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Effect of Strength, Durability and Microstructural Properties of Multi Binder


Geopolymer Concrete in Ambient Condition

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Baskara Sundararaj J1*, Kannan Rajkumar P.R2
1Centre for Advanced Concrete Research, Department of Civil Engineering, SRM Institute
of Science and Technology, Kattankulathur – 603203, Tamil Nadu, India
2Department of Civil Engineering, SRM Institute of Science and Technology,

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Kattankulathur – 603203, Tamil Nadu, India
*Corresponding Author
Email ID – baskar.sundararaj5@gmail.com

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Abstract: This research paper examines the technical feasibility of using silica fume as
admixture to develop the M30, M50 and M70 grade geopolymer (GP) concrete using industrial

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wastes fly ash (FA) and Ground Granulated Blast Furnace Slag (GGBS). The various GP mixes
have been prepared by varying the precursor FA and GGBS percentage, concentration of alkali
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activator solution and inclusion of silica fume (SF) in FA admixture. Based on the mechanical
behavior the mix design has been optimized for M30, M50 and M70 grade GP concrete. The
results demonstrated that the maximum compressive strength (CS) for M30, M50 and M70
grade are achieved with the FA:GGBS combination of 70:30 concentration of alkali activator
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(3.5M) and Liquid by Powder (L/P) ratio 0.6, FA:GGBS combination of 70:30 concentration of
alkali activator (5M) and Liquid by Powder (L/P) ratio 0.47 and FA:GGBS:SF 65:30:5 with
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constant concentration of alkali activator (5M) and L/P ratio 0.49 respectively. Using a scanning
electron microscope (SEM-EDAX) and x-ray diffraction analysis (XRD), the microstructure of
the modified mixtures was assessed and correlated with mechanical parameters. It revealed that
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the SF addition enhanced gel formation by increasing the reactivity towards alkali and filling the
pores that ultimately reflected in strength characteristics which is also have confirmed through
SEM. It can be concluded from the results that the SF admixture for the strength improvement is
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technically viable.
Keywords: Geopolymer concrete, M30, M50 and M70 grade, Mix design development,
Compressive strength, Ultrasonic pulse velocity, Microstructure
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This preprint research paper has not been peer reviewed. Electronic copy available at: https://ssrn.com/abstract=4844367
Graphical abstract:

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Highlights:

1. Optimization of mix design for GP concrete M30, M50 and M70 grades
2. Increasing the molarity of solution has positive impact on mechanical strength
3. SF enhanced the strength by availing the reactive species in the mixture
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4. Microstructure changes are matched with the strength results


5. GP concrete slabs has tested for deflection characteristics
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1. Introduction

Geopolymers offer an alternative to traditional Portland cement-based concrete. They can be


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produced with lower energy consumption and reduced carbon emissions, making them more
environmentally friendly [1]. This can contribute to sustainable construction practices and help
combat climate change. Ordinary Portland Cement (OPC) is a major source of carbon di-oxide
(CO2) emissions. aluminosilicate polymers like GP could be synthesized using industrial wastes
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such as FA and Ground granulated blast furnace slag (GGBS), which can help reduce the overall
CO2 footprint of construction projects [2]. GP research is significant for several reasons, as it
addresses various economic, environmental, and technological challenges. Geopolymer can be
made from various industrial byproducts and waste materials, such as FA, slag, and mine tailings
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[3]. This repurposing of waste materials reduces the need for landfill disposal and provides a
sustainable solution for managing industrial byproducts [4]. GP are inorganic binders that can be

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made by polymerizing silica and aluminium containing sources with an alkaline solution or acid

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solution which are chemically identical to zeolites or alumino phosphates respectively with an
amorphous structure [5]. On comparing with OPC concrete, these aluminosilicate polymers are
more durable [6]. These polymerization materials can successfully replace conventional concrete
in pre-cast applications because they have good strength characteristics. In construction projects

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like Brisbane Airport and Queensland's University (GPC of 30.000 cubic meters), the GP is
rising to prominence [7]. Energy consumption and greenhouse gas emissions are reduced when
industrial waste is used to create GP binders [8].

Numerous studies have demonstrated that the mechanical, durability, ambient curing, and early
setting capabilities of the GP are superior to those of the OPC in many aspects [9]. The GP can

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be formed using the FAand GGBS with varying combination and alkali content [10]. The FA
derived GP concrete usually requires the moderatly high temperature curing of 60-80 deg C for 1
day whereas the GGBS enable the ambient curing this revealed that the Ca rich sources can be

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used to get ambient curing with enhanced strength properties [11,12]. The CS between 35 and 40
MPa for the GP binder absed com posites was formed by several FA samples activated with

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NaOH 8–12 M and cured at 85°C for 24 h, according to Palomo et al. [13], albeit this value
increased to approximately 90 MPa when water glass (SiO2/Na2O = 1.23) was added to the
NaOH. Additionally, in such circumstances, the water-to-binder ratio must be taken into account
in addition to the SiO2/Na2O ratio as a key parameter.
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In addition, Colangelo et al. [6] noted that using eco-sustainable binders and aggregates together
would be the best environmentally beneficial course to take in order to lessen the negative effects
of regular OPC concrete on the environment. Geopolymeric recycled aggragtes has a potential
new green material that may offer good performance as well as the ability to reduce
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environmental pollution and raw material usage [14].

Rudra Pradap Singh et al., have reported the GP mortar derived from the FA, GGBS and SF with
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recycled aggregate in alkaline condition. It provided the strengths of 52.15 MPa, Flexural
strength (FS) of 5.81 MPa and Split tensile strength (STS) of 5.23 MPa with the FA:GGBS:SF
ratio 35:50:15 which is 7-34% higher than of OPC prepared under similar conditions [15].
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Hilal El-Hassan el al have reported that fly ash and GGBS derived GP with the desert dune sand
as fine aggregate using the 14 M NaOH solutions[16]. The effect of the mix proportion, setting
time super plasticizer dosage, alkali activator content, and sodium silicate solution to sodium
hydroxide ratio (SSS/SHS) on mechanical properties have determined and correlated with the
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analytical modeling results. Finally reported that the GP made with 100% GGBS and equal
proportion of FA and GGBS is good. In a similar way the mix design development for the FA
and GGBS based GP have carried out by G. Mallikarjuna Rao et al. this research utilized the
NaOH of 8 M concentration and SSS/SHS ratio 2.5, different proportions of FA and GGBS,
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liquid to binder ratio and curing condition, and experimental analysis revealed that the GGBS
content, L/B ratio and curing plays important role in determining fresh and hardened properties

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[17]. Whereas the Xie et al., have only considered the precursor combination and Water to binder

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ratio on the initial and final properties of the GP concrete with aggregate from the waste
recycling. The experimental studies conducted to study setting time, slump value, mechanical
behavior, elastic modulus, stress strain behavior, toughness, and failure mode of alkali activated
FA -Slag based concrete composites containing 100% aggregates arrived from waste recycling.

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Finally the research concluded with the half quantity FA and remaining GGBS combination
provides excellent mechanical strength with requires workability and setting time. In an another
research work, the FA GGBS variation effects have been studied on mechanical and durability
properties such as acid resistance and sulfate resistance [18, 19].

Similar to this, other researchers have developed the qualities of concrete using various alumino

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silicate sources as binding materials, such as metakaolin [23, 24] in addition to FA and GGBS
[20-22]. Additionally, other studies have shown that the material properties can also be enhanced
by replacing the fine aggregates [25, 30], SF and nano silica [26-28], other mineral admixtures

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[29] as admixture for high performance concrete and thermally stable GP concretes.

Table 1. Literatures related to geopolymer concrete derived from coal based Class F Fly Ash
and waste from steel industry GGBS
er
Concentrati Mechanical
Microstructur
e
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Material Curing characterisati Other
Author Theme on of the characterisati Observation
Used Regime on studies
solution on

GP recycled Characterised
Curing
aggregate for
temperatu
concrete - compression Optimal
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FA, GGBS, re (20-


Optimization strength, curing is at
Construction 100 °C
of curing toughness, 80°C for 12-
Wang, & with an
condition for elastic XRD and 24 hours,
Junjie, et al., Demolition interval of
the GP modulus, SEM. resulting in
[30] waste based 20°C ) for
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derived from withPoisson's improved


coarese the
the FA and ratio of GRAC properties
aggreagtes duration
slag and GP recycled like CS.
of 6, 12
waste aggregate
and 24 h
aggregates concrete).
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The use of
The study
The study FA, GGBS,
investigated
Partial investigates and GP as a
mechanical
replacemnet FA, GGBS, the effect of partial
properties,
of m-sand Manufacture granite waste replacement
including CS,
with granite d Sand (M- powder on for M-Sand
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Vishnuram, powder to STS, and


Sand), and GP fresh and in concrete,
B. achive Ambient stress-strain
et.al [31] Granite mechanical with a focus
sustainability behavior of GP
powder (GP) properties at on early
in GP concrete, at
concrete with alkaline different strength gain
different ages
solutions. molarities and reduced
(7 days, 14
(10, 12, 14, carbon
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days, and 28
and 16 M). dioxide
days
emissions.

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The detailed

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microstructur
e via SEm
"SEM and FA and
and XRD
XRD Ground
leads to
Rajini et.al characterisati- Granulated
Ambient SEM, XRD correlate
[32] on of the FA Blast
better the
and slag Furnace Slag

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strength and
based GP (GGBS)
microstructur
e
observation.

construction
and
demolition

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Mix design waste, The study
development derived highlighted
0.3 to 0.8 -
of FA-GGBS aggregates, CS of nearly the higher
Gopalakrish alkali
based alkaline Ambient 60 MPa at 28 SEM, XRD CS with the
na et.al [33] activator to
recycled activator Days recycled
binder ratios
aggregate GP solutions waste based

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concrete and binder aggregates
material
such as FA
and GGBS
er Chloride ions
affected
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consistency,
strength, and
Corrosio
microstructur
n
effect of e. FSGC had
behavio
addition of improved
Examined ur was
chloride on strength
using XRD, evaluate
the durability The increasing 38.1% to
EDS, FTIR, d
and FA GP the chloride 114.2%
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and FESEM through


microstructur concrete, have the direct higher
Prusty et.al FA-GGBS analyses, corrosio
e Ambient impact on the strength than
[34] GP concrete indicating the n
characterisati strength, by FGC, lower
presence of potential
on of sole FA decreasing the corrosion
aluminosilicate (Ecor)
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and FA- strength. activity, and


gels and C-S-H and
GGBS less chloride
gel. corrosio
derived GP content than
n current
convcete. FGC.
density
Chloride
(Icor)
binding was
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lacking in the
GP concrete
mixes.

The study
corrosion
GP concrete observed that
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performance
(Fa-GGBS) the addition
of steel in Analysis using
with and GGBS addition of NaCl led
FA-GGBS FESEM
Prusty et.al without have gained to lower CS
based GP Ambient revealed the
[35] 3.5% NaCl, more CS than and an
concrete bu formation of
and steel that of FA. increased
incorporating different gels.
reinforceme likelihood of
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the chloride
nt. corrosion
ions.
initiation and
higher

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corrosion

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current
density in
steel
reinforcemen
t within the
GPC mixes

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containing
NaCl.

CS testing was
conducted for
specimens with
various levels The
of BMWA observation

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replacement suggests that
for GGBS. Up BMWA can
to 10% be used as a
BMWA substitute for
additiuon by GGBS in GP
this study
replacing the concrete,

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mainly
"Optimisation GGBS have potentially
focussed on
of GGBS enhanced the resulting in
the study of
based of GP strength higher CS. A
Kumar.A
et.al [36]
concrete with
the addition
of bio-
medical
the effcet of
Bio-medical
waste
derived
ashes on the
Ambient
er compared to
the standard
one. The
maximum CS
-
7% BMWA
replacement
after 28 days
of curing
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waste ash (39.8 N/mm2) achieved the
GGBS based
was achieved maximum
GP concrete.
with 7% CS. Also it
BMWA has been
replacement at confirmed
28 days. that 13 M
Specimens NaOH
prepared using performed
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13 M NaOH better.
achieved better
CS after 28
days.
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The research
measures the
Evaluation of
GP concrete
properties
CS of at
FA-GGBS
Ground different ages
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based GP Higher the


Granulated An increase in
Rao, G et.al concrete and GGBS higher
Blast Ambient the proportion
[37] cost analysis - will be the
Furnace Slag of GGBS
one part CS
and FA content is
alkali
associated with
activator
increased
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solution
compression
strength.

"An The GGBS


improved incorporated
Janardhan,et.
mechanical FA and slag Ambient GP concrete
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al [38]
behaviour of have shown
GP the increment
composites in strength

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with flya sh compared to

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and GGBS." the OPCX
concrete.

The research
focuses on
the use of

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pozzolanic
materials and
GP concrete
to reduce the
environment
"Experimenta al impact of
l and cement
microstructur Mechanical production.

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al analysis of properties were The
the room evaluated, mechanical
Rao et temperature FA,GGBS, including CS SEM, XRD, and
Ambient
al.,[39] synthesised SF (53.10 MPa), EDS durability
GP FS (4 MPa), properties of
composites and STS (4 GPC were

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derived from MPa). studied, and
the FA and the existence
GGBS. of GP

er products in
the
composition
was
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confirmed
through
microstructur
al analysis.
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Similarly so many research works and modeling have performed on GP for the mix proportions
for particular strength of concrete with other fresh and hardened properties. To summarize the
literature studies, it inferred that the proper mix design for different grades not yet finalized like
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cement concrete as well all the GP preparation utilized the highly concentrated NaOH solution of
minimum 8 M. So the present work aims to develop the different grades of GP concrete M30,
M50 and M70 from the FA, GGBS and SF using low molar solution curing at ambient
temperature based on the fresh as well as hardened properties. Towards achieving this, the fresh
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concrete properties such as slump, dry and wet density of GP concrete and the mechanical
properties of compression, split tensile and FS and modulus of elasticity will be studied along
with the non-deductive test using UPV. In addition the long term properties of water absorption,
Porosity, dry and apparent density will be studied.
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2. Materials and Methods

2.1 Materials
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For this investigation, class F FA ASTM C618 [40] from ennore thermal power plant was
used and its chemical composition was found out by using X-ray fluorescence (XRF) which are

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listed in Table 1. The fine aggregate used was manufactured sand confirmed to zone II as per IS

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383:2016 [41] with specific gravity of 2.53 and fineness modulus as 3.01. Sodium silicate
solution was obtained from the Kiran Global Chemicals Private Limited with modulus
SiO2/Na2O value of 2.0, Na2O 15.5wt.%, SiO2 31.0 wt.%. Sodium hydroxide lye of 49%
concentration with Molarity 18.7 M, silica modulus of water glass was modified to 2.0 with

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values of SiO2 at 31.0 wt.% and Na2O at 15.5 wt.%.

2.1.1.Aluminosilicate sources

a) b)

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c)
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Figure 1. Normal scale image of the precursors a) Fly ash b) GGBS and c) Silica Fume
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The Class F FA was used in this study satisfies the properties mentioned as per ASTM C618
[40]. The FA is an industrial by product obtained from thermal power plant, Ennore, Tamil
Nadu, India. Chemical composition of the precursor FA, GGBS and SF obtained by Energy
Dispersive X-ray fluorescence Spectroscopy (EDXRF) analysis are provided in Table 1. Table 2
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provides the physical properties of the FA, GGBS and SF. Ground granulated blast furnace slag
(GGBS) according to ASTM C989-06 [42] was used in this investigation. The GGBS used was
obtained from JSW Cement, Hyderabad, India. GGBS by products from steel plants obtained
from blast furnaces, during the separation of iron from iron ore. SF was obtained from ELKEM
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Pvt. Ltd., Mumbai, India, ASTM C1240-20 [43]. The SF also known as micro silica, it is an
ultrafine powder collected as a by-product of the silicon and ferrosilicon alloy production.

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Table 2 Chemical composition of fly ash, GGBS, and micro-silica (XRF)

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Composition SiO2 Al2O3 Fe2O3 CaO K2O MgO Na2O TiO2 MnO SO3 LOI
(%)
Fly ash 55 26 10.17 2.09 1.65 0.80 0.40 2.29 - 0.30 1.30
GGBS 21.58 14.88 1.78 55.25 0.48 2.63 0.015 1.01 0.74 0.46 1.175

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Silica Fume 96.2 0.09 0.63 0.23 0.24 0.37 0.09 - 0.84 0.16 1.15

Table 3. Physical properties of Fly ash, GGBS and Silica fume

Properties Fly ash GGBS Silica Fume

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Appearance Light grey Half White Grey
Specific gravity 2.1 2.78 -
Fineness modulus (90 micron) 7% 23%

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Bulk Density (kg/m3) 1005 1360 500
Specific surface (Blaine) m2/kg 330
er 425 20000
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a) b)
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10 µ 10 µ

c)
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10 µ
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Figure 2. SEM images of the a) Fly ash b) GGBS and c) Silica fume

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2.1.2. Alkali Activator Solution

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In addition, to activate the FA and GGBS is called pozzolanic materials, an alkaline activator
solution (AAS) is prepared by mixing sodium hydroxide lye and sodium silicate solution.
Sodium hydroxide in the form of pellets with 97% purity and commercially available sodium

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silicate solution were used. The molar ratio of SiO2 to Na2O for the sodium silicate solution was
2.0 (SiO2 = 31%, Na2O = 15.5%, and water = 53.5%). The sodium hydroxide and sodium silicate
solution ratio is different for 3.5M and 5M as to be 1:0.25, and 1:0.67 this final solution is an
alkali activator solution (AAS).

2.1.3. Aggregates

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The coarse aggregates of sizes 10-12.5 mm were used. The fineness modulus were conducted to
determine particle size distribution as followed in IS 383: 2016 [41], while fine aggregates used
was manufacturing sand (M Sand) and their respective physical properties were selected based

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on IS 383: 2016 [41]. Figure 3 represents the particle size distribution of the fine and coarse
aggregates. The physical properties of coarse and fine aggregates are given in Table 3.

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Figure 3. Particle size distributions of aggregates

Table 4. Physical properties of fine and coarse aggregates


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Sample Specific gravity Water absorption % Fineness modulus


10-12.5 mm
2.85 0.4 2.53
aggregate
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M.Sand 2.72 2.75 3.1

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2.2. Experimental Studies

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2.2.1. Mix proportioning, optimization and cast

2.2.1.1 Mix Proportion

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Mix proportions for different grades of GP concrete details are shown in Table 4. The GP
mixtures were designed according to lab trails the optimization of the GP mixes with different
grades (M30, M50, and M70) have arrived at IS:10262 – 2009 [44]. The varying mixture of slag
includes 0%, 10%, 20%, and 30% as replacements for FA for both grades. The M70 grade GP
concrete was prepared with 5% SF as replacements for FA. The sodium hydroxide solution, with

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3.5M and 5M concentration solution used for different grades of M30 for
(GP30M1,GP30M2,GP30M3 and GP30M4), M50 for (GP50M1, GP50M2, GP50M3 and
GP50M4), and M70 (GP70M1, GP70M2, GP70M3, and GP70M4).

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The GP concretes produced with 0%, 10%, 20% and 30% replaced FA based mixes with NaOH
solution molarity of 3.5M are designated as GP30M1, GP30M2, GP30M3 and GP30M4
respectively. The GP concretes produced with 0%, 10%, 20% and 30% replaced FA based mixes
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with NaOH solution molarity of 5 M are designated as GP50M1, GP50M2, GP50M3 and
GP50M4 respectively. The GP concretes produced with the same as M50 grade with replacing
the FA with 5% SF additionally are designated as GP70M1, GP70M2, GP70M3 and GP70M4
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respectively. Table 4 represents the mix proportions of the GP concrete.

Table 5. Mix Proportions of the Geopolymer Concrete

NaOH Na2SiO3 Coarse Molarity


Mix Id Fly ash GGBS SF M.Sand L/B*
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Lye solution aggregate (M)

GP30M1 1 0 0 172.8 43.2 760 973.9 0.60 3.5


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GP30M2 0.9 0.1 0 172.8 43.2 764.7 979.7 0.60 3.5

GP30M3 0.8 0.2 0 172.8 43.2 769.4 985.5 0.60 3.5

GP30M4 0.7 0.3 0 172.8 43.2 774.1 991.3 0.60 3.5


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GP50M1 1 0 0 129.72 86.48 722.4 925.5 0.47 5

GP50M2 0.9 0.1 0 129.72 86.48 728.1 932.7 0.47 5


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GP50M3 0.8 0.2 0 129.72 86.48 733.8 939.9 0.47 5

GP50M4 0.7 0.3 0 129.72 86.48 739.5 947.1 0.47 5

GP70M1 0.95 0 0.5 135.24 90.16 722.4 925.5 0.49 5


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GP70M2 0.85 0.1 0.5 135.24 90.16 728.1 932.7 0.49 5

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GP70M3 0.75 0.2 0.5 135.24 90.16 733.8 939.9 0.49 5

GP70M4 0.65 0.3 0.5 135.24 90.16 739.5 947.1 0.49 5

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L/B – Liquid to Binder ratio

2.2.1.2. Preparation of Alkali Activated Solution

The 3.5M and 5M NaOH solution was prepared and kept to reduce the heat for attaining room
temperature then mixed with sodium silicate solutions. The prepared AAS was kept undisturbed

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in air tight container post preparation for on eday to acquire equillibrium condition.

2.2.1.3. Geopolymer Concrete Cast

Preparation of GP concrete was carried out at ambient condition in the lab in a similar way as

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mentioned in the previously published literature [45]. Initially the dry matters such as FA and
GGBS and fine and coarse aggregates were mixed in a dry state for 3 minutes to get

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homogeneity in the laboratory grade Pan Mixer. After thorough mixing, AAS were added and
mixed for 5 minutes to obtain the required mix. In case of M70 grade of concrete mix, initial
mixing was performed with coarse aggregate and micro-silica in dry condition for 5 minutes.
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Then, fine aggregates, FA and GGBS will be added for doing dry mixing in dry condition.
Afterwards the AAS were added and mixed for 5 minutes to get the required mix as GP concrete
slurry. After that, the GP concrete slurry was cast in steel molds of different sizes as per the
requirement in three layers. It was compacted as three layers using the laboratory grade vibrating
table the concrete as it is being poured to prevent air pockets and ensure an even surface. For the
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CS testing the cast can be done in 100 mm x 100 mm cubical moulds. Moulds of 100 mm
diameter and 200 mm height cylinder shaped as per ASTM C 469 [46] and ASTM C 496-90
[47] has been used for the testing of modulus of elasticity and split tensile in compliance with
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EN 12390-51997 [48] requirement.

After the cast, the specimens were kept under ambient condition till hardening, then it was
demolded after 24 h. The demolding time duration is depend upon the reaction takes place in the
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mixes. Then the CS of the cubes and tensile test of the specimens in cylindrical forms was
determined after 3, 7, 14, 28, 56 and 90 days. The MOE test of the specimens was determined
after 28 days and FSs were left at ambient temperature for 28, 56 and 90 days before testing. the
figure 4 represents the casting phases of the GP for different property evaluation.
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Figure 4. Casting phases – Geopolymer concrete.

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C,

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Figure 5. Strength test set up a) Compressive Strength b) Split Tensile Strength c) Flexural
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Strength

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2.2.2. Testing

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2.2.2.1 Fresh properties and Mechanical Testing

Fresh properties of GP paste were determined by using Vicat apparatus tests based on IS: 4031 –
1988 [49]. The slump test of the fresh concrete wa s performed according to the ASTM C143

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[50] as tabulated in Table no 4. Also, the density of the fresh GP concrete was tested as per the
ASTM standard code C138 [51].

The mechanical properties tests were performed using a universal testing machine, under a load
rate of 1.8 kN/min for CS tests and at loading rate of 1.4 kN/cm2/min for split tensile and FS

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tests in accordance with the IS516-1959 [52] standard. The workability of the fresh GP concrete
was discovered by using slump cone test as shown in Figure 4, in alliance with ASTM C143 [50]
standard.

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2.2.2.2. Ultrasonic Pulse Velocity

An ultrasonic pulse velocity test is an in-situ type nondestructive test to identify the quality of

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concrete. In the present study, The ultrasonic pulse velocity technique as non-destructive testing
of concrete was used to distinguish GP concrete quality based on the mix design, and show the
know the quality of the concrete. This was done in accordance with BS 1881 (1986): part 203
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[53] using UPV setup as in Figure 6.
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Figure 6. The UPV testing setup

2.2.2.3. Rapid Chloride Penetration Test


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The current passing through the GP concrete specimens in the different time interval has been
measured from one month to nighty days by RCPT method as per the ASTM C1202 [54]. The
resistance of the concrete chloride penetration is assessed according to the total charge passed
within that period. The samples were positioned between two acrylic cells in the RCPT. The
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cells were each filled with a 0.3 M NaOH solution and a 3% NaCl solution, respectively. A 60-
V power supply was used to power the cells. The total charge travelled through the specimen

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was calculated by integrating the current and time throughout a different period of measurement

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and recording.

Using the formula below, the total charge passed Q is derived by integrating the current-time
curve. 𝑄 = ∫ 𝐼(𝑡)𝑑𝑡

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Where, I(t) is the time-dependent total electrical current and t is the elapsed time.

2.2.2.4. Water absorption, volume of permeable voids and Porosity

In order to identify the quality of concrete, tests like absorption and permeable voids were
carried out as per ASTM C 642-97 by oven-drying method [55] by using cylindrical specimens.

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The demoulded specimens were kept at RT for 28 days. the required specimen for testing(100
mm diameter and 100 mm height) is cut from cylinder of size 100 mm diameter and 200 mm
height into samples of size the sample has to be dried at 100℃ for 24 h. then it is cooled to to a

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temperature of 20 to 25 °C and determine the mass (A). the surface dried specimen is weighed
fot its weight after wiping with the towel.(B).

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Figure 7. Volume of permeable voids testing a) prepared specimen b) Cutting of the


specimen for testing c) Specimen immersed in water and kept at hot plate
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Place the same specimen, in a suitable receptacle, covered with tap water, and boil for 5 h. after
boiling, allow the specimen to cool for 14 h to reach 20 to 25°C. Then remove the surface

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moisture by using towel and measure the mass of the specimen (C). Suspend the specimen, after

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immersion and boiling, by a buoyancy balance and determine the apparent mass in water (D).
Porosity is the percentage of volume of permeable voids divided by the total volume.
2.2.2.5. Deflection Characteristic of geopolymer concrete precast slab

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In this experimental program deflection on slabs for three optimum GP mixes GP30M4,
GP50M4, and GP70M4 studied at 28 days respectively. Slabs of size 535 x 845 x 40 mm were
cast as shown in Figure 8. In order to minimize the evaporation of liquid from slab, the slabs
were covered with plastic sheets.

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Figure 8. Geopolymer slab a) Casting phase b) before testing slab c) Slab while testing
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d) failure pattern of GP30-M4 e) failure pattern of GP50-M4

f) failure pattern of GP70-M4

After 24 h, from casting time, the slabs were demoulded and allowed to cure in ambient
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temperature for 28 days. Now the the slabs were tested by using loading frame. The slabs were
simply suppored on all the four sides and ball, hydraulic jack were made to orient on the centre
of the slab for concentrated loading condition. Loading were applied at an interval of 1 kN until
it reaches the ultimate load of failure. The dial gauges were placed at the bottom centre of the
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slab to measure the deflection of slab.


2.2.2.6. Microstructure characterization

The morphology of the GP concrete samples were analysed using Hitachi S-4800 equipped with
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an energy dispersive X-ray (EDX) analyser (Brucker 5030) with an accelerating voltage of 15
kV under a low-vacuum mode and also for chemical analysis of the powder samples taken from

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the specimens. The XRD was used to analyse the minerological composition before and after the

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geopolymeroisation with different conditions using the instrument XRD-6000 SHIMADZU X-
Ray Diffractometer. The XRD analysis was performed at a scanning angle 2h ranged between 10
and 70o. The XRD peaks were analysed using the standard ICDD Data using PCPDFWIN
software.

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3. Results and discussion
3.1. Method of optimization and basics of mix design
Optimum mix for the different grades has been obtained via the maximum experimental trial
with the good CS and slump with minimum water absorption. Among that, 12 trials are listed in
Table 4 specifically and also considering the maintenance of low alkalinity of the alkali activator

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solution. The slump value with L/B ratio and wet and dry density is listed in Table 5. The mixes
for the different grades of GP concretes M30, M50 and M70 grades have been finalized based on
the slump value, the initial and final setting time and CS. The slump value is considered as the

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basic parameter for optimizing the mix design. In optimizing the M30 grade GP concretes, at
constant molarity of solution with constant L/B ratio, the slump value for 100% FA case is 117

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mm whereas 90:10, 80:20 and 70:30 FA: GGBS ratio mixed GP concretes slump reduced to
lower values as 108 mm, 98 mm and 87 mm respectively. It inferred that when increasing the
GGBS content the slump gets decreased in all cases. GP30M1 (3 M NaOH solution) shows the
slump value of 117 mm and GP50M1 (5 M NaOH solution) 98 mm and 93 mm for GP70M1 (5
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M NaOH solution with 5% SF). It indicated that increasing the molarity tends to decrease the
slump value. This is due to the fact that the FA having lower reactivity so its flow is higher
whereas when adding GGBS, or increasing the molarity tends to faster the reaction that
ultimately reducing the slump value. The similar trend is observed in all cases. The density of
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freshly cured GP concrete was in the range of 2400 kg/m3 for the GP30 series mixes, while it
increased up to 2450 kg/m3 for the GP50 and GP70 series. The difference between the wet and
dry densities of all the mixtures is only less than 1%.
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Table 6. Fresh Properties of Fly ash and GGBS based Geopolymer Concrete

Wet Dry
Mix IDL/B Ratio Slump in Density Density
(mm)
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(kg/m3) (kg/m3)
GP30M1 0.60 117 2384 2362
GP30M2 0.60 108 2398 2378
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GP30M3 0.60 98 2411 2392


GP30M4 0.60 87 2425 2407
GP50M1 0.47 98 2408 2384
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GP50M2 0.47 92 2431 2411

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GP50M3 0.47 85 2448 2434

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GP50M4 0.47 70 2457 2445
GP70M1 0.49 93 2444 2424
GP70M2 0.49 86 2450 2436

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GP70M3 0.49 78 2452 2442
GP70M4 0.49 62 2453 2445

Figure 9 shows the graph of the initial and final setting time of the GP concrete prepared by

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varying the FA and GGBS composition, molarity of the NaOH variations, L/B ratio and addition
of the admixtures. The concentration of the alkali solution, FA and GGBS ratios, and admixtures

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all have a significant impact on how quickly GP composites set. In the GP30 series, the initial
setting time for the 100% FA mix (GP30M1) is shown to be 117 minutes, which is decreased to

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37 minutes with the 30% GGBS component (GP30M4). Similar to this, the ultimate setting time
for GP30M1 is 620 min and for GP30M4 it is 420 min. The findings showed that GGBS content
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can be increased to enable faster settings. The GP50 and GP70 series follow the same direction.
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Figure 9. Setting Time of the Geopolymer Concrete

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Comparing the 100% FA case, the GP30M1 showed higher initial setting time of 117 minutes,

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105 min and 93 min for the GP50M1 and GP70M1. This is connected with the fastening of the
reaction by increasing the alkali concentration in GP50 mix, and addition of the reactive SF in
GP70 mix. This concludes that the characteristics of faster setting are additionally rendered by

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raising the alkali concentration and adding SF.
3.2. Mechanical aspects

3.2.1. Compressive Strength

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Figure 10. Compressive Strength of Fly ash and GGBS based Geopolymer Concrete
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Numerous testing have been done and various GP concrete grades (M30, M50, and M70) have
been designed based on the IS:10262-2009 [44]. The varying slag mixture includes 0%, 10%,
20%, and 30% as replacements for FA for all concrete grades, with a constant 3.5M NaOH
solution and L/B ratio of 0.54 for M30 grade, an improved 5 M NaOH solution and L/B ratio of
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0.42 for M50 grade, and then M70 grade GP concrete with 5% SF as a replacement for FA, 5 M
NaOH, and L/B ratio of 0.44. Figure 10 shows a plot of the CSs of the various GP concrete
classes. The GP concrete's CS has varied with grade and time intervals.
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According to the findings, GP30M1 achieved CSs of 5.00, 6.84, 7.96, and 9.42 MPa at 3 days, 7
days, 14 days, and 28 days, respectively. The strength of the 100% FA on the third day is only 5
MPa, which is incredibly low. The strength of the FA-based GP mortar that was substituted with
GGBS increased fourfold over the course of the experiment, indicating that as GGBS content
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rises, so does strength, according to reports in the literature [56,57].

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The results demonstrate that the GP50M1 experienced 7 MPa and 11.46 MPa at 3 and 28 days

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have attained the strength M50 grade with the very low alkali concentration itself.
Regarding the strength M50 achieved with the low alkaline condition and ambient temperature
curing, this study is innovative. Typically, high strength GP concrete is also used. Additionally,
it is typically challenging to achieve high strength GP concrete under normal circumstances. In

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order to develop the mix design for M70 grade concrete under low alkali conditions, this study
work also made an attempt to do so. To address this, the reactive SF was added to the M70
concrete grade. Consequently, the 100% FA replaced with 5% MS and the same 5% with a
different combination of FA and GGBS with 5% SF solution instead of FA and 5 M NaOH
achieve a CS of 16.32 at 28 days. However, according to prior research, high strength GP

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concrete can be produced by replacing the aggregate, adding nano- or micro-silica, and using a
highly concentrated alkali solution [58,59]. So these results concluded that GP concrete prepared
with the FA and GGBS combination of 70:30 with solution 1 (Molarity of NaOH 3.5) optimized
for the M30 grade with slump value of 87 mm. GP concrete prepared with the FA and GGBS

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combination of 70:30 with molarity of NaOH 5M optimized for the M50 grade with slump value
of 70 mm. The M70 grade GP concrete was optimized with FA and GGBS ratio of 65:30 with

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5% SF admixture with molarity of NaOH 5M having the slump value of 62 mm.

The M30, M50 and M70 optimized GP mixes has been studied for measuring the CS up to 90
days to know the strength changes with duration. The results are presented in Figure 11. Effect
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of duration on the CS different grades of concrete was analysed. The GP concrete experienced
the increasing strength with increasing the duration. From 28 days to 90 days, the GP30M4 and
GP70M4 found to be having the strength changes of around 6% only. The GP50M4 have shown
the higher rate of strength changes which is 15.5%. There is no significant strength changes
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observed with the exposing duration.


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Figure 11. Compressive strength of geopolymer concrete at different time intervals

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3.2.2. Split tensile strength (STS) of geopolymer concrete

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A previous study revealed that in usual case the SF addition enhanced the STS with changing the
microstructure of the FA and GGBS based GP concrete. In this work, the STS of the GP concrete
by varying the precursor composition, alkali concentration and SF addition have been studies and

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presented in the figure 12. the STS of the GP concrete follows the same trend as the CS of the
GP concrete. The 90 days STS varies from 3.68 MPa to 5.97 MPa for the GP30M4 to GP70M4.
The STS comparing the 3 and 28 days, 57%, 73% and 53.9% increment in STS is observed for
GP30M4, GP50M4 and GP70M4 respectively, whereas the difference in STS between 28 days
to 90 days are comparatively less 9.52%, 9.5% and 8.9% for GP30M4, GP50M4 and GP70M4
respectively. The 5% MS addition positively impacted the STS like previously reported literature

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this might be due to the enhancement of the binder gel formation via higher reactive nature [60].

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Figure 12. Impact of alkali concentration and SF on STS of the geopolymer concrete

3.2.3. Flexural Strength


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Figure 13 reports the FS of the GP mortar at various curing times for various grades of GP
concrete The GP30M4 shows lower FS strength compared to the GP50M4 and GP70M4 like CS.
Also highlighted is the fact that the FS has significantly improved from the FS at 28 days to the
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FS at 90 days.The difference in percentage FS 13.5 %, 16.08% and 17.8 % is observed for


GP30M4, GP50M4 and GP70M4 respectively. It is observing similar trend with the CS and STS
[61].
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Figure 13. Impact SF and curing period on flexural strength of the geopolymer concrete

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3.2.4. Modulus of Elasticity

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The modulus of elasticity of the optimized GP concretes for M30, M50 and M70 grades are
presented in Figure.
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70
GP50M4 GP30M4 GP70M4
60

50
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Stress (/MPa)

40

30
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20

10
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0
0 0.001 0.002 0.003 0.004 0.005 0.006 0.007
Strain (mm/mm)

Figure 14. Modulus of Elasticity of the geopolymer concretes M30, M50 and M70
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The stress strain curve for optimised GPC mixes GP30M4, GP50M4 and GP70M4 are presented
in the figure 14. The stress strain cure obtained consists of ascent and descent stages. In the
ascent stage, the stress increases with increase in strain up to ultimate load and after ascent stage,
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in descent stage, the stress decreases with increase in stain. The increase in the stress strain curve

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slope, increases the initial tangent modulus, secant modulus and chord modulus of the mixes,

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which thereby improves the ductility of the mixes. For GP30M4 mix, Elastic Modulus, Secant
Modulus and Chord Modulus are 16.38 GPa, 20.70 GPa and 20.65 GPa respectively. For
GP50M4, Elastic Modulus, Secant Modulus and Chord Modulus are 24.71 GPa, 31.62 GPa and

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47.35 GPa respectively. In GP70M4, Elastic Modulus, Secant Modulus and Chord Modulus are
36.42 GPa, 47.35 GPa and 46.27 GPa respectively.

3.3. Ultrasonic Pulse Velocity (UPV)

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The variation in ultrasonic pulse velocity of the optimized M30, M50 and M70 grade GP
concrete at different curing periods (3,7, 28, 56 and 90 days) are presented in Figure15. Using
UPV, it is able to assess the uniformity of the concrete, maintain its quality, monitor the

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deterioration, and check for internal flaws and voids.

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Figure 15. Ultrasonic Pulse Velocity value of geopolymer concrete

The ultrasonic pulse velocity of the concrete generally varies from 3 to 4.5 which ultimately
represent the quality and grade of the concrete. The velocity of the concrete increased with
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increasing the curing period. The maximum UPV value observed for the GP70M4 mix and the
GP30M4 and GP50M4 will be in the same range of velocity. The minimum UPV was observed
for the GP30M4 at 90 days curing period. But all the UPV values are representing the good
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grade of the concrete in terms of quality. The UPV value is also influenced by the curing period
in other ways maturity of the concrete. Curing period has the direct relationship with the UPV

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values with increasing the curing days, the geopolymerization occurs effectively and pores in the

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concrete are reduced which results in increased pulse velocity. The similar trend is followed in
the previously literature also [62-66]. With respect to the ultrasonic pulse velocity, the CS of the
various classes of GP concrete rises with increasing the curing duration. According to the

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standard data, this means that all of the optimized concretes have passed the quality testing in the
range of good to excellent.

3.4. Durability aspects

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3.4.1. Rapid Chloride Penetration Test

The charge passed through the GP concrete specimens was assessed using the RCPT tests. Table
7 provides the information regarding the charge passed through the GP concrete sample which

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indicates that the charge is changing depends on the curing period. Increasing the curing period
has the inverse relationship with the curing period. The higher grade of the concrete M70

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experienced lower charge passes through in all the curing period compared to M30. So the
charge passing is following the order of M30 > M50 > M70.

Table 7. RCPT Values in Geopolymer Concrete


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Particulars GP30M4 GP50M4 GP70M4
Days RCPT value in coulombs
28 days 1750 1520 1375
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56 days 1625 1485 1358


90 days 1560 1464 1347
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3.4.2. Water Absorption, Density, Volume of Permeable Voids and Porosity

The water absorption after immersion and of the after immersion and boiling is represented in
Table 8 at different times 3, 7 and 28 days. the water absorption results shows that the % of
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water absorption varies from 4 to 5.25 %. When comparing the GP30M4 to GP70 M12, the low
strength GP (GP30M4) has the more water absorption it is correlated with the VPV values as
high porosity compared to the GP70M12. Increasing the curing period leads to the reduction in
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water absorption ultimately represents the lower porosity. It is also reflected in the strength
results as lower water absorption, higher the strength values. the VPC values of the GP concrete
falls in the range of 13 to 11% it is also related the porosity in the matrix. the similar observation
have reported in the previous literatures (9).
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Table 8. Water Absorption, Density, Volume of Permeable Voids and Porosity

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Different Absorption after Apparent
Absorption after
Mix ID ages for immersion and density VPV (%)
immersion (%)
testing boiling (%) (mg/m3)

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3 days 5.25 5.81 2.611 13.175
7 days 4.92 5.53 2.594 12.57
GP30M4 28 days 5.23 5.99 2.605 13.51
56 days 5.37 5.93 2.630 13.50
90 days 4.62 5.44 2.553 12.22

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3 days 4.89 5.69 2.558 12.71
7 days 4.55 5.39 2.589 12.24
GP50M4 28 days 4.24 5.13 2.563 11.63
56 days 4.36 5.24 2.583 11.92

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90 days 4.00 4.75 2.656 11.22
3 days 4.80 5.37 2.622 12.36
7 days 4.81 5.53 2.621 12.67
GP70M4 28 days
56 days
90 days
4.80
5.09
4.07
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5.71
4.85
2.623
2.614
2.617
12.62
12.97
11.27
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3.5. Microstructural characterization
3.5.1. SEM/EDAX analysis

a b
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Gel
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Unreacted particles
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c

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Figure 16. SEM-EDAX of the GP30M4 a) 200 μm b) 30 μm c) EDAX

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a b
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c
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)
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Figure 17. SEM-EDAX of the GP50M4 a) 200 μm b) 30 μm c) EDAX

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a b

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)

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c
)

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Figure 18. SEM-EDAX of the GP70M4 a) 200 μm b) 30 μm c) EDAX

The Figure 16, 17 and 18 provides the typical SEM microscopic images of the GP GP30M4,
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GP50M4 and GP70M4 sample at different magnification and the corresponding EDAX spectrum
respectively. All GP matrix surfaces can be seen in SEM micrographs to contain gel phases, such
as N-A-S-H and C-A-S-H types, which are produced by the alkali reaction of FA and GGBS
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with some unreacted FA particles. In addition, the SEM images at 30 micron witnessed the
spherical shaped FA particles have started dissolution which appears as the FA embedded by
gels. The same observation is seen in the 200 micron SEM pictures as well, showing that all of
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the several reaction stages-dissolution, condensation, and gel formation occur simultaneously
and continuously. The SEM pictures also reveal some unreacted particles. GP70M4 has the most
gel phases out of the GP30M4, GP50M4, and GP70M4. The GP matrix's EDAX results revealed
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the existence of Ca, Si, Al, O, and Ns as a composition with varying intensities. This attests to
the N-A-S-H type and C-A-S-H type gel's presence. Since the presence of Na and Al is virtually

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equal, GP30M4 has achieved a Na/Al ratio of 1, meaning that each aluminum ion has been

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balanced out by a single Na+ ion. In each case, it is seen. Since the Si/Al ratio for the GPC is less
than 1, the Si/Al ratio for the GP50M4 and GP70M4 was greater than 1. This shows that the gel
formation and networking were significantly influenced by the rising molarity and the inclusion

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of SF. For GP50M4, increasing the molarity of the alkali solution enhanced the rate of
dissolution, increasing the reactivity and extending the gel, which ultimately provided it a more
binding nature, increasing the strength. In the instance of GP70M4, both molarity increase and
the addition of SF further influenced the reactive species in the mixture, which in turn improved

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gel formation, binding capacity, and strength. This finding was consistent with previously
published material [28] as well as the findings regarding CS.

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3.5.2. XRD Analysis

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Figure 19 XRD patterns of fly ash and GGBS

The XRD pattern of the FA and GGBS are given in Figure 19. The peaks in raw FA are assigned
to α-quartz (SiO2, PDF#89-8934), mullite (Al2O3, PDF#84-1205) they are less reactive in nature
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with crystallinity. An amorphous hump appeared approximately at the 2θ value of 22°–35° in the
raw GGBS. In addition to this, peaks corresponding to the anhydrite (CaSO4, PDF #01-072-
0916), akermanite (Ca2MgSi2O7, PDF #01-074-0990) and gehlenite (Ca2Al2SiO7, PDF #00-035-
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0755) are seen.

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Figure 20. XRD Pattern of GP30M4, GP50M4 and GP70M4

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[M-Mullite(Al2O3, PDF#84-1205), Q-Quartz (SiO2, PDF#89-8934), A-Akermanite
(Ca2MgSi2O7, PDF #01-074-0990), G-Gehlenite (Ca2Al2SiO7, PDF #00-035-0755), S-
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Hydroxysodalite, C-S-H (Ca1·5SiO3·5H2O, PDF #00-033-0306) in which Si is partially
substituted with Al (referred to as ‘C-A-S-H’)

The XRD pattern of the GP30M4 GP50M4 and GP70M4 are in Figure 20. All GPC shows the
amorphous gel phases in the range of 20°-28° 2θ.The semi crystalline hydroxysodalite is found
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in the 2θ value of 24° which is more pronounced with higher intensity in GPC12. This may be
formed due to the presence of more reactive silica from SF. More gel formation ultimately
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increasing the strength values which can be correlated with the compresssive strength results.
The C-S-H gel is present in all cases at 28° and 29° 2θ. The GP gel formation as well as effect
of SF is observed from the XRD results. The unreacted crystalline phases remains present from
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FA and GGBS as quartz, mullite , akermanite and gehlenite.

3.6. Deflection
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Load versus deflection of all slabs for GP30M4, GP50M4, and GP70M4 mixes are shown in
Figure. The deflection results show that as the increasing the concentration of the alkali solution
and SF addition ultimately decreased the central deflection of the slab. It shows that GP30M4
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mix exhibits more deflection compared to the other high grade of concretes GP50M4 and
GP70M4 mixes. GP30M4 and GP50M4 deflection curves are more gradual and flat compared

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the steep curve of GP70M4 slab. This confirms that the reaction products from various reaction

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conditions such as increasing the molarity and SF addition enhanced the strength. The strength is
inversely proportional to the ductile and deflection characteristics which are reflected in the
deflection results as low grade GP30M4 have the more defection of 3.48 mm. the high strength

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GP70M4 slabs showing the lesser deflection of 1.84 mm.

3.6. Comparison with IS code requirements

The maximum deflection from the deflection test for different grades of GP concrete is 3.48 mm

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for GP30M4 mix. According to IS 456:2000 codal provisions [67], the span to depth ration for
slab was found to be 13.375 mm which is less than 35 for two way simply supported slab.The
results obtained for GP30M4 was found to be lesser than the span to depth ratio of 13.375.

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12
GP50M4 GP30M4 GP70M4
10

8
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Load (kN)

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6

2
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0
0 0.5 1 1.5 2 2.5 3
Deflection (mm)
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Figure 21. Load vs Deflection curve for GP30M4, GP50M4 and GP70M4

4. Conclusion
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This research paper investigated the technical feasibility of using SF as admixture to develop the
M30, M50 and M70 grade GP concrete using industrial by-products FA (FA) and Ground
Granulated Blast Furnace Slag (GGBS). The various GP mixes have been prepared by varying
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the FA and GGBS percentage, concentration of alkali activator solution and replacement of FA
with SF admixture. the experimental results have revealed the following conclusions.

 The CS results indicated that the GP concrete optimum for the M30 grade with 87
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mm of slump was made using a 70:30 FA and GGBS combination with solution 1
(Molarity of NaOH 3.5). The 70:30 FA and GGBS combination, together with a

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5M NaOH molarity, were used to make GP concrete that was optimized for the

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M50 grade and had a 70 mm slump value. With a FA and GGBS ratio of 65:30, 5%
SF additive, and a molarity of NaOH 5M, the M70 grade GP concrete was
optimized with a slump value of 62 mm.

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 The optimized GP mixes M30, M50, and M70 have been examined in order to
determine how strength varies over time by measuring CS for up to ninety days.
The GP30M4 and GP70M4 were shown to have strength fluctuations of just about
6% between 28 and 90 days. The higher rate of strength changes15.5 % has been
observed in the GP50M4. Over the course of the exposure, no discernible increases
in strength were noticed.

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 STS of the GP concrete follows the same trend as the CS of the GP concrete in all
cases.

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 The GP70M4 mix, GP30M4, and GP50M4 maximum UPV values will all fall
within the same 4 km/s velocity range. During the 90-day curing period, the


the concrete is of a high caliber. er
GP50M4's minimum UPV was noted. However, all of the UPV values indicate that

The modulus of elasticity value are following the same trend as CS. GP70M4 has
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showed the better MOE than GP50M4 and GP30M4.

 The water absorption and volume of permeable voids have the great correlation
with the CS values. The addition of SF and increased alkali concentration have
raised the CS up to 70 MPa and reduced the water absorption to less than 4%.
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 The microstructure analysis have resulted the proof for the 5% SF addition,
increasing the NaOH concentration increased the reaction by changing the reactive
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species in the medium. It appeared as denser gel in SEM for GP70M4 sample and
GP50M4 sample. In XRD the hydroxy sodalite peak intensity has increased for the
GP50M4 and GP70M4.
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With the demonstration of durability characteristics and microstructure analysis, this research
concludes that the low alkali mediated M30, M50, and M70 grade GP has been optimized for
structural applications. Since this type of concrete has low slump, it can be used in precast
applications. This will help in the creation of eco-friendly building materials.
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5. References:

1. Davidovits, Joseph. "Geopolymer cement." A review. Geopolymer Institute, Technical papers 21 (2013): 1-
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