Construction and Building Materials 262 (2020) 120924

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Construction and Building Materials

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

Deterioration of ambient-cured and heat-cured fly ash geopolymer

concrete by high temperature exposure and prediction of its residual
compressive strength
Hongen Zhang a,b,c, Lang Li a,c, Cheng Yuan b, Qingyuan Wang a,c,d,⇑, Prabir Kumar Sarker b,⇑,
Xiaoshuang Shi a,c
a
Key Laboratory of Deep Underground Science and Engineering (Ministry of Education), School of Architecture and Environment, Sichuan University, Chengdu 610065, China
b
School of Civil and Mechanical Engineering, Curtin University, GPO Box U1987, Perth, WA 6845, Australia
c
Failure Mechanics & Engineering Disaster Prevention and Mitigation Key Laboratory of Sichuan Province, College of Architecture & Environment, Sichuan University,
Chengdu 610065, PR China
d
School of Mechanical Engineering, Chengdu University, Chengdu 610106, China

h i g h l i g h t s

Residual properties of fly ash geopolymer after elevated heat exposure is studied.

Higher mass loss is found for ambient curing than for initial heat curing.

Strength loss occurred only after 600 °C for 2 h exposure.

Residual strength decreases due to increased crushing index of coarse aggregate.

Proposed residual strength equations correlated well with the test data.

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

Article history: This paper presents an investigation on the performance of ambient-cured and heat-cured low-calcium
Received 12 November 2019 fly ash geopolymer concrete after exposure to elevated temperatures. The concrete specimens were
Received in revised form 21 August 2020 heated to 100, 200, 400, 600, 800 and 1000 °C at a heating rate of 5 °C/min. The effect of high temperature
Accepted 12 September 2020
exposure on geopolymer concrete was studied by visual inspection, mass loss, extent of cracking, residual
strength and microstructure investigation. The total length of cross-section cracks and surface cracks
reached their peak values at 800 °C and then declined at 1000 °C. The results show that all the concrete
Keywords:
specimens could be heated at 600 °C for 2 h without strength loss. Heat-cured geopolymer concrete spec-
Ambient curing
Heat curing
imens showed higher residual compressive strengths than the ambient-cured specimens for all the expo-
Geopolymer concrete sure temperatures. A crushing index of 7.7% could be regarded as the threshold value for coarse aggregate
Crushing index to maintain the initial compressive strength of concrete up to 600 °C. Thus, the microstructural damage
Coarse aggregate as observed by SEM images, dehydration of geopolymer shown by thermogravimetric analysis and the
Elevated temperature reduced strength of coarse aggregate are considered as the contributing factors for strength losses at tem-
Predicted residual strength peratures higher than 600 °C. Finally, two prediction equations are proposed which correlated well with
the experimental results of this study and those reported in published literature.
Ó 2020 Published by Elsevier Ltd.

1. Introduction properties, low cost, good fire resistance, versatility and

The increase of global infrastructures is increasing the
demand of concrete due to its advantages of desirable mechanical
⇑ Corresponding authors at: Sichuan University, No. 24 South Section 1, Yihuan
Road, Chengdu 610065, China, (Q. Wang); Curtin University, GPO Box U1987, Perth,
WA 6845, Australia, (P.K. Sarker).
E-mail addresses: wangqy@scu.edu.cn (Q. Wang), P.Sarker@curtin.edu.au
(P.K. Sarker).
convenience of maintenance over other construction materials
[1,2]. The traditional binder used for producing concrete is
ordinary Portland Cement (OPC). However, manufacturing
cement contributes to a huge amount of CO2 into the atmosphere,
causing a series of environmental issues such as global warming
[3]. Therefore, it is essential to develop alternative binders using
industrial by-products to supplement OPC in production of
concrete.

https://doi.org/10.1016/j.conbuildmat.2020.120924
0950-0618/Ó 2020 Published by Elsevier Ltd.
H. Zhang et al.
Geopolymer is a newly developing environmentally friendly
binder which is formed by the effective chemical reaction between
an alkali and aluminosilicate sources, such as fly ash [4,5], ground
granulated blast furnace slag [6] and metakaolin [7]. The com-
monly used activator solutions are Na-based [8,9] or K-based alka-
lis [10]). Some recent studies showed that geopolymer concrete
could provide 25–70% reduction in greenhouse gas emissions
depending on the ingredients and mixture proportions [11].
Apart from the environmental issues, sustainability and dura-
bility of concrete is also a concern. Consideration of the perfor-
mance of concrete at elevated temperatures is necessary when
evaluating the sustainability and durability of concrete. The
mechanical properties of OPC concrete deteriorate at elevated tem-
peratures, which is attributed to the physical and chemical changes
as well as the incompatibility between binder and aggregate [12].
The research works on OPC concrete [13,14] proposed the dissoci-
ation temperatures of Ca(OH)2 and CaCO3 to be 300 to 600 °C and
700 to 1000 °C, respectively, and their melting temperature
between 1200 and 1350 °C. Some recent research investigated
the performance of geopolymer paste, mortar, concrete and com-
posites subjected to elevated temperatures [15–18]. The behavior
of high strength and normal strength metakaolin-based geopoly-
mer concrete subjected to elevated temperatures [19] or simulated
fire [20]was reported in literature. The effect of raw materials and
alkaline activators on the thermal properties of geopolymers was
also investigated [21,22].
Kong and Sanjayan [23,24] stated that the thermal incompati-
bility between geopolymer matrix and aggregate was mainly
responsible for the strength loss and the size of coarse aggregate
affected the performance of geopolymer concrete at elevated tem-
peratures. Crystallization and phase changes caused the strength
degradation of concrete subjected to elevated temperatures
[6,25]. The creation and progress of micro cracks also resulted in
the strength deterioration of concrete when exposed to elevated
temperatures [6,26]. The gradual change in the pore structure after
exposure to elevated temperature was also analyzed quantitatively
by CT technology [5,6]. Overall, most of the previous research
focused on explaining the mechanism of strength deterioration in
the micro-level.
Crushing index is a mechanical parameter used to measure the
strength of concrete coarse aggregate [27]. As aggregates occupy
about 75% to 80% volume of concrete, the change in crushing index
of coarse aggregate would also affect the mechanical properties of
concrete. Zhang et al. [28] investigated the effect of crushing index
on properties of recycled concrete. The results demonstrated that
mechanical properties (compressive strength, flexural strength
and modulus of elasticity) decreased with the increase of crushing
index. However, the influence of crushing index of coarse aggre-
gate on compressive strength of concrete (especially geopolymer
concrete) subjected to elevated temperatures has never been
reported. Hence this investigation was conducted with one aim
to determine how the crushing index of coarse aggregate affected
the geopolymer concrete’s compressive strength after exposure
to elevated temperatures. The main aim of this research is to inves-
tigate the mechanism of strength degradation at elevated temper-
atures. The crushing index of coarse aggregate was tested in all the
exposure temperatures except for 100 and 200 °C.
Sarker et al. [20] investigated the cracking, spalling and residual
strength of normal and high strength geopolymer concrete after
Table 1
Chemical compositions of fly ash.
Chemical composition SiO2 Al2O3 CaO Fe2O3
Fly ash (mass, %) 65.30 14.48 5.63 6.25
y
Loss on ignition.
2
Construction and Building Materials 262 (2020) 120924
simulated fire exposures. The authors prepared geopolymer con-
cretes of different strength using different heat curing regimes
for the same mixture. Based on the previous research, two mix-
tures were used to prepare normal strength and high strength
geopolymer concrete with both ambient curing and heat curing
methods in this study.
In this paper, the deterioration of geopolymer concrete by expo-
sure of elevated temperatures was investigated and explained in
both macro-level and micro-level by using aggregate crushing
index, scanning electron microscopy (SEM) images and thermo-
gravimetric analysis (TGA). SEM and TGA technology have made
valuable contributions to the development of geopolymer compos-
ites [29–31]. An equation to predict the residual compressive
strength of concrete after exposure to elevated temperatures is
necessary for the fire design of concrete structures [32]. However,
very limited work has been carried out to propose an equation
suitable for fly ash geopolymer concrete. Therefore, this paper
has also proposed an equation to predict the residual compressive
strength of geopolymer concrete using the test results of this study
and those reported by previous studies.
2. Experimental work
2.1. Materials
The fly ash used for making geopolymer in this investigation
was low-calcium fly ash. The chemical compositions of fly ash
was determined by X-ray fluorescence (XRF) on a dry sample basis.
The chemical compositions and loss on ignition (LOI) of the fly ash
are given in Table 1. The bulk density, granule density and water
content of fly ash are given in Table 2.
Locally available natural siliceous sand with particle size smal-
ler than 4 mm and locally crushed basalt aggregate with particle
size between 4.75 mm and 22 mm were used as fine aggregate
and coarse aggregates, respectively. The main composition of sand
is SiO2. The bulk density, granule density and water content of
aggregates are presented in Table 2.
The alkali-activator solution was composed of commercially
available liquid sodium silicate (Na2SiO3) with a modulus ratio
(Ms) of 3.23 (where Ms = SiO2/Na2O, Na2O = 8.83%, SiO2 = 27.64%
by mass), and sodium hydroxide (NaOH) solution. The density of
Na2SiO3 solution at 20 °C is 1.384 g/cm3. Sodium hydroxide (NaOH)
particles of 98% purity were dissolved in distilled water to make
sodium hydroxide (NaOH) solution. The mass of NaOH particles
depends on the concentration of the solution expressed in terms
of molarity. For example, NaOH solution with a concentration of
8 M consists of 8  40 = 320 g/L of NaOH particles, where 40 is
the molecular weight of NaOH. The density of NaOH solution with
a concentration of 8 M and 14 M at 20 °C is 1.275 g/cm3 and
1.425 g/cm3, respectively. The alkali-activator solution was pre-
pared approximately 24 h prior to use.
2.2. Specimen preparation and curing regime
2.2.1. Mixture proportions
Two sets of concrete mixtures used in this investigation are pre-
sented in Table 3. The mixtures are named in the form of ‘‘GPN-X”
or ‘‘GPH-X”, where ‘‘GP” meant geopolymer concrete, ‘‘N”
MgO K2O SO3 TiO2 Na2O ZnO LOIy
0.93 1.46 0.09 1.08 1.14 0.07 0.82
H. Zhang et al. Construction and Building Materials 262 (2020) 120924

Table 2 for about 24 h, the other batch of specimens were cured at ambient
The density and water content of fly ash and aggregates. temperature for about 72 h because of the long setting time
Materials Granule density Bulk density Water content required for these specimens [1]. After 24 h or 72 h, the specimens
(g/cm3) (g/cm3) were demoulded and cured in a controlled condition (20 °C and
Fly ash 2.6 0.6 0.5% 65% RH) until tested.
Coarse aggregate 2.6 1.5 0.3%
Fine aggregate 2.4 1.3 0.1%
2.3. Preparing samples for detecting the concrete internal structure
deterioration

represents the normal strength concrete series, ‘‘H” represents the
high strength concrete series and ‘‘X” is the curing condition. For
example, ‘‘GPN-A” means ambient-cured normal strength geopoly-
mer concrete and ‘‘GPN-H” means heat-cured normal strength
geopolymer concrete. Additionally, it is worthwhile to mention
that the water content shown in the table is calculated from the
water in the alkaline liquid and no extra water was added during
the whole casting process.
2.2.2. Casting and curing of test specimens
The mixing of the concrete was conducted in a laboratory con-
crete mixer. For the mixing procedure, all dry materials (aggregates
and fly ash) were mixed in the pan mixer for about 3 min, then the
alkali-activator solution was sequentially added and the wet-
mixing continued for another 4–6 min until a consistent mixture
was obtained. The fresh concrete was poured into steel moulds
with 100  100  100 mm to prepare cube specimens. The moulds
were filled in two layers and each layer was vibrated for about 30 s
using a vibrating table.
Right after casting, the specimens along with the moulds were
covered with plastic film to prevent moisture loss. For each set of
mixture, one batch of specimens were cured in an oven at 80 °C
In order to analyze deterioration of the internal structure, the
concrete specimens were cut into three slices by a concrete cutting
machine. The specimens were cut into pieces before temperature
exposure in order to avoid the difficulty of cutting them after tem-
perature exposure since the specimens might suffer from explosive
spalling or severe strength loss after exposure to 800 °C or 1000 °C.
The method consisted of two steps. Firstly, before exposure to the
target temperature, the concrete specimen was cut into three
slices. Secondly, the three concrete slices were then covered by a
layer of mortar with less than 2 mm thickness to be an artificial
integrated concrete block (AICB). The second step could prevent
the cross-section of concrete from being exposed to elevated tem-
perature directly. This method is also intuitively illustrated in
Fig. 1. The mortar mixture proportions used in the second step is
also presented in Table 3 Mixture proportions and curing condition
of concrete and mortar. The AICB was then subjected to the target
temperature.
2.4. Heating details
An electrical furnace designed for a maximum temperature of
1600 °C was used in this study. The specimens were exposed to

Table 3
Mixture proportions and curing condition of concrete and mortar.

Mixture design of the concrete or mortar (kg/m3)

y à § –
Mix ID CA Sand Fly ash SS SH SS/SH* M Curing temperature Water content
GPN-A 1201 539 460 142.9 57.1 2.5 8 25 °C 5.54%
GPN-H 1201 539 460 142.9 57.1 2.5 8 80 °C 5.54%
GPH-A 1201 539 460 150 50 3.0 14 25 °C 5.21%
GPH-H 1201 539 460 150 50 3.0 14 80 °C 5.21%
Mortar 0 1380 460 150 50 3.0 14 40 °C –
y
coarse aggregate.
à
Na2SiO3 solution.
§
NaOH solution.
*
the mass ratio of Na2SiO3 solution to NaOH solution.
–
the molarity of sodium hydroxide solution.

Fig. 1. The method to prepare the artificial integrated concrete block (AICB).

3
H. Zhang et al. Construction and Building Materials 262 (2020) 120924

elevated temperatures after the age of 90 days. The heating regime
used in this study is presented in Fig. 2. The cube specimens were
subjected to the peak temperatures of 100, 200, 400, 600, 800 and
1000 °C at an incremental rate of 5 °C/min from ambient temper-
ature (Stage I). The concrete was then held at each peak elevated
temperature for 2 h to ensure a uniform temperature within the
specimens (Stage II). Then the specimens were left in the furnace
to naturally cool down to ambient temperature (Stage III).
2.5. Test methods
2.5.1. Mass loss test
The samples exposed to each target temperature were also used
for the determination of mass loss ratio of fly ash-based geopoly-
mer concrete (FAGC) using Eq. (1). The mass loss ratio value was
an average of three specimens.
Mb  Ma
R¼  100%
Mb
where R was the mass loss ratio and Mb referred to mass of the sam-
ple before exposure to the target temperature and Ma represents
mass of the sample after exposure to the temperature.
2.5.2. Crushing index of coarse aggregate
Crushing index is a mechanical index used to measure the
strength of concrete coarse aggregate. Kong and Sanjayan [24]
demonstrated the expansion behavior of aggregate under elevated
temperature. Therefore, the crushing index of coarse aggregate will
also be effected after exposure to elevated temperature. Crushing
index of coarse aggregate was tested in accordance with GB/T
14685-2011[27]. Three kilograms of coarse aggregate within parti-
cle size between 9.5 and 19 mm were used to conduct the crushing
index test using YAW-2000 electro-hydraulic mechanical testing
machine at a load rate of 1 kN/s until the maximum load reached
200kN. The maximum load was held constant for 5 s and then
unloaded to zero. Then a sieve shaker was used to obtain the resid-
ual mass of the aggregate with particle size larger than 2.36 mm.
The crushing index is calculated using Eq. (2).
G1  G2
Qe ¼  100%
G1
where Q e is the crushing index (%), G1 is the mass of coarse aggre-
gate (g) and G2 is the residual mass of coarse aggregate with the
particle size lager than 2.36 mm (g).
2.5.3. Image J analysis
In order to carry out the analysis of crack geometry attribute
more intuitively, a free software ‘‘Image J” was utilized. The soft-
ware was initially developed by the National Institute of Mental
Health. Fares et al. [33] investigated the porosity of the fraction
of anhydrous elements of self-consolidating concrete using Image
J and the result was remarkable.
2.5.4. Analyzing the cracks
MATLAB software was used to analyze and calculate the length
of crack on the surface and cross-section of concrete specimens
with the help of a local-binarization method provided by Li et al.
[34]. At first, the cross-sections and surfaces of concrete were
transferred to grey-scale images with a local-binarization algo-
rithm and then the total length of cracks was calculated. In this
paper, to clearly distinguish between the cracks on surface and
those in the cross-section, the cracks on the surface were defined
ð1Þ as EXTR-cracks (external cracks) and the cracks in the cross-
section were defined as INTR-cracks (internal cracks).
2.5.5. Compressive strength test
The compressive strength test was conducted in accordance
with GB/T50081-2002 [35] using a YAW-2000 electro-hydraulic
mechanical testing machine at a load rate of 0.5 MPa/s until the
concrete specimens were crushed. This method was also used for
testing the residual compressive strength of specimens after expo-
sure to elevated temperatures.
2.5.6. Scanning electron microscopic images
Scanning electron microscopy (SEM) test was conducted using
SU3500 (HITACHI, Kyoto, Japan) instrument to characterize the
microstructures of the FAGC samples.
2.5.7. Thermogravimetric analysis (TGA)
The aggregates were removed when preparing samples for the
thermogravimetric analysis (TGA) test. Fragments of FAGC speci-
mens unexposed to elevated temperatures were powdered to con-
duct the TGA test through a METTLER TOLEDO TGA/DSC2/1600
(METTLER TOLEDO, Zurich, Switzerland) instrument in alumina
ð2Þ crucibles in the nitrogen environment (N2 flowing at 50 mL/min),
and then elevated to 1000 °C with a constant heating rate of
10 °C/min in the same gas environment.
3. Results and discussion

3.1. Residual compressive strength

1100 Stage II
Stage I 2h The compressive strengths of GPN-A, GPN-H, GPH-A and GPH-H
1000
concrete specimens before and after exposure to elevated temper-
900 atures are given in Table 4. The percentage residual strengths at
2h
800 each target temperature are also presented in Table 4. It is clear
Temperatures (°C)

from Table 4 that all the geopolymer concretes showed the highest
in

Stage III
/m

700
compressive strength value at 200 °C. At 200 °C, the compressive
°C

2h
t5

600 strength of GPN-A, GPN-H, GPH-A and GPH-H were 58.0 MPa,
ea

Nat ent tem

71.6 MPa, 69.9 MPa and 89.9 MPa, respectively. Taking GPN-H
rat

am
rua

500
ng

bi

and GPN-A geopolymer concrete for consideration, compressive

l co
ati

2h
400
He

strength of ambient-cured geopolymer concrete was lower than

olin tures

that of heat-cured specimens during the temperature range of

g to

300
per

2h 20-1000 °C. The similar trend was also shown by GPH-H and
200 GPH-A specimens.
2h At 400 °C, the percentage residual strengths of GPN-A and GPN-
100
20 H were 163.9% and 162.2%, respectively, indicating that ambient-
Time (h) cured geopolymer concrete showed marginally better strength
enhancement than oven-cured geopolymer concrete after expo-
Fig. 2. The heating regime. sure to 400 °C. The effect of curing method is more pronounced
4
H. Zhang et al. Construction and Building Materials 262 (2020) 120924

Table 4
Compressive strength and percentage residual strength after heat exposure.

Temp. (°C) GPN-A GPN-H GPH-A GPH-H

y y y
Compr. Strength (MPa) Ratio (%) Compr. Strength (MPa) Ratio (%) Compr. Strength (MPa) Ratio (%) Compr. Strength (MPa) Ratioy (%)
20 35.2  1.2 100.0 39.40.6 100.0 43.22.4 100.0 72.82.3 100.0
100 52.0  0.7 147.7 63.5  5.6 161.2 63.9 1.43 147.9 87.6  4.2 120.3
200 58.0 2.5 164.7 71.61.0 181.7 69.92.1 161.8 89.73.3 123.2
400 54.8 2.1 163.9 63.90.8 162.2 57.96.0 134.0 80.92.4 111.1
600 46.0 2.9 130.7 50.04.3 126.9 49.23.9 113.9 72.32.2 99.3
800 17.4  0.4 49.4 22.23.4 56.3 21.7  1.9 50.2 23.12.8 31.7
1000 15.3 9.5 43.5 19.5 7.8 49.5 15.35.8 35.4 15.03.8 20.6
y
The ratio of residual compressive strength to original compressive strength.

in the percentage residual strengths of GPH-A (134.0%) and GPH-H similar to the trend of change in compressive strength. The ratio of
(111.0%). GPN-H geopolymer concrete specimens was larger than that of
It can be observed from Table 4 that the compressive strengths GPH-H specimens during all the temperature range, illustrating
of GPN-A, GPN-H and GPH-A concrete at 600 °C were still higher that normal strength geopolymer concretes experienced higher
than their original compressive strength. As for GPH-H, its residual strength growth ratio and lower strength loss ratio than high
strength at 600 °C was 72.3 MPa which was also almost equal to its
original compressive (72.8 MPa). Therefore, it could be concluded
that both ambient-cured and heat-cured geopolymer concrete

Ratio of residual compressive strength to original

could be kept at 600 °C for 2 h without loss of compressive 200
strength.
180
At 800 °C, the residual compressive strengths of the four series
of concrete were smaller than the corresponding initial compres- 160
compressive strength (%)
sive strength. The compressive strength of GPH-H even dropped
from 72.3 MPa (at 600 °C) to 23.1 MPa (at 800 °C). 140
At 1000 °C, the compressive strength of all concrete mixtures 120
was smaller than 20 MPa. The percentage residual strengths of
GPN-A, GPN-H, GPH-A and GPH-H were 43.5%, 49.5%, 31.9% and 100
20.6%, respectively.
80
Fig. 3 shows the compressive strength of different concretes
after exposure to the temperature range of 20–1000 °C. Overall, 60
the compressive strength change could be divided into two stages. GPN-A GPN-H
In the first stage, compressive strength increased with the increase 40 GPH-A GPH-H
of temperature and achieved its maximum value at 200 °C. The 20
compressive strength began to decline with different strength loss
rates between 200 and 1000 °C, which was the second stage. In the 0 100 200 300 400 500 600 700 800 900 1000 110
decline stage, the compressive strength appeared a moderate Temperatures (°C )
decrease from 200 to 600 °C and a significant decline from 600
to 800 °C, and then reduced slowly between 800 and 1000 °C. Fig. 4. The ratios of residual to original compressive strength at different elevated
temperatures.
The ratio of residual strength to original strength is also illustrated
in Fig. 4. It was observed that the trend of change in the ratio was

6.0

90 22 5.5
Crushing index of coarse aggregate (%)

5.0
80 20
4.5 Water content of GPN:5.54% 5.09±0.11 %
18
MPa

70
4.0 Water content of GPH:5.21%
Mass loss (%)

60 16
3.5
Compressive strength

14
50 3.0
10.7% 12
40 2.5
GPN-A GPN-H 10
30 2.0
GPH-A GPH-H
8 1.5
20 crushing index GPN-A GPN-H
6 1.0 GPH-A GPH-H
10
7.7%
4 0.5
0
0 100 200 300 400 500 600 700 800 900 1000 1100 0.0
0 100 200 300 400 500 600 700 800 900 1000
Temperatures (°C )
Temperature (°C)
Fig. 3. Compressive strength and crushing index of coarse aggregate at elevated
temperatures. Fig. 5. The mass loss of geopolymer concrete at elevated temperatures.

5
H. Zhang et al. Construction and Building Materials 262 (2020) 120924

strength specimens. It was found that the percentage residual
strength of GPH-A was higher than that of GPH-H during all the
temperatures, indicating that ambient-cured geopolymer concrete
performed better compressive strength enhancement and lower
strength deterioration than the heat-cured ones.
3.2. Relationship between crushing index of coarse aggregate and
residual compressive strength
Coarse aggregates play a vital role in forming the concrete
skeleton. Aggregate deterioration could lead to the deterioration
of concrete skeleton, which would have a detrimental impact on
the concrete structures causing the strength loss. The results of
crushing index before and after exposure to temperatures are also
illustrated in Fig. 3. The result of crushing index was not tested at
100 °C and 200 °C, therefore, the broken line was used. It is
observed from Fig. 3 that the crushing index increased with differ-
ent ratios during the various exposure temperatures. As discussed
in section 3.1, low-calcium fly ash-based geopolymer concrete
could retain its initial compressive strength at 600 °C. Therefore,
the coarse aggregate with a crushing index of 7.7% (Fig. 3) was still
strong enough to work as the critical part of concrete skeleton. In
other words, a crushing index of 7.7% could be regarded as the
threshold value for coarse aggregate to maintain its good strength.
With the crushing index rising to 10.7% (at 800 °C), the coarse
aggregate lost most of its load capacity resulting in a significant
loss of compressive strength. After exposure to 1000 °C, the crush-
ing index increased further to 21.1% with little influence on com-
pressive strength change, which will be further discussed in the
following section.

Fig. 6. Surface images of geopolymer concrete at different temperatures.

Fig. 7. 8-bit grey-scale surface images of geopolymer concrete at different temperatures.

6
H. Zhang et al.
3.3. Mass loss of concrete after exposure to elevated temperatures
The mass loss of concrete samples resulting from the exposure
to heat was calculated through weighing the mass of specimens
before and after the target temperature exposure. The mass loss
values of specimens are presented in Fig. 5. It can be seen that
ambient-cured and heat-cured geopolymer concretes presented
similar mass loss trend. There was an increasing trend in mass loss
with the increasing elevated temperatures. The mass loss is gener-
ally attributed to the loss of free water or bonded water according
to the exposure temperatures [5,6,30]. Up to 200 °C, the mass loss
was associate with the loss of free water and partly chemically
bonded water resulting from the dehydration of geopolymer gel.
Beyond 200 °C, the mass loss was mainly resulted from further
dehydration of geopolymer gel and dehydroxylation of hydroxyl
groups [36]. Additionally, the concrete specimens cured at ambient
temperature showed higher mass losses than the heat-cured spec-
imens. It was found that mass loss values of GPH-H geopolymer
Fig. 8. Total length of EXTR-cracks of geopolymer concrete at elevated
temperatures.
Fig. 9. Cross-section images of geopolymer concrete at different temperatures.
7
Construction and Building Materials 262 (2020) 120924
concretes were higher than those of GPN-H specimens during the
temperature range of 100 to1000 °C, illustrating that the high
strength geopolymer concretes experienced higher mass loss than
the normal strength concrete at elevated temperatures. At 400 °C,
the mass loss values of the GPN-H, GPN-A, GPH-H and GPH-A sam-
ples were 2.32%, 2.61%, 2.82% and 3.35%, respectively. During the
temperature range of 600 to1000 °C, the rate of mass loss slowed
down in concrete samples. The mass loss values of GPN-H, GPN-
A, GPH-H and GPH-A at 1000 °C were 3.48%, 4.19%, 4.15% and
5.09%, respectively.
Overall, the high strength concrete samples suffered from
higher mass loss than the normal strength concrete samples
(Fig. 5). This is consistent with the results of previous study on
fly ash-based geopolymer concrete after fire exposure [20]. The
maximum mass loss was smaller than the initial water content
in the concrete and the GPH-A sample suffered the highest mass
loss value (5.09 ± 0.11%) which was very close to its initial water
content (5.21%).
3.4. The change in surface of concrete specimens
The surface images of the concrete specimens before and after
exposure to different temperatures are presented in Fig. 6. The con-
crete samples showed gray or gray-white color at ambient temper-
ature. Up to 400 °C, no noticeable color difference was observed for
all the concrete samples except for GPH-A sample that presented a
light brown color at 400 °C. The color change in GPH-A at 400 °C
might be due to its highest mass loss. From the beginning of
600 °C, there was obvious color difference from the original color.
At 800 °C and 1000 °C, the concrete specimens displayed red color
which is attributed to the high iron oxide content of the fly ash
[17]. A similar change in color in high and normal strength con-
crete subjected to simulated fire was also observed by Sarker
et al. [20].
The 8-bit grey-scale images of surface obtained from the Image
J analysis software are presented in Fig. 7.The RGB color images
(Fig. 6) were converted to 8-bit grey-scale images using threshold
segmentation method. It is worthy to mention that the threshold
value of each image was not always identical, especially for the
images at 800 and 1000 °C. It could be observed from Fig. 7 that
H. Zhang et al. Construction and Building Materials 262 (2020) 120924

Fig. 10. 8-bit grey-scale cross-section images of geopolymer concrete at different temperatures.

there were several visual initial cracks on the surface of GPN-A
concrete specimens before exposure to elevated temperatures. This
is due to the drying shrinkage of concrete. Ridtirud et al. [37] and
Jiang et al. [38] proved that the drying shrinkage was more signif-
icant for geopolymer materials cured at ambient temperature. No
obvious cracks were observed in the surfaces of GPH-A series
because the NaOH concentration in this series was up to 14 M.
Singh et al. [26] found that a higher activator concentration
(14 M) released more heat than for lower activator concentration
(8 M) during geopolymerization. The released energy would pro-
mote the geopolymerization. Therefore, 14 M-concentration NaOH
solution could provide more appropriate temperature environ-
ment as compared to 8 M, which resulted in a more completed
geopolymerization in GPH-A series.
It is observed from Fig. 7 that cracks started to become larger
(for GPN-A specimen) or to appear (for the other concrete speci-
mens) on the concrete surface after exposure to 200 °C. The
amounts of cracks and width of cracks increased with the elevated
temperature during the temperature range of 200–800 °C. For all
the four series, the amounts of cracks were most significant at
800 °C. For exposure to 800–1000 °C, the amount of cracks dis-
3.5. The change in the cross-section of concrete specimens
The original images of cross-section are presented in Fig. 9. It
can be seen that the color of cross-section showed negligible
change before exposure to 400 °C. The color of coarse aggregate
turned from grey at 600 °C to white or brown at 800 to 1000 °C.
This is different from a previous observation by Li et al. [6] in which
the color of coarse aggregate was reported to change from blue to
red. The difference in color change of aggregate is largely attribu-
ted to the composition and type of aggregate [39,40]. The color
change of concrete cross-section is a combined result of those of
geopolymer, sand and coarse aggregate where coarse aggregate
played the critical role because of its higher volumetric ratio [6].
The 8-bit grey-scale images of cross-section are illustrated in
Fig. 10. It can be seen that the INTR-cracks were distributed in
the cross-section of GPN-A sample at ambient temperature, indi-
cating the original structural defects in GPN-A samples. The
1000
Total length of INTR-cracks (mm)

played a decreasing trend. More impressive, seldom visual cracks

could be observed on the surface of GPH-H, while it is easy to find 800
several significant bulges on its surface at 1000 °C.
The length of EXTR-cracks at the target elevated temperatures
was calculated using MATLAB software and the results are pre-
600
sented in Fig. 8. It can be seen that the total length of EXTR- GPN-A GPN-H
cracks of GPN-A is higher than the other three samples before GPH-A GPH-H
600 °C. During the temperature range of 20–600 °C, the length of
400
EXTR-cracks showed a slowly increasing trend for the four sam-
ples. The length of EXTR-cracks of ambient-cured specimens
(GPN-A and GPH-A) increased dramatically in the range of
200
600~800 °C and reached its maximum value at 800 °C. At the same
time, the length of EXTR-cracks of heat-cured specimens (GPN-H
and GPH-H) presented a moderate growth in the length of EXTR-
0
cracks between 600 and 800 °C and reached its peak value at 0 100 200 300 400 500 600 700 800 900 1000 1100
800 °C. Beyond 800 °C, the EXTR-cracks of all the four series con-
ºC
crete declined at different ratios. At 1000 °C, the length value of
the EXTR-cracks of GPN-A was the largest, followed by GPN-H, Fig. 11. Total length of INTR-cracks of geopolymer concrete at elevated
GPH-A and GPH-H. temperatures.

8
H. Zhang et al. Construction and Building Materials 262 (2020) 120924

amount of cracks can be seen to decrease after exposure to 200 °C The total length of INTR-cracks is also illustrated in Fig. 11. It
which is an evidence of the secondary geopolymerization of fly ash can be seen that the initial length of INTR-cracks of GPN-A is much
geopolymers after exposure to high temperature. higher than those of the specimens of other series at ambient tem-

ºC ºC

ºC ºC

ºC ºC

ºC ºC
Fig. 12. SEM micrographs of geopolymer concrete at 20 °C.

9
H. Zhang et al.
perature, which indicates that there were many defects in the con-
crete internal macro-structure. As a result, the compressive
strength of GPN-A series was the lowest among the four concrete
series. Before 600 °C, the length of INTR-cracks of GPN-A decreased
to the bottom at 200 °C resulting from secondary geopolymeriza-
tion, and then increased with the temperature. As for GPN-H,
GPH-A and GPH-H, the length of INTR-cracks increased rather
slowly and the values were also much smaller than that of GPN-
A in the range of 20–600 °C. Contrary to the behavior of EXTR-
cracks between 600 and 800 °C, the length of INTR-cracks of
heat-cured specimens (GPN-H and GPH-H) increased dramatically
and that of ambient-cured specimens (GPN-A and GPH-A). The
same with EXTR-cracks, the peak values of INTR-cracks were still
appeared at 800 °C and the total length of the INTR-cracks of
GPN-A was also the largest followed by GPN-H, GPH-A and GPH-
H after exposure to 1000 °C.
ºC
ºC
ºC
Fig. 13. SEM micrographs of GPH-H group geopolymer concrete at different elevated temperatures.
10
Construction and Building Materials 262 (2020) 120924
3.6. Microstructure investigation
The SEM images of the samples all four series at 20 °C are
shown in Fig. 12 at two different magnifications. All the images
display heterogeneous microstructures containing unreacted fly
ash particles of different sizes. Micro-cracks can be seen in
Fig. 12 (a) and (b), which were responsible for the lower strength
of GPN-A samples at ambient temperature. The micro-cracks were
believed to be caused by the drying shrinkage. It can be seen from
Fig. 12 (a) to (d) that the microstructures of GPN-A and GPN-H
samples are less cohesive than those of GPH-A and GPH-H samples
(Fig. 12 (e) to (h)), which explains the lower compressive strengths
of GPN-A and GPN-H samples. Compared with the GPH-H sample,
the GPH-A sample has a larger proportion of unreacted fly ash par-
ticles, therefore, GPH-A samples showed lower compressive
strength than the GPH-H samples.
ºC
ºC
ºC
H. Zhang et al. Construction and Building Materials 262 (2020) 120924

101 the amounts of unreacted fly ash particles after exposure to

800 °C. Additionally, after exposure to 800 °C, several micro-
100 GPN-H GPN-A
cracks are also observed in the sample. The micro-cracks (marked
99 GPH-H GPH-A as thermal cracks in Fig. 13 (c) and (d)) were believed to be induced
98 by the thermal stress. A lot of small pores and areas of high poros-
ºC ity were observed in the sample after exposure to 800 °C (Fig. 13
97 ºC (d)), indicating the low cohesion of geopolymer matrix. Further
Mass (%)

96 increasing the temperature up to 1000 °C, no unreacted fly ash par-

ticles but amounts of large pores were observed (Fig. 13 (e) and
95
(f)). The pores were possibly due to the collapse of the geopolymer
94 matrix induced by the decomposition of geopolymer [18] and
93 phase transformations [41]. Though the SEM shows a high number
of large pores after exposure to 1000 °C, the microstructure has
92 ºC fewer impurities and it reveals a smoother texture. The smooth
91 texture is believed to be due to the melting, viscous flow and sin-
tering of unreacted fly ash particles and amorphous aluminosili-
90
0 100 200 300 400 500 600 700 800 900 1000 cate gels during heating at a high temperature of 1000 °C.

ºC
Fig. 14. The TGA curves of geopolymer samples.
The SEM images of GPH-H sample at 200 °C, 800 °C and 1000 °C
are presented in Fig. 13. A flat and intact surface was detected at
200 °C. It can be seen that there was a significant reduction in
3.7. Thermogravimetric analysis
The TGA curves of geopolymer samples are illustrated in Fig. 14.
The derivative thermogravimetry (DTG) and differential scanning
calorimetry (DSC) curves of geopolymer concrete samples are plot-
ted in Fig. 15. The mass change trend in Fig. 14 is found to be in line
with that in Fig. 5. It can be seen from Fig. 14 that geopolymer con-

Fig. 15. The DTG and DSC curves of geopolymer samples.

11
H. Zhang et al.
crete experienced four characteristic stages of mass loss. Stage I
involved evaporation of the free water and part of chemically
bound water up to 200 °C. The mass loss occurred in stage I
accounted for more than 50% of the total mass loss. Stage II is char-
acterized by the loss of chemically bound water and dehydroxyla-
tion of hydroxyl groups, which occurred between 200 and 700 °C.
The mass in stage III almost remained unchanged from 700 °C to
950 °C. The last stage is stage IV after 950 °C where the mass loss
went on to increase slightly.
The thermal behavior of geopolymer concrete after exposure to
elevated temperatures up to 1000 °C is an endothermic process
accompanied by exothermic process at some specific temperature,
which could be obtained from the DSC curves shown in Fig. 15. It
can be seen from Fig. 15 that the peak value of mass loss rate (in
DTG curves) and the peak value of endothermic peak and exother-
mic peak (in DSC curves) generally occurred at the same tempera-
ture. The first mass loss rate peak occurred at the temperature
ranging from about 43.4 °C in GPN-H sample (Fig. 15 (b)) to about
66.8 °C in GPH-A sample (Fig. 15 (b)), which was believed to be the
evaporation of free water. The different temperature values of the
first mass loss rate peak implied the different amount of free water
in different geopolymer concrete specimens. The higher the tem-
perature at the first peak of mass loss rate was, the larger amount
of free water there was in geopolymer concrete. Therefore, more
free water existed in the ambient-cured geopolymer concrete spec-
imens. As a result, ambient-cured geopolymer concrete experi-
enced higher mass loss.
At the temperature of around 75 °C (79.5 °C in Fig. 15 (c)), the
second mass loss rate peak in the DTG curves and the exothermic
peak in the DSC curves were owing to the crystallization of
geopolymer product. Some free water became the chemically
bound water during the crystallization, resulting in the decrease
of mass loss rate. For example, the maximum mass loss rate of
GPN-A samples (Fig. 15 (a)) declined from 5.2  104 at 61.4 °C
to 2.8  104 at 74.8 °C. However, the exothermic peaks in GPN-
H and GPH-H samples (Fig. 15 (b) and (d)) were not as obvious
as those in GPN-A and GPH-A samples (Fig. 15 (a) and (c)). This
is because that GPN-H and GPH-H samples were cured at 80 °C.
At about 87 °C, the third mass loss rate peak was observed in the
Fig. 16. The schematic diagram of concrete degradation between 200 and 600 °C.
12
Construction and Building Materials 262 (2020) 120924
DTG curves and an endothermic peak was found in the DSC curves,
which was because of the dehydration of chemically bound water.
The evaporation of free water and dehydration of the chemically
bound water was mainly responsible for the mass loss of geopoly-
mer concrete up to about 200 °C. At about 950 °C, an endothermic
peak was observed in the DSC curves, which was due to the melt-
ing of unreacted fly ash particles and geopolymer matrix. There-
fore, no fly ash particles were observed and large pores were
observed instead in Fig. 13 (e) and (f).
4. Discussions
Comparing Figs. 8 and 11, it was evident that the total length of
EXTR-cracks was much higher than the total length of INTR-cracks.
Therefore, the surface of concrete specimens suffered from much
more deterioration than the internal structure even though the
concrete reached thermal equilibrium. The temperature gradient
and gradual heat exchange that occurred during the cooling period
is considered as the main reason for this difference. It was found
that the length of EXTR-cracks of ambient-cured geopolymer con-
crete was longer than that of heat-cured specimens after exposure
to 800 °C. On the contrary, the length of INTR-cracks of heat-cured
geopolymer concrete was longer than that of ambient-cured spec-
imens after exposure to 800 °C.
Generally, the cracks (micro-cracks and macro-cracks) are
believed to be the result of the thermal incompatibility between
the geopolymer matrix and aggregate [17,42], pore pressure and
temperature gradient [6]. In this paper, as concrete cured at
20 °C had a relatively less dense structure than the one cured at
80 °C, water (free water, capillary water and chemically bonded
water) could move to the surface of the specimens more easily
causing more cracks in the concrete surface because of vapor pres-
sure. Fig. 9 illustrated that most of the INTR-cracks occurred
around the coarse aggregates. Therefore, the evaporation (release)
of water (free water, capillary water and chemically bonded water)
is considered as the main reason to cause the cracks on the surface
and the thermal incompatibility between geopolymer matrix and
aggregate as the main reason for the INTR-cracks generation.
H. Zhang et al. Construction and Building Materials 262 (2020) 120924

Fig. 17. Thermal macro-cracks on part of cross-section at elevated temperatures.

Fig. 18. Failure patterns at different temperatures.

13
H. Zhang et al.
It can be seen from Fig. 11 that the length of INTR-cracks was
nearly negligible up to 400 °C, except for GPN-A sample, which
demonstrated that the internal macrostructure kept relatively
stable at 400 °C. The sustainable shrinkage of fly ash-based
geopolymer matrix [23,43] and the sustainable expansion of coarse
aggregate [23] occurred after 200 °C due to the difference in their
thermal behavior. The theory that most of the shrinkage of slag-
based geopolymer is irreversible and most of expansion of aggre-
gates is reversible up to 750 °C [6] was applied for low-calcium
fly ash-based geopolymer concrete in the current study. In general,
the expansion of coarse aggregate dominated over the shrinkage of
geopolymer matrix in concrete because of its larger volume than
geopolymer. As a result, a little gap (micro-cracks or macro-
cracks) forms between geopolymer matrix and coarse aggregate.
That is how the thermal incompatibility affect the properties of
concrete subjected to elevated temperatures. However, naked
cracks were observed seldom in the cross-section (except for
GPN-A) before 600 °C (Fig. 9), thus, the thermal incompatibility
between aggregate and matrix resulted in micro-cracks. The ther-
mal incompatibility would have a detrimental influence on the
mechanical behavior of interfacial transition zone (Fig. 16) result-
ing in the strength loss between 200 and 600 °C. However, the
cracks and the crushing index value of coarse aggregate were not
noticeable enough to damage the concrete structure. As a result,
geopolymer concrete samples retained the initial strength at
600 °C.
Fig. 19. Experimental results and fitting curves of residual compressive strength versus elevated temperature.
14
Construction and Building Materials 262 (2020) 120924
At 800 °C, the length of EXTR- and INTR-cracks reached their
peak values, indicating the concrete structure suffered severe dam-
age. Additionally, the coarse aggregate lost most of its load capac-
ity due to its high crushing index value at this temperature.
Therefore, the compressive strength dropped sharply after expo-
sure to 800 °C. At 1000 °C, the length of EXTR- and INTR-cracks
decreased. It appears that the concrete showed a self-healing abil-
ity which is related to the shrinkage, sintering and melting of
geopolymer matrix. Previous research demonstrated that geopoly-
mer made from slag [44] or low-calcium fly ash [45] experienced
an obvious compressive strength increase at temperatures higher
than 800 °C. Rickard et al. [45] argued that the strength increase
at temperature higher than 800 °C was attributed to the sintering
and melting. However, the concrete strength still decreased slowly
because the coarse aggregate had lost most of its load carrying
capacity at 1000 °C in which the crushing index of coarse aggregate
was 21.1%. As aggregate occupied about 73% of the total weight,
the strength of aggregate played a decisive role in the compressive
strength of concrete at this stage.
Figs. 17 and 18 further show that the loss of compressive
strength occurred at temperatures higher than 800 °C is due to
the strength loss of coarse aggregate. The terms (radial crack, inclu-
sion crack and tangential crack in Fig. 17) used for analyzing micro-
cracks in cement-based mortar [46] were cited to distinguish dif-
ferent types of cracks in geopolymer concrete. However, they are
used here to define cracks in macro-level. The appearance of inclu-
H. Zhang et al. Construction and Building Materials 262 (2020) 120924

sion cracks indicated that the coarse aggregate lost its ability to
stand the thermal stress at 800 and 1000 °C, which was consistent
with the results of crushing index (Fig. 3).
It can be seen from Fig. 18 (a) that the coarse aggregates were
intact and well bonded with matrix (geopolymer matrix and mor-
tar matrix) and the concrete strength was 43.2 MPa. Tensile frac-
ture face and cracks appeared in some coarse aggregates as the
concrete strength reached to 89.7 MPa (Fig. 18 (b)). Therefore, it
could be concluded that coarse aggregates could remain intact
under the following external load (r) range: 43.2 MPa  r < 89.
7 MPa. Based on these results, it is expected that the concrete
strength should be at least higher than 43.2 MPa at 800 and
1000 °C because the behavior of coarse aggregates in Fig. 18 (c)
and (d) is similar to that in Fig. 18 (b). However, the tested strength
was only 23.1 MPa and 15.0 MPa at 800 and 1000 °C, respectively.
The results suggested that the strength of coarse aggregate
decreased dramatically after exposure to 800 and 1000 °C, result-
ing in the loss of concrete strength.
It is observed from Figs. 17 and 18 that coarse aggregate is bet-
ter bonded with matrix at 1000 °C than that at 800 °C due to the

Table 5
Experimental and predicted residual strengths by the proposed equation.

TEM GPN-A GPN-H GPH-A GPH-H

(°C)
Exp. (Std) Pred. Exp./ Exp. (Std) Pred. Exp./ Exp. (Std) Pred. Exp./ Exp. (Std) Pred. Exp./
[MPa] (MPa) Pred. [MPa] (MPa) Pred. [MPa] (MPa) Pred. [MPa] (MPa) Pred.
20 35.2 (1.2) – 39.4 (0.6) – 43.2 (2.4) – 72.8 (2.3) –
100 52.0 (0.7) 49.9 1.04 64.1 (5.6) 55.9 1.15 63.9 (1.0) 61.3 1.04 87.6 (2.4) 84.4 1.05
200 58.0 (2.5) 53.8 1.08 71.6 (1.0) 60.2 1.19 69.9 (2.1) 66.0 1.06 89.7 (3.3) 91.2 0.98
400 57.7 (2.1) 51.1 1.13 63.9 (0.8) 57.2 1.12 57.9 (6.0) 62.8 0.92 80.9 (2.4) 86.1 0.94
600 46.0 (2.9) 37.3 1.23 50.0 (4.3) 41.8 1.20 49.2 (3.9) 45.8 1.07 72.3 (2.2) 61.4 1.18
800 17.4 (0.4) 20.9 0.83 22.2 (3.4) 23.4 0.95 21.7 (1.9) 25.7 0.84 23.1 (2.8) 33.0 0.70
1000 15.3 (9.5) 9.0 1.70 19.5 (7.8) 10.1 1.93 14.6 (5.8) 11.1 1.32 13.6 (5.2) 13.4 1.02

Fig. 20. The comparison between experimental and predicted results by the proposed equations and existing models.

15
H. Zhang et al. Construction and Building Materials 262 (2020) 120924

melting and sintering of fly ash particles and aluminosilicate gels. 800 °C. However, the concrete strength at 1000 °C is still lower
Therefore, it is empirical to believe that the residual compressive than the strength at 800 °C (Fig. 18), which is attributed to the
strength of GPH-H sample at 1000 °C is higher than that at higher crushing index of coarse aggregate at 1000 °C (Fig. 3).

Fig. 21. Validation of the proposed equation.

16
H. Zhang et al.
Therefore, the strength loss after 600 °C is caused by the poor
load capacity of coarse aggregate. The strength loss of coarse aggre-
gate is attributed to their excessive expansions. The results suggest
that the crushing index value of coarse aggregate could be consid-
ered as a contributory factor to investigate the mechanism of
geopolymer concrete deterioration at elevated temperatures.
5. Prediction of residual compressive strength after exposure to
high temperature
5.1. Proposed analytical model
With an aim to propose a prediction model, the residual com-
pressive strengths are plotted against the elevated temperatures
for the four groups in Fig. 19. The nonlinear fitting curves for each
group are also drawn in the figure. It can be seen that the fitting
curves are in good agreement with the experimental data with
the R2 value ranging from 0.88 to 0.94.
Based on the experimental results and respective fitting curves
(Fig. 19), Eq. (3) and Eq. (4) were recommended as the proposed
model for predicting the residual compressive strength of geopoly-
mer concrete at elevated temperatures. These two equations were
obtained by using the Gaussian-based mathematical model and
finding the coefficients by analysing experimental results with
the help of MATLAB software. Eq. (3) is used for geopolymer con-
crete with compressive strength no more than 50 MPa (GPN-H,
GPN-A and GPH-A groups in this paper) and Eq. (4) is applicable
for geopolymer concrete with compressive strength higher than
50 MPa (GPH-H group in this paper).
When fc  50 MPa
T262:1 2
f cT ¼ 1:547  eð 550:1Þ f
c ð3Þ
When fc > 50 MPa
f cT ¼ 1:268  eð Þ f
T259:7 2
532:8
c ð4Þ
where,
fcT = Residual compressive strength (MPa)
fc = Original compressive strength (MPa)
T = Elevated temperatures (°C)
e = Natural constant
5.2. Analysis of the proposed model
The experimental results, predicted results and the value of
experimental to predicted residual strengths (Exp./Pred.) are given
in Table 5 Experimental and predicted residual strengths by the
proposed equation. It can be seen that the experimental compres-
sive strengths are generally higher than the predicted strengths
for GPN-A, GPN-H and GPH-A. As for GPH-H, the experimental
strengths are larger than the predicted strengths at 100 °C,
600 °C and 1000 °C. Thus, the data in Table 5 show that Eq. (3)
and Eq. (4) is generally conservative in predicting the residual
compressive strengths of geopolymer concrete at elevated
temperatures.
Eurocode EN 1994:2005 [47] provides a formula (Eq. (5)) to pre-
dict the residual compressive strength of OPC concretes grade
C40/50 at various elevated temperatures. Xiao and Falkner [48]
recommended an empirical model (Eqs. (6a) and (6b)) to estimate
residual strength of high performance OPC concrete (grade
C50 ~ C100) at different temperatures. The predicted residual
strength by the Eurocode [47] and by Xiao and Falkner’s model
[48] for geopolymer concretes after exposure to different elevated
temperatures are presented in Fig. 20. For the ease of comparison,
the experimental strength and predicted results with the proposed
17
Construction and Building Materials 262 (2020) 120924
models (Eq. (3) and Eq. (4)) are also illustrated in Fig. 20. The mean
ratio of the experimental to predicted strengths and the corre-
sponding coefficient of variation (COV) are also given in Fig. 20.
It is observed that the experimental results are very close to the
predicted results by the proposed model but much higher than
the predictions by Eurocode [47] and by Xiao and Falkner [48]. Tak-
ing GPN-A for an example, the mean values of the Exp./Pred. ratio
by Eurocode and Xiao and Falkner are 4.12 and 4.40, respectively,
indicating that the experimental values are more than four times
higher than the predicted values by these two equations. On the
other hand, the mean value of the Exp./Pred. ratio by Eq. (3) is only
1.16, indicating that the predicted values by Eq. (3) is close to the
experimental results. There is an increasing trend of the experi-
mentally determined compressive strengths up to elevated tem-
peratures of 200 °C which was ascribed to further
geopolymerization after being subjected temperature increase.
This phenomenon is different from the trend shown by OPC con-
crete and therefore, it is not considered in the existing models.
f cT ¼ l  f c ð5Þ
where m is reduction factor recommended in Eurocode EN
1994:2005 [47].
f cT ¼ ½1:011  ðT=1900Þ  f c T 6 400 C ð6aÞ
f cT ¼ ½1:44  ðT=625Þ  f c 400 C 6 T 6 900 C ð6bÞ
5.3. Further validation of the proposed model
In addition to the experimental results of this study, those avail-
able in published literature on fly ash geopolymer concrete
[20,29,31,49,50] were also employed to validate Eq. (3) and Eq.
(4). The details of the comparisons are also summarized in
Fig. 21. It is observed from Fig. 21(a), (b) and (g) that the mean val-
ues of Exp./Pred. ratio are 0.67, 0.74 and 1.36, respectively. The
variation is attributed to the different types of fly ash, alkalis and
curing method used in the preparation of geopolymer concrete.
The mean values of Exp./Pred. ratio are generally around 1.00 in
Fig. 21(c), (d), (e), and (f), implying that the difference between
experiments and predicts is within the acceptable range.
6. Conclusions
Ambient-cured and heat-cured low-calcium fly ash-based
geopolymer concrete specimens were exposed to elevated temper-
atures of 100, 200, 400, 600, 800 and 1000 °C. The mass change,
strength change and external and internal cracks of geopolymer
concrete after exposure to the target temperatures were investi-
gated. Further insights into the effect of high temperature were
achieved by using SEM images, TGA and crushing index of coarse
aggregates. Two equations are proposed to predict the residual
strengths using the test results of this study and those available
in literature. The following conclusions are drawn from the study:
1. The mass loss increased with the increase of exposure temper-
ature. Generally, the mass loss of high strength concrete was
higher than that of normal strength concrete. For the same mix-
ture, ambient-cured geopolymer concretes experienced higher
mass loss than the heat-cured specimens. It was found that
the maximum mass loss of low-calcium fly ash geopolymer
concrete was smaller than the initial water content in the
mixture.
2. The phenomenon that concrete surface suffered from more sev-
ere deterioration than the concrete’s internal structure is
mainly attributed to the temperature gradient and gradual heat
H. Zhang et al.
exchange that occurred during the cooling period. The total
length of EXTR- and INTR-cracks reached the peak values at
800 °C and then decreased after exposure to 1000 °C indicating
a self-healing ability which is related to the shrinkage and sin-
tering of geopolymer matrix.
3. Ambient-cured geopolymer concrete generally experienced
higher strength enhancement than heat-cured concrete. Nor-
mal strength geopolymer concrete showed higher strength
enhancement than high strength geopolymer concrete for both
ambient-cured and heat-cured specimens. At 400 °C, the resid-
ual compressive strengths of the concretes of four series were
higher than the corresponding initial compressive strengths.
Low-calcium fly ash-based geopolymer concrete could be
exposed to 600 °C for 2 h without strength loss.
4. The crushing index of coarse aggregate increased with the
increase of exposure temperature. The coarse aggregate was
strong enough to maintain the initial compressive strength of
concrete up to 600 °C. A crushing index of 7.7% could be consid-
ered as the threshold value for coarse aggregate in order to
maintain its strength. The cracks induced in coarse aggregates
by temperature gradient contributed to the strength loss of con-
crete at temperatures higher than 600 °C.
5. The SEM results showed that the geopolymer concrete has its
unique microstructural characteristic at different temperatures.
The mass loss of geopolymer concrete during the heating pro-
cess is attributed to the evaporation of free water and chemi-
cally bound water, and the dehydroxylation of hydroxyl
groups, which were found in the thermogravimetric analysis.
The strength loss at temperatures higher than 600 °C is also
ascribed to the microstructure deterioration and the dehydra-
tion of geopolymer gels.
6. Based on the experimental results, two empirical equations
were proposed to predict the residual compressive strength of
geopolymer concrete after exposure to different temperatures.
The proposed equations were found to correlate well with the
test data of this study and those available in the published liter-
ature on fly ash geopolymer concrete.
CRediT authorship contribution statement
Hongen Zhang: Formal analysis, Investigation, Software, Data
curation, Writing - original draft. Lang Li: Investigation, Software,
Data curation. Cheng Yuan: Methodology, Formal analysis. Qin-
gyuan Wang: Conceptualization, Methodology, Resources, Super-
vision, Funding acquisition. Prabir Kumar Sarker: Writing -
review & editing, Supervision. Xiaoshuang Shi: Visualization,
Supervision.
Declaration of Competing Interest
The authors declare that they have no known competing finan-
cial interests or personal relationships that could have appeared
to influence the work reported in this paper.
Acknowledgements
The authors are sincerely grateful for the financial support pro-
vided by the National Natural Science Foundation of China (No.
11772209 & No. 11832007 & No. 11572057), the Science & Tech-
nology Support Program of Sichuan Province (No. 2019JDS0006),
the Basic scientific research fund for Central-Government-
supported universities (Sichuan University). The first author is sup-
ported by the China Scholarship Council (CSC), which is sincerely
appreciated. Additionally, the authors also like to thank He Yi of
the Analytical & Testing Center (ATC) of Sichuan University for
his great help in the SEM test.
18
Construction and Building Materials 262 (2020) 120924
Appendix A. Supplementary data
Supplementary data to this article can be found online at
https://doi.org/10.1016/j.conbuildmat.2020.120924.
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