Journal of the European Ceramic Society 36 (2016) 4243–4249

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Journal of the European Ceramic Society

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High strength metakaolin-based geopolymer foams with variable

macroporous structure
Chengying Bai a,∗ , Giorgia Franchin a , Hamada Elsayed a , Alberto Conte a , Paolo Colombo a,b

a
Department of Industrial Engineering, University of Padova, via Marzolo, 9, Padova, Italy
b
Department of Materials Science and Engineering, The Pennsylvania State University, University Park, PA 16802, United States

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

Article history: Metakaolin-based geopolymer foams were synthesized by mechanical frothing, using hydrogen peroxide
Received 14 April 2016 as additional foaming agent; three vegetable oils were added in order for the saponification reaction to
Received in revised form 21 June 2016 occur. The combined use of the two foaming techniques (mechanical frothing and H2 O2 decomposition)
Accepted 23 June 2016
led to interconnected porosity: the in-situ formation of the soap molecules generated by the saponifica-
Available online 15 July 2016
tion reaction was exploited to generate macro-porosity. This combined route enabled the production of
geopolymer foams with a range of total porosity and strength values, with an optimal sample possessing
Keywords:
a total porosity of to ∼81 vol%, an open porosity of ∼79 vol%, and a compressive strength of ∼3.1 MPa.
Geopolymer foams
Macroporous structure
Moreover, factors that influence the compressive strength, the porosity, and the pore size distribution
Saponification were investigated. The results showed that the cell size and cell window size can be controlled by adding
Porosity different oils and different contents of peroxide.
© 2016 Elsevier Ltd. All rights reserved.

1. Introduction tion/peroxide/gelcasting combined method was proposed by Cilla

Geopolymer foams have been the focus of attention in the
field of eco-friendly porous materials because of their favorable
mechanical and chemical stability, low shrinkage after forming,
high temperature resistance, etc. [1–4]. They have been employed
in photocatalytic degradation applications or used as membrane
supports, catalyst supports, heavy metals adsorbents and so on
[4–9]. Aluminum and silicon and H2 O2 have been used as pore
foaming agents for the fabrication of geopolymer foams [1,10,11],
but the pores generated by this foaming technique are typically
closed, thereby limiting the range of applications for the compo-
nents.
Recently, alternative processing routes for the fabrication of
porous geopolymers have been proposed. An oil-based emul-
sion templating route was put forward, which enables to obtain
hierarchically porous geopolymers suitable for catalyst applica-
tions [9,12]. Other experiments related to the addition of oil
to geopolymers, showed that waste oil can be trapped inside
the geopolymeric matrix [13]. Geopolymers with a mesoporous
matrix and unidirectional lamellar macro-porosity were also
produced by the freeze-casting technique [14], and a saponifica-
et al. [15]. Although geopolymer foams with an open porosity of
∼70 vol% and a total porosity as high as ∼85 vol% were successfully
produced by the combined techniques, the compression strength
of the foams was only ∼0.45 MPa, which limited the range of appli-
cations for the components.
Despite an increasing number of papers dealing with the fab-
rication of porous geopolymers using different approaches [1–15],
more investigation is still required to improve the process, espe-
cially in reference to the amount of open porosity and mechanical
strength of the components. In particular, components possessing
high strength and a high amount of open porosity, with controlled
pore size and distribution, are of interest for several aplications.
In this study, high mechanical strength metakaolin-based
geopolymer foams (MGFs) with open porosity were fabricated
using the gelcasting/saponification/peroxide combined route. Their
porosity, cell and cell window size and mechanical properties were
controlled by adding different oils and different contents of perox-
ide.
2. Experimental procedure

Metakaolin (Argical 1200s, AGS Mineraux) was used to fabri-

cate the MGFs. A 17.6 M KOH solution was prepared by dissolving
∗ Corresponding author. potassium hydroxide pellets (Sigma-Aldrich) for at least 24 h at
E-mail addresses: chengyingbai@163.com, baichenying@gmail.com (C. Bai). room temperature [1,15]. A potassium silicate solution (KSIL 0465,

http://dx.doi.org/10.1016/j.jeurceramsoc.2016.06.045
0955-2219/© 2016 Elsevier Ltd. All rights reserved.
4244 C. Bai et al. / Journal of the European Ceramic Society 36 (2016) 4243–4249
Crosfield Italia srl) and the KOH solution were mixed to provide
the alkali activator solution. Three vegetable oils (canola oil (Great
Value, Wal-Mart, USA); sunflower oil (Panorama, Pam, Italy); olive
oil (Fragrante, Bertolli, Italy)) and a 3 wt% H2 O2 solution diluted
from 30 wt% H2 O2 (Sigma-Aldrich), were used as chemical foam-
ing agents. A previous study [1] showed that the addition of diluted
hydrogen peroxide to the system enabled to obtain uniform, less
anisotropic pores.
A suspension (S) with theoretical oxide molar ratios:
SiO2 /Al2 O3 = 3.53, K2 O/SiO2 = 0.36 and H2 O/K2 O = 11.1 was pre-
pared by mechanical mixing for 30 min at 800 rpm of the alkali
activator solution in which metakaolin (MK) was dispersed. The
oil and H2 O2 were then added successively at room temperature,
stirring at 1200 rpm for 10 min (frothing) and 600 rpm for 5 min,
respectively. The weight fraction of oil in S was defined as x, and
the weight fraction of H2 O2 in S as y.
The geopolymer foams were produced by casting the slurry
into a sealed plastic mold and curing for 24 h at room tempera-
ture and for another 24 h at 75 ◦ C in an oven. Previous works [1,14]
showed that the pre-heat treatment can contribute to improve the
physical strength and the rate of geopolymerization. To obtain the
final MGFs, an extraction step was carried out by saturating the
samples with hot water (renewed every 20 min until it remained
clear), to completely evacuate the water-soluble soap and glycerol
molecules generated by the saponification. This step also allowed
to verify the completion of the geopolymerization reaction, as
a non-fully condensed geopolymer structure would disaggregate
(undergo dehydroxylation and expansion) in water [4,15]. Prior to
characterization, the MGFs were dried at 40 ◦ C for one week.
The relative (bulk) density (␳r ) of the MGFs was obtained as the
ratio between the mass of a parallelepiped-shaped sample cut from
a larger foam and its geometrical volume (as measured with a dig-
ital caliper). The true (skeleton) density (␳0 ) was measured with a
gas pycnometer (Accupyc1330, Micromeritics, USA) at room tem-
perature on finely ground MGFs powders. The total porosity (TP)
was calculated based on the relation TP = 100 (1 − ␳r /␳0 ) × 100%
[15,16], and the corresponding open porosity (OP) was determined
by the Archimedes’ method using distilled water as the immersion
medium.
Compressive strength was measured using an Instron 1121 uni-
versal material testing machine (Canton, Massachusetts, USA), with
a cross-head speed of 1 mm/min, and at least six specimens with
a ∼10 × ∼10 × ∼15 mm3 dimension, cut from larger samples, were
tested. A Brookfield viscometer (DV-II+ Pro EXTRA, spindle R1-4,
rpm 12, USA) was used for evaluating the viscosity of the geopoly-
mer slurries at room temperature.
The crystalline phase assemblage was investigated using an X-
ray diffractometer (XRD; AXS-D8 advance, Germany), operated at
40 kV, 40 mA, with Cu K␣ radiation (step width 0.05◦ ). The mor-
phology of cut surfaces was observed using optical microscopy
(AxioCam ERc 5s, Carl Zeiss, Germany) and a Scanning Electron
Microscope (SEM; FEI Quanta 200, Netherlands). The cell size and
side distribution, as well as the cell windows size, were assessed
from SEM images using an image analysis software (Nano Measurer
1.2), and at least 100 pores were measured per sample [17]. The data
were converted to three-dimensional values using the stereological
equation Dsphere = Dcircle /0.785 [2,15].
3. Results and discussion
3.1. Effect of different types of oil
The foaming mechanism when using vegetable oils (mainly
hydrophobic triglycerides) [12] can be described as follows:
the highly alkaline geopolymer slurry mixed with the oil gen-
erates in situ a carboxylate surfactant (soap) and glycerol
(CH2 (OH)–CH(OH)–CH2 (OH)) molecules, via a saponification reac-
tion. The excess of KOH present in formulation of the slurry ensures
that the oil triglycerides convert completely into soap and glycerol.
Glycerol is a water soluble molecule which can be extracted by
hot water after the curing process leaving behind (meso-)pores.
The soap molecules formed in situ stabilize the gas bubbles gener-
ated by the mixing and the decomposition of the peroxide, leading
to open, interconnected cells [12,15]. It can therefore be expected
that the different chemical characteristics of the various oils would
affect the morphology, hence the strength, of the MGFs. Consid-
ering that the saponification value (i.e. the number of milligrams
of potassium hydroxide required to saponify 1 g of triglyceride) of
the three oils was about 190, [18,19] the ratio of K2 O/SiO2 in the
geopolymer slurry before and after the addition of the different oils
addition was 0.36 and 0.29, respectively.
The SEM images of MGFS produced using different oils (x = 0.2,
y = 0.1) are reported in Fig. 1. All samples possessed a cellular struc-
ture with a large number of partially open cells, surrounded by
relatively thick walls, having a size distribution ranging from ∼150
to ∼450 ␮m.
The type of oil used was found to have an effect on the pore struc-
ture of MGFs. The average cell pore size of the foams, computed
by image analysis for each sample, was: 339 ± 136 ␮m (canola oil,
Fig. 1A), 391 ± 151 ␮m (sunflower oil, Fig. 1B), and 247 ± 89 ␮m
(olive oil, Fig. 1C). The wide distribution of the cell size is typical of
foams produced using a direct foaming approach. Moreover, many
smaller pores were present in the cell walls and the struts (see
Fig. 1(a–c)). They are attributable to oil droplets that were trapped
in the geopolymer structure, and removed by the hot water extrac-
tion [12,13]. Their presence, particularly in the cell walls, increased
the amount of open porosity in the samples (see later), since they
increase the permeability of the structure. The average sizes for the
pores in the cell walls and struts were 15.0 ± 4.5 ␮m (canola oil),
22.8 ± 8.3 ␮m (sunflower oil) and 17.3 ± 5.3 ␮m (olive oil).
The effect of the type of oil on the compressive strength of
MGFs produced using similar processing conditions (x = 0.2, y = 0.1)
is reported in Fig. 2.
In order to assess the effect of the addition of different types of
oil on the microstructure of the samples, we should consider: (i)
the nature of the oils, (ii) the viscosity changes caused by the oils
[15,20], and (iii) the emulsion stability [21]. In fact, different oils
produce different types of soap molecules (surfactants), and any
variation in the viscosity of the mixture would affect the degree
of foaming (while the rest of the processing parameters, such as
mixing rate and amount of H2 O2 , are kept constant). It should be
noted that the amount of surfactant molecules produced was the
same for every oils, since they had a similar saponification value
and the systems contained enough potassium hydroxide to lead
to the completion of the saponification reaction. Concerning the
stability of the emulsions, the time scale for our process is typically
shorter than that for which flocculation, coalescence and Ostwald
ripening can occur in an oil/water emulsion, so we could disregard
this complex effect, at least in an initial analysis [21].
Firstly, the viscosity for the different slurries was measured.
It is also important to observe that the geopolymer mixtures are
reactive, and therefore their viscosity changes with time. The mea-
surements were therefore carried out for a time interval ranging
from 30 s to 1 h, to take into account the variation of viscosity dur-
ing processing. The data concerning the viscosity of the different
systems are listed in Table 1. The viscosity of the different pure oils
was rather similar (0.067 Pa s for olive oil, 0.058 Pa s for canola oil
and 0.050 Pa s for sunflower oil), but lower than that of the oil-free
slurry (1.60 Pa s).
The data indicate that the addition of oil increased significantly
the viscosity of the system, and this can be explained by the elastic
 C. Bai et al. / Journal of the European Ceramic Society 36 (2016) 4243–4249
Fig. 1. SEM images of MGFs produced using: canola oil (A–a); sunflower oil (B–b); olive oil (C–c). The insets of figures (A)–(C) report the cell size distribution data, and the
insets of figures (a)–(c) are a magnification of a cell to better visualize the cell windows.
Fig. 2. Porosity and compression strength of MGFs produced using different types of
oils (OP = open porosity (vol%); TP = total porosity (vol%)). Samples produced using
x = 0.2, y = 0.1.
interactions of oil droplets in the fresh mixture [13]. We should
also note that the production of soap and glycerol might also affect
the measurement, as the spindle can be lubricated by them; in fact,
the viscosity of the oil-containing slurries decreased in time until
stabilizing after about 25 min (note that due to the excess of KOH
in the system, the saponification rate is fast). No effect of the type
of oil was observed with respect to the setting (geopolymerization)
rate for the different slurries.
The fact that the use of olive oil yielded smaller cells but higher
total porosity indicates that the soap molecules formed in situ
during processing were more effective in stabilizing the liquid/air
interface in the foams.
Table 1
Viscosity values of the slurries produced using different oils.
Viscosity Slurry with different oils (x = 0.20)
Canola oil
Initial viscosity of the slurry (Pa·s) 4.20
Time for viscosity increase to 120% (min) ∼58.5
Time for viscosity increase to 150% (min) ∼63
4245
The results thus confirm that the produced pore architecture
(amount of porosity, open/closed pore ratio, cell and cell window
size) derives from the complex interaction of different intertwined
factors (viscosity of the solution, geopolymerization reaction rate,
characteristics of the surfactant molecules produced). We should
also observe that the XRD patterns, not reported here for the sake
of brevity, were similar (amorphous), for all systems indicating that
different oils did not affect the phase assemblage of the produced
geopolymers but only the characteristics of the porosity.
The specimens produced using canola and sunflower oil pos-
sessed similar porosity but lower mechanical strength than those
containing olive oil. The fact that samples obtained using olive oil
had a higher compression strength, despite the larger amount of
total porosity, is attributable to their smaller cell size; in fact, pre-
vious work [22] showed that the compression strength of porous
ceramics drops sharply with the increase of the average cell size.
The higher strength possessed by the samples, in comparison to
reported values for a similar system [15], is attributable to the
thicker struts formed during foaming.
According to the collected data, olive oil gave the best results in
terms of strength and amount of total porosity, and therefore this
system was used to investigate the effect of the amount of oil and
peroxide on these characteristics of MGFs.
3.2. Effect of different amounts of olive oil and of hydrogen
peroxide
First of all, we should report that the time required for the vis-
cosity of the system to raise by a certain percentage (120 or 150%
Slurry without oil
Sunflower oil Olive oil
7.30 14.85 1.60
∼88.5 ∼97 ∼57.5
∼91 ∼98.5 ∼60.5
4246 C. Bai et al. / Journal of the European Ceramic Society 36 (2016) 4243–4249
Fig. 3. (a–c) Morphology of MGFs produced with various amounts of olive oil ((a) x = 0.37; (b) x = 0.53; (c) x = 0.70); insets show a magnified view of a cell and surrounding
struts. (d) XRD patterns of pure MK and of different samples.
with respect to the initial value), an effect caused by the progression
of the geopolymerization in the mixtures with time, increased with
increasing olive oil content. This can be explained by the consump-
tion of OH− by acids from the oil, which increases with increasing
oil volume fraction, therefore slowing down the geopolymerization
reaction kinetics [13]. In any case, the setting times for the slurries
were of the order of 90–110 min, thus far exceeding the process-
ing time required to produce the foams, and therefore no effect of
the different rate of geopolymerization on the total porosity of the
samples could be inferred.
Fig. 3(a–c) shows the microstructure of MGFs produced using
different amounts of olive oil (the amount of olive oil (x) ranged
from 0.2 to 0.7), and Table 2 reports the porosity (total and open),
relative density, average cell size, and compressive strength data
for the different samples.
Varying the amount of olive oil, while maintaining constant the
amount of peroxide, had a significant effect on the porosity char-
acteristics. When the olive oil content increased from 20 to 70 wt%,
the total porosity fell sharply from ∼81 to ∼67 vol%, while the ratio
between the open porosity and the total porosity remained almost
constant (>93%). By adding more oil, the viscosity of the slurry
increased (in accordance with [13]) but not very significantly, so
this is not a sufficient reason to explain the observed trend. More
work will have to be conducted to further elucidate the reason for
the observed behavior.
The morphology of the cells and of the interconnecting pores
in the cell walls and struts was similar in all samples. The aver-
age cell size decreased with increasing the amount of olive oil
present, while the size of the interconnecting pores in the cell walls
and struts increased. The decrease of the average cell diameter is
attributable to the increase in viscosity with increasing oil content
as well as to the possibility of stabilizing more gas bubbles in the
slurry, due to the higher number of surfactant molecules available
[13,14], while the increase in the interconnecting pore size is possi-
bly due to the (partial) coalescence of oil droplets that form during
mixing, due to their higher number being present [21].
The effect of oil content on the mechanical strength of the sam-
ples is complex, as it has an effect on the total porosity, the average
cell size and the size of the pores in the struts and cell walls. With
increasing olive oil content, the corresponding average compres-
sive strength dropped slightly from 3.1 to 2.2 MPa, despite the
decrease in total porosity and reduction in average cell size. This
effect could be explained considering the increasing amount and
size of the small pores (derived from the oil droplets trapped in the
geopolymer matrix) present in the struts and cell walls. In order
to fully assess the influence on the strength of the distribution of
pores in the material, i.e. how much porosity is present in the cell
walls and struts with respect to the total porosity, more accurate
investigations using mercury porosimetry will have to be carried
out.
Moreover, it should be observed that, since KOH is consumed
by the saponification reaction, the value of the K2 O/SiO2 ratio
in the geopolymer decreased from 0.28 to 0.12 with increasing
amount of oil. X-ray diffraction analysis, see Fig. 3d, showed that the
structure of the produced geopolymers changed with the composi-
tion. The pattern for pure MK shows a typical broad characteristic
hump located in the 15–35◦ 2␪ range, plus some peaks attributable
to quartz, muscovite and anatase impurities in the meta-kaolin
[23,24], while the geopolymer samples display a large diffuse halo
in the 20–40◦ 2␪ region [8,11,20,23–28]. With increasing amount
of oil (decreasing K2 O/SiO2 ratio), a hump located at around 20◦ 2␪
becomes more apparent which, according to the work of Williams
[27], could be linked to the presence of disordered (unreacted)
kaolin. Indeed, the degree of dissolution of metakolin has a strong
positive correlation with the OH− concentration (mol/l) of the
alkali activating solution (the K2 O/SiO2 ratio), and the mechanical
properties increase with the amount of reacted metakaolin [25].
Previous work showed also that the ratio K2 O/Al2 O3 has a signif-
 C. Bai et al. / Journal of the European Ceramic Society 36 (2016) 4243–4249 4247

Table 2
Porosity, relative density, average cell size and compressive strength data as a function of the amount of olive oil (x) and peroxide (y).

Sample x y K2 O/SiO2 Bulk density Average size (␮m) Open porosity Total porositye Compression
(g/cm3 ) (vol%) (vol%) strength (MPa)

Cell Strut and cell wall pores

SO1 0.20 0.1 0.29 0.40 ± 0.01 247 ± 89 17.3 ± 5.3 79.5 ± 0.1 81.4 ± 0.5 3.11 ± 0.82
SO2 0.37 0.1 0.23 0.42 ± 0.01 210 ± 73 20.9 ± 6.0 75.2 ± 0.3 75.4 ± 0.6 2.57 ± 0.52
SO3 0.53 0.1 0.17 0.48 ± 0.02 169 ± 51 28.3 ± 9.6 68.4 ± 0.3 70.3 ± 1.3 2.38 ± 0.47
SO4 0.70 0.1 0.12 0.51 ± 0.02 130 ± 52 37.8 ± 13.6 62.9 ± 0.2 67.4 ± 1.3 2.19 ± 0.21
SH0 0.20 0 0.29 0.84 ± 0.01 40 ± 15 – – 62.0 ± 0.5 25.96 ± 5.12
[15] 0.25 0 0.24 0.81 ± 0.01 98 ± 12 – 59.8 66.4 –
[15] 0.25 0.06 0.24 0.34 ± 0.01 318 ± 18 – 69.2 83.5 0.45 ± 0.08
SH2 0.20 0.05 0.29 0.59 ± 0.02 125 ± 46 16.5 ± 5.4 67.0 ± 0.1 72.6 ± 0.9 8.83 ± 2.38
SH6 0.20 0.15 0.29 0.30 ± 0.01 383 ± 265 17.2 ± 5.9 84.0 ± 0.1 86.3 ± 0.5 0.78 ± 0.12
SH8 0.20 0.20 0.29 0.26 ± 0.01 490 ± 335 20.9 ± 8.6 85.8 ± 0.3 89.2 ± 0.4 0.38 ± 0.08

Fig. 4. SEM images of MGFs produced using different amounts of hydrogen peroxide ((a) y = 0.0; (b) y = 0.05; (c) y = 0.10; (d) y = 0.15. x = 0.20); the insets are a magnified view
of a cell and surrounding struts.

icant effect on the compressive strength of potassium-containing
geopolymers [25], but the specific influence of this factor in deter-
mining the strength evolution with oil content in our samples is
too complex to assess.
The SEM images of MGFS produced with different amounts of
hydrogen peroxide and the same amount of olive oil are compared
in Fig. 4, and the data concerning porosity and strength are reported
in Table 2 (see above).
We can note that, increasing the amount of hydrogen peroxide
while maintaining the same amount of olive oil, also had an effect
on the characteristics of the produced MGFs. When no hydrogen
peroxide was used, the foams had a low amount of total porosity
and, more importantly, contained only small cells/pores. Increasing
the amount of peroxide increased significantly the average cell size
as well as the total porosity, because of the higher amount of gas
generated by the decomposition of the peroxide, while the size of
the interconnecting pores in the struts was not strongly affected.
However, increasing the amount of peroxide slightly increased the
size of the cell windows from ∼16.5 (SH2) to 20.9 ␮m (SH8), leading
to a more permeable structure. Accordingly, the ratio of the open
porosity to the total porosity increased from ∼92 to ∼96%.
Foams with small cells and limited porosity had a strength about
10 times higher than that of samples possessing pores/cells of a
few hundred microns. Again, the effect of the amount of peroxide
on the mechanical strength is a complex combination of its influ-
ence of total porosity, cell size and dimension (and amount) of the
pores in the cell walls and struts. According to the minimum solid
area models proposed by Rice [29–31], when the other factors in a
porous material that may affect the mechanical strength of cellular
ceramics, such as the synthesis temperature or the pore character-
istics, are not dominant, the strength-porosity dependence can be
approximated by an exponential function:
 =  0 exp(−bp) (1)
where  is the strength at total porosity p,  0 is the value when p = 0
for the same composition, and b is an empirical constant depending
on the pore characteristics. The relation between the compression
4248 C. Bai et al. / Journal of the European Ceramic Society 36 (2016) 4243–4249
Fig. 5. Plot of compression strength vs. total porosity for MGFs produced using
different contents of H2 O2 and the same amount of olive oil (x = 0.20).
strength and the pore volume fraction for selected samples, fitted
using Eq. (1), is shown in Fig. 5.
In this study, the strength-porosity behavior of the MGFs spec-
imens could be estimated by the following equation:
 = 364404.58 exp(−15.11p)
with a correlation factor R2 = 0.957 (in the porosity range
62.0–89.2 vol%). Previous studies showed that the values of ␴0 and
b depend on the processing conditions and/or other parameters
[32].
These results demonstrate that the characteristics of MGFs can
be modified by adjusting the synthesis process by employing dif-
ferent types of oil and different contents of oil and H2 O2 , thereby
controlling their compressive strength, volume fraction of porosity,
cell and window cell sizes and distribution.
4. Conclusions
High strength and high porosity geopolymer foams with
varied pore morphology were fabricated by a combined gelcast-
ing/saponification/peroxide using H2 O2 and three different oils
(canola, sunflower and olive oil). The type of oil employed affected
only slightly the total amount of porosity, but more significantly
the compression strength of the samples, with olive oil providing
the best combination in terms of porosity and mechanical strength
values. The results depend on a complex effect of the type of surfac-
tant produced in situ by the saponification reaction, together with
a different rheology given by the presence of different oils.
Increasing the amount of oil decreased the total porosity and
cell size, because of the increase in viscosity in the system, while
the compression strength decreased because of the higher amount
of pores (deriving from the oil droplets) in the struts. The change
in composition of the geopolymer matrix with increasing oil con-
tent (lower K2 O/SiO2 ratio) could also be a contributing factor
to the variation in strength. With increasing H2 O2 content, the
total porosity increased, while the compression strength decreased,
because the minimum solid cross-sectional load bearing areas were
reduced.
Acknowledgements
Chengying Bai gratefully acknowledges the financial support of
the China Scholarship Council (CSC). The authors are grateful to
Dr. G. Ferrari, Crosfield Italia Srl (Montorio Veronese, VR, Italy) for
kindly providing the potassium silicate solution.
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