scholarly journals A new small-angle X-ray scattering model for polymer spherulites with a limited lateral size of the lamellar crystals

IUCrJ ◽  
2019 ◽  
Vol 6 (5) ◽  
pp. 968-983 ◽  
Author(s):  
Xiang-Yang Li ◽  
Jian-Jun Ding ◽  
Yan-Ping Liu ◽  
Xing-You Tian

As is well known, polymers commonly form lamellar crystals, and these assemble further into lamellar stacks and spherulites during quiescent crystallization. Fifty years ago, Vonk and Kortleve constructed the classical small-angle X-ray scattering theory (SAXS) for a lamellar system, in which it was assumed that the lamellar stack had an infinite lateral size [Vonk & Kortleve (1967), Kolloid Z. Z. Polym. 220, 19–24]. Under this assumption, only crystal planes satisfying the Bragg condition can form strong scattering, and the scattering from the lamellar stack arises from the difference between the scattering intensities in the amorphous and crystalline layers, induced by the incident X-ray beam. This assumption is now deemed unreasonable. In a real polymer spherulite, the lamellar crystal commonly has dimensions of only a few hundred nanometres. At such a limited lateral size, lamellar stacks in a broad orientation have similar scattering, so interference between these lamellar stacks must be considered. Scattering from lamellar stacks parallel to the incident X-ray beam also needs to be considered when total reflection occurs. In this study, various scattering contributions from lamellar stacks in a spherulite are determined. It is found that, for a limited lateral size, the scattering induced by the incident X-ray beam is not the main origin of SAXS. It forms double peaks, which are not observed in real scattering because of destructive interference between the lamellar stacks. The scattering induced by the evanescent wave is the main origin. It can form a similar interference pattern to that observed in a real SAXS measurement: a Guinier region in the small-q range, a signal region in the intermediate-q range and a Porod region in the high-q range. It is estimated that, to avoid destructive interference, the lateral size needs to be greater than 11 µm, which cannot be satisfied in a real lamellar system. Therefore, SAXS in a real polymer system arises largely from the scattering induced by the evanescent wave. Evidence for the existence of the evanescent wave was identified in the scattering of isotactic polypropylene. This study corrects a long-term misunderstanding of SAXS in a polymer lamellar system.

2019 ◽  
Author(s):  
Christian Prehal ◽  
Aleksej Samojlov ◽  
Manfred Nachtnebel ◽  
Manfred Kriechbaum ◽  
Heinz Amenitsch ◽  
...  

<b>Here we use in situ small and wide angle X-ray scattering to elucidate unexpected mechanistic insights of the O2 reduction mechanism in Li-O2 batteries.<br></b>


2019 ◽  
Author(s):  
Hao Wu ◽  
Jeffrey Ting ◽  
Siqi Meng ◽  
Matthew Tirrell

We have directly observed the <i>in situ</i> self-assembly kinetics of polyelectrolyte complex (PEC) micelles by synchrotron time-resolved small-angle X-ray scattering, equipped with a stopped-flow device that provides millisecond temporal resolution. This work has elucidated one general kinetic pathway for the process of PEC micelle formation, which provides useful physical insights for increasing our fundamental understanding of complexation and self-assembly dynamics driven by electrostatic interactions that occur on ultrafast timescales.


1981 ◽  
Vol 46 (7) ◽  
pp. 1675-1681 ◽  
Author(s):  
Josef Baldrian ◽  
Božena N. Kolarz ◽  
Henrik Galina

Porosity variations induced by swelling agent exchange were studied in a styrene-divinylbenzene copolymer. Standard methods were used in the characterization of copolymer porosity in the dry state and the results were compared with related structural parameters derived from small angle X-ray scattering (SAXS) measurements as developed for the characterization of two-phase systems. The SAXS method was also used for porosity determination in swollen samples. The differences in the porosity of dry samples were found to be an effect of the drying process, while in the swollen state the sample swells and deswells isotropically.


2020 ◽  
Vol 91 (12) ◽  
pp. 123501
Author(s):  
M. Šmíd ◽  
C. Baehtz ◽  
A. Pelka ◽  
A. Laso García ◽  
S. Göde ◽  
...  

2021 ◽  
Vol 14 (1) ◽  
Author(s):  
Susyn Joan Kelly ◽  
Lizette duPlessis ◽  
John Soley ◽  
Frazer Noble ◽  
Hannah Carolyn Wells ◽  
...  

Abstract Objective Small angle X-ray scattering (SAXS) analysis is a sensitive way of determining the ultrastructure of collagen in tissues. Little is known about how parameters measured by SAXS are affected by preservatives commonly used to prevent autolysis. We determined the effects of formalin, glutaraldehyde, Triton X and saline on measurements of fibril diameter, fibril diameter distribution, and D-spacing of corneal collagen using SAXS analysis. Results Compared to sections of sheep and cats’ corneas stored frozen as controls, those preserved in 5% glutaraldehyde and 10% formalin had significantly larger mean collagen fibril diameters, increased fibril diameter distribution and decreased D-spacing. Sections of corneas preserved in Triton X had significantly increased collagen fibril diameters and decreased fibril diameter distribution. Those preserved in 0.9% saline had significantly increased mean collagen fibril diameters and decreased diameter distributions. Subjectively, the corneas preserved in 5% glutaraldehyde and 10% formalin maintained their transparency but those in Triton X and 0.9% saline became opaque. Subjective morphological assessment of transmission electron microscope images of corneas supported the SAXS data. Workers using SAXS analysis to characterize collagen should be alerted to changes that can be introduced by common preservatives in which their samples may have been stored.


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