Final 1

1.
INTRODUCTION
1.1. Preamble
It is widely known that the production of Portland cement consumes considerable energy and at
the same time contributes a large volume of CO2 to the atmosphere. However, Portland cement is
still the main binder in concrete construction prompting a search for more environmentally
friendly materials. One possible alternative is the use of alkali-activated binder using industrial
by-products containing silicate materials (Gjorv, 1989; Philleo, 1989). The most common
industrial by-products used as binder materials are fly ash (FA) and ground granulated blast
furnace slag (GGBS). GGBS has been widely used as a cement replacement material due to its
latent hydraulic properties, while fly ash has been used as a pozzolanic material to enhance the
physical, chemical and mechanical properties of cements and concretes (Swamy, 1986).
Recent research has shown that it is possible to use 100% fly ash or slag as the binder in mortar
by activating them with an alkali component, such as; caustic alkalis, silicate salts, and non
silicate salts of weak acids (Bakharev, Sanjayan, & Cheng, 1999a; Talling & Brandstetr, 1989).
There are two models of alkali activation. Activation by low to mild alkali of a material
containing primarily silicate and calcium will produce calcium silicate hydrate gel (C-S-H),
similar to that formed in Portland cements, but with a lower Ca/Si ratio (Brough & Atkinson,
2002; Deja, 2002). The second mechanism involves the activation of material containing
primarily silicate and aluminates using a highly alkaline solution. This reaction will form an
inorganic binder through a polymerization process (Barbosa, MacKenzie, & Thaumaturgo, 2000;
Sindhunata, 2006a; Xu, 2002). The term Geopolymeric is used to characterise this type of
reaction from the previous one, and accordingly, the name geopolymer has been adopted for this
type of binder (Davidovits, 1994). The geopolymeric reaction differentiates geopolymer from
other types of alkali activated materials (such as; alkali activated slag) since the product is a
polymer rather than C-S-H gel.
Blast furnace slag is a by-product generated during manufacturing of pig iron and steel and may
be defined according to ACI- 116R as nonmetallic product consisting essentially of calcium
silicates and other bases that is developed in a molten condition simultaneously with iron in a
blast furnace. It consists primarily of silicates, alumina-silicate and calcium- alumina- silicates.
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The cooling process of slag is responsible mainly for generating different types of slags required
for various end users. The physical and pozzolanic properties of slag vary widely with the
process of cooling. Granulated blast furnace slag is a non-toxic material and can be a good raw
material for making high-value and user friendly cementitious material for different civil
engineering applications.
Red mud, also known as bauxite residue, is a waste produced from the alumina industry.
Depending on the quality and purity of bauxite ores, the quantity of red mud generated varies
from 55-65% of the processed ores (Paramguru et al. 2005). In addition, according to a recent
US Geological Survey report (2009), bauxite ores mined globally amount to 202 million tons
(MT) in 2007 and 205 MT in 2008, which indicates the huge quantity of red mud generated
worldwide annually. Red mud is characterized by strong alkalinity (e.g., pH = 12 -13) and high
water content. Nowadays, all over the world, the most common disposal way of red mud is to
store it within specially constructed landfill sites near the alumina refinery plants, which is very
costly and tends to be harmful to the surrounding environment due to its high alkalinity.
Although extensive research has been conducted to reuse red mud (Glanville and Winnipeg
1991; Singh and Prasad 1996; Singh et al. 1997; Marabini et al. 1998; Yalcin and Plescia 2000;
Ayres et al. 2001; Cundi et al. 2005), to date there is still no viable and environmentally
acceptable solution for utilization of red mud. In fact, there is a common agreement that
geopolymerization could convert a wide range of aluminosilicate waste materials into building
materials with excellent physical and chemical properties as well as long-term durability
(Davidovits 1991; Davidovits et al. 1994; krivenko 1998; Usherov-Marshak 1998; and Krivenko
and Skurchinskaya 1991).
The various aluminosilicate materials such as flyash, Metakaolin, GGBS, Silica fume etc can be
used as source materials for alkali-activation. Of late, most of the research on alkali-activation
has been used fly ash as the starting materials. However, studies on Alkali-activated blast furnace
slag are still very limited. Thus more study has to be carried out before arriving at any definite
conclusion. In order to have complete understanding of the possibilities of applications of AAS
in different fields, a thorough study of its manufacturing processes, synthesizing parameters, mix
design are very much essential.
This research describes the geopolymer technology as an innovative means of reuse of red mud
which features high alkalinity and provides alumina, and blast furnace slag which provides
reactive silica (amorphous phase) absent in red mud. Furthermore, sodium silicate, the only
constituent that is a non-waste used for geopolymer synthesis, will also provide additional Si and
Na for alkaline activation of red mud and GGBS. In effect, this process turns industrial waste
outputs (i.e. red mud and blast furnace slag) into an input for another industry. The objective of
this research is to investigate the potential utilization of red mud and blast furnace slag as raw
materials for the production of blended alkali activated composites that can be used as a valuable
resource for civil infrastructure constructions.
1.2. Geopolymer terminology and chemistry

In 1978, Davidovits proposed that an alkaline liquid could be used to react with the silicon (Si)
and the aluminium (Al) in a source material of geological origin or in by-product materials such
as fly ash and rice husk ash to produce binders. Because the chemical reaction that takes place in
this case is a polymerization process, Davidovits coined the term Geopolymer to represent
these binders.
Geopolymers are members of the family of inorganic polymers. The chemical composition of the
geopolymer material is similar to natural zeolitic materials, but the microstructure is amorphous
instead of crystalline.
The schematic formation of geopolymer can be shown as described by Equations (1-1) and
(1-2).
(1.1)
(1.2)
The chemical reaction may comprise the following steps :

Dissolution of Si and Al atoms from the source material through the action of hydroxide ions.
Transportation or orientation or condensation of precursor ions into monomers.
Setting or polycondensation / polymerisation of monomers into polymeric structures.
However, these three steps can overlap with each other and occur almost simultaneously, thus
making it difficult to isolate and examine each of them separately.
Water is released during the chemical reaction that occurs in the formation of geopolymers. This
water, expelled from the geopolymer matrix during the curing and further drying periods, leaves
behind discontinuous nano-pores in the matrix, which provide benefits to the performance of
geopolymers. The water in a geopolymer mixture, therefore, plays no role in the chemical reaction
that takes place; it merely provides the workability to the mixture during handling. This is in contrast
to the chemical reaction of water in a Portland cement mixture during the hydration process.
A geopolymer can take one of the three basic forms: Sialate is an abbreviation for silicon-oxoaluminate. Polysialates are chain and ring polymers with Si 4+ and Al3+ in IV-fold coordination with
oxygen and range from amorphous to semi-crystalline.
(i) Poly (sialate), which has [-Si-O-Al-O-] as the repeating unit.

(ii) Poly (sialate-siloxo), which has [-Si-O-Al-O-Si-O-] as
the repeating unit.
(iii)
Poly (sialate-disiloxo), which has [-Si-O-Al-O-Si-O-SiO-]

as the repeating unit.
Figure 1 : Possible chemical

structure of geopolymer
Figure 2 : Basic forms of Geopolymer according to Davidovits.
1.3. Historical development of Geopolymers

In the 1930s, alkalis, such as sodium and potassium hydroxide, were originally used to test iron
blast furnace ground slag to determine if the slag would set when added to Portland cement.
In the course of studying the testing systems for slag, Belgian scientist Purdon (1940) discovered
that the alkali addition formed a new, rapid-hardening binder. He examined the sodium
hydroxide on a variety of minerals and glasses containing silicon and / or aluminum and
concluded it in two steps;
(1) Liberation of silica, alumina and lime and
(2) Formation of hydrated calcium silicates, aluminates as well as regeneration of alkaline
solution.
It was proposed that the hardening mechanism of alkali activated alumino silicate binder
involves dissolution of Si or Al in the presence of sodium hydroxide, and precipitation of
calcium silicate or aluminum hydrate with the generation of sodium hydroxide. Alkali-activated
slag cements (called Trief cements) were used in large-scale construction as early as the 1950s.
The usual activation is done by adding 1.5 % NaCl and 1.5 % NaOH to 97 % ground slag mix.
In 1957, Victor Glukhovsky, a scientist working in the Ukraine at the KICE (Kiev Institute of
Civil Engineering in the USSR) investigated the problem of alkali-activated slag binders and in
the 1960s and 1970s ultimately identified both calcium silicate hydrates, and calcium and sodium
alumino-silicate hydrates (zeolites) as solidification products. He also mentioned that rocks and
clay minerals react during alkali treatment to form sodium alumino-silicate hydrates (zeolites),
confirming earlier work carried out on clay reactivity. Glukhovsky called the concretes produced
with this technology "soil silicate concretes" and the binders "soil cements".
Earlier, Flint & al (1946), at the National Bureau of Standards were developing various
synthesizing processes for the extraction of alumina starting from clays and high-silica bauxites.
Howell (1963) developed a Zeolite A type, using calcined kaolin (metakaolin) instead of
kaolinite, preventing the formation of hydrosodalite. In 1972, the ceramicist team Jean Paul
Latapie and Michel Davidovics confirmed that water-resistant ceramic tiles could be fabricated
at temperatures lower than 450C, i.e. without firing. One component of clay, kaolinite, reacted
with caustic soda at 150C. The industrial application of this kaolinite reaction with alkali began
in the ceramic industry. In 1969, Besson, Caillere and Henin at the French Museum of Natural
History, Paris, produced hydrosodalite from various phyllosilicates (kaolinite, montmorillonite,
halloysite) at 100C in concentrated NaOH solution, (Besson et al., 1969).
Finally, Davitovits synthetisized a kind of mineral polymer material with cross-linked polysialate
chain. Hydroxylation and polycondensation reaction of natural minerals such as clay, slag, fly
ash and pozzolan on alkaline activation below 1600C developed this polymeric chain. This
inorganic polymer was first named polysialate in 1976 and later coined as Geopolymer.
Milestones in alumino-silicate chemistry
1.4. Alkali-activation of cementitious materials

It is widely known that the production of Portland cement consumes considerable energy and at
the same time contributes a large volume of CO2 to the atmosphere. However, Portland cement is
still the main binder in concrete construction prompting a search for more environmentally
friendly materials.
One possible alternative is the use of alkali-activated binder using industrial by-products
containing silicate materials (Gjorv, 1989; Philleo, 1989). The most common industrial byproducts used as binder materials are fly ash (FA) and ground granulated blast furnace slag
(GGBS). GGBS has been widely used as a cement replacement material due to its latent
hydraulic properties, while fly ash has been used as a pozzolanic material to enhance the
physical, chemical and mechanical properties of cements and concretes (Swamy, 1986).
GGBS is a latent hydraulic material which can react directly with water, but requires an alkali
activator. In concrete, this is the Ca(OH) 2 released from the hydration of Portland cement. While
fly ash is a pozzolanic material which reacts with Ca(OH) 2 from Portland cement hydration
forming calcium silicate hydrate (C-S-H) gel as the hydration product. Thus, when used with
Portland cement, GGBS or fly ash will not start to react until some Portland cement hydration
has taken place. This delay causes the blended cements to develop strength more slowly at early
ages compared to the normal Portland cement.
Recent research has shown that it is possible to use 100% fly ash or slag as the binder in mortar
by activating them with an alkali component, such as, caustic alkalis, silicate salts, and non
silicate salts of weak acids (Bakharev, Sanjayan, & Cheng, 1999a; Talling & Brandstetr, 1989).
There are two models of alkali activation. Activation by low to mild alkali of a material
containing primarily silicate and calcium will produce calcium silicate hydrate gel (C-S-H),
similar to that formed in Portland cements, but with a lower Ca/Si ratio (Brough & Atkinson,
2002; Deja, 2002). The second mechanism involves the activation of material containing
primarily silicate and aluminates using a highly alkaline solution. This reaction will form an
8
inorganic binder through a polymerization process (Barbosa, MacKenzie, & Thaumaturgo, 2000;
Sindhunata, 2006a; Xu, 2002). The term Geopolymeric is used to characterise this type of
reaction from the previous one, and accordingly, the name geopolymer has been adopted for this
type of binder (Davidovits, 1994). The geopolymeric reaction differentiates geopolymer from
other types of alkali activated materials (such as, alkali activated slag) since the product is a
polymer rather than C-S-H gel.
Figure 3 : Schematic representation of the

alkali activation reaction process
1.5. Applications
According to Davidovits (1988b), geopolymeric materials have a wide range of applications in
the field of industries such as in the automobile and aerospace, nonferrous foundries and
metallurgy, civil engineering and plastic industries. Davidovits (1999) classified the type of
application according to the Si:Al ratio as presented in figure 3.
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Figure 4: Application of Geopolymer.
One of the potential fields of application of geopolymeric materials is in toxic waste

management because geopolymers behave similar to zeolitic materials that have been known for
their ability to absorb the toxic chemical wastes.
Balaguru et. al. (1997) reported the results of the investigation on using geopolymers, instead of
organic polymers, for fastening carbon fabrics to surfaces of reinforced concrete beams. It was
found that geopolymer provided excellent adhesion to both concrete surface and in the
interlaminar of fabrics. In addition, the researchers observed that geopolymer was fire resistant,
did not degrade under UV light, and was chemically compatible with concrete.
In Australia, the geopolymer technology has been used to develop sewer pipeline products,
railway sleepers, building products including fire and chemically resistant wall panels, masonry
units, protective coatings and repairs materials, shotcrete and high performance fibre reinforced
laminates (Gourley, 2003; Gourley & Johnson, 2005).
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Use of GGBS in building material industry is not new, but practical application of
geopolymerization technology allows making it much better since the discovery of alkaliactivated cements and concretes, they have commercially produced and used for different
purposes in a variety of construction projects in the former Soviet Union, China and some other
countries. These commercial products and application include: structural concrete, masonry
blocks, concrete pavements, concrete pipes , Utility poles, Concrete sinks and trenches,
Autoclaved aerated Concrete, Refractory concrete, Oil-well cement and stabilization and
solidification of hazardous and radioactive wastes.
During the past two decades, alkali-activated cements and concretes have attracted much interest
all over the world due to their advantages of low energy cost, high strength and good durability
compared to Portland cement.
1.6. Objective of the Present Research

The objective of the present research is to investigate the effect of synthesizing parameters on
engineering properties of blended alkali-activated blast furnace slag composites. The blast
furnace slag in granular form was obtained from Tata Metalliks Lltd. Kharagpur, India. Each year
India produces around eleven million tons of GGBS, which can be significantly utilized in the
manufacturing of construction materials which is environment-friendly and will greatly reduce
primary energy, saves bulk of quarrying as well as potential landfill. Red Mud was acquired from
Ujjal Chemical works, Nadia, West Bengal,India.
A comprehensive experimental program has been conducted to appreciate the engineering
properties of blast furnace slag based blended alkali activated composites at ambient as well as
elevated temperatures.
The proposed research has been followed in the path as shown below:
1. (Blast furnace slag + Red Mud) with percentage composition of 80, 20 respectively was
found to be the best paste mix from compressive strength consideration.
2. Temperature study of the paste mix - 300C, 500C, 700C for 4 hours.
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3. Mortar cubes were casted with varying alkali content (6%,8%,10%) using GGBFS:RM =
80% : 20% and sand: source material will be varied as given below
Sand: Source material
1 :
1
2 :
1
1 :
2
4. Mortar cubes were then studied under elevated temperature of 300C, 500C and 700C.
5. Study on the effect of synthesizing parameters such as Alkali content, silicate content on
the physico-mechanical properties of blended AAS composites, that is, compressive
strength, bulk density, water absorption, apparent porosity, UPV and sorptivity.
1.7. Organization of the thesis

The thesis is organized into five chapters. Chapter one describes the motivation for developing
blended alkali activated slag and as an alternative binder for concrete. Chapter two reviews the
literatures on the environmental impact of ordinary Portland cement, the history of alkali
activation of cementitious material, the reaction mechanisms and properties of Alkali Activated
Slag (AAS), the type of raw materials suitable for alkali activated binder, and chemical
degradation and the transport properties affecting the durability properties of concrete. Chapter
three reports on the experimental studies on the strength development of blended alkali activated
slag mortar. Chapter four reports on the experimental studies on the strength and other
properties of AAS, including water sorptivity, water absorption, bulk density, apparent porosity.
Chapter five includes the conclusions and recommendations for further research.
Chapter 2: Review of Existing Literature
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Preamble
Literature on blended Geopolymer is very scarce and limited. Very few studies have been carried
out where supplementary materials were used with starting material. Most of the available
literature on geopolymer materials deals with synthesizing parameters pore morphology,
microstructure survey, durability study and other structural properties.
Lot of research has been carried out to study different types of geopolymer and alkali activated
slag. Some available papers are presented here.
SL.
LITERATURE
no.
TITLE: Property of geopolymer cements
AUTHOR: Joseph Davidovits
SUMMARY: Geopolymer cement hardens rapidly at room temperature and provides

compressive strength in the range of 20 Mpa. Final 28 day compressive strength is in
the range of 70-100 Mpa. X-ray diffraction result had shown that the
polycondensation of various alkali- alumino -silicate present in geopolymer binder,
are actually amorphous material.
TITLE: Effect of mix composition on compressive strength and microstructure of fly

ash based geopolymer composites
13
AUTHOR: Prof. Dr. Somnath Ghosh & Ravindra N Thakur

SUMMARY: Alkali content, Silica content, water content and curing condition
greatly affect the Compressive Strength of geopolymer mix.
Water plays an
important role during dissolution, polycondensation & hardening stages of

geopolymerisation. Reduction of water content improved compressive strength. The
choice of curing temperature & curing time affected final compressive strength of
geopolymer. The increase in compressive strength was observed with increasing
duration of heat curing and curing temperature.
TITLE: Effect of silica fume additions on porosity of fly ash geopolymers

AUTHOR: Debabrata Dutta, Suresh Thokchom, Partha Ghosh and Prof. Dr. Somnath
Ghosh
SUMMARY: They studied the effect addition of silica fume on the pore
characteristics of fly ash based geopolymer composites. Porosity, compressive
strength, water absorption and micro structural studies have been performed for the
resulting geopolymers. It has been found that addition of silica fume to fly ash based
geopolymer mortar specimens improves the total porosity. However, it increases
porosity in case of geopolymer pastes. Incorporation of silica fume enhances the
compressive strength of mortar specimens whereas it causes a significant drop for the
paste specimens. Water absorption values were found directly related to total porosity
of specimens. For paste specimens, water absorption gradually increases with
introduction of silica fume into mix.
TITLE: Experimental study on Geo-Polymer concrete incorporating GGBS
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AUTHOR: V. Supraja, M. Kanta Rao

SUMMARY: It was found that compressive strength is increased with the increase
in the molarity of sodium hydroxide. Compared to hot air oven curing and curing by
direct sun light, oven cured specimens gives the higher compressive strength but sun
light curing is convenient for practical conditions.
TITLE: Strength and Water Penetrability of Fly Ash Geopolymer Concrete

AUTHOR: Monita Olivia and Hamid R. Nikraz
SUMMARY: Geopolymer mixtures with variations of water/binder ratio,
aggregate/binder ratio, aggregate grading, and alkaline/fly ash ratio were investigated.
They concluded that the water/solids ratio is the most influential parameter to
increase strength, and to decrease the water absorption/AVPV and water permeability.
An optimum aggregate/binder ratio of 3.50 contributed to the high strength of the
concrete, whereas, to obtain a low porosity of fly ash geopolymer, the ratio needs to
be increased to 4.70.
TITLE: Parametric Study on the Properties of Geopolymer Mortar Incorporating

Bottom Ash
AUTHOR: Djwantoro HardjitoC ,Shaw Shen Fu
SUMMARY: They concluded that increase of bottom ash content decreases the
compressive strength of geopolymer mortar. Increase of curing temperature increases
the compressive strength of the geopolymer mortar. . Increase in concentration of
KOH solution also increases the compressive strength of geopolymer mortar.Increase
of bottom ash content increases workability of fresh geopolymer mortar but it
decreases with bottom ash content more than 75%.
TITLE: Compressive Strength and Interfacial Transition Zone Characteristic of

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Geopolymer Concrete with Different Cast In-Situ Curing Conditions

AUTHOR: Muhd Fadhil Nuruddin, Andri Kusbiantoro, Sobia Qazi, Nasir Shafiq
SUMMARY: The paper explained the compressive strength development through
polymerization process of alkaline solution and fly ash blended with Microwave
Incinerated Rice Husk Ash (MIRHA). Three curing conditions, which are hot gunny
curing, ambient curing, and external humidity curing were applied. The compressive
strength development of geopolymer concrete was much affected by the curing
condition during maturing period. Therefore proper curing method was important to
obtain acceptable geopolymer concrete structures. The external exposure curing
condition used in this research was an acceptable technique to produce good concrete
structures.
TITLE: Alkali-activated fly ash-based geopolymers with zeolite or bentonite as

additives.
AUTHOR: Hu Mingyu, Zhu Xiaomin, Long Fumei
SUMMARY: They studied the synthesis of geopolymers at ambient temperature by
using fly ash as the main starting material, zeolite or bentonite as the supplementary
material, and NaOH and CaO together as activators. Though fly ash is pozzolanic
material, its reactivity is much lower than that of metakaolin. Therefore, its reaction
rate is quite low at ambient temperature. To explore this property, the following
supplementary materials were used in this study to accelerate the geopolymerization
and to improve the properties of the fly ash-based geopolymers. As an exploration, in
this work NaOH and CaO were used together as alkali-activator.
TITLE: Inflence of Slag as additive on the compressive strength of Fly Ash based
Geopolymers
16
AUTHOR: Zongjin Li and Sifeng Liu

SUMMARY: To improve the compressive strength of FA-based geopolymer at lower
temperature had been made. Moreover, slag was used as additive. Up to 4% by
weight of dry powders slag was incorporated into fly ash-based geopolymer 10%
metakaolin and 90% fly ash, to improve its compressive strength. Compressive
strength of 53.1 and 70.4 MPa cured at 30C and 70C for 14 days, respectively, have
been achieved. The mechanism of slag as an additive on compressive strength
improvement was investigated using XRD and MIP.
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TITLE: Fire-resistant geopolymer produced by granulated blast furnace slag

AUTHOR: Cheng and Chiu
SUMMARY: He found that the setting time of geopolymer paste made with GGBS
as the source material along with metakaolinite, was affected by the curing
temperature, type of alkaline activator, and the actual composition of the source
material. The setting time of geopolymer paste was observed to range from 15 to 45
minutes at 60C.
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TITLE: Effect of Incorporating Silica Fume in Fly Ash Geopolymers

AUTHOR: Suresh Thokchom, Debabrata Dutta, Somnath Ghosh
SUMMARY: They investigated the effect of incorporating silica fume on physic
mechanical properties and durability of resulting fly ash geopolymers. Silica fume in
the range of 2.5% to 5% was incorporated with the alkali activated fly ash. Durability
of geopolymer materials was assessed by regular monitoring of its physical
appearance, weight changes and compressive strength changes on exposure to
magnesium sulphate solution. It was noted that apparent porosity of geopolymer paste
specimen increases with increase in silica fume content. Geopolymer paste
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incorporated with silica fume resulted in higher sorptivity while it for geopolymer
mortars.
12
TITLE: Evaluation of Geopolymer properties with temperature imposed on

activator prior mixing with fly ash
AUTHOR: Debabrata Dutta, Suman Chakrabarty, Chandan Bose, Somnath Ghosh
SUMMARY: It provides with the effect of temperature on activators before mixing.
It was found that temperature in which activator was subjected prior mixing effects
compressive strength significantly.
13
TITLE: Effect of Curing Conditions on the Compressive Strength and

Microstructure of Alkali-activated GGBS paste
AUTHOR: Mohd. Nadeem Qureshi and Somnath Ghosh
SUMMARY: They presented the effect of curing method on the strength
development of alkali- activated blast furnace slag paste. Alkali activation was done
using a combination of potassium hydroxide and sodium silicate. The test parameters
include the curing methods (water curing at 270C, heat curing at 500C and controlled
curing with relative humidity 50%, 70% and 90 % at 270 C), alkali content with 6.41
%, 8.41 %, 10.41% and 12.41 % of the mass of GGBS. The compressive strength
results showed that there is an increase in compressive strength with the increase in
age of water curing and controlled curing specimens. A comparison of hot cured
specimens, the increase in compressive strength with age was less. Further heat
curing has shown to adversely affect compressive strength and to create internal
micro cracking as well as surface cracks. The higher compressive strengths were
obtained from water cured specimens.
14
TITLE: Hydration of alkali-activated slag: comparison

with ordinary Portland cement
18
AUTHOR: A. Gruskovnjak, B. Lothenbach, L. Holzer, R. Figi and F. Winnefeld

SUMMARY: They investigated and compared alkali-activated slag binders (AAS),
pure slag and ordinary Portland cement (OPC). The precipitation mechanisms during
binder hydration in the AAS and OPC systems exhibit significant differences: in AAS
the formation of the outer product CSH is much faster than in OPC. The high Si
concentrations in the pore solution during the early hydration of AAS are related to
the fast dissolution of Na-metasilicate. The fast reaction of Na is an important factor
for the voluminous precipitation of CSH within the interstitial space already during
the first
24 h. In addition to the Na-metasilicate component, the high fineness of the slag
represents a further important factor for the fast hydration of AAS. The small slag
particles (less than 2 micron) are completely dissolved or hydrated within the first 24
h, whereas hydration of the larger particles is much slower. The fast formation of a
gel-like matrix in AAS is the product of a fast through solution precipitation, which
contrasts with the slower dissolutionprecipitation mechanism of a topotactic
growth of CSH in OPC.
15
TITLE: Mineral Phase and Physical Properties of RedMud Calcined at

Different Temperatures
AUTHOR: Chuan-shengWu and Dong-yan Liu
SUMMARY: Different characterizations were carried out on red mud uncalcined and
samples calcined in the range of 100C1400C. In the present paper, the phase
composition and structural transition of red mud heated from room temperature were
indicated by XRD, TG-DTA, and SEM techniques. The mean particle diameter,
density, and bond strength of these samples also have been investigated. The results
indicate the decomposition of gibbsite into Al2O3 and H2O between 300C and 550C
and calcite into
CaO and CO2 in the interval of 600800C. Tricalcium aluminate and gehlenite are
formed in the range of 800900C. Combined with the SEM images, the results of
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physical property testing show that the particle size and the strength each has a
continuous rise during the heat treatment from 150C to 1350C. But the value of
density will undergo a little drop before 450C and then increases to a higher value at
the temperature of 1200C. These obtained results provide an important base for the
further studies of comprehensive utilization of red mud.
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TITLE: Effect of the addition of red mud on the corrosion parameters of reinforced
concrete
AUTHOR: D.V. Ribeiro, J.A. Labrincha, M.R. Morelli
SUMMARY: Red mud, the main waste generated in aluminum and alumina
production by the Bayer process, is considered hazardous due to its high pH. The
characteristic of high alkalinity associated with the presence of aluminosilicates
facilitates the assimilation and formation of compounds by reaction with chloride
ions. The high pH also provides greater protection of rebars, which is reflected in the
low corrosion potential and high electrical resistivity (filler effect) of concrete. In this
study, the chloride concentration was monitored by measuring the conductivity of the
anolyte. Red mud proved to be a promising additive for concrete to inhibit the
corrosion process. The corrosion potential was monitored by electrochemical
measurements and the electrical resistivity was evaluated using sensors embedded in
concrete test specimens. The results showed that the addition of red mud is beneficial
to concrete, reducing its chloride migration rate (diffusion coefficients) and corrosion
potential and increasing its electrical resistivity.
17
TITLE: The strength and microstructure of two geopolymers derived from

metakaolin
and red mud-fly ash admixture: A comparative study
AUTHOR: Jian He , Jianhong Zhang, Yuzhen Yu, Guoping Zhang
SUMMARY: The effects of source materials on the microstructure and mechanical
20
properties were studied by comparing two types of geopolymers synthesized from

metakaolin, a non-waste material, and the admixture of two wastes, red mud and fly
ash. Unconfined compression testing was conducted to assess their curing time and
mechanical properties, while X-ray diffraction and scanning electron microscopy
employed to examine geopolymerization reactions and the composition and
microstructure of the end products. For a given Si/Al ratio, the metakaolin-derived
geopolymer exhibits higher compressive strength than the waste-based one. Both
geopolymers contain a significant amount of voids and unreacted phases as inactive
fillers within the geopolymer binder, resulting in complexity and variability in their
mechanical behavior. The difference in strength and microstructure between the two
geopolymers is attributed to the different reactivity of source materials, percentage of
nonreactive fillers, and alkalinity for geopolymerization reactions.
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TITLE: Geopolymerization of Red Mud and Fly Ash for Civil Infrastructure
Applications
AUTHOR: Jian He and Guoping Zhang, A.M. ASCE, P.E.
SUMMARY: This paper presents a study that investigates the geopolymerization of
red mud, a major industrial waste from alumina refining, and fly ash, also an
industrial waste
from coal combustion, using very limited non-waste materials. Different synthesis
parameters (e.g., red mud to fly ash ratio, sodium silicate solution to solid mixture
(red mud and fly ash) ratio, and different types of sodium silicate solution) were
varied to assess their influences on the mechanical properties of final geopolymer
products. The results of unconfined compression testing show that these
factors have significant influence on the mechanical properties of the synthesized
geopolymers. Depending on the synthesis conditions, the unconfined compressive
strength ranges from 3 to 13MPa, and the high values are comparable with certain
types of Portland cement. The process of geopolymerization was confirmed by the
composition of the final products analyzed by X-ray diffraction. The findings suggest
21
that the two major industrial wastes, red mud and fly ash, can be reused to produce
geopolymers that may replace Portland cement and hence be applied in civil
infrastructure construction.
19
TITLE: Synthesis and characterization of red mud and rice husk ash-based
geopolymer composites
AUTHOR: Jian He , Yuxin Jie , Jianhong Zhang , Yuzhen Yu , Guoping Zhang
SUMMARY: A new type of geopolymer composite was synthesized from two
industrial wastes, red mud (RM) and rice husk ash (RHA), at varying mixing ratios of
raw materials and the resulting products characterized by mechanical compression
testing, X-ray diffraction, and scanning electron microscopy to assess their
mechanical properties, microstructure, and geopolymerization reactions. Prolonged
curing significantly increases the compressive strength and Youngs modulus, but
reduces the ductility. Higher RHA/RM ratios generally lead to higher strength,
stiffness, and ductility, but excessive RHA may cause the opposite effect. The
compressive strength ranges from 3.2 to 20.5 MPa for the synthesized geopolymers
with nominal Si/Al ratios of 1.683.35. Microstructural and compositional analyses
showed that the final products are mainly composed of amorphous geopolymer binder
with both inherited and neoformed crystalline phases as fillers, rendering the
composites very complex composition and highly variable mechanical properties.
Uncertainties in the composition, microstructure, the extent of RHA dissolution, and
side reactions may be potential barriers for the practical application of the RMRHA
based geopolymers as a construction material.
22
Chapter 3: Experimental Investigation

3.1 Manufacturing process of Alkali Activated Composite mix
Alkali activated composites prepared by mixing blast furnace slag and red mud with alkali
activator solution. The mixture is usually homogenous slurry which is dark gray to brown in
colour. The composite was cohesive in nature in fresh state. In present research, for
manufacturing of the composite, following range of different constituents were selected.
Blast furnace slag
Red Mud (Bauxite Mud)
Alkali content (%K2O)
Fine Aggregate
: 80% by weight of mix

: 20% by weight of mix
: 6% to 10% by weight of binding material
: 50% to 200% by weight of binding material
Figure 3.1: wooden cubical mould
Following manufacturing process was adopted for preparing alkali activated composite
specimens.
i.
Mix sodium silicate solution, sodium hydroxide pellets and water according to mix
proportion, to make alkaline activator, at least one day prior to its use in manufacturing
alkali activated slag.
ii.
Hand mixing was used for preparing alkali activated slag mix.
iii.
Mix slag, red mud and alkaline activator to make a homogeneous paste.
iv.
Transfer the mix to wooden/steel moulds.

23
v.
Vibrate fresh alkali activated binder mix in the moulds on vibration table for 2-3minutes
to remove entrapped air in the mix.
vi.
Rest period of 24 hours is given to fresh specimens. Remove specimens from moulds at
room temperature prior to placing them in water for water curing for 3days, 7days.
vii.
The specimens were left to air drying at room temperature until tested.
3.1.1 Characterization of ingredients for blended Alkali activated composite mortar

Blended alkali activated mortar was made from Blast furnace slag and red mud activated with a
combination of potassium hydroxide (KOH) and sodium silicate solution (Na 2SiO3) and mixed
with local sand. Blast furnace slag from Tata Metalliks, Jamshedpur, India was used for
investigation. Red Mud was obtained from Ranaghat, West Bengal. Consistency of the slag and
red mud was ensured it was procured in bulk from same batch, mixed and packed in the plastic
sealed container.
The river sand obtained from local source was used as fine aggregate for preparing mortar
specimen. Sand is having Fineness modulus of 3.2. The sand was made saturated surface dry
(SSD) before using in the mix to avoid water absorption from activator solution. The sand was
stored in plastic sealed container to maintain its properties.
Potassium hydroxide in pellets form (K2O=77.5%, H2O=22.5%) were supplied by Merck
Chemical with 97% purity. Sodium Silicate solution (Na2O=8%, SiO2=26.5%, H2O=65.5%) were
supplied by Merck Chemicals. The SiO 2-to-K2O ratio (Silicate modulus) in the alkaline
activating agent was adjusted by adding KOH to soluble glass in order to obtain required silicate
modulus. Laboratory tap water was used in the synthesis of blended alkali activated slag mortar.
3.2 Tests at fresh and hardened state
24
The main purpose of testing of alkali activated composites is to investigate the engineering
properties of the composites and to characterize microstructure of specimens, synthesized at
different test conditions. The laboratory tests will be conducted as per relevant Indian standard
codes and in some special tests, ASTM standard were followed. The details of various test
procedure use in the present research are described in the following sections.
3.2.1 Workability and Setting time measurements
Figure 3.2: Measurement of Workability using mini slump cone

The workability of fresh alkali activated composites mix may be determined using mini slump
cone as shown in the Figure above. The dimensions of the mini slump cone mould are: top
diameter 70mm, bottom diameter 100mm and height 60mm. The mould is fixed firmly on a flow
table and filled with fresh mortar. The mortar is tamped down with spatula to ensure proper
compaction. When the mould is full the top surface is leveled and it is immediately lifted
vertically allowing mortar to flow on flow table. The flow diameter is measured in two
perpendicular directions and average of the two is considered as flow diameter as a measure of
workability. Depending on flow diameter, workability of alkali activated composite mix may be
classified as stiff, moderate and high.
A Vicat needle, as shown in Fig., is used to measure the setting time of alkali activated binders.
The modified Vicat needle essentially consisted of a needle of 1 mm diameter cross-section and
25
100 g, conforming to ASTM C191-04. A cylindrical container of 75 mm diameter was filled with
50 mm of the freshly prepared pastes. Values of penetration distances were obtained every ten
minutes. The initial setting time is obtained when the penetration of needle is 25mm.
On the other hand, the final setting time is the time required to reach a penetration distance of
Figure 3.3: Measurement of setting time using Vicat apparatus

zero mm. At the final setting, alkali activated binders are almost in hardened state. Moulding
without causing material damage is not possible thereafter.
3.2.2 Bulk density and apparent porosity
The bulk density and apparent porosity for geopolymer specimen is determined according to
Archimedes principle with water as immersion medium.
The procedure to be adopted is as follows:
i> Dry all specimens in a ventilated oven at 65C for 48 hours.
ii> Record the weight of dried specimens as Wd.
iii> Immerse the specimens in water at room temperature (28C) for minimum 48 hours.
iv> Weight the specimens while suspended by a thin wire and completely submerged in water
26
and record Wi.

v> Remove specimens from water and allow water to drain off by placing them on a wire mesh,
removing visible surface water with a damp cloth; weigh and record saturated weight as Ws.
The bulk density and apparent porosity was then calculated as follow:
Dry density (Kg/m3 )
= [Wd / (Ws-Wi)] x 1000
Apparent Porosity (%)
= [(Ws-Wd) / (Ws-Wi)] x 100
3.2.3 Compressive strength

The direct compressive strength of hardened specimens will be obtained at the age of 7 days,
using 2000kN capacity digital compressive testing machine. At 7 days age, three identical
samples were tested in accordance with ASTM C-109 -02 and the mean values of compressive
strength are reported in relevant tables and graphs. Also for the specimens heated at elevated
temperature, compressive strength will be measured after the specimens attain room temperature.
A typical testing of mortar specimen is shown in Figure.
Figure 3.4 : Compressive

Strength Testing
Machine
3.2.4 Water Absorption
27
The volume of pore space in specimen matrix, as distinct from the ease with which a fluid can
penetrate it, is measured as absorption. Water absorption is usually measured by drying a
specimen to a constant mass, immersing it in water, and measuring the increase in mass as a
percentage of dry mass. In the present research, water absorption of specimens will be
determined as per ASTM C-642. The 28 days aged specimens is dried for 48 hours at 65C &
then immersed in water for 24 hours. The test specimens soaked in water is removed from the
immersion container, wiped clean and weighted immediately in saturated-surface-dry (SSD)
condition to find increase in mass.
Figure 3.5: setup for water absorption

3.2.5 Water Sorptivity
Permeability test measure the response of concrete to pressure, which is rarely the driving force
of fluid entering concrete, there is a need of another type of test. Such a test measures the rate of
absorption of water by capillary suction of unsaturated concrete placed in contact with water; no
head of water exists. The sorptivity test according to Neville A.M. determines the rate of
capillary rise absorption by mortar/ concrete cube. The specimens rest on small supports in a
manner such that only the lowest 2 to 5mm of the cube is submerged. The increase in the mass of
the prism with time is recorded. The specimens should be dried prior to the experiment.
28
It has been shown that there exists a relation of form.

I= St
where,
I = increase in mass per unit area (gm/mm 2) since beginning of the test per unit of crosssectional area in contact with water; as increase in mass is due to ingress of water. It is
expressed in mm.
t = time, measured in minutes, at which the mass is determined.
S = Sorptivity in mm/min0.5
The detail of experimental set up is shown in figure below.
Figure 3.6: setup for sorptivity
3.2.6 Ultrasonic Pulse Velocity (UPV)

Ultrasonic Pulse Velocity method consists of measuring the time of travel of an ultrasonic pulse,
passing through the mortar/ concrete. The mortar cube specimens having dimension 50mm
50mm 50mm will be used in this study. Typical test setup for ultrasonic testing is shown in
Figure. Direct transmission of pulse is employed for the study. Although the pulse velocity is
affected by a number of factors, the most important parameter is the porosity of mix. The
ultrasonic pulse velocity measurement was conducted as per IS 13311 (Part-1): 1992 standard
29
using a commercially available PUNDIT system. The testing system consisted of a pulsar/receiver
unit with a built-in data acquisition system and a pair of narrow band, 150-kHz transducers. UPV
measurements could be performed to monitor the internal structure of mortar nondestructively.
The test procedure is as follows: Ultrasonic pulse is produced by the transducer which is held in
contact with the surface of the specimen. The transit time (T) of the pulse is measured for path
length (L).
The Pulse Velocity (V) is given by: V = L /T
Figure 3.7: Setup for Ultrasonic Pulse Velocity
30
3.3. Detail of Mixes

Following table summarized the different mixes that were tried during the experiment with Alkali
activated blended slag mortar. Main features are:i) % of K2O is varied between 6%, 8%, 10%.
ii) SiO2/K2O is kept constant.
iii) Binding material/Sand is varied between 1:2 to 2:1.
iv) Elevated temperature range was varied between 300,500,700C.
Type
Mortar
Mortar
Mortar
Mortar
Mortar
Mortar
Mortar
Mortar
Mortar
TABLE 3.1 : DETAILS OF MIXES

SiO2/
%K2O
K2O
Binding
Material/ Sand
1:2
1:1
2:1
1:2
1:1
2:1
10
1:2
10
1:1
10
2:1
31
3.4. Detail of Experimental Programme:
TABLE 3.2 : OBJECTIVE OF THE EXPERIMENTAL PROGRAMME

Sl.
Test method
Property
No.
1
Workability
and setting time
Specimen
Number of
type
specimen
Flow characteristic of
Fresh alkali
paste/mortar
activated
Objective
To determine
the flow ability
composite
paste/mortar
2
Compressive
Compressive strength
strength test
of alkali activated
Cube
(50mm*50mm
the
*50mm)
composite.
To determine
compressive
strength of the
hardened
paste/mortar
Sorptivity test
To appreciate the
tendency of
unidirectional flow
Cube
(50mm*50mm
To appreciate
the tendency of
*50mm)
unidirectional
through the test
flow through
specimen
the test
specimen.
Water
Porosity of alkali
absorption test
activated composite
Cube
(50mm*50mm
porosity of the
*50mm)
5
Apparent
Porosity of alkali
porosity
activated composites
Cube
(50mm*50mm
material
3
Ultrasonic
Compactness of the
Pulse Velocity
material.
Cube
(50mm*50mm
*50mm)
(UPV)
To appreciate
the porosity
*50mm)
6
To measure the
level.
3
To appreciate
the density,
void, insipient
flaws, and
strength.
4. Results and discussion

32
4.1 Preamble
Mortar can function in two ways. Firstly, it should provide a uniform bedding surface for the
units. This is ensured when plastic mortar has reasonable workability so that it can be spread
easily under the influence of the trowel and it flows into all the crevices of the units, thus
correcting any dimensional irregularities. Secondly the mortar binds the units into monolithic
mass. The hardened mortar must possess sufficient strength to hold the units together and ensure
adequate durability to resist the destructive forces of the weather. The strength to sustain loads in
a masonry wall is provided by the units; the mortar is merely the "glue" that holds them together.
Thus any approach to mortar technology requires an understanding of the workability of plastic
mortar and strength of hardened mortar.
Initially (Blast furnace slag + Red Mud) with percentage composition of 80, 20 respectively was
found to be the best paste mix from compressive strength consideration.
The following table shows the detail mixes of alkali activated paste samples.
Table 4.1: Detail Mixes Of Alkali Activated Paste Samples
Sample
ID
Composition (in
%)
BF
Red Mud
S
GP 1
100
GP A
20
80
GP B
40
60
GP C
50
50
GP D
60
40
GP E
70
30
Activato
r Soln.
6%
KOH
6%
KOH
6%
KOH
6%
KOH
6%
KOH
6%
KOH
Silicate
Modulu
s
Water:
Binding
Materia
l
Curing
Condition
Compressive Strength
(in Mpa)
0.27
Water
51.48
0.26
Water
46.8
0.27
Water
26.4
0.28
Water
17.6
0.3
Water
7.2
0.3
Water
6.4
The compressive strength results are plotted and shown in Figure 4.

33
60
50
51.48
46.8
40
26.4
30
17.6
7.25 6.46
G
P
G
P
G
P
G
P
10
G
P
20
G
P
Compressive Strength (in MPa)
Sample ID
Figure 4: Compressive Strength vs percentage composition of binding material
Mortar cubes were casted with varying alkali content (6%,8%,10%) using GGBFS:RM = 80% :
20% and source material : sand was varied as given below
Source material : Sand
1 :
1
2 :
1
1 :
2
Mortar cubes were then exposed to elevated temperature of 300C, 500C and 700C. The
samples were then studied on the effect of synthesizing parameters such as Alkali content,
binding material to sand ratio, temperature level on the physico-mechanical properties of
blended AAS composites, that is, compressive strength, bulk density, water absorption, apparent
porosity, UPV and water sorptivity. The following figures show the results obtained.
4.2 Effect of alkali concentration on compressive strength
34
Compressive Strength vs Alkali Concentration

( (BFS+RED MUD) : Sand = 1:1, Normal Water Curing)
45
40
35
30
25
Compressive Strength (in MPa) 20
15
10
5
0
41.6
31.28
12.92
10
Alkali Concentration (in %)
Figure 4.1: Compressive Strength vs Alkali Concentration


50
45
40
35
30
25
20
15
10
5
0
43.88
22.24
10.2
10

35

10
9.36
8
6
4
2
0
6
10


( BM:Sand = 1:1 , Temperature = 300C)
20
17.84
13.8
15
8.56
10
5
0
6
10

36

12
10
10
4
2
0
6
10


7
6

2
1
0
6
10

37

40
35
30
25
20
15
10
5
0
34.56
12.4
8.16
10


14
12
12
10
8
6
4
2
0
6
10

38

8
7
6
5
4
3
2
1
0
3
2
10


10
8
8
6.54
6
5.8
4
2
0
6
10

39

7
5
4
2
1
0
6
10


3.5
3
2.5
1.8
Compressive Strength (in MPa) 1.5

1
0.5
0
6
10

40
4.2.1 Effect of binding material to sand ratio on compressive strength
Compressive Strength vs BM:Sand

( Alkali concentration= 6% , Normal Water Curing)
50
41.6
43.88
40
30
9.36
10
0
1:1
2:1
1:2
Binding Material : Sand
Figure 4.13: Compressive Strength vs BM:Sand


35
31.28
30
22.24
25
20
10
5
0
1:1
2:1
1:2

41

14
12.92
12
10.2
10
8
6
4
2
0
1:1
2:1
1:2

4.2.2 Effect of elevated temperature on compressive strength
Compressive Strength vs Elevated Temperature

( Alkali concentration= 6% , BM:Sand = 1:1 )
20
17.84
15
10
10
6
5
0
300
500
700
Temperature Level (in C)
Figure 4.16: Compressive Strength vs Elevated Temperature

42

16
14
12
10
8
6
4
2
0
13.8
7
4
300
500
700

( Alkali concentration= 8% , BM:Sand = 1:1)

( Alkali concentration= 10 % , BM:Sand = 1:1 )
10
8.56
8
6
6
2
0
300
500
700

43

40
35
30
25
20
15
10
5
0
34.56
12
7
300
500
700


14
12.4
12
10
8
6
3
4
2
0
300
500
700

44

10
8
8.16
7
6
4
2
2
0
300
500
700

( Alkali concentration= 10 % , BM:Sand = 2:1)

10
8
8
6
6
2
0
300
500
700

45

7
6.54
6
5
4
2
1
0
300
500
700


7
6
5.8
5
4
3
1.8
2
1
0
300
500
700

46
4.3 Effect of alkali concentration on water absorption
Wate r Absorption vs Alkali Conce ntration

( BM:Sand = 1:1 , Normal wate r curing)
16.84
18.00
16.00
14.00
12.00
10.00
8.00
Water Absorption ( in % )
6.00
4.00
2.00
0.00
10.85
9.61
10
Alkali Concentration (in % )
Figure 4.25: Water Absorption vs Alkali Concentration

( BM:Sand = 1:1 , Normal water curing)
Water Absorption vs Alkali Concentration

16.00
14.59
14.00
12.00
9.46
10.00
Water Absorption ( in %)
7.50
8.00
6.00
4.00
2.00
0.00
47
10


16.00
13.75
14.00
12.00
9.35
10.00
7.78
8.00
6.00
4.00
2.00
0.00
10


( BM:Sand = 1:1 , ElevatedTemperature = 300C)
20.00
18.54
15.00
11.87
10.00
10.13
5.00
0.00
6
48
10


25.00
19.32
20.00
15.00
11.65
12.80
10.00
5.00
0.00
6
10

( BM:Sand = 1:1 , Elevated Temperature = 500C)

25.00
19.29
20.00
15.00
14.86
15.78
10.00
5.00
0.00
49
10


18.00
16.00
14.00
12.00
10.00
8.00
6.00
4.00
2.00
0.00
16.53
11.01
11.26
10


18.00
16.84
17.00
15.63
16.00
15.00
14.13
14.00
13.00
12.00
6
50
10


20.00
17.69
15.34
15.00
18.69
10.00
5.00
0.00
6
10


18.00
16.00
14.00
12.00
10.00
8.00
6.00
4.00
2.00
0.00
15.38
11.98
9.36
51
10

( BM:Sand = 1:2 , Elevated Temperature = 300C

18.00
16.00
14.00
12.00
10.00
8.00
6.00
4.00
2.00
0.00
16.10
12.88
9.93

52
10

20.00
17.77
14.84
15.00
11.15
10.00
5.00
0.00
6
10

4.3.1 Effect of elevated temperature on water absorption

Water Absorption vs Temperature Level
( Alkali Concentration = 8% , BM : Sand = 1:1)
18.00
16.00
14.00
12.00
10.00
8.00
6.00
4.00
2.00
0.00
15.78
12.80
10.13
300
500
Figure 4.37: Water Absorption vs Temperature Level

53
700
( Alkali Concentration = 8% , BM : Sand = 1:1)

( Alkali Concentration = 10 % , BM : Sand = 1:1)
19.40
19.32
19.29
500
700
19.20
19.00
18.80
18.54
18.60
18.40
18.20
18.00
300


18.00
16.00
14.00
12.00
10.00
8.00
6.00
4.00
2.00
0.00
14.13
15.34
11.01
300
500

54
700

20.00
18.00
16.00
14.00
12.00
10.00
8.00
6.00
4.00
2.00
0.00
17.69
15.63
11.26
300
500
700

19.00
18.69
18.50
18.00
17.50
17.00
16.53
16.50
16.84
16.00
15.50
15.00
300
500

55
700

11.50
11.15
11.00
10.50
9.93
10.00
9.36
9.50
9.00
8.50
8.00
300
500
700


16.00
14.84
14.00
11.98
12.00
12.88
10.00
8.00
6.00
4.00
2.00
0.00
300
500
56
700


17.77
18.00
17.50
17.00
16.50
16.10
16.00
15.38
15.50
15.00
14.50
14.00
300
500

4.4 Effect of alkali concentration on apparent porosity
57
700
Alkali concentration vs Apparent Porosity

( BM : Sand = 1:1, Normal water curing)
35
29.35
30
25
20.8
20
Apparent Porosity ( in %)
18.76
15
10
5
0
6
10
Alkali concentration ( in %)
Figure 4.45: Alkali concentration vs Apparent Porosity


30
25
25
18.1
20
15.22
15
10
5
0
10

58

30
25.05
25
20
15.98
18.42
15
10
5
0
6
10


( BM : Sand = 1:1, Elevated Temperature = 300C)
35
31.38
30
25
22.94
19.84
20
15
10
5
0
6

59
10

35
31.87
30
25
21.88
23.51
20
15
10
5
0
6
10


32.84
35
30
27.2
28.2
25
20
15
10
5
0

60
10

30
25
27.42
21.84
21.44
20
15
10
5
0
10


30
28.9
29
28
27.02
27
26
25.87
25
24
6

61
10

31
30.68
30.5
30
29.4
29.5
28.87
29
28.5
28
27.5
10


30
27.03
23.28
25
20
18.42
15
10
5
0
6

62
10

35
29.05
30
24.12
25
20
19.15
15
10
5
0
6
10


35
30.5
30
25
26
20.98
20
15
10
5
0
6

63
10
4.4.1 Effect of elevated temperature on apparent porosity
Apparent Porosity vs Temperature Level

(Alkali Concentration = 6%, BM : Sand = 1:1)
30
25
27.2
22.94
21.88
300
500
20
15
10
5
0
700
Temperature Level (C)
Figure 4.57: Apparent Porosity vs Temperature Level


28.2
30
23.51
25
20
19.84
15
10
5
0
300
500
64
700


32.84
33
32.5
31.87
32
31.38
31.5
31
30.5
300
500

(Alkali Concentration = 10%, BM: Sand = 1:1)
65
700

(Alkali Concentration = 6% ,BM : Sand = 2:1)
35
30
25
25.87
28.87
21.84
20
15
10
5
0
300
500
700

35
30
25
27.02
29.4
21.44
20
15
10
5
0
300
500

66
700

30.68
31
30
28.9
29
28
27.42
27
26
25
300
500
700

21.5
21
20.5
20
19.5
19
18.5
18
17.5
17
20.98
19.15
18.42
300
500

67
700

26.5
26
25.5
25
24.5
24
23.5
23
22.5
22
21.5
26
24.12
23.28
300
500
700


31
30.5
30
29.05
29
28
27
27.03
26
25
300
500

68
700
4.5 Effect of alkali concentration on UPV

The ultrasonic pulse velocity method has been used to study the homogeneity and quality
grading of internal structure of Geopolymer composites. UPV is mainly related to its density and
modulus of elasticity. The following figures show the effect of alkali content, binding material to
sand ratio and elevated temperature on UPV of blended alkali activated slag mortar specimen.
69
UPV vs Alkali content

(BM : Sand = 1:1, Normal water curing)
4
3.64
3.38
3.5
2.73
3
2.5
UPV (Km/sec)
2
1.5
1
0.5
0
6
10
Alkali content (%)
Figure 4.66: UPV vs Alkali content

(BM: Sand = 1:1, Normal water curing)
4
3.73
3.25
3.5
3
2.5
2.5
UPV (Km/sec)
2
1.5
1
0.5
0
6
8
Alkali content (%)

(BM: Sand = 2:1, Normal water curing)
70
10

3.5
3
2.5
2.56
2.48
10
2
UPV (Km/sec)
1.5
1
0.5
0
6
Alkali content (%)

(BM : Sand = 1:1, Temperature level=300C)
3.5
3
2.99
2.74
2.5
2.45
2
UPV (Km/sec)
1.5
1
0.5
0
6
8
Alkali content (%)

(BM : Sand = 1:1, Temperature level=300C)
71
10

(BM : Sand =2:1, Temperature level=300C)
3.5
3.24
2.84
3
2.5
2.22
2
UPV (Km/sec)
1.5
1
0.5
0
6
10
Alkali content (%)


2.6
2.5
2.48
2.4
2.3
UPV (Km/sec)
2.2
2.12
2.1
2.08
2
1.9
1.8
6
8
Alkali content (%)

72
10

3
2.72
2.62
2.5
2.25
2
UPV (Km/sec)
1.5
1
0.5
0
6
10
Alkali content (%)

3
2.66
2.45
2.5
2
UPV (Km/sec)
2.01
1.5
1
1
0.5
0
6
8
Alkali content (%)

73
10

2.5
2.2
1.98
1.74
1.5
UPV (Km/sec)
1
0.5
0
6
10
Alkali content (%)

2.5
2
1.96
1.84
1.63
1.5
UPV (Km/sec)
1
0.5
0
6
8
Alkali content (%)
Figure 4.75 : UPV vs Alkali content

74
10

UPV (Km/sec)
1.75
1.7
1.65
1.6
1.55
1.5
1.45
1.4
1.35
1.3
1.25
1.7
1.6
1.42
10
Alkali content (%)

1.6
1.4
1.36
1.24
1.2
1.08
1
UPV (Km/sec)
0.8
0.6
0.4
0.2
0
6
8
Alkali content (%)

75
10
4.5.1 Effect of elevated temperature on UPV
UPV vs Temperature Level

(Alkali content=6%, BM:Sand=1:1)
3.5
3
2.5
2.99
2.72
1.96
UPV (Km/sec) 1.5

1
0.5
0
300
500
700
Temperature level (in C)
Figure 4.78: UPV vs Temperature Level


3
2.5
2.74
2.62
2
UPV (Km/sec)
1.84
1.5
1
0.5
0
300
500

76
700

3
2.5
2
UPV (Km/sec)
2.45
2.25
1.5
1.63
1
0.5
0
300
500
700

(Alkali content=10%, BM:Sand=1:1
3.5
3
3.24
2.5
2.66
2
UPV (Km/sec) 1.5
1.7
1
0.5
0
300
500

77
700

3
2.5
2.84
2.45
2
UPV (Km/sec)
1.5
1.6
1
0.5
0
300
500
700


2.5
2
2.22
2.01
1.5
UPV (Km/sec)
1.42
1
0.5
0
300
500

78
700

3
2.5
2
UPV (Km/sec)
2.48
2.2
1.5
1.36
1
0.5
0
300
500
700


2.5
2
2.12
1.98
1.5
UPV (Km/sec)
1.24
1
0.5
0
300
500

79
700

2.5
2
2.08
1.74
1.5
UPV (Km/sec)
1.08
0.5
0
300
500
700

4.6 Effect of alkali concentration on Sorptivity
Sorptivity vs Alkali content

(BM:Sand =1:1)
0
0
0
Sorptivity (gm/mm2/min0.5 ) 0
0
0
6
Alakli content (%)
Figure 4.87: Sorptivity vs Alkali content

80
10
(BM:Sand =1:1)

(BM:Sand =1:1)
0
0
0
0
0
0
0
6
10
Alakli content (%)

(BM:Sand =1:1)

(BM:Sand =1:1)
0
0
0
Sorptivity (gm/mm2/min0.5 )
0
0
0
0
0
6
Alakli content (%)

(BM:Sand =1:1)
81
10
4.6.1 Effect of elevated temperature on Sorptivity
Sorptivity vs Temperature level

0
0
0
0
0
0
0
300
500
700
Temperature level (C)
Figure 4.90: Sorptivity vs Temperature level


0
0
0
0
0
0
0
0
0
500
700
300

82

0
0
0
0
0
0
0
0
300
500
700


0
0
0
0
0
0
0
300
500
700
83


0
0
0
0
0
0
0
300
500
700


0
0
0
0
0
0
0
0
0
0
0
300
500
700
84

5. Concluding remarks
Currently, hydrated Ordinary Portland Cement (OPC) is the most common binder used in
concrete. The production of OPC requires large amounts of energy, emitting approximately 5%
of global CO2 emissions annually. Alkali activated slag (AAS) composites is a relatively new
material, with the potential to be an alternative to OPC. Blended AAS composites have a lower
environmental impact. This research will facilitate the implementation and wider use of blended
AAS mortar as a potential new building material and provide a foundation for future explorations
into Geopolymer composites. Based on the results of the experimental study on engineering
properties of Blended Alkali Activated Composited mortar, the following conclusions are made.
85
The preparation of AAS mortar has been accomplished by mixing of alluminosilicate source
material such as blast furnace slag, red mud with an activating solution that contains alkalinity
and soluble silicates. Potassium Hydroxide was used as alkaline solution successfully with
supplemented by Sodium Silicate as soluble silicates.
Chemistry of the source material (here Blast Furnace Slag) and supplementary material used is
red mud and activating solution affect the success of alkali activated composite. The parameters
such SiO2/K2O in the activator solution, percentage of K 2O in the composite matrix affect the
property of composite product developed.
The process of curing and hardening is different for AAS mortar compare to cement composites.
Slag based alkali activated composite gains strength with duration of water curing. Curing
duration has been found to affect the development of strength and the pore structure. Hence,
Water Sorptivity, Water absorption, Apparent porosity and density depends greatly on curing
condition. Duration of water curing is an important parameter.
Addition of water for proper mixing of mortar and addition of filler material like sand, affect the
workability and strength development of AAS mortar. Proportion of sand in excess of binding
material is responsible for reduction in the compressive strength and also increase in porosity,
water absorption. Thus ultimately affect the durability of blended AAS mortar. Use of more sand
in comparison to binding material (slag, red mud) is also uneconomical as sand is natural
resource which is depleting day by day and slag,red mud are byproduct/ waste material creating
environmental problems. Addition of water should be optimised to get a workable mixture of
reasonably good strength. Hence, the parameters water/binding material ratio, BM/sand ratio can
be suitably adjusted to get blended alkali activated composite mortar of desired specification.
AAS blended with Red mud has significantly lower resistance to elevated temperature due to its
volume expansion and cracking. This is due to the presence of Titanium dioxide in the chemical
composition of red mud.
86
Blended AAS material is not a wonder material. It needs to be specifically tailored to be able to
handle itself in certain situations, just like ordinary cement based composites. There are some
areas where future research is needed to appreciate alkali activated material in a better way
which will establish itself as a cost effective as well as more reliable material in extreme
environments compare to a cement based composites. The following areas may be considered for
future research.
1. Detail study on durability of blended slag based alkali activated composite ie. may be exposed
to acid, sulphate , chloride environment etc.
2. Effect of synthesizing parameters on shrinkage.
3. More study on the properties of blended AAS mortar produced by changing silicate modulus,
curing methods.
4. Detail study is needed to improve porosity of AAS mortar.
Reference
[1] Joseph Davidovits, Property of geopolymer cements. Geopolymer Institute 02100Saintquintin ,France.Iinternational Conference on Geopolymer cement and concrete Kiev Ukraine in
1994
[2] Somnath Ghosh, Ravindra N.Thakur Effect of Mix Composition on Compressive Strength &
Microstructure of Fly Ash Based Geopolymer Composites. ARPN Journal of Engineering &
Applied Sciences. Vol 4, No. 4 June 2009.
87
[3] Debabrata Dutta, Suresh Thokchom, Partha Ghosh and Somnath Ghosh, Effect Of Silica
Fume Additions On Porosity Of Fly Ash Geopolymers, ARPN Journal of Engineering and
Applied Sciences OCTOBER 2010 ISSN 1819-6608
[4] V. Supraja, M. Kanta Rao Experimental study on Geo-Polymer concrete incorporating GGBS
International Journal of Electronics, Communication & Soft Computing Science and
Engineering, ISSN: 2277-9477, Volume 2, Issue 2
[5] Monita Olivia and Hamid R. Nikraz, Strength and water penetrability of fly ash Geopolymer
concrete, ARPN Journal of Engineering and Applied Sciences, VOL. 6, NO. 7, JULY 2011.
[6] Hardjito & Fung- Parametric Study on the Properties of Geopolymer Mortar Incorporating
Bottom Ash ,Concrete Research Letters Vol. 1(3) 2010
[7] Muhd Fadhil Nuruddin, Andri Kusbiantoro, Sobia Qazi, Nasir Shafiq; Compressive Strength
and Interfacial Transition Zone Characteristic of Geopolymer Concrete with Different Cast InSitu Curing Conditions , World Academy of Science, Engineering and Technology 49 2011.
[8] Hu Mingyu, Zhu Xiaomin, Long Fumei Alkali-activated fly ash-based geopolymers with
zeolite or bentonite as additives,Cement and Concrete Composites, Volume 31, Issue 10
(November,2009),p.762-768. ISSN: 0958-9465 Elsevier Science
[9] Zongjin Li and Sifeng Li, Influence of Slag as additive on the compressive strength of Fly
Ash based Geopolymers, February 2012, ISSN 0899-1561, American Society Of Civil
Engineers.
[10] Cheng and Chiu. Fire-resistant Geopolymer produced by granulated blast furnace slag, by
(Minerals Engineering 16 (2003) 205210)
[11] Suresh Thokchom,Debabrata Dutta, Somnath Ghosh, Effect of Incorporating Silica Fume in
Fly Ash Geopolymers, by World Academy of Science, Engineering and Technology 60 2011
88
[12] Debabrata Dutta, Suman Chakrabarty, Chandan Bose, Somnath Ghosh Evaluation
Geopolymer properties with temperature imposed on activator prior mixing with fly
ash.,International Journal Of Civil And Structural Engineering Volume 3, No 1, 2012
[13] Mohd. Nadeem Qureshi , Somnath Ghosh, Effect of Curing Conditions on the Compressive
Strength and Microstructure of Alkali-activated GGBS paste; International Journal of
Engineering Science Invention ISSN (Online): 2319 6734, ISSN (Print): 2319 6726.
[14] A. Gruskovnjak, B. Lothenbach, L. Holzer, R. Figi and F. Winnefeld, Hydration of alkaliactivated slag: comparison with ordinary Portland cement; Advances in Cement Research, 2006,
18, No. 3, July, 119128
[15] Chuan-shengWu and Dong-yan Liu, Mineral Phase and Physical Properties of Red Mud
Calcined at Different Temperatures; Hindawi Publishing Corporation, Journal of Nanomaterials,
Volume 2012, Article ID 628592, 6 pages, doi:10.1155/2012/628592
[16] .V. Ribeiro, J.A. Labrincha, M.R. Morelli, Effect of the addition of red mud on the corrosion
parameters of reinforced concrete; Cement and Concrete Research 42 (2012) 124133,Elsevier.
[17] Jian He , Jianhong Zhang, Yuzhen Yu, Guoping Zhang, The strength and microstructure of
two geopolymers derived from metakaolin and red mud-fly ash admixture: A comparative study;
Construction and Building Materials 30 (2012) 8091,Elsevier.
[18] He and Guoping Zhang, A.M. ASCE, P.E., Geopolymerization of Red Mud and Fly Ash for
Civil Infrastructure Applications, Geo-Frontiers 2011 ASCE 2011
[19] Jian He , Yuxin Jie , Jianhong Zhang , Yuzhen Yu , Guoping Zhang, Synthesis and
characterization of red mud and rice husk ash-based geopolymer composites; Cement &
Concrete Composites 37 (2013) 108118,Elsevier
[20] J. Davidovits , Geopolymer , Man-made Rock Geosynthesis and the Resulting
Devolopment of Very Early High Strength Cement, Journal of Materials Education, 16 [2-3] 91137(1994).
[21] D. Hardjito and B. V. Rangan . (2005) Development and properties of low-calcium fly
89
ash based geopolymer concrete , Research Report GC , Faculty of Engineering , Curtin

University of Technology, Perth, Australia , 1-130 .
[22] Thokchom Suresh , Ghosh Partha , Ghosh Somnath 2009 Effect of Water Absorption ,
Porosity and Sorptivity on Durability of Geopolymer Mortars ARPN Journal of Engineering
and Applied Sciences , vol 4 , no. 7 , Sep 2009 .
[23] Neville, A. M. and Brooks, J, 1990, Concrete Technology, Essex, Longman
Group,UK
[24] Prof. Dr. Joseph Davidovits Geopolymer Institute, 30 years of successes and failures in
Geopolymer Applications. Market trends and potential breakthroughs. Geopolymer 2002
Conference, October 28-29,2002, Melbourne, Australia.
Appendix-I - Calculation regarding alkali activated GGBFS-RM mix

Calculation for different ingredients needed for producing blended alkali activated slag
mortar of specified parameters:
Parameters
% of K2O=8
SiO2/K2O in activator solution=1
Water/Binding Material (BFS+Red Mud) =0.37
BM: Sand=1:1
Assume Quantity of binding material=1000gm
Therefore quantity of K2O @ 8% of BM=80gm
Therefore quantity of SiO2 using above mentioned ratio=80gm
90
1000gm Sodium Silicate contains 265gm of SiO2, 80gm of Na2O and 655gm of water.
Therefore to get 80gm of SiO2 in activator solution
Quantity of Sodium Silicate needed=301.89gm
This amount of Sodium Silicate contains quantity of Na2O=24.15gm and water=197.74gm
Therefore rest of K2O= 80gm which was obtained from Potassium Hydroxide (KOH) solution.
1000gm Potassium Hydroxide in pellets form contains 839.29gm of K2O and 160.71gm of water.
Therefore to get 80gm K2O in activator solution
Quantity of Potassium Hydroxide needed=95.32 gm
Quantity of water present in 95.32 gm of Potassium Hydroxide in pellets form=15.32gm
Therefore Water from these chemicals = (197.74gm+15.32gm) =213.06gm
To produce a alkali activated slag based mortar specimen of Water/Fly ash=0.35, total water
needed= 350 gm
Extra water that was added= (350gm-213.06gm) =136.94gm
As in the level of the product KOH pellets is 84% pure. Considering these
Quantity of KOH required=110.57 gm.
Keeping the above mentioned parameter Sand required=1000gm.
91

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1.

1.2. Geopolymer terminology and chemistry

The chemical reaction may comprise the following steps :

(i) Poly (sialate), which has [-Si-O-Al-O-] as the repeating unit.

Poly (sialate-disiloxo), which has [-Si-O-Al-O-Si-O-SiO-]

Figure 1 : Possible chemical

Figure 2 : Basic forms of Geopolymer according to Davidovits.

1.3. Historical development of Geopolymers

Milestones in alumino-silicate chemistry

1.4. Alkali-activation of cementitious materials

Figure 3 : Schematic representation of the

Figure 4: Application of Geopolymer.

One of the potential fields of application of geopolymeric materials is in toxic waste

1.6. Objective of the Present Research

1.7. Organization of the thesis

Chapter 2: Review of Existing Literature

TITLE: Property of geopolymer cements

AUTHOR: Joseph Davidovits

SUMMARY: Geopolymer cement hardens rapidly at room temperature and provides

TITLE: Effect of mix composition on compressive strength and microstructure of fly

AUTHOR: Prof. Dr. Somnath Ghosh & Ravindra N Thakur

important role during dissolution, polycondensation & hardening stages of

TITLE: Effect of silica fume additions on porosity of fly ash geopolymers

TITLE: Experimental study on Geo-Polymer concrete incorporating GGBS

AUTHOR: V. Supraja, M. Kanta Rao

TITLE: Strength and Water Penetrability of Fly Ash Geopolymer Concrete

TITLE: Parametric Study on the Properties of Geopolymer Mortar Incorporating

TITLE: Compressive Strength and Interfacial Transition Zone Characteristic of

Geopolymer Concrete with Different Cast In-Situ Curing Conditions

TITLE: Alkali-activated fly ash-based geopolymers with zeolite or bentonite as

AUTHOR: Zongjin Li and Sifeng Liu

TITLE: Fire-resistant geopolymer produced by granulated blast furnace slag

TITLE: Effect of Incorporating Silica Fume in Fly Ash Geopolymers

TITLE: Evaluation of Geopolymer properties with temperature imposed on

TITLE: Effect of Curing Conditions on the Compressive Strength and

TITLE: Hydration of alkali-activated slag: comparison

AUTHOR: A. Gruskovnjak, B. Lothenbach, L. Holzer, R. Figi and F. Winnefeld

TITLE: Mineral Phase and Physical Properties of RedMud Calcined at

TITLE: The strength and microstructure of two geopolymers derived from

properties were studied by comparing two types of geopolymers synthesized from

Chapter 3: Experimental Investigation

: 80% by weight of mix

Figure 3.1: wooden cubical mould

Transfer the mix to wooden/steel moulds.

3.1.1 Characterization of ingredients for blended Alkali activated composite mortar

3.2 Tests at fresh and hardened state

Figure 3.2: Measurement of Workability using mini slump cone

Figure 3.3: Measurement of setting time using Vicat apparatus

and record Wi.

Dry density (Kg/m3 )

= [Wd / (Ws-Wi)] x 1000

Apparent Porosity (%)

= [(Ws-Wd) / (Ws-Wi)] x 100

3.2.3 Compressive strength

Figure 3.4 : Compressive

3.2.4 Water Absorption

Figure 3.5: setup for water absorption

It has been shown that there exists a relation of form.

Figure 3.6: setup for sorptivity

3.2.6 Ultrasonic Pulse Velocity (UPV)

Figure 3.7: Setup for Ultrasonic Pulse Velocity

3.3. Detail of Mixes

TABLE 3.1 : DETAILS OF MIXES