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Structures 33 (2021) 3461–3474

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Structures
journal homepage: www.elsevier.com/locate/structures

Analysis of the properties of the self-compacting concrete mixed with tire


rubber waste based on design of experiments
Demarcus Werdine a, Guilherme Antonio Oliver c, Fabricio Alves de Almeida b,
Mirian de Lourdes Noronha c, Guilherme Ferreira Gomes, Ph.D. c, *
a
Physics and Chemistry Institute, Federal University of Itajubá (UNIFEI), Itajubá, Brazil
b
Institute of Industrial Engineering and Management, Federal University of Itajubá, Brazil
c
Mechanical Engineering Institute, Federal University of Itajubá (UNIFEI), Itajubá, Brazil

A R T I C L E I N F O A B S T R A C T

Keywords: The increase of high demand of technological innovation in building construction have increasingly the need
Self-compacting concrete materials that have special structural characteristics. Notably, the use of self-compacting concrete (SCC) has been
Tire rubber waste described by many researchers and engineers as a major revolution in concrete technology due to its fluidity and
Mechanical properties
viscosity characteristics, besides providing energy savings during its construction. Tire waste rubber (TWR) is
Design of experiments
one of the most important residues that cause serious environmental issues. Recycling TWR in the form of ag­
gregates as supplementary construction material is advantageous in many building fronts. To obtain an optimal
SCC manufacturing parameters, this research was based on the application of design of experiments. Several
mixtures, or designs, were prepared with different TRW proportions (10%, 30% and 50%). In addition, the effect
of the rubber grain size was also considered in the model in two different levels. The specimens were submitted
to quasi-static and dynamic tests in order to evaluate their structural performance. The considered responses
were the natural frequency, damping factor, compression strength and elastic modulus for different curing pe­
riods (7 and 28 days). Statistical results showed the significance of the rubber, grain and curing time for the
responses, especially for the strength and elastic modulus. The results of this paper could be a guideline for
engineers using SCC in building field.

popularity in the construction industry, as it provides a safer and more


1. Introduction environmentally friendly way to produce concrete without compro­
mising its quality [12–14].
Self-compacting concrete (SCC) is a sophisticated high-performance According to Grünewald [15], the development of SCC is a major
concrete described as the “most revolutionary step” in concrete tech­ step towards efficiency and working conditions in construction sites and
nology in the past two decades due to its impact on economic and in the prefabricated industry. This material has a better aesthetic finish
environmental sustainability in the construction industry [1]. SCC was on the concrete surface, better characteristics in the hardened state and
first developed and defined in Japan in the 1980s. In Japan, SCC concreting in shorter times, giving structures with greater durability.
development has been strongly focused on improving the process of The benefits of this type of concrete go beyond durability and
concreting complicated structures and developing concrete for strength. SCC reduces noise pollution, since it does not use vibrators,
demanding situations. which also contributes to the reduction in electricity consumption;
SCC is known as a highly fluid concrete and has minimal resistance to minimizes the risk of accidents caused by the excess of people on the
flow and is therefore able to consolidate under its own weight without slabs, as it requires less manpower; and reduces ergonomic problems in
any vibration, which provides an improvement in the construction workers, as they make less effort in launching and finishing. The use of
environment [8–11]. SCC directs civil construction to industrialized production, increasing
SCC is a special type of material where vibration/compaction is quality, durability, confidence in the structure and the safety of workers
avoided by the addition of superplasticizer additives to mixtures in the [16].
fresh state. This relatively new technology is gaining more and more For the production of SCC, CP V-ARI cement was used, with high

* Corresponding author.
E-mail address: guilhermefergom@gmail.com (G.F. Gomes).

https://doi.org/10.1016/j.istruc.2021.06.076
Received 21 December 2020; Received in revised form 16 June 2021; Accepted 22 June 2021
Available online 30 June 2021
2352-0124/© 2021 Institution of Structural Engineers. Published by Elsevier Ltd. All rights reserved.
D. Werdine et al. Structures 33 (2021) 3461–3474

Nomenclature σC Compression strength


Ec Static Modulus of Elasticity
SCC Self-compacting concrete Р Density
CP V-ARI Portland Cement V - High Initial Strength Ξ Damping Factor
DoE Design of Experiments Ω Natural frequency
TRW Tire Rubber Waste x1 Design variable: rubber ratio
SCC – REF Self-compacting concrete – Reference (0% rubber x2 Design variable: grain size
content) x3 Design variable: curing time
ABNT NBR Brazilian Association of Technical Standards y1 Mechanical response: natural frequency
ANOVA Analysis of Variance y2 Mechanical response: damping factor
EFNARC European Federation of National Associations y3 Mechanical response: compression strength
Representing for Concrete y4 Mechanical response: elastic modulus
IET Impulse Excitation Technique R2 Coefficient of determination
ASTM American Society for Testing and Materials

reduces the duration of construction, which will be reflected in lower


Table 1 construction costs [5].
Test variables and respective levels. Civil construction is responsible for between 15 and 50% of the
Mixes Percentage of TRW Granulometry of TRW
consumption of extracted natural resources. In Brazil, the consumption
of natural aggregates in the production of concrete and mortars alone is
1 10% G1 < 0.6 mm
220 million tons/year. With the need for new materials to replace these
2 4.8 mm > G2 ≥ 0.6 mm
3 30% G1 < 0.6 mm aggregates, research is being carried out in order to replace part of the
4 4.8 mm > G2 ≥ 0.6 mm aggregate with tire rubber, contributing to the preservation of natural
5 50% G1 < 0.6 mm aggregates and offering a clean alternative way of recycling for tire
6 4.8 mm > G2 ≥ 0.6 mm rubber and searching the sustainability of production processes [6,7].
The possibility of designing self-compacting rubberized concrete is of
initial strength and high fineness, which favors the production of more great interest to achieve durable applications because this new material
fluid and cohesive mixtures; the fine aggregate used was medium nat­ can join the characteristics of SCC (high fluidity, high mechanical
ural sand, of quartz origin, for having a more rounded shape and smooth resistance, low porosity, etc.) with the resistance of rubber.
texture, in order to reduce the probability of voids; the coarse aggregate Several studies have been carried out using rubber residue in making
used was zero gravel of granitic origin, since it has a maximum char­ concrete, looking for increasingly satisfactory results in the properties of
acteristic dimension of 9.5 mm, which allows better fluidity of the concrete in the hardened state. Holmes et al. (2014), observed that
mixture. granulometry and rubber content are factors that influence the charac­
A concrete will only be considered self-compacting if three proper­ teristics of concrete. Miller (2014) proved that more than 60% of rubber
ties are achieved simultaneously: fluidity, cohesion necessary for the substitution can increase the flexural strength of concrete, increasing its
mixture to flow intact between steel bars (or through ability) and energy absorption capacity.
resistance to segregation [3]. According to Turatsinze and Garros (2008), the replacement of
SCC is characterized by its high fluidity, capable of making the ma­ natural coarse aggregates (4–10 mm) with coarse rubber aggregates of
terial fill the forms where it is applied, passing between the reinforce­ similar dimensions induces a change in fresh properties. It has been
ment bars and consolidating only by the action of its own weight, observed a great variation in the results of the studies due to the di­
without presenting segregation and without the need for any type in­ versity in the granulometry and in the proportion of residue inserted in
ternal or external vibration [4]. It is not only due to noise reduction the concrete. Thus, the use of statistical methods is considered signifi­
during the construction phase, because of avoiding vibrations, but it also cant for a more adequate analysis of the influence of the concrete con­
struction parameters in the static and dynamic responses evaluated.

Fig. 1. Tire rubber waste for grain size (a) G1 < 0.6 mm and (b) 0.6 mm ≤ G2 < 4.8 mm.

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Fig. 2. Self-compacting concrete manufacturing (a) and final specimen (b).

separately, to later perform the mixing of these two elements by setting


Table 2 the optimal volume of paste.
Test variables and respective levels. From the SCC-REF line, the natural sand in volume was partially
Control factors Symbol Levels replaced by the tire rubber residue, in the proportions and gran­
ulometries as shown in Table 1. The G1 granulometry is the one whose
Low (− 1) Middle (0) High (+1)
grains are between 0.6 mm and 4.8 mm and the G2 granulometry is the
Rubber Content (%) x1 10 30 50
one whose grains are smaller than 0.6 mm.
Rubber Granulometry (mm) x2 0.6 – 4.8
Curing Time (days) x3 7 – 28
To provide a certain number of fines that would promote the vis­
cosity and cohesion required to SCC in the fresh state, we opted, in this
research, for active silica and marble powder. As an additive, the
To the best of the authors’ knowledge, there are no (or very few) superplasticizer ADI-SUPER H25® was used. It is a high-tech additive,
studies in the literature investigating, statistically, the influence of formulated based on polymers of modified carboxylic ethers, which act
rubber waste from tires, in different percentages and granulometries, on on the cement particles with a very high dispersing effect, from which
the mechanical and dynamic properties of self-compacting concrete. highly fluid concretes are obtained with an extremely low water/cement
Due to its characteristics of dosage, production and execution, the use of ratio, long maintenance and high initial and final mechanical strengths.
self-compacting concrete, by itself, is already a great gain for the civil In this research we used the tire rubber waste (TRW) residue from un­
construction sector. This benefit is even greater when the concrete is serviceable tires, of different sizes, from the used tire retreading industry
mixed with tire rubber residue. The presence of the polymer, in addition obtained by mechanical scraping process, as shown in Fig. 1.
to providing advantages in some concrete properties, contributes to the The specimens were made according to ABNT NBR 5738: 2018, using
preservation of the replaced natural aggregate and to a sustainable metallic cylinders with 10 cm in diameter and 20 cm in height greased
destination of the waste. with mineral oil, as shown in Fig. 2. According to the requirements of the
This manuscript is organized as follows: Section 2 the methodolog­ mentioned standard, the specimens, after molding and deformation,
ical procedure is presented. Section 3 presents the main results and were submitted to the curing process inside the humid chamber until
discussion about the vibration and compression tests results of the SCC reaching the ages of the tests (7 and 28 days) and submitted to the axial
specimens as well the factorial results obtained from design of experi­ compression tests and modulus of elastic.
ments (DoE). Finally, Section 4 draws the conclusions.

2. Experimental methodology 2.2. Design of experiments – Full factorial analysis

2.1. Concrete manufacturing Experimental design is a critically important tool in the scientific and
engineering world for improving the product realization process. The
SCC-REF is the acronym given to concrete made without any type of application of experimental design technique early in process develop­
residue. The dosage method adopted in this work to produce the SCC- ment can result in improved process yields reduced variability and
REF was based on the guidelines proposed by Gomes [21], verifying closer conformance to nominal or target requirements; reduced devel­
its validity through the physical and mechanical properties of the opment time and reduced overall costs. Some applications of experi­
concrete. mental design in engineering design include: evaluation and comparison
This methodology proposes to obtain SCC of high compressive of basic design configurations; evaluation of material alternatives; se­
strength (over 40 MPa at 28 days) by optimizing the composition of the lection of design parameters so that the product will work well under a
paste (cement, water, and superplasticizers) and the granular skeleton wide variety of field conditions, that is, so that the product is robust;

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Table 3
Modal and statics responses considering a full factorial design.
Continuous variables Categorial variable Experiments

Rubber Content (%) Granulometry* (mm) Curing Time (days) Natural Frequency (Hz) Damping Factor (− ) Compression Strength (MPa) Elastic Modulus (GPa)

10 G1 7 3.50 0.04110 36.567 30.014


10 G1 28 3.25 0.01758 48.790 33.645
10 G2 7 3.25 0.01508 46.734 30.243
10 G2 28 3.25 0.03968 48.504 34.507
10 G1 7 3.50 0.01276 37.134 30.482
10 G1 28 3.00 0.03283 45.563 22.028
10 G2 7 3.50 0.02333 48.555 31.257
10 G2 28 3.25 0.01132 50.713 36.118
10 G1 7 3.50 0.01575 39.426 30.545
10 G1 28 3.25 0.02231 45.703 34.160
10 G2 7 3.25 0,03443 46.225 30.374
10 G2 28 3.25 0.04446 52.496 33.916
30 G1 7 3.50 0.01901 17.927 13.949
30 G1 28 3.25 0.04167 21.499 15.668
30 G2 7 3.50 0.02071 16.157 25.673
30 G2 28 3.25 0.06388 27.788 27.800
30 G1 7 3.50 0.02681 18.920 14.548
30 G1 28 3.25 0.02264 21.626 17.374
30 G2 7 3.50 0.02467 16.151 23.386
30 G2 28 3.50 0.10412 27.273 27.289
30 G1 7 3.50 0.02025 17.590 12.359
30 G1 28 3.25 0.01612 20.308 15.268
30 G2 7 3.50 0.02313 12.707 25.131
30 G2 28 3.00 0.08498 30.481 26.501
50 G1 7 3.50 0.02722 5.666 5.378
50 G1 28 3.25 0.04174 9.978 9.992
50 G2 7 3.25 0.03009 11.115 12.486
50 G2 28 3.25 0.03788 10.632 14.971
50 G1 7 3.50 0.02677 4.730 6.348
50 G1 28 3.25 0.03827 7.124 7.935
50 G2 7 3.50 0.02377 9.978 9.183
50 G2 28 3.25 0.08002 12.274 16.087
50 G1 7 3.50 0.02964 6.366 6.388
50 G1 28 3.50 0.05250 11.115 8.433
50 G2 7 3.25 0.03187 7.124 7.483
50 G2 28 3.25 0.06539 3.801 14.938

*G1: Granulometry < 0.6 mm; G2: 0.6 mm ≤ Granulometry ≤ 4.8 mm.

Fig. 3. Compression test setup for self-compacting concrete.

determination of key product design parameters that impact product According to Mohan (2004), this methodology is based on two
performance and formulation of new products. techniques: methodology of mixture design and response surface in
The DoE approach provides a way to reveal which factors influence which the primary approach to the general problem is to optimize the
an experiment’s response. In the present study, the key idea for using mixture whose properties depend on the proportions of the component
this methodology is to find an ideal solution for making the SCC with materials. In these techniques, instead of selecting a starting point, a set
TRW. of combinations, covering a chosen range of proportions for each

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Fig. 4. Modal testing setup considering free vibration analysis.

component, is configured according to the established statistical were submitted to the curing process inside the humid chamber until
procedure. reaching the test ages (7 and 28 days).
Wolinski (2019) states that the DoE methodology allows a significant The test, shown by the Fig. 3, was performed on the SCC specimens
reduction in the number of calculations results necessary to achieve the with and without the addition of TRW. Four cylindrical specimens of 10
assumed accuracy in determining the response surface. The design of cm in diameter and 20 cm in height were tested for each concrete mix
experiments, according to Park (2019), is a statistical approach widely developed. To perform the tests, a WAW-1000 model brand TIME
used in engineering applications, since the approach tries to present Testing Machines was used, with a load capacity of 1000 tons, installed
predictive knowledge about complex and multivariable problems with at the Civil Construction Materials Laboratory of the Federal University
few numbers of attempts. of Itajubá.
According to Aranda et al. [20], Experiment Planning is a technique
used to plan experiments, that is, to define which data, in what quantity 2.3.2. Modal Testing
and under what conditions should be collected during a given experi­ For the performance of this non-destructive test, three cylindrical
ment, basically seeking to satisfy two major objectives: the possible specimens 10 cm × 20 cm, of each line, were used at 7 and 28 days.
statistical precision in the answer and the lowest cost. Currently, this Based on ASTM E1876 [24] the specimens were submitted to the Im­
technique has been used on a large scale. pulse Excitation Technique. Initially, the lengths, diameters, and masses
Aranda et al. [20] also states that through this technique, researchers of the specimens were recorded and, subsequently, they were supported
can determine the variables that have the greatest influence on the on adjustable support.
performance of a given process, resulting in (i) reduction of process The vibration test was divided into two stages, the first being the free
variation and better agreement between the obtained nominal values vibration test, which thus obtains the natural frequencies and the
and the desired values; (ii) reduced process time; (iii) reduction in damping factors of the specimens. To obtain the results, it was necessary
operating costs and (iv) improvement in process yield. to carry out a quality experimental arrangement. The experimental
In order to adequately contemplate the experimental aspect, it was arrangement was divided into two parts: a first one for the analysis of
decided to use the DoE strategy. Initially, preliminary tests were carried free vibration, without the presence of external forces. This essay was
out to define the main parameters and also the limits (lower and upper) fundamental for the acquisition and characterization of the modal
of these. Based on these tests, the factors and levels that will be used in behavior of the evaluated concrete structures. The entire experimental
the DoE were defined, described in Table 2. It is important to note that apparatus shown in Fig. 4.
the control characteristics of the experiment are consistent with the The boundary condition used to perform this test was free-free,
literature. which constitutes that both sides of the specimen are free to vibration
After this definition, a general full factorial design (GFFD) can be (no constraint). Through an impact hammer connected to a signal
formulated, presenting factors with different levels. Thus, there are two acquisition plate, the impulse was applied, dynamically exciting the
variables at two levels (Curing Time and Rubber Granulometry), one beam. With that, the beam starts to move, and the micro accelerometer
categorical and the other continuous, respectively. In addition, a vari­ (weight less than 5 g, thus, no influence on the mas) captures the signal
able was defined at three levels (Rubber Content), also continuous. From of this movement.
this definition, the GFFD was generated with three replicates, where the The equipment configurations were with the following parameters
experimental matrix is described in Table 3. It is important to note that force equal to 21.08 mV/N (input) and speed = 8.00 mV/(mm/s)
the experiments were carried out at random, avoiding bias in (output). Trigger Source was Analog Input, Run Mode was Auto Arm
measurement. every frame, Pre/Post Points (− /+) were − 3(− 1023, +65,535), Pre/
Post Trigger Time was − 2.34 ms and the levels in % and V were both 0.
For the analysis, the number of Lines and Points was, respectively,
2.3. Experimental setup 12,800 and 32768, while the Frequency was 500 Hz and ΔT was 781.3
µs. The Adopted Acquisition Time was 26 s and the Resolution was
2.3.1. Compression Testing 0.015 Hz/point.
The compression test was performed following ABNT NBR 5739:
2007 which specifies that cylindrical concrete specimens must be mol­
ded according to ABNT NBR 5739 [22]. After molding, the specimens

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Fig. 5. Mechanical responses considering different manufacturing configurations for self-compacting concretes (legend: 7 and 28 days of curing time).

3. Results and discussion frequency (flat surfaces). In other hands, it could be seen a substantial
change in the damping factor due to the curing time (28 days).
3.1. Analysis of variance (ANOVA) On the other hand, considering the static responses (Fig. 5c and d), it
is clear that the responses have a linear trend with the decision variables.
From the DoE analysis, the ANOVA strategy was applied to verify In addition, the curing time factor was a contributing factor to the in­
whether the experimental factors are statistically compatible in the crease in compressive strength and in the increase of concrete stiffness.
arrangement, in addition to analyzing an interaction between the factors Appendix A shows the results of the modal test in terms of time and
with respect to the response of interest. frequency responses.
There were three test variables analyzed: a categorical variable Fig. 6 show the main effects graphs corresponding to each test. It can
which is the cure time (7 and 28 days); and two continuous variables, be seen from Fig. 6a that the average natural frequency of concretes with
rubber content and granulometry. 10% rubber content (average is equal to 3.31 Hz) is the lowest and is
Four tests were used to analyze the influence of the variables: natural below the total average of the data (3.35 Hz). Concretes with 30% and
frequency, damping factor, compression strength and static elastic 50% rubber content show results above the total average, and concretes
modulus. The list of these variables, of the tests and respective values, is with 30% rubber content show the highest average (3.38 Hz).
shown in Table 3. It is also observed that the mean of the group with the lowest TRW
Complementary to Table 3, Fig. 5 shows a graphic result of the four granulometry (less than 0.6 mm) has a natural frequency value above
structural responses (static and modal) evaluated in this study. It can be the total average and above the average of the group with the highest
seen that the modal responses (Fig. 5a and b) have little variability TRW granulometry.
depending on the experimental search space, especially for the natural Regarding the curing time, the average natural frequency was higher

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Fig. 6. Main effects of the manufacturing variables on the static and modal responses.

in the 7-day healing group. Fig. 6b, shows that for the damping factor, significance (indicated by α), which in this study used 95% confidence,
there was a greater influence of the variables, however, still very small. that is, α = 0.05.
The lower the rubber content, there is also a greater influence on the Fig. 6a shows the significant relevance of the process factors in the
damping factor. The particle sizes of the rubber also had no statistical natural frequency response. It is observed that only factor C (cure time),
significant influence, however, the lower this variable, the lower the was statistically significant for this modal response, a fact that was not
damping factor. As in the natural frequency, the curing time is also the observed for the other factors, not even in the combination between
variable with the greatest influence on the damping factor, and the them. Comparing these results with those obtained previously (Fig. 7a),
greater the number of days, the greater the damping factor. it is concluded that they are compatible, that is, the natural frequency
According to Fig. 6c, the rubber content was the variable that most for factors A (Rubber content) and B (Rubber granulometry) also it
influenced the axial compression strength of concretes. The mean of the varied very little.
group with 10% of TRW showed greater resistance to compression while About the damping factor (Fig. 7b), all factors and the combination
the group with 50% had the lowest value. Regarding granulometry and between them were statistically significant, that is, they crossed the
curing time, the average of the groups was close to the total average (25 reference line (1.711). It is observed that the curing time is the most
MPa), this means that these factors do not have a significant influence on significant factor and the combination between the content (factor A)
the resistance to axial compression. and the granulometry of the rubber (factor B), is less significant. These
Analyzing Fig. 6d, it is concluded that the group with 10% of TRW results also confirm those already shown in Fig. 7b.
has a higher average in the static elastic module, while the group with It can be seen from Fig. 7c that, except for the combination between
30% and 50%, and presents averages equal and less than the total the granulometry of the rubber and the curing time, all factors, and the
average, respectively. These results are compatible with the results of combinations between them are significant for the results of compres­
the damping factor, that is, while the static modulus reduces with sion strength. The rubber content is, in this case, the most significant
increasing TRW content, the damping factor increases. factor, that is, the amount of rubber has a great influence on the axial
The greater the granulometry of the rubber and the curing time, an compression strength of the concrete.
average is observed in the groups above the total average. According to Fig. 7d, the most significant factors for the result of the
static elasticity modulus are, in decreasing order, the content (factor A)
3.2. General full factorial results and the size of the rubber (factor B), the combination between them
(factor AB), and the curing time (factor C). The main effects graph for
Pareto chart results show the absolute values of the standardized the static elasticity module, represented by Fig. 6d, also presents these
effects from the highest to the lowest effect. The graph also has a results.
reference line to indicate which effects are statistically significant, that (Intentionally left blank)
is, the bars that cross the reference line are statistically significant. The The p-value is defined as the probability of observing a test statistic
reference line for statistical significance depends on the level of value greater than or equal to that found. Traditionally, the cut-off value

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Fig. 7. Pareto of standardized effects (legend: A = rubber ratio, B = grain size and C = Curing time). A gray bar represents a term not in the model.

The R2 is a statistical measure of how close the data is to the adjusted


Table 4 regression line. In this part of the study, considering the statistical
ANOVA p-value results for the three modal responses. approach, a factorial arrangement was made for planning the experi­
Factor Compression Strength (σ) Elastic Modulus (Ec) ments. The factorial arrangement leads to obtaining a linear regression
equation as a function of the decision variables of the model.
Rubber 0.000 0.000
Granulometry 0.000 0.000 Observing the results of R2pred presented in Table 5, it is concluded
Curing Time 0.000 0.000 that, the linear model for the natural frequency and damping factor
Rubber × Granulometry 0.009 0.000 explains, respectively, only 41.36% and 65.91% of the data variability
Rubber × Curing Time 0.002 – around its average. In other words, it can be concluded that 43.36% of
Granulometry × Curing Time 0.880 –
the variation of the natural frequency is linearly related to the rubber
content, granulometry and curing time. The remaining 56.64% of the
variation is the result of other factors not considered in this study. This is
Table 5 probably explained by the fact that these responses are not as significant
Results of the R2 considering the response variables for self-compacting and/or do not exhibit linear behavior.
concrete. On the other hand, for static responses, 97.18% and 95.56% of the
Responses R2 R2 adj R2 pred variation in axial compression and static elastic modulus, respectively,
Compression Strength (σc) 99.06 98.73 98.13
are linearly related to the rubber content and granulometry, and to the
Elastic Modulus (Ec) 95.67 94.76 93.09 curing time. This fact is explained by the significant influence that these
factors have on the responses.
The results of the quality of the regression adjustment (R2adj) are
for rejecting the null hypothesis (no statistical difference between 96.59% and 64.64% for the compression strength and elastic modulus,
groups) is 0.05, which means that when there is no difference, such an respectively. Equations (1) and (2) show the final results for the meta­
extreme value for the test statistic is expected in less than 5% of the time model obtained from the test specimens where the variables x1, x2 and x3
[25]. represents the rubber ratio, grain size and curing time factors, respec­
In this work, the response variable is the results of the tests per­ tively. Equations (1) and (2) represent the best possible fit of the model
formed and the term is the variables involved (rubber content and according to the adopted factorial design. In this model, the
granulometry, curing time). manufacturing variables (x1, x2, x3), as well as their interactions (x1x2,
Table 4 shows that some p-values obtained were less than 0.05, x1x3, x2x3) constitute and translate the ability to generate responses from
which means that, in these cases, we can reject the null hypothesis, that a mathematical model.
is, there is a statistically significant difference between the tests per­
formed, the variables and the combinations between them. The proba­
bility is almost zero that the test results will not be influenced if there is
any change in the variables.

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Fig. 8. Images of self-compacting concrete (SCC) reference concrete without rubber addition.

3.3. Microstructural analysis (Intentionally left blank).


In concretes with 10%, 30% and 50% rubber with G2 granulometry,
In order to contribute to the results of the physical and mechanical Fig. 10a shows Fig. 10c in addition to the large number of voids, the
tests of the various self-compacting concrete traces developed, the mi­ transition zones and the total detachment of the rubber with the cement
crostructures were evaluated. Topological analyzes were performed matrix. This fact occurs due to the greater granulometry of the rubber
using Scanning Electron Microscopy (SEM) on all lines developed to and the non-adherence between the parts.
assess the transition zone between the aggregates and the cement paste, As a matter of the fact, it is possible to verify that, with increasing
in addition to observing the location of cracks and voids present in the levels of incorporation of rubber residues in the mixtures, there is an
matrix. increase in the number and size of the pores, micro-cracks, resulting in a
Fig. 8 shows the morphology of the reference SCC (0% rubber), that less compact structure and a marked transition zone. This evidence
is, concrete without the addition of rubber. The detachment in the justifies the decrease in resistance to compression and traction in
transition zone between the coarse aggregate and the cement matrix is bending.
quite evident, which contributed to the appearance of cracks. The im­
ages were obtained by secondary electron mode.
Fig. 9a and b show the microstructure of the self-compacting con­ 3.4. Optimal manufacturing conditions
crete with 10% rubber with G1 size. It is possible to observe a surface
with some voids and, due to the low adhesion between rubber and The model obtained in Section 3.2 has the great advantage of being a
concrete, the detachment (transition zone) between the parts is clearly guideline for designers, without necessarily requiring the manufacture
perceived. In Fig. 9c–f, with 30% and 50% rubber, respectively, and with of self-compacting concrete materials. The mathematical model ob­
G1 particle size, the cement paste matrix presents a significant increase tained was able to generate responses with remarkable precision (R2). In
in voids proportional to the rubber content, a fact that it contributes to addition to all the factorial analysis, the analysis of variance still exhibits
the reduction of the mechanical resistance of the concretes, facilitating a level of sensitivity of the responses as a function of the manufacturing
the appearance and propagation of cracks. parameters (decision variables).
According to Angelin et al. [26], the presence of voids is directly As already discussed in previous section, the full factorial design will
related to the air bubbles adhered to the rubber surface that are dragged result a linear response Equation Y = f(X) as shown in Eq. (1).
during the mixing of the concrete, making the matrix extremely fragile.
Y = β0 + β1 x1 + β2 x2 + β3 x3 + β12 x1 x2 + β13 x1 x3 + β23 x2 x3 + β123 x1 x2 x3 + ε
This is the most fragile area of the concrete and, since the rubber has low
(1)
resistance, the polymer can be considered as a void in the concrete,
reducing its mechanical resistance and facilitating the propagation of where β0 is the overall mean, while β1, β2 and β3 are the effect co­
cracks and ruptures. It is possible to verify the increase in the quantity of efficients for the main effects of factors A (rubber), B (grain) and C
pores and hydration crystals, the transition zone between the rubber (curing time), respectively. β12, β13 and β23 are the effect coefficients for
residue and the cementitious matrix is very evident. the AB, AC and BC interactions, while β123 represents the ABC interac­
tion. The coefficients β were obtained from ANOVA results in Section 3.2

σ C = 40.99 − − 0.7552 x1 + 2.870 x2 + 0.5001 x3 − − 0.0299 x1 x2 − − 0.00539x1 x3 − − 0.0561x2 x3 (2)

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Fig. 9. Self-compacting concrete microstructure with different rubber content and G1 grain size.

In short, it can be said that the model evaluated in this study has a values in the order of 99%. For both mechanical responses, there is a
linear relationship to the decision variables and the evaluated responses, slight increase in responses depending on the factor x3 (cure time).
σC (Eq. (2)) and Ec (Eq. (3)). Fig. A1. Fig. A2.
Establishing some desirable conditions of maximization or minimi­
zation for the statistically significant dependent variables, the DoE
methodology was used to obtain which values for the rubber content and
Ec = 33.80 − − x1 + 0.174 x2 + 0.0304 x3 + 0.0425x2 x3 (3)
granulometry and the curing time correspond to the desired conditions.
Figs. 11 and 12 show the result of linear regression for the factorial According to Table 6, in order to obtain an SCC with a maximum
adjustment of the compressive stress responses (Fig. 11) and elastic value of the static elasticity modulus, under the conditions presented in
modulus (Fig. 12). As previously mentioned in Fig. 5, these responses this work, a 10% TRW content with a grain size between 0.6 mm and 4.8
initially presented a very strong linear relationship. This relationship mm should be used and a curing time of 28 days, and therefore, the
was then verified by the quality of the adjustment (Table 5) reaching expected result for the static modulus of elasticity will be 38.84 GPa. To

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Fig. 10. Self-compacting concrete microstructure with different rubber content and G2 grain size.

Fig. 11. Full factorial regression results for compression Strength considering curing time of (a) 7 days and (b) 28 days.

obtain a minimum value of the modulus of elasticity (6.03 GPa), the (G2) and a curing time of 28 days when making the SCC. In this case, the
TRW content should be 50% and particle size less than 0.6 mm and cure compression strength assume the value of 50.57 MPa. For the minimum
time 7 days. value of axial compression stress, the mixture must be carried out with
About compression strength, the maximum value should be obtained 50% TRW with a particle size less than 0.6 mm and a curing time of 7
using 10% TRW with a particle size between 0.6 mm and 4.8 mm and days, obtaining a value equal to 5.58 MPa.

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Fig. 12. Full factorial regression results for elastic modulus considering curing time of (a) 7 days and (b) 28 days.

Fig. A1. Acceleration time response for the whole 36 experiments set considering different manufacturing parameters.

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Fig. A2. Frequency response function (FRF) for the whole 36 experiments set considering different manufacturing parameters.

the concrete (7 and 28 days). The analysis were performed through


Table 6
fundamental tests by technical standards, both in the fresh and hardened
Optimal manufacturing configurations.
state of the concrete.
Condition Objective Rubber Granulometry Curing Predicted The first test performed for concrete in the hardened state was that of
content Time response
(%) (days)
axial compression. As it does not contain TRW, the SCC-ref presented a
high resistance of 56.911 MPa at 7 days, which met the 40 MP estab­
Maximization Max (Ec) 10 G2 28 38.8470
lished by Gomes at 28 days. All other traits, with TRW, also showed
GPa
Minimize Min(Ec) 50 G1 7 6.0380 greater resistance to 28 days of concrete curing. It was also observed that
GPa the more rubber with greater granulometry incorporated into the con­
Maximization Max(σc) 10 G2 28 50.5710 crete, the lower the compressive strength found.
MPa The elasticity modulus decreased when compared to the SCC-ref both
Minimize Min(σc) 50 G1 7 5.5873
MPa
at 7 and 28 days, and this is explained by the fact that the rubber,
incorporated into the concrete, is more deformable than the replaced
sand.
4. Conclusion The statistical analysis of this study was based on the DoE method­
ology and played an important role in this work. It was possible to
In this study, the influence of the TRW inserted in the composition of observe which established factors (rubber content and granulometry
self-compacting concrete, in partial replacement of sand, was analyzed, and curing time) and combinations between them were statistically
varying the content (10%, 30% and 50%) and the rubber granulometry significant. Compression strength and static modulus of elasticity are
(G1 < 0.6 mm and 4.8 mm > G2 > 0.6 mm) as well as the curing time of variables greatly influenced by the established factors. The p-values

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obtained were, in most cases, less than 0.05 except for the interaction [7] França VH. Aderência aço-concreto – uma análise do comportamento do concreto
fabricado com resíduos de borracha. UNESP de Ilha Solteira. 2004.
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[8] Tutikian BF. Proposição de um método de dosagem experimental para concretos
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Declaration of Competing Interest [11] Khatun A, Singh K, Sharma R. Utilization of bagasse ash as a partial replacement of
cement in self-compacting concrete. Int J Civ Eng Technol 2018;9:1078–88.
[12] Chavda UA, Parikh KB. Self-Compacting Concrete : A Review. Int J Res Appl Sci
The authors declare that they have no known competing financial Eng Technol 2018;6:2953–5.
interests or personal relationships that could have appeared to influence [13] Rahman MM, Usman M, Al-Ghalib Ali A. Fundamental properties of rubber
modified self-compacting concrete (RMSCC). Constr Build Mater 2012;36:630–7.
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with recycled coarse and fine aggregates using non destructive testing techniques.
Acknowledgements Constr Build Mater 2018;181:73–84.
[15] Grünewald S. Performance-based design of self-compacting fibre reinforced
concrete. Universidade Técnica de Delft 2004.
The authors would like to acknowledge the financial support from [16] Tutikian BF, Helene P. Capítulo 12 - Dosagem dos Concretos de Cimento Portland.
the Brazilian agency CNPq (150117/2021-3) and FAPEMIG (Fundação In: Isaia GC, editor. Concreto: Ciência e Tecnologia. São Paulo: IBRACON; 2011.
[20] Aranda MH, Jung CF, Schwengber ten Caten C. Determinação dos parâmetros
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