The electron microscope characterization of the fine structure of nylon 6: I. The supermolecular structure in melt-cast, isotropic bulk material

Schaper, Andreas; Hirte, R.; Rüscher, Claus H.; Hillebrand, R.; Walenta, E.

doi:10.1007/bf01469525

Cited by 18 publications

(15 citation statements)

References 46 publications

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“…Different cutting directions relative to the tensile axis were chosen in order to preclude misinterpretation due to possible preparation artefacts. The complicating factors in sectioning which we noticed in [33] were also operative in the present study. The e (= 3~ -1)-values were estimated from straining marks on the specimen surfaces as well as by a statistical evaluation of the spherulite elongations assuming an almost homogeneous deformation.…”

Section: Methodsmentioning

confidence: 78%

“…In the foregoing paper [33], direct TEM studies on ultra-thin sections proved that the lammellar structure of within a spherulite in bulk nylon 6 is, in principle, like that illustrated in the schematic drawing of Sharples [38], given in Figure 6. The spherulite origin is represented by an aggregate of single crystals, i. e. a lamellar cluster; the successive branching and splaying apart of the lamellae (termed "fibrils" in the scheme) during growth create a marked sheaf-like appearance of the spherulites.…”

Section: Discussionmentioning

confidence: 99%

“…The observed intensity distributions were not Lorentz-corrected in this case. Further experimental details are given in [33].…”

Section: Methodsmentioning

confidence: 99%

“…The melt-cast material primarily used for our investigations was a hydrolytically polymerized non-extracted nylon 6, which was characterized in detail in the foregoing paper [33]. Specimens for deformation experiments were prepared by milling down the middle parts of bristles of 80 mm length from 3 to 2 mm over a distance of 5 mm so as to obtain a fixed deformation region.…”

Section: Methodsmentioning

confidence: 99%

“…With these questions in mind, we performed drawing experiments on nylon 6 bristles in connection with optical and electron microscope observations and with small angle X-ray scattering (SAXS). The main attention was focussed on the direct electron microscope (EM) visualization of the oriented structure by applying the preparation technique as previously described in part I of this study [33].…”

Section: Introductionmentioning

confidence: 99%

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The electron microscope characterization of the fine structure of nylon 6: II. On the rearrangement of the structure during cold-drawing

Schaper

Hirte

Rüscher

1986

Colloid & Polymer Sci

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Abstract:The transmission electron microscope (TEM) visualization of the supermolecular structure of cold-drawn, oriented nylon 6 bulk material (bristles) by stained ultrathin sections is reported. For evaluating the electron micrographs optical diffraction (OD) has been applied in comparison with small angle X-ray scattering (SAXS). The deformation of the spherulites was followed by polarization microscopy. In addition, investigations were carried out on commercial nylon 6 fibres. As the main result a transverse structure was revealed within the drawn samples at draw ratios between 2 = 4 and 4.5, consisting of mosaic crystals which show some lateral alignment. The structure is described by a modified layer lattice model. While the long period may increase slightly during drawing, the crystallite thickness remains almost constant. Fibres with 2 = 3.4 show a similarly oriented structure though the lateral alignment of the crystals is not so pronounced.

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Section: Methodsmentioning

confidence: 78%

Section: Discussionmentioning

confidence: 99%

“…The observed intensity distributions were not Lorentz-corrected in this case. Further experimental details are given in [33].…”

Section: Methodsmentioning

confidence: 99%

Section: Methodsmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

See 3 more Smart Citations

The electron microscope characterization of the fine structure of nylon 6: II. On the rearrangement of the structure during cold-drawing

Schaper

Hirte

Rüscher

1986

Colloid & Polymer Sci

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Strukturcharakterisierung von Polymeren mit physikalischen Methoden

Fink¹,

Geiß²,

Walenta³

et al. 1989

Acta Polymerica

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Die kombinierte Anwendung der IR‐ und NMR‐Spektroskopie, der Röntgenklein‐ und ‐weitwinkelstreuung und elektronenmikroskopischer Methoden wird an ausgewählten Beispielen von Polymerfestkörpern demonstriert. Neuere Ergebnisse zu PE‐Strukturen einschließlich hochfester/hochmoduliger Fasern, zur strukturellen Erklärung von PVDF‐Polarisationseffekten sowie zu Strukturveränderungen der Cellulose infolge Natronlaugebehandlungen werden vorgestellt. Die Schlüsselrolle der IR‐Spektroskopie für die Analyse chemischer Strukturen wird an Beispielen aufgezeigt.

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Characterization of polyamide 6 made by reactive extrusion. II. Analysis of microstructure

Hornsby

Tung

1994

J of Applied Polymer Sci

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SYNOPSISConsideration is given to the characterization of microstructure in polyamide 6 prepared by polymerization of e-caprolactam in a corotating twin-screw extruder. Results obtained by FTIR, WAXD, DSC, and DMTA are discussed in terms of the molecular mass of the polymer, the thermal history of the material. and the influence of residual monomer. I NTRO DUCT1 0 NA previous investigation considered the preparation of polyamide 6 (PA6) by the catalyzed anionic polymerization of t-caprolactam in a corotating twinscrew extruder.' It was shown that, using an appropriate catalyst and activator system together with an optimized screw profile and operating conditions, high polymer could be produced with an average machine residence time of about 90 s. Molecular mass and residual monomer level were strongly influenced by screw speed. Mechanical properties compared favorably with commercial PA6 made by hydrolytic polymerization, with notched Izod impact strength and elongation at break being significantly higher for material produced by reactive extrusion.This article considers the effects of processing history and material composition on microstructure of the materials produced. In this respect, previous work has established the existence of two crystalline forms of PA6, an a-phase and a thermodynamically less stable y phase, giving rise to wide angle X-ray diffraction (WAXD) peaks at 8 = 19.6" ( a l ) , 23.5O( a 2 ) , and 21.3' ( y ) , respectively.2 In addition, differential scanning calorimetry (DSC) was used to study the effects of processing conditions and recrystallization rate on the thermal properties of PA6 fibers and yarns.3 * To whom correspondence should be addressed.Journal of Applied Polymer Science, Vol. 54,899-907 (1994) EXPERIMENTALAn earlier article discussed experimental procedures used for the preparation of PA6 by anionic polymerization of t-caprolactam in a corotating intermeshing twin-screw extruder.' In the present study, consideration is given to the structural analysis of polymer prepared in this way at specified screw speeds ranging from 50 to 150 rpm, and under different conditions of melt cooling, either by rapid quenching in water at 23"C, or after allowing the 4-mm diameter polymer extrudate to cool more slowly in air to room temperature. Some samples were also made with additions of 10% by weight of sized short glass fiber reinforcement, blended with the t-caprolactam/catalyst/activator feedstock, in order to investigate possible effects from additive nucleation on the crystalline microstructure.

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The electron microscope characterization of the fine structure of nylon 6: I. The supermolecular structure in melt-cast, isotropic bulk material

Cited by 18 publications

References 46 publications

The electron microscope characterization of the fine structure of nylon 6: II. On the rearrangement of the structure during cold-drawing

The electron microscope characterization of the fine structure of nylon 6: II. On the rearrangement of the structure during cold-drawing

Strukturcharakterisierung von Polymeren mit physikalischen Methoden

Characterization of polyamide 6 made by reactive extrusion. II. Analysis of microstructure

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