Crystallinity diffraction technique

Figure 4.7c illustrates how x-ray diffraction techniques can be applied to the problem of evaluating 6. If the intensity of scattered x-rays is monitored as a function of the angle of diffraction, a result like that shown in Fig. 4.7c is obtained. The sharp peak is associated with the crystalline diffraction, and the broad peak, with the amorphous contribution. If the area A under each of the peaks is measured, then... 

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. 

Solid state NMR is a relatively recent spectroscopic technique that can be used to uniquely identify and quantitate crystalline phases in bulk materials and at surfaces and interfaces. While NMR resembles X-ray diffraction in this capacity, it has the additional advantage of being element-selective and inherently quantitative. Since the signal observed is a direct reflection of the local environment of the element under smdy, NMR can also provide structural insights on a molecularlevel. Thus, information about coordination numbers, local symmetry, and internuclear bond distances is readily available. This feature is particularly usefrd in the structural analysis of highly disordered, amorphous, and compositionally complex systems, where diffraction techniques and other spectroscopies (IR, Raman, EXAFS) often fail. 

As with other diffraction techniques (X-ray and electron), neutron diffraction is a nondestructive technique that can be used to determine the positions of atoms in crystalline materials. Other uses are phase identification and quantitation, residual stress measurements, and average particle-size estimations for crystalline materials. Since neutrons possess a magnetic moment, neutron diffraction is sensitive to the ordering of magnetically active atoms. It differs from many site-specific analyses, such as nuclear magnetic resonance, vibrational, and X-ray absorption spectroscopies, in that neutron diffraction provides detailed structural information averaged over thousands of A. It will be seen that the major differences between neutron diffraction and other diffiaction techniques, namely the extraordinarily... 

Polyester fibers contain crystalline as well as noncrystalline regions. The degree of crystallinity and molecular orientation are important in determining the tensile strength of the fiber (between 18-22 denier) and its shrinkage. The degree of crystallinity and molecular orientation can be determined by X-ray diffraction techniques. ... 

Although the diffraction techniques are unique in providing detailed information on the structural organization at the molecular level in the different crystalline forms, there are other characterization techniques which are sensitive to the chain conformation and in some cases to the chain packing, which can be used advantageously (and in some case more efficiently than diffraction techniques) in the recognition and quantification of the different polymorphs in polymeric materials. 

Since the vibrational spectra of sulfur allotropes are characteristic for their molecular and crystalline structure, vibrational spectroscopy has become a valuable tool in structural studies besides X-ray diffraction techniques. In particular, Raman spectroscopy on sulfur samples at high pressures is much easier to perform than IR spectroscopical studies due to technical demands (e.g., throughput of the IR beam, spectral range in the far-infrared). On the other hand, application of laser radiation for exciting the Raman spectrum may cause photo-induced structural changes. High-pressure phase transitions and structures of elemental sulfur at high pressures were already discussed in [1]. 

AOTF w/c RMs bearing the silver, silver iodide and silver sulfide nanoparticles were depressurized slowly and the nanoparticles in the cell were collected and re-dispersed in ethanol. Finally, the sample grids for the TEM (FEl TECNAl G ) measurements were prepared by placing a drop of ethanolic dispersion of nanoparticles on the copper grid. The morphology and size distribution of the silver, silver iodide, and silver sulfide nanoparticles were determined by TEM at an operation voltage of 200kV. The crystallinity of the silver, silver iodide, and silver sulfide nanoparticles was studied by electron diffraction techniques. 

X-ray, neutron, and electron diffraction techniques are used to determine crystal structures and can thus be used for molecular structure determinations. Because of its high resolution and applicability to small and often weakly diffracting samples, x-ray crystallography and powder diffraction are by far the methods of choice for most structure determinations on crystalline compounds,... 

A major limitation of diffraction techniques has been the need to obtain crystalline samples. If scientists could learn how to crystallize large molecules in a routine manner, a breakthrough would result. In the biological area, this limitation is keenly experienced for membrane-bound proteins, which are important in many biological functions. Scientists are now devising techniques and strategies to crystallize these proteins—if not in three-dimensional, then in two-dimensional lattices. 

Secondly, for some crystalline systems, the structure obtained by diffraction techniques may be incomplete. For example, in some cases the diffraction data may not reveal dynamic aspects of the solid-state structure (as in the case of fluxional organo-metallics) and in others it may not be possible to distinguish clearly between different atoms (as for example 27A1 and 29Si in zeolites) and a combination of the NMR and x-ray data will yield a more complete and meaningful description of the structure. 

In the laboratories of Natta in Milan it was found that the Ziegler catalysts could polymerize (besides ethene) propene, styrene, and several a-olefins to high linear polymers. These polymers appeared crystalline when examined by X-ray diffraction techniques and were able to give oriented fibers. In less than one year since the preparation of the first polymer of propene, Natta was able to communicate, in the meeting of the Accademia dei Lincei of December 1954 in Rome, that a new chapter had been disclosed in the field of macromolecular chemistry, due to the discovery of processes to obtain polymers with an extraordinary regularity in their structure in terms of both chemical constitution and configuration of the successive monomeric units along the chain of each macromolecule. 

The assumption of membrane softness is supported by a theoretical argument of Nelson et al., who showed that a flexible membrane cannot have crystalline order in thermal equilibrium at nonzero temperature, because thermal fluctuations induce dislocations, which destroy this order on long length scales.188 189 The assumption is also supported by two types of experimental evidence for diacetylenic lipid tubules. First, Treanor and Pace found a distinct fluid character in NMR and electron spin resonance experiments on lipid tubules.190 Second, Brandow et al. found that tubule membranes can flow to seal up cuts from an atomic force microscope tip, suggesting that the membrane has no shear modulus on experimental time scales.191 However, conflicting evidence comes from X-ray and electron diffraction experiments on diacetylenic lipid tubules. These experiments found sharp diffraction peaks, which indicate crystalline order in tubule membranes, at least over the length scales probed by the diffraction techniques.123,192 193... 

Bismuth Molybdates. Bismuth molybdates are used as selective oxidation catalysts. Several phases containing Bi and/or Mo may be mixed together to obtain desired catalytic properties. While selected area electron diffraction patterns can identify individual crystalline particles, diffraction techniques usually require considerable time for developing film and analyzing patterns. X-ray emission spectroscopy in the AEM can identify individual phases containing two detectable elements within a few minutes while the operator is at the microscope. 

Nowadays a large number of functional crystals belongs to the TTB family and presents electro-optic, ferro- piezo- pyroelectric properties (e g. the well-known barium sodium niobate Ba2NaNb50i5 (BNN)). In this work iron and manganese based Kx(lvr%(]Vr )i-xF3 fluorides (0.4solid state reaction and characterised by different diffraction techniques in order to investigate their crystalline stmcture. 

Note Crystallinity may be detected by diffraction techniques, heat of measurements, etc. Some amount of disorder within the crystalline region incompatible with this concept. 

X-ray diffraction techniques can be used to establish the structure of crystalline polymers. Measurements are typically made on crystalline lamellar platelets grown from dilute solution, fibres or stretched films. Such methods have been applied to several different inorganic polymers. For example, based on measurements on stretched samples of silicone rubber, poly(dimethylsiloxane) (Me2SiO) has been shown to possess a helical conformation (Figure 8.4). ... 

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