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Article history:
Received 31 July 2015
Received in revised form
25 November 2015
Accepted 6 December 2015
Available online xxx
Alkali activated y ash/slag (AAFS), a newly evolved type of alkali-activated cements (AACs), is here
studied with the aim of developing a more sustainable alternative to Portland cement (PC), known for its
adverse environmental impact. In this study, sodium carbonate (Na2CO3) was used as the alkali activator
for the y ash (FA)/slag blends. The effects of different factors on the strength, reaction rate, hydration
products and microstructure were examined; these factors include the activator dosage, FA/slag ratio,
and curing regime. It was found that increasing the Na2CO3 dosage signicantly increased the
compressive strength. The inclusion of up to 25 wt% y ash marginally decreased the compressive
strength up to 28 days while the inclusion beyond 25 wt% can lead to a remarkable reduction in strength,
particularly for water-cured specimens. Sealed curing in general was found to be benecial to the
strength development of AAFS paste especially at a 50/50 ratio of FA/slag. Both the activator dosage and
FA/slag ratio were found to have notable inuences on reaction rate and reaction products and microstructure. Increasing the activator dosage accelerates the kinetics of the reaction while increasing the FA/
slag ratio slows the reaction rates. The main binding phase is C-(N)-A-S-H with varying Ca/Si ratios
ranging between 0.6 and 1.0 depending mainly on FA/slag ratio. The results indicated the possibility of
production of greener cementing materials by utilizing appropriate ratios of FA/slag, dosage of sodium
carbonate, and curing regimes.
2015 Elsevier Ltd. All rights reserved.
Keywords:
Fly ash
Slag
Sodium carbonate
Alkali-activated cements
Microstructure
1. Introduction
Carbon dioxide (CO2) emissions associated with Portland
cement (PC) production account for 5e10% of global man-made CO2
emissions (Scrivener and Kirkpatrick, 2008), a fact that puts an
onus on the cement industry to nd a more environmentally
benign alternative. Alkali activated cements (AACs), which have
been known about since the 1960s, are one of the candidates for
green concrete (Provis, 2013). AACs are cementitious materials
formed as a result of the dissolution of aluminosilicate precursors
from natural or industrial waste materials in an alkaline environment. These materials, when mixed with alkaline activators, set
and harden, producing a binder with good mechanical and durability properties. Most recent estimates indicated that 55%e75%
reduction of CO2 emissions compared to PC can be achieved by
using AACs in concrete (Yang et al., 2013).
* Corresponding author.
E-mail address: aalqader@gmail.com (A.F. Abdalqader).
The use of by-product materials in cement signicantly decreases the negative impacts on the environment. Firstly it is not
necessary to quarry virgin material to manufacture these byproduct materials. Secondly, it reduces the land demand for landlling. Finally, it saves energy (Higgins et al., 2011; Nehdi, 2011).
Meanwhile, these by-products are increasingly being generated on
a planetary scale (Nehdi and Mindess, 1999). Therefore, not only do
these materials improve the sustainability of cement but they also
compensate for the shortage in supply due to the increasingly high
demand of construction materials (Sarkar and Roumain, 2003).
Ground granulated blast-furnace slag (GGBS) and y ash (FA) are
the most prevalent industrial by-products used in the productions
of AACs. GGBS is a by-product from the manufacture of iron.
Globally, the annual production of GGBS is estimated to be
270e320 Mt (USGS, 2013a). While the production of 1 t of PC needs
5000 MJ of energy, with a corresponding CO2 emissions of 1 t, the
production of 1 t GGBS consumes only 1300 MJ of energy and emits
only 0.07 t CO2 to the atmosphere (Cabeza et al., 2013). FA is a byproduct material collected among other coal combustion products
from the burning of coal in power station furnaces. The worldwide
http://dx.doi.org/10.1016/j.jclepro.2015.12.010
0959-6526/ 2015 Elsevier Ltd. All rights reserved.
Please cite this article in press as: Abdalqader, A.F., et al., Development of greener alkali-activated cement: utilisation of sodium carbonate for
activating slag and y ash mixtures, Journal of Cleaner Production (2015), http://dx.doi.org/10.1016/j.jclepro.2015.12.010
Table 1
Chemical composition and physical characteristics of the materials used (based on
the suppliers' datasheets).
Component
GGBS
FA
CaO%
SiO2%
Al2O3%
Fe2O3%
MgO%
SO3%
K2O%
Na2O%
SSA (m2/kg)
L.O.I
39.24
36.79
11.51
0.42
8.10
1.03
0.63
0.37
545
0.63
6.8 3.6
49.3 6.2
24.1 0.4
9.7 1.3
1.1 0.2
3.3 1.3
3.5 0.3
1.2 0.1
2600
3.9a
Please cite this article in press as: Abdalqader, A.F., et al., Development of greener alkali-activated cement: utilisation of sodium carbonate for
activating slag and y ash mixtures, Journal of Cleaner Production (2015), http://dx.doi.org/10.1016/j.jclepro.2015.12.010
Table 2
The mix proportions used in this study.
Mix ID
GGBS%
FA%
Na2CO3%
G100F0N5 (-Sa)
G75F25N5 (-S)
G50F50N5 (-S)
G100F0N10 (-S)
G75F25N10 (-S)
G50F50N10 (-S)
100
75
50
100
75
50
0
25
50
0
25
50
5
5
5
10
10
10
2.2. Tests
The compressive strength testing was carried out using Controls
Advantest 9 with a maximum capacity of 250 kN and with a loading
rate of 2400 N/s. Three identical cubes were tested at different
periods of ageing, namely 3, 7, 28, 56, and 90 days. The cube
strength reported herein was an average of three specimens at each
period of ageing. Immediately after the compressive strength test
was performed at 28-day age, selected samples for microstructural
analyses were immersed in acetone for three days in order to stop
any further hydration. Then the samples were ltered to remove
the acetone followed by vacuum drying in a desiccator and oven
drying at 60 C for at least 24 h. Thereafter, parts of each sample
were crushed and ground in an agate mortar until passing 75 mm
sieve and the sealed in plastic vials for XRD, FTIR, and TGA analysis.
Isothermal calorimetry experiments were conducted using a
TAM Air Isothermal calorimeter, at a base temperature of
20 0.02 C. Fresh paste was mixed externally, weighed into an
ampoule, and immediately placed in the calorimeter, and the heat
ow was recorded for the rst 140 h of reaction except for the
sample G100F0N5 where the data was recorded for 72 h as it was
done as a preliminary sample before deciding to extend the
observation period to 140 h. All values of the heat release rate were
normalised by the total weight of the paste.
Powder XRD was employed to identify the crystalline phases in
the sample. The powders were placed on glass microscope slides
onto which acetone was dripped. After the acetone evaporated,
the sample was afxed to the slide and placed in the Siemens
D500 X-ray diffractometer with a CuKa source operating at 40 kV
and 40 mA, emitting radiation at a wavelength of 1.5405 . The
scanning regions were between 2q values of 5e60 , at a rate of
0.02 /step. TGA experiments (Perkin Elmer STA6000, Simultaneous Thermal Analyser) were conducted using 20 2 mg of
powder under static air in an open alumina crucible heated at
10 C/min over the range of 40e1000 C. Temperature and weight
change, DW, (mg) were recorded every 0.1 s. FTIR spectra of the
samples were taken using Perkin Elmer FTIR Spectrometer Spectrum 100 Optica. Spectra were collected in transmittance mode
from 4000 to 600 cm1 at a resolution of 1 cm1. Additionally,
backscattered electron microscopy (BSE) and energy dispersive Xray analysis (EDX) were carried out on the 28-day samples using
FEI Nova NanoSEM FEG at 15 kV accelerating voltage and a
working distance of 5 mm. The samples were impregnated in
epoxy resin prior to polishing down to 0.25 mm and thereafter
coated with carbon.
Please cite this article in press as: Abdalqader, A.F., et al., Development of greener alkali-activated cement: utilisation of sodium carbonate for
activating slag and y ash mixtures, Journal of Cleaner Production (2015), http://dx.doi.org/10.1016/j.jclepro.2015.12.010
at late ages more than in the early stages due to its low reactivity.
The long-term improvement in mechanical strength by the inclusion of FA was also reported in the literature (Chi and Huang, 2013;
Guerrieri and Sanjayan, 2010; Ismail et al., 2013b; Puertas et al.,
2000). However, increasing the content of FA to 50% (triangle
shape) decreased the strength signicantly particularly for samples
cured under water at all ages and in sealed curing at early ages. For
samples with FA/slag ratio of 50/50 and cured under water, the
strength was very low due to the slow reaction of such system with
Na2CO3. A possible explanation for this might be that the leaching
of alkali ions in water delayed the reaction kinetics and decreased
the extensive reaction of the precursors. The decrease in mechanical strength due to the increased content of FA in AAS systems,
activated by different activators, has been observed in the literature
by many researchers (Escalante Garca et al., 2006; Kim and Kim,
2012; Kumar et al., 2010; Li and Sun, 2000; Puertas et al., 2003;
Shen et al., 2011; Shi and Day, 1999; Wang et al., 1994). For
example, Li and Sun (2000) showed that inclusion of more than 10%
of FA led to a drop in the compressive strength for mixtures activated by 5% Na2CO3 combined with 5% NaOH. On the contrary,
some researchers found either insignicant change or positive
change on the strengths by adding up to 50 wt.% FA (Chen et al.,
2015; Chi and Huang, 2013; Collins and Sanjayan, 1999; Guerrieri
and Sanjayan, 2010; Shi and Day, 1999). The discrepancies in
these studies correspond to the differences in the activator type and
concentration, the aluminosilicate materials' physical and chemical
properties, and the curing conditions.
Fig. 3 shows the 28-day compressive strength of all mixes in
both curing conditions. The main feature is that the sealed curing
led to higher compressive strength than curing under water. The
most notable improvement was observed for mixes including 50%
FA. Samples G50F50N5-S and G50F50N10-S had ~4 times and 5
times higher strength than G50F50N5 and G50F50N10, respectively. The possible explanation for the improved strength by sealed
curing is that it prevents the ions from leaching into the water, thus
enhancing the reaction rate and leading to more strength-giving
products. Comparison between these types of curing has not previously been reported in the literature. However, it was suggested
that sealed curing of AAFS can yield better strength over underwater curing (Lloyd, 2008).
3.2. Isothermal calorimeter
The heat release curves, normalized by the mass of starting
materials, of mixes containing 0% and 25% y ash at both activator
Fig. 4. Heat release rate (top) and cumulative heat release (bottom) of mixes.
Please cite this article in press as: Abdalqader, A.F., et al., Development of greener alkali-activated cement: utilisation of sodium carbonate for
activating slag and y ash mixtures, Journal of Cleaner Production (2015), http://dx.doi.org/10.1016/j.jclepro.2015.12.010
observations are common for mixes containing 25% FA. The difference between the two systems was the time at which the second
peak appeared. The intensity of this peak and the starting time
depend strongly on the properties of the slag, the activator dosage,
and the mineral additives (Abdalqader et al., 2015).
Fig. 6. Effect of activator dosage and curing condition on XRD for some mixes at 28
days.
transforms to other phases with curing time as its peaks diminished with time. A low intensity peak at 11.7 2q is also observed,
assigned to hydrotalcite (Mg6Al2(CO3) (OH)16$4(H2O), which has
also previously been identied in other alkali-activated slag systems (Haha et al., 2011; Puertas and Fernandez-Jimenez, 2003).
This phase is very stable and its content increased with time as
shown in Fig. 5 (see increased peaks' intensities at 11.7 2q and 23
2q).
In the mixes with 25 wt.% FA (Fig. 5b), a poorly ordered C-S-H
type gel is also observed alongside calcite, hydrotalcite, and gaylussite. However, the peak intensity of hydrotalcite phase is much
smaller in this mix than the neat slag binders. The crystalline phase
quartz, from the unreacted y ash, was also identied. The peak of
gaylussite decreased with time and almost disappeared after 180
days indicating the transformation of these phases into other
phases. Additionally, the peak of quartz between 28 days and 180
days also decreased which may correspond to the activation of y
ash.
Fig. 6 shows the effect of activator content and curing condition
on the hydration products formed. In general, same hydration
products were detected in the mixes containing 25% FA regardless
of activator dosage and curing condition. However, it was observed
that increasing the Na2CO3 dosage from 5% to 10% facilitated the
formation of gaylussite due to the higher availability of Na and
CO2
3 ions. Furthermore, sealed curing also increased the intensity
of this phase, which can be attributed to its prevention of these ions
from leaching into the water as mentioned above. This agrees well
with the strength results. The same trend was observed for the
formation of calcite. Further evidence of enhanced hydration by
sealed curing was manifested by the reduction in the quartz peak
compared to the water curing, which indicates the increased
dissolution of FA and hence increased amounts of hydration
products.
3.4. Thermogravimetric analysis
Fig. 5. XRD for (a) G100F0N10 and (b) G75F25N10 at different ages.
Please cite this article in press as: Abdalqader, A.F., et al., Development of greener alkali-activated cement: utilisation of sodium carbonate for
activating slag and y ash mixtures, Journal of Cleaner Production (2015), http://dx.doi.org/10.1016/j.jclepro.2015.12.010
Please cite this article in press as: Abdalqader, A.F., et al., Development of greener alkali-activated cement: utilisation of sodium carbonate for
activating slag and y ash mixtures, Journal of Cleaner Production (2015), http://dx.doi.org/10.1016/j.jclepro.2015.12.010
Fig. 10. BSEM images at 28 days of mixes (a) G100F0N10, (b) G75F25N5, (c) G75F25N10, (d) G50F50N10-S.
Please cite this article in press as: Abdalqader, A.F., et al., Development of greener alkali-activated cement: utilisation of sodium carbonate for
activating slag and y ash mixtures, Journal of Cleaner Production (2015), http://dx.doi.org/10.1016/j.jclepro.2015.12.010
hydrated yet with clear hydration rims around. Likewise, Fig. 10bed
shows the same trend for slag particles. Hydration rims also were
formed around the slag and FA particles, particularly for mixes
activated by 10% Na2CO3. These reaction products grew gradually
from the outer area into the inner part of the unreacted particles. FA
particles have been embedded in the matrix (Fig. 10bed) so, when
unreacted, they can play a space-lling role. This may explain the
unchanged strength in samples containing up to 25% FA. However,
when the content of FA increased (Fig. 10d), this affected the reaction mechanism and led to strength reduction due to the low
reactivity of FA.
To determine the elemental composition of the hydration
products, EDX was performed on at least 20 points selected on the
gels and some of the slag grains on samples cured for 28 days at a
magnication of 2500. The data are presented here in a ternary
composition graph of CaeSieAl (Fig. 11a) and in a Al/Si vs Mg/Si
graph (Fig. 11b). These plots clearly show the variation in gel
composition across the different AAFS blends as a function mainly
of FA/slag ratio and to a less degree of activator dosage and curing
conditions. The main binding phase in neat slag binders is C-A-S-H
gel (dashed circle in Fig. 11a), in agreement with what have been
reported in the literature (Bernal et al., 2014; Deir et al., 2014;
Escalante-Garca et al., 2003; Ismail et al., 2013a; Puertas and
Fernandez-Jimenez, 2003). In samples containing 25% FA, a binding phase of both C-A-S-H and C-(N)-A-S-H is likely to be formed,
while increasing the FA content to 50% led to the formation of C(N)-A-S-H as the major binding-phase (dotted circle in Fig. 11a).
Again, this trend has been observed in other studies (Ismail et al.,
2014; Marjanovic et al., 2015; Puertas and Fernandez-Jimenez,
2003; Puertas et al., 2000; Puligilla and Mondal, 2015; Zhao et al.,
2007) using various alkali activators. It is suggested that the use of a
higher activator concentration enhances the incorporation of Al
into the gel structure when introducing FA (Lloyd et al., 2010). The
main modication induced in the current study mixtures is the
incorporation of carbonate-bearing products such as gaylussite and
calcite.
In Fig. 11b, the approximate linear correlation of Mg/Si with Al/Si
indicates the existence of other phases rich in aluminum and
magnesium such as hydrotalcite-like phases, which was also
detected by XRD and TGA and previous studies (Bernal et al., 2014;
Escalante-Garca et al., 2003; Ismail et al., 2014; Jin et al., 2014;
Puertas and Fernandez-Jimenez, 2003). The presence of a positive
x-axis intercept reveals the level of incorporation of Al in the C-S-H
(Table 3).
The average chemical compositions of the gels in some samples
at 28 days are shown in Table 3. The Ca/Si ratio decreased with
increasing FA due to the reduction of Ca2 ions resulted from the
partial replacement of GGBS. Al/Si values varied between 0.38 and
0.43, which is very high for either a pure chain-structured C-A-S-H
phase (Al/Si < 0.2 (Hunnicutt, 2013)) or considerable degree of
crosslinking (0.19 Al/Si 0.26) (Myers et al., 2013). Therefore, it
may correspond to the presence of additional Al-rich products
intermixed with Al-substituted C-S-H gel (Bernal et al., 2014). The
range of Na/Si in the investigated samples was from 0.14 to 0.53 as
shown in Table 3. The role of Na in the structure of the reaction
products is to balance the negative framework charge induced by
the incorporation of Al (Duxson et al., 2006; Puertas et al., 2000) as
Na Al3 Si4 (Hong and Glasser, 2002). The curing conditions
did not substantially affect the elemental composition of pastes.
3.7. Proposed reaction mechanism
Combining the results of mineralogical and microstructural
analysis, this study clearly showed that the reaction mechanism of
Na2CO3-activated FA/slag is dependent on the activator dosage,
(a)
(b)
Fig. 11. EDX analysis of some mixes at 28 days (a) ternary plot of CaeAleSi, (b) atomic
ratios Al/Si vs Mg/Si.
Please cite this article in press as: Abdalqader, A.F., et al., Development of greener alkali-activated cement: utilisation of sodium carbonate for
activating slag and y ash mixtures, Journal of Cleaner Production (2015), http://dx.doi.org/10.1016/j.jclepro.2015.12.010
Table 3
Calculated parameters from EDS results at 28 days.
Sample
Ca/Si
Al/Si
Mg/Si
Na/Si
Al substitution
Slag
G100F0N10
G75F25N5
G75F25N10
G75F25N10-S
G50F50N10-S
1.19
1.07
0.95
0.83
0.71
0.63
0.40
0.40
0.44
0.43
0.38
0.41
0.36
0.25
0.35
0.30
0.27
0.18
0.09
0.14
0.42
0.53
0.31
0.33
0.7
1.90
1.34
1.94
1.28
0.40
e
0.27
0.18
0.28
0.18
NA
NA not applicable.
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activating slag and y ash mixtures, Journal of Cleaner Production (2015), http://dx.doi.org/10.1016/j.jclepro.2015.12.010
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Please cite this article in press as: Abdalqader, A.F., et al., Development of greener alkali-activated cement: utilisation of sodium carbonate for
activating slag and y ash mixtures, Journal of Cleaner Production (2015), http://dx.doi.org/10.1016/j.jclepro.2015.12.010