1

CHAPTER 1

INTRODUCTION

1.1 GENERAL

Nanotechnology is one of the most active research areas that encompass a

number of disciplines, including civil engineering and construction materials. It
seems to hold the key that allows construction and building materials to replicate the
features of natural systems improved until perfection for millions of years.
Traditionally, nanotechnology has been concerned with developments in most of the
fields like microbiology, medicine, electronic, chemical, and materials sciences.
However, the potential for application of many of the developments in the
nanotechnology field in the area of construction engineering has been growing.
Nanotechnology is the use of very small particles of materials either by themselves
or by its manipulation to create new large scale materials.
Nano, which comes from the Greek word for dwarf, indicates a billionth. One nano
metre is a billionth of a metre. Definitions of 'nanotechnology' vary, but it generally
refers to understanding and manipulation of matter on the Nano scale, say, from 0.1
nm to 100 nm. The significance and importance of controlling matter at the nanoscale
is that at this scale different laws of physics come into play like quantum physics.
There are two ways to approach the nanoscale: shrinking from the top down, or
growing from the bottom up. The 'top down' approach entails reducing the size of the
smallest structures towards the nanoscale by machining and etching techniques,
whereas the 'bottom up' approach, often referred to as molecular nanotechnology,
implies controlled or directed self-assembly of atoms and molecules to create
structures.
 2

Addition of nanoscale materials into cement could improve its performance.

Use of nano-SiO2 could significantly increase the compressive for concrete,
containing large volume fly ash, at early age and improve pore size distribution by
filling the pores between large fly ash and cement particles at nanoscale. The
dispersion/slurry of amorphous nano silica is used to improve segregation resistance
for self-compacting concrete. It has also been reported that adding small amount of
carbon nanotube (1%) by weight could increase both compressive and flexural
strength.

Many disciplines of civil engineering, including design and construction

processes, can be benefited from nanotechnology. These include products that are
for: Lighter structure, Stronger structural composites, e.g. for bridges and others. Low
maintenance coating, Improved pipe joining materials and techniques, Better
properties of cementitious materials, Reduced thermal transfer rate of fire retardant
and insulation, Increased sound absorption of acoustic absorber, Increased reflectivity
of glass, water repellents, nano-clay filled polymers, self-disinfecting surfaces, UV
light protector, air cleaners, nano-sized sensors, and solar cells.

1.2 NANO SILICA

Nano-materials are commonly defined as the materials with a diameter less
than 100 nm or with the specific surface area > 60 m2 /g. Nano silica is the common
name for silica nanoparticles with diameter in the range of 5-100 nm and high specific
surface area. These particles are approximately 1000 times smaller than the average
cement particles. It is mainly used for thickening, flattening and reinforcing of the
matrixes in various fields. Due to finer particle size of nano silica as compared to
micro silica, its physical and chemical effects are more extensive. Nano silica
particles possess high pozzolanic activity and also act as filler, resulting
 3

in homogeneous, dense and compact microstructure. It drastically improves the

mechanical, chemical and physical properties of the cement structures.

1.3 CEMENT MORTAR

Cement mortar is the most widely used building compound made by mixing
cement and fine aggregates with the required amount of water in compliance with
Indian standard code, IS 2250-1981. It is basically used as a paste for binding together
of various construction blocks such as bricks, stones, cinder blocks, etc and other
forms of masonry such as plastering over bricks or other. The quality of cement
mortar is characterized in terms of its mobility, placeability, water retention, strength
and durability that further depend upon its constituent materials. A good mortar
should be economical, easily workable, capable of good adhesion, durable and
resistant to chemical attack.

1.4 NEED FOR STUDY

Utilization of ultra fine nano silica particles in cement mortar fill the voids in
the cement matrix and reduce the pore volume along with pore size refinement and
disconnecting the capillary action of the pores. As a result, the chemical resistance of
the cementitious structure increases and water permeability of cement matrix
decreases. The nucleation effect of nano silica particles facilitate hydration reaction
and further develop the microstructure leading to arresting of cracks. The high
reactivity of nano silica particles decreases the setting time of the mortar and results
in early hardening. The ultra fine nano silica particles exhibit enhanced pozzolanic
activity with better reaction with calcium hydroxide resulting from the hydration of
C3S to form comparatively more and highly stiff CSH gel that renders the ITZ denser
and results in the formation of more homogeneous, uniform microstructure. Thus, it
results in reduction of the crystallization of calcium hydroxide that
 4

decreases the performance of cement mortar/concrete. As a result, the strength and

durability of cementitious structure increases.

1.5 OBJECTIVES

1) To evaluate the effect of NS on fresh properties of cement paste/mortar

including consistency, setting time and workability.
2) To evaluate the effect of NS on hardened properties of cement mortar
including compressive strength at various curing ages.
3) To evaluate the effect of NS on durability properties of cement mortar
including corrosion attack.
4) To compare the pozzolanic behavior of NS through micro structural analysis
by SEM & XRD studies.

5) To determine the optimized content of individual NS with varied percentages

 5

CHAPTER 2

LITERATURE REVIEW

2.1 GENERAL

Some of the literatures had been collected to do the project and that was listed below.
They had discussed about the nano material as a partial replacement in mortar.

2.2 REVIEW OF LITERATURE

P.Janani, S.Ganeshkumar, M.Harihananth (2016)

Mechanical Properties of Nano Silica Concrete: This experimental work was

carried out to investigate the strength of the mechanical properties of Nano silica
concrete and compared with the normal cement concrete. In this study, the Nano silica
is used as a supplementary cementitious replacement material for cement. The silica
has been subjected to ball milling technique and the size of Nano silica has been
confirmed to its characterization by Scanning Electron Microscope (SEM) analysis.
The Compression test is conducted for various percentage replacements of silica to
find the optimum percentage of silica replacement. From the test, 23% replacement
of cement to silica achieves the maximum strength. Hence, the mechanical properties
such as Compression, Tensile and Flexural strength test were experimentally studied
with 23% of cement replaced with Nano silica and the results were compared with
that of Normal Cement Concrete (NCC).
 6

Mr. L. Ranjith Kumar, Q. Roger, P. Santhosh, K.Gowtham, E.D. Jothi Rajan

(2016)

Durability Study of Concrete Using Nano-Silica: The development of construction

materials technology, particularly concrete is growing very rapidly in the presence of
nanotechnology. One of the materials that deserve the attention of researchers is
nanosilica. Use of Nano silica is gaining importance due to its vital characteristics,
which helps in developing concrete. In this the influence of nanosilica on durability
of concrete has been investigated. For this purpose 2.5% of nanosilica has been added
to concrete mixture by replacing some amount of cement. Also the admixture plaster
of paris is used to increase workability .In this M25 grade of concrete is used.
Durability has been investigated through Water absorption, Sorptivity and Acid
attack test. Results of this study showed that nanosilica can be effective in improving
the durability of concrete.

Jing Xu, David J. Corr, Surendra P. Shah (2015)

Nano mechanical investigation of the effects of nanoSiO2 on C-S-H gel/cement

grain interfaces: In this paper, nano indentation and visco elastic modulus mapping
were employed to study the influence of nanoSiO2 on the properties of the interface
between C-S-H gel and cement grains. The interface width measured by modulus
mapping was around 200 nm as compared to a rough estimation of less than 5 μm by
nano indentation, due to the fact that 2 orders of magnitude increase in spatial
resolution can be achieved with modulus mapping. Although the influence of
nanoSiO2 on the interface width was not significant, its impact on nano mechanical
properties of the interface was marked. The data suggest an improvement of modulus
and hardness of the interface by nanoSiO2 in early age. This interface,
 7

which could be regarded as a layer surrounding cement grains, becomes denser by

the addition of nanoSiO2.

Peng Zhang, Xiao-Bing Dai, Ji-Xiang Ga and Peng Wang (2015)

Effect of nano-SiO2 particles on fracture properties of concrete composite

containing fly ash: A parametric experimental study has been conducted to
investigate the effect of nano-SiO2 particles on fracture properties of concrete
composite containing fly ash. Five different nano-SiO2 contents were used for this
study. By means of three-point bending method, the fracture parameters of the
effective crack length, initial fracture toughness, unstable fracture toughness, fracture
energy, critical crack opening displacement, maximum crack opening displacement
and maximum mid-span deflection of the beam specimen were measured. The results
reveal that the addition of lower SiO2 content (<5%) nano- particles may help
improve the fracture properties of concrete composite containing fly ash. Nano-SiO2
has a significant effect on the fracture relational curves of the three-point bending
beam specimen. The fracture parameters increase gradually and the fracture relational
curves become thicker as the nano-SiO2 content increases from 0% to
5%.However,thefracture parameters begin to decrease and the curves become thinner
when the nano-SiO2 content exceeds 5%.These variation rules of fracture parameters
and fracture relational curves indicate that nano-SiO2 contributes significantly to the
improvement of fracture properties of concrete composite containing fly ash only
when its content does not exceed 5%.

Ye Qian, Yaghoob Farnam and Jason Weiss (2014)

Using Acoustic Emission to Quantify Freeze–Thaw Damage of Mortar

Saturated with NaCl Solutions : Mortar samples were saturated with NaCl
 8

solutions of various concentrations and subjected to freeze–thaw cycles. Passive and

active acoustic emission (AE) testing was conducted. The freezing temperature of the
NaCl solutions in mortar corresponded with the sudden observation of passive AE
events. The acoustic energy and damage parameter were calculated to evaluate the
extent of freeze–thaw damage. The influence of the NaCl solution concentration and
whether the solution freezes on freeze–thaw damage are discussed.

S. Tanveer Hussain, K.V.S.Gopala Krishna Sastry (2014)

Study of strength properties of concrete by using micro silica and nano silica:
Nano technology is one of the most promising areas of science. The use of nano
materials in concrete is new revolution. Nano materials like nano silica, nano titanium
oxide, carbon nanotubes, nano alumina etc. which are presently used in concrete to
modify its strength properties. In the present study strength properties such as
Compressive strength, split tensile strength and flexural strength of M40 and M50
grades of concrete with the use of micro silica (5%,7.5%,10%,15%) and nano silica
(1%,1.5%,2%, 2.5%) as partial replacement of cement were studied. It was found
from the experimental study that concrete composites with superior properties can be
produced using micro silica, nano silica and combination of micro silica and nano
silica

A. E. Al-Salami and M. A. Al-Gawati (2013)

Pozzolanic Activity of Nano-Silica and Its Application for Improving Physical,

Mechanical and Structural Properties of Hardened Cement: The aim of this work
is to investigate the pozzolanic activity of nano-silica (NS) prepared by sol-gel
method and to study its application for improving physical, mechanical and structural
properties of hardened blended cement. The NS was mixed with calcium
 9

hydroxide (CH) by different ratios 10%, 20%, 30% and 50% using water to CH ratio
of 0.35, the mixtures were kept at relative humidity 100% for 7 days. After curing for
7 days, the reactions mechanisms were investigated by differential scanning
calorimeter (DSC),X-ray diffraction (XRD) and scanning electron microscope
(SEM). It was found that, NS consume the CH and produce calcium silicate hydrate
(CSH) (strength responsible phase in cement). The ratio of CH consumed increases
with increasing NS ratio. The studied NS was characterized by great reactivity i.e. it
is a good pozzolanic material that can be used for improving cement and concrete
properties. Blended cement paste samples were prepared by partial replacement of
cement by different ratios of NS 0.5%, 1%, 1.5%, 2 % and
2.5 %. The compressive strength, capillary water absorption and microstructure of
NS-blended characteristics were studied at 28 days of curing. An enhancement in
compressive strength by about 21% was obtained at 2% of NS. Capillary water
absorption was reduced with increasing NS ratio. The reduction rate was 18.29 % at
2% of NS. The microstructure of NS-blended cement appeared quite dense and
compact with less micro pores.

Sayed ABD EL-BAKY, Sameh YEHIA, Ibrahim S. KHALIL (2013)

Influence of nano-silica addition on properties of fresh and hardened cement

mortar: The aim of this study is to investigate the influence of adding nano-silica
particles, on the properties of fresh and hardened cement mortar through
measurements of workability, compressive and flexure strengths in addition
to measuring by SEM analysis. Nano-silica particles with size of 19 nm have been
used as a cement addition by 1, 3, 5, 7 and 10 % by weight of cement content. Results
indicated that the cement mortar workability decrease with increasing nano-silica
addition. On the other hand, the percentage of 7 % of nanosilica recorded as
optimum percentage in compressive and flexure strength
 10

measured for cement mortar mixed with the nano-silica. The improvement in
compressive and flexure strength measured as 55.7% and 46.9 % respectively,
compared with the conventional mortar, especially at early ages. In addition, the
scanning electron microscope (SEM) analysis of the microstructures showed that the
nano silica filled the cement paste pores, more homogeneity for cement paste and
interfacial zone, by reacting with calcium hydroxide crystals forming more calcium
silicate hydration.

Jonbi, Ivindra Pane, Binsar Hariandj, Iswandi Imran (2012)

The Use of Nano silica for Improving of Concrete Compressive Strength and
Durability: The development of construction materials technology, particularly
concrete is growing very rapidly in the presence of nanotechnology. One material that
deserves the attention of researchers is nano silica. Silica has been used on concrete,
starting from silica sand as filler to micro silica (silica fume) as a reactive pozzolanic.
Based on previous research, silica fume is proven effective to improve the mechanical
properties and durability of concrete. A novel nano technological process allows
producing amorphous nano silica with high reactivity from locally available silica
sand. In this study locally available nano silica is used on mortar and concrete thereby
limiting the use of commercial nano silica materials from semiconductor industry
waste. To obtain sustainable concrete, the mix is design to have high strength as well
as low permeability using as much possible local sources. This study also makes use
of commercial, regular silica fume combined with the locally produced nano silica.
The results show that combined use of nano silica with silica fume can increase the
compressive strength and durability.
 11

Ali Nazari, Shadi Riahi (2010)

The effects of SiO2 nanoparticles on physical and mechanical properties of high

strength compacting concrete: In this work, compressive, flexural and split tensile
strengths together with coefficient of water absorption of high strength self
compacting concrete containing different amount of SiO2 nanoparticles have been
investigated. Strength and water permeability of the specimens have been improved
by adding SiO2 nanoparticles in the cement paste up to 4.0 wt %. SiO2 nano particle
could accelerate C–S–H gel formation as a result of increased crystalline Ca(OH)2
amount especially at the early age of hydration and increase the strength of the
specimens. In addition, SiO2 nanoparticles are able to act as nano fillers and recover
the pore structure of the specimens by decreasing harmful pores. Several empirical
relations have been presented to predict flexural and split tensile strength of the
specimens by means of compressive strength at a certain age of curing. Accelerated
peak appearance in conduction calorimetry tests, more weight loss in thermo
gravimetric analysis and more rapid appearance of peaks related to hydrated products
in X-ray diffraction results, all also indicate that SiO2 nanoparticles up to 4% weight
could improve the mechanical and physical properties of the specimens.

Masayasu ohtsu, Toshiro Isoda and Yuichi Tomoda (2007)

Acoustic Emission Techniques Standardized For Concrete Structures: Acoustic

emission (AE) techniques have been extensively applied to concrete structures.
Results achieved are currently going to be standardized for the inspection and
evaluation of infrastructures in service. Test results associated with these
standardization activities for concrete structures are discussed. In order to assess the
damage levels of the structures, the Japanese Society for Non-Destructive Inspection
has established the recommended practice (NDIS 2421). Two AE indices
 12

of load ratio and calm ratio are defined for qualification of the damages. It is
demonstrated that damages qualified are in good agreement with actual damages of
reinforced concrete members. AE behavior of concrete under compression could be
analyzed, applying the rate process analysis. By evaluating intact moduli of elasticity
from AE database, relative damages of concrete cores taken from a road bridge are
quantitatively estimated. The standards contain a monitoring method for active cracks
in concrete by AE (JCMS-III B5706). The classification of cracks is successfully
applied to investigate the corrosion process of reinforcing steel-bars in concrete. The
moment tensor analysis of AE can identify cracking kinematics of location, crack-
type and crack orientation, which has been implemented as SiGMA procedure.
Nucleation of micro-cracking due to the expansion of corrosion product is studied. It
is found that the mechanisms of corrosion cracking at the meso-scale are really made
up of tensile, shear and mixed-mode cracks, while the surface crack and the diagonal
cracks of mode I are observed at the macro-scale. These results will form the basis
for proposing RILEM recommendations.

D.F. Lin, K.L. Lin, W.C. Chang, H.L. Luo, M.Q.Cai (2007)

Improvements of nano-SiO2 on sludge/fly ash mortar: Sewage sludge ash has been
widely applied to cementitious materials. In this study, in order to determine effects
of nano-SiO2 additives on properties of sludge/fly ash mortar, different amounts of
nano-SiO2 were added to sludge/flyash mortar specimens to investigate their physical
properties and micro-structures. A water-binding ratio of 0.7 was assigned to the mix.
Substitution amounts of 0%, 10%, 20%, and 30% of sludge/fly ash (1:1 ratio) were
proposed. Moreover, 0%, 1%, 2%, and 3% of nano-SiO2 was added to the mix. Tests,
including SEM and compressive strength, were carried out on mortar specimens
cured at 3,7 and 28 days. Results showed that sludge/fly ash
 13

can make the crystals of cement hydration product finer. Moreover, crystals increased
after nano-SiO2 was added. Hence, nanoSiO2 can improve the effects of sludge/fly
ash on the hydration of mortar. Further, due to the low pozzolanic reaction active
index of sludge ash, early compressive strengths of sludge/fly ash mortar were
decreased. Yet, nano-SiO2 could help produce hydration crystals, which implies that
the addition of nano-SiO2 to mortar can improve the influence of sludge/flyash on the
development of the early strength of the mortar.

Byung-Wan Jo, Chang-Hyun Kim, Ghi-ho Tae, Jong-Bin Park (2005)

Characteristics of cement mortar with nano-SiO2 particles: The properties of

cement mortars with nano-SiO2 were experimentally studied. The amorphous or
glassy silica, which is the major component of a pozzolan, reacts with calcium
hydroxide formed from calcium silicate hydration. The rate of the pozzolanic reaction
is proportional to the amount of surface area available for reaction. Therefore, it is
plausible to add nano-SiO2 particles in order to make high- performance concrete.
The experimental results show that the compressive strengths of mortars with nano-
SiO2 particles were all higher than those of mortars containing silica fume at 7 and
28 days. It is demonstrated that the nano-particles are more valuable in enhancing
strength than silica fume. In addition, the continuous hydration progress was
monitored by scanning electron micrograph (SEM) observation, by examining the
residual quantity of Ca(OH)2 and the rate of heat evolution. The results of these
examinations indicate that nanoscale SiO2 behaves not only as a filler to improve
microstructure, but also as an activator to promote pozzolanic reaction.
 14

Tao Ji (2005)

Preliminary study on the water permeability and microstructure of concrete

incorporating nano-SiO2: Water permeability resistant behavior and microstructure
of concrete with nano-SiO2 were experimentally studied. A water permeability test
shows that, for concretes of similar 28-day strength, the incorporation of nano-SiO2
can improve the resistance of water penetration of concrete. An ESEM test reveals
that the microstructure of concrete with nano-SiO2 is more uniform and compact than
that of normal concrete. Mechanism about the effect of nano-SiO2 on concrete is
described.

Hui Li, Hui-gang Xiao, Jie Yuan, Jinping Out (2003)

Microstructure of cement mortar with nano-particle: The mechanical properties

of nano-Fe2O3 and nano-SiO2 cement mortars were experimentally studied. The
experimental results showed that the compressive and flexural strengths measured at
the 7th day and 28th day of the cement mortars mixed with the nano-particles were
higher than that of a plain cement mortar. Therefore, it is feasible to add nano-
particles to improve the mechanical properties of concrete. The SEM study of the
microstructures between the cement mortar mixed with the nano-particles and the
plain cement mortar showed that the nano-Fe2O3 and nano-SiO2 filled up the pores
and reduced CaOH2 compound among the hydrates. These mechanisms explained the
supreme mechanical performance of the cement mortars with nano-particles
 15

A.K. Maji and R. Sahu (2002)

Acoustic Emissions from Reinforced Concrete: Acoustic emissions from

reinforced-concrete beams, reinforcing bars and plain concrete cylinders were
monitored. Acoustic emission events were used in a study of source locations,
frequency characteristics, and other analytical methods that have found use in the past
for evaluating acoustic-emission data in other fields of engineering.-Tests were done
on reinforced-concrete beams under flexural loading, individual reinforcing bars
under pure tension, concrete cylinders under compression, and reinforcing bars
subject to pullout tests. The experimental data were first analyzed with conventional
acoustic-emission methodology. A critical look at many acoustic-emission
techniques currently used in other materials (metals, composites, etc.) demonstrated
some of the difficulties of applying the same techniques to reinforced concrete. More
importantly, it illustrated the limitations of signal processing and parameter
estimation of acoustic-emission events as viable non destructive evaluation (NDE)
techniques for reinforced-concrete structures. Subsequently, on the basis of the
experimental results, some of the more promising aspects of developing acoustic
emission into a structural monitoring tool are discussed.
 16

CHAPTER 3

METHODOLOGY

This chapter deals with the details of methodology used for the study of the effect of
incorporating nano silica (NS) as a partial substitution of cement in cement mortar.

The following methodology has been followed in this experimental investigation.

 Preliminary tests on cement, fine aggregate, and nano silica are done.
 Mix proportion for cement mortar by using nano silica.
 Fresh property tests were conducted to find setting time and flowability for
cement mortar with and without nano silica for varying percentages.
 Casting of mortar cubes for compressive strength test and durability test with
and without nano silica are done.
 Casting of acoustical sample with and without nano silica is done.
 Compressive strength tests were carried out at the end of 7, 14 and 28 days
for cement mortar cube specimens of size 7.06cm.
 Durability was found out by steel corrosion attack test at the end of 28 days.
 Microstructure analysis for cement mortar was studied using SEM and XRD.
 17

CHAPTER 4

EXPERIMENTAL INVESTIGATION

4.1 GENERAL

This chapter presents the details of materials used, mix proportions, details of test
specimens and testing method adopted. Basic tests were conducted on cement, fine
aggregate, nano silica and water to check their suitability for cement mortar making.

4.2 MATERIALS USED

The various materials used in this investigations include cement, fine aggregate, nano
silica and water as described here.

4.2.1 CEMENT

The Ordinary Portland Cement (OPC) is generally used for major construction
practices conforming to IS 269-2013 (33 grade), IS 8112-2013 (43 grade) and IS
12269-2013 (53grade). It is the prime constituent of cement mortar and acts as a
binder due to its high pozzolanic behavior. The most commonly available Ordinary
Portland cement of 43 Grade was used for the investigation.

4.2.1.1 TESTS ON CEMENT:

A) Fineness of Cement :
Fineness of cement is carried out to check proper grinding of cement. It should be
checked with the sieve of 90 micron. It is the measure of surface area of cement
particles for Ordinary Portland cement, the fineness by weight should not be more
than 10%.

Weight of sample taken = W1 g

Weight of residue = W2 g
 18

Fineness of cement = W2 / W1
= (5.71/100) * 100
= 5.7%

B) Consistency Test on Cement :

(IS 5513: 1996 specimen for Vicat needle apparatus)

 The percentage of water required for obtaining cement paste of standard

consistency is determined using Vicat needle apparatus with 10mm diameter
and 50mm long plunger.
 Several trial pastes are prepared with varying percentage of water and the test
in conducted until the needle penetrated 5mm to 7mm above the bottom of the
mould.
Table 4.1 Consistency of Cement

Weight of Quantity of cement added

Trail No. Penetration
cement % Ml
1 400 24 96 22
2 400 25 100 17
3 400 27 108 9
4 400 28 112 5
5 400 30 120 4

The percentage of water required for obtained cement paste of standard

consistency is 28%.
 19

C) Initial and Final Setting time of Cement:

Setting time test is used to detect the deterioration of cement of due to storage. When
water is mixed with cement to form a paste, chemical reaction starts. The action of
changing of the cement paste from fluid state to solid state is called setting. It purely
depends on the quantities of Gypsum contained in it. To test the setting time, needle
of 1 mm square section is used.
The time that elapsed between the moment when water is first added to the cement
and the moment at which the needle failed to pierce the test block to a depth 5+-
0.5mm from the bottom of the mould is the Initial setting time for the cement under
the test.
The time that elapsed between the moment when water is first added to the cement
and the moment of which the needle only makes an impression on the test block, at
which the attachment fails to do is the Final setting time for the cement under the test.
The minimum initial setting time specified by IS 269, for Ordinary Portland cement
and rapid hardening cement is to be not less than 30 minutes and 60 minutes for low
heat cement. As per IS 4031, the maximum time for final setting for all types of
cement is to be not more than 10 hours.

Initial Setting time of cement

Type of cement = Chettinad cement – OPC 43grade
Weight of cement taken = 400 g
Consistency percentage of water = 28% = 112 ml
Volume of water added = 0.85x112 = 95.20 ml
 20

Table 4.2 Setting Time of Cement

Initial setting Penetration

Trial Remark
Time (min) Index reading

1 0 0 Needle 1 mm Square reaction

2 10 1
3 20 3
4 30 4

5 35 5.5 Final reading 5+- 0.5mm from

base plate.

Initial setting time = 35 minutes

Final setting time = 400 minutes

D) Specific gravity of Cement :

Table 4.3 Specific gravity of Cement

Description Weight (g)

Weight of empty Pycnometer (W1) 120

Weight of Pycnometer + Cement (W2) 200

Weight of Pycnometer + Cement + Kerosene (W3) 410

Weight of Pycnometer + Kerosene (W4) 355

Specific gravity G =
()()
 21

= ()()

= 3.15

4.2.2 FINE AGGREGATE:

Aggregate of size less than 4.75 mm are usually called as fine aggregate. Sand is
used as fine aggregate in mortar. The important functions of fine aggregate are
 To produce workability and uniformity for concrete.
 To assess the cement paste to hold the particles of coarse aggregate in
suspension and to prevent paste to hold the possibility of segregation.
 To fill up the voids in the coarse aggregate.
The sand to be used in mortar should be free from any chemicals, salts, clay,
silt, dust and organic matters should be completely passed through IS sieve of
4.75mm size and retain completely in IS sieve of 150µ size. A well graded siliceous
quartz and which contains almost all size grains in equal proportion is best suited for
mortar work. Angular grained sand is preferable to round grained sand since it
provides good interlocking properties.

4.2.2.1 TESTS ON FINE AGGREGATE:

A) Fineness modulus of Fine Aggregate:

Fineness modulus is defined as the empirical value obtained by adding the cumulative
percentage of the material retained by weight in each of a series of sieves and dividing
the total thus obtained by 100.
 22

Table 4.4 Fineness modulus of Fine Aggregate

Cumulative
Size of sieve Weight of % weight % of passing
% weight
(mm) residue (gm) retained (100-C)
retained (C)
4.75 - - - 100
2.36 20 2 2 98
1.18 375 37.5 39.5 60.5
0.60 250 23 62.5 37.5
0.30 345 34.5 97 3
0.15 20 2 99 1
0.075 10 1 100 0
Pan - - - 0

Fineness modulus = = 3

B) Specific gravity of fine aggregate:

 Specific gravity of sand is the ratio of its weight in air to the weight of an equal
volume of water at temperature of 40C.
 Specific gravity of sand is an important factor which is used in computing
other properties of sand like degree of saturation, void ratio and its unit weight.
Weight of empty pycnometer (W1) = 610 g
Weight of pycnometer + dry sand (W2) = 1120 g
Weight of pycnometer +sand+water (W3) = 1825 g
Weight of pycnometer& water (W4) = 1505 g
(W -W1)
Specific gravity of fine aggregate =
(W W
- )1 W
- W3- 4)
 23

-
=
( - )- -

= 2.68

C) Bulk density :
Bulk density of sand is the ratio between the weight of sand and its volume.
Percentage of voids represents the ratio between the volume of voids and total volume
including solid matter and voids.
Diameter of cylinder D = 10 cm
Height of the cylinder H = 5 cm
Weight of empty cylinder = w1 = 1415 gm
Weight of empty cylinder + loose sand = w2 = 2015 gm
Weight of sand in loose condition =W2 – W1 = 2015-1415 gm = 600 gm
Volume of the cylinder V = (22/7) * D2/4 = (22/7) * 0.12/4
= 3.926 * 10-4 m3
Bulk density of fine aggregate = W/V = 0.6/ 3.926* 10-4
= 1604.28 kg/m3

4.2.3 NANO SILICA:

Nano silica is available from natural resources in the form of crystalline mineral silica
such as quartz, tridymite, cristobalite as well as synthesized in the labs. However, the
nano silica extracted from natural resources generally contains metal impurities and
is not advisable for advanced scientific and industrial applications. The synthetic
nano silica is pure and produced mostly in amorphous powder forms such as silica
gels, pyrogenic silica, and precipitated silica. Nano silica can be synthesized by using
either of the two main approaches: top-down and bottom-up. In top-down technique,
the dimension of the original size is reduced by utilizing special size reduction
techniques. Bottom-up technique produces nano silica
 24

particles from atomic or molecular scale. The most common methods in use are as
follows:

1) By ion exchange, neutralization or electro dialysis using sodium

silicate
2) By peptization or milling using silica gel
3) By hydrolysis and condensation of a silicon compound
4) By direct oxidation or electrolysis of silicon.

4.2.4 WATER:

 Water used for mixing and curing shall be cleaned and free from injurious
amount of oils, acids, alkali’s, salt, sugar, organic materials or other substances
that may be deleterious to mortar.
 Portable water is generally considered satisfactory for mixing mortar. pH
value of 7 to 8 will be preferred. Locally available portable drinking water was
used in the present work.

4.3 MIX PROPORTION

4.3.1 GENERAL

Mix proportion determines the proportions of various materials used to prepare

cement mortar specimens that are economically viable as well as satisfy the need of
study. The mix proportion is most important to ensure quality and economy. The
influence of nano particles on properties of cement paste and mortar using SiO2 nano
particle with the average diameter of 18 to 40 nm were used with five different
proportions of 0.5%, 1.0%, 1.5%, 2.0% and 2.5% by weight of cement and
 25

compared with conventional mortar. The quantity of water was kept constant so as
not to affect the flowability adversely.

4.3.2 MIX PROPORATIONS OF CEMENT MORTARS

Water/Cement ratio (W/C) of 0.5 was used to prepare the mortar paste for all the
specimens with Cement/standard sand weight ratio (C/S) of 1:3. Cement was replaced
by NS with content varying from 0.5% to 2.5 % @ .5% and the specimens were
designated as NS1, NS2, NS3, NS4 and NS5 and compared with conventional mortar
(NS0).
Table 4.6 Mix Proportion

Specimen Water Cement Sand W/C Nano-SiO2

(ml) (g) (g) (g)
NS0 90 200 600 0.45 -
NS1 90 199 600 0.45 1
NS2 90 198 600 0.45 2
NS3 90 197 600 0.45 3
NS4 90 196 600 0.45 4
NS5 90 195 600 0.45 5

4.4 DESCRIPTION OF SPECIMEN

The current experimental program includes 6 specimens. The proportion of the

specimens were designated as NS0, NS1, NS2, NS3, NS4, NS5 are given below the
table. This table shows the percentage on nano silica replaced in mortar and number
of specimens casted for 7 and 28 days.
 26

Table 4.7 Description of Compression and Durability Cube Specimen

Specimen % of No. of Cubes for No. of Cubes for

Nano-
Compression Durability
SiO2
7 14 28 7 14 28
(g) days days days days days days
NS0 - 3 3 3 3 3 3

NS1 1 3 3 3 3 3 3
NS2 2 3 3 3 3 3 3

NS3 3 3 3 3 3 3 3
NS4 4 3 3 3 3 3 3

NS5 5 3 3 3 3 3 3

Table 4.8 Total No. of Test Specimens

4.5 TEST ON MORTAR

4.5.1 FRESH PROPERTIES TEST

4.5.1.1 SETTING TIME:

The too rapid and too slow setting of cement is not desirable in construction practices.
The too rapid setting of cement indicates the insufficient time to carry and place the
cement paste before it gains its rigidity. On the other hand, too slow
 27

setting not only slows up the work unnecessarily, but it may also delay the relay use
of the structure due to inadequate strength at the preferred age.

Vicat's apparatus (Figure 4.4) is the standard apparatus used to find out the initial and
final setting time of cement paste of standard consistency. It consists of 1.13 mm dia
needle and Vicat’s mould, kept on a non-porous plate, in which cement paste is filled.
The penetration of needle is observed until it reaches a set value and the time is noted.

Fig. 4.5 Initial Setting time test

Initial setting time is designated as the time period elapsed between the addition of
water to the cement and penetration of needle up to 5 mm to 7 mm from the bottom
of the mould containing the cement paste. On the other hand, final setting time is as
the time when the cement paste has completely lost its plasticity. The cement is
considered to be finally set if the gently applied needle on the surface of the
 28

specimen block makes and impression on it, but the attachment cannot do so. Now,
the time period elapsed between the addition of water to the cement and impression
made by the needle on the surface of the specimen block is designated as the final
setting time.

The cement was gauged with 0.85 times the water, required to obtain a paste of
standard consistency paste, and paste was made. The stop-watch was started with
addition of water to the cement. The Vicat mould was filled with the cement paste
and the surface of the paste was smoothened off to level it with the top of the mould.
The needle was set to just touch the top surface of the cement paste and then released
to freely fall in the paste to determine the initial setting time. The annular collar was
used to determine the final setting time.

4.5.1.2 FLOWABILITY TEST:

Workability of fresh mortar is quite significant in terms of its suitability and

application properties for various construction purposes such as masonry, plastering
or jointing and depends upon the flow of cement mortar. Flow of mortar, lime and
cement specimens is determined by using Flow table (Figure 4.5) as per IS 5512-
1983, a specially designed table that is having 254 mm diameter and 12.7 mm drop
height. It has a brass cone with 101.6 mm base dia., 69.9 mm top dia. and 50.8 mm
height. It is raised repeatedly raises to drop a known quantity of mortar sequentially
twenty five times within fifteen seconds. As the procedure continues, the mortar
spreads or flows to attain a circular form just like the shape of a pancake. The diameter
of this circular form is measured and compared to that of the initial size. The increase
in size is expressed as a percentage of the initial size; for most mortars the required
flow is in the range of 130-150 mm without using any SCMs.

A paste of 600 g sand and 200 g cement with water as per fixed water/cement ratio
of 0.50 was formed and flow of mortar was observed.
 29

Fig. 4.6 Flow Table with Mortar

4.5.2 COMPRESSIVE STRENGTH

Compressive strength of cement mortar is the most significant property in terms of

structural use and is most convenient to determine through tests of standard specimen
cubes. Hence compressive strength tests were performed for cement mortar
specimens at desired curing ages. The testing was done as per IS: 516-1959 using
compression testing machine (Figure 4.6). For compressive strength studies, thirty
six cubes of 7.06 cm (IS: 10080 - 1982) were cast for total mix proportions.

2
Compressive Strength, fck = N/mm

Where,
Load = Maximum applied load just before load, (N)
Area = Plan area of cube mould, (mm2)
 30

Fig 4.7 Compression Testing

4.5.3 DURABILITY TEST

Durability of a cementitious structure is the ability to resist against various

deterioration processes viz. chemical, weathering, abrasion etc. in aggressive
environmental conditions without any adverse affect on the identity, quality &
performance of the cementitious structure during its service life. Many physical,
chemical & electrochemical processes affect the durability of the cement mortar
leading to cracking. It is difficult to classify the exact cause of deterioration of cement
mortar because of interacting and reinforcing nature of various chemical &
electrochemical factors. The durability studies of the specimens have been analyzed
in terms of Steel Corrosion Test.

4.5.3.1 STEEL CORROSION TEST

Since corrosion of the reinforcing steel is regarded as the most serious durability
problem in construction engineering, how to eliminate the degree of steel corrosion
 31

is a headache problem in practical engineering. The combination of concrete quality

and concrete cover thickness is apparently the most important parameter that controls
the rate of carbonation and chloride ingress, hence improving the quality of concrete
has thus been considered as the primary protection method. The protection strategies
include increased concrete cover, coating rebar, stainless steel and corrosion
inhibitors.

In order to increase the bond strength of the embedded plain steel bars in existing
structures without any need for demolition and realkalization, the deep impregnation
of cement-based mortars and concrete with a solution of ethyl silicate and with
electrochemical treatments by means of a solution of sodium carbonate was
investigated The set-up of electrochemical treatment was presented in Fig. 4.8

Fig 4.8 Set-up for Elecrochemical Treatment

 32

Fig 4.9 Steel Corrosion Test on Mortar

4.5.4 MICROSTRUCTURE ANALYSIS

The microstructure of the cement matrix is a function of the composition of the

cement mortar and is a measure of the strength properties. The microstructure
analysis of cement mortar is carried out using XRD and SEM study.

4.5.4.1 SCANNING ELECTRON MICROSCOPE

` Scanning Electron Microscope is a type of electron microscope that depicts the

sample surface through the scan process by using a high-energy electrons beam in a
raster scan pattern. Electron interaction with atoms of the sample helps in generating
a signal that is most frequently used to study sample's surface topography,
composition and other properties such as electrical conductivity. It is capable of
generating high resolution images, which allow to examine the characteristics with a
high magnification and detail. SEM has a large depth of field, which can focus on the
more samples at a time and produce good shadow of three- dimensional samples.
SEM also produces high-resolution images, which means
 33

approaching shadows that can be tested with high magnification. Higher

magnification, dark field, greater resolution, and composition & information of
crystallography are the important features of SEM.

Fig 4.10 Scanning Electron Microscope

4.5.4.2 X-RAY DIFFRAACTION (XRD)

X-ray diffraction spectroscopy (X-ray Diffraction / XRD) is one of the oldest and
most commonly used method of material characterization. It is usually used to
identify the crystalline phases in the material by determining the parameters of the
lattice structure as well as to obtain particle sizes of unknown crystalline materials
including metals, minerals and inorganic compounds.

XRD has been extensively used in two fields; one is identifying the fingerprint
characteristic and the structure determination of crystalline materials such as cement
mortar. The second and most important use of XRD as used in construction
technology is in identification of crystals in the cement matrix. In this case, the
positions and the intensities of the peaks of the diffraction pattern are compared with
that of a standard from handbooks of International Centre for Diffraction Data
(ICDD) database. The major components of XRD diffractometer are X-ray tube,
incident-beam optics, goniometer, receiving-side optics and detector (Figure 4.10).
 34

X-rays are electromagnetic radiations that have a high energy of about 200 eV to 1
MeV. X-rays are produced in the X-ray tube by the striking the electron beam from
a mercury lamp or tungsten filament on anode target. X-ray wavelengths that have
the same order as the distance between the atoms, can be used as a source of crystal
diffraction. Incident-beam optics conditions the X-ray beam before it hits the sample
while receiving-side optics conditions the X-ray beam after it has encountered the
sample. Goniometer holds and moves the sample, optics, detector, and/or tube and
detector counts the number of X-Rays scattered by the sample.

Fig 4.11 X-ray diffractometer

 35

CHAPTER 5

RESULTS AND DISCUSSION

This chapter deals with the results and discussion of various experimental tests
performed to analyze the effect of partial substitution of cement by nano silica (NS).
The results have been discussed in terms of fresh properties, hardened property,
durability property, microstructural analysis and acoustical test. Setting time of
cement pastes and flowability of cement mortars have been studied in fresh properties
for all the mixes. Compressive strength of the mortar cubes have been studied in
hardened property for all the specimens at the 7 and 28 days. Steel Corrosion Test
have been studied in durability property for all the specimens. Microstructural
analysis has been performed using XRD and SEM studies. The comparative analysis
of the results has been performed to differentiate the pozzolanic action of Coventional
mortar and NS. Further acoustical test have been studied.

5.1 FRESH PROPERTIES TEST

5.1.1 SETTING TIME

Cement paste is also characterized in terms of setting time to determine the hardening
behavior of cement paste. It also depends upon the type and size of the particles as
well as water/cement ratio. Setting time of NS0 paste was examined and then
compared with that of the cement pastes with partial substitution of cement by nano
silica at varying percentages of 0.5%, 1%, 1.5%, 2% and 2.5%. The results have been
summarized in table 5.1, while the plots have been illustrated in figures
5.1 respectively.
 36

Table 5.1 Setting Time of Cement Mortar

Specimen Setting Time (min)
Initial Final
NS0 115 249

NS1 112 238

NS2 109 234

NS3 107 228

NS4 102 223

NS5 97 219

The setting time of NS1, NS2, NS3, NS4 and NS5 pastes was found to be lesser as
compared to NS0 pastes as shown in figure 5.1. The decreased setting time may be
due to the ultra fine size of nano silica particles that not only enhance the interaction
with water but also provide better packing of the cement matrix due to their filler
effect, thereby promoting the hydration process. As a result, the thickness of the paste
increases and setting process is accelerated. Further, as the percentage of NS was
increased, the setting time further decreased indicating that the presence of NS
accelerates the setting process (Table 5.1).
 37

300
Initial Setting Time (min)
Final Setting Time (min)
250
Setting Time (min)

200

150

100

50

NS0 NS1 NS2 NS3 NS4 NS5

Percentages of Nano-Silica

Fig.5.1 Setting Time of Mortar

5.1.2 FLOWABIITY TEST

Flow or workability of mortar is a very significant property that is a measure

of its performance. More flow of mortar indicates its workability for longer duration.
Flow of NS0 was examined and then compared with that of the cement mortar with
partial substitution of cement NS. The influence of substitution of cement by NS on
flow of cement mortar has been summarized in table 5.2, while the plots have been
illustrated in figure 5.2 respectively.
 38

Table 5.2 Flowability of Mortar

Specimen
Flow (mm)
NS0
155
Flow (mm)

NS1
126
NS2
120
NS3
110
NS4
101
NS5
96

The flow of NS1, NS2, NS3, NS4 and NS5 cement mortars was observed to
be lesser as compared to flow of NS0 (Table 5.2) cement mortars.

Flow (mm)
180
Flow (mm)
160
140
120
100
80

40
20

NS0 NS1 NS2 NS3 NS4 NS5

Percentages of Nano-Silica

Fig. 5.2 Flowability of Mortar

 39
The finer nano silica particles introduced better packing due to filler effect
and decreased the flow (Fig. 5.2). Further, flow of mortar decreased with increase in
content of NS. The increased content of finer particles increased the stiffness of
cement matrix leading to decrease in flow.

5.2 COMPRESSIVE STRENGTH

Compressive strength of NS0 were examined and then compared with that of
the cement mortar of all the mixes with partial substitution of cement by nano silica
(NS) at 7, 14 and 28 days. The values have been summarized in table 5.3 and plotted
in figure 5.3 respectively.

Table 5.3 Compressive Strength of Mortar

specimen % Replacement of Average compressive strength

nano slica (N/mm2)
7 days 14 days 28 days
NS0 0 18.05 22.17 28.08

NS1 1 19.06 23.61 29.10

NS2 2 20.06 24.53 30.09

NS3 3 21.27 25.95 31.29

NS4 4 25.27 27.44 33.01

NS5 5 21.87 25.05 31.09

Table 5.3 illustrates the increased compressive strength of NS1, NS2, NS3, NS4 and
NS5 cement mortars with increase in curing age as expected. Further, these
specimens with partial substitution of cement by NS exhibited increased compressive
strength in comparison to NS0 specimen in terms of comparative % substitution as
listed in table 5.3. The mixes with 0.5%, 1.0%, 1.5% , 2.0% and
 40
2.5% NS showed an increase in compressive strength by 6%, 11%, 18%, 40% and
21% at 7 days and 3%, 7%, 11%, 18% and 11% at 28 days respectively in comparison
to NS0.

Compressive strength for 7,14 and 28 days

35 33.01
31.29 31.09
30.09
29.1
30 28.08 27.44
25.95
25.05
Compressive stress(Mpa)

24.53 25.27
25 23.61
22.17 21.87
21.27
20.06
19.06
20 18.05

15

10

0
CC NS1 NS2 NS3 NS4 NS5
Percentage of cement + Nano sillica

7 Days 14 Days 28 Days

Fig. 5.3 Compressive Strength of Mortar

The observed increase is attributed to the filler effect and pozzolanic behavior of NS
that not only increases the packing of the cement matrix but also improves its
homogeneity due to production of extra CSH gel. The difference in the developed
compressive strength pertains to difference in the pozzolanic behavior of NS. The
percentage gain of compressive strength in case of NS1, NS2, NS3, NS4 and NS5
specimens was more at early ages in comparison to late ages indicating that the nano
silica reacts very fast with CH during the pozzolanic action at early ages leading to
increase in compressive strength. Further, it can be observed from figure
5.3 that the compressive strength of the specimens increased up to a NS4 and then
decreased afterwards. The decrease in compressive strength is an indication of loss
 41
of homogeneity of the cement matrix.

5.3 DURABILITY TEST

Durability of the mortar is defined as the capability of mortar to resist weathering

action and corrosion while maintaining its desired engineering properties. Factors
affecting durability of mortar are cement content, compaction, curing, cover,
Permeability.
The following durability tests are to be studied:
a) Water absorption
b) Steel corrosion

5.3.1 WATER ABSORPTION

For water absorption test the cylinder size of 100mm dia and 50mm height was used.
After De moulding the cubes are immersOed in a water for 28 days. After 28 days
of curing the cubes were taken out to measure saturated weight (w2). Thus the
specimen were dried in oven at a temperature of 105oc for 72 hours and taken it as
an oven dried weight (w1).
The water absorption was calculated as:
(𝑤2−𝑤1)/𝑤1 X100

Fig 4.4 Specimen in Oven Curing

 42

Table 5.1 Water absorption Tabulation

Mix Saturated Oven dried % of water
weight (g) weight (g) absorption
Cc 854 818 4.40

1 863 820 5.52

2 866 825 4.96

3 871 828 5.19

4 879 831 5.77

5 887 837 5.97

5.3.1 STEEL CORROSION TEST

For the durability test, Steel Corrosion test, is carried out in whch the % of
losses in steel is calculated. With the increases in nano silica % loss in steel is
decreases because due to voids the bar gets corroded fastly, by using nano silica the
voids is filled, so it takes time for corrosion.

Table 5.4 Steel Corrosion Test

Sl. % of Nano Silica % of loss in steel
No (SiO2)
1 0 8.33

2 0.5 6.66

3 1.0 5.00

4 1.5 3.33

5 2.0 2.42

6 2.5 1.98
 43

Percentage of Steel Loss

Percentage of Steel
Loss
Percentage of Steel Loss

NS0 NS1 NS2 NS3 NS4 NS5

Percentage of Nano Silica

Fig. 5.4 Loss of Steel Corrosion

 44

CHAPTER 6

CONCLUSION

This chapter deals with the conclusions drawn on the basis of results obtained
by the study of effect of partial substitution of cement with NS on fresh, hardened
and durability properties, microstructure & acoustical studies of cement mortars in
comparison to control mix (NS0).
1) Increase in content of Nano Silica from 1% to 5% resulted in a decrease in
setting time of NS1, NS2, NS3, NS4 and NS5 cement pastes due to increase
in thickening effect of ultra fine nano silica particles.

2) Increase in content of Nano Silica with filler effect from 1% to 5% resulted in

a decrease in flow of NS1, NS2, NS3, NS4 and NS5 mortar specimens due to
increase in the homogeneity and stiffness of matrix.

3) The compressive strength of NS0 was found to be lesser as compared to NS1,

NS2, NS3, NS4 and NS5. An increase in compressive strength of NS1, NS2,
NS3, NS4 and NS5 mortars was obtained with an increase in content of NS
from 1% to 4% along with a slight reduction in strength of NS5 (5% NS)
mortar as compared to NS4 (4% NS) mortar. The gain of compressive strength
was linked to the filler effect and better pozzolanic behavior of NS leading to
production of extra CHS gel as compared to NS0. The slight decrease in
compressive strength of NS5 specimen as compared to NS4 specimen was
attributed to the agglomeration of nano particles at higher content in the
cement matrix. Thus, 4 % content of NS was designated as the optimum
percentage.
 45

4) With the increases in nano silica % loss in steel is decreases because due to
voids the bar gets corroded fastly, by using nano silica the voids is filled, so it
takes time for corrosion.

5) Silica incorporated mortar enhances the crystallinity of the mortar this in turn
influences the properties too.
 46

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