scholarly journals Characterizing dislocation loops in irradiated polycrystalline Zr alloys by X-ray line profile analysis of powder diffraction patterns with satellites

2021 ◽  
Vol 54 (3) ◽  
Author(s):  
Tamás Ungár ◽  
Gábor Ribárik ◽  
Matthew Topping ◽  
Rebecca M. A. Jones ◽  
Xiao Dan Xu ◽  
...  

This work extends the convolutional multiple whole profile (CMWP) line profile analysis (LPA) procedure to determine the total dislocation density and character of irradiation-induced dislocation loops in commercial polycrystalline Zr specimens. Zr alloys are widely used in the nuclear industry as fuel cladding materials in which irradiation-induced point defects evolve into dislocation loops. LPA has long been established as a powerful tool to determine the density and nature of lattice defects in plastically deformed materials. The CMWP LPA procedure is based on the Krivoglaz–Wilkens theory in which the dislocation structure is characterized by the total dislocation density ρ and the dislocation arrangement parameter M. In commercial Zr alloys irradiation-induced dislocation loops broaden the peak profiles, mainly in the tail regions, and occasionally generate small satellites next to the Bragg peaks. In this work, two challenges in powder diffraction patterns of irradiated Zr alloys are solved: (i) determination of the M values from the long tail regions of peaks has been made unequivocal and (ii) satellites have been fitted separately, using physically well established principles, in order to exclude them from the dislocation determination process. Referring to the theory of heterogeneous dislocation distributions, determination of the total dislocation density from the main peaks free of satellites has been justified. The dislocation loop structure has been characterized by the total dislocation density of loops and the M parameter correlated to the dipole character of dislocation loops. The extended CMWP procedure is applied to determine the total dislocation density, the dipole character of dislocation loops, and the fractions of 〈a〉- and 〈c〉-type loops in proton- or neutron-irradiated polycrystalline Zr alloys used in the nuclear energy industry.

2006 ◽  
Vol 39 (1) ◽  
pp. 24-31 ◽  
Author(s):  
Paolo Scardi ◽  
Matteo Leoni

Powder diffraction data collected on a nanocrystalline ceria sample within a round robin conducted by the IUCr Commission on Powder Diffraction were analysed by two alternative approaches: (i) whole-powder-pattern modelling based upon a fundamental microstructural parameters approach, and (ii) a traditional whole-powder-pattern fitting followed by Williamson–Hall and Warren–Averbach analysis. While the former gives results in close agreement with those of transmission electron microscopy, the latter tends to overestimate the domain size effect, providing size values about 20% smaller. The origin of the discrepancy can be traced back to a substantial inadequacy of profile fitting with Voigt profiles, which leads to systematic errors in the following line profile analysis by traditional methods. However, independently of the model, those systematic errors seem to have little effect on the volume-weighted mean size.


1999 ◽  
Vol 32 (4) ◽  
pp. 799-807 ◽  
Author(s):  
Martin Oetzel ◽  
Gernot Heger

In a laboratory X-ray powder diffraction study, the evaluation of the patterns of three Bragg–Brentano powder diffractometers with different monochromator geometries has been undertaken. For the measurements on each diffractometer, the standard reference material SRM 640 (silicon) and the corundum samples SRM 674a and SRM 1976 have been used. In each case, the peak profiles were fitted with a split Pearson VII function and the FWHM (full width at half-maximum) parameters and exponentmwere determined for the left (lower 2θ) and the right (higher 2θ) sides of the Bragg peaks. It was found that there is a strong dependence of both the FWHM and the exponentmon the diffraction angle for the two configurations that included monochromators, whereas nearly constant values ofmwere found for the geometrically simplest diffractometer working without a monochromator. Finally, the two components of the CuKα doublet show systematically different peak profiles. There is a clear difference not only concerning the FWHM, which becomes more obvious at higher 2θ values, but also in the course ofmwith respect to the diffraction angle for the left and the right tails of the powder reflections. This is the main reason for the difficulties inKα2stripping and also in single-line-profile analysis when using theKα doublet. Therefore, it is not surprising that this phenomenon, which can be explained by Heisenberg's uncertainty principle, does affect the reliability (represented by standardRvalues) of structure refinement by the Rietveld method.


2004 ◽  
Vol 443-444 ◽  
pp. 255-258 ◽  
Author(s):  
Yuriy Perlovich ◽  
Margarita Isaenkova

The distributions of substructure parameters for tubes of Zr-based alloys were constructed by use of the X-ray method of Generalized Pole Figures, combining X-ray line analysis and texture measurement. Obtained distributions cover α-Zr crystallites of all orientations and give the fullest description of substructure features of the studied tubes. The interconnection of different substructure parameters are analyzed.


2001 ◽  
Vol 34 (6) ◽  
pp. 699-703 ◽  
Author(s):  
A. Boulle ◽  
C. Legrand ◽  
R. Guinebretière ◽  
J. P. Mercurio ◽  
A. Dauger

Profile fitting procedures associated with integral breadth studies and Fourier analysis are applied to the study of the complex Bi-containing layered perovskite SrBi2Nb2O9. Strong line broadening anisotropy is evidenced. Both `size' and `strain' effects contribute to the observed width. However, `size' broadening along the [00l] direction is essentially caused by stacking faults. The coherently diffracting domain sizes are deduced from Fourier analysis of the diffraction patterns and a rough estimate of the mean distance between faults is given. Thermal annealing significantly decreases the stacking fault density.


2014 ◽  
Vol 794-796 ◽  
pp. 605-610 ◽  
Author(s):  
Alex Penlington ◽  
Bradley Diak ◽  
Hai Ou Jin

An experimental 6XXX series aluminum alloy, Al-0.4Mg-1.2Si-0.49Cu-0.14Mn-0.2Fe(wt.%), was cold rolled 73% and the kinetics of its static recovery studied isochronally between 80 to 350°C, and isothermally at 175 and 205°C. Typical recovery is described by an extrinsic property such as yield stress, however, this study utilized the intrinsic dislocation density extracted from x-ray line profile analysis using a modified Williamson-Hall analysis. The static recovery of dislocation density was fit to the models of Nes [Acta Metall. Mater. 43 (1995) 2189–2207], suggesting that recovery is controlled by the migration of jogged screw dislocations assuming no lateral drift during annealing. The model fit of isothermal annealing at 175°C and 205°C yields activation energies of 0.99 and 1.7 eV/at., respectively. The change in energies can be correlated to an observed change in lattice strain with recovery.


2011 ◽  
Vol 217-218 ◽  
pp. 1743-1746
Author(s):  
Xing Long Guo

TiO2 with 20nm in diameter have been prepared by using magnetron sputtering technique. The structure of these powers was determined by X-ray diffraction experiments. The average grain size and particle size in these powers were measured by the line profile analysis method of X-ray diffraction patterns and by scan electron microscopy, respectively. The thin films were investigated by using XRD, SEM measurements.


2012 ◽  
Vol 45 (5) ◽  
pp. 944-949 ◽  
Author(s):  
A. Leineweber

X-ray powder diffraction data of an Fe3C powder consisting of polycrystalline particles shows pronouncedly anisotropic microstrain broadening of the Bragg reflections. The extent and anisotropy of the broadening can quantitatively be attributed to thermal microstresses induced by anisotropic thermal shrinkage from the preparation temperature of 873 K to the ambient analysis temperature, in conjunction with the elastic anisotropy of Fe3C.


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