X-Ray Diffraction Patterns of Crystalline Sol Rubber Prepared from Ethereal Solution

1939 ◽  
Vol 12 (3) ◽  
pp. 482-484
Author(s):  
George L. Clark ◽  
Siegfried T. Gross ◽  
W. Harold Smith

Abstract In a previous publication there was reproduced an x-ray diffraction pattern of crystals obtained from a solution, cooled to temperatures between −40° and −50° C, of an ether-gel fraction of rubber from Hevea brasiliensis. Measurements of three strong interferences indicated that the crystals were similar to those of stretched gel rubber and of frozen sol, gel and total rubber. Although many attempts were made at that time, unsatisfactory diffraction patterns were obtained with crystalline ether-sol rubber. The interferences were faint and not suitable for accurate measurement and analysis. Since the crystalline material is bulky and some specimens are more compact than others, it seemed possible that the average number of cell diameters was too small to permit sharp definition, and that more material was required for the examination by x-rays. However, it is not certain that lack of definition was caused by insufficient crystalline rubber. The possibility that parts of the long-chain molecules become crystalline and that parts remain amorphous is not excluded, and might be its cause. Additional work with crystalline sol rubber, using a slightly different experimental procedure and more material than in earlier experiments, finally resulted in a satisfactory pattern.

Author(s):  
Kannan M. Krishnan

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.


2007 ◽  
Vol 336-338 ◽  
pp. 1868-1871 ◽  
Author(s):  
Cheng Fu Yang ◽  
Chien Min Cheng ◽  
Ho Hua Chung ◽  
Chao Chin Chan

5~15 wt% MgO-CaO-Al2O3-SiO2 (MCAS, fabricated by sol-gel method) glass is used as the sintering aid of AlN ceramics. The sintering is proceeded from 1350oC~1550oC, scanning electron microscope is used to observe the sintered morphologies and X-ray diffraction pattern are used to confirm the crystal structures. From the SEM observations, as 10wt% and 15wt% MCAS is added, AlN ceramics can be densified at 1500oC and 1450oC, which are much lower than the before studies were. From the X-ray diffraction patterns, the crystal phases of MCAS-AlN ceramics are AlN, Al2O3, and cordierite phases. In this study, the dielectric characteristics of MCAS-AlN ceramics are also developed as a function of MCAS content and sintering temperature.


1989 ◽  
Vol 33 ◽  
pp. 389-396 ◽  
Author(s):  
Y. Yoshioka ◽  
T. Shinkai ◽  
S. Ohya

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.


2009 ◽  
Vol 68 ◽  
pp. 69-76 ◽  
Author(s):  
S. Thanikaikarasan ◽  
T. Mahalingam ◽  
K. Sundaram ◽  
Tae Kyu Kim ◽  
Yong Deak Kim ◽  
...  

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.


1994 ◽  
Vol 346 ◽  
Author(s):  
Carol S. Houk ◽  
Gary A. Burgoine ◽  
Catherine J. Page

ABSTRACTWe have investigated the homogeneity of sol‐gel derived YBa2Cu307‐s from the solution phase to the final product using transmission electron microscopy (TEM), x‐ray diffraction (XRD), and Energy Dispersive X‐ray (EDX) lateral mapping techniques. The starting solutions contain stoichiometric amounts of the metal 2‐(2‐methoxyethoxy)ethoxide components in 2‐(2‐methoxyethoxy)ethanol and appear to be homogeneous by TEM with a uniform distribution of particles having an average size of less than 40 â. Through elemental mapping we see elemental segregation in the high temperature (950 °C) products, which are orthorhombic by XRD. In elemental maps of gel samples fired to 700 °C, which are tetragonal by XRD, we also see elemental inhomogeneity within particles and phase zoning in maps of products from finely ground gels. A comparison of elemental maps and x‐ray diffraction patterns of the products from gel processing and conventional solid state processing is made.


1994 ◽  
Vol 9 (8) ◽  
pp. 2133-2137 ◽  
Author(s):  
Hideki Yoshioka

Thin films in the system (1 - x) PbTiO3−xLa2/3TiO3 were prepared by the sol-gel and dip-coating methods. Phases deposited in the films and the lattice parameters as a function of the composition were investigated by the x-ray diffraction method. The solid solutions with a perovskite structure were formed as a single phase with x up to 0.9. For the composition of x = 1.0, metastable La-Ti-O perovskite phase with a small amount of the impurity phase, La2Ti2O7, was obtained. Simulation of x-ray diffraction patterns based on the defect structure model shows that the structure of the La-Ti-O perovskite phase includes randomly distributed cation vacancies at the A-site, namely (La2/3□1/3)TiO3.


1938 ◽  
Vol 11 (4) ◽  
pp. 687-688
Author(s):  
R. Brill ◽  
F. Halle

Abstract As is known, natural rubber has the property of giving, when stretched, an x-ray fiber diagram, whereas in a normal state the same rubber is amorphous. Numerous other natural substances such as hair and tendon, and artificial substances such as polychloroprene, behave in the same way. However, this effect is not confined to purely organic substances, and it is to be found, for example, in the case of so-called amorphous sulfur and polyphosphornitryl chloride (PNCl2)x. All these substances have the property in common with one another of exhibiting a rubber-like elasticity within a definite temperature range, and of being composed of long-chain molecules.


1970 ◽  
Vol 14 ◽  
pp. 139-145
Author(s):  
W. S. Toothacker ◽  
L. E. Preuss

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.


2001 ◽  
Vol 19 (1) ◽  
pp. 125-131 ◽  
Author(s):  
KENICHI KINOSHITA ◽  
HIDEKI HARANO ◽  
KOJI YOSHII ◽  
TAKERU OHKUBO ◽  
ATSUSHI FUKASAWA ◽  
...  

For ultrafast material analyses, we constructed the time-resolved X-ray diffraction system utilizing ultrashort X-rays from laser-produced plasma generated by the 12-TW–50-fs laser at the Nuclear Engineering Research Laboratory. Ultrafast transient changes in laser-irradiated GaAs crystals were observed as X-ray diffraction patterns. Experimental results were compared with numerical analyses.


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