High-pressure cell for studies of ultra-short laser impulses action on materials

A high-pressure cell has been developed for in situ studies of the behavior of materials under ultra-short impulses on a sub-picosecond timescale. This set-up allows performing experiments under controlled atmosphere between a primary vacuum up to 100 MPa. We present some primarily results on hBN.     

Simultaneous electrical and X-ray diffraction studies on neodymium metal to 152 GPa

Using designer diamond anvils and angle dispersive X-ray diffraction technique at a synchrotron source, we have performed simultaneous electrical and structural studies on neodymium metal to 152 GPa in a diamond anvil cell. Four-probe electrical resistance measurement shows a 38% decrease in the electrical resistivity, associated with the delocalization of the 4f-shell electrons, starting at 100 GPa up to a final pressure of 152 GPa. The continuous decrease in electrical resistivity is consistent with the observation of a gradual phase transition to α-U structure in this pressure range. The (1 1 1) diffraction peak of α-U structure first appears at 100 GPa and increases in intensity with increasing pressure to 152 GPa. This increase in intensity is attributed to an increasing volume fraction of α-U phase and an increase in structural y-parameter from 0.07 at 118 GPa to 0.095 at 152 GPa. In contrast to the abrupt pressure-induced f-electron transition seen in cerium and praseodymium, the continuous evolution of α-U structure and electrical resistivity in neodymium confirms the gradual nature of 4f delocalization process in this element.     

Optimization of Paris–Edinburgh press cell assemblies for in situ monochromatic X-ray diffraction and X-ray absorption

We describe some important improvements allowed by the development of new cell assemblies coupled to opposed conical sintered diamond anvils in the Paris–Edinburgh press. We provide X-ray absorption and diffraction experiments carried out at pressures up to 16.5 GPa. The maximum temperature reached was 1800 K for P<10 GPa and 1300 K for higher pressures. The sintered diamond anvils are X-ray transparent and give access to a much larger X-ray window than the tungsten carbide anvils, even at the highest pressure. Therefore, X-ray measurements are performed using in situ cross-calibration simultaneously. We also describe a new heating setup used to reach high temperatures, despite the low conductivity of the sintered diamond core by deviating the electrical current using copper strips. These improvements are illustrated by recent data collected using angle dispersive in situ X-ray diffraction on liquid Fe-18%wt S and using EXAFS at the barium K-edge on Ba₈Si₄₆ silicon clathrates and at the iodine K-edge on iodine-intercalated nanotubes.     

In situ study of magmatic processes: a new experimental approach

We present an internally heated autoclave, modified in order to permit in situ studies at pressure up to 0.5 GPa and temperature up to 1000 °C. It is equipped with transparent sapphire windows, allowing the observation of the whole experiment along the horizontal axis. In the experimental cell, the sample is held between two thick transparent plates of sapphire or diamond, placed in the furnace cylinder. The experimental volume is about 0.01 cm³. Video records are made during the whole experiment. This tool is developed mainly to study the magmatic processes, as the working pressures and temperatures are appropriate for subvolcanic magma reservoirs. However, other applications are possible, such as the study of subsolidus phase equilibria as we have used well-known phase transitions, such as the system of AgI, to calibrate the apparatus with respect to pressure and temperature. The principle of the apparatus is detailed. Applications are presented, such as studies of melt inclusions at pressure and temperature and an in situ study of magma degassing through the investigation of nucleation and growth processes of gas bubbles in a silicate melt during decompression.     

Electroconductivity and pressure–temperature states of step shocked C60 fullerite

A study of electrophysical and thermodynamic properties of C₆₀ single crystals under step shock loading has been carried out. The increase and the following reduction in specific electroconductivity of C₆₀ fullerite single crystals at step shock compression up to pressure 30 GPa have been measured. The equations of state for face centred cubic (fcc) C₆₀ fullerite as well as for two-dimensional polymer C₆₀ and for three-dimensional polymer C₆₀ (3D-C₆₀) were constructed. The pressure–temperature states of C₆₀ fullerite were calculated at step shock compression up to pressure 30 GPa and temperature 550 K. The X-ray diffraction studies of shock-recovered samples reveal a mixture of fcc C₆₀ and a X-ray amorphous component of fullerite C₆₀. The start of the formation of the X-ray amorphous component occurs at a pressure P _m≈ 19.8 GPa and a temperature T _m≈ 520 K. At pressures exceeding P _m and temperatures exceeding T _m, the shock compressed fullerite consist of a two-phase mixture of fcc C₆₀ fullerite and an X-ray amorphous component presumably consisting of the nucleators of polymer 3D-C₆₀ fullerite. The decrease in electroconductivity of fullerite can be explained by the percolation effect caused by the change of pressure, size and number of polymeric phase nuclei.     

Physical and mechanical properties of C60 under high pressures and high temperatures

The physical and mechanical properties of a C₆₀ fullerene sample have been investigated under high pressure–high temperature conditions using a designer Diamond Anvil Cell. Electrical resistance measurements show evidence of C₆₀ cage collapse at 20 GPa, which leads to the formation of an insulating phase at higher pressure. Energy dispersive X-ray diffraction (EDXD) data indicated that the characteristic fcc reflections gradually decrease in intensity and eventually disappear above 28 GPa. A C₆₀ sample was laser-heated at a pressure of 35 GPa to a temperature of 1910±100 K and, subsequently, decompressed to ambient conditions. The photoluminescence spectra and the Raman spectrum of the pressure–temperature-treated sample were measured at a low temperature of 80 K. Raman peak at 1322.3 cm^?1 with full-width half-maximum of 2.9 cm^?1 was observed from the sample, which is attributed to the hexagonal diamond phase in the sample. The room temperature photoluminescence spectra showed a symmetric emission band centered in the red spectral range with a peak at 690 nm. The structural analysis of the pressure–temperature-processed C₆₀ sample using EDXD method showed strong internal structure orientation and a phase close to hexagonal diamond. Mechanical properties such as hardness and Young’s modulus were measured by nanoindentation technique and the values were found to be 90±7 and 1215±50 GPa, respectively and these values are characteristic of sp³-bonded carbon materials.     

Simple vibration-insensitive cavity for laser stabilization at the 10−16 level

We present the design and realization of two reference cavities for ultra-stable lasers addressing narrow transitions in mixed-species (¹¹⁵In⁺ / ¹⁷²Yb⁺) Coulomb crystals. With a simple set-up, we achieve a fractional frequency instability close to the thermal noise limit of a 12-cm-long cavity, reaching σ _y  = 4.7 × 10^?16 at 10 s with a linear drift of 53 mHz/s. We discuss the individual instability contributions and show that in a set-up with a lower thermal noise floor and vibration sensitivity, an instability of 1 × 10^?16 can be reached. To achieve this, we implement a vibration-insensitive design for a 30-cm-long cavity mounted horizontally and conduct first tests that show a sensitivity of 1.8 × 10^?11 ms^?2 to vertical accelerations. This is about a factor of 20 less than the value observed for the short cavity. Mechanical tolerances and ways to further reduce the sensitivity are discussed.     

Effect of plating and incubation conditions on the detection of lactic acid bacteria after high hydrostatic pressure treatment

ABSTRACT

Lactic acid bacteria (Leuconostoc mesenteroides, Enterococcus faecalis, and Lactobacillus fermentum) were subjected to high hydrostatic pressures (HHPs) of 400 and 600?MPa at 25°C for 10?min in phosphate-buffered saline. Differential plating methods were applied to evaluate HHP-treated cell populations, assuming that healthy and injured cells during plate incubation survived maximum and minimal stress, respectively. The stress was altered by using several selective media in combination with aerobic or anaerobic incubation at 25°C or 30°C. E. faecalis was detectable after 600?MPa treatment while L. mesenteroides and L. fermentum were nondetectable. Specific combinations of incubation conditions were suggested to determine maximum and minimum viable counts of L. mesenteroides and E. faecalis. The difference between the maximum and minimum counts can be used to evaluate HHP-injured population with reduced risks to overestimate healthy and/or underestimate HHP-injured cells.     

Shock compression of preheated molybdenum

A set of shock adiabats of molybdenum is constructed at various initial temperatures. It is shown that the dependence between shock velocity and particle velocity for Mo is nonlinear at high initial temperatures in a range of particle velocities 0.2<u<0.7 km/s. In a range of particle velocities 0.2 < u < 1.4 km/s the initial heating of molybdenum to 1000 K changes its shock adiabat approximately by 4%.     

Structural and electrical transport properties of FeH x under high pressures and low temperatures

We present the first successful in situ simultaneous measurement of the electrical resistance and X-ray diffraction of FeH _x (x～ 1) under high-pressure H₂ up to 25.5 GPa and low temperatures down to 9 K. The electrical resistivity ρ showed a sharp increase with the formation of iron-hydride FeH _x (x～ 1) at 3.5 GPa. The ?′-phase of FeH _x was found to be metallic up to 25.5 GPa. The ρ vs. T curves up to 16.5 GPa approximately follow Fermi-liquid law below 25 K. However, T ⁵ was found to be better fitting at 25.5 GPa. This change can be considered to be related to the previously reported ferromagnetism collapse at corresponding pressure.     

High pressure and emission spectra of Eu3+ in L-EuBO3

Effects of the high pressure on the emission spectra of Eu³⁺-activated L-EuBO₃ were considered at room temperature up to 100 kbar. The position of five 0–2 lines in the ⁵D₀→⁷F₂ transition region was determined. The pressure does not have the same effect on all these lines. In four of them, high pressure induced a red shift with different shift rates:+0.0022,+0.0035,+0.0034 and+0.0027 nm kbar^?1, respectively, whereas in the last one, high pressure induced a blue shift with shift rate?0.0034 nm kbar^?1. Possible reasons for the mentioned pressure effects on the line positions were considered.     

Equation of state and thermal expansivity of LiF and NaF

The high-pressure and high-temperature behaviors of LiF and NaF have been studied up to 37 GPa and 1000 K. No phase transformations have been observed for LiF up to the maximum pressure reached. The B1 to B2 transition of NaF at room temperature was observed at ～28 GPa, this transition pressure decreases with temperature. Unit-cell volumes of LiF and NaF B1 phase measured at various pressures and temperatures were fitted using a P–V–T Birch–Murnaghan equation of state. For LiF, the determined parameters are: α₀ = 1.05 (3)×10^?4 K^?1, dK/dT = ?0.025 (2) GPa/K, V ₀ = 65.7 (1) Å³, K ₀ = 73 (2) GPa, and K′ = 3.9 (2). For NaF, α₀ = 1.34 (4)×10^?4 K^?1, dK/dT = ?0.020 (1) GPa/K, V ₀ = 100.2 (2) Å³, K ₀ = 46 (1) GPa, and K′ = 4.5 (1).     

Experimental measurement of the electrical conductivity of pyroxenite at high temperature and high pressure under different oxygen fugacities

Electrical conductivities of pyroxenite were measured between frequencies of 10^?1 and 10⁶ Hz in a multi-anvil pressure apparatus using different solid buffers (Ni+NiO, Fe+Fe₃O₄, Fe+FeO and Mo+MoO₂) to stabilize the partial pressure of oxygen. The temperature ranged from 1073 to 1423 K (800 to 1200 °C) and the pressure from 1.0 to 4.0 GPa. We observe that: (1) the electrical conductivity (σ) of pyroxenite depends on frequency; (2) σ tends to increase with rising temperature (T), and Log σ and 1/T obey a linear Arrhenius relationship; (3) under control of the buffer Fe+Fe₃O₄, σ tends to decrease with rising pressure, nevertheless the activation enthalpy tends to increase. For the first time we have obtained values for the activation energy and activation bulk volume of the main charge carriers, which are (1.60±0.07) eV and (0.05±0.03) cm³/mol, respectively; (4) for a given pressure and temperature, σ tends to rise with increased oxygen fugacity, whereas the activation enthalpy and preexponential factor tend to decrease; and (5) the behaviour of the electrical conductivity at high temperature and high pressure can be reasonably interpreted by assuming that small polarons provide the dominant conduction mechanism in the pyroxenite samples.     

II–VI and II1−x Mn x VI semiconductor nanocrystals formed by the pressure cycle method

II–VI and II_1?x Mn _x VI nanocrystals were prepared by the pressure cycle method using the Paris–Edinburgh cell. The recovered samples are nanocrystals in the cubic phase zinc-blend (ZB) structure and were characterized using transmission electron microscopy, electron diffraction, X-ray diffraction and Raman scattering. Transmission electron micrographs show that these nanocrystals are nearly spherical with diameters ranging from 20 to 50 nm depending on the sample under investigation. The Raman scattering measurements confirm the existence of II–VI nanocrystals in the cubic phase (ZB). The magnetic properties of Cd_0.5Mn_0.5Te nanoparticles were found to vary with the particle size and were different from those observed for the Cd_0.5Mn_0.5Te bulk initial samples. The χ vs. T data show temperature hysteresis due to spin-glass form, which occurs at T _g=21 K, for both the bulk as well as for the recovered nanoparticle samples. The zero-field cooled and field-cooled χ vs. T curves for the nanoparticles showed a monotonous increase below T _g. Below ～21 K, the M vs. B curve for the recovered nanoparticle samples exhibited magnetic hysteresis, and this is attributed to a weak ferromagnetic contribution. This contribution is also observed in the χ(T) curves and is due to a large surface/volume ratio of the nanoparticles, which enhances the magnetic interaction.     

Stabilisation of Ce-Cu-Fe amorphous alloys by addition of Al

The present work describes the formation of amorphous alloys in the (Al_1?xCe_x)₆₂Cu₂₅Fe₁₃ quaternary system (0 ≤ x ≤ 1). When the amount of Ce falls in the range 0.67 ≤ x ≤ 0.83, the alloys obtained exhibit a completely amorphous structure confirmed by powder X-ray diffraction. Otherwise, at compositions x = 0.5, 0.58, 0.92 and 1, a primary crystalline phase forms together with an amorphous matrix. The crystallisation temperature (T_x) decreases with increasing Ce content, varying from 593 K for x = 0.5–383 K for x = 1. Composition x = 0.75 is considered as the best glass former, exhibiting a large supercooled liquid region of 40 K width that precedes crystallisation. In order to form bulk amorphous alloys, ribbons with this later composition were consolidated into few millimetre thick discs using pulsed electric current sintering at different temperatures, yet preserving the amorphous structure. Meanwhile, increasing temperature above 483 K triggers crystallisation of a primary phase isostructural to AlCe₃. Further increase in the temperature up to 573 K yields a higher fraction of the crystalline phase. Testing mechanical properties, using nanoindentation, revealed that both elastic modulus (E) and hardness (H) depend on the Al content, ranging from E = 85.6 ± 3.7 GPa and H = 6.2 ± 0.7 GPa for x = 0.5 down to E = 39.8 ± 1.0 GPa and H = 3.1 ± 0.2 GPa for x = 0.92.     

Phase transition of ZnS at high pressures and temperatures

The high-pressure behaviour of zinc sulphide, ZnS, has been investigated, using an in situ X-ray powder diffraction technique in a diamond anvil cell, at pressures and temperatures up to 35 GPa and 1000 K, respectively. The pressure-induced phase transition from a zincblende (B3) to a rocksalt (B1) structure was observed. This transition occurred at 13.4 GPa and at room temperature, and a negative dependence on temperature for this transition was confirmed. The transition boundary was determined to be P (GPa) = 14.4 ? 0.0033 × T (K).     

Microstructural evolution and thermal stability of Fe–Zr metastable alloys developed by mechanical alloying followed by annealing

The effect of Zr (up to 1 at.%) addition on the formation of Fe–Zr metastable alloys and their thermal stability were investigated for their possible nuclear applications. Fe–xZr (x = 0.25, 0.5, 1%) alloys were synthesised by mechanical alloying under a high-purity argon atmosphere using stainless steel grinding media in a SPEX 8000M high energy mill. The milling was conducted for 20 h with a ball-to-powder weight ratio of 10:1. The formation of metastable solid solutions after milling was confirmed from the change in the Gibbs free energy analysis as per Miedema’s model. The microstructural characterisation was carried out by analysis of X-ray diffraction, atomic force microscopy and transmission electron microscopy. The effect of Zr on the thermal stability of Fe–Zr alloys was investigated by extensive annealing experiments followed by microstructural analysis and microhardness measurements. The stabilisation was found to occur at 800 °C and thereafter, no significant change in the crystallite size was observed for the samples annealed between 800 and 1200 °C. The supersaturated solid solution, especially 1% Zr alloy, found to be highly stable up to 800 °C and the microhardness value of the same measured to be as high as 8.8 GPa corresponding to a crystallite size of 57 nm. The stabilisation effect has been discussed in the light of both the thermodynamic and kinetic mechanisms and the grain size stabilisation is attributed to the grain boundary segregation of Zr atoms and/or Zener pinning by nanoscale precipitation of the Fe₂Zr phase.     

A new dimension in structural biology: fully fledged high-pressure macromolecular crystallography

The amount of accurate crystallographic data currently available on macromolecular structures at high pressure is extremely limited, mainly due to the lack of appropriate instrumentation and X-ray sources. A technical breakthrough has been achieved with a set-up at the ESRF ID30 beamline equipped with a diamond anvil cell and a large imaging plate, and taking advantage from undulators providing a quasi-plane wave of ultrashort wavelength X-rays. The accessible pressure range is increased by nearly one order of magnitude with respect to beryllium cells. A nearly perfect long-range order is preserved in protein and virus crystals compressed below the denaturation pressure. The quality of diffraction data collected at high pressure can meet usual standards, especially in the case of high symmetry space groups.

An overview of main results and ongoing studies is given, including the 7?kbar structure of hen egg-white lysozyme refined at 1.6?Å resolution and structural investigations of cowpea mosaic virus (CPMV), the first macromolecular assembly investigated at high pressure by single crystal X-ray diffraction. The ordering effect of high pressure on the molecular packing of disordered P23 crystals was highlighted. The 2.8?Å resolution structure of CPMV at 3.3?kbar was fully refined using high completeness data collected on pressure-ordered I23 crystals.     

Laser assisted decay spectroscopy at the CRIS beam line at ISOLDE

The new collinear resonant ionization spectroscopy (Cris) experiment at Isolde, Cern uses laser radiation to stepwise excite and ionize an atomic beam for the purpose of ultra-sensitive detection of rare isotopes and hyperfine structure measurements. The technique also offers the ability to purify an ion beam that is contaminated with radioactive isobars, including the ground state of an isotope from its isomer. A new program using the Cris technique to select only nuclear isomeric states for decay spectroscopy commenced last year. The isomeric ion beam is selected using a resonance within its hyperfine structure and subsequently deflected to a decay spectroscopy station. This consists of a rotating wheel implantation system for alpha and beta decay spectroscopy, and up to three high purity germanium detectors for gamma-ray detection. This paper gives an introduction to the Cris technique, the current status of the laser assisted decay spectroscopy set-up and recent results from the experiment in November 2011.