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Journal of Scientific and Engineering Research, 2018, 5(7):270-277

ISSN: 2394-2630
Research Article CODEN(USA): JSERBR

Characterization of Geopolymer–based Materials Synthesized from Fly Ash and Rice

Husk Ash

Nguyen Hoang Luong Ngoc

Faculty of Chemical Technology, Ho Chi Minh City University of Food Industry, Viet Nam
Abstract Investigations on geopolymer-based materials are always interesting topics for researchers.
Geopolymer is environmentally friendly material which has been potential applications for many different fields
such as technical materials, building materials, insolation or refractories, and others. This study used fly ash
(FA) and rice husk ash or rice hull ash (RHA) as raw materials for geopolymerization process to develop novel
materials with high porosity. Both FA and RHA are industrial waste of coal fired thermal power plants and
agricultural wastes, respectively that need to be managed to reduce their negative impact to the environment. FA
and RHA contain high alumino-silicate resources were mixed with sodium hydroxide solution for 10 minutes to
obtain the geopolymer pastes. Sodium hydroxide solution was used as an alkaline activator to form geopolymer
paste. The geopolymer paste was filled into 5-cm cube molds according to ASTM C109/C109M 99, and then
cured at room temperature for 28 days. These products were then tested for compressive strength and volumetric
weight. Results indicated that the material can be considered lightweight with a compressive strength at 28 days
that are in the range of 18.3 to 35.5 MPa, volumetric weight around 800kg/m 3 and water absorption is under
215.65 kg/m3. The properties of raw materials and geopolymer products were also determined by analytical
techniques that included chemical composition by X Ray Flourescence (XRF), mineral composition by X Ray
Diffraction (XRD), and structural bonds by Infrared spectroscopy (IR).

Keywords Lightweight Materials, Geopolymer, Fly Ash, Rice Husk Ash, Sodium Hydroxide Solution, Alkaline
Activator, Engineering Properties
Introduction
Geopolymer, originally named as “soil cement”, is a kind of synthetic alumino-silicate material that is found to
have several applications including as a material for high-performance composites, ceramics, as well as, as a
replacement for Portland cement [1-4]. Geopolymer-based materials are capable of setting rapidly with high
final compressive strength and they are highly resistant to chemical attack. Thus, it is predicted that this new
material would be popularly applied as a sustainable construction material in the future [1].
Since the raw materials of geopolymer are mainly composed of aluminium oxide, silicon dioxide, and other
oxides, its mechanical properties are influenced by the development of its microstructure. Geopolymerization is
based on a chemical reaction between different alumino – silicate oxides (Al3+) with silicates under highly
alkaline conditions, yielding polymeric Si–O–Al–O bonds [5]. The thermal and chemical stability of these
bonds are hypothesized to be determined by the nanostructure and molecular structure within the gel phase [1,
5]. In the raw materials, these oxides are believed to be in amorphous or semi – crystalline phases that
participate in geopolymerization process whereas the crystalline phases do not take part in forming the
geopolymers [1, 5-8].
This research presents the utilization of fly ash and rice husk ash as raw materials to produce a geopolymer-
based material. These raw materials constitute the blend of the alkali-activated binder in this study. FA was used
as the primary source of reactive alumina and silicate. It is an industrial waste of coal-fired power plants, which

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is estimated to be over 650 Mt/year worldwide [9-11]. Rice husk ash was used as the primary source of reactive
silica. It is a by-product of burning agri-waste particularly rice husk, with an estimated generation rate of over
30 million metric tons per year worldwide [12-14]. It is highly porous, lightweight material with very good
pozzolanic properties which is used to produce cheap insulating refractory materials (e.g., see [11]).

Fly Ash Rice Husk Ash

Drying, Grinding, and Sieving

Sodium
Hydroxide Mixing
Solution

Molding

Curing at room
conditions for 28 days

Testing for engineering

properties

Characterizing for
microstruture
Figure 1: The flow of experimental process
In Viet Nam, There has been no study research on geopolymer using FA and RHA as raw materials and no
evaluations for effects of alkaline activators to formation of the geopolymer-based materials. Especially in
Vietnam, this is the first study which is carried out for production of Geopolymer-based materials with using the
different concentration of sodium hydroxide solution (SHS).

Materials and Methods

In this research, both FA and RHA from Vietnam were used to produce the geopolymer mixture. They are the
raw materials in geopolymerization reactions to create the mechanical strength for product. FA waste came from
Vinh Tan coal-fired thermal power plant, Binh Thuan Province, Vietnam was dried at 110 oC for 24 hours and
then passed 90µm-siever to obtain the raw material. On the other hand, rice husks from Mekong delta, South of
Viet Nam were burned at 650oC for 2 hour at Laboratory of Ceramic Materials to obtain rice husk ash. RHA
was ground using ball miller for 30 minutes, and then passed 90µm-siever to obtain the raw material in powder.
All of the raw materials were characterized for chemical and mineral compositions using XRF and XRD,
respectively. On the other hand, sodium hydroxide solution (SHS) was a commercial product from Bien Hoa
Chemical Factory, Dong Nai province, Viet Nam.

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Table 1: Mix proportions used in the design of experiments

Mixture Proportion of solid powders (%wt) Concentration of
(Sample) FA RHA SHS (M)
GeoNa0 50 50 0
GeoNa2 50 50 2
GeoNa4 50 50 4
GeoNa6 50 50 6
GeoNa8 50 50 8
GeoNa10 50 50 10
In this study, FA and RHA powder were mixed with SHS concentration from 0 to 10M, ratio of solid powder
per liquid solution was at 0.4 (in weight) using a laboratory cement mixer. Table 1 showed the mix proportions
of FA, RHA, and SHS concentration for producing of geopolymer-based materials. The fresh pastes of the
geopolymer were formed in standard cubic molds with size of 50mm and cured for 28 days at room conditions
(25 oC, 85% humidity). Engineering properties of the geopolymer products were evaluated by testing for
compressive strength (MPa), volumetric weight (kg/m3), and water absorption (kg/m3). From the experimental
data, this paper conducts for evaluation on effects of SHS to engineering properties of the geopolymer products.
All of the tests for engineering properties were carried out according to ASTM C109/C109M [19] and ASTM
C140 [20]. Moreover, the geopolymer sample with the highest strength and low water absorption and volumetric
weight was characterized microstructure using XRD and SEM.

Results and Discussion

Properties of Raw Materials
The raw materials of FA and RHA were tested for physic-chemical properties and the results as shown in Table
2. In which FA has moisture content of 6.52%, bulk density of 0.91 g/cm3, apparent density of 2.42 g/cm3, mean
particle size of 48.2 µm, and LOI value at 3.82%. For the chemical composition using X-ray fluorescence
(XRF), FA contains 35.36% of Al2O3, 47.74% of SiO2, 7.02% of Fe2O3, and others. Figure 2 shows XRD
pattern of FA which is in amorphous phases of alumina and silica suitable for geopolymerization reactions at
high alkaline condition. For mineral compositions, FA has quartz, mulite, silimanite, and hematite.
For RHA, it has moisture content of 0.59%, bulk density of 0.59 g/cm 3, apparent density of 2.17 g/cm3, mean
particle size of 66.84µm, and LOI value at 1.79%. For the chemical composition using x ray fluorescence
(XRF), RHA contains high silica with 93.2% of SiO2, 0.43% of Al2O3, and others. Figure 3 shows XRD pattern
of RHA which is in amorphous phases of silica suitable for geopolymerization reactions at high alkaline
condition. For mineral compositions, RHA has cristobalite and tridymite.

Table 2: Physico-chemical properties of DE and WGS

Physico-chemical properties FA RHA
Al2O3 35.36 0.43
SiO2 47.74 93.20
Fe2O3 7.02 0.33
Na2O 0.69 0.22
K2O 2.61 0.41
Others 2.76 3.62
L.O.I 3.82 1.79
Moisture content (%) 6.52 0.59
Bulk density (g/cm3) 0.91 0.59
Apparent density (g/cm3) 2.42 2.17
Mean particle size (µm) 48.20 66.84

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Figure 2: XRD patterns of FA

Figure 3: XRD patterns of RHA

Effects of Alkaline Activator to Engineering Properties of Geopolymer Products

The values of volumetric weight for all geopolymer-based materials are in range of 779 to 812 kg/m3 which are
less than the prescribed volumetric weight (1680 kg/m3) for a lightweight concrete brick in ASTM C55-99 and
ASTM C90-99a [21-22]. This property is inherited from the porous material of diatomite as described in term of
3.1. Moreover, the geopolymerization processes and the evaporation of water during the cured process were also
produced micro-pores in the geopolymeric structures [1-2, 4-5, 15-16].
Table 3: Engineering properties of geopolymer specimen
Samples Volumetric weight Compressive strength Water absorption
(kg/m3) (MPa) (kg/m3)
GeoNa0 784 0.46 (unformed when -
exposed in water)
GeoNa2 792 18.33 215.65
GeoNa4 812 28.68 204.44
GeoNa6 798 35.51 179.64
GeoNa8 806 32.45 180.52
GeoNa10 779 (Swelling solid with macro- 186.18
cracks)

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Volumetric Weight (kg/m3)

2000
1680

1500

1000 784 792 812 806

500

0
0 2 4 6 8 ASTM C90
SHS Concentration (M)

Figure 4: The lower values of volumetric weight compared with ASTM C90 for lightweight concrete brick
Table 3 showed that the geopolymer sample of GeoNa0 without SHS or alkaline activator had no strength and it
was failed in water (test of water absorption), because the activated alumino-silicate resources were impossible
to react geopolymerization without alkaline condition. The Geopolymer-based geopolymer specimens with SHS
10M appeared phenomena of swell and macro-cracks. This is related an increase of temperature in high sodium
geopolymer paste because of enthalpy of dissolution of the formed NaOH [17, 18]. High temperature in fresh
geopolymer pastes may cause thermal stress that produce cracks in the sample. In fact, the geopolymer
specimen with SHS 8M was decreased compressive strength at 32.45MPa and increased water absorption at
180.52 kg/m3. For SHS concentration from 2 to 6M, the geopolymer specimens increased significantly the
compressive strength from 18.33 to 35.51MPa and decreased steadily water absorption from 215.65 to 179.64
kg/m3. These are effects of SHS concentration or alkaline activators to engineering properties of the
geopolymer-based materials which are interested in investigations. Thus, the SHS concentration should be
optimized around 6M to obtain the geopolymer-based materials prescribed limit according to ASTM C55 or
C90 [21-22] requirements for lightweight concrete brick materials.
Compressive Strength (MPa)
Water Absorption (kg/m3)
40 350
35 32.45 300
35.51 288
30 28.68
215.65 250
204.44
25
179.64 200
20 18.33
180.52 150
15 11.7
100
10
5 50

0 0
2 4 6 8 ASTM C90
SHS Concentration (M)

Figure 5: Relationship among SHS concentration (%, in weight) and engineering properties of geopolymer
materials compared with lightweight concrete brick in ASTM C90.

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Engineering Properties of Geopolymer Products

The sample of geopolymer-based geopolymer of GeoNa6 had the best engineering properties on low volumetric
weight and water absorption (kg/m3) and the highest compressive strength was carried out for analysis of
microstructure using XRD and SEM.

Figure 6: XRD pattern of the geopolymer-based material with SHS 6M

The XRD pattern of the geopolymer-based material (GeoNa6) showed differences among structures of raw
material (FA and RHA) and the geopolymer product. Many key peaks of clay minerals in FA (Fig. 2) were
decreased intensity in the geopolymer (Fig. 6) such as mulite, silimanite, and hematite. This is explained that the
geopolymerization reactions were dissolved the alumino silicate to from alumino-slicate networks in amorphous
phases. The crystal phases of quartz, cristobaliteand tridymite were dissolved with low concentration and
continuously existence in the geopolymer in crystal structures. As a result, the crystal structures appeared in
XRD pattern with high intensity among background of amorphous phases in the ash-based geopolymer material.

Figure 7: SEM image of GeoNa6 sample

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Microstructures of the geopolymer-based material (sample of Na6) had changed with appearance of new
structure dissolved in background as shown in Figure 6. The porous structures of alumino-silicate have existed
with high concentration. This is easy to realize with magnification at 20,000. Thus, SEM images are explanation
for the experimental data of volumetric weight and compressive strength in terms of 3.2.

Conclusions
This paper presents an experimental study to produce and optimize a light-weight geopolymer-based material
from a blend of coal fly ash waste and rice husk ash. The ash-geopolymer based materials with a solid powder
mix of 50% FA and 50% RHA and alkaline-activator with concentration of SHS at 6M produced geopolymers
with an average 28-day compressive strength of 35.51MPa, water absorption of 179.64.9 kg/m3, volumetric
weight of 798 kg/m3. These values were in good agreement with the required values of the ASTM C55 and C90
for lightweight concrete brick. The ternary-blended geopolymer can thus be potentially used as lightweight
material for masonry walls or partitions. Future studies will consider chemical resistance of the material and
other thermal properties such as thermal conductivities, thermal expansion coefficient. Microstructure of these
geopolymers will also be studied further to understand the relationship among composition, microstructure and
macroscopic properties of such materials.

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