Ceramics International 45 (2019) 22813–22820

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Ceramics International
journal homepage: www.elsevier.com/locate/ceramint

Effect of ZrSiO4 addition on sintering and selected physicochemical T

parameters of glass-ceramic materials from the SiO2-Al2O3-Na2O-K2O-CaO-
MgO system in the presence of barium oxide
Karolina Kaczmarczyk∗, Janusz Partyka
AGH University of Science and Technology, Faculty of Materials Science and Ceramics, Department of Ceramics and Refractory Materials, Cracow, Poland

ARTICLE INFO ABSTRACT

Keywords: The aim of this research is to show the effect of zirconium silicate addition on sintering and physicochemical
Glass-ceramic properties of glass-ceramic materials from the SiO2–Al2O3–Na2O–K2O–CaO–MgO–BaO system. This paper pre-
Sintering sents the results of the most important techniques used to understand the sintering process, i.e. thermal dif-
Microstructure ferential analysis, dilatometry measurements and hot-stage microscopy. Additionally, the following techniques
have been used: X-ray diffraction (XRD) and scanning electron microscopy with a micro-analyser (SEM-EDS),
and in order to obtain surface physicochemical properties: laser confocal microscopy, glossmetry, and spec-
trophotometry. By changing the initial composition and thermal treatment of glass-ceramic materials it is
possible to shape parameters of final products which leads to obtaining a great variety of applications.

1. Introduction formation of ZrSiO4 cluster, which happens especially in raw glazes,

Glass-ceramic materials have a wider variety of applications due to
the possibility of shaping their physical and chemical properties [1,2].
To produce glass-ceramic materials first the initial oxide composition
and then the thermal treatment are needed because both they de-
termine the final phase composition, quantity of the crystalline phase,
microstructure, and chemical composition of the glassy phase, which
finally allow us to obtain materials with different surface smoothness,
gloss, color, thermal expansion coefficient, dielectric constant, re-
sistance to fracture toughness and also chemical resistance [1-4]. Zir-
conium silicate (ZrSiO4) is commonly used in ceramic glazes as an
opacifier because of its high index of refraction (1,96) [5,6]. Moreover,
zirconium silicate crystals provide excellent mechanical and chemical
resistance, but it should be noted that the properties of the final product
are impacted by such parameters as amount, size, shape, and dis-
tribution of crystals. The studies on the impact of the size of ZrSiO4
crystals on properties of glazes have shown that the glazes with smaller-
sized zirconium silicate crystals are characterized by higher whiteness
and gloss but also have the increased roughness due to the protrusion of
crystals on the surface [7]. The phenomenon of crystallinity on the
surface may not lead to the decrease of surface smoothness, the degree
of crystallinity also is not a crucial matter, and the most important
parameter is morphology of the crystals [8]. The investigations on the
role of the distribution of crystal phase in glazes have shown that the
results in a decrease of whiteness and gloss [9]. The formation of crystal
clusters is caused by the release of gas products from the decomposition
of raw materials, and this phenomenon appears much more easily by
lowering the viscosity of the firing material [10,11]. The described
phenomena prove how many aspects are concerned on the way to form
final properties of the material. Additionally, the presence of BaO is
another factor which has an influence on the properties of the material.
Barium oxide is considered to be an active fluxing agent but only in the
presence of alkaline metal oxides and when the temperature of 1250 °C
is reached [15-17]. It might be applied in a maximum temperature
range, used in the ceramic technology because of high durability in the
liquid aluminosilicate alloy. The addition of BaO to the composition of
glass-ceramic materials might increase high-temperature viscosity and
this increase has a good influence on surface gloss and also increases
mechanical durability and chemical resistance. In the quantities above
20 wt %, it is not bound entirely in the oxygen-aluminium-silicon lattice
of the glassy phase thus it might be washed-out of the structure [15-17].
2. Experimental procedure
The presented research results concern the influence of various
quantities of zirconium silicate especially with an emphasis on sintering
but also on selected physicochemical parameters of glass-crystalline
materials from the SiO2–Al2O3–Na2O–K2O–CaO–MgO–BaO system.

*
Corresponding author.
E-mail address: karolina.kaczmarczyk@agh.edu.pl (K. Kaczmarczyk).

https://doi.org/10.1016/j.ceramint.2019.07.323
Received 9 May 2019; Received in revised form 22 July 2019; Accepted 29 July 2019
Available online 30 July 2019
0272-8842/ © 2019 Elsevier Ltd and Techna Group S.r.l. All rights reserved.
K. Kaczmarczyk and J. Partyka Ceramics International 45 (2019) 22813–22820

Table 1 Table 1. The first step was to mill each batch using a planetary ball mill
Simplified oxide molar compositions of examined materials after firing. during the equal time of 40 min. After drying raw powder was used to
Material SiO2/Al2O3 Na2O K2O CaO MgO BaO ZrO2 press round-shape samples of 60 mm diameter and 7 mm thickness
under the pressure of 30 MPa. The pressed samples were fired in a
GC_1 6,69 5,33 2,29 4,91 5,32 2,14 – single cycle at three different temperatures of 1190, 1200, and 1210 °C
GC_1 + 7,5% ZrSiO4 6,76 5,03 2,21 4,67 4,73 2,18 2,37
in the laboratory electric furnace. Heating to the maximum temperature
GC_1 + 15% ZrSiO4 7,09 4,86 2,08 4,53 4,57 2,48 4,89
was carried out at a constant rate of 3°/min. The samples were kept for
15 min at the maximum temperature, cooling was carried out at a rate
Table 2 of 15°/min. The analyses of sintering and pyroplastic deformation were
Characteristic temperatures of examined materials: DL – dilatometric, HSM – performed on unfired materials. Using the Misura® FLEX-ODLT optical
hot-stage microscopy. dilatometer, the dilatometric characteristic temperatures, transition
and softening, were determined whereas, using the HSM Misura® 3 M
Material Transition DL Softening DL Half-sphere HSM
hot-stage temperature microscope, half-sphere temperatures were de-
Temperature [°C] termined, with a constant heating rate of 10°/min. The determined
characteristic temperatures were used to calculate the viscosity of
GC_1 903 1008 1267
materials during their firing. The calculations were performed by the
GC_1 + 7,5% ZrSiO4 907 1056 1272
interval between GC_1 4 48 5
hot-stage temperature microscope software, which, on the basis of the
GC_1 + 15% ZrSiO4 901 1041 1288 Vogel-Fulcher-Tamman (VFT) equation, sets waveforms of a viscosity
interval between GC_1 -2 33 21 logarithm as a function of temperature. In addition, using the Netzsch
STA 449 F3 Jupiter, thermal differential analyses DTA were performed,
the measurements were carried out while heating the samples to
1190 °C at a rate of 10°/min and cooling at the same rate. Chemical and
phase analyses were carried out on the fired samples ground to a
powder with grain sizes lower than 63 μm. Chemical compositions were
examined using a wavelength dispersive X-ray fluorescence (WDXRF)
spectrometer AxiosmAX, Phillips-PANanalytical. Phase compositions
were determined by X-ray diffraction XRD using the PANalytical X'Pert
diffractometer. The measurements were carried out with a scanning
range 10–90° (2θ) at a scanning rate of 0,05° 2θ/2s. The surface ob-
servations were conducted on the surfaces of fired samples using the
NOVA NANO SEM 200 scanning electron microscope with an EDS X-ray
chemical microanalyser, supplied by EDAX.
After firing the examined materials were also used to measure
roughness, gloss and surface whiteness. The measurements were carried
out ten times for all samples. The surface roughness was determined
using the Olympus Olympus LEXT OLS4000 laser confocal microscopy,
by means of examining the Ra parameter, denoting the arithmetic
average deviation of the roughness profile. Gloss was measured using
the Elcometer 406L-2060 glossmeter, 60° geometry was used. The
surface whiteness was determined in the CIELab system by the L* a* b*
Fig. 1. Curves of a logarithm of viscosity versus temperature of examined coordinate values with the Konica Minolta CM 700D spectro-
materials. photometer.

Those parameters were measured at three different firing temperatures 3. Results and discussion
of 1190, 1200 and 1210 °C, which was associated with 15, 18, 20%
degrees of sintering of the samples. Both temperatures and degrees of Table 1 presents the results of chemical analyses of the obtained
sintering are optimized for a potential application. materials after firing. According to the assumptions – changes in the
The measurements were carried out on the primary material examined parameters are related to various quantities of zirconium
without the addition of zirconium silicate and on the materials with silicate and further to the firing temperature.
7,5 wt % and 15 wt % addition of this material. The raw materials
which were used in the studies are as follows: barium carbonate (BaCO3
3.1. Sintering process, viscosity
supplied by Avantor Poland), talcum from Luzenac, chalk (K-45 sup-
plied by PIOTROWICE II), potassium feldspar (Quantum supplied by
The influence of the addition of zirconium silicate on the char-
Sibelco), nepheline syenite (Spectrum N-45 supplied by Sibelco), kaolin
acteristic temperatures was determined as the first step. The results of
(KOC, SURMIN), quartz (MK40, originating from the SKSM Sobótka),
measurements of transition and softening temperatures (optical dilat-
zirconium silicate (Zircosil supplied by Endeca Ceramics). Simplified
ometer) and half-sphere (hot-stage temperature microscope) are shown
oxide mass compositions of the examined materials are presented in
in Table 2. Additionally, temperature intervals for the varying content

Table 3
Phase composition of examined materials.
Material 1190 °C 1200 °C 1210 °C

GC_1 Hyalophane quartz Hyalophane quartz Hyalophane quartz

GC_1 + 7,5% ZrSiO4 zirconium silicate hyalophane quartz zirconium silicate hyalophane quartz zirconium silicate hyalophane quartz
GC_1 + 15% ZrSiO4 zirconium silicate hyalophane quartz zirconium silicate hyalophane quartz zirconium silicate hyalophane quartz

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Table 4
SEM micrographs of materials.
ZrSiO4 content 1190 °C 1200 °C 1210 °C

0 wt %

7,5 wt %

15 wt %

Table 5 to determine the dependence graph of the logarithm of viscosity as a

Logarithm of viscosity, roughness, gloss (60°) and whiteness (L*,a*,b*) values function of temperature. The Vogel-Fulcher-Tammann (VFT) equation
of examined materials. was used for these calculations (VFT) [12]:
Parameter Firing GC_1 GC_1 + 7,5% GC_1 + 15%
Log ν = A + B/(T-T0)
temperature ZrSiO4 ZrSiO4
[°C] where A, B and T0 are constants.
log ν [dPa s] 1190 6,10 7,02 6,96
Graphically, the equation describes the dependence curve of log ν in
1200 5,90 6,75 6,72 relation to 1/(T-T0). Constant A is the intersection with the ordinate
1210 5,69 6,46 6,48 axis, and B the inclination angle, T0 is the empirical constant that aims
Ra [μm] 1190 0,991 1,483 1,170 to linearize the graph. In order to estimate the above constants for a
± 0,100 ± 0,140 ± 0,102
particular system, three reference temperatures should be used: tem-
1200 1,471 1,142 1,056
± 0,071 ± 0,097 ± 0,135 perature of transition, dilatometric softening and half-sphere, for which
1210 1,065 0,733 0,526 the VFT equation assumes the following viscosities: 1012, 109,25,
± 0,099 ± 0,069 ± 0,063 103,55 Pa s [12]. The results which show viscosity expressed in the
Gloss [%] 1190 12,91 5,67 3,31 graphs by the logarithm of viscosity are presented in Fig. 1. The addi-
1200 12,44 6,86 3,76
1210 19,37 16,35 9,62
tion of zirconium silicate significantly changes the character of the
Whitness L* 1190 87,03 92,41 94,03 curve waveforms, which may result from the increase in the difference
a* 0,01 0,22 0,15 between the transition temperature and the dilatometric softening
b* 7,16 6,07 4,93 temperature observed for the samples containing ZrSiO4, while transi-
L* 1200 85,70 92,70 93,82
tion temperatures of all materials are similar, and, in the case of half-
a* -0,01 0,19 0,2
b* 7,02 5,84 4,89 sphere temperatures, the value of the calculated temperature intervals
L* 1210 88,42 93,14 94,75 decreases, and for the one containing 7,5 wt % of the additive is only 5.
a* -0,20 -0,08 -0,10 Basing on the graphs of the logarithm of viscosity in Fig. 1 and the
b* 6,46 5,42 4,46 values presented in Table 5, it can be observed that the addition of
zirconium silicate increases the viscosity of the materials, whereas for
the material with a ZrSiO4 content of 7,5 wt % up to 1205 °C a higher
of zirconium silicate are also shown. The values measured on the ma-
viscosity is observed as compared to a sample with a higher zirconium
terial without the addition of ZrSiO4 were reference temperatures.
silicate content. Above 1280 °C, the viscosity of material with an ad-
The obtained results show that the addition of zirconium silicate
dition of 7,5 wt % is lower in comparison to the material without a
does not significantly affect the transition temperature which reaches
zirconium silicate additive. It can be seen that the logarithm curve of
similar values for all materials. The values of the other characteristic
the viscosity of the primary material tends to be straight-line as a
temperatures increase for the samples containing ZrSiO4, which is most
function of temperature. However, for the materials with the addition
evident for the dilatometric softening temperatures and shows that the
of ZrSiO4 there is a tendency to increase the rate of lowering the value
addition of zirconium silicate increases the range between the transi-
of the logarithm of viscosity when raising the temperature.
tion temperature and the dilatometric softening. It can also be seen that
the higher quantity of zirconium silicate induces a larger temperature
interval only for the half-sphere temperature. 3.2. Pyroplastic deformation
The values of characteristic temperatures given in Table 2 were used
Fig. 2 shows the pyroplastic deformation behavior of the studied

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materials. The addition of zirconium silicate contributes to lowering of

the temperature at which the deformations appear and thus it affects
negatively the stability of the formed shape. The higher the proportion
of zirconium silicate, the higher the magnitude of deformations oc-
curring at a given temperature, up to a temperature close to
1170–1180 °C, in which the alignment takes place. Deformations oc-
curring during firing constitute a complex phenomenon, influenced by
both the chemical composition and the thermal treatment, but the
participation and the shape of the crystalline phases should not be ig-
nored [13,14].
Only in the case of GC_1 material, hyalophane crystallizes in the
form of needles (Table 4, Figs. 7–9); needle-shaped crystals may build a
specific, three-dimensional interlocking network, which strengthens the
material and thus protects it against deformations.

3.3. Thermal differential analysis

The next step was to perform the thermal differential analysis,

Fig. 2. Deformation behavior of examined materials.
Fig. 3. DTA curves of examined materials.
which showed the changes occurring in the materials during heat
treatment. All the measurements were carried out during heating the
samples to 1190 °C at a rate of 10 °C/min, followed by cooling at the
same rate. The results are shown in Fig. 3. The temperatures shown in
the diagrams are ONSET points determined in the Netzsch Proteus
Thermal Analysis program (defining the beginning of the process). In
order to facilitate interpretation, the graph also shows the results of
measurements made for K-45 chalk and barium carbonate, the heating
conditions were identical to those used for the tested materials. The
endothermic effects observed for both chalk and barium carbonate are
also noticeable for the tested materials, in the case of chalk the effect
starts at 740 °C, whereas for barium carbonate the effects are observed
at 575 and 808 °C. Exothermic effects observed near 1000 °C should
correspond to the crystallization of hyalophane formed by a decom-
position of barium carbonate – active BaO – in the presence of alkali
metal oxides contribute to the formation of the liquid phase at rela-
tively low temperatures, in the SiO2–BaO–K2O system at 907 °C,
whereas in the SiO2–BaO–Na2O system at 785 °C [17,18].
Also during cooling, all the materials exhibit exothermic effects
indicating crystallization. The first effects, relatively intense, near the
temperature of 1190 °C, aremost likely related to the crystallization of
hyalophane, the second, at about 1180 °C, might be associated with the
celsian crystallization occurring to a very small extent. This phase has
not been detected by an X-ray analysis, but it may be seen on the images
received by scanning electron microscopy together with an X-ray che-
mical microanalyser, SEM-EDS. The graphs of DTA did not show the

Fig. 4. X-ray diffraction patterns of examined materials after firing at 1190 °C: Hy – hyalophane (standard card number: 98-003-1192), Q – quartz (98-064-7435), Zr
– zirconium silicate (98-015-8108).

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Fig. 5. X-ray diffraction patterns of examined materials after firing at 1200 °C: Hy – hyalophane (standard card number: 98-003-1192), Q – quartz (98-064-7435), Zr
– zirconium silicate (98-015-8108).

Fig. 6. X-ray diffraction patterns of examined materials after firing at 1210 °C: Hy – hyalophane (standard card number: 98-003-1192), Q – quartz (98-064-7435), Zr
– zirconium silicate (98-015-8108).

Fig. 7. SEM-EDS image of GC_1 material after firing at 1190 °C.

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Fig. 8. SEM-EDS image of GC_1 material after firing at 1210 °C.

Fig. 9. SEM-EDS image GC_1 + 7,5% ZrSiO4 material after firing at 1190 °C.

Fig. 10. SEM-EDS image GC_1 + 7,5% ZrSiO4 material after firing at 1210 °C.

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Fig. 11. SEM-EDS image GC_1 + 15% ZrSiO4 material after firing at 1190 °C.

Fig. 12. SEM-EDS image GC_1 + 15% ZrSiO4 material after firing at 1210 °C.

presence of effects related to the recrystallization process of zirconium
silicate during cooling, if previously the grains dissolved in the forming
liquid phase.
3.4. Phase composition and microscope analysis
Phase compositions of the obtained materials are presented in
Figs. 4–6 and summarized in Table 3. The use of addition of zirconium
silicate results only in the presence of ZrSiO4 but does not contribute to
the crystallization of new phases, others than those which occurred in
the samples that do not contain it. In each of the obtained materials the
presence of quartz and barium feldspar hyalophane (K,Ba)[Al(Si,Al)
Si2O8] from the group of tectosilicates was noted. No further changes in
the phase composition depending on the applied firing temperature
were observed. The presence of the amorphous phase is evidenced by
the raised background on phase diagrams.
The images of microstructures of all materials, received by the use
of a scanning electron microscope, show crystals different in size and
shape (Table 4). From the point of view of morphology, hyalophane
crystals with a needle-like habit are interesting, they occur only in GC_1
material, where they are particularly visible at 1210 °C, the addition of
zirconium silicate suppresses their crystallization in this shape. In the
samples containing zirconium silicate, fired at the lowest temperature,
clusters of fine zirconium silicate crystals can be observed; at higher
temperatures this trend disappears and a more regular distribution of
crystals is observed, larger crystals do not form clusters in the materials.
Additionally, it should be noted that the EDS analysis results differ from
those obtained by an X-ray analysis (See Figs. 7-12) – a crystalline
phase with a chemical composition similar to the chemical composition
of barium feldspar celsian has been identified, which probably occurs in
a smaller amount than the detection threshold and/or diffraction peaks
of this phase are covered by the raised background on diffractograms.
3.5. Surface parameters
Table 5 shows the values of the logarithm of viscosity at specified
temperatures and the results of roughness, gloss and whiteness mea-
surements.
To determine the surface smoothness, Ra parameter was used which
is the arithmetic average of the absolute values of the roughness profile
deviations from the mean line. For the tested materials the values in a
range of 0,526 ÷ 1,483 μm were measured. The use of the addition of

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ZrSiO4 induces smoothing of the surfaces of fired materials at the
temperatures of 1200 and 1210 °C, a major decrease in roughness is
observed for the samples with a higher amount of ZrSiO4. At the lowest
temperature, the tested additive causes an increase in the Ra parameter,
higher when it is used in the amount of 7,5 wt %. The increase in the
viscosity of the samples during firing (Fig. 1, Table 5), involving the
introduction of zirconium silicate into the system, results in an increase
of surface roughness only at 1190 °C. However, the gloss diminishes
visibly at any temperature. A larger amount of ZrSiO4 contributes to
producing a material with better surface smoothness, but with even
lower gloss. According to this, it can be seen that only at the lowest
firing temperature a key role in smoothing the surface of materials can
be attributed to the viscosity of the materials during thermal treatment
– difficult smoothing due to higher viscosity. The obtained materials are
characterized by dullness of the surface, gloss has the values in the
range of 3.31 ÷ 19.37%. The use of zirconium silicate also causes an
increase in whiteness – the higher its quantity, the higher values were
achieved by the L* parameters, simultaneously the value of parameter
b* decreases, causing the hue to become less “warm”. It can be noticed
that a more regular distribution of crystals in the samples with the
addition of ZrSiO4, observed at the highest firing temperature, results in
a decrease in roughness and an increase in gloss and a marked increase
in whiteness. It is worth noticing that in the case of GC_1 material,
higher gloss and whiteness are also observed at this temperature,
without observing a significant difference in the distribution of any
crystals.
4. Conclusion
1) The addition of zirconium silicate induces changes in the sintering of
glass-crystalline materials from the Al2O3–Na2O–K2O–CaO–MgO–BaO
system, namely the increase of characteristic temperatures as well as
the increase of viscosity of materials during firing, with simultaneous
changes of the character of the waveform of the logarithm of viscosity
curves as a function of temperature and also it decreases the occur-
rence temperature of materials pyroplastic deformation.
2) During thermal treatment, the recrystallization of zirconium silicate
did not occur. The DTA curves of all tested materials are similar and
thermal effects that could be possibly related to recrystallization are
not visible.
3) The presence of hyalophane and celsian was found in all materials,
the use of zirconium silicate does not visibly change the content of
these two crystalline phases, but it affects the crystals morphology.
4) The addition of zirconium silicate contributes to decreased rough-
ness of materials fired at the temperatures of 1200 and 1210 °C, the
higher smoothing is observed for the samples with a higher content
of ZrSiO4. At the lowest temperature, the additive increases the
surface roughness.
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5) Zirconium silicate causes significant changes in gloss of the glass-
crystalline materials from the Al2O3–Na2O–K2O–CaO–MgO–BaO
system. Gloss decreases with higher ZrSiO4 content in the materials,
while it increases with the increase of the firing temperature.
6) The addition of zirconium silicate contributes to the increase in
materials whiteness, in the case of higher quantity the effect is
larger.
Acknowledgements
KK has been partly supported by the EU Project POWR.03.02.00-00-
I038/16-00.
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