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Optimization Of Alkaline Activator/Fly Ash Ratio On The Compressive Strength

Of Fly Ash-Based Geopolymer

Conference Paper · January 2009

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 Optimization Of Alkaline Activator/Fly Ash Ratio On The Compressive
Strength Of Fly Ash-Based Geopolymer

A. Mohd Mustafa Al- Bakari*, Omar. A.K.A.Abdul Kareem*and San Myint *

School of Material Engineering
University Malaysia Perlis (UniMAP)
01000, P.O Box 77, D/A Pejabat Pos besar,
Kangar, Perlis, Malaysia
E-mail : [email protected]

Abstract [1]. Among all the suggested alternative binders, the

Fly ash and a mixture of alkaline activators geopolymers seems to be the promising future binders
namely sodium silicate (Waterglass) and sodium because of it highly mechanical performance, total
hydroxide (NaOH) solution at different Alkaline environment friendly and inexpensive costs of
activator/Fly ash ratio (0.3, 0.35 and 0.4) were used processing. Davidovits [2, 3] proposed that an alkaline
to prepare a fly ash-based geopolymer at constant liquid could be used to react with silicon (Si) and the
(NaOH) concentration of 15M, curing temperature, aluminum (Al) in source material of geological origin
curing time and total additional water content or in by-product materials, and because the chemical
approximately (17%) of the samples weight. Optimum reaction that takes place in this case is polymerization
value of the Alkaline activator/Fly ash ratio was process, he coined the term (Geopolymer) to represent
determined with respect to the highest compression thesis binders.
strength of the 7days aging samples. The effect of the
oxide molar ratios of SiO2/Al2O3, Water content of the Geopolymers are members of the family of inorganic
alkaline activator and the Waterglass% content were polymers. The chemical composition of the
studied for each of Alkaline activator/Fly ash ratio, geopolymer material is similar to natural zeolitic
and it showed an important role on the materials, but the microstructure is amorphous.
geopolymerization process. Zeolites composition is based on aluminosilicate
framework and three dimensional network inorganic
Keywords: Geopolymer; Alkaline Activator; Fly Ash; polymers built up of (Si, Al)O4 tetrahedra linked by
Compressive Strength sharing oxygen atoms into rings and cages. The
polymerization process involves a substantially fast
1. Introduction chemical reaction under alkaline condition on Si-Al
minerals, that result in three dimensional polymeric
chains and ring structure consisting of Si-O-Al-O
The climate change due to the global warming has bonds [2]. The similarity of some fly ashes to natural
become the major concern. The global warming is aluminosilicate materials (due to the presence of Si
caused by the greenhouse gases, such as carbon and Al in the ash) has encouraged the use of
dioxide CO2, to atmosphere by human activities. The geopolymerization as a possible technological solution
fuel burning and the cement industry considered the in the making of special cement [4].
main sources of the harmful CO2. Efforts has been
held to controlling and decreasing the CO2 that The most used alkaline liquid activator is a mixture of
produced from fuel burning, and several efforts are in sodium or potassium hydroxide (NaOH, KOH)
progress to reduce the use of the Portland cement as a with sodium waterglass (nSiO2Na2O) or potassium
construction material in order to address the global waterglass (nSiO2K2O) [5-8]. In the fly ash-based
warming, and these include the utilization of geopolymer, the concentration of NaOH solution can
supplementary cementing materials such as fly ash, vary in the range between 8 to 16 M [1]. It is not
silica fume, granulated blast furnace slag, and the recommended using above or less this limit in the
development of alternative binders to Portland cement formation of fly ash-based geopolymer [7].However,
the geopolymerization process considered a complex
chemical reaction, if all other parameters like (NaOH technical grade sodium silicate (Sigma Chemicals
Chemical Component (%)
Ltd.) with modulus (3.20, SiO2 =30.1%, Na2O
=9.4%and H2O=60.5%). The sodium hydroxide
SiO2 52.11 pellets 97-99 % purity supplied from (Sigma-Aldrich
Al2O3 23.59 Co.), was used to preparing sodium hydroxide
Fe2O3 7.39 solution.
TiO2 0.88
CaO 2.61 Table 1. XRF analysis data of fly ash composition
MgO 0.78 2.2 Geopolymer synthesis
Na2O 0.42
K2O 0.80 The geopolymers were synthesized by the
P2O5 1.31 activation of fly ash with alkaline liquid activator
SO3 0.49 solution at three different Alkaline activator/Fly ash
MnO 0.03 ratios which were 0.3, 0.35, and 0.4, at specific
Loss on Ignition 5.59 constant ratio of waterglass/NaOH solution. The
solution concentration, curing temperature, curing alkaline activator of mixture sodium waterglass +
time, delay time, additional water if any, and others.) NaOH solution was prepared and mixed at constant
are constant, the amount of the ratio of Alkaline Waterglass/NaOH solution ratio of 1.00. The NaOH
activator/Fly ash plays a crucial role on the solution was prepared by dissolving sodium hydroxide
geopolymerization rate. For fly ash-based geopolymers pellets in deionised water, the concentration of the
different authors used different Alkaline activator/Fly NaOH was kept constant at 15 M. It is preferable to
ash ratio based on the type, concentration and the mix the waterglass and the NaOH solution together at
economic costs of the alkaline activators. Some fly ash least one day before adding the liquid to the solid
based geopolymer formed with using ratios of 0.25-0.3 constituent [11]. Geopolymer samples were
[7, 9 and 10]. And in other research range of (0.3- synthesized by adding the alkaline activator gradually
0.4) was used [11]. The objective of this study is to at the different mentioned Alkaline activator/Fly ash
obtain the optimum Alkaline activator/Fly ash ratio ratios. An additional water of a constant 17% of the
for the ratios range of (0.3, 0.35, and0.4) that gives samples weight was added to achieve a suitable
the highest compressive strength (highest workability. The ratio of (Alkaline activator/Fly ash =
geopolymerization rate) for a geopolymer based on the 0.25) was ignored, because it required an additional
activation of the fly ash (Class F). All other water more than 17% of the samples weight. After 15
parameters including NaOH solution of 15M, mixing min of mechanical mixing, the fresh homogeneous
time of 15 min, the total additional water content of geopolymers were poured in to (50 x 50 x 50mm)
approximately 17% of the samples weight, delay time standard steel molds. The samples aggrieved in room
of 24 hr, the curing temperature of 70°C, curing time temperature for 24 hr prior to cure in electrical low
of 24hr and the aging time of 7days were kept temperature furnace (L T Furnace, L6-1200) for one
constant during the all process. day at 70°C. The water evaporation was prevented by
sealing the top of the molds by a thin plastic layer
during the storage as well as the curing stage. After
2. Experimental method the end of curing, the molds took out from the furnace
and left cooling to room temperature, before
demolding and kept aging for 7 days at room
2.1 Materials
temperature. The samples were kept sealed from
ambient during aging period also.
The low-calcium fly ash used in this study was
obtained from Sultan Abdul Aziz power station in
Kapar, Selangor. Malaysia. The chemical composition
of the fly ash listed in Table 1. The composition
analysis indicated that (CaO) content was less than
(10%) which conforming that the fly of Class F type
[12]. The particle size distribution was measured
using Malvern Mastersizer 2000 (Malvern
Instrument). The particle size in range of (18 m). A
Table 2. Effect of (Alkaline activator/Fly ash) ratio
on the % Water content in Geopolymer, Na2O/Al2O3
ratio and Workability of the Fly ash-based
geopolymer. Act/Fly %Water in Water- Na2O/Al2O3 Work-
ash ratio g lass/ molar ratio ability
Geopolymer.
NaOH
sol.
0.3 14.1 1.00 0.4 Stiff
2.3 Compressive strength
0.35 15.9 1.00 0.46 Mode-
The samples tested after 7 days of aging. Using rate
0.4 17.5 1.00 0.53 High
(Instron, 5569 USA) mechanical testing machine with
Automatic Max. Loading of 50KN, the compressive
strength of the geopolymer tested with speed rate of 50 10

Compressive strength at
8.61
mm/min. The compression strength values were an 8 8.325

7 days (MPa)
average of testing three samples for each ratio.
6

4 3.695

3. Results and discussion 2

0
Figure 1, shows the influence of increasing the 0.25 0.3 0.35 0.4 0.45

Act/Fly ash ratio on the compressive strength of the Alkaline activator/Fly ash ratio
fly ash-based geopolymer. A rapid increasing in the
compressive strength form 3.695 to 8.325 MPa after
Figure 1. Effect of Alkaline activator/Fly ash ratio on the
increasing the Alkaline activator/Fly ash ratio form
compressive strength of Fly ash-based geopolymer.
0.3 to 0.35 followed by venially strength increasing
from 8.325 to 8.61MPa, when the ratio raised from
Furthermore, an increased in ratio of Alkaline
0.35 to 0.4. The changing in the alkaline activator
activator/Fly ash from 0.35 to 0.4 increases the
content affect on the (Si) species content, based water
SiO2/Al2O3 from 4.12to 4.18 but increased the
content, and on the (Na+ ) ions content . All of theses
compressive strength slightly increasing only from
mentioned factors have the major effect on the
8.325 to 8.61 MPa.
geopolymerization process and the strength of resulted
geopolymer. An increasing in the alkaline activator
As indicated in the Table 2, the increased in the
content (Alkaline activator/Fly ash ratio) increase the
Alkaline activator/Fly ash ratio increases the %Water
Si species content, because the alkaline activator
content of the Geopolymer. The water content
contained sodium waterglass (more Si species),
considered the most important factor in the
increased the SiO2/Al2O3 ratio and also increased the
geopolymerization process [14]. Generally, the
geopolymer strength, because as increased the
geopolymerization process can be partitioned in to two
SiO2/Al2O3 ratio, resulted more Si-O-Si bonds, which
periods: I dissolution –hydrolysis, II hydrolysis-
are stronger in comparison with Si-O-Al [13]. Figure
polycondensation. Period I including the dissolution of
2, shows the effect of SiO2/Al2O3 ratio on the
the SiO2 and Al2O3 species and hydrolyzed it [15].
compressive strength of the fly ash-based geopolymer.
Thus, the increased the water content due to increased
An increasing of the ratio of Alkaline activator/Fly ash
Alkaline activator/Fly ash ratio, resulted high
ratio from 0.3 to 0.35, the SiO2/Al2O3 increased from
dissolution of SiO2 and Al2O3 species and more
4.07 to 4.12, with increasing in compressive strength
hydrolyzed ions available to the second period, and
from 3.695 to 8.325 MPa.
also resulted in high geopolymerization rate and more
strength to geopolymer . The workability of the freshly
prepared geopolymer was found to be affected by
Alkaline activator/Fly ash the ratio, and it increased
with the increasing ratio from 0.3 to 0.4 as indicated
in Table 2.
Figure 3, shows the effect of Waterglass% content of
the alkaline activator on the compressive strength of 4. Conclusions
the fly ash –based geopolymer. The Waterglass
favours the polymerization process leading to a The ratio of the Alkaline activator/Fly ash, found to
reaction product with more Si and more mechanical have a great influence on the compressive strength of
strength [11].Furthermore, the waterglass content the fly ash-based geopolymer. It can be concluded the
approximately H2O= 60.5%, so increase its content Alkaline activator/Fly ash ratio of 0.4 has the
increased the geopolymerization rate, producing high optimum amount of alkaline liquid, which could
strength geopolymer. As in the Figure 3, the Alkaline activate the fly ash in highest rate of
activator/Fly ash ratio=0.3, the Waterglass content of geopolymerization comparing to other ratio. Firstly, it
11.5 % by geopolymer weight. provided the sufficient Si species; raise the ratio of
SiO2/Al2O3 up to 4.18, and gained the resulted
9 geopolymer highest strength 8.61MPa, than others
Compressive strength at 7

8 ratios of 0.3and 0.35. Secondly, the Alkaline

7 0.4 activator/Fly ash=0.4 ratio was found to provides the
days(MPa)

6 0.35
5 highest water content (%Water in Geopo-
4 lymer=17.5%), and resulted in high geopolymer
3 0.3 compressive strength 8.61MPa. Thirdly, the
2
waterglass content found has an important affect on
1
0 the geopolymerization rate. The ratio Alkaline
4.07 4.12 4.18 activator/Fly ash ratio=0.4, with highest waterglass
SiO2 /Al2 O3 ratio content 14%, resulting in high mechanical strength
geopolymer. Generally, the strength data for the
precious geopolymers shows a major increasing in the
Figure 2. Effect of SiO2/Al2O3 molar ratio on the strength when the Alkaline activator/Fly ash ratio
compressive strength of fly ash-based geopolymer.
changed from 0.3 to 0.35, and only a venial strength
increasing when the ratio arise from 0.35 to 0.4. The
9
8 0.4 resulted data indicated that both of 0.35 to 0.4 ratios
Comressive strength at 7

0.35
7 are suitable for producing geopolymer with high
6
compressive strength depending on the highest
days(Mpa)

5
4
geopolymerization rates they provides.
3 0.3

2
1
0 5. Acknowledgement
11.5 13 14

Watergalss%
The author wish to thank Mr. (Abdul Haqi Bin
Ibrahim), School of Environmental Engineering.
University Malaysia Perils “UinMAP”, for his help in
providing the fly ash of this study.
Figure 3. Effect of the Waterglass% of each Alkaline
activator/Fly ash ratio on the compressive strength of the
fly ash-based geopolymer.
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