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Journal of the European Ceramic Society 30 (2010) 2443–2449

Factors affecting glaze transparency of ceramic tiles manufactured by the

single firing technique
Fábio G. Melchiades a,b,∗ , Bruna T. Rego a , Silvia M. Higa a ,
Helton J. Alves a,b , Anselmo O. Boschi a,b
a LaRC – Laboratório de Revestimentos Cerâmicos, DEMa – Departamento de Engenharia de Materiais,

UFSCar – Universidade Federal de São Carlos, Rod. Washington Luiz, Km 235, 13565-905 São Carlos, SP, Brazil
b Post Graduation Program in Materials Science and Engineering – PPGCEM, UFSCar, Brazil

Received 4 December 2009; received in revised form 5 April 2010; accepted 23 April 2010
Available online 31 May 2010

Abstract
Transparency is an extremely important optical property of several glazes used in the ceramic tile sector. The present work aimed to identify the
causes of loss of transparency presented by some ceramic glazes composed of frits with chemical compositions typical of optically transparent
glasses. After identifying the causes of low transparency presented by several ceramic glazes based on microstructural analyses, X-ray diffraction
and scanning electron microscopy, attempts were made to increase the transparency of these glazes by altering their chemical compositions. The
results suggest that the addition of alumina – through distinct mineral sources – may be an interesting alternative to prevent the crystallization of
calcium silicates, which reduce the transparency of glazes used in the ceramic tile sector.
© 2010 Elsevier Ltd. All rights reserved.

Keywords: Optical properties; Glass; Al2 O3 ; Electron microscopy; Ceramic frits

1. Introduction floor tiles, the design of the product is applied in the form
of very thin layers of colored glazes, over which a thicker
1.1. Rationale and objectives layer of highly transparent glaze must be applied (Fig. 1). This
layer of glaze protects the product by preventing the abrasive
Ceramic glazes1,2 are applied on the surface of a variety wear6 the ceramic tile undergoes when in use from reach-
of products to waterproof them, facilitate cleaning and give ing the underlying colored glazes, thus losing their decorative
them their final esthetic appearance. They are applied by dif- effect. At the same time, the presence of this layer on the
ferent technologies3 and develop their properties of interest surface of the product should not prevent the colors of the
after firing at high temperatures. Given that glazes are respon- designs applied on the lower layers from remaining visible, thus
sible for the esthetic properties of glazed ceramic products, making the high transparency of this protective glaze layer an
their optical properties – such as gloss, color, transparency essential characteristic of the product.
and opacity – take on a special relevance within the set of Because the firing cycles used in the manufacture of ceramic
properties that glazes should present. In several applications tiles are extremely rapid – usually less than 30 min – and the
the objective is to achieve transparent glazes4,5 on the surface maximum firing temperatures do not exceed 1200 ◦ C, the glazes
of ceramic materials. In the case of ceramic tiles, especially used on these products consist basically of ceramic frits.7 How-
ever, many of the frits commercially available today present a
certain degree of opacity (loss of transparency) when fired in
typical conditions of ceramic tile manufacture, especially when
∗ Corresponding author at: LaRC – Laboratório de Revestimentos Cerâmicos, the glazes are formulated with high frit contents to produce sur-
DEMa – Departamento de Engenharia de Materiais, UFSCar – Universidade
faces with high gloss and minimal roughness. In this situation,
Federal de São Carlos, Rod. Washington Luiz, Km 235, 13565-905 São Carlos,
SP, Brazil. Tel.: +55 16 3351 8249; fax: +55 16 3361 5404. the product may undergo shade variations8 that impair the colors
E-mail address: [email protected] (F.G. Melchiades). of the end product, since the visibility of the decorations applied

0955-2219/$ – see front matter © 2010 Elsevier Ltd. All rights reserved.
doi:10.1016/j.jeurceramsoc.2010.04.030
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2444 F.G. Melchiades et al. / Journal of the European Ceramic Society 30 (2010) 2443–2449

Glaze devitrification has been studied exhaustively in

response to the growing interest in vitroceramic glazes12–14 in
recent years. This phenomenon is directly related to the chemical
composition of the starting glaze and to the sintering conditions.
Devitrification begins with the appearance of small nuclei, which
lead to the growth of crystalline phases in a vitreous matrix.
The size and quantity of crystals that are formed, which depend
Fig. 1. Diagram of the layers that make up a ceramic tile. on the nucleation and growth rates, directly affect the proper-
ties of the resulting glazes, e.g., their mechanical, optical and
under this layer is impaired by the low transparency of the top chemical properties.15 Most of the existing studies in the litera-
layer. ture involving the devitrification of ceramic glazes deal with the
The purpose of this work, therefore, was to contribute to increment of mechanical properties,16–18 which can be obtained
the identification of the causes of loss of transparency of sev- through vitroceramic systems. Some of these systems, such
eral glossy frits used in ceramic tiles fabricated by the single as Li2 O–Al2 O3 –SiO2 and CaO–MgO–Al2 O3 –SiO2 , have been
firing technique and to propose alternatives to maximize the explored with greater emphasis for some time.5,14 However,
transparency of these frits. devitrified crystalline phases usually present higher refractive
indices than those of glassy matrices, resulting in glazes with low
transparency.
1.2. Interaction of light with glassy materials
The phenomenon of vitreous phase separation is observed
by electron microscopy analysis of many transparent and opti-
To develop highly transparent glazes further understanding
cally homogeneous glasses. The literature19 also highlights
of the mechanisms of interaction between materials and light is
that the technical properties of the ceramic glazes depend
required. Transparency is achieved when materials are able to
on a lack of structural homogeneities. Aparici et al.8 states
transmit large fractions of incident electromagnetic radiation,9
that the loss of transparency of single-fired ceramic frits
while opaque materials reflect higher fractions of incident light.
and the bluish and/or milky aspect of glazes obtained from
Generally speaking, homogeneous glasses tend to present high
them occurs as a result of the separation of vitreous phases
transparency because they allow light to be transmitted inside
of certain glaze compositions as a function of the cooling
them without offering barriers for the development of this
rate applied in rapid firing cycles. When immiscible vitre-
phenomenon. However, heterogeneous glasses may contain bar-
ous phases show significant differences in surface tension, the
riers to light transmission and, through refractive and reflective
phase with the highest surface tension adopts the shape of
phenomena, increase the reflected fractions of incident light,
spherical droplets. If the dimensions of the droplets reach the
especially when they contain phases with different refractive
dimensions of the wavelength of visible light, the vitreous
indices.2
material undergoes loss of transparency. Under certain condi-
Considering the nature of ceramic glazes and the process
tions, the heterogeneities may evolve into crystalline nuclei, at
used in the manufacture of ceramic tiles, the possible sources of
which point the separated phase is considered to be in a pre-
heterogeneity that can potentially generate loss of transparency
crystalline state, with a higher degree of order than the glassy
in glazes are:
matrix.
The great majority of studies about phase separation in glassy
• porosity (air bubbles); materials involve simple glass compositions, such as binary sil-
• devitrification (formation of crystalline phases during firing); icate or borosilicate glasses.20 In these glasses, the nature and
and molar fraction of the network-modifier elements is a determining
• separation of vitreous phases (generated by the immiscibility factor of the tendency for phase separation.19 The smaller the
of liquids during firing). size of the network-modifier cation and the higher its electric
charge the easier the separation of vitreous phases. The prob-
All ceramic glazes contain air bubbles,10,11 which occupy ability of vitreous phase separation decreases considerably as
distinct volumetric fractions and present different size distribu- the coordination requirements of the network former and modi-
tions according to the nature of the product and the conditions of fier elements become similar.19 Therefore, alumina can be used
manufacture. Air bubbles may be formed from gases released by to prevent phase separation in these glass material systems,
the support during firing, from the combustion of organic sub- since the Al3+ ion can form tetrahedral configurations similar
stances used in the application of the decorations, from the air to those found in SiO4 4− tetrahedrons.19 In the case of ceramic
that remains occluded among the frit particles in the green com- tile glazes, several authors4,21 have studied ranges of chemi-
pact, or even through the incorporation of air bubbles previously cal compositions of frits and raw materials from which highly
present in the suspensions used for wet glaze application. Since transparent glazes can be obtained. Poyraz et al.4 concluded
the refractive index of air (n = 1.0) is considerably lower than that pumice – a volcanic material found in the Mediterranean
that of glasses (n = 1.5), the presence of appreciable volumetric area – could replace feldspar in transparent raw glazes. In frit-
fractions of air bubbles may impair not only the transparency ted glazes, results show design of experiments as a tool for
but also other technical properties of glazes. increasing transparency and the role of alumina in this kind of
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F.G. Melchiades et al. / Journal of the European Ceramic Society 30 (2010) 2443–2449 2445

Table 1 Table 2
Chemical composition of the frits expressed in wt%. Composition of the glazes expressed in wt% of raw materials.
Oxides Frit A Frit B Raw materials Glaze A Glaze B

LOI (%) – 0.1 Frit A (%) 67.6 –

SiO2 (%) 59.8 60.3 Frit B (%) – 67.6
AI2 O3 (%) 6.3 8.1 Bentonite (%) 0.7 0.7
Fe2 O3 (%) 0.1 0.2 Sodium tripolyphosphate (%) 0.15 0.15
CaO (%) 15.8 17.3 CMC (%) 0.15 0.15
MgO (%) 0.6 1.0 Water (%) 31.4 31.4
Na2 O (%) 1.2 2.1
K2 O (%) 4.2 4.0
ZnO (%) 7.3 –
B2 O3 (%) 4.5 7.0 to manufacture the product with the support and glaze in ques-
tion. Heating and cooling rates were about 90 ◦ C/min and the
soak time at 1060 ◦ C was 3 min.
composition,21 making glaze less prone to immiscible liquid- The transparency of the glazes was evaluated based on a
phase separation. colorimetric analysis of the glazed surface of the test speci-
mens using a Minolta CM-2600d spectrophotometer. The results
2. Materials and methods are expressed by the trichromatic coordinates: L* indicates the
degree of whiteness; a* presents the variation between green
This work was divided into two steps. First, we sought to and red colors; and b* indicates the variation between blue and
identify the possible causes of loss of transparency presented by yellow colors. Highly transparent glazes show the tile support
two commercial glossy frits used in the ceramic tiles sector. In color and consequently they have low L* values and more posi-
the second step, based on the findings of the first, several experi- tive a* and b* parameters. To complement the results, the gloss
mental tests were carried out aiming to increase the transparency of the glazes (β60 ) was determined by glossmeter analysis, using
of the frits characterized in the first step. a Zehntner ZGM1110 equipment.
To better understand the results, the glazes were characterized
2.1. Causes of low transparency of ceramic glazes microstructurally by X-ray diffraction (XRD) and scanning elec-
tron microscopy (SEM). The X-ray diffraction was performed
Samples of two glossy frits were chosen and their chemical from 5◦ to 70◦ (2θ scale), at a scan velocity of 3◦ /min, with
compositions were determined by X-ray fluorescence (Table 1), the X-ray beam focused directly onto the glazed surface. The
except for the B2 O3 content, which was analyzed by atomic SEM analysis was carried out on the cross section of the glaze
absorption spectrometry. on the test specimens, which were previously cut and their cross
The frits were then ground in a rapid milling laboratory sections sandpapered and polished.
ball miller, following the composition of glazes indicated in
Table 2. In addition to frit and water, a suspending agent (ben- 2.2. Effects of the addition of alumina on transparency
tonite), a deflocculant (sodium tripolyphosphate) and a ligand
(carboxymethylcellulose – CMC) were used to obtain the sus- This stage of the study consisted of preparing glazes from
pension. The material was ground until a residue of 2.0% was the same frits used earlier, but with the addition of alumina to
obtained in an ASTM #325 sieve (44 ␮m mesh). the glaze composition. An evaluation was made of the effects of
The frit suspensions were then applied onto the surface of introducing two different contents of Al2 O3 to the solid fraction
industrial ceramic tile supports using a regulated glaze applica- of the glaze – 2.4% and 4.0%, using kaolin and calcined alumina
tor for the deposition of raw layers with 0.4 mm thickness. The of known chemical compositions were evaluated.
test specimens were then fired in a laboratory-scale rapid-cycle Table 3 lists the glaze compositions used in this stage of the
furnace at a firing temperature of 1060 ◦ C, which, in the labora- study. The glaze processing conditions (grinding, application
tory furnace, corresponded to the temperature used industrially and firing) were the same as those employed in the previous stage

Table 3
Composition of the glazes with alumina additions expressed in wt% of raw materials.
Raw materials (in wt%) GIz.A 2.4 K GIz.A 4.0 K GIz.A 2.4 AC GIzA 4.0 AC GIz.B 2.4 K GIz.B 4.0 K GIz.B 2.4 AC GIz.B 4.0 AC

Frit A 64.2 61.5 66.0 64.9 – – – –

Frit B – – – – 64.2 61.5 66.0 64.9
Bentonite – 0.7 0.7 – – 0.7 0.7
Kaolin 4.1 6.8 – – 4.1 6.8 – –
Calcined alumina – – 1.6 2.7 – – 1.6 2.7
Sodium tripolyphosphate 0.15 0.15 0.15 0.15 0.15 0.15 0.15 0.15
CMC 0.15 0.15 0.15 0.15 0.15 0.15 0.15 0.15
Water 31.4 31.4 31.4 31.4 31.4 31.4 31.4 31.4
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Table 4
Colorimetric coordinates and glossmeter analysis of the Glaze A and Glaze B.
Glazes Chromatic coordinate β60

L* a* b*

Glaze A 67.6 12.0 3.5 89.2

Glaze B 65.8 10.9 12.6 92.6

of this work. Similarly, the transparency and microstructural

analysis of the resulting glazes followed the same procedures
described earlier herein, in order to ensure the comparability of
the results.

3. Results
Fig. 2. SEM micrograph of Glaze A.
3.1. Causes of low transparency of ceramic frits

Table 1 lists the chemical compositions of the two industrial

frits used in this study. Frit A was found to present a chemical
composition typical of transparent frits used in the manufacture
of porous ceramic tiles by single firing. These frits are charac-
terized by their low content of alkaline oxides and high content
of calcium and zinc oxides as network modifiers.7 Frit B corre-
sponds to a type of frit widely used in Brazil, which consists of
an adaptation of traditional glossy frits used in porous products
fabricated by single firing, in which the zinc oxide is eliminated
from the composition for economic reasons22 and the content
of the other oxides are readjusted correspondingly. The selected
frits represent the main types of frits used in the ceramic tile
industry today.
Table 4 shows the results of the colorimetric analysis of the
Fig. 3. SEM micrograph of Glaze B.
transparency of the frits. L* and b* parameters show whiteness
and yellow or blue color tendency, respectively. In the same
table, the results of the glossmeter analysis are expressed. As A presented slightly larger sizes, on average, than those found
can be seen, the two frits present low transparency and, most in Frit B, and that the volumetric fraction occupied by these
importantly, their surfaces show differences in shade. Note that crystals in the glaze was also higher. Determination of the mean
parameter b* of Frit A indicates a considerably bluer shade than crystals sizes indicates 1.47 and 0.81 ␮m in Glaze A and Glaze
that of Frit B. The latter, in turn, albeit slightly more transpar- B, respectively.
ent and with less bluish shade than frit A, can also be visually Since calcium silicate crystals usually present refractive
classified as a highly milky or opaque frit (as indicated by the indices of 1.61–1.65,19 it can be stated that the loss of trans-
parameter L*), which impairs the visibility of the colors of the parency of the glazes under study is related to the devitrification
substrate on which it is applied. The two frits are glossy, but
their gloss values (β60 ) are not very high. Table 5
These samples were characterized microstructurally by SEM Semi-quantitative chemical analysis carried out by SEM/XRD.
and XRD. Figs. 2 and 3 present the SEM images, while Table 5 Elements (%) Glaze A Glaze B
lists the results of the semi-quantitative chemical analysis carried Matrix Crystal Matrix Crystal
out by SEM/XRD. Fig. 4 depicts the results of the qualitative
XRD analysis of the crystalline phases in the glazes. C 0.4 0.4 0.4 0.4
0 2.3 1.7 1.8 1.2
These analysis indicated the presence of crystalline phases in Na 3.2 1.8 0.7 0.4
the glazes obtained from the two frits under study. Both glazes Mg 0.8 0.9 1.3 0.7
showed the formation of elongated crystals with lengths varying Al 7.2 4.7 10.5 4.5
from 0.5 to 5 ␮m. The pointwise chemical analysis and X-ray Si 65.4 61.6 64.1 55.8
diffractions indicated that calcium silicate crystals were formed K 4.6 3.4 6.8 2.8
Ca 14.5 24.6 14.2 34.0
in the glazes from the two frits, although the diffraction pattern Fe – – 0.2 0.2
also revealed that these crystals has distinct crystalline struc- Zn 1.6 1.0 – –
tures. Moreover, it can be stated that the crystals detected in Frit
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F.G. Melchiades et al. / Journal of the European Ceramic Society 30 (2010) 2443–2449 2447

Fig. 6. Influence of the addition of Al2 O3 on the transparency of Glaze B.

Fig. 4. Diffractograms of the of the glazes obtained from the two frits.
seen by the progressive reduction of the chromatic coordinate
L* (loss of milkiness) and the increase in the chromatic coordi-
of these crystalline phases. Differences of transparency found
nate b* (loss of the bluish aspect and improved visibility of the
between the two frits can be explained by differences in devit-
yellowish color of the ceramic support upon which the glazes
rification detected in the SEM analysis. Frit A, rich in ZnO and
were applied).
lower in alkaline elements, probably tends to undergo vitreous
The incorporation of Al2 O3 into the glazes led to consider-
phase separation more easily. This phenomenon may occur pre-
able gains in transparency, independently of the mineral source.
cursory to devitrification19 and create more favorable conditions
As can be seen in Figs. 5 and 6, the chromatic coordinates L*
for nucleation and growth of crystals.
and b* in the glazes containing kaolin and calcined alumina are
very similar at the same added content of Al2 O3 . In addition
3.2. Effects of the addition of alumina on transparency to increased transparency, the gloss of the glazes shows slight
increase (Glz.A 4.0 K presents β60 = 98.2 and Glz.B 4.0 K shows
The literature reports that devitrification can be prevented by β60 = 99.3).
incorporating small amounts of other components into the vit- To confirm the efficacy of the addition of Al2 O3 as an alter-
reous network, such as alumina.15,19 Therefore, in this stage of native to increase the transparency of the glazes by preventing
the study, an evaluation was made of the influence of the incor- their devitrification, the glazed surfaces of samples Glz.A 4.0 K
poration of alumina – added in the form of kaolin and calcined and Glz.B 4.0 K (Glazes A and B with the addition of 4.0% of
alumina – on the transparency of these glazes. Al2 O3 through kaolin) were analyzed microstructurally by SEM
Figs. 5 and 6 illustrate the results of the colorimetric analy- and XRD.
sis of the different glazes obtained with the addition of Al2 O3 Figs. 7 and 8 illustrate the results of the SEM analysis, while
through the introduction of kaolin and calcined alumina in the Fig. 9 depicts the diffractograms of the surfaces of the glazes.
glazes. The incorporation of small amounts of Al2 O3 was found These results explain the high transparency shown by these
to lead to a significant increase in their transparency, as can be glazes, indicating that they contain significantly low volumetric

Fig. 5. Influence of the addition of Al2 O3 on the transparency of Glaze A. Fig. 7. Micrograph of sample Glz.A 4.0 K.
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2448 F.G. Melchiades et al. / Journal of the European Ceramic Society 30 (2010) 2443–2449

as the cause of this phenomenon. In this case, the most probably

hypothesis is that vitreous phase separation occurs precursory
to devitrification. Frit A, rich in ZnO and lower in alkaline
elements, has a higher tendency to phase separation and conse-
quently enables the development of larger and more numerous
crystals than Frit B.
The incorporation of Al2 O3 proved to be a viable alternative
to maximize the transparency of the glazes obtained from the
frits in question. Small additions (in the order of 2.0–4.0%) may
suffice to produce substantial increases in transparency. Effects
of the alumina addition on the other technical properties were not
evaluated in this study. However, considering that the crystals
avoided by alumina addition were calcium silicates, losses are
not expected to abrasion or chemical resistance.
The incorporation of Al2 O3 through kaolin of calcined alu-
Fig. 8. Micrograph of sample Glz.B 4.0 K.
mina produced very similar results insofar as the transparency of
the glazes is concerned. Therefore, the two raw materials can be
used successfully for this purpose, and represent very interesting
options to increment the transparency of ceramic tile glazes, in
which this characteristic is an essential requisite.

Acknowledgment

This work was developed with financial support from

FAPESP, process n. 06/53665-6.

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