Applied Clay Science 83–84 (2013) 253–262

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Applied Clay Science

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

Research paper

Characteristics and applications of flash metakaolins

R. San Nicolas 1, M. Cyr ⁎, G. Escadeillas
Université de Toulouse, LMDC (Laboratoire Matériaux et Durabilité des Constructions), INSA/UPS Génie Civil, 31077 Toulouse CEDEX 04, France

a r t i c l e i n f o a b s t r a c t

Article history: This paper presents physical, chemical and mechanical characteristics of metakaolins obtained from an industrial
Received 24 March 2012 flash calciner, in order to compare their properties with standard industrial metakaolin produced in a rotary kiln
Received in revised form 14 August 2013 calciner. Three kaolins, with three levels of purity, were calcined by these two different methods to give six dif-
Accepted 16 August 2013
ferent metakaolins for the study. The results showed that the method of calcination did not affect the chemical
Available online 17 September 2013
composition of the metakaolins formed but did influence their physical properties and performance as a supple-
Keywords:
mentary cementitious material when blended with Portland cement, and in geopolymer synthesis. Flash
Metakaolin metakaolins have a lower water demand than rotary metakaolins, which can be explained by the morphological
Flash calcination properties of the flash metakaolin, induced by the calcination process. Traditional rotary-calcined metakaolins
Spherical metakaolin tend to be angular layered particles, whereas flash metakaolins contain spherical particles. Mechanical test re-
Supplementary cementitious material sults showed that the two methods of calcination can lead to metakaolins with equivalent performance in the
Geopolymer synthesis of construction materials.
© 2013 Elsevier B.V. All rights reserved.

1. Introduction
Metakaolinite (MKaol) is obtained by heating kaolinite (Kaol) at tem-
peratures between 700 and 850 °C (Brindley and Nakahira, 1959a,b;
Brindley et al., 1967; Gniewek, 1987; Horvath and Kranz, 1980; White
et al., 2010, 2011). This heating induces the dehydroxylation of Kaol, lead-
ing to the production of an amorphous material that is usually very reactive
in basic environments such as cement-based materials (Courard et al.,
2003; Frı́as et al., 2000; Garcia-Diaz, 1995; He et al., 1995; Khatib and
Hibbert, 2005; Khatib et al., 1996; Takemoto and Uchikawa, 1980) and
geopolymers (Barbosa et al., 2000; Davidovits, 1994; Duxson et al., 2005,
2007a,b; Palomo et al., 1992). On an industrial scale, most metakaolins
(MK) are obtained from a three-stage method that comprises a selection/
grinding process, then calcination of the raw Kaol for several hours in a ro-
tary kiln, followed by grinding of the burned material. Typical physical
characteristics of MK are a flaky, irregular morphology and a high specific
surface area (SSA) (Bich, 2005; Cyr, 2000). MK is essentially composed of
silica and alumina (more than 90% in total), and commercial products
have a SiO2/Al2O3 ratio between 1.5 and 2.5, depending on the purity of
the raw kaolin (K) material used in their production.
More recently, a new industrial process has begun to be used in
metakaolin production: flash calcination. Flash calcination is an industri-
al process based on rapid calcination of a material, for only a few tenths
of a second. It can be used for different kinds of materials: magnesite ore
(Erşahan et al., 1994), limestone (Ying et al., 2000), and Kaol (Davies,
1984; Gaurier, 1987; Meinhold et al., 1994; Salvador, 1992). After several
pilot studies, industrial producers have started using this method of cal-
cination of clay with increasing frequency, as they have already done in
the mineral sector (WO9855418A1 and Malet, 1998). In this process, a
solid, usually in finely divided form, is heated rapidly, held at tempera-
ture for a short time, and cooled at a rate of the order of 103–105 °C
per second. Flash calcination enables the dehydroxylation of powdered
Kaol in K within several tenths of a second, and the resulting MK does
not need to be crushed after calcination because it does not have suffi-
cient time to agglomerate, unlike in a rotary kiln. At the end of the
flash calcination process, particles have substantially the same size as be-
fore the calcination (Ingram-Jones et al., 1996; Salvador, 1995).
The physical transformation of powdered K associated with the rapid
dehydroxylation of Kaol during flash calcination leads to physical changes
of MKaol in the MK, compared to traditional MK as described in the liter-
ature (Frı́as et al., 2000; He et al., 1995; Khatib et al., 1996). The aim of this
paper is to highlight the differences between a series of six flash and tra-
ditional MK obtained in industrial-scale processes, and to analyse how the
flash-calcined metakaolin (MKF) behaves in different applications where
traditional MK is used in industrial practice, including as a supplementary
cementitious material blended with Portland cement, or in geopolymers.

2. Rotary kiln vs. flash calcination

⁎ Corresponding author. Tel.: +33 5 61 55 67 7; fax: +33 5 61 55 99 49. 2.1. Rotary kiln calcination
E-mail addresses: rsan@unimelb.edu.au (R. San Nicolas), Martin.Cyr@insa-toulouse.fr
(M. Cyr), gilles.escadeillas@insa-toulouse.fr (G. Escadeillas).
1
Current address: Department of Chemical & Biomolecular Engineering, University of Rotary kiln calcination is one of the most common processes used to
Melbourne, Victoria 3010, Australia. produce commercial MK (Argical M 1000 in France, Whitemud in

0169-1317/$ – see front matter © 2013 Elsevier B.V. All rights reserved.
http://dx.doi.org/10.1016/j.clay.2013.08.036
254 R. San Nicolas et al. / Applied Clay Science 83–84 (2013) 253–262

Canada, Metacaulim in Brazil, and others). The installation is similar to
the kilns used for cement production, although it is operated under dif-
ferent conditions. The kiln is a cylindrical vessel, slightly inclined from
the horizontal, which is rotated slowly about its axis. The K to be
processed is fed into the upper end of the cylinder, which is 60–90 m
in length and 4–6 m in diameter. The cylindrical vessel is a steel tube
filled with a refractory lining. As the kiln rotates, the material gradually
moves down towards the lower end, and may undergo a certain amount
of stirring and mixing. Hot gases pass along the kiln, sometimes in the
opposite direction (counter-current) to the process material. The calci-
nation process, between 650 and 700 °C, which lasts about 3 to 5 h,
drives the particles of MK to agglomerate in pellets of 5 to 10 cm diam-
eter. These pellets are then crushed to the desired fineness.
2.2. Flash calcination process
Several types of flash calcination systems have been used to process
different materials. Here, we describe the flash calcination process used
by one of the two French producers of MK. After a pre-treatment, K is
air-dried in a warehouse then transported and crushed (with elimina-
tion of coarse particles of quartz), and finally dried at 100 °C.
During the first stage of calcination, a stream of upward-flowing
hot air takes dried clay to a 200 μm sieve, from which it is fed into
the calciner (Fig. 1). Particles of clay turn around the flame, which
has a temperature of between 1000 and 1200 °C. Clay spends only
a few tenths of a second in the calciner, just enough time to reach
700 °C and be transformed to MK, before being sent to air cooling cy-
clones. In this step, MK is quickly cooled to 100 °C. Finally, the prod-
uct is packed in silos and allowed to cool to room temperature before
being sold.
This installation consumes 2.2 MJ/t of MK, which is 80% less than the
energy consumed during cement production (San Nicolas, 2011).
analysed by thermogravimetry (TG) (Fig. 2a) and X-ray diffraction
(XRD) (Fig. 2b). Through these methods, including Rietveld analysis of
the XRD data, the amounts of Kaol and quartz in Ks were determined.
K1 (from Surinam) was relatively pure K with 92% Kaol; K2 and Kl3
(from France) had 65% and 55% Kaol respectively. If all the Kaol present
is dehydroxylated during calcination, these values will give the approx-
imate concentrations of MKaol in the final materials, as quartz is the
main impurity and is not expected to be altered during the calcination
process. Thus, this amount of MKaol may be linked to the reactivity of
each product. All the K had a thin layered, hexagonal flaky morphology,
as shown in Fig. 3. Samples were named MKRx for the rotary calcined
metakaolins (MKR) and MKFx for the flash calcined metakaolins in pre-
viously described condition (Sections 2.1 and 2.2), with x being the
number of the K.
3.1.2. Other materials
3.1.2.1. Cement-based material applications. The cement used was a CEM I
52.5N, as specified in European Standard NF EN 196-1 (AFNOR,
2006). Its chemical composition and physical properties are given
in Table 1. The aggregate used in mortar production was a normal-
ized quartz sand (NF EN 196-1) with particle size ranging between
0.08 and 2 mm.
3.1.2.2. Geopolymer applications. MK was used as the primary alumino-
silicate source. Sodium silicate was obtained as a commercial solution
(26% SiO2, 8% Na2O, and 66% H2O by mass; density 1330 kg/m3). Sodi-
um hydroxide pearls (99.9% purity) and distilled water were also used
throughout the work. Normalized quartz sand (NF EN 196-1) with par-
ticle sizes between 0.08 and 2 mm was used as an aggregate where
needed.

3. Materials and methods 3.2. Mixture proportions

3.1. Materials 3.2.1. Cement-based-material applications

3.1.1. Kaolins
Three K are specifically studied in this paper. Table 1 presents the
chemical composition of these clays, and the raw materials were also
The water/(cement + MK) ratio used in all mortar samples was
0.50, and the sand to binder ratio was 3.0. One reference mixture was
made with a 100% cement binder (CEM I 52.5N). The six other mixtures
contained 25% of each MK, respectively, and 75% of cement as the bind-
er. All samples were cured at 20 °C and N 99% humidity and tested at 2,
7, and 28 days.

Solid input 3.2.2. Geopolymer applications

Geopolymer mortars were prepared by first dry-mixing each of the
Flame (1200°C)

MK with sand (mass ratio of sand to MK: 3.0), then combining with al-
kaline activating solution in a mechanical mixer. Sodium silicate activat-
ing solution was prepared at a SiO2/Na2O molar ratio of 1.5, by adding
solid NaOH to the sodium silicate solution. The solids to solution mass
ratio used was 0.65. All samples were cured at 40 °C for 24 h in moulds,
then demoulded and cured at 25 °C before being tested at the specified
times. Compressive strength testing was performed according to
Air input European Standard NF EN 197-1 (detailed in Table 2), with results

Table 1
Chemical composition of the cement and K1, K2 and K3.

Composition, CaO SiO2 Al2O3 Fe2O3 SO3 Na2O K2O MgO LOI
mass %
1m
Cement CEM I 65.00 20.42 5.03 2.82 3.12 0.14 0.86 1.41 1.21
52.5 N
K1 0.10 58.06 37.98 1.49 ND⁎ 0.08 1.22 0.12 0.94
Solid + Gas output K2 0.16 63.62 32.44 1.78 0.01 0.09 0.92 0.14 0.84
K3 1.13 68.44 26.93 2.57 ND⁎ 0.01 0.12 0.11 0.68

Fig. 1. Schematic representation of a flash calciner used in MK production. ⁎ ND: not detected.
 R. San Nicolas et al. / Applied Clay Science 83–84 (2013) 253–262 255

Temperature (°C)
(a) 250 350 450 550 650 750 850
0
-1
-2
-3
-4

Weight lost (%)

-5
-6
-7 K3
-8
K2
-9
-10
-11
-12
K1
-13

Q. Quartz Q
(b) Kaol. Kaolinite
C. Calcite
Kaol

Q Kaol
Kaol
Kaol
Kaol Kaol C KaolQ
KaolQ Q Q K3
Counts

K2

K1

5 10 15 20 25 30 35 40 45 50
2θ
θ Kα
α Co

Fig. 2. (a) TG and (b) XRD patterns of K1, K2 and K3. In the XRD, Kaol is kaolinite, Q is quartz, and C is calcite.

Fig. 3. SEM images of K3.

256 R. San Nicolas et al. / Applied Clay Science 83–84 (2013) 253–262

Table 2 4.1.2. Mineralogical characteristics

Experimental methods applied. The X-ray diffractograms (Fig. 4) of the materials show that both
Properties Test methods applied methods of calcination are efficient, as there is no trace of Kaol.
Moreover, the XRD patterns (Fig. 4) and mineralogical compositions
Chemical analysis
Major oxides Atomic absorption with flame atomization calculated by Rietveld analysis (Table 4) show that the six samples
Minor elements Inductively coupled plasma-mass spectrometry (ICP-MS) are mainly composed of quartz (Q) from the raw materials and an
Mineralogy X ray diffraction (XRD), Co Kα radiation (λ = 0.1789 nm) 2θ step X-ray amorphous phase: MKaol. Additional crystal phases seen are
interval of 0.02° (5–70°) and acquisition time of 10 s
illite (I) from the raw materials, which is not dehydroxylated
Physical analysis below 760 °C (Mackenzie, 1970), and also anatase (A) from the
Absolute density Hydrostatic weighing of powder in non reactive liquid raw material. Finally, there was formation of mullite, which can be
SSA Brunnauer, Emmett and Teller (BET) method, using nitrogen
obtained when the temperature of calcination exceeds 850 °C
sorption
Particle size Laser granulometry (dry), Mastersizer 2000 (Malvern), pump (Brindley and Lemmatize, 1987; Brindley and Nakahira, 1959a,b).
distribution speed 2500 tr/min for 2 min under ultrasound polydispersion. This phase is crystalline and not reactive. There was around 3 to
Morphology Scanning electron microscopy (SEM), JEOL JSM-6380 LV, coupled 9% of this crystal in the MK according to the Rietveld refinement re-
with elemental analysis (EDX); RÖNTEC. The acceleration voltage sults, showing that an overcalcined part exists in each MK. The pres-
is 15 kV and 20 kV respectively for secondary and backscattered
ence of mullite can be explained through the details of each
electron mode. Samples were vacuum dried and platinum coated
before investigation, and representative secondary electron im- calcination process. First, in a rotary kiln, K is usually introduced
ages of each type of particle shape present in MK powder were into the furnace as small balls about 5 cm in diameter. This form
collected. means that the heat energy received varies from the surface to the
Optical microscope coupled with a particle analyzer (GM),
heart of the ball. This difference then leads to the production of
Malvern, Morphology G3S.
Etching 48 h in 37% HCl
balls composed mainly of MKaol, but also with mullite on the sur-
face (overcalcined) and sometimes some Kaol remaining in the
Mechanical tests
heart (undercalcined). In the flash calcination process, mullite can
Workability Flow under vibration using LCL apparatus (NF EN 12350-1)
(AFNOR, 2009)
be formed from particles that travel through the flame rather than
Activity index Compressive strength of 4 × 4 × 16 cm prisms (crosshead speed turning around its edges.
2400 N/s ± 200 N/s) (NF EN 196-1)
Hydration time: 2-7-28 days 4.2. Differences between MKF and MKR
Each value is an average of 6 tests

The morphological properties of MK are shown in Fig. 5. Under

low magnification, MKFx and MKRx do not appear to have markedly
reported as the mean of six samples. Samples were tested at 2, 7 and different particle shapes, as shown in Fig. 5(a) and (e). However,
28 days after synthesis. with a higher magnification (Fig. 5(b)), spherical particles of MK
with diameters around 10 μm appear in the flash-calcined products
but are not present in MKRx. This population of spherical particles
3.3. Experimental methods can be explained by the flash calcination process: melting in a hot
gas stream promotes a spherical shape, as is widely observed in fly
The properties of the reaction products were studied in two parts, ashes for particles which are also formed through the melting of
firstly the MK products themselves, and also their behaviour in applica- clay minerals. Additionally, the trends of chemical compositions, ob-
tions. Experimental methods used for the chemical, physical and reac- servable in the spectrums in Fig. 5 from multiple EDX analyses, show
tivity characterization of the MK are given in Table 2. that the surfaces of these spheres seemed to have a higher silica con-
tent. So the smooth surfaces of the spheres can be explained by the
vitrification of these highly siliceous aluminosilicates at the surface
4. Results and discussion because, after acidic attack, the excess of siliceous material disap-
pears. As the particles are cooled in tenths of a second and so freeze,
4.1. Similarities between MKF and MKR they keep these shapes. Selective dissolution provided additional in-
formation about these particles, and Fig. 6 shows a SEM image of a
4.1.1. Chemical characteristics spherical particle that has been partially etched for 48 h in 37% HCl.
The MK tested were essentially composed of silica and alumina The surface of the sphere, which was originally smooth, appears to
(more than 90%) and had a SiO2/Al2O3 ratio between 1.5 and 2.5. The be composed of thin particles, interlinked with each other and
chemical compositions of the MK studied are detailed in Table 3. forming the skeleton of the spheres. According to EDX analysis, the
These results show that there was no significant difference in chemical skeleton is composed of aluminosilicate, similar to MKaol or mullite.
composition between MKRx and MKFx. This morphology has already been observed in fly ash by various au-
thors (Hulett et al., 1980; Ollivier et al., 1995), and is associated with
mullite. So, this could mean that a fraction of these spheres corre-
sponds to the mullite observed in XRD analysis.
Table 3
Chemical compositions of all MK (wt%).
At a higher magnification, Fig. 5(c) and (g), particles of MKaol are
flat, hexagonal particles like Kaol, but now separated. This dispersion
MKR1 MKF1 MKR2 MKF2 MKR3 MKF3 is very clear in Fig. 5(c), where the leaf-like structures that are usual-
CaO 0.10 0.10 0.20 0.20 1.00 1.10 ly stuck against each other in K are separated, giving the impression
SiO2 58.00 57.24 63.19 62.67 67.83 67.16 of an “accordion” formation. This separation takes place during
Al2O3 37.43 37.50 31.79 31.98 26.37 26.83
dehydroxylation, with the water molecules creating this shape as
Fe2O3 1.50 1.39 1.79 1.79 2.30 2.60
TiO2 1.10 1.59 1.29 1.49 1.60 1.40 they evaporate quickly from the material (Soro, 2003). This accordi-
Na2O 0.08 0.08 0.08 0.09 0.01 0.01 on shape has been observed only in flash calcined samples. It is likely
K2O 0.89 1.22 0.89 0.91 0.10 0.12 that, as the dehydroxylation is very fast, the leaves do not have
LOIa 0.89 0.91 0.74 0.68 0.79 0.83 enough time to separate completely. Moreover, as the particles are
a
LOI: Loss on ignition. immediately cooled at the exit of the calciner, they keep this atypical
 R. San Nicolas et al. / Applied Clay Science 83–84 (2013) 253–262 257

Q Q
Q. Quartz
M. Mullite Q
A. Anatase Q
Ph. Phyllites M Q
Am. Amorphous phase A Q

M M M M M MKF3
A
Am

Am MKR3

Ph Q A Q
M
Ph Q Q
Q
M Ph M M M Q
Counts

A M
Am MKF2

Q
Am MKR2
AM
Ph Q K
Ph
M
M M M Q M
K Am A M MKF1

Am
MKR1

5 10 15 20 25 30 35 40 45 50
θ Kα
2θ α Co

Fig. 4. X-ray diffraction patterns for the six MK.

form. MKRx seems to have more thin particles, which can be associ- of 30,000 particles for each MK. Fig. 7 shows plots of the circularity
ated with broken leaves or with the grinding. Finally, at the highest (defined as the ratio of the equivalent perimeter to the real perime-
magnification, the two kinds of MK look similar, as shown in ter of a particle, where the equivalent perimeter is the perimeter of a
Fig. 5(d) and (h). disk with the same area as the particle) against particle size for each
The spheres in MKFx, as shown in the SEM images, are specifically of the MK.
produced by the flash calcination process, and granular morpholog- From the plots in Fig. 7, the difference in shape (as also observed by
ical analysis can provide more information about the existence and SEM) between MKFx and MKRx is evident. It can be observed that a high
concentration of these spherical particles. This method uses an opti- proportion of MKFx particles have a circularity between 0.90 and 1.00,
cal microscope coupled with image analysis software to generate in- meaning that they are close to spherical shape. Particles of MKRx have
formation regarding particle sizes and shapes. Here, a scan was made a variety of forms, with a higher population density of more angular
(circularity b0.9) particles. Plots of the number of particles against the
circularity show that, in all cases, the MKFx samples have at least
Table 4 three times more near-spherical particles than the MKRx samples. By
Results of Rietveld refinement of X-ray diffraction data for the six MK. summing the number of particles with diameters between 1 and
wt% Amorphous phase Quartz Mullite Anatase Kaolinite Illite 20 μm, and with circularity between 0.95 and 1, we obtain 12%, 15%
and 10% of spherical particles for MKF1, MKF2 and MKF3, respectively,
MKF3 45 48 5 1 1 0
MKR3 46 47 4 1 2 0
compared to 2%, 4% and 3% for MKR1, MKR2 and MKR3. In the SEM in-
MKF2 55 38 6 1 0 5 vestigation, no spherical particles were observed in these MKRx, so the
MKR2 54 37 7 1 0 5 number of spherical particles estimated by optical microscopy may be
MKF1 66 15 9 1 2 7 above the actual number, and the few percent found are just spherical
MKR1 70 17 2 1 1 5
agglomerations of small particles.
258 R. San Nicolas et al. / Applied Clay Science 83–84 (2013) 253–262

Fig. 5. SEM images of MKFx (a, b, c, d) and of MKRx (e, f, g, h), and EDX analyses of particles on the right.

4.3. Activity of MK in practice
4.3.1. MK in Portland cement concrete
4.3.1.1. Fresh state. Before moulding, the workability (flow) of each mor-
tar mixture with 75% CEM I and 25% MK was tested. The workability of
mortar is defined as the ability of freshly mixed mortar or concrete to
flow. Although mortars containing MK always had higher flow times
(i.e. more resistance to flow) than 100% cement mortar (Fig. 8), it can
be seen that all mortars with MKF had lower flow times than those
with MK from a rotary kiln, meaning that flash calcination seems to re-
duce the undesirable effect of reduced workability present in standard
MK. This phenomenon cannot be explained purely by the fact that the
SSA of the MKF are smaller than those of the corresponding MKaR sam-
ples (Table 5), as shown in Fig. 9. According to Felekoglu (2009) and
Hentschel and Page (2003), other factors, including particle shape, mea-
surable as circularity or roughness, can also modify the workability of
mortars. So, the higher circularity of MKF, as observed in Section 4.2,

1600 Al
1400 O
1200 Si
1000
EDX-D
cps/eV

800
600
D
400
C
200 Fe
Ti Fe KeV
2.0µm 1.0µm 0
0 1 2 3 4 5 6 7 8

Fig. 6. SEM images of a spherical particle of MKF3 after 48 h in acidic solution, with EDX analysis.
 R. San Nicolas et al. / Applied Clay Science 83–84 (2013) 253–262 259

Fig. 7. Population density of particles against particle diameter between 1 and 100 μm for all MK. The images between the plots show examples of the shapes which correspond to given
circularity values.

can also explain the higher workability of mortars with 25% of MKF
compared to the corresponding MKR mortars.
4.3.1.2. Hardened state. Fig. 10 gives the activity index, defined as the ef-
fect of MK addition on compressive strength (ratio of strength of blended
mortar to strength of control mortar), for cement-MK mixtures after 2, 7
and 28 days. Generally, strength was lower during the first 7 days in
mortars containing MK compared to the reference (activity index b1).
After 28 days, the strength of the blended mortars was higher than
that of the control. The increased rate of strength development between
260 R. San Nicolas et al. / Applied Clay Science 83–84 (2013) 253–262

25 1.35 1.45
1.30 1.31
1.18
20.3 1.10
0.98 1.10 1.01
20 0.91 0,99 0.98 1.02 1.00
0.96

Activity index
0.93 0.95
0.90
1
14.7
Flow time (s)

15 13.0

10 8.0 8.0

5.0
5 0
3.0 2 days 7 days 28 days

MKR1

MKR2

MKR3

MKR1

MKR2

MKR3

MKR1

MKR2

MKR3
MKF1

MKF2

MKF3

MKF1

MKF2

MKF3

MKF1

MKF2

MKF3
0
MKR1 MKF1 MKR2 MKF2 MKR3 MKF3 Ref
Fig. 10. Activity indices of all MK in mortars (on the basis of compressive strength) at 2, 7
Fig. 8. Flow time of mortar mixtures, measured according to the LCL flow test (NF EN 196- and 28 days.
1). Higher flow time indicates greater resistance to flow.

notable influence on the compressive strength when its surface area ex-
Table 5
BET, SSAs of all MK and the cement used. ceeds this value. The fact that, after 7 days and 28 days, the mortars with
MKR1 and MKF1 still had a much better activity index than the other
Cement MKR1 MKF1 MKR2 MKF2 MKR3 MKF3
mortars can also be explained by the higher purity of K1 and thus its
BET (m2/g) 1 29 24 20 18 14 13 higher content of reactive components.

4.3.2. MK in alkali activated (geopolymer) binders

7 and 28 days in mortars containing MK was attributed to the pozzolanic
Fig. 12 shows the compressive strengths of geopolymer mortars at 2,
reaction caused by the amorphous silica and alumina content of this ma-
7 and 28 days. In each case, considering the standard deviation associat-
terial (Badogiannis et al., 2002; Khatib et al., 1996). Due to its pozzolanic
ed with the results, there are no significant mechanical differences be-
nature, the MK reacts with the portlandite (Ca(OH)2) produced during
tween mortars with fMKF and mortars with MKR. As in the discussion
cement hydration, and causes an increase in long-term strength
of Portland cement binders above, the purity of the MK influences com-
(Ogawa et al., 1980; Wild and Khatib, 1997). Fig. 9 shows a small differ-
pressive strength: the purer the MK, the higher the compressive
ence in the activity index between mortars with MKF and those with
strength of geopolymer mortars.
MKR, although this could be due to the small gap in SSA between the
As has been observed elsewhere in the literature, the compressive
two MK (Table 5 and Fig. 10), which is associated with the grinding
strength of this kind of geopolymer decreases from 7 to 28 days. This
step following rotary-kiln calcination. This phenomenon is highlighted
phenomenon may be due to structural changes occurring in MK-
when we examine the difference between the MK derived from K1 and
derived geopolymeric gels within the first month, which alter the me-
those from the other two K sources. Even after 2 days, the activity index-
chanical properties (Duxson et al., 2007a,b; Lloyd, 2008). According to
es of MKF1 and MKR1 are greater than 1. This can be explained by the
some authors, it can be due to the conversion to less dense hydrogarnet
fact that MKR1 and MKF1 have the highest SSA of the MK studied, and
of CAH10 and C2AH8, or to the high level of water available inside (Provis
so improve the kinetics of the hydration of cement (de Silva and
and van Deventer, 2009).
Glasser, 1993). Moreover, Fig. 11 shows an inflexion point in the curves
for a SSA around 20 m2/g, which means that MK only begins to show a
90% Kaol
(K1)
20

18 90 28d
16 60% Kaol
Compressive strength (MPa)

rotary

80 (K2)
14
52% Kaol
Flow time (s)

flash

12 (K3)
70
10 7d
rotary

8
60
flash
rotary
flash

6 2d
4 50
MKR
2 MKF
0 40
10 15 20 25 30 10 15 20 25 30
Specific surface area (m2/g) Specific surface area (m2/g)

Fig. 9. Flow time of mortars as a function of SSA. Fig. 11. Compressive strength as a function of SSA of all MK.
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MKF2

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3. The rotary-kiln metakaolins have a higher specific surface area than tion. Part. Part. Syst. Charact. 20 (1), 25–38.
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of this production method. This difference can explain the difference Hulett, L.D., Weinberger, A., Ferguson, N., Northcutt, K.J., Lyon, W.S.A.J., 1980. Trace ele-
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Dehydroxylation sequences of gibbsite and boehmite: study of differences between
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