Effects of Nano-Silica On Slag Based Geopolymer: A Project Report Submitted by

EFFECTS OF NANO-SILICA ON SLAG BASED GEOPOLYMER
A Project Report
Submitted by
Medaaihun Marngar (B16CE019)
Na oo saki Garod (B16CE019)
Karasaphi Shabong (B16CE027)
In the partial fulfillment for the award of the degree of

Bachelor Of Technology
in
Civil Engineering
Department Of Civil Engineering

National Institute of Technology Meghalaya
Bijni Complex, Laitumkhrah
Shillong-793003, Meghalaya, India
CERTIFICATE
It is certify that the project entitled, “Effects of Nano-Silica on Slag Based Geopolymer"
submitted by Medaaihun Marngar (B16CE001), Na oo saki Garod (B16CE019) and
Karasaphi Shabong (B16CE02) is a bonafide work carried out by us in partial fulfillment of
the requirements for the award of the Bachelor of Technology in Civil Engineering at
National Institute of Technology Meghalaya during the period 28th January, 2020 to 15th
May, 2020 (8th semester) under the supervision of Dr. Dibyendu Adak, Assistant professor,
NIT Meghalaya.
This is to certify that the above statement made by the students is correct to the best of my
knowledge. I recommend this project report for evaluation.
Dr. Dibyendu Adak

Assistant professor
NIT Meghalaya
Date: 25th May, 2020.
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ACKNOWLEDGEMENT
We convey our sincere gratefulness to the Department of Civil Engineering, National
Institute of Technology Meghalaya for giving us a chance to channelize our knowledge and
skills by giving us an opportunity to work on our final year project work.
We are grateful to God Almighty for giving us the strength and wisdom for carrying our
project work and for sustaining our efforts which many a times did oscillate.
We would like to express our special thanks of gratitude to our supervisor Dr. Dibyendu
Adak, Assistant Professor of NIT, Meghalaya who has given us his valuable support,
cooperation and suggestion in our times of need.
We are also over helmed in all humbleness and gratefulness to thank Mr. Samuel Bennett for
his guidance in doing the experiments for the laboratory session and our fellow friends for
their help and support.
Finally, we would like to thank our parents for their constant support and motivation.
Date: 25th May, 2020.
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CONTENTS
TITLE PAGE NUMBER

CHAPTER 1:
1.0 INTRODUCTION 1-2
1.1 GOAL OF THE STUDY 3
CHAPTER 2: LITERATURE REVIEW
2.0 HISTORY OF GEOPOLYMER 5-6
2.1 SOURCE MATERIALS USED IN GEOPOLYMER CONCRETE 6
2.2 ALKALINE LIQUIDS USED IN GEOPOLYMER CONCRETE 7
2.3 MIX PROPORTION OF GEOPOLYMER CONCRETE 7-9
2.4 CURING CONDITION OF GEOPOLYMER CONCRETE 9-10
2.5 NANO SILICA BASED GEOPOLYMER CONCRETE 10-11
2.6 APPLICATION OF NANO-MATERIALS IN CEMENT BASED 11-12
COMPOSITE
2.7 GEOPOLYMER CURED AT AMBIENT TEMPERATURE 12-17
2.8 HEAT-ACTIVATED GEOPOLYMER CONCRETE FLY ASH 17-19
BASED
2.9 HEAT ACTIVATED SLAG BASED GEOPOLYMER MORTAR 19-22
2.10 HEAT ACTIVATED GEOPOLYMER MORTAR (OTHERS) 22-24
CHAPTER 3: EXPERIMENTAL WORK
3.0 INTRODUCTION 26
3.1 MATERIALS 26-28
3.2 MIXTURE PROPORTION 28-30
3.3 SAMPLE PREPARATION AND TESTING 30
CHAPTER 4: RESULTS AND DISCUSSION
4.0 RESULTS AND DISCUSSIONS 32-33
CHAPTER 5: FUTURE SCOPE
5.0 FUTURE SCOPE 35
REFERENCES 36-43
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LISTS OF TABLES
Table no. Name of tables Page no.
3.1 Composition of GGBFS 26
3.2 Composition of GGBFS 26
3.3 Properties of aggregates 27
3.4 Properties of Colloidal Nano-silica 28
3.5 Mix proportion 29
LIST OF FIGURES
Figures no. Name of the figure Page no.
1 Ground granulated blast furnace slag 27
2 Geopolymer concrete mix 30
Compressive strength of 8(M) geopolymer and

control mortar mix with / without nano silica at
3 32
different ages.
Compressive strength of 10(M) geopolymer

and control mortar mix with / without nano
4 33
silica at different ages.
Compressive strength of 12(M) geopolymer

and control mortar mix with / without nano
5 33
silica at different ages.
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Abbreviations
A Ash
AAFS Alkali-Activated Fly Ash-Slag
AAHFAC Alkali-Activated High-Calcium Fly Ash Concrete
AAM Alkali Activated Material
AAS Alkali Activated Slag
ACI American Concrete Institute
Al Alkaline Activator
Al/Bi Alkaline solution to binder
ALA Alkaline Activators
ALC Alcoffine
AMLF Acid Mass Loss Factor
B Binder
BA Bottom Ash
BET Brunauer-Emmett-Teller
BFS Blast Furnace Slag
CAC Calcium Aluminate Cement
CASH Calcium Aluminate Silicate Hydrate
CF Cotton Fabric
CNS Colloidal Nano Silica
CSH Calcium Silicate Hydrate
CSH Calcium Silicate Hydrate
DSC Differential Scanning Calorimetry
EDS Energy Dispersive X-ray Spectra
EDS Energy Dispersive X-Ray Spectroscopy
EDX Energy Dispersive X-Ray
EFNARC European Federation of National Associations
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Representing for Concrete
EGC Engineered geopolymer composites
FA Fly Ash
FESEM Field Emission Scanning Electron Microscope
FS Ferrochrome Slag
FTIR Fourier Transform Infrared Spectroscope
FTIR Fourier Transform Infrared
GGBFS Ground Granulated Blast Furnace Slag
GO Graphene Oxide
GPC Geopolymer Concrete
GRAC Green Recycled Aggregate Concrete
HVFA High Volume Fly Ash
HWGC Heavy Weight Geopolymer Concrete
IPCs Inorganic Polymer Concretes
ISO International Standards Organization
ITZs Interfacial Transition Zones
KANDOXI Kaolinite, Nacrite, Dickite Oxide
MK Metakaolin
NASH Sodium Aluminate Silicate Hydrate
NWG Sodium Waterglass
OPA Oil Palm Ash
OPC Ordinary Portland Cement
PCC Portland Cement Concrete
POFA Palm Oil Fuel Ash
RA Recycled Aggregate
RH Relative Humidity
RHBA Rice Husk-Bark Ash
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S Solution
SCC Self Compacting Concrete
SCGC Self Compacting Geopolymer Concrete
SEM Scanning Electron Microscope \
SEM Scanning Electron Microscope
SF Silica Fume
SFGC Slag/FA-Based Geopolymer Concrete
SFRGC Steel Fibre Reinforced Geopolymer Concrete
SH Sodium Hydroxide
SPs Superplasticizers
SS Sodium Silicate
SS/SH Sodium silicate to sodium hydroxide
TGA-DTA Thermogravimetric method
TPB Three-Point Bending
UCS Unconfined Compressive Strength
UHPC Ultra-High Performance Concrete
VPV Volume of permeable voids
WCF Waste Concrete Fines
XRD X-ray diffraction
XRD X-Ray Powder Diffraction
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ABSTRACT
In general, the slag based geopolymer concrete/mortar needs heat activation for early strength
developments depending on the molar concentration of activator. To overcome these
shortcomings, an experimental program has been taken up on slag based geopolymer mortar
having three molar concentrations (8M, 10M and 12M) of alkali activator liquids along with
different percentage of nano- silica addition (0%, 4%, 6% and 8% of GGBFS) Geopolymer
mortar with the addition of 6% of nano-silica shows appreciable improvement in compressive
strength at 28 days under ambient temperature curing.
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CHAPTER 1
1.0 Introduction
According to the World Business Council for Sustainable Development, “Concrete is the
most widely used material on earth apart from water, with nearly three tons used annually for
each man, woman, and child.” Concrete industry contributes at least 5 - 8% of the global
carbon dioxide emissions [1]. The decomposition of lime stone emits a substantial amount of
CO2 in the atmosphere and reduces the lime stone resources during the manufacturing of
cement. Therefore, there is a need to develop an alternative material, which will not only
reduce the demand for Portland cement, but also decrease the CO2 emission. From these
criteria, the proposed material must possess mechanical and structural properties comparable
to the Portland cement, but it should emit at a much lower rate. A possible solution to this
problem might be the use of slag based geopolymer mortar/concrete.
Ground Granulated Blast Furnace Slag (GGBFS) is a by-product of iron manufacturing
industry and is formed by the combination of constituents of iron ore with limestone flux.
When molten slag is cooled, it forms a fine, granular, almost fully non-crystalline, glassy
form known as granulated slag. Such granulated slag when finely ground and combined with
Portland cement, exhibits excellent cementatious properties [2]. The production of GGBFS
requires more energy as compared with the energy needed for the production of Portland
cement. By replacing the Portland cement with GGBFS will result in reduction of CO2
emission. It is therefore an environmental friendly construction material.
Geopolymers are a novel class of materials that are formed by the polymerization of silicon,
aluminium and oxygen species from an amorphous three dimensional structure [3-5]. There
are two main constituents of geopolymers, namely the source material and alkaline activator
liquid. The source materials for geopolymer based on alumina-silicate should be rich in silica
and aluminium. The source materials could be obtained from natural minerals such as
kaolinite, clays, etc. and the by-product materials such as silica fume (SF), slag, red mud and
FA. The combination of sodium hydroxide or potassium hydroxide and sodium silicate or
potassium silicate are used for geopolymerisation. Davidovits claims that the Egyptian
Pyramids were built by casting geopolymer on site [6]. He also reported that this geopolymer
material has excellent mechanical properties, does not dissolve in acidic solutions, and does
not generate any deleterious alkali-aggregate reaction even in the presence of high alkalinity
[7].
1
GGBFS had been widely used as a cement replacement material due to its latent hydraulic
properties. GGBFS shows an important role in the development of the compressive strength
of alkali activated geopolymer concrete. GGBFS based geopolymer concrete in the presence
of high concentration of alkaline solution results higher compressive strength when heat
cured at C from 6 to 24 hours [8-10].
Fly ash (FA) is an industrial by-product, which are most common sources for geopolymer
mortar/concrete because it is available throughout the world. Low calcium FA (ASTM Class-
F) based geopolymer mortar/concrete have been used as the binder, instead of Portland or any
other hydraulic cement paste, to produce concrete [11]. The FA-based geopolymer matrix
binds the loose coarse aggregates, fine aggregates and other un-reacted materials together to
form the geopolymer concrete. There are several factors that on which depends the strength
and durability of FA based geopolymer concrete, such as concentration of alkali activator,
mix proportion, curing temperature and curing time, etc. It has been noted that a higher
molarity of sodium hydroxide used as an alkali activator appeared to provide higher
compressive strength at early age [12, 13]. Sodium hydroxide leaches the silicon and
aluminium in the amorphous phase of slag and the sodium silicate acts as a binder. Also,
mechanical strength of geopolymer mortar/concrete depends on the ratio of sodium
hydroxide and sodium silicate [14-17]. In general heat activation is a much needed property
for geopolymer mortar/concrete in the presence of alkali activator. Several researchers have
been reported that mechanical strength and durability of geopolymer concrete depends on
heat curing period and temperature [18-21]. The compressive strength of such geopolymer
mortar is more at C comparable to C for a given molar concentration [16-21].
However, geopolymer mortar / concrete provides poor strength at ambient temperature of
about 27 ± C curing due to slow polymerization process. Thus the scope of geopolymer
concrete is limited to the precast member due to requirement of heat activation after casting.
The motivation behind the present study is (a) the development of slag based geopolymer
concrete without heat activation after casting and (b) assessment of structural behaviour of
such modified geopolymer mortar / concrete and their microstructural studies.
2
1.1 Goal of the study:
1) To optimize the slag based geopolymer concrete at different percentages of nano-
silica and at different molar concentration of alkali solution.
2) To study the effects of different percentage of nano-silica addition in slag based
geopolymer mortar of different concentrations and cured at the ambient temperature.
3) To study the mechanical strength of such geopolymer mortar by analysing the
compressive strength, flexural strength and split tensile strength.
4) To study the durability of such geopolymer mortar based on rapid chloride ion
permeability test and water absorption test.
3
CHAPTER 2
LITERATURE REVIEW
4
In this literature, the effects of different mineral admixtures on concrete properties like
workability, strength development, etc. are reviewed.
2.0 History of geopolymer:
The term ‘geopolymer’ is coined in the 197 s by Prof. Joseph Davidovits, to describe a
family of mineral binders with a chemical composition similar to zeolite but with an
amorphous structure. Geopolymers are a member of family of inorganic polymers, and are a
chain structures formed on a backbone of Al and Si ions. The polymerization of an Si-Al
minerals is a very fast chemical reaction in presence of highly alkaline condition, which
forms a three dimensional polymeric chain and ring structure consist of Si-O-Al-O. The three
known chemical units in the geopolymer structure are:
1. Si-O-Al-O, or poly sialate group,
2. Si-O-Al-O-Si-O, or poly (sialate - siloxo) group, and
3. Si-O-Al-O-Si-O –Si-O, or poly (sialate - disiloxo) group.
This polymeric chain binds the inert aggregate to form geopolymer concrete.
There are two main constituents of geopolymers, namely the source materials and the alkaline
liquids. The source materials for geopolymers based on alumina-silicate should be rich in
silicon (Si) and aluminium (Al). These could be natural minerals such as kaolinite, clays,
micas etc. whose empirical formula contains Si, Al and Oxygen (O). Alternatively, by-
product materials such as FA, SF, slag etc. could be used as source materials. The choice of
the source materials for making geopolymers depends on factors such as availability, cost and
type of application and specific demand of the end users. The alkaline liquids are from
soluble alkali metals that are usually sodium or potassium based.
Davidovits [22] worked with kaolinite source material with alkalis Sodium Hydroxide (SH),
Potassium Hydroxide (KOH) to produce geopolymers. The technology for making the
geopolymers had been disclosed in various patents issued on the applications of the so called
“SILIFACE-Process”.
Davidovits also introduced a pure calcined aolinite called A D I Aolinite,
acrite, Dic ite Ide which had been calcined for hours at 7 C. The calcined kaolinite
like other calcined materials performed better in making geopolymers compared to the
natural ones.
Palomo et al. [24] reported on FA based geopolymers where combinations of SH with
sodium silicate (SS) and KOH with potassium silicate (PS) as alkaline liquids had been used.
The type of alkaline liquid had been found as a significant factor affecting the mechanical
strength, and that the combination of SH and SS had given the highest compressive strength.
5
Gourley [25] stated that the presence of calcium in FA in significant quantities could interfere
with the polymerisation setting rate and also the microstructure. He also stated the use of Low
Calcium (ASTM Class F) FA being more preferable than High Calcium (ASTM Class C) FA
as a source material to make geopolymers.
2.1 Source materials used in geopolymer concrete:

John et al. [26] investigated on the mechanical properties of geopolymer concrete using red
mud and GGBFS as the source materials at varying percentage ratios (80%:20%, 70%:30%,
60%:40%). It reported a decrease in the workability and an increase in the compressive
strength with the increase in the red mud content. However, no significant rise in strength had
been observed with the addition of more than 30% of red mud.
Behfarnia et al. [27] reported that the partial replacement of the slag used in Alkali Activated
Slag (AAS) concrete with nano-silica and micro-silica had some effect on the permeability as
well as the microstructure of the paste. When replacement had been done with nano-silica,
the AAS concrete showed undesirable results with permeability whereas when replacement
had been done with micro-silica, the AAS concrete showed significantly reduced porosity
and permeability. Also, the replacement of slag with either of them had been found to
increase the compressive strength of AAS concrete.
Rika et al. [28] reported that the partial replacement of cement with volcanic ash at various
replacement levels (2%, 4%, 6% and 8%) resulted in a compressive strength which had been
found close to the same with the normal concrete mix design.
Narmatha et al. [29] investigated on the mechanical properties of the concrete specimens
with 5%, 10%, 15%, 20% and 25% replacement of cement by Meyakaolin (MK). It had been
observed that 15% replacement of cement with MK had shown better performance compared
to concrete without MK.
Jaarsveld et al. [30] reported that the particle size, calcium content, alkali metal content,
amorphous content, morphology and origin of the FA affected the properties of the
geopolymers. It had been revealed that the calcium content in FA played a significant role in
strength development and final compressive strength because higher the calcium content had
resulted in faster strength development and higher compressive strength.
6
2.2 Alkaline liquids used in geopolymer concrete:
Kannan et al. [31] reported in their study which had been based on the analysis of various
geopolymer specimens of 3M, 5M and 7M solutions that higher concentration of SH resulted
in higher strength of geopolymer concrete.
Deventer et al. [32] reported that the addition of SS solution to the SH solution as the alkali
activator enhanced the reaction between the source material and the solution. Furthermore,
after a study of the geopolymerisation of sixteen natural Al-Si, it had been found that the SH
solution caused a higher extent of dissolution of minerals than the KOH solution.
Shankar et al. [33] investigated on the performance of SS and SH solutions as the alkaline
liquid with varying ratio of 2, 2.5, 3 and 3.5 on different grades of FA based geopolymer
concrete (M30, M40, M50 and M60) where the mixes had been designed for 8M and
concluded that the workable flow of the geopolymers concrete depend on the ratio by mass of
SS and SH solution and that an increase in the workability of the freshly prepared
geopolymers had been observed with the increase in the ratio of alkaline solution. The
optimum dosage for alkaline solution had been found to be 2.5 because at this ratio maximum
strength in compression and tension for the geopolymer concrete specimens of any grade had
been observed.
Raijiwala et al. [34] concluded from their experiment that the addition of 50% SH and 50%
KOH along with SS as alkali activators to FA based geopolymer concrete at 80 C had a
positive impact on the strength and durability properties of geopolymer concrete.
Deb et al. [35] studied the effect of different proportions of GGBFS and activator content on
the workability and strength properties of FA based geopolymer concrete. In their study,
GGBFS had been added as 0%, 10% and 20% of the total binder with variable activator
content (40% and 35%) and SS to SH ratio (1.5 – 2.5). Significant increase in strength and
some decrease in the workability had been observed in geopolymer concretes with higher
GGBFS and lower SS to SH ratio in the mixtures. Similar to OPC concrete, development of
tensile strength correlated well with the compressive strength of ambient-cured Geopolymer
Concrete (GPC).
2.3 Mix proportion of geopolymer concrete:

Reddy et al. [36] investigated on the mechanical and water absorption properties of concrete
consisting of FA, Alcoffine (ALC) and Colloidal Nano-silica (CNS) with various
replacement levels of cement (FA at 25%, ALC at 10% and CNS at 0.5%, 1%, 2% and 3%) at
water cement ratio of 0.43 under ambient temperature curing at 7, 28 and 56 days curing
7
period. When compared with the conventional concrete mixes, it had been found that the
tetranary blended mixes made with CNS showed higher compressive strength, split tensile
strength and flexural strength. Also, an improvement in the mechanical and water absorption
properties had been found to be most effective when the mix had been done with a
combination of 25% FA, 10% ALC and 1% CNS. A reduction in the strength and water
absorption properties had been observed beyond 1% CNS.
According to the investigations made by Adak et al. [37] the strength, durability, water
absorption and permeability of the geopolymer mortar had been improved by the addition of
different percentage of nano-silica (4%, 6%, 8% and 10% of FA) on low calcium FA
geopolymer mortar having three molar concentrations (8M, 10M and 12 M) of activator
liquids and this had been due to the transformation of amorphous compound to crystalline
compound as noted in the X-ray powder diffraction (XRD) and Field Emission Scanning
Electron Microscope (FESEM) analysis. An appreciable improvement in the compressive,
flexural and tensile strength at 28 days under ambient temperature curing had been achieved
with the addition of 6% addition of nano-silica. The water absorption and permeability had
been observed to be comparatively less for the 6% addition of nano-silica modified
geopolymer mortar.
Ravitheja et al. [38] investigated on the performance of concrete which includes a mix of FA-
slag-nano-silica with SH (12M) and SS solution as alkaline activator. The compressive
strength, flexural strength and split tensile strength of the mix had been found to be higher as
compared to that showed by the control PC mi only FA . It had been observed that
nano-silica showed the ma imum effect on the strength at days of curing at ambient
temperature 7 C). It had been further observed that the increased strength began to
decline when the concentration of nano-silica exceeded 6%. This had been due to the excess
amounts of unreacted particles in the geopolymer matrix that resulted in cracking and
excessive self-desiccation, eventually reducing the strength. This finding had given an
implication that the concentration of 6% of nano-silica in the GGBFS-blended FA based
geopolymer reacted completely and any further increase in the concentration of nano-silica
did not improve the strength. The incorporation of GGBFS with nano-silica in FA based GPC
had also resulted in increased deformation capacity of concrete due to the formation of
hydrated products at a larger scale. It had also been observed that GGBFS-blended FA based
GPC with 6% nano-silica addition yields better performance of concrete than that of binary
blended concrete comprising of only FA based GPC with 6% addition of nano-silica.
8
Ramezanianpour et al. [39] investigated on the mechanical and durability performances of
AAS mortars when nano- powder at the dosages of 2% and 4% and SF at the dosages of 5%,
7.5%, and 10% had been incorporated into the mortar mixes as GGBFS replacement. A
solution of SH or KOH dissolved in water with a molarity of 6M and SS in the form of a
solution with a silicate modulus of (SiO2/Na2O) of 2.33 had been used to activate the slag. A
microstructural analysis had been performed through scanning electron microscope (SEM)
micrographs and EDX analysis. Results had shown that filler effect of nano-silica had been
more significant when this material had been dry mixed with other materials.
Wang et al. [40] investigated that the addition of nano-silica into alkali activator mortar
improved the pore size distribution of hardened paste and its micro-structures, due to more
hydration products generated where the mesopores had been increased, and the micropores
and total porosity had been decreased. The investigation had been done using ground steel
slag powder and blast furnace slag powder as alumino-silicate source with various dosages of
nano-silica (0%, 0.5%, 1%, 2% and 3%) and SH solution as alkaline activator. The samples
had been cured at temperature 20 ± C and 95 ± RH. It had been concluded that the
compressive strength at early stage had been affected (increased) more than at later stage
when adding nano-silica, owing to the high activity of nano-silica. The hydration process had
been promoted and the nano-silica mainly affected hydration process at the early stage.
2.4 Curing condition of geopolymer concrete:
Kumaravel [41] investigated on the various curing (steam, hot air and ambient temperature)
effect of nominal strength GPC in which FA had been used as the base material with an
additional amount of GGBFS and which had been reacted by an alkaline solution. It had been
concluded that the compressive strength of hot cured concrete (60 C) had been much higher
than that of ambient cured (27 C) concrete. The results had also shown that slag as a part of
FA binder had been effective to accelerate the setting time of GPC in ambient condition [31].
Li and Liu 4 investigated that the utilization of slag as an additive for fly ash based
geopolymer had resulted in a significant increase in the compressive strength of the
geopolymer. It had been reported that the compressive strength of geopolymer with 4 slag
reached Pa and 7 Pa when cured for 14 days at C and 7 C, respectively. A
refined pore size and reduced porosity volume had been e hibited after 4 slag addition,
especially for geopolymer cured at 7 C.
Wetzel et al. [43] investigated the influence of SF on properties of fresh and hardened Ultra-
High Performance Concrete (UHPC) based on AAS. The results had shown that the addition
of fines like SF and MK to slag based alkali activated material (AAM) with high al aline
9
activation increased the pac ing density to achieve PC. A good wor ability had been
realized with very low w b ratio of . but also down to .17 with a silica content of 1 .
by weight. The concrete samples cured at C which contain no portland cement, had shown
a very high compressive strength and a low capillary porosity comparable to PC- PC.
These findings had shown that a high early compressive strength can already be reached by
curing under slightly increased temperature C) which can be realised in precast element
production.
Sarker et al. [44] concluded that there had been a reduction in the workability and setting
time with the increase of GGBFS in the FA based geopolymer mixture. However, an
increased workability and setting time had been observed when alkaline liquid content had
been increased from 35% to 45% of the total binder with reduced compressive strength. The
addition of slag up to 30% of the total binder resulted in a compressive strength of concrete
up to 55 MPa and that of mortar up to Pa at days. It had been found that the concrete
and mortar samples cured without heat developed strength gradually over the age while
samples cured at C for 1 day achieved high early strength which increased negligibly over
the age. Hence, the FA based geopolymer modified with GGBFS had been found to be a
suitable binder for low to moderate strength concrete production at ambient curing condition,
as the necessity of heat curing had been eliminated. The mixtures having 10% slag, 40%
alkaline activator and SS/SH ratio of 1.5-2.5 with no extra water had been considered as the
optimum mixture for reasonable compressive strength in ambient curing condition.
2.5 Nano- silica based geopolymer concrete:
Riahi et al. [45] observed that the dissolution degree of Si and Si-Al phases increased when
nano-silica had been added to the GPC specimens and these phases strongly improve the
polymerization process.
Sudipta et al. [46] concluded that nano-silica and also titanium di-oxide showed satisfactory
amount of compressive strength when added with low calcium FA based GPC.
Chiranjeevi et al. [47] found that the compressive strength properties of GPC had been
increased with 70% FA replacement than the conventional concrete and that the compressive
strength properties of GPC had been decreased with 90% FA replacement than the
conventional concrete.
Gopala et al. [48] observed that the addition of 6% nano-silica in GGBFS blended FA based
GPC cured at ambient temperature improved compressive strength, split tensile strength and
flexural strength of 46.54%, 50.72% and 48.29% over control GPC mix.
10
Abdulkadir et al. [49] investigated in their study the effect of nano-silica on short term severe
durability performance of FA based GPC. It had been found that nano-silica addition to FA
GPC improved both durability and residual mechanical strength due to lower porosity and
more dense structure.
Patel et al. [50] concluded that nano-silica has an impact on compressive and durability
properties of FA GPC. For the same percentage of nano-silica i.e. 5% the compressive
strength of GPC specimens with 12M had been observed to be 1.2 times more than GPC
specimens with 8M.
According to the investigations made by F.U.A. Shaikh et al. [51] it had been observed that
nano-silica contributed to later age compressive strength gain of High Volume Fly Ash
(HVFA) system and hence low early age compressive strength of HVFA system can be
compensated by the addition of nano-silica.
Zang et al. [52] found that an increase in the rate of cement and slag hydration with the
incorporation of 1% nano-silica in the cement pastes with high volumes of FA or slag. Also,
the incorporation of 2% nano-silica by mass of cementatious materials reduced initial and
final setting time by 90 and 100 min, and increased 3- and 7- day compressive strengths of
high-volume FA concrete by 30% and 25%, respectively , in comparison to the reference
concrete with 50% FA.
Khater et al. [53] Addition of nano-silica results in an enhancement in mechanical and
morphological characteristics of the formed geopolymer specimens incorporating fired and
unfired precursors. The enhancement and modification of the geopolymer specimens
achieved when using nano-silica up to 2,5%, however further increase results in
agglomeration and decreased in the efficiency of the added nano materials.
2.6 Application of nano-materials in cement based composite:
Chuah et al. [54] reviewed the impact of nanomaterials in the form of 0D particles, 1D fibres
and 2D sheets on cement and concrete composites. Inclusion of nanomaterials caused
degradation in the workability of cement pastes, which may be attributed to the adsorption of
free water onto the surface of nanomaterials. However, the use of nanomaterials accelerated
the hydration of cement by providing attachment site for the CSH gel. Pore refinement by
nanomaterials contributed to the durability and strength. Reinforcement by 1D fibres and 2D
nanosheets had been responsible for the crack bridging behaviour for strengthening cement.
Among all the mentioned nanofillers, Graphene Oxide (GO) had appeared to be an ideal
candidate to enhance the properties of cement-based composites. The excellent intrinsic
11
properties of the 2D nanosheet strengthened the brittle cement matrix. Furthermore, the
oxygen-bearing functional groups contributed to the homogeneous dispersion of GO in
cement matrix, nucleation of CSH and densification of the microstructure.
Lu et al. [55], reported that with the addition of 0.08 wt% of GO had improved the cement
hydration rate by accelerating the cement dissolution. The use of GO in cement matrix had
improved the resistance against carbonation attack, restricted the 28 days drying shrinkage of
cement paste due to compacted microstructures and self-curing effect at early age. With
0.03% by weight of cement increased the flexural strength of GO-cement composite up to
67%.
Chuah et al. [56] investigated on the dispersion of GO in cement composites using different
surfactant treatments. The use of surfactants such as polycarboxylate and gum Arabic ensure
GO nanosheets remain dispersed in the cement alkaline environment to effectively reinforced
cement paste.
Bai et al. [57] investigated on the effects of SF content on performances of cement paste
containing graphene in terms of mechanical and electrical properties and found that an
improvement in the dispersion of graphene and also an increase in the interfacial strength
between graphene and hydration products had been shown by the addition of SF. Also, the
mechanical and electrical performances had been improved by the addition of appropriate
amount of SF in case of composite containing low content of graphene.
Li et al. [58] investigated the effect of the incorporation of Graphene Oxide (GO) into
cement paste on workability, hydration, microstructure and compressive strength of cement
paste. The results showed a reduction in the workability when GO had been added upto
0.03% of cement. The incorporation of GO also showed a refinement in the pore structure of
cement paste due to filling of large pores by the GO agglomerates as well as an acceleration
in the hydration of cement and an increased in the compressive strength of cement paste.
2.7 Geopolymer cured at ambient temperature:
Xie et al. [59] reported an experimental study on the behaviour of FA, BA and blended FA
and BA-based GPC cured at ambient temperature. The workability of the coal ash-based
PC’s had been directly related to the mass ratio of FA: BA and the liquid to binder ratio
(l/b) and the mixes with a higher FA content and l/b ratio exhibited a better workability. The
Compressive, flexural and modulus of elasticity of coal ash-based (BA and FA) GPC
increased with a decreased in l/b ratio, or in an increased FA: BA ratio. SEM micrographs
showed that the density and homogeneity of the GPC increased with an increased in the mass
12
ratio of FA: BA ratio. This indicated that FA undergoes a higher degree of polymerization as
compared to that of BA. The ambient temperature cured coal ash-based PC’s exhibited a
higher drying shrinkage compared to that of OPCs due to the large amount of unreacted coal
ash particles in the hardened GPC structure due to lower degree of polymerization at ambient
temperature curing.
Temuujin et al. [60] reported the mechanical activation of FA results in particle size and
morphology changes with concomitant increase in reactivity with alkaline liquid. Mechanical
activation of FA in a vibration mill with milling media to powder ratio of 10:1 leads to a
reduction of particle size and change in the particle shape but little change in the
mineralogical composition. Mechanically activated ash based geopolymer paste cured at
ambient temperature showed 80% increase in compressive strength than raw FA based
geopolymer paste. The main contribution of increased compressive strength of geopolymer is
attributed to reduction in particle size and change in morphology allowing a higher
dissolution rate of the FA particles.
Wongpa et al. [61] reported that an ambient temperature cured Inorganic Polymer Concretes
(IPCs) can be produced from Rice Husk-Bark Ash (RHBA) combined with Fly Ash (FA).
The compressive strength of RHBA and FA modified GPC cured at ambient temperature had
been influenced by the ratios between the paste content and the aggregate content and the
weight ratio between the solution content (S) and ash content (A). The solution to ash ratio
had the most important factor that controlled the rate of reduction in compressive strength of
IPCs while paste to aggregate ratio had the less influence. The higher the S: A ratio, the lower
the compressive strength. On the other hand, for the same solid to ash ratio, the mixtures
containing higher paste to aggregate ratio produce lower compressive strength than that with
lower paste to aggregate ratio 0.34 and solid to ash content ratio showed the highest
compressive strength at ambient temperature curing.
Ngernkham et al. [62] reported that the effect of adding nano- SiO2 and nano- Al2O3 on the
properties of high calcium fly ash geopolymer pastes. The compressive strength and flexural
strength of geopolymer pastes containing nano- SiO2 and nano- Al2O3 had been higher than
that of the control paste. The addition of nano- SiO2 as additive to high calcium FA
geopolymer paste resulted in the decrease of setting time due to the formation of CSH which
accelerated the setting and hardening of geopolymer pastes. While the addition of same
amount of nano- Al2O3 resulted in only a slight reduction in setting time. Mechanical strength
of high calcium FA based GPC cured at ambient temperature increased with the addition of
nano- SiO2 and nano- Al2O3 due to the formation of additional CSH or Calcium Silicate
13
Aluminate Hydrate (CASH) and Sodium Aluminate Silicate Hydrate (NASH) gels in
geopolymer matrix.
Kumar et al. [63] investigated the performance of GPC cured in ambient condition with the
incorporation of nano-silica in the FA based geopolymer binders. Low calcium FA had been
used as the principal source of alumina-silicate and it had been blended with blast furnace
slag (BFS) in small percentages in order to accelerate the curing at room temperature. CNS
had been added at different rates to the total binder in order to understand its effect on the
strength properties. The 28 days strength properties of only FA based GPC with Nano-silica
had a considerable improvement over the control GPC mix. Based on this experimental
study, it had been concluded that, addition of 6% Nano-silica in only FA based GPC cured at
ambient temperature, improves compressive strength of 25.9% over control GPC mix.
Similarly, split tensile and flexural strengths improve 29.02% and 36.80% over respective
control GPC strengths. The strength properties of GGBFS blended FA GPC mix with Nano-
silica shows significant improvement over the control GPC mix. It had been observed that,
addition of 6% nano-silica in GGBFS blended FA based GPC cured at Ambient temperature
improves compressive strength, Split tensile strength and flexural strength of 46.54%,
50.72% and 48.29% over Control GPC mix.
Fang et al. [64] investigated the effect on the workability and mechanical properties of alkali-
activated FA-slag concrete cured at ambient temperature. In this study, the workability,
setting time and mechanical properties of Alkali Activated Fly Ash Slag (AAFS) with
different slag content, alkaline liquid / binder (AL/B) ratio, molarity of SH and SS/SH ratio
had been investigated. Afterwards, the optimal mixtures of AAFS had been proposed. The
results showed that workability and setting time decreased with the increase of slag content
and molarity of SH solution as well as the decrease of AL/B ratio. Compressive strength
increased with the increase of slag content and molarity of SH as well as the decrease of
alkaline activator to binder (AL/B) ratio, but it did not have significant relationship with
SS/SH ratio. In addition, equations provided by ACI code, Eurocode and previous researchers
for OPC concrete overestimated the values of splitting tensile strength, flexural strength and
dynamic elastic modulus of AAFS concrete. The mixtures of AAFS with slag replacement
level from to , AL B ratio of .4, 1   of S , and SS S ratio in the range of 1. to
2.5 had been considered as optimal mixtures regarding the performance criteria of
workability, setting time and compressive strength.
Xie et al. [65] had been reported an experimental study on the behavior of fly ash (FA),
bottom ash (BA) and blended fly and BA-based GPC cured at ambient temperature. The tests
14
of compressive strength, elastic modulus, flexural strength, workability, drying shrinkage and
absorption capacity had been carried out to determine the properties of fresh concrete and
mechanical and durability-related properties of hardened concrete. Test parameters included
the mass ratio of FA-to-BA, liquid alkaline-to-coal ash binder ratio, coal ash content and
concrete type. The results indicated that the selected parameters significantly affect the
microstructure and the behavior of GPCs. It had been seen that BA-based GPCs exhibited
significantly lower geopolymerization than that of the FA-based GPCs, resulting in the
inferior behavior of the former compared to the latter.
Parveen et al. [66] studied the fresh and hardened properties of alcofine activated
geopolymer concrete like workability, water absorption, compressive, splitting tensile and
flexural strengths as per Indian Standards. The prepared samples had been investigated
through X-ray diffraction (XRD) and SEM for the determination of their phase, composition
and microstructural properties. The results showed that GPC prepared with alcofine at
ambient temperature not only improves the properties but also encourages replacing the
conventional concrete. Furthermore, GPC specimens prepared with alcofine emerge to ensure
a densification process. The results of this study revealed that alcofine have a significant
effect on the polymerization of the GPC which in turn improves the strength and
microstructural features. Also, increased molarity and FA content, improved the strength of
all tested specimen.
Zaheer et al. [67] evaluated the viability of developing high strength geopolymer
composite by using low calcium FA as a principal binder and its partial replacement with
slag, hydrated lime and ultra-fine FA in the mortar mixtures. The solid precursors had
been activated with a multi-compound mixture of 12 M SH and D-grade SS at an
alkaline liquid/binder ratio of 0.60 at ambient temperature. The results indicated that the
compressive strength of geopolymer binder depend upon the nature of source materials
for a selected alkali-activating solution. Ambient cured geopolymer composites with
very high compressive strength, i.e. more than 100 MPa had been obtained with adequate
workability by including an optimum amount of slag in low calcium FA geopolymer.
The results also reflected a dense microstructure and reduced porosity for FA-slag
geopolymer composites.
Alomayri et al. [68] presented the mechanical and thermal properties of cotton fabric
(CF)-reinforced FA-based geopolymer composites cured under ambient condition.
Setting and hardening of above composite at ambient temperature are achieved by partial
replacement of small amount of FA with OPC. The effects of different quantities of OPC
15
on flexural strength, fracture toughness, impact strength and thermal stability of above
composite are evaluated, and the microstructural characterisation of each composite and
its matrix had also been conducted. Results showed that the mechanical properties of the
composites are improved with the addition of OPC; however, SEM images of fracture
surfaces reveal that OPC hinders toughening mechanisms by limiting the prevalence of
fibre pull out and fibre debonding. At high temperatures, the thermal stability of the
geopolymer composites increases with the presence of either OPC or CF layers.
Lee et al. [69] investigated the setting and the mechanical properties of the alkali activated
FA/slag concrete manufactured at the room temperature. It also examines to what extent the
slag in the alkali activated FA/slag mixture improves the mechanical properties of the
mixture under the room temperature curing conditions. A series of tests of compressive
strength, elastic modulus, split tensile strength, flow, setting time, and porosity of the alkali
activated FA/slag concrete had been carried out. The test results showed that the setting time
decreased as the amount of slag and the concentration of the SH solution increased. The
proper slag content in the alkali activated FA/slag mixture had been determined to be 15-20%
of the total binder by weight considering the setting time and compressive strength of the
alkali activated FA/slag concrete cured at room temperature. In addition, the modulus of
elasticity and split tensile strength of the alkali activated FA/slag concrete had been slightly
lower than those of the ordinary concrete as predicted by the American Concrete Institute
(ACI) code and Eurocode 2. The total porosity of the alkali activated FA/slag morta rhad
shown a similarity to that of the ordinary cement mortar, whereas mean pore size tended to be
smaller than that of the ordinary cement mortar.
Nath et al. [70] studied to achieve FA based geopolymers suitable for curing without elevated
heat. The results showed that FA based GPC for curing in ambient condition can be
proportioned for desirable workability, setting time and compressive strength using GGBFS
as a small part of the binder. Inclusion of GGBFS with class F FA helped to achieved setting
time and compressive strength comparable to those of OPC.
Hadi et al. [71] used the Taguchi method to design optimum mix proportions for GPC with
GGBFS as alumina-silicate source at ambient curing condition. The influences of binder
content, alkaline activator to binder content (Al/Bi) ratio, SS/SH ratio, and SH concentration
on the GPC had been investigated. Mix designs had been evaluated and it had been found that
specimens with a binder content of 450 kg/m3, Al/Bi ratio of 0.35, SS/SH ratio of 2.5, and
SH concentration of 14 M produced the highest 7-day compressive strength (60.4 MPa).
However, the setting time had been found to be short. Hence, FA, MK, and SF had been used
16
as partial replacement of GGBFS in different proportions to increase the setting time. It had
been found that the setting time improved for the partial replacement of GGBFS with FA,
MK, and SF.
2.8 Heat-activated geopolymer concrete fly ash based:
Wallah [72] investigated the study of drying shrinkage of heat-cured FA-based GPC. GPC
used low-calcium FA as its source material, alkaline solution and aggregates normally used
for OPC concrete. Four series of test specimens with different compressive strength had been
prepared to study the drying shrinkage of this concrete. The test results had been compared
with the calculated results of drying shrinkage as predicted by Gilbert Method which had
been normally used for OPC concrete. Test results showed that the heat-cured FA-based GPC
undergoes very low drying shrinkage. The drying shrinkage strain at one year as calculated
using Gilbert Method had been much higher, about five to seven times, compared to the
measured drying shrinkage strain from the tests.
Prof. Bhosale et al. [73] investigated on the usage on fly ash (FA) based geopolymer concrete
(GPC) in construction. This paper, reported on the study of the processing of geopolymer
using FA and alkaline activator with geopolymerization process. The factors that influence
the early age compressive strength such as molarities of SH had been studied. SH and SS
solution had been used as an alkaline activator. These studies comprised the comparison of
the ratios of Na2Si03&SH at the values 0.39 and . 1.The geopolymer paste samples had
been cured at C for 1 day and keep in room temperature until the testing days. The
compressive strength had been done at 7 and 28 days. The result showed that the geopolymer
paste with SH concentration, compressive strength increase with molarities increased.
Sarker et al. [74] investigated the cracking, spalling and residual strength behaviours of GPC
in order to understand its fire endurance for it to be used as a building material. FA based
geopolymer and PC concrete cylinder specimens had been e posed to fires at different
temperatures up to 1 C, with a heating rate of that given in the International Standards
Organization (ISO) 834 standard. Compressive strength of the concretes varied in the range
of 39–58 MPa. After the fire exposures, the GPC specimens had been found to suffer less
damage in terms of cracking than the OPC concrete specimens. The OPC concrete cylinders
suffered severe spalling for C and 1 C exposures, while there had been no spalling in
the GPC specimens. The GPC specimens generally retained higher strength than the OPC
concrete specimens. The SEM images of GPC showed continued densification of the
microstructure with the increase of fire temperature. The strength loss in the GPC specimens
17
had been mainly because of the difference between the thermal expansions of geopolymer
matrix and the aggregates.
Luhar et al. [75] had been reported a comparative study of thermal resistance of FA
based GPC and rubberized GPC. In this study, rubberized FA based GPC had been prepared
using waste rubber tire fibres as a partial substitute for natural river sand, providing an
efficient solution to the disposal problems of both FA and waste rubber. Changes in the
weight, compressive strength, density, and microstructure of control and rubberized FA based
PC at room temperature, and after thermal treatment at  C, 4  C,  C and  C for
two hours, had been investigated using X-ray diffraction (XRD), Fourier
transform spectrometry (FTIR) and thermo-gravimetric analysis (TGA-DTA). Results
indicated that the loss in strength for rubberized GPC at elevated temperatures had been only
slightly higher than that of the control GPC because of the probable mismatch between
the coefficients of thermal expansion of the integral materials.
Junaid et al. [76] investigated the behavior of GPC at elevated temperatures by using a
recently developed lightweight non-pelletized aggregates made entirely from FA (named fly
ash as replacement for conventional natural aggregates. Tests for the ambient and residual
properties of PC made using these new aggregates e posed to temperatures up to 1 C
had been carried out. The obtained results in terms of compressive strength, splitting strength,
and modulus of elasticity had been reported and compared with those obtained for GPC
produced using ordinary natural aggregates as well as with those reported in the literature for
OPC concretes. The effects of heat cycling, as well as, duration of heating on the strength and
deformational behavior of GPC had been also investigated.
Mehta et al. [77] investigated the sulfuric acid resistance of FA based GPC blended with an
additional calcium source. OPC had been added as additional calcium in the geopolymer
system as FA replacement (0, 10, 20 & 30%). The specimens had been exposed to 2%
sulfuric acid solution up to the age of 365 days, and the deterioration had been identified in
terms of mass loss and compressive strength retained. Microstructural analysis; SEM, XRD,
and EDS had also been carried out. The results indicated that the inclusion of OPC (as FA
replacement) improved the compressive strength of FA based GPC specimens significantly
whereas it did not have a similar effect on its resistance to sulfuric acid. The increase in
compressive strength for the unexposed GPC specimens had been due to the additional
calcium hydrated products which co-existed with alumina-silicate polymer structures. On the
other hand, for the specimens exposed to sulfuric acid for 365 days, the inclusion of OPC at
10% showed the maximum retained compressive strength of around 52% of the strength
18
value achieved for unexposed specimens at the same age. However, OPC inclusion beyond
10% decreases the ability of GPC specimens to retain compressive strength. Maximum
deterioration had been observed when FA had been replaced by OPC at 30%. This had been
due to the formation of additional calcium sulfate which increased with the increase in
calcium products in the mixture. Microstructural changes had also been observed for the
exposed specimens at 365 days and confirmed the presence of sulfur compounds as a major
cause for the deterioration.
Jay et al. [78] the effect of different commercial superplasticizers (SPs) such as naphthalene,
melamine and modified Polycarboxylate based on the workability and strength of a class F
FA geopolymer paste activated by two different activator combinations, i.e. 8 M SH solution
and a multi-compound activator composed of 8 M SH solution (28.6%) + SS (71.4%) with a
SiO2/Na2O ratio of 2.0. These SPs at a dosage of 1% by mass of FA had been added to the
fresh paste and flow-ability of the activated FA paste had been measured via mini slump test
and compared with that of the paste without using any SP. The experimental results indicated
that the effect of different SPs on the workability and strength of FA based geopolymer
directly depends on the type of activator and the SP. In the case of using 8 M SH solution as
the activator, naphthalene based SP had been an effective type; whereas modified
Polycarboxylate based SP had been the most efficient type when the multi-compound
activator had been used.
Sujatha et al. [79] investigated about the heat-cured GPC slender circular columns using
ASTM Class F FA. This research focuses on the adaptability of Indian FA into GPC
structural members used primarily to support compressive loads. In this paper, GPC slender
circular columns of size 100 mm diameter and length 1800 mm with 2.16 % reinforcement
had been casted, tested and results had been compared with its OPC concrete counterparts.
Totally, 12 specimens of M30 and M50 grade slender columns had been fabricated. Six
specimens each for low calcium FA based reinforced GPC as well as for OPC reinforced
concrete. The results have shown that the GPC columns have exhibited increase in load
carrying capacity, stiffness and ductility until failure.
2.9 Heat activated slag based geopolymer mortar:
Karakoc et al. [80] investigated the effects of alkali dosage and silica modulus when using
sodium metasilicate solution at different curing conditions on the geopolymerization of
ferrochrome slag (FS). As alkali activation for geopolymerization, SH and SS solution had
been used. Geopolymer cement had been produced using FS as raw material with 3 different
19
silica modulus (0.50, 0.60 and 0.70) and 4 different Na2O concentrations (4%, 7%, 10% and
12%). The setting time, hydration heat and compressive strength of geopolymer paste
samples and compressive strength of geopolymer mortar samples had been obtained. The
setting time varied between 120 and 870 min, it showed variability depending on Na2O
content. The highest 28 day compressive strength of the geopolymer paste samples had been
obtained from one with Na2O concentration of 7% and silica modulus of 0.70. Geopolymer
mortars had been prepared for the determination of compressive strength by adding FS: sand:
Al ratio 1: : . , . and .4 . The specimens had been cured at C and C kept for
20 h and the other mortar samples had been stored under laboratory conditions. Compressive
strength of the material decreased, when w: b (water: binder) ratio increased. The highest
28 day strength of the geopolymer mortar had been obtained at 0.30 w: b ratio and laboratory
temperature curing conditions. The hydration heat of geopolymer paste samples had been
found to be less than normal Portland cements. Scanning electron microscopy (SEM) and X-
ray diffraction (XRD) had been investigated to study the microstructural properties of the
geopolymers.
Islam et al. [81] investigated on the use of optimum level of Palm Oil Fuel Ash (POFA),
GGBFS (GGBFS) and low calcium FA with manufactured sand (M-sand) to produce
geopolymer mortar. Eleven mixtures had been prepared with varying binder contents with the
POFA content varying between 25% and 100%; the other constituent materials such as fine
aggregate and water had been ept constant. All the specimens had been cured in oven for
4 h at C and thereafter ept in room temperature about – 9 C) before testing for the
compressive strength. The highest compressive strength of about 66 MPa had been achieved
for the mortar containing 30% of POFA and 70% of GGBFS with a total binder content of
460 kg/m3. The increase in the POFA content beyond 30% reduced the compressive strength.
The density reduction after 3 days had been found negligible.
Degirmenci et al. [82] investigated the resistance of pozzolan-based geopolymer mortars
subjected to high temperatures and freeze-thaw cycles. Low calcium FA and granulated BFS
as waste pozzolans and natural zeolite as a natural pozzolan had been used as base materials
for producing geopolymer mortar. The other purpose of the research had been to study the
effect of alkaline activator ratio (SS: SH) on the performance of pozzolan-based geopolymer
mortar specimens subjected to extreme temperatures. The influence of high temperatures on
the properties of mortars had been investigated at C, C, and 9 C. Fire and freeze-
thaw and resistance of mortars had been investigated in terms of visual appearance, weight
loss and residual compressive strength. The minimal values of the residual compressive
20
strength had been obtained at 9 C for all mixtures. The residual compressive strength of all
specimens had been lower than the values obtained for specimens not subjected to any freeze-
thaw resistance test, except those containing GGBFS. The SS: SH ratios of the alkaline
activator solution used to prepare the geopolymer mortars have an effect on the weight losses
and residual compressive strengths of the specimens subjected to high temperatures and
freeze-thaw cycles. As the SS: SH ratios increased, the weight and strength losses decreased.
Goriparthi et al. [83] investigated the strength characteristics of GPC developed with FA and
GGBFS as binders, combined SS and SH solution as ALA. The parameters considered in this
research wor had been proportions of FA and BFS 7 - and - , curing conditions
utdoor curing and oven curing at C for 24 hours), two grades of concrete (GPC20 and
GPC50).The mechanical properties such as compressive strength, split tensile strength and
flexural strength along with durability characteristics had been determined. For studying the
durability characteristics of GPC 5% H2SO4 solutions had been used and the specimens had
been immersed up to an exposure period of 56 days. The main parameters considered in this
study had been Acid Mass Loss Factor (AMLF), Acid Strength Loss Factor (ASLF) and
products of degradation. The results concluded that GPC with sufficient strength can be
developed even under Outdoor curing using FA and GGBFS combination i.e., without the
need for any heat curing.
Rashad et al. [84] investigated the elevated temperature performance of alkali-activated
GGBFS/SF at ratios of 100/0, 95/5, 90/10 and 85/15 wt.%, activated with SS. The specimens
had been exposed to elevated temperatures ranging from 4 C to 1 C with an increment
of C. Compressive strengths before and after firing had been measured. Water quenching
test had been applied to determine thermal shock resistance of various mixtures. The various
decomposition phases formed had been identified using -ray diffraction D , scanning
electron microscopy SE and ED spectra. The results indicated that the compressive
strengths before and after firing increased with the presence of SF up to C, then
decreased at 1 C in comparison with neat activated slag specimens. The relative strength
of the neat alkali-activated slag paste had been superior and the inclusion of SF had adversely
impact on the thermal shock resistance.
Patare [85] investigated the effect of CaO content on GGBFS based GPC. Mix design
procedure used had been proposed on the basis of quantity, fineness of FA, quantity of water,
grading of fine aggregate, fine to total aggregate ratio and GGBFS had been used for M40
grade of GGBFS based GPC. During experimental work, variation of different parameter like
ratio of alkaline solution ratio (SS/SH) of 2 had been taken. Different molarities such as 12M
21
and 16M of SH had been taken. In addition, different percentage of such as 0%, 20%, 40 ,
of BFS with solution to FA ratio . and SS to S ratio had been ta en. The
samples had been cured in oven at 4 C temperature for 24 hrs. The results showed an
increase in the strength of GPC with an increase in percentage of GGBFS in the mix. The
strength increase up to 40% replacement of FA with GGBFS after that it starts decreasing.
2.10 Heat activated geopolymer mortar (others):
Tippayasam et al. [86] investigated how potassium alkali concentration and heat treatment
affected MK-based geopolymer. Geopolymers prepared using KOH and K2SiO3 alkali
solution instead of the more common SH and SS had been reported. The influence of KOH
concentration, curing temperature and heat treatment on the properties of MK-based
geopolymers had been studied. The KOH concentrations had been varied at 6, 8, 10, 20, 30
and 40 M, the K2SiO3 ratios used had been 1 and 1. and curing temperatures of 4 C
and C for 4 h had been applied. esults showed that geopolymer with 1 , cured
at 4 C, 24 h and heat treated at C gave the highest compressive strength at 28 days. The
heat treatment process caused the porosity of geopolymer increased because water had been
eliminated from the geopolymer structure by the applied heat, therefore, the density
decreased whereas the water absorption and the porosity of geopolymer specimens increased.
The microstructure of heat-treated specimens showed more mature geopolymer matrix than
that of non heat-treated ones leading to higher compressive strength in the former
geopolymers and had ceramic-like property.
Kamseu et al. [87] investigated on the enhanced thermal stability in K2O-MK-based GPCs by
Al2O3 and SiO2 fillers addition. Based on the principle of stability of geopolymer gel as
refractory binder, a geopolymeric paste in the K2O–Al2O3–SiO2 system had been developed
and used to produce refractory concretes by adding various amount of α-quartz sand (grain
size in the range 0.1 μm to 1 mm) and fine powder alumina (grain size in the range 0.1–
100 μm . The consolidated samples had been characterized before and after sintering using
optical dilatometer, DSC, D and SE . The total shrin age in the range of –9 C had
been less than 3%, reduced with respect to the most diffused potassium or sodium based
geopolymer systems, which generally records a shrin age. The ma imum shrin age of
the basic geopolymer composition had been recorded at 1 C with a 17% shrinkage which
had been reduced to 12% by alumina addition. The temperature of maximum densification
had been shifted from 1 C to 11 or 1 C by adding 75 wt α-quartz sand or fine
powder alumina respectively. The sequences of sintering of GPCs could be resumed as
22
dehydration, dehydroxylation, densification and finally plastic deformation due to the
importance of liquid phase. The geopolymer formulations developed in this study appeared as
promising candidates for high-temperature applications: refractory, fire resistant or insulating
materials.
Rovnanik [88] investigated the effect of curing temperature 1 C, C, 4 C, C and
C) and time on the compressive and flexural strengths, pore distribution and
microstructure of alkali activated MK material. The results had shown that the treatment of
fresh mixture at elevated temperatures accelerates the strengths development but the 28 days
mechanical properties had been deteriorated in comparison with results obtained for mixtures
that had been treated at an ambient or slightly decreased temperature. The influence of curing
temperature on microstructure of geopolymer matrix had been verified in terms of pore
distribution studied by means of mercury intrusion porosimetry. The study revealed a
tendency to increase pore size and cumulative pore volume with rising temperature, which
had been reflected in mechanical properties. It had been also shown the possibility of
monitoring the geopolymerization reaction by means of Infrared Spectroscopy.
Salih et al. [89] investigated effects of curing temperature on al ali activation of P FA.
Compression test had been conducted on samples activated with a mi ture of SS and S at
different curing temperatures ambient, C, 7 C, and C. Also, XRD, TGA, FTIR, and
SEM/EDX tests had been performed to trace changes due to geopolymerization. Results
showed that the ambient temperature can be applied to activate mixes with 100% POFA.
Compressive strength of up to 36.8 MPa had been obtained when samples cured at ambient
temperature. The threshold temperature for activation of P FA had been 7 C.
Salami et al. [90] investigated on the comparative effects of added water and naphthalene-
based superplasticizer (SP) on the compressive strength and microstructure of the developed
POFA engineered geopolymer composites (POFA-EGC). Three differently prepared
50 mm × 50 mm × 50 mm specimens (with 10% water, with 10% SP and with 5% SP & 5%
water) had been used to study the synthesis of POFA and alkali-activating solutions (8 M
NaOH(aq) + Na2SiO3 s . . volume fraction of P A fibres had been added to
engineer the cementitious composite mi ture. All the specimens had been cured in an oven
for 4 h at C to accelerate the geopolymer reaction process to generate the binder.
After testing, the obtained results showed that while specimens with added water only gave
the compressive strength of 29.4 MPa, there had been a 19% decrease in compressive
strength for samples with SP only at 28 days. The specimens which have water and SP
combined have the least strength. Microstructural examinations (SEM) and material
23
characterization (XRD, FTIR) of the alkali-activated composite also revealed the superior
performance of the specimens with water over SP. The significant finding of this research
work had been the better performance of POFA-EGC prepared with only water in both fresh
and hardened states.
Ahmad et al. [91] investigated the influence of Al(OH)3 as alumina source on the
compressive strength of POFA alkali-activated mortar (POFA AAM). The synthesis of the
developed POFA AAM stems from the mixture proportioning of Na2SiO3, NaOH, POFA and
Al(OH)3. At the th day, after  C heat and laboratory curing, the compressive strength of
the POFA AAM had been tested. It had been observed that the compressive strength of all the
POFA AAM specimens with Al(OH)3 addition had been lower than those of the specimens
without Al(OH)3 addition. The only exception had been with the POFA AAM at 2%
Al(OH)3 addition in all SH molarities. The compressive strength losses recorded in some
POFA AAM had been due to weak interfacial zones creation between the activated products
and the zeolitic phases, which became more apparent at higher Al(OH)3 additions. The
strength development of the POFA AAM microstructure had been studied with the aid of
SEM/ Energy Dispersive X-ray Spectroscopy (EDS), XRD and FTIR.
Hawa et al. [92] investigated on the microstructure, compressive strength, and drying
shrinkage of MK based geopolymers produced by partially replacing MK by oil palm ash
(OPA). The OPA had been used as raw material producing different molar ratios of
SiO2/Al2O3 and CaO/SiO2. The geopolymer samples had been cured at C for 1, 2, or 4
hours and kept at ambient temperature until testing. The compressive strength had been
measured after 2, 6, and 24 hours and 7 and 28 days. The testing results revealed that the
geopolymer with 5% OPA (SiO2: Al2O3    . : 1 gave the highest compressive strength.
Scanning electron microscopy (SEM) indicated that the 5% OPA sample had a dense-
compact matrix and less unreacted raw materials which contributed to the higher compressive
strength. In the X-ray diffraction (XRD) patterns, the change of the crystalline phase after
heat curing for 4 hours had been easily detectable compared to the samples subjected to a
shorter period of heat curing.
24
CHAPTER 3
EXPERIMENTAL WORK
25
3.0 Introduction:
In this chapter, the materials, mixture proportions, manufacturing and curing of the test
specimens are explained.
3.1 Materials:
The materials used in this experimental study are Ground Granulated Blast Furnace Slag
(GGBFS) as the source material, Fine Aggregates, alkaline liquids (NaOH and Na2SiO3
solution), nano-silica and water.
3.1.1 Ground Granulated Blast Furnace Slag (GGBFS):
The GGBFS is a by-product of iron manufacturing which when added to concrete improves
its properties such as workability, strength, and durability. This material is obtained by
heating of iron ore, limestone and coke at a temperature of 1500 C. The main constituents of
blast furnace slag are CaO, SiO2, Al2O3, and MgO and its composition is given in the table
3.1. The GGBFS has been collected from TATA steel Jamshedpur, Jharkhand, which a waste
material of the steel plant.
Table - 3.1: Composition of GGBFS
Size Percentage
> 500 micron NIL
300-500 micron 0.05
212-300 micron 0.62
150-212 micron 5.41
<150 micron 93.93
Table - 3.2: Composition of GGBFS

Constituents % Composition
Mg 4.94
Al 16.19
Si 20.94
K 0.91
Ca 55.85
Ti 1.17
26
Figure – 1: Ground Granulated Blast Furnace Slag.
3.1.2 Fine Aggregates:

Fine aggregate is an essential ingredient in concrete that consists of natural sand and crushed
stones. The quality and fine aggregate density strongly influenced the hardened properties of
the concrete. The aggregates we used here passed through the 2.36 mm IS sieve which has
the properties as given in Table 3.3 which are locally available.
Table - 3.3: Properties of aggregates
Property Value
Type Uncrushed (Natural)
Gradation Zone II
Specific gravity 2.5
Maximum size 2.36 mm
3.1.3 Alkaline Liquids:

The alkaline liquid used was a combination of sodium silicate solution and sodium hydroxide
solution. The SS solution (Na2O = 13.7%, SiO2 = 29.4%, and water = 55.9% by mass) in gel
form was purchased in bulk and was dissolved in water to make the solution. The sodium
hydroxide (NaOH) in pellets form with 97 – 98% purity was also purchased in bulk. The
NaOH solids were dissolved in water to make the solution.
3.1.4 Properties of Colloidal Nano-silica:
Silicon dioxide nano-particles are also known as nano-silica. It is a chemical compound that
is an oxide of silicon. It has been known since ancient times/ Silica is most commonly found
in nature of quartz, as well as various living organisms. In many parts of the world, silica is
the major constituent of sand. Silica is one of the most complex and most abundant families
of materials, existing both as several minerals and being produced synthetically.
The physical properties of nano-silica are as shown below in the Table - 3.4:
27
Table - 3.4: Properties of Colloidal Nano-silica
Colloidal Properties of colloidal nano-silica

Nano-silica
Average particle Solid content Viscosity pH Solid density
CemSynXLP
size (nm) (Wt. %) (PaS) (gm/cc)
20 to 40 nm 30% 8.5 9.0 - 9.6 2.37
3.2 Mix proportion and curing:

Three molar concentration of NaOH such as 8 (M), 10 (M), and 12 (M) were mixed with
Na2SiO3 in the proportion of 1:1.75 (by weight) to make alkali activator fluid with an extra
amount of water. Colloidal Nano-silica with 4%, 6% and 8% of GGBFS by weight was also
added to the fluid. Locally available sand was used for the present study. The ratio of
GGBFS: sand and activator fluid (with/ without nano-silica) to GGBFS were fixed at 1:3 (by
weight) and 0.40 respectively. At first, sand and GGBFS was dry mixed for two minutes and
the appropriate amount of activator fluid (with/without) nano-silica was added and mixed
thoroughly. For the preparation of controlled mortar sample, OPC of 43 grade (IS 8112) was
mixed with sand. The geopolymer mortar specimens without nano-silica were cured at 60
temperature for 48 hours within the hot air oven after 2 days of casting and were kept at
ambient temperature until testing. However, the geopolymer mortar specimens with nano-
silica were removed from the mould after one day of casting and were placed at ambient
temperature (27 ) until testing. The details of all the mixtures are shown in Table 3.5.
28
Table - 3.5: Mix proportion
Sample GGBFS: NaOH: Molar % of Nano Curing Conditions
Mark Sand Na2SiO3 Concentration Silica
CM 1:3 - - - Conventional water
(C:S) curing
8GMH 1:3 1.75 8 (M) 0.00 Heat cured at 60 for
48 h
8GM0 1:3 1.75 8 (M) 0.00 Ambient temperature (27
) curing
) curing
) curing
) curing
48 h
) curing
) curing
) curing
) curing
48 h
) curing
) curing
) curing
) curing
29
Figure – 2: Geopolymer Concrete Mix.
3.3 Sample Preparation and Testing:

The standard mortar cube specimens of size 70.6 mm x 70.6 mm x 70.6 mm is preprated for
different mixes to determine the compressive strength of mortar. All the specimens are tested
at 7 days, 14 days and 28 days after casting to determine the compressive strength of different
ages. The flexural strength testing are carried out on 50 mm x 50 mm x 200 mm geopolymer
mortar bar at different molar concentration and percentage of nano-silica addition. These
specimens is tested after 28 days from the date of casting. The centre point loading method is
adopted for determination of flexural strngth (AASHTO T 67). Water absorption test were
done on standard cube samples of size 70.6 mm x 70.6 mm x 70.6 mm after 28 days of
casting.
30
CHAPTER 4
RESULT AND DISCUSSION
31
4.0 Result and discussion:
Figure 4.1 shows compressive strength of GGBFS based geopolymer mortar samples
having molar concentration of 8(M) without nano silica (with heat curing) and 4%, 6%, 8%
& 10% of nano silica. The strength of controlled sample made with OPC cement is also
compared. Similar results are presented in figure 4.2 and 4.3 for molar concentration of
10(M) and 12(M). It is well accepted that the strength of slag based geopolymer mortars
without nano silica and cured at 60 C for 48 hours is more than conventional cement mortar
(control) at all ages. The compressive strength of geopolymer mortars with or without nano
silica is more at higher molar concentration due to the higher rate of alkali activation.
Figure – 4.1: Compressive strength of 8(M) geopolymer and control mortar mix with /
without nano silica at different ages.
However addition of nano silica in the GGBFS based geopolymer mortar up to 6% of nano
silica seems to provide comparable strength at ambient temperature curing as shown in figure
4.2 and 4.3) at 28 days. Beyond 6% of nano silica addition, there is a reduction in
compressive strength at all ages. It is observed that with the increase in molar concentration
the mixture becomes more viscous. It is also noted for particular molar concentration mainly
at 10(M) and more, the addition of nano silica makes the mix less workable but more
cohesive. However this will not affect the degree of compaction during casting of samples.
32
Although at the early ages, the compressive strength gain of geopolymer mortar with nano
silica cured at ambient temperature is not so satisfactory. It may be concluded that at about
6% colloidal nano silica addition provides optimum 28 days strength without any heat curing
for activation. This suggests the use of modified geopolymer mortar with nano silica in
practical application.
33
CHAPTER 5
FUTURE SCOPE
34
5.0 Future scope:
The future scope of the present work could be as given below:
1. The flexural and bond strength of such geopolymer mortar.
2. The durability property of such geopolymer mortar based on rapid chloride ion
permeability test, carbonation test, corrosion test and water absorption test.
3. The resistance of such geopolymer mortar to acid and sulphate attack.
4. Identifying the long properties of such geopolymer mortar like:
a. Creep behaviour under sustained load.
b. Drying shrinkage behaviour.
5. As geopolymer concrete requires proper mixing proportions for the development of
high strength, high performance concrete which may not be possible manually. So,
some global optimization technique can be developed to get the desired results with
greater accuracy and time saving.
35
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EFFECTS OF NANO-SILICA ON SLAG BASED GEOPOLYMER

In the partial fulfillment for the award of the degree of

Department Of Civil Engineering

Medaaihun Marngar (B16CE001)

Na oo saki Garod (B16CE019)

Karasaphi Shabong (B16CE027)

Dr. Dibyendu Adak

Date: 25th May, 2020.

Medaaihun Marngar (B16CE001)

Na oo saki Garod (B16CE019)

Karasaphi Shabong (B16CE027)

Date: 25th May, 2020.

TITLE PAGE NUMBER

Table no. Name of tables Page no.

3.1 Composition of GGBFS 26

3.2 Composition of GGBFS 26

3.3 Properties of aggregates 27

3.4 Properties of Colloidal Nano-silica 28

3.5 Mix proportion 29

Figures no. Name of the figure Page no.

1 Ground granulated blast furnace slag 27

2 Geopolymer concrete mix 30

Compressive strength of 8(M) geopolymer and

Compressive strength of 10(M) geopolymer

Compressive strength of 12(M) geopolymer

2.1 Source materials used in geopolymer concrete:

2.3 Mix proportion of geopolymer concrete:

2.5 Nano- silica based geopolymer concrete:

2.6 Application of nano-materials in cement based composite:

2.7 Geopolymer cured at ambient temperature:

2.8 Heat-activated geopolymer concrete fly ash based:

2.9 Heat activated slag based geopolymer mortar:

2.10 Heat activated geopolymer mortar (others):

Table - 3.2: Composition of GGBFS

3.1.2 Fine Aggregates:

3.1.3 Alkaline Liquids:

Colloidal Properties of colloidal nano-silica

3.2 Mix proportion and curing:

3.3 Sample Preparation and Testing:

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