Hello Sean Clark,

First, you need to perform the subtraction of instrumental broadening using a standard for more accurate results. Then, the calculation of crystallite size by XRD will vary depending on the method that you use, commonly Debye–Scherrer equation is used with the most intense peak, in carbon materials (002) reflection is choose. Saying that my question is why you only calculate the crystallite from (100) reflection?

For a complete analysis you must calculate the crystallite size of (002) plane, so you will have the crystallite sizes along the c axis Lc and from the a axis La, which corresponding to (002) and (100) planes respectively and make the average crystallite size from both reflections, even from the (101) plane since is present in your diffractograms.

Also, you can perform the so-called Williamson-Hall, which take in count all the reflections of the present in your diffractogram and give you an average crystallite size. Usually, La tends to be bit bigger than Lc, since it is the reflection along the basal plane in graphitic skeleton (graphene layer). There are some reports that gives a crystallinity index depending on the intensities ratio of the (002) and (100) planes on carbon materials.

For a mor detailed analysis of the disorder degree in carbon materials you can perform too Raman spectroscopy, which can give mor structural details of your samples, obviously after spectra processing.

I let you some literature hopping might help you.

Regards.

https://doi.org/10.1021/ef030144+

Article Study of Stacking Structure of Amorphous Carbon by X-Ray Dif...

Rafael Valentin Tolentino-Hernandez

One minor correction. There is no Debye-Scherrer equation. There's a Debye-Scherrer camera, the Scherrer equation (to which you refer) and the Debye model (referring to Peter Debye) not to be confused with Debye-Hückel theory. Lots of references to this point on ResearchGate.

Rafael Valentin Tolentino-Hernandez Thank you for you response Rafael!

I have fit both the 002 and 100 reflections and applied the Scherrer equation to both. My focus on the 100 band in the question was to compare with Raman spectra as many investigators have tried to obtain a relation between Raman and XRD signatures for La. So I have been attempting to use the two approaches as a means of checking my fitting routine.

I was mainly just concerned about the La size of the amorphous C-12 material. When comparing the peaks of all three materials, from the aC-12 shape, I was expecting a much smaller crystallite size for the 100 reflections (Lc I found to be ~1.8nm). So was hoping to get feedback on whether my model seemed reasonable.

Haven't paid much attention to the Williamson Hall as my focus is on the carbon. Unfortunately, in my amorphous materials there is some contamination (especially the C-13), so I have steered clear from that analysis for the moment, but perhaps it is worth looking into.

Thanks again!

Best regards

By following this structured approach—preprocessing, peak identification, appropriate curve fitting, and validation—you can accurately fit and analyze the Raman spectra of carbon materials with varying degrees of disorder. Automating the process using Python/MATLAB will help efficiently handle 100 peaks across multiple spectra.