Construction and Building Materials 314 (2022) 125480

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Construction and Building Materials

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Mechanical and microstructural characterization of fly ash blended

self-compacting concrete containing granite waste
Abhishek Jain a, Sandeep Chaudhary b, Rajesh Gupta c, *
a
Department of Civil Engineering, Swami Keshvanand Institute of Technology, Management & Gramothan, Jaipur 302017, Rajasthan, India
b
Department of Civil Engineering, Indian Institute of Technology Indore, Simrol, Indore 453552, India
c
Department of Civil Engineering, Malaviya National Institute of Technology, Jaipur 302017, Rajasthan, India

A R T I C L E I N F O A B S T R A C T

Keywords: This study examines the mechanical characteristics (compressive strength, split tensile and flexural strength) and
Fly ash microstructure characteristics (scanning electron microscopic (SEM), energy dispersive X-ray spectrometry
Granite waste (EDS), X-ray diffraction (XRD) and Fourier transform infrared radiation (FTIR)) of fly ash blended self-
Self-compacting concrete
compacting concrete (SCC) comprising of granite waste (GW). Mechanical performance of fly ash blended
Mechanical characteristics
Microstructural characteristics
SCC augmented on the incorporation of up to 40% GW as a substitution of fine aggregate. SEM analysis revealed
that the incorporation of GW densified the binder-aggregate matrix of resulting SCC. However, EDS, XRD and
FTIR analysis revealed that there was a negligible effect of GW on the development of hydration products. It was
thus concluded that the enhancement in the mechanical performance of the resulting SCC (prepared with GW)
was mainly due to the filler efficacy of GW.

1. Introduction
Self-compacting concrete (SCC) is the upgraded version of normally
vibrated concrete (NVC) that can smoothly move in narrower and jam-
packed reinforced sections. It has many advantages over NVC, for
example, increases construction speed, improves quality of concrete
without voids and honeycombing, and reduces labour cost and noise
pollution [1–5]. Due to several advantages of SCC, the utilization of SCC
has become escalated with the advancement in construction technology.
However, the cost of SCC is very high as compared to the NVC since it
comprises excessive cement content and chemical admixture for
attaining adequate stability and flowability. Several investigations have
been done by earlier researchers who had effectively employed diverse
secondary cementitious materials such as fly ash, ground granulated
blast furnace slag, metakaolin, and silica fume in SCC to reduce the
cement amount [6–13]. These cementing materials generally augment
the engineering characteristics of concrete by the action of pore
refinement provided by their small size particles as well as pozzolanic
activity [11,14,15]. Furthermore, to improve the cost-effectiveness and
sustainability of SCC, the waste materials or recycled sand, especially
having higher fines can be utilized as a substitute for river sand aggre­
gate. These types of materials can also contribute to the filler content of
SCC and additionally may improve fresh and hardened characteristics of
SCC.
Granite waste (GW) is one such type of waste material produced
during the extraction and transformation of granite stones, which
comprises a high quantity of fines. Accumulation of this waste is
endlessly increasing, which is polluting the environment as well as
affecting the human too. Earlier, studies have been performed on the use
of GW in the development of mortar and NVC. However, few studies are
available on its application in SCC. Cheah et al., [16] produced ternary
blended mortar by full volumetric replacement of fine aggregate with
GW and obtained the highest compressive strength at 60% replacement
level of GW. Vyas and Gupta [17] found better mechanical and dura­
bility performance of granite blended mortar as compared to the con­
ventional cement mortar. Vijayalakshmi et al., [18] and Ghannam et al.,
[19] found the highest compressive strength at a very low substitution
level (i.e. 10%) of natural fine aggregate with GW in NVC. Improvement
in compressive and flexural strength of NVC was also observed by Singh
et al., [20,21] on the substitution of fine aggregate with GW. Ghorbani
et al., [22] found about 11% and 8% improvement in compressive and
split tensile strength characteristics, respectively, at 10% substitution
level of cement with GW.
Elyamany et al., [23] and Sadek et al., [24] stated the improvement

* Corresponding author.
E-mail address: rgupta.ce@mnit.ac.in (R. Gupta).

https://doi.org/10.1016/j.conbuildmat.2021.125480
Received 10 July 2021; Received in revised form 21 September 2021; Accepted 28 October 2021
Available online 13 November 2021
0950-0618/© 2021 Elsevier Ltd. All rights reserved.
A. Jain et al. Construction and Building Materials 314 (2022) 125480

in compressive strength on the incorporation of GW (by weight of

cement) in SCC as a mineral additive. Karmegam et al., [25] prepared
SCC by replacement of cement up to 20% with GW and obtained
enhancement in compressive strength on replacement of up to 10% of
GW. Aarthi and Arunachalam [26] also reported a positive result on the
inclusion of GW in SCC as a substitute of cement.
It has also been well recommended that SCC exhibits superior me­
chanical performance as compared to that of NVC due to the better-
refined microstructure contributed by the presence of higher fine con­
tent in SCC [27]. There are several microstructural technologies such as
scanning electron microscopic (SEM), energy dispersive spectroscopy
(EDS), X-ray diffraction (XRD) and Fourier transform infrared (FTIR)
spectroscopy which is being extensively utilized to investigate the
change in morphological and chemical behaviour of modified mortar/
concrete matrix [4,16,21,28–35]. Some of the researchers have analysed
the microstructure behaviour of granite modified mortar/concrete ma­
trix [16,21,24]. Cheah et al., [16] observed improvement in micro­
structure of blended mortar matrix containing GW through SEM analysis Fig. 1. Microstructure of fly ash.
mainly due to the filler effect of GW. Singh et al., [21] carried out SEM
and XRD analysis for evaluating microstructural behaviour of granite
based NVC. They found dense microstructure of developed granite based Table 1
concrete matrix due to the additional formation of calcium silicate hy­ Chemical composition of cement, fly ash, fine aggregate and GW.
drated (CSH) gel. Sadek et al., [24] realized a more refined micro­ Chemical composition (%) Cement Fly ash Fine aggregate GW
structure for granite based SCC matrix as compared to marble based SCC
CaO 45.88 0.90 2.51 0.89
matrix using SEM analysis. SiO2 31.30 58.19 77.25 69.77
Previous studies indicated that GW has the potential to enhance the Al2O3 3.49 26.93 6.14 10.74
performance of concrete either as an alternative to cement or fine Fe2O3 3.30 4.27 1.12 1.80
aggregate. However, fewer investigations have been conducted on the Na2O 0.22 0.07 1.08 3.13
K2O 0.69 1.10 4.28 4.84
incorporation of GW (as a fine aggregate) in fly ash blended SCC. The MgO 5.21 0.69 0.34 0.54
effect of GW on the microstructural characterization of fly ash blended P2O5 0.05 0.21 0.05 0.05
SCC has also not been fully investigated in past studies. The contradic­ MnO 0.05 0.06 0.04 0.03
tory behaviour regarding the microstructural behaviour was also LOI 3.97 0.45 – –
observed on incorporating GW in concrete matrix. Moreover, SCC ren­
ders considerable changes in microstructural variation due to the high
amount of fine powder content. This study has thus been conducted to
assess the comprehensive mechanical and microstructural behaviour of
fly ash blended SCC containing GW. Compressive strength, flexural
strength and split tensile strength were evaluated to determine me­
chanical performance of SCC up to 180 days curing. SEM, EDS, XRD and
FTIR analysis were conducted at 28 days and 180 days curing to
determine microstructural behaviour of SCC. It is expected that an
engineered combination of two industrial wastes as a substitution of
natural resources would not only lessen cost of SCC mixes but also
protect the environment by preserving the natural resources as well as
solving the disposal issue of industrial wastes.

2. Experimental program

2.1. Materials
Ordinary Portland cement (OPC 43 grade), fly ash (class F), fine
aggregate (river sand of maximum 4.75 mm size), granite waste
(maximum 4.75 mm size) and coarse aggregate (basalt stone of
maximum 10 mm size) were utilized for the production of SCC. OPC and
fly ash used, in this study, were agreeing to BIS 8112 [36] and ASTM
C618 [37], respectively. Specific surface area of cement and fly ash were
measured using Blaine air permeability method as per the BIS 4031 (part
2) [38]. Cement and fly ash have a specific gravity of 3.16 and 2.28, and
specific surface area of 297 m2/kg and 353 m2/kg, respectively. Fig. 1
displays the smooth and rounded morphology of fly ash. Chemical
composition of cement, fly ash, fine aggregate, and GW are presented in
Table 1. Fig. 2 illustrates the gradation of fine aggregate, coarse aggre­
gate and GW. The gradation of aggregates complied with BIS 383 [39].
The sieve analysis results for fine aggregate and GW indicated that the
size of GW particles is smaller than the fine aggregate. Fine aggregate
and GW have a specific gravity of 2.64 and 2.57, and water absorption of
Fig. 2. Gradation of aggregate and GW [15].
1.00% and 4.49%, respectively. Fig. 3 displays the surface morphology
of fine aggregate and GW, which indicated that GW has rough and
angular morphology than the relatively smooth and granular
morphology of fine aggregate. The results of X-ray diffraction analysis
indicated that GW primarily comprises phases of quartz (SiO2), albite
(NaAlSi3O8) and microcline (KAlSi3O8), whereas fine aggregate pri­
marily comprises phases of quartz (SiO2). A high range water reducer
superplasticizer (SP) of Glenium Sky 8777 (polycarboxylate ether (PCE)
based) was utilized.
2.2. Mix proportion
Nine SCC mixes were formulated having a uniform binder content of
548.53 kg/m3 and effective water to binder ratio of 0.35. Out of nine
SCC mixtures, one mixture (OPC-SCC-GW0) was prepared with only

2
A. Jain et al. Construction and Building Materials 314 (2022) 125480

(b)

Fig. 3. Microstructure of (a) fine aggregate; (b) GW.

OPC binder named as OPC based control mixture, one mixture (FA-SCC-
GW0) was prepared by integrating cement and fly ash at a level of 70%
and 30%, respectively, named as fly ash blended control mixture. While
remaining mixtures, which are fly ash blended, were formulated by the
replacement of fine aggregate with GW at varying amounts of 20%,
25%, 30%, 35%, 40%, 50%, and 60%. The amount of fly ash and GW
was chosen based on an earlier study carried out by the authors [40].
Other researchers have also recommended the incorporation of fly ash
up to 35% as a cement replacement in the concrete mixtures [8,41,42].
Water correction was applied for compensating the water absorption of
aggregates [43,44]. However, the effective water to binder ratio was
maintained as 0.35 only. The water content was changed to bring the
aggregate to saturated surface dry condition. SP dosages were adjusted
to attain the target slump flow of 750 ± 30 mm. Details of all SCC
mixture and their mixture ID are presented in Table 2.
2.3. Testing procedure
Fresh characteristics of developed SCC mixtures were evaluated
complying to EFNARC standards [45,46]. Authors of this study earlier
found that all the SCC mixtures met the requirement laid down by
EFNARC standard for successful SCC mixture [47].
Compressive and flexural strength were evaluated according to
BIS:516 [48], whereas split tensile strength was evaluated according to
BIS: 5816 [49]. Cubes of size 100 × 100 × 100 mm, 150 × 150 × 150
mm, and beams of size 500 × 100 × 100 mm were cast for compressive
strength, split tensile strength, and flexural strength, respectively.
Compressive strength was evaluated at the water curing ages of 7, 28, 90
and 180 days, whereas both flexural and split tensile strength were
evaluated at the water curing ages of 28, 90 and 180 days. Two point
loading setup was used for flexural strength test.
SEM, EDS, XRD and FTIR analysis were conducted to determine the
microstructural and chemical behaviour of developed SCC mixtures.
SEM analysis was performed for characterizing the microstructure or
morphology of the developed SCC samples. Nova Nano SEM-450
apparatus was utilized for SEM analysis. A 10 × 10 × 10 mm concrete
sample was prepared for each mix, which was obtained from 100 mm
cube specimens. EDS analysis was conducted in conjunction with SEM
imaging analysis. This analysis was conducted to obtain the elemental
composition of developed SCC mixes.
For the XRD analysis of SCC samples, the Rigaku powder diffrac­
tometer apparatus was utilized. This test was performed for identifying
the mineral phases in composites. The test was conducted on powder
samples having a size less than 90 µm, which were obtained by 100 mm
cube specimens through crushing and grinding techniques. The data was
collected for an angle of 2θ ranged between 5 and 80◦ with a step size of
0.02◦ . For analysing the collected data, the X’pert high score plus soft­
ware was utilized [29,50,51].
For FTIR analysis, the Perkin Elmer apparatus was utilized to identify
the molecular groups in concrete samples with the scan range of
400–4000 cm− 1. The powder sample adopted for this analysis was
similar to the XRD analysis. Pellets were formed by blending 1 mg of
powder sample with 300 mg of KBr powder.

Table 2
SCC mix proportions (Kg/m3).
Mixture ID Cement Fly ash Fine aggregate GW Coarse aggregate Water## SP dosage

OPC-SCC-GW0* 548.53 – 968.35 – 698.17 204.47 2.61

FA-SCC-GW0** 383.97 164.56 968.35 – 698.17 204.47 0.82
FA-SCC-GW20# 383.97 164.56 774.68 193.67 698.17 211.23 0.77
FA-SCC-GW25# 383.97 164.56 726.26 242.09 698.17 212.92 0.74
FA-SCC-GW30# 383.97 164.56 677.85 290.51 698.17 214.60 0.80
FA-SCC-GW35# 383.97 164.56 629.43 338.92 698.17 216.29 0.93
FA-SCC-GW40# 383.97 164.56 581.01 387.34 698.17 217.98 1.04
FA-SCC-GW50# 383.97 164.56 484.18 484.18 698.17 221.36 1.21
FA-SCC-GW60# 383.97 164.56 387.34 581.01 698.17 224.74 1.70

* Ordinary Portland cement based control mixture (without fly ash and GW).
** Fly ash blended control mixture (without GW).
# Fly ash blended mixtures (with 20% to 60% GW).
## Effective water was 191.99 kg/m3 in each mix.

3
A. Jain et al.
3. Result and discussion
3.1. Mechanical characteristics
3.1.1. Compressive strength
Fig. 4 displays the compressive strength for all the SCC mixes at 7,
28, 90 and 180 days of curing periods. As compared to the OPC based
control SCC mixture (OPC-SCC-GW0), the 7, 28 and 90 days compres­
sive strength of fly ash blended control SCC mixture (FA-SCC-GW0) were
found to be lower. However, decrement in the loss of compressive
strength was found with the prolonging in curing times. The 180 days
compressive strength of FA-SCC-GW0 mixture was found to be higher
than OPC-SCC-GW0 mixture. These outcomes indicated the noticeable
pozzolanic reactivity of fly ash at higher curing times. The continuous
development of CSH gel by the action of slower pozzolanic reactivity of
fly ash causes to increase the densification of concrete matrix, resulting
in increased compressive strength with the prolonging in curing time.
The findings are in match with past studies [52–54].
Furthermore, as compared to FA-SCC-GW0 mixture, fly ash blended
SCC mixtures containing up to 40% GW exhibited higher compressive
strength at all curing ages. The binary blended concrete mixture con­
taining 30% GW (FA-SCC-GW30 mixture) exhibited the highest
compressive strength at all the curing times (except 7 days curing time),
whereas FA-SCC-GW60 mixture exhibited the lowest compressive
strength. The enhancement in compressive strength on the incorpora­
tion of GW might be due to the pore refinement of SCC matrix, which
was related to the smaller size of GW (Fig. 2) than the fine aggregate.
The rough and irregular microstructure of GW (Fig. 3) than the fine
aggregate also made a better bond amid the binder and aggregate phase,
which caused the higher compressive strength [16]. SEM images are
shown in the subsequent section (3.2.1) also corroborate this claim.
Gupta et al., [55] also stated that the inclusion of finer and rough nature
of stone dust particles as an alternative to fine aggregate augments the
interfacial transition zone (ITZ) and packing density of concrete matrix.
However, as compared to the FA-SCC-GW0 mixture, the lower
compressive strength was perceived for the replacement of fine aggre­
gate beyond 40% with GW at all curing ages. This might be due to the
reduction of binder content for binding the aggregate phase as GW had a
smaller size than the fine aggregate. The reduction of binder content
ultimately led to developing a weak ITZ amid mortar and aggregate
phase with an opposing impact on compressive strength. Further, the
significant viscosity and entrapment of water within the concrete matrix
for higher replacement of GW has been observed by authors in an earlier
study [47], which formed voids on the hardening of concrete and ulti­
mately caused the reduction in strength. Additionally, at higher GW
replacement level (>40%), the extra added water highly increased the
Fig. 4. Compressive strength of blended SCC containing varied percentage
of GW.
4
Construction and Building Materials 314 (2022) 125480
water to binder ratio for SCC mixture, which caused a poor gradation of
the concrete mixture [43,44]. Such a phenomenon developed porous
microstructure, at higher GW content, by overcoming the filler effect of
fly ash and GW resulting in reduced compressive strength. SEM images
are shown in the subsequent section (3.2.1) also corroborate above
claims.
Earlier researchers observed a similar modification to compressive
strength for different types of granite modified concrete. Vijayalakshmi
et al., [18] and Ghannam et al., [19] perceived the improvement in
compressive strength of NVC on swapping of up to 10% and 20% fine
aggregate by GW, respectively. Singh et al., [20] and Singh et al., [21]
perceived the highest compressive strength of NVC at swapping of 25%
of fine aggregate with GW. Karmegam et al., [25] and Sadek et al., [24]
also noticed an improvement in compressive strength of granite based
SCC as compared to the conventional SCC. Enhancement in strength of
mortar composite was also perceived by Gupta and Vyas [17] and Cheah
et al., [16] on swapping of fine aggregate by GW.
3.1.2. Split tensile and flexural strength
Figs. 5 and 6 display the split tensile and flexural strength results,
respectively, for all the SCC mixes at 28, 90 and 180 days of curing
periods. The values of split tensile and flexural strength are in good
conformity with the values observed for compressive strength. Similar to
compressive strength, FA-SCC-GW0 mixture showed lower tensile
strength for 28 and 90 days curing as compared to OPC-SCC-GW0
mixture. Whereas, for 180 days curing, both strength values of FA-
SCC-GW0 mixture were found to be higher than OPC-SCC-GW0 mixture.
Furthermore, for all the curing times, the split tensile and flexural
strength were found to be higher on the replacement of up to 50% fine
aggregate with GW than the FA-SCC-GW0 mixture. Thereafter, only at
60% GW content, both strength characteristics were found to be lower as
compared to FA-SCC-GW0 mixture. Moreover, the highest split tensile
strength was observed for FA-SCC-GW30 mixture at all the curing days.
Whereas, the highest flexural strength was observed for FA-SCC-GW35
mixture. This increment in tensile strength performance may be due to
the efficient packing between the aggregate and mortar phase (Fig. 7(c)
and 8(c)). The presence of rough and angular particles of GW might have
provided the better interlocking amid binder and aggregate phase,
which enhanced the tensile strength performance of developed concrete.
SEM images are shown in the subsequent portion (3.2.1) corroborate
above claims. Improvement in tensile strength performance might also
be due to the higher resistivity of crack propagation on tensile loading
through the better interlocking between GW and binder phase [16]. The
outcomes of split tensile and flexural strength indicated that the inclu­
sion of GW was significantly efficient in improving the tensile strength
Fig. 5. Split tensile strength of blended SCC containing varied percentage
of GW.
A. Jain et al.
Fig. 6. Flexural strength of blended SCC containing varied percentage of GW.
capacity of SCC matrix.
A similar modification to improvement in tensile strength was
perceived by Singh et al., [21] on swapping of GW in NVC as a fine
aggregate. Another study done by Singh et al., [20] perceived>10%
increase in 28 days flexural strength on swapping 50% fine aggregate by
GW in NVC. Whereas, at 28 curing days, a maximum of 14.25% and
23.84% increase in flexural strength was observed for FA-SCC-GW35
mixture as compared to OPC-SCC-GW0 and FA-SCC-GW0 mixture,
respectively. The enhancement in flexural strength of granite mortar
composites was also observed by Cheah et al., [16] on the replacement
of NFA with GW.
3.2. Microstructure characteristics
SEM, EDS, XRD and FTIR analyses were conducted for microstruc­
tural characterization of developed SCC mixtures. These analyses were
conducted on four typical concrete mixtures (OPC-SCC-GW0, FA-SCC-
GW0, FA-SCC-GW30, FA-SCC-GW60) for water curing durations of 28
days and 180 days. Moreover, OPC-SCC-GW0 and FA-SCC-GW0 are the
OPC based and fly ash blended control mixture, respectively. Whereas
FA-SCC-GW30 and FA-SCC-GW60 exhibited optimum and least me­
chanical performance, respectively. Therefore, studies related to
microstructure analyses were restricted to these mixtures only.
3.2.1. Scanning electron microscopic (SEM)
SEM images (at 5000x) are shown in Fig. 7(a-d) and Fig. 8(a-d) for
curing durations of 28 days and 180 days, respectively. Mortar matrix
around the aggregates and ITZ amid mortar matrix and aggregates are
the prime most phases of concrete matrix, which profoundly influence
its characteristics [6,56]. Both mortar matrix and ITZ phases were
examined via SEM images to reveal the influence of fly ash and GW on
the mechanical performance of developed SCC mixtures.
At both the curing durations (28 days and 180 days), relatively more
homogenous mortar matrix and dense ITZ were observed for FA-SCC-
GW0 mixture (Fig. 7(b) and Fig. 8(b), respectively) as compared to
OPC-SCC-GW0 mixture (Fig. 7(a) and Fig. 8(a), respectively). The better
filler efficacy of small size fly ash particles provided the homogenous
mortar matrix and dense ITZ in the FA-SCC-GW0 mixture. However, at
28 days curing periods, the unreacted fly ash particles (of smooth and
spherical shape) can be observed in the FA-SCC-GW0 mixture (Fig. 7(b))
as compared to OPC-SCC-GW0 mixture (Fig. 7(a)). The presence of
smooth and spherical morphology of fly ash particle in FA-SCC-GW0
mixture (Fig. 7(b)), at 28 days curing duration, indicated the inert na­
ture of fly ash at initial days. On the other hand, at 180 days curing
periods, the denser and improved ITZ/paste matrix were observed in the
fly ash based control mixture. Rough spherical surfaces of fly ash sur­
rounding with CSH gel can be noticed in Fig. 8(b), which indicated
5
Construction and Building Materials 314 (2022) 125480
pozzolanic reactivity of fly ash. It was reported that latent pozzolanic
reactivity of fly ash particles develops a considerable amount of CSH gel
in the vacant space of the concrete matrix, at later ages, which leads to
an improvement in paste matrix and ITZ phases [53]. The continuous
evolution of CSH gel, at later ages, improved the mechanical perfor­
mance of FA-SCC-GW0 mixture as compared to that of OPC-SCC-GW0
mixture. By comparing the microscopic images of FA-SCC-GW0
mixture at both curing duration, it can be inferred that physical filler
efficacy of fly ash acted at an early age, whereas pozzolanic/chemical
reactivity of fly ash acted at a later age. Though fly ash acted as a filler at
an early age, it did not improve 28 days mechanical performance of FA-
SCC-GW0 concrete mixture as compared to OPC-SCC-GW0 mixture. This
was because of the replacement of 30% cement content with fly ash,
which led to a reduction of cementing material in fly ash based concrete.
Fig. 7(c) and Fig. 8(c) present the microscopic images of fly ash based
concrete mixture containing 30% GW (FA-SCC-GW30) at the 28 days
and 180 days curing duration, respectively. The highly dense and ho­
mogenous paste matrix/ITZ can be observed in FA-SCC-GW30 mixture
(Fig. 7(c) and 8(c)). The smaller size of GW particles assists in the filling
of voids and ultimately leads to a compacted SCC matrix. The better
interlocking between the GW and paste matrix can be observed in FA-
SCC-GW30 mixture (Fig. 7(c) and 8(c)). The improved and compact
matrix was the reason for the better mechanical performance of the FA-
SCC-GW30 mixture. However, at higher GW replacement level, the extra
added water had negatively affected the mechanical performance of
concrete. Fig. 7(d) and Fig. 8(d) present the microscopic images of fly
ash based concrete mixture containing 60% GW (FA-SCC-GW60) at the
28 days and 180 days curing duration, respectively. As compared to
other mixtures for respective curing ages, relatively porous matrix and
higher voids/cracks were found in the FA-SCC-GW60 mixture. The
agglomeration of GW particles can also be seen in FA-SCC-GW60
mixture (Fig. 7(d)). The higher incorporation of GW resulted in the
poor gradation of concrete constituents and hence led to the porous
microstructure. Besides, the highly increased water to powder ratio, at
higher GW replacement level, developed significant voids within the
concrete matrix. The evolution of porous microstructure was the reason
for the lower mechanical performance of the FA-SCC-GW60 mixture.
3.2.2. Energy dispersive X-ray spectrometry (EDS)
The elemental compositions (obtained via EDS) are presented in
Table 3 for the selected SCC mixtures at 28 days and 180 days curing.
The lower calcium to silicon (Ca/Si) ratio normally indicates larger
development of CSH gel or vice versa [6]. At 28 days, the values of Ca/Si
ratio were found to be 0.92, 1.24, 1.14 and 1.3 for OPC-SCC-GW0, FA-
SCC-GW0, FA-SCC-GW30, FA-SCC-GW60 mixture, respectively. It can
be seen that fly ash blended mixtures (prepared with and without GW)
exhibited higher Ca/Si ratio than that of OPC-SCC-GW0 mixture. The
higher Ca/Si value indicated lower development of CSH gel in all the fly
blended mixtures causing the lower compressive strength. Despite the
lower formation of CSH gel, the FA-SCC-GW30 mixture exhibited su­
perior compressive strength. This was due to the better bonding of GW
with paste content (as observed in Fig. 7(c) and 8(c) via SEM analysis)
which compensated the loss of compressive strength on the substitute of
cement with fly ash. However, at higher GW replacement level (>30%),
extra added water resulted in the more porous microstructure in the SCC
matrix which ultimately caused the reduction of strength.
At 180 days, the values of Ca/Si ratio were found to be 1.08, 0.94,
0.82 and 1.12, respectively, for OPC-SCC-GW0, FA-SCC-GW0, FA-SCC-
GW30, FA-SCC-GW60 mixture. It can be seen that the values of Ca/Si
ratio in fly blended mixtures reduced with the progress of curing days,
which caused the higher formation of CSH gel as related to the latent
pozzolanic activity of fly ash. However, values of Ca/Si ratio in OPC-
SCC-GW0 mixture increased with the progress of curing days which
might be due to the continuous production of portlandite along with
CSH gel resulting from the cement hydration. The results of strength
characteristics also indicated that at later ages, the growth in strength
A. Jain et al. Construction and Building Materials 314 (2022) 125480

(a) (b)
Aggregate

ITZ Crack
ITZ
Void

Fly ash
Aggregate
Void
Void

(c) (d)
Fly ash Agglomeration
CSH of GW
GW
Crack
Crack
Crack

GW Fly ash
Fly ash GW Voids

Fig. 7. Microscopic images of SCC at 28 days curing: (a) OPC-SCC-GW0, (b) FA-SCC-GW0, (c) FA-SCC-GW30 and (d) FA-SCC-GW60.

was not substantial in OPC-SCC-GW0 mixture than the fly ash blended
mixtures. This might be due to the lower formation of CSH gel with time
in OPC-SCC-GW0 mixture.
Furthermore, fly ash blended mixtures (prepared with and without
GW) did not exhibit much variation in the values of Ca/Si ratio, which
indicated that the GW did not have a remarkable impact on the forma­
tion of hydration products. Besides, the aluminum (Al) composition was
also found to be in higher amount in fly ash blended SCC mixtures than
the OPC-SCC-GW0 mixture which was due to the presence of excessive
alumina content in fly ash. The traces amounts of other elements (such
as K, Fe, Na and Mg) were also perceived by EDS.
3.2.3. X-ray diffraction (XRD)
The results of XRD analyses, for both curing duration of 28 days and
180 days, are shown in Fig. 9(a-d) and 10(a-d), respectively. The
following mineral phases were detected: quartz (SiO2), calcium hy­
droxide or portlandite (Ca(OH)2), calcium silicate hydrate or CSH gel
(Ca6H2O13Si3), calcite (CaCO3), albite (NaAlSi3O8) and microcline
(KAlSi3O8), ettringite (Ca6Al2(SO4)3(OH)2⋅26H2O), calcium aluminate
silicate hydrate or CASH (Ca4Al8Si8O32⋅16H2O), dicalcium silicate or
belite (C2S). These phases are represented by alphabet numbers (A-I) in
the figures.
The intensity peaks of SiO2, at 28 days and 180 days of curing, were
observed to be at around 2 theta of 26.65, 20.85 and 50.14 for all the
mixtures. The presence of the quartz phase primarily was due to the sand
and GW particles.
The unhydrated cement phases (C2S) were observed, at curing
duration of 28 days, in concrete mixtures. However, the peaks of C2S
disappeared, at 180 days of curing, which might be due to the contin­
uous hydration activity with the progress of curing.

6
A. Jain et al. Construction and Building Materials 314 (2022) 125480

(a) CSH (b) Fly ash Aggregate

ITZ
Voids CSH
Aggregate Voids
Voids

Voids
Voids
Voids

Fly ash
CSH
Crack
CSH

(c) (d)
Voids
Aggregate

Fly ash
GW

Crack
CSH
ITZ
GW
Voids

CSH

Fig. 8. Microscopic images of SCC at 180 days curing: (a) OPC-SCC-GW0, (b) FA-SCC-GW0, (c) FA-SCC-GW30 and (d) FA-SCC-GW60.

Table 3
Elemental composition (%).
Elements (symbol) Curing days

28 days 180 days

OPC-SCC-GW0 FA-SCC-GW0 FA-SCC-GW30 FA-SCC-GW60 OPC-SCC-GW0 FA-SCC-GW0 FA-SCC-GW30 FA-SCC-GW60

Oxygen (O) 50.29 46.94 48.37 50.65 45.24 47.34 47.59 48.31
Calcium (Ca) 16.74 18.76 16.69 21.98 21.78 18.85 16.91 20.84
Silicon (Si) 18.18 15.08 14.67 15.98 20.20 19.99 20.58 18.62
Aluminium (Al) 3.03 6.05 5.94 5.58 2.08 5.47 4.36 4.56
Potassium (K) 3.12 2.90 1.77 1.04 1.86 2.65 1.59 2.00
Iron (Fe) 1.74 1.42 1.40 1.04 0.00 0.00 1.53 0.00
Magnesium (Mg) 1.59 1.32 1.35 0.48 1.18 1.18 1.15 1.46
Sodium (Na) 0.79 1.56 2.20 0.67 0.66 1.78 0.79 1.15
Carbon (C) 4.54 5.99 7.60 2.61 7.02 3.00 5.55 3.10
Ca/Si ratio 0.92 1.24 1.14 1.38 1.08 0.94 0.82 1.12

7
A. Jain et al.
Fig. 9. XRD patterns of SCC at 28 days curing: (a) OPC-SCC-GW0, (b) FA-SCC-GW0, (c) FA-SCC-GW30 and (d) FA-SCC-GW60.
The intensity peaks of Ca(OH)2, at 28 days of curing, for all the
mixtures were found at around 2 theta of 18.00, 34.10, 47.12 and 50.81.
Fly ash blended mixtures exhibited lower peaks of Ca(OH)2 than OPC-
SCC-GW0 mixture which might be because of the dilution of cement.
The replacement of cement with fly ash generally reduces the clinker
phases (i.e. C3S and C2S), resulting in the lower generation of Ca(OH)2.
The peaks of Ca(OH)2 significantly lowered or disappeared, especially in
fly ash blended mixtures, on the 180 days of curing, as shown in Fig. 10
(a-d). This might be due to the pozzolanic reaction of fly ash, where Ca
(OH)2 chemically reacted with siliceous or aluminous phases to form
additional hydration products [6,54].
The maximum intensity peaks of CSH, at 28 days of curing, were
observed at around 2 theta of 29.09 for all the mixtures. The formation
of CSH gel generally dominates the mechanical performance of concrete
matrix. From the study, it can be observed that fly ash blended mixtures
exhibited the lower intensity peaks of CSH gel than OPC-SCC-GW0
mixture, which might be due to the dilution of cement paste. Whereas,
the addition of GW did not result in any major changes in the formation
of CSH. Furthermore, at the early curing age, the FA-SCC-GW0 mixture
exhibited the lower intensity peaks of CSH gel than OPC-SCC-GW0
mixture, which indicated the low reactivity of fly ash. Nevertheless,
the higher formation of CSH gel peaks was observed, especially for fly
ash blended mixtures, with the progress of curing duration. From Fig. 10
(a-d), it can be perceived that fly ash blended mixtures (except FA-SCC-
GW60 mixture) exhibited the higher peaks of CSH gel than OPC-SCC-
8
Construction and Building Materials 314 (2022) 125480
GW0 mixture, which imparted the higher mechanical performance of
fly ash blended mixtures (prepared with and without GW) than OPC-
SCC-GW0 mixture at 180 days curing.
The mineral phase of ettringite was found at around 2 theta of 9.06
and 15.72. The peaks of ettringite were found to higher for fly ash
blended mixtures at 28 days of curing. This might be because of the
higher alumina content of fly ash [57]. The formation of ettringite
generally supports the densification of concrete matrix. However, at
later ages of curing, the peaks of ettringite disappeared which might be
due to the conversion of the ettringite phase into calcium monosulphate
phase [58]. It was also possible that hydration phases of fly ash, at later
curing ages, could not be easily detected by XRD which might be due to
their non-crystalline nature, as reported earlier by other researchers
[59].
The mineral phase of CASH was found in the form of gismondine at
around 2 theta of 18.05 and 33.15. The peaks of gismondine were found
to be significantly lower at 28 days curing. It was stated by Tang et al.,
[60] that due to the low crystallinity degree of gismondine at early
hydration age (i.e. at 28 days curing), it is generally difficult to detect
the gismondine phase by XRD technique. The peaks of gismondine were
found to be significantly higher for fly ash blended mixtures (prepared
with and without GW) than OPC-SCC-GW0 mixture, which might be
because of the presence of high aluminate phases in fly ash. It was stated
by Gupta and Vyas [17] that the presence of the mullite (aluminium
silicon oxide) phase in fly ash reacts with portlandite to form CASH or
A. Jain et al.
Fig. 10. XRD patterns of SCC at 180 days curing: (a) OPC-SCC-GW0, (b) FA-SCC-GW0, (c) FA-SCC-GW30 and (d) FA-SCC-GW60.
gismondine. Also, the formation of gismondine along with CSH gel
partially enhances the densification of cement paste [60].
The mineral phases of albite and microcline were also found in all the
mixtures. However, the fly ash blended SCC mixtures prepared with GW
(FA-SCC-GW30, FA-SCC-GW60) exhibited larger peaks of albite and
microcline than the control mixtures (OPC-SCC-GW0, FA-SCC-GW0)
because these mineral phases were the primary components of GW. It
has been reported that albite phases are generally helpful for the addi­
tional formation of CSH gel [61]. This additional formation of CSH gel in
fly ash blended SCC mixture, prepared with GW, might be responsible
for the higher mechanical performance of such mixtures. The intensity
peaks of calcite were found to be lower in all the mixtures which did not
cause any major impact on the mechanical performance of SCC matrix.
Overall, no remarkable modification was observed in the formation
of hydration products (Ca(OH)2, CSH, ettringite and CASH) on the
incorporation of GW in the concrete matrix. Therefore, the increase of
strength characteristics with an increase of GW content majorly was due
to the inert filler efficacy of GW. Furthermore, at 180 days of curing, the
presence of pozzolanic material (i.e. fly ash) provided a beneficial
outcome in the formation of sufficient hydration products (i.e. CSH gel
and gismondine). Thus, at 180 days of curing, the combined action of fly
ash and GW lead to the better mechanical performance of fly ash
blended concrete mixtures containing GW than OPC-SCC-GW0 mixture.
9
Construction and Building Materials 314 (2022) 125480
3.2.4. Fourier transform infrared spectroscopy (FTIR)
FTIR indicates the presence of molecular groups, in the concrete
matrix, in terms of absorbance bands at distinct wavelengths. The ex­
istence of various molecular groups in the developed SCC matrix for 28
days and 180 days curing are shown in Fig. 11(a-d) and 12(a-d),
respectively. Absorbance bands around the wave number of 450–650
cm− 1 and 778 cm− 1 can be ascribed to quartz (SiO2) [62,63]. The
presence of quartz bands, in the present study, might be due to sand and
GW particles. The absorbance bands around the wave number of
2850–2925 cm− 1 can be ascribed to methyl and methylene groups. The
existence of methyl and methylene groups in demoulding oil were
responsible for this band in the present study [64]. The absorbance
bands around the wave number of 882 cm− 1 and 1422 cm− 1 can be
ascribed to carbonates (CaCO3) which occurred due to the portlandite
carbonation [56]. Whereas, the bands around the wave number of 1646
cm− 1 and 3444 cm− 1 can be ascribed to water molecules groups [56].
Fig. 12.
The absorbance bands around the wave number of 3646 cm− 1 can be
ascribed to O–H bond or portlandite (Ca(OH)2) [65–67]. At 28 days
curing, the bands of portlandite were observed to be 3650, 3634, 3630
and 3641 cm− 1 for OPC-SCC-GW0, FA-SCC-GW0, FA-SCC-GW30, FA-
SCC-GW60 mixtures, respectively. At 180 days of curing, the bands of
portlandite were observed to be 3656, 3623, 3611 and 3633 cm− 1 for
OPC-SCC-GW0, FA-SCC-GW0, FA-SCC-GW30, FA-SCC-GW60 mixtures,
A. Jain et al.
Fig. 11. FTIR patterns of SCC at 28 days curing: (a) OPC-SCC-GW0, (b) FA-SCC-GW0, (c) FA-SCC-GW30 and (d) FA-SCC-GW60.
respectively. It can be noticed that fly ash blended mixtures exhibited
lower wave number than the OPC-SCC-GW0 mixture. The shifting of
bands to lower wave number indicates the dwindling of bond length or
consumption of portlandite [29,66]. However, amongst the fly ash
blended mixtures (prepared with and without GW), relatively lower
shifting of wave numbers was observed for portlandite bands. This
indicated that no significant changes occurred on the inclusion of GW in
fly ash blended control mixture. Furthermore, with the progress of
curing, the bands of portlandite for fly ash blended mixtures (prepared
with and without GW) shifted to the lower side. This shifting of bands to
lower side indicated the consumption of portlandite, which might be
because of the adequate pozzolanic reaction of fly ash.
The absorbance bands around the wave number of 996 cm− 1 and
1005 cm− 1 can be ascribed to Si-O bond or CSH. The bands of CSH, at 28
days curing, were observed to be 1002, 994, 999 and 991 cm− 1 for OPC-
SCC-GW0, FA-SCC-GW0, FA-SCC-GW30, FA-SCC-GW60 mixtures,
respectively. The bands of CSH, at 180 days of curing, observed were
1012, 1021, 1029 and 1008 cm− 1 for OPC-SCC-GW0, FA-SCC-GW0, FA-
SCC-GW30, FA-SCC-GW60 mixtures, respectively. It can be noticed that
the wave number of CSH for fly ash blended control mixture (FA-SCC-
GW0) was found to be slightly lower and higher, than OPC-SCC-GW0
mixture, at 28 days and 180 days of curing, respectively. This
10
Construction and Building Materials 314 (2022) 125480
observation indicated the decrease and increase in Si-O bond length for
FA-SCC-GW0 mixture than OPC-SCC-GW0 mixture, at 28 days and 180
days curing, respectively. The decrease in Si-O bond length causes the
lower mechanical performance and vice versa. Furthermore, relatively
less shifting in the wave number of CSH gel was observed for the fly ash
blended mixtures (prepared with and without GW). It can also be
observed that the wave number of Si-O bond appreciably shifted to the
higher side with the progress of curing, which indicated the increase in
polymerization degree of CSH gel.
Finally, the observation of FTIR analysis concluded that the GW
particles have an insignificant impact on the formation of hydration
products. The results of XRD and EDX analyses also support this claim.
4. Conclusion
This study investigates the effect of GW on the mechanical and
microstructure characteristics of fly ash blended SCC. The following
inferences can be drawn based on investigation:
• Mechanical characteristics testing showed that for all the curing days
(7, 28, 90 and 180 days), fly ash blended SCC mixtures (made with
GW) showed higher compressive strength and tensile strength on the
A. Jain et al.
Fig. 12. FTIR patterns of SCC at 180 days curing: (a) OPC-SCC-GW0, (b) FA-SCC-GW0, (c) FA-SCC-GW30 and (d) FA-SCC-GW60.
incorporation of up to 40% and 50% GW than fly ash blended control
mix (made without GW), respectively. Whereas, fly ash blended
mixtures containing up to 50% GW showed better mechanical per­
formance than OPC based control mixture for 180 days curing time.
The higher mechanical performance of fly ash blended SCC mixtures
(made with GW) than OPC based control mixture was because of the
filler effect of GW as well as pozzolanic activity of fly ash.
• SEM analysis revealed that incorporation of fly ash and GW improves
the densification of SCC matrix.
• EDS analysis indicated that the incorporation of GW does not
significantly change the Ca/Si ratio in the SCC matrix. Furthermore,
the values of Ca/Si ratio in fly blended mixtures reduced with the
progress of curing days, which caused the higher formation of CSH
gel.
• XRD and FTIR analysis indicated that there was no remarkable
modification observed in the hydration product of Ca(OH)2, CSH gel,
ettringite and CASH on the incorporation of GW in SCC matrix.
• The microstructure analyses showed the morphological and chemi­
cal changes in the developed SCC matrix. The results of EDS, XRD
11
Construction and Building Materials 314 (2022) 125480
and FTIR analysis indicated that GW did not have any remarkable
impact on the formation of hydration products. However, the SEM
analyses indicated that GW can make better bonding with paste
content, which caused the improvement in the mechanical perfor­
mance of fly ash blended concrete mixture containing GW.
• Based on the mechanical and microstructural characteristics, the GW
up to 40% as a replacement of fine aggregate can be utilized in the
production of sustainable SCC.
CRediT authorship contribution statement
Abhishek Jain: Conceptualization, Methodology, Writing – original
draft, Investigation, Data curation, Visualization. Sandeep Chaudhary:
Supervision, Writing – review & editing, Project administration. Rajesh
Gupta: Supervision, Writing – review & editing, Project administration.
A. Jain et al.
Declaration of Competing Interest
The authors declare that they have no known competing financial
interests or personal relationships that could have appeared to influence
the work reported in this paper.
Acknowledgments
The authors gratefully acknowledge MNIT Jaipur, IIT Indore and IIT
Kanpur for the microstructure characterization facilities.
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