GPC Swamy

“PERFORMANCE OF GEOPOLYMER CONCRETE AT ELEVATED
TEMPERATURE ”
Dissertation submitted to
VISWESVARAIAH TECHNOLOGICAL UNIVERSITY,

BELGAUM, KARNATAKA
In partial fulfillment of the requirements for the award of the degree of
MASTER OF TECHNOLOGY
IN
CONSTRUCTION TECHNOLOGY
By
KEDARA SWAMY .U
Reg. No. 1BM05CCT07
Under the guidance of
Dr. SAKEY SHAMU
Mr. M. S. SUDARSHAN
Department of Civil Engineering

B. M. S. COLLEGE OF ENGINEERING
BANGALORE - 560 019
OCTOBER- 2007
“PERFORMANCE OF GEOPOLYMER CONCRETE AT ELEVATED
TEMPERATURE ”
Dissertation submitted to
VISVESWARAIAH TECHNOLOGICAL UNIVERSITY,

BELGAUM, KARNATAKA
In partial fulfillment of the requirements for the award of the degree of
MASTER OF TECHNOLOGY
IN
CONSTRUCTION TECHNOLOGY
By
KEDARA SWAMY .U
Reg. No. 1BM05CCT07
Under the guidance of
Dr. SAKEY SHAMU
Mr. M. S. SUDARSHAN
Department of Civil Engineering

B. M. S. COLLEGE OF ENGINEERING
BANGALORE - 560 019
OCTOBER- 2007
CERTIFICATE
This is to certify that the dissertation entitled an “PERFORMANCE OF

GEOPOLYMER CONCRETE AT ELEVATED TEMPERATURE ” being submitted by
Mr. Kedara swamy .U to the Visveswaraya Technological University, Belgaum for the award
of degree of Master of Technology in Construction Technology, is a record of bonafide
work carried out by him during the year 2006-2007. Mr. Kedara Swamy U. has worked under
my guidance and supervision and has fulfilled the requirements for the submission of this
thesis, which to my knowledge has reached the requisite standards.
Dr. Sakey Shamu Dr. R. V. Ranganath

Professor Professor & H.O.D
Dept. of Civil Engg. Dept. of Civil Engg.
B. M. S. College of Engg B.M.S. College of Engg
Bangalore Bangalore
Mr. M. S. Sudarshan Dr. M. K. Venkatesha

Director (Technical) Principal
Civil Aid Techno clinic Pvt. Ltd. B. M. S.College of Engg.
Bangalore Bangalore
Examiners: Signature with Date

1.
2.
DECLARATION
I, the undersigned declare that this dissertation work entitled “PERFORMANCE OF
GEOPOLYMER CONCRETE AT ELEVATED TEMPERATURE”, is a bonafide work
carried out by me (during 2006 – 2007) in partial fulfillment of the requirements for the award
of post graduate degree of Master of Technology in Construction Technology of
Visveswaraiah Technological University, Belgaum and is based on the study carried out under
the guidance of Dr. Sakey Shamu & Mr. M. S. Sudarshan in B. M. S. College of
Engineering, Bangalore. I also declare that this thesis has not been submitted to any other
university or institution for the award of any degree.
KEDARA SWAMY.U
Reg. No. 1BM05CCT07
B. M. S. College of Engineering
Bangalore.
ACKNOWLEDGEMENT
I wish to express my sincere regards and heartfelt gratitude to Dr. Sakey Shamu, Professor
Department of Civil Engineering & Mr. M. S. Sudarshan, Director, Civil Aid Techno Clinic
Pvt. Ltd, under whose guidance, this study was carried out. Their constant encouragement,
valuable suggestions and deep involvement were the source of inspiration and motivation for
successful completion of this project.
I am grateful to Dr. R. V. Ranganath, Head of the Civil Engineering Department, B. M. S.

College, Bangalore, for his informative inputs during the course of this project.
I am grateful to Dr. N. Suresh, Director, BFRC, NIE, Mysore, who has given me the
opportunity to carry out work in his organization.
I am also extremely thankful to staff of Civil Aid Techno Clinic Pvt. Ltd, Bangalore for their
co-operation throughout the course of this study.
I am thankful to Mr. C. V. Parthasarathy and all the technicians of concrete laboratory for
helping me in the experimental work.
I am deeply indebted to all the faculty members of Department of Civil Engineering, BMSCE,
Bangalore for their knowledgeable advice throughout the course of this study.
I wish to convey my special thanks to all the staff of Geo-Technical laboratory for their
constant help and co-operation.
My deepest and utmost sincere thanks to my classmates Mr. Hanamanth Reddy G Furme
and Mr. Mohammed Saleh for their constant help throughout the experimental work.
I wish to express my heartfelt gratitude to my parents and family members for their moral
support and valuable suggestions during my study.
Last, but not the least, I thank my classmates and friends for the encouragement and support
throughout my course.
KEDARA SWAMY.U
ABSTRACT
The increase in the green house effect causes ecological imbalance contributing to global
warming which is at alarming rate. The cement industry is responsible for about 6% of all CO 2
emissions, because the production of one ton of Portland cement emits approximately one ton
of CO2 into the atmosphere. In order to over come the green house effect caused by the
manufacturing of the ordinary Portland cement an immediate need arise to find a suitable
substitute for ordinary Portland cement.
The discovery of geopolymers is a breakthrough which provides a cleaner and

environmentally-friendlier alternative to Ordinary Portland Cement (OPC). Geopolymer is a
new breed of fly ash which is an end product in thermal power plant. Geopolymer concrete is a
revolutionary substitute to conventional ordinary Portland cement concrete with lot of
advantages.
Fire represents one of the most severe exposure conditions and hence provisions for
appropriate fire resistance for structural members are major safety requirements in any building
design. In order to predict the fire resistance of a structure, the temperatures in the structure
must be determined. The fire resistance of structural members is dependent on the thermal and
mechanical properties at elevated temperatures, of the materials of which the members are
composed. This project aims at studying the performance of geopolymer concrete under
elevated temperature. Performance of different GPC mixes were studied at varying test
temperatures sustained for different durations. The specimens were heated for different
temperatures namely 250 0 C, 400 0 C, 600 0 C,800 0 C sustained for duration of 2 hours and 4
hours.
The mechanical properties like compressive strength, Young’s modulus, modulus of rupture
were studied. A non destructive test was also conducted to assess the quality of the specimens
exposed to different temperature ranges. SEM investigations were carried out to study the
change in the microstructures at different temperatures.
Experimental investigations have shown that geopolymer concrete is likely to behave
differently from the conventional concrete when exposed to high temperatures. The
compressive strength exhibited by the geopolymer concrete was in the range of (17.3- 94.93)
MPa. The ultra sonic pulse velocity (non-destructive test) of geopolymer concrete was in the
range of (0.8-4.0) km/s.
It is evident from the experimental research that the strength of the geopolymer concrete was
greatly influenced by the curing temperature to which it is subjected and the duration, the
chemical contents like sodium silicate to sodium hydroxide ratio is one of the governing
factors.
CONTENTS
CHAPTER 1 INTRODUCTION
1.1 General 1
1.2 Need for the present study 3
1.3 Objective of the study 4
1.4 Scope of the study 4
1.5 Organization of the thesis 5
CHAPTER 2 LITERATURE REVIEW 6
CHAPTER 3 GEOPOLYMER MATERIALS AND PROCESS
3.1 Geopolymer materials 13

3.1.1 Fly ash 13
3.1.2 Alkaline liquids 13
3.2 Geopolymerisation process 14
CHAPTER 4 EXPERIMENTAL INVESTIGATIONS
4.1 Experimental investigation 18

4.1 Materials
4.1.1 Flyash 18
4.1.2 Characteristics of aggregates used in the study 19
4.2 Proportioning of geopolymer concrete mix 21
4.3 Preparation of the specimens 21
4.3.1 Casting of the specimens 22
4.3.2 Curing of the specimens 23
4.4 Details of number of specimens 23
4.5 Exposing the specimens to Elevated Temperature 24
4.6 Test conducted 26
4.7 Physical Observation 26
4.7.1 Change in Colour 26
4.7.2 Aggregates 27
4.7.3 Cracks 27
4.7.4 Spalling 28
4.8 Compressive Strength test 28
4.9 Modulus of Elasticity test 29
4.10 Ultra Sonic Pulse Velocity test 31
4.11 Modulus of Rupture test 32
CHAPTER 5 RESULTS AND DISCUSSIONS
5.1 Physical observations 34

5.1.1 Discolouration 34
5.1.2 Aggregates 34
5.1.3 Cracking 35
5.1.4 Spalling 35
5.2 Results of Ultra Sonic Pulse Velocity test 36
5.3 Results of Compressive Strength test 43
5.4 Results of Modulus of Elasticity test 50
5.5 Results of Modulus of Rupture test 54
5.6 SEM results 62
CHAPTER 6 SUMMARY AND CONCLUSIONS
6.1 Summary 66
6.2 Conclusions 66
6.3 Scope for future study 68
LIST OF TABLES
4.1 - Physical characteristics of Fly Ash (RTPS) 17
4.2 - Chemical composition of Fly Ash 18
4.3 - Physical Characteristics of Aggregates 18
4.4 - Sieve Analysis Results of Fine Aggregate 19
4.5 - Sieve analysis results of Coarse Aggregate. 19
4.6 - Details of Geopolymer Concrete Mixtures 20
4.7 - Velocity criterion for Cement Concrete Quality Grading 31
5.1 - Physical Observation of the specimens in terms of Colour and Cracks. 34
5.2 - Ultra Sonic Pulse Velocity test results for the specimens subjected to
different temperature and different sustained duration for mix 1. 36
5.6 - Compressive Strength test results for the specimens subjected to different
temperature and different sustained duration for mix 1. 45
5.8 - Compressive Strength test results for the specimens subjected to
5.10 - Shows the results of Modulus of Elasticity of Geopolymer Concrete. 54
5.11 - Modulus of Rupture test results for the specimens subjected to different
temperature and different sustained duration. 57
5.12 - Shows the Compressive Strength and Ultra Sonic Pulse Velocity results. 58
5.13 - Shows the Compressive Strength and Young’s Modulus results. 60
5.14 - Shows the Compressive Strength and Flexure Strength results. 61
LIST OF FIGURES
4.1 - Details of the specimens subjecting to different temperature and different
sustained duration. 23
5.1(a) - Ultra Sonic Pulse Velocity test of the specimens sustained for 2 hours
Subjected to different temperature for mix 1. 36
5.1(b)Ultra Sonic Pulse Velocity test of the specimens sustained for 4 hours
subjected to different temperature for mix 1. 37
5.1(c) Ultra Sonic Pulse Velocity test results for the specimens subjected to
5.2(a)Ultra Sonic Pulse Velocity test of the specimen sustained for 2 hours
5.2(b)Ultra Sonic Pulse Velocity test of the specimen sustained for 4 hours
5.5(a) Variation of the Compressive Strength of specimens sustained for 2

hours at different temperature for mix 1. 46
5.5(b) Variation of the Compressive Strength of specimens sustained for 4

5.5(c) Variation of the Compressive Strength of specimens sustained for

different duration at different temperature for mix 1. 47


5.6(c) Variation of the Compression Strength at different temperature and

different sustained duration for mix 2. 49

5.7(b) Variation of the compressive strength of specimens sustained for 4

5.7(c) Variation of the compression strength at different temperature and
different sustained duration for mix 3. 51


5.8(c) Variation of the compression strength of specimens at different

temperature and different sustained duration of mix 4. 53
5.9 - Comparison of results of Modulus of Elasticity of different mixes at

different temperature sustained for 4 hours. 54
5.10(a) - Stress Strain Curves for mix 1, at different temperature sustained for 4 hours. 55
5.10(b) - Stress Strain Curves for mix 2, at different temperature sustained for 4 hours. 55
5.10(c) - Stress Strain Curves for mix 3, at different temperature sustained for 4 hours. 56
5.10(d) - Stress Strain Curves for mix 4, at different temperature sustained for 4 hours. 56
5.11 - Modulus of Rupture of different mixes at different temperature. 59
5.12 - Shows the Compressive Strength and Ultra Sonic Pulse Velocity results. 59
5.13 - Shows the Compressive Strength and Young’s Modulus results. 62
5.14 - Shows the Compressive Strength and Flexure Strength results. 62

5.15 - Micrographs of Geopolymer Concrete of mix 4 at different temperatures
sustained for 4 hours. 63
LIST OF PLATES
Plate 1: Preparation of the specimen 22
Plate 2: Specimens kept in Oven for heat curing. 23
Plate 3: Specimens kept in Electric Oven for Elevated Temperature. 25
Plate 4: Specimens showing the change in Colour. 27
Plate 5: Surface cracks, and change in Colour on the specimen. 28
Plate 6: Compression test arrangement. 29
Plate 7: Arrangement for Modulus of Elasticity test. 30
Plate 8: Ultra Sonic Pulse Velocity test. 31
Plate 9: Shows the Arrangement of Flexure Test 33
CHAPTER 1
1.1 INTRODUCTION
Fire represents one of the most severe exposure conditions. So the provisions for appropriate
fire resistance for structural members are major safety requirements in any building design. In
order to predict the fire resistance of a structure, the temperatures in the structures must be
determined. The fire resistance of the structural members is dependent on the thermal and
mechanical properties, at elevated temperatures, of the materials of which the members are
composed. In recent years, the construction industry has shown significant interest in the use of
various newer generations concrete. These concretes are likely to behave differently from the
conventional concrete when exposed to high temperatures. The exposure of concrete to
elevated temperature affects the physical and mechanical properties. Elements could distort
and displace, and under certain conditions, the surface could spall due to the build up of steam
pressure. Because thermally induced dimensional changes, loss of structural integrity, an
release of moisture resulting from the migration of free water could adversely affect the
structures operation and safety, a complete understanding of the behavior of new generation
concrete under long term elevated temperature exposure is essential for reliable design
evaluations.
The demand for cement concrete as a construction material is on the increase. Due to increase
in infrastructure developments, the demand for concrete would increase in the future. 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). The global warming is caused by the emission of
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 ton of Portland
cement emits approximately one ton of CO2 into the atmosphere (Davidovits, 1994c;
McCaffrey, 2002).
One of the efforts to produce more environmentally friendly concrete is to replace the amount
of Portland cement in concrete with by-product materials such as fly ash. An important
achievement in this regard is the development of high volume fly ash (HVFA) concrete that
utilizes up to 60 percent of fly ash, and yet possesses excellent mechanical properties with
enhanced durability performance. The test results show that HVFA concrete is more durable
than Portland cement concrete (Malhotra 2002). Another effort to make environmentally
friendly concrete is the development of inorganic alumina-silicate polymer, called
Geopolymer, synthesized from materials of geological origin or by-product materials such as
fly ash, metakaolin, silica fume, granulated blast furnace slag and rice husk ash, that are rich in
silicon and aluminum (Davidovits 1994, 1999).
In 1978, Davidovits introduced the word geopolymer which was used to describe an
environmentally friendly material which possesses excellent strength and chemical properties.
It also exhibits ceramic like properties with superior resistance to fire at elevated temperature.
The low energy requirements of production from common raw materials and their
inflammability at high temperatures, the geopolymers are attracting increasing interest as
ecologically friendly fire proof building material, sound and heat insulators and materials for
encapsulating hazardous wastes for storage or disposal. In this respect, the geopolymer
technology proposed by Davidovits (1988a; 1988b)shows considerable promise for application
in concrete industry as an alternative binder to the Portland cement. In terms of reducing the
global warming, the geopolymer technology could reduce the CO2 emission to the atmosphere
caused by cement and aggregates industries by about 80% (Davidovits, 1994c).
Fly ash, one of the source materials for geopolymer binders, is available abundantly world
wide, but to date its utilization is limited. From 1998 estimation, the global coal ash production
was more than 390 million tons annually, but its utilization was less than 15% (Malhotra
1999). It is estimated that by the year 2010 the production of the fly ash will be about 780
million tones annually (Malhotra 2002). Accordingly, efforts to utilize this by-product material
in concrete manufacture are important to make concrete more environmentally friendly. For
instance, every million tons of fly ash that replaces Portland cement helps to conserve one
million tons of lime stone, 0.25 million tons of coal and over 80 million units of power, not
withstanding the abatement of 1.5 million tons of CO2 to atmosphere (Bhanumathidas and
Kalidas 2004).
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 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 effect of elevated temperatures on the
fire performance of Fly ash based Geopolymer concrete. Four different mixes were prepared
by varying the aggregate and Fly ash ratio and are subjected to elevated temperatures of
250°C, 400°C, 600°C and 800°C with a sustained duration of 2 hours and 4 hours.
The present investigation is carried out with the following objective:-
 To study the residual properties of Geopolymer concrete in terms of compressive

strength, modulus of elasticity and modulus of rupture.
 To carry out a non-destructive test for determining the homogeneity of the matrix and
aggregates at different temperatures.
 To study the micro-structure of the specimens subjected to different temperatures and

sustained duration.
1.4 SCOPE OF THE STUDY
The experimental work was conducted to obtain the residual strength of the Fly ash based
Geopolymer concrete at elevated temperature. In the experimental work only one source of dry
low-calcium Fly ash (class F) from local power station was used. The tests and analytical
methods that were available for Ordinary Portland Cement were used to predict the results.
1.5 ORGANISATION OF THE THESIS

The second chapter deals with the various investigations carried out by research workers in the
field of study of the performance of geopolymer concrete at elevated temperatures.
Chapter three comprises of the brief introduction of geopolymer materials and the
geopolymerisation process.
Chapter four deals with the materials and the tests carried out on the materials used and the
experimental procedure followed.
The fifth chapter deals with the results and discussion of the experiments.
The sixth chapter includes the important conclusions and scope for future study.
CHAPTER 2
LITERATURE REVIEW
It has been reported very good heat resistant properties of material prepared using sodium
silicate, potassium silicate and metakaolin; having thermal stability up to 1200-1400°C.
Kovalchuk. Investigated heat resistant geopolymer materials manufactured using class F fly
ash, which had good thermal resistance properties up to 800° C.
Geopolymer prepared using either fly ash or metakaolin have frame work structures originating
from condensation of tetrahedral aluminosilicate units varying Al/Si ratio such as (Al- O- Si-
O-) M, (Al-O-Si-O-Si-O-)M,(Si-O-Al-O-Si-O-Si-O-)M etc. M is an alkali ion, typically Na or
K, which balances the charge of the tetrahedral Al [1]. Geopolymer prepared using class F fly
ash are largely amorphous in nature.
Two series of test samples were made, differing in their composition and method of moulding.
In series I samples were prepared using sodium hydroxide, potassium silicate and sodium
silicate solutions, providing 8-9% Na or K in mixtures and water binder ratios of 0.27-0.35.
Water/binder ratio given in this paper was calculated as a ratio of total mass of water to mass
of fly ash. The pastes were cast in plastic cylinders and sealed with the lid. Because of low
flow ability of mixes hand compaction using cylinder plunger was utilized at a filling stage. In
series 2 fly ash samples were prepared using 8-9% Na or K in mixtures and water/binder of
0.09-0.166. In series 2 mixes of very dry consistency were used, thus some of the samples were
pressure compacted. It was shown that prolonged initial curing of samples at room temperature
before the application of heat was beneficial for strength development of geopolymer samples
prepared using fly ash. The method of curing mixtures of series 1 and 2 was the same, initially
samples were cured for 24 hours at room temperature, after that the mixtures were ramped
wither to 80° or 100° C series cured respectively, at 80° -100° C, and cured at this temperature
for 24 hours.
The 25X50mm diameter cylinder samples were exposed to firing at 800°, 1000° and 1200° C
for 4 hours at a heating rate 10° C/min. The polished specimens were used for the SEM
examinations. To prepare the polished specimens, 1mm thick slices were cut from the cylinder
samples using a low diamond saw, impregnated with ultra low viscosity resin and then
polished. For the examination using SEM the polished specimens were carbon coated. X-ray
diffraction analysis of powdered specimen was made using a Rigaku Giegerflex D-max II
automated diffractometer with following conditions: 40kV, 22.5mA, Cu-Kα radiation. The
XRD patterns were obtained by scanning at 0.1° per minute and in steps of 0.05°. The slow
scanning rate was used to improve resolution of peaks. The materials were also analyzed using
mercury intrusion porosimeter to study porosity and average pore diameter before and after
firing.
The strength evolution in geopolymer specimens prepared using sodium containing activator
and w/b in a range of 0.09-0.3. The experiment showed that the specimen prepared at w/b=
0.09 developed shrinkage cracking when exposed to 800 0 C. shrinkage cracking increased with
increase of w/b ratio. After exposure to temperature above 800 0 C strength of all the specimens
0
prepared using Na-containing activator deteriorated rapidly. The specimens cured at 100 C
had initial strength 50-100% higher than that of the specimens cured at 80 0 C. All specimens
had a tendency of increasing strength upon firing. After firing the compressive strength of the
pressure compacted specimens was lower than that of the hand compacted specimen. On firing,
specimens manufacture using pressure 1-3 MPa increased strength up to 30 %, while other non
compacted specimen had strength increased 44%. However, after exposure to temperature
above 8000 C strength of specimen prepared using Na-containing activator rapidly deteriorated.
strength loss was rapid in specimens prepared using heat curing at 1000 C, which had higher
initial strength than specimens cured at 800 C.
The compressive strength of the specimens prepared using potassium silicate and fly ash at
w/b=0.166-0.345 and cured at 800 C to 1000 C. Specimens manufactured using w/b=0.166 were
compacted using applied pressure of 2,6and 10 MPa. The initial strength of 2-5 MPa was
measured for materials prepared at w/b =0.166 and 0.345 and cured at 800 C, while for the
materials prepared at w/b=0.166 and cured at 1000 C the highest compressive strength of 12
MPa was achieved. Materials prepared at w/b= 0.345 and 0.166 and cured at 800 C had a
similar strength evolution after exposure to 8000 ,10000, and 12000 C, achieving maximum
strength of 53 MPa after firing at 10000 C, while further increasing of firing temperature
caused deterioration of strength. The specimen w/b= 0.166 compacted by hand and cured at
1000 C had an increasing strength up to 12000 C. Observation of strength evolution of the
specimens compacted at 2-10 MPa show that pressure compaction does not induce significant
improvement of initial strength, but can be detrimental for strength development on firing.
Materials prepared using K-containing activators had significantly increased their initial
strength, while materials prepared using Na-containing activators had very high loss of strength
at temperature exceeding 8000 C. Previously materials prepared using metakaolin showed
thermal resistance up to 13000 C for sodium polysialate geopolymers and up to 13000C–14000C
for potassium polysialite geopolymers (V.F.F.Barbosa, K.J.D.Mackenzie, 2003) they reported
that increased amounts of water and/or sodium and silicon could cause reduced thermal
resistance of geopolymer material when exposed to firing.
The curing at the elevated temperature increased the initial strength and fire resistance of the
geopolymer materials. Loss of strength on firing was possibly connected to the deterioration of
aluminosilicate gel. After decomposition of the aluminosilicate gel free sodium, silicon, and
aluminum produced Na-feldspars. Presence of the Na- feldspars is responsible for the increase
of porosity and deterioration of strength. here the experimental results indicated that a loss of
compressive strength in materials prepared using Na- containing activator when exposed to
firing was associated with a significant increase of the average pore size and shrinkage
cracking. The presence of significant amounts of iron oxide in the fly ash used for materials
preparation and poor polymerization of geopolymers in samples utilizing fly ash causes
degradation of fire resistance properties of the geopolymer materials.
Densification reduced shrinkage of materials on firing in case of materials activated by Na and

K containing activators. Curing at 800 and 1000 C was utilized in the specimen preparation.
Curing at 1000 C lead to an increased initial compressive strength, and improved fire
resistance, which were attributed to improved activation of fly ash at elevated temperature. The
additional tests need to be performed to verify heat conduction through the layer of
geopolymer when exposed to standard heating curve.
This investigation showed that prepared geopolymer materials compare favorably with organic
polymers, they are non flammable, do not release toxic fumes and have very low weight loss 5-
12 % as compared to 50- 80 % for fire resistant polymer nano composites when heated up to
10000 C. The geopolymer materials were found superior to Portland cement concretes in their
thermal properties when exposed to 8000- 10000 C.
Volume expansion was observed in some of the geopolymer mixes with increased content of
silica it was attributed to expansion on heating of un-combined silica. In this case the
expansion increased with an increase of firing temperature to a point, when a large volume of
foam was produced at 12000 C.
The flyash used in another paper [5], the fly ash used was glassy with some crystalline
inclusions of mullite, hematite and quartz. The chemicals used were sodium silicate solution
and potassium hydroxide flakes of 90% purity, potassium hydroxide solution. The chemicals
were combined to obtain a molarity of 7 molar. The specimens were cured undisturbed for 24
hours at room temperature before being subjected to elevated temperature of 80 0 C for a further
24 hours. Temperature exposed specimens were subjected to temperature of 800 0 C at an
incremental rate of 4.40 C per minute from room temperature. Once the temperature of 8000 C
was attained, it was maintained for a further 1 hour before the specimens were allowed to cool
naturally to room temperature. The compressive strength assessment of concrete specimens
were conducted using load control regime with a loading rate of 20 MPa/min, the specimens
were tested for 3 day strength.
Effect of Sodium Silicate to Potassium Hydroxide on Geopolymer Concrete.

The 3 day compressive strength measurements for fly ash based binder prepared at various
sodium silicate to potassium hydroxide ratios. Ratios ranged from 0.5-2.5 there was a
noticeable improvement in strength with increasing ratio. The curing temperature selected was
800 C. However the observed strength of fly ash-based binder increased after temperature
exposure. This means that the fly ash activation was incomplete within the introduced curing
regime. (24 hour precuring at room temperature and 24 hour elevated curing at 80o C). The
geopolymerisation of the fly ash was only completed as it was exposed to elevated
temperature. Unexposed strengths may be improved by increasing the elevated curing
temperature or by prolonging the curing period.
Fly Ash to Alkaline Silicate Activator Ratio Influence on Geopolymer Paste
The strength performances in terms of fly ash to activator ratio similar to water to cement ratio
typically used as a fundamental method of quantifying compressive strength in OPC. There
was a general decrease in strength when the amount of activator introduced into the system was
increased. The mass of activators is a sum of masses for Na 2SiO3 and KOH. The solids/liquid
ratio contributes to the porosity level of the hardened geopolymer paste. Thus, the solids/
liquids ratio affects the volume of voids in the pastes which directly influences the strength of
the geopolymer. However, the trends were reversed when the activator content was increased.
Consequently lowering the fly ash-to- activator ratio. It was find that the strength of the binder
with lower fly ash-to activator ratio (FA/act = 2.0) decreased after elevated temperature
exposure, unlike previous relations where strength increased after exposure (FA/act = 3.0).
This trend is similar to that of metakaolinite-based binder investigated in the previous work.
Influence of Binder Age on Geopolymer Paste

In order to study the effect of the binder age influence on compressive strengths, the pastes
were prepared at various Na2SiO3 /KOH ratios and tested for 3-day and 7-day strengths. It was
found that there was an insignificant increase in strength when the age at which the specimens
were tested was increased. The chemical reaction of a geopolymer paste is a rapid
geopolymerisation process, the compressive strength does not vary with the age of concrete
when heat accelerated cured for 24 hours. This observation is in contrast to the well known
behavior of a Portland cement, which requires a hydration process and under goes strength gain
over time.(A.M. Neville(1990) properties of concrete).
Influence of Curing Period

The results have indicated that a longer curing period does not significantly affect strength
performances. The authors believe the geopolymerisation of fly ash binder was complete
within the 24 hours of accelerated curing. Van Jaarsveld et al. claimed that curing for longer
periods of time at elevated temperatures appear to weaken the structure. However, the
experimental findings in this section proved other wise within the time frames investigated.
Elevated Temperature Performance of Geopolymer Concrete

The fly ash to activator and Na2SiO3 /KOH ratios were kept constant at 3.0 and 2.5
respectively. Qualitative observations were recorded only after temperature exposure. All
specimens performed very well under exposure to temperature. Apart from decolourisation,
which was similar to the effect observed in the paste, there was no Spalling observed on any of
the concrete cylinders.
Residual strength
The compressive strength of fly ash-based concrete was higher than those recorded in the fly
ash-based paste. The introduction of the aggregates to the geopolymer paste increased the room
temperature strengths from 59.0 MPa to 70.5 MPa and 61.8 MPa for basalt and slag aggregates
respectively. However the strength of the geopolymer concrete decreased after exposed to
elevated temperature. The temperature exposed specimens were weaker than their unexposed
counterparts. The results show a 58 % droop of strength in the basalt based concrete. And a 65
% drop in slag based concrete after temperature exposure. As observed, the phenomenon of
temperature exposed strengths being higher than unexposed strengths does not exist as in the
previous pure paste mixture.
Comparison of geopolymer concrete with the OPC concrete fire performance

The findings above do not necessary substantiate that the geopolymer concrete performed
poorly when exposed to elevated temperature. In fact , the 3-day strength geopolymer concrete
which degraded to 42 % of the original strength was considered to be an improvement
compared the 67-day strength of the high strength concrete (HSC) which reduced to 22 % of
the original strength when subjected to an elevated temperature of 8000 C. So, the performance
of fly ash based binder at elevated temperature declined with the inclusion of aggregates to
make concrete. It is hypothesized that this is caused by the incompatibility and differential
thermal expansion between the aggregates and the binder.
Thermal expansion of geopolymer paste
There was a length change of the geopolymer paste with respect to its original length, lo. When
initially heated upto 1500C, the hardened geopolymer paste expanded. Between 1500C and
2200 C, no further expansion occurred. The geopolymer paste then shrunk between 2200 C and
8000 C. Shrinkage occurred due to the mass loss when subjected to elevated temperature. The
TGA was able to measure the mass loss as a function of temperature. Rapid dehydration
occurred at the peak of the 1200 C to 1300 C heating range. Generally , the total percentage of
mass remaining after being heated to 8000 C averaged at 88.8%. All specimens experienced a
rapid decline in percentage within the first 2000 C and stabilized after until approximately 7000
C. After 7000 C, there was little change in the percentage of mass remaining.
The expansion of concrete at elevated temperature is strongly affected by the aggregates

because aggregates generally occupy 75-80 % of the volume of the concrete. The expansion of
aggregates predominates over the contraction of the geopolymer paste subjected to temperature
beyond 2200 C, which produces a net result of expansion in concrete. Meanwhile, a differential
thermal expansion exists between the aggregates and the paste. The results prove the
hypothesis that the thermal incompatibility relating to the paste and aggregates is the primary
reason for the performance loss at elevated temperatures between the geopolymer paste and
concrete specimens.
CHAPTER 3
GEOPOLYMER MATERIALS AND PROCESS:
3.1 GEOPOLYMER MATERIALS

3.1.1 FLY ASH:
Fly ash is a finely divided residue resulting from the combustion of ground or powdered coal in
electricity generating plant. Fly ash consists of earthly minerals, which include silicon,
aluminum, iron, calcium, magnesium and traces of titanium and organic matter, such as
carbon. The fly ash is solidified while it is being suspended in he exhaust gases, and is
collected from the exhaust gases by electrostatic precipitators. Therefore, fly ash particles are
generally spherical in shape because the solidification process occurs while the solid is in gas
suspension. Furthermore, the collision between particles results in some larger particles or
particles made up of several smaller ones bonded together. The particle size of fly ashes ranges
from <1 to 200 µm, and the particles are typically spherical in shape (Hemmings and Berry,
1988)
The types of coal determine the types of fly ash produced. Generally, anthracite and
bituminous coals produce fly ashes which are classified as Class F fly ash. Class F – being
mainly silica and alumina (80-85 weight %) and < 10 weight % CaO.Class C fly ash is
produced by burning lignite or sub-bituminous coal. Class C fly ash has lower silica and
alumina content, but higher CaO content (20-40 weight %).
3.1.2 ALKALINE LIQUID
In this experimental investigation a combination of sodium hydroxide and sodium silicate

solution was chosen as the alkaline liquid. It is reported that mineral shows a higher extent of
dissolution in sodium based solution than potassium based solution [1]. The sodium hydroxide
was in the form of flakes (commercial grade), with 97% purity. The sodium hydroxide solution
was prepared by dissolving flakes in distilled water (normal). The mass of NaOH solids used in
the solution was of 16 molar. In this experiment 16 molar solution is used, NaOH solution with
a concentration of 16M consisted of 16X40=640 grams of NaOH solids dissolved in one litre
of water, where 40 is the molecular weight of NaOH. In this study 16M sodium hydroxide
solution was used.
A commercially available sodium silicate solution was used. The specific gravity and
chemical composition of such a sodium silicate solution was 1.53 and Na2o=27.62%,
SiO2=32.08%, H2o=40.3% by mass respectively
3.2 GEOPOLYMERISATION PROCESS:
The researchers have reported that binders could be produced by a polymeric reaction of
alkaline liquids with the silicon and the aluminum in source materials of geological origin or
by product materials such as flyash and rice husk ash, metakaoline, blast furnace slag, known
as geopolymers.
Geopolymerisation is a geo synthesis (a reaction that chemically integrates minerals)that

involves naturally occurring silico-aluminates. The silicon(Si)and aluminum(Al)atoms react to
form molecules that are chemically and structurally comparable to those binding natural rock
that allows for products to exhibits the most ideal properties of rock-forming elements namely,
hardness, chemical stability and longetivity.
The synthesis of geopolymer is believed to consist of three steps:

First the dissolution of alumino-silicate under strong alkali solution, second, the reorientation
of ion clusters, and the third, polycondensation. But each step may include many pathways.
Different pathway can create different ion cluster, which directly determine the final properties
of geopolymer. Thus, it is very important to under stand the actual pathway for producing
geopolymer in order to gain insight into the mechanism of geopolymerisation. However, until
now, these mechanisms are not well documented due to rapid rate of formation of geopolymer.
Experimentally it is very difficult to separate out these steps.
Poly(sialates) are chain and ring polymers with Si4+ and AL3+ in coordination
with oxygen and range from amorphous to semi-crystalline with the
empirical
formula:
Mn (-(SiO2) z–AlO2)n . wH2O (2-1)
Where “z” is 1, 2 or 3 or higher up to 32; M is a monovalent cation 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 .
A geopolymer can take one of the three basic forms.
Poly(sialate), which has[-Si-O-Al-O-] as the repeating unit.

Poly(sialate-siloxo), which has [-Si-O-Al-O-Si-O-] as the repeating unit.
Poly(sialate-disiloxo), which has [-Si-O-Al-O-Si-O-Si-O-] as the repeating unit.
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.
(-)
(Si2O5, Al2O2)n + nSiO2 + nH2O NaOH, KOH 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
Unlike ordinary Portland/pozzolanic cements, geopolymers do not form

calcium silicate-
hydrates (CSHs) for matrix formation and strength, but utilize 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, 1994a;
Palomo et. al., 1999; Roy,1999; van Jaarsveld et. al., 2002a).
CHAPTER 4
4.1 EXPERIMENTAL INVESTIGATION
The present experimental work deals with the study of the performance of fly ash based
geopolymer concrete at different elevated temperatures namely 2500 C , 4000 C, 6000 C, 8000 C,
At different sustained durations of 2 hours and 4 hours.
The details of the materials used in the present work, the mix design, method of mixing,
casting of specimen, curing and heating to different temperatures along with the tests carried
out on the heated specimens are explained in this chapter.
4.2 MATERIALS
4.2.1 FLY ASH
Fly ash used in this experimental work is brought from Raichur thermal power station (RTPS)
Karnataka. It is a class F fly ash (the fly ash which contains less than 10 % of the calcium)
which is called low calcium fly ash. The physical characteristics of fly ash was conducted and
the results are tabulated in Table 4.1
Table 4.1 – Physical Characteristics of Fly Ash (RTPS)
Sl No Details Results
1. Specific Gravity 2.05
2. Fineness (Blaine’s air permeability 439
(m2/kg)
Chemical test on fly ash
The chemical test was conducted o the fly ash and the results were tabulated in the Table 4.2
Table 4.2 Chemical Composition of Fly Ash
SL
TEST CONDUCTED RESULTS
NO
Silicon dioxide plus aluminum
1 oxide plus iron oxide, percent 94.40
by mass
Silicon dioxide percent by
2 60.88
mass
Magnesium oxide percent by
3 0.98
mass
Total sulphur as sulphur
4 trioxide. percent by mass, 0.20
(maximum)
Loss on ignition, percent by
5 1.13
mass
4.2.2 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, 4.4, 4.5.
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 (kg/m3) 1536 1290
Dry rodded bulk density 1640 1500
(kg/m3)
Table 4.4 - Sieve Analysis Results of Fine Aggregate
Sieve Size Weight Cumulative Cumulative Zone - Specifications as per

Retained % Retained % Passing
(gm) IS:383-1970 for % Passing
I II III IV
4.75 mm 33 3.3 96.7 90-100 90-100 90-100 95-100
2.36 mm 36 6.9 93.1 60-95 75-100 85-100 95-100
1.18 mm 186 25.5 74.5 30-70 55-90 75-100 90-100
600µ 313 56.8 43.2 15-34 35-59 60-79 80-100
300µ 202 87 13 5-20 8-30 12-40 15-50
150µ 122 99.2 0.8 0-10 0-10 0-10 0-10
Pan 8 - - --- --- --- ---
The fine aggregate tested conforms to Zone-II as per IS:383.
Table 4.5 – Sieve Analysis results of Coarse Aggregate.
Cum.
Wt. retained % Wt.
Sl. No. Sieve size (mm) %Wt. % Passing
(gm) retained
retained
1. 16 0 0 100
0
2. 12.5 200 4 4 96
3. 10 1280 25.6 29.6 70.4
4. 4.75 3200 64 93.6 6.4

Pan 320 6.4 -
5. -
Coarse aggregate tested confirms to the size of 12.5 mm of nominal size of aggregate as per IS
383 – 1970.
4.3 PROPORTIONING OF GEO POLYMER 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.
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 4.6
Table 4.6: Details of Geopolymer Concrete Mixtures
Fly ash (F) NaOH Na2SiO3 Water/Fly

MIX AGGREGATE
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
4.4 PREPARATION OF THE SPECIMEN

All the ingredients were mixed in the laboratory using pan mixer. The capacity of the
pan mixer is 60 liters. Initially all the dry ingredients such as the fly ash, fine aggregates,
coarse aggregates were mixed for 3 minutes, after which, the alkaline solutions were added
which were prepared one day prior and then all the ingredients were mixed thoroughly for 4
minutes.
4.4.1 Casting of the specimen
The mixed concrete is cast in 100X100X100 mm cube, 150X300mm cylinders and

400X75X75mm beams. All specimens were prepared in accordance with IS 516:1959. The
casting of cubes is done in 3 layers. Each layer is given 25 blows with tamping rod and after
completing all the layers, the cube mould was vibrated for 30 seconds on vibrating table.
Similarly, cylinders are cast in 3 layers. Each layer is given 30 blows and after completing the
layers, it is vibrated for 30 seconds. In a similar way beams are also cast and vibrated.
After casting, the specimens were wrapped with a thick plastic cover, to cover the
surface, in order to avoid the evaporation of water during high temperature curing.
Plate 1: Preparation of the specimen
4.4.2 Curing
The curing of the specimens is carried out by subjecting the specimen to a temperature
of 65° C for 20 hours along with the mould. After subjecting the specimen to temperature
curing, the specimens were allowed to cool down to ambient temperature and then de moulded
and wrapped in thick polythene bags and kept for air curing for further 7 days.
Plate 2: Specimens kept in Oven for Heat Curing
4.5 DETAILS OF SPECIMENS
For each mix of geo polymer concrete and each test temperature and each sustained duration 3
specimens are considered. To compare the properties of geo polymer concrete before and after
subjecting to elevated temperature. For each mix 3 controlled specimens were also cast.
GPC
MIX 1 MIX 2 MIX 3 MIX 4

45.9 MPa 49.2 MPa 86.9 MPa 94.9 MPa
250 DEG
400 DEG
600 DEG
800 DEG
Figu
2 hour 4 hour
3 specimens
from each mix
re 4.1: Details of the specimens subjecting to different temperature and different

sustained duration.4.6
4.6 EXPOSING THE SPECIMENS TO ELEVATED TEMPERATURE
The specimens were subjected to elevated temperature for specified duration in a special
heating chamber of size 2.1 X 1.1 X 1 m. the chamber is heated through electrical coil and is
capable of attaining a max temperature of 10000 C.
The oven is installed below the ground with top sliding cover at ground level. Electrical
sensors are provided in the oven to measure the temperature inside the oven. The temperature
is controlled in the control panel in which the temperature can be set to required degree and can
be maintained to required time without any increase or decrease in the temperature.
The specimens were heated in electric oven and were kept in such a way, leaving equidistance
from each sample, so that all the sides of the samples could be exposed to heat. As the heat
reached to the testing temperature, this temperature is maintained constantly for the required
period such as 2hours and 4 hours, the rate of temperature rise was set as 50 C per minute.
After exposing the samples to the required temperature and for required duration the heating of
the samples was stopped and was allowed in the electric oven to cool down. Later on when
oven cooled down to ambient temperature, the specimens were taken out and were wrapped in
the plastic bag and kept for observation and testing. Three specimens were tested for each
exposed and for each sustained duration, only the average values are reported.
Plate 3: Specimens kept in Electric Oven for Elevated Temperature
4.7 TEST CONDUCTED
The tests proposed are such that they indicate the degradation, changes in strength properties
due to exposure to elevated temperature. The residual properties were measured in terms of
compressive strength, modulus of elasticity and modulus of rupture. In addition, ultra-sonic
pulse velocity test was conducted and densities of concrete were also measured to observe the
possible variations.
4.8 PHYSICAL OBSERVATIONS
Before the specimens were subjected to various tests, the physical changes after exposing the
specimen to different temperature and for different sustained duration were observed. The
observation includes change in dimensions, colour, development of cracks etc. The
observations are furnished in the Table. 5.1.
4.8.1 Change in colour

Similar to Portland cement concrete, geopolymer concrete exhibits change in colour, when
exposed to elevated temperature the change in colour observed is as follows:
Upto 250° C, which was sustained for 2 hours and 4 hours, there was no change in
colour, the colour remained the same as that of unheated specimen.
 @ 400° C which was sustained for 2 hours and 4 hours, in these specimens exhibit slight
pink colouration.
 @ 600° C which was sustained for 2 hours and 4 hours, the change in the colour of the
specimen was quite prominent. The specimen turned pink mixed with brown colour.
 @ 800° C which was sustained for 2 hours and 4 hours, the specimen exhibits brown
colour. The colour of the aggregates and the matrix had turned into brown colour, as
observed from the crushed specimen.
Plate 4: Specimens showing the change in Colour
4.8.2 Aggregates
Commonly used aggregates are thermally stable up to 650° C. At higher temperature when the
specimen was subjected to compression test, it was observed that the failure occurs not only in
the interfacial vicinity between aggregates and geopolymer but failure occurs through the
aggregates. These aggregates were so weak that they could be crushed very easily by hand.
This shows that the aggregates at higher temperatures was unstable and become very weak.
4.8.3 Cracks
The specimen which was subjected to 250° C and 400° C temperature for 2 hours and 4 hours
did not show any cracks. Where as specimens that was subjected to 600° C and 800° C for 2
hours and 4 hours sustained duration showed surface cracks, and these cracks were
predominantly in the matrix. The micro cracks observed on the surface were in the form of
map cracking.
Plate 5: Surface Cracks, and change in Colour on the specimen
4.8.4 Spalling
Spalling was not observed in any of the specimens which were subjected to different high
temperatures at different sustained temperature.
The physical observation of the specimens in terms of colour and cracks are shown in the
Table.5.1.
4.9 COMPRESSIVE STRENGTH TEST
Tests were carried out to find out the effect of elevated temperatures on the residual
compressive strength. The compressive strength of the cubes exposed to elevated temperatures
are tested after 7 days curing.
Concrete cubes, 100X 100 X 100 mm in size were tested for compressive strength as per IS:
516-1959. The cubes were centrally placed in the compression testing machine of capacity
3000 KN and load was applied gradually and uniformly without shock. The loading rate was
adjusted to 140Kg/cm2/min. The load was applied until the specimen fails and the maximum
load carried by each specimen during the test was recorded. From the failure load compression
strength of each specimen is calculated. The results obtained are presented in Tables 5.6-5.9
and Figures 5.5-5.8.
Plate 6: Compression test arrangement
4.10 MODULUS OF ELASTICITY IN COMPRESSION
The cylindrical specimens of 150X300 mm dimensions were used to test modulus of elasticity
in compression, the test was performed with universal testing machine which has a capacity of
3000 KN. The test is carried out based on the guide lines in IS 516-1959. The aluminum angles
were attached to the cylinder surface to measure the average strain. These were attached at the
distance of gauge length to hold the dial gauge. An electronic dial gauge capable of measuring
deformation up to 0.001mm was used. Loading was done in three cycles the loading rate was
140 kg/sq cm/min until an average stress of (C+5) kg /sq cm is reached where C is one third of
average compressive strength of the cube calculated to the nearest 5 kg/sq cm. The load is
maintained for one minute and then reduced gradually to 1.5 kg/sq cm till the reading is noted.
The same rate of loading is carried on to the second cycle of loading until an average stress of
(C+1.5) kg/sq cm is reached and the load is reduced gradually to 1.5 kg/sq cm. The third cycle
of loading and unloading is done similar to second cycle. Unusual behavior of any, was
corrected during the second and third loading. The applied load and longitudinal deformation
was noted. These readings were plotted on stress vs. strain graph. The slope of the initial linear
portion of the curve is taken as the modulus of elasticity.
Plate 7: Arrangement for Modulus of Elasticity test
4.11 ULTRA SONIC PULSE VELOCITY TEST

To assess the change in microstructure of the geopolymer concrete subjected to high
temperature, the Specimens were subjected to Pulse velocity test as per 13311-Part 1. The
equipment used - PUNDIT has a time measurement capability of 0.1 micro seconds. The time
taken by the ultrasonic pulse to travel through the specimen between transducer and receiver
held in contact with the specimen was noted. The path length divided by the time taken gives
the pulse velocity. The quality grading of the cement concrete based on the values are given in
the Table 4.7.
Plate 8: Ultra Sonic Pulse Velocity test
Table 4.7 Velocity Criterion for Cement Concrete Quality Grading

(Ref. 13311-Part -1:1992)
Sl.No UPV for cement concrete Concrete Quality
(Km/Sec) grading
1 Above 4.5 Excellent
2 3.5 to 4.5 Good
3 3.0 to 3.5 Medium
4 Below 3.0 *Doubtful
This table is used as a guide line to verify the UPV values and quality grading of geopolymer
concrete.
4.12 MODULUS OF RUPTURE
The flexure test was carried out on the specimens of 75X75X400 mm dimensions. The
test was performed with two points loading in the flexure testing machine. In the bed of testing
machine two steel rollers of 38 mm dia are provided on which the specimen is placed which
serves as support point. The load is applied through two similar rollers mounted at the third
points of the supporting span, the load was divided equally between two rollers. The load is
applied axially and without subjecting the specimen to any torsional stress or restraints and the
maximum load (P)at failure is noted.
The modulus of rupture was calculated using the formula 2PL/bd2.
• Where , P= the applied load.

• L= length of the specimen.
• B= breadth of the specimen.
• D= depth of the specimen.
The results are furnished in the Table 5.11. and in Figure 5.14.
Plate 9: Arrangement of flexure test
CHAPTER 5
RESULTS AND DISCUSSION

5.1 PHYSICAL OBSERVATION
The physical observation made on the geo polymer concrete specimens regarding the
colour, propagation of cracks and spalling soon after heating the specimens to high
temperatures are reported below
5.1.1 Discolouration
The discolouration in geopolymer concretes exposed to elevated temperatures can be attributed
to the changes in iron compounds present in the constituent materials such as fly ash, fine
aggregates and coarse aggregates. Flyash being present in significant quantities contributes
considerable amount of iron compounds into the mix and hence, the discoloration is
prominently observed in geopolymer concretes.
The duration of the temperature exposure seems to have no effect on the discolouration, since
the samples exposed to duration of 2 hours and 4 hours do not exhibit any difference in
discolouration.
The change in colour can be used as a tool to arrive at the probable temperature exposure in
geopolymer concrete, as in the case of Portland cement concrete.
5.1.2 Aggregates
The aggregates, when exposed to high temperature were found to be unstable and were very
weak this is due to the action of heat on the aggregate. As the aggregate composed of many
minerals, which may under go crystal transformation at high temperatures and also may under
go expansion causing cracks making the aggregate very weak and unstable.
5.1.3 Cracks
The appearance of the cracks can be attributed to the contraction of the mortor due to water
evaporation. The contraction is higher than that of cement concrete due to higher fine content
present in geopolymer concrete.
5.1.4 Spalling
No Spalling was observed in any of the specimens which were subjected to different high
temperatures at different sustained temperature. This is because of the formation of the micro
cracks which were seen on the specimens. Since there will be a lot of water pressure inside the
specimen when it is heated to high temperature, the formation of micro cracks will reduce the
pressure. These micro cracks create the path for the water vapour to escape from the specimen.
But where as in Portland cement concrete the spalling can be seen. This is because there may
not be micro cracks at the higher temperature, which results in the built up of water pressure
inside the specimen. This pressure causes the spalling of specimen as the temperature is raised.
Table.5.1. Physical Observation of the specimens in terms of Colour and Cracks.
Temperature Duration Change in Cracks

Colour
2500 C 2H No change No cracks

2500 C 4H No change No cracks
4000 C 2H Slight pink No cracks
4000 C 4H Slight pink No cracks
6000 C 2H Pink mix brown Surface cracks

6000 C 4H Pink mix brown Surface cracks
8000 C 2H brown Surface cracks
8000 C 4H brown Surface cracks
5.2 RESULTS OF ULTRA SONIC PULSE VELOCITY TEST

The pulse velocity transmission depends on the quality of concrete such as density, presence of
micro cracks, pores etc., in geopoymer concrete the increase in temperature causes degradation
in the matrix due to formation of micro cracks. Further at higher temperatures coarse
aggregates also cracks, increasing micro cracks in concrete. This is clearly shown in the UPV
readings. Apart from this more pores are observed at a temperature of 600° C and above, as a
result the ultra sonic pulse velocity values are also less. The period of sustain temperature of 2
hours and 4 fours has no effect on ultra sonic pulse velocity readings.
The continuous decrease in pulse velocity values are almost same for the specimens which
were subjected to increasing temperature @ different sustained durations. The graph shows
that the UPV values are increasing as the compression strength increase. Where as, the UPV
values when compared with the different temperatures shows the variation. The results are
tabulated in the Tables 5.2- 5.5 and Figures 5.1-5.4.
The results of the specimen when subjected to a elevated temperature of 800° C shows the
lesser values of UPV when compared to the results of the specimens subjected to the increasing
temperatures of 250° C,400° C, and 600° C . This is because at 800° C the matrix will become
very porous which results in the poor values of UPV.
Note: The value zero in the X-axis is referred as ambient temperature in the Figures
5.1- 5.4.
Table 5.2 Ultra Sonic Pulse Velocity test results for the specimens subjected to different
temperature and different sustained duration for mix 1.
Mix 1 Temperature in 0 C Pulse velocity in KM/S

Duration
(45.90 N/mm2)
2 hours 4 hours
Controlled 3.7 3.7
250 2.1 1.8
400 1.5 1.6
600 1.0 1.0
800 0.8 0.8
UPV TEST
4
3.5
3
UPV Km/s
2.5
2 2 HOUR
1.5
1
0.5
0
0 200 400 600 800 1000
TEMPERATURE DEGREES
Figure 5.1(a)Ultra Sonic Pulse Velocity test of the specimen sustained for 2 hours
subjected to different temperature for mix 1.
UPV TEST
4
3.5
3
UPV Km/s
2.5
4 HOUR
2
1.5
1
0.5
0
0 200 400 600 800 1000
TEMPERATURE DEGREES
Figure 5.1(b)Ultra Sonic Pulse Velocity test of the specimen sustained for 4 hours
UPV TEST
4
3.5
3
2.5
UPV Km/s
2 HOUR
2 4 HOUR
1.5
1
0.5
0
0 200 400 600 800 1000
TEMPERATURE DEGREES
Figure 5.1(c) Ultra Sonic Pulse Velocity test results for the specimens subjected to
different temperature and different sustained duration for mix 1.
Mix 2 Temperature in 0 C Pulse velocity in KM/S

Duration
(49.20 N/mm2)
2 hours 4 hours
Controlled 3.9 3.9
250 2.2 1.9
400 1.7 1.6
600 1.1 1.0
800 0.8 0.8
UPV TEST
4
UPV Km/s
3
2 HOUR
2
0
0 200 400 600 800 1000
TEMPERATURE DEGREES
UPV TEST
UPV Km/s 3
4 HOUR
2
0
0 200 400 600 800 1000
TEMPERATURE DEGREES
UPV TEST
4.5
4
3.5
3
UPV Km/s
2.5 2 HOUR
2 4 HOUR
1.5
1
0.5
0
0 200 400 600 800 1000
TEMPERATURE DEGREES
Table 5.4 Ultra Ssonic Pulse Velocity test results for the specimens subjected to different
Mix 3 Temperature in 0 Pulse velocity in KM/S

(86.93 N/mm2) C Duration
2 hours 4 hours
Controlled 3.9 3.9
250 2.0 2.1
400 1.7 1.8
600 1.1 1.1
800 0.9 0.9
UPV TEST
4
UPV Km/s
3
2 HOUR
2
1
0
0 200 400 600 800 1000
TEMPERATURE DEGREES
UPV TEST
4
UPV Km/s
3
4 HOUR
2
1
0
0 200 400 600 800 1000
TEMPERATURE DEGREES
UPV TEST
4
UPV IN Km/s
3 2 hour
2 4 hour
0
0 200 400 600 800 1000
TEMPERATURE IN DEGREES
Figure 5.3 Ultra Sonic Pulse Velocity test results for the specimens subjected to different
Mix 4 Temperature Pulse velocity in KM/S

(94.93 N/mm2) in 0 C Duration
2 hours 4 hours
controlled 4.0 4.0
250 2.1 2.0
400 1.7 1.7
600 1.1 1.0
800 1.0 0.9
UPV TEST
4
UPV Km/s
3
2 HOUR
2
0
0 200 400 600 800 1000
TEMPERATURE DEGREES
UPV TEST
UPV Km/s
3
4 HOUR
2
0
0 200 400 600 800 1000
TEMPERATURE DEGREES
UPV TEST
4
UPV Km/s
3 2 HOUR
2 4 HOUR
0
0 200 400 600 800 1000
TEMPERATURE DEGREES
5.3 RESULTS OF COMPRESSIVE STRENGTH TEST:
The reduction in the strength of mix I (7 day strength was 45.9 N/mm2) @ 250° C was 45%
from there on wards the reduction in the strength is not very significant. the reduction was very
slow, maximum reduction of Mix I has occurred @ 800° C which is about 64%, the variation
in strength of specimens exposed to different temperature for duration of 2 hours and 4 hours
was not significant.
The reduction in the strength of Mix II (7 day strength was 49.2 N/mm2) @ 250° C was about
49% and the further increase in the temperature did not cause much variation in the strength,
The maximum reduction occurred @ 800° C sustained at 4 hours it was about 58%. Here also
the variation in strength of specimens exposed to different temperature for duration of 2 hours
and 4 hours was not significant.
The Mix-III (7 day strength was 86.93 N/mm 2) falls under high strength concrete category.
Initially it was tested @ 250° C where the reduction in the strength was 65%. So as to access
the large variation of strength it was tested for 150° C and found that there was a reduction in
strength. This shows that the decrease in strength is linear from 150° to 250° C and also for
further temperatures. The geopolymer concrete strength starts decreasing from 150° C and the
decrease was about 35% of the 7 day strength for this mix. The maximum reduction occurred
was about 76% in which the specimen was exposed to 800° C.
It reveals that the decrease in strength result follows the same trend as that of Portland cement
concrete in which it suffers a loss 55% to 70% of its original strength when it reached @ 550°
C (B.Georfali, P.E.Tsakiridis- Microstructure of fire damaged concrete, A case study).
In mix IV (7 day strength was 94.93 N/mm2) the loss of strength observed was about 35% ,
when the specimen was exposed to 250° C, and maximum of 75% loss in strength when it is
exposed to 800° C. This loss of strength may be due to the expansion or contraction between
the geo polymer and aggregates. As it is well known that aggregate plays a significant role in
the strength when they are subjected to elevated temperature. In this case this is due to the
differential expansion and contraction of the aggregates and geo polymer paste.
The geo polymer paste starts contracting between 150° C and 220° C the aggregate starts
expanding[5], which results in the incompatibility between geo polymer paste and aggregate
results in the reduction of strength. The results of the compressive strength test are tabulated in
the Tables 5.6 -5.9 and Figures 5.5-5.8.
In Portland cement@ 300° C strength reduction would be in the range of 15-40% (B.Georgali,
P.E.Tsakiridis) from the previous works and from literature review. It is well known that
percentage reduction in strength in high strength Portland cement concretes are lesser when
compared to normal strength Portland cement concrete when exposed to high temperatures
(T.Morita et al, “Residual Mechanical Properties of high strength concrete members exposed to
high temperature- part I”)
Note: The value zero in the X-axis is referred as ambient temperature in the Figures
5.5- 5.8.
Table 5.6 Compressive Strength test results of the specimens subjected to different
Mix 1 Temperature Compressive Percentage Compressive Percentage
(45.90 N/mm2 in 0 C strength in MPa decrease in strength in decrease in
Duration 2 hours strength MPa strength
(N/mm2) Duration (N/mm2)
4hours
controlled 45.9 - 45.9 -
250 24.53 46.55 24.1 47
400 23.4 49 22.43 52
600 22.6 50 17.93 61
800 16.36 64 17.3 62
com pression test
50
compressive strength
40
30
MPa
2 hr
20
10
0
0 200 400 600 800 1000
tem perature in degrees
Figure 5.5(a) Variation of the Compressive Strength of specimens sustained for 2 hours at
different temperature for mix 1.
com pression test
50
compression strength
40
30
MPa
4 hr
20
10
0
0 200 400 600 800 1000
Figure 5.5(b) Variation of the Compressive Strength of specimens sustained for 4 hours
at different temperature for mix 1.
compression test
50
compression strrength
40
2 hr
30 4 hr
MPa 20
10
0
0 200 400 600 800 1000
Figure 5.5(c) Variation of the Compressive Strength of specimens sustained for different
duration at different temperature for mix 1.

(49.20 N/mm2 in 0 C strength in MPa decrease in strength in decrease in
Duration 2 hours strength MPa Duration strength
(N/mm2) 4hours (N/mm2)
controlled 49.2 - 49.2 -
250 27.8 43 23.49 52
400 24.73 49 23.43 52
600 21.5 56 23.53 52
800 22.1 55 20.57 58
compression test
60
50
40
MPa
30 2 hour
20
10
0
0 200 400 600 800 1000
te m pe rature in degree s
compression test
60
50
40
MPa
30 4 hour
20
10
0
0 200 400 600 800 1000
tem perature in degree
compression test
60
50
40
2 hour
MPa 30
4 hour
20
10
0
0 200 400 600 800 1000
Figure 5.6(c) Variation of the Compression Strength at different temperature and

different sustained duration for mix 2.

(86.93) in 0 C strength in MPa decrease in strength in decrease in
N/mm2 Duration 2 hours strength MPa Duration strength
(N/mm2) 4 hours (N/mm2)
Controlled 86.93 - 86.93 -
150 56 35.5 56 35.5
250 30.27 65 26.5 69.5
400 27.97 67.8 24.07 72
600 22.17 74 24.17 73
800 20.03 77 20.90 76
compression test
100
80
MPa 60
2 hour
40
20
0
0 200 400 600 800 1000
compression test
100
compresive strength
80
60
MPa
4 hour
40
20
0
0 200 400 600 800 1000
Figure 5.7(b) Variation of the compressive strength of specimens sustained for 4 hours at
compression test
100
80
60 2 hour
MPa
40 4 hour
20
0
0 200 400 600 800 1000
Figure 5.7(c) Variation of the compression strength at different temperature and

different sustained duration for mix 3.

(94.93) in 0 C strength in MPa decrease in strength in decrease in
N/mm2 Duration 2 hours strength MPa strength
(N/mm2) Duration (N/mm2)
4hours
controlled 94.93 - 94.93 -
250 61.47 35 51.3 46
400 41.9 56 40.2 57
600 33.8 64.4 31.67 66.6
800 23.3 75 25.5 73
compression test
100
80
60
MPA
2 hour
40
20
0
0 200 400 600 800 1000
tem pe rature in degrees
compression test
100
80
60
MPa
4 hour
40
20
0
0 200 400 600 800 1000
temperature in degrees
compression test
100
compressive strength MPa 80
60 2 hour
40 4 hour
20
0
0 200 400 600 800 1000
Figure 5.8 Variation of the compression strength of specimens at different temperature

and different sustained duration of mix 4.
5.4 RESULTS OF MODULUS OF ELASTICITY TEST:
Tests were carried out to find out the effect of elevated temperatures on the modulus of
elasticity in compression on geopolymer concrete. The sensitivity of variation in elasticity at
lower strain was measured and hence initial tangent modulus was calculated. Three specimens
were tested and the initial tangent modulus was drawn and then was normalized to get an
average value. The test results here shows that the rate of compressive strength reduction in
cubes due to high temperature is more when compared to reduction in modulus of elasticity.
The results are tabulated in the Table 5.10 and are represented in Graphical form 5.9.
In this test it can be observed that the values of young’s modulus increase with increase in
compression strength up to a certain increase in temperature. After that the young’s modulus
decrease with increase in compression strength.
This is because the specimen will be suffering lack of stiffness due to the evaporation
of the liquid content in the matrix. Which will make the specimen to under go deformation
when subjected to compressive stress.
Table 5.10 Results of modulus of elasticity of geopolymer concrete.
Temperature in Modulus of elasticity in N/mm2 Elasticity ratio =Residual modulus of

0
C sustained elasticity / Modulus of elasticity of the
for 4 hours control specimen
Mix1 Mix2 Mix3 Mix4 Mix1 Mix2 Mix3 Mix4
controlled 3077 35046 44786 48369 1.0 1.0 1.0 1.0
4
400 2059 21003 27595 18335 0.669 0.599 0.616 0.379
9
600 1866 19678 23284 18614 0.606 0.561 0.519 0.384
5
800 1799 17563 23132 16404 0.584 0.501 0.516 0.339
4
RESIDUAL MODULUS OF ELASTICITY

RATIOES OF MIX 1,2,3& 4
MODULUS OF ELASTICITY
0.8
MIX 1
0.6
RATIOES
MIX 2
0.4
MIX 3
0.2
MIX 4
0
400 600 800
TEMPERATURE IN DEGREE
Figure 5.9 Comparison of results of Modulus of Elasticity of different mixes at different
temperature sustained for 4 hours.
7
compressive stress in N/mm2
4
400 deg,mix1
3
600deg,mix1
2
800deg,mix1
1
Poly. (400
0 deg,mix1)
Poly.
0 0.0002 0.0004 0.0006 (600deg,mix1)
Poly.
compressive strain
(800deg,mix1)
Figure 5.10(a) Stress strain curves for mix 1, at different temperature sustained for 4
hours.
8.0000
7.0000
6.0000
5.0000
400deg,mix2
4.0000
3.0000 600deg,mix2
2.0000 800deg,mix2
1.0000
Poly.
0.0000
(400deg,mix2)
0.00000 0.00050 0.00100 Poly.
com pr es s ive s train (600deg,mix2)
Poly.
(800deg,mix2)
Figure 5.10(b) Stress strain curves for mix 2, at different temperature sustained for 4
hours.
9.00000
8.00000
7.00000
6.00000
5.00000 400deg, mix3
600deg, mix3
4.00000 800deg, mix3
3.00000
2.00000
1.00000
0.00000
0.000 0.000 0.001
00 50 00
Compressive strain
Figure 5.10(c) Stress strain curves for mix 3, at different temperature sustained for 4
hours
7.0000

6.0000 400 deg,mix 4
5.0000 600 deg,mix4
4.0000 800 deg,mix 4
3.0000
Poly. (400
2.0000 deg,mix 4)
Poly. (600
1.0000 deg,mix4)
Poly. (800
0.0000 deg,mix 4)
0.000 0.000 0.000 0.000
00 20 40 60
compressive strain
Figure 5.10(d) Stress strain curves for mix 4, at different temperature sustained for
4 hours
5.5 RESULTS OF MODULUS OF RUPTURE TEST
The modulus of rupture test was carried out to find out the effect of elevated temperatures on
geopolymer concrete. Higher the strength, higher is the loss of flexure strength. It is evident
from the results that mix 3 and mix 4 has higher loss of strength compared to mix 1 and mix 2.
As mix 3 and mix 4 are high strength mixes. This is because for higher strength mix lesser is
the water to fly ash ratio when these specimens are heated to higher temperature there will be a
loss of water in the mix which results in the weaker bond in the matrix, more porous are
formed, more micro cracks are developed totally the specimens become very dry which
resulted in the heavy loss of strength in the high strength mixes. The results are tabulated in
Table 5.11 and also represented Graphically 5.11.
It can be seen that as the compression strength increases the flexure values is also increasing.
But the flexure values when compared with the different temperatures shows the variation. The
results of the specimen when heated to a elevated temperatures of 800° C shows the lesser
values of flexure when compared to the results of the specimen subjected to 400° C and600° C.
This shows that when the specimens were heated to high temperature they tend to loose their
strength. Here the temperature plays a key role in decreasing the flexure values.
Table 5.11 Modulus of Rupture test results of the specimens subjected to different
temperature and different sustained duration.
Mix Modulus of rupture in N/mm2

Temperature in degree
Controlled 400 600 800
1 8.175 2.915 0.785 1.845
2 8.96 3.41 0.85 1.985
3 12.515 3.415 1.205 2.06
4 13.3 3.55 1.065 2.135
Table 5.12 Compressive Strength and Ultra Sonic Pulse Velocity results.
MIX TEMPERATURE COMPRESSIVE UPV IN Km/s

STRENGTH
MIX 1 AMBIENT 45.9 3.7

MIX 2 49.2 3.9
MIX 3 86.93 3.9
MIX 4 94.93 4.0
MIX 1 250 DEGREES 45.9 1.8

MIX 2 49.2 1.9
MIX 3 86.93 2.1
MIX 4 94.93 2.0
MIX 1 400 DEGREES 45.9 1.6

MIX 2 49.2 1.6
MIX 3 86.93 1.8
MIX 4 94.93 1.7
MIX 1 600 DEGREES 45.9 1.0

MIX 2 49.2 1.0
MIX 3 86.93 1.1
MIX 4 94.93 1.0
MIX 1 800 DEGREES 45.9 0.8

MIX 2 49.2 0.8
MIX 3 86.93 0.9
MIX 4 94.93 0.9
MODULUS OF RUPTURE
MODULUS OF RUPTURE IN
14
12
10 AMBIENT
8 400 DEG
MPa
6 600 DEG
4 800 DEG
2
0
0 1 2 3 4 5
DIRRERENT MIXES
Figure 5.11 Modulus of Rupture of different mixes at different temperature.

UPV VS COMPRESSION STRENGTH
UPV in Km/s 4 AMBIENT

250 DEG
3
400 DEG
2
600 DEG
1 800 DEG
0
45.9 49.2 86.93 94.93
COMPRESSION STRENGTH in MPa
Figure 5.12 Compressive Strength and Ultra Sonic Pulse Velocity results.
Table 5.13 Compressive Strength and Young’s Modulus results.
MIX TEMPERATURE COMPRESSIVE YOUNG’S

STRENGTH
MPa MODULUS
MIX 1 AMBIENT 45.9 30774
MIX 2 49.2 35046
MIX 3 86.93 44786
MIX 4 94.93 48369
MIX 1 400DEGREES 45.9 20599

MIX 2 49.2 21003
MIX 3 86.93 27595
MIX 4 94.93 18335
MIX 1 600DEGREES 45.9 18665

MIX 2 49.2 19678
MIX 3 86.93 23284
MIX 4 94.93 18614
MIX 1 800DEGREES 45.9 17994

MIX 2 49.2 17563
MIX 3 86.93 23132
MIX 4 94.93 16404
Table 5.14 Compressive Strength and Flexure Strength results.
MIX TEMPERATURE COMPRESSIVE FLEXURE

STRENGTH STRENGTH
MIX 1 AMBIENT 45.9 8.175

MIX 2 49.2 8.96
MIX 3 86.93 12.51
MIX 4 94.93 13.3
MIX 1 400 DEGREES 45.9 2.915

MIX 2 49.2 3.41
MIX 3 86.93 3.415
MIX 4 94.93 3.55
MIX 1 600 DEGREES 45.9 1.865

MIX 2 49.2 1.985
MIX 3 86.93 2.06
MIX 4 94.93 2.135
MIX 1 800 DEGREES 45.9 0.785

MIX 2 49.2 0.85
MIX 3 86.93 1.205
MIX 4 94.93 1.065
YOUNGS MODULUS VS COMPRESSIVE
STRENGTH
YUMGS MODULUS IN
60000
50000
ambient
40000
400 deg
MPa
30000
600 deg
20000
800 deg
10000
0
0 20 40 60 80 100
COMPRESSIVE STRENGTH IN MPa
Figure 5.13 Compressive Strength and Young’s Modulus results.
FLEXURE STRENGTH VS COMPRESSIVE

STRENGH
FLEXURE STRENGTH IN
14
12
10 AMBIENT
8 400 DEG
MPa
6 600 DEG
4 800 DEG
2
0
0 20 40 60 80 100
COMPRESSIVE STRENGTH IN MPa
Figure 5.14 Compressive Strength and Flexure Strength results.

5.6 SEM RESULTS
Figure 5.15 Micrographs of Geopolymer Concrete of mix 4 at different temperatures

Sustained for 4 hours.
Mix 4, unexposed to temperature

Mix 4, exposed to 2500 C, sustained for 4 hours.

SEM results of the mix 4 specimens sustained for 4 hours for different temperatures.
Mix 4 , ambient temperature specimen
The matrix can be seen as dense compact geopolymeric reaction product indicating complete
reaction of particles. Some unreacted fly ash particles can also be seen. Small micro pores of
the order of 1-2 microns can also be seen which are probably formed at the process of
polymerization due to expulsion of water.
Mix 4, 2500 C, sustained for 4 hours.
The dense compact matrix appears to be disintegrating and the interfacial separation of
geopolymer concrete matrix along with the aggregates can be seen. How ever still some
unreacted fly ash particles found sticking to the geopolymer matrix, and it is also generally
seen more number of voids which are likely due to the result of expulsion of water.
Mix 4, 4000 C , sustained for 4 hours.
There is a visible evidence of paste tending towards the process of sintering. More visible
pores can be seen, disintegrated matter from the original compact paste can be seen deposited.
Further more disassociation of fly ash particles from the surface are observed which might
have resulted in the reduction of compression strength.
It can be seen that there is more disintegration of paste and sintering process has taken place.
The compact paste as seen in micrograph is completely disintegrated and appears like a
sintered texture, more pores can be seen, and unreacted fly ash particles totally disassociated or
detached indicating the lack of binding. Similar trends can be observed in the specimens which
were sustained for 2 hours at different temperatures.
CHAPTER 6
SUMMARY AND CONCLUSIONS
6.1 SUMMARY
The present investigation work was carried out to find out the effect of elevated
temperature on the relative performance of fly ash based geopolymer concrete in terms of their
residual properties and temperature ranging from 250 º C to 800 ºC which were sustained for 2
hours and 4 hours. The residual properties of all the specimens in terms of strength, modulus of
elasticity and modulus of rupture were measured. A non destructive test was also conducted to
assess the quality of the specimens exposed to different temperature ranges. SEM
investigations were carried out to know the change in the microstructures at different
temperatures and at different durations.
6.2 CONCLUSIONS
From the present experimental investigation the following conclusion can be drawn:
1. The physical observations such as change in colour micro cracks on surfaces can give
the valuable information regarding the temperature exposure of geopolymer concrete.
2. From the results of different sustained temperature duration studies, it can be
concluded that the strength reduction of the geopolymer concrete depends more on the
temperature to which it is subjected, but not on the sustained duration.
3. From the studies it can be concluded that geopolymer concrete of higher strength (86.9
N/mm2and 94.9 N/mm2 ) have shown reduction in strength at 2500 C and 4000 C at
much higher rate than the geopolymer concrete of medium strength concrete ( 45.9
N/mm2 and 49.2 N/mm2 ).
4. Based on the study conducted on the modulus of elasticity and modulus of rupture it
can be concluded that the reduction in the properties is similar to that of compression
strength.
5. The reduction in strength is considerable to the extent of 65 % at 2500 C beyond which
the rate of reduction in strength reduces with the increase in temperature, 74 % up to
6000 C and 77 % up to 8000 C. the tests have indicated that up to 2500C the reduction
in strength is linear.
6. Ultra sonic pulse velocity measurements can be used effectively to access the quality
of the geopolymer concrete. The ambient specimens results show the high values due
to density. But after heating, the ultra sonic pulse velocity measurements was less due
to the formation of large number of pores.
7. At ambient temperature the ultra sonic pulse velocity results on geopolymer concrete
are comparable to that of cement concrete, how ever, at elevated temperature due to
formation of interface cracks between aggregates and matrix, and degradation of the
matrix rapid reduction in ultra sonic pulse velocity values are evident in geopolymer
concrete.
8. From scanning electron microscope study it can be concluded that at elevated

temperature the geopolymer concrete under goes degradation both in terms of inter
face crack formation at matrix and aggregates and degradation of matrix itself resulting
in sintering. At temperature beyond 6000 C the formation of interface cracks appears to
be influencing the mechanical properties more than that of matrix degradation.
6.3 SCOPE FOR FUTURE STUDY
1. The future study on the geopolymer concrete can be focused on trying with different
curing temperature and different durations.
2. The study can be focused on different ratios of sodium silicate solution and sodium
hydroxide solution.
3. The studies related to different thermal expansion of aggregates, matrix can be

taken up separately to understand the individual behaviour which can through
more light on the geopolymer concrete
4. The residual strength and bond strength of geopolymer concrete to steel

reinforcement can be studied with different types of reinforcing bars at elevated
temperatures.
5. Experiment can be conducted by using the fly ash from different sources.
6. The amount and the size of the pores can be found at elevated temperatures since
geopolymer concrete becomes more porous at high temperatures.
REFERENCES
1. S.E.Wallah and B.V.Rangan “ Low Calcium Fly Ash Based Geopolymer Concrete;
Long Term Properties” Research Report GC2 (2006), Curtin University of Technology
Perth, Australia.
2. D.Hardjito, B.V.Rangan (2005) “Development and Properties of low-calcium Fly Ash
Based Geopolymer Concrete” Research Report GC1 Curtin University of Technology
2005.
3. D.J.Sumajouw and B.V.Rangan “Low-calcium Fly Ash Based Geopolymer Concrete”
Research Report GC3 Curtin University of Technology 2006.
4. Sindhunatha “ A Conceptual Model of Geopolymerisation” Bachelor of Engineering
(Hons), Department of Chemical and Biomolecular Engineering, University of
Melbourne.
5. Daniel Kong, Jay Sanjayan and Kwesi Sagoe “The Behaviour of Geopolymer Paste and
Concrete at Elevated Temperatures” Department of Civil Engineering, Monash
University, Clayton, Australia.
6. T.Bakharev “Thermal Behaviour of Geopolymers Prepared Using Class F Fly Ash and
Elevated Temperature Curing” Department of Civil Engineering, Monash University,
Australia.
7. R.V.Ranganath, Mohammed Saleh, Sreenivasulu.T “Geo-Polymer –An alternative to
cement based materials”, National conference on Recent trends in Concrete
Technology, Kongo College of Engineering, Erode, March 2007.
8. Ana M.Fernandez-Jimenez, Angel Palomo, and Cecilioi Lopez-Hombardos
“Engineering Properties of Alkali-Activated Fly Ash Concrete” ACI Material Journal,
March-April 2006, pp 106-111.
9. Zhang Yunshen and Sun Wei, “Fly Ash Based Geopolymer Concrete”, The Indian
Concrete Journal, Jan 2006, pp 20-24.
10. IS: 13311, Part I, (1992), Non-Destructive Testing of Concrete-Methods of Testing,
Ultrasonic Pulse Velocity, BIS, New Delhi.
11. IS:516 – 1959 (Reaffirmed 1999), Methods of Tests for Strength of Concrete, New
Delhi.
12. IS:383 – 1970 Specification for Coarse and Fine Aggregate

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“PERFORMANCE OF GEOPOLYMER CONCRETE AT ELEVATED

VISWESVARAIAH TECHNOLOGICAL UNIVERSITY,

In partial fulfillment of the requirements for the award of the degree of

Department of Civil Engineering

VISVESWARAIAH TECHNOLOGICAL UNIVERSITY,

In partial fulfillment of the requirements for the award of the degree of

Department of Civil Engineering

This is to certify that the dissertation entitled an “PERFORMANCE OF

Dr. Sakey Shamu Dr. R. V. Ranganath

Mr. M. S. Sudarshan Dr. M. K. Venkatesha

Examiners: Signature with Date

I, the undersigned declare that this dissertation work entitled “PERFORMANCE OF

GEOPOLYMER CONCRETE AT ELEVATED TEMPERATURE”, is a bonafide work

of post graduate degree of Master of Technology in Construction Technology of

the guidance of Dr. Sakey Shamu & Mr. M. S. Sudarshan in B. M. S. College of

university or institution for the award of any degree.

I am grateful to Dr. R. V. Ranganath, Head of the Civil Engineering Department, B. M. S.

The discovery of geopolymers is a breakthrough which provides a cleaner and

CHAPTER 2 LITERATURE REVIEW 6

CHAPTER 3 GEOPOLYMER MATERIALS AND PROCESS

3.1 Geopolymer materials 13

CHAPTER 4 EXPERIMENTAL INVESTIGATIONS

4.1 Experimental investigation 18

CHAPTER 5 RESULTS AND DISCUSSIONS

5.1 Physical observations 34

CHAPTER 6 SUMMARY AND CONCLUSIONS

4.2 - Chemical composition of Fly Ash 18

4.3 - Physical Characteristics of Aggregates 18

4.4 - Sieve Analysis Results of Fine Aggregate 19

4.5 - Sieve analysis results of Coarse Aggregate. 19

4.6 - Details of Geopolymer Concrete Mixtures 20

4.7 - Velocity criterion for Cement Concrete Quality Grading 31

5.1 - Physical Observation of the specimens in terms of Colour and Cracks. 34

5.10 - Shows the results of Modulus of Elasticity of Geopolymer Concrete. 54

5.13 - Shows the Compressive Strength and Young’s Modulus results. 60

5.14 - Shows the Compressive Strength and Flexure Strength results. 61

5.5(a) Variation of the Compressive Strength of specimens sustained for 2

5.5(b) Variation of the Compressive Strength of specimens sustained for 4

5.5(c) Variation of the Compressive Strength of specimens sustained for

5.6(a) Variation of the Compressive Strength of specimens sustained for 2

5.6(b) Variation of the Compressive Strength of specimens sustained for 4

5.6(c) Variation of the Compression Strength at different temperature and

5.7(a) Variation of the Compressive Strength of specimens sustained for 2

5.7(b) Variation of the compressive strength of specimens sustained for 4

5.8(a) Variation of the Compressive Strength of specimens sustained for 2

5.8(b) Variation of the Compressive Strength of specimens sustained for 4

5.8(c) Variation of the compression strength of specimens at different

5.9 - Comparison of results of Modulus of Elasticity of different mixes at

5.11 - Modulus of Rupture of different mixes at different temperature. 59

5.13 - Shows the Compressive Strength and Young’s Modulus results. 62

5.14 - Shows the Compressive Strength and Flexure Strength results. 62

Plate 2: Specimens kept in Oven for heat curing. 23

Plate 3: Specimens kept in Electric Oven for Elevated Temperature. 25

Plate 4: Specimens showing the change in Colour. 27

Plate 5: Surface cracks, and change in Colour on the specimen. 28

Plate 6: Compression test arrangement. 29

Plate 7: Arrangement for Modulus of Elasticity test. 30

Plate 8: Ultra Sonic Pulse Velocity test. 31

Plate 9: Shows the Arrangement of Flexure Test 33

1.2 NEED FOR THE PRESENT STUDY

 Increasing green house gases.

The present investigation is carried out with the following objective:-

 To study the residual properties of Geopolymer concrete in terms of compressive