SWAXS Characterisation of Nanostructures - SAXSpace

Nanostructured samples and materials can be efficiently and reliable characterized using Anton Paar’s SAXSpace small- and wide-angle X-ray scattering (SWAXS) system. Users can obtain the size, shape, and size distribution of nano-sized samples and particle domains with the help of the SAXSpace. The device is ideally suited for the analysis of colloidal, biological (Bio-SAXS), and isotropic samples.

The SWAXS system also has a wide selection of accurate and versatile sample stages to meet each SAXS application. Easy handling and automatic alignment facilitate smooth operation. With the unique combination of robust design, short measurement time, and high system uptime, the device not only provides superior WAXS or SAXS results but also ensures high sample throughput. These capabilities make SAXSpace ideally suited to explore nanostructure in various materials, including surfactants, pharmaceuticals, proteins, foods, polymers, and nanoparticles.

Key Features

The key features of the SAXSpace are as follows:

A Small Genius

  • Scatterless beam collimation concept for superior resolution
  • Features such as push-button alignment and auto-detection of sample stages ensures smooth operation
  • The combination of high signal-to-noise ratio and X-ray beam flux ensures quick measurements and very high SWAXS data quality

Outstanding Features

  • Small footprint due to the integration of all system components into a single compact platform
  • TrueFocus – Easy and time-saving alignment can be obtained at the click of a button
  • SmartSAXS – Offers high sample throughput and unlimited experimental opportunities, thanks to dual beam concept with several beam line options
  • TrueSWAXS – Small- and wide-angle scattering measurements can be simultaneously performed at scattering angles up to 74° 2θ

Full Experimental Flexibility

  • High-throughput screening of solid and liquid nanostructured samples
  • StageMaster – Accurate XYZ stage with auto-detection of sample stages
  • Wide choice of sample holders and stages to suit virtually all applications, including temperature-dependent SWAXS studies and measurements under controlled humidity
  • Optimized design for low-concentrated and weakly scattering samples like biomaterials

Powerful Control and Data Analysis Software

  • Versatile software for sophisticated SAXS data interpretation
  • SAXSquant™ – Simple and rapid data processing with the help of customizable templates
  • SAXSdrive™ – Full system control for automated SWAXS analyses

Applications of SWAXS System

The SAXSpace system was used to examine microfilbril angle (MFA) in coir fibers during tensile straining. The system was operated in point collimation mode, combined with the integrated TS 600 tensile stage. Structural changes in complicated materials can be defined during mechanical tests.

Introduction

A key structural feature for natural fibers and wood is lignocellulosics, where the angle of the helical windings of cellulose microfibrils in the secondary cell is defined as its MFA. The changes in the MFA value can alter the mechanical properties of the tissues, such as fracture stress, strain, and Young’s modulus.

Here, coir fibres obtained from the coconut’s mesoscarp were studied using the SAXSpace system, equipped with a TS 600 tensile stage. This common natural fiber primarily consists of cellulose and lignin, and is enhanced for maximum fracture strain. The resulting fibre exhibits the highest possible MFA of roughly 45°. In earlier studies, the coir deformation behaviour was examined under tensile stress using the synchrotron radiation. These studies suggest that the MFA of the cellulose fibers varies in proportion to the degree of the applied strain.

Experiment and Results

Coir fibers, similar to the ones investigated in earlier studies, were coupled to a plastic support and mounted onto the TS 600 tensile stage. Using the SAXSpace system in point-collimation mode, 2D diffraction patterns of individual fibers were obtained at different levels of strain. The next step was collecting the signal in wide-angle mode, because of the diffraction of cellulose fibers at comparatively large diffraction angles of roughly 23°. The SAXSquant software package was used to azimuthally integrate the resulting 2D diffraction data of each strain level along the De-bye-Scherrer rings of the cellulose 200 reflections (Figure 1).

2D diffraction pattern of coir fiber mounted in the TS 600 tensile stage while straining the sample.

Figure 1. 2D diffraction pattern of coir fiber mounted in the TS 600 tensile stage while straining the sample.

The MFA between the cellulose fibers for the unstrained fibers was 45°. Upon stretching the fiber, the MFA didn’t change significantly until reaching a strain of 3%. Beyond this threshold value, the MFA between the cellulose fibers started to decrease. At 7% strain level, the MFA was reduced to a value of 38° (Figure 2).

Azimuthal integration along the 200 reflections. The position of the maximum is shifted to the center for the strained fiber.

Figure 2. Azimuthal integration along the 200 reflections. The position of the maximum is shifted to the center for the strained fiber.

The study results have demonstrated that the SAXSpace system, in combination with a built-in TS600 tensile stage, provides a robust tool for in-situ analysis of structural changes occurring in materials during mechanical tests. This approach helps to determine the relationship between the structure and the property of thin foils of biomaterials, metals, and polymers under laboratory conditions.

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