scholarly journals Novel silica stabilization method for the analysis of fine nanocrystals using coherent X-ray diffraction imaging

2016 ◽  
Vol 23 (4) ◽  
pp. 953-958 ◽  
Author(s):  
Marianne Monteforte ◽  
Ana K. Estandarte ◽  
Bo Chen ◽  
Ross Harder ◽  
Michael H. Huang ◽  
...  
Keyword(s):  
National Laboratory ◽  
Argonne National Laboratory ◽  
Three Dimensional ◽  
High Energy ◽  
Silica Matrix ◽  
Stabilization Method ◽  
X Ray ◽  
Novel Device ◽  
Powerful Analytical Tool ◽  
Diffraction Imaging

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.

scholarly journals Maximum a posteriori estimation of crystallographic phases in X-ray diffraction tomography

2015 ◽  
Vol 373 (2043) ◽  
pp. 20140392 ◽  
Author(s):  
Doĝa Gürsoy ◽  
Tekin Biçer ◽  
Jonathan D. Almer ◽  
Raj Kettimuthu ◽  
Stuart R. Stock ◽  
...  
Keyword(s):  
National Laboratory ◽  
Spinous Process ◽  
Argonne National Laboratory ◽  
Three Dimensional ◽  
Polycrystalline Materials ◽  
Reconstruction Method ◽  
Diffraction Tomography ◽  
A Posteriori ◽  
X Ray Diffraction ◽  
X Ray

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.

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 ◽  
...  
Keyword(s):  
Data Quality ◽  
Light Source ◽  
National Laboratory ◽  
Argonne National Laboratory ◽  
Three Dimensional ◽  
Objective Lens ◽  
Low Density ◽  
Experimental Conditions ◽  
X Ray ◽  
Volume Fractions

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.

High-energy micrometre-scale pixel direct conversion X-ray detector

2021 ◽  
Vol 28 (4) ◽  
Author(s):  
Christopher C. Scott ◽  
Michael Farrier ◽  
Yunzhe Li ◽  
Sam Laxer ◽  
Parmesh Ravi ◽  
...  
Keyword(s):  
Phase Contrast ◽  
Detection Efficiency ◽  
National Laboratory ◽  
Argonne National Laboratory ◽  
Direct Conversion ◽  
High Energy ◽  
Amorphous Selenium ◽  
Resolving Power ◽  
Modulation Transfer ◽  
X Ray

The objective of this work was to fabricate and characterize a new X-ray imaging detector with micrometre-scale pixel dimensions (7.8 µm) and high detection efficiency for hard X-ray energies above 20 keV. A key technology component consists of a monolithic hybrid detector built by direct deposition of an amorphous selenium film on a custom designed CMOS readout integrated circuit. Characterization was carried out at the synchrotron beamline 1-BM-B at the Advanced Photon Source of Argonne National Laboratory. The direct conversion detector demonstrated micrometre-scale spatial resolution with a 63 keV modulation transfer function of 10% at Nyquist frequency. In addition, spatial resolving power down to 8 µm was determined by imaging a transmission bar target at 21 keV. X-ray signal linearity, responsivity and lag were also characterized in the same energy range. Finally, phase contrast edge enhancement was observed in a phase object placed in the beam path. This amorphous selenium/CMOS detector technology can address gaps in commercially available X-ray detectors which limit their usefulness for existing synchrotron applications at energies greater than 50 keV; for example, phase contrast tomography and high-resolution imaging of nanoscale lattice distortions in bulk crystalline materials using Bragg coherent diffraction imaging. The technology will also facilitate the creation of novel synchrotron imaging applications for X-ray energies at or above 20 keV.

Electron and ion irradiation-induced dissolution of mechanical twins in the intermetalic U3Si: An in situ HVEM study

1989 ◽  
Vol 47 ◽  
pp. 652-653
Author(s):  
Charles W. Allen ◽  
Robert C. Birtcher
Keyword(s):  
Elevated Temperatures ◽  
Ion Irradiation ◽  
Ion Beam ◽  
National Laboratory ◽  
Argonne National Laboratory ◽  
Heavy Ion ◽  
High Energy ◽  
Mechanical Twinning ◽  
In Situ Experiments

The uranium silicides, including U3Si, are under study as candidate low enrichment nuclear fuels. Ion beam simulations of the in-reactor behavior of such materials are performed because a similar damage structure can be produced in hours by energetic heavy ions which requires years in actual reactor tests. This contribution treats one aspect of the microstructural behavior of U3Si under high energy electron irradiation and low dose energetic heavy ion irradiation and is based on in situ experiments, performed at the HVEM-Tandem User Facility at Argonne National Laboratory. This Facility interfaces a 2 MV Tandem ion accelerator and a 0.6 MV ion implanter to a 1.2 MeV AEI high voltage electron microscope, which allows a wide variety of in situ ion beam experiments to be performed with simultaneous irradiation and electron microscopy or diffraction.At elevated temperatures, U3Si exhibits the ordered AuCu3 structure. On cooling below 1058 K, the intermetallic transforms, evidently martensitically, to a body-centered tetragonal structure (alternatively, the structure may be described as face-centered tetragonal, which would be fcc except for a 1 pet tetragonal distortion). Mechanical twinning accompanies the transformation; however, diferences between electron diffraction patterns from twinned and non-twinned martensite plates could not be distinguished.

Synchrotron X-ray studies of metal-organic framework M2(2,5-dihydroxyterephthalate), M = (Mn, Co, Ni, Zn) (MOF74)

2012 ◽  
Vol 27 (4) ◽  
pp. 256-262 ◽  
Author(s):  
W. Wong-Ng ◽  
J. A. Kaduk ◽  
H. Wu ◽  
M. Suchomel
Keyword(s):  
Powder Diffraction ◽  
Metal Organic Framework ◽  
National Laboratory ◽  
Argonne National Laboratory ◽  
Lattice Parameter ◽  
X Ray ◽  
Metal Organic ◽  
Sorbent Materials ◽  
Diffraction Patterns ◽  
Unsaturated Metal Sites

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).

Epitaxial Ni nanoparticles on CaF2(001), (110) and (111) surfaces studied by three-dimensional RHEED, GIXD and GISAXS reciprocal-space mapping techniques

2017 ◽  
Vol 50 (3) ◽  
pp. 830-839 ◽  
Author(s):  
S. M. Suturin ◽  
V. V. Fedorov ◽  
A. M. Korovin ◽  
N. S. Sokolov ◽  
A. V. Nashchekin ◽  
...  
Keyword(s):  
Lattice Structure ◽  
Three Dimensional ◽  
Grazing Incidence ◽  
High Energy ◽  
Reciprocal Space ◽  
Mapping Technique ◽  
Face Centered Cubic ◽  
X Ray ◽  
Cubic Lattice ◽  
Face Centered

The development of growth techniques aimed at the fabrication of nanoscale heterostructures with layers of ferroic 3dmetals on semiconductor substrates is very important for their potential usage in magnetic media recording applications. A structural study is presented of single-crystal nickel island ensembles grown epitaxially on top of CaF2/Si insulator-on-semiconductor heteroepitaxial substrates with (111), (110) and (001) fluorite surface orientations. The CaF2buffer layer in the studied multilayer system prevents the formation of nickel silicide, guides the nucleation of nickel islands and serves as an insulating layer in a potential tunneling spin injection device. The present study, employing both direct-space and reciprocal-space techniques, is a continuation of earlier research on ferromagnetic 3dtransition metals grown epitaxially on non-magnetic and magnetically ordered fluorides. It is demonstrated that arrays of stand-alone faceted nickel islands with a face-centered cubic lattice can be grown controllably on CaF2surfaces of (111), (110) and (001) orientations. The proposed two-stage nickel growth technique employs deposition of a thin seeding layer at low temperature followed by formation of the islands at high temperature. The application of an advanced three-dimensional mapping technique exploiting reflection high-energy electron diffraction (RHEED) has proved that the nickel islands tend to inherit the lattice orientation of the underlying fluorite layer, though they exhibit a certain amount of {111} twinning. As shown by scanning electron microscopy, grazing-incidence X-ray diffraction (GIXD) and grazing-incidence small-angle X-ray scattering (GISAXS), the islands are of similar shape, being faceted with {111} and {100} planes. The results obtained are compared with those from earlier studies of Co/CaF2epitaxial nanoparticles, with special attention paid to the peculiarities related to the differences in lattice structure of the deposited metals: the dual-phase hexagonal close-packed/face-centered cubic lattice structure of cobalt as opposed to the single-phase face-centered cubic lattice structure of nickel.

scholarly journals NDE Development for Ceramics for Advanced Heat Engines

1991 ◽  
Author(s):  
R. W. McClung ◽  
D. R. Johnson
Keyword(s):  
Computed Tomography ◽  
Process Development ◽  
Low Voltage ◽  
National Laboratory ◽  
Argonne National Laboratory ◽  
Ceramic Technology ◽  
X Ray ◽  
Oak Ridge ◽  
Heat Engines ◽  
X Ray Computed

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.

scholarly journals A study on the relationship between internal nozzle geometry and injected mass distribution of eight ECN Spray G nozzles.

2017 ◽  
Author(s):  
Katarzyna E Matusik ◽  
Daniel J Duke ◽  
Nicholas Sovis ◽  
Andrew B Swantek ◽  
Christopher F Powell ◽  
...  
Keyword(s):  
Mass Distribution ◽  
National Laboratory ◽  
Argonne National Laboratory ◽  
Gasoline Direct Injection ◽  
Nozzle Geometry ◽  
Hole Density ◽  
Full Spectrum ◽  
Length Scales ◽  
X Ray ◽  
The Relationship

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

On the structure of aragonite

2005 ◽  
Vol 61 (2) ◽  
pp. 129-132 ◽  
Author(s):  
E. N. Caspi ◽  
B. Pokroy ◽  
P. L. Lee ◽  
J. P. Quintana ◽  
E. Zolotoyabko
Keyword(s):  
High Resolution ◽  
National Laboratory ◽  
Argonne National Laboratory ◽  
Orthorhombic Symmetry ◽  
X Ray ◽  
Impurity Atoms ◽  
Synchrotron Powder Diffraction ◽  
Refinement Procedure ◽  
Photon Source

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.

Three-dimensional X-ray diffraction imaging of process-induced dislocation loops in silicon

2011 ◽  
Vol 44 (3) ◽  
pp. 526-531 ◽  
Author(s):  
David Allen ◽  
Jochen Wittge ◽  
Jennifer Stopford ◽  
Andreas Danilewsky ◽  
Patrick McNally
Keyword(s):  
Semiconductor Industry ◽  
Three Dimensional ◽  
Crystal Defects ◽  
Three Dimensions ◽  
Dimensional Structure ◽  
Dislocation Loops ◽  
X Ray Diffraction ◽  
X Ray ◽  
Diffraction Imaging ◽  
Relationship Of

In the semiconductor industry, wafer handling introduces micro-cracks at the wafer edge and the causal relationship of these cracks to wafer breakage is a difficult task. By way of understanding the wafer breakage process, a series of nano-indents were introduced both into 20 × 20 mm (100) wafer pieces and into whole wafers as a means of introducing controlled strain. Visualization of the three-dimensional structure of crystal defects has been demonstrated. The silicon samples were then treated by various thermal anneal processes to initiate the formation of dislocation loops around the indents. This article reports the three-dimensional X-ray diffraction imaging and visualization of the structure of these dislocations. A series of X-ray section topographs of both the indents and the dislocation loops were taken at the ANKA Synchrotron, Karlsruhe, Germany. The topographs were recorded on a CCD system combined with a high-resolution scintillator crystal and were measured by repeated cycles of exposure and sample translation along a direction perpendicular to the beam. The resulting images were then rendered into three dimensions utilizing open-source three-dimensional medical tomography algorithms that show the dislocation loops formed. Furthermore this technique allows for the production of a video (avi) file showing the rotation of the rendered topographs around any defined axis. The software also has the capability of splitting the image along a segmentation line and viewing the internal structure of the strain fields.

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