Developments in Analytical Diffraction Using Isotopic X-Ray Sources

1970 ◽  
Vol 14 ◽  
pp. 139-145
Author(s):  
W. S. Toothacker ◽  
L. E. Preuss
Keyword(s):  
Exposure Time ◽  
Specific Activity ◽  
X Rays ◽  
X Ray Diffraction ◽  
Glass Capillary ◽  
X Ray ◽  
Oak Ridge ◽  
Position Sensitive ◽  
Diffraction Patterns ◽  
Intense Source

AbstractLobov et al., in Leningrad, and workers at this laboratory have been working on the idea of using x rays from radioactive sources for x ray diffraction analysis. The Russians have been using iron-55 produced by the (n, Y) reaction in their work with a small focusing camera which operates in the back reflection region. We have been using iron-55 produced by the (p,n) reaction in conjunction with a small Debye-Scherrer camera. The preliminary work of this laboratory was reported at this conference two years ago. At that time a 13 mCi iron-55 source was used in a two inch diameter Debye-Scherrer camera to obtain x-ray diffraction patterns of LiF. The exposure times were of the order of 120 hours and the reflection from the 200 plane was about 3 degrees wide. Since that time a new and more intense source has been constructed at Oak Ridge National Laboratories. With the new source it was possible to produce LiF diffraction patterns of the same density and resolution as before in a period of less than ten hours.The above mentioned diffraction patterns were made with the LiF powder placed in a 1.0 mm diameter glass capillary. After reduction of the glass capillary diameter to 0.5 mm and appropriate reduction of the collimator width, we were able to improve the resolution considerably with no accompanying reduction in line density. The LiF patterns obtained in this way required an exposure time of about 20 hours and the width of the reflection from the 200 plane has been reduced to about 1.5 degrees.Hence we are able to report a reduction in exposure time from 116 hours to 20 hours and an increase in resolution by a factor of two over the data reported here two years ago. Thus the concept of using x rays from an isotope for powder diffraction has changed from a laboratory curiosity into a technique with practical possibilities. Both sources mentioned above were produced by the (p, n) reaction. The 135 mCi source had a specific activity of about 400 Ci/gm. Since iron-55 sources have been made with specific activities of about 1000 Ci/gm, a considerable decrease in exposure time could be accomplished by using such a source. The application to this work of a position sensitive proportional counter as developed by Semmler will also be discussed.

The Use of 2-D Detector Utilizing Laser-Stimulated Luminescence for X-ray Diffraction Studies on Mechanical Behaviour of Materials

1989 ◽  
Vol 33 ◽  
pp. 389-396 ◽  
Author(s):  
Y. Yoshioka ◽  
T. Shinkai ◽  
S. Ohya
Keyword(s):  
Fracture Analysis ◽  
X Rays ◽  
Large Reduction ◽  
X Ray Diffraction ◽  
Crystalline Materials ◽  
X Ray ◽  
Material Evaluation ◽  
Position Sensitive ◽  
Diffraction Patterns ◽  
Position Sensitive Detectors

The development of linear position-sensitive detectors (PSD) has resulted in a large reduction of data acquisition times in the field of x-ray stress analysis. However, we also require two-dimensional (2-D) diffraction patterns for material evaluation. Especially, the microbeam x-ray diffraction technique gives valuable information on the structure of crystalline materials and this technique has been applied to fracture analysis by x-rays. Many kinds of 2-D PSD have been developed that have insufficient spatial resolution. So x-ray film has still been used as a 2-D detector, but it requires relatively long exposure times and then the process after exposure is very troublesome.

Evaluation of Freezing Methods by Low Temperature X-Ray Diffraction

1977 ◽  
Vol 35 ◽  
pp. 330-333
Author(s):  
T. Gulik-Krzywicki ◽  
M.J. Costello
Keyword(s):  
Biological Materials ◽  
Molecular Organization ◽  
X Ray Diffraction ◽  
Glass Capillary ◽  
X Ray ◽  
Rate Dependent ◽  
Before And After ◽  
Freeze Etching ◽  
Diffraction Patterns ◽  
Set Up

Freeze-etching electron microscopy is currently one of the best methods for studying molecular organization of biological materials. Its application, however, is still limited by our imprecise knowledge about the perturbations of the original organization which may occur during quenching and fracturing of the samples and during the replication of fractured surfaces. Although it is well known that the preservation of the molecular organization of biological materials is critically dependent on the rate of freezing of the samples, little information is presently available concerning the nature and the extent of freezing-rate dependent perturbations of the original organizations. In order to obtain this information, we have developed a method based on the comparison of x-ray diffraction patterns of samples before and after freezing, prior to fracturing and replication.Our experimental set-up is shown in Fig. 1. The sample to be quenched is placed on its holder which is then mounted on a small metal holder (O) fixed on a glass capillary (p), whose position is controlled by a micromanipulator.

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.

Micro Diffraction Imaging of Bulk Polycrystalline Materials

2006 ◽  
Vol 524-525 ◽  
pp. 273-278
Author(s):  
Thomas Wroblewski ◽  
A. Bjeoumikhov ◽  
Bernd Hasse
Keyword(s):  
High Spatial Resolution ◽  
Polycrystalline Materials ◽  
X Rays ◽  
X Ray Diffraction ◽  
Short Sample ◽  
X Ray ◽  
Detector Distance ◽  
Transmission Geometry ◽  
Diffraction Imaging ◽  
Position Sensitive

X-ray diffraction imaging applies an array of parallel capillaries in front of a position sensitive detector. Conventional micro channel plates of a few millimetre thickness have successfully been used as collimator arrays but require short sample to detector distances to achieve high spatial resolution. Furthermore, their limited absorption restricts their applications to low energy X-rays of around 10 keV. Progress in the fabrication of long polycapillaries allows an increase in the sample to detector distance without decreasing resolution and the use of high X-ray energies enables bulk investigations in transmission geometry.

X-Ray Diffraction

2021 ◽  
pp. 408-480
Author(s):  
Kannan M. Krishnan
Keyword(s):  
Point Group ◽  
Polycrystalline Materials ◽  
X Rays ◽  
X Ray Diffraction ◽  
Symmetry Point Group ◽  
X Ray ◽  
Atomic Scattering ◽  
Scattering Factor ◽  
Diffraction Patterns ◽  
Lattice Planes

X-rays diffraction is fundamental to understanding the structure and crystallography of biological, geological, or technological materials. X-rays scatter predominantly by the electrons in solids, and have an elastic (coherent, Thompson) and an inelastic (incoherent, Compton) component. The atomic scattering factor is largest (= Z) for forward scattering, and decreases with increasing scattering angle and decreasing wavelength. The amplitude of the diffracted wave is the structure factor, F hkl, and its square gives the intensity. In practice, intensities are modified by temperature (Debye-Waller), absorption, Lorentz-polarization, and the multiplicity of the lattice planes involved in diffraction. Diffraction patterns reflect the symmetry (point group) of the crystal; however, they are centrosymmetric (Friedel law) even if the crystal is not. Systematic absences of reflections in diffraction result from glide planes and screw axes. In polycrystalline materials, the diffracted beam is affected by the lattice strain or grain size (Scherrer equation). Diffraction conditions (Bragg Law) for a given lattice spacing can be satisfied by varying θ or λ — for study of single crystals θ is fixed and λ is varied (Laue), or λ is fixed and θ varied to study powders (Debye-Scherrer), polycrystalline materials (diffractometry), and thin films (reflectivity). X-ray diffraction is widely applied.

Correction of X-ray Diffraction Profiles Measured by PSPC System

1989 ◽  
Vol 33 ◽  
pp. 397-402 ◽  
Author(s):  
Shin'ichi Ohya ◽  
Yasuo Yoshioka
Keyword(s):  
Profile Analysis ◽  
X Rays ◽  
X Ray Diffraction ◽  
Diffraction Profile ◽  
X Ray ◽  
Geometrical Problem ◽  
Straight Line ◽  
Background Line ◽  
Diffraction Angle ◽  
Position Sensitive

When an x-ray diffraction profile Is measured for stress analysis or profile analysis by the use of a linear (straight line) position sensitive proportional counter (PSPC) , a convex-type background line is obtained because of the geometrical problem and the absorption of x-rays. Such phenomenon is remarkable when a wide angular range is set on a linear PSPC and it is, in particular, necessary to correct with a straight background for accurate measurement of diffraction angle or half-value breadth of the broadened diffraction profile.

Electrochemical Deposition and Characterization of Cd-Fe-Se Thin Films

2009 ◽  
Vol 68 ◽  
pp. 69-76 ◽  
Author(s):  
S. Thanikaikarasan ◽  
T. Mahalingam ◽  
K. Sundaram ◽  
Tae Kyu Kim ◽  
Yong Deak Kim ◽  
...  
Keyword(s):  
Thin Films ◽  
Hexagonal Structure ◽  
X Rays ◽  
X Ray Diffraction ◽  
X Ray ◽  
Iron Selenide ◽  
Glass Substrates ◽  
Diffraction Patterns ◽  
Cadmium Iron Selenide ◽  
Deposited Films

Cadmium iron selenide (Cd-Fe-Se) thin films were deposited onto tin oxide (SnO2) coated conducting glass substrates from an aqueous electrolytic bath containing CdSO4, FeSO4 and SeO2 by potentiostatic electrodeposition. The deposition potentials of Cadmium (Cd), Iron (Fe), Selenium (Se) and Cadmium-Iron-Selenide (Cd-Fe-Se) were determined from linear cathodic polarization curves. The deposited films were characterized by x-ray diffraction (XRD), scanning electron microscope (SEM), energy dispersive analysis by x-rays (EDX) and optical absorption techniques, respectively. X-ray diffraction patterns shows that the deposited films are found to be hexagonal structure with preferential orientation along (100) plane. The effect of FeSO4 concentration on structural, morphological, compositional and optical properties of the films are studied and discussed in detail.

Image intersification applied to biological problems

1972 ◽  
Vol 5 (3) ◽  
pp. 295-347 ◽  
Author(s):  
George T. Reynolds
Keyword(s):  
Specific Activity ◽  
Biological Research ◽  
Biological Processes ◽  
X Rays ◽  
Radioactive Tracers ◽  
X Ray Diffraction ◽  
Time Intervals ◽  
X Ray ◽  
Rapid Sequence ◽  
Short Time

In many important types of observations in biological research, the information provided by the specimens is in the form of photons-quanta of visible light, u.v., or X-rays. The process of observation becomes one of recording this information in useful form, with as high an efficiency as possible. The problem becomes particularly important when for some reason or other the total number or rate of quanta provided by the specimen is small. Examples of such limitations are included in the following: (i) Processes permitting only low-intensity illumination in order not to interfere with the biological processes under observation. (ii) Processes changing very rapidly and requiring rapid sequence recording. (iii) Processes providing only a limited number of photons per event, such as bioluminescence. (iv) Processes in which radioactive tracers are utilized, and observation of radioactivity is desirable at low specific activity or within short time intervals. (v) X-ray diffraction processes where the specimen is weakly diffracting or where the X-ray intensity must be kept low in order not to damage the specimen. (vi) Processes involving the observation of fluorescence, where the intensity is low because of limitations on the amount of tagging material.

scholarly journals Reciprocal Space Mapping of Epitaxial Materials Using Position-Sensitive X-ray Detection

1994 ◽  
Vol 38 ◽  
pp. 201-213 ◽  
Author(s):  
S. R. Lee ◽  
B. L. Doyle ◽  
T. J. Drummond ◽  
J. W. Medernach ◽  
P. Schneider
Keyword(s):  
Space Mapping ◽  
Reciprocal Space ◽  
X Rays ◽  
X Ray Diffraction ◽  
Reciprocal Space Mapping ◽  
Rocking Curve ◽  
X Ray ◽  
Position Sensitive ◽  
Average Size ◽  
Short Time

Abstract Reciprocal space mapping can be efficiently carried out using a position-sensitive x-ray detector (PSD) coupled to a traditional double-axis diffractometer. The PSD offers parallel measurement of the total scattering angle of all diffracted x-rays during a single rocking-curve scan. As a result, a two-dimensional reciprocal space map can be made in a very short time similar to that of a one-dimensional rocking-curve scan. Fast, efficient reciprocal space mapping offers numerous routine advantages to the x-ray diffraction analyst. Some of these advantages arc the explicit differentiation of lattice strain from crystal orientation effects in strain-relaxed heteroepitaxial layers; the nondestructive characterization of the size, shape and orientation of nanocrystalline domains in ordered-alloy epilayers; and the ability to measure the average size and shape of voids in porous epilayers. Here, the PSD-based diffractometer is described, and specific examples clearly illustrating the advantages of complete reciprocal space analysis are presented.

scholarly journals X-Ray Diffraction from Magnetically Oriented Microcrystal Suspension

2014 ◽  
Vol 70 (a1) ◽  
pp. C1136-C1136
Author(s):  
Kazuaki Aburaya ◽  
Chiaki Tsuboi ◽  
Fumiko Kimura ◽  
Kenji Matsumoto ◽  
Masataka Maeyama ◽  
...  
Keyword(s):  
Single Crystal ◽  
Magnetic Circuit ◽  
X Ray Diffraction ◽  
Glass Capillary ◽  
Uv Curable ◽  
X Ray ◽  
Novel Method ◽  
Diffraction Patterns ◽  
Magnetic Field Generator

A three dimensionally magnetically oriented microcrystal array (3D-MOMA) is attractive to determination of a crystal structure as well as a molecular structure because it does not require a single crystal with sufficient size and quality for diffraction studies. We have developed a novel method to fabricate 3D-MOMA and determined several crystal structures using the 3D-MOMAs[1],[2]. However, the structure determination through MOMA requires a solidification treatment with UV curable monomer prior to X-ray diffraction experiment. We have developed a new X-ray diffractometer equipped with a magnetic field generator, which makes it possible to collect diffraction data without the solidification treatment. In this poster, we describe X-ray diffraction analyses of a magnetically oriented microcrystal suspension (MOMS) of L-alanine without the solidification treatment. A suspension of L-alanine microcrystals was poured in a glass capillary and rotated at a constant speed in a magnetic circuit attached in the X-ray diffractometer. Then, diffraction images were collected every 60 seconds. In the initial phase, the diffraction pattern showed a broad shape similar to that from a powder sample. As time goes on, diffraction patterns have gradually changed to single-crystal like patterns. After 2 hours, the shape of diffraction spots became as sharp as that of a single crystal. This observation shows that the microcrystals are oriented in the same direction. Owing to the improvement of the magnetic circuit and X-ray diffractometer, the quality of the diffraction has been greatly improved compared to that reported previously[3]. Further details of the analyses will be shown in the poster.

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