It have been very difficult for me to get proper XRD peaks for the Fe3O4 nps. It might be due to too much impurity in my sample during preparation. I am using standardized sol gel method.
Yes, preparation method play a role in crystalline property, which of course affect XRD peaks. May be nano particles are very small and have amorphous nature.
The XRD pattern of a powdered sample depends not only on the chemical nature of a crystalline sample but also on the alignments of particles in preferred planes. This is quite prominent in the case of thin films where the intensities of peaks reflect the relative amount of particles aligned in the planes corresponding to the diffractions observed. Different preparation techniques can give different sized and different shaped nanoparticles and different alignments also. If the particles such as 1-D nanomaterials are aligned only in one plane you should get only one peak in its XRD. If they are aligned along only two planes then two peaks will be observed and so on. Therefore, it is quite obvious that different preparation methods of the same material will give different XRD patterns.