scholarly journals Validation study of small-angle X-ray scattering tensor tomography

2020 ◽  
Vol 27 (3) ◽  
pp. 779-787 ◽  
Author(s):  
Manuel Guizar-Sicairos ◽  
Marios Georgiadis ◽  
Marianne Liebi

Small-angle scattering tensor tomography (SASTT) is a recently developed technique able to tomographically reconstruct the 3D reciprocal space from voxels within a bulk volume. SASTT extends the concept of X-ray computed tomography, which typically reconstructs scalar values, by reconstructing a tensor per voxel, which represents the local nanostructure 3D organization. In this study, the nanostructure orientation in a human trabecular-bone sample obtained by SASTT was validated by sectioning the sample and using 3D scanning small-angle X-ray scattering (3D sSAXS) to measure and analyze the orientation from single voxels within each thin section. Besides the presence of cutting artefacts from the slicing process, the nanostructure orientations obtained with the two independent methods were in good agreement, as quantified with the absolute value of the dot product calculated between the nanostructure main orientations obtained in each voxel. The average dot product per voxel over the full sample containing over 10 000 voxels was 0.84, and in six slices, in which fewer cutting artefacts were observed, the dot product increased to 0.91. In addition, SAXS tensor tomography not only yields orientation information but can also reconstruct the full 3D reciprocal-space map. It is shown that the measured anisotropic scattering for individual voxels was reproduced from the SASTT reconstruction in each voxel of the 3D sample. The scattering curves along different 3D directions are validated with data from single voxels, demonstrating SASTT's potential for a separate analysis of nanostructure orientation and structural information from the angle-dependent intensity distribution.

2018 ◽  
Vol 74 (1) ◽  
pp. 12-24 ◽  
Author(s):  
Marianne Liebi ◽  
Marios Georgiadis ◽  
Joachim Kohlbrecher ◽  
Mirko Holler ◽  
Jörg Raabe ◽  
...  

Small-angle X-ray scattering tensor tomography, which allows reconstruction of the local three-dimensional reciprocal-space map within a three-dimensional sample as introduced by Liebiet al.[Nature(2015),527, 349–352], is described in more detail with regard to the mathematical framework and the optimization algorithm. For the case of trabecular bone samples from vertebrae it is shown that the model of the three-dimensional reciprocal-space map using spherical harmonics can adequately describe the measured data. The method enables the determination of nanostructure orientation and degree of orientation as demonstrated previously in a single momentum transferqrange. This article presents a reconstruction of the complete reciprocal-space map for the case of bone over extended ranges ofq. In addition, it is shown that uniform angular sampling and advanced regularization strategies help to reduce the amount of data required.


1984 ◽  
Vol 17 (5) ◽  
pp. 337-343 ◽  
Author(s):  
O. Yoda

A high-resolution small-angle X-ray scattering camera has been built, which has the following features. (i) The point collimation optics employed allows the scattering cross section of the sample to be directly measured without corrections for desmearing. (ii) A small-angle resolution better than 0.5 mrad is achieved with a camera length of 1.6 m. (iii) A high photon flux of 0.9 photons μs−1 is obtained on the sample with the rotating-anode X-ray generator operated at 40 kV–30 mA. (iv) Incident X-rays are monochromated by a bent quartz crystal, which makes the determination of the incident X-ray intensity simple and unambiguous. (v) By rotation of the position-sensitive proportional counter around the direct beam, anisotropic scattering patterns can be observed without adjusting the sample. Details of the design and performance are presented with some applications.


Nature ◽  
2015 ◽  
Vol 527 (7578) ◽  
pp. 353-356 ◽  
Author(s):  
Florian Schaff ◽  
Martin Bech ◽  
Paul Zaslansky ◽  
Christoph Jud ◽  
Marianne Liebi ◽  
...  

2008 ◽  
Vol 81 (4) ◽  
pp. 541-551 ◽  
Author(s):  
Hiroyuki Kishimoto ◽  
Yuya Shinohara ◽  
Yoshiyuki Amemiya ◽  
Katsuaki Inoue ◽  
Yoshio Suzuki ◽  
...  

Abstract We investigated the hierarchical structure of silica, especially agglomerate structure, in stretched rubber by time-resolved two-dimensional ultra-small-angle X-ray scattering (2D-USAXS). Time-resolved 2D-USAXS measurements give us the in-situ structural information up to 5 μm during sample deformation. The results are summarized as follows: at first, the agglomerate is turned so that the long axis of the agglomerate is parallel to the stretching direction, and the “weakly-bonded agglomerates” weakly bonding between agglomerates is broken down. Second, the distance between agglomerates increases with the small deformation of agglomerate. Finally, the “tightly-bonded agglomerates” strongly bonding between agglomerates start to deform. Existence of silane-coupling agents causes the differences in the manner of agglomerate deformation. These kinds of structural information will be a key to understanding the origin of rubber reinforcement by filler such as carbon black and silica.


2007 ◽  
Vol 994 ◽  
Author(s):  
Myriam Dunmont ◽  
Vanessa Coulet ◽  
Gabrielle Regula ◽  
Françoise Bley

AbstractThe techniques of small angle X-ray scattering and transmission electron microscopy are applied to characterize the size distribution of nanocavities in a (111) Si wafer multi-implanted with He+ in the Mev range energy. The comparison between both methods shows that they all give access to the same structural information but small angle X-ray scattering additionally offers the possibility to monitor the cavity size distribution during a thermal treatment. Moreover, providing that the collected data are of good quality, the former method also allows the knowledge of the porosity of the implanted Si wafer.


2014 ◽  
Vol 47 (2) ◽  
pp. 788-798 ◽  
Author(s):  
Ying Su ◽  
Christian Burger ◽  
Benjamin S. Hsiao ◽  
Benjamin Chu

Cellulose nanofibers, extracted from wood pulps using the (2,2,6,6-tetramethylpiperidine-1-yl)oxyl (TEMPO)-mediated oxidation method, are low-cost, sustainable and high-performance materials with potential usage in many applications. The structural information of these cellulose nanofibers in aqueous suspension was characterized by synchrotron small-angle X-ray scattering (SAXS). A simplified ribbon model having a near rectangular cross section was found to give the best fit to the SAXS results. The analytical expression of the ribbon model also led to a higher calculation efficiency compared with the more conventional parallelepiped model. The extracted structural information included the cross-section size and size distribution of the cellulose nanofibers. For example, for nanofibers prepared from the dried pulp of the maritime pine, the size-weighted averages of thickness and width were 3.2 and 12.7 nm, respectively, and the corresponding standard deviations were 2.2 and 5.5 nm, respectively. The scattering results of the size-weighted average of the nanofiber width are also consistent with those determined directly from transmission electron microscopy.


2018 ◽  
Vol 51 (6) ◽  
pp. 1633-1640 ◽  
Author(s):  
Guangfeng Liu ◽  
Yiwen Li ◽  
Hongjin Wu ◽  
Xibo Wu ◽  
Xianhui Xu ◽  
...  

The biological small-angle X-ray scattering (BioSAXS) beamline (BL19U2) at the Shanghai Synchrotron Radiation Facility, China, is dedicated exclusively to small-angle scattering experiments for biological macromolecules in solution. With recent advances in data-analysis algorithms and X-ray detectors, SAXS becomes an ideal complementary technique to other structural and biophysical methods, but it can also be applied alone to obtain important structural information. Owing to the increasing interest in solution scattering studies from the biological community, the workload on BL19U2 has steadily risen. A major upgrade of BL19U2 was performed to improve the beamline data quality, to enrich the possible sample environments and to provide a user-friendly interface. These upgrades involved the major components of BL19U2, including the optical system (slits, beamstop), the electronics, the control and acquisition software, and the sample environments, which resulted in improvements to the collected angular range in BL19U2. These upgrades have significantly broadened the scope of macromolecule size (from kilodaltons to gigadaltons) analysed at the beamline. The dedicated BL19U2 BioSAXS beamline now offers fully automated data-collection and remote-control possibilities. These developments have paved the way for high-throughput studies that generate significant quantities of structure information over a short period of time.


2008 ◽  
Vol 41 (4) ◽  
pp. 715-722 ◽  
Author(s):  
Norbert Stribeck ◽  
Ulrich Nöchel

A method for collimation correction and combination of anisotropic scattering patterns recorded in tandem experiments is proposed. It includes both an advanced two-dimensional extrapolation procedure for the center of the pattern and (compared with the `blind deconvolution' method) a more justified procedure for desmearing from an unknown broad primary beam profile. This semi-blind deconvolution rests on the availability of unsmeared data in a region of the smeared image. Materials exhibiting both ultra-small-angle X-ray scattering (USAXS) and small-angle X-ray scattering (SAXS) must be studied in both angular bands (tandem experiment), in order to collect the complete range of discrete scattering for nanostructure analysis. Merging of the patterns requires desmearing of at least the SAXS pattern from its point-spread function,i.e.the primary beam profile. The distorting effect of single-band experiments on the reconstructed nanostructure of polymer materials is demonstrated.


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