Int J Civ Eng (2016) 14:425–438
DOI 10.1007/s40999-016-0027-0
RESEARCH PAPER
Efflorescence Formation and Control in Alkali-Activated
Phosphorus Slag Cement
Hojjatollah Maghsoodloorad1 • Ali Allahverdi1,2
Received: 3 March 2015 / Revised: 28 November 2015 / Accepted: 27 January 2016 / Published online: 30 May 2016
Ó Iran University of Science and Technology 2016
Abstract Efflorescence formation is an important sound-
ness issue to be considered with alkali-activated cements.
In this study, the impact of activator type on the efflores-
cence formation severity and methods of efflorescence
reduction in alkali-activated phosphorus slag cement are
investigated. Different alkaline activators including NaOH,
KOH and liquid sodium silicate of different silica modules
(Ms = SiO2/Na2O) were used for alkali-activation of
phosphorus slag. Additions of high alumina cements (Secar
71 and 80) and application of hydrothermal curing condi-
tion at 85 °C for 7 h with different pre-curing times (1, 3
and 7 days) in humid environment (relative humidity of
95 %) and 25 °C were used for efflorescence control in
alkali-activated phosphorus slag cement. Sodium contain-
ing activators resulted in more severe efflorescence for-
mation compared with those of potassium containing
activators. Also presence of liquid sodium silicate inten-
sified efflorescence formation. Based on the results
obtained, application of an optimum pre-curing stage in
humid environment before hydrothermal curing regime
stabilizes the cement matrix and improves the effectiveness
of hydrothermal conditions.
Keywords Efflorescence  Phosphorus slag  Alkali-
activation  Hydrothermal curing
& Ali Allahverdi
ali.allahverdi@iust.ac.ir
1
Research Laboratory of Inorganic Chemical Process
Technologies, School of Chemical Engineering, Iran
University of Science and Technology, Narmak,
Tehran 1684613114, Iran
2
Cement Research Center, Iran University of Science and
Technology, Narmak, Tehran 1684613114, Iran
1 Introduction
Portland cement is the most common binder for con-
struction purposes. The energy crisis and the environ-
mental impacts of the production process of Portland
cement due to greenhouse gasses emission, have moti-
vated researchers to find proper alternative binders
exhibiting good durability, high environmental compati-
bility and potential of using industrial wastes as starting
precursors [1–3]. Some of the alkali-activated and
geopolymer cements can be considered as the most suit-
able alternatives to Portland cement. Alkali-activated slag
cement was first produced by Purdon in 1940 using blast-
furnace slag and sodium hydroxide [4]. Later in 1978,
Joseph Davidovits applied the same technology to reac-
tive aluminosilicate materials and developed geopolymer
cements [5].
Alkali-activated and/or geopolymer cements can be
produced by mixing alkaline materials such as NaOH,
KOH, sodium silicate, and Na2CO3 [6] with suitable start-
ing precursor materials like blast-furnace slag [7–11],
metakaolin [12–15], fly ash [16–19] natural pozzolans
[20, 21] and their mixtures [12, 19, 22–24].
An important soundness issue encountered with alkali-
activated and/or geopolymer cements is efflorescence for-
mation [25]. Efflorescence formation results from migra-
tion of un-reacted alkalis from bulk regions of the material
to its surface followed by carbonation reaction with
atmospheric CO2 [26–28]. The produced carbonates
deposit on the surface and inside regions close to the sur-
face of the material. Continued migration of alkalis fol-
lowed by carbonation then gradually results in internal
stresses due to the growth of crystals. Disintegrating
stresses caused by crystals growth in the surface region can
potentially damage the binder structure.
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The destructive effects of this phenomenon and its
control methods are investigated extensively for Portland
cement [29–32]. However, there is little research on
efflorescence formation and control in alkali-activated and/
or geopolymer cements. For example, Najafi et al. [26]
tried to reduce efflorescence formation in alkali-activated
natural pozzolan by employing hydrothermal curing con-
ditions at different temperatures instead of normal curing in
humid conditions. They also investigated the potential of
some reactive additives like blast-furnace slag, metakaolin,
and high alumina cement (Secar 81) in controlling efflo-
rescence formation. According to their results, using
hydrothermal curing condition at temperatures higher than
65 °C and addition of high alumina cements can effectively
reduce efflorescence formation in alkali-activated natural
pozzolan. According to Škvara et al. [33, 34], exposing the
hardened alkali-activated fly ash paste specimens to high
temperatures (e.g. flame) considerably reduces the efflo-
rescence formation.
In this study, the impact of activator type on the efflo-
rescence formation severity and methods of efflorescence
reduction in alkali-activated phosphorus slag (PHS) cement
are investigated. Few research results published in recent
decades indicate that high quality cement can be produced
by activating PHS with suitable alkalis [35–37]. Phospho-
rus slag is a non-metallic slag and industrial by-product of
elemental phosphorus manufacturing industry. Approxi-
mately ten tons of slag per each ton of elemental phos-
phorus is produced by smelting a phosphate rock in an
electric-arc furnace during the production of yellow phos-
phorus [6, 35]. Therefore, production of relatively high
volumes of PHS is an environmental issue in countries of
high phosphorus production capacities like China (pro-
duced approximately 16 million tons of PHS in 2006) [38].
The current work is devoted to the impact of activator
type on the efflorescence formation severity in alkali-ac-
tivated PHS cement. The impact of pre-curing time in
humid environment before applying hydrothermal curing
condition on the effectiveness of efflorescence control has
been investigated. In addition, attempts were made to
control efflorescence formation by adding small amounts
of high alumina cements. The two techniques were then
compared with each other.
2 Experimental Procedure
2.1 Materials
Granulated PHS was purchased from Iranian acid phos-
phoric Company (southeast of Tehran). The results of its
chemical analysis based on ASTM C311 are reported in
Table 1. This PHS has very low Al2O3 content comparing
to the slags in other countries. Specific gravity of the slag
was measured according to the ASTM C118 and found
equal to 2.94 g/cm3. The basicity coefficient (Kb = (-
CaO ? MgO)/(SiO2 ? Al2O3)) and hydration modulus
((CaO ? MgO ? Al2O3)/SiO2) of this slag are 1.04 and
1.44, respectively. These show that the PHS is a neutral
slag exhibiting sound hydration property [39]. The slag was
ground in a laboratory ball mill (38 cm length and 11 cm
radius) to attain a Blaine fineness of 3000 ± 50 cm2/g.
Potassium hydroxide (84 % KOH, Merck), sodium
hydroxide (99 % NaOH, Merck) and liquid sodium silicate
(Na2SiO3: 8.50 % Na2O and 28.73 % SiO2, Merck) were
used as alkali-activators. High alumina cements (Secar 71
and Secar 80, Kerneos, France) were also used as additives
for efflorescence control. Table 2 represents the chemical
composition of high alumina cements.
2.2 Experimental Procedure
Alkali-activators were prepared by mixing adequate
amounts of potassium hydroxide, sodium hydroxide,
sodium silicate and/or their combinations in accordance
with compositions given in Table 3. The alkalinity and
silica modulus of the alkali-activators were adjusted at
different levels of 1, 3, 5 and 7 (wt% of the slag) and 0.5, 1
and 1.5, respectively. The silica modulus of sodium silicate
solution was adjusted by adding given amounts of NaOH or
KOH. The prepared activators with enough distilled water
were then added to PHS and mixed for 5 min to prepare

Table 1 Chemical composition

Oxide SiO2 Al2O3 Fe2O3 CaO MgO P2O5 K2O Na2O SO3 Cl LOI
of phosphorus slag
wt% 38.42 7.65 0.90 45.14 2.60 1.50 0.56 0.43 ND ND 1.87

Table 2 Chemical composition

Name Chemical Composition
of high alumina cements (wt%)
SiO2 Al2O3 Fe2O3 CaO MgO SO3 K2O Na2O

Secar 71 0.55 70.20 0.20 28.30 0.20 0.10 0.10 0.25

Secar 80 0.30 79.00 0.20 20.00 0.10 0.10 – 0.15

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Table 3 Chemical compositions of alkali-activators
Alkalinity Type of activator
1, 3, 5, 7 % NaOH
1, 3, 5, 7 % KOH
1, 3, 5, 7 % LSS ? NaOH
Ms = 0.5, 1, 1.5
1, 3, 5, 7 % LSS ? KOH
Ms = 0.5, 1, 1.5
cement pastes. For each mixture, the amount of distilled
water was determined for a w/c ratio providing a fixed flow
of 175 ± 5 mm in diameter in 25 drops of the flow table,
according to ASTM C230 [40] standard. The mixes were
then molded in 29292 cm3 cubic molds and kept in 95 %
relative humidity environment for 24 h at room tempera-
ture. After that, the specimens were removed from the
molds and held at the desired curing conditions until the
testing time.
Two different curing conditions of classical and
hydrothermal were considered for the current study, (1)
classical curing conditions: including curing in 95 % rel-
ative humidity at 25 °C for 28 days and (2) hydrothermal
curing conditions: including a pre-curing stage in classical
curing conditions and then a 7-h hydrothermal curing
regime at 85 °C.
A uniaxial digital hydraulic press apparatus (SCL; STD
30) with ±1 % accuracy was used for compressive strength
tests. For each measurement, three specimens were used
and the average of the three test results was reported. The
standard deviation of the compressive strength varied from
0.2 to 3 %. The cement mixes exhibiting compressive
strengths higher than 60 MPa after 28 days of classical
curing were then compared for efflorescence formation
qualitatively. For this reason, from each mix a 28-day cured
specimen was immersed in 40 mL of distilled water in a
small container and kept at laboratory environmental con-
ditions for complete evaporation of water. The specimens
were then compared visually for their efflorescence for-
mation severity. Mixes showing relatively high severity of
efflorescence formation were excluded from the rest of the
work. In the next step, the cement mixes were compared for
efflorescence formation quantitatively. For such a compar-
ison, from each mix 1.0 ± 0.0001 g of 28-day cured
cement paste was finely ground and added to 30 mL of
distilled water. After 24 h, the water was filtered and
evaporated inside an oven at 90 °C for 24 h. The leached
salts were then weighted and recorded as a quantitative
criterion for efflorescence formation.
Attempts were made to control the efflorescence for-
mation phenomenon by applying hydrothermal curing
427
Raw materials Alkali activator
Mixing and molding
Classical curing (curing at more than 95% relative humidity at
25 °C) for 28 days
Selection of cement mixes exhibiting 28-day compressive strengths
higher than 60 MPa
Qualitative efflorescence formation test
Selection of cement mixes with low to
moderate efflorescence formation visually
Quantitative efflorescence formation test
Selection of cement mixes of relatively lower
efflorescence (lower than 5 g salt/100 g hardened
paste)
Efflorescence reduction by applying
hydrothermal curing conditions or using high
alumina cements as additives
Fig. 1 Experiment procedure
conditions after a pre-curing stage and using small amounts
of high alumina cements as additives to mixtures.
Application of hydrothermal curing conditions was
previously reported as a relatively effective technique for
controlling efflorescence formation [26]. Current work,
however, focuses on the impact of pre-curing stage on the
effectiveness of the technique. For this reason, different
pre-curing times of 1, 3, and 7 days were considered before
the application of hydrothermal curing. The effectiveness
of high alumina cements additives for efflorescence for-
mation control was compared to the application of
hydrothermal curing. Secar 71 and 80 were added to the
mixtures at three different levels of 3, 5 and 7 wt% (by
weight of slag). These three addition levels were selected
because of, first, the high alumina cement is expensive; and
therefore relatively higher addition levels are not reason-
able and cost-effective. Second, small amounts of high
alumina cement were added just to increase the cross-
linking between the hydrated products to control the
severity of the efflorescence formation. Figure 1 represents
the simplified block diagram of the experimental procedure
applied.
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Hardened pastes of cement mixes exhibiting optimum
properties were then characterized by Fourier transform
infrared spectroscopy (FTIR; Nicolet 740), X-ray diffrac-
tometry (XRD; Philips Expert System, Cu Ka9-radiation
and Ni-filter), and scanning electron microscopy (SEM;
CamScan MV 2300, EDS; Oxford 7538) analyzes.
3 Results and Discussion
3.1 Effect of Activator Type and Dosage
on Efflorescence Formation
Results of both qualitative and quantitative efflorescence
formation tests are reported in Table 4. In qualitative test,
cement mixes were classified into four groups of very high,
high, medium, and low efflorescence forming based only
on visual observations. These four groups of mixes are
represented by letters of A, B, C and D, respectively.
Figure 2 shows typical examples of these four groups.
Based on the data reported in Table 4, all mixes acti-
vated with NaOH solution exhibit more or less
efflorescence formation. As seen, the tendency for efflo-
rescence formation increases with increasing the alkalinity
content of the mixes. Visual observations, however, show
that mixes activated with KOH solution do not exhibit any
tendency for efflorescence formation.
This can be attributed to the reactivity of potassium
compared to that of sodium. The atomic radius of potas-
sium is greater than that of sodium. In potassium, the
outermost electron is more easily lost than it is in sodium.
Thus, potassium can form K? more readily than sodium
can form Na?. Mixes activated with KOH solution,
therefore, contain significantly lower contents of un-re-
acted or free alkali than those activated with NaOH solu-
tion. On the other hand, compared to sodium carbonate,
potassium carbonate exhibits a relatively lower tendency
toward hydration and crystallization. This means that
mixes containing potassium show a visually lower ten-
dency for efflorescence formation [33, 34].
Another interesting point is that use of sodium silicate in
combination with NaOH and KOH increases the tendency
for efflorescence formation. Most of the mixes activated
with combinations of sodium silicate and NaOH show a

Table 4 Effect of alkalinity and silica modulus on tendency for efflorescence formation
Mix no. Type of activator Ms Alkalinity (%) Efflorescence severitya Compressive strength (MPa) Efflorescence (g/per 1 g)

1 NaOH – 3 C 80 0.0409
2 NaOH – 5 B 88 0.0490
3 NaOH – 7 A 81 –
4 KOH – 3 D 77 0.0502
5 KOH – 5 D 82 0.0508
6 KOH – 7 D 99 0.0512
7 LSS ? NaOH 0.5 3 A 68 –
8 LSS ? NaOH 0.5 5 A 93 –
9 LSS ? NaOH 0.5 7 B 66 0.0583
10 LSS ? NaOH 1 3 C 68 0.0420
11 LSS ? NaOH 1 5 A 108 –
12 LSS ? NaOH 1 7 A 85 –
13 LSS ? NaOH 1.5 3 A 81 –
14 LSS ? NaOH 1.5 5 A 105 –
15 LSS ? NaOH 1.5 7 A 97 –
17 LSS ? KOH 0.5 3 C 63 0.0442
18 LSS ? KOH 0.5 5 C 81 0.0553
19 LSS ? KOH 0.5 7 C 102 0.0482
20 LSS ? KOH 1 3 B 98 0.0598
21 LSS ? KOH 1 5 C 112 0.0498
22 LSS ? KOH 1 7 B 121 0.0612
23 LSS ? KOH 1.5 3 C 87 0.0400
24 LSS ? KOH 1.5 5 A 113 –
25 LSS ? KOH 1.5 7 A 120 –
a
A, very high efflorescence; B, high efflorescence; C, Medium efflorescence; D, low efflorescence

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Fig. 2 28-day cured paste specimens of different cement mixes
exhibiting very high, high, medium, and low tendencies for efflores-
cence formation from left to right: a sodium silicate ? NaOH with
very high tendency for efflorescence formation and are
classified in group A. Also efflorescence class of mixes
activated with combinations of sodium silicate and KOH
moved to an upper level. This phenomenon can be attrib-
uted to the type of sodium and potassium bond in hydration
product(s). According to literature, sodium and potassium
participate as Na(H2 O)þ þ
n and K(H2 O)n (n: 2–8) instead of
? ?
Na and K to balance the negative charge on the 6-valent
aluminum. These bonds are weaker than those with Na? or
K? and they can easily be broken in the humid environ-
ment providing a higher tendency for efflorescence for-
mation [33, 34, 41].
Bonk et al. [42] used Na-NMR analysis to examine the
formed bonds in blast-furnace slag activated with pure
NaOH and its combination with sodium silicate. They
observed that Na-NMR peaks appear at different positions
of -0.9 and -2.5 ppm in the spectra, respectively. Based
on the Lee and Stebbins study [43], difference between
-0.9 and -2.5 ppm can be attributed to the number of
water molecules count in the aluminosilicate matrix
showing that the n value of Na(H2 O)þ þ
n and K(H2 O)n in
cement mixes activated with pure NaOH is lower than
those activated with sodium silicate or its combination with
NaOH. This results in higher strength of these bonds in the
formed matrix and, therefore, lowers the tendency of the
alkalis for migration to the surface and efflorescence for-
mation [33].
In addition, due to the interaction of Na? and K? ions
with SiO2 of sodium silicate, some Na? and K? ions in the
mixture are remained un-reacted with SiO2. These un-re-
acted ions with their high solubility in water also result in a
higher tendency for efflorescence formation. Consequently,
the mixes activated with pure NaOH show lower tendency
for efflorescence formation than those activated with the
combinations of sodium silicate with NaOH.
In general, there are two alkali sources for efflorescence
formation: un-reacted or free alkalis remained in the matrix
after alkali-activation and hydrated alkali ions weakly bond
429
Ms = 1.5 and 7 % alkalinity, b NaOH with 5 % alkalinity, c NaOH
with 3 % alkalinity, d KOH with 5 % alkalinity
to 4- or 6-valent aluminum for charge balancing of the
matrix. It has been shown that charge balancing alkalis can
be simply replaced by hydronium ions (H?) and move to
the surface especially if they are exposed to an acid med-
ium [44, 45]. However, it is obvious that free alkalis are
more easily accessible to efflorescence formation than
bond alkalis.
There are evidences in the literature showing that alkali-
activated and/or geopolymer cements suffer from efflo-
rescence formation not only at early ages, but also at late
ages over long periods of time [34, 46, 47]. These obser-
vations may help in dividing the efflorescence formation
phenomenon in alkali-activated and/or geopolymer
cements into two primary and secondary types as in Port-
land cements. The primary efflorescence formation is
mainly due to the migration of free alkalis and is expected
to appear at early ages, whereas the secondary efflores-
cence formation is more due to the migration of hydrated
bond alkalis exchanged with hydronium ions and is
expected to appear slowly over longer time periods. In this
case, one may conclude that this study is mainly focused on
the control of primary efflorescence formation.
3.2 Effect of Curing Conditions on Efflorescence
Formation
Three different pre-curing times of 1, 3 and 7 days were
considered before applying hydrothermal curing condi-
tions. All the specimens pre-cured for 1 day cracked
severely after hydrothermal curing. Figure 3 shows some
typical cracked specimens.
This cracking phenomenon can be attributed to the
matrix instability and variations in the amount of hydration
products where their reaction activation energies are sup-
plied in the hydrothermal curing conditions. This non-
uniformity in distribution of hydration products results in
non-uniform shrinkage in the matrix due to different
shrinkage behaviors of un-reacted slag and reactions’
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430
Fig. 3 Cracking in typical specimens cured hydrothermally after
1 day pre-curing in humid environment
products. By employing (Si and Al) NMR analyzes, Bonk
et al. [42] showed that the paste specimens of blast-furnace
slag activated with pure NaOH and its combination with
sodium silicate contain significant amounts of un-reacted
slag and alkaline material and a small amounts of formed
polymers (mainly of Q2 type of CSH structure) after just
1 day of curing in humid environment. They also showed
that after 3 days of curing in humid environment cement
mixes contained significant amounts of hydration products
mainly of types Q1 of CSH and Q2 (Al). Specimens cured
for 7 days at the same conditions developed stable matrixes
containing Q1 and Q2 of CSH and Q2 (Al).
Figure 4 represents the FTIR spectra of PHS and the
mix activated with sodium silicate and KOH with Ms = 1
and 5 % alkalinity after 1, 3, and 7 days of curing in humid
environment and also after 7 days of pre-curing followed
by hydrothermal curing.
The broad peak appeared at 1000 cm-1 for slag is due to
all the Q structures of SiO2 [48, 49]. As the pre-curing time
in humid environment increases from 1 to 7 days, the peak
becomes sharper and shifts to lower wave number of
994 cm-1. This observation can be attributed to the
increase in the polymer phase contents, e.g. the C–S–H
phase, of the cement matrix and decrease in the amount of
slag remained un-reacted in the matrix [50]. As seen in
Fig. 4, the mentioned peak for the 1-day cured paste
appeared at 998 cm-1 is very similar to that of slag indi-
cating the presence of lot of un-reacted slag particles and
alkaline materials in the cement matrix. 1 day curing in
humid environment, therefore, does not result in the
development of a stable matrix for hydrothermal curing.
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Int J Civ Eng (2016) 14:425–438
When under hydrothermal conditions activation energy is
supplied to such instable cement matrixes, which are not
enough hardened the non-uniform progress of hydration
reactions results in a non-uniformity distribution of
hydration products. Disintegrating stresses can, therefore,
develop inside the matrix due to differences in shrinkage
behaviors of un-reacted slag and reactions’ products.
In some cases, when alkali-activated slag pastes are
cured hydrothermally different types of zeolites, such as
xonotlite, tobermorite and sodium-zeolite NAS2H3 were
observed in hydration products [6, 19, 51, 52]. As a result,
the amorphous polymer phases of the cement matrix which
act as binder are decreased and this may also result in the
possibility of crack formation. In addition, as applying the
hydrothermal curing conditions the volume of the free
water present in the specimen’s pores increases resulting in
internal stresses inside the cement matrix, which is not
enough hardened.
The effects of hydrothermal curing after 3 days of pre-
curing in humid environment on efflorescence formation
and compressive strength development are shown in
Table 5. As seen, efflorescence formation is reduced in all
cement mixes. The highest reduction in efflorescence for-
mation is observed for mix 21. Compared to 28-day clas-
sical curing in humid environment, compressive strength is
also reduced for all cement mixes except for the two mixes
19 and 21. The decrease in compressive strength can again
be attributed to the matrix instability after just 3 days of
pre-curing that leads to non-uniformity in the distribution
of hydration products as discussed for the case of
hydrothermal curing without any pre-curing.
As seen in Fig. 4, the broad FTIR peak attributed to the
polymer phase and un-reacted slag contents of the material
appeared at the wavenumber of 998 cm-1 after 3 days of
curing in humid environment. This peak is very similar to
the corresponding broad peak observed at the wavenumber
of 1000 cm-1 for slag. This means that a 3-day curing time
in humid environment is not enough for the progress of
hydration reactions and formation of a stable matrix.
Application of hydrothermal curing conditions after just
3 days of pre-curing in humid environment, therefore,
lowers the compressive strength of almost all cement
mixes. The only mixes showing increased compressive
strength are mixes 19 and 21, which are among formula-
tions having activators of relatively higher reactivity, i.e.
activators of higher alkalinity of the type potassium.
Table 6 represents the effects of hydrothermal curing
after 7 days of pre-curing in humid environment on efflo-
rescence formation and compressive strength development.
As seen, all the tested cement mixes show reduced efflo-
rescence and increased compressive strength. Efflorescence
formation shows a reduction between 25 to almost 50 % by
weight that is 1.5–2 times higher than values measured for
Int J Civ Eng (2016) 14:425–438 431

Fig. 4 FTIR spectra of

phosphorus slag (Slag) and
cement mix activated sodium Slag
silicate and KOH with Ms = 1
and 5 % alkalinity after 1 (1-D),
3 (3-D), and 7 (7-D) days of 1-D
curing in humid environment 1000
and also after 7 days of pre-

Transmission (%)
curing followed by
hydrothermal curing (Hyd.) 3-D
998

994 7-D

Hyd.
994

970

0 500 1000 1500 2000 2500 3000 3500 4000 4500 5000
Wavenumber (cm-1)

Table 5 Effects of hydrothermal curing after 3-day pre-curing on the efflorescence formation and compressive strength development
Mix no. Efflorescence amount (g salt Efflorescence Compressive Change in compressive
per 100 g hardened paste) reduction (%) strength (MPa) strength (%)

1 2.99 26.89 72.50 -9.38

2 3.84 21.63 77.50 -11.93
10 3.70 11.90 66.50 -2.21
17 3.38 23.53 60.00 -4.76
19 3.91 18.88 112.50 10.29
21 3.41 31.53 132.50 18.30
23 3.12 22.00 70.00 -19.54

Table 6 Effects of hydrothermal curing after 7-day pre-curing on the efflorescence formation and compressive strength development
Mix no. Efflorescence amount Efflorescence Compressive Change in compressive
(g salt per 100 g hardened paste) reduction (%) strength (MPa) strength (%)

1 2.11 48.41 95.5 ?19.38

2 3.08 37.14 113 ?28.41
10 3.12 25.71 110.5 ?62.50
17 2.60 41.18 79.5 ?26.19
19 3.14 34.85 135 ?32.35
21 2.73 45.18 136 ?21.43
23 2.33 41.75 105.5 ?21.26

3 days curing. Compressive strength also shows an
increase in the range of about 20–60 % compared to cor-
responding values measured after classical curing, i.e.
28 days in humid environment. Mixes 19 and 21 show the
highest compressive strengths, i.e. 135 and 137 MPa,
respectively. These improvements in both efflorescence
formation and compressive strength confirm the effective-
ness of hydrothermal curing after 7 days of pre-curing.
Figure 4 also shows that the FTIR peak attributed to the
polymer phase and un-reacted slag contents of the material

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became sharper and appeared at the wave number of
994 cm-1 after 7 days of curing in humid environment.
This peak is very similar to the corresponding peak
observed for the cement mix cured hydrothermally after
7 days of pre-curing. As previously confirmed by Bonk
et al. paste specimens of alkali-activated blast furnace slag
cured for 7 days in humid environment developed
stable matrixes containing significant amounts of different
polymeric hydration products [42].
These observations show that application of hydrother-
mal curing conditions can significantly improve both
efflorescence formation tendency and compressive strength
development of alkali-activated PHS if an optimum pre-
curing stage is considered. In this case, the activation
energy supplied to the stable cement matrix results in both
faster hydration reactions and higher extents of hydration
reactions progress [6, 7, 9]. Faster hydration reactions are
responsible for attainment of higher final compressive
strengths over a comparatively shorter time period of cur-
ing and higher degrees of hydration reactions progress are
responsible for the involvement of more slag and alkali in
hydration reactions, which in turn reduces the tendency for
efflorescence formation.
3.3 Effect of High Alumina Cement Additives
on the Efflorescence Formation
Figures 5 and 6 represent the amount of efflorescence
reduction and change in compressive strength of the
cement mixes incorporating high alumina cements of Secar
71 and Secar 80 at addition levels of 3, 5 and 7 % by
weight of PHS. As seen, in all mixes incorporation of
alumina cements reduces the amount of efflorescence. The
Fig. 5 Effect of high alumina
cement additives on the
efflorescence reduction; Secar
Efflorescence reduction (%)
71 (S 71) and Secar 80 (S 80)
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Int J Civ Eng (2016) 14:425–438
higher the addition level, the lower is the amount of
efflorescence. Changes in compressive strength also rep-
resent a similar trend in all mixes except for the mixes No.
1 and 2 showing about 10 and 14 % lower compressive
strengths at addition level of 3 %, respectively.
Improvements in both efflorescence formation and
compressive strength in all mixes, except mixes 1 and 2,
are attributed to the highly reactive alumina in the form of
calcium aluminate (CaAl2O4) incorporated into the cement
mixes. Increasing the amount of reactive alumina in the
reacting mixes results in more cross-linking (Si–O–Al) in
the molecular structure of the hydration products [26].
Extension of the 3-dimensional molecular structure and
production of more polymeric hydration products improves
the mechanical properties of the cement and also leads to
the participation of more alkalis for the charge-balancing
role, hence lowering the amount of un-reacted alkalis and
reducing the tendency of the cement for primary efflores-
cence formation.
The reductions in compressive strength of mixes 1 and 2
can be attributed to their odd activators comprising of only
sodium hydroxide. The absence of sodium silicate in these
two mixes significantly lowers the amount of reactive sil-
ica. In this case, part of added sodium hydroxide reacts
with calcium aluminate phases present in alumina cements
resulting in the formation of aluminum hydroxide and
calcium carbonate [53]:
yields
CA + NaOH ! AH3 þ CaCO3
This undesired reaction that is known as alkaline
hydrolysis consumes part of sodium hydroxide and lowers
the compressive strength of mixes 1 and 2 compared to the
corresponding control mixes cured in humid condition for
50
40
30
20
10
0
3% (S 71) 5% (S 71) 7% (S 71) 3% (S 80) 5% (S 80) 7% (S 80)
Weight percentage of admixture (additive name)
No. 1 No. 2 No 10 No. 17 No .19 No. 21 No. 23
Int J Civ Eng (2016) 14:425–438
Fig. 6 Effect of high alumina
cement additives on
Change in compressive strength (%)
compressive strength; Secar 71
(S 71) and Secar 80 (S 80)
28 days. In addition, Secar 71 is richer than Secar 80 in
calcium aluminate phases [54] and this is probably the
reason for the higher reductions in compressive strength
with Secar 71 than with Secar 80. Increasing the addition
level in these two mixes, however, increases the com-
pressive strength as observed in all the other mixes. This is
simply due to the increases in the contents of CA and CA2
phases in the mixes. At increased addition levels, a higher
proportion of these reactive phases can take part in the
hydration reactions and produce more cross-linked
molecular structures of improved compressive strength.
The efflorescence reduction in these two mixes is due to the
effective consumption of sodium oxide in both alkaline
hydrolysis reaction of calcium aluminates and charge bal-
ancing of the tetrahedral aluminum.
A comparison between the two alumina cements clearly
shows that Secar 80 is more effective than Secar 71 in both
reducing the efflorescence formation and increasing the
compressive strength. This is due to the higher reactive
alumina content of Secar 80 that is responsible for more
cross-linking (Si–O–Al) in the molecular structure of the
hydration products [26].
As observed, both techniques of using high alumina
cement additives and application of hydrothermal curing
are effective in reducing the tendency for efflorescence
formation and increasing the compressive strength of
alkali-activated PHS cement. Comparison of the maximum
and the average values of improvements achieved, how-
ever, reveals the fact that hydrothermal curing technique is
more effective than the technique of adding high alumina
cements. For the technique of high alumina cement addi-
tion, the maximum improvements in both efflorescence
reduction and compressive strength increase were achieved
by adding 7 % of Secar 80. In this case, the maximum and
433
60
50
40
30
20
10
-10
-20
3% (S 71) 5% (S 71) 7% (S 71) 3% (S 80) 5% (S 80) 7% (S 80)
Weight percentage of admixture (additive name)
No. 1 No. 2 No 10 No. 17 No .19 No. 21 No. 23
the average values for efflorescence reduction are 44.00
and 31.53 % and for compressive strength increase are
51.19 and 23.48 %, respectively. Application of
hydrothermal curing condition after 7 days of pre-curing
resulted in higher improvement values. For this technique,
the achieved maximum and average values for efflores-
cence reduction are 48.41 and 39.17 %, and for compres-
sive strength increase are 62.50 and 31.17 %, respectively.
3.4 Complementary Tests
The cement mix 21 showing the greatest improvement in
both efflorescence and compressive strength was selected
for some complementary studies by XRD, FTIR and SEM
analyzes. Figure 7 represents the X-ray diffraction patterns
of PHS (a) and cement mix 21 cured under; classical humid
conditions for 28 days (b), hydrothermal conditions with
7 days pre-curing in humid conditions (c) and the same
mix improved with incorporating Secar 80 at 7 wt%
addition level and then cured in humid conditions for
28 days (d). The absence of any diffraction peak in the
patterns of the cement mixes and the increased background
at the 2h of 30° that is due to an overall scattered
diffraction confirm that all the studied samples are mainly
amorphous in character [55]. There are only few small
diffraction peaks in the PHS, which are due to the presence
of small amounts of periclase phase. As seen, the small
amount of periclase that was originally present in the slag
was greatly reduced or disappeared in the cement mixes.
This is due to its tendency for hydration that results in the
formation of amorphous magnesium hydroxide. Under
classical curing conditions, this hydration usually happens
over a time period of several weeks, but under hydrother-
mal curing condition it happens quickly [56].
123
434
Fig. 7 X-ray diffraction
patterns of phosphorus slag
(a) and cement mix 21 cured
under; classical humid
conditions for 28 days (b),
hydrothermal curing conditions
after 7 days of pre-curing in
humid conditions (c) and the
same mix improved with
incorporating Secar 80 at 7 wt%
addition level and then cured in
humid conditions for 28 days
(d)
Many researchers reported that the main phase produced
in the alkali-activation of slag is C–S–H [6, 57, 58].
However, due to its amorphous to very low crystallinity
character, it is usually impossible to recognize its presence
using the technique of XRD [6] and suitable analytical
techniques such as FTIR spectroscopy must be used.
FTIR spectra of PHS (a) and cement mix 21 cured
under; classical humid conditions for 28 days (b),
hydrothermal conditions with 7 days pre-curing in humid
conditions (c) and the same mix improved with incorpo-
rating Secar 80 at 7 wt% addition level and then cured in
humid conditions for 28 days (d) are shown in Fig. 8. The
main peaks appeared in the spectra and their sources are
also given in Table 7.
As seen in the spectra of the cement mixes, the bands
appearing at the wavenumbers in the range 470–440 cm-1,
which are due to the bending vibration of Si–O–Al bonds
[52, 59], are sharper and more intensified compared to the
corresponding band in the spectrum of PHS. This indicates
the formation of more Si–O–Al bonds in the cement mixes
compared to slag. These additional Si–O–Al bonds formed
in the cement mixes in the course of alkali-activation
reactions are those of geopolymeric character participating
in the binding properties of the cement mixes. However, it
must be noted that geopolymeric Si–O–Al bonds are not
the main cause of binding properties in alkali-activated slag
cements. As mentioned before, the main phase imparting
cementing properties to alkali-activated slag cement is C–
S–H [6, 57, 58].
The peaks appeared at around 1000 cm-1 in the spec-
trum of slag are due to the vibrations of Si–O bond in its
123
Int J Civ Eng (2016) 14:425–438
4-sided structure, i.e. silica tetrahedral. These peaks in the
spectra of cement mixes shifted to lower wavenumbers in
the range 968–972 cm-1 and became sharper and stronger
indicating that alkali-activation reactions resulted in the
polymerization and formation of amorphous C–S–H (SiQ2)
or C–A–S–H [48–50].
There are some peaks at wave numbers of 3450–3475
and *1650 cm-1 in the spectra of the cement mixes.
These peaks are due to the stretching vibration of OH
groups found in water molecules or in Na(H2 O)þ n [61].
The peaks at approximately 1480 cm-1 in the FTIR
spectra of the cement mixes are caused by the non-sym-
metrical stretching of C–O bonds in CO32-. Appearance of
these peaks is an indication of absorption of atmospheric
carbon dioxide and carbonation of un-reacted alkalis in the
cement mixes [60].
Figure 9 represents the SEM images prepared from
hardened pastes of cement mix 21 cured under classical
humid conditions for 28 days (a), the same mix improved
with incorporating Secar 80 at 7 wt% addition level and
then cured in humid conditions for 28 days (b), and the
same mix cured under hydrothermal curing conditions after
7 days of pre-curing in humid conditions (c). As seen, SEM
analysis also confirms the fact that alkali-activation reac-
tions result in the formation of a uniform glassy matrix.
Un-reacted slag particles (shown by arrows) embedded in
the matrix can also be seen. Comparative observations,
however, revealed a more uniform microstructure with
lower content of un-reacted slag particles for the cement
paste cured hydrothermally (c) compared to the other
cement pastes (a, b). This observation supports the highest
Int J Civ Eng (2016) 14:425–438 435

Fig. 8 FTIR spectra of

phosphorus slag (a) and cement
mix 21 cured under; classical (a)
1649
humid conditions for 28 days 1485
1421
(b), hydrothermal curing
507
conditions after 7 days of pre-
1000
curing in humid conditions 1481 (b)
(c) and the same mix improved 1645

Transmission (%)
with incorporating Secar 80 at
7 wt% addition level and then
459 3450
cured in humid conditions for
968 (c)
28 days (d)
1483 1654

455
3475
970 (d)
1483 1654

455
3475
972

0 500 1000 1500 2000 2500 3000 3500 4000 4500 5000
Wavenumber (cm-1)

Table 7 Major FTIR peaks of phosphorus slag of phosphorus slag in humid conditions (c) and the same mix improved with incorpo-
(a) and cement mix 21 cured under; classical humid conditions for rating Secar 80 at 7 wt% addition level and then cured in humid
28 days (b), hydrothermal curing conditions after 7 days of pre-curing conditions for 28 days (d)
Mixes Origin Reference
(a) (b) (c) (d)

Wavenumber (cm-1) 507 455 455 459 Si–O–Al bending [52, 59]
1000 970 972 968 Bonds in C–S–H [48, 49]
1421 - 1485 1421 - 1483 1430 - 1483 1429 - 1481 C–O bond in CO32- [60]
1649 1654 1654 1645 O–H bond [61]
– 3475 3475 3450 O–H bond [61]

compressive strength (137 MPa) achieved by the same
cement mix and the superior effectiveness of hydrothermal
curing technique in improving the mechanical properties of
alkali-activated PHS compared to the technique of incor-
porating small amount of high alumina cements.
4 Conclusions
Experimental results based on both qualitative and quan-
titative measurements of efflorescence confirm that the
severity of efflorescence formation in alkali-activated PHS
is dependent upon the type and dosage of the used acti-
vator. Visual observations showed that mixes activated
with KOH solution do not exhibit any tendency for efflo-
rescence formation, while those activated with NaOH
solution exhibit more or less efflorescence formation. Also,
the use of sodium silicate in combination with NaOH and
KOH increases the tendency for efflorescence formation. In
addition, the tendency for efflorescence formation increa-
ses with increasing the alkalinity content of the mixes.
Based on the experimental results, the two techniques of
using high alumina cements as additives and application of
hydrothermal curing are both effective in reducing the
tendency of alkali-activated PHS cement for efflorescence
formation and also increasing its compressive strength.
Hydrothermal curing technique, however, could be more
effective than using additives of high alumina cements if an
optimum pre-curing stage in humid environment is con-
sidered. Without an optimum pre-curing, the non-unifor-
mity in distribution of hydration products and the resulting
non-uniform shrinkage in the matrix due to different
shrinkage behaviors of un-reacted slag and reaction prod-
ucts result in disintegrating internal stresses. For the stud-
ied PHS, a 3-day pre-curing in humid environment is not
enough and the paste specimens show severe cracking.

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436 Int J Civ Eng (2016) 14:425–438

Fig. 9 SEM images of

hardened pastes of cement mix
21 cured under classical humid
conditions for 28 days (a), the
same mix improved with
incorporating Secar 80 at 7 wt%
addition level and then cured in
humid conditions for 28 days
(b), and the same mix cured
under hydrothermal curing
conditions after 7 days of pre-
curing in humid conditions (c)

With a 7-day pre-curing, however, reductions up to 50 %
in efflorescence formation and increases up to 60 % in
compressive strength were observed.
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