Piston-cylinder Pressure Cell Research Articles

Three-wall piston-cylinder type pressure cell for muon-spin rotation/relaxation experiments

ABSTRACT A three-wall piston-cylinder type high pressure cell for muon-spin rotation/relaxation experiments was designed, manufactured, tested and commissioned. The outer cylinder of the cell body is made from MP35N and the middle and inner cylinders are made from NiCrAl nonmagnetic alloys. The mechanical design and performance of the pressure cell are evaluated and optimised using finite-element analysis. The outcomes of the experimental testing closely match the modelling results. The high pressure cell is shown to reach pressure of up to 3.3 GPa at ambient temperature, corresponding to 3.0 GPa at low temperatures, without irreversible damage.

Y3Ba5Cu8Ox Superconductor Under Hydrostatic Pressure

Superconducting Y3Ba5Cu8O18 samples were prepared by standard solid-state reaction method in comparison with Y1Ba2Cu3O7 sample. Resistance vs. temperature of both samples was measured under hydrostatic pressures up to 0.93 GPa using a piston–cylinder pressure cell. Applying the pressure resulted in a decrease in resistance in the normal state and an increase of the transition temperature Tc for both polycrystalline samples. This phenomenon is then explained in terms of the increase in carrier concentrations. Our results show a positive value of $${\mathrm{dT}}_{\mathrm{c}}/\mathrm{dP}$$ =1.1 K/GPa and 1.4 K/GPa for Y123 and Y358, respectively.

Fabrication and evaluation via nuclear quadrupole resonance of a palm cubic-anvil pressure cell.

A "palm" cubic-anvil pressure cell (PCAC) having an outer diameter of 60 mm, the smallest cubic-anvil cell to date, was fabricated to insert in a large-bore superconducting magnet. The pressure cell has a sample space of ϕ 2.5 × 1.5 mm2, which is fairly large for a pressure cell that can reach a high pressure above 4 GPa. Pressure homogeneity was monitored from the 63Cu nuclear-quadrupole-resonance linewidth of Cu2O up to 6.7 GPa. The linewidth first increased with increasing pressure up to 4 GPa and then saturated above 4 GPa. The pressure homogeneity was better than that of a piston-cylinder pressure cell. The PCAC is advantageous because a large sample space and high pressure homogeneity are secured even at high pressures.

Measurements of elastoresistance under pressure by combining in-situ tunable quasi-uniaxial stress with hydrostatic pressure

Uniaxial stress, as well as hydrostatic pressure are often used to tune material properties in condensed matter physics. Here, we present a setup that allows for the study of the combined effects of quasi-uniaxial stress and hydrostatic pressure. Following earlier designs for measurements under finite stress at ambient pressures [e.g., Chu et al., Science 337, 710 (2012)], the present setup utilizes a piezoelectric actuator to change stress in situ inside the piston-cylinder pressure cell. We show that the actuator can be operated over the full temperature (from 30 K up to 260 K) and pressure range (up to ≈2 GPa), resulting in a clear and measurable quasi-uniaxial strain. To demonstrate functionality, measurements of the elastoresistance (i.e., the change of resistance of a sample as a response to quasi-uniaxial strain) under finite hydrostatic pressure on the iron-based compound BaFe2As2 are presented as a proof-of-principle example and discussed in the framework of electronic nematicity. Overall, this work introduces the combination of in situ tunable quasi-uniaxial stress and large (up to ≈2 GPa) hydrostatic pressure as a powerful combination in the study of novel electronic phases. In addition, it also points toward further technical advancements which can be made in the future.

Use of Cernox thermometers in AC specific heat measurements under pressure.

We report on the resistance behavior of bare-chip Cernox thermometers under pressures up to 2 GPa, generated in a piston-cylinder pressure cell. Our results clearly show that Cernox thermometers, frequently used in low-temperature experiments due to their high sensitivity, remain highly sensitive even under applied pressure. We show that these thermometers are therefore ideally suited for measurements of heat capacity under pressure utilizing an ac oscillation technique up to at least 150 K. Our Cernox-based system is very accurate in determining changes in the specific heat as a function of pressure as demonstrated by measurements of the heat capacity on three different test cases: (i) the superconducting transition in elemental Pb (Tc = 7.2 K), (ii) the antiferromagnetic transition in the rare-earth compound GdNiGe3 (TN = 26 K), and (iii) the structural/magnetic transition in the iron-pnictide BaFe2As2 (Ts,N = 130 K). The chosen examples demonstrate the versatility of our technique for measuring the specific heat under the pressure of various condensed-matter systems with very different transition temperatures as well as amounts of removed entropy.

29Si NMR of aqueous silicate complexes at gigapascal pressures

Geochemists have models to predict solute speciation and mineral equilibria in aqueous solutions up to 1200 °C and 6 GPa. These models are useful to uncover reaction pathways deep in the Earth, though experimental confirmation is extremely difficult. Here we show speciation changes among aqueous silicate complexes to pressures of 1.8 GPa through use of a high-pressure solution-state NMR probe. The radiofrequency circuit uses a microcoil geometry that is coupled with a piston-cylinder pressure cell to generate and maintain these high pressures. The 1.8 GPa pressure corresponds to pressures reached at the lower crust or upper mantle. Although these experiments are limited to ambient temperature, we show that the increased pressure affects complexation and oligomerization reactions by eliminating bulk waters and that the pressure effects are completely reversible.

Development and application of 2.5 GPa–25 T high-pressure high-field electron spin resonance system using a cryogen-free superconducting magnet

We have developed a high-pressure electron spin resonance probe and successfully installed into the world’s highest-field cryogen-free superconducting magnet having a maximum central field of 24.6 T. The high pressure of 2.5 GPa is achieved by the specially designed piston-cylinder pressure cell using THz-wave-transparent components. In the first application of this high-pressure high-field ESR system, we observed that the orthogonal dimer spin system SrCu2(BO3)2 undergoes a quantum phase transition from the dimer singlet ground to the plaquette singlet ground states.

A low-background piston–cylinder-type hybrid high pressure cell for muon-spin rotation/relaxation experiments

ABSTRACTA low background double-wall piston–cylinder-type pressure cell is developed at the Paul Scherrer Institute. The cell is made from BERYLCO-25 (beryllium copper) and MP35N nonmagnetic alloys with the design and dimensions which are specifically adapted to muon-spin rotation/relaxation (μSR) measurements. The mechanical design and performance of the pressure cell are evaluated using finite-element analysis (FEA). By including the measured stress-strain characteristics of the materials into the finite-element model, the cell dimensions are optimized with the aim to reach the highest possible pressure while maintaining the sample space large (6 mm in diameter and 12 mm high). The presented unconventional design of the double-wall piston–cylinder pressure cell with a harder outer MP35N sleeve and a softer inner CuBe cylinder enables pressures of up to 2.6 GPa to be reached at ambient temperature, corresponding to 2.2 GPa at low temperatures without any irreversible damage to the pressure cell. The nature of the muon stopping distribution, mainly in the sample and in the CuBe cylinder, results in a low-background μSR signal.

Development of an optical time-resolved measurement system under high-pressure and low-temperature with a piston-cylinder pressure cell.

To perform the femtosecond pump-probe spectroscopy under high pressure and low temperature, we constructed a measurement system with a piston cylinder type pressure cell installing an optical fiber bundle. The applied pressure was achieved to 6 kbar and the cell was cooled down to 15 K. Several demonstrations revealed that broadening and change of polarization of pulse (duration of ∼120 fs) owing to the dispersions in the fiber bundle are much small indicating that those have little influence on the measurement of carrier relaxation dynamics. In the measurements of κ-(BEDT-TTF)2Cu(NCS)2 under 1.3 kbar at 43 K, we have successfully detected the polarization anisotropy of the carrier relaxation dynamics and estimated the decay time in the same way as the normal measurement.

Development of multi-frequency ESR system for high-pressure measurements up to 2.5 GPa

A new piston-cylinder pressure cell for electron spin resonance (ESR) has been developed. The pressure cell consists of a double-layer hybrid-type cylinder with internal components made of the ZrO2-based ceramics. It can generate a pressure of 2GPa repeatedly and reaches a maximum pressure of around 2.5GPa. A high-pressure ESR system using a cryogen-free superconducting magnet up 10T has also been developed for this hybrid-type pressure cell. The frequency region is from 50GHz to 400GHz. This is the first time a pressure above 2GPa has been achieved in multi-frequency ESR system using a piston-cylinder pressure cell. We demonstrate its potential by showing the results of the high-pressure ESR of the S=1 system with the single ion anisotropy NiSnCl6·6H2O and the S=1/2 quantum spin system CsCuCl3. We performed ESR measurements of these systems above 2GPa successfully.

Development of High-Pressure and Multi-Frequency ESR System and Its Application to Quantum Spin System

We have developed a high-pressure and multi-frequency electron spin resonance (ESR) system in the submillimeter wave region. The pressure is generated by the piston–cylinder pressure cell whose inner parts are all made of ceramics. The requirements for the inner parts of the pressure cell are toughness and transmission in the submillimeter wave region and they enable us to observe the transmitted light through a sample subjected to high pressure. It was found that both properties can be achieved by the combination of the inner parts made of the ZrO2-based ceramic and the Al2O3 ceramic. For the Shastry-Sutherland compound SrCu2(BO3)2, we observed the direct ESR transition from the singlet ground state to the first excited triplet sates at 1.5 GPa successfully in the frequency region from 300 to 700 GHz.

Development of High-Pressure ESR System Using Micro-coil

We have developed the high-pressure electron spin resonance (ESR) system using a micro-coil in the frequency region up to around 2 GHz and potentially 10 GHz. The hybrid-type piston-cylinder pressure cell whose maximum pressure reaches 4 GPa was used. In this study, we obtained ESR spectra at 2.3 GPa successfully, which can never be obtained by the single-layer piston-cylinder pressure cell. The minimum detectable spin number was estimated to be the order of 1012 spins/G. Moreover, it is shown that the sensitivity can be improved by two orders of magnitude using the field modulation technique. This high-pressure ESR technique is a promising one to achieve the sensitivity and the high pressure simultaneously.

High-pressure environments of single crystal neutron diffractometer SENJU/J-PARC

High-pressure technique is a powerful tool for physical property measurements and structural analyses as well as other external conditions, such as magnetic fields and temperatures. In the field of neutron experiments, measurements under high-pressure conditions are also useful and attractive; because pressure is one of important thermodynamic parameter that can be used to tune magnetic property, crystal field, and other parameters to obtain insight into the microscopic physics of many phenomena. SENJU have been constructed for a single crystal time-of-flight neutron Laue diffractometer at beamline 18 (BL18) of Materials and Life Science Experimental Facility (MLF) at Japan Proton Accelerator Research Complex (J-PARC) [1], designed in consideration of precise crystal and magnetic structure analyses for small size single crystals, 1 mm3 or less in volume: and also taking account of the neutron diffraction measurements under multiple extreme conditions. In this research we are planning to introduce high-pressure sample environments into SENJU. Two types of compact high-pressure cells have been prepared, one is clamp type piston-cylinder cell made of copper-beryllium alloy (< 2 GPa), and the other is clamp type opposite anvil cell, can be expected to reach maximum pressure of 10 GPa. A taurine single crystal (3 mm3) was enclosed in the piston-cylinder pressure cell together with deuterated glycerol (pressure transmitting medium) and pressurized up to 1 GPa. Accelerator power of J-PARC was 300 kW and the exposure time was 6 hours. We can observe many distinct Bragg reflections from the sample crystal (taurine) even through the pressure cell body, as shown in the figure. In this presentation, we will show more details and current status of high-pressure sample environments in SENJU.

A high-pressure NMR probe for aqueous geochemistry.

A non-magnetic piston-cylinder pressure cell is presented for solution-state NMR spectroscopy at geochemical pressures. The probe has been calibrated up to 20 kbar using in situ ruby fluorescence and allows for the measurement of pressure dependencies of a wide variety of NMR-active nuclei with as little as 10 μL of sample in a microcoil. Initial (11)B NMR spectroscopy of the H3BO3-catechol equilibria reveals a large pressure-driven exchange rate and a negative pressure-dependent activation volume, reflecting increased solvation and electrostriction upon boron-catecholate formation. The inexpensive probe design doubles the current pressure range available for solution NMR spectroscopy and is particularly important to advance the field of aqueous geochemistry.

Development of High-Field ESR System Using SQUID Magnetometer and its Application to Measurement under High Pressure

We have developed a high-field and high-frequency ESR system using a commercially available magnetometer equipped with the superconducting quantum interference device (SQUID). This is magnetization detection type ESR and ESR is observed as a change of the magnetization at the resonance condition under irradiation of the electromagnetic wave. The frequency range is from 70 to 315 GHz and the maximum magnetic field is 5 T. The sensitivity is estimated to be 10 13 spins/G. The advantage of this system is that the high-field ESR measurements can be made very easily and quantitatively. Moreover, this high-field ESR can be applied to the measurements under pressure by using a widely used piston-cylinder pressure cell.

Pressure Effects on Emim[FeCl4], a Magnetic Ionic Liquid with Three-Dimensional Magnetic Ordering

We report a combined study using magnetization and Raman spectroscopy on the magnetic ionic liquid 1-ethyl-3-methylimidazolium tetrachloroferrate, Emim[FeCl4]. This material shows a long-range antiferromagnetic ordering below the Néel temperature T(N) ≈ 3.8 K. The effects of pressure on the magnetic properties have been studied using a miniature piston-cylinder CuBe pressure cell. This three-dimensional ordering is strongly influenced when hydrostatic pressure is applied. It is observed that low applied pressure is enough to modify the magnetic interactions, inducing a transition from antiferromagnetic to ferrimagnetic ordering. Raman spectroscopy measurements reveal important information about the existence of isolated [FeCl4](-) anions and the absence of dimeric [Fe2Cl7](-) units in the liquid and solid states. These features seem to suggest that the superexchange pathways responsible for the appearance of magnetic ordering are mediated through Fe-Cl-Cl-Fe. Furthermore, the liquid-solid phase transition exhibits a magnetic hysteresis near room temperature, which can be tuned by weak pressures.

Development of Hybrid-Type Pressure Cell for High-Pressure and High-Field ESR Measurement

A hybrid-type piston-cylinder pressure cell for the electron spin resonance (ESR) measurement has been developed. The cylinder of this pressure cell consists of a NiCrAl inner cylinder and a CuBe outer sleeve, and all inner parts are made of zirconium oxide which has good transmittance to the millimeter and submillimeter waves. We confirmed that the pressure reaches 2.1 GPa. We have also developed a transmission-type high-field ESR system having two different modulation methods for this pressure cell. A test measurement without pressure cell for the two-dimensional orthogonal-dimer spin system of SrCu2(BO3)2 has been done successfully in the wide frequency region. The combination of this electromagnetic wave transmission-type pressure cell and this high-field ESR system is a promising tool for the study of the pressure-induced phase transition of SrCu2(BO3)2.

Development of high-pressure and high-field ESR system using SQUID magnetometer

We have developed a high-pressure and high-field electron spin resonance (ESR) system using the combination of a commercially available superconducting quantum interference device (SQUID) magnetometer and a clamp-type piston cylinder pressure cell. The magnetic field range is up to 5T, and the maximum pressure reaches 1.5GPa. The most characteristic feature of this system is its easy handling as compared with other high-pressure ESR systems. Moreover, the macroscopic magnetization measurement can be performed simultaneously with the microscopic ESR measurement. In addition to these features, the well-established pressure calibration method utilizing the change of superconducting transition temperature of tin can be applied to this system. By using this system, we obtained pressure dependence of the single ion magnetic anisotropy parameter D of NiSnCl6·6H2O up to 1.5GPa precisely, and the magnetization behavior of this material under pressure was explained well by its pressure dependence of the D value.

Large volume high-pressure cell for inelastic neutron scattering

Inelastic neutron scattering measurements typically require two orders of magnitude longer data collection times and larger sample sizes than neutron diffraction studies. Inelastic neutron scattering measurements on pressurised samples are particularly challenging since standard high-pressure apparatus restricts sample volume, attenuates the incident and scattered beams, and contributes background scattering. Here, we present the design of a large volume two-layered piston-cylinder pressure cell with optimised transmission for inelastic neutron scattering experiments. The design and the materials selected for the construction of the cell enable its safe use to a pressure of 1.8 GPa with a sample volume in excess of 400 mm(3). The design of the piston seal eliminates the need for a sample container, thus providing a larger sample volume and reduced absorption. The integrated electrical plug with a manganin pressure gauge offers an accurate measurement of pressure over the whole range of operational temperatures. The performance of the cell is demonstrated by an inelastic neutron scattering study of UGe(2).

Pressure dependence of superconducting-transition temperature of YbGa1.1Si0.9

Pressure dependence of the superconducting transition temperature Tc has been investigated in YbGa1.1Si0.9, which is the AlB2-type layered superconductor with Tc = 2.4 K. The electrical resistivity measurements were carried out under hydrostatic pressure up to 2.5 GPa using a piston-cylinder type pressure cell. With increasing pressure, the Tc of YbGa1.1Si0.9 decreases from 2.4 K to 1.1 K at 2.5 GPa with a pressure derivative of Tc, dTc/dP, of – 0.78 K/GPa. This negative pressure derivative of Tc is similar to the other superconducting AlB2-type silicides. The relative pressure derivative of Tc, dlnTc/dP, for YbGa1.1Si0.9 is – 0.33 GPa−1, which is about ten times larger than those for other layered superconductors.