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, Kohji; Nishiyama, Asami; Tsuji, Sawako; Hashida, Tomoko; Hanesaka, Makoto; Takeda, Shin‐ichi; Cao, Wei; Reddy, Kummetha Raghunatha; Masunaga, Hiroyasu; Sasaki, Sono; Ito, Kazuki; Takata, Masaki

doi:10.1088/1742-6596/184/1/012002

Cited by 9 publications

(6 citation statements)

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“…Such an irreversible change in two-dimensional SAXS pattern from a four-point pattern to a two-point pattern was also detected in the transition between the LT and HT phases of a VDF73% sample, in which the CL phase was not involved in the transition (Tashiro et al, 2002). Similar large changes in SAXS pattern were also observed in the case of a phase transition of aliphatic nylon 10/10 occurring in the hightemperature region near the melting point (Tashiro, 2007;Tashiro et al, 2009). These remarkable changes in the higher-order structure may be related to thermally activated translational motion of chains along the orientation axis.…”

Section: Vdf52% Copolymersupporting

confidence: 58%

In-house simultaneous collection of small-angle X-ray scattering, wide-angle X-ray diffraction and Raman scattering data from polymeric materials

et al. 2014

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An in‐house X‐ray scattering system, which can simultaneously measure small‐angle X‐ray scattering (SAXS) and wide‐angle X‐ray diffraction (WAXD) data, as well Raman scattering data, has been developed to study the phase transitions of polymeric materials. To date, these types of measurements have been limited to synchrotron radiation. The present system is an in‐house SAXS system combined with a WAXD detector and a Raman spectrometer. A rotating‐anode X‐ray generator and multilayer optic are employed to provide a high‐flux X‐ray beam. Two two‐dimensional hybrid pixel detectors are utilized for the rapid‐scan time‐resolved SAXS and WAXD measurements. The Raman unit consists of a compact probe with a near‐infrared excitation laser operating at a wavelength of 1064 nm. This long‐wavelength laser produces less fluorescence than conventional excitation lasers with wavelengths of 532 or 785 nm. The performance of this system was tested by investigating the thermally induced ferroelectric phase transition of vinylidene fluoride–trifluoroethylene (VDF‐TrFE) copolymers. It has been demonstrated that the combination of SAXS, WAXD and Raman techniques gives useful information for revealing the relationship between the structural change in the crystal lattice and the morphological change in the lamellar stacking mode in polymer samples of complicated hierarchical structure.

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Section: Vdf52% Copolymersupporting

confidence: 58%

In-house simultaneous collection of small-angle X-ray scattering, wide-angle X-ray diffraction and Raman scattering data from polymeric materials

et al. 2014

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“…17,18,32 X-ray powder diffraction data reported by Tashiro et al on the early stages of the isothermal crystallization of PA1010 at 176 °C after melting at 210 °C suggest also that a pleated (rather than a rippled) sheet structure has been produced. 34,35 The detailed analysis is developed in S10. Note, for the future reference, that comparable but not identical thermal treatments (annealing and/or self-seeding and recrystallization at high T°) yield apparently nearly "pure" PA1010 rippled sheet (Yan and Li 17,18 ) or nearly "pure" PA1010 pleated sheet structures (Tashiro et al 34 ), which underlines the close parenthood of the two structures but also the sensitivity of the structural outcome to the specific thermal treatments used.…”

Section: ■ Resultsmentioning

confidence: 99%

“…34,35 The detailed analysis is developed in S10. Note, for the future reference, that comparable but not identical thermal treatments (annealing and/or self-seeding and recrystallization at high T°) yield apparently nearly "pure" PA1010 rippled sheet (Yan and Li 17,18 ) or nearly "pure" PA1010 pleated sheet structures (Tashiro et al 34 ), which underlines the close parenthood of the two structures but also the sensitivity of the structural outcome to the specific thermal treatments used.…”

Section: ■ Resultsmentioning

confidence: 99%

“…54 The variation is linear, in the form: T B = 2.894 L -89.18. For a long period of ≈130 Å, 34 the extrapolated Brill transition would be 287 °C. In other words, the domain of existence of the pleated/ rippled sheet structures is always located below the Brill transition corresponding to its lamellar thickness even though they may be formed at very high temperature, near the melting temperature of the same material with "conventional" lamellar thickness.…”

Section: ■ Discussionmentioning

confidence: 99%

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Original Crystal Structures of Even–Even Polyamides Made of Pleated and Rippled Sheets

Lotz

2021

Macromolecules

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Original crystal structures of even−even polyamides are introduced. They are based on twisted conformations at the amide-aliphatic part links and are reminiscent of the pleated and rippled protein sheet structures introduced by Pauling and Corey in the early 1950s. Pleated sheets are chiral, and rippled sheets are made of two conformational isomers. They have specific X-ray diffraction "profiles". Publications on even−even polyamides describe such profiles, indicating that both pleated and rippled sheet variants exist. The pleated sheet structure is the stable crystal form of the whole family of nylons 2,2n. The rippled sheet applies for a high-temperature "alpha phase variant" of nylons with long aliphatic parts and more generally appears to be (one of?) the so-called "high-temperature α phase(s)" of even−even nylons. Pleated and rippled sheet crystal structures appear to be the entropically favored, high-temperature crystal form(s) of nylons. This new family of crystal structures and their possible variants with different sequences of twisted amide-aliphatic part junctions open a possible way for the (re)analysis of rare and unusual crystal morphologies produced at high Tc after partial melting/self-seeding.

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“…Besides, it is better to distinguish the behavior of the two methylene segments of the monomeric unit. Then, the deuterated methylene segment was introduced as the CO-side methylene units: –(NH(CH 2 ) 10 NHCO(CD 2 ) 8 CO) n – [13,42]. As shown in Figure 12b, the IR CH 2 bands shifted before and after the partial deuteration, making it easier to trace the behaviors of these two different types of the methylene segments.…”

Section: Resultsmentioning

confidence: 99%

Structural Evolution Mechanism of Crystalline Polymers in the Isothermal Melt-Crystallization Process: A Proposition Based on Simultaneous WAXD/SAXS/FTIR Measurements

Tashiro

Yamamoto

2019

Polymers

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Time-resolved simultaneous measurements of wide-angle X-ray diffraction (WAXD) and small-angle X-ray scattering (SAXS) (and FTIR spectra) were performed for various kinds of crystalline polymers in isothermal melt-crystallization processes, from which the common features of the structural evolution process as well as the different behaviors intrinsic to the individual polymer species were extracted. The polymers targeted here were polyethylene, isotactic polypropylene, polyoxymethylene, aliphatic nylon, vinylidene fluoride copolymer, trans-polyisoprene, and poly(alkylene terephthalate). A universal concept of the microscopically viewed structural evolution process in isothermal crystallization may be described as follows: (i) the small domains composed of locally regular but more or less disordered helical chain segments are created in the melt (this important information was obtained by the IR spectral data analysis); (ii) these domains grow larger as the length and number of more regular helical segments increase with time; (iii) the correlation among the domains becomes stronger and they approach each other; and (iv) they merge into the stacked lamellar structure consisting of the regularly arranged crystalline lattices. The inner structure of the domains is different depending on the polymer species, as known from the IR spectral data

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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

Cited by 9 publications

References 5 publications

In-house simultaneous collection of small-angle X-ray scattering, wide-angle X-ray diffraction and Raman scattering data from polymeric materials

In-house simultaneous collection of small-angle X-ray scattering, wide-angle X-ray diffraction and Raman scattering data from polymeric materials

Original Crystal Structures of Even–Even Polyamides Made of Pleated and Rippled Sheets

Structural Evolution Mechanism of Crystalline Polymers in the Isothermal Melt-Crystallization Process: A Proposition Based on Simultaneous WAXD/SAXS/FTIR Measurements

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