The XRD method of the determination of the size distribution of the
nanocrystalline materials

W. Arabczyk, R. Wróbel
Technical University of Szczecin, Institute of Chemical and
Environment Engineering, Pulaskiego 10, 70-322 Szczecin, Poland

The proposed method is a modification of the Warren-Averbach's one. It
is based on the reaction mechanism of the nanocrystalline substance
with a gas, when the rate of the process is limited by the rate of the
adsorption on the nanocrystalline material surface. In the result of
this process the phase transition occurs according to the crystallites
size, from the smallest to the greatest. The greater crystallites do
not undergo to the phase transition until the smaller ones are
converted. The chemical reaction enables to really separate the
fractions corresponding to a given range of dimensions, then to obtain
the distribution of the crystallites size. The proposed method was
verified on the example of the nanocrystalline iron in the nitriding
reaction. The samples having different conversion degree have been
obtained by a freezing of the process. The obtained samples were
analysed using the XRD method. The Scherrer's method has been used to
determine a mean crystallite size of the phases a-Fe and g'-Fe[4]N. On
the basis of the dependence of the mean crystallite size on the
conversion degree, the size distribution was determined.
Contrary to others, the presented method is very simple from the point
of view of the mathematical description as well as of the experimental
equipment.

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1. The XRD study of the nanostructured TiC/C and TiN/C composites.
2. The kinetics of the nanocrystalline iron nitrides reduction
3. Study of the Kinetics of the Nitriding of the Nanocrystalline Iron Using the TG and XRD Methods