态分离式Hopkinson压杆(SHPB)标定实验,系统地讨论了传感器的动态响应特性,其中包括测量电路、PVDF表面应力集中、压电计的材料及结构特性和同一压电计受多次撞击对测试信号的影响,为PVDF压电计的制作工艺研究提供参考。利用标定好的压电计测试了橡胶材料在SHPB实验中的动态应力均匀过程。结果表明:调节并联电阻值可以提高压电计的传感精度;增大压电计的敏感面积可以减小因应力集中所造成的信号失真;材料的热粘塑性性质、摩擦效应等将使信号振荡幅度偏小;多次撞击对信号的加载与卸载段都将产生影响,但当传感器表面未发生明显损伤时,测试的应力平台平均值与真实信号近似相同。     

二级轻气炮发射过程中前冲气体的初步研究

 在二级轻气炮发射过程中,靶室内的残存气体和绕行到弹丸前方的推进气体都有可能对实验结果造成影响。利用石英传感器测量并得到了二级轻气炮高速弹丸发射时前冲气体的压力信号,并计算得到了相应的压力。实验结果表明：二级轻气炮发射时确实存在前冲气体现象,但其压力幅值较小,约为10^-2 GPa量级,不会对高压物理实验的结果造成明显的影响。     

126.5 GPa准静水压下的光谱学实验

 本文介绍了作者利用国内加工的金刚石压砧装置及组建的微区光谱系统进行100 GPa（百万大气压）准静水压光谱学实验的概况，证明压力产生装置和微区光谱系统的多功能性是充分可靠的。实验中遇到的压力产生能力超过压力测量能力的事实，反映了高压光谱学实验在压力范围扩大时所遇到的挑战。文中对高压下的拉曼、发射、吸收及反射光谱的实验原理和实验方法也作了概略的介绍。     

Permanent densification of silica glass for pressure calibration between 9 and 20 GPa at ambient temperature

Permanent density increase of silica glass was used to calibrate pressure generation delivered by cupped sintered diamond anvils (‘dimple anvils’) [Haberl B, Molaison JJ, Neuefeind JC, et al. Simple modified Bridgman anvil design for high pressure synthesis and neutron scattering. High Press. Res. submitted] within the Paris-Edinburgh press between approximately 9 and 20?GPa. Raman spectral changes of recovered silica glass with increased density were used to determine the maximum pressure reached by following an established calibration curve [Deschamps T, Kassir-Bodon A, Sonneville C, et al. Permanent densification of compressed silica glass: a Raman-density calibration curve. J. Phys. Condens. Matter. 2013;25:025402]. The monotonic Raman shift of the Main Band spectral region (～200–700?cm^?1) of silica glass recovered from 9 to 20?GPa allows for continuous pressure calibration and is applicable to all presses that operate within this pressure range. Radial & axial Raman profiles were conducted to determine the pressure distribution within the sample chamber. This technique has been verified by in situ resistance measurements of the insulator-to-metal phase transition of ZnS near 15?GPa.     

Superconducting phase diagram of Li metal in nearly hydrostatic pressures up to 67 GPa

The dependence of the superconducting transition temperature T(c) on nearly hydrostatic pressure has been determined to 67 GPa in an ac susceptibility measurement for a Li sample embedded in helium pressure medium. With increasing pressure, superconductivity appears at 5.47 K for 20.3 GPa, T(c) rising rapidly to approximately 14 K at 30 GPa. The T(c)(P) dependence to 67 GPa differs significantly from that observed in previous studies where no pressure medium was used. Evidence is given that superconductivity in Li competes with symmetry breaking structural phase transitions which occur near 20, 30, and 62 GPa. In the pressure range 20-30 GPa, T(c) is found to decrease rapidly in a dc magnetic field, the first evidence that Li is a type I superconductor.     

An ionization gauge with plane electrode system and emission current modulation

The paper is devoted to the study of an ionization gauge with parallel plane electrodes. It deals with the emission current modulation by means of a low-frequency signal, and in particular with the question of the ratio of the anode current to the total emission current and with the effect of this ratio on the ion current. Next it presents the calibration curves of gauges without and with the emission current modulation, and discusses the effect of the capacity between the ion collector and the modulator grid on the lower limit of the gauge measuring range. The results of the gauge calibration in a magnetic field, which prove the usefulness of the gauge for pressure measurements in magnetic fields of variable magnitude, are given in the conclusion of the paper.In conclusion the atuhor wishes to express his thanks to Professor Dr. V. Kunz! for the stimulus to the preparation of this paper, and to A. Ryska and J. Bla~ek for the construction of experimental gauges and for the making of some of the preliminary experiments.     

十种稀土金属电阻的压力效应

 使用Bundy和Dunn发展起来的带有烧结金刚石砧的Drickamer型高压装置，用固定点测压法标定实验压力，在室温及0~43 GPa的压力范围内测量了稀土金属中Pr、Nd、Sm、Gd、Tb、Dy、Ho、Tm、Lu和Yb的电阻随压力的变化。在各稀土元素的电阻随压力变化的曲线上，观测到了若干“凸起”和斜率突变点，根据Jayaraman提出的三价稀土在压力作用下的相变顺序，得到了这些突（凸）变点分别对应着hcp→Sm-type→dhcp→fcc相变顺序中的某一类型的相变压力。此外还观测到了Pr、Gd、Tb的fcc相随着压力再增高而发生的相变，根据已报导的关于Pr的工作，推测Gd和Tb的这一相变应为fcc→dfcc相变，它们分别发生在22.0和24.5 GPa。在本工作所得结果基础上对Johansson的三价稀土总相图进行了修正。     

High pressure electrical transport behavior in organic semiconductor pentacene

The high pressure electrical transport behavior of pentacene has been investigated by alternating current impedance techniques and direct current resistivity measurement in a diamond anvil cell (DAC). The resistance decreases with increasing pressure below 17.4?GPa, while it increases above 17.4?GPa, which is caused by the transition of pentacene from an ordered state to the disordered state under higher pressure. From the Raman spectra under various pressures, pentacene becomes amorphous above 17.3?GPa, which is consistent with the impedance results. The charge transport operates in the hopping regime with charges jumping between interacting molecules, and the hopping mechanisms are related to the vibration modes. Above 17.4?GPa, the pressure dependence of the relaxation activation energy is 21.7?meV/GPa and pentacene keeps semiconductor characteristics up to 28.3?GPa.     

Performance on absolute scattering intensity calibration and protein molecular weight determination at BL16B1, a dedicated SAXS beamline at SSRF

The optical system and end‐station of bending‐magnet beamline BL16B1, dedicated to small‐angle X‐ray scattering (SAXS) at the Shanghai Synchrotron Radiation Facility, is described. Constructed in 2009 and upgraded in 2013, this beamline has been open to users since May 2009 and supports methodologies including SAXS, wide‐angle X‐ray scattering (WAXS), simultaneous SAXS/WAXS, grazing‐incidence small‐angle X‐ray scattering (GISAXS) and anomalous small‐angle X‐ray scattering (ASAXS). Considering that an increasing necessity for absolute calibration of SAXS intensity has been recognized in in‐depth investigations, SAXS intensity is re‐stated according to the extent of data processing, and the absolute intensity is suggested to be a unified presentation of SAXS data in this article. Theory with a practical procedure for absolute intensity calibration is established based on BL16B1, using glass carbon and water as primary and secondary standards, respectively. The calibration procedure can be completed in minutes and shows good reliability under different conditions. An empirical line of scale factor estimation is also established for any specific SAXS setup at the beamline. Beamline performance on molecular weight (MW) determination is provided as a straightforward application and verification of the absolute intensity calibration. Results show good accuracy with a deviation of less than 10% compared with the known value, which is also the best attainable accuracy in recent studies using SAXS to measure protein MW. Fast MW measurement following the demonstrated method also enables an instant check or pre‐diagnosis of the SAXS performance to improve the data acquisition.