In operando quantitation of Li concentration for a commercial Li‐ion rechargeable battery using high‐energy X‐ray Compton scattering

Compton scattering is one of the most promising probes for quantitating Li under in operando conditions, since high‐energy X‐rays, which have high penetration power, are used as the incident beam and the Compton‐scattered energy spectrum has specific line‐shapes for each element. An in operando quantitation method to determine the Li composition in electrodes has been developed by using line‐shape (S‐parameter) analysis of the Compton‐scattered energy spectrum. In this study, S‐parameter analysis has been applied to a commercial coin cell Li‐ion rechargeable battery and the variation of the S‐parameters during the charge/discharge cycle at the positive and negative electrodes has been obtained. By using calibration curves for Li composition in the electrodes, the change in Li composition of the positive and negative electrodes has been determined using the S‐parameters simultaneously.     

3-D PTV measurement of Marangoni convection in liquid bridge in space experiment

Microgravity experiments have been conducted on the International Space Station in order to clarify the transition processes of the Marangoni convection in liquid bridges of high Prandtl number fluid. The use of microgravity allows us to generate large liquid bridges, 30?mm in diameter and up to 60?mm in length. Three-dimensional particle tracking velocimetry (3-D PTV) is used to reveal complex flow patterns that appear after the transition of the flow field to oscillatory states. It is found that a standing-wave oscillation having an azimuthal mode number equal to one appears in the long liquid bridges. For the liquid bridge 45?mm in length, the oscillation of the flow field is observed in a meridional plane of the liquid bridge, and the flow field exhibits the presence of multiple vortical structures traveling from the heated disk toward the cooled disk. Such flow behaviors are shown to be associated with the propagation of surface temperature fluctuations visualized with an IR camera. These results indicate that the oscillation of the flow and temperature field is due to the propagation of the hydrothermal waves. Their characteristics are discussed in comparison with some previous results with long liquid bridges. It is shown that the axial wavelength of the hydrothermal wave observed presently is comparable to the length of the liquid bridge and that this result disagrees with the previous linear stability analysis for an infinitely long liquid bridge.     

Reductive coupling of aliphatic cyclic imides and ω-amidoesters with benzophenones by low-valent titanium: Synthesis of 5-diarylmethylene-1,5-dihydropyrrol-2-ones, 6-diarylmethyl-2-pyridones,and ω-(diarylmethylene)lactams

The reductive coupling of cyclic imides and ω-amidoesters with benzophenones by Zn-TiCl₄ in THF and subsequent acid-catalyzed dehydration gave 5-diarylmethylene-1,5-dihydropyrrol-2-ones A, 6-diarylmethyl-2-pyridones B, and ω-(diarylmethylene)lactams C. In a similar manner, 3-((benzyloxy)carbonyl)amino substituted A, B, and C were synthesized from the corresponding 3-((benzyloxy)carbonyl)amino cyclic imides and ω-((benzyloxy)carbonyl)amino-ω-amidoesters prepared from L-aspartic and L-glutamic acids. In addition, 4- and 5-((benzyloxy)carbonyl)amino substituted C were also obtained by the same procedures from 2-((benzyloxy)carbonyl)amino-ω-amidoesters prepared from L-asparagine and L-glutamine, respectively.     

High-throughput solid-phase extraction of metal ions using an iminodiacetate chelating porous disk prepared by graft polymerization

A chelating porous sheet for use in solid-phase extraction was prepared by radiation-induced graft polymerization and subsequent chemical modifications. An epoxy-group-containing vinyl monomer was graft-polymerized onto a porous sheet made of polyethylene. The produced epoxy group of the graft chain was converted into an iminodiacetate group. The chelating porous sheet with a density of the iminodiacetate group of 2.1 mol/kg was cut into disks 13 mm in diameter to fit an empty cylindrical cartridge with a capacity of 6 mL. Breakthrough curves using the chelating-porous-disk-packed cartridge overlapped irrespective of the flow rate of the solution ranging up to 1500 mL/h because of negligible diffusional mass-transfer resistance of the copper ions to the iminodiacetate group of the graft chain.     

Palladium-Catalyzed Annulation of Acyl Fluorides with Norbornene via Decarbonylation and CO Reinsertion

A palladium-catalyzed annulation of acyl fluorides with norbornene is described. This study reports the first example of an annulation of acyl fluorides in the presence of a transition-metal catalyst. Polycyclic ketones are obtained from the cleavage of the C−F and C−H bonds of the acyl fluoride and the rearrangement of the carbonyl moiety by decarbonylation and CO reinsertion.     

Amphiphilic polysilane-methacrylate block copolymers — Formation and interesting properties —

Several polysilane block copolymers have been prepared by the newly developed method, anionic polymerization of masked disilenes. Especially amphiphilic block copolymers of poly(1,1-dimethyl-2,2-dihexyldisilene) and poly methacrylate are focused. Poly(1,1-dimethyl-2,2-dihexyldisilene)-b-poly(2-hydroxyethyl methacrylate) (PMHS-b-PHEMA) is the first example of the amphiphilic polysilane copolymer that can form micelles in polar solvents. Poly(1,1-dimethyl-2,2-dihexyldisilene)-b-poly(methacrylic acid) (PMHS-b-PMAA) is more polar than (PMHS-b-PHEMA), soluble in water to form micelles. The cross-linking reaction of (PMHS-b-PMAA) with 1,10-diaza-4,7-dioxadecane and 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride afforded the first shell cross-linked micelles (SCM) of polysilane. In addition to interesting properties, SCM is indicated to be able to form hollow sphere particles (hollow shell cross-linked micelles, HSCM) by a photochemical process. Reversible encapsulation of guest molecules by SCM and HSCM is demonstrated. Finally, SCM can be used as the template for the synthesis of metal nanoparticles, which may be used as catalysts.