Kinetics and Catalysis, Vol. 45, No. 2, 2004, pp. 279287. Translated from Kinetika i Kataliz, Vol.

45, No. 2, 2004, pp. 299307.

Original Russian Text Copyright 2004 by Ratko, Romanenkov, Bolotnikova, Krupenkina.

Hydrothermal Synthesis of Porous Al2O3/Al Metal Ceramics:

IV. Synthesis of Composite Porous Ceramics in the Presence
of Microporous and Mesoporous Adsorbents
A. I. Ratko*, V. E. Romanenkov**, E. V. Bolotnikova*, and Zh. V. Krupenkina*
* Institute of General and Inorganic Chemistry, Belarussian Academy of Sciences, Minsk, 270072 Belarus
** Institute for the Advanced Training and Retraining of Personnel,
Ministry of Education of the Republic of Belarus, Minsk, Belarus
Received December 5, 2001; in final form, March 14, 2003

AbstractThe formation of the structure and properties of mesoporous composite ceramics based on an
ASD-1 aluminum powder and commercial adsorbent powders (zeolites and active alumina) was studied. It was
found that the mechanism of the formation of contacts between the particles of commercial adsorbents and aluminum is analogous to the mechanism of synthesis of an Al(OH)3/Al composite. The dissolution of aluminum
and the precipitation of the hydroxo complexes of aluminum from solution to the region of interparticle contacts
are responsible for this mechanism. The resulting composite ceramics exhibited a polydisperse pore structure
and high values of mechanical strength, gas permeability, and thermal conductivity; it can be used as a block
adsorbent and catalyst support.

INTRODUCTION
Porous ceramics used as adsorbents and catalyst
supports in processes with high mass-transfer space
velocities should contain a considerable fraction of
macropores, which are responsible for low hydraulic
resistance to liquid and gas flows at the maximally possible use of the sorption surface and low diffusion resistance. Moreover, such a material should exhibit high
mechanical strength, thermal conductivity, and thermal
stability. For the most part, pelletized uniformly porous
adsorbents and supports are currently used in sorption
and catalytic processes. To prepare heterogeneous
(biporous) structures, the method of building or
assembling homogeneous disperse particles with the
use of binding agents (gels; sols; various clays;
cements, in particular, aluminosilicate and aluminophosphate binding materials; etc.) is applied [13].
However, this method is insufficiently effective for a
considerable increase in the macropore size, gas permeability, mechanical strength, and thermal conductivity.
Block supports are also prepared based on ceramic
materials with a honeycomb structure; highly porous
cellular materials; metal wire, gauze, fibers, and sheets;
and permeable powder metallurgical materials [48].
The block supports thus prepared exhibit high gas permeability, mechanical strength, and thermal conductivity; however, they rank much below pelletized (loose)
materials in sorption capacity and specific surface area.
Therefore, their geometric surface is coated with a secondary support layer using colloid-chemical methods.
The oxidation of aluminum powder with water at
100C followed by thermal dehydration gives mechanically strong porous Al2O3/Al metal ceramics with a

great macropore volume and a high specific surface

area, which are characteristic of, on the one hand, permeable powder materials and, on the other hand, adsorbents and catalyst supports. This method provides wide
opportunities for the development of versatile porous
materials. Materials with a unique set of performance
characteristics, which cannot be reached by traditional
methods of colloid chemistry and powder metallurgy,
can be prepared by the above method with the use of
powdered components of different compositions, physicochemical natures, and reactivities toward a hydrolysis reaction. Previously [911], we studied the process
mechanism of formation of the structure and properties
of a porous Al2O3/Al composite. This paper is devoted
to a study of the formation of the structure and properties of highly porous block composite ceramics prepared based on ASD-1 aluminum powder and commercial adsorbent powders (zeolites and -Al2O3) under
hydrothermal conditions at 100C.
EXPERIMENTAL
To prepare composite ceramics, commercial pelletized adsorbents (zeolites NaX, NaY, and NaA and
-Al2O3) were mechanically crushed and screen-fractionated. The resulting adsorbent powder was mixed
with ASD-1 aluminum powder in a certain weight ratio
(3 : 1 or 2 : 1 by weight); the mixture was loaded in a
mold of corrosion-resistant steel and hydrothermally
treated at 100C for 1.52 h. Changes in the pH and the
volume of released hydrogen with time were studied
with the intense stirring of the mixture of aluminum and
adsorbent powders. The porous blocks formed in the

0023-1584/04/4502-0279 2004 MAIK Nauka /Interperiodica

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RATKO et al.

pH
10.5

0.6

3
10.0

0.4

3
2

9.5
0.2

9.0
8.5
0

5
t, h

8.0

5
t, h

Fig. 1. Changes in the conversion of aluminum with time in

the oxidation of aluminum with water at 100C in the presence of adsorbents (adsorbent/Al ratios of 3 : 1): (1) NaX,
(2) -Al2O3, and (3) pure aluminum powder.

Fig. 2. Changes in the pH of solution with time in the oxidation of aluminum with water at 100C in the presence of
adsorbents (adsorbent/Al ratios of 3 : 1): (1) NaX, (2)
-Al2O3, and (3) pure aluminum powder.

course of hydrothermal treatment were cylindrically

shaped and had various diameters and heights. They
were dried at 120C for 30 min and calcined at 550C
for 1 h. The shape and size of the interparticle contacts
and the character of particle aggregation in the samples
synthesized were studied with the use of procedures
described elsewhere [9]. The thermal conductivity of
samples 15 mm in diameter and 3 mm in thickness was
determined using the one-sided heating of the sample
with an external heat flow [12]. The thermal capacity
coefficient was determined with the use of a dynamic
C-calorimeter with a heat meter and an adiabatic jacket.

aluminum with water in the kinetic region. The zeolites

used in the experiments contained compensating
sodium cations, which partially passed into solution;
because of this, the pH of the solution increased more
intensely. The solubility of aluminum hydroxide
increased because of an increase in the concentration of
OH ions, and the reaction of aluminum with water proceeded more deeply.
In the presence of silica gel powder, the hydrolytic
reaction of aluminum with water did not occur, and a
porous composite was not formed. This is because a
monomer film, which is impermeable to water molecules, of silicon dioxide colloid particles is formed on
any solid surface that carries OH groups, in particular,
on aluminum particles, because of the partial dissolution of the silica gel. It was found [13] that a silicon
dioxide film about 23 nm in thickness deposited onto
the surface of nickel powder from a colloid solution
prevented the metal from reacting with water.

RESULTS AND DISCUSSION

Kinetics of Oxidation of Aluminum Powder
with Water in the Presence of Adsorbent Powders
To study the effects of adsorbent powders on the
kinetics of aluminum oxidation, we performed a comparative analysis of the kinetic curves reported previously [9] for the initial aluminum powder and the functions for the mixtures of aluminum powder with powdered commercial adsorbents. The time dependence of
the degree of conversion in the oxidation of the initial
aluminum powder and in the oxidation in the presence
of powdered -Al2O3 exhibited the same character
(Fig. 1). Consequently, powdered -Al2O3 is a neutral
substance, and it has no effect on the oxidation of aluminum; this is supported by the almost complete coincidence of curves that characterize changes in pH with
time (Fig. 2). In the presence of zeolite powder, the conversion of aluminum and the pH of solution were
higher than those for the initial aluminum. Moreover,
the kinetic curve exhibited a rectilinear portion, which
is indicative of the occurrence of a chemical reaction of

Ultramacropore Structure Peculiarities

of the Synthesized Materials
A study of the prepared samples on a scanning electron microscope allowed us to examine the shape, size,
and aggregation of particles in the synthesized material
and the structure of the interparticle contacts formed. In
the test samples, porous aggregates of adsorbent particles (6001000 m) and much smaller aluminum particles (3050 m) formed a texture basis (Figs. 3, 4).
Adsorbent particles, which were arbitrarily shaped
debris with wide planes of brittle fractures, formed
upon the dispersion of adsorbent granules, were covered with a layer of aluminum particles. The aluminum
particles were bound to each other and to the adsorbent
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HYDROTHERMAL SYNTHESIS OF POROUS Al2O3/Al METAL CERAMICS: IV.

281

()
25

(b)
6000
Fig. 3. Electron micrographs of the Al2O3/Al + zeolite NaY composite ceramics (zeolite fraction of 0.61 mm; NaY/Al ratio of
3 : 1): (a) 25 and (b) 6000.

particles through oxide contacts formed in the course of

synthesis. The material exhibited a polydisperse structure with two types of transport pores as spaces
between joined aluminum particles and spaces between
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porous aggregates. Joining with each other, the chains

of aluminum particles formed a locally ordered spatial
openwork skeleton, in which cavities were regularly
alternated with particles. Regions with disordered par-

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RATKO et al.

100 m

()

(b)

10 m

Fig. 4. Electron micrographs of the Al2O3/Al + -Al2O3 composite ceramics (-Al2O3/Al ratio of 3 : 1): (a) 25 and (b) 6000.

ticle packing were also observed because the thickness

of the aluminum powder layer that covered adsorbent
particles was nonuniform. The surface morphology of
aluminum particles and contacts formed between the
particles of aluminum and powdered adsorbents essentially depended on the nature of the adsorbent. A porous
hydroxide layer was formed on aluminum particles oxidized in a mixture with zeolite (Fig. 3b). The structure
of this layer consisted of a matrix of aluminum hydroxide aggregates formed as a result of the polynuclear
precipitation from solution; this structure was analo-

gous to the structure of a porous layer in the

Al(OH)3/Al composite [9]. The surface of aluminum
particles oxidized in the presence of -Al2O3 was
smoother. Pronounced contacts between aluminum and
adsorbent particles were observed, whose surface was
also smoothed. Evidently, the properties of the resulting solution significantly affected the morphology of
the precipitate.
Based on a stereological analysis of micrographs
taken at different magnifications, we also found that the
pore structure had a system of mutually intersecting
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HYDROTHERMAL SYNTHESIS OF POROUS Al2O3/Al METAL CERAMICS: IV.

channels formed by joined aluminum particles and particle aggregates. The porous skeleton of a ceramic composite had a corpuscular structure and contained two
dimensional spatial orientation systems: two types of
mutually intersecting macropores. Figure 5 demonstrates the bar diagrams of macropore-size distributions. The percentage of macropores depended on the
dispersion of adsorbent powder particles and on the
packing density of aggregates. Table 1 summarizes the
results of a study of the hydraulic properties of the
materials synthesized. The results of the study of
hydraulic characteristics (maximum and average
macropore diameters) are consistent with the data of
stereological studies. The pore size and permeability
coefficient correspond to porous materials prepared by
powder metallurgy [14].

%
30

Study of the Adsorption and Texture Characteristics

of the Synthesized Materials

20

A hysteresis loop over the entire region of rising isotherm is characteristic of the adsorptiondesorption of
benzene on the synthesized composites based on the
zeolites NaA, NaX, and NaY and -Al2O3 (Fig. 6).
After an initially gentle rise, the adsorption isotherms
passed at practically equal slopes with respect to the
axis of P/Ps, whereas an inflection point at P/Ps 0.4
0.6 and a sharp rise up to P/Ps = 1.0 were observed. At
the initial stage of the desorption of benzene, the isotherms decreased gently and then sharply at P/Ps 0.3
0.4 up to joining to the isotherm of adsorption. This
loop is typical of adsorbents with open capillaries with
approximately equal effective radii (for example, aluminosilicates). The shape of the isotherms of benzene
adsorptiondesorption on a series of samples (the
slopes of branches, the widths of hysteresis loops, and
the values of P/Ps before the beginning of hysteresis)
remained almost unchanged in samples with different
adsorbents. Consequently, the pore structures of the test
samples were of the same character. Sorption-active
components (zeolites and -Al2O3) were primarily
responsible for the sorption parameters of the samples
prepared. The sorption volume of a composite based on
zeolite NaA is greater than that of the parent zeolite.
This is because the pore diameter of zeolite NaA is
smaller than the diameter of a benzene molecule, and
the sorption volume of this composite depends on the
phase of Al2O3. Table 2 summarizes the adsorption and

15

283

(a)

25
20
15
10
5
0
20

40

60

80

100

120

(b)

25

10
5
0
40

80

120 160 200 240 280 320 360

d, m

Fig. 5. Bar diagrams of macropore-size distributions in

porous composites: (a) Al2O3/Al + -Al2O3 (-Al2O3/Al
ratio of 3 : 1) and (b) Al2O3/Al + zeolite NaY (zeolite fraction of 0.61 mm; NaY/Al ratio of 3 : 1).

texture characteristics of the porous composites synthesized based on powdered aluminum, zeolites, and
active aluminum oxide. Because the contribution of the
porous Al2O3/Al composite to the adsorption characteristics of composite ceramics is very small, the sorption
pore volumes and specific surface areas of composites
almost completely depend on the properties of the parent commercial adsorbents, the weight ratio between a
powdered adsorbent and aluminum powder, and the
grain size of sorption-active components. The contact
area between two phases decreased as the grain size of
sorption-active components was increased. This fact

Table 1. Hydraulic properties of the synthesized materials

Permeability coefficient
1013, m2

Maximum
pore diameter, m

Average pore
diameter, m

-Al2O3 + Al (3 : 1)

2.85.5

4177

2137.8

NaX + Al (3 : 1) (zeolite fraction of 0.30.5 mm)

5.66.6

5889

2638

Sample composition

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284

RATKO et al.
V, m3/g
0.40

(a)

(b)

(c)

(d)

(e)

(f)

0.35
0.30
0.25
0.20
0.15
0.10
0.05
0
0.40
0.35
0.30
0.25
0.20
0.15
0.10
0.05
0
0.40
0.35
0.30
0.25
0.20
0.15
0.10
0.05
0
0.40

(g)

(h)

0.35
0.30
0.25
0.20
0.15
0.10
0.05
0

0.2

0.4

0.6

0.8

1.0 0
P/Ps

0.2

0.4

0.6

0.8

1.0
P/Ps

Fig. 6. Isotherms of benzene adsorptiondesorption on pure adsorbents and porous composites at 25C: (a) NaY, (b) Al2O3/Al +
NaY (1 : 3), (c) NaX, (d) Al2O3/Al + NaX (1 : 3), (e) -Al2O3, (f) Al2O3/Al + -Al2O3 (1 : 3), (g) NaA, and (h) Al2O3/Al + NaA (1 : 2).
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HYDROTHERMAL SYNTHESIS OF POROUS Al2O3/Al METAL CERAMICS: IV.

285

Table 2. Adsorption and texture characteristics of composite materials

Composition
of materials

Adsorbent fraction,
mm

Sorption pore volume,

cm3/g

Specific surface area,

m2/g

Average pore radius,

nm

0.30.5
0.10.3
0.30.5
0.51.0
0.30.5
0.10.3
0.30.5
0.51.0
0.30.5
0.10.3
0.30.5
0.51.0
0.30.5
0.10.3
0.30.5
0.51.0

0.02
0.115
0.07
0.07
0.34
0.34
0.26
0.29
0.38
0.31
0.28
0.3
0.26
0.24
0.23
0.25

64
48
49

420
391
441
310
143
204
226

347
294
320

0.42*
3.6
2.9
2.85

1.55
1.33
1.3
2.45
4.3
2.75
2.65

1.4
1.6
1.6

NaA (parent)
NaA + Al
(2 : 1 by weight)
NaY (parent)
NaY + Al
(3 : 1 by weight)
-Al2O3 (parent)
Al2O3 + Al
(3 : 1 by weight)
NaX
NaX + Al
(3 : 1 by weight)

* Breck, D., Zeolite Molecular Sieves, New York: Wiley, 1974. Translated under the title Tseolitovye molekulyarnye sita, Moscow: Mir,
1976.

more largely affected the strength properties of composites rather than the texture properties.
Results of a Study of the Thermophysical and Strength
Properties of Synthesized Ceramics
Porous ceramics used as catalyst supports or the
capillary structures of heat-transfer devices should
exhibit high thermal conductivity. Porous materials
prepared with the use of powder metallurgy by sintering bulk or compacted powder metals (copper, bronze,
corrosion-resistant steel, nickel, and titanium) [14, 15],
as well as block supports, which were described previously [48], exhibit high thermal conductivities of
about 210 W m1 K1. However, they do not have a
developed system of sorption pores and a high specific surface area. In contrast, commercial adsorbents exhibit a developed pore structure; however,
their thermal conductivity and heat capacity are relatively low. Thus, the heat capacity of dry active carbon is 0.84 J g1 K1, and the thermal conductivity (at
30C) is 0.170.28 W m1 K1. The heat capacity of
silica gel is no higher than 0.92 J g1 K1, and the thermal conductivity (at 30C) is 0.2 W m1 K1 [16].
Figure 7 illustrates the results of the determination
of the thermal conductivity of the composite ceramics
synthesized based on zeolite NaY. For comparison, the
temperature dependence of the thermal conductivities
of the parent zeolite, the zeolite with a binder based on
polyaniline [17], the synthesized porous composite
(Fig. 3) containing powdered zeolite NaY with a partiKINETICS AND CATALYSIS

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cle size of 100300 m and aluminum powder (3 : 1 by

weight), and the porous Al2O3/Al composite are given
in the graph. The parent zeolite exhibited the lowest
thermal conductivity (<0.1 W m1 K1) over the test
temperature range. The addition of the polymer binder,
Thermal conductivity, W m1 1
0.8

0.6

0.4
2
0.2
1
0

50

100

150

200
T, C

Fig. 7. The temperature dependence of the thermal conductivity of porous materials: (1) NaY, (2) NaY with a polyaniline binding agent, (3) Al2O3/Al + NaY (1 : 3), and
(4) porous Al2O3/Al composite.

286

RATKO et al.

Heat capacity, J kg1 1

3

1400

1200

1
1000

800

1
2
3
0

50

100

150

200

250
,

Fig. 8. The temperature dependence of the heat capacity of

porous materials: (1) porous Al2O3/Al composite, (2) active
carbon, (3) porous Al2O3/Al composite + NaY (1 : 3).

which joined the particles of zeolite powder to form a

porous block, increased the thermal conductivity by a
factor of almost three. The porous material that consisted of zeolite and the porous Al2O3/Al composite
exhibited a much higher thermal conductivity. The thermal conductivity increased with the aluminum powder
content of the starting mixture of powdered components, and it was equal to 0.60.8 W m1 K1 for the
porous Al2O3/Al composite itself. The high thermal
conductivity of the ceramics synthesized was due to the
presence of isolated aluminum particles; an increase in
the concentration of these particles increases the thermal conductivity.
Figure 8 demonstrates the results of the determination of the temperature dependence of the specific heat
capacities of various porous materials: the porous
Al2O3/Al composite, active carbon, and the synthesized
porous material of zeolite NaY and aluminum powder
(3 : 1 by weight). Over the test temperature range, the
heat capacities of all the materials were higher than
1 J g1 K1, and they almost equally increased with
temperature. The composite consisting of the zeolite
and aluminum powder exhibited the highest heat capacity. The above graphics illustrate the averaged values of
heat capacities for a series of tests. Based on the data
shown in Fig. 8, we can conclude that up to 200C the
heat capacities of all the materials were approximately
equal, and the zeolite-based material exhibited a higher
heat capacity only at T > 200C.
The mechanical strength of the porous composites synthesized generally decreased from 4050 to 1520 MPa as
the particle size of zeolite powder was increased and
the weight content of aluminum was decreased. This
can be explained by the fact that the mechanical
strength depends on the number of contacts per unit
volume of a porous solid, all other factors being the
same. In the porous composite synthesized, aluminum

powder plays the role of a heat-conducting binding

material, and a decrease in the amount of this material
per unit volume decreased the mechanical strength.
We found experimentally that the formation of
porous composite ceramics occurs by a controlling
mechanism of hydroxide dissolutioncrystallization on
surfaces of negative curvature (the regions of contacts
between the parent adsorbent and aluminum particles).
As a result, a macroporous structure is formed because
of the formation of phase (crystallization) contacts
between adsorbent particles and aluminum particles as
a porous polycrystalline aggregate of primary aluminum hydroxide particles with the formation of a
mechanically strong porous solid (block). The
micropore structure of a block composite thus prepared
depends on the texture of parent adsorbents and on the
formation of compounds resulting from dissolution and
crystallization from aqueous solutions under hydrothermal conditions. The ultramacropore structure of
blocks is organized through gaps between the contacting particles of powdered parent components. A combination of powder metallurgy with the methods of colloid chemistry provides an opportunity to prepare
porous block ceramics with high gas permeability,
mechanical strength, and thermal conductivity and with
a polydisperse pore structure. Micropores and mesopores occurred in parent standard adsorbents; they were
also formed in the course of precipitation from solution, whereas ultramacropores 40250 m in diameter
were formed by gaps between the contacting particles
of parent powders. In terms of their properties, the
block porous materials synthesized occupied an intermediate place between commercial adsorbents and
powder metallurgical porous materials.
In main outward appearances, the synthesis of the
Al2O3/Al metalloceramic composite and highly porous
ceramics from powdered components is analogous to
the formation of a crystallization disperse structure in
the hydration hardening of mineral binding agents,
such as hemihydrate gypsum or calcium aluminosilicate and other cements, on their reaction with water
[18]. In the course of the dissolution of a disperse
phase, a new colloidal disperse system is formed, and
crystallization contacts between small crystals of a
sparingly soluble disperse phase are formed at the sites
of contacts. A rapid increase in the number of precipitate nuclei with the subsequent growth of these nuclei
results in the strengthening of contacts between sparingly soluble particles and in the formation of the
strength properties of the material. In this series of
papers, we reported on the synthesis of composite
ceramics with the use of aluminum powder with a particle size of ~20 m. Materials with a wide range of
properties for various purposes can be obtained by
changing the dispersity of aluminum and by controlling
its solubility.
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