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Abstract
This paper presents the first scientific attempt to develop and study the performance of rice husk
ash (RHA) and ultra-fine slag (UFS) based sustainable geopolymer concrete with different ratio
of corn cob ash (CCA). NaOH (8M) and Na2SiO3 were employed as alkaline activators. CCA acted
mainly as amorphous silica and was utilised as a substitute for RHA. The effects of different CCA
contents (0%, 3%, 6%, 9% and 12% by RHA mass) on the performance of geopolymer concrete
in terms of fresh, hardened and durability properties have been evaluated. Different characteristics,
i.e. density, air content, workability, compressive, flexural and split tensile strengths, Young’s
modulus of elasticity were investigated. Meanwhile, the durability performance was also evaluated
by using different methods such as rapid chloride penetration test, chloride conductivity test, water
sorptivity test and DIN (Deutsches Institut für Normung) water permeability test. The outcomes
of this research have shown that UFS and CCA improved the compressive strength by 14-15%.
They significantly improved the polymerisation and thus enhanced the strength and durability of
sustainable geopolymer concrete. Furthermore, CCA and UFS acted as micro fillers and increased
the CaO as well as SiO2 contents which enhanced the densification. Additionally, the development
of hydration products in the matrix, enhanced the pore structure and thus the strength. This study
revealed that CCA (up to 6%) can be utilised as a substitute binder to produce sustainable
geopolymer concrete, and has the potential to replace conventional concrete for structural
applications.
Keywords: Corn cob ash, drying shrinkage, electrical resistivity, concrete strength, ultra-fine slag.
Abbreviations:
1
1. BD - Bulk density
2. CSH - Calcium silicate hydrate
3. CASH - Calcium aluminate silicate hydrate
4. CCA - Corn cob ash
5. ER – Electrical resistivity
6. MOE – Modulus of elasticity
7. NASH – Sodium aluminate silicate hydrate
8. RHA - Rice husk ash
9. SEM - Scanning electron microscopy
10. UFS – Ultra-fine slag
11. WR - Wenner four-probe resistivity
12. XRD - X-ray diffraction.
1. Introduction
Apart from supplementary cementitious materials and admixtures, cement, water, and aggregates
are generally used to produce the most common construction material, i.e. concrete [1]. Current
practices which are adopted in producing the concrete ingredients, have considerable consumption
of energy and high release of greenhouse gases due to enourmous volume of concrete produced
worldwide [2]. Approximately 0.65-0.85 tons of carbon dioxide (CO2) is produced per ton of
cement production [3]. Accordingly, researchers are looking forward to reducing the massive CO2
emission, energy consumption and natural resources, in order to develop sustainable and green
concrete [4]. Meanwhile, by-products from the industries like fly ash (FA), blast furnace slag
(BFS), RHA, glass powder (GP), CCA and agricultural wastes, are posing great disposal and
dumping problems [5]. Therefore, utilisation of these by-products will decrease the need of
landfills and the pressure on municipal committees [6].
Geopolymer concrete is generally produced using waste materials from industries and activated
using alkaline solutions [7] like sodium silicate (Na2SiO3), potassium hydroxide (KOH) and
sodium hydroxide (NaOH). Recently, researchers focus on using waste-based activators instead of
alkaline activators in the geopolymer concrete in order to further minimise the CO2 footprints [8–
10]. Recent advancements in the field of geopolymer concrete [11] showed that it appears to be a
green construction material due to the fact that it utilises industrial by-products [12] and reduces
2
the energy requirements as well as the efforts required for waste disposal [13]. Furthermore, CO2
imprints of the sustainable geopolymers are about 9% lesser than ordinary Portland cement-based
concrete [14]. In addition, the strength and durability performance of sustainable geopolymer
concrete is comparable to conventional concrete [15]. A range of studies have been done on
geopolymer concrete, like the inclusion to concrete mixes [16], repair and retrofitting of materials
and fireproofing of structures [17]. Remarkable results, principally in the field of pavements [18],
masonry structures [19], reinforced geopolymer composites [20] and repair materials [21] have
been achieved. Therefore, sustainable geopolymer/green concrete can be adopted as an alternative
building as well as construction material.
Apart from ultra-fine slag (UFS), this investigation considered two waste materials, namely RHA
and CCA, for different reasons as discussed below:
• Every year, an average of 20 million tons of paddy, 24 million tons of rice husk and
approximately 4.4 million tons of RHA are produced in India [22]. Worldwide, around
22% of the 648.9 million tons of rice cultivated annually, constitutes of RHA [23].
• Approximately, 1070 and 26 million tons of corn are produced worldwide and in India,
respectively. Accordingly, 170-190 kgs of corn cob waste are generated from 1,000 kg of
corn production [24].
• The physical properties and chemical characteristics shows that utilization of RHA and
CCA may be helpful in the production of geopolymer concrete. For instance, the CaO
(13%) present in the CCA will help in developing the CSH and CASH gels along with
NASH products, similar investigations have not been investigated earlier.
• There is global concern about the reduction in natural resources due to boost up in
population, urbanisation, development, and clearance of the abovementioned by-products.
The reutilisation of wastes for valuable purposes is not only environmentally friendly but
also cost effective [25].
Previous studies have shown that the utilisation of RHA and CCA has conclusive impacts on the
OPC based concrete [24]. Both RHA and CCA both have approximately 70% of the combined
content of SiO2 and CaO [6]. Previous studies on the RHA-based geopolymer concrete revealed
that RHA can be used by employing a mixture of NaOH and Na2SiO3 [26] as activators.
3
Furthermore, CCA and slag based sustainable geopolymer concrete showed good long-term
performance, and thus can be utilised as structural members or non-load bearing concrete [27].
Since the last two decades, significant amount of research works have been done on the
geopolymer concrete using different industrial by-products and waste. However, geopolymer
concrete made of RHA, UFS and CCA is yet to be studied. The novelty of this investigation is to
explore the combined effects of RHA, UFS and CCA on the properties of geopolymer concrete.
This study aimed to figure out both the positive and negative effects of CCA on properties of fresh
and hardened geopolymer concrete, i.e. the workability, compressive, flexural and split tensile
strengths and modulus of elasticity. In addition, XRD, SEM and EDS techniques were used to
study the microstructural characteristics. Finally, potential structural applications of the proposed
material are also suggested.
2. Experimental program
2.1 Materials
2.1.1 Water
Tap water with total alkalinity and pH of 65.8 mg/l and 8.05, respectively, was used in the mixes.
The above values of total alkalinity and pH were within prescribed limits to produce the
geopolymer concrete. Also, sulphate and chloride ions were not detected in the tap water [28].
4
Table 1: Chemical composition and physical properties of processed RHA, CCA and UFS.
Physical and chemical properties Rice husk ash Corn cob ash Ultra-fine slag
Specific Gravity 2.26 2.18 2.70
Mean particle size (d50) μm 11.86 28.23 4.4
BET, Specific surface area m2/kg 910.60 653.20 1200
SiO2(%) 86.20 37.27 38.87
K2O (%) 4.60 15.00 -
P2O5 (%) 2.43 - -
CaO (%) 1.10 13.00 32.20
MgO (%) 0.77 7.35 6.20
Fe2O3 (%) 0.43 1.19 1.20
Al2O3 (%) 0.46 2.37 21.40
MnO (%) 0.11 - -
SO3(%) - 1.32 0.13
Loss on Ignition(%) 3.90 22.50 -
- Not measured.
5
(c) UFS
Fig. 1: SEM images of (a) RHA, (b) CCA and (c) UFS.
6
100
90
80
70
Percentage passing
60
50
40
RHA
30
20 CCA
10 UFS
0
0.001 0.010 0.100 1.000
Particle size (mm)
7
14mm
10mm
Cumulative % passing
7mm
Cumulative % finer
Cum % finer
IS min range
IS max range
1 10 100 0.1 1 10
Sieve size (mm) Log sieve opening (mm)
(a) Coarse aggregate (b) Fine aggregate
Fig. 4: Grading curve of (a) Coarse aggregates (b) Fine aggregates.
8
Rice Corn Total
Fine Coarse Ultra-fine Cob NaOH Na2SiO3
Mixture Husk Alkaline Super -
Aggregate Aggregate Slag Ash [kg/m3] [kg/m3]
Ash Solution plasticizer
S1-R 508 1186 400.0 - - 180.0 51.42 128.5 8.0
S2-R-U 508 1186 360.0 40 - 180.0 51.42 128.5 8.0
S3-R-U-C3 508 1186 349.2 40 10.8 180.0 51.42 128.5 8.0
S4-R-U-C6 508 1186 338.4 40 21.6 180.0 51.42 128.5 8.0
S5-R-U-C9 508 1186 327.6 40 32.4 180.0 51.42 128.5 8.0
S6-R-U-C12 508 1186 316.8 40 43.2 180.0 51.42 128.5 8.0
9
U concrete has approximately 2% higher density than Mix S1-R. UFS increased the density of the
mix because the specific gravity of the UFS was more than RHA (2.7 vs 2.26). Also, UFS has a
larger surface area and smaller particle size, which might have filled more pores. Furthermore, the
addition of CCA into the mixes decreased the density values from 2430 (S2-R-U) to 2,185 kg/m3
(S6-R-U-C12), which is approximately 12%. RHA and CCA have high water requirements, and
therefore they were responsible for the lower fresh density of the concrete. In a study conducted
by Pinto j. et al., they developed the light weight concrete by using CCA and they observed similar
outcomes, in which the addition of CCA resulted in lower density and lower compressive strength
[45].
10
Table 5: Air content of fresh geopolymer concrete.
Mixes
S1-R S2-R-U S3-R-U-C3 S4-R-U-C6 S5-R-U-C9 S6-R-U-C12
1.52 1.48 1.53 1.55 1.75 1.92
1.55 1.56 1.57 1.59 1.69 1.88
Air Content [%]
3.1.3 Workability
The slump values in terms of time are shown in Fig. 5. The slump values varied between 65 to 150
mm. Mixes S2-R-U (150 mm at 0 minute) and S6-R-U-C12 (65 mm at 80 minutes) represented
the maximum and minimum values of the slump, respectively. A noticeable decrease in slump
values was observed with the increase in CCA percentage. Accordingly, the initial slump values
of Mixes S3-R-U-C3, S4-R-U-C6, S5-R-U-C9 and S6-R-U-C12 were 3%, 13%, 16% and 28%,
respectively, lesser than that of Mix S1-R.
The irregular shape and high water demand of RHA and CCA lead to the decrease in slump values.
Meanwhile, the spherical and small particle size of UFS enhanced the slump values. Therefore, it
is suggested that saturated RHA and CCA should be used if higher slump values are desirable.
Furthermore, the superplasticiser amount can be increased to improve workability performance.
Parveen et al. [3] showed that workability can be improved by using UFS. According to Jindal et
al. [46], UFS and RHA particles combined with the lubricating effect of alkaline solution enhanced
the slump values. The decrease in slump values with time and with the increase in CCA
percentages may be due to high molarity of NaOH solution and limited pozzolanic activity of CCA
[47,48].
11
Fig. 5: Slump values of different mixes at different periods.
12
the age of 7 days the percentage reduction in compressive strength of mix S6-R-U-C12 was
approximately 38-39%, when compared with mix S2-R-U.
Also, the compressive strength increased with time, for example, an increment of approximately
12-14% and 5-7% was noticed when the compressive strength at the age of 7 and 28 days, 28 and
56 days were compared, respectively. The strength improvement was less pronounced at greater
age period, and it may be due to the fact that CCA diluted the polymerisation effect. However,
UFS enhanced the strength, and in some cases, the strength of UFS and CCA-based geopolymer
concrete was comparable to the RHA-based geopolymer concrete. This may be due to the effect
of the formation of calcium silicate gel into the matrix [49–51]. It can be concluded from the results
that the same grade of geopolymer concrete (like S1-R) can be produced by using S5-R-U-C9
design mix. Although, the study on the CCA-based geopolymer concrete has not been reported so
far, the results of this study were in agreement with the previous studies based on the UFS [6,51].
Furthermore, the effect of CCA on the geopolymer concrete was similar to its effects on
conventional concrete [52,53]. The strength gain behaviour of geopolymer concrete was not
similar to conventional concrete due to the fact that geopolymer concrete achieves maximum
strength at the age of 7 days when heat curing is adopted. Meanwhile, in this study, conventional
concrete was not developed, and results from the existing literature were referred for comparison.
13
Fig. 6: Compressive strength of different mixes at the age of 7, 28 and 56 days.
14
might have been the reason for adequate strength. Adesanya et al. [54] and Parveen et al. [55]
previously reported that the use of high silious and calcium based materials in the production of
geopolymer concrete led to an increase in the compressive and split tensile strengths while the
specific gravity plays an important role in the strength development.
Fig. 7: Split tensile strength of different mixes at the age of 7, 28 and 56 days.
15
S2-R-U, i.e. 5.09, 5.76 and 6.16 MPa at 7, 28 and 56 days, respectively. The percentage decrease
in the flexural strength after incorporating the CCA into the matrix were 20-25% of its maximum
strength at all ages. Furthermore, the percentage increase in the flexural strength after adding UFS
were 11-14% and 17-20% of its 7 days strength for all the specimens. It is a well-known fact that
the tensile properties of geopolymer concrete are greater than conventional concrete [56].
Although, CCA addition decreased the flexural strength, but reasonable values were obtained for
S4-R-U-C6 mix specimens. Pranav et al. [57] studied the properties of CCA based concrete with
replacement of cement up to 20%. The optimum replacement ratio was found to be at 10%. Nath
et al. [58] compared the mechanical properties of GPC with different additives and corresponding
OPC, and concluded that flexural strength of GPC cured at ambient temperature mostly followed
similar development trend as that of flexural strength of OPC concrete. Hardjito et al. [59] and
Diaz et al. [60] also proved in their studies that when compared with OPC, GPC of similar grade
exhibited higher flexural strength OPC. Furthermore, this was consistent for both heat cured and
ambient cured GPC’s. The reported trend was similar to the current study.
16
Fig. 8: Flexural strength of different mixes at the age of 7, 28 and 56 days.
17
yielded comparable MOE to that of GPC. The minimum MOE was observed for mix S6-R-U-C12
(28.38 GPa at 7 days) while S2-R-U exhibitted the maximum MOE (38.67 GPa at 28 days).
Luhar et al. [56] reported that the MOE of GPC depends upon geopolymeric microstructure, and
not on the aggregate size. The CCA addition reduced the density of concrete, and therefore lower
values of MOE were obtained with higher CCA content. Additionally, high CCA content might
have affected the rigidity properties of the sustainable GPC and in turn, led to lower MOE. The
MOE of the GPC mixes was slightly lower (range 4.90-4.97*√fc, GPa) than that of conventional
concrete (5.0*√fc, in GPa, where fc is the 28-day compressive strength) [61] with the same strength
at the age of 7 days, after 28 days it was equivalent or on the higher side. Similar observations
have been reported in the literature, where the MOE of GPC varied from 20-31.50 GPa
(compressive strength varied from 24.0 to 61.5 MPa) and that for OPC concrete ranged from 18-
27.50 GPa (compressive strength varied from 25.4 to 56.9 MPa) [56]. The results in this study are
compared to those reported by different studies in the literature as shown in Table 6. The MOE of
GPC depends upon the various factors like, density, paste, types of aggregates, curing methods
and compressive strength, therefore, a variation can be observed for MOE values. It is also worth
noting that the significant variation of the MOE within the margin of ±20% from the mean value
is common and acceptable as recommended in Australia standard 1012.14:2018 [62]. Joseph et al.
[63] studied the performance of GPC at elevated temperature and reported high values of MOE’s
(42.36-59.06 GPa). Furthermore, results of this investigation were closely related to the results
obtained from the equation predicted by ACI 318 [64]. Ultrafine slag enhanced the microstructure
of the GPC, thus a higher range of modulus of elasticity was obtained in this investigation, and
comparable to those in the previous studies, given a similar strength.
Table 6: Comparison of the MOE from this study and other studies
18
43.79 32.67 33.34 29.90 32.95 28.69 23.21 23.23
48.92 31.92 33.34 31.02 34.97 28.69 24.23 24.55
54.75 34.22 36.58 32.21 36.92 31.48 25.33 25.97
59.83 36.62 39.85 33.18 38.68 34.29 26.24 27.15
19
resistance against chloride ion penetration [68] as shown in Fig. 10. The electrical conductance of
the samples was further decreased when RHA was replaced with CCA. A reduction of
approximately 70, 74, 76 and 79% were observed when samples S2-R-U, S3-R-U-C3, S4-R-U-
C6, S5-R-U-C9 and S6-R-U-C120 were compared with S1-R mix, respectively. This trend at the
age of 56 days was the same, and therefore it can be concluded that CCA blended samples have
better durability as more resistance was offered by the samples at all ages. Further, it falls under
“very low” permeability concrete as per standards [68]. The primary reasons behind its very low
permeability were: (a) silica present in the RHA and CCA were reactive and lowered down the
pore solution conductivity, and (b) calcium present in the UFS enhanced the pore structure by
lowering the pore conductivity. Similar trends were reported in the previous studies based on
geopolymer concrete [55,69] where sugar cane ash and RHA were utilized.
20
Fig. 10: Total charge passed for different mixes at the age of 28 and 56 days.
Chloride conductivity index (CCI) of different mixes were measured at the age of 28 and 56 days,
respectively, and shown in Fig. 11. The CCI indices of sustainable geopolymer concrete with CCA
were lower than the reference samples with 0% CCA. For instance, a reduction of approximately
35% was observed when sample S6-R-U-C120 was compared with S1-R, and at the age of 28
days. Although CCI indices of all the specimens were lower at 56 days when compared with 28
days CCI indices, the trend was similar to that obtained at the age of 28 days. This observation
indicated that lower permeability of the samples was due to the effects of polymeric and hydration
products. To analyse the effects of CCA on geopolymer concrete properties, a comparison of CCA
and RCPT results at the age of 56 days was employed and the outcome is shown in Fig. 12. It is
worth noting that CCI results agree well with the trends observed in RCPT. Excellent pozzolanic
reactivity of UFS and CCA enhanced the pore structure and was responsible for better durability
in terms of chloride resistance penetration.
21
Fig. 11: Chloride conductivity index for different mixes at the age of 28 and 56 days.
22
Fig. 12: Comparison of RCPT and CCI at the age of 56 days.
23
properties. Also, the presence of UFS helped in reducing the depth of water penetration, which
provides further resistance against aggressive environments [70]. Furthermore, the higher values
of water penetration depth for the samples without CCA, may be attributed to the higher curing
temperature since the ambient curing condition has been suggested in standards. UFS improved
the pore structure, and its finer size fills up the voids, which further helped in reducing the water
penetration depth values as also reported in the previous study [71].
Fig. 13: Depth of penetration for different mixes at the age of 28 and 56 days.
24
In the water sorptivity tests, conditioned specimens were placed on wedges or rollers (placed at
the bottom of a tray) and calcium hydroxide solution was poured into the tray up to a level of 2
mm above the bottom surface of the specimens. The specimens were removed periodically for
mass measurement, and the surface was gently wiped with a moist paper towel to achieve saturated
surface dry condition on the exposed face. Mass of the specimen was measured on a balance with
an accuracy of 0.01 g. The sorptivity index was calculated as the average of the water sorptivity
of at least three tested specimens in this study. Water sorptivity index is the resistance offered
against water movement by capillary suction through the exposed surface of the specimens. Since
the pore structures and curing period influenced the sorptivity index, therefore it were determined
for all the specimens at the age of 56 days. Results of the sorptivity tests shown in Fig.14 indicates
that marginal difference was observed in the values of all the mixes. Water sorptivity index varied
from 8.75 to 9.95, and the lowest value was obtained from mix S2-R-U. Water sorptivity index is
greatly affected by surface characteristics rather than permeability [72,73], and this would have
been the reason for the indifferent performance of the CCA, and UFS sustainable geopolymer
concretes. Sorptivity index has a wide range of classification, starting from less than 6 to greater
than 15 [74]. The higher initial water absorption shows higher sorptivity value as reported by the
previous study [75]. The addition of CCA at higher percentage increased the sorptivity index
values, and it may be due to the fact that surface characteristics such as pore geometry and pore
volume of the specimens were highly influenced by the CCA content [74].
25
Fig. 14: Sorptivity index for different mixes at the age of 56 days.
Next, the comparison of water penetration depth and sorptivity index was carried out and
represented in Fig. 15. The results of water penetration and sorptivity reveal a little bit different
trend of water movement in the hardened concrete surface as this phenomenon was also observed
in the previous study [72]. RHA content affects the structural compatibility by hindering the
polymeric reaction. As a result, it enhances the capillary suction [76] due to the smaller particle
with higher surface area (RHA, slag) [75] which is higher in both depth of water penetration and
sorptivity tests.
26
Fig. 15: Comparison of sorptivity index and depth of penetration for different mixes at 56 days
curing.
27
and 8.89 kΩ cm, at 28 and 56 days, respectively. Besides, the results show that with an increase in
CCA content from 3-12% in geopolymer concrete, the electrical resistivity and corrosion values
showed a decreasing trend. The present study also found that the electrical resistivity decreased
substantially with increase in curing age, from 28 days to 56 days.
Fig. 16: Electrical resistivity for different mixes at the age of 28 and 56 days.
A comparative study was conducted between electrical resistivity and chloride conductivity at 56
days of age, as shown in Fig. 17. A substantial reduction in the resistivity of concrete with respect
28
to the reduction of the chloride conductivity index within the specimen is observed. It is more
likely that the risk of corrosion increases in the specimen when the percentage of CCA replacement
increases from 3-12%, such as S1-R-U-C3, S1-R-U-C6, S1-R-U-C9 and S1-R-U-C12 in
geopolymer concrete, compared with the specimen containing only RHA and RHA with UFS
material. The use of S1-R and S6-R-U-C12 is more vulnerable to corrosion as compared to the
other mixes.
Fig. 17: Comparison between electrical resistivity and chloride conductivity at the age of 56
days.
29
3.9 Drying shrinkage
The change in length with respect to curing age is depicted in Fig. 18. At the initial stage, the rate
of drying shrinkage was comparatively higher than as observed at later ages. Furthermore, the
difference between the drying shrinkage values of all the samples was not significant. There was
insignificant difference in the observed values of drying shrinkage due to the addition of CCA into
the matrix. The addition of UFS increased the drying shrinkage values. The outcomes of this study
agree with the study done by other researchers [74,78]. It can be concluded from this study that
UFS plays a prominent role to change the pore structure by improving the polymerisation process.
The formation of products like CSH, CASH, and NASH has been confirmed in the earlier studies
which improved the structure [21]. The drying shrinkage values acquired in this study were also
well below the limits (800 microstrain for moist cured concrete and between 730 to 788 microstrain
for steam cured concrete) as recommended in the report of ACI 209 committee [79].
30
4. Conclusions
In this study, the performance of sustainable geopolymer concrete with CCA and UFS partially
replacing RHA was investigated. Six mixes were prepared to study its mechanical properties and
durability. The main conclusions are drawn as follows:
The detailed investigation of the strength and durability properties suggest that CCA can be used
as RHA substitution (up to 6%) to produce sustainable and good quality geopolymer concrete.
31
Acknowledgement
The authors wish to thank Raicon Labs Private Limited, Haryana, India for giving support to test
the samples in their laboratory. The financial support from Small Grant, Curtin University is
greatly appreciated.
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