Construction Materials Proceedings of the Institution of Civil Engineers

Construction Materials 164 December 2011 Issue CM6

Volume 164 Issue CM6
Utilisation of waste material in
geopolymeric concrete
Nuruddin, Qazi, Kusbiantoro and Shafiq
Pages 315–327 http://dx.doi.org/10.1680/coma.2011.164.6.315
Paper 1000045
Received 30/06/2010 Accepted 02/11/2010
Keywords: concrete technology & manufacture/strength and
testing of materials/waste management & disposal

ice | proceedings ICE Publishing: All rights reserved

Utilisation of waste material in

geopolymeric concrete
Muhammad Fadhil Nuruddin PhD Andri Kusbiantoro MSc
Associate Professor, University Teknology PETRONAS, Tronoh, Perak, PhD student, University Teknology PETRONAS, Tronoh, Perak, Malaysia
Malaysia Nasir Shafiq PhD
Sobia Anwar Qazi MSc Associate Professor, University Teknology PETRONAS, Tronoh, Perak,
PhD Student, University Teknology, MARA, Shah Alam, Malaysia Malaysia

Fly ash, silica fume and rice husks are hazardous waste materials that have no use and in the past have been landfilled.
However, landfilling is becoming expensive and causes contamination to soil and ground water. Utilisation of waste material
in concrete is also very effective in overcoming the problems caused by the production of cement; namely the emission of
carbon dioxide and degradation of the environment due to the quarrying of raw materials (limestone and clay) for the
production of cement. This research study was based on the complete elimination of ordinary Portland cement from concrete
that can achieve 28 days target cube strength in the range of 40–50 MPa with the emphasis on the curing techniques
applicable for in situ construction; namely ambient and external exposure curing. Fly ash was utilised as a base source
material and silica fume and microwave-incinerated rice husk ash were used as replacements for the fly ash by 3, 5 and 7%.
Alkaline activators, namely sodium hydroxide and sodium silicate solution were used as activators of silica and aluminium in
the source material and sugar was incorporated in the mix to increase the hardening time of the concrete. Compressive
strength, flexural strength and scanning electron microscopy tests were conducted on the specimens and the results showed
that at 3, 7, 28, 56 and 90 days the fly ash along with silica fume, microwave-incinerated rice husk ash and alkaline activators
could be a good replacement of cement. The compressive strength of external exposure curing for the geopolymeric concrete
reached up to 48?7 MPa at 28 days and this concrete had a well-developed microstructure shown by scanning electron
microscopy analysis. The flexural strength showed values which were comparable with ordinary Portland cement concrete.

1. Introduction decompose sufficiently to be used in manure (Zemke and

Material by-products such as fly ash (FA) and silica fume (SF)
which are derived from ever-expanding industrial processes or
waste, such as rice husks from agricultural activities, are
undesirable materials for the environment if they are not
properly disposed of. These materials may eventually find their
way to landfills, but landfills are becoming scarce and expensive
to maintain (Fytianos et al., 1998). Over time this may lead to a
waste disposal crisis. Fly ash is composed of smaller particle
sizes that contain some toxic elements such as arsenic,
chromium, boron, vanadium and antimony (Sushil and Batra,
2006). The toxic elements contained within the fly ash may be
leached from them after being placed in landfills. Unfortunately,
power plants produce millions of tonnes of fly ash annually, the
greater portion of which is mostly wasted in landfills at a cost of
around US$ 1 billion. The global production of fly ash is
expected to rise by 800 million tons annually in 2010 (Izquierdo
et al., 2009). The disposal costs of fly ash can be saved if, for
example, fly ash is used in the manufacture of concrete; the
actual cost of this fly ash is 11–22 cents/kg (Rohatgi et al., 2006).
On the other hand, disposal of rice husk is difficult because of
its low nutritional value; a long time period is required for it to
Woods, 2009). Almost 2.2 million of tons rice husks are
produced per year from agricultural activity in Malaysia,
contributing to an annual production of rice husks of 500–
600 million metric tonnes worldwide (Bouman et al., 2007).
The utilisation of waste material in concrete as a replacement for
cement can also be useful in overcoming problems caused by the
production of cement, namely the emission of carbon dioxide
and degradation of the environment due to quarrying of raw
materials (limestone and clay) for the production of cement.
Global concrete production in the world is expected to rise from
about 10 billion tons in 1995 to almost 16 billion tons in 2010
(Odd and Koji, 2000). Cement production also reached a new
record amount of 2?31 billion metric tons with an annual
increase of 5?5%, and that is expected to rise by 4?1% globally to
3?5 billion metric tonnes in 2013 (World Cement Industry, 2010).
The contribution of the global cement industry to greenhouse
gas emissions that give rise to global warming, is around
1?35 billion tons annually, which is 7% of the total man-made
greenhouse gas emissions in the Earth’s atmosphere (Malhotra,
2002). Apart from the issue of carbon dioxide emissions

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 Construction Materials Utilisation of waste material in
Volume 164 Issue CM6 geopolymeric concrete
Nuruddin, Qazi, Kusbiantoro and
Shafiq

derived from the production of cement, the quarrying of raw for the precast concrete industry such as adapting oven curing
materials (limestone and clay) for the production of cement is for the production of geopolymeric concrete (Fernández-
increasingly becoming a source of environmental degradation Jiménez et al., 2005; Rangan, 2008). Nonetheless, given the
(Naik, 2005). For example, to produce 1 ton of ordinary inherent strength and durability properties of polymer
Portland cement (OPC), 1?6 tons of raw materials are needed concrete, there is a dire need to develop its use further for in
and the rate of extraction of raw materials from the Earth is situ construction. This is an obvious gap in the previous
20% greater than the capacity of the Earth to replenish itself. research and the information obtained in the present study
Hence, raw materials consumed in 12 months would take 14?4 may help to provide a useful contribution.
months to be replenished (Naik, 2005).
2. Methodology
In 1979, Davidovits created and applied the term geopolymer
2.1 Material selection
because the process of polymerisation takes place, in which silica
The materials used in this research study were chosen according
and aluminium, present in the source material (i.e. fly ash (FA)/
to specifications that met the requirements of the appropriate
silica fume (SF)/rice husk), reacts with the alkaline liquid to
British Standards as well as the objectives of this research.
produce binders. Geopolymeric cements produced in this
manner produce 80 to 90% less carbon dioxide emissions in
The FA was obtained from Manjung power station, Lumut,
comparison with that produced in OPC (Davidovits, 2008).
Perak, Malaysia. The densified SF was obtained from Elkem
Such reductions in carbon dioxide emissions ultimately support
Materials (Malaysia) and had a bulk density of 500–700 kg/m3,
decreases in global warming and the depletion of ozone layer.
whereas the microwave-incinerated rice husk (MIHRA) was
obtained from the Bernas rice-milling plant, Kuala Selangor,
For a geopolymer concrete, the polymerisation occurs through
Malaysia. The chemical compositions of FA, SF and MIRHA
a condensation process in which water and heat is released
are shown in Table 1.
during the endothermic chemical reaction. Within the geo-
polymerisation process, the polycondensation of alumino-
The coarse aggregate used in this experiment was crushed
silicate oxides (Si2O5, Al2O2) with alkali polysilicates (sodium
granite stone with a maximum size of 20 mm (BSI, 1989)
or potassium silicate) takes place producing silica (Si)–oxygen
whereas the fine aggregate was a natural Malaysian sand with
(O)–aluminium (Al) bonds (Hardjito and Rangan, 2005).
a fineness modulus of 2?7, classified in zone 3. Fine aggregate
was also sieved to exclude sizes of less than 5 mm.
The chemical reaction comprises the following steps (Xu and
Van Deventer, 2000)
Sodium silicate (Na2SiO3; Grade A53) was used in solution and
mixed with 56?31% (wt) of water, 29?43% (wt) of silica oxide
(a) dissolution of silica and aluminium atoms from the source
(SiO2) and 14?26% (wt) of sodium oxide (Na2O). Sodium
material through the action of hydroxide ions
hydroxide (NaOH) used was in the form of pellets. The
(b) transport, orientation or condensation of precursor ions
concentration of the sodium hydroxide solution was 8 mol/l
into monomers
and 29?4% (wt) of pellets were added to the water to make 1 kg
(c) polymerisation (through the polycondensation process) of solution.
and set of monomers into geopolymeric structures
Sugar was used to increase the setting time of concrete. The
The hardening of concrete depends on curing temperature and intention in adding refined white sugar to the concrete mix was
curing time. For FA-based concrete, the setting time was
decreased by a factor of six when the temperature was increased
Compounds FA: % SF: % MIRHA: %
from 6 to 80 ˚C (Brooks, 2002) and according to Wang et al.
(2004), the increased temperature during cure gives rise to SO2 51?19 96?36 86?10
pozzolanic reactions. The reaction of FA is very slow at ambient Al2O3 24?00 0?20 0?17
temperatures (Puertas et al., 2000) and this delays the initiation Fe2O3 6?60 0?77 2?87
of the setting of concrete (Kirschner and Harmuth, 2004). CaO 5?57 0?23 1?03
MgO 2?40 0?52 0?84
Previously, research has been completed on the development of SO3 0?88 0?55 0?41
mixture proportions for FA-based geopolymer concrete K2O 1?14 1?02 4?65
(Hardjito et al., 2004) and for which were determined the Na2O 2?12 0?1
short-term and long-term performance properties of mixes
having low calcium content (Wallah and Rangan, 2006). Table 1. Chemical composition of FA MIRHA and SF
Researchers have up to now only found solutions appropriate

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 Construction Materials Utilisation of waste material in
Volume 164 Issue CM6 geopolymeric concrete
Nuruddin, Qazi, Kusbiantoro and
Shafiq

Type of Fly ash: MIRHA/ silica MIRHA/ silica Coarse agg.: Fine agg.: NaOH: Na2SiO3: Extra water/ Sugar/3%:
curing kg/m3 fume: % fume: kg/m3 kg/m3 kg/m3 kh/m3 kg/m3 10%: kg/m3 kg/m3

Ambient 350 0 0 1200 645 41 103 35 10?5

curing 339?5 3 10?5
332?5 5 17?5
325?5 7 24?5
External 350 0 0 1200 645 41 103 35 10?5
exposure 339?5 3 10?5
curing 332?5 5 17?5
325?5 7 24?5

Table 2. Mix design proportions

to prevent the cement from fully combining with the water and using a digital compressive testing machine. Three concrete
thus retard the hardening process (McDonnell, 2006; Nuruddin cubes at ages of 3, 7, 28, 56 and 90 days were tested. During the
et al., 2009). Sugar is an organic compound which is chemically testing, the concrete cubes were loaded at a constant rate of
named as sucrose or saccharose. The molecular formula of sugar 6?8 kN/s without any suddenly applied loads.
used in this study is C12H22O11. Water used in the mix was tap
water in accordance with BS 3148:1980 (BSI, 1980). Flexural strength tests were completed according to BS EN 12390-
5 (BSI, 2000) using a 2000 kN digital compressive and flexural
2.2 Design of mix proportions testing machine. Beams of dimensions 100 mm 6 100 mm 6
The proportions of the different materials used in the mix design 500 mm were cast, cured and tested for each mix after 28 days of
are given in Table 2. The base binder for all mixes was FA (bulk curing.
density of 350 kg/m3). The FA used in the control mix was
replaced by 3, 5 and 7% of SF and MIRHA. All other material Scanning electron microscopy (SEM) was performed with a
quantities were kept constant such that the effects of replace- LEO 1430 VP scanning electron microscope using Inca X-Sight
ment of FA with SF and MIRHA on the strength, both in Oxford Instruments software. Specimens of 0?5 mm diameter
compression and flexure, and the workability properties of the were cored from sample cubes of concrete that had been cured
concrete could be determined. The sodium silicate to sodium for 28 days.
hydroxide weight ratio was 2?5 and coarse to fine aggregate
weight ratio was approximately 1?86. 3. Results and discussion
3.1 Properties of fresh geopolymeric concrete
Sugar was incorporated into the mix in proportions of 3% by
In order to find out the fresh properties of geopolymeric
weight of the total binder. Extra water (other than the water
concrete, its workability was measured through a slump test.
present in the alkaline solutions) was added to the mixture
Extra water (10%) was added to all the mixes, decided as an
equal to 10% by weight of the total binder to ensure the
appropriate amount after several trial mixes. Slump test results
required workability (Table 2).
are shown in Table 3. To improve the workability of geo-
polymeric concrete, naphthalene-based superplasticiser was
2.3 Casting and curing
Cubes of concrete of dimension 100 mm were cast and after 24 h
of casting, the moulds were opened according to EN 12390-1 Type of mix Slump: mm
(CEN, 1996). Specimens were cured under two types of conditions:
FA 230
ambient and external exposure conditions. For ambient curing
FA-MIRHA 3% 220
conditions, samples were placed in the shade outside the
FA-MIRHA 5% 210
laboratory, whereas for the curing of samples in external exposure
FA-MIRHA 7% 200
conditions, samples were placed in a stand covered by a
FA-SF 3% 230
transparent white plastic sheet and exposed to direct sunlight.
FA-SF 5% 230
FA-SF 7% 230
2.4 Test procedure
Compressive strength tests were performed on concrete Table 3. Slump test results for each mix
samples in accordance with BS EN 12390-3:2002 (BSI, 2002)

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 Construction Materials
Volume 164 Issue CM6
10 mm EHT = 5.00 kV Signal A = SE2
WD = 7.2 mm Mag = 1.00 KX
Figure 1. FESEM of fly ash
also investigated (i.e. used by Rangan (2008)) but the concrete
hardened in a short span of time due to the fast setting time of
geopolymeric concrete which made the preparation of samples
harder with prolonged vibrations for compaction. In the
present study, sugar was added to delay the setting time of the
concrete making it easier to produce the samples.
Fly ash particles are spherical in shape with smooth surfaces
(Figure 1) which reduced the water demand in concrete, but
the addition of MIRHA to FA-based geopolymeric concrete
increased the water demand in the concrete by reducing the
value of the slump by 5 and 7%, approximately, in comparison
with the SF mix and control mix, respectively. With the
increase in percentage of MIRHA, slump was decreased, which
showed that as the MIRHA content increased the water
quantity should also be increased in order to maintain the
required consistency of the mix. The decrease in workability
was due to the cellular particles (Figure 2) of MIRHA that
were absorptive in nature. MIRHA is a hygroscopic material
having a specific surface area that is greater than that of
cement; it therefore absorbed more water.
On the other hand, in the case of SF addition to the fly ash-
based geopolymeric concrete, there was no change in the slump
value for 3 and 5% replacement but a 5% decrease could be
seen in the 7% replacement of SF. This shows that for the 7%
increment (or more) of SF, the water requirement in the
concrete increased which was due to the increased amount of
silica in the mix. Because of larger surface area and smaller
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Utilisation of waste material in
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Nuruddin, Qazi, Kusbiantoro and
Shafiq
Date: 1 Apr 2010 Time: 13:11: 32
Universiti Teknologi PETRONAS
particle size (Figure 3), SF requires more water when increased
after a certain amount. In comparison with the control mix the
slump value of the SF mix decreased by 1?8%.
3.2 Suitable curing regime for FA-MIRHA
geopolymeric concrete
Figure 4 shows that a 5% (wt) addition of MIRHA to the
concrete mix provided the highest compressive strength of the
concrete samples cured in ambient conditions, specifically,
28?3 MPa at 90 days. This value was 38?6% greater than that
obtained for the mix having 3% addition, 50?7% greater than
that of the mix with a 7% addition and 19% greater than the
control mix. With respect to the mix having 5% addition of
MIRHA, this quantity was found to be the optimum amount
for FA-based geopolymeric concrete.
External exposure curing conditions (Figure 5) resulted in the
highest compressive strength in comparison with concrete
cured under ambient conditions. Among mixes having
replacements of FA, the 7% replacement by MIRHA gave
the highest compressive strength at 90 days (46 MPa), which
was 48?4% greater than the 5% MIRHA mix and 11?7% less
than the control mix. In the control mix 67% of the 90 day
strength was developed in the first 3 days, which then led to
51?36 MPa at 90 days, the highest strength value of all the
mixes. Between 7 and 28 days, the highest increase in strength
was for the 3% MIRHA mix, for which a 30% strength increase
was obtained in comparison with the control mix. All results
are given in Table 4.
 Construction Materials Utilisation of waste material in
Volume 164 Issue CM6 geopolymeric concrete
Nuruddin, Qazi, Kusbiantoro and
Shafiq

10 mm EHT = 1.00 kV Signal A = SE2 Date: 1 Apr 2010 Time: 13: 20: 49
WD = 4.9 mm Mag = 1.00 KX Universiti Teknologi PETRONAS

Figure 2. FESEM image of MIRHA

These results explained the importance of heat in the curing of
geopolymeric concrete which was insufficient in ambient curing
conditions to produce the strength increases that were evident for
the concrete cured under external exposure conditions. The
increase in temperature during cure gave rise to a pozzolanic
reaction. When cured in the external exposure conditions the
geopolymeric reaction was enhanced by the heat from sunlight
which helped develop early age strength. It was supposed that the
additional heat helped promote the dissolution of silica and
aluminium atoms from the amorphous portion of the source

100 mm EHT = 5.00 kV Signal A = SE2 Date: 1 Apr 2010 Time: 13:16: 44
WD = 7.2 mm Mag = 100 X Universiti Teknologi PETRONAS

Figure 3. FESEM image of silica fume

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 Construction Materials Utilisation of waste material in
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Nuruddin, Qazi, Kusbiantoro and
Shafiq

60
60
50
Compressive stress: MPa

Compressive stress: MPa

50
40
40
30
30
20
20

10 10

0 0
1 10 100 1 10 100
Age: days Age: days
Control mix 3%MIRHA 5%MIRHA 7%MIRHA Control mix 3%MIRHA 5%MIRHA 7%MIRHA

Figure 4. Compressive strength of FA–MIRHA-based polymeric Figure 5. Compressive strength of FA–MIRHA-based polymeric
concrete with ambient curing concrete with external exposure curing

material by the action of hydroxide ions and concurrently these
precursor ions converted to monomers that further advanced the
polycondensation process (hardening process), ultimately to form
a geopolymeric structure as described by Davidovits (2008).
The performance of geopolymeric concrete incorporating
MIRHA depended upon the proper utilisation of its particles
from which the aluminium and silicon content could easily
dissolve to form a supersaturated aluminosilicate solution that
further transformed into a gel. This gel consisted of a network
of oligomers which continued to develop until the maximum
volume of alkaline liquids was used. Following this, the gel
started to harden and the hardening process was enhanced if
samples were cured under the external exposure conditions
given the heat generated from exposure to sunlight.
Figure 6 shows that a 7% (wt) addition of MIRHA in the mix
provided the highest values for flexural strength for concrete
cured under ambient and external exposure conditions,
attaining 8?38 and 6?52 MPa, respectively. Ambient curing
provided the best in MIRHA geopolymeric concrete.
According to the commentary given in ACI (Neville, 1990)
the tensile strength in flexure should be 10–15% of the
compressive strength, which was slightly better for geopoly-
meric concrete. The ratio of flexural to compressive strength
was found to be more than 10–15%, which is perhaps an
indication of good flexural strength for the geopolymeric
concrete as compared with OPC concrete.
3.3 Suitable curing regime for FA–SF geopolymeric
concrete strength
Figure 7 shows that 3% (wt) addition of SF in the FA-based
geopolymeric concrete yielded the highest compressive strength
(32?55 MPa) as compared to the control and other mixes. This value
was 37% greater than the control mix and 5% greater than the SF
sample having a 5% (wt) addition to the FA-based geopolymeric
concrete, which showed the lowest strength among all mixes.
This sample gained the most strength within 28 days, after
which no marked difference in strength is evident, whereas over

Curing type MIRHA: % Compressive strength: MPa

3 days 7 days 28 days 56 days 90 days

Ambient 0 9?50 14?11 19?73 21?92 23?77

curing 3 9?00 11?90 17?92 19?19 20?42
5 9?77 15?89 24?08 27?00 28?30
7 8?55 11?00 16?75 17?03 18?78
External 0 34?50 42?30 48?70 50?60 51?36
exposure 3 18?50 25?98 33?80 37?30 38?50
curing 5 14?98 22?13 27?58 29?80 31?00
7 23?80 31?90 40?70 44?50 46?00

Table 4. Compressive strength of FA-based polymeric concrete

replaced by MIRHA

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 Construction Materials Utilisation of waste material in
Volume 164 Issue CM6 geopolymeric concrete
Nuruddin, Qazi, Kusbiantoro and
Shafiq

9 60
Flexural strength at 28 days: MPa

Compressive stress: MPa

50
7
6 40
5
30
4
3 20

2 10
1
0
0 1 10 100
0 3 5 7
Percentage replacement of fly ash with MIRHA Age: days
Control mix 3%SF 5%SF 7%SF

Figure 6. The 28 day flexural strength of FA–MIRHA-based

Figure 8. Compressive strength of FA–SF-based polymeric
polymeric concrete: vertical lines shading, ambient curing;
concrete with external exposure curing
horizontal lines shading, external exposure curing

network. Once the polymerisation process was initiated, it

a 3–7 day period a gain of 106% in strength was observed for
the 5% SF mix.
Figure 8 shows that the control mix provided the highest
compressive strength results, specifically, 32?4% higher than
the 3% SF mix, 56% higher than the 5% SF mix and 10?5%
higher than the 7% SF mix. Among all replacement quantities,
the 7% SF replacement amount provided the highest compres-
sive strength which was comparable with the MIRHA mix
having the same replacement value. The results obtained for
SF as replacement were slightly better than those for MIRHA
because MIRHA absorbed more liquid due to its hygroscopic
characteristic whereas SF needed water after exceeding a
certain amount. This made it possible for the precursor ions to
fully mobilise and thereafter orient themselves into monomers
within the liquid provided. These monomers were then
transformed into oligomers and within the gelation process
were reorganised to form a three-dimensional aluminosilicate
enhanced the aluminosilicate network that, with the additional
heat from exposure to sunlight, produced a more hardened
matrix, which ultimately resulted in higher compressive
strengths. All results are given in Table 5.
Figure 9 shows that in external exposure curing conditions, 7%
inclusion of SF showed the highest values for flexural strength
(7?91 MPa), whereas for ambient curing conditions the best
flexural strength (6?58 MPa) was achieved by the 5% inclusion
of SF.
3.4 Microstructure analysis of geopolymeric
concrete
In 3% MIRHA (Figure 10(b)) mix the microstructure was better
hardened in comparison with the control mix (Figure 10(a)),
which was due to the greater amount of silica present in
MIRHA, therefore more silica atoms were expected to

9
60
Flexural strength at 28 days: MPa

8
50 7
Compressive stress: MPa

6
40
5
30 4
3
20
2
10 1
0
0 0 3 5 7
1 10 100 Percentage replacement of fly ash with MIRHA
Age: days
Control mix 3%SF 5%SF 7%SF

Figure 9. The 28 day flexural strength of FA–SF-based polymeric

Figure 7. Compressive strength of FA–SF-based polymeric concrete: vertical lines shading, ambient curing; horizontal lines
concrete with ambient curing shading, external exposure curing

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Nuruddin, Qazi, Kusbiantoro and
Shafiq

Curing type SF: % Compressive strength: MPa

3 days 7 days 28 days 56 days 90 days

Ambient 0 7?46 14?11 19?73 21?92 23?77

curing 3 12?07 24?04 30?27 31?75 32?55
5 5?35 11?04 12?97 15?10 16?54
7 11?90 18?39 26?50 28?82 29?98
External 0 34?50 42?30 48?70 50?60 51?36
exposure 3 22?00 28?30 35?00 37?50 38?80
curing 5 19?10 25?10 30?50 32?00 32?90
7 31?90 37?00 42?30 45?10 46?50

Table 5. Compressive strength of FA-based geopolymeric concrete

replaced by SF

1 mm EHT = 15.00 kV Signal A = VPSE Date: 29 Jul 2009 Time: 11: 10: 26 2 mm EHT = 15.00 kV Signal A = VPSE Date: 30 Jul 2009 Time: 16: 34: 18
WD = 10.4 mm Mag = 5.00 X Universiti Teknologi PETRONAS WD = 11.4 mm Mag = 2.00 X Universiti Teknologi PETRONAS
(a) (b)

10 mm EHT = 15.00 kV Signal A = VPSE Date: 29 Jul 2009 Time: 12: 12: 06 2 mm EHT = 15.00 kV Signal A = VPSE Date: 29 Jul 2009 Time: 12: 12: 00
WD = 9.7 mm Mag = 1.00 X Universiti Teknologi PETRONAS WD = 10.8 mm Mag = 2.00 X Universiti Teknologi PETRONAS

(c) (d)

Figure 10. SEM images of ambient-cured FA-based polymeric

concrete with MIRHA: (a) control mix; (b) 3% MIRHA; (c) 5%
MIRHA; (d) 7% MIRHA

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 Construction Materials Utilisation of waste material in
Volume 164 Issue CM6 geopolymeric concrete
Nuruddin, Qazi, Kusbiantoro and
Shafiq

200 nm EHT = 2000 kV Signal A = VPSE Date: 31 Mar 2010 Time: 12: 40: 50
WD = 9.5 mm Mag = 30.00 KX Universiti Teknologi PETRONAS

Figure 11. FESEM image of polymeric paste showing

aluminosilicate gel

dissolve from the source material and participate in the having 3% addition of MIRHA in terms of the extent of
geopolymeric reaction to produce aluminosilicate gel, which hardening of the gel because the amount of dissolved silica
has a tube-like structure (Figure 11) unlike that of calcium– increased with the increase in the amount of MIRHA. Although
silicate–hydrate (C–S–H) gel as found in OPC concrete (Famy some precipitated particles were present in the matrix, these were
et al., 2003). The composition of aluminosilicate gel was not converted to aluminosilicate gel because of the reduced
examined by energy dispersive X-ray (EDX) analysis temperature during the ambient curing period. The average
(Figure 12). Fewer micropores were present in the matrix; temperature was 20–25˚C in ambient curing. For the 7%
this was due to the inclusion of fine MIRHA particles that MIRHA mix (Figure 10(d)) the amount of undissolved particles
filled these pore spaces. was greater in comparison with those evident for the
3 and 5% MIRHA mixes and this showed that additions of
The microstructure of the sample with the addition of 5% (wt) more than 5% of MIRHA increased the amount of silica in the
MIRHA (Figure 10(c)) was even better than the sample mix mix which was not able to fully react with alkaline liquids. Owing
to low heat the polymeric reaction was slow and the time taken
for the alkaline liquids to leach out of the mix before properly
Si Element Weight% Atomic%
coming into contact with the reactive solid material increased. As
O 48.56 64.15
a result, a greater number of unreacted particles were present in
Na 3.25 2.99
Mg 4.26 3.70 the matrix in comparison with the reactive ones, which
Al 3.35 2.62
O consequently caused a reduction in the compressive strength.
Si 24.84 18.70
K 1.00 0.54
Ca 11.58 6.11
The addition of 3% (wt) of SF to the geopolymeric concrete mix
Fe 3.17 1.20
Fe Al Ca (Figure 13(b)) was found to produce a better yield in
Mg 100.00
Total comparison with the 5% (Figure 13(c)) and 7% inclusion
K Na
Ca K K Ca Fe Fe (Figure 13(d)) unlike MIRHA because SF contained more silica
1 2 3 4 5 6 7 8 9 10
content in comparison with MIRHA. This showed that beyond
Full scale 2514 cts cursor: 0.000 keV an addition of 3% of SF, the alkaline liquids were not sufficient
for the mix to dissolve silica from the source material. Unreacted
Figure 12. EDX analysis of aluminosilicate gel after 7 days particles were still present, given that there was insufficient heat
from the surroundings, which in turn prevented the precipitated

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 Construction Materials Utilisation of waste material in
Volume 164 Issue CM6 geopolymeric concrete
Nuruddin, Qazi, Kusbiantoro and
Shafiq

1 mm EHT = 15.00 kV Signal A = VPSE Date: 29 Jul 2009 Time: 11: 10: 26 10 mm EHT = 15.00 kV Signal A = VPSE Date: 30 Jul 2009 Time: 12: 00: 54
WD = 10.4 mm Mag = 5.00 X Universiti Teknologi PETRONAS WD = 7.8 mm Mag = 1.00 KX Universiti Teknologi PETRONAS

(a) (b)

10 mm EHT = 15.00 kV Signal A = VPSE Date: 30 Jul 2009 Time: 12: 36: 28 10 mm EHT = 15.00 kV Signal A = VPSE Date: 30 Jul 2009 Time: 12: 46: 37
WD = 9.8 mm Mag = 1.00 KX Universiti Teknologi PETRONAS WD = 10.9 mm Mag = 1.00 X Universiti Teknologi PETRONAS

(c) (d)

Figure 13. SEM images of ambient-cured FA-based polymeric

concrete with SF: (a) control mix; (b) 3% SF; (c) 5% SF; (d) 7% SF

particles from converting into a gel. For those mixtures to which
5 and 7% of SF was added, unreacted particles were abundantly
present in the matrix which was also porous because sufficient
gel had not formed to fill these pores.
In comparison with the ambient curing conditions, the curing of
concrete samples in external exposure conditions provided
better microstructural development, which was thought to be
due to the additional heat available during the external exposure
curing period in comparison with that of the ambient cure.
Greater heat helped in greater dissolution of silica from the
pozzolan (FA/MIRHA/SF) and the additional heat apparently
accelerated the geopolymeric reaction which, in turn, resulted in
the production of aluminosilicate gel that filled voids at the
interfacial transitional zone (ITZ) and within the matrix.
Unlike the setting times obtained for concrete samples cured
under ambient conditions, the setting time of geopolymeric
concrete cured under external exposure conditions was not
delayed. This is thought to be due to the additional heat
provided by exposure to sunlight which readily promoted
contact of alkaline solutions with the reactive solid material
before being leached from the mix. The average temperature in
external exposure curing was 35–40˚C. All mixes replaced by
MIRHA (Figure 14) or SF (Figure 15) showed a compact
microstructure with a smaller number of unreacted particles,
which led to a better strength of concrete. The ITZ was properly
developed as no evident interface can be observed between
aggregates and the geopolymeric matrix. Such microstructural
properties were consistent with the 28 day compressive strength
of 48?7 MPa, which was as good as OPC concrete.

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 Construction Materials Utilisation of waste material in
Volume 164 Issue CM6 geopolymeric concrete
Nuruddin, Qazi, Kusbiantoro and
Shafiq

Hardened paste

Aggregate

10 mm EHT = 15.00 kV Signal A = VPSE Date: 30 Jul 2009 Time: 16: 13: 06
WD = 6.6 mm Mag = 500 X Universiti Teknologi PETRONAS

Figure 14. SEM images of external exposure-cured FA-based

polymeric concrete with MIRHA

Aggregate

Hardened paste

10 mm EHT = 15.00 kV Signal A = VPSE Date: 30 Jul 2009 Time: 12: 56: 28
WD = 8.9 mm Mag = 300 X Universiti Teknologi PETRONAS

Figure 15. SEM images of external exposure-cured FA-based

polymeric concrete with SF

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 Construction Materials
Volume 164 Issue CM6
On the other hand, in the case of SF addition to the FA-
based geopolymeric concrete, there was no change in the
slump value for replacement values of 3 and 5%, whereas a
5% decrease in slump can be seen for a 7% replacement with
SF. This shows that for the 7% increment (or more) of SF,
the water requirement in the concrete increased, which was
due to the increased amount of silica in the mix. It is
apparent that given the smaller particle size and large
surface area of SF, SF requires more water when added to
an FA mix beyond replacement values of 7% (wt). In
comparison with the control mix, the slump value of the SF
mix decreased by 1?8%.
4. Conclusions
(a) Geopolymeric concrete was developed that achieved a
target strength compressive strength at 28 days equal to
that of OPC concrete. The results of a microstructure
study helped verify the cementing potential of geopoly-
meric concrete to be used in the construction industry;
this study was able to show the dense microstructure of
the geopolymeric concrete and the well-developed ITZ
between particles and cement paste.
(b) External exposure curing conditions were found to be the
best curing regime for geopolymeric concrete given that it
showed the highest value of compressive strength in
comparison with similar concretes cured under ambient
curing in this study.
(c) The compressive strength of the geopolymeric concrete
under external exposure conditions developed up to 28
days; however; there was no significant increase in
strength beyond this time.
(d) The flexural strength of geopolymeric concrete was
comparable to OPC concrete.
(e) The best performing geopolymeric concrete mix
design, based on the results of compressive strength
tests and a microstructure study, was the concrete mix
cured under external exposure conditions. This mix
comprised
(i) fly ash: 350 kg/m3
(ii) sodium hydroxide (NaOH): 41 kg/m3
(iii) sodium silicate (Na2SiO3): 103 kg/m3
(iv) table sugar: 10?5 kg/m3 (3% of FA)
(v) extra water: 35 kg/m3 (10% of FA)
(vi) fine aggregate: 645 kg/m3
(vii) coarse aggregate: 1200 kg/m3.
Acknowledgements
The authors would like to acknowledge the University
Teknology PETRONAS for providing facilities to complete
this research study.
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Utilisation of waste material in
geopolymeric concrete
Nuruddin, Qazi, Kusbiantoro and
Shafiq
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