Cement and Concrete Research 100 (2017) 14–22

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Cement and Concrete Research

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

Hot-pressed geopolymer MARK

a,⁎ b a c
Navid Ranjbar , Mohammad Mehrali , Mahmoud R. Maheri , Mehdi Mehrali
a
Department of Civil Engineering, Shiraz University, 71345-1676 Shiraz, Iran
b
Process and Energy Department, Delft University of Technology, Leeghwaterstraat 39, 2628 CB Delft, The Netherlands
c
DTU Nanotech, Department of Micro- and Nanotechnology, Technical University of Denmark, 2800 Kgs. Lyngby, Denmark

A R T I C L E I N F O A B S T R A C T

Keywords: This research explores the use of simultaneous heating and pressing techniques in order to enhance the
Hot-pressing mechanical properties of fly ash (FA) based geopolymer under relatively low temperature conditions to ensure
D. Alkali activated cement minimum-porosity. Four effective parameters of pressing force, alkali activator/FA, duration of hot-pressing and
D. Fly ash sodium concentration are studied. Together with detailed experimental studies, our results reveal that the most
A. Acceleration
dominant factor is the induced pressure. The main results indicated that the highest compressive strength of the
B. Characterization
geopolymer (134 MPa) could be obtained by employing the hot pressing, temperature and duration of 41.4 MPa,
350 °C and 20 min, respectively. The microstructure of the hot-pressed specimens showed more developed
geopolymer matrix compared with conventional ones leading to higher compressive strength in much shortest
time. The improved mechanical properties are generally attributed to the dense structure of the material and
higher geopolymer gel production during the hot pressing process. However, further reaction of partially reacted
particles improves the mechanical properties over time.

1. Introduction geopolymerization and their consequent setting and mechanical proper-

ties such as the role of silicate, aluminate, sodium, water, and curing
Precast concrete construction has several advantages compared to temperatures [4,10–14]. Curing of the geopolymers is possible in a
the in situ concrete regarding quality, fast assembling, safety, and wide range of temperatures. However, most of the previous studies
reduction in manpower demand [1]. However, the importance of the have focused on the lower temperatures which are more applicable to
space availability and material supply according to work schedule is conventional construction. These conventional methods of curing are
highlighted more in precast construction since the concept of just-in- limited to the ambient and oven curing. It has been known that the
time construction is a key consideration [2]. In view of the fact that increase in curing temperature has a significant effect on kinetics of FA-
numerous precast members need to be fabricated in a short time, based geopolymers by increasing both dissolution and polycondensa-
satisfying the design code specifications and being able to withstand the tion rates at high temperature and the consequent fast setting of the
lifting loads, a fast curing method for concrete is required [3]. Among material [15,16]. However, rapid setting results in an increase in the
different curing methods of concrete, steam curing, electrical curing, pore volume, preventing the mixture from forming a compact structure;
and heat supply curing are classified as accelerated curing methods this mechanism leads to a decrease in the ultimate compressive strength
which are based on the increase of the curing temperature of the of the geopolymer. Whereas, if the geopolymer is cured at ambient
materials [4–6]. Steam curing is one of the most common methods in temperatures, the material gradually fills some of the pore fractions and
the fast development of the Portland cement-based composites, increas- thus forming a denser matrix [5,17]. Although the ultimate strength
ing the strength to about 70% of the ultimate strength in one day [3,7]. reduction is not preferable, the high early strength at elevated
This strength is almost enough for lifting, safe transportation, and fast temperatures (mostly 45–85 °C) makes the geopolymers suitable for
installation, however, this method of curing consumes a considerable precast construction [18]. To speed up the rate of hardening, micro-
amount of energy. wave curing has been used to provide a uniform and fast heating. This
Geopolymers are considered as alternatives to Portland cement due phenomenon is owed to the interaction between the polar molecules
to their superior properties of low carbon dioxide release, high early and microwave electric fields. Such a superfast efficient microwave
strength (at the present of heat) and elevated temperature resistance curing leads to the formation of a high strength geopolymer (100 MPa),
[8,9]. Several parameters have been studied to enhance the kinetics of which may be heated up to 1000 °C without cracking, failure or

⁎
Corresponding author.
E-mail addresses: n.ranjbar@shirazu.ac.ir, navid0ranjbar@gmail.com (N. Ranjbar).

http://dx.doi.org/10.1016/j.cemconres.2017.05.010
Received 28 October 2016; Received in revised form 22 April 2017; Accepted 9 May 2017
0008-8846/ © 2017 Elsevier Ltd. All rights reserved.
N. Ranjbar et al. Cement and Concrete Research 100 (2017) 14–22

vitrification [19,20]. Although this method of curing has promising 65 °C for 24 h and further cured at room temperature up to the time of
applications to geopolymers, this technology may have some drawbacks testing) as described in our previous study [22]. Noteworthy, to have a
in practice. A preferred method would be the use of already available workable mix some amount of water is needed to be used in the
equipment for precast construction. conventional method to have a final alkali activator mass ratio of
Herein, we demonstrate the construction of an integrated high sodium silicate:NaOH:H2O of 2.5:1.0:0.7. A summary of the specimen
strength and ultra-fast hardening FA-based geopolymer through hot- preparation is shown in Table 2.
pressing method. The geopolymer specimens are subjected to heat
treatment at a fixed temperature of 350 °C together with pressure. The 2.3. Analysis methods
effects of changes in curing pressure, curing duration, alkali activator/
FA and sodium concentration on the performance of hot pressed FA- X-ray fluorescence (XRF- PANalytical Axios mAX, Netherlands) was
based geopolymer are studied. The initial and long term compressive used to determine the oxide composition of the FA. The XRD patterns
strength, hardness and fracture toughness of this FA-based geopolymer were measured on an Empyrean PANALYTICAL diffractometer
are evaluated. To characterize the microstructure and kinetic of the (Netherlands) with monochromated Cu Kα radiation
reaction, thermogravimetric analysis (TGA), differential scanning ca- (λ = 1.54056 Å), operated at 45 kV and 40 mA with a step size of
lorimetry (DSC) analysis, X-ray diffraction analysis (XRD), Fourier 0.026° and a scanning rate of 0.1° s− 1 in the 2θ range of 5 to 80°. FTIR
transform infrared spectroscopy (FTIR), scanning electron microscopy spectroscopy was carried out using a Perkin Elmer System series 2000
(SEM) and density measurement are conducted. The strategy of using (USA) spectrophotometer in a frequency range of 4000–400 cm− 1 to
hot-pressing offers a new path to development of high performance and identify the functional group of the geopolymer specimens. DSC
integrated geopolymer composites. (Mettler DSC 820, Switzerland) was applied to evaluate the kinetics
of the geopolymer gel formation and hardening during the process of
2. Materials and methods hot pressing over a temperature range of 30 to 350 °C with a rate of
10 °C·min− 1. TGA was conducted using a STA 449 F3 Jupiter thermo-
2.1. Row materials characterization gravimetric analyzer (NETZSCH, Germany) device with a heating rate
of 10 °C·min− 1 from 30 °C to 350 °C. SEM-BSE images were taken using
In this study, a low calcium (class F) FA collected from Lafarge a Phenom ProX scanning electron microscope (Phenom-World Inc.,
Malayan Cement Bhd (Malaysia) was used to prepare the geopolymer Netherlands). The images were processed using multispectral analysis
paste. This FA was a waste product of coal power stations and consists to do a supervised classification of pores and geopolymer mixture made
of typical spherical particles. The chemical composition of the FA was on MultiSpec© (Purdue Research Foundation). The multispectral
analyzed by X-ray florescence (XRF) using a PANalytical Axios mAX images were analyzed by imageJ software to quantify the pore,
instrument as it is shown in Table 1. The median particle size and geopolymer gel, and unreacted particle fractions. Nanoindentation
specific gravity of the FA were indicated to be 12.19 μm and 2.18 g/ experiments were also performed using a nanomechanical test system
cm3, respectively. (Micro Materials Ltd. Wrexham, U.K.) employing Berkovich diamond
A mixture of sodium silicate and sodium hydroxide has been tip with a radius of 20 nm. The test was conducted using 100 mN in a
prepared with mass ratio of 2.5:1.0 to activate the aluminosilicate load-controlled mode with a dwell time of 10 s and indentation velocity
particles. The sodium silicate was used in liquid form with about 1.5 g of 3 nms− 1. To prepare the samples for nanoindentation test, the
water per milliliter at 20 °C with a SiO2/Na2O mass ratio of 2.5, geopolymer specimens were ground using a fine silicon carbide paper
obtained from PC Laboratory Reagent (West Malaysia). The NaOH (up to 2000 grit size) and polished to a mirror finish using diamond
pellets were provided by Merck (Germany). powders of different grades from 15 to 0.25 μm in an auto polisher
(laboforce-3, Struers, Denmark). The minimum of ten indentations were
2.2. Geopolymer specimen preparation using a hot press applied to determine an average value for each sample. Based on the
obtained load–displacement unloading curves, the Elastic modulus of
The geopolymer specimens were fabricated by mixing as-received each specimen was calculated using the Oliver–Pharr method [25]. The
FA with alkali activator for 5 min, poured into a steel pressing mold and reduced modulus (Er) is taken from the nanoindentation data and is
hot-pressed using a Mount Press and a mold heater (Buehler Ltd., USA). related to the sample's elastic modulus (Es). The following equation was
The heating temperature was fixed at 350 °C for all the specimens. This used to calculate the sample's elastic modulus (Es) [26]:
temperature was chosen due to the reported positive effects on 1 − ν s2 1 1 − ν 2i
mechanical properties of FA-based geopolymers [16,21]. Following = −
Es Er Ei (1)
the hot-pressing treatment, the heater was removed and the mold
cooled down by a cooler in 5 min. Finally, the specimens were removed where the elastic modulus (Ei) and Poisson's ratio (νi) of the indenter
and kept in an ambient environment until the testing time. Four sets of are 1140 GPa and 0.07, respectively. The Poisson ratio of the sample
specimens are prepared to evaluate the influence of induced pressure (νs) is taken to be 0.2 since the effect of variation in Poisson's ratio in
(13.8 to 41.4 MPa), hot pressing duration (15, 20, 25 and 30 min), the range 0.18–0.22 has been reported to be insignificant for similar
alkali activator/FA mass ratio (0.25, 0.30, 0.35 and 0.40) and sodium systems [27–30].
concentration (8 to 16 M) on the compressive strength and micro- The fracture toughness was determined by the following equation
structure performance of the hot-pressed FA-based geopolymer. To [31].
evaluate the effects of hot pressing, the characteristics of hot-pressed
⎛ E ⎞1 2 ⎛ P ⎞
geopolymers are compared with those of the corresponding geopoly- KIC = 0.016 ⎜, ⎟ ⎜ 2 3 ⎟
⎝ H⎠ ⎝C ⎠ (2)
mers prepared by the same materials employing a typical curing
1/2
method (after mixing and vibration, the specimens were placed at where, KIC is the indentation toughness (MPa m ) signifying fracture

Table 1
Chemical composition of FA.

Composition SiO2 Al2O3 Fe2O3 K2O TiO2 CaO SO3 MgO P2O5 Na2O ZrO2 MnO LOI

FA (%) 75.76 15.86 3.90 1.14 0.97 0.95 0.35 0.26 0.21 0.16 0.13 0.06 6.8

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N. Ranjbar et al. Cement and Concrete Research 100 (2017) 14–22

Table 2
Summary of specimen preparation variables.

Set specimens Hot pressing variables

Pressure (Mpa) Duration (min) Alkali actovator/fly ash (%) NaOH molarity (M) Heating temperature (°C)

Set 1 Induced pressure 13.8 to 41.4 20 35 16 350

Set 2 Hot press duration 41.4 15–30 35 16 350
Set 3 Alkali activator/fly ash 41.4 20 25–40 16 350
Set 4 Sodium concentration 41.4 20 35 8–16 350
Conventional method – 1440 50a 16 65

a
Water/FA = 10%.

resistant, 0.016 is a material-independent constant for Vickers radial This liquid is mostly comprised of water (in steam form) since it has
crack, E is the elastic modulus of the geopolymer specimens (GPa) from lower boiling temperature compared with those of sodium hydroxide
the nanoindentation of 10 experiments, H is the Vickers hardness (GPa) and sodium silicate. About 80% of water evaporates below 200 °C
of the ceramic material, which is a measure of the resistance to however, it continues to evaporate until approximately 350 °C, at which
deformation, P is the indentation load (N), and C (m) is the half-length the bulk of the free water has been liberated. This dehydration period
of the radial cracks on the surface after indentation. can be extended when fast heat rates are applied [9]. The water
Brittleness is one of the most important mechanical properties since expulsion causes a reduction in volume and consequently a loss of
brittle material fails by fracture at only slightly beyond the yield stress pressure (Fig. 1c). To make a condensed matrix, pressure is increased to
and releases a considerable amount of accumulated energy [32]. the initial level continuously. As a result of the hot pressing, the
Similar to other cementitious materials, unreinforced geopolymers conversion of solid particles to geopolymer gel is accelerated by the
often show brittle failure [33]. Since geopolymers have more potential formation of dissolved species that cross-link to form oligomers, which
for prefabrication industries, the brittleness index (BI) as a quantitative in turn produce sodium silicoaluminate gel. Such a reaction is an
evaluation of the machinability becomes an important parameter. BI endothermic event that can be observed in DSC thermograms of Fig. 2a
has been determined by the following equation [34]: and b. This step leads to another pressure loss since the air which is
trapped within the spherical particles is removed, resulting in a
H
BI = reduction in volume (Fig. 1d). Subsequent increasing of pressure to
KIC (3)
initial condition causes a condensed matrix with the proper shape of the
In the present study, the average values of H and KIC were used for mold (Fig. 1e). Beyond this step, the system becomes thermodynami-
BI calculation. cally stable and the matrix becomes hardened due to the polycondensa-
Compressive strength tests were carried out by ELE International tion and the formation of a three-dimensional aluminosilicate network
Auto Compressive Test Machine (UK) on cylindrical specimens of at the hot pressing condition; therefore, no more pressure loss is
31.5 × 31.5 mm at a pacing rate of 0.7 kN·s− 1. The specimens were observed. Subsequently, the hardened geopolymer is cooled under the
tested immediately after preparation. However, some samples were initial pressing condition and finally, the pressure is removed from the
tested after 1, 7, 28 and 100 days to determine the specimen strength cooled geopolymer specimen. An amorphous to semi-crystalline geo-
development over time. The apparent density was obtained by dividing polymer is therefore formed and the specimen is now ready to sustain
the specimen's mass by the volume it occupies. load (Fig. 1f).

3. Results and discussion

3.2. X-ray diffraction analysis
3.1. Mechanism of hot pressing
The FA efficacy in geopolymerisation is strongly influenced by the
Fig.1 shows a schematic image of the hot pressing mechanism. In total glassy fraction and their rate of transformation into the alumino-
this method, workability of the fresh matrix is not considered since the silicate gel. The availability of vitreous material controls the geopoly-
pressure is used to shape the specimens. Hence, the appearance of the merisation in which the continuation of the reactions, gel production
fresh matrix is quite similar to a wet ash with a large volume of trapped and the consequence strength development of each stage, depends on
air. First, the matrix is poured into the mold (Fig. 1a). A pressure is then this fraction [37]. Fig. 3 compares the mineralogy composition of the
applied to remove the unwanted large volume of air to produce a as-received FA and the corresponding geopolymers cured by different
condensed matrix (Fig. 1b). At the next stage, the condensed matrix is methods including the proposed hot press method and the conventional
subjected to a 350 °C to accelerate the gel formation. Simultaneous oven curing at 65 °C [22]. The XRD patterns show that irrespective of
thermogravimetric and differential scanning calorimetry analyses were the curing method, geopolymers have an amorphous to semi-crystalline
performed on the fresh geopolymer matrix to characterize the mechan- structure with crystalline phases of quartz and mullite originating from
ism as is shown in Fig. 2. During the heating period, the geopolymer- undissolvable FA particles. The broad hump which is located between
ization could be partitioned into approximately three steps of; extra 2θ = 17° and 35° in the patterns is produced by diffuse scattering of the
water expulsion, dissolution–hydrolysis and hydrolysis–polycondensa- amorphous material. This hump is associated to glassy phases in FA
tion. However, these three steps probably occur simultaneously during pattern. While, in geopolymer specimens, the similar hump represents
the heat treatment. the remaining glassy portions of unreacted particles that partially
Once the temperature of the matrix is increased, the pressure of the overlapped with sodium aluminosilicate products [38,39]. The amor-
system increases leading to a decrement of the viscosity in the liquid phous aluminosilicate products are comprised of tetrahedra aluminosi-
phase [35]. As a result, the liquid phases distribute homogeneously licate units (formed through the dissolution of FA particles by the alkali
through the matrix in a short period while aluminate and silicate activators), self-polymerizing species such as monomers and oligomers
monomers are released by alkali attack on solid aluminosilicate sources. (produced when the soluble silicate catalyses the polymerization), and
The reaction is accelerated significantly with temperature increment polymerization between silicate oligomers and/or between AlO4− and
[14,36]. The high pressure of the system forces the extra liquid out. silicate oligomers [40].

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N. Ranjbar et al. Cement and Concrete Research 100 (2017) 14–22

Fig. 1. Schematic mechanism of geopolymerization under hot pressing.

3.3. Fourier transform infrared spectroscopy chain along with the amount of bridging oxygen or the silicate
tetrahedral where the four oxygen atoms are bridging (SiQ4) that
IR spectra of hot pressed geopolymers with different sodium manifests itself as recrystallization of amorphous phase to quartz
concentration are compared with that of the conventionally cured mineral as it has Q4 structure [47]. Unlike conventional geopolymer,
specimen at 65 °C in Fig. 4. The IR spectra of the geopolymers appear to another structural reorganization of FA is observed in hot pressed
be similar to FA. This implies that most vibrant forms of the FA specimens by reduction of the absorption band at about 790 cm− 1
molecular chains are retained in the geopolymerization products. The (AlO4 vibrations) [45] and the appearance of new band at 560 cm− 1
most characteristic difference observed between the FTIR spectrums of assigned to the symmetric stretching vibrations of AleOeSi [48], which
FA and that of conventional geopolymer is associated with the broad- is concerned as the formation of amorphous to semi-crystalline
band at about 1060 cm− 1(asymmetric stretching vibrations of SieOeSi aluminosilicate products [45,49]. The band at about 2300 cm− 1, of
and AleOeSi) which is shifted to lower frequencies of about 995 cm− 1 either FA or geopolymer spectrums, is assigned to stretching vibration
in the spectra of the geopolymer. This shift shows the dissolution of the OH and HeOeH due to the presence of weak H2O bonds that are
FA amorphous phase in alkali activators and formation the amorphous absorbed into the surface or are trapped among the particles of the
aluminosilicate gel phase [42–46]. However, this band is returned to a materials [33,50]. However, new bands appeared at 1645 cm− 1 and
higher frequency, ~1045 cm− 1, in FTIR spectrums of hot pressed 3735 cm− 1 in all geopolymers which are attributed to HeOeH bending
specimens. This shift is assigned to the increase in length of silicate vibration eOH stretching vibration. These changes are because of the

Fig. 2. TGA and DSC analysis of fly ash based geopolymerization over a) temperature b) time.

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N. Ranjbar et al. Cement and Concrete Research 100 (2017) 14–22

Fig. 5. The effect of hot press on 20 min compressive strength and the nominal density of
the FA based geopolymer specimens.
Fig. 3. XRD patterns of the FA based geopolymer cured by the hot press and the
conventional oven curing method.
subjected to higher pressures, the air bubbles which are trapped in
the matrix are removed resulting in an increase in density. It is known
location of water molecules in aluminosilicate network formation in a that when a brittle cementitious material is subjected to compression,
geopolymer structure [15]. Moreover, an atmospheric carbonation was axial splitting micro-cracks are formed parallel to the direction of the
observed in all the geopolymer specimens, which was shown in the compressive load, where inelastic volume dilatancy are dominant. This
infrared spectral region of 1410–1500 cm− 1 as the stretching vibration is attributed to a high deviatoric stress; such stress is more critical in
O-C-O [46]. This is due to the presence of sodium carbonate in the porous matrices where the effective cross section is lower [52]. There-
geopolymers [51]. fore, reduction in pore volume enhances the strength property of the
material. However, further pressure, over 27.6, has a minimal effect on
3.4. Mechanical properties compressive strength development since the free pore fraction of the
material is almost removed when it is subjected to 27.6 MPa load and
The compressive strength of hot-pressed geopolymer specimens is the remaining pore fractions are those trapped in hollow spheres which
influenced by pressing force, FA/alkali activator, duration of hot are harder to remove.
pressing and sodium concentration. Among these parameters, pressure Fig. 6 presents the load-penetration depth from nanoindentation
force has the most influence on the compressive strength of the matrix. experiments to identify the effect of induced pressure on material
As observed in Fig. 5, increasing the hot pressure force from 13.8 to stiffness and Table 3 compares the corresponding calculated values. The
27.6 MPa leads to strength improvement from about 84 MPa to micro hardness, elastic modulus and fracture toughness are highly
133 MPa (20 min compressive strength). This is attributed to the relevant to the induced pressure and the consequent porous structure of
porosity of specimens. When the fresh geopolymer matrices are the material. Increasing the pore volume changes the failure mechan-

Fig. 4. FTIR spectra of the FA and geopolymers cured conventionally and by hot pressing conditions.

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N. Ranjbar et al. Cement and Concrete Research 100 (2017) 14–22

Fig. 6. a) The load-penetration curve from nanoindentation, the surface of material b) before and c) after the indentation.

Table 3 machinability of ceramics as the lower the brittleness index, the higher
Influence of pressing force on elastic modulus, microhardness, fracture toughness and the machinability of the material. A good machinability occurs when
brittleness index.
the brittleness index of the ceramic is lower than 4.3 μm− 0.5 [56].
Pressing Elastic Microhardness Fracture Brittleness Although this value does not follow a particular trend when the
(MPa) modulus (GPa) toughness (MPa index geopolymer is subjected to different pressure, it varies between about
(GPa) m1/2) 1.57 to 1.7 μm− 0.5. Such a low brittle index increases the efficiency of
the material when the application is optimized based on the cutting
13.8 36 ± 4.5 1.10 ± 0.05 0.70 ± 0.04 1.57
20.7 43 ± 4.3 1.26 ± 0.08 0.74 ± 0.02 1.70
energy.
27.6 50 ± 3.8 1.43 ± 0.04 0.90 ± 0.02 1.59 Fig. 7 shows the SEM images of the polished hot pressed geopolymer
34.5 56 ± 3.0 1.64 ± 0.05 1.04 ± 0.03 1.58 specimens subjected to different pressures during their curing process.
41.4 68 ± 3.2 1.93 ± 0.08 1.15 ± 0.02 1.68 Fig. 7a and b indicate an obvious reduction in pore size and pore
volume of geopolymers when subjected to 17.4 MPa pressure compared
with 5.8 MPa pressure. To determine a quantitative measurement of
ism to a local layer crashing of composites under compression since it
different volume fractions (including unreacted particles, pores and
facilitates the formation of microcracks. Therefore, porous specimens
geopolymer solid phases), multi-label thresholding of several high-
are more prone to the reduction of fracture toughness and elastic
resolution SEM images was applied based on the known microstructural
modulus [53–55].
features of FA particles and the FA-based geopolymer, as in Fig. 7c to e.
Brittleness index can be used as a quantitative assessment of the
The increase in the induced pressure not only leads to a reduction of the

Fig. 7. FESEM images and image processing of the hot-pressed geopolymers of different initial applied pressures; microstructure of hot-pressed geopolymer with a) 13.8 MPa b) 41.4 MPa,
BSE of material c) before and d) after image analysis e) phase fraction variation of hot-pressed geopolymer with different curing pressure, e) pore structure of FA based geopolymer.

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N. Ranjbar et al. Cement and Concrete Research 100 (2017) 14–22

Fig. 8. a) The effect of alkali activators/FA and hot pressing duration on compressive strength of the FA based geopolymer specimens, b) schematic cross section of the hot pressing
mechanism for different alkali activator content.

Fig. 10. The compressive strength of the FA-based geopolymer specimens using a hot
press over 100 days.
Fig. 9. Influence of sodium concentration of compressive strength of hot press cured FA-
based geopolymer. phase. It appears that when the liquid phase is low, some FA particles
remain intact and formation of a uniform geopolymer matrix becomes
pore volume but also to an increase in geopolymer/unreacted particle less possible (Fig. 8b). As a result, the strength of the matrix is reduced.
ratio. In other words, the increased strength of the higher induced Furthermore, it is found that the optimum heating period for hot
pressure is not only attributed to the dense structure but also to the pressing at 350 °C is 20 min while, further heating has an adverse effect
higher geopolymer gel formation. As observed in Fig. 7e, some portion on the mechanical strength of the material.
of the pore volume is inevitable due to the unreactive hollow particles As it was observed in TGA analysis (Fig. 2b), the specimen under-
(trapped pore) while some others (free pore) are removable when the goes slight weight loss after about 20 min. This is attributed to the
fresh geopolymer is subjected to a higher pressure. These two types of Na2O–Al2O3–SiO2–H2O amorphous phase(s) which is susceptible to
pore fractions are shown in Fig. 7f. crystallization. Therefore, this reduction in strength is related to the
As observed in Fig. 8a, for a constant pressure of 41.4 MPa, alkali appearance of small pockets of crystalline phase(s) in the mixture with
activator/FA of 0.35 shows higher strength together with higher prolonged curing [57]. This behavior is similar to that of the conven-
thermal stability at different processing durations. This variation of tional method in which keeping the matrix under higher temperatures
strength is attributed to the liquid phase content of the matrix. As it was for long periods adversely affects the mechanical properties of material
mentioned earlier, when the matrix is subjected to hot pressure, it is [5,58].
transformed to a gel form with a reduced volume. Further application of Fig. 9 indicates that the increase in the sodium concentration of the
pressure in the hot condition removes the liquid phase consisting of the matrices from 8 to 16 M, slightly enhances the mechanical properties of
reactive components of geopolymerization. As a result, the compressive the geopolymer specimens (about 5%). This is reasonable since the
strength of specimen with alkali activator/FA of 40% is reduced. This dissolution of the FA is higher due to the higher OH– concentration in
phenomenon was not observed in the specimens with a lower liquid high molarities [59]. However, the role of sodium in the hot-pressed

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N. Ranjbar et al. Cement and Concrete Research 100 (2017) 14–22

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strength and microstructural analysis of fly ash/palm oil fuel ash based geopolymer
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