The effect of profile-step counting time on the determination of crystal structure parameters by X-ray Rietveld analysis

1984 ◽  
Vol 17 (5) ◽  
pp. 297-306 ◽  
Author(s):  
R. J. Hill ◽  
I. C. Madsen
Keyword(s):  
Crystal Structure ◽  
Goodness Of Fit ◽  
Structural Parameters ◽  
Rietveld Analysis ◽  
Structure Parameters ◽  
Model Errors ◽  
Diffraction Profile ◽  
X Ray ◽  
Counting Time ◽  
Step Counting

Crystal structure parameters have been obtained for α-Al2O3, β-PbO2 and (Mg, Fe)2SiO4 by Rietveld analysis of Cu Kα X-ray powder diffraction data collected on a conventional diffractometer using counting times ranging from 0.01 to 5 s per step. For all but the 0.01 s data collected on (Mg, Fe)2SiO4 the structural parameters obtained at different counting times are statistically identical at the 3 σ level, and the spread in the values is essentially the same as that obtained by sample repacking at a fixed counting time of 1 s per step. The parameter e.s.d.'s and conventional agreement indices Rwp and RB decrease to values limited by residual model errors as the counting time increases, but the goodness-of-fit parameter becomes unacceptably larger than its ideal value of unity. When more than a few thousand counts are accumulated for the maximum step intensity in the diffraction profile a weighting scheme based solely on counting variance is inappropriate and the parameter e.s.d.'s are no longer a reflection of their accuracy.

Structure of Carbonated Hydroxyapatite Based on Rietveld Method

2008 ◽  
Vol 368-372 ◽  
pp. 1187-1189
Author(s):  
Xu Ran ◽  
Jun Guo Ran ◽  
Li Gou ◽  
Ji Yong Chen ◽  
Jiao Min Luo
Keyword(s):  
Crystal Structure ◽  
Sintering Temperature ◽  
Rietveld Method ◽  
Rietveld Analysis ◽  
Structure Parameters ◽  
X Ray Diffraction ◽  
Carbonated Hydroxyapatite ◽  
X Ray ◽  
Quantitative Results ◽  
Distortion Index

The crystalline structures of B-type carbonated hydroxyapatite (CHA) powders sintered at 700, 900 and 1100°C, respectively, were studied by Rietveld analysis of powder X-ray diffraction (XRD) data. A series of structure parameters, including lattice parameters (a and c), bond length and the distortion index of PO4 tetrahedron (Dind) were calculated by Rietveld method to characterize the fine structure of CHA. The broadening effect of XRD reflections was separated to calculate the micro-strain and crystalline size. The results showed that CHA become more stable with the increase of sintering temperature, but the CO3 2- is almost lost at temperature of 1100°C. The quantitative results about crystal structure of CHA based on crystalline structure simulated by Rietveld method are obtained.

Effect of Iron Substitution on Structure and Optical Properties of Nanocrystalline CaTiO3

2008 ◽  
Vol 3 ◽  
pp. 123-128 ◽  
Author(s):  
A. Bandyopadhyay ◽  
S. Mondal ◽  
M. Pal ◽  
Umapada Pal ◽  
M. Pal
Keyword(s):  
Crystal Structure ◽  
Particle Size ◽  
Iron Concentration ◽  
Rietveld Analysis ◽  
Exothermic Peak ◽  
Optical And Electrical Properties ◽  
X Ray Diffraction ◽  
Chemical Route ◽  
X Ray ◽  
Soft Chemical Route

Nanocrystalline CaTiO3 powders doped with Fe2O3 have been prepared using a soft chemical route. Precipitation of CaTiO3 nanocrystals has been studied by monitoring the exothermic peak in their DSC spectra. The crystal growth temperature of the samples depends on the concentration of iron. Surface morphology, crystal structure, optical and electrical properties of the nanostructures are investigated. X-ray diffraction study shows that the as-prepared powders are amorphous in nature and CaTiO3 phase formation starts at around 500 0C. Rietveld analysis revealed that the particle size of iron substituted CaTiO3 is in nanometer range. Optical bandgap of the nanostructures varies from 4.3 to 3.7 eV for the variation of iron concentration from 0.05 to 0.2 mole %.

Full-Profile Approximation of the X-Ray Diffractogram for Nanographite Powder Including γ-Band by Taking into Account Radial Dependence of Interatomic Distances

2018 ◽  
Vol 386 ◽  
pp. 394-399
Author(s):  
Nikita S. Saenko ◽  
Albert M. Ziatdinov
Keyword(s):  
Structural Parameters ◽  
Radial Dependence ◽  
Angular Range ◽  
X Ray Diffraction ◽  
Interatomic Distances ◽  
Diffraction Profile ◽  
Percentage Content ◽  
X Ray ◽  
Full Profile

This paper outlines the procedure for determining the sizes, structural parameters and percentage content of various particle types in nanographite powders by full-profile approximation of the X-ray diffractogram of sample with using a set of X-ray diffraction profiles for powders of model nanographites. It was shown that taking into account the model nanographites with the radial dependence of interatomic distances within the layer and the dependence of interlayer distances on average number of atoms in the layer allows to describe the X-ray diffraction profile of nanographite powder in the wide angular range including so-called γ-band in small angles without assumptions on presence of other structures in it.

scholarly journals Role of chemical substitution in the photoluminescence properties of cerium samarium tungstates Ce(2-x)Smx (WO4)3 (0≤x≤0.3)

2020 ◽  
Vol 225 ◽  
pp. 01013
Author(s):  
K. Derraji ◽  
C. Favotto ◽  
J-C Valmalette ◽  
S. Villain ◽  
J-R. Gavarri ◽  
...  
Keyword(s):  
Solid Solution ◽  
Rietveld Analysis ◽  
Excitation Energies ◽  
Diffraction Profile ◽  
Vacancy Defects ◽  
X Ray ◽  
Cell Parameters ◽  
Structural Distortions ◽  
Ir Emission

In the general framework of the development of materials with tunable photoluminescence, a series of cerium samarium tungstates Ce(2-x)Smx(WO4)3 with x≤0.3 was synthesized by a coprecipitation method followed by thermal treatment at 1000 °C. The polycrystalline compounds were characterized by X-ray diffraction, scanning electron microscopy and photoluminescence experiments. In the present work, the objective would be to determine the role of PL emitting centers in the variations of PL intensities. Firstly, Rietveld analysis showed a decrease of cell parameters and confirmed that a solid solution was obtained. Diffraction profile analyses showed that structural distortions increasing with composition x were observed: they were ascribed to difference in cation sizes of Ce3+ and Sm3+, and to defects generated during crystal growth. The photoluminescence (PL) spectra were obtained under X-Ray (45 kV-35 mA) and UV (364.5 nm) excitations. Two PL emissions of Ce3+ were observed only under UV excitation. Four PL emissions of Sm3+ were observed under UV and X-ray excitations, and their intensities decreased with increasing composition x. Two additional transitions were observed under UV and X-ray excitations: they were attributed to oxygen vacancy defects. In the range 800 to 1000 nm, an increasing IR emission is observed: it was ascribed to emissions due to other oxygen vacancies. The main results are reported in Table 1. The chromaticity diagram (see Figure 1) showed that the colors associated with PL responses vary with Sm composition and excitation energies. This offers the opportunity to develop materials with tunable PL. To better understand this complex behavior, now, we plan to study the solid solution in the composition range x>0.3.

A semi-empirical asymmetry function for X-ray diffraction peak profiles

1995 ◽  
Vol 10 (3) ◽  
pp. 204-206 ◽  
Author(s):  
P. Riello ◽  
P. Canton ◽  
G. Fagherazzi
Keyword(s):  
Goodness Of Fit ◽  
Rietveld Method ◽  
Rietveld Analysis ◽  
Opening Angle ◽  
X Ray Diffraction ◽  
X Ray ◽  
Asymmetry Function ◽  
The Asymmetry ◽  
Fit Index ◽  
Semi Empirical

A new semi-empirical approximation for the asymmetry function to be used in the X-ray Rietveld analysis has resulted in lower values of the so-called goodness-of-fit index, defined as S = Rwp/Rexp, where Rwp is the R-weighted pattern and Rexp is the R-expected [R. A. Young, The Rietveld Method (Oxford U.P., Oxford, 1993)], with respect to the corresponding values obtained with the classical approximation used by Rietveld in his fundamental paper. A comparing test of the two asymmetry functions was carried out for the cubic Y2O3 and for αAl2O3 using either pseudo-Voigt or Pearson VII symmetrical functions and two diffractometers. As in the case of the Rietveld approximation, the present one, which employs an exponential function, is optimized using only one fitting parameter. Experimentally, the asymmetry can be considerably diminished by using Soller slits with a small opening angle (≤2°).

Structure of TlSr2PrCu207−x by Rietveld analysis

1994 ◽  
Vol 9 (3) ◽  
pp. 194-199
Author(s):  
Hoong-Kun Fun ◽  
Ping Yang ◽  
Rusli Othman ◽  
Tsong-Jen Lee ◽  
Chiou-Chu Lai ◽  
...  
Keyword(s):  
Low Temperature ◽  
Crystalline Structure ◽  
Powder Diffraction ◽  
Room Temperature ◽  
Goodness Of Fit ◽  
Rietveld Analysis ◽  
Crystal Data ◽  
X Ray ◽  
Tetragonal System

The crystalline structure of new TlSr2PrCu207−x was obtained at room temperature (300 K) and low temperature (100 K) from X-ray powder diffraction with CuKα radiation using Rietveld analysis. TlSr2PrCu207−x has an isotypical structure with TlBa2CaCu207 (1212). At 300 K, crystal data: Tl0.864Sr2PrCu2O6.75, Mr=727.811, the tetragonal system, P4/mmm, a =3.85404(5) Å, c = 12.1046(2) Å, V=179.80 Å3, Z=1, Dx =6.7218 g cm−3, μ =1143.922 cm−1 (λ = 1.54051 Å), F(000)=317.0, the structure was refined with 28 parameters to Rwp=5.29%, Rp = 3.65% for 3551 step intensities and Rb=7.40%, Rf=639% for 155 peaks, “goodness of fit” 5=3.05. At 100 K, crystal data: Tl0.858Sr2PrCu2O6.61, Mr=724.345, the tetragonal system, P4/mmm, a =3.84872(6) Å, c = 12.0771(3) Å, V=178.89 Å3, Z=1, Dx=6.7235 g cm−3, μ=1146.939 cm−1 (λ= 1.54051 Å), F(000) = 315.4, the structure was refined with 26 parameters to Rwp=6.70%, Rp=5.11% for 2926 step intensities and Rb=7.83%, Rf=6.70% for 131 peaks, “goodness of fit” S = 1.75.

Crystal Structure Analysis in the Dehydrogenation Process of Mg(NH2)2-LiH System

2006 ◽  
Vol 971 ◽  
Author(s):  
Tatsuo Noritake ◽  
Masakazu Aoki ◽  
Shin-ichi Towata ◽  
Yuko Nakamori ◽  
Shin-ichi Orimo
Keyword(s):  
Crystal Structure ◽  
Rietveld Analysis ◽  
Crystal Structure Analysis ◽  
Diffraction Measurement ◽  
Hydrogen Storage Materials ◽  
X Ray Diffraction ◽  
X Ray ◽  
Structure Changes ◽  
Li Ion ◽  
Cation Sites

ABSTRACTMg(NH2)2-LiH system which have the properties of reversible hydrogenation and dehydrogenation is one of the promising candidates for new hydrogen storage materials. For understanding of the reversible reaction mechanism, we investigated the crystal structure changes in 3Mg(NH2)2-12LiH system using the pressure-composition (p-c) isotherm measurement and synchrotron X-ray diffraction. The sample was prepared by the hydrogenation of Mg3N2 + 4Li3N. At the several dehydrogenation stages of the p-c isotherm measurement at temperature 523 K, the sample was taken out and X-ray diffraction measurement was performed. By the amount of desorbed hydrogen, the reaction was expressed as the following formula, Mg(NH2)2 + 4LiH → LixMg(NH2)2-x(NH)x + (4-x)LiH + xH2 (x = 0∼2). The crystal structures of LixMg(NH2)2-x(NH)x, similar to CaF2-type one, formed during the dehydrogenation reaction were determined by Rietveld analysis. As a result, it is considered that the dehydrogenation process might relate to the diffusion of Li+ ion in cation sites of Mg(NH2)2.

Phase diagram of the Nd2Fe14B–Sm2Fe14B pseudo-binary system

2016 ◽  
Vol 49 (1) ◽  
pp. 64-68 ◽  
Author(s):  
Ch. F. Xu ◽  
K. H. Chen ◽  
Z. F. Gu ◽  
L. Y. Cheng ◽  
D. D. Ma ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Phase Diagram ◽  
Binary System ◽  
Solid Solutions ◽  
Structure Parameters ◽  
Rietveld Refinements ◽  
X Ray ◽  
Full Profile ◽  
Cell Volumes ◽  
Scanning Electron

The phase relations in the (1−x)Nd2Fe14B–xSm2Fe14B system over the whole concentration range have been studied by means of X-ray powder diffraction (XRD), differential thermal analysis (DTA) and scanning electron microscopy with energy-dispersive X-ray spectroscopy. Crystal structure parameters for all studied compositions of (Nd1−xSmx)2Fe14B have been determined by full-profile Rietveld refinements. These results revealed that all intermediate alloys of (Nd1−xSmx)2Fe14B are similar to the end member of the investigated system, Nd2Fe14B, with a tetragonal structure (space groupP42/mnm). The formation of continuous solid solutions has been found in this system. The normalized lattice parameters and unit-cell volumes of (Nd1−xSmx)2Fe14B solid solutions decrease linearly with increasing Sm content. The DTA measurements show that the melting temperature of (Nd1−xSmx)2Fe14B increases linearly with increasing Sm content and no metastable phases were detected. Based on the DTA data and XRD results, a tentative phase diagram for the pseudo-binary system Nd2Fe14B–Sm2Fe14B has been constructed.

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