Silicon (2023) 15:1085–1091
https://doi.org/10.1007/s12633-022-01745-0
ORIGINAL PAPER
Glass Formation in the MgO–B2O3–SiO2 System
Yu. S. Hordieiev1
· E. V. Karasik1 · A. V. Zaichuk1
Received: 29 December 2021 / Accepted: 6 February 2022 / Published online: 3 September 2022
© Springer Nature B.V. 2022
Abstract
The glass formation region in the MgO–B2O3–SiO2 system was determined by the conventional melt-quenching technique
at 1450 °C. The homogeneous transparent glasses were obtained in the central part of the magnesium borosilicate system
in the region between 40 and 60 mol% MgO content. The amorphous and crystalline phases were examined by means of
X-ray diffraction, differential thermal analysis, and Fourier-transform infrared spectroscopy. According to differential thermal analysis data, the glass transition temperature ranges between 645 and 705 °C, and the glass crystallization temperature
varies between 830 and 985 °C. The thermal stability of glasses decreases with the increase of MgO content. Some physical
characteristics (thermal expansion coefficient, density, molar volume, and volume resistivity) of the glass samples were
estimated as well. The thermal expansion coefficient, density, and molar volume of the MgO–B2O3–SiO2 glasses obtained
in this study ranged from 5.4 to 7.6 ppm/°С, 2.53 to 2.70 g/cm3, and 18.56 to 22.51 ­cm3/mol, respectively, depending on
the glass composition. Fourier transform infrared spectroscopy results showed that the network of glasses consists mainly
of ­BO3 and ­SiO4 structural units. These results may lead to the development of new materials with interesting applications
in diverse fields because of their particular structural and physicochemical properties.
Keywords Borosilicate glass · Glass formation · Thermal expansion · Thermal stability · Glass structure
1 Introduction
Borosilicate glasses have become important recently, from
both scientific and technological points of view, owing to
their unique properties and promising potential applications
in various fields [1]. Boron oxide is combined with silicon
oxide to reduce the melting temperature, viscosity and thermal expansion coefficient of the glass [2, 3]. The physical,
thermal and structural properties of borosilicate glasses can
be modified within a wide range by introducing oxides of
alkaline earth metals that modify the structure of boron [4].
Besides, alkaline earth oxides in borosilicate glasses improve
glass-forming capability and thermal stability [5]. Alkaline
earth borosilicate glasses and glass-ceramics are widely used
in instrument engineering and rocket production as heatresistant electrical insulating coatings [6–8], in the energy
sector as sealants in solid oxide fuel cells [9–11], and in the
* Yu. S. Hordieiev
yuriihordieiev@gmail.com
1
Department of Ceramics, Glass and Construction materials,
Ukrainian State University of Chemical Technology, 8
Gagarin Avenue, Dnipro 49005, Ukraine
production of heat-resistant and radio-transparent materials
for the aerospace and military applications [12–14].
Glasses in the MgO–B 2O 3–SiO 2 system with MgO
content of more than 30 mol% can be promising for solving these process tasks. The addition of magnesium oxide
improves the glass-forming capability, thermal stability and
dielectric properties of the glasses. The above system is a
relevant source for the synthesis of new materials that present value and, at the same time, specific properties such
as mechanical strength, thermal stability, radio-transparent,
high electrical and chemical resistance [15]. However, there
is no sufficient information in the technical literature with
regard to the conditions of glass formation and properties of
the magnesium borosilicate glasses, which is required for the
substantiation of their production technology and selection
of the optimal composition. Thus, this topic continues to be
an active area of research. Advances in the experimental and
computational study will better understand glass structure
and its relationship to physical properties, perhaps leading to
additional commercial and scientific opportunities [16, 17].
Understanding the thermal and structural behavior of
glasses is crucial for developing heat-resistant glasses for
advanced aerospace, military, and electronic applications.
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Silicon (2023) 15:1085–1091
Therefore, the aim of this study is to investigate the glassforming region in the MgO–B2O3–SiO2 system and to determine the thermal and structural properties of the obtained
glasses by DTA, X-ray diffraction and FTIR spectroscopies.
2 Materials and Methods
Glasses of the MgO–B2O3–SiO2 system were prepared by
the conventional melt-quenching technique. The chemical
compositions of the glasses are given in Table 1. The glass
batches were prepared by mixing high purity chemicals of
magnesium oxide, boric acid, and silicon dioxide in agate
mortar with a pestle to ensure complete homogeneity. The
homogeneous glass batches were melted in the alumina crucibles with the volume of 50 mL in an electric furnace with
silicon carbide heaters at the temperature of 1450 °С for
60 min. The homogeneous melts were quickly cast onto a
preheated stainless-steel mold to obtain glasses which were
then transferred into a muffle furnace preset to 600 °C.
According to their transparency, the resultant substances
were classified as glass, opaque, and sinter.
The glass transition temperature ­(Tg) and crystallization
temperature ­(Tc) were determined using a derivatograph
Q–1500D at a heating rate of 10 °C/min from room temperature to 1000 °C in an air atmosphere. The reference substance was alumina powder of high purity, and the temperature error was ±5 °C. The thermal stability of the samples
was evaluated using the different ΔT between the exothermic
effect of crystallization ­(Tс) and that for glass transition temperature ­Tg (ΔT = ­Tс-Tg). Higher values of ΔT indicate better
stability against crystallization [18].
Crystalline phases precipitated during heat treatment
were identified by X-ray diffractometer DRON-3М using
Co-Kα radiation in the 10 < 2Θ < 90 range.
The FTIR spectra of the glasses were recorded in the
1600–400 ­c m −1 region using the KBr pellet technique
(Thermo Nicolet Avatar 370 FTIR Spectrometer).
The thermal expansion coefficient (TEC) of the glasses
with a dimension of 5 × 5 × 50 mm was examined using a
dilatometer (Dilatometer1300 L, Italy) at a heating rate of
3 °C/min from 25 °C to 400 °C. The density of the glasses
was determined at room temperature by the Archimedes
principle using distilled water as the immersion liquid and
a digital balance of sensitivity 1­ 0−4 g. The weight of each
glass sample was measured three times, and an average was
taken to minimize the sources of error. The volume resistivity of MgO–B2O3–SiO2 glasses was measured on flat-parallel plates in a cell with graphite electrodes in the temperature
range of 100–400 °C at a heating rate of 5°/min using the
teraohmmeter Е6-13А.
3 Results and Discussion
Twenty-one glass samples with different compositions
were prepared to determine the glass formation range of the
MgO–B2O3–SiO2 system are shown in Fig. 1. Eleven glass
samples were visually obtained as homogenous transparent glasses. The transparent glasses were obtained in the
central part of the MgO–B2O3–SiO2 system from compositions containing 40–60 mol% MgO, 10–50 mol% B
­ 2O3, and
10–50 mol% ­SiO2. The amorphous nature of the glass samples was checked by X-ray diffraction study, which shows a
broad halo pattern typical for a fully glassy structure. Compositions containing 10 mol% ­B2O3 and above 50 mol%
MgO were not melted up to 1450 °C and only sintered products were obtained. Partially and fully opaque glass samples
with a heterogeneous structure were obtained from compositions outside the glass formation range (Fig. 1). Glass
Table 1 The chemical composition (mol %) and the values of the characteristic temperatures ­(Tg, ­Tc and ΔT), thermal expansion coefficient
(TEC), density (d), molar volume ­(Vm), volume resistivity (lgρ) of MgO–B2O3–SiO2 glasses
Glass samples No.
MgO
B2O3
SiO2
Tg, (°С)
Tc, (°С)
ΔT, (°С)
TEC, (ppm/°С)
d, (g/cm3)
Vm, ­(cm3/mol)
lgρ at
150°С
(Ohm·cm)
2
3
4
8
9
10
13
14
17
18
20
40
50
60
40
50
60
40
50
40
50
40
50
40
30
40
30
20
30
20
20
10
10
10
10
10
20
20
20
30
30
40
40
50
650
645
640
660
650
645
670
660
680
700
710
900
870
830
985
950
860
–
960
–
940
–
255
220
170
330
290
210
–
300
–
240
–
5.4
6.1
7.4
5.5
6.2
7.6
5.5
6.4
5.5
6.5
5.6
2.53
2.58
2.61
2.55
2.61
2.70
2.56
2.64
2.57
2.68
2.58
22.51
20.93
19.57
21.95
20.33
18.56
21.50
19.73
21.04
19.08
20.59
12.57
12.43
11.71
12.34
12.23
11.85
12.13
11.92
11.96
11.84
11.89
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Silicon (2023) 15:1085–1091
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Fig. 1 Compositions of the
glass samples and glass formation in the MgO–B2O3–SiO2
system: 1 transparent glass, 2
opaque glass, 3 partially opaque
glass, 4 sinter and 5 glass formation boundary
samples No.1 and No.7 showed a stable phase separation
region in the form of two different phases as opaque and
transparent.
According to data reported by Stolyarova et al. [19], the
glass of the MgO–B2O3–SiO2 system melted in the platinum crucible was obtained at the MgO content of up to
50 mol%. Expansion of the glass formation region in the
MgO–B2O3–SiO2 system up to 60 mol% MgO content in
the case of melting in the alumina crucibles is due to their
corrosion (Fig. 2). Corrosion of the alumina crucible by
molten glass leads to the leaching of a part of A
­ l2O3 from the
crucible material into the glass melt, which contributes to
the formation of glass with high MgO content. The alumina,
in this case, acts as a glass-forming oxide and enters the
glass network in the form of ­AlO4 tetrahedra. The aggressiveness of the glass batches and glass melt in relation to
the material of ceramic crucibles were also established in
the studies of glasses of the RO–B2O3–SiO2 (R = Ba; Ca;
Sr) system [20–22].
Differential thermal analysis (DTA) was employed to
determine the thermal behavior of the MgO–B2O3–SiO2
glasses. The DTA curves of the glass powder samples in
Fig. 2 Corrosion of the alumina
crucible by molten glass No.2
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the temperature range of 500–1000 °C are shown in Fig. 3,
and the thermal analysis values of the curves are given in
Table 1. The glass transition temperature, crystallization
temperature and thermal stability are essential characteristics of glass materials. According to the DTA data, all the
glass samples showed an endothermic change between 645
and 705 °C, which can be attributed to the glass transition
temperature. For constant MgO compositions, ­Tg values
showed a decrease with increasing ­B2O3 or decreasing ­SiO2
content, and this behavior is shown in Fig. 3 for 40 mol%
MgO-containing samples. The glass samples No.2 and No.8
have one sharp exothermic peak at 900 and 985 °C, respectively, indicating strong crystallization. The exothermic peak
shifts to higher temperatures with increasing S
­ iO2 content.
MgO–B2O3–SiO2 glasses showed glass thermal stability
values varying between 170 and 330 °C, indicating good
thermal stability of the glass samples. The thermal stability
of the studied glasses increases with the increase of S
­ iO2
content and decreases with the increase of MgO content.
Fig. 3 DTA curves of the glass powder samples: a No.2, b No.8, c
No.13, d No.17 and e No.20
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Silicon (2023) 15:1085–1091
In order to identify the crystalline phase corresponding
to each exothermic peak on DTA curves, the glass powder was heated above the crystallization temperature at the
heating rate of 5 °C/min and held at peak temperature for
2 hours. Leaching of A
­ l2O3 from the alumina crucibles into
the glass melt is confirmed by the X-ray phase analysis of
heat-treated glass samples No.2 and No.8 (Fig. 4), the glass
batches of which did not contain A
­ l2O3. As observed, werdingite ­(Mg2Al14Si4B4O37) is the only phase that crystallizes
in both heat-treated glass samples.
The changes in physicochemical properties of glasses are
closely related to their chemical composition and structure.
The variations in density and molar volume for all glasses
are listed in Table 1. The density of the MgO–B2O3–SiO2
glasses exhibits an inverse behavior to the molar volume
ranging from 2.53 g/cm3 to 2.70 g/cm3 and 22.51 ­cm3/
mol to 18.56 ­cm3/mol, respectively. The density of glasses
increased gradually with the increase of MgO content.
The probable role of MgO as a network modifier leads to
the breaking of Si–O–Si bonds and the formation of new
Si–O–Mg bonds in the glass network. This hypothesis is
confirmed by the regular decrease of the molar volume with
the increased MgO content. Decrease in ­Tg and increase in
thermal expansion coefficient suggest that the addition of
MgO results in a weakening of the glass network. Watts et al.
[23] suggested that the newly formed Si–O–Mg bonds have,
on average, a significantly lower bond strength with respect
to Si–O–Si bonds in the glass network, resulting in the
observed reduction in Tg. The replacement of ­SiO2 by ­B2O3
causes insignificant changes in the values of TEC and density, but​at the same time, causes a significant increase in the
volume resistivity and molar volume of MgO–B2O3–SiO2
glasses. At the temperature of 150°С, the volume resistivity
of glasses is in the range of ­1011–1012 Ohm·cm, indicating
their high electrical insulation properties.
Fourier-transform infrared (FTIR) spectroscopy is sensitive to the materials’ local structure, and it is quite useful for the elucidation of materials’ structural changes as a
function of composition [24]. For borosilicate glasses, the
analysis of FTIR is usually accomplished by determining
the changes of vibrational modes in frequency and intensity.
The influence of varying ­B2O3 content substituted for ­SiO2
on the structural properties of the MgO–B2O3–SiO2 glasses
was investigated by detecting their FTIR spectrum (Fig. 5)
in the range 1600–400 ­cm−1. The band intensity and position in the FTIR spectra of all glasses were fairly similar
and varied slightly. The main peaks are due to borate and
silicate groups which are present in higher mol % in the
sample. The peaks at 460 ­cm−1 and 510 ­cm−1 are mostly
associated with bending vibrations of Si–O–Si, Si–O–Mg
and Si–O–Al linkages, respectively [25–27]. The strong
absorption band centered around 700 ­cm−1 is ascribed to the
bending vibration of B–O–B in [­ BO3] [27–29]. The intensity
Silicon (2023) 15:1085–1091
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Fig. 4 X-ray diffraction patterns
of glass powders heat treated at
the crystallization temperature
of this band decreased distinctly with increasing of S
­ iO2
content. When the S
­ iO2 content was higher than 10 mol%,
two peaks located at 780 ­cm−1 and 800 ­cm−1 were found.
The absorption peak near 780 ­cm−1 belongs to the bending
vibration of Al–O–Al in [­ AlO4] [12, 28]. In addition, the
peak near 800 ­cm−1 may be related to the symmetric stretching vibration of Si–O–Si and Si–O–Al linkages [24, 29]. The
absorption peak observed at 1080 ­cm−1 corresponds to the
asymmetric stretching vibration of Si–O–Si in [­ SiO4] [12,
29]. The Si–O–Si stretching vibration band is increased with
an increase of the S
­ iO2 content. The absorption bands centered at 1280 ­cm−1 and 1420 ­cm−1 are due to the vibration
of the boroxol rings and the stretching vibrations of B–O–B
in ­[BO3] triangles, respectively [12, 27–31].
Considering the above analysis, we can conclude that
the structure of MgO–B2O3–SiO2 glasses is formed by a
network of B
­ O3 triangles and S
­ iO4 tetrahedra. The replacement of ­BO3 units by ­SiO4 units lead to an increase in the
glass transition temperatures and thermal stability of the
studied glasses since tetrahedral S
­ iO4 units strengthen the
network by increasing its dimensionality [32]. The literature
mentions that the glass transition temperature of an oxide
glass increases with bond strength and cross-link density of
the glass network [31, 32].
4 Conclusions
The glass formation region in the MgO–B2O3–SiO2 system was determined. The homogeneous transparent glasses
were obtained in the central part of magnesium borosilicate the system from compositions containing 40–60 mol%
­ iO2. The valMgO, 10–50 mol% B
­ 2O3, and 10–50 mol% S
ues of the thermal properties of the studied glasses in the
MgO–B2O3–SiO2 system varies over a wide range: thermal
expansion coefficient from 5.4 to 7.6 ppm/°С, glass transition temperature from 645 to 705 °C, thermal stability from
170 to 330 °C, depending on the glass composition. The
density of the MgO–B2O3–SiO2 glasses exhibits an inverse
behavior to the molar volume ranging from 2.53 g/cm3 to
2.70 g/cm3 and 22.51 ­cm3/mol to 18.56 ­cm3/mol, respectively. The main building units forming the glass network
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Silicon (2023) 15:1085–1091
Fig. 5 FTIR spectrum of glass
samples: a No.2, b No.8, c
No.13, d No.17 and e No.20
are ­BO3 (peak at 700, 1280, 1420 ­cm−1) and S
­ iO4 (peak at
460, 1080 ­cm−1). The replacement of B
­ O3 units by S
­ iO4
units increases the glass transition temperatures and thermal
stability of the studied glasses because tetrahedral S
­ iO4 units
strengthen the network by increasing its dimensionality.
Investigation of the physical properties of glasses showed
that the equimolar substitution of MgO by ­B2O3 + ­SiO2
increased the density values while decreasing the molar
volume. In addition, the decrease of the glass transition temperatures and thermal stability for all glass compositions
suggests that MgO acts as a network modifier weakening
of the glass structure. The results obtained in determinations of the physical, thermal and structural properties of
the studied glasses indicate that they can be recommended
for some purposes in aerospace or instrument engineering as
heat-resistant electrical insulating glass- and glass-ceramicto-metal seals and coatings.
Acknowledgments The authors gratefully acknowledge the financial
support from the Ministry of Education and Science of Ukraine (project
No. 0120 U101969).
Author Contributions Hordieiev Yu.S. wrote the manuscript, conceived and designed the experiments, performed experimental work;
Karasik E.V. assisted in experimental work; Zaichuk A.V. provided
the reagents and assisted in statistical analysis. All authors read and
approved the final manuscript.
13
Funding This work was supported by the Ministry of Education and
Science of Ukraine (project No. 0120 U101969).
Data Availability The data that support the findings of this study are
available from the corresponding author on reasonable request.
Declarations
The manuscript has not been published elsewhere and that it has not
been submitted simultaneously for publication elsewhere.
Ethics Approval Not applicable.
Consent to Participate Not applicable.
Consent for Publication Not applicable.
Competing Interests The authors declare that they have no conflict
of interest. The authors declare that they have no known competing
financial interests or personal relationships that could have influenced
the work reported in this paper.
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