Diffraction patterns catalysts

Zeolites and Catalytic Cracking. The best-understood metal oxide catalysts are zeoHtes, ie, crystalline aluminosihcates (77—79). The zeoHtes are well understood because they have much more nearly uniform compositions and stmctures than amorphous metal oxides such as siUca and alumina. Here the usage of amorphous refers to results of x-ray diffraction experiments the crystaUites of a metal oxide such as y-Al202 that constitute the microparticles are usually so small that sharp x-ray diffraction patterns are not measured consequendy the soHds are said to be x-ray amorphous or simply amorphous. 

Figure 1 is a TEM photograph of the Cu (10wt%)/Al2O3 catalyst prepared by water-alcohol method, showing the dispersed state of copper and was confirmed the particle sizes from XRD data. Figure 2 is X-ray diffraction patterns of above-mention catalysts, was used to obtain information about phases and the particle size of prepared catalysts. Metal oxide is the active species in this reaction. Particle sizes were determined fix)m the width of the XRD peaks by the Debye-Scherrer equation. 

Table 1 shows that the physicochemical properties of the support material were modified by the pre-treatment process. The particle sizes. Dp, which are summarized in the Table 1 were calculated from the X-ray diffraction patterns of prepared catalysts and a commercial catalyst(30 wt% Pt-Ru/C E-TEK) by using Scherrer s equation. To avoid the interference from other peaks, (220) peak was used. All the prepared catalysts show the particle sizes of the range from 2.0 to 2.8nm. It can be thought that these values are in the acceptable range for the proper electrode performance[7]. For the prepared catalysts, notable differences are inter-metal distances(X[nm]) compared to commercial one. Due to their larger surface areas of support materials, active metals are apart from each other more than 2 3 times distance than commercial catalyst. Pt-Ru/SRaw has the longest inter-metal distances. 

The effect of oxidation pretreatment and oxidative reaction on the graphitic structure of all CNF or CNF based catalysts has been studied by XRD and HRTEM. From the diffraction patterns as shown in Fig. 2(a), it can be observed the subsequent treatment do not affect the integrity of graphite-like structure. TEM examination on the tested K(0.5)-Fe(5)/CNF catalysts as presented in Fig.2(b), also indicates that the graphitic structure of CNF is still intact. The XRD and TEM results are in agreement with TGA profiles of fi-esh and tested catalyst there is no obviously different stability in the carbon dioxide atmosphere (profiles are not shown). Moreover, TEM image as shown in Fig. 2(b) indicates that the iron oxide particle deposited on the surface of carbon nanofibcr are mostly less than less than 10 nm. 

In catalyst characterization, diffraction patterns are mainly used to identify the crystallographic phases that are present in the catalyst. Figure 4.5 gives an example where XRD readily reveals the Pd reflections in two Pd/Si02 catalysts. 

Combined analyses by XRD and TEM showed that the aurichalcite mineral was sufficiently similar to the synthetic aurichalcite to be used as a model compound, to study the microstructural changes occurring during the catalyst preparation procedures. Calcination of the mineral and synthetic samples led to highly preferred orientations of ZnO. ZnO electron diffraction patterns with [lOlO] and [3031] zone... 

We review our work on techniques and methods for examining the diffraction patterns from supported Pt,Pd and alloy catalysts, as well as the results that have been obtained in the last decade with these procedures in our group. 

Zeolites. In heterogeneous catalysis porosity is nearly always of essential importance. In most cases porous materials are synthesized using the above de.scribed sol-gel techniques resulting in so-called amorphous catalysts. Porosity is introduced in the agglomeration process in which the sol is transformed into a gel. From X-ray Diffraction patterns it is clear that the material shows only weak broad lines, characteristic of non-crystalline materials. Silica and alumina are typical examples. Zeolites are an exception they are crystalline materials but nevertheless exhibit high (micro) porosity. Zeolites belong to the class of molecular sieves, which are porous solids with pores of molecular dimensions, i.e., typically the pore diameter ranges from 0.3 to 10 nm. Examples of molecular sieves are carbons, oxides and zeolites. 

The poly(5-fnethyl-l, 4-hexadiene) fiber pattern (Figure 6) gave an identity period of 6.3 A, indicating a 3 isotactic helix structure. The X-ray diffraction pattern was not very sharp, which may be due to the difficulty of the side chain with a double bond to fit in a crystalline lattice. The crystallinity was determined to be 15% using the Hermans and Weidinger method (27). A Chloroform-soluble fraction free from catalyst residues showed no improvement in the sharpness of the X-ray diffraction pattern. These data show that the configuration of the 1,2-polymerization units in the homopolymer of 5-methyl-1,4-hexadiene is isotactic. 

Although conventional electron-probe microanalysis appears to be unsuitable for analysis of the exposed surface layer of atoms in an alloy catalyst, recent developments have shown that X-ray emission analysis can still be used for this purpose (89, 90). By bombarding the surface with high energy electrons at grazing incidence, characteristic Ka radiation from monolayer quantities of both carbon and oxygen on an iron surface was observed. Simultaneously, information about the structure of the surface layer was obtained from the electron diffraction pattern. 

FIGURE 4.10 X-ray diffractograms of the spent 20 wt% Co/Al203 catalyst after the run (in Figure 4.9) compared to a freshly reduced catalyst in wax. The wax was melted in situ in nitrogen at 120°C to remove interfering diffraction patterns.63... 

In catalyst characterization, diffraction patterns are mainly used to identify the crystallographic phases that are present in the catalyst. Figure 6.2 gives an example where XRD readily reveals the phases in an Fe-MnO Fischer-Tropsch catalyst [7], The pattern at the top is that of an MnO reference sample. The diffraction pattern of the reduced Fe-MnO catalyst shows a peak at an angle 29 of 57°, corresponding to metallic iron, and two peaks which are slightly shifted and broadened in comparison with the ones obtained from the bulk MnO reference. The Mossbauer spectrum of the reduced catalyst contains evidence for the presence of Fe2+ ions in a mixed (Fe,Mn)0 oxide [7], and thus it appears justified to attribute the distortion of the XRD peaks to the incorporation of Fe into the MnO lattice. Small particle size is another possible reason why diffraction lines can be broad, as we discuss below. 

Figure 6.4 X-ray diffraction patterns of Rh-Mn catalysts on Si02. Left catalyst with atomic ratio Rh/Mn=l after calcination in air at the indicated temperatures right calcined Rh-Mn catalyst (atomic ratio Rh/Mn=2) after reduction in H2 at the indicated temperature (from Kunimori et a/.[12]). 

Analytical electron microscopy of individual catalyst particles provides much more information than just particle size and shape. The scanning transmission electron microscope (STEM) with analytical facilities allows chemical analysis and electron diffraction patterns to be obtained from areas on the order of lOnm in diameter. In this paper, examples of high spatial resolution chemical analysis by x-ray emission spectroscopy are drawn from supported Pd, bismuth and ferric molybdates, and ZSM-5 zeolite. 

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. 

Nickel silicate, as catalyst, 20 106-109 differential thermogram of xerogel, 20 107 infrared spectra of, 20 108 preparation by SHCP method, 20 106 properties and structure of, 20 107-109 X-ray diffraction pattern of, 20 109 Nickel sulfate hexahydrate, dehydration of, dislocations and, 19 389 Nickel sulfides... 

A possible economically attractive alternative would be the production of acrylic acid in a single step process starting from the cheaper base material propane. In the nineteen nineties the Mitsubishi Chemical cooperation published a MoVTeNb-oxide, which could directly oxidise propane to acrylic acid in one step [6], Own preparations of this material yielded a highly crystalline substance. Careful analysis of single crystal electron diffraction patterns revealed that the MoVTeNb-oxide consists of two crystalline phases- a hexagonal so called K-Phase and an orthorhombic I-phase, which is the actual active catalyst phase, as could be shown by preparing the pure phases and testing them separately. 

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