Journal of Cleaner Production 147 (2017) 330e339

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Journal of Cleaner Production

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

Alkali activated slag foams: The effect of the alkali reaction on foam
characteristics
Ailar Hajimohammadi a, *, Tuan Ngo a, Priyan Mendis a, Alireza Kashani a,
Jannie S.J. van Deventer b, c
a
Department of Infrastructure Engineering, University of Melbourne, Victoria 3010, Australia
b
Department of Chemical and Biomolecular Engineering, University of Melbourne, Victoria 3010, Australia
c
Zeobond Pty Ltd, P.O. Box 23450, Docklands, Victoria 8012, Australia

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

Article history: The effect of the alkali activation reaction on the characteristics of slag-based foams made by the me-
Received 27 September 2016 chanical foaming technique is investigated. The mechanical foaming method is selected in order to
Received in revised form control the density and quantity of the pre-made foam and minimise the impact of alkali reaction on the
16 January 2017
amount of initial foaming. Despite the similarity of the pre-made foams mixed with the altered binder
Accepted 24 January 2017
Available online 26 January 2017
formulae, a change in the alkali reaction is shown to affect the pore size distribution, pore homogeneity,
density and properties of the inorganic foams. The water content of the binders is shown to be the key
factor affecting the bubble breakage and foam sorting during the mechanical mixing stage. Later in the
Keywords:
Low-CO2
reaction, the reaction rate of the binders and the size of the gel particulates govern the pore size dis-
Slag foam tribution and directional homogeneity of pore distribution within the matrix. Also, the reaction rate and
Thermal conductivity the size of the gel particulates regulate the final density of the inorganic foams. The thermal conductivity
Porosity is higher in the samples with higher density, but it is largely affected by the directional homogeneity of
Strength pore distribution. Apart from the strength of binding matrix and size distribution of pores, the directional
homogeneity of porosity is shown to be the vital factor for high strength development.
© 2017 Elsevier Ltd. All rights reserved.

1. Introduction
Foam concrete is a lightweight construction material which has
air voids entrapped in its cementitious matrix. Lightweight con-
crete brings some advantages to the construction industry such as
improving the insulating properties, acoustic insulation and
improving housing affordability (Ramamurthy et al., 2009; Zhang
et al., 2015). Geopolymer and alkali-activated binders have also
been used to make foam concretes with the aim of producing more
environmentally friendly construction materials compared to the
Portland cement-based cellular concretes (Hlava
cek et al., 2015;
Zhang et al., 2014). Foam concretes have been widely used for
various non-structural construction applications such as precast or
cast-in-situ wall elements, insulation screeds, facades, slabs, or as a
core of lightweight sandwich panels that are becoming increasingly
popular in construction.
There are two methods usually used for introducing voids into
* Corresponding author.
E-mail address: ailar.hm@unimelb.edu.au (A. Hajimohammadi).
the concrete matrix: (1) the mechanical foaming method in which
the concrete paste is physically mixed with a pre-made foam
(Lassinantti Gualtieri et al., 2015; Strozi Cilla et al., 2014), and (2)
the chemical foaming technique where a gas generated by a
chemical reaction is trapped in the concrete during the setting and
hardening stages of the matrix (Abdollahnejad et al., 2015; Ducman
and Korat, 2016; Masi et al., 2014). Alkali-activated slag has been
successfully used to make foam concretes (Esmaily and Nuranian,
2012; Yang et al., 2014), and life cycle assessment studies show
the reduction in environmental impact by using slag-based foam
concrete compared to Portland cement foam concrete (Yang et al.,
2014).
The majority of the research on alkali-activated foam concretes
is focused on the application of various foaming agents and
different preparation procedures in order to improve the properties
of foam concretes (Henon et al., 2012; Lassinantti Gualtieri et al.,
2016). Not much research has been conducted to explain the
impact of the reaction mechanism on foam characteristics, and the
manipulation of binder formulation for controlling the character-
istics of inorganic foams has not been investigated so far. The

http://dx.doi.org/10.1016/j.jclepro.2017.01.134
0959-6526/© 2017 Elsevier Ltd. All rights reserved.
 A. Hajimohammadi et al. / Journal of Cleaner Production 147 (2017) 330e339
common practice for controlling the characteristics of inorganic
foams made with the mechanical foaming technique is by adjusting
the density and quantity of pre-made foams, or by controlling the
mixing procedure of foams with the binders pastes (Lassinantti
Gualtieri et al., 2015; Strozi Cilla et al., 2014; Zhang et al., 2015). It
is logical that even with careful controlling of the quality and
quantity of the pre-made foam, the resulting inorganic foams will
have different characteristics if the binders undergo different re-
action paths. The objective of this study is to compare three
different one-part mix alkali-activated slag foams and correlate the
kinetics of their alkali reaction with the characteristics of the final
inorganic foams.
2. Literature review
Alkali-activated binders are clinker-free construction materials
which are usually produced by the activation of pozzolanic mate-
rials such as slag, metakaolin and fly ash with alkali-rich activators
such as sodium hydroxide and sodium silicate (Davidovits, 1994;
Palomo et al., 1999; Perna
and Hanzlí cek, 2016). Alkali-activated
concretes have many advantages over conventional concretes,
and these advantages have made alkali activation a very interesting
topic for scientific and commercial studies (Abdalqader et al., 2016;
Mithun and Narasimhan, 2016).
The production process of alkali-activated concrete usually
consumes much less energy and releases lower amounts of carbon
dioxide to the atmosphere. Also, alkali-activated concretes have the
potential to gain high mechanical strength in the early ages of their
curing along with high resistance to fire and aggressive chemicals
(Abdalqader et al., 2016; Abdollahnejad et al., 2015; Yang et al.,
2013). It should be mentioned that there are also some issues
with alkali activated concretes that need to be investigated further,
i.e., the high cost of alkali activators, low resistance to carbonation,
and being prone to the formation of efflorescence (Pacheco-Torgal
et al., 2012).
One-part (just add water) geopolymer mixtures are a new class
of cementitious materials which are developed to increase the
commercial viability of geopolymers. In traditional (two-part)
geopolymer binders, alkali-activating solutions are mixed with
solid source materials to make binders. However, alkali solutions
are corrosive, viscose and they are not user-friendly for bulk pro-
duction. One-part geopolymer mixes are designed as a solid
mixture that can be activated by just adding water (similar to
cement).
Different methods have been used for making one-part mix
geopolymers. The usual methods include blending aluminosilicate
precursors with solid activators (Abdollahnejad et al., 2014;
Hajimohammadi and van Deventer, 2016a, b; Nematollahi et al.,
2015), using source materials that precontain high amount of al-
kalis (Ke et al., 2015; Ye et al., 2016), or thermally activating source
materials together with alkaline materials (Feng et al., 2012; Peng
et al., 2014).
In this paper, alkali-activated slag is used as a cementitious
binder to make one-part mix lightweight inorganic foams. A me-
chanical foaming method is used to minimise the effect of alkali
reaction on the quantity of initial foaming. Three different formu-
lations that represent different reaction kinetics are selected to
study the effect of mix design on the characteristics of the foams.
Pre-made foam with the same density and quantity is added to all
three formulations, and the final foam characteristics (which are
directly related to the alkali reaction) are investigated.
3. Materials and methods
The GBFS with the average particle size of 16 mm is obtained
331
Table 1
Oxide composition of GBFS as determined by XRF.a.
SiO2 TiO2 Al2O3 Fe2O3 MnO MgO CaO K2O P2O5 SO3 LOI
31.00 0.49 13.96 0.32 0.33 6.33 40.92 0.31 0.01 2.17 2.11
a
Mass %. LOI: loss on ignition at 1000  C.
from Independent Cement and Lime Pty Ltd, Australia. The X-Ray
Fluorescence (XRF) analysis of GBFS is presented in Table 1. The
activators used in this paper are solid sodium silicate with the
brand name of SS20 obtained from PQ Australia, with a composi-
tion of 75 wt % SiO2 and 23.3 wt % Na2O and sodium hydroxide
obtained from Aldrich with a composition of 99.9 wt % NaOH.
To make GBFS alkali-activated binders, GBFS is dry-mixed with
solid sodium silicate to attain Si/Al molar ratios of 3.6:1 and 4.5:1,
then water is added to the solid mixture to achieve a sample with
an effective H2O/Na2O molar ratio of 14:1, 17:1. Sodium hydroxide is
also blended with the mixtures to match the Na/Al ratios across the
sample set (the Na/Al molar ratio was kept constant at 1.6). A
similar method has been used previously to analyse and compare
geopolymer formulations (Rees et al., 2007a, b). For all samples
studied here, compositional calculations in Table 1 are based on the
silica and alumina content of the raw materials as determined by
XRF. The samples are named according to their compositional ra-
tios. The number outside parentheses refers to the Si/Al molar ratio,
and the number in the parentheses is the H2O/Na2O molar ratio.
Table 2 shows the mass percentage of the components in three
samples studied here.
GBFS 3.6(14) and GBFS 3.6(17) samples have similar Si/Al molar
ratios (3.6), but different H2O/Na2O ratios (14 and 17). Conse-
quently, the impact of H2O/Na2O ratio is considered in these two
samples while keeping similar Si/Al and Na/Al ratios. GBFS 3.6(14)
and GBFS 4.5(14) samples have similar H2O/Na2O ratios (14), but
their Si/Al ratio is different (3.6 and 4.5). Therefore, the impact of
different Si/Al ratios is investigated by comparing these two sam-
ples while keeping similar H2O/Na2O and Na/Al ratios. This method
of research has been used previously to study and characterise
various one-part geopolymer mix designs (Hajimohammadi and
van Deventer, 2016a, b).
Non-porous GBFS mixes are prepared to compare the binder
formulae before foaming. A pre-made foam (with 70 kg/m3 den-
sity) is used to introduce voids in the binder pastes. Sodium dodecyl
sulphate solution (30% concentration) is purchased from Sigma-
Aldrich and diluted with water (1:60 surfactant to water weight
ratio) as a foaming agent. Foam is then produced with the aid of
compressed air in a Dema compressed air foam generator.
In order to synthesise each formula, dry material is measured
according to the weight ratios in Table 2, and mixed in a bowl for a
few seconds. Water is first added to the dry mix, and the paste is
mixed manually for 1 min followed by mixing with the Hobart
mixer for another 1 min. Non-porous GBFS one-part mix pastes are
mixed with standard quartz sand, with 2 g of sand per gramme
binder (calculated as solid plus solution) and poured in
50
50
50 mm cubic moulds at this stage. For the porous
samples, the pre-made foam with 11.5% of the total mass of binders
was added to the binder mixtures in two stages. 20% of the foam is
Table 2
Mass % of each component in GBFS samples.
GBFS Sodium silicate NaOH Water
GBFS 3.6(14) 50.4 19.0 3 27.6
GBFS 3.6(17) 47.7 18.0 2.8 31.5
GBFS 4.5(14) 47.2 27.1 0 25.7
332 A. Hajimohammadi et al. / Journal of Cleaner Production 147 (2017) 330e339
initially added to the mix to increase the paste workability, and the
remaining 80% of foam was gently blended afterwards. The wet
foam mixture is then poured into 50
50
50 mm cubic moulds.
Samples are sealed and cured in a 60  C oven for 24 h, and then
removed from the oven and kept sealed at room temperature until
the day of testing. In this study, we aim to investigate the impact of
the shift in geopolymer chemistry on foam characteristics. Since
development of an optimal mix design is not the purpose of this
study, a relatively high molar ratio of alkalinity is used in these
systems, and all of the samples are cured at 60  C. If each system is
studied and optimised separately, it would be possible to cure some
of the samples at ambient temperature.
The compressive strength of foamed samples is measured by an
Instron 5569A instrument. The loading rate of the machine is
adjusted with a crosshead displacement rate of 1 mm per minute.
An ELE ADRAuto 1500 compression testing machine is also used for
testing the mechanical strength of non-porous binders using
50 mm mortar cubes. Samples are loaded in the testing instrument
at a rate of 0.5 kN/s until failure. All strength results reported are
the average of three samples.
A Vicat instrument is used to measure the setting time of the
alkali activated pastes following the ASTM C191 standard (ASTM-
International, 2013). The slag and water are first mixed and the
setting time is measured at room temperature (23  C) from the time
the alkali activator is added to the mixture. A TAM Air isothermal
calorimeter is used to conduct the calorimetry experiments at a
base temperature of 23 ± 0.02  C. Fresh alkali activated pastes are
prepared first, mixed externally and weighed into ampoules. Then,
the ampoules are immediately placed in the instrument, and the
amount of heat flow is measured over time. The heat flow values
reported are normalised by total weight of the paste.
The crystalline phases of the GBFS one-part mixtures are studied
using powder X-Ray Diffraction (XRD) collected on a Philips PW
1800 diffractometer with CuKa X-rays generated at 30 mA and
40 kV with 0.02 2q steps, 2s step1. Jade 7 software version
5.1.2600 is used to identify the crystalline phases by comparing
diffraction patterns to the ICDD PDF4 database from the Interna-
tional Centre for Diffraction Data.
Attenuated Total Reflectance Fourier Transform Infrared Spec-
troscopy (ATR)-FTIR is used to analyse the nanostructure of samples
using a Varian FTS 7000 FT-IR spectrometer, with a Specac MKII
Golden Gate single reflectance diamond ATR attachment with KRS-
5 lenses and heater top plate. Absorbance spectra are collected from
4000 to 400 cm1 at a resolution of 2 cm1 and a scanning speed of
5 kHz with 32 scans.
In order to study the directional homogeneity of pore distribu-
tion, the ultrasonic pulse velocity within the cubic samples is
measured by a Pundit PL-200 machine (obtained from Proceq). The
overall ultrasonic pulse velocity is measured by a 50 mm diameter
transducer, and the velocity measurement results from three di-
rections are used to compare the homogeneity of pores in different
samples. The pore size distribution of samples is calculated by
image analysis. The 50
50
50 mm cubes are cut in half using a
bench saw, and the Leica M205FA automated microscopy unit is
used to produce microscopic images from the cross-section of
samples to measure the pore size distribution of different formulae.
The transient method is used for thermal conductivity tests,
using the needle probe. Small cylindrical samples with a diameter
of 50 mm and a height of 110 mm are prepared with the hollow
core. A heat transfer gel is applied to the probe, and the probe is
inserted into the hollow core. The temperature is then recorded for
10 min under constant heat dissipation through the probe length
with a voltage of 3 V. To calculate the thermal conductivity, the
inverse value of thermal resistivity is calculated based on the
temperature difference.
4. Results and discussion
4.1. The effect of mix formulation
4.1.1. Crystalline phases
Fig. 1 shows the result of XRD analysis of the GBFS one-part mix
samples. The crystalline phases identified in this one-part-mix
system are kilchoanite (Ca6 (SiO4) (Si3O10); PDF: 00-029-0370),
and gypsum (CaSO4.2H2O; PDF: 00-033-0311) which were present
in unreacted slag (displayed in Fig. 1a), and partially crystalline
calcium silicate hydrate (“C-S-H”; Ca1.5SiO3.5 $xH2O; PDF: 00-033-
0306) and albite ((Na,Ca)(Si,Al)4O8 PDF: 00-009-0456) which are
formed during the reaction. Kilchoanite has been seen in XRD re-
sults of slag in the literature (Glukhovsky et al., 1980; Zhu and Li,
2013). However, gypsum is not usually found in slag. It is a com-
mon practice in Australia to blend gypsum with GBFS during the
grinding process (Yip et al., 2005).
After two days of reaction, new crystal phases have begun to
form in samples, and the crystallinity of the C-S-H gel slightly in-
creases over time. There are some differences in the degrees of
crystallinity between the GBFS 3.6(14) (Fig. 1b) and GBFS 3.6(17)
(Fig. 1a) samples with different water content. The degree of crys-
tallinity slightly increases upon increasing the water content in
GBFS one-part mix binders after 6 days, which is consistent with
observations in the literature (Provis et al., 2005) regarding the
effect of water on the crystallinity of two-part alkali-activated
systems. The differences in crystallinity is not obvious after longer
aging times.
Also, there are some differences between the XRD results for the
GBFS 3.6(14) and GBFS 4.5(14) samples, with different Si/Al ratios.
After 2 days, the GBFS 4.5(14) sample with higher the Si/Al ratio
(Fig. 1c) is less crystalline than the GBFS 3.6(14) sample (Fig. 1b),
and the differences become less evident after longer aging of
samples. A higher Si/Al ratio at constant alkalinity might have
reduced the extent of reaction in the GBFS 4.5(14) sample, causing
slower changes in its structure in comparison with GBFS 3.6(14).
However, alternative analytical techniques are required to better
explain the differences in reaction kinetics and binder behaviour in
these alkali-activated binders.
4.1.2. Nanostructural analysis
The results of FTIR analysis of GBFS one-part mix samples with
different Si/Al ratios and different water contents are presented in
Fig. 2. GBFS (Fig. 2a) has a broad band between 750 and 1050 cm1
and a band at about 1100 cm1 which include many stretching and
bending vibrations of the silicate and sulphate structures in slag (Li
et al., 2010; Zhang et al., 2007), and this broad band covers the
range of wavenumbers where the Si-O-Si and Si-O-Al vibrations of
aluminosilicate gels usually appear. Sharper peaks recognisable in
these areas are related to vibrations of SO2- 4 in gypsum (Anbalagan
et al., 2009). There is a band at about 670 cm1 which is also related
to bending vibrations of SO2- 4 in gypsum (Anbalagan et al., 2009).
It is obvious from the FTIR results of GBFS samples that over time
there is a reduction in the intensity of the band at 1085 cm1, and at
the same time, the intensity of the band at about 960 cm1 in-
creases. The band at 1085 cm1 is related to Si-O-Si stretching vi-
brations of the silica in the newly mixed pastes; a small increase in
this band after few days of aging (as is observed in the day 4
spectrum in Fig. 2c) is due to an increase in the degree of poly-
merisation of silicates within the remaining gel as SieOeSi bonds
form (Bernal et al., 2010). The position of the band related to cal-
cium sulphate materials in slag is close to this wavenumber, but
XRD results show that calcium sulphate materials react almost
completely within the first two days. Therefore, this band is
assigned to the reaction product in GBFS-sodium silicate systems.
 A. Hajimohammadi et al. / Journal of Cleaner Production 147 (2017) 330e339 333

Fig. 1. XRD diffractograms of GBFS one-part mix samples over time. Numbers refer to the age of samples in days. G: gypsum, K: kilchoanite, CS: calcium silicate hydrate, Al: albite.
The peak marked with * is due to the aluminium sample holder.
334 A. Hajimohammadi et al. / Journal of Cleaner Production 147 (2017) 330e339

966
a) b) 870

1085

20
870
14

GBFS 4

0
1200 1100 1000 900 800 700 600
-1
Wavenumber (cm )

966 d) 969
c)
870 870
1085
1085
20

20 14

14 8

8 6

6 4

4 2
2

0 0

1200 1100 1000 900 800 700 6

600 1200 1100 1000 900 800 700 600
-1
Wavenumber (cm ) -1
Wavenumber (cm )

Fig. 2. Ex-situ FTIR spectra of: a) GBFS, b) GBFS 3.6(14), c) GBFS 3.6(17) and d) GBFS 4.5(14) samples. Numbers refer to age of samples in days.

In alkali activated slag systems, it is usually assumed that the band
observed around 950e980 cm1 is the result of the formation of a
calcium silicate hydrate type gel (C-S-H) (Mozgawa and Deja, 2009;
Puertas and Ferna
ndez-Jime
nez, 2003).
The increase in the intensity of the Si-O-T band over time in-
dicates an increase in the polymerisation of forming CeSeH gel
(Puertas and Ferna
ndez-Jime
nez, 2003; Sakulich et al., 2009).
Comparing the FTIR results of the GBFS 3.6(14) (Fig. 2b) and GBFS
3.6(17) (Fig. 2c) samples, with different water contents, indicates
that increasing the amount of water decreased the extent of
changes happening in the binder structure. This difference is
clearer after two days of reaction. It is notable, however, that these
changes are only in the intensities of the peaks, while the final
wavenumber is the same in both samples. Also, comparing the FTIR
results for the GBFS 3.6(14) and GBFS 4.5(14) (Fig. 2d) samples, with
different Si/Al ratios, shows that increasing the silica content has
led to a lower extent of reaction in the GBFS 4.5(14) sample, and the
position of the main band is at slightly higher wavenumbers for the
GBFS 4.5(14) sample.
This observation is consistent with the XRD data for GBFS one-
part mixtures (Fig. 1), as a lower extent of crystallinity was detected
in the higher-Si sample at early ages. Additionally, when the
asymmetric stretching vibration of SieOeT bonds is at lower
wavelengths, it indicates that less Si is present in the CeSeH gels
(Bernal et al., 2010), while participation of aluminum atoms in
tetrahedral coordination causes a shift of the most intense bands in
this region to lower wavenumbers (Mozgawa and Deja, 2009).
Therefore, it can be suggested that increasing the Si/Al ratio leads to
more participation of Si in the C-S-H gel structure in the slag
samples studied here, similar to the known effect of silica modulus
on two-part alkali activated slag systems (Bernal et al., 2010).
There is another minor difference between these spectra which
is related to the intensity of the raw material (sodium silicate) Si-O-
Si band at 1085 cm1. A larger shoulder in this area after two days
means less dissolution of silica particles in this sample. Therefore, it
means that in GBFS one-part mix systems, the dissolution of silica
particles in early hours of reaction slightly increases with
increasing Si/Al ratio.
 A. Hajimohammadi et al. / Journal of Cleaner Production 147 (2017) 330e339
90
80
Strength (MPa)
70
60
50
40
30
20
10
0
7 days 14 days 28 days
Time
Fig. 3. Strengths of one-part mix GBFS binders.
4.1.3. Mechanical strength
Early strength development is very important in lightweight
concrete. Even though foam concretes are not mainly used for load
bearing applications, the cementitious binder needs to gain enough
early strength to hold the porous structure together. Fig. 3 shows
the results of strength testing for three formulae of GBFS samples
over time. As expected from reaction kinetics observed in the FTIR
results, the early strength of GBFS samples slightly decreases with
increasing water content, and the GBFS sample with lower Si/Al
ratio is much stronger than the sample with higher Si/Al ratio. This
observation confirms the FTIR results showing a higher degree of
reaction in the GBFS 3.6(14) sample over time. While the strengths
of GBFS 3.6(14) and GBFS 3.6(17) do not change much over time, the
strength of the sample GBFS 4.5(14) slightly increases over time. By
reaching an average 82 MPa, the GBFS 3.6(14) sample is the
strongest one-part alkali activated slag studied here.
4.2. Characterising inorganic foams
As explained above, inorganic foams made of three different
formulations are prepared with a mechanical foaming technique.
Samples are categorised in this section according to their porosity
and properties, and the differences in foam characteristics are
related to the differences in the reaction mechanisms observed in
different formulations.
4.2.1. Pore size distribution
Microscopic images of the interior arrangement of voids are
presented in Fig. 4, which shows some differences in the size of the
air voids in different GBFS formulations. In order to better compare
the differences, image analysis is carried out to determine the pore
size distribution in the microscopic images, as depicted in Fig. 5.
Fig. 5 shows the result of the pore size distribution based on the
image analysis of microscopic images. Three images from the cross
section of geopolymer foams were collected to cover about 12 cm2
area of the surface, and the image analysis was performed on the
combined images for each sample.
Fig. 4. Microscopic images of the cross section of samples for a) GBFS 3.6(14), b) GBFS 3.6(17) and c) GBFS 4.5(14).
335
GBFS 3.6(14) has the smallest size of the air voids with the
majority of the voids (more than 60%) smaller than 0.5 mm. The
pore size in GBFS 3.6(17) is relatively larger than GBFS 3.6(14) with
GBFS 3.6(14)
about 45% of the voids smaller than 0.5 mm, about 35% between
0.5 mm and 1.5 mm, and the rest of the voids bigger than 1.5 mm.
GBFS 3.6(17)
GBFS 4.5(14) has the largest pore size distribution with only about
GBFS 4.5(14) 30% of the voids smaller than 0.5 mm, about 45% between 0.5 mm
and 2 mm, and few large pores.
In alkali activated foams, the liquid film around the bubbles will
be populated by colloidal particles (gels) which undergo polymer-
isation and hardening stages. There are two different characteris-
tics of the gels that can impact the final size of the voids; i.e. the
setting and hardening process of the binding skeleton and the size
of the gels and particulates around the bubbles. Faster setting re-
sults in trapping and maintaining small voids within the matrix
before they join and grow bigger (Ostwald ripening effect).
Consequently, faster setting helps with maintaining small pores
while the alkali activated foam is made. On the other hand, the size
of the gel particulates also has an important impact on the final size
of the voids. If the surface of the initially formed bubbles is much
smaller than their surrounding particulates, the bubbles tend to
coalesce until their surfaces are protected by a stabilising layer of
particles (Dickinson, 2010). Subsequently, larger pore size distri-
butions will be observed when the gel size is large during the initial
setting of the binding skeleton. The aggregation and polydispersity
of colloidal particles are the reason why it is very difficult to make
particle-stabilised foams with very small bubble size (Dickinson,
2010; Murray and Ettelaie, 2004).
In order to correlate the pore size distribution of the samples
with the kinetics of reaction and size of gel particulates, Vicat and
calorimetry tests have been conducted on unfoamed alkali acti-
vated pastes. Fig. 6 shows the result of the Vicat test on the three
samples. According to the results, GBFS 3.6(14) sets quicker than
GBFS 3.6(17) which was predictable due to the higher amount of
water in the GBFS 3.6(17) sample. Also, the initial setting of the
GFBS 4.5(14) happens much quicker than the other two samples.
The differences in the reaction rate and the water content of the
GBFS pastes in GBFS 3.6(14) and GBFS 3.6(17) samples should be the
reason for the small differences in their pore size distribution. Ac-
cording to the Vicat and FTIR results, the rate of the reaction in the
GBFS 3.6(14) sample is higher than that in the GBFS 3.6(17) sample
with more water content, and therefore the setting and hardening
are faster in the GBFS 3.6(14) sample. Also, when the foam is mixed
with the mixer, bubbles break up into smaller bubbles under shear
stress. In concentrated foams, bubble break up is facilitated by the
interaction of neighbouring bubbles (Golemanov et al., 2008). In
3.6(14) samples with lower water content, the concentration of
foam will be higher and therefore mixing of the foam can lead to
more bubble break up in this system. Thus, a number of small size
voids exists in the GBFS 3.6(14) sample at the beginning, and the
faster hardening of the skeleton helps to maintain small bubbles in
the matrix. Therefore, a higher number of small voids (<0.5 mm) is
found in the GBFS 3.6(14) sample.
336 A. Hajimohammadi et al. / Journal of Cleaner Production 147 (2017) 330e339
Fig. 5. Pore size distribution analysis using the microscopic images of the cross-section of GBFS samples.
Fig. 6. Vicat needle penetration depth as a function of time for alkali-activated slag
pastes.
However, despite the fastest setting of the GBFS 4.5(14) sample,
the larger pore size distribution is observed in this alkali activated
paste. As explained before, the size of the gel particulates during
the initial setting is another important factor that governs the size
of the voids in alkali activated foams. By combining calorimetry
results of alkali activated slags with Nuclear Magnetic Resonance
(NMR) and FTIR studies, Ferna
ndez-Jime
nez and Puertas had
shown previously that where the curves of heat evolution rate
showed a large single peak, the start of the setting was coincident
with the maximum formation and precipitation of the main alkali
reaction products (the calcium silicate hydrate) with a high degree
of polymerisation (Ferna
ndez-Jime
nez and Puertas, 2001). How-
ever, when the initial and final setting of the pastes occurred before
the induction period, the setting was related to the formation of a
pre-induction peak in curves of heat evolution rate (Fern
andez-
Jime
nez and Puertas, 2001). In this case, the setting was related
to the precipitation of an initial calcium silicate hydrate with a low
degree of polymerisation (Ferna
ndez-Jime
nez and Puertas, 2001).
While the purpose of the Fern
andez-Jime
nez and Puertas was to
study the effect of different types of activators, their work on
correlating the calorimetric results with the size of the hydration
products during the initial setting time is very useful here.
Fig. 7 shows the result of the calorimetry experiments on three
unfoamed samples. Maximum three peaks can appear in the curves
of heat evolution rate in alkali activated slag pastes (Ferna
ndez-
Jime
nez and Puertas, 2001; Gebregziabiher et al., 2015; Krizan
and Zivanovic, 2002), i.e. the first which is the dissolution peak,
the second which is the pre-induction peak, and the third the ac-
celeration peak. The acceleration peak is associated to the
maximum precipitation of reaction products. In this study, the
acceleration peak (single peak) is observed in the GBFS 4.5(14)
sample with the fast initial setting while in the other two samples
pre-induction peaks are also observed. According to the Fern
andez-

nez and Puertas conclusions, this calorimetry result suggests
Jime
that the precipitation products in the GBFS 4.5(14) sample during
the initial setting is a highly polymerised calcium silicate hydrate
while the initial calcium silicate hydrates (with small size) are
responsible for the initial setting of the GBFS 3.6(14) and GBS
3.6(17) samples. This can explain the larger size distribution of the
bubbles in the GBFS 4.5(14) sample since large gel particulates
cannot maintain very small voids (Dickinson, 2010).
4.2.2. Pore homogeneity
The homogeneity of pore distribution inside the foam matrix is
as important as the size distribution of the pores. Usually, there is a
slight difference between foam densities in different layers of the
foam. High water content and the shear stress caused by mixing
facilitate a layering of bubble sizes, so this re-arrangement of
bubbles according to size is less in drier foams (Hutzler et al., 2000).
Ultrasonic Pulse Velocity (UPV) is a non-destructive technique
usually used to study the homogeneity of concrete (Güneyisi et al.,
2015; Lim and Cao, 2013). The existence of the cracks and voids or
formation of honeycomb within the concrete matrix drops the
pulse velocity, and therefore it can give a good indication of the
quality of concrete.
In this study, UPV is used to measure the homogeneity of pore
distribution in GBFS foams. The pulse velocity is measured in three
different directions from side to side and from top to bottom of the
cubic samples. The noticeable difference in pulse velocity mea-
surements in different directions means that the pores are not
distributed homogeneously in the samples. Fig. 8 shows the result
of the UPV test on the three GBFS samples. The pulse velocities from
side to sides are very similar in all three samples, but there is an
obvious difference between the velocities of side to sides and top to
bottom. This difference shows the extent of bubble size arrange-
ment from top to bottom within the samples. The homogeneity
percentage is calculated by finding the standard deviation of ve-
locity measurements in three directions.
The highest homogeneity is related to the GBFS 3.6(14) sample,
and the lowest homogeneity is related to the GBFS 3.6(17) sample.
The lower homogeneity percentage in the GBFS 4.5(14) sample
should be related to the wider size distribution of the voids
observed in this system. In the GBFS 3.6(17) sample, the homoge-
neity percentage is the lowest among all three samples. The high
amount of water together with the slower dissolution of source
materials (according to the FTIR results) significantly increases the
workability of the GBFS 3.6(17) sample compared to the other two
 A. Hajimohammadi et al. / Journal of Cleaner Production 147 (2017) 330e339
Fig. 7. Heat evolution of alkali-activated slag pastes over time.
Fig. 8. a) Ultrasonic pulse velocities in three different directions of cubic GBFS samples
and b) pore homogeneity results.
samples. The extent of foam sorting and bubble size re-
arrangement is higher in foams with higher water content
(Hutzler et al., 2000), as evidenced by the observation that the
layering of the foam in GBFS 3.6(17) is the highest among all three
samples.
4.2.3. Engineering properties
4.2.3.1. Thermal conductivity. One of the important properties of
foam concretes is their insulating capacity. The air voids in foam
concrete significantly drop their thermal conductivity and act as an
effective barrier against the heat flow within concrete blocks.
Density and thermal conductivity of three GBFS foams are pre-
sented in Fig. 9. In spite of adding a similar amount of pre-made
337
Fig. 9. Thermal conductivity results of three GBFS foams.
foam to all three formulae, the final density of the samples is
different with the GBFS 3.6(17) sample being the lightest and the
GBFS 4.5(14) sample being the densest foam.
The combination of initial workability of the GBFS binders and
their reaction rate is the reason behind the differences in densities.
The GBFS 3.6(17) sample has the highest amount of water, and
according to FTIR results, this sample has slow dissolution of source
materials, and therefore, has very high workability. Also, as
explained before, the size of the gel particulates is relatively small
in this sample during the initial setting. High water content in this
sample protects bubbles from breaking during the initial mixing of
the foam (as evident in size distribution analysis). On the other
hand, the relatively small gel particulates on the bubble films
protect them from coarsening. Therefore, the density of this sample
will be the lowest.
The amount of water in the GBFS 3.6(14) and GBFS 4.5(14)
samples is lower, and as a result the initial workability of the paste
is not as high as the GBFS 3.6(17) sample, so some of the pre-made
foam will collapse because of high shear stresses during the initial
mixing of the foam and pastes resulting in relatively higher den-
sities. On the other hand, the size of the gel particulates in the GBFS
3.6(14) sample is smaller than the GBFS 4.5(14) sample and
therefore, GBFS 3.6(14) can better protect the foam from drainage.
As a result, the density of GBFS 3.6(14) is lower than GBFS 4.5(14).
338 A. Hajimohammadi et al. / Journal of Cleaner Production 147 (2017) 330e339

Lower density is usually because of a higher number of voids 3.6(17) sample.

and leads to lower thermal conductivity. The thermal conductivity
results in Fig. 9 follow this trend with the GBFS 3.6(17) sample with
5. Conclusions
the lowest density having the lowest thermal conductivity and the
GBFS 4.5(14) sample with the highest density having the highest
Inorganic foams were made from alkali-activated slag with
thermal conductivity. However, the differences in thermal con-
three different mix formulations. The structural evolution and the
ductivities are not as significant as the differences in densities. The
properties of non-porous binders were analysed, and the effect of
reason should be related to the re-arrangement of the voids in foam
the reaction mechanism on the foam characteristics was explored.
concretes. Although the existence of more voids usually means
In order to minimise the effect of alkali reaction on the amount of
higher air content in concretes and consequently better thermal
initial foaming, a mechanical foaming method was used. The same
resistance, the relative orientation and position of the pores can
amount of pre-made foam with the same density was added to
considerably affect the insulating properties (Zhao et al., 2006).
three formulations, and the effect of alkali reaction on pore size
If the pores are arranged perpendicular to the heat flow, more
distribution, homogeneity of pore distribution, density and prop-
heat should pass through the pores and the concrete foam will
erties of final inorganic foams were investigated.
show more thermal resistance. However, if a layer of pores is
The water content of mix formulation affects the initial con-
populated in parallel with the heat flow direction, it will enforce a
centration of the foam. The higher concentration of the foam leads
smaller resistance to heat flow (Loeb, 1954). Hence, the intensive
to more bubble breakage in sheared foam and smaller bubble sizes.
layering of pores from top to the bottom observed in GBFS 3.6(17)
However, it also facilitates the rupture of liquid film around the
has a negative effect on its insulating properties. That is why even
bubbles inducing foam drainage. Foams with higher water content
with much lower density, GBFS 3.6(17) does not have notably lower
are more prone to bubble size re-arrangement (foam sorting)
conductivity compared to the other two samples.
during mixing and pouring into the moulds. The bubble size
arrangement of the foam results in poor homogeneity of pore size
distribution and has some negative effects on strength develop-
4.2.3.2. Strength of the foams. The strength development of
ment and thermal conductivity of lightweight slag-based foams.
unfoamed geopolymer pastes are shown earlier in Section 4.1.3. In
Samples with lower thermal conductivity will have better thermal
this section, the strength result of alkali activated slag foams are
insulation capacity.
presented, and the correlation between the strength results to the
The GBFS formulations with faster setting times can maintain
pore characteristics and the strength of the binding skeleton is
most of the voids within the matrix and reach lower densities with
discussed. Strength development in three inorganic foams is
a similar amount of foam added to them. Also, samples with smaller
measured, and the 28 days strength results are presented in Fig. 10.
size of gel particulates (during the initial setting) can avoid the
The strength of the samples was measured for 7 days, 14 days and
coarsening of the voids and result in the smaller pore size distri-
28 days and no considerable changes in strength development was
bution. If the pore distribution is homogeneous within the matrix,
observed in any of the samples over time. Also, because of the large
the strength of the binding skeleton combined with size distribu-
difference between sample densities, the strength results are
tion of pores are the key factors for strength development. The
calculated by dividing the average strength of the samples by their
characteristics of the inorganic foams do not have to be controlled
average densities to be able to compare the results.
by the quality and quantity of pre-made foam. By manipulating the
As expected from the strength results of non-porous samples,
binder formulation, it is possible to change the density and prop-
the GBFS 3.6(14) foam is the strongest foam among all three for-
erties of the final inorganic foams and achieve the desired product.
mulations. This result is related to its strong binding skeleton
There are a few limitations in this study to compare the different
together with smaller pores and more homogenous distribution of
alkali activated slag foams with different mix designs. Since the
the voids within the matrix. However, contrary to the strength
purpose of this study was to compare three different formulae, a
results of non-porous samples, the GBFS 4.5(14) foam is slightly
relatively high amount of alkali is used and the samples are cured in
stronger than the GBFS 3.6(17) sample. Also, the pore size distri-
the oven. This preparation procedure of the slag-based foams could
bution result showed the presence of larger pores in the GBFS
be over-conservative to make sure all three formulae successfully
4.5(14) sample compared to the GBFS 3.6(17) foam. Therefore, the
make alkali activated foams. In future research, samples with a
loss of strength in the GBFS 3.6(17) foam should be mainly related
lower level of alkalinity cured at ambient conditions can be
to the foam sorting in this sample observed in UPV test results. The
investigated.
top layers with the large voids are very weak under compression
and significantly affect the compressive strength of the GBFS
Acknowledgment

Strength / Density Density This work was funded in part by the ARC Linkage Grant
1.5 800 [LP140100504, 2014], in part by the Centre for Sustainable Resource
Average Density (kg/m3)
Average Strength / Average

700 Processing through the Geopolymer Alliance, and in part by the

600
Density (kNm/kg)

Australian Research Council (including partial support through the

1.0 500 Particulate Fluids Processing Centre). The authors would like to
400 acknowledge Mr Christopher Ling Zhong Yi, Mr Christy Ribi Pra-
0.5 300 setyo, Mr Richard Alan Faulkner and Mr Stephen Gondokusumo for
200 their assistance with some of the experimental work, and the
100 guidance and advice received from Prof John L. Provis of the Uni-
0.0 0 versity of Sheffield during the early part of this research is greatly
GBFS 3.6(14) GBFS 3.6(17) GBFS 4.5(14) appreciated. This work is performed in part at the Materials Char-
Fig. 10. Compressive strength results of foamed samples after 28 days of aging. Nor-
acterisation and Fabrication Platform (MCFP) at the University of
malised strength results are calculated by dividing the average strength of the samples Melbourne and the Victorian Node of the Australian National
by their average densities. Fabrication Facility (ANFF).
 A. Hajimohammadi et al. / Journal of Cleaner Production 147 (2017) 330e339 339

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