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Advanced Sol-Silicate Paint

Article in Lecture Notes in Electrical Engineering · April 2020

DOI: 10.1007/978-3-030-42351-3_6

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Advanced Sol-Silicate Paint
Valentina Loganina , Yerkebulan Mazhitov , Roman Fediuk ,
Vatin Nikolai and Roman Timokhin

Abstract Deficiencies of silicate paints are revealed. Novel sol-silicate paint

obtained by mixing liquid glass and silica sol has been developed. The nominal
viscosity of the paintwork was determined using a VZ-4 viscometer. The relative
hardness of the coatings was determined using the M-3 pendulum device. The tensile
strength (cohesive strength) was determined on a tensile testing machine IR 5057-
50. Analysis of the IR spectra shows that the presence in the composition of the
polysilicate binder of various polymer silica provides increased durability of silicate
coatings. Dependence of the relative hardness of the films based on the polysilicate
solution on their thickness is calculated. The presence of polymer varieties of sil-
ica in the polysilicate binder was established, which provides increased durability
of silicate coatings. A correlation between the content of high-polymer fractions
of silicon-oxygen anions in the polysilicate solution and the tensile strength of the
films was revealed, which consists in the fact that with an increase in the content of
SiO2 , an increase in the tensile strength of the films is observed. Thus, in accordance
with its exploitation characteristics, the developed sol-silicate paint can be used for
decoration of both external and internal walls of buildings.

Keywords Paint · Painting · Coatings · Silicates · Pigments

V. Loganina · Y. Mazhitov
Department of Quality Management and Technology of Construction Production, Penza State
University of Architecture and Construction, 28 Germana Titova Street, Penza, Russian Federation
R. Fediuk (B) · R. Timokhin
Department of Hydrotechnics, Theory of Buildings and Structures, Far Eastern Federal
University, 8 Sukhanova Street, Vladivostok, Russian Federation
e-mail: [email protected]
V. Nikolai
Department of Construction of Buildings and Structures, Peter the Great St. Petersburg
Polytechnic University, 29 Politekhnicheskaya Street, St. Petersburg, Russian Federation

© Springer Nature Switzerland AG 2020 67

B. Anatolijs et al. (eds.), Proceedings of EECE 2019, Lecture Notes
in Civil Engineering 70, https://doi.org/10.1007/978-3-030-42351-3_6

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68 V. Loganina et al.

1 Introduction

Silicate paints are widely used for decoration of external and internal walls of build-
ings [1–4]. These paints made on the basis of liquid glass (potassium or sodium)
have a low cost, but they have a number of disadvantages, such as insufficient crack
resistance and water resistance [5–7].
The insufficient water resistance of silicate paints is due to the fact that liquid
glass itself is a highly soluble product and therefore is well washed out of paints. To
circumvent this drawback, substances (chalk, clay, infusorian clay, dolomite, etc.)
are added to the liquid glass to react with it to form insoluble silicic acid compounds
[8, 9]. It is advantageous to add these substances to water glass before painting so
that the reaction between water glass and the substances added to it occurs after the
paint layer is applied to the surface to be painted, i.e., in the paint film. However, the
need to observe the exact proportions and time of adding modifiers make the process
unstable and difficult to reproduce at the construction site [10, 11].
Increased crack resistance of silicate paints occurs because their film is a stony
formation with a complete lack of elasticity—a property so characteristic of oil
paint films [12, 13]. This circumstance often leads to the fact that upon changes
in the volume of a colored object due to a change in its moisture content, rather
characteristic cracks for silicate paints are formed on the film rather quickly and
gradually increase. These cracks sometimes also form in the film either because of
its usual drying out or because of reactions in it, entailing compression of it. To
eliminate this drawback of silicate paints, glue, starch, rubber, and other solutions
are added to them. Some excess liquid glass in the paint is also useful. However, as in
the cases with other additives described above, it is difficult to guarantee the desired
effect [14, 15].
In addition, silicate paint is a two-packing (in one package a mixture of pigments,
hardener, in the second package—liquid glass). However, liquid glass needs to be
diluted to a density of 1.15, which under construction conditions are difficult to
control.
Given the increasing demands on the quality of finishes and the fact that coatings
based on silicate paints have insufficient durability during operation, it is urgent to
develop methods for modifying liquid glass, which will make it possible to obtain
coatings with higher protective and decorative properties. As liquid glass modifiers,
for example, silicon-containing compounds are used [16]. So, in the case of using
silicon oxide as a liquid glass modifier, the modification process is carried out either
by mixing liquid potassium or sodium glass with silicon dioxide or by mixing liquid
sodium glass with tetraethoxysilane. In particular, the process of modifying liquid
glass with silicon dioxide is carried out at an elevated temperature, of the order of
60–80 °C, and with stirring [17].
The open literature presents compositions of silicate paint, including sodium liq-
uid glass, ground granulated electrothermophosphorus slag, ground cullet, ground
white wollastonite and pigments, and plasticized polyvinyl acetate emulsion has been

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Advanced Sol-Silicate Paint 69

Table 1 Silica sol characteristics

Characteristic KO-168 PVAC
pH 9–10.8 9–10.6
Mass concentration of silica (g/L) 220–237 329–362
Mass concentration of sodium oxide (g/L) 3–7 2.5–6.5
Silicate module 50–90 55–100
Specific surface area (m2 /kg) 220–370 220–300

proposed as a modifier [18–20]. However, coatings based on these compositions have

low-level protective properties due to the high porosity of the coatings [21–25].
The aim of the work is to study the possibility of using silica sol as a liquid glass
modifier to increase the durability of silicate paints.

2 Materials and Methods

2.1 Materials

Liquid glass with a module M = 2.78 was used in research. Microcalcite (MK-2, Rus-
sia) and talc grade (MT-GSHM, Russia) were used as filler. Nanosil 20 and Nanosil
30 silicic acid sols manufactured by Promsteklotsentr (Russia), the characteristics of
which are given in Table 1, were used as liquid glass modifiers.
The following pigments were used: rutile titanium dioxide Crimea CR-02
(Crimean titanium, Russia); ocher (Russia); saturnine red (Russia); chromium oxide
Cr2 O3 (OKHP-1, Russia).

2.2 Experimental Methods

The physicochemical properties of the starting components, as well as the rheological

and physicomechanical characteristics of the coatings, were evaluated in accordance
with current standards.
The mass fraction of silicon dioxide was determined by the photocolorimetric
molybdate method.
The nominal viscosity of the paintwork was determined using a VZ-4 viscometer
(Zapadpribor, Russia). The method is based on determining the expiration time (in
seconds) of 100 ml of polymer solution through a nozzle with a diameter of 4 mm.
The dynamic viscosity of coatings was determined by the Stokes method. To do
this, the test liquid was poured into a measuring cylinder, a metal ball of known
density ρ b and radius r was brought to the surface and lowered (without a jolt). As

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70 V. Loganina et al.

soon as the movement of the ball becomes uniform, the stopwatch was turned on and
the travel time t of the ball for way L was determined. The viscosity of the liquid
was found by the formula:

2 2 (ρb − ρl ) · t
η= gr (1)
9 L

where g—gravity acceleration (m/s2 ); ρ l —paint density (kg/m3 ).

The surface tension was determined by the drop counting method (stalagmometric
method). From a special capillary-stalagmometer squeeze the equal volumes of water
of the investigated fluid or solution. The number of droplets formed from the same
volume of liquid is proportional to the density of this liquid and inversely proportional
to surface tension. Drops were counted five times, and the arithmetic mean was taken.
Distilled water with a temperature of 20 °C with a density of 0.9982 g/cm3 and a
surface tension of 72.8 mN/m was used as a reference liquid.
The relative hardness of the coatings was determined using the M-3 pendulum
device (Zapadpribor, Russia). Determination of the hardness of a coating by the M-3
pendulum device is based on determining the ratio of the decay time of the oscillations
of the pendulum mounted on the paintwork to the decay time of the same pendulum
mounted on the glass plate.
The method for determining the spreadability was to apply five parallel strips
of paint and determine the degree of spreadability by the number of stuck together
strips. Paint with working viscosity was applied to a glass plate 200 × 100 × 1.2 mm
in size. The degree of spreading of five parallel strips was assessed using a ten-point
“spreadability” scale.
The adhesion work W a of the paint composition in the cement substrate was
calculated using the Dupre–Young thermodynamic equation.
The equilibrium wetting angle was determined on a KRUSS DSA-30 device (Ger-
many). The energy state was determined by the OWRK method (Ougs, Wendt, Rabel,
and Kjelbe method), which took into account the polar and dispersion components
of the material.
Tests for freeze-thaw resistance of coatings passed in the following mode. The
samples of cement–sand mortar stained with the proposed composition, after satura-
tion in water, were placed in a freezer with a temperature of −15 °C and kept for 4 h,
after which they were placed in water with a temperature of 18–20 °C for 4 h (one
cycle). It considered the number of cycles before the loss of the exploitation ability
of the coating.
The tensile strength (cohesive strength) was determined on a tensile testing
machine IR 5057-50 (Russia). The method is based on the stretching of the test
sample with a size of 10 × 50 mm to rupture at a strain rate of 1 mm/min. The
film samples were fixed in the clamps of the tensile testing machine so that its lon-
gitudinal axis was located in the direction of tension, and the applied forces acted
uniformly over the entire cross section of the sample. The tests were carried out at
an air temperature of 20 ± 2 °C and relative humidity of 64%.

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Advanced Sol-Silicate Paint 71

Drying time was determined by the time during which the finishing layer turns
into a layer with the desired degree of drying.

3 Results and Discussion

3.1 Mix Design

During the study, the influence of the density of liquid glass and the temperature of
the addition of silica sol on the gelation process of liquid glass was diluted with water
to obtain different densities. Then, silica sol was added in a ratio of 1:0.1; 1:0.15;
1:0.2; 1:0.3 with continuous stirring at a temperature of 80 °C for 1 h.
Figure 1 shows the pH dependence of solutions for various concentrations of
silicic acid sol. It was found that with an increase in the amount of silicic acid sol
added (increase in silicate module), a decrease in the pH of solutions is observed at
a constant alkali concentration. So, with a sol content of silicic acid in an amount
of 5% by weight of potassium liquid glass, the pH is 11.4–12.4, and with a content
of sol of silicic acid in an amount of 15%, pH = 11.0–12.1, while as in the control
composition (without adding sol)—pH = 12.7. Similar patterns are characteristic of
sodium liquid glass too.

Fig. 1 Kinetics of pH change in silica solutions: 1—potassium liquid glass; 2—potassium liquid
glass + 5% Nanosil 20; 3—potassium liquid glass + 10% Nanosil 20; 4—potassium liquid glass
+ 15% Nanosil 20; 5—sodium liquid glass; 6—sodium liquid glass + 5% Nanosil 20; 7—sodium
liquid glass + 10% Nanosil 20; 8—sodium liquid glass + 15% Nanosil 20

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Fig. 2 Change in viscosity of sodium polysilicate solution depending on the content of silica sol.
The circles indicate gelation points. 1—after preparing; 2—after 1 day; 3—after 3 days; 4—after
5 days; 5—after 7 days

The addition of a silicic acid sol leads to a change in the viscosity of the solutions,
and at the initial stage, the higher the content of silicic acid sol, the significant decrease
in viscosity is observed (Fig. 2).
Table 2 shows the effect of the addition of silicic acid sol on the rheological
properties of potassium liquid glass.

3.2 Silicate Content of the Developed Compositions

Table 3 lists the effect of the addition of Nanosil 20 silicic acid sol on the change in
the silicate module of sodium liquid glass.
Thus, the use of sol in the amount of 15–30% by weight of liquid glass with a
module of M = 2.78 allows to get polysilicate solutions with a module of M = 4.25–
5.29. It was found that the addition of sol (increase in silicate modulus) contributes
to an increase in the fraction of high-polymer fractions of silicon-oxygen anions, and
with an increase in the sol content, the fraction of the polymer form of silica increases.
So, when adding Nanosil 20 silicic acid sol in an amount of 5% by weight of sodium
liquid glass, the content of the polymeric form of γ-SiO2 silica increases to 5.34%, in

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Table 2 Effect of the addition of silicic acid sol on the rheological properties of potassium liquid
glass
Liquid glass Sol content Density Viscosity (s) Dynamic Kinematic
+ silicic acid (%) (kg/m3 ) viscosity viscosity
sol (mPa s) (m2 /s ×
10−6 )
Liquid glass – 1348 8.72 1576.0 1169.1
Nanosil 20
Solution 1 5 1333 7.98 1426.8 1070.3
Solution 2 10 1325 7.74 1375.6 1038.2
Solution 3 15 1316 7.56 1334.5 1014.0
Nanosil 30
Solution 1 5 1340 8.09 1454.1 1085.1
Solution 2 10 1331 7.69 1372.9 1031.5
Solution 3 15 1325 7.71 1371.3 1034.9

Table 3 Effect of the addition of Nanosil 20 silicic acid sol on the change in the silicate module
of sodium liquid glass
Mix ID Composition Name of indicators
Silicate module Viscosity (s)
1 Liquid glass with density 1.2 g/cm3 2.78 7.75
2 Liquid glass with density 1.2 g/cm3 + 10% sol 3.30 7.21
3 Liquid glass with density 1.2 g/cm3 + 20% sol 4.60 7.55
4 Liquid glass with density 1.2 g/cm3 + 30% sol 5.29 7.70
5 Liquid glass with density 1.3 g/cm3 + 10% sol 3.86 7.50
6 Liquid glass with density 1.3 g/cm3 + 15% sol 4.25 7.50
7 Liquid glass with density 1.3 g/cm3 + 30% sol 4.80 7.40
8 Liquid glass with density 1.46 g/cm3 + 5% aerosil 3.13 –

an amount of 15–12.04%, while in the control composition (without sol additives)—

2.78%. In the potassium polysilicate solution, the content of the polymeric form of
silica γ-SiO2 is 19.93% with a sol content of 15% (Table 4).
The dependence of the silica content of α-SiO2 at the early stages of the interaction
of the sol with liquid glass is extreme. The maximum content of α-SiO2 is observed
after 60 min, depending on the type of water glass and the amount of sol introduced.
So, after 60 min, the content of α-SiO2 silica in the sodium polysilicate solution is
18.54% at the content of 5% sol, and in the potassium polysilicate solution is 6.97%
at the content of 5% sol.
When potassium water glass is mixed with sol, the formation of α-SiO2 at the
initial stage proceeds more slowly compared to the sodium water glass, and their

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74 V. Loganina et al.

Table 4 Changes in the composition of liquid glass solutions containing Nanosil 20 silicic acid sol
Sol Sodium liquid glass Potassium liquid glass
content Total SiO2 α-SiO2 + γ-SiO2 Total SiO2 α-SiO2 + γ-SiO2
(%) content β-SiO2 content content β-SiO2 content
(%) content (%) (%) content (%)
(%) (%)
0 23.72 20.94 2.78 21.90 19.39 2.51
5 25.63 20.28 5.35 27.71 18.61 9.10
10 27.02 19.80 7.22 31.39 17.71 13.68
15 30.57 18.53 12.04 34.93 15.00 19.93

final content after 360 min is lower than for sodium: 15.68% and 6.74%, respectively
(when the content of sol in the amount of 5%).
When liquid glass is mixed with silica sol due to the high alkalinity of the medium
(pH = 10.7–12.4), a high dissolution rate of colloidal SiO2 particles is ensured. The
resulting low-polymer silica in solution exists in the form of residues of low-polymer
and oligomeric polysilicic acids. As a result, alkalinity decreases and stabilizes in
the range of pH 10.3–11.4 depending on the sol content. Obviously, the participa-
tion of OH− ions in the process of depolymerization of colloidal SiO2 is partially
compensated by the release of hydroxide ions in the hydrolysis reaction and during
the condensation of silicic acid residues as they accumulate in the solution. In this
regard, the rate of dissolution of particles becomes much lower; however, the process
of dissolution gradually continues.
When studying the state of silicic acid in polysilicate solutions depending on the
sol content, it was found that an increase in the sol content contributes to an increase
in the proportion of high-polymer fractions of silicon-oxygen anions. So, with a
sol content of Nanosil 20 in a potassium polysilicate solution in an amount of 5%,
the content of high-polymer fractions increases to 7.1% and with a sol content of
15%, up to 19.95%. Replacing the sol of Nanosil 20 with Nanosil 30 contributes to
an increase in the proportion of the fraction of high-polymer fractions to 22.01%.
Similar patterns are characteristic of sodium liquid glass.

3.3 IR Spectra Results

Figure 3 shows the IR spectra of multiple violations of the total internal reflection of
the silicic acid sol Nanosil 20 and Nanosil 30 in the spectral range 750–4350 cm−1 .
The IR spectra of the studied sols Nanosil 20 and Nanosil 30 are almost identical,
which indicates a close qualitative composition. The studied sols Nanosil 20 and
Nanosil 30 have a number of characteristic absorption bands that correspond to
vibrations of Si–O–Si bonds in the spectral range 1000–1250 cm−1 . There is a deep
absorption band with a minimum transmission at 1114–1134 cm−1 , associated with

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Advanced Sol-Silicate Paint 75

Fig. 3 IR spectra of Nanosil 20 (1) and Nanosil 30 (2) sols

longitudinal, transverse, and mixed vibrations of Si–O–Si bonds. The absorption

peak at 966–972 cm−1 corresponds to stretching vibrations of Si–OH bonds. There
are wide reflection bands with maxima of 1655–1666 cm−1 , which correspond to
stretching and deformation vibrations of water molecules. In the spectral range 1000–
1250 cm−1 , an increase in the fraction of IR radiation passing through the Nanosil
20 sol is observed. This is explained by a decrease in the mass fraction of silicon
hydroxide, which is typical for Nanosil 20. In the spectral range 3277–3765 cm−1 ,
which corresponds to stretching vibrations OH bonds, there is a slight decrease in
the proportion of infrared radiation passing through the Nanosil 20 sol, which is
explained by an increase in the content of H2 O in the composition of the sol.
When analyzing the IR spectra of liquid glass and a polysilicate solution, absorp-
tion bands characteristics of liquid glass were found that correspond to vibrations of
the Si–O–Si groups (1084 cm−1 ), H–O–H (1645 cm−1 ) and vibrations of the –OH
groups of water (several bands in the interval 3273–3670 cm−1 ) (Fig. 4, curve 1).

Fig. 4 IR spectra of potassium water glass (1) and potassium polysilicate solution (2) with a sol
content of Nanosil 30 in an amount of 15%

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76 V. Loganina et al.

Reflections in the region of 980–880 cm−1 (963 and 969 cm−1 in Fig. 4) characterize
the Si–OH stretching vibrations of three types of hydroxyls.
Analysis of the IR spectra shows that the polysilicate solution contains water.
This is indicated by wide reflection bands with maxima at 3300 and 3688 cm−1 and
bands with maxima at 1640 cm−1 , which correspond to stretching and deformation
vibrations of water molecules. The deepening of the 1111 cm−1 band corresponds to
the vibrations of Si–O–Si. A shift of the band toward higher frequencies compared
with liquid glass indicates a greater degree of polymerization. The reflection bands
with maxima of 978–900 cm−1 correspond to the hydroxyl vibrations in the Si–O–H
groups, which are obviously caused by the polycondensation of hydrated ions HSiO4
and H3 SiO4 . Absorption bands are recorded at 1064, 789 cm−1 , which correspond to
the vibrations of the Si–O and Si–O–Si bonds. Thus, the conducted studies indicate
the complex nature of the composition of the polysilicate solution. The presence in the
composition of the polysilicate binder of various polymer silica provides increased
durability of silicate coatings.

3.4 Polysilicate Binder Film Curing Kinetics

It was revealed that films based on developed polysilicate solutions are characterized
by faster curing. Figure 5 shows the kinetics of curing films, characterized by a

Fig. 5 Change in time of the relative hardness of films based on polysilicate solutions: 1—potassium
liquid glass; 2—potassium liquid glass + 5% Nanosil 20; 3—potassium water glass + 10% Nanosil
20; 4—potassium water glass + 15% Nanosil 20

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Fig. 6 Dependence of tensile strength of films based on potassium polysilicate solution on the
content of silicic acid in the polymer form of γ-SiO2

change in relative hardness. At the age of 24 h, the relative hardness of the film
based on the control composition is 0.28 and when Nanosil 20 sol is added to the
composition in the amount of 5, 10, 15% by weight of liquid glass, respectively, 0.38,
0.43, and 0.47. The curing process occurs within 7 days.
Figure 6 shows that there is a correlation between the content of γ-SiO2 in the
polysilicate solution and the tensile strength of the films, namely with an increase in
the silica content in the form γ-SiO2 polymer form, an increase in the tensile strength
of the films is observed.
According to the obtained experimental data, with an increase in the thickness of
the polymer coating from 0.1 to 0.3 mm, the relative hardness decreases from 0.48 to
0.6 MPa. Dependence of the relative hardness of the films based on the polysilicate
solution on their thickness is calculated and has the form:

y = 0.983 − 3.333x

The rather high tensile strength indices can be explained by the increase in the
proportion of high-polymer fractions of silicon-oxygen anions in the structure of a
polysilicate binder compared to liquid glass.

4 Conclusions

Novel polysilicate solutions obtained by mixing liquid glass and sol of silicic acid
are proposed as a binder in the manufacture of silicate paints. It has been established
that the addition of a silica sol into liquid glass contributes to an increase in the
proportion of high-polymer fractions of silicon-oxygen anions. It has been revealed

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78 V. Loganina et al.

that the dependence of the silica content in the monomeric form at the early stages
of the interaction of a silicic acid sol with liquid glass is extreme. It is shown that
when potassium water glass is mixed with silica sol, the formation of silica in the
monomeric form at the initial stage proceeds more slowly compared to the sodium
water glass.
Using IR spectroscopy, a band shift corresponding to Si–O–Si vibrations to an
area of higher frequencies compared to liquid glass was revealed, which indicates
a greater degree of polymerization of silica. The presence of polymer varieties of
silica in the polysilicate binder was established, which provides increased durability
of silicate coatings.
It was found that the addition of a silicic acid sol leads to an increase in the silicate
modulus and contributes to an increase in the fraction of high-polymer fractions of
silicon-oxygen anions. It is shown that coatings based on polysilicate solutions are
characterized by faster curing. A correlation between the content of high-polymer
fractions of silicon-oxygen anions in the polysilicate solution and the tensile strength
of the films was revealed, which consists in the fact that with an increase in the content
of SiO2 , an increase in the tensile strength of the films is observed.

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