We discuss the construction of a new SAXS/WAXS beamline at the Advanced Light Source at Lawrence Berkeley Laboratory. The beamline is equipped with a multilayer monochromator in order to obtain a high X-ray flux. The detrimental effects that the increased bandwidth transmitted by this monochromator could have on the data quality of the SAXS and WAXS patterns is shown to be negligible for the experimental program intended to be operated on this beamline.

https://iopscience.iop.org/article/10.1088/1742-6596/247/1/012007/pdf

A SAXS/WAXS/GISAXS Beamline with Multilayer Monochromator

We examined the melt and solid-state structures of a series of diblock copolymers containing polyethylene as the minority block, with a rubbery hydrocarbon majority block. When the interblock segregation strength during crystallization is sufficiently high (approximately 3 times the segregation strength at the order−disorder transition), crystallization can be effectively confined within spherical domains formed by microphase separation in the melt; the process is homogeneously nucleated, and the resulting kinetics are first-order (Avrami n = 1). Below this critical interblock segregation strength, crystallization disrupts the spherical microdomains, resulting in sigmoidal kinetics (n > 1). Cylinder-forming materials are more complex:  there exists a range of intermediate segregation strength where crystallization is templated but not wholly confined within the nanoscale domains prescribed by microphase separation; while the melt morphology is generally retained on cooling, local distortions and connectio...

Modes of Crystallization in Block Copolymer Microdomains: Breakout, Templated, and Confined

Gelatinisation of starch: a combined SAXS/WAXS/DSC and SANS study

We examine the crystallization behavior of polyethylene-b-poly(vinylcyclohexane) diblock copolymers, E/VCH, using a combination of transmission electron microscopy (TEM), dilatometry, and time-resolved small-angle X-ray scattering (SAXS). The glassy VCH matrix effectively restricts E crystallization to within the spheres, cylinders, gyroid channels, or lamellae formed by microphase separation in the melt. The VCH matrix can contract in response to crystallization of the E microdomains, so crystallization proceeds without cavitation. The crystallization kinetics strongly reflect the connectivity of the E microdomains:  homogeneous nucleation and first-order crystallization kinetics for spheres or cylinders of E; conventional sigmoidal kinetics for the highly interconnected gyroid structure. Lamellar materials show an interesting two-step crystallization behavior:  at higher temperature, heterogeneous nucleation permits the crystallization of lamellae interconnected through grain boundaries or defects, and ...

Polymer crystallization confined in one, two, or three dimensions

It has previously been shown that there are many benefits to be obtained in combining several techniques in one in situ set-up to study chemical processes in action. Many of these combined set-ups make use of two techniques, but in some cases it is possible and useful to combine even more. A set-up has recently been developed that combines three X-ray-based techniques, small- and wide-angle X-ray scattering (SAXS/WAXS) and quick-scanning EXAFS (QEXAFS), for the study of dynamical chemical processes. The set-up is able to probe the same part of the sample during the synthesis process and is thus able to follow changes at the nanometre to micrometre scale during, for example, materials self-assembly, with a time resolution of the order of a few minutes. The practicality of this kind of experiment has been illustrated by studying zeotype crystallization processes and revealed important new insights into the interplay of the various stages of ZnAPO-34 formation. The flexibility of this set-up for studying other processes and for incorporating other additional non-X-ray-based experimental techniques has also been explored and demonstrated for studying the stability/activity of iron molybdate catalysts for the anaerobic decomposition of methanol.

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Implementation of a combined SAXS/WAXS/QEXAFS set-up for time-resolved in situ experiments

A differential scanning calorimeter with a temperature range of 77 to 873 K has been developed for use in combination with either time-resolved X-ray scattering or high-resolution energy-dispersive powder diffraction studies using synchrotron radiation. The first results of successful experiments are briefly described.

B. E. Komanschek

Papers

The combination of thermal analysis and time-resolved X-ray techniques: a powerful method for materials characterization

Morphology in binary blends of poly(vinyl methyl ether) and epsilon-caprolactone-trimethylene carbonate diblock copolymer