Conformational disorder in the Brill transition of uniaxially-oriented nylon 10/10 sample investigated through the temperature-dependent measurement of X-ray fiber diagram

Tashiro, Kohji; Yoshioka, Yayoi

doi:10.1016/j.polymer.2004.07.024

Cited by 39 publications

(48 citation statements)

References 33 publications

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“…After that they started to become stronger furthermore, just when the methylene segments of the CO side were regularized in conformation. The methylene segments of the NH side were still in the disordered state [1]. Figure 3 shows the time dependence of WAXD and SAXS profile in the isothermal crystallization process of nylon 10/10 at 176 o C. For the quantitative analysis of SAXS data in the time region of 0 -60 sec, we assumed that (i) in the earliest stage the locally-formed weak hydrogen bonds in the melt might cause the generation of some domains with relatively high density.…”

Section: Methodsmentioning

confidence: 99%

“…(According to the infrared spectra measured for the partially-deuterated nylon 10/10 sample, the methylene segments of the NH side are still in the conformationally-disordered state even when the methylene segments of the CO side are already regularized. The reason for the difference in conformational regularization between these two kinds of methylene segments is not solved yet [1].) Figure 5.…”

Section: Structural Evolution Process Of Nylon 10/10mentioning

confidence: 99%

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Structural evolution in the isothermal crystallization process of the molten nylon 10/10 traced by time-resolved infrared spectral measurements and synchrotron SAXS/WAXD measurements

Tashiro

Nishiyama

Tsuji

et al. 2009

J. Phys.: Conf. Ser.

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Structural evolution in the isothermal crystallization process of the molten nylon 10/10 traced by timeresolved infrared spectral measurements and synchrotron SAXS/WAXD measurements Abstract. The structural evolution in the isothermal crystallization process of nylon 10/10 from the melt has been clarified concretely on the basis of the time-resolved infrared spectral measurement as well as the synchrotron wide-angle and small-angle X-ray scattering measurements. Immediately after the temperature jump from the melt to the crystallization point, the isolated domains consisting of the hydrogen-bonded random coils were formed in the melt, as revealed by Guinier plot of SAXS data and the infrared spectral data. With the passage of time these domains approached each other with stronger correlation as analyzed by Debye-Bueche equation. These domains transformed finally to the stacked crystalline lamellae, in which the conformationally-regularized methylene segments of the CO sides were connected each other by stronger intermolecular hydrogen bonds to form the crystal lattice.

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Section: Methodsmentioning

confidence: 99%

Section: Structural Evolution Process Of Nylon 10/10mentioning

confidence: 99%

Structural evolution in the isothermal crystallization process of the molten nylon 10/10 traced by time-resolved infrared spectral measurements and synchrotron SAXS/WAXD measurements

Tashiro

Nishiyama

Tsuji

et al. 2009

J. Phys.: Conf. Ser.

Self Cite

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“…The two strong reflections at d-spacings of 4.4 and 3.7 Å merge into a single peak at the Brill transition. According to a conformational study on the transition, the mobility of the methylene segments between the amide groups increases at the Brill transition, although the hydrogen bonds between the neighboring chains are maintained [24,25]. As a result, the packing of the molecular chains changes from triclinic or orthorhombic to quasi-hexagonal.…”

Section: Temperature Variation Of the Crystal Structure In The Scsmentioning

confidence: 99%

Polymorphism of poly(nonamethyleneoxamide) crystal

Nakagawa

Nozaki

Maeda

et al. 2015

Polymer

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The crystal structures of poly(nonamethyleneoxamide) (nylon-9,2) were investigated by wide-angle X-ray diffraction (WAXD) and differential scanning calorimetry. Nylon-9,2 shows a polymorphism with two different structures depending on the conditions of sample preparation.Monoclinic form I is the dominant crystalline phase for the solution-crystallized sample. For melt-crystallized samples, form I and new monoclinic form I′ coexist. Variable-temperature WAXD measurements were used to investigate the stability of each crystal form and the phase transition. Form I does not undergo any phase transitions prior to melting, although the orthorhombic molecular chain packing in form I at low temperature comes close to the quasihexagonal one during the heating process. Form I′ shows no phase transition on heating until its melting, too. The crystal lattice simply expands due to the thermal expansion. Form I is believed to be more stable, because the melting temperature of form I is higher than that of form I′.

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“…Recent works based on FTIR data suggest that high temperature pseudohexagonal arrangements are a result of the conformational disorder of polymethylene segments rather than of disruption of hydrogen bonds [35][36][37].…”

Section: Introductionmentioning

confidence: 99%

Reversible changes induced by temperature in the spherulitic birefringence of nylon 6 9

Murase

Casas

Martínez

et al. 2015

Polymer

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Spherulitic morphologies of nylon 6 9 as an example of an even-odd nylon were studied by optical microscopy. A well-defined dependence on crystallization temperature was found. In particular, positively birefringent spherulites were characteristic for temperatures higher than 232 ºC, low birefringence spherulites developed between 232 and 225 ºC, positive ringed spherulites were found between 225 and 220 ºC, and finally negative fibrillar spherulites were formed at temperatures lower than 220 ºC. These optical properties were clearly different from those observed with even-even nylons (e.g., negative and positive birefringence for high and low temperatures, respectively), and may derive from the peculiar crystalline structures determined for even-odd nylons.Furthermore, low birefringence spherulites were characterized by a flat-on lamellar disposition and reversibility of the birefringence sign in the 80-120 ºC temperature interval (positive and negative values at high and low temperatures, respectively).Real time WAXD profiles taken during heating and cooling processes demonstrated that different crystalline structures (named I, II and III) developed depending on the temperature and crystallization procedure of samples (e.g., from solution or from the melt state). Crystalline structures were characterized by the formation of hydrogen bonds along two crystalline directions in all cases, a peculiar arrangement that may account for the development of positive and negative spherulites in a more simple way than formulated for conventional polyamides having a single hydrogen bonding direction. DSC and FTIR data also showed a complex structural behavior with structural transitions in the 80-120 ºC range, a region that corresponds to birefringence sign reversibility.

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Conformational disorder in the Brill transition of uniaxially-oriented nylon 10/10 sample investigated through the temperature-dependent measurement of X-ray fiber diagram

Cited by 39 publications

References 33 publications

Structural evolution in the isothermal crystallization process of the molten nylon 10/10 traced by time-resolved infrared spectral measurements and synchrotron SAXS/WAXD measurements

Structural evolution in the isothermal crystallization process of the molten nylon 10/10 traced by time-resolved infrared spectral measurements and synchrotron SAXS/WAXD measurements

Polymorphism of poly(nonamethyleneoxamide) crystal

Reversible changes induced by temperature in the spherulitic birefringence of nylon 6 9

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