ISSN 1087-6596, Glass Physics and Chemistry, 2017, Vol. 43, No. 4, pp. 368–375. © Pleiades Publishing, Ltd., 2017.
Original Russian Text © N.Yu. Koval’ko, M.V. Kalinina, A.N. Malkova, S.A. Lermontov, L.V. Morozova, I.G. Polyakova, O.A. Shilova, 2017, published in Fizika i Khimiya Stekla.
Synthesis and Comparative Studies of Xerogels, Aerogels,
and Powders Based on the ZrO
N. Yu. Koval’ko
*, M. V. Kalinina
, A. N. Malkova
, S. A. Lermontov
, L. V. Morozova
I. G. Polyakova
, and O. A. Shilova
Grebenshchikov Institute of Silicate Chemistry, Russian Academy of Sciences, St. Petersburg, 199034 Russia
Institute of Physiologically Active Substances, Russian Academy of Sciences, Chernogolovka, Moscow oblast, 142432 Russia
Ul’yanov (Lenin) St. Petersburg State Electrotechnical University LETI, St. Petersburg, 197022 Russia
Received December 29, 2016
Abstract—The technology of liquid-phase synthesis of mesoporous xerogels and aerogels based on ZrO
is developed. Xerogels are obtained by the coprecipitation of hydroxides, while aerogels are
obtained in accordance with the sol–gel technology: the average pore size is 1.5–17.2 nm and the specific sur-
face area is 120–878 m
/g. Aerogels are characterized by a high degree of porosity: the pore volume attains
/g. Based on precursor xerogels, nanopowders of a tetragonal solid solution of the
composition with a particle size of 5–9 nm and S
= 74 m
/g were fabri-
cated. Due to the high values of their specific surface area, the synthesized xerogels and aerogels are promis-
ing as sorbents, catalysts, or catalyst supports.
Keywords: zirconium dioxide, xerogels, aerogels, hydroxide coprecipitation, sol–gel technology, mesoporos-
ity, physical–chemical properties
Recently, the interest in studies of materials with
particle size not exceeding a few nanometers has been
constantly increasing due to the core differences of
their properties from those of micro-sized powders
and materials based on them [1, 2]. The unique elec-
tric, mechanical, magnetic, optic, and other proper-
ties of nanomaterials are responsible for their applica-
tion in various fields of medicine, power and mechan-
ical engineering, etc.
Among numerous ceramic materials, the most
promising in terms of application are those based on
zirconium dioxide partially stabilized with oxides of
rare-earth elements in cubic and tetragonal structures.
Materials of this type are characterized with a wide
range of physical–chemical properties: chemical and
thermal stability, mechanical strength, hardness,
strong resistance to cracking, low heat conductivity,
high ionic electroconductivity, etc. Transition to
nanosized structures allows increasing the values of
the specific surface area and adsorption capacity, as
well as improving the materials’ chemical reactivity
and catalytic properties. However, creating the tech-
nologies for the production of materials on the basis of
nanopowders is impossible without reliable data on
their morphological, size, and structural characteris-
tics. Thus, studying the primary products of the syn-
thesis of ceramic materials (xerogels and aerogels)
constitutes a necessary task, as the very stage of xerogel
formation is the one, during which the structure and
size of the grains of ceramics on its basis are formed.
Aerogels are produced by the sol–gel method with
subsequent supercritical drying of alcogels, namely,
the removal of the solvent from pores of the gel at tem-
peratures exceeding the critical temperature [3–8].
Nanodispersed xerogels and aerogels based on zir-
conium dioxide are wide applied as superlight con-
struction materials and modifying additives to them,
heterogeneous catalysts, and catalyst supports [9–11].
To produce low-agglomeration xerogels, aerogels, and
highly dispersed powders on their basis, different methods
of liquid-phase synthesis are used: combined hydroxide
coprecipitation, sol–gel method, etc. [12, 13].
The objective of the present work consisted in the
synthesis of xerogels, aerogels, and powders in the
system by different liquid-phase
methods (coprecipitation and sol–gel method) and
the study of their physical–chemical properties.