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.

Dislocation densities and crystallite size distributions in nanocrystalline ball-milled fluorides,MF2(M= Ca, Sr, Ba and Cd), determined by X-ray diffraction line-profile analysis

2005 ◽  
Vol 38 (6) ◽  
pp. 912-926 ◽  
Author(s):  
G. Ribárik ◽  
N. Audebrand ◽  
H. Palancher ◽  
T. Ungár ◽  
D. Louër
Keyword(s):  
Crystallite Size ◽  
Line Profile ◽  
Interference Effect ◽  
Profile Analysis ◽  
Line Profile Analysis ◽  
Size Distributions ◽  
X Ray Diffraction ◽  
X Ray ◽  
Diffraction Line Profile ◽  
Dislocation Densities

The dislocation densities and crystallite size distributions in ball-milled fluorides,MF2(M= Ca, Sr, Ba and Cd), of the fluorite structure type have been determined as a function of milling time by X-ray diffraction line-profile analysis. The treatment has been based on the concept of dislocation contrast to explain strain anisotropy by means of the modified Williamson–Hall and Warren–Averbach approaches and a whole-profile fitting method using physically based functions. In most cases, the measured and calculated patterns are in perfect agreement; however, in some specific cases, the first few measured profiles appear to be narrower than the calculated ones. This discrepancy is interpreted as the result of an interference effect similar to that described by Rafaja, Klemm, Schreiber, Knapp & Kužel [J. Appl. Cryst.(2004),37, 613–620]. By taking into account and correcting for this interference effect, the microstructure of ball-milled fluorides is determined in terms of dislocation structure and size distributions of coherent domains. A weak coalescence of the crystallites is observed at longer milling periods. An incubation period in the evolution of microstrains is in correlation with the homologous temperatures of the fluorides.

Synthesis of TiFe Compound from Ball Milled TiH2 and Fe Powders Mixtures

2014 ◽  
Vol 802 ◽  
pp. 61-65 ◽  
Author(s):  
Railson Bolsoni Falcão ◽  
Edgar Djalma Campos Carneiro Dammann ◽  
Cláudio José da Rocha ◽  
Rodrigo Uchida Ichikawa ◽  
Michelangelo Durazzo ◽  
...  
Keyword(s):  
Profile Analysis ◽  
High Vacuum ◽  
High Energy ◽  
Planetary Mill ◽  
Line Profile Analysis ◽  
X Ray Diffraction ◽  
Sample Number ◽  
Heat Treated ◽  
Crystallite Sizes ◽  
Energy Ball

TiFe compound was produced by high-energy ball milling of TiH2and Fe powders, followed by heating under vacuum. TiH2was used instead of Ti in order to avoid the strong particles adhesion to grinding balls and vial walls. Mixtures of TiH2and Fe powders were dry-milled in a planetary mill for times ranging from 5 to 40 hours. The amount of sample, number and diameter of the balls were kept constant in all experiments. After milling, samples were heated under dynamic high-vacuum for the synthesis reaction. As-milled and heat-treated materials were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and differential thermal analysis (DTA). The mean crystallite sizes and microstrains were determined by XRD line profile analysis using the Warren-Averbach method. As-milled materials presented only Fe and TiH2phases. Nanostructured TiFe compound was formed after heat treatment. TiH2was effective for providing low adherence of the powders during milling.

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〉.

Defect Structures in Neutron Irradiated 6H-SiC Studied by X-Ray Diffraction Line Profile Analysis

2000 ◽  
Vol 640 ◽  
Author(s):  
C. Seitz ◽  
A. Magerl ◽  
R. Hock ◽  
H. Heissenstein ◽  
R. Helbig
Keyword(s):  
Line Profile ◽  
Correlation Length ◽  
Defect Structure ◽  
Profile Analysis ◽  
Line Profile Analysis ◽  
Defect Structures ◽  
X Ray Diffraction ◽  
X Ray ◽  
Annealing Temperatures ◽  
Diffraction Line Profile

ABSTRACTWe have investigated by x-ray diffraction defect structures in 6H-SiC after neutron irradiation with different fluences and followed by different annealing procedures. An interpretation along a model of Klimanek [1, 4–6] shows, that higher fluences lead to a stronger than linear reduction of the correlation length, whereas higher annealing temperatures correlate with a better recovery of the correlation length. In addition defects of 1st kind created by irradiation are reduced by annealing. We find that annealing changes the character of the defects and it accentuates a defect structure already present in the original samples.

X-Ray Diffraction Study of Shock-Modified Tetragonal Phases of SnO2 and MnO2

1992 ◽  
Vol 36 ◽  
pp. 595-601
Author(s):  
P. Newcomer ◽  
B. Morosin ◽  
R. A. Graham
Keyword(s):  
Shock Loading ◽  
Crystal Size ◽  
Lattice Strain ◽  
Profile Analysis ◽  
Line Profile Analysis ◽  
X Ray Diffraction ◽  
Pressure Shock ◽  
X Ray ◽  
Diffraction Line Profile ◽  
Coherent Crystal

AbstractX-ray diffraction line-profile analysis on tetragonal forms of SnO2 (cassiterite), MnO2 (pyrolusite), and previously studied TiO2 (rutile), which were subjected to high pressure shock loading, show that residual lattice strain and coherent “crystal” size are a function of shock parameters. An interesting observation on a sample of MnO2 concerns the recovery of cubic Mn2O3 (bixbyite) in the material subjected to 22 GPa, indicating a shock-induced chemical synthesis.

Planar faults in layered Bi-containing perovskites studied by X-ray diffraction line profile analysis

2001 ◽  
Vol 34 (6) ◽  
pp. 699-703 ◽  
Author(s):  
A. Boulle ◽  
C. Legrand ◽  
R. Guinebretière ◽  
J. P. Mercurio ◽  
A. Dauger
Keyword(s):  
Fourier Analysis ◽  
Profile Analysis ◽  
Layered Perovskite ◽  
Strong Line ◽  
Line Profile Analysis ◽  
X Ray Diffraction ◽  
Diffraction Line Profile ◽  
Profile Fitting ◽  
Fitting Procedures ◽  
Diffraction Patterns

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.

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