Effect of nano-silica on strength and
microstructure of cement silica fume
paste, mortar and concrete
Abhik Ghosh, V. Sairam and B. Bhattacharjee
In this study the effect of nano-silica on cement-silica
fume paste, mortar and concrete is studied at three
different water-binder ratios: 0.20, 0.25 and 0.30. By
adopting a systematic procedure most suitable nano-
silica was selected from a set of commercially available
nano-silicas. Most effective superplasticiser was selected
from a set of super plasticisers and used in the paste,
mortar and concrete to achieve maximum dispersion of
the particles in the cementitious system so as to attain
maximum flow. The compressive strength of these
systems was tested at curing ages of 3,7,14, 28 and 56
days. The microstructure of the same system was also
studied using the various instruments such as X-ray
Diffraction (XRD), Scanning Electron Microscope
(SEM) and Atomic Force Microscope (AFM). The
results obtained from the specimens were compared with
controlled specimens. As expected, the results showed
that nano-silica increased the compressive strength as
well improved the microstructure due to pozzolanic as
well as iller action.
Keywords : Silica fume, Nano-silica, Durability, Strength.
High strength cement based matrices are generally
provided with Ordinary Portland Cement (C), silica
fume (SF) together with suitable aggregate and High
range water reducing admixture (HHWRA). For low
water-cement ratio cement based matrices, HRWRA
plays an important role in improving workability.
Recently, nano-silica (NS), by virtue of its large surface
area due to high ineness, reportedly has been used to
enhance the compressive strength of some cement based
material. It reacts with calcium hydroxide (CH) at very
early stage to form C-S-H gel.1 The interaction of CH with
NS or SF improves the microstructure of the hardened
cement paste (HCP) at the interface between HCP and
aggregate at early ages.2 The durability and mechanical
properties of HPC are mainly dependent on the gradual
reinement of structure of HCP and the improved paste-
aggregate interface, and the role of SF in this regard
is well known.3 But the activity of SF at early ages is
relatively low according to the literature.4-7 Mitchell et al.
reported from the XRD pattern of SF put into saturated
calcium hydroxide (CH) solution, changed little up to 7
days and extensive C-S-H formation occurred only after
120 days.4 Li et al. observed that only 78% of silica fume
was consumed in a cementitious mixture containing 10%
silica fume and 90% cement after 90 days of hydration.7
Nano-silica addition to cement-silica fume system on
the other hand enhances the early strength possibly due
to its larger speciic surface and higher pozzolanacity
leading to rapid strength development.8 Additionally
nano-silica further reduces the porosity of the matrix and
that in the interfacial transition zone.9 The nano-silica
when used in colloidal suspension behaves much better
than the agglomerated silica because dry silica cannot
JUNE 2013 THE INDIAN CONCRETE JOURNAL 11
exhibit the whole speciic surface area of its primary
particles.9 Most of the reported works with nano-silica
adopt w/c of 0.35 or above, hence relevant to normal
strength concrete. Beneit of nano-silica addition is likely
to be realised also in high strength concrete. Therefore a
detailed experimental study was conducted in this work
whereby strength enhancement of high strength paste,
mortar and concrete due to the addition of nano-silica
in cement-silica fume based matrices was investigated.
Further, the effect of nano-silica on microstructure
improvement was studied through AFM, SEM and
XRD.
Experimental investigation
The main purpose of this investigation was to evaluate
the effectiveness of nano-silica for strength enhancement
and improvement of microstructure in high strength C-
SF based material. The experimental factors have been
chosen accordingly.
Materials
A commercially available Ordinary Portland Cement
(OPC Grade-43), with Blains ineness (274 m2/kg) and
28 days compressive strength of 50.6 N/mm2 conforming
to IS 8112:1989 and ASTM Type I speciications, was
used for experiment.10 Silica fume 920D grade (chemical
composition SiO2-89.2%) from a well known supplier
was used for the experimental program. Six types of
Nano-silicas were procured from different sources
for the project. The details of the samples and their
properties as supplied by the manufacturers are given
in Table 1. Further size veriication of the nano-silica
was not carried out. Instead, a systematic procedure,
discussed later, was adopted to select the most suitable
nano-silica and was used for the intended strength
enhancement study. High range water reducers used
were fourth generation polycarboxylic ethers. The
general properties of HRWRA are given in Table 2. Six
HRWRA were considered and most suitable one was
used for the strength enhancement study of paste, mortar
and concrete. The procedures adopted for selection of
HRWRA and nano-silica are discussed in later sections.
Locally available land quarried sand known as Badarpur
sand, available near Delhi was used for the experimental
purpose. The ineness modulus, speciic gravity and
packing density of sand were 2.67, 2.61 and 0.659
respectively. The grading of ine aggregate satisied the
(Zone-II) Indian standard IS: 383-1970.11 Crushed graded
aggregate having a maximum size of 10 mm and speciic
gravity of 2.63 was used as coarse aggregate. The packing
density of the sample was 0.597. The packing density

Table 1. Physical characteristics of nano-silica

Product NS1 NS2 NS3 NS4 NS5 NS6
Speciic gravity 1.1 1.4 1.31 1.08-1.11 1.30-1.32 1.20-1.22
Particle Size, nm 6-7 23-25 14-16 12-16 14-18 8-10

Viscosity, cP <10 <15 <15 13-14 14-15 12-13

% solids 15 50 40 14-16 40-41.5 30-32
pH 10.0 9.5 9.4 9.3-9.6 9.4-9.8 9.0-10.0
Appearance Clear liquid, no Opalescent, no --------- Clear liquid, no Clear liquid, no Clear liquid, no smell
smell or taste smell or taste smell or no taste smell or taste or taste

Table 2. Physical characteristics of admixtures

Product designation Compliance with Speciic gravity Colour Type
ASTM C-494 Type-A
HRWRA1 1.17 Light Yellow Liquid Poly carbo-ether based
and F, IS 9103-1999
HRWRA2 IS 9103: 1999 1.10 Brown Liquid Modiied Polycarboxylate
ASTM C-494 Type-G
HRWRA3 1.15 Light Yellow Liquid Poly carbo-ether based
and IS 9103-1999
ASTM C-494 Type F
HRWRA4 1.09 Light Brown Liquid Polycarboxylate Polymers
and IS 9103-1999
HRWRA5 Not provided 1.16 Light Yellow Liquid Poly carbo-ether based
HRWRA6 AS1478.1-2000 1.10 Brown Liquid Modiied Polycarboxylate

12 THE INDIAN CONCRETE JOURNAL JUNE 2013

was obtained by measuring the bulk density as per
IS 2386 (Part III):1963 procedure, i.e., by compaction
of the dry aggregate in three layers in a container up
to a known marked fixed level.12 The volume was
determined by illing the container with water up to
the marked level. Solid volume of the aggregate was
calculated from the knowledge of mass of aggregate
and speciic gravity. The obtained bulk density of the
aggregate divided by its measured speciic gravity is
the packing density which is the ratio of the volume
of solids to the bulk volume of the solid particles.
Thus, when VC is the volume of the container up to the
marked level obtained as above and measured mass
of the aggregate compacted up to the same level is Ma;
then the packing density is given by Ma/(GaVc) where,
Ga is the speciic gravity of the aggregate. The overall
grading requirement of coarse aggregate satisied Indian
standard IS 383:1970.11 Distilled water was used for the
entire experiment involving pastes and mortars.
W/b ratios, levels of SF and NS for paste
and mortar
To obtain high strength concrete it is necessary to use
a water-to-binder ratio as low as possible. W/b ratio
generally adopted for high strength concrete when cured
at ambient condition is lower than 0.3. Considering this
fact, three w/b ratios namely, 0.20, 0.25 and 0.30 were
adopted in the experimental investigation to obtain
high strength cement paste and mortar. Silica fume,
because of its high pozzolanicity and higher ineness,
is the other cementitious material generally used in
high strength matrices. The range of silica fume content
in total cementitious materials in such high strength
materials usually is restricted to a maximum of 15%.
Thus 3 silica fume contents, namely, 5%, 10% and 15%
of SF by mass of total cementitious material was used
in this experimental program for both paste and mortar.
Thus nine paste mixes were used in the experimental
programme for casting cube samples for compressive
strength tests. These pastes were designated by a
combination of three alpha-numeric symbols namely,
P1A, P1B, P1C, P2A, P2B, P2C, P3A, P3B and P3C. Here
P stands for paste, the second digit signiies the level of
w/b ratio, e.g., 1, 2 and 3 represent 0.20, 0.25 and 0.30
w/b respectively. The next letter represents the level
of SF e.g., A, B and C represent 5%,10% and 15% SF
respectively All these pastes were used for choosing
most suitable admixture and inally the chosen HRWRA
was mixed with all the pastes to obtain adequate low
prior to cube casting.
For the cases of mortar, the paste used had the same
composition as above. The volume proportions of the
paste in the mortar were adopted on the basis of packing
density of the sand and low characteristics of the mortar.
The void content of the sand was obtained by subtracting
the measured packing density of the ine aggregate from
unity i.e. 1- where is the packing density of the sand.
The volume fraction of paste used in the mortar was in
excess of the void content by 0.20 for SF content 5% and
was in excess of the void content by 0.25 for SF content
10% and 15%. This was done to ensure adequate low
property of the mortar as discussed in a later section.
Thus, nine mortar mixes were used for casting cube
JUNE 2013 THE INDIAN CONCRETE JOURNAL 13
specimens after ascertaining their low through the
low table test.

At each w/b level one case was selected on the basis of

maximum 28-day compressive strength. For the selected
cases, NS was added at 2%, 4% and 6% by mass of cement
for both paste and mortar. Thus nine mixes with nano-
silica were used for studying the compressive strength
enhancement of both paste and mortar. For preparing
the paste and mortar a planetary mixer (Digi Mortar
Mixture AIM 412-4) which conforms to the speciication
of IS 10890 was used.13

Admixture selection for paste and mortar

Mini slump test was used to ind out the best admixture
and corresponding optimal dosage for different cement
paste mixes. The mini slump method is the miniature
version of the conventional slump test. Dosages of
admixtures were varied to obtain optimal dose and
most suitable admixture. The mixing of the paste
was performed as par the mixing procedure used for
mortar mixes recommended in IS 1727 after dosing
the admixture.14 The dosage of admixture is expressed
as fraction by mass of cementitious material. After the
addition of all the water, admixture was added to the mix
and the mixer was allowed to run for the 30 seconds so
that the paste attains required consistency. Immediately,
the paste was poured into the mini slump cone mounted
on a low table and the cone was gently tapped 15
times to remove the air bubbles. The mini slump cone
and the low table is shown in Figure 1. The cone was
lifted vertically to allow the paste to spread over the
low table. Flow diameter was measured in any two
perpendicular directions and its average reported as the
low value for a given trial. This procedure was repeated
with increased dosage of admixture until the increase
in low with increased dosage of the admixture became
appreciably insigniicant. The dosage corresponding
to maximum low is considered as the optimal dosage.
The parameters chosen for selection of best admixture
were maximum low, optimal dosage for maximal low,
upper limit of maximum dosage as per manufacturer
specification and 7-day compressive strength. The
admixtures exhibiting optimal dosage more than the
maximum limit recommended by the manufacturer
were rejected. The ratio of maximum low to optimal
dosage was calculated. High low to dosage ratio and
7-day compressive strength was used for selecting the
best admixture for cement paste mixes. The elimination
of HRWRA was done in stages. First the paste P1A was
considered and optimal dosage was determined for all
six HRWRA. Figure 2 shows the variation of mini slump
low against dosage for six HRWRA in case of paste
P1A. The optimal dosage, corresponding low, low to
optimal dosage ratio, maximum dosage prescribed by
manufacture and 7-day compressive strength of 5 cm
cubes are given Table 3. In Table 3 it is observed that ratio
of low/optimum dosage for HRWRA1 and HRWRA4
was less compared to that of other HRWRAs. 7-day

Table 3. Comparison performance of hrwra for mix P1a

Optimum Flow/optimum 7-day compressive
Prescribed dosage,
Manufacturer name dosage, Flow, cms dosage ratio strength , N/mm2
%
%
HRWRA1 3.25 20.00 6.15 3.00 63.60
HRWRA2 1.75 19.25 11.00 2.50 78.80
HRWRA3 2.75 19.25 7.00 2.50 69.40
HRWRA4 3.00 18.75 6.25 3.00 60.80
HRWRA5 1.75 16.50 9.43 2.50 75.50
HRWRA6 2.75 18.00 6.55 3.00 74.70

14 THE INDIAN CONCRETE JOURNAL JUNE 2013

compressive strengths were also lower for these two
HRWRAs compared to other admixtures. The optimal
dosage for HRWRA1 was more than the maximum
prescribed by the manufacturer and that for HRWRA4
was exactly same as that prescribed by the manufacturer.
Hence considering these three aspects, these two
HRWRAs were discarded from further study. After the
elimination of above two HRWRAs, another three mixes
were chosen for further elimination of HRWRA and to
select suitable brand and corresponding dosage. These
three mixes were P1C, P3A and P3C which were in the
extreme levels in terms of w/b and SF and all other
mixes were in between extremities. It may be worthwhile
to mention that the paste P1C is the critical case with
respect to low as the w/b in this case is least while the
SF is maximum. For all three pastes, results similar to
those given in Figure 2 and in Table 3, were generated.
HRWRA2 and HRWRA6 exhibited higher 7 day strengths
for all three pastes. Maximum low to optimum dosage
ratio was observed for HRWRA2 in all cases and dosages
of HRWRA2 in all cases were lower than the upper
limit prescribed by the manufacturer. HRWRA6 on the
other hand exhibited better strength than HRWRA3 and
HRWRA5 in all cases and ratio of low to dosage were
also higher in two cases. Thus HRWRA6 performed
better than HRWRA3 and HRWRA5. Hence HRWRA2
and HRWRA6 were tried with remaining 5 pastes. For
these 5 pastes again HRWRA2 consistently exhibited 7
day strength comparable or better than HRWRA6 and
much better low as well as low to optimum dosage
ratio. The optimal dosage for HRWRA2 never exceeded
the upper limit prescribed by manufacturer while for
HRWRA6 the case was not so. Thus HRWRA2 was
inally selected as the most suitable HRWRA.
The same HRWRA was used for mortar as well. Flow
table test as par IS 1727-1967 was used to decide upon
the required dosage of admixture for mortar.14 After
weighing the constituents the mixing was done in mortar
mixture as per IS 1727:1967. Flow table top was cleaned
and dried. Mould was placed at the centre of table and
illed in two layers of about 25 mm thick. Each layer was
tamped 20 times with a tamping rod. Tamping pressure
was just suficient to ensure uniform illing of mould.
Excess mortar was cut off to a plane surface lush with
the top of mould by drawing a straight edge. Table top
was cleaned and mould was lifted. Immediately table
was dropped though a height of 12.5 mm, 25 times in 15
seconds. The low was the resulting increase in average
base diameter of the mortar mass, measured on at least at
four diameters, expressed as a percentage of the original
base diameter. Numbers of trial tests were conducted by
gradually increasing the water content till required low
of 1055% or higher was achieved. The required dosage
1055% low was determined by linear interpolation
where ever required.
Selection of most suitable nano-silica
To select the most suitable nano-silica a systematic
procedure was proposed and adopted as given
below. Cement reactivity test as par IS 1727:1967 with
appropriate modiication was used to select the most
suitable nano-silica sample for experimental works. The
mixture containing cement, silica fume (pozzolana) and
sand as per recommendation of the code (1:2M:9) and
also nano-silica at 2% by mass of cement was used for
this test. The control mix devoid of nano-silica was also
considered. With six varieties of nano-silica in total 7
mixes were considered. The test was conducted in two
steps. At irst the admixture effect was not considered
and corresponding w/b was found out 0.58 to get the
speciied low (1055%) mentioned earlier, before adding
any nano-silica. Then different nano-silica was added to
the mix which reduced the above speciied low. Hence
additional water had to be added to increase the low
to the speciied level of 1055% mentioned earlier. The
low was constant for all the mixes which ensured that
the compaction would be similar for all the mixes. The
cement reactivity was obtained as the compressive
strength of the 50 mm side length cubes tested as par
recommendation of IS 1727:1967 at 3, 7 and 28-day.
The strength ranged from 13.5 to 17.5 MPa, 19.2 to
26.7 MPa and 24.5 to 38.8 MPa at 3, 7 and 28-day
respectively. The control mix exhibited a cement
reactivity values of 14.7, 21.7 and 30 MPa respectively
at 3, 7 and 28-day. Two nano-silica designated as NS1
and NS4 exhibited maximum and next to maximum
strengths at all 3, 7 and 28-day were chosen for next step
where admixture effect was considered. The strength
representing cement reactivity, exhibited by NS1 and
NS4 are 17.5 and 17.4 MPa at 3-day, 26.7 and 26.5 MPa
at 7-day and 35.5 and 38.8 MPa at 28-day respectively.
It may be mentioned here that the rest of the four nano-
silica did not demonstrate significant enhancement
in cement reativity vis--vis control specimens at all
3 ages. However, as per manufacturers speciication
NS2 was expected to perform excellently for strength
enhancement for low w/b concrete, therefore it was also
shortlisted for next step in the investigation.
To investigate on the low performance of these 3 nano-
silica remaining in the consideration, the control mortar
mix likely to exhibit worst low performance amongst
all the the mortar mixes was chosen as control. Thus mix
P1C designate with least water content i.e. least w/b
ratio (w/b=0.2) and maximum SF content (15%) was
JUNE 2013 THE INDIAN CONCRETE JOURNAL 15
 Table 4. Comparison between nano-silica for M1C
mix
NS name
3-day strength, 7-day strength, 28-day strength,
N/mm2 N/mm2 N/mm2
Controlled 74.53 79.67 82.00
mix
NS1 81.47 84.47 90.00
NS2 83.60 88.93 101.47
NS4 76.33 87.93 95.40
chosen. Nano-silica was added at 2% by mass of cement.
Admixture dose was added to make the constant low for
all three cases NS1, NS2 and NS4 nano-silica addition.
The results are given in Table 4. From these observations
it was found that the strength enhancement of NS2 was
higher than that of others. Hence NS2 was selected as
suitable nano-silica for the experiment.
Concrete mix proportions
Two mortar mixes with nano-silica were selected on the
basis of their higher 28day compressive strength from all
9 mortar mixes mentioned earlier, and concrete samples
were prepared using these mortars incorporating coarse
aggregate. 10 mm m.s.a aggregate was used to minimise
the stress concentration effect at the Interfacial transition
zone (ITZ). Mortar in excess by 0.10, 0.20 and 0.30 of void
fraction in aggregate sample, were adopted for concrete
mixes. The packing density of the coarse aggregate was
0.597 hence volume fractions of the mortar in above three
cases were (1-0.597) +0.1= 0.503, (1-0.597) +0.2=0.603
and (1-0.597) +0.3 = 0.703 respectively. Corresponding
volume fractions of coarse aggregate were 0.497, 0.397
and 0.297 respectively, hence coarse aggregate contents
were 0.4972630=1307, 0.3972630=1044 and 0.297
2630=781 kg/m3. Correspondingly the proportions
of other ingredients were calculated from the mix
proportions of the selected mortar. Further, nano-silica
was introduced at 1.5% and 3% by mass of cement to
investigate on its role on the strength enhancement of
concrete. The details of concrete mix proportions are
given in a table mentioned later.
was used for mixing purpose. The standard mixing
procedure was followed. All the dry materials placed
in bowl were mixed for 1 min. Later water was added
and mixed for half a minute followed by the addition
of admixture. Mixing was carried out till the admixture
effect was visible. In the case of mortar, sand was added
at slow rate after the complete mixing of dry pozzolanic
materials. Initially while adding sand, the machine was
allowed to run at slow speeds and later on at medium
speed for 30 seconds. The mix was placed in the 50 mm
cube mould in a layer of 25 mm thickness and tamped
25 times with the help of a tamping rod. Then the
mould was illed completely, vibrated at a frequency of
12000 400 cycles per minute and the top layer was cut
with the help of a straight edge of a trowel. In the case
of concrete mix, the freshly mixed concrete was placed
in 15 cm cubes in three layers and a plate vibrator with
frequency varying from 43 cycles/sec to 60 cycles/sec
was used for compaction. At last the top layer was
cut with the help of the straight edge of a trowel. After
casting, two curing regimes were chosen i.e. normal
curing and accelerated curing for mortar and concrete.
For normal curing, specimens were placed in a curing
chamber at standard condition. Accelerated curing was
done in an autoclave at a pressure of 0.20 MPa and a
temperature of 1200C for 8 hrs.
The compressive strength test for paste and mortar was
performed in compliance with IS 1727:1967. Cubes were
taken out of the curing tank and moisture was wiped
off the surface using a clean cloth. The cubes were
tested for their compressive strength in a Compression
Testing Machine. The average failure stress of three

Casting, curing and testing

The cube specimens were cured by immersion in a
curing tank at 27 2oC as per Indian Standard for 3, 7,
14, 28 and 56 days. For this experiment 50 mm cubes
were cast for different mix proportion for cement paste
and cement mortar specimen and 15 cm cubes were
cast for concrete specimen. Mechanical mixer machine

16 THE INDIAN CONCRETE JOURNAL JUNE 2013

 compressive strengths were exhibited by P2B and
P3C pastes. These pastes had 10% and 15% silica fume
content respectively. These are taken as reference mixes
for further investigation with nano-silica addition and
the corresponding compressive strength results are
given in Table 6. From Tables 5 and 6 it is observed that
strength generally increases with age and reduces with
increase in w/b ratio as expected. However, the variation
of strength with silica fume content as presented in Table
5, depends on w/b ratio and a similar pattern is observed
at all ages. While at 0.20 w/b highest strength is exhibited
for SF equals to 5%, at w/b ratio 0.30 highest strength
is exhibited at 15% SF. For common OPC, a maximum
of 15% pure silica can be consumed through pozzolanic
reaction on complete hydration. 15 Thus for higher
degree of hydration more Calcium Hydroxide would
be released and more silica fume can take part in the
pozzolanic reaction. Hydration is w/b ratio dependent
cubes was considered as the representative compressive and is higher for higher w/c ratio.16,17 Further for low
strength of the particular mix. The cubes were tested in w/b range such as 0.20-0.30, dispersion of cementitious
uniaxial compression. Flow loss is one of the important particle with HRWRA is likely to be higher at higher
parameters in the concrete at fresh state which measures w/b. Thus at w/b as low as 0.20, smaller quantity of
the workability of the concrete mix. In this experiment, silica fume will be effective in pore illing as well as in
the low loss was measured for cement mortar mix at contribution to pozzolanic reaction. Excess silica fume on
controlled conditions as well as after the addition of the other hand, being isolated, may generate additional
nano-silica at different dosages to ind out the effect of pores leading to strength reduction. For higher w/b
additional nano-silica on workability of the mix. The low ratio, higher quantity of silica fume would take part in
table test was used to ind out the low loss at different pozzolanic reaction due to more hydration and better
time intervals. The low loss of mortar M1A, M1B and dispersion.
M1C with different silica fume content is shown in
Figure 3. It is observed that although the initial low was From Table 6, it is obvious that nano-silica up to certain
nearly same for all three mortars, the low loss increases percentages results in an increase in early strength as well
with the increase in silica fume content. The behaviours as strength at later ages for pastes. Being very ine these
exhibited by M2 and M3 mortars however are different. particles may adhere to the surface of larger cement and
Thus the effect of SF on low loss as observed is not silica fume particles, results in disturbing the packing
systematic when considered simultaneously with w/b and may even hinder hydration process. This effect is
ratio. On the other hand, low reduces and the loss also pronounced when nano-silica content is high. Thus up
increases with the addition of nano-silica to 4% nano-silica addition by mass of cement
in all cases. Typical flow versus time
curves for M1A with 2, 4 and 6% nano- Table 5. Compressive strength of cement-silica fume paste samples
silica addition are shown in Figure 4. Compressive strength, MPa
Mix No.
3-day 7-day 14-day 28-day 56-day
Compressive strength study P1A 72.40 78.60 86.00 96.80 100.20
Cement silica fume nano-silica P1B 72.20 75.60 86.20 89.00 96.40
pastes P1C 62.60 70.60 82.60 93.40 91.20
Compressive strength results for cement- P2A 65.40 70.60 76.40 86.40 94.60
silica fume pastes are given in Table 5. P2B 70.00 78.20 86.40 92.00 94.40
From this table it is observed that the P2C 66.00 72.40 82.80 85.60 90.40
maximum 28day compressive strength
results is for w/b equals to 0.20 and P3A 60.60 65.60 69.00 74.20 79.00
is 96.80 MPa. Similarly for w/b ratios P3B 64.60 65.00 77.40 82.40 86.80
0.25 and 0.30 the maximum 28 day P3C 70.40 75.00 82.40 87.20 92.60

JUNE 2013 THE INDIAN CONCRETE JOURNAL 17

 Table 6. Compressive strength of nano-silica cement-silica fume paste samples
Compressive strength*, MPa
Mix No. NS/C, %
3-day 7-day 14-day 28-day 56-day
P1A 0.00 72.40 78.60 86.00 96.80 100.20
P1A2 2.00 80.40 (11.05) 90.40 (15.01) 96.20 (11.86) 100.40 (3.72) 104.60 (4.39)
P1A4 4.00 84.20 (16.30) 90.60 (15.27) 102.40 (19.07) 110.60 (14.26) 115.00 (14.77)
P1A6 6.00 84.20 (16.30) 82.40 (4.83) 88.00 (2.33) 92.80 (-4.13) 92.60 (-7.58)
P2B 0.00 70.00 78.20 86.40 92.00 94.40
P2B2 2.00 80.00 (14.29) 87.00 (11.25) 92.00 (6.48) 104.80 (13.91) 105.60 (11.86)
P2B4 4.00 80.00 (14.29) 90.40 (15.60) 96.40 (11.57) 104.60 (13.70) 108.40 (14.83)
P2B6 6.00 74.60 (6.57) 78.80 (0.77) 82.60 (-4.40) 84.00 (-8.70) 84.40(-10.59)
P3C 0.00 70.40 75.00 82.40 87.20 92.60
P3C2 2.00 72.60 (3.12) 82.20 (9.60) 89.40 (8.50) 96.80 (11.01) 102.60 (10.80)
P3C4 4.00 68.80 (-2.27) 76.60 (2.13) 82.00 (-0.49) 88.60 (1.61) 96.20 (3.89)
P3C6 6.00 60.40 (-14.20) 64.00 (-14.67) 72.60 (-11.89) 80.00 (-8.26) 84.80 (-8.42)
* The values in the parenthesis indicates the percentage increase in compressive strength with respect to control mixes

is effective in increasing the strength, and not beyond
this. At higher w/b ratio, more hydration is possible thus
above effect of excess nano-silica addition is even more
pronounced because of hindrances to hydration process.
SiO2 presents in the nano-silica as well as that in silica
fume would take part in secondary pozzolanic reaction
between SiO2 and Ca(OH)2 in a similar manner, but the
rate of reaction may be different owing to their physical
difference. The pastes prepared using nano-silica alone
was thicker compared to that prepared using silica fume
alone. The compressive stength of hardended cement
paste is enhanced with nano-silica at early ages like 1 and
3 days, but the strength of cement silica fume is enhanced
only after the 3 days because of the pozzolanic activity of
nano-silica being greater than that of silica fume. Nano-
silica consumes more CH crystals at the interface and
can improve the interface structure more effectively than
silica fume. Nano-silica accelerates the cement setting
process and the hydration process as well.18
Cement silica fume nano-silica moratrs
Compressive strength results for cement-silica fume
sand mortars are given in Table 7. From Table 7 it is
observed that maximum 28 day compressive strength
results for w/b ratio 0.20 is 94.60 MPa and corresponds
to SF 5%. Similarly, for w/b 0.25 and 0.30 the maximum
28 day compressive strengths were exhibited by M2A
and M3A mortars. These mortars also have silica fume
content corresponding to SF 5%. These mixes are taken
as reference mixes for further investigation with nano-

Table 7. Compressive strength of cement-silica fume mortar samples

Compressive strength, MPa
Mix No. Moist Curing Autoclaving
3-day 7-day 14-day 28-day 56-day 1-day 56-day
M1A 74.20 80.40 86.00 94.60 100.00 86.40 92.60
M1B 70.00 75.60 82.20 88.00 93.40 82.60 87.80
M1C 70.80 74.60 78.80 82.20 85.60 80.00 82.00
M2A 68.40 74.00 80.60 86.00 90.40 80.40 84.80
M2B 70.60 70.40 76.20 80.60 86.00 78.80 82.80
M2C 71.60 74.40 80.80 82.00 86.60 81.40 86.80
M3A 65.80 70.00 76.40 80.20 84.60 77.20 80.00
M3B 65.00 68.40 72.00 78.60 82.60 72.00 78.40
M3C 68.20 70.00 70.60 76.60 82.40 75.80 80.00

18 THE INDIAN CONCRETE JOURNAL JUNE 2013

 Table 8. Compressive strength of nano-silica cement-silica fume mortar samples
Mix No. NS/ Compressive strength*, MPa
C,
Moist Curing Autoclaving
%
3-day 7-day 14-day 28-day 56-day 1-day 28-day
M1A 0 74.20 80.40 86.00 94.60 100.00 86.40 92.60
M1A2 2 86.40 (16.44) 90.40 (12.44) 98.60 (14.65) 104.00 (9.94) 110.80 (10.80) 98.80 (14.35) 103.60 (11.88)
M1A4 4 86.60 (16.71) 86.40 (7.46) 90.40 (5.12) 98.60 (4.23) 102.40 (2.40) 92.00 (6.48) 94.60 (2.16)
M1A6 6 76.80 (3.50) 80.60 (0.25) 84.00 (-2.33) 88.60 (-6.34) 88.40 (-11.60) 84.60 (-2.08) 86.00 (-7.12)
M2A 0 68.40 74.00 80.60 86.00 90.40 80.40 84.80
M2A2 2 68.80 (0.58) 82.00 (10.81) 82.60 (2.48) 92.40 (7.44) 98.60 (9.07) 86.60 (7.71) 89.60 (5.06)
M2A4 4 72.60 (6.14) 80.40 (8.65) 85.20 (5.71) 94.40 (9.77) 102.80 (13.72) 86.20 (7.21) 90.20 (6.37)
M2A6 6 64.00 (-6.43) 72.80 (-1.62) 80.00 (-0.74) 88.20 (2.56) 92.20 (1.99) 86.00 (6.97) 88.60 (4.48)
M3A 0 65.80 70.00 76.40 80.20 84.60 77.20 80.00
M3A2 2 72.60 (10.33) 78.60 (12.29) 82.40 (7.85) 86.60 (7.98) 94.00 (11.11) 80.80 (4.66) 82.80 (3.50)
M3A4 4 68.40 (3.95) 70.60 (0.86) 76.00 (-0.52) 78.60 (-2.00) 86.00 (1.65) 75.00 (-2.85) 78.40 (-2.00)
M3A6 6 68.60 (4.26) 70.00 (0.00) 76.40 (0.00) 84.60 (5.49) 92.80 (9.69) 74.20 (-3.89) 76.00 (-5.00)
* The values in the parenthesis indicates the percentage variation in compressive strength with respect to control mixes

silica addition and the corresponding compressive
strength results are given in Table 8. The ranges of the
strength are almost similar to that observed for pastes.
Thus interfacial transition zone (ITZ) has very little
inluence on the strength of mortar in this case. This is
because silica fume is very ine and is known to improve
signiicantly the ITZ in a way, such that it is no longer
the weakest link in the system. It is also observed that,
at all w/b the maximum 28 day compressive strength
is achieved at SF 5% unlike the pastes; this is because,
the addition of sand particles makes mortar matrix
dryer, dispersion of iner particles are constrained in
to the packing of sand and enhancement of hydration
with increase in w/b ratio may not be realised to extent
it is realised in pastes. In case of autoclaved sample,
approximately 14 day compressive strength is achieved
by 1day autoclaving. During additional 56 day dry
curing strength development is comparatively less
and approximately equivalent to 28 day normal curing
strength.
From Table 8, it is obvious that nano-silica up to certain
percentages results in an increase in early strength as
well as strength at later ages of mortar. From Table 8 it
is observed that maximum strength enhancement was
achieved by addition of 2% nano-silica in reference
control mix M1A and M3A. In case of mix M2A,
addition of 4% nano-silica exhibited maximum strength
enhancement. As discussed earlier for pastes, nano-silica
being ine adheres to the surface of larger cement and
silica fume particles, thus disturbing the packing and
hindering hydration process at higher percentage of
addition.
In case of autoclaving again, approximately 14 day
compressive strength was achieved by 1 day autoclaving.
The rate of enhancement is high when the nano-silica
addition is comparatively less. During additional 28 day
dry curing strength development is comparatively less
and approximately equivalent to 28 day normal curing
strength. The autoclave treated concrete generally will
have better sulphate resistance, as well as reduced
shrinkage and creep when compared with normal cured
concrete. Hence, the presence of unutilised gypsum ,if
present, in the cement will not be a concern for long
term stability of hardened matrix. The ettringite which
is formed due to the reaction of C3A with gypsum will
be converted into monosulphate after 24 hours because
of sulphate ions depletion.19
Cement siica fume nano-silica concretes
The two mortar mixes exhibiting maximum 28 day
compressive strength (designated as M1A and M2A)
were selected for making 15 cm concrete cube specimens
as discussed earlier. The details of mix proportions of
concrete are given in Table 9.

JUNE 2013 THE INDIAN CONCRETE JOURNAL 19

 Table 9. Mix design of controlled concrete sample
Excess mortar Fine Coarse
Cement, SF , water, hrwra,
Mix No. Mortar Type volume aggregate, aggregate,
kg/m3 kg/m3 kg/m3 kg/m3
fraction kg/m3 kg/m3
C1 0.10 493 25.8 602 1307 104 9.0
C2 M1A 0.20 591 31.0 722 1044 124 10.9
C3 0.30 690 36.3 842 781 145 12.7
C4 0.10 450 23.7 602 1307 118 5.4
C5 M2A 0.20 540 28.4 722 1044 142 6.5
C6 0.30 629 33.1 842 781 166 7.6

Table 10. Compressive strength of nano-silica concrete samples

Concrete Mix with nano-silica
Mix
No. 1-day 1-day
3-day 7-day 28-day 3-day* 7-day* 28-day*
autoclaving autoclaving*
C1A 78.60 (8.41) 88.30 (10.93) 98.60 (11.79) 92.60 (9.72)
C1 72.50 79.60 88.20 84.40
C1B 79.70 (9.93) 88.30 (10.93) 104.90 (18.93) 99.00 (17.3)
C2A 82.90 (4.54) 90.60 (2.95) 100.30 (7.16) 94.50 (4.30)
C2 79.30 88.00 93.60 90.60
C2B 86.10 (8.58) 97.50 (10.80) 105.50 (12.71) 102.60 (13.25)
C3A 88.20 (5.76) 96.00 (6.90) 105.80 (7.19) 98.60 (4.01)
C3 83.40 89.80 98.70 94.80
C3B 93.00 (11.51) 102.50 (14.14) 110.40 (11.85) 104.50 (10.23)
C4A 73.90 (6.18) 81.10 (6.01) 92.40 (9.09) 88.60 (11.03)
C4 69.60 76.50 84.70 79.80
C4B 76.40 (9.77) 84.40 (10.33) 97.00 (14.52) 95.00 (19.05)
C5A 82.70 (7.68) 88.00 (6.41) 96.60 (8.66) 92.00 (6.98)
C5 76.80 82.70 88.90 86.00
C5B 82.80 (7.81) 90.00 (8.83) 99.40 (11.81) 95.00 (10.47)
C6A 86.40 (5.62) 92.40 (3.01) 101.20 (7.66) 94.20 (3.29)
C6 81.80 89.70 94.00 91.20
C6B 89.40 (9.29) 98.60 (9.92) 103.20 (9.79) 98.20 (7.68)
Note: 1. Addition of nano-silica in control mix is represented by Letter A and B for 1.5% and 3% respectively, e.g. C1A means addition of
1.5% nano-silica in control mix C1. Likewise C1B means addition of 3 % nano-silica in control mix C1.
* The values in parenthesis indicate the percentage variation of compressive strength with respect to control concrete samples.

The compressive strength results for concrete cubes
are given in Table 10. It can be observed from Tables 8
and 10, that cube strength of concrete is comparable or
higher than that of the mortar cube strength when the
proportion of mortar is in excess of the void by 0.10, at all
ages up to the age of 28 days. For proportion of mortar
being in excess of the void by 0.20 and 0.30, concrete cube
strengths are higher than those of the corresponding
mortar at all ages upto 28 days. This is inspite of the fact
that size of the concrete cube is 15 cm while mortar tests
were conducted with smaller cubes for which strength
expected were more. Thus, it is conirmed that silica
fume improves the ITZ and is no longer the weakest
link in the system. The inclusion of coarse aggregates
reduces the overall porosity and improves the modulus
of elasticity of the solid system, hence this improvement
in strength is realised.20 The more the proportion of the
mortar, the higher the strength because of reduction of
shrinkage of paste at ITZ. Thus shrinkage cracks are
absent due to global bulk shrinkage of the material rather
than shrinkage of paste at aggregate interface. Nano-
silica had been added at two levels, 1.5% and 3%. On
addition of nano-silica, strength enhancement up to 19%
is observed. Further 3% nano-silica addition enhanced
the strength more when compared to 1.5% nano-silica
addition. Further, the strength enhancement is higher
for lower w/b ratio concrete. Thus, it is inferred that
nano-silica as an admixture can enhance the strength of
cement-silica fume concrete up to 19% when concrete
mixture proportion is appropriate and implications
for high strength concrete are positive. The effect of
autoclaving is similar to that observed in the case of
mortar. The methodology adopted in this work for
obtaining the mix proportion of concrete, when suitably
modiied, may also serve as a method for obtaining mix
proportion of concrete.

20 THE INDIAN CONCRETE JOURNAL JUNE 2013

JUNE 2013 THE INDIAN CONCRETE JOURNAL 21
Microstructure study
In addition to the study of compressive strength
enhancement due to nano-silica addition, some
investigations were carried out for the effect of nano-
silica addition on the microstructure of cement paste
through X-ray diffraction (XRD), Scanning Electron
Microscopy (SEM) and Atomic Force Microscopy (AFM).
The results of these investigations are presented in this
section.
22 THE INDIAN CONCRETE JOURNAL JUNE 2013
XRD results for cement-silica fume paste and cement-
silica fume and nano-silica paste carried out on paste
P1A and P1A2, P1A4, P1A6, are given in Figure 5.
Comparison of peaks in these figures reveals no
difference in mineralogical features of pastes, with and
without nano-silica, thus polycrystalline mineralogical
characteristics of the cement-silica fume paste do not
alter with nano-silica addition.
SEM micrographs of the P1A and P1A2, P1A4, P1A6,
pastes are given in Figure 6. These images were taken at
10000x magniication. Not much difference is observed
in these SEM scans except for reduction of some micro-
cracks.
Some preliminary surface morphology studies were also
carried out on pastes P1A and P1A2, P1A4, P1A6 using
AFM. The AFM used in the present study, i.e. Nano Surf
Easy Scan 2 AFM is capable of capturing 3 dimensional
images with planar area of maximum 71.1 x 71. 1 m
and up to depth of 15.6 m. The AFM is operated in
contact mode. Small cube samples of side length 2 cm
were cast and polished following standard procedure
of grinding and polishing generally adopted for optical
microscopy. It is observed that from the representative
sample images given in Figure 7 for P1A and P1A2, at
curing age of 56 days in both cases that, dark pore areas
reduced after the addition of nano-silica.
Nano-silica being extremely ine is able to penetrate into
the interstitial spaces within silica-fume particles and
make the microstructure sounder, resulting in reduction
in micro-cracks, as observed through SEM in the case
of samples with nano-silica. This may also be the cause
of reduction in pores as observed from the surface
morphology study carried out through AFM.
Hence it can be concluded from the above microstructure
investigations that, the addition of nano-silica in cement
silica fume cementitious system for concrete, does not
adversely affect the microstructure of the material, rather
may cause improvement.
Conclusions
Concrete and other cement based materials (CBM)
prepared with hydraulic cement binder can be regarded
as chemically bonded ceramics. These composite
materials in their microstructure contain random
features over a wide range of length scales, from
nanometre (CSH gel) through micro-metre (HCP) to
millimetre (mortar and concrete) with each length scale
presenting a new random composite. Well-compacted
concrete prepared with hard low porosity aggregates
may be assumed to be a multiphase material consisting
of coarse aggregates embedded in mortar matrix. The
mortar matrix consists of ine aggregates, the solid
JUNE 2013 THE INDIAN CONCRETE JOURNAL 23
cement hydrates, un-hydrated cement etc., and the
pore system. The pores system present in the mortar of
concrete however, is markedly different from the pores
of a well-compacted paste prepared independently
using identical proportions of the relevant ingredients
due to the transition zone pores present at the mortar
aggregate interface. Hence in this study cement paste,
mortar as well as concrete properties were studied and
the following conclusions were drawn.
1. A systematic procedure has been presented in
this paper, considering concrete as a multiphase
material described above to arrive at a suitable
mix proportion of high strength concrete with
nano-silica as an additive. The procedure can
be suitably modiied, to serve as a method for
obtaining mix proportion of concrete in general.
2. Adding of nano-silica causes reduction of low
and increases the low loss in case of mortar and
possibly thus for concrete as well.
3. Through this investigation it is reafirmed again
that, silica fume when present in the cementitious
system, improves the ITZ, thus, ITZ ceases to
be the weakest link in high strength concrete or
mortar.
4. Nano-silica as an admixture can enhance
the strength of cement-silica fume concrete
considerably, even up to 19% when concrete
mixture proportions are appropriate.
5. Nano-silica addition does not adversely affect
the microstructure of paste to induce negative
inluence on properties of concrete.
Acknowledgements
We sincerely thank CICO, FOSROC, BASF, SIKA and
ASIAN LABORATORY for providing us with the
required superplasticisers for conducting this research
work. We also thank ELKEM for providing silica fume
to complete this work as well as EKA, BEECHEM for
providing us nano-silica samples.
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24 THE INDIAN CONCRETE JOURNAL JUNE 2013
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 Abh ik Gh osh holds B.E. degree in Civil Engineering
from Bengal Engineering & Science Universit y, Shibpore
( BESUS) , M.Tech. degree in Const ruct ion Technology
and Managem ent from I ndian I nst it ut e of Technology,
Delhi ( I I T- Delhi) and Post Graduat e Diplom a in Business
Adm inist rat ion ( PGDBA) in Finance from Sym biosis
Cent re for Dist ance Learning ( SCDL) . He is Assist ant
Manager at Larsen & Toubro Lim it ed. His int erest s
Be an I C J Author
include st udies on st rengt h and m icrost ruct ure by incorporat ing
nano- silica in cem ent- silica fum e based cem ent it ious syst em s.

V. Sa ir a m holds a B.Tech degree from Bapat la

Engineering College, Bapat la and M.Tech degree from
S.J.C.E. Mysore. He is present ly pursuing his PhD in t he
Depart m ent of Civil Engineering at t he I ndian I nst it ut e
of Technology ( I I T) , Delhi, I ndia. His research int erest s
include m icrost ruct ure m odelling by incorporat ing
nano- silica and silica fum e in cem ent based m at erials.

We at ICJ offer an opportunity to our

D r . Bish w a j it Bh a t t a ch a r j e e , B.Tech ( Hons.) ,
M.Tech., PhD, is Professor at t he Depart m ent of Civil
readers to contribute articles and be a part
Engineering, I ndian I nst it ut e of Technology Delhi. His of a big family of ICJ authors.
areas of act ive research int erest includes corrosion
of rebar in concret e, high- perform ance concret e,
m icrost ruct ure m odelling of concret e, chloride
In particular, we will appreciate receiving
ingress, service life predict ion and life cycle cost ing contributions on the following:
of concret e st ruct ures besides condit ion evaluat ion
and healt h m onit oring of st ruct ures. Minor area of research and
t eaching int erest s are Building Physics and Building Engineering, Articles bearing on innovative design
Const ruct ion Technology and Const ruct ion m anagem ent . He is and construction
Fellow of I ndian Associat ion of St ruct ural Engineers. He is Life
m em ber of 1) I ndian Concret e I nst it ut e, 2) I ndian Societ y for
Const ruct ion Mat erials and St ruct ure. 3) I ndian Societ y for Technical Articles dealing with challenging
Educat ion. 4) Am erican Societ y of Civil Engineers I ndia Sect ion construction problems and how they
( ASCE- I S) 5) Maharasht ra Chapt er of Am erican Concret e I nst it ut e were solved.
( ACI ) et c. He has aut hored m ore t han 90, well cit ed, j ournal
and conference papers in leading I nt ernat ional j ournals such as
ACI m at erials Journal, Journal of Mat erials in Civil Engineering, Just a Point of view covering your
ASCE; Cem ent and Concret e research and The I ndian Concret e
opinion on any facet of concrete,
Journals and ot hers, besides aut horing st at e of t he art report , lect ure
not es and art icles in workshop proceeding et c. He also had a visit ing construction and civil engineering
posit ion in EPFL Swit zerland and involved in collaborat ive research
program s wit h Germ an Universit ies and Universit y of Dundee UK. He
has handled m ore t han 200 consult ancy and research proj ect s and
All contributions will be reviewed by
is act ively involved in various nat ional com m it t ees. Dr. Bhat t acharj ee expert Editorial Committee. Limit your
has supervised 125 M. Tech. and 11 Ph.D. t hesis t ill dat e and current ly contribution to about 2000 words only.
guiding 7 M.Tech. t hesis work besides 10 ongoing Ph.D. research
proj ect s. He is also m em ber of t he edit orial board of Magazine of
Concret e Research and I nt ernat ional Journal of 3Rs. Contact: The Editor, The Indian Concrete Journal,
ACC Limited, L.B. Shastri Marg, Thane 400 604.
Tel: +91 (22) 33027646 E-mail: editor@icjonline.com

JUNE 2013 THE INDIAN CONCRETE JOURNAL 25