CHAPTER 1

INTRODUCTION
1.1 General

Concrete is one of the most widely used construction materials; it is

usually associated with Portland cement as the main component for making
concrete. The demand for concrete as a construction material is on the increase. It
is estimated that the production of cement will increase from about from 1.5
billion tons in 1995 to 2.2 billion tons in 2010 (Malhotra, 1999).

On the other hand, the climate change due to global warming, one of the
greatest environmental issues has become a major concern during the last decade.
The global warming is caused by the emission of Co 2 greenhouse gases,
such as Co2, to the atmosphere by human activities. Among the greenhouse
gases, Co2 contributes about 65% of global warming (McCaffrey, 2002). The
cement industry is responsible for about 6% of all Co2 emissions , because the
production of one tonne of Portland cement emits approximately one tonne of Co2
into the atmosphere (Davidovits, 1994; McCaffrey, 2002).

Although the use of Portland cement is still unavoidable until the

foreseeable future, many efforts are being made in order to reduce the use of
Portland cement in concrete. These efforts include the utilization of
supplementary cementing materials such as fly ash, silica fume, granulated
blast furnace slag, rice-husk ash and metakaolin, and finding alternative
binders to Portland cement.

Inspired by the geopolymer technology and the fact that fly ash is a waste

1
material abundantly available, in 2001, the geopolymer Concrete Research
Group at Curtin University of Technology commenced a comprehensive research
programme on ‘Study on Fly Ash-Based Geopolymer Concrete’. The
first part of this research studied the development of mixture proportions, the
manufacture of fly ash-based geopolymer concrete, the effect of main
parameters on the short-term engineering properties of fresh and hardened
concrete (Djwantoro and Rangan 2005).

The motivation for using fly ash as the main raw material is driven by
various factors:

(1) It is cheap and available in bulk quantities

(2) It is currently under-utilized except for its use as an additive in OPC

(3) It has high workability and

(4) It requires less water (or solution) for activation.

1.2 Need for the present study

It is evident from the present scenario that ordinary Portland cement is causing
much of the environmental hazards such as-

 Increasing green house gases.

 Enormous consumption of power for the manufacture of cement.
 Economic point of view.

So considering all above points there is a need to find some alternative

material. Any material which contains silicon and aluminum in amorphous state
can be a source of binding material, and Fly ash which contains this is considered
2
to be a waste product which can be utilized effectively to overcome the effects
caused by Ordinary Portland Cement.

Long term application of any material can be taken up only when it is tested
for the drastic conditions, and one among the severe or extreme case is susceptible
to fire. When geopolymer concrete is subjected to high temperatures as in a fire,
there is likely deterioration in its properties. Of particular importance are loss in
compressive strength, loss of elastic modulus, cracking and spalling of the
concrete. To ascertain whether a structure can be repaired rather than demolished
after a fire, an assessment of structural integrity must be made. Assessment of fire
damaged concrete usually starts with visual observation of colour change, crazing,
cracking, and spalling. So there exists a need to find the fire resistance of the Fly
ash based geopolymer concrete.

1.3 Objective of the study

The objective of the present investigation is, to study the performance
characteristics of the source materials

1) To study the flexural and compressive strength of geopolymer concrete.

2) To study the durability properties of geopolymer concrete.
3) To study the chemical composition of fly ash obtained from Thermal power
station, Neyveli Lignite Corporation Limited.

3
 CHAPTER 2

LITERATURE REVIEW
2.1 Introduction

This Chapter presents a brief review of the terminology and

chemistry of Geopolymers, and past studies on Geopolymers. Additional
review of Geopolymer technology is available elsewhere (Hardjito and Rangan,
2005).

2.2 Geopolymers

2.2.1 Terminology and Chemistry

The term ‘Geopolymer’ was first introduced by Davidovits in 1978 to

describe a family of mineral binders with chemical composition similar to
zeolites but with an amorphous microstructure. He also suggested the use of the
term ‘poly(sialate)’ for the chemical designation of Geopolymers based on
silico-aluminate (Davidovits,1988a, 1988b, 1991; van Jaarsveld et. al., 2002a);
Sialate is an abbreviation for silicon-oxo-aluminate.

Poly(sialates) are chain and ring polymers with Si4+ and Al3+ in IV-fold
coordination with oxygen and range from amorphous to semi-crystalline
with the empirical formula:

M n (-(SiO2) z –AlO2) n . wH 2 O (2-1)

where “z” is 1, 2 or 3 or higher up to 32; M is a monovalent cation

4
such as potassium or sodium, and “n” is a degree of polycondensation
(Davidovits, 1984, 1988b, 1994b,1999). Davidovits (1988b; 1991; 1994b; 1999)
has also distinguished 3 types of polysialates, namely the Poly (sialate) type
(-Si-O-Al-O), the Poly(sialate-siloxo) type (-Si-O-Al-O-Si-O) and the Poly
(sialate-disiloxo) type (-Si-O-Al-O-Si-O). The structures of these polysialates
can be schematized as in Figure 2.1.

Fig. 2.1 Chemical Structures of Polysialates

Geopolymerization involves the chemical reaction of alumino-silicate oxides

(Si2O5, Al2O2) with alkali polysilicates yielding polymeric Si – O – Al bonds.
Polysilicates are generally sodium or potassium silicate supplied by
chemical industry or manufactured fine silica powder as a by-product of
ferro-silicon metallurgy. Equation 2-2 shows an example of polycondensation
by alkali into poly (sialate-siloxo).

(-)
Naoh, KOH
(Si2O5, Al2O2) n + nSiO2 + nH2O n(OH)3-Si-O-Al-O-Si-(OH)3

(OH)2

(-) (-)
n(OH)3 -Si-O-Al-O-Si-(OH)3 Naoh, KOH
(Na,K)(+) –(-Si-O-Al-O-Si-O-) + nH2O

(OH)2 O O O

(2-2)
5
 Unlike ordinary Portland/pozzolanic cements, geopolymers do not form
calcium- silicate-hydrates (CSHs) for matrix formation and strength, but
utilise the polycondensation of silica and alumina precursors and a high alkali
content to attain structural strength. Therefore, geopolymers are sometimes
referred to as alkali- activated alumino silicate binders (Davidovits, 1994;
Palomo et. al., 1999; Roy, 1999; van Jaarsveld et. al., 2002). However,
Davidovits (1999; 2005) stated that using the term ‘alkali-activated’ could create
significant confusion and generate false granted ideas about geopolymer
concrete. For example, the use of the term‘ alkali-activated cement’ or ‘alkali-
activated fly ash’ can be confused with the term‘ Alkali-aggregate reaction
(AAR)’, a harmful property well known in concrete.

The last term of equation 2-2 indicates that water is released during the
chemical reaction that occurs in the formation of Geopolymers. This water is
expelled from the mixture during the curing process.

2.2.2 Source Materials and Alkaline Liquids

There are two main constituents of Geopolymers, namely the source

materials and the alkaline liquids. The source materials for Geopolymers based
on alumino-silicate should be rich in silicon (Si) and aluminium (Al). These
could be natural minerals such as kaolinite, clays, micas, andalousite, spinel, etc
whose empirical formula contains Si, Al, and oxygen (O) (Davidovits, 1988 ).
Alternatively, by-product materials such as fly ash, silica fume, slag, rice-husk ash,
red mud, 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

6
are from soluble alkali metals that are usually Sodium or Potassium based

Since 1972, Davidovits (1988; 1988) worked with kaolinite source material
with alkalis (NaOH, KOH) to produce Geopolymers. The technology for making
the Geopolmers has been disclosed in various patents issued on the applications of
the so- called “SILIFACE-Process”.Later, Davidovits (1999) also introduced
a pure calcined kaolinite called KANDOXI (KAolinite, Nacrite, Dickite Oxide)

which is calcined for 6 hours at 750ºC. This calcined kaolinite like other calcined
materials performed better in making Geopolymers compared to the natural ones.

Xu and Van Deventer (1999; 2000) have also studied a wide range of
alumino- silicate minerals to make Geopolymers. Their study involved sixteen
natural Si-Al minerals which covered the ring, chain, sheet, and framework
crystal structure groups, as well as the garnet, mica, clay, feldspar, sodalite
and zeolite mineral groups. It was found that a wide range of natural alumino-
silicate minerals provided potential sources for synthesis of Geopolymers. For
alkaline solutions, they used sodium or potassium h ydroxide . The test
results have shown that potassium hydroxide (KOH) gave better results in
terms of the compressive strength and the extent of dissolution.

Among the waste or by-product materials, fly ash and slag are the most
potential source of Geopolymers. Several studies have been reported related to the
use of these source materials. Cheng and Chiu (2003) reported the study of
making fire-resistant Geopolymer using granulated blast furnace slag combined
with metakaolinite. The combination of potassium hydroxide and sodium
silicate was used as alkaline liquids. Van Jaarsveld ET. al., (1997; 1999)
identified the potential use of waste materials such as fly ash, contaminated
7
soil, mine tailings and building waste to immobilise toxic metals. Palomo et. al.,
(1999) reported the study of fly ash-based Geopolymers. They used combinations
of sodium hydroxide with sodium silicate and potassium hydroxide with
potassium silicate as alkaline liquids. It was found that the type of alkaline liquid
is a significant factor affecting the mechanical strength, and that the combination
of sodium silicate and sodium hydroxide gave the highest compressive strength.

Van Jaarsveld et. al. (2003), reported that the particle size, calcium
content, alkali metal content, amorphous content, and morphology and origin of
the fly ash affected the properties of geopolymers. It was also revealed that the
calcium content in fly ash played a significant role in strength development and
final compressive strength as the higher the calcium content resulted in faster
strength development and higher compressive strength. However, in order to
obtain the optimal binding properties of the material, fly ash as a source material
should have low calcium content and other characteristics such as unburned
material lower than 5%, Fe2O3 content not higher than 10%, 40-50% of reactive
silica content, 80-90% particles with size lower than45 µm and high content of
vitreous phase (Fernández-Jiménez & Palomo, 2003). Gourley (2003) also
stated that the presence of calcium in fly ash in significant quantities could
interfere with the polymerisation setting rate and alters the microstructure.
Therefore, it appears that the use of Low Calcium (ASTM Class F) fly ash is
more preferable than High Calcium (ASTM Class C) fly ash as a source
material to make Geopolymers.

Swanepoel and Strydom (2002), Phair and Van Deventer (2001;

2002), Van Jaarsveld (2002; 2002) and Bakharev (2005; 2005; 2005) also
presented studies on fly ash as the source material to make Geopolymers.
8
Davidovits (2005) reported results of his preliminary study on fly
ash based Geopolymer as a part of a EU sponsored project entitled
‘Understanding and mastering coal fired ashes Geopolymerisation process
in order turn potential into profit’, known under the acronym of GEOASH.

Every source material has advantages and disadvantages. For example,

metokaolin as a source material has high dissolvability in the reactant
solution, produces a controlled Si/Al ratio in the Geopolymer, and is white in
colour (Gourley, 2003). However, metakaolin is expensive to produce in large

volumes because it has to be calcined at temperatures around 500oC – 700oC for

few hours. In this respect using waste materials such as fly ash is economically
advantageous.

2.2.3 Fields of Applications

According to Davidovits (1988), Geopolymeric materials have a wide

range of applications in the field of industries such as in the automobile and
aerospace, non- ferrous foundries and metallurgy, civil engineering and plastic
industries. The type of application of Geopolymeric materials is determined by
the chemical structure in terms of the atomic ratio Si:Al in the polysialate.
Davidovits (1999) classified the type of application according to the Si:Al ratio as
presented in Table 2.1. A low ratio of Si:Al of 1, 2, or 3 initiates a 3D-Network
that is very rigid, while Si:Al ratio higher than 15 provides a polymeric character
to the Geopolymeric material. It can be seen from Table 2.1 that for many
applications in the civil engineering field a low Si:Al ratio is suitable.

One of the potential fields of application of Geopolymeric materials is in

toxic waste management because Geopolymers behave similar to zeolitic materials
9
that have been known for their ability to absorb the toxic chemical wastes
(Davidovits, 1988). Comrie et. al., (1988) also provided an overview and
relevant test results of the potential of the use of Geopolymer technology in toxic
waste management. Based on tests using GEOPOLYMITE 50, they recommend
that Geopolymeric materials could be used in waste containment.
GEOPOLYMITE 50 is a registered trademark of Cordi-Geopolymere SA, a
type of Geopolymeric binder prepared by mixing various alumina-silicates
precondensates with alkali hardeners (Davidovits, 1988).

Table 2.1 Applications of Geopolymeric Materials Based on Si:Al Atomic

Ratio

Si:Al ratio Applications

1 Bricks

Ceramics
2 Low CO2 cements and concretes
- Fire protection
Radioactive and toxic waste encapsulation
3 Fire protection fibre glass composite
Foundry equipments
Heat resistant composites, 200oC to1000oC
>3 S`1ealants for industry, 200oC to 600oC
- Tooling for aeronautics titanium process
Tooling for aeronautics SPF aluminium
20 – 35 Fire resistant and heat resistant fibre
composites

Another application of Geopolymer is in the strengthening of concrete

structural elements. Balaguru et. al. (1997) reported the results of the
10
investigation on using Geopolymers, instead of organic polymers, for fastening
carbon fabrics to surfaces of reinforced c o n c r e t e b e a ms . It w a s found t h a t
G e o p o l y m e r p r o v i d e d e x c e l l e n t 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).

2.2.4 Properties of Geopolymers

Previous studies have reported that Geopolymers possess high early

strength, low shrinkage, freeze-thaw resistance, sulfate resistance, corrosion
resistance, acid resistance, fire resistance and no dangerous alkali-aggregate
reaction.

Based on laboratory tests, Davidovits (1988b) reported that Geopolymer

cement can harden rapidly at room temperature and gain the compressive strength
in the range of 20 MPa after only 4 hours at 20oC and about 70-100 MPa after 28
days. Comrie et. al., (1988) conducted tests on Geopolymer mortars and reported
that most of the 28- day strength was gained during the first 2 days of curing.

Geopolymeric cement was superior to Portland cement in terms of heat

and fire resistance, as the Portland cement experienced a rapid deterioration in
11
compressive strength at 300oC, whereas the Geopolymeric cements were
stable up to 600oC (Davidovits, 1988; 1994). It has also been shown that
compared to Portland cement, Geopolymeric cement has extremely low
shrinkage.

The presence of alkalis in the normal Portland cement or concrete could

generate dangerous Alkali-Aggregate-Reaction. However the Geopolymeric
system is safe from that phenomenon even with higher alkali content. As
demonstrated by Davidovits (1994; 1994), based on ASTM C227 bar expansion
test, Geopolymer cements with much higher alkali content compared to
Portland cement did not generate any dangerous alkali-aggregate reaction where
the Portland cement did.

Geopolymer cement is also acid-resistant, because unlike the Portland

cement, Geopolymer cements do not rely on lime and are not dissolved by acidic
solutions. As shown by the tests of exposing the specimens in 5% of sulfuric acid,
Geopolymer cements were relatively stable with the weight lose in the range of 5-
8% while the Portland based cements were destroyed and the calcium alumina
cement lost weight about 30-60% (Davidovits, 1994). Some recently published
papers (Bakharev, 2005; Gourley & Johnson, 2005; Song et. al., 2005) also
reported the results of the tests on acid resistance of Geopolymers and
Geopolymer concrete. By observing the weight loss after acid exposure, these
researchers concluded that Geopolymers or Geopolymer concrete is superior to
Portland cement concrete in terms of acid resistance as the weight loss is much
lower. However, Bakharev and Song et. al has also observed that there is
degradation in the compressive strength of test specimens after acid exposure and
the rate of degradation depended on the period of exposure. Tests conducted by
12
U.S. Army Corps of Engineers also revealed that Geopolymers have superior
resistance to chemical attack and freeze/thaw, and very low shrinkage coefficients
(Comrie et. al., 1988; Malone et. al., 1985).

The elastic properties of hardened Geopolymer concrete and the

behavior and strength of reinforced Geopolymer concrete structural members
are similar to those observed in the case of Portland cement concrete [Sofi et al,
2007; Chang, 2009]. Heat-cured low-calcium fly ash-based Geopolymer concrete
also shows excellent resistance to sulfate attack, good acid resistance,
undergoes low creep, and suffers very little drying shrinkage [Wallah and
Rangan, 2006].

The behaviour and failure modes of reinforced Geopolymer concrete

columns and beams were similar to those observed in the case of reinforced
Portland cement concrete columns [Sumajouw and Rangan, 2006; Sumajouw et
al, 2007]. Test results demonstrated that the methods of calculations used in
the case of reinforced Portland cement concrete columns and beams are
applicable for reinforced Geopolymer concrete columns. Mid-span deflection at
service load of reinforced Geopolymer concrete beams was calculated using the
elastic bending theory and the serviceability design provisions given in
Standards. Good correlation of test and calculated deflections at service load
was observed.

13
 CHAPTER 3

MATERIALS AND METHODS

3.1 Geopolymer concrete

1. Fly ash

Low calcium class F type fly ash

2. Alkaline liquid

Sodium hydroxide (97% purity in pure form)

Sodium silicate solutions.

3. Coarse aggregate

Coarse Aggregate (20mm & 12.5mm)

4. Fine aggregate

Fine aggregate (fineness modulus 2.6 — 2.8)

5. Distilled Water

3.2 Necessity of using Geopolymer

The application of Geopolymer technology in the mining, energy,

construction and waste containment industries offers the opportunity to address a
variety of sustainability issues currently experienced by these industries. These
issues include:

 Converting by-products currently treated as wastes to useful and valuable

Products – from a cost to a new input in their own right.
 Enhancing product features across the building materials market.
 Providing new long-term management options for a number of waste
14
 Containment problems, particularly low level toxic wastes.
 Reducing greenhouse gas emissions by significant amounts, particularly in
the concrete industry.

3.3 Advantages of using Geopolymer

 Rapid development of mechanical strength, fire resistance, dimensional

stability.
 Increased acid resistance, excellent adherence to aggregates and
reinforcements.
 Geopolymer concrete derived from fly ash, the cost of the material is
generally lower than OPC by a factor of about 10–30%.
 Improved properties when compared to traditional Portland cement concrete.
 Geopolymers can be used as adhesives, coatings and hydro ceramics which
increases the binding compatibility.(Metakaolin or other synthetically
derived aluminosilicate raw material sources)
 The exposure of Geopolymer in acid solution shows weight loss due to the
exposure about only 0.5% compared to normal concrete when immersed in
sulphuric acid.

3.4 Fly ash in India

India at present produces around 120 Million Tones of Ash per annum. The
power requirement of the country is rapidly increasing with increase in growth of
the industrial sectors. India depends on Thermal power as its main source (around
80% of power produced is thermal power), as a result the quantity of Ash produced
shall also increase. Indian coal on an average has 35 % Ash and this is one of the

15
prime factors which shall lead to increased ash production and hence, Ash
utilization problems for the country. Out of the total ash produced, Fly ash
contributes to a small percentage, majority being Pond ash and bottom ash.

3.5 Methodology

FLY ASH COARSE AGGREGATE FINE AGGREGATE

WEIGH BATCHING 1:1:2. FOR GEOPOLYMER CONCRETE

MIXING: FINE AGGREGATE + FLYASH + COARSE AGGREGATE+ ALKALINE LIQUID

FLYASH BASED GEOPOLYMER CONCRETE

CASTING: BEAM {700x150x150}mm

ROOM TEMPERATURE (27 to 30 degree)

TESTING: FOR 7 DAYS AND 28 DAYS

STRENGTH

Fig 3.1 Methodology

16
 CHAPTER-4

EXPERIMENTAL INVESTIGATION
4.1 Introduction

The focus of the study was to identify the salient parameters that influence
the mixture proportions and the properties of low calcium fly ash-based
Geopolymer concrete mix to with optimum strength and workability to handle
manual compaction methodologies.

This chapter gives a detailed explanation of the experimental work giving

specific citing to materials used, mix proportions, manufacturing process, curing
and testing of the specimens as far as possible. The current practice used in the
manufacture and testing of ordinary Portland cement (OPC) concrete was
followed. The aim of following this procedure is to ease the production of this fly
ash based Geopolymer concrete in construction industry.
In order to satisfy the development process, the compressive strength, pH
ranges were selected as the benchmark parameter.

4.2 Fly Ash

In the present experimental work, low calcium, Class F (American Society
for Testing and Materials) dry fly ash obtained from the silos of Thermal Power
Station, Neyveli Lignite Corporation Limited, Tamil Nadu, was used as the base
material.
The chemical composition of the ASTM class F Fly ash and OPC is given
below in Table. It clearly shows that the major constituent of fly ash is silica
(52.8%) whereas in OPC it is lime which is completely absent in Fly ash.

17
 Fig.4.1 Fly Ash Used For Geopolymer Concrete

Table 4.1 Chemical composition of Lignite Fly ash

Characteristics Fly ash(%wt)

Silica 35-59%

Iron oxide 0.5-2%

Aluminium oxide 20-33%

Calcium oxide 5-16%

Magnesium oxide 1-5.5%

Sulphates 0.5-1.5%

Loss on ignition 1-2%

18
 Table 4.2 Physical Properties of low calcium class F Fly Ash

Physical properties Properties of Properties of fly ash

according to
fly ash used
IS 1320-1981
Specific gravity 2.51 -

initial setting time 120 minutes -

final setting time 280 minutes -

Fineness specific 320 340

surface in m2/kg min
Lime reactivity avg 4.00 6.200
compressive strength

1) In the research work, low calcium, class F dry fly ash obtained from
Thermal power plant ,Neyveli Lignite Corporation, Tamil nadu is used as base
material to make the Geopolymers.

2) Sodium silicate (Na2SiO3) mixed with sodium hydroxide (NaOH) as an

alkaline activator has been used in this study, NaOH in pellet form with 97% purity
& Na2SiO3 consist of Na2O=9.4%, SiO2=30.1% & H2O=60.5%, with weight
ratio SiO2/Na2O=3.20-3.30)

4.3 Aggregates

The type of fine aggregate used in this study is locally available sand. The
type of coarse aggregates used for this study is crushed granite (Angular) which is
locally available. Maximum size of aggregate used is 12.5 mm. Physical
characteristics of the sand used are presented in Table 4.3

19
 Table 4.3 - Physical Characteristics of Aggregates

Physical properties Fine aggregate Coarse aggregate

(sand) (12.5 mm down)

Specific gravity 2.60 2.61
Fineness modulus 2.78 -
Loose bulk density 1536 1290
(kg/m3)
Dry rodded bulk density 1640 1500
(kg/m3)

4.4 Alkaline liquid

A combination of sodium silicate solution and sodium hydroxide solution

was chosen as the alkaline liquid. Sodium-based solutions were chosen because
they were cheaper than Potassium-based solutions. The sodium hydroxide solids
were either a technical grade in flakes form (3 mm) or a commercial grade in
pellets form with 97% purity.
The sodium hydroxide (NaOH) solution was prepared by dissolving either
the flakes or the pellets in water. The mass of NaOH solids in a solution varied
depending on the concentration of the solution expressed in terms of molar, M. For
instance, NaOH solution with a concentration of 8M consisted of 8x40 = 320
grams of NaOH solids (in flake or pellet form) per litre of the solution, where 40 is
the molecular weight of NaOH. The mass of NaOH solids was measured as 262
grams per kg of NaOH solution of 8M concentration. Similarly, the mass of NaOH
solids per kg of the solution for other concentrations were measured as 10M: 314
grams, 12M: 361 grams, 14M: 404 grams, and 16M: 444 grams. Note that the mass

20
of NaOH solids was only a fraction of the mass of the NaOH solution, and water is
the major component.

Fig.4.2 Alkaline Solution for Geopolymer Concrete

4.5 Preparation of Alkaline Solution

The sodium hydroxide (NaOH) solids were dissolved in water to make the
solution. The mass of NaOH solids in a solution varied depending on the
concentration of the solution expressed in terms of molar, M. The sodium silicate
solution and the sodium hydroxide solution were mixed together at least one day
prior to use to prepare the alkaline liquid. On the day of casting of the specimens,
the alkaline liquid was mixed together and the extra water (if any) to prepare the
liquid component of the mixture.
1. Preparation of sodium hydroxide solution with a concentration of 10 M

Distilled water = 10 liters

NaOH solid = 4 kg

Total 20 litres of distilled water NaOH solids 8 kg

21
 Sodium Silicate Geopolymer concrete:

Sodium hydroxide solution + Sodium Silicate Solution = 1:2.5 by weight

Sodium hydroxide solution = 10 kg

Sodium hydroxide solution = 25 kg

Total = 35 kg

2. Preparation of sodium hydroxide solution with a concentration of 8 M

Distilled water = 10 liters

NaOH solids = 3.2 kg

Total 20 litres of distilled water NaOH solids 6.4 kg

Sodium Silicate Geopolymer concrete:

Sodium hydroxide solution + Sodium Silicate Solution = 1:2.5 by weight

Sodium hydroxide solution = 10 kg

Sodium Silicate Solution = 25 kg

Total = 35 kg

4.6 Proportioning of Geopolymer Concrete mixes

The different concrete mixes were obtained by absolute volume method

assuming the wet density of the Geopolymer concrete as 2400 kg/m3 based on the
preliminary tests in our laboratory.
22
The water content was fixed at 140 kg/m3. The fly ash content was varied in range
of 315 kg/m3 (15% of total particulate matter) to 566 kg/m3 (27% of total
particulate matter) considering workability criteria and desired compressive
strength of Geopolymer concrete.

The alkaline solution used was the combination of sodium hydroxide and
sodium silicate solution where the concentration of the sodium hydroxide solution
was kept constant at 16 molarities, ratio of sodium silicate solution to sodium
hydroxide solution was kept constant at 2.5 respectively. The details of the mix
proportions are shown in the Table 4.4

Table 4.4 Details of Geopolymer Concrete Mixtures

AGGREGATE Fly ash Water/Fly

NaOH Na2SiO3
MIX (F) ash (W/F)
No. Coarse fine kg/m³ kg/m³
kg/m³
1 1016 767 315 86.56 216.41 0.44
2 980 739 377 86.56 216.41 0.37
3 944 712 441 86.56 216.41 0.32
4 872.6 658 566 86.56 216.41 0.25

4.7 Preparation of the specimen

All the ingredients were mixed in the laboratory using mixer machine. The
capacity of the mixer machine is 0.25 m3. Initially all the dry ingredients such as
the fly ash, fine aggregates, coarse aggregates were mixed for 3 minutes, after
23
which, the alkaline solutions were added which were prepared one day prior and
then all the ingredients were mixed thoroughly for 4 minutes. For compaction of
the specimens, each layer was given 40 to 50 manual strokes using a Roding bar,
and then vibrated for 30 to 60 seconds on a vibrating table. Before casting the test
specimens the workability of the concrete was assessed using slump test and the
slump value was in between the range 90mm to 120mm.

Fig .4.3 Mixer Machine Used for Preparation of Specimen

Fig.4.4 Slump Test for Workability

24
4.8 Casting of the specimen
The mixed concrete is cast in 700X150X150 mm beam. The compaction of
beam is done in 3 layers. Each layer is given 25 blows with tamping rod and after
completing all the layers, the beam mould was vibrated for 30 seconds on vibrating
table. After casting, the specimens are kept at room temperature.

Fig.4.5 Beam Specimens of Geopolymer Concrete

4.9 Testing
The casted specimens were tested by flexural strength testing machine as per
Indian standards.

Fig.4.6 Set Up For Flexural Strength

25
 Fig.4.7 Beam Specimen after failure

The specimens for each mix are tested and the average value is calculated.

The casted specimens were tested after 7th day of casting and 28th day of casting.

4.10 Acid Attack Test

The concrete cube specimens of 10 Molarity and 8 Molarity of size 150 mm

x 150mm x 150mm were casted and after 7 days and 28 days of ambient curing,
the weights of concrete cube specimen were taken. The acid attack test on concrete
cube was conducted by immersing the cubes in the acid water for 7 days and 28
days. Suphuric acid (H2SO4) with pH of about 2 at 5% weight of water was added
to water in which the concrete cubes were stored. The pH was maintained
throughout the period of 7 days and 28 days.
The acid containing water is continuously changed to arrest the lowering of
salt concentration which in turn would provide the protection to the surface of the
specimen. The chemical resistance of the concretes was studied through chemical
attack by immersing them in an acid solution. After 7 days period of curing the
26
specimens were removed from the curing tank and their surfaces were cleaned with
a soft nylon brush to remove weak reaction products and loose materials from the
specimen. The initial weights were measured and the specimens were identified
with numbered plastic tokens that were tied around them. Then, the specimens
were tested for compressive strength.
The resistance of concrete to acid attack was found by the % loss of weight
of specimen and the % loss of Compressive strength on immersing concrete cubes
in acid water. Similarly, after 28 days of immersion, the specimens were tested for
compression strength following the procedure prescribed in IS: 516-1959.
One of the main causes of deterioration in concrete structures is the
corrosion of concrete due to its exposure to harmful chemicals that may be found
in nature such as in some ground waters, industrial effluents and sea waters. The
most aggressive chemicals that affect the long term durability of concrete
structures are the chlorides and sulfates.

Fig 4.8 Set Up For Acid Resistant Concrete

27
 Fig 4.9 Mixing of Suphuric Acid to Water Containing Concrete Cubes

Fig 4.10 Final Stage of Mixing of Sulphuric Acid to Water

These specimens were tested after 7 days and 28 days of curing. The initial
weights were measured for each specimen and compressive strength for each
specimen is tested.

28
4.11 Compression Strength Test

The compressive strength of concrete is one of the most important and

useful properties of concrete. In most structural application concrete is implied
primarily to resist compressive stress. In this experimental investigation, only
Geopolymer concrete cubes are used for testing compressive strength. The load at
which the control specimen ultimately fail is noted, compressive strength is
calculated by dividing load by area of specimen.
fc = ρ /a
Where fc = cube compressive strength in N∕mm2
ρ = cube compressive load causing failure in N
a = cross sectional area of cube in mm2

The compressive strength for mix designations 8 Molarity and 10 Molarity

are shown in tables at 7 days and at 28 days. It is observed that as the molarity and
Na2SiO3 / NaOH ratio is increased the compressive strength increases. Result for
compressive strength will be for 7 days & 28 days for oven drying & ambient
temperature.

Fig 4.11 Casted Cubes Of Geopolymer Conrete

29
 Fig 4.12 Set up For Compressive Strength

4.12 Curing of Test Specimen

After casting, the specimens were placed in the oven for dry curing at
optimum temperature of 260°C.

After the curing period, the test specimens were left in the moulds for at
least six hours in order to avoid a drastic change in the environmental conditions.
After remolding, the specimens were left to air−dry in the laboratory until the day
of test.

Fig 4.13 Curing In Oven

30
4.13 Curing time

The test specimens were cured for 4 hours in oven and was found that
prolonged curing time was not found to alter the compressive strength of concrete.

4.14 Setting time

Setting time of Geopolymer depend on many factors such as composition of

alkaline solution and ratio of alkaline liquid to fly ash by mass. However, the
curing temperature is the most important factor for Geopolymer.

31
 CHAPTER 5

RESULTS AND DISCUSSION

From the above experimental investigation we got results of flexural
strength of Geopolymer concrete beams 8 molarity and 10 molarity of sodium
Hydroxide solution of alkaline solution were casted and tested after the 7 days of
casting and 28 days of casting.

The flexural strength of Geopolymer concrete beam for 7 days testing is

mentioned in the table 5.1 for 8 molarity and10 molarity.

The flexural strength of Geopolymer concrete beam for 28 days testing is

mentioned in the table 5.2 for 8 molarity and 10 molarity.

Table 5.1 Flexural strength test results at 7 days for Beam 700X150X150mm

Flexural strength Avg. flexural strength

Specimen N/mm2 N/mm2

Sample 1 1.84

Sample 2 1.93
8M 1.86
Sample 3 1.81

Sample 1 2.57

10M Sample 2 2.44

2.57
Sample 3 2.71

32
 0.1

0.08
Flexural strength
N/mm2 0.06
10 molarity
0.04
8 molarity

0.02

0
1 2 3
No. of Beams

Fig 5.1 Chart of Flexural Strength of Geopolymer Concrete Beam for 7 Days

Table 5.2 Flexural strength test results at 28 days for Beam 700X150X150mm

Flexural strength Avg.flexural strength

Specimen
N/mm2 N/mm2

Sample 1 2.24

Sample 2 2.37
8M 2.41
Sample 3 2.64

Sample 1 3.82

10M Sample 2 3.73

3.79
Sample 3 3.82

33
 0.16
0.14
0.12
0.1
Flexural strength
N/mm2 0.08
10 molarity
0.06
8 molarity
0.04
0.02
0
1 2 3

No. of Beams

Fig 5.2 Chart of Flexural Strength of Geopolymer Concrete Beam for 28 Days

From the above experimental investigation we got results of compressive

strength for acid resistant test of Geopolymer concrete cubes 8 molarity and 10
molarity of sodium Hydroxide solution of alkaline solution were casted and tested
after the 7 days of casting and 28 days of casting.

The compressive strength for acid resistant test of Geopolymer concrete

cubes for 7 days testing is mentioned in the table 5.3 for 8 molarity and10 molarity.

The compressive strength for acid resistant test of Geopolymer concrete

cubes for 28 days testing is mentioned in the table 5.4 for 8 molarity and 10
molarity.

34
Table 5.3 Compressive Strength for Acid Resistant Test results at 7 days for
Cube 150X150X150mm

Compressive strength Avg.compressive strength

Specimen
N/mm2 N/mm2

Sample 1 1.84
Sample 2 1.93
8M 1.86
Sample 3 1.81

Sample 1 3.82

10M Sample 2 3.73

3.79
Sample 3 3.82

4
3.5
3
2.5
Compression
strength N/mm2 2
10 molarity
1.5
8 molarity
1
0.5
0
1 2 3
No. of Cubes

Fig 5.3 Chart of Compressive Strength for Acid Resistant Test of Geopolymer
Conrete Cubes for 7 Days

35
Table 5.4 Compressive Strength for Acid Resistant Test results at 28 days for
Cube 150X150X150mm

Compressive Avg.compressive strength

Specimen
strength N/mm2 N/mm2

Sample 1 3.37
Sample 2 3.35
8M 3.34
Sample 3 3.30

Sample 1 5.24

10M Sample 2 5.37

5.41
Sample 3 5.64

4
Compression
strength N/mm2 3 10 molarity
2 8 molarity

0
1 2 3
No. of Cubes

Fig 5.4 Chart of Compressive Strength for Acid Resistant Test of Geopolymer
Conrete Cubes for 28 Days

36
 From the above experimental investigation we got results of compressive
strength of Geopolymer concrete cubes 8 molarity and 10 molarity of sodium
Hydroxide solution of alkaline solution were casted and tested after the 7 days of
casting and 28 days of casting.

The compressive strength of Geopolymer concrete cubes for 7 days testing is

mentioned in the table 5.5 for 8 molarity and10 molarity.

The compressive strength of Geopolymer concrete cubes for 28 days testing

is mentioned in the table 5.6 for 8 molarity and 10 molarity

Table 5.5 Compressive Strength Test results at 7 days for Cube

150X150X150mm

Compressive Avg.compressive strength

Specimen strength N/mm2 N/mm2

Sample 1 1.84

8M Sample 2 1.93 1.86

Sample 3 1.81

Sample 1 2.57

10M Sample 2 2.44 2.57

Sample 3 2.71

37
 3

2.5

2
Compression
strength 1.5
N/mm2 10 molarity
1 8 molarity
0.5

0
1 2 3
No. of Cubes

Fig 5.5 Chart of Compressive Strength of Geopolymer Concrete Cubes for 7

Days

Table 5.6 Compressive Strength test results at 28 days for Cube

150X150X150mm

Compressive strength Avg.compressive strength

N/mm2 N/mm2
Specimen

Sample 1 5.52

Sample 2 5.79
5.58
8M
Sample 3 5.43

Sample 1 7.71

Sample 2 8.58
10M 7.88
Sample 3 7.53

38
 10
9
8
7
6
Compression
5
strength N/mm2
4 10 molarity
3 8 molarity
2
1
0
1 2 3
No. of Cubes

Fig 5.6 Chart of Compressive Strength of Geopolymer Concrete Cubes for 28

Days

From the above experimental investigation we got results of compressive

strength of curing temperature of Geopolymer concrete cubes 8 molarity and 10
molarity of sodium Hydroxide solution of alkaline solution were casted and tested
after the 7 days of casting and 28 days of casting.

The compressive strength of curing temperature of Geopolymer concrete

cubes for 7 days testing is mentioned in the table 5.7 for 8 molarity and10 molarity.

The compressive strength of curing temperature of Geopolymer concrete

cubes for 28 days testing is mentioned in the table 5.8 for 8 molarity and 10
molarity.

39
Table 5.7 Compressive Strength for Curing test results at 7 days for Cube 150

X150X150mm

Compressive strength Avg.compressive strength

Specimen N/mm2 N/mm2

Sample 1 7.63

Sample 2 7.54
8M 7.46
Sample 3 7.23

Sample 1 9.53

10M Sample 2 9.38

9.49
Sample 3 9.56

10

Compression 6
strength N/mm2
10 molarity
4
8 molarity
2

0
1 2 3
No. of Cubes

Fig 5.7 Chart of Compressive Strength for Curing of Geopolymer Concrete

Cubes for 7 Days
40
Table 5.8 Compressive Strength for Curing test results at 28 days for Cube
150X150X150mm

Compressive Avg.compressive strength

Specimen strength N/mm2 N/mm2

Sample 1 10.12

Sample 2 11.23
8M 10.65
Sample 3 10.61

Sample 1 13.54

10M Sample 2 14
14.05
Sample 3 14.61

16
14
12
10
Compression
strength N/mm2 8
10 molarity
6
8 molarity
4
2
0
1 2 3
No. of Cubes

Fig 5.8 Chart of Compressive Strength for Curing of Geopolymer Concrete

Cubes for 28 Days

41
 CHAPTER 6

SUMMARY AND CONCLUSIONS

6.1 Introduction

This chapter presents a detailed summary and important conclusion that

were drawn from the project. After arriving the conclusions of the project, some
economic benefits of using Geopolymer concrete for masonry works involving
cubes, blocks are being furnished.

6.2 Summary of Work

With the information available about the Geopolymer concrete from the
literature surveying and from the past researches done on this topic. The mixture
proportion was selected so as to have a balanced workability and strength. The
mixing was done manually. The compaction was done by mechanically and testing
was done for compressive strength.

6.3 Conclusion

The construction industry is in demand of ecofriendly & greener materials

which are durable. As compared to the existing concrete materials, fly ash is
advantageous but its uses as tested against strength & durability needs to be
confirmed. The present project work emphasis on the research & development
activity in construction materials using fly ash with geopolymers.The project work
revels with preparation of test samples of fly ash with geopolymers of different
molarities such as 8,10.

42
 Tests for flexural strength, compressive strength, acid resistant test and
curing of test specimen are carried out on samples as above for ambient
temperature (A.T) for 7 & 28 days, as per prevailing standards for respective
properties. The details of the results are summarized as under.

 As higher concentration in terms of molar of solutions, results in higher

flexural strength of fly ash based geopolymer concrete.
 It is identified that, there is considerable increase in loss of strength only
with Flyash replacement.
 It is observed that, when quantity of sodium silicate & sodium hydroxide is
reversed by mass, it is observed that compressive strength increases as
increase in molarity.
 It is observed that, compressive strength is more for oven drying as compare
to specimen left in ambient temperature.

6.4 Economical Benefits

The cost of one ton of fly ash is only a small fraction otherwise negligible
also in some place. When compared with bricks and OPC concrete beam with the
Geopolymer beam, the Geopolymer concrete uses only waste materials from the
chemical industry and power plants, which materials unless otherwise utilized may
become harmful.

More over the usage of waste is highly reduced which makes it more
cheaper than conventional OPC concrete products.

43
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