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At least 91 records · Page 5

Low fractional volume superconductivity in single crystals of Pr{sub 4}Ni{sub 3}O{sub 10} under pressure

Magnetotransport measurements of P⁢r4⁢N⁢i3⁢O10 single crystals performed under externally applied pressures up to 73 GPa in diamond anvil cells with either KBr or Nujol oil as pressure media yield signatures of superconductivity with a maximum onset temperature of approximately 31 K. True zero resistance was not observed, consistent with a nonpercolating superconducting volume fraction. Magnetization measurements provided corroborating evidence of superconductivity, with a pressure-dependent diamagnetic signal occurring below the onset temperature, and an estimate from the absolute value of the susceptibility suggests a superconducting volume fraction on the order of 10%. We observe sample to sample variations in the magnitude and pressure dependence of 𝑇𝑐 as well as a dependence on the configuration of electrical contacts on a given sample. Possible causes of this behavior may be significant inhomogeneities in the pressure and/or damage to the samples induced by the pressure media as well as inhomogeneities in the crystals themselves. The results imply that our as-grown P⁢r4⁢N⁢i3⁢O10 single crystals are not bulk superconductors but that there is a minority structure present within the crystals that is indeed superconductin

Chen, Xinglong↗

Long-Range Ordered Amorphous Atomic Chains as Building Blocks of a Superconducting Quasi-One-Dimensional Crystal

Crystalline and amorphous structures are two of the most common solid-state phases. Crystals having orientational and periodic translation symmetries are usually both short-range and long-range ordered, while amorphous materials have no long-range order. Short-range ordered but long-range disordered materials are generally categorized into amorphous phases. In contrast to the extensively studied crystalline and amorphous phases, the combination of short-range disordered and long-range ordered structures at the atomic level is extremely rare and so far has only been reported for solvated fullerenes under compression. Here, a report on the creation and investigation of a superconducting quasi-1D material with long-range ordered amorphous building blocks is presented. Using a diamond anvil cell, monocrystalline (TaSe4)(2)I is compressed and a system is created where the TaSe(4)atomic chains are in amorphous state without breaking the orientational and periodic translation symmetries of the chain lattice. Strikingly, along with the amorphization of the atomic chains, the insulating (TaSe4)(2)I becomes a superconductor. The data provide critical insight into a new phase of solid-state materials. The findings demonstrate a first ever case where superconductivity is hosted by a lattice with periodic but amorphous constituent atomic chains.

combination of crystalline and amorphous structure↗

Montel mirror based collimating analyzer system for high-pressure resonant inelastic X-ray scattering experiments

Resonant inelastic X-ray scattering (RIXS) is increasingly playing a significant role in studying highly correlated systems, especially since it was proven capable of measuring low-energy magnetic excitations. However, despite high expectations for experimental evidence of novel magnetic phases at high pressure, unequivocal low-energy spectral signatures remain obscured by extrinsic scattering from material surrounding the sample in a diamond anvil cell (DAC): pressure media, Be gasket and the diamond anvils themselves. A scattered X-ray collimation based medium-energy resolution (~100 meV) analyzer system for a RIXS spectrometer at the Ir L 3 -absorption edge has been designed and built to remediate these difficulties. Due to the confocal nature of the analyzer system, the majority of extrinsic scattering is rejected, yielding a clean low-energy excitation spectrum of an iridate Sr 2 IrO 4 sample in a DAC cell. Finally, the energy resolution of different configurations of the collimating and analyzing optics are discussed.

73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗

Experiments at high temperature and pressure - Laser heating through the diamond cell

CW laser heating through a diamond anvil cell by means of a focused Nd:YAG laser has resulted in the achievement of temperatures in the 1500-5000 K range for pressures of 10-100 GPa. Temperatures are determined radiometrically, with an accuracy of about 200 K, and temperature variation across the laser-heated spot is derived by means of spatial filtering with a slit that can be scanned. Melting temperatures are thus determined either on the basis of observed temperature at the liquid-solid interface or on that of the peak temperature at which glass is first produced with increasing laser power.

Jeanloz, R.↗

X-ray diffraction measurements and pressure determination in nanosecond compression of solids up to 600 GPa

X-ray diffraction measurements under laser-driven dynamic compression now allow us to investigate the atomic structure of matter at TPa pressures and thousands of degree temperatures with broad implications for condensed matter physics, planetary science and astronomy. Furthermore, pressure determination in these experiments often relies on velocimetry measurements coupled with modeling that requires accurate knowledge of the optical and thermo-mechanical properties of a window material, resulting in significant systematic uncertainty. Here we demonstrate different approach applicable to X-ray diffraction experiments under quasi-isentropic ramp-compression based on the use of in-situ pressure calibrants, similar to the methods often adopted in static-compression experiments with diamond anvil cells. Focusing on experiments using a diamond window, we discuss challenges and mitigation strategies for the novel approach. Our study, in addition to providing new structural information of 5 metals up to hundreds of GPa, provides validation to the currently used methods based on time-resolved measurement of the diamond free-surface velocity, and reveals that the use of in-situ calibrants enables a factor of four reduction in the pressure uncertainty in these experiments.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Multi-extreme conditions at the Second Target Station

Three concepts for the application of multi-extreme conditions under in situ neutron scattering are described here. The first concept is a neutron diamond anvil cell made from a non-magnetic alloy. It is shrunk in size to fit existing magnets and future magnet designs and is designed for best pressure stability upon cooling. This will allow for maximum pressures above 10 GPa to be applied simultaneously with (steady-state) high magnetic field and (ultra-)low temperature. Additionally, an implementation of miniature coils for neutron diamond cells is presented for pulsed-field applications. The second concept presents a set-up for laser-heating a neutron diamond cell using a defocused CO 2 laser. Cell, anvil, and gasket stability will be achieved through stroboscopic measurements and maximum temperatures of 1500 K are anticipated at pressures to the megabar. The third concept presents a hybrid levitator to enable measurements of solids and liquids at temperatures in excess of 4000 K. This will be accomplished by a combination of bulk induction and surface laser heating and hyperbaric conditions to reduce evaporation rates. The potential for deployment of these multi-extreme environments within this first instrument suite of the Second Target Station is described with a special focus on VERDI, PIONEER, CENTAUR, and CHESS. Furthermore, considerations for deployment on future instruments, such as the one proposed as TITAN, are discussed. Overall, the development of these multi-extremes at the Second Target Station, but also beyond, will be highly advantageous for future experimentation and will give access to parameter space previously not possible for neutron scattering.

47 OTHER INSTRUMENTATION↗

Raman scattering of rhenium for secondary pressure calibration

With the increasing number of 100 s GPa experiments in the diamond anvil cell (DAC), improved accuracy in secondary pressure calibrations to extreme pressures is essential. The rhenium equation of state has been proposed as a pressure calibrant via x-ray diffraction with potentially broad applications as it is commonly used as a gasket material in DAC experiments. In this work, we conducted Raman spectroscopy experiments on rhenium in the DAC and report the pressure shift of the E2g mode, a refined high-pressure C44 and mode-Grüneisen parameter above 200 GPa. We used flat, beveled, and toroidal diamond anvils under quasi-hydrostatic and non-hydrostatic conditions. By measuring the E2g mode from the culet edge to the center, we analyzed pressure distribution based on culet type and distance from the anvil center. The shift in the E2g mode can be expressed as a function of pressure, and diamond edge measurements appear reliable across all anvil types. Comparing the center and edge pressures reveals anvil cupping, offering insights into predicting or preventing anvil failure during materials properties measurements at extreme conditions.

Diamond anvil cells↗

Performance of Carbide Alloy Compounds in Carbon Doped MoNbTaW

In this work, the performance of the carbon doped compositionally complex alloy (CCA) MoNbTaW was studied under ambient and high pressure and high temperature conditions. TaC and NbC carbides were formed when a large concentration of carbon was introduced while synthesizing the MoNbTaW alloy. Both FCC carbides and BCC CCA phases were detected in the sample compound at room temperature, in which the BCC phase was believed to have only refractory elements MoNbTaW while FCC carbide came from TaC and NbC. Carbides in the carbon doped MoNbTaW alloy were very stable since no phase transition was obtained even under 3.1 GPa and 870 °C by employing the resistor-heating diamond anvil cell (DAC) synchrotron X-ray diffraction technique. Via in situ examination, this study confirms the stability of carbides and MoNbTaW in the carbon doped CCA even under high pressure and high temperature.

36 MATERIALS SCIENCE↗

Melting of the Fe–C–H System and Earth's Deep Carbon–Hydrogen Cycle

The occurrences and cycling of slab-originated carbon and hydrogen are considered to be controlled by their reactions with metallic iron from mantle disproportionation and slab serpentinization, to form Fe alloys containing carbon and hydrogen. In this work, we show experimental results on the phase relations and melting of the Fe-C-H system using laser-heated diamond anvil cell and X-ray diffraction techniques up to 72 GPa. The incorporation of hydrogen was found to lower the eutectic melting temperatures of Fe-C alloy by ~50–178 K at 20–70 GPa, facilitating the formation of metallic liquids in the deep mantle and thus enhancing the mobility and deep cycling of subducted carbon and hydrogen. Hydrogen also substitutes with carbon in Fe-C metal to form hydride and diamond at relatively high-temperature conditions (e.g., 42.6 GPa, >1885 K and 71.8 GPa, >1798 K). The hydrogen-carbon-enriched metallic liquids provide the necessary fluid environment for superdeep diamond growth.

58 GEOSCIENCES↗

Observation of pressure-induced electron transfer in SnC 2 O 4

We examined the high pressure behavior of stannous oxalate via Raman and X-ray absorption spectroscopy (XAS) inside a diamond anvil cell. Phase transitions were observed to occur near 2.6 and 15 GPa which were reversible upon decompression to ambient conditions. When further pressurized above 15 GPa, the colorless material sustains irreversible chemical alterations and becomes bright red colored – darkening at higher pressures. Another irreversible phase transition occurred above 20 GPa. Concomitant with color change of the sample, we observed a softening of the ν(C–C) modes of the C 2 O 4 2- anion via Raman spectroscopy. We performed a separate XAS experiment which indicates that the Sn 2+ cation undergoes a partial reduction of the 2+ oxidation state with pressure which persists when the sample was depressurized to ambient conditions. Thus, electron density within the C–C bond in the oxalate anion appears to migrate toward the tin cation with pressure. This observation suggests that pressure can offer a very controllable means to vary cation–anion and unit cell dimensions (and thus the electric interactions causing electron movement) and thus the pressure-induced synthesis of novel materials.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Carbide Formation in Refractory Mo 15 Nb 20 Re 15 Ta 30 W 20 Alloy under a Combined High-Pressure and High-Temperature Condition

In this work, the formation of carbide with the concertation of carbon at 0.1 at.% in refractory high-entropy alloy (RHEA) Mo 15 Nb 20 Re 15 Ta 30 W 20 was studied under both ambient and high-pressure high-temperature conditions. The x-ray diffraction of dilute carbon (C)-doped RHEA under ambient pressure showed that the phases and lattice constant of RHEA were not influenced by the addition of 0.1 at.% C. In contrast, C-doped RHEA showed unexpected phase formation and transformation under combined high-pressure and high-temperature conditions by resistively employing the heated diamond anvil cell (DAC) technique. The new FCC_L1 2 phase appeared at 6 GPa and 809 °C and preserved the ambient temperature and pressure. High-pressure and high-temperature promoted the formation of carbides Ta 3 C and Nb 3 C, which are stable and may further improve the mechanical performance of the dilute C-doped alloy Mo 15 Nb 20 Re 15 Ta 30 W 20 .

36 MATERIALS SCIENCE↗

A novel means to generate high pressure

Diamond anvil cells are the most popular means of generating pressures above 2 GPa. However, in many experiments, such as nuclear magnetic resonance and x-ray absorption, the metallic pressurizing gasket (which confines much of the sample) represents an occluding barrier that requires a low Z gasket material (e.g., Be), a split gasket, or other means to enable better coupling of the sample to electromagnetic radiation. In this paper, we demonstrate a novel method for generating high pressures that confines the sample just above the plane of the gasket by using a diamond with a laser hole drilled into the center of the tip. The sample is then confined by the hole, which is sealed by a flat gasket that fits over the hole. When load is applied to the diamonds, metal flows from the deformed gasket into the hole thereby pressurizing the sample similarly to how a piston pressurizes gas inside a cylinder. The pressurized sample is above the metallic gasket plane just inside the tip of the diamond, and thus easily accessible via x rays or visible light that skims just above the plane of the gasket providing an enhanced aperture of radiation collection. Furthermore, we have demonstrated the utility of this method by obtaining Raman spectra of SnC 2 O 4 and x-ray diffraction spectra of seleno-DL-cystine, all at high pressures.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Metallic hydrogen: Study of metastability

Metallic hydrogen (MH) has been predicted to be metastable, a high temperature superconductor, and a powerful rocket propellant. If true, MH could have an enormous impact on society. We have produced MH in a diamond anvil cell and studied its metastability. At a temperature of 5 K, the load on the metallic hydrogen was stepwise reduced until the pressure was essentially zero. While turning the load or pressure down, the sample evidently transformed to the molecular phase and escaped; the hole in the gasket containing the MH closed. We were unable to determine this value of the metastability pressure. Metallic hydrogen was not observed to be metastable at zero pressure, with no uncertainty.

36 MATERIALS SCIENCE↗

Investigation of warm dense matter by combining static and dynamic compression

Shock-compressing material samples that are precompressed with diamond-anvil cells (DACs) enables benchmarking equation of state measurements over a wide range of high-pressure conditions, in particular, warm dense matter relevant to planetary science, astrophysics, and inertial confinement fusion. These targets provide optical access to the shocked sample, so optical velocity interferometry and pyrometry are typical diagnostics. We present a scaling for the coupling of the laser drive to the shock pressure in DACs based on over 150 prior experiments that can be used to design future experiments. For initial static pressures ≤ 5 GPa, using a sapphire window mitigates the effect of photoionization compared to diamond windows and allows the measurement of shock pressures up to 1 TPa with optical diagnostics.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

In situ study on the compression deformation of MoNbTaVW high-entropy alloy

The excellent mechanical properties of high-entropy alloys (HEAs) make them promising materials for advances in science and technology. However, the underlying mechanism of plastic deformation is not well understood. In situ experiments are urgently required to provide a fundamental understanding of the plastic deformation under high pressure. We performed in situ synchrotron X-ray diffraction (XRD) experiments to study compression deformation behavior of the HEA MoNbTaVW in a radial diamond anvil cell (rDAC). Our results show that the strength and ratio of the stress-to-shear modulus values are ~1.5 and 3 times that of pure tungsten (W), respectively. MoNbTaVW showed plastic deformation above 5 GPa and displayed a much stronger texture. In this work, we found that the active dislocation behavior is mainly responsible for the high strength in MoNbTaVW under compression. This unique technique opens a new avenue to investigate the in situ mechanical properties and their mechanism in other types of HEAs.

36 MATERIALS SCIENCE↗

Stress-Induced Structural Transformations in Au Nanocrystals

Nanocrystals can exist in multiply twinned structures like icosahedron or single crystalline structures like cuboctahedron. Transformations between these structures can proceed through diffusion or displacive motion. Experimental studies on nanocrystal structural transformations have focused on high-temperature diffusion-mediated processes. Limited experimental evidence of displacive motion exists. We report structural transformation of 6 nm Au nanocrystals under nonhydrostatic pressure of 7.7 GPa in a diamond anvil cell that is driven by displacive motion. X-ray diffraction and transmission electron microscopy were used to detect the structural transformation from multiply twinned to single crystalline. Single crystalline nanocrystals were recovered after unloading, then quickly reverted to the multiply twinned state after dispersion in toluene. Furthermore, the dynamics of recovery was captured using TEM which showed surface recrystallization and rapid twin boundary motion. Molecular dynamics simulations showed that twin boundaries are unstable due to defects nucleated from the interior of the nanocrystal.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

Structure and Stability of Iron Fluoride at High Pressure–Temperature and Implication for a New Reservoir of Fluorine in the Deep Earth

Fluorine (F) is the most abundant halogen in the bulk silicate Earth. F plays an important role in geochemical and biological systems, but its abundance and distribution in the terrestrial mantle are still unclear. Recent studies suggested that F reservoirs in the deep mantle are potentially hosted in terrestrial oxide minerals, especially in aluminous bridgmanite. However, the knowledge about the formation and stability field of fluoride in the Earth’s interior is rare. In this study, we combine in situ laser-heated diamond anvil cell, synchrotron X-ray diffraction, and first-principles structure search to show that a new tetragonal structure of FeF 3 is stable at pressures of 78–130 GPa and temperatures up to ~1900 K. Simulation predicted the tetragonal phase takes a much denser structure due to the rotation of FeF 6 octahedral units. The equations of states of tetragonal FeF3 are determined by experiment and verified by simulation. Our results indicate that FeF 3 can be a potential key phase for storing F in the Earth’s lower mantle and may explain some mantle-derived magma with high F concentration.

58 GEOSCIENCES↗

The stress state in bismuth to 298 GPa and its use as a pressure transmitting medium and pressure marker at multi-megabar pressures

We have conducted diffraction studies of bismuth (Bi) to 298 GPa using both conventional and toroidal diamond anvil cells (DACs) to investigate its suitability as a pressure-transmitting medium (PTM) to such pressures. Using microfocused x-ray beams, we have determined the pressure dependence of the uniaxial stress component (⁠t⁠) in cubic Bi-V from 7 to 298 GPa and find that at 298 GPa, t < 0.5 GPa. Bi-V, therefore, cannot support significant shear stresses, making it an excellent PTM. We have also measured the compressibility of Bi-V against that of copper (Cu) and gold (Au), allowing it to be used as a pressure marker as well as a PTM.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗