Novel Near Field Detector for Three-Dimensional X-Ray Diffraction Microscopy

MRS Advances ◽  
2018 ◽  
Vol 3 (39) ◽  
pp. 2341-2346 ◽  
Author(s):  
Scott Annett ◽  
Sergio Morelhao ◽  
Darren Dale ◽  
Stefan Kycia
Keyword(s):  
New Technologies ◽  
Spatial Information ◽  
Near Field ◽  
Three Dimensional ◽  
High Energy ◽  
Field Of View ◽  
Large Field ◽  
X Ray Diffraction ◽  
Synchrotron Source ◽  
X Ray

AbstractThree dimensional X-ray diffraction (3DXRD) microscopy is a powerful technique that provides crystallographic and spatial information of a large number, of the order of thousands, of crystalline grains in a sample simultaneously. A key component of every 3DXRD microscopy experiment is the near field detector that provides high resolution spatial information of the grains. In this work we present a novel design for a semi-transparent, 16 megapixel near field detector. As opposed to a typical single scintillator phosphor detector, this design, we call the Quad Near Field Detector, uses four quadrants. It has a total field of view is 5.3 mm x 5.3 mm with an effective pixel size of 1.3 µm x 1.3 µm. The detector’s relatively large field of view can be used to obtain higher order diffraction spots which we anticipate will lead to improved spatial resolution in grain reconstructions. The large field of view can also enable the detector to be positioned further from the sample, in this way increasing the working distance and enabling larger environmental cells for in-situ studies. Many alignment parameters can be resolved by careful mechanical design. For this reason a novel translation stage for focusing the microscopes was developed, tested, and implemented. The near field detector was calibrated and characterized at the Cornell High Energy Synchrotron Source. The operational feasibility of such a multi-plate detector demonstrated in this work paves the way for new technologies in instrumentation of 3DXRD microscopy.

scholarly journals Three-dimensional α colony characterization and prior-β grain reconstruction of a lamellar Ti–6Al–4V specimen using near-field high-energy X-ray diffraction microscopy

2015 ◽  
Vol 48 (4) ◽  
pp. 1165-1171 ◽  
Author(s):  
E. Wielewski ◽  
D. B. Menasche ◽  
P. G. Callahan ◽  
R. M. Suter
Keyword(s):  
Near Field ◽  
Three Dimensional ◽  
High Energy ◽  
Grain Structure ◽  
X Ray Diffraction ◽  
Orientation Field ◽  
X Ray ◽  
Hexagonal Close Packed ◽  
Flood Fill ◽  
Diffraction Microscopy

Near-field high-energy X-ray diffraction microscopy has been used to characterize the three-dimensional (3-D) crystallographic orientation field of the hexagonal close-packed α phase in a bulk Ti–6Al–4V specimen with a lamellar (β-annealed) microstructure. These data have been segmented using a 3-D misorientation-based grain finding algorithm, providing unprecedented information about the complex 3-D morphologies and spatial misorientation distributions of the transformed α lamella colonies. A 3-D Burgers orientation relationship-based flood-fill algorithm has been implemented to reconstruct the morphologies and crystallographic orientations of the high-temperature body-centered cubic prior-β grains. The combination of these data has been used to gain an understanding of the role of the prior-β grain structure in the formation of specific morphologies and spatial misorientation distributions observed in the transformed α colony structures. It is hoped that this understanding can be used to develop transformation structures optimized for specific applications and to produce more physically realistic synthetic microstructures for use in simulations.

Evaluation of grain-average stress tensor in a tensile-deformed Al–Mn polycrystal by high-energy X-ray diffraction

2017 ◽  
Vol 50 (4) ◽  
pp. 1144-1157 ◽  
Author(s):  
Loïc Renversade ◽  
András Borbély
Keyword(s):  
Rotation Axis ◽  
Three Dimensional ◽  
Calibration Method ◽  
High Energy ◽  
Normal Strain ◽  
X Ray Diffraction ◽  
Synchrotron Source ◽  
X Ray ◽  
Strain Stress ◽  
Individual Grains

Three-dimensional X-ray diffraction was applied to characterize the strain/stress evolution in individual grains of an Al–0.3 wt% Mn polycrystal deformedin situat a synchrotron source. Methodological aspects concerning the calibration of the geometrical setup and the evaluation of the strain/stress tensors are discussed. A two-step calibration method separately treating the detector and the rotation axis allows one to determine the centre-of-mass position and crystallographic orientation of grains with standard errors of about 1.5 µm and 0.02°, respectively. Numerical simulations indicate that the error of normal strain components (about 1 × 10−4) is mainly caused by calibration errors, while the error of shear components (about 0.5 × 10−4) is largely influenced by counting statistics and random spot-centre errors due to detector distortion. The importance of monitoring the beam energy is emphasized.

scholarly journals In Situ Stress Tensor Determination during Phase Transformation of a Metal Matrix Composite by High-Energy X-ray Diffraction

Materials ◽  
2018 ◽  
Vol 11 (8) ◽  
pp. 1415 ◽  
Author(s):  
Guillaume Geandier ◽  
Lilian Vautrot ◽  
Benoît Denand ◽  
Sabine Denis
Keyword(s):  
Phase Transformation ◽  
Stress Tensor ◽  
Metal Matrix Composite ◽  
Matrix Composite ◽  
Metal Matrix ◽  
High Energy ◽  
X Ray Diffraction ◽  
Synchrotron Source ◽  
X Ray

In situ high-energy X-ray diffraction using a synchrotron source performed on a steel metal matrix composite reinforced by TiC allows the evolutions of internal stresses during cooling to be followed thanks to the development of a new original experimental device (a transportable radiation furnace with controlled rotation of the specimen). Using the device on a high-energy beamline during in situ thermal treatment, we were able to extract the evolution of the stress tensor components in all phases: austenite, TiC, and even during the martensitic phase transformation of the matrix.

Three-dimensional grain resolved strain mapping using laboratory X-ray diffraction contrast tomography: theoretical analysis

2022 ◽  
Vol 55 (1) ◽  
Author(s):  
Adam Lindkvist ◽  
Yubin Zhang
Keyword(s):  
Near Field ◽  
Three Dimensional ◽  
Simulated Data ◽  
Three Dimensions ◽  
X Ray Diffraction ◽  
Strain Mapping ◽  
X Ray ◽  
Microstructural Parameters ◽  
Diffraction Contrast ◽  
Sample Distance

Laboratory diffraction contrast tomography (LabDCT) is a recently developed technique to map crystallographic orientations of polycrystalline samples in three dimensions non-destructively using a laboratory X-ray source. In this work, a new theoretical procedure, named LabXRS, expanding LabDCT to include mapping of the deviatoric strain tensors on the grain scale, is proposed and validated using simulated data. For the validation, the geometries investigated include a typical near-field LabDCT setup utilizing Laue focusing with equal source-to-sample and sample-to-detector distances of 14 mm, a magnified setup where the sample-to-detector distance is increased to 200 mm, a far-field Laue focusing setup where the source-to-sample distance is also increased to 200 mm, and a near-field setup with a source-to-sample distance of 200 mm. The strain resolution is found to be in the range of 1–5 × 10−4, depending on the geometry of the experiment. The effects of other experimental parameters, including pixel binning, number of projections and imaging noise, as well as microstructural parameters, including grain position, grain size and grain orientation, on the strain resolution are examined. The dependencies of these parameters, as well as the implications for practical experiments, are discussed.

Structure of Glass and Liquid Studied with a Conical Nozzle Levitation and Diffraction Technique

2007 ◽  
Vol 539-543 ◽  
pp. 2012-2017 ◽  
Author(s):  
Akitoshi Mizuno ◽  
Shinji Kohara ◽  
Seiichi Matsumura ◽  
Masahito Watanabe ◽  
J.K.R. Weber ◽  
...  
Keyword(s):  
Amorphous Materials ◽  
High Energy ◽  
Conical Nozzle ◽  
Atomic Configuration ◽  
X Ray Diffraction ◽  
Synchrotron Source ◽  
X Ray ◽  
3 Dimensional ◽  
Glass Forming ◽  
The Third

Two topics are described for structure analyses of glass and liquid using a combination of conical nozzle levitation (CNL) technique and diffraction experiments. The structure of high-purity bulk forsterite (Mg2SiO4) glass synthesized by a CNL technique has been determined by a combination of high-energy x-ray, neutron diffraction, and reverse Monte Carlo (RMC) modeling technique. The 3-dimensional atomic configuration derived from RMC modeling revealed that unusual network structure. In order to study structures of high-temperature and undercooled liquids, a CNL system has been developed and integrated with the two-axis diffractometer for glass, liquid, and amorphous materials at SPring-8, which is one of the third-generation synchrotron source. High-energy x-ray diffraction experiments were performed to obtain reliable diffraction data for the liquid phase of metallic glass-forming Zr-Cu binary alloys.

Development and Characterisation of New Biocompatible Sn-Mg Lead-Free Solder

2019 ◽  
Vol 31 ◽  
pp. 6-10
Author(s):  
Martin Ďurišin ◽  
Juraj Ďurišin ◽  
Ondrej Milkovič ◽  
Alena Pietriková ◽  
Karel Saksl
Keyword(s):  
Melt Spinning ◽  
High Energy ◽  
Grain Structure ◽  
Lead Free ◽  
Lead Free Solder ◽  
X Ray Diffraction ◽  
Synchrotron Source ◽  
Heterogeneous Distribution ◽  
X Ray ◽  
Free Solder

This work is focused on a development and research of a new lead-free Sn-Mg solder, alloy compatible with the human body. Tin and magnesium are biocompatible elements which do not cause an inflammation or allergic reactions with living tissues. We have prepared the Sn97Mg3 solder (wt. %) by a rapid solidification of its melt on a copper wheel (melt-spinning technique). This solder may find applications in electronic devices for intracorporeal utilisation. The microstructure of the prepared solder exhibits a heterogeneous distribution of the SnMg2 intermetallic particles within the β-Sn matrix. Structure of the solder was studied by an in-situ high energy X-ray diffraction experiment (energy of an X-ray photon: 60 keV) where 2D XRD patterns were collected from the sample in the temperature range from 298 K to 566 K. The experiment was performed at a high brilliance 3rd generation synchrotron source of radiation (PETRA III storage ring, DESY, Hamburg, Germany) at the P02 undulator beamline. From the measured X-ray diffraction data by applying the Rietveld refinement technique we have obtained thermal volume expansion data, mean positions of atoms as well as isotropic atomic displacement parameters of the constituent SnMg2 and the β-Sn crystalline phases. Thermal behaviour was studied by differential scanning calorimetry at heating rates of 5, 15, 30 and 60 K.min-1 and compared with the measured X-ray data. Our main goal lies in a preparation of a lead-free solder with fine grain structure made exclusively of biocompatible elements. We demonstrated that the rapid melt solidification technique leads to in an improvement and better thermal stability of this alloy.

Determining grain resolved stresses in polycrystalline materials using three-dimensional X-ray diffraction

2010 ◽  
Vol 43 (3) ◽  
pp. 539-549 ◽  
Author(s):  
Jette Oddershede ◽  
Søren Schmidt ◽  
Henning Friis Poulsen ◽  
Henning Osholm Sørensen ◽  
Jonathan Wright ◽  
...  
Keyword(s):  
Near Field ◽  
Three Dimensional ◽  
Polycrystalline Sample ◽  
Polycrystalline Materials ◽  
Interstitial Free ◽  
Outlier Rejection ◽  
X Ray Diffraction ◽  
Positional Accuracy ◽  
X Ray ◽  
Elastic Loading

An algorithm is presented for characterization of the grain resolved (type II) stress states in a polycrystalline sample based on monochromatic X-ray diffraction data. The algorithm is a robust 12-parameter-per-grain fit of the centre-of-mass grain positions, orientations and stress tensors including error estimation and outlier rejection. The algorithm is validated by simulations and by two experiments on interstitial free steel. In the first experiment, using only a far-field detector and a rotation range of 2 × 110°, 96 grains in one layer were monitored during elastic loading and unloading. Very consistent results were obtained, with mean resolutions for each grain of approximately 10 µm in position, 0.05° in orientation, and 8, 20 and 13 × 10−5in the axial, normal and shear components of the strain, respectively. The corresponding mean deviations in stress are 30, 50 and 15 MPa in the axial, normal and shear components, respectively, though some grains may have larger errors. In the second experiment, where a near-field detector was added, ∼2000 grains were characterized with a positional accuracy of 3 µm.

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