I would like to know if there is a reason for these twin peaks in my XRD. The starting material is CuO with hydrazine as the reducing agent. End product is metallic Cu.
you change the concentration of CuO relative to hydrazine by a factor of 6 when going from your curve a to c. So you gradually go from CuO (curve c) to Cu (curve a) as you have explained in the text. So you will have a superposition of XRD spectra of propably Cu and CuO.
Please see that your small twin peak at the right side in curve b) and c) is sitting just at the position of the large peak In curve a). To my opinion is that there is no peak splitting but a superposition of XRD spectra of two different materials ( e.g. Cu and CuO) or you see some kind of XRD signal from your substrate/sample holder in addition to that of your sample depending on the progess of CuO reduction.
May be alternatively a superposition of Cu2O and CuO XRD spectra as Alan suggested..
If there are mixture of materials, with one being major phase than the other may be minor phase, that could happen...purity of material also can be known from such peaks...
please add XRD spectra of Cu powder (as curve ao), CuO without hydrazine (as curve d) and if you have availble Cu2O (as curve e). So you will be able to see directly which material is in your spectra a) to c).
The peak at about 43.3° is due to Cu, in fact is the only present when you have an high amount of hydrazine (pattern a). In the other cases there is a mixture of Cu and Cu2O (peak at about 42.3°). To confirm this phase you should see also a peak at about 36.4° (its main peak). If so I think that this is the correct explanation (in pattern c with small amount of hydrazine the peak of Cu2O is more evident than in pattern b)