In the last decade,
Cu2ZnSnS4 (CZTS) has
been a promising earth-abundant, nontoxic candidate material for absorption
layers within thin-film solar cells. One major issue preventing this
type of solar cells from achieving competitive efficiency is impurity
phases and structural defects in the bulk of the absorber; as a four-element
compound, the formation of CZTS is highly sensitive to synthesis conditions.
The impurity phases and defects differ by the fabrication method,
and thus experimental characterization is vital for the successful
development of CZTS photovoltaics. In this work, we characterize CZTS
nanoparticles obtained by the hot-injection method and a standard
N2/S annealing procedure. Phase-pure kesterite CZTS samples
in the desired compositional range were characterized by standard
means, i.e., Raman spectroscopy, X-ray diffraction, and energy-dispersive
X-ray spectroscopy. However, using synchrotron X-ray diffraction with
Rietveld refinement, we show that the as-synthesized nanoparticles
consist of a mixture of the tetragonal and the fully disordered cubic
sphalerite phase and transform into the tetragonal structure after
heat treatment. Sn vacancies are seen in the annealed samples. X-ray
total scattering with pair distribution function analysis furthermore
suggests the presence of a nanostructured CZTS phase along with a
bulk material. Finally, this study compares the benefits of applying
synchrotron radiation instead of a standard laboratory X-ray diffraction
when characterizing highly complex materials.