SAXS-Fiber Computer Tomography. Method Enhancement and Analysis of Microfibrillar-Reinforced Composite Precursors from PEBA and PET

Stribeck, Norbert; Nöchel, Ulrich; Fakirov, S.; Feldkamp, Jan M.; Schroer, Christian G.; Timmann, Andreas; Kuhlmann, Marion

doi:10.1021/ma8015322

Cited by 21 publications

(34 citation statements)

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“…With the advent of the nanotechnologies requiring a strict and rigorous control over the structures on the nanometer scale, this method can be of some importance for both industry and academia. The latest invention is the fast tomographic imaging method based on SAXS data from a scanning-microbeam experiment [67]. By means of this method, real-time X-ray experiments using mechanical testers for slow or fast load-cycling test can be incorporated into the synchrotron beamline.…”

Section: Discussionmentioning

confidence: 99%

X‐Ray Scattering Studies on Multiphasic Polymer Systems

Denchev¹,

Viana²

2011

Handbook of Multiphase Polymer Systems

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At present, multiphase and multicomponent materials such as polymer alloys, blends, and composites consume over 80 wt% of all commercially-produced resins. The increase of this particular segment of the plastics industry is about three times faster than of the industry as a whole. The reason is that the modification by blending may improve significantly the resins' mechanical performance and processability, being at the same time cost effective. Those few resins that are used without adding of other components are most frequently semicrystalline, i.e. they already have a multiphase structure that makes other modification less urgent [1].Recently, a large window has opened for new structural applications of the multicomponent polymer systems with the advent of nanoscale filled polymer composites. Changing the type, size, shape, volume fraction, interface, and degree of dispersion or aggregation of the nanofillers enables a great amount of unique combinations of properties with high potential for successful commercial development [2].In technical literature the terms 'phase' and 'component' are often used interchangeably.In thermodynamics, however, a clear distinction is made. Thus, a phase is defined as a chemically and physically uniform quantity of matter that can be separated mechanically from a nonhomogeneous mixture. Hence, multiphasic polymer systems would comprise at least two different phases, e.g. semicrystalline single polymers featuring amorphous and crystalline phases or polymorphic polymers containing different concomitant crystalline phases. Many polymer systems with industrial importance such as blends, colloidal polymers, polymer composites/ filled polymers, etc. comprise two or more chemically distinct components, each one of them being able to contain various phases as well. These components may have different sizes, with microscopic to nanoscopic blocks being present.

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Section: Discussionmentioning

confidence: 99%

X‐Ray Scattering Studies on Multiphasic Polymer Systems

Denchev¹,

Viana²

2011

Handbook of Multiphase Polymer Systems

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“…Fig. 1) is sufficient to guarantee perfect reconstruction, and deviations of the real structure from this assumption lead to well-defined [6,7] reconstruction aberrations from which additional information on the structure itself is obtained. Last but not least, this technique is fast enough to sweep the microbeam across the fiber while the specimen is subjected to thermal or mechanical load.…”

Section: Structure Gradients In Polymer Fibersmentioning

confidence: 99%

“…Application. In an application-oriented feasibility study [7] composites based on poly(ether)-blockamide (PEBA) are studied. The results from a direct analysis of the smeared measured patterns are compared to results obtained after tomographic reconstruction.…”

Section: Structure Gradients In Polymer Fibersmentioning

confidence: 99%

“…In the core of the strand negative-intensity equatorial streaks indicate over-reconstruction. Thus, at least a fraction of the equatorial streak observed in the shell zone must be attributed [7] to shingle-shaped voids in radial orientation that violate LFS. The central voxel (ρ f = 0) does not fit into the series.…”

Section: Structure Gradients In Polymer Fibersmentioning

confidence: 99%

“…The central voxel (ρ f = 0) does not fit into the series. The reason is, that another type of LFS violation ("tangential grain" [7]) leads to a reconstruction aberration that is always accumulated in the central voxel of the reconstructed SAXS. …”

Section: Structure Gradients In Polymer Fibersmentioning

confidence: 99%

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Advanced X-Ray scattering methods for the study of structure and its evolution in soft materials with fiber symmetry

Stribeck¹

2010

IOP Conf. Ser.: Mater. Sci. Eng.

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Abstract. Three recently developed evaluation methods for the automated quantitative analysis of Xray scattering data (small-angle (SAXS) and wide-angle (WAXS)) are presented. They are applicable to extensive series of 2D patterns that are recorded in studies of polymer materials with uniaxial symmetry. The experiments comprise time-resolved studies (melting, crystallization, mechanical properties and fatigue) as well as microbeam-scanning for the study of nanostructure gradients. The methods appear suitable to manage the data flood from modern synchrotron radiation setups aiming at the extraction of quantitative information on the structure evolution inside the material.In microbeam-scanning experiments the recorded scattering patterns are smeared. It is proposed to reconstruct desmeared scattering patterns by an X-ray scattering fiber-computer-tomography (XS-FCT). Reconstruction aberrations yield additional structure information. The true structure variation along the fiber radius is established. Compared to general tomography the experiment is faster by a factor of 100, and reconstruction is faster by a factor of 10 4 . In WAXS fiber patterns should first be mapped into reciprocal space before analysis. After having corrected an erroneous tilt-angle equation, automatic tilt-angle tracking and mapping becomes possible. If polymers fail at low strain, the determination of strain and of structural parameters from the scattering patterns require very high accuracy because the observed variations are subtle. Suitable methods are presented both for the high-precision determination of the macroscopic strain, and for the determination of subtle variations of structure parameters.

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In situ WAXS/SAXS structural evolution study during uniaxial stretching of poly(ethylene therephthalate) nanocomposites in solid state: Poly(ethylene therephthalate)/montmorillonite nanocomposites

Todorov

Martins

Viana

2012

J of Applied Polymer Sci

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This work investigates the solid state uniaxial stretching of neat polyethylene therephthalate, PET, and its montmorillonite, MMT, nanocomposites (0.3 wt % of MMT particles with different initial agglomerate sizes) showing intercalated and tactoid morphologies, followed by in situ WAXS and SAXS experiments under an X-ray synchrotron source. The distinct nanocomposite morphologies were assessed by WAXS and transmission electron microscopy. The in situ WAXS experiments during stretching evaluated the evolution of phase's mass fractions and the average level of molecular orientation upon uniaxial deformation, and the in situ SAXS experiments assessed the evolution of craze-like structures and void sizes. Multiscale structure evolution models are proposed and compared for neat PET and its nanocomposites. Main global mechanisms are identical although with distinct evolutions of phase mass fractions. Also craze-like/voids structures evolve with distinct sizes. Intercalated MMT morphology induces an earlier formation of periodical mesophase, a retarded widening of craze-like structures and the smallest void sizes.V C 2012 Wiley Periodicals, Inc. J.Appl. Polym. Sci. 128: 2884-2895, 2013

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SAXS-Fiber Computer Tomography. Method Enhancement and Analysis of Microfibrillar-Reinforced Composite Precursors from PEBA and PET

Cited by 21 publications

References 50 publications

X‐Ray Scattering Studies on Multiphasic Polymer Systems

X‐Ray Scattering Studies on Multiphasic Polymer Systems

Advanced X-Ray scattering methods for the study of structure and its evolution in soft materials with fiber symmetry

In situ WAXS/SAXS structural evolution study during uniaxial stretching of poly(ethylene therephthalate) nanocomposites in solid state: Poly(ethylene therephthalate)/montmorillonite nanocomposites

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