Applied Clay Science 143 (2017) 430–436

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Applied Clay Science

journal homepage: www.elsevier.com/locate/clay

Research paper

Performance enhancement of the ceramic products by adding the sand, MARK

chamotte and waste brick to a porous clay from Bir Mcherga (Tunisia)
Hiba Zouaoui⁎, Jamel Bouaziz
LCI: Laboratory of Industrial Chemistry, National School of Engineering, Box 1173, Sfax University, Sfax 3038, Tunisia

A R T I C L E I N F O A B S T R A C T

Keywords: Investigations were undertaken to assess the chemical, physical and mechanical changes of porous clay and non-
Porous clay plastic clays mixtures fired between 900 and 1150 °C. Five mixtures (S1: 70 mass % clay +30 mass % chamotte,
Sand S2: 70 mass % clay +15 mass % chamotte + 15 mass % sand, S3: 70 mass % clay + 30 mass % sand, S4: 70 mass
Chamotte % clay + 30 mass % waste brick and S5: 70 mass % clay +15 mass % waste brick +15 mass % sand) from
Waste brick
Tunisia were evaluated for their possible ceramic applications. X-ray diffraction (XRD), thermal analysis (DTA/
Tensile strength
TG), dilatometry, scanning electron microscopy (SEM) and physical-mechanical analyses such as tensile
Tunisia
strength, water absorption, linear shrinkage and bulk density were used to assess the phase evolution and
microstructure of the sintered mixtures. The formations of both the anorthite and mullite phases and the vitreous
phase have improved the required ceramic product performance. S4 and S5 had the highest values of tensile
strength at 1150 °C. These mixtures, according to the European Norm EN 14411, are suggested for porcelainized
and fully vitrified stoneware. S3 sample is suitable for the production of vitrified stoneware. S1 and S2 mixtures
are suitable the production of earthenware and unglazed stoneware.

1. Introduction
Works on clayey materials are of growing interest in Tunisia.
Because of the increasing demands of national construction projects,
the Tunisian clay industry has been one of the most dynamically
developing businesses in Tunisia over the last decade (Boussen et al.,
2016). Several Tunisian localities have been investigated and few
studies have been carried out on the clays or of raw materials used
for traditional ceramic in Tunisia. For example, Mahmoudi et al. (2016)
studied the mineralogical, physic-chemical and geotechnical analyses of
representative Aptian clays from Jebel Ressas region in the north-east of
Tunisia for their use in ceramic industry. Bennour et al. (2015) studied
the mineralogical, chemical and geotechnical characterization of
Tunisian clays from Chouamekh region in south-eastern Tunisia and
their possible use in the ceramic industry. Particular attention should be
paid to the exploitation of raw materials in Bir Mcherga region from
Tunisia for ceramic products. Previous studies were carried out on the
chemical and mineralogical compositions and on the thermal behavior
of this clay (Krichen et al., 2009). This study revealed that this clay raw
materials seemed to be relatively poor in phyllosilicates (44 mass%)
and rich in quartz (25 mass%), carbonates (20 mass%) and goethite (7
mass%). Even after sintering for 4 h at 1150 °C, the clay shows the
presence of an important porosity. Because of its lower bulk density
value and to order to obtain the required ceramic product performance,
this clay should be amended with non-plastic materials.
The aim of this paper was to evaluate the ceramic properties of
Tunisian clay from Bir Mcherga region mixed with non-plastic minerals
such as the sand, the waste brick and the chamotte in order to improve
their physical and mechanical properties. The possible ceramic applica-
tions of five clay and non-plastic minerals mixtures (S1, S2, S3, S4 and
S5) from Tunisia were investigated. In order to optimize the production
process and enhance the quality of the final products, a correlation
between tensile strength, bulk density, linear shrinkage and water
absorption is performed according to the sintering temperature and the
nature and the amount of the non-plastic clay materials.
2. Experimental
2.1. Materials
The studied clay was selected from Bir Mcherga (North Tunisia); it
mainly contains illite (23 mass%), montmorillonite (10 mass%),
kaolinite (11 mass%), quartz (25 mass%), calcite (8 mass%), dolomite
(12 mass%) and goethite (7 mass%) (Krichen et al., 2009). The non-
plastic minerals are waste brick, chamotte and sand which were
supplied respectively by CARTHAGO CERAMIC S.A, CHEMI-PHARMA

⁎
Corresponding author.
E-mail address: hibazouaoui@hotmail.com (H. Zouaoui).

http://dx.doi.org/10.1016/j.clay.2017.04.015
Received 30 November 2016; Received in revised form 11 April 2017; Accepted 12 April 2017
Available online 28 April 2017
0169-1317/ © 2017 Elsevier B.V. All rights reserved.
H. Zouaoui, J. Bouaziz Applied Clay Science 143 (2017) 430–436

Table 1
Chemical composition (mass %) of clay (Krichen et al., 2009) and non-plastic clay.

Oxides Al2O3 SiO2 K2 O MgO CaO Fe2O3 Mn2O3 Na2O TiO2 ZnO SO2 P2O5 L.O.I* Total

Clay 15.18 46.51 2.68 3.22 8.62 6.62 0.11 0.84 0.69 0.38 – – 15 99.86
Waste brick 12.79 59.36 4.03 1.15 4.79 12.87 – 1.41 – – 0.48 1.1 2 99.98
Chamotte 34.65 62.53 1 – – – – 0.68 – – 0.35 0.32 0.43 99.96
Sand 0.93 94.58 0.29 – – – – 3.81 – – – – 0.36 99.97

* Loss of Ignition at 1200 °C.

and CTMCCV. The chemical composition, determined by ICP analysis,
is summarized in Table 1. The major elements present in the clay are
the SiO2 and Al2O3. The quantity of Fe2O3 and CaO are significant
while K2O, Na2O and MgO are present in relatively minor amounts. The
chemical composition of the sand shows that the major constituent is
SiO2 as expected, while Na2O appears as the main associated oxide.
The major elements present in the waste brick are SiO2, Fe2O3 and
Al2O3. The amounts of CaO and K2O are higher than those of MgO,
Na2O and P2O5 (in relatively minor amounts). The major elements
present in the chamotte are Al2O3 and SiO2.
The XRD diagrams of the clay and the non-plastic constituents are
represented in Fig. 1. The characteristic peaks of the minerals that have
been identified are indicated on the diagram. The Waste brick is mainly
constituted of anorthite, hematite and quartz, while the sand is
constituted only of quartz phase and the chamotte is made up of
mullite, cristobalite and quartz.
2.2. Preparation of mixtures and ceramic products
clay, the following composition has been investigated: 70 mass% clay
with 30 mass% of non-plastic mineral materials. Table 2 summarizes
the composition of the various samples. The mixtures were homoge-
nized by humid way according to the following experimental protocol:
• The powders were dispersed in distilled water by mechanical
agitation for 5 min;
• The water was evaporated progressively under continuous agitation
at 110 °C until getting a dough;
• The dough was dried at 110 °C during 24 h;
• The homogeneous mixture clods were finally ground using a mortar.
The obtained powders were dried pressed at 150 MPa. Cylindrical
pellets were produced with dimensions suitable for the Brazilian test
(20 mm diameter and 5 mm thickness). The specimens were then fired
in an electric furnace between 900 and 1150 °C using heating and
cooling rates of 10 °C/min and 12 min dwell time at maximum
temperature.

The raw materials were crushed, ground finely (< 63 μm) and 2.3. Method
heated for two hours at 350 °C for the organic complete combustion.
According to the great amount of quartz already present in the starting X-ray diffraction (XRD) of the powder was carried out by means of a

M Q

M
M M
C
C M
M
Q M
M C Q
M Q C M M
M M M

Q
Q

Q
A Q Q
H A AQ Q Q
A A H H Q Q Q
Q QQ Q Q Q

Fig. 1. XRD diffractograms of the clay (a) (Krichen et al., 2009), the chamotte (b), the waste brick (c) and the sand (d). Legend: Kaol: kaolinite, I: illite, Mt.: montmorillonite, D: dolomite,
C: calcite, Q: quartz, A: anorthite, H: hematite, M: mullite and C: cristobalite.

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H. Zouaoui, J. Bouaziz Applied Clay Science 143 (2017) 430–436

Table 2
Sample composition (mass %).

Sample label Clay Waste brick Sand Chamotte

S1 70 – – 30
S2 70 – 15 15
S3 70 – 30 –
S4 70 30 – –
S5 70 15 15 –

powder diffractometer “D8 Bruker Advance” using Kα1 radiation of Cu Fig. 3. Linear shrinkage versus temperature of S1, S2, S3, S4 and S5 (heating and cooling
rates of 10 °C/min).
(λ = 0.15406 nm). XRD experiments were achieved in step-scan mode
from 15° to 55° (2θ). Quantification of the different phases was carried
out using the computer program X'-pert High Score. ing under a constant dry air flow at a heating rate of 10 °C/min between
A Perkin Elner 8300 DV ICP-AES plasma torch was used to measure room temperature and 1200 °C. Previously fired alumina was used as
the major and trace elements in the sample. The sample was previously the reference material for all experiments.
dissolved within an acidic solution using a microwave device under Thermal expansion-shrinkage of the powder compact (6 mm dia-
appropriate pressure and temperature cycles. meter and 5 mm thickness) pressed at 25 MPa was measured with a
The thermal analyses (DTA/TG) of 64 mg of the relevant powdered dilatometer “SETARAM Setsoft 2000 apparatus” at a heating rate of
sample were realized using a “SETARAM Setsys 24”apparatus, operat- 10 °C/min between room temperature and 1150 °C, under dry air
atmosphere. Scanning electron microscopy was performed on the flat

0 100 200 300 400 500 600 700 800 900 1000 1100 1200 0 100 200 300 400 500 600 700 800 900 1000 1100 1200
0 2 1
EXO 2 T (°C) T (°C)
EXO 1 0
-1
1 0
-1
-2 -1
0
-2
-3 -2
-1
-3
DTA (µV)

-3
DTA (µV)

TGA (%)
TGA (%)

-4
-2 -4 -4
-5 -5
-3 -5
-6
-4 -6
-6
-7
-5 -7 -7
-8

-6 -8 -9 -8

(a) (b)
0 100 200 300 400 500 600 700 800 900 1000 1100 1200
2 0
EXO T (°C)
0 -1

-2
-2

-3
-4
DTA (µV)

DTG (%)

-4
-6
-5
-8
-6

-10
-7

-12 -8

(c)

0 100 200 300 400 500 600 700 800 900 1000 1100 1200 0 100 200 300 400 500 600 700 800 900 1000 1100 1200
2 0 2 1
EXO T (°C) EXO 0 T (°C)
0 -1 0

-2 -2
-2 -1
-4 -4
-3
-2
-6 -6
-4
-3
DTA (µV)

-8
DTA (µV)

TGA (%)

-8
TGA (%)

-5
-10 -10 -4
-6
-12 -12
-5
-7 -14
-14
-6
-16 -8 -16

-9 -18 -7
-18

-20 -10 -20 -8

(d) (e)
Fig. 2. DTA/TG diagrams of (a): S1, (b): S2, (c): S3, (d): S4 and (e): S5 (heating rate: 10 °C/min).

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H. Zouaoui, J. Bouaziz Applied Clay Science 143 (2017) 430–436

Q A
Q
A
Q
A Q C
C A Au A
Q M M H Au M A M Au A M H Q Q QM Q Q AQ A A Au Q
M A Au M Q Q M QA A Q AA Au

Q A M Q QA Q
M I C A A G M MH Q Q M Q M I C M A G M HQ Q QM Q Q I

Q
A Q
A H Au AA HQ QQ Au Q A Q

Q
I A H A G HQ QQ Q Q Q I

A Q
A Q
H
A H Au A Au A Q A
Q A A A Au Au A Q Q Au Q A AA A AA AA Au A A H A Au A A A A H Q Q Q AA A Au
A Au
Q Q

Q Q
I A H A A A G HQ QQ Q Q Q I I A H A A A G HQ QQ Q Q Q I

Fig. 4. XRD diagrams for S1 (a), S2 (b), S3 (c), S4 (d) and S5 (e) sintered at 900 °C and 1150 °C. Legend: Q: quartz, I: illite, H: hematite, A: anorthite, M: mullite, C: cristobalite, Au: augite,
G: gehlenite.

polished surface to ensure investigation on the real bulk structure of the the linear shrinkage in percentage.
sintered products. The water absorption values were measured (4 pellets for each
The microstructure was analyzed using the “CAMBRIDGE S260 experimental point) from the difference between the dry and the water
Scanning Electron Microscopy (SEM)” working with 15KV accelerating saturated fired bodies according to the standards (NT 28.27).
voltage. The samples were coated with a gold layer for more electronic The bulk density was determined (4 samples for each experimental
conductivity. point) using a density analyzer instrument type Micromeritics AccuPyc
The mechanical properties of the fired samples were assessed using II 1340. The measurement of bulk density was performed on the
a compressive test. The Brazilian test was used to measure the tensile samples after 24H in an oven at 110 °C.
strength of the sintered compacts (ISRM, 1978; ASTM, 1984). Brazilian
tests consist of crushing a bedded cylindrical specimen between two
crushing plates. The usual way of evaluating the tensile strength (MPa) 3. Results and discussion
from the diametrical compression test is through the following equation
(Elliott, 1994): 3.1. Thermal behavior and phase evolution of the mixtures
σr = (2∗P) (π∗D∗t)
The DTA-TG analysis curves of S1, S2, S3, S4 and S5 are illustrated
where P is the maximum applied load (N), D the diameter (mm) and t in Fig. 2. The endothermic peaks near 90 °C and 165 °C are related to
the thickness of the sample (mm). the removal of adsorbed and interlayer water (Baran et al., 2001). This
The tensile strength is calculated on the assumption that failure is is confirmed by the first mass loss event (0.8, 0.9, 0.9, 1.1 and 0.9 mass
initiated at the point of maximum tensile stress (Fairhurst, 1964). The % for S1, S2, S3, S4 and S5, respectively). The dehydroxylation of
influence of the sample diameter, D, and the thickness, t, on the failure kaolinite is well evidenced by the endothermic phenomenon observed
stress was studied for compacted powder (Dorémus et al., 2001). at around 530 °C (Hajaji et al., 2002) with a mass loss of 1.6, 1.7, 1.8, 2
According to this study, the ratio t/D ≤ 0.25 ensures plane stress and 1.8 mass % for S1, S2, S3, S4 and S5, respectively. The endothermic
conditions. The tensile strength was determined (4 samples for each effect which occurred at 573 °C can be attributed to the transformation
experimental point) using Lloyd EZ50 apparatus on cylindrical samples of quartz α to quartz β (Manaoharan et al., 2012). The decarbonation of
of approximately 5 mm in thickness and 20 mm in diameter. the calcite and dolomite phases is characterized by an endothermic
For the linear shrinkage, the diameter of the specimens was peak between 650 and 850 °C and a mass loss of 4.9, 4.7, 4.6, 4.9 and
measured (4 pellets for each experimental point) before and after firing 3.8 mass% for S1, S2, S3, S4 and S5, respectively. The exothermic peaks
using an electronic caliper. The resulting values are used to calculate observed near 900 and 920 °C are related to the crystallisation of the

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H. Zouaoui, J. Bouaziz
Fig. 5. Physical and mechanical properties of fired products: (a) linear shrinkage (%), (b) bulk density (g/cm3), (c) tensile strength (MPa) and (d) water absorption (%).
gehlenite (CaAl2SiO7) and the anorthite (CaAl2Si2O8), respectively
(Traore et al., 2003). The endothermic peak characteristic of the second
step of the illite dehydroxylation which occurs at 900 °C is not seen
(Gualtieri and Ferrari, 2006).
The dilatometric behavior observed of the studied samples (Fig. 3)
show that all these mixtures display a slight expansion followed by a
shrinkage between room temperature and 100 °C, which can be
attributed to the diminution of adsorbed water. The expansion observed
between 550 and 600 °C corresponds to the polymorphic α-β transition
of quartz (at 573 °C) (Baccour Zghal et al., 2012) and to the dehydrox-
ylation of clay (Ben M'barek Jemai et al., 2015). The expansion
observed between 600 and 850 °C begins during the CO2 departure. It
can be related to the volume change associated to the decomposition of
the dolomite and calcite phases. The shrinkage observed between 860
and 960 °C is characteristic of structural reorganisation. The rapid
densification observed above 1080 °C should be related to a vitreous
phase-type sintering.
The XRD patterns of S1, S2, S3, S4 and S5 treated at 900 and
1150 °C are presented in Fig. 4. The crystalline phases identified in both
S1 and S2 fired at 900 °C are quartz, illite, anorthite, gehlenite,
hematite, mullite and cristobalite. The crystalline phases identified in
S3 are quartz, illite, anorthite, gehlenite and hematite, while those
identified in both S4 and S5 at 900 °C are quartz, illite, anorthite,
gehlenite and hematite. After firing at 1150 °C, illite and gehlenite are
not detected and the augite peaks appear. The amount of residual
quartz decreases with increasing temperature due to consumption by
ongoing mineral reactions. Anorthite, hematite and mullite peaks
intensities start to increase, while quartz correlates negatively and
decreases.
3.2. Physical and mechanical properties of the mixtures
Results of the mechanical and physical properties of the fired
products (Fig. 5) indicate that all the mixtures present a moderate
change in the fired properties from 900 to 1050 °C. Above 1050 °C, the
linear shrinkage is up to 0.6% (Fig. 5a). Fig. 5b reveals that the bulk
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Applied Clay Science 143 (2017) 430–436
density remains almost constant between 900 and 1050 °C (1.8–1.96 g/
cm3). This is compatible with the low tensile strength (Fig. 5c) and with
the high porosity as observed from SEM micrographs (Fig. 6). However,
above 1100 °C, significant changes can be observed such as an increase
in the linear shrinkage, bulk density and tensile strength together. This
enhancement can be explained by the densification of the samples. The
densification is directly correlated to the sintering temperature which is
a determinant parameter affecting the mechanical resistance of the
ceramic products. This is due to the progressive formation of the
calcium silicates and the vitreous phase that fills the open porosity. The
addition of waste brick and chamotte enhanced the mechanical proper-
ties of the materials. In fact, this is due to the formation of strong phases
helping to reinforce the tensile strength of the materials such as the
anorthite and the mullite (Li et al., 2012; Ndjigui et al., 2016; Traore
et al., 2003). Fig. 5d shows the evolution of the products water
absorption upon firing. Water absorption ranges from 13.44–14.78%
at 900 °C to 0.09–13.24% at 1150 °C. At 1150 °C, the lowest water
absorption is registered for S4 and S5 (0.09 and 0.1%), while the
highest is measured in S1and S2 samples (13.24 and 11.6%). Mean-
while, water absorption shows an opposite trend relative to the bulk
density (Fig. 5b) which ranges from 1.81–1.92 g/cm3 at 900 °C to
1.9–2.33 g/cm3 at 1150 °C. S4 has the highest bulk density values and
this is in accordance with high tensile strength values due to vitrifica-
tion. According to the European Norm EN 14411, at tempera-
tures ≤ 1100 °C, all the mixtures belong to the BIII group (water
absorption > 10%) which are suitable for the production of earth-
enware and unglazed stoneware except S3 fired at 1100 °C (water
absorption = 5.8%) which belongs to the BIIa group and is promising
for the production of stoneware. At 1150 °C, S3 mixture with water
absorption = 0.6% belong to BIb group which is suitable for the
production of vitrified stoneware, S4 and S5 mixtures (water absorp-
tion ≤ 0.5%) belong to the BIa group which are suggested for
porcelainized and fully vitrified stoneware while the S1 and S2
mixtures belong to the BIII group which are suitable for the production
of earthenware and unglazed stoneware.
H. Zouaoui, J. Bouaziz Applied Clay Science 143 (2017) 430–436

a b

c d

e f

g h

i j
Fig. 6. Microstructure of fired products: S1 (a) (900 °C), (b) (1150 °C); S2 (c) (900 °C), (d) (1150 °C); S3 (e) (900 °C), (f) (1150 °C); S4 (g) (900 °C), (h) (1150 °C) and S5 (i) (900 °C), (j)
(1150 °C).

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H. Zouaoui, J. Bouaziz
3.3. Microstructure of the mixtures
Fig. 6 shows the scanning electron microscopy images of the
ceramic bodies fired at 900 and 1150 °C for 12 min. SEM micrographs
show the progression of improved densification with increasing tem-
perature. At 900 °C, the SEM images are typical illustrations of the
heterogeneous microstructures and the existence of large pores within
the samples. High porosity is related to dense zones resulting from
carbonate decomposition with the evolution of CO2. Porosity decreases
significantly after vitrification (1080 °C). The presence of alkaline-rich
phase quantities (K2O, Na2O) in the fired samples accelerates the
vitrification process due to the fluxing effect of these oxides. The
amorphous silica liberated during the metakaolin decomposition could
also give rise to a vitreous phase formation. This phase tends to
approach the particles and therefore the open porosity decreases and
the closed porosity increases when the temperature is increased. The
closed porosity is due to larger, isolated and spherical pores. At
1150 °C, in agreement with the sintering process, the bodies presented
a more densified microstructure. In this state, the open porosity has
been reduced and spherical isolated pores can be observed, which could
explain the great advance in mechanical properties with decrease in the
pore fraction (Sousa and Holanda, 2005). The SEM images of S1 and S2
mixtures show that the bodies present a high porosity, which can be
explained by the insufficient of the vitreous phase quantity to fill all the
pores. This is compatible with the high water absorption values of these
samples.
4. Conclusion
At 900 °C, XRD analyses show that the major products are anorthite,
gehlenite, augite and hematite phases. At this temperature, the sinter-
ing process is not complete, so the ceramic pieces are still quite porous
due to calcite and dolomite decarbonation. The presence of fluxing
agents favors the vitrification of the ceramic bodies. However, the rapid
densification observed above 1080 °C should be related to a vitreous
phase-type sintering. At 1150 °C, the illite and gehlenite peaks are not
seen and the densification is better. The physical mechanical properties
of the fired products are enhanced with the increase of the firing
temperature. This result is explained by the formation of the vitreous
phase which helps to reduce porosity and by the formation of a new
phases relative to anorthite, augite and mullite which are a strong
phases helping to improve the mechanical properties. The red color of
the ceramic bodies is attributed to the presence of hematite. The
presence of quartz phase helps to reduce the firing shrinkage. The
results show that S4 and S5 sintered at 1150 °C for 12 min exhibits both
a better tensile strength (23.8 and 23.1 MPa, respectively) and a high
densification. According to the European norms (EN 14411), all the
mixtures are promising for the production of earthenware and unglazed
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Applied Clay Science 143 (2017) 430–436
stoneware at temperatures ≤ 1100 °C (E > 10%) except S3 sintered at
1100 °C (E = 5.8%) which is suitable for the production of stoneware.
At 1150 °C, S4 and S5 are suggested for porcelainized and fully vitrified
stoneware thanks to their low water absorption (0.09 and 0.1%,
respectively). S3 sample is suitable for the production of vitrified
stoneware (E = 0.6%), S1 and S2 mixtures (13.24 and 11.6%, respec-
tively) are suitable for the production of earthenware and unglazed
stoneware.
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