Russian Journal of Applied Chemistry, 2010, Vol. 83, No. 8, pp. 1413−1416.
Pleiades Publishing, Ltd., 2010.
Original Russian Text
I.I. Lebedeva, N.B. Kondrashova, V.I. Karmanov, E.V. Saenko, V.N. Strel’nikov, 2010, published in Zhurnal Prikladnoi Khimii,
2010, Vol. 83, No. 8, pp. 1308−1311.
The Effect of Composition of the Reaction Medium
on the Structural-Textural Characteristics
of Mesoporous Silicon Dioxide
I. I. Lebedeva, N. B. Kondrashova, V. I. Karmanov,
E. V. Saenko, and V. N. Strel’nikov
Institute of Technical Chemistry, Russian Academy of Sciences, Ural Branch, Perm, Russia
Received March 23, 2010
Abstract—The conditions for the preparation of mesoporous silicon dioxide in water–alkali, alcohol–alkali,
water–ammonia, alcohol–ammonia, and acid media were determined and its textural characteristics were studied.
Preparation of mesoporous mesophase materials
(MMMs) by the liquid-crystal templating [1, 2] was
the beginning of a new direction in the chemistry of
mesoporous materials. The above materials have spa-
tially ordered structure of pores uniformly distributed
by size (2–50 nm diameter), large speciﬁ c surface area
), and large pore volume (~1 cm
Depending on the synthesis conditions, the material
has the hexagonal, cubic, or lamellar structure (denoted
as MSM-41, MSM-48, and MSM-50, respectively).
The key parameters in MMM synthesis are hydrogel
composition, type and length of the surfactant, pH
and composition of the reaction medium, synthesis
temperature, and synthesis time . Preliminary
temperature aging of silicon-organic mesophase 
and its hydrothermal treatment in mother liquor 
assist structural ordering. The structural perfection
of mesoporous material, and consequently, regions of
its further possible application, are determined by the
balance of processes of its formation (osmotic expan-
sion, surface hydrolysis, and polymerization), which
are largely determined by the composition of a reaction
medium . Therefore, the study of the effect exerted
by composition of the reaction medium on the textural-
structural characteristics of the material is urgent and
this is the goal of the study.
The samples under study were synthesized by the
liquid-crystal templating at 80°С at constant agitation for
3 h. As template was used cetyltrimethylammonium bro-
mide (CTAB). Then, the reaction mixture was subjected
to static hydrothermal treatment at 120°С for 48 h. The
stoichiometric ratios of the components chosen for the
synthesis and рН of the reaction media are given in the
table. After the synthesis was complete, the precipitates
obtained were ﬁ ltered, washed to neutral рН, and dried
in air at 80°С. The template was removed by calcinations
in air at 650°С for 5 h.
The structure of the samples was studied by the low-
angle X-ray phase analysis [Shimadzu XRD-7000 dif-
fractometer (Japan), Cu
and Raman spectros-
copy [Bruker SENTERRA multifunctional spectrometer
The textural parameters of the samples were deter-
mined by nitrogen sorption at –196°С with an ASAP
2020 system (Micromeritics) after degassing the material
in a vacuum at 350°С for 3 h. The speciﬁ c surface area
of the samples was determined by the BET method and
the pore-size distribution, from the desorption isotherms
using the BJH model.
The diffraction patterns of the products formed in