Journal

J. Am. Ceram. Soc., 93 [2] 541547 (2010)

DOI: 10.1111/j.1551-2916.2009.03414.x
r 2009 The American Ceramic Society

Statistical Analysis of Strength Development as a Function of Various

Parameters on Activated Metakaolin/Slag Cements

Oswaldo Burciaga-D az, Jose Ivan Escalante-Garc a,w Raul Arellano-Aguilar, and Alexander Gorokhovsky
Cinvestav IPN Unidad Saltillo, Ceramics Engineering, Saltillo, CP 25000, Coahuila, Mexico

aggressive media, and thermal stability.911 The resulting properties depend strongly on the chemistry of the alkaline activant,
the nature of the raw materials, and curing conditions.12,13
In contrast, although the kind of activator inuences the nature of the hydrates formed, the reaction products obtained
from the activation SiO2CaOAl2O3-rich materials (such as
BFS) are mainly calcium silicate hydrates (CSH) and others
like calcium aluminate hydrates (CAH), and hydrated gehlenite (C2ASH8)14,15; hydrotalcite (Mg6Al2(CO3)(OH)16  4(H2O)
forms under specic conditions.16 Some advantages of these cements over Portland cement are: higher mechanical properties,
lower permeability, lower heat of hydration, and better chemical
resistance. However, they present some disadvantages such as
high shrinkage, quick setting, and in some cases, carbonation
and alkalisilica reaction.15,17
The activation of both types of raw materials described above
has advantages and disadvantages. It has been proposed that the
disadvantages of one type of activation process can be balanced
with the advantages of another.18 However, the literature offers
only a small number of studies on the alkaline activation of
BFSMk composites cement.17,19 Such reports have greatly contributed to the understanding of the mechanisms and processes
of reaction, but the main factors that affect the development of
mechanical properties have not been considered using a statistical approach. Among such factors are the time and the temperature of curing, the specic surface area of the raw materials;
proportioning of raw materials; modulus of the alkaline solution; concentration of the Na2O, etc. There are numerous publications on the alkaline activation of BFS, y ash, and, with less
on the activation of Mk, where the inuence of these factors has
been studied independently.2024 For this reason, the objective
of this work is to study the inuence of factors such as the BFS/
Mk weight ratio, activator concentration, and time of curing,
and how they interact on the development of mechanical properties in composite cement systems based on BFS and Mk.

This investigation statistically examines the strength development on alkaline activation of metakaolin (Mk)/blast furnace
slag (BFS) pastes. The main parameters studied are: BFS/Mk
weight ratio (100/0, 80/20, 50/50, 20/80, and 0/100), modulus
of the alkaline solutions of sodium silicate (M 5 SiO2/NaO2 at
0, 1, 1.5, 2), %Na2O (5%, 10%, and 15%), and curing time.
Cubes were cured at 201C for up to 360 days; the compressive
strength and other characteristics were investigated. A fully factorial experimental design was used to determine the inuence of
each variable. The curing time and the interaction of the factors
BFS/Mk ratio-%Na2O were the most important, followed by
the modulus and then the %Na2O; others such as the interaction
BFS/Mk ratio modulus were less important. The results indicated that the addition of Mk to BFS reduced the strength, more
notably at contents above 50%. For strength development, the
most effective modulus was Ms 5 1 and higher %Na2O were
required with higher Mk loads.

I. Introduction

synthesis of cementitious materials by means of chemical

activation requires the use of raw materials of an amorphous nature; this favors the reactivity required to promote
good physical and chemical properties. The literature describes1
7
the chemical activation of various raw materials of different
origins, chemical compositions, and physical characteristics.
This chemical activation promotes the formation of several
types of cementitious materials of a wide variety of physical
and chemical properties that depend on the type of reaction
products. The chemical composition of the raw materials can be
divided into those rich in SiO2 (microsilica, geothermal wastes,
etc.), those rich in SiO2 and Al2O3 (silicoaluminates such as
metacaol n (Mk), y ash, volcanic materials, etc.), and those rich
in SiO2, CaO, and Al2O3 (such as blast furnace slag (BFS) and
other metallurgical slags).
Some advantages of alkali-activated cements over Portland
cement are: low economic cost, major incorporation of industrial wastes, use of abundant raw materials without the need for
strict control of purity, lower CO2 emissions and hence lower
environmental impact, and better technological properties.1
The reaction products formed by the chemical activation of
the aluminosilicates (such as Mk) are commonly called inorganic geopolymers, which are generated from the dissolution of
Al and Si in an alkaline medium, followed by a polycondensation, forming an amorphous network based on SiO4 and AlO4
units.2,8 These materials are characterized by their development
of high mechanical strength, excellent resistance to chemically
HE

II. Experimental Procedure

(1) Materials
The chemical composition and specic surface areas of the Mk
and BFS used in the manufacture of the composites pastes are
shown in Table I. The Mk used was obtained by calcination of
kaolinite at 8001C for 6 h. Both raw materials were amorphous
to X-ray diffraction. The alkaline solutions were mixtures of
sodium silicate (SiO2 5 29.5%, Na2O 5 14.7%, and H2O 5
55.8%; modulus M 5 %SiO2/%Na2O 5 2) and sodium hydroxide pellets; the NaOH was dissolved in water before the mixing
with the sodium silicate. The solution was cooled at 201C before
mixing with the powders.
During the manufacture of the pastes, the alkaline solutions
and the powders were mixed for 3 min and then cast in cubic
molds of 5 cm  5 cm, with vibration for 45 s used to eliminate
the entrapped air. Because of the surface area differences between the raw materials, the quantity of water was adjusted to
obtain the same workability.
The samples were left covered for 24 h at 201C to avoid water
losses. The demolded cubes were wrapped in plastic, to prevent

D. Viehlandcontributing editor

Manuscript No. 25478. Received November 10, 2008; approved September 2, 2009.
Presented in part at the at 28th Cement and Concrete Science, The Institute of Materials, Manchester England, September 2008.
This work was nancially supported by Conacyt Mexico Project 53563, Burciaga-Diaz
scholarship from Conacyt (203549).
w
Author to whom correspondence should be addressed. e-mail: ivan.escalante@
cinvestav.edu.mx

541

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Journal of the American Ceramic SocietyBurciaga-Daz et al.

Table I. Chemical Composition (wt%) of the Starting

Materials

SiO2
Al2O3
Fe2O3
CaO
TiO2
Na2O
K2O
MgO
MnO
SO3
Blaine (m2/kg)

Slag

Metakaolin

33.4
11.3
0.5
37.8
1.4
0.5
0.9
8.9
0.5
3.4
4653

51.05
45.26
0.34
0.10
1.76
0.06
0.15

9469

water loss, and cured isothermally at 201C for up to 360 days.

Samples were tested for compressive strength (CS) at 1, 3, 7, 14,
28, 90, 180, and 360 days. The strength reported was the average
of four measurements and the CS results obtained were statistically analyzed as described below.
Fragments of fractured cubes were selected for characterization by scanning electron microscopy. The samples were
mounted in resin and polished using diamond pastes down to
1/4 mm. Further carbon coating was necessary to make the samples conductive under the scanning electron microscope (ESEM
Philips XL30, Eindhoven, the Netherlands) accessorized with
energy-dispersive spectroscopy (EDS).

(2) Statistical Analysis

In order to investigate the effect of such factors and their interactions on the CS in the BFSMk pastes, a fully factorial experimental design (42  31  51) was carried out. A total of 60
compositions were manufactured, in which various parameters
were changed (independent variables). The nomenclature
adopted to describe the variables (factors) was A, BFS/Mk ratio; B, modulus (M) of the alkaline solution; C, %Na2O; and D,
curing time; Table II summarizes the number of levels and
values for each factor. The response (dependent) variable
considered in the experiment was the CS at 1, 28, 90, and
360 days.
The statistical signicance of each single factor and the interactions between some of them, over the strength development,
were quantitatively determined by means of an analysis of variance (F-ANOVA). In the ANOVA analysis, various quantities
such as degrees of freedom, sums of squares, mean squares, etc.,
were organized in a standard tabular format (see Table III),
which allowed the determination of Fcalculated.25,26 The F-test on
the ANOVA data statistically denes the relative importance
of each factor; the values of Ftabulated were extracted from the
table, F.05 (f1, f2), 95% condence as reported in many statistical
books.25,27,28 When Ftabulated was lower than Fcalculated, the contribution of each factor, or their interactions, was considered
statistically important on the response variable with a 95% condence level.25,26 The order of importance of the statistical signicance of each factor, single or combined, was determined by
the difference among Fcalculated and Ftabulated (DF); the greater

Table III. Statistical F-Values Obtained with a Condence

Level of 95%
Factors
3

A
B4
C5
D1
AB
AC2
AD
BC6
BD
CD
e
Total

DF

SC

CM

Fcalculated

Ftabulated

DF

4
3
2
3
12
8
12
6
9
6
174
239

25248.04
18265.89
9340.73
41288.14
9722.47
64941.96
6231.19
9003.82
1686.48
1285.64
51621.35
238635.69

6312.01
6088.63
4670.36
13762.71
810.21
8117.74
519.27
1500.64
187.39
214.27
296.67

21.28
20.52
15.74
46.39
2.73
27.36
1.75
5.06
0.63
0.72

2.37
2.60
2.99
2.60
1.75
1.93
1.75
2.09
1.87
2.09

18.91
17.92
12.75
43.79
0.98
25.43

2.97

The superindexes in the column of Factors denote the order of importance of

each factor. DF, freedom degrees; SC, sum of squares; CM, medium squares; e,
experimental error.

the difference, the more important the inuence of the factor.

The statistical model used can be represented by.27

yijkl m Ai Bj Ck Dl ABij ACik

ADil BCjk BDjl CDkl eijkl

where yijkl is the value of the response (dependent) variable estimated at i, j, k, and l factor levels (from Table II); m is the
general mean of the estimated value of the treatment; Ai, Bj, Ck,
and Dl represent the single effects of the four factors considered;
and ABij, ACik, ADil, BCjk, BDjl, and CDkl represent the effect of
the combined interactions among the four factors. eijkl represents the random errors associated with the combination of the
mathematical treatments; every effort was taken to maintain
consistent experimental procedures in order to minimize additional sources of error.

III. Results and Discussion

Table III shows the values of Ftabulated and Fcalculated obtained
for the single and combined factors. The results showed that the
order of importance of the factors on the strength development
was: %Na2OoModulus of the solutionoBFS/Mk ratiooBFS/
Mk ratio-%Na2OoCuring time; i.e. (CoBoAoACoD).
Based on these results, only the important factors, and their
combinations, were chosen and are discussed below.

Table II. Factors and Levels Considered

Factors

A, BFS/Mk ratio
B, modulus of the alkaline
solution (M)
C, percentage of Na2O
D, curing time (days)

Levels

100/0; 80/20; 50/50; 20/80;

0/100
0; 1; 1.5; 2
5%; 10%, 15%
1; 28; 90; 360

(1)

Fig. 1. Inuence of the factor D on the compressive strength.

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Statistical Strength Analysis of Alkali Activated Slag/Metakaolin Composites

543

(1) Curing Time (Factor D)

Figure 1 shows the inuence of curing time on the CS development (estimated value of the response variable). The increase in
the curing time led to a constant increase in strength for all the
formulations analyzed. It is interesting to note that curing for up
to 90 days at 201C seems to allow a gradual progress of the reaction processes and densication of the matrix of the reaction
products. However, the increase in CS after curing for more
than 90 days was not signicant. The explanation for this would
be that at early ages, there is an intense dissolution of species,
and the condensation of the reaction products gradually takes
up the spaces initially occupied by the alkaline solution. At later
ages, the formation of reaction products reduces the available
space of the alkaline solution and the reactions are slowed down
as additional reaction products form by slower diffusion processes. The densication of the matrix of reaction products and
the consumption of reactants contribute to a slow further evolution, which results in a slow CS development.
(2) BFS/Mk Ratio-%Na2O (Interaction AC)
The combined interaction of factors AC has a very strong inuence on the development of CS. Figure 2 shows a pattern in
which increasing the Mk fraction (reducing that of BFS) reduced the CS, and that higher amounts of Na2O were required
to reach the highest CS. The results indicate that for the range
of %Na2O used, the BFS reacts more intensively than the Mk,
favoring higher nal strengths. For 5% Na2O, the lowest concentration used, the highest CS of all formulations were those of
pastes of 100% BFS, for which higher %Na2O were unfavorable for CS. This is in agreement with Wang et al.,23 who indicated that 28% Na2O, by BFS weight, is usually necessary to
obtain a stable activation; however, for %Na2O48, they
pointed out that CS development was low and carbonation occurred due to the presence of free unreacted alkalis. The results
suggest that with such a relatively low alkalinity, the BFS was
effectively dissolved and formed mainly calcium silicate hydrates, which are responsible for CS development.16
In contrast, the replacement of 20 and 50% of BFS with Mk
required 10% Na2O to reach the highest CS; moreover, those
formulations of 80 and 100% Mk required 15% Na2O to reach
an acceptable CS of only about 40 MPa. Thus, as the amount
of Mk increased, more Na2O was needed to activate the reactions by promoting the dissociation of the mineral in silicates
and aluminate species, with the subsequent geopolymerization
process and formation of stable reaction products of high CS.
However, the CS for composites of high Mk and high %Na2O
were lower than those of 100, 80, and 50% BFS. Yip et al.,17

Fig. 3. Inuence of the factor B on the compressive strength.

found that the presence of a moderate amount of a calcium

source in an Mk system had a positive impact on the mechanical
properties, which is consistent with the results in this work.
However, it is not clear how the calcium is integrated into the
structures for improvement of the mechanical properties of a
geopolymer, and whether it takes part in the geopolymeric
structure or forms products of higher intrinsic strength like calcium silicate hydrates as indicated by the results.

(3) Modulus of the Activator (Factor B)

Another statistically important factor was the modulus (M) of
the alkaline solution. Figure 3 shows that an increase in the M
of the alkaline solution from 0 to 1 improved the hydration reaction processes and favored higher compressive strengths; however, for M41, the strength was reduced. An explanation for
this is that for a xed %Na2O, an increase in the M reduces the
alkalinity in the solution (less Na2O present), and higher
amounts of solution are required to satisfy the xed %Na2O;
this brings more soluble silicate species into the system, necessary for the formation of the reaction products, affecting the
resulting chemical composition and properties. During the reaction processes, not all of the SiO2 takes place in the reaction,
any unreacted SiO2 condenses as a silica gel contributing to the
compressive strength; however, an adequate M seems to exist in
which the chemical composition of the products and the amount
of condensing silica gel favor better CS. For example, a solution

Fig. 2. Inuence of the interaction AC on the compressive strength.

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Journal of the American Ceramic SocietyBurciaga-Daz et al.

Vol. 93, No. 2

pointed that for BFS, activation with %Na2O above a certain

value was not benecial but detrimental due to brittleness and
eforescence. In this case, a %Na2O410% possibly promoted
saturation of sodium cations in the systems; as a consequence, a
greater quantity of Na does not take place during the formation
of mechanically stable phases. The resulting matrix is mechanically weak, soft, and in some cases, undergoes deleterious carbonation; this was shown for cements activated with a relatively
high concentration of Na2O (Fig. 5). Various negative effects
were observed, such as carbonation, softening, and cracking,
due to various reactions, which will be discussed in another
publication (O. Burciaga, unpublished data).

Fig. 4. Inuence of the factor C on the compressive strength.

of M 5 1.52 is chemically less aggressive and more prone to

condensation 29 than one of M 5 0 or 1; thus, a higher M would
result in less dissolution of the BSF,16,30 and similar pattern
is obvious for Mk particles (as they required higher %Na2O).
Less reaction is detrimental to the mechanical properties. The
results obtained are in agreement with Wang et al.,23 who found
that for the alkaline activation of basic BFS, the optimum modulus of waterglass solution was 11.5. This modulus was sufcient to yield the highest CS, which in turn reect an adequate
activation in the BFS, Mk, and binary compositions of BFS-Mk.

(4) %Na2O (Factor C)

Figure 4 presents the mean values of CS as a function of
%Na2O in the binders, the factor that was statistically less important according to Table III. The CS increased as %Na2O
increased from 5 to 10%; however, addition of 410% Na2O
induced a decrease in the mechanical properties in the analyzed
systems.
It is known that the CS in alkali-activated systems is related
to the degree of condensation of stable phases such as CSH
and geopolymeric products. Considering this and based on the
results obtained, it could be concluded that increasing the
%Na2O within a given range would affect positively the mechanical properties of the obtained cements.31 Wang et al.23

(5) Scanning Electron Microscopy

SEM images of samples formulated with 100% Mk, Ms 5 1.5,
and 15% Na2O are presented in Fig. 6. After 1 day of curing,
unreacted particles of Mk remained, identied by an irregular
morphology of small agglomerates distributed homogeneously
throughout the microstructure. According to the results of
chemical composition measured by EDS spot analysis, the reaction products are formed by an amorphous gel (composed of
Si, Al, and Na) showing a gray shade darker than that of the
unreacted Mk. The brightness of the features in the microstructures observed by backscattered electron images depends directly on the average atomic number of the irradiated zone; the
incorporation of water into such a gel reduces the mean atomic
number, making it appear darker. After 360 days of curing, the
reactions had progressed and the microstructures were noticeably denser and homogenous and had very few unreacted Mk
particles. These observations are in agreement with the relatively
high values of CS developed for this binder (100% Mk,
Ms 5 1.5, and 15% Na2O). The cracks in the samples could
have been caused by the drying of the samples under the vacuum
of the microscope.
After 1 day, the reaction products had molar ratio SiO2/
Al2O3 5 4.2 (calculated from EDS measurements), and after 1
year the ratio was 3.7. This reduction of SiO2/Al2O3 with time
suggests that as the reactions progressed, higher amounts of Al
dissolved from the Mk; however, the reactions seemed to stop
after a certain period as discussed before. After 1 year, the measured SiO2/Al2O3 ratio of the reaction products was still greater
than that of the starting chemical composition of the whole mix
(solids and solution) SiO2/Al2O3 5 2.8; considering the presence
of unreacted Mk, altogether, this suggests that not all of the
sodium silicate added was incorporated into the geopolymeric

Fig. 5. Carbonated and cracked samples of BFS, due to the effect of free alkali at 360 days of curing.

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Statistical Strength Analysis of Alkali Activated Slag/Metakaolin Composites

545

Fig. 6. SEM micrographs and energy-dispersive spectroscopy of a system (with 100% Mk; Ms 5 1.5; 15% Na2O) at 1 and 360 days.

reaction products, and that some quantity of silica gel condensed in the microstructures. However, gray shade differences
between the geopolymeric gel and the silica gel were not noticeable; this suggests that the matrix of the geopolymeric binders is
formed by an intimate intermixture of these two gels not resolvable by the resolution of the images.

Figure 7 shows the microstructures of the composite 50%

BFS50% Mk, Ms 5 1.5, and 15% Na2O at 1 and 360 days.
After 1 day, the microstructures showed partially reacted BFS
and Mk. EDS indicated that the reaction products formed
around the Mk particles, and had higher concentrations of Si,
Al, and Na, suggesting the presence of a geopolymeric gel. In

Fig. 7. SEM micrographs and energy-dispersive spectroscopy of a composite system (with 50% BFS; 50% Mk; Ms 5 1.5; 15% Na2O) at 1 and 360
days.

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Journal of the American Ceramic SocietyBurciaga-Daz et al.

Vol. 93, No. 2

Fig. 8. SEM micrographs and energy-dispersive spectroscopy of a system (with 100% BFS; Ms 5 1.5; 5% Na2O) at 1 and 360 days.

contrast, the zones around the BFS particles showed high concentrations of Si, Ca, Al, and Na, indicating the possible formation of CSH, C2ASH8, C4AH13, and other hydrates as
reported by Escalante-Garcia et al.16 The results indicate that at
early ages, a slow dissolution of the BFS and Mk occurred, and
the silica gel condensed (from the alkaline solution) together
with some quantities of CSH and the geopolymeric gel (NS
AH)32 in localized points of the microstructure. Both processes
resulted in products of a darker gray tone than unreacted BFS
and Mk because they incorporate water.
After 360 days, the concentration of Na in the geopolymeric
gel was higher than in the CSH around BFS particles (calcium-rich area). This demonstrates that the Na added is structurally more important in the geopolymeric gel than for the C
SH. Yip et al.33 found that the presence of Na in the CSH gel
is possibly due to the formation of various sodium precipitates
such as sodium silicate, sodium carbonate, sodium sulfate, and
various forms of sodium aluminosilicate or aluminate. Also, after 1 year, the concentration of Ca increased around BFS particles and decreased around the Mk particles, whereas the
inverse trend was noted for Al. This indicates, in agreement
with,34 that during the reaction process, some additional Al dissolved from Mk and BFS, and some Al diffused out of BFS
zones to participate in the formation of geopolymeric gel (NA
SH). After 360 days, further condensation of CSH and
geopolymeric gel occurred, resulting in a dense consolidated
matrix with a more homogeneous gray tone of the reaction
products.
Figure 8 shows the microstructures of a binder with 100%
BFS; Ms 5 1.5; 5% Na2O at 1 and 360 days. After 1 day of
curing, unreacted BFS particles, identied by a bright gray tone
and a sharp irregular morphology, were observed to be homogenously dispersed in the matrix of reaction products. The latter,
from the interaction of the alkaline solution with the BFS,
showed a dark gray tone and were rich in Si and Ca, with
SiO2/CaO 5 1.59; other elements that were present in lower
contents were Al, Mg, and Na. This indicated that the hydra-

tion products (CSH, C4AHx, C2ASH8, hydrotalcite, etc.)

formed from the dissolution of BFS under an alkaline attack.
After 360 days, a more intense dissolution of BFS was observed, in agreement with the CS development. The EDS results
conrmed that the main hydration product was CSH with a
SiO2/CaO 5 1.11, possibly with other hydration products as mentioned above.16 The SiO2/CaO of the CSH for various cementitious systems has been reported as 0.5 for Portland cement, 0.57
for composites of BFS and Portland cement,34 and as 1.21.8 for
alkali-activated BFS.35 The higher SiO2/CaO indicates that much
more SiO2 is detected by the EDS in the spot analysis; this would
evidence the intimate precipitation of CSH from the BFS and
silica gel from the unreacted SiO2 added thorough the alkaline
solution, which is in agreement with previous reports.36 The reaction products of the activated BFS showed Al2O3/CaO ratios
higher than Portland cement and BFS-portland cement; this
could be interpreted as indicating the formation of CASH,
or as the formation of intimate mixtures of CSH with Al2O3bearing products such as C4AHx, C2ASH8, etc. Dark rims of reaction products, with high Mg contents, formed around the BFS
particles. A high localized Mg concentration has been observed
in BFS-activated cements, and has been attributed to the presence
of hydrotalcite36,37 intermixed with CSH in a submicrometer
scale in the hydration rims. The presence of such rims evidences
that at later stages, the formation of reaction products continues
by a solid-state mechanism.

IV. Conclusions
(1) Of the main factors (independent variables) investigated,
the ones most inuential on the strength development were:
Modulus of the alkaline solutionoBFS/Mk ratio-%Na2Oo
Curing time.
(2) The addition of BFS was positive on the compressive
strength for composites with Mk contents below 80% Mk.

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Statistical Strength Analysis of Alkali Activated Slag/Metakaolin Composites

(3) The results indicated that a modulus of 11.5 is sufcient

to promote an adequate activation of binders of BFS and Mk
and their binary mixes.
(4) The demand of Na2O increased with the load of Mk;
however, 10% Na2O was sufcient to promote adequate activation in BFSMk binders. Moreover, the interaction of the
factors BFS/Mk ratio and %Na2O was statistically most signicant.
(5) The addition of high amounts of Na2O in BFS binders
produces the degradation of the binders, mostly by carbonation
as the excess Na2O do not participate in the reactions.
(6) The main reaction products observed in binders with
100% Mk were geopolymeric products composed by Si, Al, and
Na, nely intermixed with silica gel.
(7) The simultaneous condensation of a geopolymeric gel
and CSH occurred in systems with 50% BFS50% Mk.
(8) For 100% BFS, the main reaction product was CSH,
which formed by a dissolution and precipitation mechanism
during the early stages of curing, but at later stages, the reaction
continued by a solid-state mechanism.

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