An opposed-anvil-type apparatus with an optical window and a wide-angle aperture for neutron diffraction

We designed new anvil assemblies for acquiring high-quality neutron diffraction data and ruby fluorescence spectra inside a sample chamber. The conical aperture of Ni-binded WC anvils was expanded by a factor of two. A hybrid gasket made of TiZr- and Al-alloy was developed to prevent outward extrusion. A small and optically transparent window of moissanite was introduced to allow for the determination of pressure and hydrostaticity by measurement of ruby fluorescence spectra. High pressure-generation tests that make use of Bi electrical conductivity and ruby pressure markers revealed that pressure could be determined over 10 GPa. In situ synchrotron X-ray diffraction experiments were also carried out using NaCl as the pressure calibrants. The maximum pressure achieved was approximately 13 GPa. The neutron diffraction intensity from the newly generated anvil assemblies was 2.5–3.0 times greater than that using the standard toroidal anvil assemblies used previously.     

Stabilities of SiO2 stishovite and CaSiO3 perovskite under lower mantle condition

Abstract

Stabilities of SiO₂ stishovite and CaSiO₃ perovskite were studied up to 120 GPa, using diamond-anvil type high pressure apparatus combined with a laser heating system. High pressure in situ X-ray observation clarified that stishovite distorts into slightly dense CaCl₂-type structure above 80 GPa while cubic perovskite type CaSiO₃ remains stable up to 120 GPa.     

Real‐time non‐invasive detection of inhalable particulates delivered into live mouse airways

Fine non‐biological particles small enough to be suspended in the air are continually inhaled as we breathe. These particles deposit on airway surfaces where they are either cleared by airway defences or can remain and affect lung health. Pollutant particles from vehicles, building processes and mineral and industrial dusts have the potential to cause both immediate and delayed health problems. Because of their small size, it has not been possible to non‐invasively examine how individual particles deposit on live airways, or to consider how they behave on the airway surface after deposition. In this study, synchrotron phase‐contrast X‐ray imaging (PCXI) has been utilized to detect and monitor individual particle deposition. The in vitro detectability of a range of potentially respirable particulates was first determined. Of the particulates tested, only asbestos, quarry dust, fibreglass and galena (lead sulfate) were visible in vitro. These particulates were then examined after delivery into the nasal airway of live anaesthetized mice; all were detectable in vivo but each exhibited different surface appearances and behaviour along the airway surface. The two fibrous particulates appeared as agglomerations enveloped by fluid, while the non‐fibrous particulates were present as individual particles. Synchrotron PCXI provides the unique ability to non‐invasively detect and track deposition of individual particulates in live mouse airways. With further refinement of particulate sizing and delivery techniques, PCXI should provide a novel approach for live animal monitoring of airway particulates relevant to lung health.     

Anaerobic biodegradation tests of poly(lactic acid) and polycaprolactone using new evaluation system for methane fermentation in anaerobic sludge

The anaerobic biodegradation tests of polycaprolactone (PCL) and poly(lactic acid) (PLA) powders were done at thermophilic temperature (55 °C) under aquatic conditions (total solid concentrations of the used sludge were 1.73% (undiluted sludge) and 0.86% (diluted sludge)) using a newly developed evaluation system. With this system, the evolved biogas is collected in a gas sampling bag at atmospheric pressure. This method is more convenient than using a pressure transducer or inverted graduated cylinder submerged in water. The biodegradation of PCL powder (10 g, 125–250 μm) in the diluted sludge stopped in about 47 days when the biodegradability reached 92%. The biodegradability of PLA powder (10 g, 125–250 μm) in undiluted sludge was 91% at about 75 days. The biodegradability of PLA powder (10 g, 125–250 μm) in diluted sludge was 79% at about 100 days. The biodegradability of PLA powder (5 g, 125–250 μm) in diluted sludge was 80% at about 85 days. It was found that the PCL and PLA powders were quite degraded using the new evaluation method. In addition, the smaller particle size PCL powder was biodegraded faster.     

Preparation of Photoluminescent Porous Silicon Nanoparticles by High‐Pressure Microfluidization

The use of high‐shear microfluidization as a rapid, reproducible, and high‐yield method to prepare nanoparticles of porous silicon (pSi) with a narrow size distribution is described. Porous films prepared by electrochemical etch of a single‐crystal silicon wafer are removed from the substrate, fragmented, dispersed in an aqueous solution, and then processed with a microfluidizer, which generates high yields (57%) of pSi nanoparticles of narrow size distribution (PDI = 0.263) without a filtration step. Preparation of pSi nanoparticles via microfluidization improves yields (by 2.4‐fold) and particle size uniformity (by 1.8‐fold), and it lowers the total processing time (by 36‐fold) over standard ultrasonication or ball milling methods. The average diameter of the nanoparticles can be adjusted over the range 150–350 nm by appropriate adjustment of processing steps. If the fluid carrier in the microfluidizer contains an oxidant for Si, the resulting pSi particles are prepared with a core–shell structure, in which an elemental Si core is encased in a silicon oxide shell. When an aqueous sodium tetraborate processing solution is used, microfluidization generates photoluminescent core–shell pSi particles with a quantum yield of 19% in a single step in less than 20 min.     

Torsion-bar antenna for low-frequency gravitational-wave observations

We propose a novel type of gravitational-wave antenna, formed by two bar-shaped test masses and laser-interferometric sensors to monitor their differential angular fluctuations. This antenna has a fundamental sensitivity to low-frequency signals below 1 Hz, even with a ground-based configuration. In addition, it is possible to expand the observation band to a lower limit determined by the observation time, by using modulation and up-conversion of gravitational-wave signals by rotation of the antenna. The potential sensitivity of this antenna is superior to those of current detectors in a 1 mHz-10 Hz frequency band and is sufficient for observations of gravitational waves radiated from in-spiral and merger events of intermediate-mass black holes.     

Perfect softening of the ferroelectric mode in the isotope-exchanged strontium titanate of SrTi18O3 studied by light scattering

The mode of the isotope-induced ferroelectric strontium titanate shows a perfect softening at the ferroelectric phase transition temperature , where the frequency of the underdamped mode approaches completely to zero within the instrumental resolution. The spectra of the Raman inactive soft mode have been successfully observed owing to local symmetry breaking and by long-term accumulation of the spectral intensity with a high resolution technique. The mechanism of the phase transition is concluded to be an ideal displacive-type accompanied with perfect softening of the Slater-type polar mode. The difference between the soft mode behavior of and indicates that the origin of the quantum paraelectric state of lies in the quantum fluctuation of the oxide octahedron in the perovskite structure.     

Surface chemical states of gold nanoparticles prepared using the solution-plasma method in a CsCl aqueous solution

In this study, gold nanoparticles (AuNPs) prepared in a 5 mM CsCl aqueous solution using the solution-plasma method are characterized via transmission electron microscopy (TEM) and X-ray photoelectron spectroscopy with synchrotron radiation (SR-XPS). The particle diameter is measured over the process time via TEM. During the solution-plasma process, small particles of 2.1 to 2.2-nm diameter are generated in the CsCl aqueous solution; these particles then enlarge via Ostwald ripening over time until they reach an equilibrium size of ~13 nm after 36 days. In addition, the surface chemical states of the AuNPs are characterized at different depths via SR-XPS. The SR-XPS measurements obtained using incident X-ray energy (hν) of 945.0 eV revealed that Cs─Au, Cl─Au, and Cs─Cl─Au bonds are present 1.2 nm below the surface. The measurements obtained at an incident X-ray energy of 2515.0 eV showed that Cs─Cl─Au bonding is also present 2.5 nm below the surface, indicating that Cs and Cl strongly interact with Au. The TEM and SR-XPS measurements revealed that 2 processes occur cyclically during the growth process via Ostwald ripening: (i) the Cs and Cl in the aqueous solution adsorb on the AuNP surface and (ii) Au atoms subsequently bond to the AuNPs surface.     

Synthesis,crystal structure and properties of a quaternary oxide with a new structure type,BiGaTi4O11

A new quaternary oxide, BiGaTi₄O₁₁ (bismuth gallium tetratitanium undecaoxide), was prepared by heating a mixture of the binary oxides at 1373 K in air. BiGaTi₄O₁₁ melts at 1487 K and prismatic single crystals were obtained from a sample melted at 1523 K and solidified by furnace cooling. The structure of BiGaTi₄O₁₁ was analyzed using single‐crystal X‐ray diffraction to be of a new type that crystallized in the space group Cmcm. A Bi³⁺ site is coordinated by nine O^2? anions, and three oxygen‐coordinated octahedral sites are statistically occupied by Ga³⁺ and Ti⁴⁺ cations. A relative dielectric constant of 46 with a temperature coefficient of 57 ppm K^?1 in the temperature range 297–448 K was measured for a polycrystalline ceramic sample at 150 Hz–1 MHz with a dielectric loss tan δ of less than 0.01. Electrical resistivities measured at 1073 K by alternating‐current impedance spectroscopic and direct‐current methods were 1.16 × 10^?4 and 1.14 × 10^?4 S cm^?1, respectively, which indicates that electrons and/or holes were conduction carriers at high temperature. The optical band gap estimated by the results of diffuse reflectance analysis was 2.9–3.0 eV, while the band gap obtained from the activation energy for electrical conduction was 3.5 eV.     

High pressure generation using double-stage diamond anvil technique: problems and equations of state of rhenium

We have developed a double stage diamond anvil cell (ds-DAC) technique for reproducible pressure by precisely fabricating 2nd stage anvils using a focused ion beam system. We used 2nd stage micro-anvils made of ultra-fine (V/V₀?=?0.633 for the smallest d-spacing. The calculated pressure for this minimum volume varies from 430 to 630?GPa, depending on the choice of the equation of state of rhenium. We conclude that the most likely pressure achieved for the minimum volume of rhenium is in a range of 430–460?GPa based on a calibration using the platinum pressure scale to 280?GPa and the latter value of 630?GPa is unreasonably high, suggesting that the pressures in an earlier study for the equation of state of rhenium would have been significantly overestimated.