It is shown that wide-angle X-ray scattering patterns can be obtained from single polymeric fibers with a 2 μm synchrotron radiation beam in a few seconds per pattern. Preferred orientation was obs...

Microdiffraction Experiments on Single Polymeric Fibers by Synchrotron Radiation

Ultrasonic standing waves, excited in an (111) crystal through magnetoelastic coupling, are visualized using synchrotron radiation diffraction imaging (`topography'). This observation relies on the possibility at the ESRF of recording images with long sample-to-film propagation distances (up to 1.5 m) without substantial loss of resolution. The crystal acts as an x-ray focusing lens periodically in time, an effect that strongly depends both on the amplitude of the magnetic field excitation and on the propagation distance. The standing-wave-related contrast is hardly visible close to the sample, very sharp for a focusing distance (typically ) whereas beyond this position the intensity maxima broaden due to the defocusing effect. We propose a model which accounts for the presented results, allows the understanding of the details of the resonance patterns and gives access to the main characteristics of the vibration: amplitude, shape, polarization, wavelength and sound velocity. This effect could be used to simultaneously monochromatize and focus the x-ray beam simultaneously.

A study of the x-ray focusing effect of a magnetoacoustically excited crystal using synchrotron radiation diffraction imaging

Instrumentation, data analysis, radiation damage, and related issues of synchrotron radiation micro- and nanodiffraction techniques applied to soft condensed matter science are reviewed in this chapter. The current instrumental capabilities at the ESRF-ID13 beamline provide beam sizes from a few microns into the range of 100 nm. A further reduction to about 30 nm can be expected. The reduction of beam size is accompanied by an increase in beam divergence, which limits the accessible lower Q-limit as compared to SAXS cameras with optimized resolution due to low-divergence beams. The availability of recursive data reduction routines allows the extraction of structural information from large 2D detector data sets.

Fundaments of Soft Condensed Matter Scattering and Diffraction with Microfocus Techniques

Noble metal nanoparticles with ligand shells are of interest for applications in catalysis, thermo-plasmonics, and others, involving heating processes. To gain insight into the structure-formation processes in such systems, self-assembly of carbohydrate-functionalized gold nanoparticles during precipitation from solution and during further heating to ca. 340 °C was explored by in situ combination of nanobeam SAXS/WAXS and nanocalorimetry. Upon precipitation from solution, X-ray scattering reveals the appearance of small 2D domains of close-packed nanoparticles. During heating, increasing interpenetration of the nanoparticle soft shells in the domains is observed up to ca. 81 °C, followed by cluster formation at ca. 125 °C, which transform into crystalline gold nuclei at around 160 °C. Above ca. 200 °C, one observes the onset of coalescence and grain growth resulting in gold crystallites of average size of about 100 nm. The observed microstructural changes are in agreement with the in situ heat capacity me...

Thermal transformations of self-assembled gold glyconanoparticles probed by combined nanocalorimetry and X-ray nanobeam scattering.

Instrumentation and selected applications for X-ray microdiffraction experiments on polymer and biopolymer fibers at the European Synchrotron Radiation Facility (ESRF) microfocus beamline are reviewed. Combined SAXS/WAXS experiments can be performed on single fibers with a beam size down to about 5 μm. WAXS experiments can be performed down to about 2 μm and in exceptional cases down to 0.1 μm beam size. The instrumental possibilities are demonstrated for the production line of spider silk.

Applications of micro-SAXS/WAXS to study polymer fibers

The use of borosilicate-glass-capillary optics at a chosen wavelength for low scattering has been explored using an undulator beam at the ESRF. With a 2.3 μm beam at 0.092 nm wavelength, a silver behenate powder sample was scanned in two dimensions with a 2 μm step width. Scattering from single crystallites with d001 = 5.83 nm could be observed. The limit for observation, at low angles, was ca s ≃ 0.1 nm−1 (s = 1/d for d ≃ 10 nm).

Low-angle synchrotron radiation diffraction with glass-capillary optics.

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Low-angle synchrotron radiation diffraction with glass-capillary optics.