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Sato Harumi,Murakami Rumi,Zhang Jianming,Ozaki Yukihiro,Mori Katsuhito,Takahashi Isao,Terauchi Hikaru,Noda Isao The Polymer Society of Korea 2006 Macromolecular Research Vol.14 No.4
Temperature-dependent, wide-angle, x-ray diffraction (WAXD) patterns and infrared (IR) spectra were measured for biodegradable poly(3-hydroxybutyrate) (PHB) and its copolymers, poly(3-hydroxybutyrate-co-3-hydroxyhexanoate) P(HB-co-HHx) (HHx=2.5, 3.4, 10.5, and 12 mol%), in order to explore their crystal and lamellar structure and their pattern of C-H...O=C hydrogen bonding. The WAXD patterns showed that the P(HB-co-HHx) copolymers have the same orthorhombic system as PHB. It was found from the temperature-dependent WAXD measurements of PHB and P(HB-co-HHx) that the a lattice parameter is more enlarged than the b lattice parameter during heating and that only the a lattice parameter shows reversibility during both heating and cooling processes. These observations suggest that an interaction occurs along the a axis in PHB and P(HB-co-HHx). This interaction seems to be due to an intermolecular C-H...O=C hydrogen bonding between the C=O group in one helical structure and the $CH_3$ group in the other helical structure. The x-ray crystallographic data of PHB showed that the distance between the O atom of the C=O group in one helical structure and the H atom of one of the three C-H bonds of the $CH_3$ group in the other helix structure is $2.63{\AA}$, which is significantly shorter than the sum of the van der Waals separation ($2.72{\AA}$). This result and the appearance of the $CH_3$ asymmetric stretching band at $3009 cm^{-1}$ suggest that there is a C-H...O=C hydrogen bond between the C=O group and the $CH_3$ group in PHB and P(HB-co-HHx). The temperature-dependent WAXD and IR measurements revealed that the crystallinity of P(HB-co-HHx) (HHx =10.5 and 12 mol%) decreases gradually from a fairly low temperature, while that of PHB and P(HB-co-HHx) (HHx = 2.5 and 3.5 mol%) remains almost unchanged until just below their melting temperatures. It was also shown from our studies that the weakening of the C-H...O = C interaction starts from just above room temperature and proceeds gradually increasing temperature. It seems that the C-H...O=C hydrogen bonding stabilizes the chain holding in the lamellar structure and affects the thermal behaviour of PHB and its copolymers.
Kenji Ohwada,Tatsuo Fukuda,Jun’ichiro Mizuki,Kazuma Hirota,Hikaru Terauchi,Satoshi Tsutsui,Alfred Q. R. Baron,Hidehiro Ohwa,Naohiko Yasuda 한국물리학회 2011 THE JOURNAL OF THE KOREAN PHYSICAL SOCIETY Vol.59 No.31
Pb(In_(1/2)Nb_(1/2))O_3 (PIN) can be antiferroelectric (AFE), ferroelectric (FE) or a relaxor depending upon the perovskite B-site randomness. In order to clarify the effect of B-site randomness, we studied the dynamics of ordered PIN without B-site randomness (O-PIN, AFE), which will give us a clear picture of the AFE/relaxor nature of the ground state due to B-site randomness. The quasielastic (QE) scattering shows a critical slowing down near the Γ-point and the transverse acoustic (TA) mode shows a softening trend at a finite wavenumber position (not at the Γ-point) towards the AFE phase transition temperature (T_N ∼ 450 K). On the other hand, the transverse optic (TO) mode shows a softening near the Γ-point toward low temperature with no clear anomaly at T_N. These results indicate that the AFE phase transition is associated with the TA mode and the origin of the QE scattering while a ferroelectric correlation exists behind the AFE ordering. The effect of B-site randomness is finally discussed on the basis of the results.