scholarly journals A comparative study of X-ray tomographic microscopy on shales at different synchrotron facilities: ALS, APS and SLS

2012 ◽  
Vol 20 (1) ◽  
pp. 172-180 ◽  
Author(s):  
Waruntorn Kanitpanyacharoen ◽  
Dilworth Y. Parkinson ◽  
Francesco De Carlo ◽  
Federica Marone ◽  
Marco Stampanoni ◽  
...  

Synchrotron radiation X-ray tomographic microscopy (SRXTM) was used to characterize the three-dimensional microstructure, geometry and distribution of different phases in two shale samples obtained from the North Sea (sample N1) and the Upper Barnett Formation in Texas (sample B1). Shale is a challenging material because of its multiphase composition, small grain size, low but significant amount of porosity, as well as strong shape- and lattice-preferred orientation. The goals of this round-robin project were to (i) characterize microstructures and porosity on the micrometer scale, (ii) compare results measured at three synchrotron facilities, and (iii) identify optimal experimental conditions of high-resolution SRXTM for fine-grained materials. SRXTM data of these shales were acquired under similar conditions at the Advanced Light Source (ALS) of Lawrence Berkeley National Laboratory, USA, the Advanced Photon Source (APS) of Argonne National Laboratory, USA, and the Swiss Light Source (SLS) of the Paul Scherrer Institut, Switzerland. The data reconstruction of all datasets was handled under the same procedures in order to compare the data quality and determine phase proportions and microstructures. With a 10× objective lens the spatial resolution is approximately 2 µm. The sharpness of phase boundaries in the reconstructed data collected from the APS and SLS was comparable and slightly more refined than in the data obtained from the ALS. Important internal features, such as pyrite (high-absorbing), and low-density features, including pores, fractures and organic matter or kerogen (low-absorbing), were adequately segmented on the same basis. The average volume fractions of low-density features for sample N1 and B1 were estimated at 6.3 (6)% and 4.5 (4)%, while those of pyrite were calculated to be 5.6 (6)% and 2.0 (3)%, respectively. The discrepancy of data quality and volume fractions were mainly due to different types of optical instruments and varying technical set-ups at the ALS, APS and SLS.

Author(s):  
Doĝa Gürsoy ◽  
Tekin Biçer ◽  
Jonathan D. Almer ◽  
Raj Kettimuthu ◽  
Stuart R. Stock ◽  
...  

A maximum a posteriori approach is proposed for X-ray diffraction tomography for reconstructing three-dimensional spatial distribution of crystallographic phases and orientations of polycrystalline materials. The approach maximizes the a posteriori density which includes a Poisson log-likelihood and an a priori term that reinforces expected solution properties such as smoothness or local continuity. The reconstruction method is validated with experimental data acquired from a section of the spinous process of a porcine vertebra collected at the 1-ID-C beamline of the Advanced Photon Source, at Argonne National Laboratory. The reconstruction results show significant improvement in the reduction of aliasing and streaking artefacts, and improved robustness to noise and undersampling compared to conventional analytical inversion approaches. The approach has the potential to reduce data acquisition times, and significantly improve beamtime efficiency.


2016 ◽  
Vol 23 (4) ◽  
pp. 953-958 ◽  
Author(s):  
Marianne Monteforte ◽  
Ana K. Estandarte ◽  
Bo Chen ◽  
Ross Harder ◽  
Michael H. Huang ◽  
...  

High-energy X-ray Bragg coherent diffraction imaging (BCDI) is a well established synchrotron-based technique used to quantitatively reconstruct the three-dimensional morphology and strain distribution in nanocrystals. The BCDI technique has become a powerful analytical tool for quantitative investigations of nanocrystals, nanotubes, nanorods and more recently biological systems. BCDI has however typically failed for fine nanocrystals in sub-100 nm size regimes – a size routinely achievable by chemical synthesis – despite the spatial resolution of the BCDI technique being 20–30 nm. The limitations of this technique arise from the movement of nanocrystals under illumination by the highly coherent beam, which prevents full diffraction data sets from being acquired. A solution is provided here to overcome this problem and extend the size limit of the BCDI technique, through the design of a novel stabilization method by embedding the fine nanocrystals into a silica matrix. Chemically synthesized FePt nanocrystals of maximum dimension 20 nm and AuPd nanocrystals in the size range 60–65 nm were investigated with BCDI measurement at beamline 34-ID-C of the APS, Argonne National Laboratory. Novel experimental methodologies to elucidate the presence of strain in fine nanocrystals are a necessary pre-requisite in order to better understand strain profiles in engineered nanocrystals for novel device development.


2014 ◽  
Vol 21 (6) ◽  
pp. 1370-1377 ◽  
Author(s):  
Mark A. Le Gros ◽  
Gerry McDermott ◽  
Bertrand P. Cinquin ◽  
Elizabeth A. Smith ◽  
Myan Do ◽  
...  

Beamline 2.1 (XM-2) is a transmission soft X-ray microscope in sector 2 of the Advanced Light Source at Lawrence Berkeley National Laboratory. XM-2 was designed, built and is now operated by the National Center for X-ray Tomography as a National Institutes of Health Biomedical Technology Research Resource. XM-2 is equipped with a cryogenic rotation stage to enable tomographic data collection from cryo-preserved cells, including large mammalian cells. During data collection the specimen is illuminated with `water window' X-rays (284–543 eV). Illuminating photons are attenuated an order of magnitude more strongly by biomolecules than by water. Consequently, differences in molecular composition generate quantitative contrast in images of the specimen. Soft X-ray tomography is an information-rich three-dimensional imaging method that can be applied either as a standalone technique or as a component modality in correlative imaging studies.


2012 ◽  
Vol 27 (4) ◽  
pp. 256-262 ◽  
Author(s):  
W. Wong-Ng ◽  
J. A. Kaduk ◽  
H. Wu ◽  
M. Suchomel

M2(dhtp)·nH2O (M = Mn, Co, Ni, Zn; dhtp = 2,5-dihydroxyterephthalate), known as MOF74, is a family of excellent sorbent materials for CO2 that contains coordinatively unsaturated metal sites and a honeycomb-like structure featuring a broad one-dimensional channel. This paper describes the structural feature and provides reference X-ray powder diffraction patterns of these four isostructural compounds. The structures were determined using synchrotron diffraction data obtained at beam line 11-BM at the Advanced Photon Source (APS) in the Argonne National Laboratory. The samples were confirmed to be hexagonal R 3 (No. 148). From M = Mn, Co, Ni, to Zn, the lattice parameter a of MOF74 ranges from 26.131 73(4) Å to 26.5738(2) Å, c from 6.651 97(5) to 6.808 83(8) Å, and V ranges from 3948.08 Å3 to 4163.99 Å3, respectively. The four reference X-ray powder diffraction patterns have been submitted for inclusion in the Powder Diffraction File (PDF).


Author(s):  
R. W. McClung ◽  
D. R. Johnson

Following an assessment of needs for NDT and characterization of ceramics for the DOE program, Ceramic Technology for Advanced Heat Engines (CTAHE), many NDT projects have been implemented under the sponsorship of CTAHE to address the needs. Tasks at Argonne National Laboratory have involved X-ray computed tomography and nuclear magnetic resonance imaging. The Oak Ridge National Laboratory has emphasized high-frequency ultrasonics, low-voltage radiography, and an advanced system for X-ray computed tomography. A brief investigation was made by Radiation Sciences, Inc., into the feasibility of synchrotron-computed tomography for ceramics. New programs recently initiated at Allison and Garrett integrate ultrasonics, radiography, and other methods into a major effort on life prediction. New programs at Norton and GTE on advanced processing of ceramics also place heavy emphasis on several methods of NDT for process development and control. Initial work on NDT standards has begun in ASTM Committees E-7 and C-28.


Author(s):  
Katarzyna E Matusik ◽  
Daniel J Duke ◽  
Nicholas Sovis ◽  
Andrew B Swantek ◽  
Christopher F Powell ◽  
...  

Gasoline direct injection (GDI) nozzles are manufactured to meet geometric specifications with length scales onthe order of a few hundred microns. The machining tolerances of these nominal dimensions are not always knowndue to the difficulty in accurately measuring such small length scales in a nonintrusive fashion. To gain insight intothe variability of the machined dimensions as well as any effects that this variability may have on the fuel spraybehavior, a series of measurements of the internal geometry and fuel mass distribution were performed on a set ofeight nominally duplicate GDI “Spray G” nozzles provided by the Engine Combustion Network. The key dimensionsof each of the eight nozzle holes were measured with micron resolution using full spectrum x-ray tomographicimaging at the 7-BM beamline of the Advanced Photon Source at Argonne National Laboratory. Fuel densitydistributions at 2 mm downstream of the nozzle tips were obtained by performing x-ray radiography measurementsfor many lines of sight. The density measurements reveal nozzle-to-nozzle as well as hole-to-hole density variations.The combination of high-resolution geometry and fuel distribution datasets allows spray phenomena to be linked tospecific geometric characteristics of the nozzle, such as variability in the hole lengths and counterbore diameters,and the hole inlet corner radii. This analysis provides important insight into which geometrical characteristics ofthe nozzles may have the greatest importance in the development of the injected sprays, and to what degreethese geometric variations might account for the total spray variability. The goal of this work is then to further theunderstanding of the relationship between internal nozzle geometry and fuel injection, provide input to improvecomputational models, and ultimately aid in optimizing injector design for higher fuel efficiency and lower emissionsengines.DOI: http://dx.doi.org/10.4995/ILASS2017.2017.4766


2005 ◽  
Vol 61 (2) ◽  
pp. 129-132 ◽  
Author(s):  
E. N. Caspi ◽  
B. Pokroy ◽  
P. L. Lee ◽  
J. P. Quintana ◽  
E. Zolotoyabko

High-resolution synchrotron powder diffraction measurements were carried out at the 32-ID beamline of the Advanced Photon Source of Argonne National Laboratory in order to clarify the structure of geological aragonite, a widely abundant polymorph of CaCO3. The investigated crystals were practically free of impurity atoms, as measured by wavelength-dispersive X-ray spectroscopy in scanning electron microscopy. A superior quality of diffraction data was achieved by using the 11-channel 111 Si multi-analyzer of the diffracted beam. Applying the Rietveld refinement procedure to the high-resolution diffraction spectra, we were able to extract the aragonite lattice parameters with an accuracy of about 20 p.p.m. The data obtained unambiguously confirm that pure aragonite crystals have orthorhombic symmetry.


1997 ◽  
Vol 3 (S2) ◽  
pp. 905-906
Author(s):  
Mark L. Rivers ◽  
Stephen R. Sutton ◽  
Peter Eng ◽  
Matthew Newville

The Advanced Photon Source (APS) at Argonne National Laboratory is a third-generation synchrotron x-ray source, optimized for producing x-rays from undulators. Such undulator sources provide extremely bright, quasi-monochromatic radiation which is ideal for an x-ray microprobe. Such microprobes can be used for trace element quantification with x-ray fluorescence, or for chemical state determination with x-ray absorption spectroscopy. The GeoSoilEnviroCARS (GSECARS) sector at the APS is building an x-ray microprobe for research in earth, planetary, soil and environmental sciences.The GSECARS undulator source is a standard APS Undulator “A” which is a 3.3 cm period device with 72 periods. The energies of the undulator peaks can be varied by adjusting the gap, and hence the magnetic field of the undulator. The energy of the first harmonic can be varied in this way from approximately 3.1 keV to 14 keV. A measured undulator spectrum is shown in Figure 1.


Author(s):  
O. Coutier-Delgosha ◽  
A. Vabre ◽  
M. Hocevar ◽  
R. Delion ◽  
A. Dazin ◽  
...  

The present paper presents an experimental method to measure velocity fields in a cavitating flow. Dynamics of the liquid phase and of the bubbles are both investigated. The measurements are based on ultra fast X-ray imaging performed at the APS (Advanced Photon Source) of the Argonne National Laboratory. This is collaboration between research teams devoted to fluid mechanics (LML laboratory, Laboratory for water and turbine machines) and experts in X-ray imaging (French atomic commission, Argonne National Laboratory). The experimental device consists of a millimetric Venturi test section associated with a transportable hydraulic loop. Various configurations of velocity, pressure, and temperature have been investigated. This first paper focuses on the experimental equipment and process, and also the description of the image processing which is performed to analyze the results and obtain the velocity fields of both phases within the cavitating areas. Promising preliminary results are also presented.


2018 ◽  
Vol 51 (3) ◽  
pp. 867-882 ◽  
Author(s):  
Jan Ilavsky ◽  
Fan Zhang ◽  
Ross N. Andrews ◽  
Ivan Kuzmenko ◽  
Pete R. Jemian ◽  
...  

Following many years of evolutionary development, first at the National Synchrotron Light Source, Brookhaven National Laboratory, and then at the Advanced Photon Source (APS), Argonne National Laboratory, the APS ultra-small-angle X-ray scattering (USAXS) facility has been transformed by several new developments. These comprise a conversion to higher-order crystal optics and higher X-ray energies as the standard operating mode, rapid fly scan measurements also as a standard operational mode, automated contiguous pinhole small-angle X-ray scattering (SAXS) measurements at intermediate scattering vectors, and associated rapid wide-angle X-ray scattering (WAXS) measurements for X-ray diffraction without disturbing the sample geometry. With each mode using the USAXS incident beam optics upstream of the sample, USAXS/SAXS/WAXS measurements can now be made within 5 min, allowingin situandoperandomeasurement capabilities with great flexibility under a wide range of sample conditions. These developments are described, together with examples of their application to investigate materials phenomena of technological importance. Developments of two novel USAXS applications, USAXS-based X-ray photon correlation spectroscopy and USAXS imaging, are also briefly reviewed.


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