Impurities diffraction

FIGURE 9.6 X-ray diffractograms of DND (a) and CVD diamond film on silicon substrate (b) and diamond particles produced from HPHT diamond by milling method (c). Positions for interplanar distances are marked. The corresponding intensities are given by the lengths of the dashed lines. Positions of diffraction maxima are marked by corresponding Miller indexes. The asterisk identifies an impurity diffraction maximum. The (b, c) curves are received with CoK and CuK radiation. 

Figure 1 shows the decomposition sequence for several hydrous precursors and indicates approximate temperatures at which the activated forms occur (1). As activation temperature is increased, the crystal stmctures become more ordered as can be seen by the x-ray diffraction patterns of Figure 2 (2). The similarity of these patterns combined with subtie effects of precursor crystal size, trace impurities, and details of sample preparation have led to some confusion in the Hterature (3). The crystal stmctures of the activated aluminas have, however, been well-documented by x-ray diffraction (4) and by nmr techniques (5).

The last twenty years have seen a rapid development of surface physics. In particular, the properties of clean perfect surfaces (with two-dimensional periodicity) are henceforth well known and understood. In recent years, the focus has been put onto surfaces with defects (adatoms, steps, vacancies, impurities...) which can now be investigated experimentally due either to the progress of old techniques (field ion microscopy or He diffraction, for instance) or to the rapid development of new methods (STM, AFM, SEXAFS...). 

Fig. 6 a-c. X-ray diffraction spectra (CuKa) of unoriented samples of a) a form b) y form c) p form containing only minor a form impurities [41]... 

MS2 NiSAl-91 < X < 2.1) Nii j,CUySi.93 (0.03 < y < 0.1) Investigation of structural, electronic, and magnetic properties by means of X-ray diffraction, densitometry, resistivity, susceptibility, and Ni Mossbauer spectroscopy as function of x temperature of phase transition from semimetalhc to metallic state as function of x different Ni sites with different (l/f l) and different angle between H and EFG axis effect of Cu impurities... 

Zeolite structures sometimes remain unsolved for a long time, because of either their complexity, the minute size of the crystallites or the presence of defects or impurities. One extreme example of stacking disorder is provided by zeolite beta [1,2], Different stacking sequences give rise to two polymorphs (A and B) in zeolite beta that always coexist in very small domains in the same crystal. Not only do the small domains make the peaks in the powder X-ray diffraction pattern broad and thereby exacerbate the reflection overlap problem, but the presence of stacking faults also gives rise to other features in the diffraction pattern that further complicate structure solution. 

We have observed large variations in the sorption capacities of zeolite samples characterized by (ID) channel systems, as for instance AFI (AIPO4-5 zeolite) and MTW (ZSM-12 zeolite) architectural framework types. Indeed, for such unconnected micropore networks, point defects or chemisorbed impurities can annihilate a huge number of sorption sites. Detailed analysis, by neutron diffraction of the structural properties of the sorbed phase / host zeolite system, has pointed out clear evidence of closed porosity existence. Percentage of such an enclosed porosity has been determined. 

Besides the inelastic component, always a certain number of He atoms are elastically scattered in directions lying between the coherent diffraction peaks. We will refer to this scattering as diffuse elastic scattering. This diffuse intensity is attributed to scattering from defects and impurities. Accordingly, it provides information on the degree and nature of surface disorder. It can be used for example to study the growth of thin films or to deduce information on the size, nature and orientation of surface defects Very recently from the analysis of the diffuse elastic peak width, information on the diffusive motion of surface atoms has been obtained. ... 

The vapor sample under investigation may not eontain only one kind of speeies. It is desirable to learn as mueh as possible about the vapor composition from independent sources, but here the different experimental conditions need to be taken into account. For this reason, the vapor composition is yet another unknown to be determined in the electron diffraction analysis. Impurities may hinder the analysis in varying degrees depending on their own ability to scatter electrons and on the distribution of their own intemuclear distances. In case of a conformational equilibrium of, say, two conformers of the same molecule may make the analysis more difficult but the results more rewarding at the same time. The analysis of ethane-1,2-dithiol data collected at the temperature of 343 kelvin revealed the presence of 62% of the anti form and 38% of the gauche form as far as the S-C-C-S framework was concerned. The radial distributions calculated for a set of models and the experimental distribution in Figure 6 serve as illustration. 

The data base of some 27,000 powder diffraction patterns that is used in the CIS (5) is in fact a direct descendant of that with which Hanawalt carried out his pioneering work. A problem that arises in connection with this particular component stems from the fact that powders, as opposed to crystals, are frequently impure and so the patterns that are obtained experimentally are often combinations of one or more file entries. A reverse searching program, that examines the experimental data to see if each entry from the file is contained in it, has been written after the general approach of Abramson (23), and seems to cope with this particular difficulty. It is currently running in test on the NIH PDP-10 and will be made available to the scientific community during the latter part of 1978. 

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