Powder diffraction pattern digitized

The powder diffraction pattern is first obtained in digitized form as a set of intensities yi where i identifies a scattering angle increment in the pattern. Typically,the increment size is... 

Figure 4.20. Experimental powder diffraction pattern of NiMnOaCOH) (top) compared with the digitized PDF records 49-1170 (middle, solid lines) and 43-0318 (bottom, dashed lines). Downward arrows indicate peaks present in the latter record but absent in the measured pattern. Upward arrows shown on the experimental pattern indicate observed Bragg peaks that are missing in the nickel manganese oxide hydroxide, ICDD record No. 43-0318.

Here 1)" is the observed and is the calculated intensity of a point i of the powder diffraction pattern, k is the pattern scale factor, which is usually set tk= because scattered intensity is measured on a relative scale and k is absorbed by the phase scale factor (e.g. see Eqs. 7.3 and 7.4, below), and n is the total number of the measured data points. Hence, a powder diffraction pattern in a digital format, in which scattered intensity at every... 

The outline of Rietveld analysis of the structure is to compare the digital intensity y of a powder diffraction pattern obtained by experiment to intensity yc of calculation by a model, and the difference between the two models leads to the excursion amendatory value of structure parameters by the least squares method, and by adding it to the corresponding model structure parameters, the difference between y, and yci achieves the minimum value. 

Recent developments and prospects of these methods have been discussed in a chapter by Schneider et al. (2001). It was underlined that these methods are widely applied for the characterization of crystalline materials (phase identification, quantitative analysis, determination of structure imperfections, crystal structure determination and analysis of 3D microstructural properties). Phase identification was traditionally based on a comparison of observed data with interplanar spacings and relative intensities (d and T) listed for crystalline materials. More recent search-match procedures, based on digitized patterns, and Powder Diffraction File (International Centre for Diffraction Data, USA.) containing powder data for hundreds of thousands substances may result in a fast efficient qualitative analysis. The determination of the amounts of different phases present in a multi-component sample (quantitative analysis) is based on the so-called Rietveld method. Procedures for pattern indexing, structure solution and refinement of structure model are based on the same method. 

A digitized representation of powder data is quite compact and is especially convenient for comparison with other patterns, provided a suitable database is available. In addition to a digitized pattern, each entry in such a database may (and usually does) contain symmetry, imit cell dimensions, and other useful information phase name, chemical composition, references, basic physical and chemical properties, etc. Powder diffraction databases find substantial use in both simple identification of compounds (qualitative analysis) and in quantitative determination of the amounts of crystalline phases present in a mixture (quantitative analysis). 

The diffraction pattern from a single crystal is also unique but due to the complexity of a three-dimensional distribution of intensities, phase recognition is difficult to formalize. Powder data are one-dimensional, and they can be converted into digitized patterns, which are in a way, unique barcodes enabling automated pattern recognition. 

Phase identification using powder diffraction data requires a comparison of several key features present in its digitized pattern with known compounds/phases. This is usually achieved by searching powder diffraction database(s) for records, which match experimentally measured and digitized pattern. Thus, a powder diffraction database or at least its subset should be available in addition to a suitable search-and-match algorithm. 

The most complete and most often used powder diffraction database is the Powder Diffraction File (PDF), which is maintained and periodically updated by the fritemational Centre for Diffraction Data (ICDD ). PDF is a commercial database, and complete information about both the ICDD and Powder Diffraction File is available on the Web at http //www.icdd.com. This database is quite unique it contains either or both the experimentally measured and calculated digitized powder patterns for hundreds of thousands of compounds, including minerals, metals and alloys, inorganic materials, organic compounds and pharmaceuticals. The PDF is available as a whole or in subsets. Each record in the database is historically called the card."... 

Recently the ICDD Powder Diffraction File underwent a substantial and useful upgrade calculated patterns based on single crystal data from the ICSD file have been included into the PDF-2/PDF-4 Full File calculated patterns of structures stored in the CSD file, have been included into the PDF-4 Organics (see Table 4.3). These additions make it possible to conduct searches and find matches with computed digitized powder patterns in addition to experimentally measured powder diffraction data, thus improving automation, simplifying phase identification process and considerably expanding the applicability of the powder method for a qualitative phase analysis. 

Raw X-ray diffraction data, either digital or acquired on a strip recorder, are used make mineral identifications as summarized above. Whole sample data collected from random powder mounts are compared to patterns of known minerals either manually or using a computer search-match program such as /zPDSM (Marquart, 1986). Because each component in a mixture of crystalline materials produces its own characteristic pattern that is independent of others, the identification process becomes one of simply unscrambling the superposed patterns. 

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