Effect of fly ash and nanosilica on

compressive strength of concrete at early age

N. M. Garcı́a*1, L. E. Zapata2, O. M. Suárez3 and M. Cabrera-Rı́os4
The replacement of cement by mineral admixtures in concrete has been of increasing interest in
the construction industry. Nevertheless, several of the potential replacements, such as fly ash
class F, lower the compressive strength of concrete at early age. This project investigates the use
of nanosilica to compensate for such loss of compressive strength. A statistical experimental
design involving mixtures of Portland cement, fly ash and nanosilica, in addition to water/binder
ratio as an external factor, is proposed to study their combined effect on the compressive strength
of concrete. This design allows estimating a cubic regression model that properly accounts for the
effects of the mixture components within a constrained experimental region. The range of each
factor was selected according to levels normally used in the industry. Finally, an optimisation
strategy permits to recommend the use of nanosilica when high percentages of cement
replacement by fly ash are present.
Keywords: Fly ash, Nanosilica, Concrete, Design of experiments, Optimisation, Early age

Introduction contains SCM requires more curing days than conven-

Since concrete is the most used material in construction,
reduction on concrete fabrication energy costs and CO2
emissions are critical.1,2 For that reason, new efforts are
dedicated to partly replace cement with mineral admix-
tures (MAs). Such cement replacement, in a concrete
mix, helps to lower the total mix cost while lessening the
environmental damage.
The most common MAs, known as supplementary
cementing materials (SCM), which are often added to
concrete mixtures, are fly ash (FA) and silica fume.3 Fly
ash is a manufacturing waste produced during coal
burning and is the SMC most frequently used to replace
Portland cement (PC) in concrete mixtures.3 Researchers
found that after 90 days, FA increases the strength and
durability of concrete, and that product is more
environment friendly and cheaper than cement.3,4–7
However, in some cases when FA class F is used as
SCM, the material loses compressive strength at early
age due to a slower reaction;4 the material physico-
chemical properties effect the slow reaction. Fly ash, in
this case, needs a pozzolanic reaction to form com-
pounds that bear cementitious properties.4 This reaction
requires more days than the hydration process of the
conventional mixes. In addition, a concrete mixture that
1
Graduate Program of the Department of Industrial Engineering, University
of Puerto Rico, Mayagüez 00681-9000, Puerto Rico
2
Department of Civil Engineering, University of Puerto Rico, Mayagüez
00681-9000, Puerto Rico
3
Department of General Engineering, University of Puerto Rico, Mayagüez
00681-9000, Puerto Rico
4
Department of Industrial Engineering, University of Puerto Rico,
Mayagüez 00681-9000, Puerto Rico
*Corresponding author, email nitza.garcia@upr.edu
tional mixtures. The construction industry is fast paced;
for this reason, a concrete mixture with MAs translates
into economic losses. This situation can represent more
days to remove the wood from the structure and other
ancillary costs.
When SCM is present, the ‘early age’ scale can extend
to more than 28 days, as it is usually considered for
regular concrete with PC; for example, when FA is used,
the early age can be considered to up to 56 days.
However, due to the scope of the present work, for the
ensuing experiment, we call ‘early age’ the first 28 days
of curing.
Essentially, this project is intended to study concrete
strength during the said time to avoid accidents resulting
from structure weakness. We propose the use of
nanosilica (nS) to compensate the loss of concrete
compressive strength at early age due to cement
replacement. Additionally, this project investigates the
alternative of use nS as an accelerator of the concrete
hardness process, resulting in higher compressive
strength at early age and long durability afterwards.
We seek to shed more light on the understanding of
compressive strength gains when adding nS to a concrete
mixture using cement with MAs, as opposed to perfectly
reproducing the behaviour of a conventional mixture
with just PC. For the sake of comparison, Fig. 1
illustrates the gain of compressive strength when nS is
added to a PC with MA mixture compared to the
compressive strength of a conventional PC mixture.
Literature review
In the last decade, cement replacement such as SCM, in
general, and FA and silica fume, in particular, became of
much research interest.5,8 Unfortunately, FA is the SCM

ß 2015 Institute of Materials, Minerals and Mining

Published by Maney on behalf of the Institute
Received 18 June 2014; accepted 11 August 2014
DOI 10.1179/1743676114Y.0000000200 Advances in Applied Ceramics 2015 VOL 114 NO 2 99
Garcı́a et al. Effect of FA and nS on compressive strength of concrete
1 Compressive strength in mixtures bearing different proportions of cement as function of mixture age
with the highest variability in chemical composition,
causing sometimes unpredictable results. Mixtures that
contain FA are considered as eco-concrete mixtures,
which are commercially attractive and help reduce
emissions of CO2. To compensate for the detrimental
effects, alternatives such as introducing calcium directly
during the burning coal process and using nS as an
additive to the cement blend are being studied.3,9
The use of nS in addition to raise the concrete
compressive strength also accelerates the concrete hard-
ening process, increases its density, reduces its porosity
and improves the binding among cement paste and
aggregates or the strength of the interfacial transition
zone.10–13 However, it is not well known how much
compressive strength is earned when specific amounts of
nS are used. To assess this effect, we deemed it necessary
to develop a statistical methodology able to analyse the
use of these materials (FA and nS) and study their
interaction in the concrete mixture. Hence, this work
proposes a statistical design of experiments for mixtures
to investigate the effect of FA and nS in concrete
compressive strength at its early age.
Experimental conditions
Materials and experimental procedures
A preliminary sieve analysis allowed establishing the
experimental proportions of the aggregates: 30% lime-
stone, 35% processed aggregate and 35% of clean beach
sand. The maximum diameter of the limestone was
9?5 mm. In addition, the processed aggregate had a
maximum diameter of 4?8 mm. The fineness modulus of
beach sand was 2?02. Portland cement type I was utilised
to prepare the mixtures, and its specific gravity was 2?9.
Fly ash class F was characterised and used for the
mixtures. The specific gravity of the FA was 2?22. The
particles of nS were suspended in water (slurry) and were
obtained from Nissan Chemical Industries in Texas. The
polycarboxylate superplasticiser (SP) used was ADVA
575 obtained from Instron in Puerto Rico. Furthermore,
mixture behaviour, i.e. segregation, bleeding, slump loss
and consistency, was taken into account to determine
the quantity of SP necessary for each mixture.
A Blakeslee Mixer machine was utilised to mix the
concrete components. The aggregates were first intro-
duced in the mixer for 0?5 min at 60 rev min21 followed
by half of the required water. Portland cement was
mixed dry with FA (when used) and then added to the
100 Advances in Applied Ceramics 2015 VOL 114 NO
mixer for 0?5 min at 60 rev min21. The nS and SP were
diluted in water in order to spread the particles through
the mixture and added to the mixer (when used) for
5 min at 120 rev min21. Fifteen cylinders were filled by
the rodding method (ASTM C192, 2013). The dimen-
sions of the test cylinders prepared for each mixture had
50 mm of diameter and 100 mm of length (ASTM C470,
2002).
Three cylinders were tested for compressive strength
at 1, 3, 7, 14 and 28 days of curing. These compressive
tests were performed in a 3000 kN Forney universal test
machine according to ASTM C39 (2014). The first three
cylinders were demoulded and then tested. The other
ones were placed in limewater until tested at normal
curing conditions (20–23uC and RH5100%). The
temperature (23–25uC) in the experiment was deemed
invariant enough.
Additionally, while concrete strength upon the hard-
ening state is important, one cannot disregard the
workability during the fresh state. Additional water is
required when nS is added to the mixture;11 due to this
fact, it was important to study and analyse the
behaviour and workability of the mixture during its
fresh state when two water/binder (w/b) ratios were
utilised. Furthermore, the two values of w/b ratio
allowed observing the reactivity of the materials in
different aqueous states. In addition to more water, SP
was needed to maintain the workability of the mixture
for a longer time. This mixture workability was assessed
in the slump analysis of the mixtures.
The design of experiments for mixtures was used since
coarse and fine aggregate, water and PC compose the
concrete mixture. Since the focus of the project was
cement replacement, the work focused specifically on the
cement mixture that is added to the final concrete
mixture (Fig. 2).
The design used PC, FA and nS as the cement mixture
components where the sum of all component propor-
tions should equal to one. The lower and upper
experimental limits of each component were as follows.
Fly ash varied from 0 to 40%, which is a common upper
limit in industrial practice. The nS amount was varied
from 0 to 6% since more than 6% is not recommended
because it may lead to chemical incompatibilities due to
dispersion problems.11 Portland cement was varied from
54 to 100% (Table 1). Therefore, a design of experiments
based on mixtures with extreme vertices was consid-
ered;14,15 the feasible region can be observed in Fig. 3.
2
 Garcı́a et al. Effect of FA and nS on compressive strength of concrete

2 Experiment design with mixtures including cement mix

within concrete mixture

In addition, the w/b ratio was included in the 3 Mixture proportions (design points) evaluated during
experiment as an external factor in two levels: 0?3 experiment
(low) and 0?5 (high); this allowed varying the amount of
water in the mixture. These levels reflected the limits
so on. All the results of the residuals analyses, i.e.
found in the industrial fabrication of structural con-
normality test, independence test and variance analysis,
crete.16 The points in the experimental design prescribe
were deemed acceptable. Table 2 shows a summary of
the proportions for each mixture to be evaluated. Three
the results that represent the significance of terms base
replicates were measured on each design point. The total
on p values. The terms that affected all the models were
number of design points considering the w/b factor was
the interactions between PC and w/b ratio, and FA with
18. Equation (1) presents the cubic regression model
w/b ratio; however, different interactions were important
fitted to study the compressive strength, i.e. the response
at different points of concrete’s age. The decision to
variable, for different days.
keep all terms obeyed to the idea of keeping the results
^ ^ ^ ^ ^ precise.
Yi ~b1 PCzb2 FAzb3 nSzb4 PC|FAzb5 PC|nSz
The mixtures with higher compressive strength were
^ ^ ^ w ^ w
b6 FA|nSzb7 PC|FA|nSzb8 PC| zb9 FA| the ones with w/b ratio of 0?3 (see Fig. 4); the range in
b b compressive strength obtained was 11?51 MPa (at
^ w ^ w ^ w 1 day) to 86?32 MPa (at 28 days). The lower ones were
zb10 nS| zb11 PC|FA| zb12 PC|nS| z
b b b those with a w/b ratio of 0?5 (see Fig. 5), ranging from
^ w ^ w 2?79 MPa (at 1 day) to 49?85 MPa (at 28 days). The
b13 FA|nS| zb14 PC|FA|nS| (1)
b b individual mixtures with higher compressive strength
where PC, FA and nS represent PC, FA and nS were those with only PC and nS. These two mixtures, i.e.
proportions respectively added to the concrete mixture; 13 and 12, exceeded the control one, i.e. 7, with only PC;
w/b is the value of water/binder ratio used in the mixture, all these mixtures contained a w/b of 0?3 (Table 3).
and Yi is compressive strength measured in the ith day in However, since the interest of this project was the
MPa. cement replacement by FA, these mixtures were not

Results Table 2 Computed p values for interaction terms

After completing the mixture analysis, the interaction between mixture components
terms that significantly affect the response variable as a
Term Y1 Y3 Y7 Y14 Y28
function of the age in days were identified. Y1 in our
experiments correspond to the compressive strength PC6FA 0.000 0.434 0.860 0.398 0.017
measurements taken at day 1, Y3 for those at day 3 and PC6nS 0.183 0.453 0.520 0.013 0.372
FA6nS 0.037 0.532 0.536 0.031 0.416
Table 1 Lower and upper proportion limits for cement PC6FA6nS 0.005 0.902 0.964 0.890 0.265
mixture components PC6w/b 0.000 0.000 0.000 0.000 0.000
FA6w/b 0.000 0.000 0.000 0.000 0.000
Mixture components Lower limit/% Upper limit/% nS6w/b 0.155 0.145 0.187 0.400 0.118
PC6FA6w/b 0.000 0.759 0.207 0.193 0.863
Portland cement 54 100 PC6nS6w/b 0.069 0.141 0.253 0.456 0.157
Fly ash 0 40 FA6nS6w/b 0.080 0.335 0.071 0.234 0.077
Nanosilica 0 6 PC6FA6nS6w/b 0.000 0.003 0.901 0.313 0.205

Advances in Applied Ceramics 2015 VOL 114 NO 2 101

Garcı́a et al. Effect of FA and nS on compressive strength of concrete

4 Compressive strength of concrete cylinders fabricated with w/b ratio of 0?3 after curing

5 Compressive strength of concrete cylinders fabricated with w/b ratio of 0?5 after curing

Table 3 Average compressive strength of three replicates in each testing day

Compressive strength

Mix no. Portland cement Fly ash Nanosilica Water/binder Y1/MPa Y3/MPa Y7/MPa Y14/MPa Y28/MPa

1 0.94 0.00 0.06 0.5 14.98 30.45 47.38 48.56 48.81

2 0.80 0.20 0.00 0.3 22.20 38.20 49.67 53.76 67.50
3 0.54 0.40 0.06 0.5 4.25 12.90 18.33 20.31 26.90
4 0.57 0.40 0.03 0.5 2.98 7.83 15.67 16.62 21.49
5 0.60 0.40 0.00 0.5 2.98 6.19 10.00 14.59 19.87
6 1.00 0.00 0.00 0.5 8.41 19.27 27.04 27.90 32.06
Control 7 1.00 0.00 0.00 0.3 32.03 52.09 64.01 68.50 78.58
8 0.60 0.40 0.00 0.3 16.46 23.68 32.11 43.70 54.70
9 0.57 0.40 0.03 0.3 16.40 28.14 45.77 51.19 60.94
10 0.80 0.20 0.00 0.5 5.62 12.39 16.87 21.65 28.89
11 0.74 0.20 0.06 0.3 24.92 51.52 63.90 68.44 75.31
12 0.97 0.00 0.03 0.3 30.59 55.65 66.99 75.05 80.04
Non-practical 13 0.94 0.00 0.06 0.3 30.56 58.58 73.15 80.51 84.43
14 0.97 0.00 0.03 0.5 11.90 25.79 33.08 37.68 41.92
Mix of interest 15 0.77 0.20 0.03 0.3 21.35 44.52 58.44 67.02 76.34
16 0.54 0.40 0.06 0.3 12.24 36.63 52.42 58.24 64.78
17 0.77 0.20 0.03 0.5 6.46 16.60 25.14 31.88 31.66
18 0.74 0.20 0.06 0.5 6.94 18.73 30.23 33.08 37.43

102 Advances in Applied Ceramics 2015 VOL 114 NO 2


6 Mixture growth divided in two linear fits
considered practical. This behaviour remained the same
for both w/b ratio levels.
An optimisation problem of maximising concrete
compressive strength was formulated in MS Solver, an
optimisation tool available in Microsoft Excel, to search
for an optimal mixture that would satisfy all the
restrictions and, simultaneously, be a practical mixture
utilising cement replacement. First, the data were
divided in two groups with distinct behaviour: before
and after 7 days of age. During the former, maturity of
the concrete compressive strength increases rapidly,
while in the latter, it increases at a slower rate. A linear
fit for data on days 1, 3 and 7 (group 1) was obtained for
each mixture. Another linear model for the datasets of 7,
14 and 28 days (group 2) was also obtained. This
analysis provides the slope and intercept of each line for
each mixture (Fig. 6). Slope 1 and intercept 1 represent
the fit for group 1; slope 2 and intercept 2 represent the
fit for group 2. Since we sought to obtain the highest
value of compressive strength in early age, higher values
of slopes and intercepts are convenient. Cubic regression
models were utilised to represent the slope and intercept
values as functions of the mixture proportions.
Afterwards, the regression model of Y7, Y28 and slope
1 were used in the solver to see if the suggested mixture
proportions that maximise the compressive strength
were the same. In this case, slope 1 was selected because
the expectation is to increase it in order to achieve higher
compressive strength. Regression models for Y7 and Y28
were selected because the search looks for a mixture with
replacement that has the highest compressive strength in
days 7 and 28.
Optimisation problem:
Find PC, FA, nS, w/b to
Maximise equation (1)
Subject to
Component restrictions (equations (2)–(4))
0:54ƒPCƒ1 (2)
0ƒFAƒ0:40 (3)
0ƒnSƒ0:06 (4)
Convexity (equation (5))
PCzFAznS~1 (5)
Garcı́a et al. Effect of FA and nS on compressive strength of concrete
Change of variable (equations (6)–(8))
w=b~0:3Z1 z0:5Z2 (6)
Z1 zZ2 ~1 (7)
Z1 ,Z2 as binary variables (8)
where PC, FA and nS are the proportions of PC, FA
and nS respectively; w/b is the water to binder ratio; Z1
and Z2 are used to restrict the values of w/b to those
considered in the experiment.
Discussion of results
The results show that the three optimisation formula-
tions for slope 1, Y7 and Y28 converge almost to the
same proportions for each mixture component; hence, if
one of them is maximised, the others will be maximised,
too. However, the suggested proportions correspond to
a non-practical mixture of 94%PC, 6%nS and 0%FA.
Therefore, the regression model of Y7 was selected to
maximise the concrete compressive strength but this
time forcing the model to include some proportion of
FA to the mixture for being of interest to the project.
The constraint of FA .0 was modified by FA greater
than some value of epsilon e. The values of e were set at
values of 0?00, 0?10, 0?20, 0?30 and 0?40. Then, the
component proportions found through the optimisation
procedure were recorded as the ones that maximise the
response variable (Table 4 and Fig. 7).
This analysis shows that the optimisation procedure
always selects the lowest value allowed of FA and the
highest value of nS. The results were compared with real
experimental values when available for validation
purposes, within 1% of difference. The percentage of
loss of compressive strength intensifies as the proportion
of FA increases in the mixture. If we replace PC with a
combination of 20%FA and 6%nS (resulting in a total of
26%), the subsequent loss of compressive strength will be
10?8%. However, if we replace PC with a combination of
40%FA and 6%nS (resulting in a total of 46%), the
subsequent loss of compressive strength will be 26?3%.
If the optimisation procedure is let free to select a
solution between the original component constraints,
the use of FA is not necessary in the mixture to
maximise the compressive strength (Table 4). Figure 7
Advances in Applied Ceramics 2015 VOL 114 NO 2 103
Garcı́a et al. Effect of FA and nS on compressive strength of concrete

7 Variation in concrete compressive strength as amounts of FA change (nS set at 0?06)

shows that when the model is forced to include FA in the
mixture, the user has to be willing to lose compressive
strength although at a lower rate than that of a linear
loss. When a lower bound is set for FA, the optimiser
keeps nS fixed at its highest level while varying the PC
fraction. This indicates that there is a greater loss of
compressive strength by reducing nS than by reducing
PC.
An additional analysis was carried out (Table 5),
varying the nS proportion in the mixture controlled by
its upper bound. In this occasion, the optimiser kept the
quantity of nS at the highest value allowed to gain more
compressive strength. The gain becomes approximately
linear when FA is its lowest (zero in this case). Figure 8
shows the increment in compressive strength as propor-
tions of nS are added. Following this figure, for
example, adding 3%nS, the compressive strength will
increase 8?9%, and adding 6%, the compressive strength
rises by 14?1% in the absence of FA (Table 5).
In the proceeding analysis, the value of nS was set to
0% in the optimisation model, and the lower bound of
FA was varied to compare the results with the previous
analyses. Figure 9 shows the difference between repla-
cing cement with just FA and replacing cement with FA
combined with nS. It is apparent that as more cement is
replaced, the percentage of difference between the two
replacement approaches increases (Table 6). For exam-
ple, based on the evaluated experimental conditions, if
cement is replaced in a concrete mixture with 40%FA,
the expected compressive strength in day 7 will be
33?03 MPa, but if cement is replaced with 40% of FA
and with an additional 6%nS, the expected compressive
strength in day 7 equals to 53?10 MPa. Therefore, if nS
is added, there will be a difference of 60?8% in
compressive strength at that point in time.
Three replicates were considered in this experiment as
per ASTM C192 (2013). Such sample size, when
analysed statistically through the use of an operating
characteristic curve, is capable to detect differences in
compressive strength larger than 8 MPa. A difference of
8 MPa can be correctly detected with a probability of
78?5%. Because the minimum difference between mixtures

Table 4 Optimisation results varying lower constraint of FA

Variation of fly ash e 0 0.10 0.20 0.30 0.40
Optimiser value/MPa Z 72.09 68.63 64.31 59.14 53.10
Experimental value/MPa Z 73.15 … 63.90 … 52.42
Decision variables in proportions PC 0.94 0.84 0.74 0.64 0.54
FA 0.00 0.10 0.20 0.30 0.40
nS 0.06 0.06 0.06 0.06 0.06
w/b 0.3 0.3 0.3 0.3 0.3
Percentage of loss of Compressive strength … 4.8% 10.8% 18.0% 26.3%

Table 5 Optimisation results varying of upper constraint of nS

Variation of nanosilica e 0 0.01 0.02 0.03 0.04 0.05 0.06
Optimiser value/MPa Z 63.20 65.33 67.20 68.82 70.17 71.26 72.09
Experimental value/MPa Z 64.01 … … 66.99 … … 73.15
Decision variables in proportions PC 1.00 0.99 0.98 0.97 0.96 0.95 0.94
FA 0.00 0.00 0.00 0.00 0.00 0.00 0.00
nS 0.00 0.01 0.02 0.03 0.04 0.05 0.06
w/b 0.3 0.3 0.3 0.3 0.3 0.3 0.3
Percentage of gain of compressive strength … 3.4% 6.3% 8.9% 11.0% 12.7% 14.1%

104 Advances in Applied Ceramics 2015 VOL 114 NO 2

 Garcı́a et al. Effect of FA and nS on compressive strength of concrete

8 Variation in concrete compressive strength as nS increases (FA level50?0)

9 Comparison graph between mixtures containing FA with and without nS

with and without nS in our experiment was 8?89 MPa
(Table 6), the chosen number of replicates was deemed
adequate for analysis.
Conclusions
A design of experiments with mixtures was proposed
and carried out here to characterise compressive proper-
ties in time as a function of the proportions of PC, FA,
nS and the w/b ratio. This experiment allowed obtaining
regression models that were subsequently used to set up
a series of optimisation problems to maximise compres-
sive strength.
The addition of FA to concrete, as shown in this
experiment, results in loss of compressive strength at early
age. To offset such loss, the addition of nS is proved a
feasible alternative. The results provided in this study
serve as guide to balance these additions to design a
material to a desired nominal value of compressive
strength. Additional mechanical properties will be mea-
sured in the future and characterised parametrically as in
this work to better understand concrete modification.

Table 6 Comparison between optimiser results of mixtures with and without nS

Variation of fly ash e 0 0.10 0.20 0.30 0.40
Optimiser value with nS50.06/MPa ZnS 72.09 68.63 64.31 59.14 53.10
Optimiser value with nS50.0/MPa ZwnS 63.20 56.75 49.57 41.66 33.03
Difference/MPa … 8.89 11.88 14.74 17.47 20.07
Percentage of difference … 14.1% 20.9% 29.7% 41.9% 60.8%

Advances in Applied Ceramics 2015 VOL 114 NO 2 105

Garcı́a et al. Effect of FA and nS on compressive strength of concrete
Acknowledgements
This material is based upon work supported by the
National Science Foundation under grant no. HRD
0833112 (CREST program). Additional support was
provided by the US Department of Education through
grant no. P120A120097 (MSEIP programme).
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