You can calculate the crystallinity of each phase from XRD. First, calculate the area under all the peaks (total area). Second, you need to calculate the area under each phase in all orientations. Dividing the second/first*100, it will give you the percentage of crystallinity. However, I need to mention that this method is useful only for crystalline phases.

Dear Hadi Parsamehr

Thank you for your answer but I do not think it works for highly textured thin films with two phases. For powders, I know that the Rietveld method can be used but for thin films, neither the Rietveld method nor the method you suggested could be precise or even acceptable.

Dear Alireza

The mostly used diffraction geometry in commercial diffractometers is the symmetric diffraction geometry in parafocusing Bragg-Brentano (BB) arrangement. “Symmetric“ in this case means that the incident and diffracted beam (which is just registered by a detector) make both the same angle with the surface of a flat sample. This is given by the double angular speed of the detector arm in comparison with the rotation of the sample. In such a case only the diffraction from crystallographic planes which are parallel to the sample surface is registered in any diffraction angle. The measured reflections thus correspond to the diffraction of the incident X-ray beam on different sets of grains. And because the intensity of the diffracted beam is a function of volume fraction of grains in given orientation, it is clear, that this method can be used as a simplest tool for an assessment of occurrence of a texture. When there is a prevailing “number” of grains with (111) planes parallel to the sample surface then the intensity of reflection from these planes will be relatively higher in comparison with the case of a random grain orientation. The aim of the complete texture analysis is to determine the whole profile of the orientation distribution function of grains which is done in such a way that a selected reflection is measured with the detector fixed at the corresponding diffraction angle and the sample orientation is gradually changed to scan almost the whole hemisphere above or behind the sample. The technical details are at the moment less important. Let us only mention that both. The texture and stress analysis can also be performed in some cases using the BB diffractometer with decoupled sample and detector axes. Another special diffraction geometry is the grazing incidence X-ray diffraction (GIXD) which is mainly used for a study of epitaxial layers. The aim of this method is to follow the diffraction from planes which are perpendicular to the sample surface. To do this the sample must be tilted in such a way that its surface lies close to the diffraction plane, i.e., the incident and the diffracted beams make both the same very small angle with the sample surface. A proper sample rotation around its normal (which is now almost perpendicular to the diffraction plane) is necessary before measurement being started to find a reflection from selected crystallographic planes. Then a normal diffraction measurement is done with the detector coupled to the sample rotation around the goniometer axis with the angular speed ratio 2:1. The measured parameters are the interplanar lattice spacing (and consequently strain in the surface plane), the degree of grain disorientation (“texture” in azimuthal directions) and the lateral grain size.

Once you can check the following attachment it may help you.

Regards

Dear M. S. Alkathy

Thank you very much for your answer and the attached file.

Hello Alireza,

Would TaC and Ta2C not be "easily" discriminated thanks to EBSD ? The poles figures would confirm you the different texture, and the amount of each phase may also be determined.

Dear Arnaud Porcher

Thank you for your response. I have never done such an analysis. I have to think about that if it is feasible. but I think it is plausible.

Dear Alireza Farhadizadeh,

Instead of SEM use OIM(orientation Image Microscopy) for texture analysis.

The crystallographic texture can be described by an orientation distribution function (ODF) that is determined from pole densities experimentally measured by diffraction methods (Advanced X-ray Diffraction Techniques- the measured diffraction patterns are used to describe phase and texture evolution during heating and crystallization of solution-derived thin films). The diffraction images can be measured sequentially while heating the thin film with an infrared lamp. The ODF is then approximated by a finite number of texture components. The volume fraction and sharpness of a texture component is a quantitative measure that is used for comparative studies and monitoring of texture evolution during thermal treatments. The precision and accuracy of the method is discussed and linked to the quality of the experimental data. Specific examples are presented for electroplated Cu thin films that are of interest for integrated circuit metallization.

Hope this is helpful for you.

Ashish