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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

tional mixtures. The construction industry is fast paced;

Since concrete is the most used material in construction, for this reason, a concrete mixture with MAs translates

reduction on concrete fabrication energy costs and CO2 into economic losses. This situation can represent more

emissions are critical.1,2 For that reason, new efforts are days to remove the wood from the structure and other

dedicated to partly replace cement with mineral admix- ancillary costs.

tures (MAs). Such cement replacement, in a concrete When SCM is present, the ‘early age’ scale can extend

mix, helps to lower the total mix cost while lessening the to more than 28 days, as it is usually considered for

environmental damage. regular concrete with PC; for example, when FA is used,

The most common MAs, known as supplementary the early age can be considered to up to 56 days.

cementing materials (SCM), which are often added to However, due to the scope of the present work, for the

concrete mixtures, are fly ash (FA) and silica fume.3 Fly ensuing experiment, we call ‘early age’ the first 28 days

ash is a manufacturing waste produced during coal of curing.

burning and is the SMC most frequently used to replace Essentially, this project is intended to study concrete

Portland cement (PC) in concrete mixtures.3 Researchers strength during the said time to avoid accidents resulting

found that after 90 days, FA increases the strength and from structure weakness. We propose the use of

durability of concrete, and that product is more nanosilica (nS) to compensate the loss of concrete

environment friendly and cheaper than cement.3,4–7 compressive strength at early age due to cement

However, in some cases when FA class F is used as replacement. Additionally, this project investigates the

SCM, the material loses compressive strength at early alternative of use nS as an accelerator of the concrete

age due to a slower reaction;4 the material physico- hardness process, resulting in higher compressive

chemical properties effect the slow reaction. Fly ash, in strength at early age and long durability afterwards.

this case, needs a pozzolanic reaction to form com- We seek to shed more light on the understanding of

pounds that bear cementitious properties.4 This reaction compressive strength gains when adding nS to a concrete

requires more days than the hydration process of the mixture using cement with MAs, as opposed to perfectly

conventional mixes. In addition, a concrete mixture that 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

1

Graduate Program of the Department of Industrial Engineering, University added to a PC with MA mixture compared to the

of Puerto Rico, Mayagüez 00681-9000, Puerto Rico compressive strength of a conventional PC mixture.

2

Department of Civil Engineering, University of Puerto Rico, Mayagüez

00681-9000, Puerto Rico

3

Department of General Engineering, University of Puerto Rico, Mayagüez Literature review

00681-9000, Puerto Rico

4

Department of Industrial Engineering, University of Puerto Rico, In the last decade, cement replacement such as SCM, in

Mayagüez 00681-9000, Puerto Rico general, and FA and silica fume, in particular, became of

*Corresponding author, email nitza.garcia@upr.edu much research interest.5,8 Unfortunately, FA is the SCM

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, mixer for 0?5 min at 60 rev min21. The nS and SP were

causing sometimes unpredictable results. Mixtures that diluted in water in order to spread the particles through

contain FA are considered as eco-concrete mixtures, the mixture and added to the mixer (when used) for

which are commercially attractive and help reduce 5 min at 120 rev min21. Fifteen cylinders were filled by

emissions of CO2. To compensate for the detrimental the rodding method (ASTM C192, 2013). The dimen-

effects, alternatives such as introducing calcium directly sions of the test cylinders prepared for each mixture had

during the burning coal process and using nS as an 50 mm of diameter and 100 mm of length (ASTM C470,

additive to the cement blend are being studied.3,9 2002).

The use of nS in addition to raise the concrete Three cylinders were tested for compressive strength

compressive strength also accelerates the concrete hard- at 1, 3, 7, 14 and 28 days of curing. These compressive

ening process, increases its density, reduces its porosity tests were performed in a 3000 kN Forney universal test

and improves the binding among cement paste and machine according to ASTM C39 (2014). The first three

aggregates or the strength of the interfacial transition cylinders were demoulded and then tested. The other

zone.10–13 However, it is not well known how much ones were placed in limewater until tested at normal

compressive strength is earned when specific amounts of curing conditions (20–23uC and RH5100%). The

nS are used. To assess this effect, we deemed it necessary temperature (23–25uC) in the experiment was deemed

to develop a statistical methodology able to analyse the invariant enough.

use of these materials (FA and nS) and study their Additionally, while concrete strength upon the hard-

interaction in the concrete mixture. Hence, this work ening state is important, one cannot disregard the

proposes a statistical design of experiments for mixtures workability during the fresh state. Additional water is

to investigate the effect of FA and nS in concrete required when nS is added to the mixture;11 due to this

compressive strength at its early age. fact, it was important to study and analyse the

behaviour and workability of the mixture during its

Experimental conditions fresh state when two water/binder (w/b) ratios were

utilised. Furthermore, the two values of w/b ratio

Materials and experimental procedures allowed observing the reactivity of the materials in

A preliminary sieve analysis allowed establishing the different aqueous states. In addition to more water, SP

experimental proportions of the aggregates: 30% lime- was needed to maintain the workability of the mixture

stone, 35% processed aggregate and 35% of clean beach for a longer time. This mixture workability was assessed

sand. The maximum diameter of the limestone was in the slump analysis of the mixtures.

9?5 mm. In addition, the processed aggregate had a The design of experiments for mixtures was used since

maximum diameter of 4?8 mm. The fineness modulus of coarse and fine aggregate, water and PC compose the

beach sand was 2?02. Portland cement type I was utilised concrete mixture. Since the focus of the project was

to prepare the mixtures, and its specific gravity was 2?9. cement replacement, the work focused specifically on the

Fly ash class F was characterised and used for the cement mixture that is added to the final concrete

mixtures. The specific gravity of the FA was 2?22. The mixture (Fig. 2).

particles of nS were suspended in water (slurry) and were The design used PC, FA and nS as the cement mixture

obtained from Nissan Chemical Industries in Texas. The components where the sum of all component propor-

polycarboxylate superplasticiser (SP) used was ADVA tions should equal to one. The lower and upper

575 obtained from Instron in Puerto Rico. Furthermore, experimental limits of each component were as follows.

mixture behaviour, i.e. segregation, bleeding, slump loss Fly ash varied from 0 to 40%, which is a common upper

and consistency, was taken into account to determine limit in industrial practice. The nS amount was varied

the quantity of SP necessary for each mixture. from 0 to 6% since more than 6% is not recommended

A Blakeslee Mixer machine was utilised to mix the because it may lead to chemical incompatibilities due to

concrete components. The aggregates were first intro- dispersion problems.11 Portland cement was varied from

duced in the mixer for 0?5 min at 60 rev min21 followed 54 to 100% (Table 1). Therefore, a design of experiments

by half of the required water. Portland cement was based on mixtures with extreme vertices was consid-

mixed dry with FA (when used) and then added to the ered;14,15 the feasible region can be observed in Fig. 3.

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

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

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

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

Compressive strength

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

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

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

considered practical. This behaviour remained the same Change of variable (equations (6)–(8))

for both w/b ratio levels.

An optimisation problem of maximising concrete w=b~0:3Z1 z0:5Z2 (6)

compressive strength was formulated in MS Solver, an

optimisation tool available in Microsoft Excel, to search Z1 zZ2 ~1 (7)

for an optimal mixture that would satisfy all the

restrictions and, simultaneously, be a practical mixture Z1 ,Z2 as binary variables (8)

utilising cement replacement. First, the data were

where PC, FA and nS are the proportions of PC, FA

divided in two groups with distinct behaviour: before

and nS respectively; w/b is the water to binder ratio; Z1

and after 7 days of age. During the former, maturity of

and Z2 are used to restrict the values of w/b to those

the concrete compressive strength increases rapidly,

considered in the experiment.

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, Discussion of results

14 and 28 days (group 2) was also obtained. This The results show that the three optimisation formula-

analysis provides the slope and intercept of each line for tions for slope 1, Y7 and Y28 converge almost to the

each mixture (Fig. 6). Slope 1 and intercept 1 represent same proportions for each mixture component; hence, if

the fit for group 1; slope 2 and intercept 2 represent the one of them is maximised, the others will be maximised,

fit for group 2. Since we sought to obtain the highest too. However, the suggested proportions correspond to

value of compressive strength in early age, higher values a non-practical mixture of 94%PC, 6%nS and 0%FA.

of slopes and intercepts are convenient. Cubic regression Therefore, the regression model of Y7 was selected to

models were utilised to represent the slope and intercept maximise the concrete compressive strength but this

values as functions of the mixture proportions. time forcing the model to include some proportion of

Afterwards, the regression model of Y7, Y28 and slope FA to the mixture for being of interest to the project.

1 were used in the solver to see if the suggested mixture The constraint of FA .0 was modified by FA greater

proportions that maximise the compressive strength than some value of epsilon e. The values of e were set at

were the same. In this case, slope 1 was selected because values of 0?00, 0?10, 0?20, 0?30 and 0?40. Then, the

the expectation is to increase it in order to achieve higher component proportions found through the optimisation

compressive strength. Regression models for Y7 and Y28 procedure were recorded as the ones that maximise the

were selected because the search looks for a mixture with response variable (Table 4 and Fig. 7).

replacement that has the highest compressive strength in This analysis shows that the optimisation procedure

days 7 and 28. always selects the lowest value allowed of FA and the

Optimisation problem: highest value of nS. The results were compared with real

Find PC, FA, nS, w/b to experimental values when available for validation

Maximise equation (1) purposes, within 1% of difference. The percentage of

Subject to loss of compressive strength intensifies as the proportion

Component restrictions (equations (2)–(4)) of FA increases in the mixture. If we replace PC with a

combination of 20%FA and 6%nS (resulting in a total of

0:54ƒPCƒ1 (2)

26%), the subsequent loss of compressive strength will be

10?8%. However, if we replace PC with a combination of

0ƒFAƒ0:40 (3) 40%FA and 6%nS (resulting in a total of 46%), the

subsequent loss of compressive strength will be 26?3%.

0ƒnSƒ0:06 (4) If the optimisation procedure is let free to select a

solution between the original component constraints,

Convexity (equation (5))

the use of FA is not necessary in the mixture to

PCzFAznS~1 (5) maximise the compressive strength (Table 4). Figure 7

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

shows that when the model is forced to include FA in the FA was varied to compare the results with the previous

mixture, the user has to be willing to lose compressive analyses. Figure 9 shows the difference between repla-

strength although at a lower rate than that of a linear cing cement with just FA and replacing cement with FA

loss. When a lower bound is set for FA, the optimiser combined with nS. It is apparent that as more cement is

keeps nS fixed at its highest level while varying the PC replaced, the percentage of difference between the two

fraction. This indicates that there is a greater loss of replacement approaches increases (Table 6). For exam-

compressive strength by reducing nS than by reducing ple, based on the evaluated experimental conditions, if

PC. cement is replaced in a concrete mixture with 40%FA,

An additional analysis was carried out (Table 5), the expected compressive strength in day 7 will be

varying the nS proportion in the mixture controlled by 33?03 MPa, but if cement is replaced with 40% of FA

its upper bound. In this occasion, the optimiser kept the and with an additional 6%nS, the expected compressive

quantity of nS at the highest value allowed to gain more strength in day 7 equals to 53?10 MPa. Therefore, if nS

compressive strength. The gain becomes approximately is added, there will be a difference of 60?8% in

linear when FA is its lowest (zero in this case). Figure 8 compressive strength at that point in time.

shows the increment in compressive strength as propor- Three replicates were considered in this experiment as

tions of nS are added. Following this figure, for per ASTM C192 (2013). Such sample size, when

example, adding 3%nS, the compressive strength will analysed statistically through the use of an operating

increase 8?9%, and adding 6%, the compressive strength characteristic curve, is capable to detect differences in

rises by 14?1% in the absence of FA (Table 5). compressive strength larger than 8 MPa. A difference of

In the proceeding analysis, the value of nS was set to 8 MPa can be correctly detected with a probability of

0% in the optimisation model, and the lower bound of 78?5%. Because the minimum difference between mixtures

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%

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%

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

with and without nS in our experiment was 8?89 MPa a series of optimisation problems to maximise compres-

(Table 6), the chosen number of replicates was deemed sive strength.

adequate for analysis. 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

Conclusions feasible alternative. The results provided in this study

A design of experiments with mixtures was proposed serve as guide to balance these additions to design a

and carried out here to characterise compressive proper- material to a desired nominal value of compressive

ties in time as a function of the proportions of PC, FA, strength. Additional mechanical properties will be mea-

nS and the w/b ratio. This experiment allowed obtaining sured in the future and characterised parametrically as in

regression models that were subsequently used to set up this work to better understand concrete modification.

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%

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

Acknowledgements admixtures in mortars: quantification of the physical and chemical

effects of fine admixtures in relation with compressive strength’,

This material is based upon work supported by the

Cem. Concr. Res., 2006, 36, 264–277.

National Science Foundation under grant no. HRD 9. J. Björnström, A. Martinelli, A. Matic, L. Börjesson and I. Panas:

0833112 (CREST program). Additional support was ‘Accelerating effects of colloidal nano-silica for beneficial calcium–

provided by the US Department of Education through silicate–hydrate formation in cement’, Chem. Phys. Lett., 2004, 392,

grant no. P120A120097 (MSEIP programme). 242–248.

10. A. Bakri, A. M. Mustafa, H. Kamarudin, M. Bnhussain, A. R.

Rafiza, and Y. Zarina: ‘Effect of Na2SiO3/NaOH ratios and

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