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Geopolymers For Kaolin
Geopolymers For Kaolin
H OSTED BY
Universit de Yaound 1, Laboratoire de Chimie Inorganique Applique, Facult des Sciences, B.P. 812, Yaound, Cameroon
Universit de Toulouse, Laboratoire Matriaux et Durabilit des Constructions, INSA/UPS Gnie Civil, 31077 Toulouse CEDEX 04, France
Universit de Douala, Laboratoire de Chimie Bio-Inorganique, Analytique et Structurale, Facult des Sciences, B.P. 24157, Douala, Cameroon
a r t i c l e
i n f o
Article history:
Received 7 September 2014
Received in revised form
18 November 2014
Accepted 2 December 2014
Available online 20 December 2014
Keywords:
Rate
Calcination
Residual kaolin
Metakaolin
Setting time
Compressive strength
a b s t r a c t
Kaolin samples of the same mass were treated at 700 C for the same duration of 30 min by varying the rate
of calcination (1, 2.5, 5, 10, 15 and 20 C/min) in order to obtain metakaolins which were used to produce
geopolymers. Depending on the nature of each type of material, kaolin, metakaolins and geopolymers
were characterized using thermal analysis, chemical analysis, XRD, FTIR, particle size distribution, specic
surface area, bulk density, setting time and compressive strength. FTIR and XRD analyses showed that
metakaolins except at 1 C/min contained residual kaolinite whose quantity increased with the rate of calcination of kaolin and which inuenced the characteristics of geopolymers. Thus as the rate of calcination
of kaolin increased, the setting time increased (226 min (rate of 1 C/min)773 min (rate of 20 C/min))
while the compressive strength reduced (49.4 MPa (rate of 1 C/min)20.8 MPa (rate of 20 C/min)). From
the obtained results the production of geopolymers having high compressive strength along with low
setting time requires that the calcination of kaolin be carried out at a low rate.
2014 The Ceramic Society of Japan and the Korean Ceramic Society. Production and hosting by
Elsevier B.V. All rights reserved.
1. Introduction
The term geopolymer refers to inorganic aluminosilicate
polymers. These materials nd applications in areas such as construction and civil engineering [13], encapsulation of certain toxic
waste [47], removal of certain heavy metal cations from aqueous solutions [68] or the development of biomaterials [9]. These
inorganic polymers are generally obtained by polymerization reaction between aluminosilicate and strongly basic alkaline solution
[10]. Aluminosilicate raw materials commonly used for the synthesis of geopolymers are y ash, blast furnace slag, volcanic ash
or metakaolin [1,4,11,12]. The variability of chemical composition of y ash, blast furnace slag or volcanic ash usually leads
to geopolymers whose physical and mechanical properties vary
from one aluminosilicate raw material to another [7,11]. Regarding
metakaolin, the characteristics of resulting inorganic aluminosilicate polymers depend on the conditions of calcination of kaolin
Corresponding author. Tel.: +237 677 612 623; fax: +237 222 234 496.
E-mail address: aelimbi2002@yahoo.fr (A. Elimbi).
Peer review under responsibility of The Ceramic Society of Japan and the Korean
Ceramic Society.
http://dx.doi.org/10.1016/j.jascer.2014.12.003
2187-0764 2014 The Ceramic Society of Japan and the Korean Ceramic Society. Production and hosting by Elsevier B.V. All rights reserved.
B.B. Kenne Diffo et al. / Journal of Asian Ceramic Societies 3 (2015) 130138
131
FTIR, XRD were performed on kaolin, metakaolins and geopolymers. The setting time and compressive strength were determined
as well on geopolymers.
2. Materials and methods
2.1. Materials processing
Metakaolins used in this study were obtained from kaolin provided by the NUBRU HOLDING Group which is involved in the
valorization of certain local raw materials in Cameroon. Before
being used, the kaolin was enriched with kaolinite by the sedimentometry process based on Stokess law [18]. The clay fraction
obtained labeled as K was rst maintained at ambient laboratory
temperature for a week, cured at 105 C until its mass became constant and then it was ground and sifted through a sieve of mesh
90 m. The resulting material was calcinated at 700 C, the choice
of this temperature being based on the work of Elimbi et al. [11].
Soaking of a mass of 1.5 kg of K at 700 C in an electric mufe furnace on ceramic plates (Nabertherm Mod LH 60/14) lasted 30 min
at the following rates of calcination: 1 C/min, 2.5 C/min, 5 C/min,
10 C/min, 15 C/min and 20 C/min. The obtained metakaolins
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Table 1
Bulk density and specic surface area of metakaolins.
Metakaolin
MK1
MK2.5
MK5
MK10
MK15
MK20
2.54 0.02
128,710
2.54 0.02
128,200
2.54 0.02
129,480
2.56 0.02
125,490
2.54 0.02
128,720
2.5 6 0.02
127,790
B.B. Kenne Diffo et al. / Journal of Asian Ceramic Societies 3 (2015) 130138
133
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Table 2
Chemical compositions (mass%) of metakaolins.
Chemical composition
SiO2
Al2 O3
CaO
MgO
Fe2 O3
Na2 O
K2 O
TiO2
SO3
Loss on ignition
Total
SiO2 /Al2 O3 (molar ratio)
Metakaolin
MK1
MK2.5
MK5
MK10
MK15
MK20
54.60
40.60
0.12
0.22
0.53
0.12
0.53
0.57
0.01
2.26
99.57
2.28 0.01
53.60
39.86
0.11
0.22
0.52
0.11
0.52
0.56
0.01
5.11
100.64
2.28 0.01
52.50
39.04
0.11
0.21
0.51
0.11
0.51
0.55
0.01
6.92
100.49
2.28 0.01
52.10
38.74
0.11
0.21
0.51
0.11
0.51
0.54
0.01
6.93
99.78
2.28 0.01
52.00
38.67
0.11
0.21
0.51
0.11
0.51
0.54
0.01
6.95
99.62
2.28 0.01
51.40
38.22
0.11
0.21
0.50
0.11
0.50
0.53
0.01
7.73
99.34
2.28 0.01
B.B. Kenne Diffo et al. / Journal of Asian Ceramic Societies 3 (2015) 130138
135
at 1114 and 1025 cm1 and then at 998 and 789 cm1 expressed
respectively the vibrations of Si O Si and Si O Al groups of the
network. The bands at 908 and at 789 cm1 indicated the presence
of the stretching vibration of Al OH with Al in coordination VI. The
band at 522 cm1 indicated the vibrations of Si O Si and Si O Al
groups of the network.
3.1.2. Characteristics of metakaolins
Thermal treatment of kaolin generally causes transformations
which effects are among other things increasing of specic surface area and average particle grain size [20]. From Table 1 it
was clear that the variation of the rate of calcination of kaolin
had no signicant effect on the bulk density of metakaolins. As
for the specic surface area of metakaolins, an outline observation on the different values did not allow to draw meaningful
conclusion on the effect of the rate of calcination of kaolin. According to the curves of Figs. 1 and 5, metakaolins and powder of K
almost exhibited the same particle size distribution tendency. The
chemical composition (Table 2) showed that the mass percentages of SiO2 and Al2 O3 decreased contrary to the loss on ignition.
This meant that when the rate of calcination of kaolin increased,
the minerals in the kaolin (e.g. gibbsite and kaolinite) were less
decomposed and led to a lower production of active compounds
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during the heating of kaolin, kaolinite dehydroxylation, metakaolinite structure change, exothermic structural organization along
with mullite formation are very sensitive to the heating temperature rate. In particular, the lower the rate of calcination of kaolin,
the lower is the temperature of commencement of dehydroxylation
of kaolinite [15]. Accordingly, when kaolin was calcined at 700 C
for the same soaking time, kaolinite was more dehydroxylated for
a low heating rate. FTIR spectra of metakaolins (Fig. 7) also conrmed that except for MK1 , metakaolins contained kaolinite. In fact
the absorption bands assigned to kaolinite (36883648, 3619, 908
and 788 cm1 ) were observed in the spectra of MK2.5 MK20 . Conversely, the FTIR spectrum of MK1 was mainly characterized by the
band at 1046 cm1 which corresponded to stretching vibration of
Si O Si and Si O Al groups of the metakaolin network [26].
3.2. Characterization of geopolymers
3.2.1. XRD
The X-ray diffractograms of geopolymer pastes (Fig. 8) showed
the presence of all the crystalline phases initially encountered
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137
4. Conclusion
Metakaolins obtained at 700 C for the same duration (30 min)
by varying the rate of calcination (120 C/min) of samples of equal
mass of kaolin were used to produce geopolymers. Chemical analysis of metakaolins revealed that loss on ignition increased with
the rate of calcination of kaolin. This resulted from the presence
of residual kaolinite in metakaolins and whose quantity increased
with the rate of calcination of kaolin. XRD and FTIR analyses of
geopolymers also revealed the presence of residual kaolinite. Thus
the synthesis of geopolymers was affected by both amorphous
phase and quasi no residual kaolinite of metakaolins. This simultaneous effect impacted on the setting time and the compressive
strength: the setting time increased while the compressive strength
fell away. To produce geopolymer having low setting time and
high mechanical strength, the calcination of kaolin needs to be
performed at a low speed.
Acknowledgments
One of us (B.B. Kenne Diffo) is delighted to acknowledge the
French Government for granting a scholarship for PhD studies
through the Service de la Coopration et dAction Culturelle
(SCAC) of the Embassy of France in Cameroon and the staff of the
Laboratoire Matriaux et Durabilit des Constructions (LMDC) for
the reception and infrastructural support he received during his
stay at INSAUPS Toulouse (France). Also, nancial supports from
the Bureau Afrique Centrale et des Grands Lacs de lAgence Universitaire de la Francophonie (BACGL-AUF) under the grant N S0020
*** 10406 and The World Academy of Sciences (TWAS) under the
grant N 13-018 RG/CHE/AF/AC G - UNESCO FR: 3240277723 are
acknowledged.
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Fig. 11. Relation between compressive strength (geopolymers) and loss on ignition
(metakaolins).
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