Determination of percent crystallinity by XRD, the determination is based on the relative intensity of specific peaks: In a fully crystalline material, the peaks have well-defined intensities. Determination of content of From A in Material B using XRD analysis can be based on the internal standard method:
When percent crystallinity is determined via XRD, the crystallinity is also calculated by dividing the total area of crystalline peaks by the total area under the diffraction curve (crystalline plus amorphous peaks).
Prof Shen-Ming Chen well addresses the case. My contribution based on that the percent of crystallinity is a relative value determined from the intensity height progress of the main peak toward the full crystalline peak height value centered on more or less the same 2 theta value on condition that the characterization output done by the same XRD device and same operation parameters and conditions and plotted to the same print scale (counts scale). So for ultimate reasonable results it is height change rather than area change. In this respect, the percent of crystallinity reflect the state of material between its poor crystalline state and well crystalline state except for pseudo-crystalline materials.
Unfortunately XRD occurres only for lattice periodicity which only exists in the centre of nanoparticls that's why HRTEM is used for srtuctue investigation. For more information see the article Physica B 404, 5203, (2009) and articles related
An estimate can be got from XRD. Prof Shen Ming's answer gives you enough inputs. Other answers too. You can get an estimate, themn improve on that, if needed.
Reitveld method is most accurate. For well crystalline powders, the crystallinity can be calculate with simple method by dividing the total area of crystalline peaks by the total area under the diffraction curve, but it is not very accurate. It is only a relative information.
Your question is not very well defined. If you have an amorphous materials under crystallization, the VOLUME % of the new phase can be estimated using X-Ray diffraction, microscopy, Raman, etc. In the case of X-ray powder diffraction, of course you need a calibration curve, to work quantitatively.
well percent crystallinity is determined by XRD, the crystallinity is calculated by dividing the total area of crystalline peaks by the total area under the diffraction curve (crystalline plus amorphous peaks).
% Crystallinity = (total area of crystalline peaks) / (total area of all peaks)