Compressive Strength and Microstructural Properties

of Fly Ash–Based Geopolymer Concrete

Gaurav Nagalia 1; Yeonho Park, Ph.D., M.ASCE 2; Ali Abolmaali, Ph.D., M.ASCE 3; and Pranesh Aswath, Ph.D. 4
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Abstract: This study examines the role of alkali hydroxide and its concentration on the microstructure and compression strength of fly ash–
based geopolymer concrete. Geopolymer is an innovative ceramic material, composed of long chains and networks of inorganic molecules,
that is used as an alternative to conventional portland cement for civil infrastructure applications. Some of the advantages of geopolymer
concrete are its fast setting time, rapid strength development, and its significantly reduced carbon footprint. In this study, aluminosilicate
geopolymers with different alkaline solutions [NaOH, KOH, Ba ðOHÞ2 , and LiOH] were prepared by mixing Class C (9.42% CaO) and Class
F-fly ash (1.29% CaO). The samples were cured under different experimental conditions and then tested for compressive strength. X-ray
diffraction (XRD) and scanning electron microscopy/energy dispersive spectroscopy (SEM/EDS) have been used to identify the new phases
formed in the geopolymeric matrix. The results revealed that microstructural properties of fly ash particles and calcium content have a
significant effect on the setting time and the compressive strength of geopolymer concrete, and the structure of the formed geopolymer
is typically glasslike. The early polymerization of geopolymer concrete is dependent on the concentration of the sodium hydroxide solution
(NaOH). The exclusive use of NaOH showed the highest compressive strength when compared with other combinations of alkali hydroxides.
DOI: 10.1061/(ASCE)MT.1943-5533.0001656. © 2016 American Society of Civil Engineers.
Author keywords: Fly ash (FA); Geopolymers; Microstructure; Mechanical strength.

Introduction of studies have examined the chemistry behind geopolymer binders

The worldwide cement industry emits approximately 1.65 billion
tons of greenhouse gases annually (Malhotra 2002; McCaffrey
2002; Hardjito et al. 2004), which has a significant effect on global
warming. The production of one ton of portland cement (PC) emits
approximately one ton of CO2 into the atmosphere (Davidovits
1994; McCaffrey 2002). Because of the production of portland ce-
ment, it is estimated that by the year 2020, emissions will rise above
the current levels by approximately 50% (Naik et al. 2005; Vijai
et al. 2012). Geopolymers, an inorganic binder, is a viable alterna-
tive to portland cement. A French scientist, Joseph Davidovits
coined the word geopolymer in 1991 (Davidovits 1991), to re-
present a broad range of materials characterized by networks of
inorganic molecules. It is an alkali-activated binder, produced by
a polymeric reaction of alkaline liquids with the silicon and the
aluminum oxides in source materials of geological origin, like
metakaolinite (calcined kaolinite), or by-product materials such
as fly ash (FA) and rice husk ash (Davidovits 1999). A number
1 crete (Sofi et al. 2007; Fernandez-Jimenez et al. 2006; Hardjito and
Research Assistant, Dept. of Material Science and Engineering, Univ.
of Texas at Arlington, Nedderman Hall 417, 416 Yates St., Arlington, TX
76019. E-mail: gaurav.nagalia@mavs.uta.edu
2
Postdoctoral Researcher, Dept. of Civil Engineering, Univ. of Texas
at Arlington, Nedderman Hall 417, 416 Yates St., Arlington, TX 76019.
E-mail: ypark@uta.edu
3
Professor, Dept. of Civil Engineering, Univ. of Texas at Arlington,
Nedderman Hall 417, 416 Yates St., Arlington, TX 76019. E-mail:
abolmaali@uta.edu
4
Professor, Dept. of Material Science and Engineering, Univ. of Texas
at Arlington, Nedderman Hall 417, 416 Yates St., Arlington, TX 76019
(corresponding author). E-mail: aswath@uta.edu
Note. This manuscript was submitted on December 10, 2015; approved
on March 30, 2016; published online on June 23, 2016. Discussion period
open until November 23, 2016; separate discussions must be submitted for
individual papers. This paper is part of the Journal of Materials in Civil
Engineering, © ASCE, ISSN 0899-1561.
to provide insight to geopolymerization kinetics. These studies are
typically performed using a highly pure source of silica and alu-
mina, such as metakaolin (Provis and van Deventer 2007; De Silva
and Sagoe-Crenstil 2008; Provis et al. 2005).
Fly ash exhibits a significantly different particle morphology
and chemistry that affects the mechanical properties of the resulting
geopolymer (Provis et al. 2010) and typically contains other impu-
rities that vary from one fly ash source to another. Thus, it is not
easy to predict the properties of a fly ash–based geopolymer.
Several studies have been performed (Fernandez-Jimenez and
Palomo 2003; Van Jaarsveld et al. 2003; Diaz-Loya et al. 2010)
to identify the characteristics inherent to the fly ash that affect
its potential as source material for geopolymerization. Other studies
have focused on investigations that promote the use of geopolymer,
highlighting the environmental benefits of recycling fly ash into
geopolymer concrete (Van Jaarsveld et al. 2002; Weil et al. 2007).
Some studies have focused on developing an understanding of the
effects of mix proportions, activator solution concentrations, and
curing conditions on the mechanical properties of geopolymer con-
Rangan 2005). Limited information has been presented, however,
on some of the fundamental issues such as the variability in the fly
ash and its effect on geopolymer mechanical properties, and the
study of the kinetics of the geopolymerization process.
The main objective of this study is to determine the underlying
relationship between the chemical makeup of the fly ash and the
mechanical properties of the geopolymer that is formed by its re-
action with alkaline solutions. Two different sources of fly ash are
examined, one with low calcium content and the other with high
calcium content. The fabricated geopolymer cylinders were evalu-
ated in terms of chemical composition, microstructure properties,
and mechanical strength as a function of setting time, curing time,
and various mix designs. Discerning the relationships between
the physical, chemical, and crystallographic characteristics of fly
ash and the mechanical properties of geopolymer concrete is an

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 Table 1. Chemical Composition of Different Types of Fly Ash as the alkaline solution, water, and super plasticizer (SP), based on
Determined by XRF (Mass%) polycarboxylic ether with pH-value (20°C) from 6.5 to 8.5 were
Class C Class F added, then mixed with the source materials for another two to
Chemical composition (Rockdale-TX) (Stillesboro-GA) three minutes. For all specimens, amount of water and SP were
SiO2 (silicon dioxide) 58.05 54.70
constant with 40 kg=m3 and 37 kg=m3 , respectively. The con-
Al2 O3 (aluminum oxide) 21.59 29.00 trolled geopolymer concrete mix design was 408 kg=m3
Fe2 O3 (iron oxide) 5.10 6.74 (687 lb=yd3 ) of fly ash, 1,320 kg=m3 (2,222 lb=yd3 ) of coarse ag-
MgO (magnesium oxide) 1.86 0.80 gregate, 590 kg=m3 (993 lb=yd3 ) of sand (fine aggregate),
SO3 (sulfur trioxide) 0.39 0.10 40 kg=m3 (67 lb=yd3 ) of water, 37 kg=m3 (62 lb=yd3 ) of SP
Na2 O (available alkalis) 0.92 1.88 (20% solution) and 125 kg=m3 (210 lb=yd3 ) of alkaline solution
CaO (calcium oxide) 9.42 1.29 (sodium silicate + alkali hydroxides).
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important step toward producing large quantities of geopolymer
concrete with reasonably consistent and predictive engineering
properties.
Experimental Approach
The materials used in this research for the manufacturing of geo-
polymer concrete are low and high calcium fly ash (Class F and C)
as the source material, aggregates of different sizes (9.5 and
16 mm), alkali hydroxides, water, and super-plasticizers. The fly
ash used in this study came from Stillesboro, GA and Rockdale,
TX. Class F fly ash (from Stillesboro) contained 1.29% of CaO,
and Class C fly ash (from Rockdale) contained 9.42% of CaO.
Table 1 shows the chemical composition of the different types
of fly ash, as determined by X-ray fluorescence (XRF) analysis.
Four different alkali hydroxides (NaOH, KOH, BaðOHÞ2 and
LiOH) were employed in this study; combinations of these hydrox-
ide solutions and sodium silicate solution (Na2 SiO3 ) were also
studied.
Mixture Proportions
Based on the research on geopolymers available in the literature
and the experience gained during the preliminary experimental
work, the following ranges were selected for the constituents of
the mixtures:
• Four different alkali hydroxides (NaOH, KOH, BaðOHÞ2 ,
LiOH) and combinations thereof;
• Ratio of sodium silicate to alkali hydroxide ¼ 2.0;
• Ratio of activator solution to fly ash ¼ 0.31;
• Molarity of NaOH ¼ 8M, 12M, and 14M;
• Aggregates (coarse and fine) constituted 75–80% of entire mix
by mass; and
• Super Plasticizer constituted (20% solution) = 2% of entire mix
(except fine aggregate) by mass.
Geopolymer Mix Procedure
Consistency was a major component of the basic procedure for pre-
paring the mix. The required amount of sodium hydroxide flakes
were weighed and dissolved in a measured quantity of water to
prepare either an 8 or 14M solution (For 1M sodium hydroxide
solution, 40 g of NaOH flakes were dissolved in one liter of water).
Because the reaction is exothermic, the solution was allowed to
cool for an hour before a measured quantity of sodium silicate sol-
ution was added to it. A 2∶1 mass ratio of sodium silicate to sodium
hydroxide solutions was prepared. This mixture of sodium hydrox-
ide and sodium silicate solutions was prepared 24 h before use.
Measured quantities of aggregates, sand, and fly ash were added
to the concrete mixer and mixed for approximately two minutes,
until a uniform mixture was obtained. Measured quantities of
Curing Conditions
Curing is a term in polymer chemistry that refers to the toughening
or hardening of a polymer material by the cross-linking of polymer
chains, brought about by electron beams, heat, or chemical addi-
tives. In the case of geopolymer concrete, curing is an ongoing pro-
cess and can be accelerated by thermal activation. The different
curing methods used in this research included:
• Oven-curing : dry conditions, 55°C (131°F) and 70°C (158°F);
• Steam-curing : 100% humidity, 46°C (115°F); and
• Curing at room temperature, 25°C (77°F).
These curing methods were utilized to determine the effect of
different temperatures and the curing environment on the mechani-
cal properties of the geopolymer. The geopolymer cylinders were
wrapped in plastic and kept in a chamber under the necessary con-
ditions. Lastly, curing at room temperature was carried out so that
there would be a reference for comparison.
Compressive Cylinder Test
Cylinders were produced from different mix designs and tested ac-
cording to ASTM C39 (ASTM 2015). In this test, the compressive
load was applied axially to the cylinder at a rate within a prescribed
range until failure occurred. The compressive strength of the cyl-
inder was then determined by dividing the maximum load obtained
during the test by the cross-sectional area of the cylinder. Cylinders
with the dimensions of 100 × 200 mm (4 × 8 in:) were produced
with the help of a table-type vibrator, demolded after six hours
casting and tested at 1, 3, 7, and in some cases, 28 days after pro-
duction. Since the cylinders were prepared by using the dry cast
method, the compressive strength obtained in 7 days was sufficient
for comparison purpose. At least eight cylinders were prepared
from each mix design. After curing, the cylinders were stripped
from their molds and capped at each end to create a smooth and
leveled testing surface [ASTM C617 (ASTM 2012)]. Sulfur flake
was used as a capping material. The rate at which the cylinder was
tested was 0.25  0.05 MPa=s (35  7 psi=s). This was applied
continuously and slowly, without shock, throughout the test. For
all mix designs, at least eight specimens were produced (1st group:
three specimens for compressive strength/2nd group:-three speci-
mens for compressive strength/3rd group: two specimens for mi-
crostructural analysis).
Mechanical Test Results
This study was aimed at gaining a better understanding of the
relationship between the chemical composition of the fly ash, its
reaction with alkaline materials, and the mechanical properties
of the geopolymer. To better understand this relationship, different
formulations of geopolymer mixes were created, and the geopol-
ymer concrete cylinders were tested for compressive strength under
different conditions. Two sources of fly ash were used for the

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 Table 2. Mix Designs of Geopolymer Concrete With Respect To Hydroxide Solutions
Aggregate (kg=m3 )
Mix Fly ash Na2 SiO3 Concrete of Na2 SiO3 =
numbera class-C (kg=m3 ) 9.5 (mm) 16 (mm) Sand Hydroxide solution solution (kg=m3 ) hydroxide solution (M) hydroxide solution
1 408b 1,320 — 590 100% NaOH 83.2 14 2.0
2, 22 408b 1,320 — 590 100% KOH 83.2 14 2.0
3 408b 1,320 — 590 100% BaðOHÞ2 83.2 14 2.0
4 408b 1,320 — 590 100% LiOH 83.2 14 2.0
5 408b 1,320 — 590 NaOH∶KOH ¼ 9∶1 83.2 14 2.0
6, 22 408b 1,320 — 590 NaOH∶BaðOHÞ2 ¼ 9∶1 83.2 14 2.0
7 408b 1,320 — 590 NaOH∶LiOH ¼ 9∶1 83.2 14 2.0
8 408b 1,320 — 590 NaOH∶AlðOHÞ3 ¼ 9∶1 83.2 14 2.0
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9 408b 1,320 — 590 NaOH∶KOH ¼ 5∶5 83.2 14 2.0

10 408b 1,320 — 590 NaOH∶BaðOHÞ2 ¼ 5∶5 83.2 14 2.0
11 408b 1,320 — 590 NaOH∶LiOH ¼ 5∶5 83.2 14 2.0
12 408b 1,320 — 590 NaOH∶AlðOHÞ3 ¼ 5∶5 83.2 14 2.0
a
At least 8 specimens were produced and tested for each case.
b
CaO of 9.42%.

mixes: (1) 9.42% CaO fly ash (Class C) and (2) 1.29% CaO fly ash
(Class F). Some of the factors which have been known to affect the
strength of the mix are:
1. Type of fly ash [varies with the percentage of CaO
(9.42%, 1.29%)];
2. Source of fly ash;
3. Type of alkaline solution used [NaOH, KOH, BaðOHÞ2
and LiOH];
4. Molarity of alkaline solution (8, 12, and 14M);
5. Source material aggregate size;
6. Curing time (1, 3, and 7 days); and
7. Curing temperature (46, 55, and 70°C).
Alkaline Solutions
The alkaline solutions interacted with the aluminosilicates to
generate a new binder, such as alkaline-earth hydroxides [αOH,
α ðOHÞ2 ]; acid salts (α2 CO3 , Na2 SO4 , and CaSO4 ); and
α2 OðnÞSiO2 -type siliceous salts, where α is an alkaline ion such
as Na, K, or Li (Torres-Carrasco and Puertas 2015). All other
parameters were kept constant, and only the type of alkaline sol-
ution [NaOH, KOH, Ba ðOHÞ2 and LiOH] varied with 9.42% CaO
fly ash. All the mixes were cured at 46°C (115°F) for 24 h and then
tested for compressive strength after 7 days. The mixtures shown in
Table 2 to examined the effect of using different combination of
alkaline hydroxide solutions on the compressive strength of geo-
polymer concrete.
All the mixes from these tables were based on the 9.42% CaO
fly ash with 14 M alkaline solution. The only parameter that varied
was the type of alkaline hydroxide solution.
Fig. 1(a) depicts the data for replacing 100% NaOH with various
other alkaline solutions. Results showed that using any alkaline sol-
ution other than sodium hydroxide solution (NaOH) significantly
reduced the compressive strength. Fig. 1(b) depicts the replacement
of NaOH, the only alkaline complex mix which comes close to the
100% sodium hydroxide (NaOH) mix, with a 90% NaOH þ 10%
KOH solution. Fig. 1(c) shows that the compressive strength of
the cured cylinders made by replacing half of the NaOH with other
mixes was much lower than those made with 100% NaOH mix. By
comparing Figs. 1(a–c), it becomes obvious that as the amount of
sodium hydroxide in the alkaline solution was reduced, the strength
reduced drastically. Although, there was some amount of curing
reaction taking place, as is shown from comparing the one-day
compressive strength results to the three-day compressive strength
results, the increase was too small to be considered significant.
It can therefore be postulated that a significant amount of curing
occurs in the first 24 h. In terms of compressive strength, the most
effective alkaline solution was NaOH, which is consistent with the
results of Provis et al. (2005) and Palacios and Puertas (2007).
Molarity of Solution
Mixes 13 through 16 in Table 3 were formulated to study the effect
the concentration of the sodium hydroxide (NaOH) solution has, in
terms of molarity, on the compressive strength of the geopolymer
concrete.
Two types of fly ash were considered: 9.42% CaO and 1.29%
CaO. All the mixes were cured at 46°C (115°F) for 24 h and then
tested for compressive strength after 7 days. According to Fig. 2,
with an increase in molarity of the sodium hydroxide solution, there
was an increase in the compressive strength for the 9.42% CaO fly
ash–based geopolymer and a decrease in the compressive strength
of the 1.29% CaO fly ash–based geopolymer. The higher CaO fly
ash was able to react with the higher molarity NaOH, resulting in an
increase in strength. The lower CaO fly ash had an incomplete
reaction with CaO, resulting in lower compressive strength. This
indicates that the compressive strength of the geopolymer concrete
is dependent on an optimum ratio of CaO to alkaline solution.
Increase in compressive strength with higher concentration of al-
kaline solution and CaO content might be attributed to the change
in microstructure of geopolymer. This is probably a calcium alu-
minosilicate glass structure that is significantly more reactive with
water than the siliceous glass structure (Palomo et al. 1999) and
leads to the formation of calcium silicate hydrate compounds, in
addition to the geopolymerization products, augmenting the
mechanical strength of the hardened matrix (see section “X-ray
Diffraction (XRD) Analysis”). Moreover, there was also a domi-
nant presence of calcium silicate glass structure, which was reactive
with water and formed calcium silicate hydrated compounds that
boosted the mechanical strength values of the resultant geopolymer
[Eq. (1)]
Size and Amount of Aggregates (16 or 9.5 mm or Both)
As shown in Table 4, mixes 17 through 22 were prepared to study
the effect of size and amount of aggregates on the compressive
strength of the concrete. Three types of mixes with different sizes
and amounts of aggregates were prepared. Mixes 17 to 19 were
based on the 9.42% CaO fly ash, and mixes 20 to 22 were based
on the 1.29% CaO. Fourteen (14) M alkaline solutions were used in
all 6 mixes as shown in Fig. 3. The cylinders cast from these mixes

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Fig. 1. Effect of complex alkaline hydroxide solutions on average compressive strength

Table 3. Mix Designs of Geopolymer Concrete With Respect To Molarity

Aggregate (kg=m3 )
Mix Fly ash Hydroxide Na2 SiO3 solution Concrete of hydroxide Na2 SiO3 =
number (kg=m3 ) 9.5 (mm) 16 (mm) Sand solution (kg=m3 ) (kg=m3 ) solution (M) hydroxide solution
13 408a 1,320 — 590 41.6 (100% NaOH) 83.2 8 2.0
14, 22 408a 1,320 — 590 41.6 (100% NaOH) 83.2 14 2.0
15 408b 1,320 — 590 41.6 (100% NaOH) 83.2 8 2.0
16 408b 1,320 — 590 41.6 (100% NaOH) 83.2 14 2.0
a
CaO = 9.42%.
b
CaO = 1.29%.

were cured at 46°C (115°F) in the oven for 24 h, then tested for
compressive strength after 7 days.
A substantial change occurred on the surface area of the aggre-
gates in which the chemical reaction between the fly ash and the
alkaline solution took place. The total weight of the aggregates for
the three mixes was kept at 53 kg. However, mix A had larger
(16 mm), medium (9.5 mm), and small (sand) aggregates, whereas
mixes B and C were composed of different combinations of
medium and small aggregates. Comparison of the compressive
strength for mixes A and B makes it evident that there was only
a slight deterioration in the properties of high CaO fly ash as the
size of the aggregates changed from large to medium size as shown
in Fig. 3. When mixes B and C are compared, however, it is clearly
evident that as a higher proportion of finer aggregates was used, the
Fig. 2. Effect of molarity of solution on the average compressive
properties deteriorated significantly. This trend was also observed
strength
in fly ash with a lower CaO content; however, those mixes had poor

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 Table 4. Mix Designs of Geopolymer Concrete With Respect To Size of Aggregates
Aggregate (kg=m3 )
Mix Fly ash Hydroxide Na2 SiO3 Concrete of hydroxide Na2 SiO3 =
number (kg=m3 ) 9.5 (mm) 16 (mm) Sand solution (kg=m3 ) solution (kg=m3 ) solution (M) hydroxide solution
17 408a 830 250 830 41.6 (100% NaOH) 83.2 14 2.0
18b, 22 408a 1,320 — 590 41.6 (100% NaOH) 83.2 14 2.0
19 408a 990 — 920 41.6 (100% NaOH) 83.2 14 2.0
20 408c 830 250 830 41.6 (100% NaOH) 83.2 14 2.0
21 408c 1,320 — 590 41.6 (100% NaOH) 83.2 14 2.0
22 408c 990 — 920 41.6 (100% NaOH) 83.2 14 2.0
a
CaO = 9.42%.
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b
Same mixture of Mix-1.
c
CaO = 1.29%.

Fig. 3. Average compressive strength versus type of mix

Table 5. Mix Designs of Geopolymer Concrete With Respect To Curing Method

Aggregate (kg=m3 )
Mix Fly ash Hydroxide Concrete of hydroxide Curing Curing
number (kg=m3 ) 9.5 (mm) 16 (mm) Sand solution (kg=m3 ) solution (M) method temperature (°C)
23 408a 1,320 — 590 41.6 (100% NaOH) 8 Steam 46
24, 22 408a 1,320 — 590 41.6 (100% NaOH) 8 Oven 55
25 408a 1,320 — 590 41.6 (100% NaOH) 8 Oven 70
26 408a 1,320 — 590 41.6 (100% NaOH) 14 Steam 46
27 408a 1,320 — 590 41.6 (100% NaOH) 14 Oven 55
28 408a 1,320 — 590 41.6 (100% NaOH) 14 Oven 70
a
CaO = 9.42%.

properties to start with, as the CaO content was much smaller. It can
be concluded that the percentage of CaO present and the amounts
of medium and fine-sized aggregates in fly ash play a significant
role in the compressive strength of the geopolymer concrete.
Curing Temperature and Curing Method
Mixes 23 through 28 in Table 5 were made so that the effect of
different curing temperatures and curing methods on the compres-
sive strength of the geopolymer concrete could be studied. The
curing methods included oven curing and steam curing. The tests
were carried out for 9.42% CaO fly ash–based geopolymer for both
8M and 14M alkaline solutions. The cylinders cast were cured at
46°C (115°F), 55°C (131°F), and 70°C (158°F) for 24 h, then tested
for compressive strength after 7 days. The compression strength
detailed in Fig. 4 provides details on the role of temperature
and environment on the properties of the geopolymer. It is evident
that the oven-cured material with the highest temperature had the
best properties. Steam curing was carried out at 100% humidity to
avoid evaporation of water from the geopolymer concrete.
In Fig. 4, it can be observed that the compressive strength in-
creased with an increase in temperature. The highest compressive
strength was obtained by oven curing at 70°C (158°F), which is
almost 50% higher than the temperatures used for steam-cured
specimens. It can be concluded that the NaOH reaction that took
place was a temperature-driven process. In addition, 8M NaOH is
not sufficient to complete the reaction with fly ash; 14M NaOH
is needed to ensure reaction with fly ash.
Curing Time
Mixes 29 through 32 in Table 6 were prepared to study the effect of
curing time on the compressive strength of the concrete. The mixes
for both the 8 and 14M alkaline solutions were based on the 9.42%
CaO fly ash–based geopolymer. The mixes were cured for 24 and
48 h in the oven at 55°C (131°F), then, after 7 days, were tested for

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Fig. 4. Average compressive strength versus curing conditions for
9.42% CaO fly ash–based geopolymer
compressive strength. Fig. 5 shows that the mix cured for 48 h
yielded higher compressive strength than the mix cured for 24 h.
Thus, it can be concluded that the polymerization reaction that took
place was time-dependent. The higher molarity of NaOH enhanced
the kinetics of the reaction, resulting in peak strength being
achieved after one day; in the lower molarity NaOH geopolymer,
there was a significant increase in strength between one and two
days. The early polymerization of the geopolymer concrete is de-
pendent on NaOH concentration.
In summary of compressive strength test results, the cylinder
compressive strength of the geopolymer concrete increase with
(1) the increase in the amount of sodium hydroxide in alkaline
solution, (2) the increase of concentration of alkaline solution,
(3) the increase of CaO content, and (4) the increase in curing
temperature. The highest compressive strength was obtained when
the class C fly ash (CaO: 9.42%) was activated by higher concen-
trated sodium hydroxide–based alkaline solution with higher
curing temperature.
Microstructural and Chemical Analysis Results
The primary focus of this study was to pinpoint the variables that
affect the mechanical strength of geopolymer. This was accom-
plished by identifying the physical, chemical, and crystallographic
factors of the fly ash and the formed geopolymer by X-ray diffrac-
tion (XRD), scanning electron microscopy (SEM), and energy dis-
persive spectroscopy (EDS) analyses. Microstructural and chemical
analyses were performed, using a single class fly ash (9.42% CaO)
as a potential source material for geopolymer concrete as shown
in Fig. 6.
Fig. 5. Average compressive strength versus time for 9.42% CaO fly
ash–based geopolymer
Combinatorial Study of Molarity of NaOH, Cure Time,
and Temperature of Properties of Geopolymer with
9.42% CaO Fly Ash
The attributes of the geopolymer mix that are considerably influ-
enced by fly ash characteristics are the setting time and the overall
mechanical properties. The setting time is influenced primarily by
the CaO content in fly ash. To reduce the number of dependent
variables, compressive strength was the only mechanical property
that was used as a response value. The compressive strength of geo-
polymer cement is dependent on reaction of the fly ash with NaOH
and Na2 SiO3 . For this mix design, three different concentrations of
sodium hydroxide solutions (8, 12, and 14M) and two curing tem-
peratures of 46°C (115°F) and 70°C (158°F) were used. The cast
cylinders were tested for compressive strength after 1, 7, and
28 days. Three batches of 36 cylinders were made to understand
and evaluate the underlying relationship between the chemical
composition of fly ash and the mechanical strength of the geopol-
ymer formed.
Fig. 6 shows the variations of compressive strength of high
calcium fly ash–based geopolymer concrete after 1, 7, and 28 days.
As depicted in Fig. 6, a significant increase in the compressive
strength was observed when the material in the geopolymer con-
crete, formed by reacting with 8M, 12M, and 14M NaOH and cured
at both 46°C (115°F) and 70°C (158°F), aged from 1 to 28 days. The
setting times measured in accordance with ASTM C807-13 (using a
standard Vicat needle) for all 8, 12, and 14M NaOH mixes and
were measured from the time the fly ash made a contact with NaOH
solution until the penetration of a two millimeter diameter needle
was less than 10 mm. The setting time results were the average of
three specimens and were observed to be approximately 20, 16, and
8 min for 8, 12, and 14M NaOH mixes, respectively. The setting
time was influenced primarily by the CaO content in the fly ash and
initial strength development increased as the molarity of NaOH

Table 6. Mix Designs of Geopolymer Concrete With Respect To Curing Time

Aggregate (kg=m3 )
Mix Fly ash Hydroxide Concrete of hydroxide Curing Oven-curing
number (kg=m3 ) 9.5 (mm) 16 (mm) Sand solution (kg=m3 ) solution (M) time (h) temperature (°C)
29 408a 1,320 — 590 41.6 (100% NaOH) 8 24 55
30, 22 408a 1,320 — 590 41.6 (100% NaOH) 8 48 55
31 408a 1,320 — 590 41.6 (100% NaOH) 14 24 55
32 408a 1,320 — 590 41.6 (100% NaOH) 14 48 55
a
CaO = 9.42%.

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Fig. 6. Compressive strength versus time for 9.42% CaO fly ash–based geopolymer for microstructural analysis

increased. It is consistent results with Diaz-Loya et al. (2011)
and Hardjito and Rangan (2005). However, mix 23 (9.42%
Cao /8M/ 46°C steam-curing) was found to be too weak to produce
reasonable compressive strength. Compressive strength increased
with the increase of curing time, curing temperature, and the
molarity of NaOH.
(SiO2 ) reduced significantly as the curing time and molarity were
increased. The intensity of quartz peak decreased with a concomi-
tant increase in the peak intensity of a sodium alumina silicate com-
plex such as NaAlSi3 O8 with the increase of molarity and curing
time. The main peaks corresponded to NaAlSi3 O8 , which was
formed because of the interaction between the Al2 O3 and SiO2

X-ray Diffraction (XRD) Analysis

A mineralogical analysis by X-ray diffraction (XRD) was per-
formed to explain the mechanical performances of mixes as shown
in Fig. 6. XRD data were obtained by using a Bragg-Brentano
geometry powder diffractometer with the following testing param-
eters: 40KV, 30mA, and CuKα radiation. The XRD patterns were
obtained by a scanning rate of one degree per minute from 10 to 80
degrees (2θ) and steps of 0.05 degrees (2θ). The wave length se-
lected was 6.065 × 10−7 in (15.40562 nm) (Cu). Fig. 7 shows the
X-ray diffraction pattern with details of the crystalline phases
present in the fly ash with 9.42% CaO. Instead of sharp diffraction
peaks, a broad diffusion indicated a noncrystalline state.
A single letter or set of letters was assigned to each phase to
facilitate easier representation. The major components of raw fly
ash are quartz (SiO2 ) and sodium-aluminum-silica complex (de-
noted X), such as albite and microcline. The other trace materials
present in this curve were alumina, larnite, brownmillerite, peri-
clase and calcite. The presence of a broad elevation, i.e., hump from
20° to 40°, indicates the presence of amorphous silicates, which are
difficult to characterize. Amorphous compounds dissolve easier
than crystalline compounds during the first step of geopolymeriza-
tion (dissolution of species), yielding higher amounts of reactive
SiO2 and Al2 O3 to combine during the precipitation of the geopoly-
meric reaction product. This results in a higher degree of geopol-
ymerization and higher mechanical strength (Fernandez-Jimenez
and Palomo 2003; Van Jaarsveld et al. 2003).
Fig. 8 illustrates the XRD pattern for 9.42% CaO raw fly ash and
fly ash–based geopolymer fabricated by reactions with 8, 12, and
14M sodium hydroxide solutions, cured at 46°C (115°F) and tested
after 1 day and 28 days. Approximately 5 g of the geopolymer was
collected after carrying out the compressive test for the cast cylin-
der. The collected pieces of geopolymer were ground to a fine pow-
Fig. 7. X-ray diffraction pattern 9.42% CaO fly ash; the peaks are iden-
der by using a mortar and pestle. This powder consisted of particles
tified as follows: Q = quartz or SiO2, C = calcite or CaCO3,
with sizes of 100 μm or less. This was insured by passing the
A ¼ alumina ¼ Al2 O3 , X = complex silicate such as albite and mono-
ground powder through a sieve shaker with a 100 μm sieve. In
cline, M = mullite or Al6 Si2 O13, B = brownmillerite or Ca2 ðAl; FeÞ2 O5,
all cases, the diffraction pattern changed significantly after the
P = periclase or MgO, and L = larnite or Ca2 SiO4
fly ash was activated by NaOH (8/12/14M). The peak of Quartz

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Fig. 8. Comparison of X-ray pattern of 9.42% CaO fly ash and geo-
polymer made with fly ash and NaOH: (a) FLY ash; (b) fly ash + 8M
NaOH cured for one day; (c) fly ash + NaOH cured for 28 days; (d) fly
ash; (e) fly ash + 12M NaOH cured for one day; (f) fly ash + 12M
NaOH cured for 28 days; (g) fly ash; (h) FLY ash + 14 M NaOH cured
for one day; (i) Fly ash + 14M NaOH cured for 28 days; the peaks are
identified as follows, Q = quartz or SiO2, C = calcite or CaCO3,
A ¼ alumina ¼ Al2 O3 , X = complex silicate such as albite and mono-
cline, M = mullite or Al6 Si2 O13, B = brownmillerite or Ca2 ðAl; FeÞ2 O5,
P = periclase or MgO and L = larnite or Ca2 SiO4
present in the fly ash and the alkaline NaOH solution. The uniden-
tified complex peaks can be attributed to the formation of calcium
aluminum silicate hydrate glass structures in addition to the geo-
polymerization products augmenting the strength of the hardened
© ASCE
J. Mater. Civ. Eng., 2016, 28(12): 04016144
matrix. Comparison of the three samples tested at 1 day and 28 days
revealed a sharpening in the calcite peaks, which indicated a con-
tinuous reaction in the mix. The increase in mechanical strength
was the result of the reactive amorphous phase that cannot be
identified by X-ray diffraction. When comparing the XRD pattern
of the fly ash from Fig. 7 with the XRD patterns of the geopoly-
mers, it is shown that there was an obvious change in the fly ash
chemistry after crystalline phases such as quartz (SiO2 ) and mullite
(Al2 O3 · 2 SiO2 ) react with the alkali hydroxide. In addition, the
amount of residual fly ash was reduced with an increase in molarity
of NaOH and curing time. That indicates that a higher molarity of
NaOH accelerates the kinetics of the process. In addition, the broad
amorphous background feature in region 2θ ¼ 20–40°, presented
in all samples after thermal treatment, suggests that the main
reaction product formed was alkaline aluminosilicate glass with
low-ordered crystalline structure. This is probably a calcium alu-
minosilicate glass structure that is significantly more reactive with
water than the siliceous glass structure (Palomo et al. 1999) and
leads to the formation of calcium silicate hydrate compounds, in
addition to the geopolymerization products, augmenting the
mechanical strength of the hardened matrix.
Scanning Electron Microscopy (SEM) Energy
Dispersive Spectroscopy (EDS) Analysis
After sectioning, mounting, and polishing the surfaces, SEM
micrographs of the samples were measured using a Hitachi
S-3000N variable pressure scanning electron microscope. The di-
mensions of the piece were approximately 13 × 9 mm. These sam-
ples were then cast in epoxy to get a smooth surface finish. The cast
sample was cut and polished before coating it with a layer of
conductive silver to carry out the necessary imaging. Secondary
electron images were acquired to examine the ash particles’ mor-
phology and chemistry before and after the geopolymerization
process. The role of particle morphology has been emphasized
by many authors for its significant effect on the resulting geopol-
ymer (Provis et al. 2010; Duxson et al. 2005). For this analysis, the
working distance was approximately 10–25 mm, the accelerated
voltage was between 20 and 25 kV, and the images were observed
at 60–100X magnification. The scanning electron microscope was
equipped with an energy dispersive spectrometer that was used to
characterize the microstructure and the chemical compositions of
the 18 geopolymer samples.
Fig. 9 shows the elemental mapping of a geopolymer specimen
(9.42% CaO fly ash with 8M /14 M NaOH solution) oven cured at
70°C. This illustrates the different elemental species present in the
mix. The elementary chemical distribution of aluminosilicate glass
consisted primarily of silicon, calcium, aluminum, and smaller por-
tions of sodium, potassium, and iron, suggesting the formation of
silicate-activated glass by polymerization. The early polymeriza-
tion of the geopolymer concrete is dependent on NaOH concentra-
tion. As the concentration of NaOH increases, the intensity of EDS
curve on each chemical ingredient increases. This correlates with
the published works of Lee and Van Deventer (2002), which stated
that in a medium with a high concentration of dissolved silica, the
species dissolved from the surface of fly ash particles migrate from
the surface into the bulk solution. In addition to Si, Al, and Ca, a
small amount of Fe, Na, K, and Mg was also observed in the glass
by EDS analysis. These remnants (Fe, K, and Mg) obviously
represent the fly ash phases, which for various reasons, did not dis-
solve during alkali activation. The presence of silica may be attrib-
uted to the fine aggregates of sand present in the mix. This silica
phase was embedded in a sodium calcium silicate and calcium
aluminosilicate rich matrix. From these figures, it is obvious that
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Fig. 9. Elemental mapping of geopolymer cured at cured at 46°C for 7 days: (a) 8M NaOH þ 9.42% CaO fly ash; (b) 14M NaOH þ 9.42% CaO
fly ash

the main chemical species present were silicon and calcium. From
the elemental mapping, it is clear that there were three zones that
were present, which included a silicon-rich zone, a calcium-
enriched zone, and a complex zone which contained all species,
including calcium, silicon, aluminum, iron, sodium, oxygen, mag-
nesium, and carbon. All the crystalline phases were identified by
the X-ray diffraction method. The complex amorphous phase
seems to have formed a reaction zone around the unreacted silica
particles and may have been responsible for the binder properties in
the geopolymer concrete. The calcium-enriched zone must have
been from the calcium alumino silicate. These silica structures were
embedded in a thin layer of reacted material, which is characteristic
of a siliceous glass structure. Based on these EDS images, the
amorphous phase was identified as accumulation of feldspars.
There was also a dominant presence of calcium silicate glass struc-
ture, which was reactive with water and formed calcium silicate
hydrated compounds that boosted the mechanical strength values
of the resultant geopolymer. Although the CaO content does not
represent all of the CaO in the glass phase (a small amount of cal-
cium is contained in the crystalline phases), there is a strong cor-
relation between the CaO content and the mechanical strength of
the geopolymer. These structures could be attributed to the forma-
tion of feldspar-type amorphous materials. Silica and alumina are
the main precursors for geopolymer binder formation, and these
are assumed to dissolve from fly ash in a highly alkaline solution
and then recombine, using sodium as a charge-balancing agent to
form geopolymer glass. This is consistent with the results of
Davidovits (1994).
A comparison of Fig. 9(a) (8M NaOH and 9.42% CaO fly ash)
and Fig. 9(b) (14 M NaOH and 9.42 CaO fly ash] both cured at
46°C for a period of 7 days illustrates some distinctive differences.
The geopolymer with 8M NaOH has barely reacted SiO2 and there
is very little intermixing of the constituents. In contrast, the geo-
polymer with 14M NaOH exhibits significant interfacial reaction
as evidenced by the boundary layer between the SiO2 particles
and activated alkali solution. At the boundary of the SiO2 in the
14 M NaOH we can see evidence for the presence of of a sodium
calcium silicate, calcium aluminosilicate and possibly quarternary
sodium calcium aluminosilicate.
Some possible chemical reactions, based on dissolution and pre-
cipitation of Al, Ca and Si, observed from the XRD & SEM-EDS
study, are detailed in Eq. (1)

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Fig. 10. SEM images: (a) 9.42% Cao fly ash+8M NaOH; (b) 9.42% Cao fly ash+14M NaOH
NaOH þ Na2 SiO3 þ Al2 O3 þ CaO þ SiO2 → NaAlSi3 O8
þ Ca2 SiO4 þ a-SiOx ð1Þ
In addition, NaAlSi3 O8 can hydrate in the presence of water,
resulting in an increasingly alkaline amorphous glass ceramic
through the reactions in Eqs. (2) and (3)
NaAlSi3 O8 þ 5H2 O þ 3NaOH → AlðOHÞ4− þ 3ðOHÞ3SiO− þ 4Naþ
ð2Þ
KAlSi3 O8 þ 5H2 O þ 3NaOH → AlðOHÞ4−
þ 3ðOHÞ3 SiO− þ 3Naþ þ Kþ ð3Þ
From these equations, a relationship can be developed
between the mechanical properties and the chemical properties
of fly ash. When the molarity shifts from 8 to 14M, there typically
should be a shift in the reactions towards the right side. This
could result in the stimulation of precipitation of sodium silicate,
calcium silicate, and sodium aluminosilicate. In Eqs. (2) and (3),
the hydrated precipitates could be Nau Siv Alw Ox · H2 Oy , where
u ¼ 1  n1 , y ¼ 3  n2 , and w ¼ n3 , where n1 , n2 , and n3 are
fractional changes off stoichiometry with the overall neutrality
of the ionic glass maintained. These chemistries are typical of
common feldspars or hydrated feldspars. This could lead to
water deficiency and thus raise alkalinity of the mixture, promoting
kinetics of the polycondensation/geopolymerization reaction.
This may be one of the reasons for the increase in mechanical
strength for 9.42% CaO on changing the molarity of NaOH from
8M to 14M and/or increasing the cure time and/or temperature of
the cure.
Fig. 10 shows a glasslike matrix of the amorphous aluminosil-
icate glass in which some unreacted fly ash particles and pores are
embedded. The SEM image of the geopolymer formed with the 8M
NaOH shows a significantly larger number of pores and hollow
spheres than that of 14M NaOH geopolymer. This might be attrib-
uted to insufficient geopolymerization since the amount of NaOH
was not sufficient for complete conversion to NaAlSi3 O8 . Regard-
less of the concentration of alkaline solution, larger particles
(>20 um) do not react chemically, but become physically em-
bedded in the glassy matrix.
© ASCE 04016144-10
J. Mater. Civ. Eng., 2016, 28(12): 04016144
Conclusions
This is a comprehensive study that examines the role of fly ash
chemistry, type, and concentration of alkali hydroxides, cure tem-
perature and time, and mix designs of properties of geopolymer. It
shows that higher concentrations of CaO in the fly ash resulted in
significantly higher strengths in the finished geopolymer. Of the
different alkali hydroxides used to make the geopolymer, NaOH
was the only one that resulted in mechanical strengths that are
comparable to portland cement. Using mixtures of alkali hydrox-
ides did not provide any benefit. Higher curing temperatures and
longer curing times resulted in a significant increase in compressive
strength, and it is clear from the study that higher molarity of NaOH
improves kinetics, with the higher CaO containing fly ash. The
chemistry of the fly ash and the geopolymers were examined using
X-ray diffraction and scanning electron microscopy, coupled with
energy dispersive spectroscopy. Results indicated the formation of
NaAlSi3 O8 feldspar and an amorphous calcium silicate glassy
matrix. From this study, it appears that the water in the mix can
hydrate the silicates, resulting in an improvement in compressive
strength of the geopolymer.
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