Ekaterina Abdulmenova

The Quantification of crystalline phases can be done through Rietveld refinement.

You can go through the attached pdf for reference.

Best Regards,

Dipayan

Generally speaking; (I) the peak height or the maximum intensity in XRD spectra represents an approximation for the peak intensity, (II) the peak area a.k.a. the integral intensity can be considered as the real measure for the peak intensity that is related to the crystal structure that is commonly used to determine the amount of a particular phase, while (III) peak width or Full Width at Half Max (FWHM) aka half width represent crystallite size, and defects in form of strain and disorder (with line asymmetry associated with particle size). More detail description could be find at: http://www.fhi-berlin.mpg.de/acnew/department/pages/teaching/pages/teaching__wintersemester__2015_2016/frank_girgsdies__peak_profile_fitting_in_xrd__151106.pdf

Also, an example for the application of Rietveld method used in application of XRD in phase analysis can be seen at: http://www.icdd.com/resources/axa/vol47/v47_40.pdf

1. A representative peak for each of the phases presenting in the pattern should be selected. Integral intensity of each peak should be calculated after a peak refinement (see Rietweld procedure)

2. Pair-phases calibration curves for each pair of the existing phases should be experimentally obtained.

3. For examined N-phase sample, N-1 pair-phase calibration curves should be used to build N-1 equations. The additional equation should be a normalizing one, so a system of N linear equation with N unknown variables (phase contents) should be solved.

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Dear Ekaterina,

in general case:

Start your procedure by making a Pawley intensity extraction, to have a reasonable peak profile description.

(i) It is much more reliable to do it via Rietveld refinement instead of peak intensity.

(ii) For the fitting process, you need to use the same profile fitting for both phases, and if you have at least 2, you can choose different peak descriptions. However, they are hard to compare, please choose the same description, let say PseudoVoight for all phases.

(iii) Do not use preferred orientation in your fitting, if you already checked and know there is preferred orientation in your sample, treat it before, got knew X-ray experiment and only after that, with no observed preferred orientation observed, proceed with the phase quantification.

(iv) Take into account that more phases you have, less success on the real quantification, especially if some overlap occurs, you will face a competitive fitting for width and profile distortion that is not present in your original sample.

(v) all of that is reliable if we are talking about crystalline phases if one amorphous phase is present you need to treat it entirely apart.

Best regards,

WNM

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