We have previously shown in simulations that X-ray Interferometry using Modulated Phase Gratings can create an interference pattern in clinical detectors from which attenuation, differential phase, and dark-field contrast images can be formed. This interferometric technique is advantageous since it eliminates the need to use an absorption grating as compared to Talbot-Lau grating systems, providing better dose-efficiency. In this work we experimentally evaluated this modulated phase grating system using initial test gratings obtained from Microworks GmbH, Germany. Experiments with the MPG gratings were conducted at the monochromatic 8 keV beamline at the LSU Center for Advanced Microstructures and Devices (CAMD). After analyzing our fringe pattern and eliminating the effect of source grating (G0), we observed stable fringe patterns for our MPG system at different source grating (G0) to MPG distances. The fringe pattern results from these experiments that indicate the feasibility and potential of an X-ray MPG system that could be functional with only a single-phase grating (and source grating) as opposed to a standard interferometry system that additionally requires an absorption grating near the detector.
Phase contrast X-ray not only provides attenuation of tissue, but two other modalities (phase and scatter) in same scan. Scatter (dark-field) images provided by the technology are far more sensitive to structural and density changes of tissue such as lungs and can identify lung disease where conventional X-ray fails. Other areas poised to benefit greatly are mammography and bone joint imaging (eg. imaging arthritis). Of the various interferometer techniques, the two at the forefront are: Far-field Interferometry (FFI) (Miao et al, Nat. Phy. 2015) and Talbot-Lau interferometry (TLI) (Momose JJAP 2005, Pfeiffer Nature 2006). While the TLI has already made clinical strides, the newer FFI has advantage of not requiring an absorption grating (“analyzer”) and provides few-fold higher scatter sensitivity. In this work, a novel 2D single phase-grating (not requiring the analyzer), near-field phase contrast system was simulated using Sommerfeld- Rayleigh diffraction integrals. We observed 2D fringe patterns (pitch 800nm) at 50mm distance from the grating. Such a pattern period of 0.05mm, can be imaged by the LSU-interferometers with CT detector resolution (0.015mm) or Philips mammography detector resolution (0.05mm) making this practical system. Our design has a few advantages over Miao et al FFI system. We accomplish in one X-ray grating the functionality that requires 2-3 phase-grating in their design. And our design can also provide a compact system (source to detector distance < 1m) with control over the fringe pattern by fine tuning grating structure. We retain all the benefits of far-field systems -- of not requiring analyzer and high scatter sensitivity over Talbot-Lau interferometers.
Synchrotron X-ray tomography offers many advantages for the study of flame retardants in polymer blends. The time to acquire the raw projection data is relatively short, the time required to reconstruct and view a 3D image is acceptable, and multiple data sets can be combined to yield 3D chemical distributions, a rather remarkable achievement. However, the workflow is not yet optimized, with too many steps requiring the interaction of a skilled scientist, the re-writing of complex computer codes, and the continued quest for new and improved data analyses. From the point-of-view of the industrial scientists, the attitudes range from “I need to learn more about this experiment" to “just give me a picture". Herein, we discuss the capabilities and resources at the beamline versus the needs of the industrial user. It is a rapidly evolving relationship with a bright future. Recent advances include grating-based phase contrast imaging, dynamic tomography, VisTrails workow, and Apple's iBook Authoring, with the last providing an informal, guided instruction for advanced topics in tomography.
Several methods have been proposed for imaging biological tissue structures at the near micron scale and with user-control of contrast mechanisms that differentiate among the tissue structures. On the one hand, treatment with high-Z contrast agents (Ba, Cs, I, etc.) by injection or soaking and absorption edge imaging distinguishes soft tissue from cornified or bony tissue. This experiment is most compatible with high-bandpass monochromators (ΔE/E between 0.01 - 0.03), such as recently installed at the LSU synchrotron (CAMD). On the other hand, phase contrast imaging does not require any pre-treatment except preservation in formalin, but places more demands upon the X-ray source. This experiment is more compatible with beam lines, such as 13 BM-D at APS, which operates with a narrow bandpass monochromator (ΔE/E ≈ 10-4). Here, we compare imaging results of soft, cornified and bony tissues across the 2x2 matrix of absorption edge versus phase contrast, and high versus narrow bandpass monochromators. In addition, we comment on new data acquisition strategies adapted to the fragile character of biological tissues: (a) a 100 % humidity chamber, and (b) a data acquisition strategy, based on the Greek golden ratio, that more quickly leads to image convergence. The latter incurs the minor cost of reprogramming, or relabeling, images with order and angle. Subsequently, tomography data sets can be acquired based on synchrotron performance and sample fragility.
A fiberglass-reinforced polymer blend with a new-generation flame retardant is studied with multi-energy synchrotron
X-ray tomography to assess the blend homogeneity. Relative to other composite materials, this sample
is difficult to image due to low contrast between fiberglass and the polymer blend. To investigate the chemical
composition of this polymer blend, new procedures and algorithms were developed to produce, segment and analyze
a chemical concentration distribution that assesses the flame retardant distribution throughout the blend.
The results show an extremely homogenous system to the level of the tomography resolution, 3.26 μm. The
processes and algorithms used herein include: (a) correction of reconstructed subvolumes absorption values, (b)
model for chemical distribution, including the fiberglass matrix, (c) model for chemical distribution, excluding
the fiberglass matrix, and (d) an algorithm for generating the radial concentration distribution about the glass
fibers in the polymer matrix.
The conversion of 3D data sets of x-ray absorption images into 3D composition maps requires accurate mass absorption values, high-quality images, and a robust fitting algorithm. We evaluate the status of convenient x-ray absorption databases, the impact of various CCD parameters and imaging strategies (minimal vs over-determined), and styles of least-squares fits of the images (optionally including volume constraints). Concerns raised include the impact of NEXAFS features and limited CCD dynamic range. In the absence of these effects, the reduction of images to composition is fast and robust, as tested with simulations based on element-labeled Shepp-Logan phantoms. These studies allow one to evaluate a recent experiment in which synchrotron X-ray tomography is used to image a multicomponent sample. Those samples consisted of a mixture containing high-impact polystyrene (HIPS) and a two-component flame retardant, a brominated phthalimide dimer and a synergist, antimony oxide (Sb2O3). Complete tomography data sets were acquired at 3.34 micron spatial resolution using seven X-ray energies in the range of 12 to 40 keV, closely spanning Br and Sb 1s electron binding energies at 13.474 and 30.491 keV, respectively.
A tomography beamline has been built recently at the LSU CAMD synchrotron. The instrument consists of a Linux/LabVIEW-controlled CCD and Macintosh/LabVIEW controlled positioning stages. The two computers communicate via LabVIEW/TCP/IP. A Macintosh G4/Linux cluster has been installed for the purpose of on-site reconstruction. Instrument alignment and reconstruction programs are written in LabView, Matlab, and IDL. Applications to date are many. The blending of flame retardants (brominated aromatics, phosphates, and antimony oxide) in high-impact polystyrene is being studied with tomography; this work complements solid-state 81Br NMR. Also, several biological samples are to be studied as part of a multi-investigator project on biological visualization and computational studies. This project gives the tomography workers close access to an ImmersaDesk R2 and other computational resources.
Synchrotron X-ray microtomography shows vesicular structures for toluene/cement mixtures prepared with 1.22 to 3.58 wt% toluene. Three-dimensional imaging of the cured samples shows spherical vesicles with diameters ranging from 20 to 250 microns; a search with electron microscopy for vesicles in the range of 1 - 20 microns proved negative. However, the total vesicle volume, as computed from the microtomography images, accounts for less than 10% of initial toluene. Evidence for toluene in the cement matrix comes from 29Si MAS NMR spectroscopy, which shows a reduction in chain silicates with added toluene. Also, 2H NMR of d8-toluene/cement samples shows high mobility for all toluene and thus no toluene/cement binding. A model that accounts for all observations follows: For loadings below about 3 wt%, most toluene is dispersed in the cement matrix, with a small fraction of the initial toluene phase separating from the cement paste and forming vesicular structures that are preserved in the cured cement. Furthermore, at loadings above 3 wt%, the abundance of vesicles formed during toluene/cement paste mixing leads to macroscopic phase separation.
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