The electrochemical reaction between aqueous ferric chloride solution and M
g powder has been carried out in open atmosphere to prepare iron nanopartic
les. Since iron particles get easily oxidised to alpha -Fe2O3, gamma -Fe2O3
and Fe3O4, the final product contains the oxides in different proportions
with different dimensions depending on the concentration of the FeCl3 solut
ion in the electrochemical reaction. The final products were characterised
using X-ray and Mossbauer spectroscopy. The results may be summarised as: (
1) concentrated solution yields Fe particles of smallest size with a superp
aramagnetic doublet in the Mossbauer spectrum arising from oxide nanopartic
les; (2) moderately diluted solution yields Fe particles of maximum size, a
nd the Mossbauer spectrum was a superposition of a sextet line arising from
Fe3O4, a superparamagnetic singlet, and doublet from Fe and its oxides; (3
) fairly diluted solution yields Fe particles of intermediate size and the
Mossbauer spectrum was a superposition of a sextet line corresponding to me
tallic alpha -Fe and superparamagnetic line similar to case (2). The experi
mental results are discussed in terms of consecutive processes in the elect
rochemical reaction. (C) 2001 Elsevier Science B.V. All rights reserved.