Recently I used improved Hummer's method to synthesize Graphene Oxide. Then I analysed it with XRD, but beside ~10 degree peak of GO, the was high intensity before the peak that should be straight and no peak, different from others results I read,. Does anyone know something about this result? Please help me.
Here is my result (the circled area is where I need help): https://imgur.com/lcEO79x
Hi Manh Le,
Judging from the tilted baseline, I am hesitant to claim that the broad peak you labelled is an actual peak from your sample. Your spectrum starts at 5 degrees. If I remember correctly, the accuracy of powder XRD at such a low diffraction angle is poor. Therefore, the broad peak could simply come from the background. Have you perform a blank run with the same range of the diffraction angle? You might be able to identify the source of the labelled peak.
a very strange diffraction pattern indeed. What's the form of your specimen? This might be your issue.
You can see two peaks from GO, but your background is not clean. I suppose you are using a parafocusing geometry (Bragg-Brentano conventional diffractometer). In that case, the primary beam is divergent and therefore the lower the angle, the more the beam spreads over a large surface of the specimen. Besides getting a large asymmetry of the peaks, if you have large slits, part of the beam starts to get into the detector and the background. Artifacts at lower angle are common. The specimen should be uniform and sufficiently large tat the beam does not spill out.
As suggested, try measuring a large powder sample (most common materials don't have peaks at those low angles) or a flat polycrystalline specimen down to the lowest angle you can safely reach (for the detector). In that case you should see a clean background. Then try preparing your specimen in a different way (e.g. spreading it uniformly over a large area) or try measuring the specimen with narrower slits.
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