Combined ultrasonic elastic wave velocity and microtomography measurements at high pressures

Combined ultrasonic and microtomographic measurements were conducted for simultaneous determination of elastic property and density of noncrystalline materials at high pressures. A Paris-Edinburgh anvil cell was placed in a rotation apparatus, which enabled us to take a series of x-ray radiography images under pressure over a 180° angle range and construct accurately the three-dimensional sample volume using microtomography. In addition, ultrasonic elastic wave velocity measurements were carried out simultaneously using the pulse reflection method with a 10° Y-cut LiNbO(3) transducer attached to the end of the lower anvil. Combined ultrasonic and microtomographic measurements were carried out for SiO(2) glass up to 2.6 GPa and room temperature. A decrease in elastic wave velocities of the SiO(2) glass was observed with increasing pressure, in agreement with previous studies. The simultaneous measurements on elastic wave velocities and density allowed us to derive bulk (K(s)) and shear (G) moduli as a function of pressure. K(s) and G of the SiO(2) glass also decreased with increasing pressure. The negative pressure dependence of K(s) is stronger than that of G, and as a result the value of K(s) became similar to G at 2.0-2.6 GPa. There is no reason why we cannot apply this new technique to high temperatures as well. Hence the results demonstrate that the combined ultrasonic and microtomography technique is a powerful tool to derive advanced (accurate) P-V-K(s)-G-(T) equations of state for noncrystalline materials.     

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.     

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.     

Wire-mesh sensors for high-resolving two-phase flow studies at high pressures and temperatures

Wire-mesh sensors are used for a high-speed visualization of a gas–liquid flow as well as for the measurement of void fraction profiles, bubble size distributions and gas velocity distributions. Recent progress was made in designing and constructing such sensors for an application in a hot steam–water mixture. Two types are presented: (1) a sensor with an inner diameter of 52.3 mm with a measuring matrix of 16×16 and (2) a sensor of 195 mm inner diameter with 64×64 measuring points. Both devices can be operated at 7 MPa and a temperature of max. 286 ^∘C. The spatial and temporal resolutions are equal to earlier used sensors for air–water flow at ambient conditions (3 mm, 2500 fps). In the paper, the function of the sensors is illustrated by presenting flow visualizations obtained at two vertical test sections of the Rossendorf TOPFLOW facility. The pipes are approximately 9 m long and have inner diameters equal to the diameters of the measuring cross sections mentioned above. The results show how the flow structure depends on the thermodynamic parameters by comparing measurements performed at 1, 2, 4 and 6.5 MPa and 180, 212, 250 and 280 ^∘C, correspondingly, under adiabatic conditions with earlier air–water tests.     

Dynamic properties of outwardly propagating spherical hydrogen-air flames at high temperatures and pressures

Computational experiments on fundamental unstretched laminar burning velocities and flame response to stretch (represented by the Markstein number) of hydrogen-air flames at high temperatures and pressures were conducted in order to understand the dynamics of the flames including hydrogen as an attractive energy carrier in conditions encountered in practical applications such as internal combustion engines. Outwardly propagating spherical premixed flames were considered for a fuel-equivalence ratio of 0.6, pressures of 5 to 50 atm, and temperatures of 298 to 1000 K. For these conditions, ratios of unstretched-to-stretched laminar burning velocities varied linearly with flame stretch (represented by the Karlovitz number), similar to the flames at normal temperature and normal to moderately elevated pressures, implying that the “local conditions” hypothesis can be extended to the practical conditions. Increasing temperatures tended to reduce tendencies toward preferential-diffusion instability behavior (increasing the Markstein number) whereas increasing pressures tended to increase tendencies toward preferential-diffusion instability behavior (decreasing the Markstein number).     

Simultaneous measurement of CO and CO2 at elevated temperatures by diode laser wavelength modulated spectroscopy

One single semiconductor distributed-feedback (DFB) laser is used to demonstrate the possibility of simultaneous measurements of CO and CO₂ at elevated temperatures. Wavelength modulation spectroscopy with second-harmonic detection is used to improve the detection sensitivity and accuracy. The concentrations of CO and CO₂ are determined from the WMS-1-normalized absorption-based WMS-2f signal peak heights of a proper line pair of CO and CO₂ near 6357.814 cm⁻¹ and 6357.312 cm⁻¹, which are selected using some line-selection criterions for the target temperature range of 300–1000 K. The CO and CO₂ concentrations measurements are within 2.86% and 2.69% of the expected values over the tested temperature range 300–1000 K. The minimum detectable concentrations of CO and CO₂ at 1000 K are 250 ppm m and 280 ppm m respectively.     

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.     

High efficiency multichannel collimator for structural studies of liquids and low-Z materials at high pressures and temperatures

A high efficiency multichannel collimator (MCC) device has been developed at the high pressure beamline ID27 of the European Synchrotron Radiation Facility to drastically reduce the x-ray background from the sample environment in the Paris-Edinburgh press. The main technical difficulty, which resides in the minimum slits size achievable using the classical mono-bloc design, has been resolved using an original concept based on a set of independent slits. Then, a very small slit size of 50 μm was manufactured resulting in a great improvement of the signal to background ratio. In addition, the transfer function of the MCC has been measured using the x-ray diffusion signal of a metal doped glass and efficiently applied to correct the raw data. The potential of this new device is illustrated in two challenging examples: iron-sulfur liquid structures and C(60) polymerization process at high pressure and high temperature.     

Method for the determination of the specific heat of metals at low temperatures under high pressures

Efforts are made to determine the absolute specific heat of metals as a function of pressure with an accuracy, which, for the first time, will permit a direct evaluation of the pressure variation of the electronic and phonon parameters gamma and vartheta(D'), respectively. This is achieved by employing the ac method of Sullivan and Seidel, and choosing a suitable sample configuration within a piston-cylinder pressure cell. Essential is the use of diamond powder as a pressure transmitting medium, which because of its low heat capacity and high thermal resistance, couples the sample loosely to the temperature bath, represented by the pressure cylinder. Thus, the thermal requirements of the ac method are met, and corrections--if necessary--are fully tractable. High sensitivity even at the lowest temperatures is obtained by the use of thin slices, prepared from standard carbon resistors, for thermometers. Although delicate, these sensors withstand pressures of more than 20 kbars and remain sensitive. A thorough comparison of results on indium with the literature data at zero pressure is undertaken. It shows that the accuracy of the present results is comparable with that from literature data. Preliminary results at pressures up to 8 kbar are shown; they will be discussed in a separate paper.     

Development of a simultaneous Hugoniot and temperature measurement for preheated-metal shock experiments: melting temperatures of Ta at pressures of 100 GPa

Equations of state of metals are important issues in earth science and planetary science. A major limitation of them is the lack of experimental data for determining pressure-volume and temperature of shocked metal simultaneously. By measuring them in a single experiment, a major source of systematic error is eliminated in determining from which shock pressure release pressure originates. Hence, a non-contact fast optical method was developed and demonstrated to simultaneously measure a Hugoniot pressure-volume (P(H)-V(H)) point and interfacial temperature T(R) on the release of Hugoniot pressure (P(R)) for preheated metals up to 1000 K. Experimental details in our investigation are (i) a Ni-Cr resistance coil field placed around the metal specimen to generate a controllable and stable heating source, (ii) a fiber-optic probe with an optical lens coupling system and optical pyrometer with ns time resolution to carry out non-contact fast optical measurements for determining P(H)-V(H) and T(R). The shock response of preheated tantalum (Ta) at 773 K was investigated in our work. Measured data for shock velocity versus particle velocity at an initial state of room temperature was in agreement with previous shock compression results, while the measured shock data between 248 and 307 GPa initially heated to 773 K were below the Hugoniot evaluation from its off-Hugoniot states. Obtained interfacial temperatures on release of Hugoniot pressures (100-170 GPa) were in agreement with shock-melting points at initial ambient condition and ab initio calculations of melting curve. It indicates a good consistency for shock melting data of Ta at different initial temperatures. Our combined diagnostics for Hugoniot and temperature provides an important approach for studying EOS and the temperature effect of shocked metals. In particular, our measured melting temperatures of Ta address the current controversy about the difference by more than a factor of 2 between the melting temperatures measured under shock and those measured in a laser-heated diamond anvil cell at ～100 GPa.     

Note: a sample holder design for sensitive magnetic measurements at high temperatures in a magnetic properties measurement system

A sample holder design for high temperature measurements in a commercial MPMS SQUID magnetometer from Quantum Design is presented. It fulfills the requirements for the simultaneous use of the oven and reciprocating sample option (RSO) options, thus allowing sensitive magnetic measurements up to 800 K. Alternating current susceptibility can also be measured, since the holder does not induce any phase shift relative to the ac driven field. It is easily fabricated by twisting Constantan? wires into a braid nesting the sample inside. This design ensures that the sample be placed tightly into a tough holder with its orientation fixed, and prevents any sample displacement during the fast movements of the RSO transport, up to high temperatures.     

Simultaneous measurement of the velocity of an ultrasonic shear wave and the thickness of a test object with plane-parallel boundaries using two antenna arrays

Methods for the determination of the unknown velocity of the propagation of shear US waves and the unknown thickness of a test object were considered. Two antenna arrays working in the double-scanning mode, where echo signals are recorded, which were emitted and received by all pairs of antenna-array elements, were suggested. Antenna arrays on prisms were mounted on the test-object surface towards each other. An algorithm for the treatment of measured echo signals was designed using a method that is similar to the least-squares method. The use of the algorithm enables one to simultaneously determine the sound velocity and thickness of a test object with plane-parallel boundaries with an exactness greater than 0.5%. In this article, the factors were studied that affect the exactness of measurements and methods of their elimination or minimization. The results of numerical experiments and the use of the method on three samples relative to measurements using an IN-5101A instrument are given.     

A stiff scanning tunneling microscopy head for measurement at low temperatures and in high magnetic fields

We have developed a measurement head for scanning tunneling microscopy (STM) and specifically for spectroscopic imaging STM which is optimized for high mechanical stiffness and good thermal conductivity by choice of material. The main components of the microscope head are made of sapphire. Sapphire has been chosen from several competing possibilities based on finite element modeling of the fundamental vibrational modes of the body. We demonstrate operation of the STM head in topographic imaging and tunneling spectroscopy at temperatures down to below 2 K.     

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.     

Synchrotron x-ray spectroscopy of EuHNO3 aqueous solutions at high temperatures and pressures and Nb-bearing silicate melt phases coexisting with hydrothermal fluids using a modified hydrothermal diamond anvil cell and rail assembly

A modified hydrothermal diamond anvil cell (HDAC) rail assembly has been constructed for making synchrotron x-ray absorption spectroscopy, x-ray fluorescence, and x-ray mapping measurements on fluids or solid phases in contact with hydrothermal fluids up to approximately 900 degrees C and 700 MPa. The diamond anvils of the HDAC are modified by laser milling grooves or holes, for the reduction of attenuation of incident and fluorescent x rays and sample cavities. The modified HDAC rail assembly has flexibility in design for measurement of light elements at low concentrations or heavy elements at trace levels in the sample and the capability to probe minute individual phases of a multiphase fluid-based system using focused x-ray microbeam. The supporting rail allows for uniform translation of the HDAC, rotation and tilt stages, and a focusing mirror, which is used to illuminate the sample for visual observation using a microscope, relative to the direction of the incident x-ray beam. A structure study of Eu(III) aqua ion behavior in high-temperature aqueous solutions and a study of Nb partitioning and coordination in a silicate melt in contact with a hydrothermal fluid are described as applications utilizing the modified HDAC rail assembly.     

Development of a nuclear magnetic resonance system for in situ analysis of hydrogen storage materials under high pressures and temperatures

A NMR system for in situ analysis of hydrogen storage materials under high pressure and temperature conditions was developed. The system consists of a gas pressure and flow rate controlling unit, a temperature controller, a high temperature NMR probe tunable for both (1)H and other nuclei, and a sample tube holder. Sample temperature can be controlled up to 623 K by heated N(2) gas flow. Sample tube atmosphere can be substituted by either H(2) or Ar and can be pressurized up to 1 MPa under constant flow rate up to 100 ml/min. During the NMR measurement, the pressure can be adjusted easily by just handle a back pressure valve. On the blank NMR measurement, (1)H background noise was confirmed to be very low. (1)H and (11)B NMR spectrum of LiBH(4) were successfully observed at high temperature for the demonstration of the system. The intensity of the (1)H NMR spectra of H(2) gas was also confirmed to be proportional to the applied pressure.     

Simultaneous measurement of magnetization and magnetostriction in 50 T pulsed high magnetic fields

To simultaneously perform magnetization and magnetostriction measurements in high magnetic fields, a miniaturized device was developed that combines an inductive magnetometer with a capacitive dilatometer and, therefore, it is called "dilamagmeter." This combination of magnetic and magnetoelastic investigations is a new step to a complex understanding of solid state properties. The whole system can be mounted in a 12 mm clear bore of any cryostat usually used in nondestructive pulsed high field magnets. The sensitivity of both methods is about 10(-5) A m(2) for magnetization and 10(-5) relative changes in length for striction measurements. Measurements on a GdSi single crystal, which are corrected by the background signal of the experimental setup, agree well with the results of steady field experiments. All test measurements, which are up until now performed in the temperature range of 4-100 K, confirm the perfect usability and high stability in pulsed fields up to 50 T with a pulse duration of 10 ms.     

Pressure dependence of mass burning rates in diluent premixed flames of H2/O2 at high pressures

Pressure dependence of mass burning of diluted hydrogen premixed flames is studied numerically over a full range of pressure. Mass burning rate is selected to be a parameter for burning capability of flames. First, positive linear dependence of mass burning rate has been confirmed at low pressures and negative pressure dependence has appeared in the medium range of pressure, which complies with the results reported in previous experimental works. And then, when the pressure range is extended more, positive pressure dependence is recovered or shows up again at high pressures. The flame structures of temperature and species profiles in each pressure regime are demonstrated. They show that the latter two dependences of negative and positive can be explained by enhanced recombination reactions producing HO₂ at high pressures and chain re-branching to OH production via H₂O₂, respectively. There are three distinct dependences of mass burning or global chemistry in hydrogen flames. Two onset pressures, at which pressure dependence changes, depend on equivalence ratio, degree of dilution, diluent species, and unburned-gas temperature. Accordingly, the onset pressure can be used as a parameter characterizing burning of premixed flames.     

The interfacial transfer of aluminium to steels and ceramic materials under loaded contact at high temperatures II: Both surfaces at high temperatures

The rolling contact between aluminium strips and rolls of different materials, in which the rolls were heated in situ with an auxiliary furnace to a temperature similar to that of the strips, was studied. Rolls of solid alumina failed during the rolling of the aluminium strip; all the other rolls, including plasma spray-coated rolls, remained undamaged. Examination of the structure and composition of the coatings which developed on the rolls showed that there was more transfer for all the different rolls but that the variations between the rolls were much less than they were when the rolls were at ambient temperatures. The thick coatings formed on the rolls were predominantly aluminium metal and the characteristic structure was independent of the original roll surface structures.     

一重载高速机械臂的结构与控制同时设计

拟订了机械臂的工作原理,建立了机械臂的受控动力学方程,运用优化算法设计了PD控制器的增益,计算了机械臂在不同角度下的刚体动力学响应。为了确定合理的机械臂截面尺寸,运用有限元法建立了机械臂的弹性动力学方程,求解了不同截面尺寸下的机械臂弹性动力响应,评价了机械臂的弹性振动。实践证明,所确定的机械和控制设计方案满足设计要求。