Diffraction amorphous materials

TEM offers two methods of specimen observation, diffraction mode and image mode. In diffraction mode, an electron diffraction pattern is obtained on the fluorescent screen, originating from the sample area illuminated by the electron beam. The diffraction pattern is entirely equivalent to an X-ray diffraction pattern a single crystal will produce a spot pattern on the screen, a polycrystal will produce a powder or ring pattern (assuming the illuminated area includes a sufficient quantity of crystallites), and a glassy or amorphous material will produce a series of diffuse halos. 

X-ray Diffraction (XRD) is a powerful technique used to uniquely identify the crystalline phases present in materials and to measure the structural properties (strain state, grain size, epitaxy, phase composition, preferred orientation, and defect structure) of these phases. XRD is also used to determine the thickness of thin films and multilayers, and atomic arrangements in amorphous materials (including polymers) and at inter ces. 

EXAFS is a nondestructive, element-specific spectroscopic technique with application to all elements from lithium to uranium. It is employed as a direct probe of the atomic environment of an X-ray absorbing element and provides chemical bonding information. Although EXAFS is primarily used to determine the local structure of bulk solids (e.g., crystalline and amorphous materials), solid surfaces, and interfaces, its use is not limited to the solid state. As a structural tool, EXAFS complements the familiar X-ray diffraction technique, which is applicable only to crystalline solids. EXAFS provides an atomic-scale perspective about the X-ray absorbing element in terms of the numbers, types, and interatomic distances of neighboring atoms. 

This mechanism is also confirmed by X-ray diffraction measurements [94, 100]. It is also mentioned that the absence of reflexes belonging to Li3NbC>4, in X-ray diffraction patterns obtained for mixtures treated at relatively low temperatures, could be explained by the formation of an amorphous material at the very beginning of the process [103]. 

One of the most important areas of application of the solid-state NMR technique is the investigation of the structures of cross-linked amorphous materials in cases where X-ray diffraction technqiues are not applicable. Polymeric resins are one such important class of materials. A lot of work has been done in this area by several investigators 36,37 38 since the beginning of the 80. Some solid-state NMR data of phenolic resins are presented in Fig. 10. Comparison with liquid state data for... 

Klug, H. P. Alexander, L. E. "X-Ray Diffraction Procedures for Polycrystalline and Amorphous Materials " Wlley-Interscience, 1974 pp 634-642. 

A final point needs to be made. Theory has indicated that AB cements should be amorphous. However, a degree of crystallization does sometimes occur, its extent varying from cement to cement, and this often misled early workers in the field who used X-ray diffraction as a principal method of study. Although this technique readily identifies crystalline phases, it cannot by its nature detect amorphous material, which may form the bulk of the matrix. Thus, in early work too much emphasis was given to crystalline structures and too little to amorphous ones. As we shall see, the formation of crystalUtes, far from being evidence of cement formation, is often the reverse, complete crystallinity being associated with a non-cementitious product of an acid-base reaction. 

H. P. Klug, L. E. Alexander, X-Ray Diffraction Procedures for Poly crystalline and Amorphous Materials, Wiley, New York, NY, 1974. 

TUD-1 is an amorphous material. Unlike crystalhne stractnres, it has no characteristic x-ray diffraction pattern. Figure 41.1 illustrates the pore diameter of TUD-1 in comparison to some major molecular sieves - ZSM-5, Zeohte Y, and MCM-41. It is important to note that the pore diameter of TUD-1 can be varied from about 40A to 250 A. 

Klug HP, Alexander LE (1974) X-Ray Diffraction Procedures for Polycrystalline and Amorphous Materials. 2nd edn., John Wiley Sons, New York... 

X-ray crystallographic techniques when extended to polymeric solids some interesting features of the internal structure of these substances. It was found that good majority of polymers diffract X-rays like any crystalline substance but many behave like amorphous materials giving very broad and diffuse X-ray diffraction patterns. This is seen in following figure. 

When sodium trimetaphosphate Na3P309 was ground in humid air, the relative volume of the amorphous ingredient (determined from the X-ray diffraction data) and the lattice distortion increased with the duration t of the grinding186. The authors concluded that the variation of Qp was mainly attributable to production of an amorphous material . It is hoped that comparisons similar to those in Motooka s work will be more common in the future. 

The structures of crystalline polymer-salt complexes provide insight into the structure of the more conducting amorphous materials. To date, large single crystals of polymer-salt complexes have not been prepared, but it has been possible to obtain structural information from single crystal X-ray diffraction applied to stretched oriented fibres in the PEO NaI and PEOiNaSCN systems (Chatani and Okamura, 1987 Chatani, Fujii, Takayanagi and Honma, 1990). One of the most detailed studies is of (PEO)3 NaI, Fig. 5.11(a). The sodium ion in this structure is coordinated to both the polymer and to the iodide ion and the polymer is coiled in the form of an extended helix. 

The problem with limited selectivity includes some of the minerals which are problems for XRD illite, muscovite, smectites and mixed-layer clays. Poor crystallinity creates problems with both XRD and FTIR. The IR spectrum of an amorphous material lacks sharp distinguishing features but retains spectral intensity in the regions typical of its composition. The X-ray diffraction pattern shows low intensity relative to well-defined crystalline structures. The major problem for IR is selectivity for XRD it is sensitivity. In an interlaboratory FTIR comparison (7), two laboratories gave similar results for kaolinite, calcite, and illite, but substantially different results for montmorillonite and quartz. 

Klug, H.P. Alexander, L.E. (1974) X-ray diffraction procedures for polycrystalline and amorphous materials. J. Wiley Sons, New York, 966 p. 

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