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Abstract: The geopolymer of fly ash (FA) and rice husk ash (RHA) was prepared. The burning temperature of rice husk, the RHA
fineness and the ratio of FA to RHA were studied. The density and strength of the geopolymer mortars with RHA/FA mass ratios of
0/100, 20/80, 40/60, and 60/40 were tested. The geopolymers were activated with sodium hydroxide (NaOH), sodium silicate, and
heat. It is revealed that the optimum burning temperature of RHA for making FA-RHA geopolymer is 690ºC. The as-received FA
and the ground RHA with 1%-5% retained on No.325 sieve are suitable source materials for making geopolymer, and the obtained
compressive strengths are between 12.5-56.0 MPa and are dependent on the ratio of FA/RHA, the RHA fineness, and the ratio of so-
dium silicate to NaOH. Relatively high strength FA-RHA geopolymer mortars are obtained using a sodium silicate/NaOH mass ratio
of 4.0, delay time before subjecting the samples to heat for 1 h, and heat curing at 60ºC for 48 h.
Key words: geopolymer; fly ash; rice husk ash; sodium hydroxide; sodium silicate
[This work was financially supported by the National Science and Technology Development Agency (NSTDA) through the Reversed
Brain Drain Program (No.01-49-005), Thailand.]
Table 2. Physical properties of RHA Commercial grade sodium hydroxide (NaOH) and
Rice husk / Max. burning Specific sodium silicate solutions with 15.32wt% Na2O,
LOI
kg temperature / ºC gravity 32.87wt% SiO2, and 51.81wt% water were used. The
10 580 3.62 1.95 distilled water was used for the whole experiment.
15 610 3.33 1.96 Sodium hydroxide was dissolved in distilled water
20 690 3.25 1.97 prior to the mixing of geopolymer. Local river sand
25 710 2.84 1.99 with a specific gravity of 2.64 and a fineness modulus
50 940 1.94 1.98 of 2.85 was used for making mortar.
Fig. 1. SEM photomicrographs of as-received fly ash (a) and ground RHA (b).
2.2. Preparation of mortar the mixing, flow of mortar was determined in accor-
The mixing was carried out in an air conditioned dance with ASTM C124 [11]. All geopolymer mortars
room at approximately 25°C. FA and RHA were were made with a sand to solid binder (FA+RHA)
thoroughly mixed for 2 min until a uniform color was mass ratio of 2.75. After the determination of flow, the
obtained. Sand was then added and mixed for 3 min. fresh mortar was placed in the 50 mm×50 mm×50 mm
The NaOH, sodium silicate, and extra water were then cube moulds. The specimens were compacted in
added and mixed for another 5 min. Extra water was two-layer with tamping as described in ASTM C109
needed to maintain the workable mortar. Right after [12]. Additional vibration of 10 s was applied using a
722 International Journal of Minerals, Metallurgy and Materials, Vol.16, No.6, Dec 2009
vibrating table. The specimens were wrapped with tested in accordance with ASTM C109. The reported
vinyl sheets to protect moisture loss and kept in the results were the average of three samples.
controlled room at 23±2°C. After a delay period, the 2.3. Series of tests
specimens were then placed in the oven for heat cur-
ing. After the heat curing, the specimens were put in The mortars were mixed using sufficient water to
the laboratory to cool down and demoulded the next produce the flow of 110±5%. The mix proportions for
day and kept in the controlled room. The bulk density making mortars are given in Table 3. In addition to the
and compressive strength of mortars were determined strength test, the mortars were tested for bulk densi-
at the age of 7 d. The compressive strengths were ties.
(1) Temperature of burning of the rice husk (b) Duration of heat curing. In this test, the periods
To test RHA burnt at different temperatures, the of heat curing were 6, 12, 18, 24, 48, 60, and 72 h.
specimens of 80FA20RHA-B and 80FA20RHA-C The specimens were placed in the oven at 75°C using
were used with no delay time and curing at 75°C for delay time of 1 h based on the result of delay time test.
48 h, and 3RHA was used in the specimens. (c) Temperature of heat curing. The curing tem-
(2) Effect of the sodium silicate to NaOH mass ra- peratures of 60, 75, and 90°C were assigned in this
tio and SiO2/Al2O3 molar ratio test. The specimens were placed in the oven using a
delay time of 1 h, and the duration of heat curing of 48
To test the effect of the sodium silicate to NaOH
h in the oven based on the result of the duration of
mass ratio, all the specimens shown in Table 3 were
heat curing test.
used with SiO2/Al2O3 molar ratios of 4.1, 6.1, 9.5, and
16.3, no delay time, and curing at 75°C for 48 h and (4) Fineness of RHA
3RHA was chosen for the specimens. In this test, the 3 different RHAs, namely, 1RHA,
(3) Effect of curing 3RHA, and 5RHA, were used in 80FA20RHA-B. The
specimens were placed in the oven with a delay time
The effects of delay time, temperature of heat cur- of 1 h and a duration of heat curing of 48 h at 60°C
ing and period of heat curing were investigated. Series based on the temperature of heat curing test.
B was used with 3RHA.
(a) Delay time before heat curing. Delay time is the 3. Results and discussion
time duration before placing the specimens in the oven.
3.1. Burning temperature of rice husk
In this test, the delay time of 1, 3, 6, 12, 24, 36, and 48
h were used. After the delay time, the specimens were The results of strength of mortars made from RHA
placed in the oven at 75°C for 48 h. burnt at different temperatures as shown in Fig. 2 in-
S. Detphan et al., Preparation of fly ash and rice husk ash geopolymer 723
dicate that the strength is dependent on the burning contained in the geopolymer pore system and de-
temperature of rice husk. The optimum temperature of creased the strength and performance of geopolymers
RHA burning at 690°C provided the highest strengths [14]. The results of Fig. 4 and Table 1 indicate that the
of 22.5 and 37.0 MPa for the sodium silicate/NaOH increase in the RHA content results in the increases in
mass ratios of 2.5 and 4.0, respectively. The burning the SiO2/Al2O3 molar ratios. The normal FA mortar
temperature of less than 700°C produces amorphous consisted of SiO2/Al2O3 molar ratio of 4.08. For the
silica, which is reactive [13]. Although low burning mortar containing RHA of 60wt%, the SiO2/Al2O3
temperature produced amorphous silica, at very low molar ratio increased to 16.32 with a slight decline in
temperature, the burning is incomplete. This results in the strength of mortars owing to the increased water
the undesirable high amount of the unburnt materials. requirement and the increase in the silica to alumina
As shown in Table 2, the LOI of RHA decreased from molar ratio [8].
3.6 to 1.9 as the temperature of burning increased. On
the other hand, the higher temperature of burning
produces a larger amount of crystalline silica, which is
less reactive [7, 13].
The relationship of the duration of heat curing and mortars. The strengths of mortars made with 5RHA,
strength is shown in Fig. 6. The strength increases 3RHA, and 1RHA were 34.5, 37.0, and 43.0 MPa, re-
with an increase in curing time from 6 to 48 h. Heat spectively. The increase in the fineness of RHA in-
curing beyond 48 h had little effect on the strength of creased its surface area and its reactivity and hence
the geopolymer. An increase in heat curing duration is resulted in an increase in strength of geopolymer
expected to improve the strength characteristics of the mortars. Increases in strength with the use of fine
geopolymer. Similar strength development with high RHA in the partial replacement of Portland cement
temperature curing has been reported [15, 17]. have also been reported [9-10]. RHA with 1%-5% re-
tained on No.325 sieve were suitable source materials
for making geopolymer. Although the very fine 1RHA
gave high strength geopolymer mortars, it required
intense grinding. For practical purpose, 3RHA was
recommended as it gave reasonably high strength geo-
polymer mortars.
The result shown in Fig. 8(b) also indicates a con- tio of 3.68 and a Na2O/Al2O3 molar ratio of 2.22 was
tinuous mass of binder, unreacted FA, and a minor observed. The increase in RHA content increased the
phase of sodium silicate of the FA-RHA geopolymer. ratio of SiO2/Al2O3 and resulted in geopolymers with
The sample of the matrix with a SiO2/Al2O3 molar ra- a lower strength and a higher elasticity [8, 21].
Fig. 8. SEM-EDX photomicrographs analysis of 100FA-B (a) and 40FA60RHA-B (b) (3RHA, delay time of 1 h, curing at
60°C for 48 h).
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