Electron-microscopic procedure for acrylic rubber

The electron-microscopic visualization of acrylic rubber dispersed in a heterogeneous structural resin composition consisting of a rubber-modified two-phase plastic comprising essentially a butyl acrylate rubber phase and an acrylonitrile–styrene copolymer phase, respectively, has been accomplished. This procedure consists of the following: The molded resin specimen is treated with hydrazine hydrate solution to produce the acrylic acid hydrazides. Allow the treated specimen to soak in osmium tetroxide solution. The acrylic rubber may be indirectly fixed and stained. Some micrographs of ultrathin sections of two or three resin compositions, cut by an ultramicrotome, are presented.     

Synthesis of poly(tetrahydrofuran-b-ε-caprolactone) macromonomer via the Sml2-induced transformation

Summary A novel well-defined macromonomer consisting of different types of monomers in polymerization mechanisms was synthesized for the first time through the SmI₂-induced transformation. The macromonomer, -methacryloylpoly-(tetrahydrofuran-b--caprolactone), was prepared by the reaction of methacryloyl chloride with living poly(tetrahydrofuran-b--caprolactone) [poly(THF-b-CL)] which was obtained by the two-electron reduction of the cationic growing center of poly(THF) by samarium iodide (SmI₂) followed by the polymerization of CL. ¹H NMR analysis indicated the quantitative introduction of the methacryloyl group onto the polymer end. The molecular weight distribution of the macromonomer was relatively narrow, and the unit ratio of THF to CL could be controlled by both polymerization time of THF and the amount of CL, resulting from the living nature of both CL- and THF-polymerizations. Radical copolymerization of the produced macromonomers with methyl methacrylate in the presence of AIBN resulted in a polymethacrylate backbone grafted with poly(THF-b-CL) block copolymers.     

Photocatalytic Activity of a TiO<Subscript>2</Subscript> Photocatalyst Doped with C<Superscript>4+</Superscript> and S<Superscript>4+</Superscript> Ions Having a Rutile Phase Under Visible Light

C⁴⁺ and S⁴⁺-codoped titanium dioxide (TiO₂) having a rutile phase was prepared. By doping C⁴⁺ and S⁴⁺ ions into a TiO₂ lattice, the absorption edge of rutile TiO₂ powder was largely shifted from 400 to 700 nm. 2-Methylpyridine and methyleneblue were photocatalytically oxidized at high efficiency on C⁴⁺ and S⁴⁺-doped TiO₂ under visible light at a wavelength longer than 5 nm.     

Morphology of CuO through precipitation process under 2.45 GHz microwave irradiation

The morphology of CuO powders formed by a homogeneous precipitation process from aqueous copper precursor complex was investigated. The effect of 2.45 GHz microwave irradiation appeared in the characteristic morphology of the CuO microcrystal with comparison of an ordinal synthesis process. The crystallographic orientation of CuO microcrystals in the particle was examined by HRTEM. Using microwave irradiation, it was demonstrated that the morphology of the particles was kept through the decomposition of the precursor. Also the rapid transformation of a precursor to CuO in aqueous solution under microwave irradiation condition was discussed.     

Isolation of Solid Solution Phases in Size‐Controlled LixFePO4 at Room Temperature

State‐of‐the‐art LiFePO₄ technology has now opened the door for lithium ion batteries to take their place in large‐scale applications such as plug‐in hybrid vehicles. A high level of safety, significant cost reduction, and huge power generation are on the verge of being guaranteed for the most advanced energy storage system. The room‐temperature phase diagram is essential to understand the facile electrode reaction of Li_xFePO₄ (0 < x < 1), but it has not been fully understood. Here, intermediate solid solution phases close to x = 0 and x = 1 have been isolated at room temperature. Size‐dependent modification of the phase diagram, as well as the systematic variation of lattice parameters inside the solid‐solution compositional domain closely related to the electrochemical redox potential, are demonstrated. These experimental results reveal that the excess capacity that has been observed above and below the two‐phase equilibrium potential is largely due to the bulk solid solution, and thus support the size‐dependent miscibility gap model.     

Determination of optimal sending voltage profile in distribution systems with distributed generators

Sending voltage profile of distribution feeder is controlled by changing a tap of distribution transformer. In a distribution network with distributed generators, for reasons of effect of reversed flows from them and existence of a great number of sending voltage profile candidates, it is not easy to control sending voltage profile within the acceptable voltage limit. In this paper, in order to determine the optical sending voltage profile of distribution transformer in a distribution network with distributed generators, the authors propose a new method to determine the optimal sending voltage profile so as to minimize the total number of tap position's change per day under constraints of acceptable voltage limit. In the proposed method, after calculating acceptable range of three‐phase voltage of distribution feeder, the optimal profile of tap position within the calculated acceptable voltage range is determined among these candidates by using reduced ordered binary decision diagram (ROBDD) which is an efficient enumeration algorithm. In order to check the validity of the proposed method, numerical simulations are carried out for a distribution network model with a distributed generator. © 2007 Wiley Periodicals, Inc. Electr Eng Jpn, 161(2): 16–24, 2007; Published online in Wiley InterScience ( www.interscience.wiley.com ). DOI 10.1002/eej.20393     

Palladium‐Catalyzed Hydroxymethylation of Aryl‐ and Heteroarylboronic Acids using Aqueous Formaldehyde

Cyclometallated NHC palladium complexes prepared from palladium(II) acetate [Pd(OAc)₂] and unsymmetrical 1,3‐diarylimidazolinium salts catalyzed the hydroxymethylation of (hetero)arylboronic acids using an excess amount of formalin to afford (hetero)arylmethanols in good to satisfactory yields.

     

Characterization of electrode/electrolyte interface for lithium batteries using in situ synchrotron X-ray reflectometry—A new experimental technique for LiCoO2 model electrode

A new experimental technique was developed for detecting structure changes at electrode/electrolyte interface of lithium cell using X-ray reflectometry and two-dimensional model electrodes with a restricted lattice-plane. The electrodes were constructed with an epitaxial film of LiCoO₂ synthesized by pulsed laser deposition method. The orientation of the epitaxial film depends on the substrate plane; the 2D layer of LiCoO₂ is parallel to the SrTiO₃ (1 1 1) substrate (_(0 0 3)LiCoO₂//_(1 1 1)SrTiO₃)$({(003)}_{\text{LiCo}{\text{O}}_2}//{(111)}_{\text{SrTi}{\text{O}}_3})$, while the 2D layer is perpendicular to the SrTiO₃ (1 1 0) substrate (_(1 1 0)LiCoO₂//_(1 1 0)SrTiO₃)$({(110)}_{\text{LiCo}{\text{O}}_2}//{(110)}_{\text{SrTi}{\text{O}}_3})$. The anisotropic properties were confirmed by electrochemical measurements. Ex situ X-ray reflectivity measurements indicated that the impurity layer existed on the as-grown LiCoO₂ was dissolved and a new SEI layer with lower density was formed after soaking into the electrolyte. In situ X-ray reflectivity measurements indicated that the surface roughness of the intercalation (1 1 0) plane increased with applying voltages, while no significant changes in surface morphology were observed for the intercalation non-active (0 0 3) plane during the pristine stage of the charge–discharge process.