A software package "SADP Tools" is developed as a complementary diffraction pattern analysis tool. The core program, called AutoSADP, is designed to facilitate automated measurements of d-spacing and interplaner angles from TEM selected area diffraction patterns (SADPs) of single crystals. The software uses iterative cross correlations to locate the forward scattered beam position and to find the coordinates of the diffraction spots. The newly developed algorithm is suitable for fully automated analysis and it works well with asymmetric diffraction patterns, off-zone axis patterns, patterns with streaks, and noisy patterns such as Fast Fourier transforms of high-resolution images. The AutoSADP tool runs as a macro for the Digital Micrograph program and can determine d-spacing values and interplanar angles based on the pixel ratio with an accuracy of better than about 2%.
Match! is an easy-to-use software for phase analysis using powder diffraction data. It compares the diffraction pattern of your sample to a database containing reference patterns in order to identify the phases which are present. Additional knowledge about the sample like known phases, elements or density can be applied easily. In addition to this qualitative analysis, a quantitative analysis (using Rietveld refinement) can be performed as well. You can easily setup and run Rietveld refinements from within Match!, with the actual calculations being performed automatically, using the well-known program FullProf (by J. Rodriguez-Carvajal) in the background. Match! provides a gentle introduction into Rietveld refinement, from fully automatic operation to the "Expert" mode. The software runs natively on Windows, macOS and Linux.
Diffraction Pattern Analysis Software
As reference database, you can apply the included free-of-charge COD database, use any ICDD PDF product, and/or create a user database based on your own diffraction patterns. The user database patterns can be edited manually, imported from peak files, calculated from crystal structure data (e.g. CIF files), or imported from your colleague's user database. A list of Match!'s most prominent features can be found here.
A common question for new GISAXS users is: "What software can I use to analyze my data?" Unfortunately, there is no single package that will allow you to perform any possible analysis. This is in part due to the diversity of possible kinds of data analysis one might want to do on GISAXS or GIWAXS images. The following lists a variety of packages that are available.
_ Compatible with different diffractometer models and makers: Bruker - SMART APEX, GADDS, PROTEUM - , Oxford Diffraction - SAPPHIRE -, Mar Research, ADSC, Rigaku RMax, Nonius KCCD, TIFF, BMP._ Compatible with different detector geometries: Flat, Cylindrical (Debye-Scherrer or Guinier cameras), Spherical._ Generate multiple types of scans: 2Theta, Psi, X and Y scans. _ Multiple parameters fitting (wavelength, distance to detector, detector size, direct beam coordinates using a standard._ Mineral database and identification tool_ Compatible with Xpowder, JADE and EVA X-ray diffraction analysis software._ Logbook reporting all user actions and processed information _ Batch processing of an unlimited number of files _ Pole figure generation and analysis tool._ Operating system: Windows 98, 2000, XP and Vista. _ Custom features can be develop upon request. Important information Download XRD2DScan 4.1.1 Installation software (updated on August 10, 2011)
More recently, the Rietveld method [10] was adapted for quantitative XRD analysis [11,12]. Rietveld quantitative analysis involves calculating diffraction patterns of individual components of a mixture using a crystal structure model. The resultant simulated pattern is fit to an observed pattern by varying parameters of the model(s). The Rietveld method is very powerful and provides not only abundances but also provides other quantitative measurements such as unit-cell parameters, atomic occupancies, and information on crystallite size/strain. Most XRD instrument manufactures today offer some form of Rietveld refinement in their XRD software packages. Current Rietveld refinement programs typically require that the crystal structure of all component phases is known and that the phases are three-dimensionally ordered, which excludes materials such as glasses, polymers, and even natural geologic materials such as clay minerals.
An alternate method which is based on fitting of full XRD patterns to observed data has been proposed for obtaining quantitative abundances [13-18]. This method blends the advantages of the RIR and Rietveld methods. The full-pattern fitting method is similar to the RIR method but instead of using a single reflection, entire diffraction patterns are used. By using full diffraction patterns, including the background which contains important information on sample composition and matrix effects, explicit analysis of amorphous or partially ordered materials can often be readily accomplished if the amorphous/disordered phases are included in the analyses as distinct phases to be fit. In this case, the amorphous abundance can be measured directly rather than being determined as the difference from 100%. Like the Rietveld method, full-pattern fitting routines typically use least-squares minimization to optimize the fit of the library standards to the observed pattern, thereby minimizing user intervention. The use of full patterns compensates for preferred orientation and chemical variability (averaging reflections that are too strong with reflections that are too weak). The method can be easily applied to any mineralogical or materials system and requires little crystallographic background, as long as suitable standards are available. This paper describes the methodology behind full-pattern fitting and provides information for creating/generating standard patterns for quantitative analysis.
Full-pattern fitting for QXRD analysis requires generation of a library of standard patterns, including a pattern for each phase expected in the analysis. These libraries generally contain patterns of well-ordered phases, but they can include patterns for any material including glasses, polymers, clay minerals, organic materials, gels, pharmaceuticals, etc. In addition, simulated or calculated patterns may also be included in the library if it is not possible to obtain a pure sample of a material of interest. As with the traditional RIR method [2], an internal standard should be used to compensate for instrumental and sample matrix effects and to put all standard patterns on an equal-intensity basis so that unconstrained-total analyses can be made. This is readily accomplished if standards and samples are prepared in the same way, by adding to each a small, known portion of an internal standard. The internal standard may be any consistent material, but corundum has been the material of choice for many years [4] as it is stable, readily available, and typically has few peak overlaps on the phases of interest in the unknown samples. Using corundum as the reference material also facilitates analysis and preparation of standards, as most databases such as the ICDD powder diffraction file often list an I/Ic value (intensity of the phase 100% peak divided by the 100% peak of corundum). Any ratio of internal standard to sample can be used, but in our laboratories we have found that a mixture of 80% sample to 20% corundum is an optimal ratio.
ture containing a significant amount of volcanic glass. This example demonstrates the ability of the full-pattern fitting method to analyze samples containing amorphous or poorly ordered phases. This analysis was not constrained and did not require that the sum of all phases in the mixture, including the amorphous component, be normalized to 100% as it would with the RIR and many Rietveld programs. Because the entire pattern including the background was used, the amorphous component was treated simply as another phase in the least-squares refinement. As seen in the difference plot, the fit for this analysis is very good, with an unconstrained total of 98.2 weight%.
Although it is desirable to add an internal standard to unknown samples, as this allows unconstrained analyses, there are times when the addition of an Al2O3 standard to a sample is undesirable. Fortunately, the full-pattern fitting method can be applied without the addition of an internal standard, making the analysis analogous to the adiabatic flushing method described by [3]; this approach assumes that all the standard library patterns have been scaled to a constant corundum intensity. In this case, analyses are conducted as with the internal standard method, but the assumption is made that the sum of all phases must be 100%. However, because amorphous and disordered phases are included as independent phases in the analyses, their relative abundances are also determined independently during the analysis. The last step in the analysis is to simply normalize the relative percentages so that the sum of all phases is 100%.
As with any analytical method using standards, selection of standards matching the materials in unknowns is crucial, and this is no exception with full-pattern fitting QXRD. Individual machine configurations can significantly affect measured diffraction patterns. For example, theta-compensating slits, size of incident slits, Soller slits, radius of the goniometer circle, sample area, sample thickness, sample mount material, etc., can all have profound influence on measured diffraction patterns. Therefore, it is important to recognize that the quality of fullpattern quantitative analysis depends strongly on the quality of the standard library patterns. One should use patterns generated on another instrument or with different instrumental configurations only when necessary. Indeed, we do not share our measured standard patterns without this caveat. Figure 4 compares the diffraction pattern of a kaolinite: Al2O3 80:20 mixture collected on a Siemens D500 diffractometer with that produced from a Bruker D4 optimized for rapid throughput of production runs. Although many of the instrumental parameters such as goniometer radius and incident-beam optics are similar, the D4 machine has been optimized for maximum intensity for high sample throughput. These optimizations result in an elevated background, including low-angle artifacts resulting from scattering from the sample mount. Rietveld methods often experience difficulty modeling these low-angle artifacts, and the lowest-angle data are often excluded from refinement. However, such instrumental 2ff7e9595c
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