Oxidation of Metallic Iron with Oxygen
via Mechanochemical Activation
A. P. Il’in, A. A. Il’in, and N. N. Smirnov
Ivanovo State University of Chemistry and Technology, State Educational Enterprise
for Higher Professional Education, Ivanovo, Moscow oblast, Russia
Received December 1, 2009
Abstract—The X-ray phase analysis and X-ray diffraction, as well as IR and Mössbauer spectroscopic
techniques were employed to study mechanochemical oxidation of iron metal powder with oxygen. The phase
composition of the products of mechanochemical activation of iron in a vibrating mill was determined. The
extent of oxidation of iron was examined in relation to the particle-size distribution of the starting iron powder.
INORGANIC SYNTHESIS AND INDUSTRIAL
ISSN 1070-4272, Russian Journal of Applied Chemistry, 2010, Vol. 83, No. 9, pp. 1535–1539. © Pleiades Publishing, Ltd., 2010.
Original Russian Text © A.P. Il’in, A.A. Il’in, N.N. Smirnov, 2010, published in Zhurnal Prikladnoi Khimii, 2010, Vol. 83, No. 9, pp. 1435–1439.
Iron oxides and hydroxides belong to the most
widespread oxide materials that are extensively used
today in production of inorganic pigments, magnetic
information carriers, catalysts, and sorbents [1–3].
Iron oxide is the principal component of catalysts
used for carbon monoxide conversion in ammonia
production, which can be prepared by thermal decom-
position of various compounds: hydroxide, nitrate,
carbonate, sulfate, chloride, alcoholate, etc. [4–6]. The
main disadvantages of the known methods used for
iron oxide preparation consist in large amounts of
chemicals spent, the need to strictly control the
coprecipitation parameters, and generation of abundant
wastewater. The process utilizing metal powders as
raw material for catalyst preparation eliminates
contamination of the resulting product, reduces the
number of energy-intensive stages, and is charac-
terized by high economic efficiency and environmental
Preparation of solid compounds with desired
physicochemical properties, particle size, and defect
structure ranks among the principal tasks assigned to
catalyst technology. Ever increasing application for
synthesis purposes is found today by mechanical ac-
tivation. When applied for catalyst production, this
method allows increasing the catalytic activity of exist-
ing systems, simplifying the process by decreasing the
number of stages it involves, and expanding the range
of available raw materials. Mechanochemical reactions
hold promise for development of new, unconventional,
so-called dry processes that are more environmentally
friendly and economically efficient than the existing
processes [6, 7, 10].
Mechanical treatment of inorganic materials in
various milling devices is a convenient and fairly
simple procedure attracting much interest for synthesis
of nanocrystalline and amorphous powders. This offers
wide prospects for preparation of materials superior in
properties to those synthesized by conventional methods.
The exclusive technical significance of iron and its
alloys has motivated numerous experimental studies
dedicated to iron oxidation in air, as well as by oxygen
and other oxidants [7–10].
Here, we studied mechanochemical oxidation of
iron metal powder in a vibrating mill in an oxygen
atmosphere, examined the phase composition of the
product mixture yielded by mechanochemical activa-
tion (MChA) and subsequent thermolysis, and
determined the particle size distribution and specific
surface area of the resulting material.
We used PZhR iron metal powder separated into
three fractions: <15, 40–200, and 160–315 μm.
Mechanochemical activation of the iron metal powder
was carried out in a VM-4 vibrating annular roller mill
operated at the vibration frequency of 930 min