Achieving grazing-incidence ultra-small-angle X-ray scattering in a laboratory setup

Abstract

A grazing‐incidence sample stage was designed for realizing grazing‐incidence scattering measurements, especially in the ultra‐small‐angle regime, in a modified Xenocs Xeuss system in the laboratory. The designed sample stage, which is composed of four separate motorized positioning stages, allows the sample to be moved along four different directions to locate it in the proper position for scattering measurement. In an effort to realize grazing‐incidence ultra‐small‐angle scattering (GIUSAXS) measurements, both the separation of the collimation slit systems and the sample‐to‐detector distance have been lengthened. At a separation of the collimation slit systems of 2400 mm and a sample‐to‐detector distance of 6558 mm, the effective smallest scattering vector magnitude qmin reaches 0.01 nm−1. A colloidal crystalline thin film obtained from drying a polystyrene latex dispersion on silicon substrate was measured in the setup in GIUSAXS mode at different beam sizes. The resultant GIUSAXS patterns at smaller beam sizes reveal fine crystalline structures in the film.

Discovery and Insights into Organized Spontaneous Emulsification via Interfacial Self-Assembly of Amphiphilic Bottlebrush Block Copolymers

“…Ultra-small-angle X-ray scattering (USAXS) and cross-sectional SEM are employed to characterize the porous structures formed within different microparticles (Figure ). As shown in Figure a, three ordering peaks are evident in the USAXS spectra of the obtained samples with the q ratios close to 1: √3: √7, which can be assigned to the (100), (110), and (210) lattice planes, respectively, of the HCP nanopore arrays . The average domain spacing ( d -spacing) of the (100) plane increases from 182 to 390 nm with the increase of DP from 96 to 151, calculated according to d = 2π/ q * (Figure b).…”

“…As shown in Figure 5a, three ordering peaks are evident in the USAXS spectra of the obtained samples with the q ratios close to 1: √3: √7, which can be assigned to the (100), (110), and (210) lattice planes, respectively, of the HCP nanopore arrays. 31 The average domain spacing (dspacing) of the (100) plane increases from 182 to 390 nm with the increase of DP from 96 to 151, calculated according to d = 2π/q* (Figure 5b). Analogously, the pore diameter increases with the increase of DP PEO as shown in Figure S8, and was obtained based on the image analysis of the cross-sectional SEM (Figure 5c−h).…”

A high-throughput assembly of beam-shaping channel-cut monochromators for laboratory high-resolution X-ray diffraction and small-angle X-ray scattering experiments

“…In an extreme case, it was possible to obtain a SAXS resolution of better than 13 mm (Stasiecki & Stuhrmann, 1978), but this experiment required the construction of a 50 m long scattering device. More recently, a resolution of up to 600 nm was reported using a modified commercial laboratory setup (Zheng et al, 2015) this device was almost 9 m long.…”

Exploiting the potential of beam-compressing channel-cut monochromators for laboratory high-resolution small-angle X-ray scattering experiments

“…Employing synchrotron radiation and grazing-incidence ultra-SAXS (GIUSAXS), a resolution of 13 mm has been achieved in direct imaging mode (Mü ller-Buschbaum et al, 2007). Recently, a laboratory GIUSAXS setup utilizing a pinhole collimator was reported by Zheng et al (2015).…”