Arab J Sci Eng

DOI 10.1007/s13369-014-1314-1

RESEARCH ARTICLE - CIVIL ENGINEERING

Advantages of Applying a Steam Curing Cycle for the Production

of Kaolinite-Based Geopolymers
Arwa Hamaideh · Kostas Komnitsas ·
Muayad Esaifan · Juma’a K. Al-Kafawein ·
Hubert Rahier · Mazen Alshaaer

Received: 7 October 2013 / Accepted: 28 February 2014

© King Fahd University of Petroleum and Minerals 2014

Abstract In this study, a new approach, which involves the
application of a steam curing cycle for the production of
kaolinite-based geopolymers, is investigated. This approach
aimed to accelerate geopolymeric reactions and eliminate the
content of residual alkalis within the geopolymer mass and
the formation of efflorescence at the surface of the speci-
mens, thus increasing their mechanical strength. The exper-
imental procedure involved initial curing followed by steam
curing for different periods, up to 24 h. The mineralogy and
the morphology of the produced specimens were determined
using X-ray diffractometry, scanning electron microscopy
and energy-dispersive X-ray spectroscopy. Thermogravimet-
ric analysis was also used. The physical and mechanical
properties of the final products were determined for dry
and immersed in water specimens and involved compres-
sive strength, bulk density, water absorption and shrinkage.
Finally, the effect of steam curing on the presence of resid-
ual alkalis and the formation of water-soluble salts during
geopolymerization was investigated.
Keywords Geopolymers · Steam curing cycle · Kaolinite

A. Hamaideh
Water, Energy and Environment Center, University of Jordan,
11942 Amman, Jordan

K. Komnitsas
School of Mineral Resources Engineering, Technical University
Crete, 73100 Chania, Greece

M. Esaifan
Department of Mechanics of Materials and Constructions
(MEMC), Vrije Universiteit Brussel (VUB), Pleinlaan 2,
1050 Brussels, Belgium

J. K. Al-Kafawein
Department of Chemistry, King Faisal University, P.O. Box 380,
Al Hofuf 31982, Kingdom of Saudi Arabia

H. Rahier
Department of Physical Chemistry and Polymer Science, Vrije
Universiteit Brussel (VUB), Pleinlaan 2, 1050 Brussels, Belgium

M. Alshaaer
Department of Physics, Salman Bin Abdulaziz University,
Al-Kharj, Kingdom of Saudi Arabia
1 Introduction
M. Alshaaer (B)
Deanship of Academic Research, University of Jordan,
Amman 11942, Jordan It is known that through chemical polymerization, alu-
e-mail: mazen72@yahoo.com minosilicates such as clays can be hardened and trans-

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formed within a short period of time into geopolymers [1,2].
Geopolymers consist of an amorphous, three-dimensional
network resulting from the polymerization of aluminosilicate
monomers, i.e., orthosilicate ions, with the use of an alkaline
solution [3,4]. Although numerous studies have been car-
ried out to elucidate kinetics and solution chemistry, some
mechanisms still remain unclear [5–7]. Geopolymers are
solid, hard and stable materials similar to hydroxysodalite,
feldspathoid or zeolite [8–10]. These materials, which may
be partially amorphous or microcrystalline, consist of SiO4
and AlO4 tetrahedra linked alternately by sharing all oxygen
atoms. When aluminum is four coordinated to oxygen atoms,
a negative charge is developed, and therefore, the presence
of cations, such as Na+ , K+ , Li+ , Ca2+ , Ba2+ , NH+ 4 and
+
H3 O , is essential to balance this charge [11].
Kaolinite-based geopolymers are ideal construction mate-
rials since they can be produced easily at local scale, are quite
cheap and may satisfy to a certain degree housing needs of
the people in developing countries [12]. The raw material
used, namely kaolinite, is abundant and easy to extract in
all Middle East and Arab countries. This special clay min-
eral if mixed with a simple binder, compressed to obtain the
desired shape and then heated in an oven at temperatures not
exceeding 80 ◦ C, can be transformed to a geopolymer [13].
Although kaolinite-based geopolymers have several bene-
ficial properties, if compared to other commonly used con-
struction materials, they are not as widely used as anticipated
in practice. One of the main reasons for this is the lower reac-
tivity of kaolinite, compared to other aluminosilicate mate-
rials used as precursors such as fly ash or metakaolin [14–
17]. Kaolinite requires less energy during processing com-
pared to metakaolin, reacts partially with alkali solutions and
participates in geopolymerization reactions to form alkali-
activated binders, as has been well proven through NMR
studies [15]. It is also known that the compressive strength
of geopolymers decreases sharply when the alkali concen-
tration exceeds an optimum value [18]. This is due to the
presence of residual alkalis in the mass of geopolymers and
the formation of water-soluble salts. Some of these alkali
ions may also migrate to the surface of the specimens, react
with atmospheric CO2 and cause the formation of efflores-
cence. As a result of these reactions, the strength and sta-
bility of the end products decrease. Furthermore, heating of
the geopolymer pulp after casting should be carried out care-
fully in order to prevent swelling that also weakens the final
structure and thus limits the number of potential applications
[13,19].
The present study investigates and discusses a new
approach for alkali activation, involving the use of a “steam
curing cycle” (SCC), in order to overcome some of the pre-
viously mentioned limitations and improve the mechanical
and physical properties of kaolinite-based geopolymers.
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Arab J Sci Eng
Table 1 Chemical composition of kaolinite (JK)
Compound % Compound %
CaO 0.68 SiO2 48.80
Na2 O 0.21 TiO2 0.86
K2 O 1.40 Al2 O3 25.10
P2 O5 0.16 Fe2 O3 7.50
SO3 2.93 Cl 0.10
L.O.I. 12.00 MgO 0.21
2 Materials and Methods
2.1 Materials
Geopolymers were synthesized using Jordan kaolinite (JK),
silica sand and alkaline activator, namely sodium hydrox-
ide. Kaolinite with a purity of 60 % [12] was sampled from
El-Hiswa deposit, which is located in the south of Jordan
about 45 km to the east of Al-Quweira town. The deposit
contains also micro-crystalline quartz and feldspar. Prepara-
tion of kaolinite involved crushing to −425 µm using a jaw
crusher (RETCH-BB1A), oven drying at 105 ◦ C for 24 h and
homogenization for 30 min in a 50 l plastic drum. The chem-
ical analysis of kaolinite was determined by X-ray Fluores-
cence (Bruker System S4 Pioneer) and is given in Table 1. Sil-
ica sand, purchased from International Silica Industries Co.,
Jordan, is one of the most well-known inert fillers which are
used for the production of materials with cementitious prop-
erties. It has usually low price and high resistance to chemi-
cal attack. The filler is well crystalline and does not contain
impurities such as organic matter or minerals that may cause
swelling or shrinkage of the final products. Prior to use, the
silica sand was washed with dilute HCl (0.1 N) for 10 min to
remove any impurities and then sieved to −400 µm.
NaOH solution, which was used as alkaline activator for
the dissolution of aluminosilicate phases, was prepared by
dissolving NaOH flakes of 98 % purity (Scharlau) in dis-
tilled water. The molarity of the solution was 13 M since
previous studies involving geopolymerization of aluminosil-
icates have shown that this is the optimum solution strength
[13,18].
2.2 Synthesis of Kaolinite-Based Geopolymers
Silica sand and kaolinite were dry mixed first and then added
to the sodium hydroxide solution. All reagents were mixed
for 15 min in a glass beaker under intense stirring. The pulp
was molded immediately in stainless steel cylinders (diame-
ter of 25 mm and height of 50 mm) to avoid decrease of the
workability of the paste. The pulp was compacted by apply-
ing a pressure of about 15MPa using a Carver hydraulic lab-
oratory press [13,20,21].
Arab J Sci Eng

Table 2 Experimental configuration by comparing their properties with those of the reference
Phase Curing period (h) Series ID geopolymers (S0).

S0 S4 S8 S12 S16 S20 S24

2.3 Water Absorption, Shrinkage and Compressive
I Initial curing 24 20 16 12 8 4 0 Strength of Geopolymers
II Steam curing 0 4 8 12 16 20 24
III Drying 24 24 24 24 24 24 24 Water absorption, W %, of the immersed specimens (Group
2) was determined using Eq. 1.

W % = ((Ww − Wd )/Wd ) × 100 % (1)

where Ww and Wd are the weight of the specimen before and

after immersion in water, respectively.
In order to determine the dimensional changes after curing
and thus determine shrinkage, a digital micrometer was used.
Linear shrinkage, L%, was determined using Eq. 2.

L% = ((L i − L c )/L i ) × 100 % (2)

where L i and L c are the length of the specimen before and

Fig. 1 Schematic diagram of the different curing options: reference
curing (S0), steam curing cycle (S4, S8, S12, S16, S20), and only steam
curing (S24)
For the preparation of the mixture, the following w/w
ratios were used: silica sand/kaolinite 1, and NaOH/kaolinite
0.36. The percent weight of kaolinite that was used in each
series was 42 % w/w and the weight of each specimen was
60 g.
Seven series of each mixture were subjected to different
curing procedures as shown in Table 2. The overall period of
curing for the first two phases, namely Phase I which involves
typical curing in an oven (Binder, Germany) prior to steam
curing and Phase II which involves steam curing using water
vapor, was 24 h. Curing temperature in both phases was 80 ◦ C
[13]. Steam curing of the specimens was carried out in a mod-
ified Veterinary Tabletop Steam Sterilizer (MS-T24), China,
under atmospheric pressure. Phase III involved heating of all
specimens at 80 ◦ C for 24 h. The specimens subjected only
to initial curing for 24 h (S0) were the reference specimens
[12,14,20,21]. The compressive strength for all specimens
was determined 7 days after drying. A schematic diagram
showing the different curing options is shown in Fig. 1.
Eight specimens produced in each of the seven series (S0,
S4, S8, S12, S16, S20 and S24) and used for additional stud-
ies and analyses. Three specimens (Group 1) were further
dried in an oven at 40 ◦ C for 7 days. Three more specimens
(Group 2) were immersed for 7 days in plastic containers
filled with tap water at room temperature, in order to further
assess their integrity. The remaining two specimens (Group
3) were used for additional studies including leaching tests
and mineralogical analyses through X-ray diffraction (XRD).
The effect of the different steam curing periods was assessed
after curing, respectively.
The compressive strength was determined using a CON-
TROLS testing machine (Model T106 modified to suit stan-
dard testing), by applying a load with a displacement rate
of 2 mm/min. Three dried specimens of Group 1 and three
immersed specimens of Group 2 were used for compressive
strength measurements.
Two specimens were used for each measurement. If differ-
ence in measurement exceeded 10 %, a third specimen was
used.
2.4 Microstructure of Geopolymers
Mineralogical analyses were carried out on powdered
geopolymer samples using an X-ray diffractometer-6000
(Shimadzu, Japan) in order to identify major crystalline and
potentially newly formed phases. The XRD patterns were
obtained from 5◦ to 80◦ 2θ at a scan rate of 2◦ /min. The min-
eralogical phases were identified using the software provided
by the manufacturer.
The morphology of the specimens was examined using an
Inspect F50 Scanning Electron Microscope (Netherlands).
The samples were pre-coated with platinum in an argon
atmosphere. Energy-dispersive X-ray spectroscopy (EDX)
was used for elemental analysis.
Thermal gravimetric analysis (TGA) was carried out using
an STA 409 thermal analyzer (NETZSCH) with a constant
heating rate of 5◦ /min.
2.5 Presence of Water-Soluble Salts
The following procedure was used to determine the presence
of water-soluble salts in the mass of the final geopolymers:

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1 A representative geopolymer sample of Group 3, after
determining the compressive strength, was powdered and
thoroughly homogenized.
2 The powdered sample was dried at 105 ◦ C for 24 h.
3 About 5 g of the powdered sample was mixed in a beaker
with 200 mL of distilled water.
4 The solution was stirred in a mechanical shaker until all
water-soluble salts were dissolved and a constant elec-
trical conductivity (EC) value was reached. EC and pH
values in the solution were measured using WTW multi-
line P4, pH and EC meters.
5 The concentration (in mg L−1 ) of dissolved Na, which is
the dominant cation in the solution, was either deter-
mined using an atomic absorption spectrophotometer
(PerkinElmer model Analyst 200) or a flame photometer
(Sherwood Model 410).
3 Results and Discussion
3.1 Microstructural Characteristics
The XRD patterns of the raw material (JK) and the reference
geopolymers (S0) are shown in Fig. 2. Several sharp peaks
corresponding to quartz and kaolinite are shown for the raw
material. After geopolymerization, the intensity of kaolin-
ite peaks decreases and peaks corresponding to plagioclase
feldspar (NaAlSi3 O8 ) appear. The presence of peaks corre-
sponding to kaolinite in the produced reference geopolymers
confirms the partial reactivity of the precursor under the con-
ditions used.
Scanning electron microscopy analysis (Fig. 3) indicates
clearly the coexistence of geopolymer gel and partially unre-
acted kaolinite layers in the final products. The unreacted dis-
torted kaolinite is distributed in a random and heterogeneous
manner in the microstructure of the final geopolymer. This
heterogeneity is most probably due to the uneven evaporation
of water during geopolymerization and results in concentra-
Fig. 2 X-ray diffraction spectra of the precursor (JK), and the kaolinite
reference geopolymers (S0)
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Arab J Sci Eng
Fig. 3 SEM images of the kaolinite reference geopolymers (S0)
tion gradients and thus in local differences in reactivity. The
fact that the clay mineral particles have different dimensions
also plays an important role in the process. Larger particles
react slower and remain partially unreacted since diffusion
is the reaction rate determining step [18,22–24].
Figure 4a, b shows the EDX spectra of the geopolymers
S0 and S24 surface, respectively. The presence of a Na peak
at about 1.05 keV, a C peak at about 0.5 keV and the absence
of the corresponding Al and Si peaks in the EDX spectrum
of S0 specimen indicate the formation of a Na–C–O surface
layer. The EDX spectrum shows that the C/Na molar ratio is
almost 1, Fig. 4a. Thus, this layer is more likely composed
of sodium carbonate hydroxide. This is a result of reference
curing (S0), which involves only initial curing and drying
at 80 ◦ C. During curing, part of water may evaporate while
part of the residual alkali, i.e., NaOH, may migrate to the
surface where it reacts with CO2 (atmospheric carbonation)
to form a surface layer of sodium carbonate, as efflorescence.
The application of steam curing, as in S24, results in the
transformation of this surface layer to geopolymer gel as
shown in Fig. 3b, where the Si/Al and the Na/Al molar ratios
are 1.75 and 0.35, respectively. C and Fe can be also detected
at the surface of S24 specimen. Kaolinite is the source of Fe
as shown in Table 1, while carbon indicates the presence of
sodium carbonate.
More detailed information regarding phase composition
and the presence of bound water in the geopolymeric struc-
ture was provided by TGA. Figure 5 illustrates the TGA
results for S0 (reference specimen) and S24 (full SCC)
geopolymers. The total weight loss as a result of dehydrox-
ylation of S0 and S24 geopolymers between 400 and 620 ◦ C
is comparable for both samples, namely 1.4 % and 1.6 %
respectively, as shown in Fig. 5a. The derivative of the TGA
Arab J Sci Eng

Fig. 4 Energy-dispersive X-ray (EDX) spectra of geopolymers: reference geopolymers, S0 (a) and geopolymers after steam curing, S24 (b)

curve reveals that thermal events occur in two temperature

ranges, 25–400 and 400–620 ◦ C, respectively, as shown in
Fig. 5b. In the first range (25–400 ◦ C), the decrease in weight
can be attributed to the release of fine-pore moisture. In the
second range (400–620 ◦ C), the decrease in weight is mainly
caused by the dehydroxylation of unreacted kaolinite and
the release of strongly bound fine-pore moisture or hydroxyl
groups.

3.2 Mechanical and Physical Properties

Figure 6 shows the effect of the duration of steam curing

on bulk density, shrinkage, and water absorption of the final
geopolymers. As shown in Fig. 6a, geopolymers produced
after the application of a full SCC (S24) have lower bulk
density (1.86 g cm−3 ) than those which were subjected first
to initial curing and then to steam curing for shorter periods.
Thus, it is obvious that the application of a long SCC results
in a volume increase and thus decrease of the bulk density of
the final geopolymers which can reach 9 % (Fig. 6a).
However, initial curing at 80 ◦ C even for a short period of
4 h prior to steam curing results in a bulk density of 1.97 g
cm−3 which is comparable to that of the reference geopoly-
mers (S0). As a result of volume expansion, water absorption
(Fig. 6c) is higher and reaches 13 % for specimen S24 com- Fig. 5 Thermo gravimetric analysis of kaolinite (precursor), S0 and
pared to 10 % determined for the reference specimen S0. S24 (geopolymers)
Figure 7 shows the compressive strength of the produced
geopolymers, which reaches a maximum value after steam compared to the values recorded for reference geopolymers
curing for 8 h (S8), 47 and 29 MPa for dry and immersed (S0), 38 and 22 MPa respectively. These results clearly show
specimens, respectively. These values are 20–30 % higher the positive effect of steam curing on the increase of mechan-

123

Fig. 6 a Bulk density, b shrinkage and c water absorption % (average
of four cured samples) of geopolymers produced after different steam
curing periods
ical strength. The fact that only the application of steam cur-
ing (S24) does not improve mechanical properties is proba-
bly linked to the high swelling of the specimen in this case.
Thus, a period of about 8 h of initial curing at 80 ◦ C prior to
steam curing is required so that the specimens obtain suffi-
cient strength.
3.3 Effect of Steam Curing on the Formation
of Water-Soluble Salts
The electrical conductivity of the solution in which geopoly-
mers were immersed decreased by ∼30 %, from 1967
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Arab J Sci Eng
Fig. 7 Compressive strength of geopolymers produced after steam cur-
ing for different periods
µS cm−1 to 1350 µS cm−1 , when the period of steam cur-
ing increased from 0 to 16 h. In addition, Na+ concentra-
tion in the solution followed an almost identical trend and
decreased after seam curing by ∼ 26 %, from 1,141 mg L−1
to 844 mg L−1 . Based on the above, it is concluded that steam
curing reduces significantly the content of water-soluble salts
both in the mass and the surface of kaolinite-based geopoly-
mers. Steam curing increases the percentage of alkalis that
participate in geopolymerization reactions, and the formation
of gel that improves the mechanical properties of the final
products. Also, it is deduced from the experimental results
that a period of 8h of steam curing is required.
However, in order to obtain the highest mechanical
strength, initial curing at 80 ◦ C is required prior to steam
curing. During this initial curing stage, water participates
in geopolymerization reactions and the development of a
three-dimensional structure. This structure remains intact
after steam curing and renders a compact and hard speci-
men. Shorter periods of steam curing lead to a more porous
structure, lower density and thus reduced final compressive
strength.
4 Conclusions
The experimental results of this study show that the appli-
cation of a SCC improves the properties of kaolinite-based
geopolymers. Steam curing accelerates geopolymeric reac-
tions and reduces significantly the content of residual alkalis
and thus of water-soluble salts both in the mass and the sur-
face of kaolinite-based geopolymers and results in the pro-
duction of more gel that improves the mechanical properties
of the final products. The compressive strength of kaolinite
geopolymers increases from 38 to 47 MPa and from 22 to
29 MPa under dry and immersed conditions, respectively.
However, application of only steam curing results in
higher swelling and deteriorates the quality of the produced
Arab J Sci Eng

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Acknowledgments The financial support of the project “Flood Man-
national Conference Technology for Developing Countries, vol. 3,
agement in Semi-arid Areas” funded by the Deanship of Academic
pp. 1085–1092. Jordan (2002)
Research at the University of Jordan is gratefully acknowledged. We
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laboratory facilities. The authors would also like to thank the Vlaamse
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