Cement and Concrete Research 54 (2013) 106113

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Cement and Concrete Research

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Inuence of the composition of cement kiln dust on its interaction with

y ash and slag
Piyush Chaunsali a, Sulapha Peethamparan b,
a
Department of Civil and Environmental Engineering, University of Illinois, Urbana-Champaign, IL 61801, USA
b
Department of Civil and Environmental Engineering, Clarkson University, Potsdam, NY 13699, USA

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

Article history: Cement kiln dust (CKD), a by-product of the cement industry, contains signicant amounts of alkali, free lime,
Received 26 May 2012 chloride and sulfate. Wide variation reported in the chemical composition of CKDs limits their potential applica-
Accepted 2 September 2013 tion as a sustainable binder component in concrete. In the current study, the performance of two different CKDs
as components in a novel binder is evaluated. Several binders are developed by blending CKDs with y ash or
Keywords:
slag. Binders with 70% CKD were prepared at a water-to-binder ratio of 0.4, and heat-cured at 75 C to accelerate
Cement kiln dust (CKD) (D)
X-ray diffraction (B)
the strength development. The hydration progress was monitored using X-ray diffraction, and morphological ex-
Scanning electron microscopy (B) amination was performed using scanning electron microscopy (SEM) and transmission electron microscopy
Transmission electron microscopy (B) (TEM). Ettringite and calcium aluminosilicate hydrate (C-A-S-H) were identied as the main hydration products
in the hardened binder system. Strength development of CKD-based binder was found to be signicantly
inuenced by its free lime and sulfate contents.
2013 Elsevier Ltd. All rights reserved.

1. Introduction
Cement kiln dusts (CKDs) are byproduct materials generated during
the clinker manufacturing process. They contain signicant amounts of
alkali, sulfate and chlorides. A large portion of CKD with lower alkali,
sulfate and chloride contents is recycled as raw material in the cement
kiln; the remainder of CKDs is landlled. Although CKD generation has
been reduced signicantly in recent years through continuous improve-
ment in the cement manufacturing process, a considerable amount of
CKD is still being landlled. Efforts are underway to utilize the CKD in
conjunction with other industrial byproducts in order to develop an
alternative binding material for sustainable concrete. The effective utili-
zation of CKD could reduce the environmental issues associated with
the disposal of CKDs in landlls.
The chemical composition of CKD changes among cement plants and
within each cement plant over time, resulting in an uncertainty in the
prediction of its performance as a binder component. Wide variations
observed in the chemical composition of CKDs limit their potential appli-
cation as value-added products. The alkali (Na2Oeq), sulfate, and free lime
contents of CKD have been reported to be as high as 8, 16, and 30%, re-
spectively [1]. The alkali present in CKD may play an important role in ac-
tivating aluminosilicate-containing minerals, y ash and slag, when CKD
is used as a major component in such binder systems. In fact, commercial
alkalis have been traditionally used in activating aluminosilicate contain-
ing materials [26]. Additionally, the presence of free lime and calcium
Corresponding author. Tel.: +1 315 268 4435; fax: +1 315 268 7985.
E-mail addresses: chaunsa2@illinois.edu (P. Chaunsali), speetham@clarkson.edu
(S. Peethamparan).
sulfate may also act as activators for aluminosilicates [79]. The strength
development in lime-containing binder systems is mainly attributed to
the formation of calcium silicate hydrate gel (C-S-H) as a result of a poz-
zolanic reaction, whereas the system containing CaSO4 results in the for-
mation of ettringite (AFt), monosulfate (AFm) and syngenite phases in
addition to the C-S-H gel formation [1,10,11]. It was also reported that
the presence of alkali makes CaSO4 more effective in activating the slag
in the binder system [12,13]. In general, CKDs containing a combination
of these activators (CaO, CaSO4, and different forms of alkalis) could po-
tentially result in a binding system with favorable mechanical properties
when used in conjunction with y ash and slag. Recent studies have
shown positive initial results supporting this hypothesis [1419].
In order to understand the inuence of the physico-chemical charac-
teristics of CKD on its performance as an effective binder component, a
detailed investigation on the interaction of two types of CKDs with y
ash and slag was undertaken. Elevated temperature curing was used
in addition to room temperature curing to expedite strength develop-
ment. The compressive strength development of both binders was mon-
itored under various curing conditions. The hydration progress and
microstructural changes were examined using X-ray diffraction (XRD),
scanning electron microscopy (SEM), and transmission electron micros-
copy (TEM).
2. Materials and experimental methods
2.1. Materials
Fig. 1 shows the particle size distribution of the CKDs used in this
study in comparison with that of the y ash and slag. CKD(I) was ner

0008-8846/$ see front matter 2013 Elsevier Ltd. All rights reserved.
http://dx.doi.org/10.1016/j.cemconres.2013.09.001
 P. Chaunsali, S. Peethamparan / Cement and Concrete Research 54 (2013) 106113 107

100 Fig. 2(c) shows the XRD patterns of both y ash and slag. The XRD
CKD (I)
pattern of class F y ash shows a diffuse band (peak at about 22) cor-
CKD (II)
Slag responding to the glassy phase as well as peaks indicating the presence
80 Class F Fly Ash of crystalline phases of silica and alumina. Similarly, a broader diffuse
Percentage Passing (%)

band was observed in slag, suggesting a higher fraction of amorphous

content compared to y ash.
60
2.2. Experimental methods

40
20
0
0.1 1 10 100
Particle Size (m)
Fig. 1. Particle size distribution.
than CKD(II). CKD(I) was generated in a cement plant that uses a dry
processing technology and a long cement kiln for the clinker produc-
tion, whereas CKD(II) was generated in a cement plant that uses a
long cement kiln but a wet processing technology. This difference in
the clinker processing technology is reected in the chemical composi-
tion presented in Table 1. The concentration of most of the reactive
oxide components was slightly higher in CKD(I), except for CaO and
K2O. The main difference in composition of the two CKDs was the alkali
(Na2Oeq) content (3.1 versus 6%, respectively), the sulfate (SO3) content
(10.62 versus 7.69%, respectively) and the free lime content (5 vs. 1.5%).
In addition, CKD(II) had approximately 0.62% chloride which was nearly
absent in CKD(I). In reinforced concrete, the permissible water-soluble
chloride content of ~0.15% (by weight of cement) has been suggested
[20]. The consequence of the high chloride content, in one of the
CKDs, on the onset of corrosion of reinforcing bar in CKD-containing
concrete is beyond the scope of this paper. Fig. 2(a) and (b) presents
the difference in mineralogy of the two CKDs used in the study. Calcium
carbonate (CaCO3), quartz (SiO2), anhydrite (CaSO4) and free lime
(CaO) were the crystalline phases present in both the CKDs. CKD(II)
contained a signicant amount of alkali in the form of sylvite (KCl)
and syngenite (K2CaSO42H2O), as shown in Fig. 2(b).
2.2.1. Sample preparation
Previous study by the authors examined the mineralogical and
microstructural evolution of CKD(I)-based binders [17,18]. The purpose
of this study was to compare the performance of CKDs from two dif-
ferent sources. The strength development, hydration progress and mi-
crostructure evolution of CKD(I) and CKD(I)-based binders were
examined. All binders contained 70% (by weight) CKD. A constant tem-
1000
perature (75 1 C), and xed curing duration (48 h) were used for
both CKD(I) and CKD(II)-based binders. Class F y ash/ground granulat-
ed blast furnace slag was homogenized with 70% CKD(I)/(II) (by mass of
the total binder) in dry conditions prior to mixing with water. A con-
stant water-to-binder ratio (w/b) of 0.40 was used to prepare the
CKDFA/CKDSlag pastes following ASTM C 305 procedure. The pre-
pared paste was then poured into 50 mm Plexiglas cube molds for
compressive strength testing and 31.75 mm-diameter cylindrical
molds for characterization studies. These molded specimens were
then compacted on a vibrating table. The compressive strength test
specimens were subsequently nished with a at trowel. All specimens
were sealed using a layer of plastic wrap followed by a layer of alumi-
num foil. The samples underwent 24 h of sealed curing at ambient tem-
perature (23 2 C), followed by 48 h of heat curing in a precision
laboratory oven set to 75 1 C. During the 48 h of heat curing, the
specimens were placed in sealed plastic boxes. After the initial heat cur-
ing, the samples were immersed in saturated lime water until the spec-
ied day of test.
Microstructural characterization was performed at various ages:
i) 1 day (after 24 h of sealed curing at ambient temperature),
ii) 3 days (after 24 h of sealed curing at ambient temperature and
48 h of heat curing), and iii) 31 days (after 24 h of sealed curing at am-
bient temperature, 48 h of heat curing and 28 days of saturated lime
water curing). Finally, the compressive strengths of cubes were deter-
mined after heat curing (3 days) and subsequent saturated lime water
curing (31 and 59 days) according to ASTM C 109.
2.2.2. Characterization techniques

2.2.2.1. X-ray diffraction. X-ray diffraction was performed using the

Table 1 Bruker DX-8 diffractometer operating at 40 kV and 30 mA. CuK radia-
Chemical composition of materials. tion of wavelength 1.5405 was used. Samples were scanned from 5
to 65 (2 range) at the rate of 0.02 per second. The samples used for
% weight
the analysis were ground to produce particles below 75 m size.
CKD(I) CKD(II) GGBFS Fly ash (class F)

Chemical composition 2.2.2.2. Thermogravimetric analysis. A Perkin-Elmer thermogravimetric

SiO2 14.55 11.69 36.00 50.20 analyzer was used for thermal analysis. A powdered sample (b75 m
Al2O3 4.46 2.20 10.53 28.70
Fe2O3 2.11 2.93 0.67 5.72
particle size) weighing approximately 25 mg was heated from 50 C
CaO 61.15 66.11 39.80 5.86 to 1000 C in a nitrogen environment (ow rate: 40 ml/min) at a
MgO 3.84 0.87 7.93 1.74 10 C per minute heating rate.
Na2O 0.80 0.87 0.27 0.96
K2O 3.45 7.24 0.15
2.2.2.3. Scanning electron microscopy. The fractured surface of paste sam-
SO3 10.62 7.69 2.11 0.51
Cl 0.62 ples was examined using a JEOL JSM-7400F electron microscope at ac-
Total 100.98 95.17 97.46 93.69 celerating voltage of 15 keV under secondary electron mode. The
samples were fractured to expose the fresh surface before mounting
Additional information
Na2Oeq 3.10 6.00 0.32 0.96 them on aluminum stubs using carbon paint. The samples were then
Loss on ignition 23.40 29.06 3.00 1.85 sputter-coated with goldpalladium for SEM examination.
Mean particle size ~4 m ~7 m ~7 m ~11 m

Note: The minor components such as TiO2, MnO and P2O5 are excluded from the oxide 2.2.2.4. Transmission electron microscopy. For transmission electron mi-
composition. croscopy (TEM) analysis, the powdered sample (passing through
108 P. Chaunsali, S. Peethamparan / Cement and Concrete Research 54 (2013) 106113

CC

CC

Q CC
CC Q
CC
CC
A L CC
L
CKD(I) CC CKD(II)
CC S CC CC
Arc CC A CC
Sg CC
Q L S

10 15 20 25 30 35 40 45 50 55 60 65 10 15 20 25 30 35 40 45 50 55 60 65
2-Theta (degrees) 2-Theta (degrees)
(a) (b)
Q

Q
Mu
Mu Mu
Fly Ash

Slag

10 15 20 25 30 35 40 45 50 55 60 65
2-Theta (degrees)
(c)
Fig. 2. X-ray diffraction patterns of: (a) CKD(I), (b) CKD(II), and (c) class F y ash and slag (A Anhydrite, CC Calcite, L Free lime, S Sylvite, Sg Syngenite, Q Quartz, Mu Mullite).

75 m) was rst diluted in isopropanol. Then a drop of solution was dis- higher neness of CKD(I) compared to CKD(II) (see particle size distri-
persed on a copper grid. The grids were kept under vacuum before ex- bution in Fig. 1) also might have contributed towards better perfor-
amination in a JEOL 2010 TEM instrument under an acceleration mance of CKD(I)-based binders.
voltage of 200 kV.
50
3. Results
CKD(I)-FA
CKD(II)-FA
CKD(I)-Slag
Compressive Strength (MPa)

3.1. Inuence of CKD type on the strength development of CKD-based 40

binders CKD(II)-Slag

The compressive strength of CKDFA and CKDSlag binders with 30

two different CKDs was determined as per ASTM C 109. Fig. 3 shows
the compressive strength of CKD-based binders (pastes) at three differ-
ent curing periods (3, 31, and 59 days) which includes the 48 h of heat 20
curing after initial 24 h of ambient curing and subsequent lime water
curing. As shown in Fig. 3, CKD(I)-based binders gained higher strength
than the CKD(II)-based binders. The compressive strength of the 10
CKD(I)Slag binder was in the range of 2540 MPa, whereas the
CKD(II)Slag binder exhibited only 1520 MPa strength under various
curing conditions. Similar performance of CKDFA binders can be seen 0
in Fig. 3, where CKD(II)FA resulted in lowest compressive strength 0 10 20 30 40 50 60 70
under all curing conditions. The higher strength of the CKD(I)-based Age (days)
binders can be attributed to several factors; the higher free lime, sulfate,
and other reactive components such as silica and alumina. Moreover, Fig. 3. Effect of CKD type on strength development of CKDFA and CKDSlag pastes.
 P. Chaunsali, S. Peethamparan / Cement and Concrete Research 54 (2013) 106113 109

3.2. Hydration progress in CKD-based binders
3.2.1. CKDFA binder
The growth of crystalline phases during the hydration of CKDFA
binders was monitored using XRD. The XRD patterns collected from
samples after subjecting them to various curing conditions are
presented in Fig. 4(a) and (b) for CKD(I)FA and CKD(II)FA mixtures,
respectively. The crystalline hydration products identied in 1 day-old
CKD(I)FA paste sample before heat curing were ettringite (E), calcium
hydroxide (CH), and gypsum (G). As expected, the pozzolanic reaction
between calcium hydroxide and amorphous phases of y ash was accel-
erated by heat curing. At the end of 48 h of heat curing, the amount of
CH was signicantly reduced, potentially due to its consumption during
the pozzolanic reaction. Additionally, during the heat curing, the
alkalis and sulfates were adsorbed onto the reaction products, mainly
to C-S-H [10]. The adsorbed sulfates and the alkalis were presumably
released into the pore solution later during the lime water curing
period, which contributed to additional precipitation of ettringite and
arcanite (Fig. 4(a)).
The main difference in the mineralogy of CKD(II)FA binder com-
pared to the CKD(I)FA binder was the presence of Friedel's salt and
sylvite (Fig. 4(b)) in heat cured samples at 3 days. Although ettringite
was detected in one day old CKD(II)FA sample, the peak almost
disappeared after heat curing at 3 days. Friedel's salt and sylvite were
found only in 3-day old samples; subsequent lime water curing led to
an increase in the amount of ettringite and the disappearance of sylvite.
The chlorides seem to have released into the pore solution during the
lime water soaking period. Analysis of the pore solution can provide in-
formation regarding the fate of chlorides at later ages. Although the pore
solution analysis and the fate of the chloride ions are important for
predicting the corrosion resistance of reinforced concrete that contain
the CKD-based binders, this analysis was beyond the scope of the
current study. The use of CKD with high chloride content might cause
chloride induced corrosion durability issues in reinforced concrete and

CC

CC

CKD(I)-FA
CKD(II)-FA

E Q Q
Arc
E CC CC
E CC CC CC 31 d E Q CC CC
E CC CC CC 31 d
E

3d
S 3d
Fr

CH
G 1d 1d

5 10 15 20 25 30 35 40 45 50 55 60 65 5 10 15 20 25 30 35 40 45 50 55 60 65
2-Theta (degree) 2-Theta (degree)

(a) (b)
Fig. 4. X-ray diffraction patterns of CKD(I)FA and CKD(II)FA paste (Arc arcanite, CH calcium hydroxide, CC calcite, E ettringite, Fr Friedel's salt, G gypsum, Q quartz,
S sylvite).
110 P. Chaunsali, S. Peethamparan / Cement and Concrete Research 54 (2013) 106113

hence should be evaluated thoroughly prior to using it in the eld. Only
traces of CH were present in the CKD(II)FA mixture, mainly because of
the low free lime content of CKD(II).
3.2.2. CKDSlag binder
Fig. 5 compares the hydration progress of CKD(I)Slag and CKD(II)
Slag binder. Ettringite was present in both binders at all ages, although
it was found in smaller quantities in CKD(II)Slag binder. Interestingly,
the precipitation of Friedel's salt (C3ACaCl210H2O) was observed in
CKD(II)Slag binder at early ages (i.e., before and after heat curing)
(Fig. 5(b)). Konsta-Gdoutos and Shah also observed the Friedel's salt at
early-age in CKDSlag binder prepared with CKD having high chloride
content [14]. In their study, Friedel's salt was observed in the CKDs with
1.4% and 1.8% chloride content. After saturated lime water curing, Friedel's
salt was not detected in CKD(II)Slag binder. It is known that heat curing
results in adsorption of sulfate ions into C-S-H gel [10], and after subse-
quent saturated lime water curing, the concentration of sulfate ions in
the pore solution increases, presumably due to the desorption of the sul-
fate ions from the C-S-H. This increase of sulfate concentration in the pore
solution favors the precipitation of ettringite at later ages along with the
depletion of Friedel's salt as shown in Fig. 5(b). As discussed before, it ap-
pears that the chloride ions were released into pore solution during the
saturated lime water curing. Contrary to what was observed in CKD(I)
Slag binder, only traces of CH were detected in CKD(II)Slag binder. This
can be attributed to the relatively low free lime present in CKD(II).
3.3. Microstructural changes in CKD-based binders
3.3.1. CKDFA binder
3.3.1.1. SEM. Fig. 6(a) and (b) shows the morphological difference in the
reaction products of CKD(I)FA and CKD(II)FA mixtures after 48 h of
heat curing, respectively. It appears that, as shown in Fig. 6(a), almost
all of the y ash particles were covered with reaction products in
CKD(I)FA mixture, whereas in CKD(II)FA mixtures the reaction was
not that extensive. Even ne y ash particles were present without
showing any signs of reaction (Fig. 6(b)). Fig. 7(a) and (b) shows
the SEM micrographs of a y ash grain and the surrounding area in

CC CC

CKD(I)-Slag CKD(II)-Slag

E Q Q
CC CC CC CC CC
CC CC 31 d E CC
E CC CC 31 d
E E E Q

3d 3d

Fr Sg
CH 1d 1d
G

5 10 15 20 25 30 35 40 45 50 55 60 65 5 10 15 20 25 30 35 40 45 50 55 60 65
2-Theta (degree) 2-Theta (degree)

(a) (b)
Fig. 5. X-ray diffraction patterns of CKD(I)Slag and CKD(II)Slag paste (CH calcium hydroxide, CC calcite, E ettringite, Fr Friedel's salt, G gypsum, Q quartz, Sg syngenite).
 P. Chaunsali, S. Peethamparan / Cement and Concrete Research 54 (2013) 106113 111

Fig. 6. SEM micrographs of: (a) CKD(I)FA, and (b) CKD(II)FA after heat curing (3 days).

CKD(I)FA and CKD(II)FA binders, respectively. Higher reactivity of y of reaction gel can be observed in Fig. 9(a) and (b). The difference in
ash in CKD(I)FA binder also resulted in higher strength in comparison the morphology of reaction gel may also have an inuence on strength
to CKD(II)FA binder. development in CKDSlag binders.

3.3.1.2. TEM. To further examine the morphology of C-A-S-H gel present
in CKD-based y ash binders, the microstructure was examined under a
TEM. A brillar morphology for C-A-S-H is clearly evident in this TEM
micrograph. In TEM examination, some of the regions (including the lo-
cation around the y ash particle) had a relatively different morphology,
as seen in Fig. 8(b).
3.3.2.2. TEM. TEM examination revealed the brillar morphology of C-S-H
gel formed in CKD(I)Slag and CKD(II)Slag binders (Fig. 10).
4. Discussion
4.1. Factors inuencing the development of compressive strength

3.3.2. CKDSlag binder It is evident that CKD(I)-based binders attained higher strength than
CKD(II)-based binders. The y ash and slag were activated by calcium
3.3.2.1. SEM. Fig. 9 shows the microstructure of CKD(I)Slag and hydroxide and alkalis released during CKD hydration. Furthermore, cal-
CKD(II)Slag paste after heat curing. A relatively different morphology cium sulfate acted as an activator in the presence of alkalis [10,12].

Fig. 7. SEM micrographs of: (a) CKD(I)FA, and (b) CKD(II)FA after heat curing (3 days).
112 P. Chaunsali, S. Peethamparan / Cement and Concrete Research 54 (2013) 106113
Fig. 8. (a) TEM micrograph of CKD(I)FA after heat curing (3 days), and (b) the light morphology of C-S-H around the shell of y ash particle.
Higher strength of CKD(I)-based binders can be attributed to higher
amount of ettringite and increased activation of y ash and slag parti-
cles. Ettringite was present in larger amounts in CKD(I)-based binders
than in CKD(II)-based binders, possibly due to higher SO3 and alumina
contents. In addition, the higher lime content of CKD(I) resulted in a
larger amount of C-A-S-H gel formed during the pozzolanic reaction in
CKD(I)-based binders than in CKD(II)-based binders. In spite of the
higher alkali content, CKD(II) did not exhibit better performance com-
pared to CKD(I) with respect to the strength development. The calcium
hydroxide formed during CKD hydration triggers the pozzolanic reac-
tion in y ash-containing binders and results in the formation of C-A-
S-H. Since CKD(I) had higher free lime content, larger amounts of reac-
tion gel are expected to form in CKD(I)FA based binders. In addition,
higher sulfate content in CKD (I) caused more ettringite formation in
CKD(I)-based binders. It seems that the small difference in free lime
and sulfate contents of the CKD signicantly alters the strength of the
resulting binder. The results of this study agree with the ndings of a
previous study where the sulfate and lime contents of CKD were
found to be the key factors inuencing the binder system's strength de-
velopment [14].
4.2. Implication of CKD chemistry on the composition and morphology of
microstructure
The morphology of reaction gel in CKD-based binders was observed
to be brillar, as illustrated by TEM examination. Furthermore, SEM
Fig. 9. SEM micrographs of: (a) CKD (I)Slag and (b) CKD(II)Slag paste after 48 h of heat curing (3 days).
analysis indicated a difference in the morphology of the binder resulting
from two different CKDs. The dissolution of y ash particles, as shown
by SEM examination of the CKDFA binders, indicated the y ash's
higher reactivity in the presence of CKD(I), which resulted due to
CKD(I)'s higher lime and sulfate contents. It is noted that the elevated
temperature curing might alter the morphology of the reaction product
(C-A-S-H) in CKD-based binders. Therefore, the results presented here
are solely for the samples heat cured at 75 C.
4.3. Role of alkalis and sulfates on stability of ettringite
In this study, ettringite was found to be stable in CKD(I)-based
binders even at high temperature (75 C), as indicated by X-ray diffrac-
tion. On the other hand, the amount of ettringite was reduced after heat
treatment in CKD(II)-based binders. The stability of ettringite at a par-
ticular temperature depends on the pH of the pore solution and the
availability of sulfate ions. Damidot and Glasser [21] reported the pH
ranges for ettringite stability as 10.8712.25 and 10.4312.52 for 85 C
and 25 C respectively. Their study suggests that the upper threshold
for pH is reduced with an increase in temperature. Similarly, the sulfate
concentration dictates which form would be dominant between AFt and
AFm phases. Therefore, higher alkali content and lower sulfate content
of CKD(II) appear to have decreased the stability of ettringite at 75 C.
Experimental ndings in this work clearly show the benecial effect
of free lime and sulfate contents in strength development of CKD-based
binders. However, the efcacy of alkalis in CKD needs to be investigated
 P. Chaunsali, S. Peethamparan / Cement and Concrete Research 54 (2013) 106113
Fig. 10. TEM micrographs of: (a) CKD(I)Slag paste, and (b) CKD(II)Slag paste after heat curing (3 days), showing the brillar morphology.
further to determine their role on mechanical strength development of
the binder.
5. Conclusions
The inuence of CKD composition on the microstructure and
strength development of CKD-based binders is discussed in this study.
The essential ndings are summarized as follows:
Free lime and sulfate contents of CKD inuenced the strength devel-
opment of CKD-based binders signicantly. The CKD with higher
free lime and sulfate contents attained higher compressive strength.
Ettringite and C-S-H are the main hydration products found in CKD-
based binders. In CKD with higher alkali content and lower sulfate
content, the formation of ettringite was decreased during the heat
curing.
TEM investigation revealed the brillar morphology of C-S-H gel in
CKD-based binders.
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