Line broadening analysis using integral breadth methods: a critical review

2004 ◽  
Vol 37 (3) ◽  
pp. 381-390 ◽  
Author(s):  
P. Scardi ◽  
M. Leoni ◽  
R. Delhez
Keyword(s):  
Ball Milling ◽  
Critical Review ◽  
Nickel Powder ◽  
Profile Analysis ◽  
Line Profile Analysis ◽  
Line Broadening ◽  
Integral Breadth ◽  
Nanocrystalline Ceria ◽  
Quantitative Results ◽  
Hall Method

Integral breadth methods for line profile analysis are reviewed, including modifications of the Williamson–Hall method recently proposed for the specific case of dislocation strain broadening. Two cases of study, supported by the results of a TEM investigation, are considered in detail: nanocrystalline ceria crystallized from amorphous precursors and highly deformed nickel powder produced by extensive ball milling. A further application concerns a series of Fe–Mo powder specimens that were ball milled for increasing time. Traditional and modified Williamson–Hall methods confirm their merits for a rapid overview of the line broadening effects and possible understanding of the main causes. However, quantitative results are generally not reliable. Limits in the applicability of integral breadth methods and reliability of the results are discussed in detail.

XRD Line Broadening Analysis with Ball Milled Palladium

2004 ◽  
Vol 443-444 ◽  
pp. 119-122 ◽  
Author(s):  
I. Lucks ◽  
P. Lamparter ◽  
Jian Xu ◽  
Eric J. Mittemeijer
Keyword(s):  
Profile Analysis ◽  
Planetary Mill ◽  
Line Profile Analysis ◽  
Size Distributions ◽  
Line Broadening ◽  
X Ray Diffraction ◽  
Diffraction Line Profile ◽  
Crystallite Sizes ◽  
Palladium Powder ◽  
Quantitative Results

Palladium powder was deformed by ball milling under an argon atmosphere in two types of mills for different milling times. Two methods for X-ray diffraction line profile analysis, the Williamson-Hall method and the Warren-Averbach method, yielded similar trends, but different quantitative results for crystallite sizes (column lengths) and microstrains. With both methods, from the anisotropic line broadening for planetary milled Pd smaller crystallite sizes and larger microstrains were obtained along the <100> direction than along <111>. Milling in a shaker mill causes microstrain higher by a factor of about two than milling in a planetary mill. The evolution of the crystallite size upon milling was discussed in terms of bimodal size distributions.

The Microstructure of Nanocrystalline Powders from Line Profile Analysis

2004 ◽  
Vol 443-444 ◽  
pp. 71-76 ◽  
Author(s):  
Nathalie Audebrand ◽  
Daniel Louër
Keyword(s):  
Line Profile ◽  
Profile Analysis ◽  
Theoretical Background ◽  
Nanocrystalline Powders ◽  
Line Profile Analysis ◽  
Line Broadening ◽  
Experimental Conditions ◽  
Profile Fitting ◽  
Propagation Of Errors ◽  
Structure Imperfection

The theoretical background currently used in line profile analysis is reviewed. It covers the size and structure imperfection effects at the origin of diffraction line broadening. The propagation of errors, i.e. old errors and new errors related to profile fitting techniques, is commented. The experimental conditions for minimising errors are described. Representative examples of microstructure characterisation of nanopowders are presented.

Peak Profile Evaluation for Thin Films

2014 ◽  
pp. 212-241
Keyword(s):  
Thin Films ◽  
Crystallite Size ◽  
Line Profile ◽  
Interference Effect ◽  
Profile Analysis ◽  
Reciprocal Lattice ◽  
Partial Coherence ◽  
Line Profile Analysis ◽  
Line Broadening ◽  
Diffraction Line Profile

The special phenomena in X-ray diffraction line profile analysis occurring in thin films is overviewed in this chapter. In the case of textured nanocrystalline thin films, the line broadening caused by the crystallite size increases with the length of the diffraction vector. This effect is explained by the interference of X-rays scattered coherently from adjacent crystallites with close orientations. The partial coherence of adjacent nanocrystallites is caused by the overlapping of their reciprocal lattice points. The smaller the size and the stronger the orientation preference of crystallites, the better the coherence. This interference effect yields narrowing of line profiles at small diffraction angles, while it has no influence on line broadening at large angles. Therefore, the traditional line profile evaluation methods give much larger crystallite size than the real value and may detect a false microstrain broadening. Some ways for the correction of the interference effect are proposed. Detailed case studies are given for the determination of the defect structure in thin films by line profile analysis.

An evaluation of methods of diffraction-line broadening analysis applied to ball-milled molybdenum

2004 ◽  
Vol 37 (2) ◽  
pp. 300-311 ◽  
Author(s):  
I. Lucks ◽  
P. Lamparter ◽  
E. J. Mittemeijer
Keyword(s):  
Line Profile ◽  
Strain Field ◽  
Fourier Coefficients ◽  
Field Method ◽  
Diffraction Line ◽  
Line Profile Analysis ◽  
Cauchy Type ◽  
Line Broadening ◽  
Integral Breadth ◽  
Crystallite Sizes

A comparison has been carried out of different methods of X-ray diffraction-line profile analysis for the determination of crystallite sizes and microstrains, namely the integral breadth method and three methods based on Fourier analysis of diffraction lines, namely the Warren–Averbach method, an `alternative method' and a profile synthesis strain field method. The analyses have been applied to Mo powder ball milled in two types of mills: an attritor and a planetary mill. Using the Williamson–Hall integral breadth method, the line broadening at moderate deformation is attributed solely to microstrain,i.e.practically no size broadening is detected. The three methods based on the Fourier coefficients of diffraction lines yield comparable values for crystallite sizes and microstrains. With the profile synthesis strain field method, if a size effect is included, it is possible to fit the experimental Fourier coefficients over the entire range of the relevant scale of correlation distances. The line profile shape due to microstrains, as derived with the strain field method, exhibits a systematic dependence on the integral breadth. With increasing breadth, the shape changes from a Cauchy type to a Gaussian type, suggesting a change of the dislocation arrangement with increasing plastic deformation of molybdenum powders.

Determination of Nanocrystalline Fe80Cr20 Powder Based Alloys Using Williamson-Hall Method

2010 ◽  
Vol 129-131 ◽  
pp. 999-1003 ◽  
Author(s):  
Hendi Saryanto ◽  
S. Khaerudini Deni ◽  
Pudji Untoro ◽  
Mat Husin Saleh ◽  
Darwin Sebayang
Keyword(s):  
Mechanical Alloying ◽  
Crystallite Size ◽  
Line Profile ◽  
Profile Analysis ◽  
Line Profile Analysis ◽  
X Rays ◽  
Diffraction Line Profile ◽  
Transmission Electron ◽  
Microstructure Morphology ◽  
Hall Method

The aim of this study is to determine the nanocrystalline size by using Williamson-Hall method of Fe80Cr20 powder which prepared by mechanical alloying process. X-rays diffraction line profile analysis was adopted to analyze the crystallite size and microstrains of Fe80Cr20 alloys powder. Transmission Electron Microscopy (TEM) was used to examine the microstructure morphology of the nanosized of Fe80Cr20 alloys. The crystallite size, microstrain, and lattice parameters were estimated by Williamson–Hall plot. The results showed that the mechanical alloying processes resulted the final product in nanocrystalline size range (below 12 nm) which confirmed by TEM observation and XRD line profile analysis.

Ex-oxalate magnesium oxide, a strain-free nanopowder studied with diffraction line profile analysis

2006 ◽  
Vol 21 (3) ◽  
pp. 190-199 ◽  
Author(s):  
Nathalie Audebrand ◽  
Christine Bourgel ◽  
Daniel Louër
Keyword(s):  
Magnesium Oxide ◽  
Profile Analysis ◽  
Spherical Shape ◽  
Diffraction Line ◽  
Line Profile Analysis ◽  
Line Broadening ◽  
Temperature Range ◽  
Diffraction Line Profile ◽  
Pattern Decomposition ◽  
Nanocrystalline Magnesium Oxide

An analysis of the microstructure of nanocrystalline magnesium oxide produced by thermal decomposition of magnesium oxalate, in the temperature range 500 °C–1200 °C, is described. The study is based on diffraction line broadening analysis carried out with the integral breadth (Langford) and Fourier methods, combined with the pattern decomposition technique. Additionally, the whole pattern matching method is also applied. No marked line broadening anisotropy is observed in the patterns. It is shown that the nanopowders are characterized by minimal strain and that crystallites have an average spherical shape. Volume-weighted and area-weighted apparent sizes are in the ranges 98–480 Å and 72–282 Å, respectively, within the temperature range considered. The results obtained from line broadening analysis are compared to those observed with scanning electron microscopy and surface area measurements. A satisfactory agreement is found between sizes derived from the different techniques.

X-ray diffraction line broadening due to dislocations in non-cubic crystalline materials. III. Experimental results for plastically deformed zirconium

1989 ◽  
Vol 22 (4) ◽  
pp. 299-307 ◽  
Author(s):  
R. Kužel ◽  
P. Klimanek
Keyword(s):  
Profile Analysis ◽  
Theoretical Calculations ◽  
Diffraction Line ◽  
Line Profile Analysis ◽  
Line Broadening ◽  
X Ray Diffraction ◽  
X Ray ◽  
Diffraction Line Profile ◽  
Analytical Functions ◽  
Profile Fitting

Procedures of X-ray diffraction line profile analysis for the evaluation of the dislocation content in plastically deformed hexagonal materials were tested by means of conventional powder diffractometry on polycrystalline zirconium deformed under tension at 77 K. In order to obtain a representative picture of the dislocation-induced X-ray line broadening a series of reflections was measured. The integral breadths and the Fourier coefficients were evaluated by both direct profile-shape analysis and profile fitting with analytical functions. The results show a significant anisotropy of the line broadening. The 0001 reflections are clearly less broadened than most of the others. According to the theoretical calculations presented previously such a phenomenon can be expected if the plastic deformation favours generation of dislocations with Burgers vectors a/3 〈2{\bar 1} {\bar 1}0〉.

Recrystallization of BCC Metals: Distribution of Strain Hardening and Texture Formation

2013 ◽  
Vol 753 ◽  
pp. 534-537 ◽  
Author(s):  
Yuriy Perlovich ◽  
Margarita Isaenkova ◽  
Olga Krymskaya
Keyword(s):  
Volume Fraction ◽  
Profile Analysis ◽  
Residual Deformation ◽  
Line Profile Analysis ◽  
Stored Energy ◽  
Line Broadening ◽  
X Ray ◽  
Bcc Metals ◽  
Pole Figures ◽  
Cold Rolled

Data are presented on the x-ray line broadening distribution over the texture of cold-rolled Nb and Mo sheets. The method of generalized X-ray pole figures, which combine texture measurements with X-ray line profile analysis, is employed. The X-ray line broadening is considered as an indicator of residual deformation effects. It was revealed that these effects in cold-rolled BCC metals rise as the grain orientation shifts away from texture maxima towards texture minima. The intensity of X-ray reflections change during annealing at 200 – 500C and this change correlates with the line broadening. The recrystallization texture of BCC metals is dominated by orientations deflected from the peak maxima by 25 – 30 deg. These orientations in the deformed structure have relatively high stored energy. Their volume fraction is sufficient for them to be able to consume most of the deformed matrix.

A study of nanocrystalline yttrium oxide from diffraction-line-profile analysis: comparison of methods and crystallite growth

2002 ◽  
Vol 17 (4) ◽  
pp. 262-269 ◽  
Author(s):  
D. Louër ◽  
T. Bataille ◽  
T. Roisnel ◽  
J. Rodriguez-Carvajal
Keyword(s):  
Yttrium Oxide ◽  
Profile Analysis ◽  
Line Profile Analysis ◽  
Crystallite Growth ◽  
Line Broadening ◽  
Diffraction Line Profile ◽  
Pattern Decomposition ◽  
Refinement Method ◽  
Two Samples ◽  
On Line

An analysis of the microstructure of nanocrystalline yttrium oxide produced by thermal decomposition of a double oxalate yttrium and ammonium, at temperatures in the range 600 °C to 900 °C, is described. The study is based on line broadening analysis carried out with the (Voigt/Langford) integral breadth and Fourier methods combined with the pattern decomposition technique. Due to the line overlap arising from the density of diffraction lines, the whole pattern refinement method (pattern matching and Rietveld approaches) is also applied. No marked line broadening anisotropy is observed in the patterns. It is shown that for the two samples prepared at the highest temperatures the results are similar whatever the method used and the material can be considered as strain free. For the two lowest temperatures only the whole pattern refinement method is applied. The results suggest that a small amount of lattice microdistortion is present in these two last samples. It is shown that the crystallite growth varies exponentially with temperature. The results obtained from line broadening analysis are compared to those observed with scanning electron microscopy, from which a good accordance is noted between the two techniques.

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