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CERAMICS
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Ceramics International 39 (2013) 4953–4960
www.elsevier.com/locate/ceramint

Dolomite, wollastonite and calcite as different CaO sources

in anorthite-based porcelain
Shanjun Ke, Xiaosu Cheng*, Yanmin Wang, Qianghong Wang, Hui Wang
College of Materials Science and Engineering, South China University of Technology, Guangzhou 510640, China

Received 23 October 2012; received in revised form 26 November 2012; accepted 27 November 2012
Available online 5 December 2012

Abstract

Anorthite-based porcelain was fabricated by using ball clay, quartz, alumina, feldspar and three different sources of CaO as raw
materials. The effect of CaO sources such as dolomite, wollastonite and calcite on the mechanical, thermal and aesthetical properties of
anorthite-based porcelain was investigated. X-ray diffraction (XRD) and scanning electron microscopy (SEM) studies were also carried
out to analyze the microstructure. Anorthite was formed as major phase in all the samples fired at their optimum sintering temperatures
(1200, 1215 and 1230 1C). The sample with dolomite had the highest bulk density but the smallest flexural strength due to formation of
substantial glassy phase. The maximum flexural strength ( 110 MPa) was reached in the sample containing wollastonite, which was
mainly attributed to the favorable microstructure. Anorthite as the single crystalline phase was found in the sample with calcite and the
sample showed the lowest thermal expansion coefficient and the highest whiteness, which was similar to bone china in appearance.
& 2012 Elsevier Ltd and Techna Group S.r.l. All rights reserved.

Keywords: D. Porcelain; Anorthite; CaO sources

1. Introduction The TEC of glass phase detected in bone china from 20 to

350 1C is calculated to be 3–4.5  10  6 K  1, while the
Bone china is a highly specialized product in terms of its approximate TEC of b-tricalcium phosphate from 50 to
appearance; being exceptionally white and translucent makes 400 1C is 12  10  6 K  1 [8]. Apparently, b-tricalcium phos-
it the world’s most expensive type of tableware [1]. Typical phate crystalline phase has a negative effect on thermostability
composition of bone china is about 50 wt% animal bone of bone china. Meanwhile, anorthite has a refractive index of
ash, 25 wt% china clay and 25 wt% Cornish stone or  1.58 [9], which is close to that of the glass phase ( 1.5) [10].
feldspar [2]. After sintering, the phases in the fired body That is, anorthite crystalline phase can increase translucency
generally consist of 40 wt% b-tricalcium phosphate performance of bone china. Therefore, anorthite-based por-
(b-Ca3(PO4)2), 30 wt% anorthite (CaO  Al2O3  2SiO2), and celain can be used in tableware to improve heat stability and
30 wt% calcium aluminosilicate glass phase [3,4]. So, bone decoration quality.
china is a highly crystalline ( 70%) whiteware that exhibits In recent years, many studies [10–15] have been under-
good resistance to edge chipping and a high flexural strength taken to develop anorthite-based porcelain to replace tradi-
value of  100 MPa [5,6]. tional porcelain (including bone china and hard porcelain).
However, the glaze applied to bone china is easily scratched Capoglu [10–12] designed low-clay translucent whiteware,
and the fired body thermal shock resistance is poor. The which was produced from prefired materials and a small
former is due to its alkaline rich glaze and the latter is amount of clay at 1370 1C for 3 h. The low-clay whiteware
attributed to mismatch of thermal expansion coefficient consisted of anorthite, mullite (3Al2O3  2SiO2) crystalline
(TEC) of different phases in the fired body. The TEC of phases and glassy phase with high crystalline to glassy phase
anorthite [7] from 20 to 500 1C is  4.3  10  6 K  1. ratio. Taskiran [13,14] also reported a new porcelaneous
stoneware, which was obtained from a mixture of wollasto-
n
Corresponding author. Tel.: þ 86 20 87114217; fax: þ 86 20 87110273. nite, alumina, quartz, magnesia and ball clay by powder
E-mail address: guangzhouscut@163.com (X. Cheng). pressing and sintering at 1225 1C. The material had anorthite

0272-8842/$ - see front matter & 2012 Elsevier Ltd and Techna Group S.r.l. All rights reserved.
http://dx.doi.org/10.1016/j.ceramint.2012.11.091
4954 S. Ke et al. / Ceramics International 39 (2013) 4953–4960

as its major phase with corundum, cristobalite and glass as CaO sources. Feldspar was used to obtain dense porcelain
minor phase. body at a relatively low temperature. The high content of
In addition, aluminous cement (CaO  Al2O3 and CaO  CaO decreases the liquid phase viscosity of the porcelain at
2Al2O3), limestone (CaCO3), colemanite (2CaO  3B2O3  high temperatures, which makes it particularly easy to
5H2O), wollastonite (CaO  SiO2), calcite (CaCO3) and dolo- generate shape distortion of the porcelain bodies. To resist
mite (CaCO3  MgCO3) can all be used in the production of high-temperature deformation, a small amount of indus-
anorthite-based porcelains as a CaO source [16–20]. Mean- trial alumina is added as a source of aluminum to increase
while, the production of anorthite ceramics was studied with the viscosity of high-temperature melted liquid. The start-
different sources of CaO such as Ca(OH)2, CaCO3, marble ing raw materials were purchased from Guangdong Sitong
powder and gypsum mold waste by Kurama [21]. However, Group Co. Ltd. (Chaozhou, China). Table 1 shows the
the above mentioned study only aimed to produce dense chemical composition of raw materials.
anorthite ceramics from different CaO sources, and there was
little attention paid to the microstructure and the other 2.2. Sample preparation
properties. For tableware, the applicability and decoration
quality is very important for its marketing. So, not all calcium- Compositions were prepared on the basis of the approx-
containing minerals are appropriate for the manufacture of imate stoichiometric anorthite compositions with different
anorthite-based porcelain for daily use. In China, dolomite, CaO sources (dolomite, wollastonite and calcite) and were
wollastonite and calcite are rather abundant, and are cheaper labeled as A, B and C (Table 2), respectively. These
than other calcium-containing minerals. In a previous study powders were wet mixed and milled in a planetary mixer
[22], the preparation of anorthite-based porcelain was fabri- with zirconia ball millstone for 6 h. The particle size
cated using calcite as a source of CaO. The present work, distributions of the milled slurry were analyzed by a
which is a part of an extended research program, aims to BT-9300S model laser diffraction particle size analyzer
elucidate the influence of dolomite, wollastonite and calcite on (Dangdong Bettersize Instruments Ltd., China). The result
the microstructure and technological properties of anorthite- is given in Fig. 1. It can be seen that all samples have
based porcelain, including sintering character, flexural approximate results with similar log-normal distribution
strength, thermal expansion and appearance quality. presenting one maximum point. Meanwhile, the particle
sizes are less than 10 mm, which are centered at 1–5 mm.
2. Experimental procedure The slip casting was used for forming, which could
obtain green body with high-strength [19]. Slips were cast
2.1. Raw materials in a plaster mold into rectangular blocks of 60 mm 
60 mm  10 mm dimensions. The consolidated rectangular
Ball clay and quartz were used as starting raw materials. blocks were removed from the mold after 45 min. Natural
Dolomite, wollastonite and calcite were chosen as different drying time of the consolidated specimens was determined

Table 1
Chemical composition of raw materials.

Raw materials Constituents (wt%)

SiO2 Al2O3 Fe2O3 TiO2 CaO MgO K2O Na2O L.O.I

Ball clay 48.61 36.14 0.21 0.14 0.16 0.21 0.98 0.24 12.7
Quartz 98.38 1.02 0.03 0.01 0.08 0.02 0.07 0.04 0.23
Alumina – Z99.0 – – – – – – –
Feldspar 65.56 18.85 0.08 0.02 0.23 0.03 12.39 2.28 0.56
Dolomite 1.32 0.45 0.04 0.03 29.90 19.41 0.02 0.36 48.46
Wollastonite 50.13 0.92 0.20 0.02 44.80 0.82 – – 3.21
Calcite 3.02 0.61 0.04 0.01 53.98 2.13 0.04 0.11 39.82

Table 2
Composition of the investigated samples A, B and C (wt%).

Sample Raw materials

Ball clay Quartz Alumina Feldspar Dolomite Wollastonite Calcite

A 20 14 21 – 45 – –
B 20 7 15 18 – 40 –
C 20 20 12 18 – – 30
 S. Ke et al. / Ceramics International 39 (2013) 4953–4960 4955

Fig. 1. Particle size distributions of samples A, B and C milled for 6 h.

for 24 h in air at room temperature and then the specimens Fig. 2. XRD patterns of samples A, B and C fired at 1200 1C, 1215 1C
and 1230 1C respectively.
were dried in an oven for 12 h at 90 1C. Subsequently, the
specimens were processed into required size (5 mm 
5 mm  55 mm) by cutting. The firing was performed in Table 3
an electric furnace at a temperature from 1155 to 1260 1C XRF chemical analysis result of the fired samples A, B and C.
for 1 h. Sample Oxides (wt%)

2.3. Measurements and analyses SiO2 Al2O3 Fe2O3 TiO2 CaO MgO K2O Na2O

A 32.10 37.47 0.11 0.03 18.00 11.70 0.29 0.28

The bulk density and water absorption of the fired body B 48.66 29.83 0.16 0.03 18.83 0.39 1.77 0.33
were determined by the Archimedes method according C 49.60 26.79 0.09 0.03 19.20 0.81 2.89 0.58
to ASTM C373 [23]. The flexural strength of samples
(3 mm  4 mm  50 mm) as measured using an electronic
universal tester (Model 5569, Instron Ltd.) by a three point prepared from the SiO2–Al2O3–B2O3–MgO–CaO–Na2O–F
bending fixture span of 30 mm and cross head speed of system by Ventura [24]. Literature [25] also reported that the
0.5 mm/min. The thermal analysis was investigated by phases of anorthite, spinel and mullite (3Al2O3  2SiO2) were
differential scanning calorimetry (DSC, STA449C, generated from kaolin–dolomia mixtures. Moreover,
Netzsch Instruments Ltd., Germany), at a heating rate of anorthite as the single crystalline phase is obtained in the
10 K/min, under air atmosphere. The thermal expansion sample C while a small amount of corundum (Al2O3)
coefficient of sintered specimens was determined between crystalline phase is shown in Fig. 2B, which can be explained
room temperature and 500 1C using an automatic dilat- with a content of Al2O3 in sample B higher than that of the
ometer (DIL402EP, Netzsch Instruments Ltd., Germany), sample C in Table 3.
at a heating rate of 10 K/min. The crystalline phases were Differential scanning calorimetry (DSC) is used to study
determined by an X-ray diffractometer (XRD, Philips PW- all the transformations involving heat exchange occurring in
1710, the Netherlands), using CuKa radiation. The micro- a material during a heating cycle. Therefore, it is a suitable
structures were observed by a scanning electron microscope technique for identifying phenomena such as phase transi-
(SEM, Philips L30FEG, the Netherlands). The Lnanbn color tions, crystallization or melting. Fig. 3 shows the DSC curves
parameters of samples were measured using a differential of samples A, B and C at temperatures from ambient
colorimeter (X-Rite Color Premier 8200, USA). temperature to 1250 1C. Clearly, the tendency of all DSC
curves is consistent, when the temperature is below 600 1C.
3. Results and discussion There is one exothermic peak at around 350 1C and two
endothermic peaks at around 500 and 576 1C. The exother-
The XRD patterns of samples fired at the optimal firing mic peak is related to the combustion of the organic matter,
temperature are shown in Fig. 2. Obviously, anorthite is the which is a component of the ball clay, and the first
primary crystalline phase, presenting some glassy phases in endothermic peak corresponds to the matrix dehydroxyla-
all samples. Akermanite (2CaO  MgO  2SiO2) and spinel tion process according to the following reaction [26]:
(MgO  Al2O3) are observed only in sample A, because
dolomite is not only a kind of CaO source, but also a Al2 O3 U2SiO2 U2H2 OðkaoliniteÞ-Al2 O3 U2SiO2 ðmetakaoliniteÞ þ 2H2 O
source of MgO. The akermanite-based glass–ceramic was ð1Þ
4956 S. Ke et al. / Ceramics International 39 (2013) 4953–4960

Fig. 3. DSC curves of samples A, B and C.

Fig. 4. Water absorption variation of samples A, B and C as a function of
temperature.
For the third peak, the small endothermic peak was
attributed to a- to b-quartz transition.
Above 600 1C, the DSC curves of samples A, B and C
have great differences. On the curve A, two endothermic
peaks and two exothermic peaks are observed at 687, 770,
838 and 940 1C. Two sharp endothermic peaks were
assigned to dolomite and calcite decarbonation. In another
work [27], the reaction process was researched by Lagzdina
in detail; related reactions are as follows:
CaMgðCO3 Þ2 ðdolomiteÞ-CaCO3 ðcalciteÞþ MgO þ CO2
ð2Þ

CaCO3 ðcalciteÞ-CaO þ CO2 ð3Þ

And the exothermic peaks occurred from crystallization of
new crystals, including anorthite, akermanite and spinel
(Fig. 2). According to the thermal analysis results, samples B
and C showed some differences compared with sample A. On
the curve B, the exothermic peak was observed at 992 1C due Fig. 5. Bulk density variation of samples A, B and C as a function of
to an unknown crystal formation. On the curve C, one drastic temperature.
endothermic peak and one exothermic peak were observed at
773 and 968 1C, respectively. The former corresponds to the
decomposition of CaCO3, while the latter indicates the small fall of bulk density mainly due to expansion of the
formation of anorthite (Fig. 2). Furthermore, as seen from entrapped gases, that is, blisters and bloating [28].
Fig. 3, they present steep slope indicating the formation of Moreover, it can be seen from Fig. 5 that sample A has
high-temperature melt suddenly between 1000 and 1200 1C. In significant difference compared with samples B and C.
general, the melted glassy phase plays a flux role and makes Sample A has the highest bulk density (2.67 g cm  3). The
the material increase bulk density easily [19]. maximum bulk density of sample B is 2.45 g cm  3, and
Fig. 4 shows the behavior of the water absorption as a 2.41 g cm  3 for sample C. Table 4 summarizes the impor-
function of temperature. The water absorption decreases tant physical properties of crystalline phases identified in
with increase in heating temperature due to reduction of this study. Sample A has the highest density value due to
the apparent porosity through liquid phase sintering. formation of a substantial spinel phase (3.58 g cm  3) [29].
Samples A, B and C reach a value of water absorption For the same reason, a small amount of corundum
of 0.00% at the firing temperatures of 1200, 1215 and (4.05 g cm  3) [28] makes the density of sample B higher
1230 1C, respectively. Fig. 5 displays the variation in bulk than that of sample C.
density with heating temperature. At first, the bulk density Fig. 6 shows the flexural strength behavior as a function
value continues to increase, and optimum values are of sintering temperature. The flexural strength of all
achieved when the water absorption reached a minimum samples increases with an increase in sintering tempera-
value tending to be nearly zero. Further firing results in a ture. On further heating, the flexural strength values reach
 S. Ke et al. / Ceramics International 39 (2013) 4953–4960 4957

maximum values of around 85 MPa for sample A, measured over the temperature range from 30 to 500 1C using
100 MPa for sample B, and 110 MPa for sample C and a dilatometer. The expansion ratios have almost linear increase
then decrease with a corresponding decrease in density. over the entire measured temperature range. For practical
Theoretically, flexural strength developed in a porcelain application of high-strength porcelain for tableware, thermal
body is maximum when apparent porosity decreases to expansion below 150 1C is important in order to withstand the
zero. A similar result is observed in the present study. thermal shock of heat disinfection or washing [35]. According
Furthermore, according to Figs. 4 and 6, an abnormal to thermal expansion coefficients, the average TEC values
phenomenon is found where sample A has the highest of all the samples in the area of the tested temperature are
density but the smallest strength. The low strength of calculated and listed in Table 5. From the table, the TEC of
sample A can be explained by the substantial glassy liquid samples A, B and C below 300 1C were calculated as
formation due to high content of MgO (11.7 wt%). 7.2  10  6 K  1, 5.1  10  6 K  1 and 4.9  10  6 K  1, respec-
Porosity and microstructure are considered important tively. According to the simple rule of mixtures [1], the value of
parameters regarding the mechanical properties of fired TEC could be calculated by using simple rule of mixtures
porcelain body. Fig. 7 shows SEM micrographs of the which is consistent with the relative proportions of the phases.
polished surface of samples A, B and C fired at their Sample A has a high TEC because of the presence of
optimal firing temperatures. Sample A presents larger, akermanite (10.3  10  6 K  1) [36] and spinel (8.2  10  6
isolated, spherical pores in the range of 30–40 mm K  1) [34]. A small amount of corundum (7–8  10  6 K  1)
(Fig. 7A). Samples B and C are characterized by small [37] crystalline phase has a negative effect on decreasing the
isolated pores (10–20 mm), which are less spherical (elon- TEC of sample B. Sample C has a low TEC value of
gated or ellipsoid). Additionally, sample C presents a 4.9  10  6 K  1 due to the formation of a single anorthite
larger number of pores than sample B, which is due to phase, whose TEC value is  4.3  10  6 K  1 from 20 to
calcite decarbonation generating residual entrapped gas. 500 1C [7], while the TEC for glasses of the compositions
Thus, a clear relation between strength and porosity can be detected in common glaze [1] from 20 to 350 1C were
confirmed. That is, high porosity and big flaw sizes are calculated to be 3–4.5  10  6 K  1. Therefore, samples B
unfavorable to the strength of fired porcelain body.
The SEM images of the fracture surface of samples
chemically etched with hydrofluoric acid for 30 s are
shown in Fig. 8. Characteristic octahedral spinel crystals
are clearly seen in Fig. 8A. Akermanite and anorthite are
not easily recognizable due to their being surrounded by a
large amount of glass phase. In Fig. 8B, very small
anorthite crystals together with a small amount of glassy
phase are observed. Lamellar crystals of anorthite are
cemented with residual glass, and the grain sizes are less
than 3 mm (Fig. 8C). Marques [30] also fabricated
anorthite crystals with similar shape. Comparing Fig. 8A,
B and C, it is easy to make a qualitative comparison for
the content of the residual glass phase. And it follows the
general order C o B o A. So, sample C possesses a high
crystalline to glass ratio, which also may show high
strength [31–33].
The thermal expansion coefficient (TEC) is a key factor
when considering the thermal matching between glaze and Fig. 6. Flexural strength variation of samples A, B and C as a function of
body [34]. Fig. 9 shows the TEC curves of samples A, B and C temperature.

Table 4
Crystalline phases of samples A, B and C fired at 1200 1C, 1215 1C and 1230 1C respectively.

Sample Temperature (1C) Crystalline phases Physical property

Density (g cm  3) TEC  10  6 (K  1) Refractive index

A 1200 Anorthite 2.76 4.5 1.58

Akermanite 2.95 10.3 1.64
Spinel 3.58 8.2 1.72
B 1215 Anorthite 2.76 4.5 1.58
Corundum 4.05 7–8 1.76
C 1230 Anorthite 2.76 4.5 1.58
4958 S. Ke et al. / Ceramics International 39 (2013) 4953–4960

Fig. 7. Pore structures of samples A, B and C fired at 1200 1C, 1215 1C and 1230 1C respectively.

Fig. 8. SEM images of the fracture surface of samples A, B and C fired at 1200 1C, 1215 1C and 1230 1C respectively.

and C can be matched with applicable glaze easily. Moreover, anorthite-based ceramic were compared with commercially
this relatively low TEC also indicates that the materials would produced bone china. The color difference values (an, bn) and
be very resistant to being thermally shocked. the Ln parameters (whiteness) are represented in Table 6. The
In modern technology for the production of vitrified an parameter reflects the scale extending from green ( an) to
porcelainware, particularly for tableware, greater attention is red (þ an), while the bn parameter reflects the scale extending
paid to the whiteness of porcelain body [38]. In the present from blue ( bn) to yellow (þ bn). It can be seen that negative
study, the color of fired body was measured using a spectro- value of an and positive value of bn were measured from all
meter used in the reflection mode. The Lnanbn system was samples, indicating that the values lie in the upper left
chosen for this study because it best quantifies color as quadrant (green and yellow region) with coordinates. A lower
perceived by the human eye [39]. As is known to all, bone value of an and bn on sample C indicates that there is very low
china has the most excellent appearance such as translucency coloring grade. Meanwhile, the degree of whiteness of sample
and whiteness [40]. In order to explain quantitatively the effect C can reach  94, which is the highest of all the samples due
on the degree of whiteness, the values of three types of to the lowest content of coloring impurities such as Fe2O3 and
 S. Ke et al. / Ceramics International 39 (2013) 4953–4960 4959

phases. For sample C, there is only one crystalline phase and

the anorthite crystal has a refractive index value of 1.58 [9],
which is close to that of the glass phase. So, sample C shows
excellent translucency behavior which could achieve a high-
quality decorative effect similar to bone china. On the
contrary, the relatively larger difference in refractive index
[42] could cause a negative effect on the translucency behavior
of samples A and B because of the presence of multiphase.

4. Conclusions

Anorthite-based porcelains were prepared by using three

different CaO sources including dolomite, wollastonite and
calcite. Effect of different CaO sources on the microstructure
and technological properties such as sintering behavior,
flexural strength, thermal expansion and appearance quality
Fig. 9. Thermal expansion ratio curves of samples A, B and C measured
in the range from 30 to 500 1C. was investigated. The experimental results showed that the
microstructure and property of porcelain were affected by
different CaO sources.
Table 5 Anorthite was the primary crystalline phase in all samples
Average TEC values of samples A, B and C measured in the range from
fired at optimum sintering temperatures (1200, 1215 and
30 to 500 1C.
1230 1C). Anorthite as the single crystalline phase was only
Temperature (1C) Thermal expansion coefficient, a  10  6(K  1) generated from the sample including calcite and the single
anorthite porcelain possessed high crystalline to glassy phase
A B C
ratio. The sample containing dolomite easily formed substan-
30–100 6.2748 4.4888 4.6472 tial glassy phase due to the existence of magnesium element.
30–200 6.9009 4.9382 4.8745 The maximum flexural strength could reach  110 MPa when
30–300 7.2094 5.1233 4.9142 the source of CaO was wollastonite, which was attributed to
30–400 7.4943 5.3458 5.0601
30–500 7.8267 5.4822 5.1189
relatively advantageous microstructure.
When the source of CaO was wollastonite or calcite, the
anorthite-based porcelain has low thermal expansion coeffi-
Table 6 cient due to formation of substantial anorthite phase, which
Lnanbn parameters of samples A, B, C and bone china. could be matched with applicable glaze easily. The single
anorthite porcelain had high whiteness (Ln ¼ 94). Moreover,
Sample code Color coordinate
the relatively low refractive index value between anorthite and
Ln an bn glassy phase would facilitate the attainment of high translu-
cency behavior, which was similar to bone china in
A 92.59  1.47 4.31 appearance.
B 91.01  0.89 4.86
C 94.37  0.54 1.92
Bone china 93.15  0.43 3.17 Acknowledgments

This work was supported by the Major Scientific and

TiO2 for raw materials. Moreover, a lower glassy phase
Technological Projects of Guangdong Province (No.
formed in sample C may be another reason for high whiteness.
2010A080804001) and the ChanXueYan Special Funds of
The literature [13] has also explained that the glassy phase had
Guangdong (No. 2011B090400201).
a negative effect on the increase in whiteness of anorthite-
based stoneware. Therefore, sample C has a higher appearance
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