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PII: S0959-6526(20)31166-5
DOI: https://doi.org/10.1016/j.jclepro.2020.121119
Reference: JCLP 121119
Please cite this article as: Jingming Cai, Xiaopeng Li, Jiawei Tan, Brecht Vandevyvere, Fly ash-
based geopolymer with self-heating capacity for accelerated curing, Journal of Cleaner Production
(2020), https://doi.org/10.1016/j.jclepro.2020.121119
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accelerated curing
USA
Abstract:
Geopolymers has gained increasing attentions in recent decades because of its
potential for CO2 emission reductions. In order to further increase the curing efficiency
and save energy, the self-electrical heating fly ash based geopolymer was developed in
this paper. In this work, carbon black and steel fibers were added into the fly ash based
geopolymer to increase its electrical property. The feasibility of curing fly ash based
behaviours of geopolymer specimens. The results showed that the maximum surface
The three-point bending test results showed that the flexural strength for specimen
significantly increased after self-electrical heating. With the proper addition of carbon
black and steel fiber, the fly ash based geopolymer specimen cured after electrical
heating possesses a denser micro-structure and therefore exhibits higher strength and
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better ductility. Besides, self-electrical heating method can significantly increase the
eco-efficiency of geopolymer.
bending test
Highlights
The feasibility of developing self-electrical heating fly ash based geopolymer was
discussed.
tested.
The three-point bending test for geopolymer specimens after electric-heating were
conducted.
1. Introduction
2013). As such, sustainable alternatives need fewer natural resources and emit less
carbon dioxide (Kajaste and Hurme, 2016) has gained increasing attentions during the
near decades. One feasible approach is to replace OPC with geopolymers made of
industrial by-product materials such as granulated blast furnace slag (GBFS) (Crossin,
2015), fly ash (Nuaklong et al., 2016) and construction and demolition waste (CDW)
than normal cement, its industry applications are significantly restricted by its curing
conditions (Puertas et al., 2000). Firstly, curing temperature would dramatically affect
activation barrier during the geopolymerization process (Bakharev, 2005). Fly ash
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Bakria et al., 2011) while the compressive strength growth for those cured at ambient
temperature (about 20 ºC) is negligible. Low curing temperature would lead to the low
chemical activity of fly ash and thus result in a slow geopolymerization processes (Assi
et al., 2016). Secondly, it may be very difficult to cure fly ash-based geopolymer by
using ovens at the construction site due to the size of the geopolymer elements. As a
result, precast technology which is capable of providing thermal curing seems to be the
only solution, which, to some degree, restrict the development of geopolymer. Thirdly,
in electrical oven, the heating process for geopolymer specimen initiates from the
exterior to the interior, which leads to a non-uniform temperature distribution inside the
powders (e.g. slag) into the matrix (Cheah and Samsudin, 2017). However, the setting
time and workability geopolymer would rapidly decrease with the addition of slag
(Nath and Sarker, 2014). Moreover, and fast hardening or flash setting would occur
with the addition of steel fiber and carbon black. The addition of steel fiber and carbon
black could increase the conductivity of geopolymer, then the geopolymer specimen
would be capable of generating heat from interior to exterior while being energized.
The generated heat could evenly heat the geopolymer specimen, which enables the
specimen to be cured by itself rather than the heating equipment. Meanwhile, the steel
fiber added into the matrix can positively increase the ductility of geopolymer specimen
Totally fourteen fly ash based geopolymer beam specimens with different dosages
of steel fiber and carbon black were casted. The effects of curing temperature on the
2. Experimental procedure
Low calcium (Class F) fly ash, steel fiber and carbon black were used as raw
materials in this paper. The chemical composition of fly ash described in Table 1 shows
that the content of calcium is as low as 3.71%, indicating that an extra high temperature
curing for geopolymer samples is essential. The specific surface area of the fly ash used
in this paper is about 350 m2/kg. For fly ash based geopolymer, the content of calcium
can significantly affect its geopolymerization processes as the calcium ions are capable
morphology of carbon black (Shanghai Kajet Chemical Technology co. LTD) is shown
in Fig.1(a). The electric resistance of carbon black is lower than 1 Ω·m. Steel fibers
used in this experiment is 25.4 mm long and the macro morphology of steel fiber is
shown in Fig.1(b). Detailed physical properties of steel fiber are shown in Table 2.
and KOH activator solutions was applied to prepare the alkali activator. The KOH
solution, with the alkali concentration of 12 mol/L, was prepared by dissolving KOH
flakes (98% of purity) in water. Both Na2SiO3 and KOH activator solutions were mixed
together for 24 hours prior to being mixed with solid mixture. A constant liquid to
binder ratio of 0.5 and the Na2SiO3/KOH ratio of 1.5 were adopted in this paper. A high
of 1.5% by weight was used in the mixing of geopolymer to maintain good flowability.
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Fly ash 3.71 50.86 28.16 6.24 1.28 0.67 0.85 1.27
All the specimens have the same matrix but different dosages of carbon black and steel
fiber. The nomenclature of each specimen can indicate its composition. For example,
specimen G-4-2 indicates the dosage for carbon black and steel fiber are 4% and 2% by
volume, respectively.
Two geopolymer specimens were casted for each mixture, one was applied in the
electric heating test while another one was cured under ambient conditions (20 ± 5ºC,
with humidity of 50% ± 10%). The dimension of geopolymer specimens was designed
The binder materials, including fly ash, carbon black and steel fiber were firstly mixed
for 1 minute before being blended with alkaline activator and water-reducer for about
5 minutes. After the mixing procedure, the fresh geopolymer was poured into the plastic
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molds and all specimens were cured in the molds for 24 hours in the natural atmosphere
G-0-0 0 0
G-0-2 0 2
G-2-0 2 0
G-4-0 4 0
G-6-0 6 0
G-4-2 4 2
G-6-2 6 2
geopolymerization process of fly ash based geopolymer, the calorimetry test with
different the curing temperature (15℃, 25℃, 50℃ and 70℃) was conducted for
specimen G-0-0. The eight channel TAM Air isothermal calorimeter with the operating
preweighted fly ash and alkaline activator were firstly stored in the glass ampoule and
plastic injector, respectively. The glass ampoule and plastic injector were then placed
in the calorimeter for 6 hours. After achieving the thermal equilibrium condition, the
alkaline activator was injected into the glass ampoule and the mini stirrer for a 5-minute
mixing. During the geopolymerization processes, the heat flow was automatically
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The test set-up for electric-heating experiment is shown in Fig.3. The copper
sheets were pasted on the both ends of electric-heating specimen, and then connected
to a power supply (Gaaten Electronic Technology co. LTD, China) with the voltage of
110V. The silver paste was glued between copper sheets and geopolymer specimen to
increase the electric conductivity. In order to measure the electric current during the
test, a multimeter (F8808A, Fluke Cooperation, China) was connected with the copper
sheets. As can be seen in Fig.4, the temperature sensor was attached on the surface of
the specimen to record the temperature variation during the experiments. After
electrification, the specimen was uniformly heated. It is hypothesized that the local
temperature variation of the temperature sensor could reflect the temperature change of
as well as the control geopolymer specimens were cured under ambient curing
conditions for another 7 days. The electro-hydraulic servo testing machine with a
capacity of 100 kN was applied to conduct the three-point bending test and the
displacement rate was set as 0.001 mm/s. After the bending test, the microstructures of
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(a) (b)
The calorimetry test has been proven to be an effective way to reflect the
and Vollpracht, 2018; Zhang et al., 2014), since the geopolymerization process was
accompanied with exothermic changes. The heat release rate and cumulative heat of fly
ash based geopolymer at different curing temperature are shown in Fig.5. It can be seen
that both heat flow peak and cumulative heat increased with the curing temperature,
indicating the geopolymerization process was accelerated and more geopolymer gel
was formed while being cured at a higher curing temperature. For instance, the heat
flow peak was about 7.3 mW/g at the curing temperature of 70℃, while the heat flow
peak was about only 1.8 mW/g when the temperature was 50℃. While when the curing
temperature was 25℃ or 15℃, the corresponding heat flow peak was kept lower than
0.5 mW/g. Similar results can be observed from the cumulative heat shown in Fig.5(b).
Clearly, fly ash based geopolymer released more heat when cured at higher temperature.
For example, the cumulative released heat for geopolymer at 70℃ was about 11.7 J/g
after 12 hours, while the value for geopolymer at 15℃ was about 0.8 J/g. This seems to
Based on the calorimeter test results, the curing temperature can be concluded to
have a significant effect on the geopolymerization process of fly ash based geopolymer.
An initial high temperature curing is very essential for fly ash based geopolymer. The
geopolymerization process for fly ash based geopolymer is very complex and can be
simplified as three steps (Komnitsas et al., 2007). As shown in Fig.6, the first step is
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shown in Eq.2. After the polycondensation process shown in Eq.3, the hydrated
products as well as geopolymer gel will be formed in the matrix (Provis, 2014). It is
the calcium content is very low, as shown in Table 1. The first step in the
geopolymerization process is the most critical step, in which high temperature curing
is conducive to the dissolve of alumina and silica in alkaline solution (Palomo, 2015).
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Cumulative heat(J/g)
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Heat flow (mW/g)
10
6
5 8
70℃
4 50℃ 6
3 25℃
15℃ 4
2
2
1
0 0
0 2 4 6 8 10 12 0 1 2 3 4 5 6 7 8 9 10 11 12
Time (h) Time (h)
geopolymer
According to the calorimeter test, the elevated temperature curing was found to be
essential for fly ash based geopolymer. With the proper addition of conductive materials,
the geopolymer specimen would be self-heating after electrification due to the thermal
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effect of electric current. In this case, the geopolymer specimen itself can be regarded
as an electric heater. All the geopolymer specimens were electric-heated for two hours
and the surface temperature were recorded automatically by the temperature sensors.
During the electric-heating stage, the surface temperature for different geopolymer
For specimen G-0-0, the surface temperature was constant as 25℃ during the
electric-heating stage. It can be inferred that the electrical resistivity for specimen G-
0-0 was too high, since there is no conductive materials, i.e., steel fiber and carbon
black, in the geopolymer matrix. Even though it has been reported that the electrical
resistivity of geopolymer is much lower than that of normal cement (Payakaniti et al.,
For geopolymer specimens G-2-0, G-4-0 and G-6-0 with different pure carbon
black dosages, the surface temperature increased with the increase of carbon black
dosage, showing that carbon black can effectively increase the electrical conductivity
of geopolymer. For cementitious materials, it has also been reported that the electrical
resistance will decrease dramatically with the addition of carbon black (Monteiro et al.,
2017a; Monteiro et al., 2017b). However, as can be seen in Fig.7(a), the maximum
surface temperature for specimen G-6-0 was only 33 ℃. According to the calorimeter
test shown in Fig.4, a curing temperature of 33 ℃ may be not high enough in terms of
facilitating the geopolymerization process. It was also noticed that the surface
the electrical resistance became higher due to the electric polarization effects (Wen and
Chung, 2001).Similarly, for geopolymer specimen G-0-2 which contains 2% pure steel
fiber by volume, the maximum surface temperature was about only 28 ℃, indicating
the single addition of steel fiber was not feasible to make geopolymer conductive
enough to be self-curing .
Bentz, 1999), both carbon black and steel fiber were added in geopolymer matrix
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(specimen G-6-2 and specimen G-4-2) in this study. As can be seen in Fig.7(a), the
surface temperature for specimen G-6-2rapidly increased during the first 30 minutes
and it reached 67 ℃ after 30-min heating. Calorimeter tests infer that the
conventional oven curing method, the geopolymer specimen was much more uniformly
cured from. The steel fiber as well as carbon black particles can be regarded as electrical
heaters embedded in the geopolymer matrix, which will generate heat and thus further
increase the geopolymerization process. After reaching its peak value, the surface
temperature for specimen G-6-2 gradually decreased due to the electric polarization
effect, but it maintained higher than 50℃ at the end of electric-heating stage.
The electric powers of different specimens are shown in Fig.7(b). The voltage kept
constant as 110V during the experiment and the electric current was automatically
recorded by the multimeter. It can be seen that the electric power for all geopolymer
demonstrates that the electrical resistance increased due to the polarization effects. As
can be seen in Fig.7(b), for those geopolymer specimens with single addition of steel
fiber or carbon black, the electric power is much lower than geopolymer specimens
containing both steel fiber and carbon black. For example, the electric power for
specimen G-6-2 is as high as 62 W during the initial stage, which is about 2 times higher
than specimen G-6-0. It can be concluded that the combined addition of fly ash and
steel fiber is more effective in terms of improving the conductive behavior of fly ash
based geopolymer.
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70 60
40
50
G-0-0 G-0-2 30
40 G-2-0 G-4-0 G-0-0 G-0-2
G-6-0 G-4-2 20 G-2-0 G-4-0
G-6-2 G-6-0 G-4-2
30 10 G-6-2
20 0
0 30 60 90 120 0 30 60 90 120
Time(minute) Time(minute)
The possible reasons for this phenomenon are illustrated in Fig.8. For geopolymer
matrix with the single addition of carbon black shown in Fig.8(a), the carbon black
contact length for each carbon black particle hinders the conductive network formation.
Thus, the electric conductivity of the system is very low due to the very fact that no
conductive network existing in the matrix. For those geopolymer matrixes with the
single addition of steel fiber, as shown in Fig.8(b), the steel fiber can be regarded as
conductive network is hard to be constructed due to the poor dispersibility of steel fiber.
The electrical resistance would dramatically increase while steel fibers disconnecting
with each other. In this experiment, the maximum content of steel fiber was set as 2%
mixtures containing both carbon black and steel fiber, as can be seen in Fig.8(c), the
zero and one-dimension conductive material have an effective synergistic effect, which
facilitate the formation of conductive network in this matrix. Thus, the electrical
resistance would dramatically decrease with the addition of both carbon black and steel
fiber.
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Fig.8. The schematic diagram for (a) carbon black geopolymer (b) steel fiber
reinforced geopolymer (c) carbon black and steel fiber reinforced geopolymer
electric-heating) were cured in the natural atmosphere for another 7 days after the
electric-heating test. Then, the thee-point bending tests were conducted for all
geopolymer specimens. The test setup and specimen installation are shown in Fig.9.The
load-displacement curves for all specimens are shown in Fig.10, where the suffix “H”
in each specimen indicates the electrical-heated specimen. The flexural strength results
1200
Load(N)
G-6-2-H
600 G-0-0 G-4-0
G-4-0-H 1000
G-0-0-H 400 G-6-0
G-0-2 800
400 G-6-0-H
G-0-2-H 600
200 400
200
200
0 0 0
0.0 0.1 0.2 0.3 0.4 0.5 0.6 0.00 0.05 0.10 0.15 0.20 0.25 0.0 0.1 0.2 0.3 0.4 0.5 0.6
Displacement(mm) Displacement(mm) Displacement(mm)
fiber (b) carbon black (c) both steel fiber and carbon black
2000
Ambient curing
Electric-heating curing 1729
Flexural strength(N)
1500 1439
1000 936
875
780 823 781 808
721
663 702 707
610 576
500
0
G-0-0 G-0-2 G-2-0 G-4-0 G-6-0 G-4-2 G-6-2
Sample ID
mixture containing single steel fiber (G-0-2) are shown in Fig.10(a). The load-
displacement curve for specimen G-0-0 was very similar with those curves for normal
cement or concrete. With electrical heating, however, the specimen G-0-0-H showed
identical flexural behavior with specimen G-0-0, which can be attributed to the over-
high electrical resistance for specimen G-0-0. With the addition of steel fiber, the
specimen G-0-2 exhibits both higher peak load and ductility during the post-peak stage,
indicating the addition of steel fiber is an effective way to reduce the brittleness of
geopolymer (Mucsi., 2018). With being heated for 2 hours, the specimen G-0-2-H
achieved similar flexural strength with specimen G-0-2, once again demonstrates that
the geopolymer is still not conductive enough with the single addition of steel fiber.
Fig.10(b), it is noticed that all the specimen was very brittle as the load suddenly
dropped in the experiments. The flexural strength gradually decreased with the carbon
black dosage increasing from 0% to 6%. For example, the flexural strength for
specimen G-6-0 is 27% lower than that of specimen G-0-0, which may be attributed to
the reason that the addition of carbon black introduces more interfaces and flaws into
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the matrix.
And the interfaces and flaws would make the geopolymer specimen more porous and
easier to crack. After being heated for 2 hours, the carbon black geopolymer specimens
are still very brittle while the flexural strength gradually increased with the carbon black
dosage. For example, the flexural strength for specimen G-6-0-H is about 35.6% times
higher than that for specimen G-6-0, showing that the addition of carbon black
The flexural behaviors of geopolymers containing both carbon black and steel
fiber are shown in Fig.10(c). For specimens G-4-2 and G-6-2, the displacement
corresponding to the peak load dramatically increased due to the bridge-effect of steel
fibers inside the geopolymer matrix. The flexural strength for G-4-2 and G-6-2
significantly increased after 2-hours electrical heating. As can be seen in Fig.11, the
flexural strength of specimens G-4-2-H and G-6-2-H is 78.1% and 144.6% higher than
that of specimens G-4-2 and G-6-2, respectively. The typical microstructures for
specimen G-6-2 and G-6-2-H are shown in Fig.12. For specimen G-6-2, numerous
unreacted fly ash particles can be observed, as shown in Fig.12(a). This is reasonable
since the chemical activity for fly ash based geopolymer cured in ambient conditions is
relatively lower. With proper electrical heating for 2 hours, as can be seen in Fig.12(b),
more fly ash particles were dissolved in the alkali activator and more silica-alumina
gels were formed in the matrix, thus the specimen was more dense and rigid after the
electrical heating.
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It can be concluded that with the proper addition of steel fiber and carbon black,
could possess higher strength and better ductility with electric heating. In this case, steel
fibers in the geopolymer matrix play two roles. On the one hand, the bridge-effect of
steel fiber increased the ductility of geopolymer. On the other hand, the steel fiber can
be regarded as resistance heating wire after electrification . It should also be noted that
the heating process is quite different from normal curing methods such like electrical
heating oven, the temperature field of the former uniformly distributes rather than
In this paper, the feasibility of curing fly ash based geopolymer by using self-
electrical heating method was investigated. As has been mentioned above, high
generated in geopolymer producing process and thus greatly reduces the environmental
of increasing the strength of geopolymer samples. In order to further study the eco-
experiment. Steel fibers and carbon black were added into the samples and the
percentage were consistent with that of specimen G-6-2. An electric oven was used for
curing samples and the temperature inside the oven ranged from 40 ºC to 80 ºC. All the
samples were cured in the oven for 2 hours before being cured under ambient conditions
(20±5ºC, with humidity of 50% ±10%) for another 7 days. Fig.13 describes the
2000
Flexural strength (N)
1500
1000
500
0
40 50 60 70 80
Oven curing temperature( oC )
Fig.13 Compressive strength of samples under different curing conditions
Previous studies proposed a method of using a relevant indicator to define the eco-
efficiency of binder materials (Damineli and Kemeid, 2010). In this study, the following
CO2 intensity (𝐶𝑖) taking into account the relationship between the flexural strength of
geopolymer and CO2 emissions was adapted to compare the eco-efficiency of different
curing method.
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𝐶𝑖 = 𝐶𝑑/𝑓
Where 𝐶𝑑 is the CO2 emissions (kg/m3) resulting from the curing process and 𝑓
The CO2 emissions generated by curing was estimated based on the energy
expended by self-electrical heating method and oven curing method. According to the
previous studies (Turner and Collins, 2013; European Commission, 2012), consuming
one unit of electricity (KW h) would eventually result in 1.35 kg CO2 emission. The
CO2 emission efficiency for oven curing was estimated based on the results shown in
Fig.5 (b). The CO2 intensity (𝐶𝑖) for oven curing method and self-electrical heating
2.0
Self-electrical heating method
CO2 intensity
1.5
1.0
0.5
0.0
40 50 60 70 80
Oven curing temperature( oC )
Fig.14 CO2 intensity of samples under different curing conditions
Fig.14 shows that the CO2 intensity (𝐶𝑖) of samples cured by oven gradually
decreased with the curing temperature, the calculated CO2 intensity (𝐶𝑖) values of the
specimens cured at 40ºC, 50 ºC, 60 ºC, 70 ºC and 80 ºC were 1.78, 1.77, 1.64, 1.4 and
1.36, respectively. The CO2 intensity (𝐶𝑖) values for sample G-6-2 cured by self-
electrical heating method is 1.035, which is significantly lower than that of oven curing
samples. This can be likely explained by its lower energy cost and higher curing
efficiency.
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4. Conclusions
In this work, carbon black and steel fibers were added into the fly ash based
geopolymer to increase its electrical property and the feasibility of curing fly ash based
geopolymer by using self-electrical heating was investigated. The main conclusions can
be drawn as following:
1.According to the calorimeter test, the curing temperature has a significant effect
process of fly ash based geopolymer under ambient curing condition is very slow.
2.The maximum surface temperature for specimen could reach 67℃. It is feasible
recommended to add both steel fiber and carbon black into the geopolymer matrix.
4.The three-point bending tests showed that the flexural strength for specimen
significantly increased after the self-electrical heating. With the proper addition of
carbon black and steel fiber, the fly ash based geopolymer specimen cured after
can significantly increase the eco-efficiency because its lower energy cost and higher
curing efficiency.
Acknowledgments
This work was financially supported by Open Foundation of Key Laboratory of
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Dear Editors,
We declare that we have no financial and personal relationships with other people or
organizations that can inappropriately influence our work, there is no professional or
other personal interest of any nature or kind in any product, service and/or company
that could be construed as influencing the position presented in, or the review of, the
manuscript entitled “Fly ash-based geopolymer with self-heating capacity for
accelerated curing”.
Yours sincerely,
Jiawei Tan
Department of Civil Engineering
KU Leuven, Belgium
E-mail: jiawei.tan@kuleuven.be
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Authors’ contributions
Jingming Cai: Conceived and designed the study; Experiments; Data analysis; Writing
- Original Draft; Review & Editing
Xiaopeng Li: Review & Editing
Jiawei Tan: Review & Editing; Writing - Original Draft
Brecht Vandevyvere: Review