Synthesis of cerium oxide (CeO2) by co-precipitation for application as a reference material for X-ray powder diffraction peak widths

2018 ◽  
Vol 33 (1) ◽  
pp. 21-25 ◽  
Author(s):  
Anderson Márcio de Lima Batista ◽  
Marcus Aurélio Ribeiro Miranda ◽  
Fátima Itana Chaves Custódio Martins ◽  
Cássio Morilla Santos ◽  
José Marcos Sasaki
Keyword(s):  
Powder Diffraction ◽  
Function Analysis ◽  
Diffraction Peak ◽  
Debye Function ◽  
Fourier Decomposition ◽  
Diffraction Peaks ◽  
Diffraction Patterns ◽  
Pattern Modeling ◽  
Co Precipitation ◽  
Peak Widths

Several methods can be used to obtain, from powder diffraction patterns, crystallite size and lattice strain of polycrystalline samples. Some examples are the Scherrer equation, Williamson–Hall plots, Warren/Averbach Fourier decomposition, Whole Powder Pattern Modeling, and Debye function analysis. To apply some of these methods, it is necessary to remove the contribution of the instrument to the widths of the diffraction peaks. Nowadays, one of the main samples used for this purpose is the LaB6 SRM660b commercialized by the National Institute of Standard Technology; the width of the diffraction peak of this sample is caused only by the instrumental apparatus. However, this sample can be expensive for researchers in developing countries. In this work, the authors present a simple route to obtain micron-sized polycrystalline CeO2 that have a full width at half maximum comparable with the SRM660b and therefore it can be used to remove instrumental broadening.

scholarly journals A review of Debye Function Analysis

2013 ◽  
Vol 28 (S2) ◽  
pp. S2-S10 ◽  
Author(s):  
Kenneth R. Beyerlein
Keyword(s):  
Diffraction Pattern ◽  
Powder Diffraction ◽  
Function Analysis ◽  
Reciprocal Space ◽  
Spherical Particles ◽  
Complete Agreement ◽  
Line Profiles ◽  
Debye Function

The employment of the Debye function to model line profiles in the powder diffraction pattern from small crystallites is briefly reviewed. It is also demonstrated that for the case of very small spherical particles, it is necessary to average patterns from multiple constructions of the particle to have complete agreement with reciprocal space models. In doing so it is demonstrated that the technique of Debye function analysis is best suited for systems with only a few possible atomic arrangements.

scholarly journals Testing the Debye Function Approach on a Laboratory X-ray Powder Diffraction Equipment. A Critical Study.

2013 ◽  
Vol 28 (S2) ◽  
pp. S11-S21 ◽  
Author(s):  
Ruggero Frison ◽  
Antonio Cervellino ◽  
Giuseppe Cernuto ◽  
Antonietta Guagliardi ◽  
Norberto Masciocchi
Keyword(s):  
Powder Diffraction ◽  
Diffraction Data ◽  
Function Analysis ◽  
Average Particle Size ◽  
Lattice Parameter ◽  
Critical Study ◽  
Average Particle ◽  
Debye Function ◽  
Laboratory Equipment ◽  
Nanosized Materials

Total Scattering Methods are nowadays widely used for the characterization of defective and nanosized materials. They commonly rely on highly accurate neutron and synchrotron diffraction data collected at dedicated beamlines. Here, we compare the results obtained on conventional laboratory equipment and synchrotron radiation when adopting the Debye Function Analysis method on a simple nanocrystalline material (a synthetic iron oxide with average particle size near to 10 nm). Such comparison, which includes the cubic lattice parameter, the sample stoichiometry and the microstructural (size-distribution) analyses, highlights the limitations, but also some strengthening points, of dealing with conventional powder diffraction data collections on nanocrystalline materials.

Two computer programs for the automatic analysis of powder diffraction patterns

1995 ◽  
Vol 28 (5) ◽  
pp. 646-649 ◽  
Author(s):  
S. M. Clark
Keyword(s):  
Phase Transition ◽  
Ammonium Chloride ◽  
Powder Diffraction ◽  
Kinetic Studies ◽  
Tricalcium Silicate ◽  
Automatic Analysis ◽  
Powder Pattern ◽  
Large Numbers ◽  
Diffraction Peaks ◽  
Diffraction Patterns

Two programs for the automatic analysis of large numbers of powder diffraction patterns have been developed. The first, PEAKFIT, fits functions describing the diffraction peaks and baseline to single or multiple peaks in a number of predefined regions of each powder pattern. The second, FULFIT, fits the entire powder pattern with a combination of functions describing the diffraction peaks and background. The use of these programs is illustrated with data analysed as part of kinetic studies of the I–II phase transition in ammonium chloride and the hydration of tricalcium silicate.

Powder diffraction line profiles from the size and shape of nanocrystallites

2011 ◽  
Vol 44 (5) ◽  
pp. 945-953 ◽  
Author(s):  
K. R. Beyerlein ◽  
R. L. Snyder ◽  
P. Scardi
Keyword(s):  
Powder Diffraction ◽  
Numerical Procedure ◽  
Tangent Plane ◽  
Diffraction Peak ◽  
Line Profiles ◽  
Integration Technique ◽  
Debye Function ◽  
Size And Shape ◽  
Crystallite Sizes ◽  
Good Agreement

A numerical procedure to carry out the integral on the powder diffraction sphere in reciprocal space and obtain accurate powder diffraction peak profiles for small crystallites is presented. In doing so, the literature surrounding the effect of crystallite size and shape on the powder peak profile is briefly reviewed. Powder patterns simulated by this technique are compared with those calculated by the tangent plane approximation and Debye function for spherical, cubic and cylindrical crystallites having sizes of only a few nanometres. The tangent plane approximation is found to produce inaccurate peak profiles and peak positions in simulated patterns of the cubic and cylindrical nanocrystallites. This performance is in contrast to that of the proposed powder integration technique, which results in powder patterns that are in good agreement with those from the Debye function, for all crystallite sizes and shapes considered here.

Method of Simulation of Diffraction Pattern for Nanosize Crystalline Systems

2008 ◽  
Vol 3 (4) ◽  
pp. 47-51
Author(s):  
Dmitriy A. Yatsenko ◽  
Sergey V. Tsybulya
Keyword(s):  
Diffraction Pattern ◽  
Powder Diffraction ◽  
X Ray ◽  
Original Algorithm ◽  
Diffraction Peaks ◽  
Diffraction Patterns ◽  
Definition Of ◽  
Integrated Intensities

The original algorithm and the software for calculation of x-ray powder diffraction patterns from ensemble of nanocrystal particles are developed. Test calculations are carried out. Errors in definition of positions, integrated intensities and halfwidth of diffraction peaks are estimated.

Real-space calculation of powder diffraction patterns on graphics processing units

2010 ◽  
Vol 43 (3) ◽  
pp. 647-653 ◽  
Author(s):  
Luca Gelisio ◽  
Cristy Leonor Azanza Ricardo ◽  
Matteo Leoni ◽  
Paolo Scardi
Keyword(s):  
Powder Diffraction ◽  
Graphics Processing Units ◽  
Real Space ◽  
Parallel Structure ◽  
Debye Function ◽  
Representative Case ◽  
The Core ◽  
Computation Algorithm ◽  
Diffraction Patterns ◽  
Graphics Processing

A new software for calculating the powder diffraction pattern of nano-sized objects has been developed to run on graphics processing units (GPUs). This solution is well suited to the inherently parallel structure of the Debye function, which is the core of the computation algorithm. Advantages and perspectives in view of the improving performance of GPUs are illustrated by several representative case studies.

Analysis of X-Ray Powder Diffraction Patterns of Perovskite-Like PrNiO3

1991 ◽  
Vol 6 (1) ◽  
pp. 36-39
Author(s):  
T. C. Huang ◽  
W. Parrish ◽  
J. B. Torrance ◽  
P. Lacorre
Keyword(s):  
Solid State ◽  
Powder Diffraction ◽  
Solid State Reaction ◽  
Room Temperature ◽  
Rhombohedral Phase ◽  
Diffraction Peak ◽  
Line Broadening ◽  
X Ray ◽  
Figures Of Merit ◽  
Diffraction Patterns

AbstractX-ray powder diffraction patterns of orthorhombic- and rhombohedral-distorted perovskite PrNiO3 obtained at room temperature, 200°, 400°, 500°, and 600°C were analyzed and evaluated. An examination of the diffraction profiles shows essentially no line broadening indicating that the PrNiO3 powders synthesized by solid state reaction are well-crystallized and probably strain-free. The reliability and accuracy of the patterns were evaluated, and the figures-of-merit were in triple digits for the 500° and 600°C patterns of the rhombohedral phase and double digits for the more complex orthorhombic diffraction patterns recorded at room-temperature, 200°, and 400°C. Values of lattice parameters refined from the observed diffraction peak positions agree with those obtained from the Rietveld whole-pattern fitting analysis to within 1–2 × 10−4.

Control of the phase composition of advanced calcium phosphates using an x-ray diffractometer with a curved position-sensitive detector

2020 ◽  
Vol 86 (6) ◽  
pp. 29-35
Author(s):  
V. P. Sirotinkin ◽  
O. V. Baranov ◽  
A. Yu. Fedotov ◽  
S. M. Barinov
Keyword(s):  
Phase Composition ◽  
Calcium Phosphates ◽  
Position Sensitive Detector ◽  
Sensitive Detector ◽  
X Ray Diffraction ◽  
X Ray ◽  
Impurity Phases ◽  
Position Sensitive ◽  
Diffraction Peaks ◽  
Diffraction Patterns

The results of studying the phase composition of advanced calcium phosphates Ca10(PO4)6(OH)2, β-Ca3(PO4)2, α-Ca3(PO4)2, CaHPO4 · 2H2O, Ca8(HPO4)2(PO4)4 · 5H2O using an x-ray diffractometer with a curved position-sensitive detector are presented. Optimal experimental conditions (angular positions of the x-ray tube and detector, size of the slits, exposure time) were determined with allowance for possible formation of the impurity phases during synthesis. The construction features of diffractometers with a position-sensitive detector affecting the profile characteristics of x-ray diffraction peaks are considered. The composition for calibration of the diffractometer (a mixture of sodium acetate and yttrium oxide) was determined. Theoretical x-ray diffraction patterns for corresponding calcium phosphates are constructed on the basis of the literature data. These x-ray diffraction patterns were used to determine the phase composition of the advanced calcium phosphates. The features of advanced calcium phosphates, which should be taken into account during the phase analysis, are indicated. The powder of high-temperature form of tricalcium phosphate strongly adsorbs water from the environment. A strong texture is observed on the x-ray diffraction spectra of dicalcium phosphate dihydrate. A rather specific x-ray diffraction pattern of octacalcium phosphate pentahydrate revealed the only one strong peak at small angles. In all cases, significant deviations are observed for the recorded angular positions and relative intensity of the diffraction peaks. The results of the study of experimentally obtained mixtures of calcium phosphate are presented. It is shown that the graphic comparison of experimental x-ray diffraction spectra and pre-recorded spectra of the reference calcium phosphates and possible impurity phases is the most effective method. In this case, there is no need for calibration. When using this method, the total time for analysis of one sample is no more than 10 min.

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