The measurement of orientation distribution and its application to quantitative X-ray diffraction analysis

Clay Minerals ◽  
1966 ◽  
Vol 6 (3) ◽  
pp. 127-142 ◽  
Author(s):  
R.M. Taylor ◽  
K. Norrish

AbstractUsing X-ray techniques, the orientation distributions of crystal planes in laboratory prepared and naturally occurring aggregates were measured. A small specimen was mounted on the axis of a goniometer and the diffracted intensity measured as the specimen was rotated. Mo radiation was used to reduce the absorption effects. A mathematical relation between the distribution of particles and the distribution of crystal planes was derived for platy and fibrous particles in flake-like and rod-shaped specimens.When diffracted intensities of the 001 reflection of several different kaolinites were corrected for the degree of orientation in the respective specimens, a constant value was obtained. This would enable quantitative diffraction analyses to be made without the large errors that can be introduced by orientation effects. The degree of particle orientation achieved appeared to be more dependent on particle morphology than on the method of sample preparation or formation.

2004 ◽  
Vol 19 (11) ◽  
pp. 3414-3422 ◽  
Author(s):  
Jacob L. Jones ◽  
Elliott B. Slamovich ◽  
Keith J. Bowman

Preferred orientation in textured ceramics is often assessed by comparing the relative intensities of x-ray diffraction reflections to those of a randomly oriented ceramic using the Lotgering degree of orientation (f). However, this paper provides evidence that indiscriminate assessments of f can be misleading. Using measured intensities of a modestly textured tape cast bismuth titanate (Na0.5Bi4.5Ti4O15) ceramic, calculated f values vary from 7.4 to 73.2% depending on the reflections included in the calculation. The texture is also quantified by calculating the orientation distribution function (ODF) using measured pole figures. A model is then presented that demonstrates f is nonlinear with the multiple of preferred (00l)-orientations, the standard unit of the 00l pole figure.


Clay Minerals ◽  
1999 ◽  
Vol 34 (1) ◽  
pp. 89-98 ◽  
Author(s):  
N. J. Elton ◽  
L. F. Gate ◽  
J. J. Hooper

AbstractX-ray diffraction (XRD), infra red (IR) spectroscopy, gloss goniophotometry and stylus profilometry were used to investigate the alignment of kaolinite applied as a thin coating on a polyester film substrate. The principles and applicability of the analytical methods are reviewed and discussed in the context of a kaolinite coating. X-ray diffraction and transmission IR were used to measure kaolinite misalignment and orientation distribution in the coating. Transmission IR measures the coating bulk; XRD data are surface biased, but contain contributions from the bulk. Attenuated total reflectance-IR (ATR-IR) provides a direct measure of kaolinite alignment within ~1 µm of the coating surface and also allows an assessment of surface smoothness. Gloss goniophotometry and contact profilometry measure surface microroughness and macroroughness, respectively, rather than kaolinite particle orientation. However, the properties of roughness and orientation are related. Bulk and surface texture are not necessarily correlated and a combined approach using both bulk and surface sensitive techniques is required for a full understanding of coating structure.


2014 ◽  
Vol 70 (a1) ◽  
pp. C726-C726
Author(s):  
Aline Dellicour ◽  
Alain Pautrat ◽  
Bénédicte Vertruyen ◽  
Mark Rikel ◽  
Luca Lutterotti ◽  
...  

Bi2Sr2CaCu2O8+δ HTSC superconductor is characterized by a very strong normal-state resistivity anisotropy, with ρc/ρab typically above 10E4. The aim of this study is to use Quantitative Texture Analysis from x-ray diffraction measurements to estimate the orientation effect on the anisotropic macroscopic resistivity in melt-cast bulk Bi2Sr2CaCu2O8+δ superconductors. Our approach uses the geometric mean [1] of the single crystal resistivity tensor weighted by the Orientation Distribution Function (ODF) to quantitatively estimate the macroscopic resistivity tensor of the samples. The ODF is obtained from x-ray Combined Analysis [2], using the E-WIMV algorithm of the MAUD software. The GMA applies to the rank-two resistivity tensor of the orthorhombic space group considered tetragonal due to the small difference of a- and b-axes of the phase, with only two independent tensor components. We relate a relatively good agreement between measured and calculated macroscopic anisotropic resistivity ratios. Even with ρc/ρab between 10E4 and 10E5 for Bi2212 at room temperature in single crystals [3], we experiment macroscopic ratio in our bulk samples of around only 2. This small ratio is explained by the weak planar- or fiber-like (Figure) texture achieved in the melt-cast samples, characterized by maxima of orientation distributions not larger than 10 mrd. Calculated resistivities, based on homogeneous crystallites, perfect grain boundaries and no secondary phases, are 10 times larger than the observed ones. This suggests that the observed minor phases positively affect conductive pathways between grains. Calculated and measured anisotropic resistive ratios are coherent with one another, and Combined Analysis gives good predictions of these former.


Author(s):  
W. W. Barker ◽  
W. E. Rigsby ◽  
V. J. Hurst ◽  
W. J. Humphreys

Experimental clay mineral-organic molecule complexes long have been known and some of them have been extensively studied by X-ray diffraction methods. The organic molecules are adsorbed onto the surfaces of the clay minerals, or intercalated between the silicate layers. Natural organo-clays also are widely recognized but generally have not been well characterized. Widely used techniques for clay mineral identification involve treatment of the sample with H2 O2 or other oxidant to destroy any associated organics. This generally simplifies and intensifies the XRD pattern of the clay residue, but helps little with the characterization of the original organoclay. Adequate techniques for the direct observation of synthetic and naturally occurring organoclays are yet to be developed.


Processes ◽  
2021 ◽  
Vol 9 (7) ◽  
pp. 1238
Author(s):  
Garven M. Huntley ◽  
Rudy L. Luck ◽  
Michael E. Mullins ◽  
Nick K. Newberry

Four naturally occurring zeolites were examined to verify their assignments as chabazites AZLB-Ca and AZLB-Na (Bowie, Arizona) and clinoptilolites NM-Ca (Winston, New Mexico) and NV-Na (Ash Meadows, Nevada). Based on powder X-ray diffraction, NM-Ca was discovered to be mostly quartz with some clinoptilolite residues. Treatment with concentrated HCl (12.1 M) acid resulted in AZLB-Ca and AZLB-Na, the chabazite-like species, becoming amorphous, as confirmed by powder X-ray diffraction. In contrast, NM-Ca and NV-Na, which are clinoptilolite-like species, withstood boiling in concentrated HCl acid. This treatment removes calcium, magnesium, sodium, potassium, aluminum, and iron atoms or ions from the framework while leaving the silicon framework intact as confirmed via X-ray fluorescence and diffraction. SEM images on calcined and HCl treated NV-Na were obtained. BET surface area analysis confirmed an increase in surface area for the two zeolites after treatment, NM-Ca 20.0(1) to 111(4) m2/g and NV-Na 19.0(4) to 158(7) m2/g. 29Si and 27Al MAS NMR were performed on the natural and treated NV-Na zeolite, and the data for the natural NV-Na zeolite suggested a Si:Al ratio of 4.33 similar to that determined by X-Ray fluorescence of 4.55. Removal of lead ions from solution decreased from the native NM-Ca, 0.27(14), NV-Na, 1.50(17) meq/g compared to the modified zeolites, 30 min HCl treated NM-Ca 0.06(9) and NV-Na, 0.41(23) meq/g, and also decreased upon K+ ion pretreatment in the HCl modified zeolites.


2021 ◽  
Vol 19 (1) ◽  
pp. 745-754
Author(s):  
Khoirina Dwi Nugrahaningtyas ◽  
Eddy Heraldy ◽  
Rachmadani ◽  
Yuniawan Hidayat ◽  
Indriana Kartini

Abstract The properties of three types of CoMo/USY catalysts with different synthesized methods have been studied. The sequential and co-impregnation methods followed by activation using calcination and reduction process have been conducted. The properties of the catalysts were examined using Fourier-transform-infrared (FTIR) spectroscopy, X-ray diffraction (XRD) with refinement, and surface area analyzer (SAA). The FTIR spectrum study revealed the enhanced intensity of its Bronsted acid site, and the XRD diffractogram pattern verified the composition of pure metals, oxides, and alloys in the catalyst. The SAA demonstrated the mesoporous features of the catalyst. Scanning electron microscopy showed an irregular particle morphology. Additional analysis using the transmission electron microscopy indicated that the metal has successfully impregnated without damaging the USY structure.


1964 ◽  
Vol 5 (1) ◽  
pp. 25-29 ◽  
Author(s):  
L.G. Kazaryan ◽  
D.Ya. Tsvankin

1992 ◽  
Vol 45 (12) ◽  
pp. 2089 ◽  
Author(s):  
EL Ghisalberti ◽  
BW Skelton ◽  
AH White

The structure of the compound obtained on heating the naturally occurring clerodane furanoditerpene (1) had been formulated as (2) on the basis of spectroscopic studies. A single-crystal X-ray diffraction study on the dihydro derivative of (2) has confirmed this and provides support for the stereochemistry previously assigned to (1) on the basis of chemical evidence.


2017 ◽  
Vol 898 ◽  
pp. 1431-1437
Author(s):  
Hong Yang Shao ◽  
Kan Zhang ◽  
Yi Dan Zhang ◽  
Mao Wen ◽  
Wei Tao Zheng

The δ-NbN thin films with different thickness have been prepared by reactive magnetron sputtering at different deposition time and exhibited alternating textures between (111) and (200) orientations as a function of thickness. In addition, the grain size, peak position, morphology, residual stress and orientation distributions of the deposited films were explored by X-ray diffraction, low-angel X-ray reflectivity, scanning electron microscopy and surface profiler. The film deposited at 300 s showed a (111) preferred orientation, changing to (200) preferred orientation at 600 s, and exhibited alternating textures between (111) and (200) preferred orientations. With further increasing deposition time, in which (200) peak position and the full width at half maximum of (111) peak also displayed a trend of alternating variation with varying deposition time. The intrinsic stress for δ-NbN films calculated by Stoney equation alternately changed with alternating textures, in which (111) orientation always takes place at relatively high intrinsic stress state and vice versa. Meanwhile, the film with (111) preferred orientation showed higher density than (200) preferred orientation. The film deposited at 4800 s owned a mixed texture of (111) and (200), showing an anisotropy distribution of (111)-oriented and (200)-oriented grains, while film deposited at 7200 s owned a strong (200) texture, displaying an isotropy distribution of (200)-oriented grains. The competitive growth between (111)-oriented and (200)-oriented grains was responsibility for alternating texture.


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