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  • Author or Editor: H. Yoshida x
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Abstract  

Phase transitions of hexatriacontane (C36) and octacosane (C28), both as the solution grown single crystal (SGC) and polycrystalline aggregates (MCC) prepared by cooling at 1 K min–1 from the isotropic liquid state, were measured by the simultaneous DSC-FTIR method. MCC of C36 showed the freezing of the high temperature stable phase, which had a slight lower order of the lattice vibration mode comparing with the room temperature stable phase. MCC of C28 demonstrated thermo-reversible phase transition, however, had a binomial distribution of crystal stability of the monoclinic phase.

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Abstract  

The phase transition and nano-scale ordered structure of four types of blends prepared from four di-block copolymers, consisting of hydrophilic poly(ethylenoxide) and hydrophobic poly(methacrylate) derivative, PEOm-b-PMA(Az)n having different PEO molecular length and same degree of polymerization of PMA(Az) were investigated. All blend systems formed hexagonal packed PEO cylinder structure, which was same with the nano-scale structure of these parent block copolymers. The SAXS and AFM observation suggested that the size of hexagonal structure of blend was larger than the average size of parent block copolymers. The melting enthalpy of PEO in blends was larger than the average value of parent block copolymers. DSC, SAXS and AFM observations indicated the miscible blend systems.

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Abstract  

Monolayers of amphiphilic di-block copolymer, PEO40-b-PMA(Az)19 on water surface and solid surfaces, such as silicon wafer and quartz glass, were analyzed by surface pressure — molecular area (π-A) isotherm, UV-Vis spectroscopy, atomic force microscopy (AFM) and total X-ray reflectivity (TXR). The monolayer prepared at 22 mN m-1 consisted of H aggregated azobezene (Az) moieties, which orientated perpendicular to the solid surface. The monolayer structure, including H aggregated Az and orientation of Az, was stable after annealing at 98�C, at which temperature the hydrophilic PEO domain was the liquid phase and the hydrophobic PMA(Az) was in the smectic A phase.

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Abstract  

The size effect of silica nanoparticles (SiO2) on thermal decomposition of poly(methylmethacrylate) (PMMA) was investigated by the controlled rate thermogravimetry. Thermal degradation temperature of PMMA–SiO2 composites depended on both fraction and size of SiO2, the thermal degradation temperature of 23 nm (diameter) SiO2–PMMA (6.1 wt%) was 13.5 °C higher than that of PMMA. The thermal stabilities of 17 nm SiO2–PMMA (3.2 wt%) and 13 nm SiO2–PMMA (4.8 wt%) were 21 and 23 °C, respectively, higher than that of PMMA without SiO2. The degree of degradation improvement was increased linearly with the surface area of SiO2. The number of surface hydroxyl group in unit volume of SiO2 particle increased with increasing the specific surface area of SiO2, and the interaction between hydroxide group of SiO2 and carbonyl group of PMMA had an important role to improve the thermal stability of PMMA.

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Abstract  

A solvent extraction method is presented for the separation of95Nb from95Zr.95Nb is extracted quantitatively into a chloroform solution of α-benzoinoxime from 5N hydrochloric acid solution. By following the recommended procedure, a separation factor higher than 104 is achieved.95Nb can be back-extracted into concentrated hydrochloric acid. The radiochemical purity of the95Nb separated has been ascertained by half-life and γ-ray energy measurements. The whole procedure takes less than 20 min.

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Abstract  

The nanosecond pulse radiolysis technique has been applied to study the rate constants for charge transfer and substitution reactions of radical ions. Electron transfer from biphenyl anion to styrene derivatives shows a correlation with the reduction potential of the acceptors expected from the Marcus theory. The positive charge transfer from biphenyl cation to the same acceptors shows a much larger rate constant, suggesting a considerable shift of the free energy relationship to the positive side of Go. The substitution reaction of fluorenone anion with organic halides shows an SN2 character, while that of diethyl fumarate shows electron transfer nature. The dimerization of radical anions has been proven for benzophenone and fluorenone, when their lifetime of the parent anions are prolonged by countercations.

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Abstract  

Water molecules in hydrogels were classified into three categories according to phase transition behavior; non-freezing, freezing bound and free water. Melting, crystallization, and glass transition of water in hydrogels reflected the state of the water interacting with polysaccharides. Freezing bound water formed metastable ice by slow cooling and formed amorphous ice by quenching. From the isothermal crystallization measurement, nucleation rate and crystal growth rate were obtained. The crystal growth rate of freezing bound water was about ten times slower than that of free water. The DSC characterization of water in hydrogels was summarized.

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Abstract  

The crystallization dynamics of Nylon 66/Nylon 6 blends, the crystalline/crystalline polymer blends, was analyzed by DSC under isothermal conditions. The crystal growth rate (G) and the nucleation rate (N) depended on both the degree of supercooling (ΔT) and the blend mass fraction (ϕ). The ΔT /T m 0 values obtained at the fixed G, which corresponded to the chemical potential difference of molecules between liquid and crystal states, and the surface free energy parameters evaluated from G and N depended on ϕ for blends. The results suggested that Nylon 66/Nylon 6 blends with ϕN66≥0.80 or ϕN66≤0.15 are miscible.

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Abstract  

The concept of crystallization dynamics method evaluating the miscibility of binary blend system including crystalline component was proposed. Three characteristic rates, nucleation, crystal growth rates (N*, G*) and growth rate of conformation (G c*) were used to evaluate the miscibility of PVDF/at-PMMA and PVDF/iso-PMMA by the simultaneous DSC-FTIR. N*, G* and G c* depended remarkably on both temperature and blend fraction (ϕPMMA) for PVDF/at-PMMA system, which indicated the miscible system. PVDF/iso-PMMA showed small ϕPMMA dependency of N*, G* and G c*, was estimated the immiscible system. The ΔT/T m 0 values, corresponding to Gibbs energy required to attend the constant G* and G c*, evaluated from G* and G c* showed the good linear relationships with different slope. The experimental results suggested that the concentration fluctuation existed in PVDF/iso-PMMA system.

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Abstract  

Cellulose acetate-based polycaprolactones (CAPCL's) were synthesized by the polymerization of -caprolactone which was initiated by non-substituted OH group in cellulose acetate. The CL/OH (mol mol–1) ratios of the CAPCL's were changed from 2 to 20. Thermal and viscoelastic properties of the CAPCL sheets were studied by differential scanning calorimetry (DSC) and dynamic mechanical analysis (DMA). Glass transition, cold crystallization and melting were determined by DSC. Dynamic modules (E'), dynamic loss modules (E'') and tan were measured in a temperature range from –150 to 50°C by DMA. Apparent activation energy of a dispersion was calculated from the frequency dependency of E'' peak temperature. It was found that the main chain motion of both CA and PCL is observed in a CL/OH ratio from 0 to 10 mol mol–1. However, when CL/OH ratio exceeds 10 mol mol–1, the crystalline region which is rearranged by the PCL chain association is observed and only the main chain motion of PCL can be detected.

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