scholarly journals Quantitative analysis of turbostratically disordered nontronite with a supercell model calibrated by the PONKCS method

2012 ◽  
Vol 45 (6) ◽  
pp. 1295-1302 ◽  
Author(s):  
Xiaodong Wang ◽  
Robert D. Hart ◽  
Jian Li ◽  
Robbie G. McDonald ◽  
Arie van Riessen

Two calibration-based quantitative X-ray diffraction (XRD) models for turbostratically disordered Bulong nontronite, the PONKCS (partial or no known crystal structure) approach and the supercell structural model, were compared in terms of the accuracy and refinement error from Rietveld quantitative phase analysis. The PONKCS approach achieved improved nontronite quantitative results with synchrotron diffraction patterns compared with those achieved with laboratory XRD data as a result of better data quality and the use of Debye–Scherrer geometry with significantly reduced preferred orientation effects. The introduction of a peak shape modifier (spherical harmonics) to correct the quantification result is mainly useful for laboratory XRD patterns containing nontronite collected from Bragg–Brentano geometry with appreciable preferred orientation effects. A novel calibration approach for the nontronite supercell model was developed, based on the Rietveld quantitative formula in theTOPASsymbolic computation system. The calibrated supercell model achieved better accuracy (deviation within 1 wt%) and lower refinement error than the PONKCS approach because the physically based description of turbostratic disorder requires fewer refinable parameters than the PONKCS approach. The drawbacks and limitations of the supercell approach are also discussed.

2003 ◽  
Vol 18 (1) ◽  
pp. 7-15 ◽  
Author(s):  
M. Courtial ◽  
M.-N. de Noirfontaine ◽  
F. Dunstetter ◽  
G. Gasecki ◽  
M. Signes-Frehel

So-called alite is a solid solution of tricalcium silicate Ca3SiO5 with a few percent of impurities. It constitutes the major phase of anhydrous Portland cement. In industrial compounds, alite crystallizes into two monoclinic forms designated M1 and M3. The possibility of correlation between the crystallographic structure of the clinker and its reactivity is still an open question. The answer of such a question involves a proper quantitative analysis of the various phases—including the exact alite polymorph—of the industrial product. The rather similar structure of the two alites makes it difficult to distinguish them from their XRD patterns. This paper shows that five angular windows in the X-ray diffraction patterns can be used with synthetic alites as well as industrial compounds, to identify the nature of the actual polymorph (M1 or M3) present and the structural model to be used (with or without superstructure) in subsequent Rietveld analysis of the data.


2000 ◽  
Vol 33 (2) ◽  
pp. 389-391 ◽  
Author(s):  
Toyoko Yamanoi ◽  
Hiromoto Nakazawa

A parallel-beam X-ray diffraction geometry using X-ray guide tubes is proposed to eliminate preferred-orientation effects in powder X-ray diffraction (XRD) patterns and for new applications of XRD. A bundle of X-ray guide tubes (polycapillaries) is used to provide an intense quasi-parallel (approximately 0.2° divergence) and large-diameter (approximately 20 mm) beam of X-rays needed for parallel-beam diffractometry. Mica and silicon particles were agitated inside a cylindrical chamber by a steady flow of N2gas so that they were randomly oriented. The quasi-parallel incident X-ray beam passed through the cloud of floating particles. The diffracted X-rays were detected using a standard 2θ diffractometer. The integrated intensities observed agree well with those calculated from the known model of the crystal structure. This result demonstrates that this type of diffractometry is capable of avoiding preferred-orientation effects and of collecting XRD data for moving powder samples.


1997 ◽  
Vol 29 (1-2) ◽  
pp. 77-87
Author(s):  
M. O. Figueiredo ◽  
F. Margarido

A texture effect in the silicon phase of industrial Fe-Si alloys was noticed in the X-ray diffraction patterns through the reinforcement of the 111 reflection. A similar effect was also apparent in a commercial silicon standard pellet used as reference material and supposed to be texture-free.A quick correction procedure to account for preferred orientation effects was developed, based on a previous algorithm currently applied for the automatic profile fitting of powder diffractometer data. “Modified Wilson plots” are established for visualizing the efficiency of texture correction according to the proposed method.


1998 ◽  
Vol 4 (S2) ◽  
pp. 342-343 ◽  
Author(s):  
S. D. Walck ◽  
P. Ruzakowski-Athey

The analysis of Selected Area Diffraction (SAD) patterns that are collected from a single phase material having sufficient crystallites to provide continuous rings is relatively straightforward. However, when this condition is not met and there may be several phases present having rings of a spotty nature, the pattern is complex and can be quite difficult to analyze manually because of the vast number of discrete spots. WinJade from MDI is an X-ray diffraction (XRD) analysis program with an Electron Diffraction Program Module (EDPM) that can be used to aid in the analysis of SAD patterns. The EDPM produces Integrated Circular Density Plots (ICDP), which are one-dimensional intensity profiles plotted as a function of equivalent XRD 20 values or crystal d-spacings. These ICDP's can be overlayed with XRD patterns or with reference lines from the NIST and JCPDS crystalline databases for direct comparisons.


1999 ◽  
Vol 32 (6) ◽  
pp. 1069-1083 ◽  
Author(s):  
J. A. Elliott ◽  
S. Hanna

A model-independent maximum-entropy method is presented which will produce a structural model from small-angle X-ray diffraction data of disordered systems using no other prior information. In this respect, it differs from conventional maximum-entropy methods which assume the form of scattering entitiesa priori. The method is demonstrated using a number of different simulated diffraction patterns, and applied to real data obtained from perfluorinated ionomer membranes, in particular Nafion™, and a liquid crystalline copolymer of 1,4-oxybenzoate and 2,6-oxynaphthoate (B–N).


1996 ◽  
Vol 11 (4) ◽  
pp. 288-289 ◽  
Author(s):  
H. Hashizume ◽  
S. Shimomura ◽  
H. Yamada ◽  
T. Fujita ◽  
H. Nakazawa ◽  
...  

A system enabling X-ray diffraction patterns under controlled conditions of relative humidity and temperature has been devised and combined with an X-ray powder diffractometer. Relative humidity in the sample space is controlled by mixing dry N2 gas with saturated water vapor. Temperatures of the sample and inner wall of the sample chamber are monitored by two attached thermocouples and the information was fed back to the control unit. Relative humidity between 0% and the 95%, and temperature between room temperature and 60 °C can be controlled. All parameters including those for XRD are programmable and the system runs automatically. The function of the system was checked by recording the XRD patterns of montmorillonite (a clay mineral) and NaCl under increasing and decreasing relative humidity.


2009 ◽  
Vol 73 (5) ◽  
pp. 883-890 ◽  
Author(s):  
I. V. Rozhdestvenskaya ◽  
T. Kogure ◽  
E. Abe ◽  
V. A. Drits

AbstractThe crystal structure of charoite was investigated mainly by using selected-area electron diffraction (SAED), X-ray diffraction (XRD) and high-resolution electron microscopy (HREM). SAED and XRD patterns indicate that the structure has a monoclinic cell: a = 32.296, b = 19.651, c = 7.16 Å, β = 96.3° and V = 4517 Å3. The space group inferred from systematic absences and HREM images is P21/m. A model of the charoite structure is proposed that is based on the features of related Ca-alkaline silicate structures and HREM images. The structure of charoite consists of three different silicon-oxygen radicals (polymerized SiO4 tetrahedra) which are located between Ca polyhedra. Two of these radicals form continuous tubular structures comprising pectolite-like tetrahedral chains. Calcium polyhedra are joined to form blocks, each of which consists of four columns sharing edges and apices. Potassium and H2O molecules are probably located inside the tubular silicate radicals. From these results, a general formula is derived: K6-7(Ca,Na)18[(Si6O17)(Si12O30)(Si18O45)](OH,F)2.nH2O with two formula units in the unit cell (Z = 2).


2008 ◽  
Vol 55-57 ◽  
pp. 841-844 ◽  
Author(s):  
Pasinee Siriprapa ◽  
Anucha Watcharapasorn ◽  
Sukanda Jiansirisomboon

This research studied the effects of sintering temperature and La3+ doping content on phase, microstructure and densification of bismuth lanthanum titanate (Bi4-xLaxTi3O12; BLT) ceramics when x = 0, 0.25, 0.5, 0.75 and 1.0, respectively. The BLT powders were prepared using a mixed-oxide method. The mixtures were calcined at 750°C for 4 h before being pressed and sintered at 1000-1150°C for 4 h. The result of phase analysis by X–ray diffraction (XRD) indicated the existence of orthorhombic phase for all sintering temperatures. The XRD peak intensities of the ceramics showed preferred orientation of a particular set of {00l}-type planes. The ceramics mainly composed of plate-like grains. Increasing the sintering temperature increased grain size and increased preferred grain orientation. The present of La3+ in BLT ceramics reduced preferred orientation especially at higher sintering temperature. Results of microstructural investigation agreed well with X-ray diffraction patterns.


2017 ◽  
Vol 19 (38) ◽  
pp. 26072-26084 ◽  
Author(s):  
Bo-wen Sun ◽  
Hong-yu Yu ◽  
Yong-jing Yang ◽  
Hui-jun Li ◽  
Cheng-yu Zhai ◽  
...  

To date, there have been only a few studies focusing on the assignment of X-ray diffraction (XRD) patterns in graphitic carbon nitrides (g-C3N4) and contradictory determination for a broad peak around 12°–14° has been perplexing.


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