Construction and Building Materials 277 (2021) 122323

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Construction and Building Materials

journal homepage: www.elsevier.com/locate/conbuildmat

Micro-characterisation of alkali activated paste with fly ash-GGBS-

metakaolin binder system with ambient setting characteristics
Muralidhar Kamath, Shreelaxmi Prashant, Mithesh Kumar
Department of Civil Engineering, MIT, MAHE, Manipal, Karnataka, Udupi District 576104, India

h i g h l i g h t s g r a p h i c a l a b s t r a c t

 FA-GGBS-MKwere activated using an

alkaline solution to develop a binder
system.
 FA- GGBS -MK ternary powders have
produced highly workable paste.
 FA- GGBS -MK binders have
developed high strength paste when
cured at ambient conditions.
 FA- GGBS -MK pastes produce CSH,
CASH-NASH as the products of the
reactions
 FA- GGBS -MK pastes compositions
have been studied using FESEM, EDS,
XRD, and FTIR

a r t i c l e i n f o a b s t r a c t

Article history: The study reports properties of a stable and high strength ternary binder matrix using Fly Ash (FA),
Received 17 October 2020 Ground Granulated Blast Furnace Slag (GGBS), and Metakaolin (MK). The bulk of the binder system is
Received in revised form 2 January 2021 composed of Fly Ash and Ground Granulated Blast Furnace Slag (GGBS), while Metakaolin is added in
Accepted 5 January 2021
three levels of 20%, 10%, 5% by weight, as suggested by the design of experiments. Alkali solution consist-
ing of sodium hydroxide flakes and sodium silicate solution was used as the alkali activator. Fresh prop-
erties of all the Alkali Activated binder Pastes were studied to understand the Setting time and Mini-
Keywords:
Slump. Mechanical properties of the hardened fly ash based ternary binder mortar were tested for com-
Fly Ash (FA)
Ground Granulated Blast Furnace Slag
pressive strength and ultrasonic pulse velocity (UPV) after 3, 7,28, and 56 days of curing. X-Ray
(GGBS) Diffraction (XRD), Field-Emission-Scanning-Electron-Microscope (FESEM), Energy-Dispersive-
Metakaolin (MK) Spectroscopy (EDS), and Fourier transform infrared spectroscopy (FTIR) were conducted in order to study
Fly ash based ternary paste the microstructural properties fly ash based ternary paste cured for 7 days. The compressive strength of
hardened fly ash based ternary samples varied between 57.14 and 102.04 MPa. Ternary mixtures were
observed to have a homogeneous and denser microstructure, with the development of various gels like
CSH, CASH, NASH, and (N, C)-ASH.
Ó 2021 Elsevier Ltd. All rights reserved.

1. Introduction

Cement is a popularly used binder system for concrete and

E-mail addresses: muralidhar.kamath@learner.manipal.edu (M. Kamath), shree-
laxmi.p@manipal.edu (S. Prashant), mithesh.kumar@learner.manipal.edu (M. Ku-
related applications. With rising environmental concerns, there
mar) has been a need for an alternative binder system that can consume

https://doi.org/10.1016/j.conbuildmat.2021.122323
0950-0618/Ó 2021 Elsevier Ltd. All rights reserved.
M. Kamath, S. Prashant and M. Kumar
a lot of industrial waste or serve as an energy-efficient system.
Alkali Activated Binders are one such range of binder systems that
possess the properties close to the conventional cement-based bin-
der system. Fly ash is an industrial by-product of the thermal
power-plant and GGBS is a leftover of the steel industry, large scale
use of these in the concrete industry can help design a low energy,
green binder system. The total amount of fly ash available in India
is 168 million tonnes and the amount of fly ash unused is 48 mil-
lion tonnes. The Central Electricity Authority (CEA) has recently
announced that the fly ash used in the cement industry is 26 per-
cent and the total unused fly ash is 22 percent[1]. The production
of steel in India consists of 24 million tonnes of blast furnace slag
and 12 million tonnes of steel slag annually. By 2030, BF slag pro-
duction is projected to hit about 45–50 million tonnes and & BOF
slag about 15–20 million tonnes per year. Of this, just 25% is reused
in India, compared to 70–100% in other countries and that too for
highway project[2]. Alkali activated binder is such type system
which can utilise the ample amount of waste material like fly
ash and Slag.
Nevertheless, there are two main problems related with the
production of the alkali activated material. These are the issues
in handling of high concentrations of corrosive and viscous alkaline
liquid and the need for heat curing to boost the activation and
polymerisation. Alkali-activated binder materials are normally
subjected to heat treatment at temperatures above 50 °C for sev-
eral hours [3]. This issue needs to be addressed for making it a pop-
ular building material.
Micro-Characterisation of the alkali-activated system is essen-
tial to understand the physical, chemical, and thermal characteris-
tics [4–6]. Alkali activated binders have, in recent times, gained
the attention of researchers worldwide due to its low embodied
energy compared to Ordinary Portland Cement (OPC)[7]. Energy-
efficient and sustainable binders, which can produce green con-
crete, is the need of the hour. Generally, Alkali Activated Binders
essentially consists of an industrial leftover and construction
industry waste majorly rich in SiO2-Al2O3 (Silica-Alumina) and
then activated with an alkaline solution [8,9]. The chemical activa-
tor usually consists of sodium hydroxide (SH), sodium silicate (SS)
or a blend of the two. The proportion varies with the strength
requirement and composition of the base material. Fly-ash (FA)
and blast furnace slag (GGBS) are the typical precursor of indus-
trial waste and used extensively because of their easy availability.
Similarly, metakaolin (MK) naturally available for pozzolanic
material formed by kaolinite clay calcination at temperatures
between 600 and 800° C. Various combinations of FA-slag-MK
mixes are studied for their applicability as a binder system is stud-
ied and presented in this paper.
Alkali Activated Binder (CaO-SiO2-Al2O3) systems can be cate-
gorized into three types of the gel system, which can vary with
the calcium content of the binder. The first one is the typical pre-
decessor using GGBS, which contains high calcium unit (Na,
K)2O-CaO-Al2O3-SiO2-H2O), a significantly produces gel-like cal-
cium alumina silicate hydrate (C-A-S-H) as a reaction product.
The second is with Class F fly-ash and meta-kaolin base particles
for the low calcium unit ((Na, K)2O Al2O3 SiO2 H2O) and N–A–S–H
is the specific reaction product. The third one is a hybrid alkaline
unit (Na, K)2O-CaO-Al2O3-SiO2-H2O) formed of the previous two
has also been defined recently. A chemical compound is a new
form of binder known as a mixed or alkali-activated binder result-
ing from alkaline activation of materials with CaO, SiO2, and Al2O3
content in various proportions [10–15]. The precipitating reaction
compound in this hybrid alkaline cement is a very multifaceted
binder system, consisting of a mixture of alkaline gels like
calcium-aluminosilicate-hydrate (C-A-S-H) (which absorbs Na +
into its structure) and turn into (N, C)-A-S-H (high Ca2+ sodium-
aluminosilicate-hydrate) [16]
2
Construction and Building Materials 277 (2021) 122323
Fly ash-based alkali-activated concrete with increase poz-
zolanic material which content CaO, SiO2, and Al2O3 replacement
activated with alkaline liquid reveals optimal combinations with
respect to slump, performance criteria, consistency, and strength
properties. Micro-graphs help to confirm the increased compact-
ness of the structure of the concrete through the denser matrix
and fewer microcracks, voids, firm achieved higher strength.
Increased sodium hydroxide molarity improves the mechanical
strength thus decreases workability of geopolymer concrete [17–
25]. With the alkaline solution, the external layer of the aggregates
reacted while the internal structure remained relatively stable over
the 28 days , resulting in the disappearance of the inter-
transitional state in full volume fly ash mortars and decreased flow
compared to the cement mortars [26,27].
Slag based alkali-activated concrete has exhibited improved
properties such as high mechanical strength, flowability, water
absorption, and denser microstructure. The increased compressive
strengths are likely due to the higher binder content, which leads
to more C-S-H and C-A - S-H gels being formed. It is evident from
the microstructural features that significantly less inter transi-
tional zone shaped and limited pores made the matrix much den-
ser in these mixtures, resulting in a much lower water absorption
[28–31].
Use of SS to SH ratios, the SS / SH ratio of 2.5 resulted in superior
compressive strength in alkali-activated concrete without nano-
SiO2[32]. The SEM micrograph has also confirmed these observa-
tions in which, compared to another replacement percentage,
alkali-activated binder paste prepared with 5 percent nano-SiO2
showed a homogeneous and denser microstructure with fewer
unreacted particles. Because of improved polymerization and par-
ticle size packing, the alkali-activated binder paste microstructure
made with different doses of nano-SiO2 showed enrichment in the
reaction materials.[33–36]. The presence of GGBS improves the
strength characteristics of the FA-based geopolymer because of
its high reactivity. The geopolymer with high GGBS volume sets
quickly and has high early compressive strength. Blended geopoly-
mer mortars with relatively low GGBS volume (e.g., FA / GGBS ratio
of 4) may achieve similar OPC-like properties (e.g., fluidity, setting
time, strength growth, volume stability, and chloride permeability)
[37,38].
Metakaolin based geopolymers concrete with the variation of
industrial sludge have studied the microstructure and compressive
strength than compared with fly ash geopolymers concrete [39].
The XRD study reveals that the formed reaction products are amor-
phous in nature. The activation of calcined industrial sludge by
sodium silicate solution leads to the formation of a type alumi-
nosilicate rich in SiO2 and Al2O3, similar to a geopolymer based
on metakaolin. The major reaction product is sodium alumina sil-
icate hydrate (NASH). The compressive strength behaviour of
industrial sludge-based calcined geopolymer similar to the
geopolymer based on metakaolin [40,41]. The metakaolin replace-
ment with slag have showed improved workability, setting time,
and good mechanical properties at ambient temperature compared
to cement mortar[42].
Metakaolin comprises a significant percentage of alumina and
silica, but little or no research has been conducted to investigate
the adequacy of the ternary mixture in this framework. It is, there-
fore, necessary to understand the behaviour of FA-GGBS-MK based
ternary binders when cured at ambient temperature. The particle
size of FA, GGBS, and MK leads to particle packing, which improves
reactivity, polymerization, and properties of the paste. Thus, this
paper aimed to develop high-strength alkali-activated ternary
paste with FA-GGBS-MK at ambient temperature. To make the
stable and high-strength fly ash based ternary paste, FA-GGBS-
MK as starting based raw materials have been activated using alka-
line liquid solutions which contains Na2SiO3 and NaOH.
M. Kamath, S. Prashant and M. Kumar Construction and Building Materials 277 (2021) 122323

2. Materials and experiment design

The properties of FA-slag-MK based alkali-activated binder sys-

tem is planned to be studied experimentally 9 combinations of fly
ash, slag, and metakaolin have been studied and compared with
OPC. Properties of base materials and their combinations, along
with experimental methodology, are presented herewith.

2.1. Materials

2.1.1. Starting base raw material

GGBS and MK have been procured from Astraa Chemical Lim-
ited Chennai, India, the low calcium fly ash was collected from a
thermal power station in Raichur, India. The grain size analysis of
the starting-base raw materials has been determined by an inte-
grated liquid and dry dispersion system using a CILAS 1064, rang-
ing from 0.04 mm to 500 mm/100 classes. The particle size Fig. 2. Ternary Diagram of Starting Base Raw Materials.
distribution of FA, GGBS, MK, and OPC is presented in Fig. 1, while
the physical and chemical properties of FA, GGBS, MK, and OPC in
vator solution, NaOH Flakes with (97 percent purity) of
Table 2. The FA, GGBS, MK, and OPC mean grain (particle) size is
commercial-grade SH and SS solution is used in the formulation.
found to be 12 lm, 16.04 lm,5.22 lm, and 16.77 lm, respectively.
Chemical composition of SS solution is 14.7 percent Na2O + 32.8
The FA, GGBS, MK, and OPC specific surface area is 4.54 m2/ g, 5 m2/
SiO2 + 52.5 percent H2O by weight while its density is 1570 kg /
g, 19–20 m2/g, and 3.3 m2/g, respectively, while the FA, GGBS, MK,
m3. The alkaline formulations are prepared using the potable water
and OPC specific densities are 2.24, 2.67, 2.6, and 3.15. The compo-
with a solution to binder (S/B) ratio of 0.35. The water present in
sition of oxides such as silica oxides, alumina oxides, and iron oxi-
the SS is also taken into account while preparing the alkaline solu-
des in the FA, GGBS, and MK fulfill the pozzolanic activity
tion. The prepared chemical (alkaline) solution is allowed to cool
requirements as per clause of the ASTM C618 [43]. In Fig. 2, the
and stabilize at least for 24 h or until mixing as the case may be,
predecessors are plotted as a ternary illustration of the CaO-SiO2-
to reduce the heat produced, and prevent rapid setting.
Al2O3 connection. The chemical properties of MK are closer to FA
as both have low calcium oxide aa against GBBS, which has high
calcium oxide; hence it acts as a hydraulic binder. 2.2. Alkali activated ternary paste
The mineralogical structure is shown by X-ray diffraction (XRD)
of the base raw materials shown in Fig. 4. SiO2 (Quartz) is the pri- In this study, 9 paste have been prepared using the combination
mary crystalline phase in particles of MK and FA that showed of FA, GGBS, and MK in varying proportions, as shown in Table 3
almost the same crystalline phase with little variation, since GGBS and compared with OPC paste. The design of experiments was
was found to be in an amorphous phase. The Field-Emission-Scan done and three-levels of MK (%) variation were studied, i.e., 20%,
ning-Electron-Microscope (FESEM) of starting powders (Fig. 3) 10%, 5%. The solution-to-binder ratio of 0.35 is used for all the
reveals that even though the structure of MK was irregularly paste formulations. The samples cast in cubic moulds of size
formed, it appears to be reasonably smooth, angular porous sur- 40  40  40 mm were used for micros-characterization. The sam-
face, and flaky. Besides that, the particles of FA were rela- ples were de-molded after 24 h, and air cured for up to 7 days
tively smooth and spherical, and most of the particles of OPC and before testing.
GGBS were irregular and angular in shape.
2.3. Alkali activated ternary mortar
2.1.2. Alkaline solution
An alkaline solution of 12 M and SH to SS ratio 2.5 is used to Alkali Activated Ternary Mortar of 9 mixes have been prepared
activate the base aluminosilicate materials. For preparing the acti- using the combination of FA, GGBS, and MK in varying proportion
as shown in Table 3 and is compared with OPC mortar. The ratio of
binder to Sand is kept constant at 1:3. According to IS 383–2016
[44] standard sand is used to prepare mortar and specific gravity
of sand is 2.65. The mortar samples prepared in cubic molds (70.
6  70.6  70.6 mm).

2.4. Test methods

Setting time is one of the vital characteristics of binder materi-

als. As per provision prescribed in ASTM C191 [45], the initial and
final setting time test of alkali activated paste with Vicat apparatus
was conducted. Fresh properties of the fly ash based ternary paste
were tested as per provision prescribed in ASTM C1437 [46]
slump-flow test. A steel tape was used to calculate the average hor-
izontal free flow of the paste in a perpendicular direction using -
slump flow test. The material characteristics of the hardened fly
ash based ternary binder mortar were tested for compressive
strength in accordance with ASTM C109[47] at 3, 7, 28 and 56 days
Fig. 1. Particle Size Distribution of Starting Base Raw Materials. of curing. In addition, the ultrasonic pulse velocity (UPV) test was
3
M. Kamath, S. Prashant and M. Kumar
Fig. 3. FE-SEM images of starting materials.
Fig. 4. XRD of starting materials.
conducted at 3, 7, 28 and 56 days of curing according to ASTM
C597 guidelines [48]. The Field-Emission-Scanning-Electron-Micro
scope (FESEM) test was conducted on a Carl Zeiss FESEM, Oxford
Instrument. Additionally, the Energy-Dispersive-Spectroscopy (E.
D.S.) was performed to investigate and measure chemical elements
at 7 days for the final fly ash based ternary paste. Samples was
ground for X-Ray Diffraction (XRD) experiments using grinder
and the residual powder obtained was sieved through a 45-mm
sieve. XRD investigation was used to examine the spectroscopic
phases of the 7-day cured pastes using a Rigaku Mini-flex 600
4
Construction and Building Materials 277 (2021) 122323
(5th gene) with a broad-angle measurement of (5-130°) 2 h value.
FTIR tests were carried out on all mixtures cured for 7 days to eval-
uate the various chemical compounds present in the hardened fly
ash based ternary paste samples using JASCO FT / IR-6300 with a
wavelength range of 400 to 4000 cm. The summary of experimen-
tal tests conducted is presented in Table 1.
3. Result and discussion
3.1. Flow properties of ternary paste FA-Slag-MK
3.1.1. Influence of Metakaolin on setting time of ternary paste FA-Slag-
MK
Initial and final setting times of 9 combinations of alkali acti-
vated paste tested is plotted in Fig. 5. For comparison, results of
similar study conducted on OPC is also presented. The initial and
final setting time varies from 140 to 280 min and from 180 to
315 min. The initial and final OPC paste setting time is found to
be 95 min and 320 min. From the Fig. 5, it is seen that as the per-
centage of metakaolin decrease initial setting time reduces. The
outcomes of setting time depend strongly on metakaolin inclusion
to the alkali activated paste. Initial and Final setting time with 20%
metakaolin is observed to be highest compared to samples con-
tains 10% and 5% metakaolin.
Saha and Rajasekaran (2017) [49] ,have studied setting time of
FA-GGBS paste with variation of GGBS found that initial setting
time reduces from 420 480 min to 25–130 min and final setting
time from 1425 1600 min to 90–355 min. Guohao Fang et al.
M. Kamath, S. Prashant and M. Kumar Construction and Building Materials 277 (2021) 122323

Table 1
Summary of experimental tests conducted.

Sr.no. Tests Specimen Standards/Instrument

1 Setting time a. Ternary Pastes ASTM C191[45]
b. OPC Paste
2 Mini Slump Flow a. Ternary Pastes ASTM C1437[46]
b. OPC paste
3 Compressive strength a. Ternary Paste Mortar ASTM C109[47]
b. OPC Paste Mortar
4 Ultra-Sonic Pulse velocity a. Ternary Mortar ASTM C597[48]
b. OPC Mortar
5 Field-Emission-Scanning-Electron-Microscope a. Ternary Pastes Carl Zeiss FESEM, Oxford Instrument
6 Energy-Dispersive-Spectroscopy a. Ternary Pastes Carl Zeiss FESEM, Oxford Instrument
7 X-Ray Diffraction a. Fly Ash, GGBS and Metakaolin Rigaku Mini-flex
b. Ternary Pastes
8 Fourier transform infrared spectroscopy a. Ternary Pastes JASCO FT / IR-6300

Table 2
Physical and Chemical properties of Starting Base Raw Materials.

Material Fly Ash GGBS Meta-Kaolin OPC

Physical Properties Specific surface area(m2/g) 4.54 5 19–20 3.3
Specific Gravity (g/cc) 2.24 2.67 2.6 3.15
Particle Size(mm) d10 2.17 2.33 0.71 3.70
d50 8.72 13.37 3.75 14.83
d90 27.99 33.36 11.37 32.20
Chemical Properties (wt.%) SiO2 54.11 40 52 20.21
Al2O3 26.51 4.1 46 9.08
Fe2O3 6.4 2 0.6 3.64
Ca O 4.7 42 0.09 59.67
Mg O 1.04 6.2 0.03 2.02
SO3 1.29 0.1 – 2.41
Na2O 2.22 – 0.1 –
K2O 0.87 – 0.03 –
TiO2 – – 0.65 0.45
LOI 2.85 0.25 – 1.45

Table 3
Mixture Proportion of Composite Paste.

Mix ID Designation FA (%) GGBS (%) MK (%) Alkali(M) SH/SS S/B T(°C)
1 F50G30M20 50 30 20 12 2.5 0.35 Ambient
2 F40G40M20 40 40 20 12 2.5 0.35 Ambient
3 F30G50M20 30 50 20 12 2.5 0.35 Ambient
4 F50G40M10 50 40 10 12 2.5 0.35 Ambient
5 F40G50M10 40 50 10 12 2.5 0.35 Ambient
6 F30G60M10 30 60 10 12 2.5 0.35 Ambient
7 F45G50M5 45 50 5 12 2.5 0.35 Ambient
8 F50G45M5 50 45 5 12 2.5 0.35 Ambient
9 F40G55M5 40 55 5 12 2.5 0.35 Ambient
10 OPC (100%) – – – – – 0.35 Moist

*F-Fly Ash G-GGBS M Metakaolin

(2018) [50], noted decreases in the initial setting time of pastes
from 374 min to 126 min and decreases in the final setting from
499 min to 139 min when the slag content with fly ash varies from
10% to 30%. Fig. 5 shows the results of setting time conducted on
the pastes tested. As compared to FA-Slag binder system, the tern-
ary binder system produced with addition of MK, the Si/Al ratio
increase. The ternary system also contains Ca+2 ions, on activation
with alkaline solution CASH and NASH are produced. These pro-
duct of alkaline activation influence the setting times[51–53].
Slag introduces calcium into the system, which in turn increase
the heat developed during the activation and polymerisation. This
boosts the processes thereby reducing the difference between ini-
tial and final setting time. The role GGBS plays in the system is that
of an accelerator. Hence the need for heat curing is eliminated,
making it set at ambient condition [54,55].
3.1.2. Influence of Metakaolin on flow of ternary paste FA-Slag-MK
The slump flow values of the 9 paste combinations were found
to ranging from 135 to 170 mm is compared to OPC the slump
value of which is 190 mm as shown in Fig. 6. The slump spread
diameter values are observed after 10 min. The workability inves-
tigations revealed that among the paste combination tested,
F50G45M5 developed highly workable fly ash based ternary paste,
as the results of all slump flow tests were greater than 90 mm [21].
The fluidity of alkali activated pastes have sustained up to 35–
40 min in all the mixes. Xiaodi Dai et.al. (2020) [56] and A Bayat
et.al. (2018) [57] have reported similar outcomes with respect to
slump time.
The high surface area of MK and its irregular form as appears in
Fig. 3, could be the reason for stiffer mix and reduced slump value
made the F50G30M20 paste stiffer than its corresponding increase

5
M. Kamath, S. Prashant and M. Kumar
Fig. 5. Initial and Final Setting time of all paste.
Fig. 6. Slump Flow of paste.
in the binder system. With a rise in GGBS content and a fall in FA
content, in all categories, flowability trended downward. Theoret-
ically, this is due to FA-GGBS-MK’s physical and chemical proper-
ties. The proportion of small and most of irregular particles in the
ternary mixtures is increasing and the resulting high specific sur-
face area will adversely affect the workability of the ternary paste
[58,59].
In addition, GGBS content produces higher quantity of amor-
phous phase in the mixtures, which can also rise the alkaline acti-
vation reaction, thereby rapidly consumes the mixing water due to
higher rate of reaction, finally resulting into lower workability. The
rise in the proportion of FA increased the amount of smooth and
round particles in the ternary mixtures, which helps to minimise
the demand for water and surface resistance, consequently
improve the flowability of the mixtures. [60].
3.2. Hardened properties of ternary paste mortar FA-Slag-MK
3.2.1. Influence of Metakaolin on compressive strength of ternary paste
mortar FA-Slag-MK
Mortar compressive strength of the fly ash based ternary binder
are shown in Fig. 7 for specimen subjected to ambient curing for 3,
7, 28, and 56 days. Compressive strengths varied between 57.14
and 102.04 MPa at ambient temperatures after 56 days of curing.
Amongst the mixes tested the mixes containing 20 percent MK
6
Construction and Building Materials 277 (2021) 122323
Fig. 7. Compressive Strength of mortar at an ambient temperature.
have been found to have higher compressive strength.
F30G50M20 has the highest compressive strength of 102 MPa after
56 days of curing, amongst the tested samples while F45G50M5
showed the lowest strength value of 59 MPa. MK median particle
size (d50) was found to be 2.32, 3.56 and 3.95 times finer than
FA, GGBS and OPC respectively. Finer grain size enhances rate of
alkali activation, hence the mechanism of gel formation also
improve, resulting into improved mechanical properties. [61].
Table 2 reveals that MK has approximately 98% combined with
SiO2 and Al2O3. As described above, higher concentrations of SiO2
and Al2O3 in MK increase the alkaline activation reaction, resulting
in the formation of C-S - H, C-A - S-H and N-A - S-H gels, in com-
parably higher amounts enhancing the density as well as mechan-
ical properties.
MK has greater surface area and complexity in reaction prod-
ucts, as demonstrated by the XRD and XRF tests shown in Table 2
and Fig. 3, respectively. Indicating the higher presence calcium oxi-
des (CaO) in the GGBS, during the alkali-activation cycle, a signifi-
cant amount of Ca2+ ions has leached into the network, which was
already rich in Silica (Si4+) and Alumina (Al3+) molecules. C-S-H
(Calcium-Silicate-Hydrate) and C-A-S-H (Calcium-Aluminate-Sili
cate-Hydrate) gels are subsequently shaped. Increased GGBS bin-
der has resulted in a denser formation of gel that significantly
improves the compressive strength. Furthermore, as measured in
the EDS analysis, the rise in GGBS powder reduced the Si / Al ratio
in the alkali-activated ternary mixture, which will be discussed in
section 3.3.3. An increase in compressive strength is normally asso-
ciated with higher Si / Al ratios [16,62]. Si4+ and Al3+ ions have been
involved in the development of N-A-S-H (Sodium-Aluminate-Sili
cate-Hydrate gel), resulting in lower compressive strength than
C-S-H or C-A-S-H gels. [11,41].
A high strength fly ash-based ternary paste containing 20% MK
binders with GGBS and FA exhibits to the modified ternary binder
effect. A robust 3-D structure of C-S-H, C-A-S-H and N-A-S-H gels
that are formed as reaction products of FA-MK-GGBSS which
is mixed alkaline activation compounds[11].
3.2.2. Influence of Metakaolin on UPV of ternary paste mortar FA-Slag-
MK
UPV (Ultra-Sonic-Pulse-Velocity) is a non-destructive tool used
to determine concrete homogeneity and relative uniformity, detect
voids and cracks, and determine the crack repair effectiveness. UPV
is an indirect indicator of long-term properties and hardened
strength. UPV has been effective used to qualitatively estimate
the tests improvements in concrete materials, such as the growth
of compressive strength and intensity of cracking or deterioration.
The UPV test results for the samples of ternary binder mortar
and OPC mortar are tabulated in Table 4. The UPV values for tern-
M. Kamath, S. Prashant and M. Kumar Construction and Building Materials 277 (2021) 122323

Table 4 ing age and the rate of UPV increase dropped after 28 days of time.
Ultrasonic Pulse Velocity (UPV) values of mortar Samples. The compressive strength of the tested mortar samples also fol-
Mix UPV (m/s) lows the same trend. The fly ash based ternary binder mortar with
3-Days 7-Days 28-Days 56-Days MK-20% mixes are found to have higher UPV values than the MK
F50G30M20 2586 3625 4106 4575 10% and 5%. The trend corresponds to the formation of extra gels
F40G40M20 2886 3358 4180 4195 that eventually decreases the porosity of the hardened ternary
F30G50M20 2679 3565 4354 4640 paste, which is a critical requirement for the development of a den-
F50G40M10 2620 3113 3323 3733
F40G50M10 2641 3163 3337 4133
ser and compact morphology that eventually improved the
F30G60M10 2857 3187 3517 4261 strength and durability of fly ash based ternary binder mortar sam-
F45G50M5 2847 3011 3342 3589 ples[63,64]. Additionally, as FA content increased, the UPV of all
F50G45M5 2671 2991 3849 4259 ternary mortar samples decreased. Since calcium aluminosilicate
F40G55M5 2651 3126 3807 4076
material which is FA that is low in calcium and crystalline content,
OPC 2646 3088 3513 3895
additional gels produce in lower amounts. Similar trends were
demonstrated by the UPV and compressive strength results,
increasing with rise in GGBS volume and curing age. The increase
in MK has resulted increase in UPV and compressive strength val-
ues. This is due to this higher pozzolanic reactivity and additional
C-A-S-H, N-A - S-H gel formation. A linear regression model was
used to understand the connection between the fly ash based tern-
ary binder mortar compressive strength and UPV values, shown in
Fig. 8. The trends follow the equation y = 30.18x + 1647.39 with an
R2 value of 0.9587. This shows that the UPV and compressive
strength were strongly associated.

3.3. Influence of Metakaolin on microstructure of ternary paste FA-

Slag-MK

Fig. 8. Linear fit of UPV versus Compressive Strength.
ary binder mortar range from 3589 to 4640 m/s after 56 days of
curing and while that of OPC is 3895 m/s. The UPV values of all
fly ash based ternary binder mortar specimens improved with cur-
3.3.1. FE-SEM
Morphological and micro-level properties of the proposed 9
mixes were studied using Field-Emission-Gun--Scanning-Electron
optical microscope (FESEM) imaging. Fig. 9 (a to i) shows the
FESEM images with a scale of 1 lm and magnification of 10 K.X.
The FE-SEM micrographs suggest that the developed alkali acti-
vation phases contained an entirely different morphology from the
base raw materials. The Meta-kaolin alkaline activation with low

Fig. 9. FESEM images of all ternary paste at 7 days from a to i of Mix Id 1 to 9, *F-Fly Ash G-GGBS M Metakaolin c.MK5.

7
M. Kamath, S. Prashant and M. Kumar
calcium FA and GGBS resulted in the leaching of Si-O-Al materials,
producing a cross-linking polyhedral polymer that forms the stable
and three-dimensional structure as seen in the Sem micrographs
[65].
Figure 9b showed a compact and very well-dispersed morphol-
ogy surrounded by partly reacted powders of F50G30M20 mix. In
contrast, the samples with MK 10 %and 5% shown in Fig. 9. (b
and c) exhibited a less compact and dispersed morphology with
more unreacted raw starting binders. This morphology change
may be due to inconsistencies in the distribution of the FA, GGBS,
and MK in chemical properties, shapes, and particle size. The exis-
tence of various gels such as calcium-silicate-hydrate (CSH),
calcium-alumina-silicate-hydrate (CASH), and sodium-alumina-
silicate-hydrate (NASH) is observed in Fig. 11. Due to structural
changes taking place in the various compound, the morphology
variations are noticed. From Fig. 9.b as the amount of GGBS
Fig. 10. FESEM images of OPC Paste.
Fig. 11. XRD patterns of ternary paste at 7 days a. Metakaolin 20% b. Metakaolin 10% c. Metakaolin 5%
8
Construction and Building Materials 277 (2021) 122323
increase that disperse as Ca2+ ions, the volume change (Shrinkage)
is observed and CASH gel is alleviated which results into
microstructural cracks [66,67].Fig. 13
Fig. 9(d to f) shows the FE-SEM images of the mixes with 10%
MK. It shows a less dispersed and compact morphology compared
to the mixes with 20% MK . With decrease in MK, more cracks are
observed along with less dense structure. This micro-
structure variation may be attributed to varying amounts of Ca2+,
Na2+, Si, and Al produced with varying proportion of base ingredi-
ents. The synthesis of paste is controlled by the chemical reaction
of the surface on the ingredients. [68].
Since MK particle size is very fine, compact and dense structure
is seen to have been formed in the mixes. This is because of higher
rate of alkali reactivity of MK, compared to FA and GGBS. While
GGBS on the other hand is seen to have undergone partial activa-
tion and the products of reaction being precipitated on the sur-
M. Kamath, S. Prashant and M. Kumar
faces. Since the activation is partial, micro-cracks and pores are vis-
ible. Mixes that contain higher GGBS content have higher amounts
of CSH and (N,C)-ASH formed as the activation products [40,69,70].
The microscopy images show that with increased MK content,
the fly ash based ternary paste samples exhibit a denser
microstructure as is revealed on comparing the 5% and 20%, MK
blends. The MK with 5% FE-SEM micrographs refer to Fig. 9(g to
i) mixes showed a loose, fractured morphology. Also, large
amounts of unreacted or partially reacted grains found in the
F45G50M5, F55G45M5, and F40G55M5 mixes. In line with the
findings, of Ravikumar et al. [71] , the hydrated gel formed by
the higher reactivity of alkali-activated low calcium FA and lower
GGBS content was primarily the N-A -S-H.
Besides the hydrated N-A - S-H gel, as the volume of GGBS
increased in the FA-GGBS-MK binder process, the Ca2+ ions reached
the MK and to FA system and a Si-O-Al-O structure is formed pro-
ducing the C-A-S-H gel [61].
The mixes with 20% MK appear more compact, uniform and
homogeneous, with far fewer unreacted particles. Furthermore,
as shown by the XRD test in Fig. 11, The amorphous nature of GGBS
has helped to raise the reaction rate of alkaline activation of ele-
ments, which has increased the output of C-S - H and (N, C)-A-S-
H, thereby facilitating increases in compressive strength
[28,55,72]. The micrographs of OPC were compared with the alkali
activated ternary pastes studied. As illustrated in Fig. 10, the OPC
paste morphology appears to be less dense and compact compared
to the alkali activated pastes studied. However, the 28 days OPC
paste appears to be more dense than the pastes studied. c
3.3.2. XRD
X-ray diffraction was used to identify the mineralogical compo-
sitions of the paste samples after 7-day ambient curing. Fig. 11
shows the X-ray diffraction results of samples based on alkali-
activated FA-GGBS-MK. Microscopy images 11.a, 11.b, and 11.c
shows the results for samples containing MK at the range of 20%,
10%, and 5% respectively. Chemical reaction of the ternary pastes
leads to the new semi-crystalline peaks, resulting in the formation
of complex compounds. Some impurities from the FA-GGBS-MK
base raw materials are seen to have existed in their crystalline
peaks throughout the process of alkali activation.
As predicted SiO2 is the predominantly inorganic crystalline
mineral compound in all ternary alkaline-activated samples.
Quartz is present in all fly ash based ternary paste samples as an
unreacted particle, as noted at 21.64°, 27.12°, 39.74°, and 50.48°,
respectively (PDF: 00–005-0490). This result coincides with earlier
work by Yao et al. (2009)[73]. The mixes with 20% MK samples typ-
ically display higher crystalline SiO2 intensities than the those with
MK 10% and 5%. Since the MK is finer than FA and GGBS, ternary
mixes have experienced full or partial alkaline activation reaction
that is revealed on observing the reduced the peak intensity of
SiO2. Higher content of CaO promoted the phase separation within
the ternary mixes by decreasing unreacted particulates[74] The
SiO2 peak intensity decreased significantly as the amount of GGBS
increased in the ternary mixes. Since higher GGBS content resulted
in a higher alkaline activation which add significant gels to the
paste. The cross-linking mechanism enhances the ineffectiveness
of FA with MK which provides a more compact system that
enhances the compressive strength significantly [75]. The FESEM
micrographs of the fly ash based ternary paste combinations also
support the results.
MK reaction with low calcium FA and GGBS has been found to
have introduced semi-crystalline mineral peaks into the ternary
gel matrix. These compounds shaped as a result of ternary alkali
activation of FA-Slag-MK ternary paste combinations, consists
mainly of synchronized alkaline amorphous aluminosilicate gels.
These molecules are primarily the result of a combination of alkali
9
Construction and Building Materials 277 (2021) 122323
activation, which includes almost entirely of alkaline simultaneous
amorphous calcium and sodium aluminosilicate gels. Significant
peaks may be characterized as follows: (1) For all fly ash based
ternary paste specimens C-S-H gels (calcium-silicate-hydrate) ,
(Fig. 11) noticed at 29.96°,43.14° and 55.52° (PDF: 00–003-0649)
and (2) For all fly ash based ternary paste specimens, calcium
and sodium aluminosilicate gels (C-A-S-H and N-A- S-H) exist
simultaneously in the form of sodium-calcium-alumino-silicate
hydrate (N,C)-A-S-H) observed at 33.92°, 35.74° and 41.24° (PDF:
00–025-0777) .Previous researchers have reported similar out-
comes [76–78].
3.3.3. EDS
The results of the Energy-Dispersive-Spectroscopy (EDS) study
are shown in table 5 for the FA-GGBS-MK based ternary paste sam-
ples. The EDS study reveals that gel of alumino-silicate was primar-
ily the main component of the reaction. Besides Si and Al, a large
percentage of Ca was observed in all ternary specimens, and the
quantity of Ca as well as the Ca/Si ratio was also found to rise with
an increase in the GGBS binder content in the ternary paste blends.
Ternary fly ash-based paste samples contained a contributes to the
rise of Si and Al, with an increasing amount of GGBS binder. Earlier
research showed that higher compressive strength corresponds to
with lower Si / Al ratios [79,80]. There are higher Ca / Si ratios in
the ternary paste and lower Si / Al ratios that increase their
strength with an increase in proportion MK % in the mix. The ratio
of Ca/ (Si + Al) versus Na/ (Si + Al), Na/Si versus Na/Al and Ca/Si ver-
sus Ca/Al is plotted and shown in the Fig. 12. The results are found
to be comparable with previous studies [32,81–83]. In addition, the
formation of C-A-S-H and N-A- S-H has also been confirmed with
FTIR review, to be addressed lately in section 3.3.4. The Si / Al ratios
for the all ternary samples were in the range of 2.03 to 2.4, Na / Al
and Na / Si, in the range of 0.6 – 1.05 and 0.29 – 0.45. respectively
[11,84].Moreover the Ca/Si , Ca/ (Si + Al) and Na/ (Si + Al) are in the
range of 0.29 – 0.53 , 0.19–0.39 and 0.19–0.28 which is similar to
that reported in previous studies on the same lines [32,81–83].
Fig. 12 and Table 5 shows the comparison with similar studies.
OPC paste of 28 days cured samples has resulted Si / Al, Ca/Si,
Ca/ (Si + Al) and Ca/Al ratio are in range of 1.45 ,1.4673,0.868
and 2.1295. The Si / Al ratio of OPC paste is less than ternary paste
and Ca/Si, Ca/ (Si + Al), while Ca/Al ratio of OPC paste is greater
than the ternary paste.
3.3.4. FTIR
FTIR spectra is shown in the Fig. 14 of fly ash based ternary
paste specimens after 7 days of curing time. According to yaseri
et.al (2017) [85] the vibration bands at 3400 to 3600 cm 1 and
1657 cm 1 are corelated with the presence of hydroxyl OH– groups
and magnetized (structural) water, while intensity band of C-O
carbonates groups is attributable to 1400 to 1460 cm 1, vibrations
at 440 to 1050 cm-1 is corelated to T-O-T (T: tetrahedral Si or Al)
bonds occurring in tetrahedral or aluminum–silicon-oxygen
bridges. The FTIR result are in strong agreement with the observa-
tions of XRD and FESEM. The magnitude of the quartz peaks in all
the mixtures decreased considerably with increased MK content,
due to the higher reactivity and higher Si-Al components of MK,
multiple kinds of alkali-activated gels are formed.
The final location of the band (985 cm 1) was defined by Guo-
hao Fang et.al.(2020) [35] in Fly Ash-GGBS alkali-activated paste at
a lower wave number than in alkali activated fly ash paste
(1020 cm 1), suggesting that the existence of calcium (Ca2+) con-
tributes to the development of N,C-ASH. It is noted that the final
position of the bands in the ternary paste is higher (1170 cm 1).
A lower spectral band of 1056 cm 1 is associated with the
asymmetric stretching of the AlO4 group in Al-O-Si bonds within
the CASH gels. This means that the Al content of CASH gels is
M. Kamath, S. Prashant and M. Kumar Construction and Building Materials 277 (2021) 122323

Table 5
EDS analysis of binder paste samples.

Mix Elements (% by wt.) and their ratio

Si Al Ca Na Si + Al Si/Al Ca/ (Si + Al) Na/ (Si + Al) Ca/Si Na/Al Na/Si Ca/Al
F50G30M20 18.96 9.34 5.62 7.2 28.3 2.03 0.1986 0.2544 0.2964 0.7709 0.3797 0.6017
F40G40M20 14.91 7.17 3.9 4.37 22.08 2.0795 0.1766 0.1979 0.2616 0.6095 0.2931 0.5439
F30G50M20 17.3 8.41 7.39 7.45 25.71 2.0571 0.2874 0.2898 0.4272 0.8859 0.4306 0.8787
F50G40M10 20.24 9.38 6.07 7.78 29.62 2.1578 0.2049 0.2627 0.2999 0.8294 0.3844 0.6471
F40G50M10 14.12 6.34 6.24 5.4 20.46 2.2271 0.305 0.2639 0.4419 0.8517 0.3824 0.9842
F30G60M10 18.86 8.16 8.78 8.58 27.02 2.3113 0.3249 0.3175 0.4655 1.0515 0.4549 1.0760
F45G50M5 12.41 5.17 5.77 4.53 17.58 2.4004 0.3282 0.2577 0.4649 0.8762 0.3650 1.1161
F50G45M5 15.51 6.89 5.16 5.6 22.4 2.2511 0.2304 0.25 0.3327 0.8128 0.3611 0.7489
F40G55M5 12.81 5.41 6.82 4.59 18.22 2.3678 0.3743 0.2519 0.5324 0.8484 0.3583 1.2606
OPC (28d) 28 19.3 41.1 2.70 47.3 1.45 0.868 0.05 1.4673 0.139 0.09 2.1295

stretching paradigm of carboxylic acid group C-O bonds at

Fig. 12. Compressive strength variation with Ca/ (Si + Al), Na/ (Si + Al), Ca/Si.
improved, resulting in increased polymerization and cross-linking
of CASH gels. The intense band between 1455 and 1510 cm 1 is
connected to the CO2–3 asymmetric stretching structure of O-C-O
bonds, suggesting that during the curing process some superficial
sample carbonation occurred. The intense band is matched to the
1736 cm 1. Finally, the SiO4 bending vibration is corelated to the
495 cm-1 band, indicating the attendance of vitreous silica in the
ternary mixture.
Jamsheer et al. (2018) [86] , have studied the FTIR spectra for
OPC and OPC with nano silica. The bands Si-O are found to lie in
the range of 800 to 1200 cm 1 indicating asymmetric and symmet-
ric stretching vibration bands. The occurrence of C-S-H has been
showed at bands of 970 cm 1. Peaks at 875 cm 1 and between
1400 and 1500 cm 1 are related to O-C-O stretching and vibration
band. Additionally, the calcite peaks are seen at the band of
1480 cm 1, 875 cm-1and 720 cm 1.
The stretching and vibration bond O-C-O appeared in the
1423 cm 1 and 1489 cm 1 bands due to atmospheric carbonation,
which is in good terms with outcome stated in Bouaissi et.al.
(2019) [87] and Zawrah et al. (2018) [74]. O – H stretching and
bending (Water absorption) connected with alkali activation reac-
tion hydrated gels were seen in all the 9 ternary paste specimens at
a broad absorption band of about 3450 cm 1 and at a low band of
about 1630 cm 1 [64,69]. In the fly ash based ternary paste, O – H
broadband frequency tend to be higher than FA-based and GGBS-
based paste, because of the higher fineness of MK which eventually
resulted in increased gel formation. In addition, peak intensity
value increased with an increase in GGBS powder, resulting in

Fig. 13. EDS elements a. Na/ (Si + Al) vs Ca/ (Si + Al), b. Na/ Si vs Na/ Al, c. Ca/ Si vs Ca/ Al.

10
M. Kamath, S. Prashant and M. Kumar
Fig. 14. FTIR patterns a.MK20%, b. MK10%, and c.MK 5%
the development of extra hydrated ternary alkali-activated gels
such as CASH and CSH. Comparable outcomes have been reported
by Zawrah et al.(2018) [88]. The main band for alkali-activated
hydrated gel at around 1170 cm 1 was developed for all fly ash-
based ternary paste specimens associated with Si-O-T (T: tetrahe-
dral Si or Al) asymmetric stretching vibration phase, respectively.
These peaks apply to the core of the alkali activation reaction prod-
ucts, which is mostly associated with the ternary hydrated alkali
activated gel asymmetric stretching phase. Due to the gradual
growth of tetrahedral gels such as CSH, NASH, and CASH, the
increase in the number of these band waves [18]. The degree of
cross-linking in the FA and MK hydrated gels is usually higher than
in the GGBS and the rise in the content of GGBS has increased the
cross-linking of the gels. The results of the mechanical properties
and micrographs are consistent with this finding.
4. Conclusion
This paper investigates the properties of FA-GGBS-MK activated
using alkaline liquid that cured under ambient condition. Follow-
ing are the conclusions drawn from the experimental investigation.
FA-Slag-MK based ternary mixes have been found to set and
harden at room temperature and ambient conditions similar to
Portland cement
The studies pastes proportions produce CSH, CASH-NASH as the
reactions products that are physically and chemically stable as ver-
ified by FESEM, EDS, XRD and FTIR tests.
Fly ash based ternary pastes studied exhibits good workability
with slump values ranging between 135 and 170 mm, lower being
for the samples containing higher MK contents.
Compressive strength of mixes are found to be ranging between
57.14 and 102.04 MPa and are sufficient for the paste combinations
to be used for general and high strength structural concrete.
Mixes containing higher amount of MK exhibited dense and
compact morphology with reduced pores on comparing with OPC
paste.
Analysis of EDS has revealed higher ratio of Ca / Si, Ca/ (Si + Al)
and Na/ (Si + Al), which means, it has a potential to produce a
dense, and compact binding material on hardening.
11
Construction and Building Materials 277 (2021) 122323
CRediT authorship contribution statement
Muralidhar Kamath: Methodology, Formal analysis, Investiga-
tion, Validation, Visualization, Project administration, Writing -
original draft, Writing - review & editing. Shreelaxmi Prashant:
Conceptualization, Supervision, Methodology, Resources, Valida-
tion, Project administration, Writing - review & editing. Mithesh
Kumar: Formal analysis, Investigation, Data curation.
Declaration of Competing Interest
The authors declare that they have no known competing finan-
cial interests or personal relationships that could have appeared
to influence the work reported in this paper.
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