Analysis of Metakaolin As Partial Substitution of Ordinary Portland Cement in Reactive Powder Concrete

Advances in Civil Engineering Materials
doi:10.1520/ACEM20190224 / Vol. 9 / No. 1 / 2020 / available online at www.astm.org
Joaquín Abellán-García,1 María Alejandra Santofimio-Vargas,2 and

Nancy Torres-Castellanos3
Analysis of Metakaolin as Partial

Substitution of Ordinary Portland Cement
in Reactive Powder Concrete
Reference
J. Abellán-García, M. A. Santofimio-Vargas, and Nancy Torres-Castellanos, “Analysis of
Metakaolin as Partial Substitution of Ordinary Portland Cement in Reactive Powder Concrete,”
Advances in Civil Engineering Materials 9, no. 1 (2020): 368–386. https://doi.org/10.1520/
ACEM20190224
ABSTRACT
Manuscript received December 4, Over the last 20 years, remarkable advances have taken place in the research on reactive pow-
2019; accepted for publication der concrete (RPC). However, because of the high contents of cement and silica fume (SF)
May 15, 2020; published online
July 10, 2020. Issue published July
usually used in those types of concrete, the cost and environmental impact of RPC is consid-
10, 2020. erably higher than conventional concrete. Hence, the use of supplementary cementitious ma-
1
terials as partial substitution of cement and SF has been an object of great interest by the
Department of Civil Engineering,
Polytechnic University of Madrid, scientific community. However, the replacement of cement and SF can result in the deterio-
Madrid, Spain, and Escuela ration of certain properties of RPC, such as the early strength; however, RPC usually needs
Colombiana de Ingeniería Julio great amounts of cement and SF. This work presents a study to analyze the effect of meta-
Garavito, Bogotá, Colombia
(Corresponding author), e-mail:
kaolin (MK) as a partial substitute of cement in a previously optimized mixture of RPC using
j.abellang@alumnos.upm.es, statistical tools such central composite design, main effect plot analysis, and response surface
https://orcid.org/0000-0002- methodology. In addition to MK, supplementary cementitious materials such as SF, limestone
0353-322X
powder and recycled glass powder, and fine Type III cement were used. Based on the labo-
2
Escuela Colombiana de Ingeniería ratory experiments results and statistical analysis, it was concluded than MK develops a high
Julio Garavito, AK.45 No. 205-59, activity in the hydration process of RPC, helping it reach high strength at early ages, such as
Bogotá, Colombia, https://
orcid.org/0000-0002-9864-1345
1 and 7 days, which may be of interest for applications such as the connection of prefabricated
elements or accelerated bridge construction. However, the effect of the partial substitution of
3
Department of Civil Engineering,
Type III cement by MK on 28-day compressive strength was nonsignificant. Moreover, the MK
Escuela Colombiana de Ingeniería
Julio Garavito, AK.45 No. 205-59, inclusion in RPC provides a significant decrease in workability as the amount of MK increases.
Bogotá, Colombia, https://
orcid.org/0000-0003-3293-5444
Keywords
reactive powder concrete, supplementary cementitious materials, packing density, metakaolin,
central composite design, response surface methodology
Copyright © 2020 by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959 368
ABELLÁN-GARCÍA ET AL. ON MK AS PARTIAL SUBSTITUTION OF OPC IN RPC 369
Introduction
Over the past decade, development of high-performance cementitious composites has made enormous progress in
the construction industry worldwide and has led to a new material with ultrahigh performance and superb, im-
proved material properties. Namely, a new type of ultrahigh-performance cement-based composite material with
ultrahigh compressive strength, known as reactive powder concrete (RPC), was developed by the French company
Bouygues.1,2 Such superb mechanical properties can be ascribed to this composite’s low porosity and high packing
density due to its low water-to-binder ratio, special mixture design, and mixing procedure, which leads to an
extremely optimized grain-binder matrix.3–10 Long-term durability is another outcome of the low porosity and
high packing density.3,10 In recent years, applications of RPC have increased in Europe, North America, Japan,
Korea, China, and Australia, whereas in some other countries, such as Colombia, there has only been limited
application. Among others, use of RPC includes construction of pedestrian bridges, liner tunnel segments, special
prestressed and precast concrete elements, concrete structure rehabilitation, precast deck panel bridge joints, urban
furniture, overlay on damaged pavements and industrial floors, and architectural applications.3,8,10–14
Nevertheless, in terms of cost efficiency and sustainability, this class of material must still be evaluated re-
garding its value and the higher average dosage of binder relative to the current concrete.9 A typical RPC mix
contains over 800 kg/m3 of portland cement, and high amounts of silica fume (SF), quartz powder, microsilica
sand (SS), high-range water reducers superplasticizers (HRWRs), and sometimes steel fiber.1,13,15 The coarse
aggregates are eliminated to improve the homogeneity of the matrix. The inclusion of steel fiber provides ductility,
tensile, and flexural capacity.11,16 Abellan et al.3 depicted the composition of an average dosage mixture of RPC
based on 150 dosages from published research, sharing characteristics such as compressive strength over
150 MPa, maximum size of aggregate between 0.5 and 0.6 mm, and 2 % of steel fiber volume fraction. This
dosage and the cost implication of its components are depicted in figure 1.
Therefore, over the past few years, the interest in reducing the CO2 footprint of the material has increased.
This is achieved primarily by lowering the amount of cement via use of supplementary cementitious materials
(SCMs) while maintaining or even improving some of the properties of the concrete.3,13,17–21 The inclusion of
SCM not only allows partial substitution of cement, but also of SF, leading therefore to a less expensive
material.22–26 Subsequently, the amount of cement and SF may be reduced without a substantial change in
the particle packing density of the mixture, which is the basis of the outstanding properties of RPC.1,22,24,25
However, a reduction in the amount of cement and SF in RPC could result in the deterioration of certain
properties, such as early strength.10 The high and ultrahigh early strength of concrete is often achieved by adding
high amounts of cement, SF, or nanosilica, the latter of which costs even more than SF.27
SCMs are usually amorphous in nature with high SiO2/Al2O3 content, which can react with the calcium
hydroxide formed during hydration of portland cement through pozzolanic reaction.28 Several researchers
FIG. 1 Average dosage of 150 dosages from published research. Components and their implications on cost.3

370 ABELLÁN-GARCÍA ET AL. ON MK AS PARTIAL SUBSTITUTION OF OPC IN RPC
previously focused on identifying the influence of SCM on the properties of high and ultrahigh-performance
cementitious materials. Among others, recycled glass powder (RGP), metakaolin (MK) and limestone powder
are two SCMs that can be used as a partial substitutes for ordinary portland cement, and SF can be used in high-
and ultrahigh-performance cementitious composites.13,29–31 Abellán et al.24 showed an optimized dosage of
ultrahigh-performance glass concrete using limestone powder and two sizes of RGP. According to their results,
a compressive strength over 150 MPa could be achieved with low cement and SF content. Li et al.18 demonstrated
an improved hydration process at an early age by adding limestone powder to ultrahigh-performance concrete.
Ahmad, Hakeem, and Maslehuddin30 showed the possibility of partial substitution of cement and SF without the
commitment of rheological and mechanical properties of RPC when using various locally available materials in
Saudi Arabia, such as limestone powder. Huang and Cao observed a 17 % increase in compressive strength when
adding nano-limestone powder to RPC.32 Vaitkevičius, Šerelis, and Hilbig31 and Šerelis, Vaitkevičius, and
Kerševičius33 analyzed the effect of glass powder on the microstructure of ultrahigh-performance concrete
(UHPC). Their results showed that glass powder increased the dissolution rate of portland cement under heat
treatment; thus, the hydration process was accelerated. Soliman and Tagnit-Hamou34 evaluated fine glass powder
as a partial substitution of SF in RPC. They concluded that compressive strength values of 235 and 220 MPa under
2 days of steam curing can be reached, respectively, when replacing 30 and 50 % of SF with fine glass powder with
an average particle size (d50) of 3.8 μm. In another study, Soliman and Tagnit-Hamou11 and Tagnit-Hamou,
Soliman, and Omran13 studied the possibility of using RGP to replace quartz sand, cement, and quartz powder
particles.
On the other hand, MK is a commonly used pozzolanic material that shows a high level of pozzolanic
activity—not higher than SF but greater than fly ashes.35 MK is made by calcining natural clay.17 In
Colombia, where this research took place, the price of MK is approximately 50 % higher than that of cement
but a quarter of the price of SF. On the other hand, the embodied CO2 generated to produce 1 ton of MK is around
330 kg/ton, whereas the amounts for cement and SF are around 700 and 4 kg/ton, respectively.19,36
There are several investigations that address the use of MK as a supplementary cementitious material in
UHPC. Tafraoui et al.37 analyzed the effect of partially substituting SF with MK in UHPC. They concluded that
the equal mass substitution of SF with MK made it possible to produce UHPC with equivalent mechanical proper-
ties; however, the mixing time increased slightly. Li and Rangaraju38 proved that the increase in the MK content
resulted in a significant decrease in the workability and improvement of the 1-day compressive strength of UHPC
that was due to its reactive SiO2/Al2O3 content. However, those investigations analyzed the effect of the inclusion
of MK in high cement content concrete dosages (over 800 kg/m3). On the other hand, to the best knowledge of the
authors, there is no previous work that analyzed the effect of MK in a low cement content (620 kg/m3) RPC.
It is important to highlight the fact that some applications, such as the connection of prefabricated elements
or the accelerated bridge construction, give rise to the necessity for the use of high early strength.27 Thus, it would
be of interest to analyze the effect of MK as a partial substitution of cement on the properties of a previously
optimized low cement and low SF content RPC.
The research program reported on herein was aimed at determining the effects of MK on the partial sub-
stitution of Type III cement in a previously optimized RPC.23 The study of these effects was based on statistical
techniques such as design of experiments (DoE), response surface methodology (RSM), and main effect plots of
the performance of the RPC mixtures. All statistical methodologies were performed utilizing R version 3.5.239 by
using the qualitytools function.40
Materials and Methods

MATERIALS
The RPC mixtures were prepared with raw materials locally available in Colombia. Cement CEM III 42.5 HE was
used. The cement had a specific gravity of 3.15 and an average particle size (d50) of 8 μm. The SF used in the mixture
proportioning complied with ASTM C1240, Standard Specification for Silica Fume Used in Cementitious Mixtures,

and had a specific gravity of 2.20 and d50 of 0.15 μm. The RPC was also designed with a SS of a specific gravity of 2.65,
maximum particle size (dmax) of 600 μm, and d50 of 165 μm. RGP with a specific gravity of 2.55 and d50 of 28 μm was
used, and limestone powder with a specific gravity of 2.73 and d50 of 2 μm, and MK with a specific gravity of 2.66 and
d50 of 10 μm were used as SCMs. RGP was obtained by grinding recycled glass with a jet mill. Table 1 shows the
chemical composition of the materials used in this study. Figure 2 provides the particle size distribution of the
cement, SF, LP, MK, RGP, and SS. Figure 3 shows a photograph of the raw materials used in the research.
A polycarboxylate superplasticizer with a specific gravity of 1.07 and solid content of 40 % was used.
The SCMs (MK, limestone powder, and RGP) used in this research were analyzed by scanning electron
microscopy (SEM) as depicted in figure 4. Results show the lack of porosity of the RGP, contrary to what
is generally observed with limestone powder and MK particles.
TABLE 1
Chemical properties of materialsa
Chemical Analysis OPC SF MK LP RGP SS
SiO2% 19.42 92.9 52.17 0.90 72.9 95.0

Al2O3% 4.00 0.59 39.11 0.10 1.67 0.11
CaO% 64.42 3.89 0.78 55.1 9.73 0.38
MgO% 1.52 0.26 0.07 0.70 2.08 0.20
SO3% 1.93 0.07 0.22 0.10 0.01 0.52
Na2O% 0.19 0.31 0.61 0.03 12.4 0.25
K2O% 0.39 0.54 0.06 0.00 0.76 3.49
TiO2% 0.38 0.01 1.48 0.00 0.04 0.25
Mn3O4% 0.05 0.01 0.00 0.01 0.01 0.01
Fe2O3% 3.61 0.24 2.69 0.05 0.81 0.09
Loss of ignition % 2.58 0.60 4.22 42.1 1.00 0.31
Specific gravity (gr/cm3) 3.16 2.20 2.66 2.73 2.55 2.65
Note: OPC = ordinary portland cement; a

Based upon a single analysis.
FIG. 2 Particle size distribution of the used materials.

FIG. 3 Materials used in this research: (A) CEM III 42.5 HE, (B) condensed silica fume, (C) metakaolin, (D) limestone
powder, (E) recycled glass powder, and (F) silica sand.
The X-ray powder diffraction (XRD) of the cement and the cementitious materials are shown in figure 5.
Figure 5A depicts the mineralogical analysis obtained for the CEM III. The XRD pattern for SF is presented in
figure 5B. The intense broad peak observed for SF indicates that this material is totally amorphous. The analysis
exhibited in figure 5C showed a majority composition of calcite for the limestone powder. The XRD analysis
carried out on RGP (fig. 5D) revealed its amorphous nature. Also, in the case of MK (fig. 5E), a material of
amorphous characteristics is shown.
The pozzolanic activity of MK was determined from compressive strength using ASTM C311, Standard
Test Methods for Sampling and Testing Fly Ash or Natural Pozzolans for Use in Portland-Cement Concrete,
and ASTM C618, Standard Specification for Coal Fly Ash and Raw or Calcined Natural Pozzolan for Use in
Concrete. As indicated by the standard, mortars were made with standard sand and replacement of cement
by the cementitious addition at 20 %. Specimens were prepared and cured by immersing them in lime-saturated
water at room temperature for time periods of 1, 3, 7, and 28 days. Table 2 shows the results of the pozzolanic
activity index at different ages.
For the evaluation of the pozzolanic activity index, the ASTM C61841 standard requires a minimum poz-
zolanic index of less than 75 % at 28 days of curing in order to consider a material as a pozzolan. According to
Table 2, the MK complies with that parameter.

FIG. 4 SEM of supplementary cementitious materials used in research: (A) metakaolin, (B) limestone powder, and (C)
recycled glass powder.
MIXTURE DESIGN METHODOLOGY

DoE
A DoE consists of a specific set of experiments that must be performed by the researcher. The main objective of
this mathematically based procedure is to optimize a process by performing each trial and to extract conclusions
about the significant behavior of the studied response from the results of the experiments. Taking into account the
costs of a single trial, reducing the number of performed experiments is always a goal.10 With DoE, this number is
kept as low as possible while the most informative combination of factors is chosen. Therefore, DoE is an effective
and economical solution.10,42 Hence, the advantages of using such a mathematical instrument includes: (i) the
setting-up of a statistical model containing the relevant factors and their corresponding responses, (ii) a reduction
in the number of runs to be carried out, and (iii) the analysis of the interrelationship between factors.5,10,43,44
A central composite design (CCD) is an efficient experimental design, useful in RSM for constructing a
quadratic order regression model for the response variable without needing to perform a full factorial experi-
ment.45 The second-order model regression, also known as canonical polynomial of Scheffé, is widely used in this
methodology for the following reasons: (i) the second-order polynomial is very flexible as an approach to the real
response surface. It can take on a wide variety of functional forms, so it will usually work as an approximation to
the real response surface; (ii) it is not complicated to estimate the parameters—the a’s in equation (2)—in the
quadratic polynomial regression model; and (iii) there is a considerable amount of experience indicating that
those models perform well in solving real response surface problems. As mentioned previously, CCDs are

FIG. 5 XRD of: (A) CEM III, (B) SF, (C) limestone powder, (D) RGP, and (E) MK.
fractional factorial design. They are composed by center points that are augmented with a group of star points
(also called axial points), which increase the variable space and allow estimation of curvature. If the distance from
the center of the design space to a factorial point is ±1 unit for each factor (according to the codification), the

TABLE 2
Pozzolanic activity index for the MK at different curing ages41
Days Index of Pozzolanic Activity (%)
1 72.5
3 78.8
7 81.1
28 92.9
FIG. 6
CCD for three design
variables at two levels.
distance from the center of the design space to an axial point is |α| > 1. The precise value of α depends on certain
properties desired for the design and on the number of factors involved. A total of 18 set points, four center points
(two axial plus two cube), two blocks (cube and axial), and α = ±1.78885 was used in this research. A graphic of a
three-dimensional CCD for three independent variables is shown in figure 6.
The statistical analysis was performed on the coded data sets in order to simplify the evaluation of the results.
The coding was carried out according to equation (1):
X j = ðZ j − Z 0j Þ=ðZ maxj − Z minj Þ (1)
where Xj is the coded value of the independent variable (i.e., factor) j, Zj is the real value of the independent
variable j, Z0j is the real value of the factor j at the center point, and Zmaxj and Zminj are the maximum and
minimum value of the factor j in the domain space, respectively.
To estimate each response, a second-order polynomial equation calculated according to equation (2) was
used:
X X X
Y = a0 + ai x i + aii x2i + aij xi xj (2)
where Y was the estimate of the response (i.e., dependent variable), a0 is the overall mean response, ai are linear
coefficients, aii are quadratic coefficients, aij are coefficients of the interaction, and xi and xj represent the factors
considered in the design. In each response model, some of the terms may not be significant; therefore, a backward
elimination technique was used to remove insignificant terms from the model. Once the model was generated, an
analysis of variance (ANOVA) was performed to investigate its significance using R computing language.39 Once
the models were validated, the RSM plots could be developed.
Factors Considered in the DoE

Owing to the fact that the addition of MK in the mixtures reduces the workability of the mixtures35,38 the water-
to-binder ratio and the amount of superplasticizer have to be included in the DoE as factors in addition to partial

TABLE 3
Range of variation of Factor A
Factor A
Coded −1.7889 −1 0 1 1.7889

CEM III (kg/m3) 448.47 528.43 554.23 580.00 620.00
Metakaolin (kg/m3) 131.53 91.57 65.77 40.00 0.00
TABLE 4
Range of variation of Factor B
Factor B
Coded −1.7889 −1 0 1 1.7889

w/b (%) 0.156 0.160 0.165 0.170 0.174
Note: w/b = water-to-binder ratio.
TABLE 5
Range of variation of Factor C
Factor C
Coded −1.7889 −1 0 1 1.7889

HRWR (% Vol) 1.64 1.80 2.00 2.20 2.36
substitution of cement with MK. In this research, CCD with three factors or independent variables were used.
Factor A represents the partial substitution of cement by MK, whereas Factor B represents the water-to-binder
ratio and Factor C represents the amount of superplasticizer used in each point of the DoE.
Only 18 trials are needed for three independent variables (Factors A–C) varied over five levels, as an alter-
native to 53 (n = 125) possible combinations. As shown in Table 3, the maximum amount of CEM III considered
is 620 kg/m3, which corresponds with the reference dosage without MK. As Factor A decreases, the MK content
rises to a maximum value of 131.5 kg/m3. It is important to highlight that the sum of the weights of cement and
MK is equal to 620 kg/m3 in all cases.
Factor B represents the water-to-binder ratio, and Factor C represents the HRWR content in volume frac-
tion. Their range of variation for both coded and real values are shown in Tables 4 and 5, respectively.
Reference Mixture Design

The reference used in this study was a previously optimized mixture with low cement content (620 kg/m3), a
maximum SF content of 100 kg/m3, and one that uses RGP and limestone powder as SCMs.23 To ensure a densely
compacted cementitious matrix, the reference mixture was calculated using the modified Andreasen & Andersen
particle packing model (A&Amod)46 with a q value of 0.264, according to equation (3). Once the reference dosage
was settled, the rest of the runs are ruled by the DoE. Table 6 depicts the mixture proportions of the CCD used,
whereas the reference dosage without MK and with the maximum amount of CEM III 42.5 HE can be observed as
Run-12.
Dq − Dq min
PðDÞ = (3)
Dq max − Dq min
where D is the particle size, P (D) is the weight fraction of total solids that are smaller than D, Dmax and Dmin are
the maximum and minimum particle sizes, respectively, and q is the Fuller exponent. The value of q was de-
termined in previous research.10

TABLE 6
Proportion of concrete mixtures expressed as a function of the weight of the cement
N CEM III SF RGP LP MK HRWR SS w/b VPDa
1 1 0.189 0.587 0.487 0.173 0.037 1.545 0.160 0.804

2 1 0.172 0.534 0.443 0.069 0.033 1.421 0.160 0.805
3 1 0.189 0.587 0.487 0.173 0.037 1.48 0.170 0.802
4 1 0.172 0.534 0.443 0.069 0.033 1.362 0.170 0.803
5 1 0.189 0.587 0.487 0.173 0.045 1.540 0.160 0.804
6 1 0.172 0.534 0.443 0.069 0.041 1.417 0.160 0.804
7 1 0.189 0.587 0,487 0.173 0.045 1.475 0.170 0.802
8 1 0.172 0.534 0.443 0.069 0.041 1.358 0.170 0.802
9 1 0.180 0.559 0.464 0.119 0.039 1.447 0.165 0.803
10 1 0.180 0.559 0.464 0.119 0.039 1.447 0.165 0.803
11 1 0.205 0.635 0.526 0.269 0.044 1.621 0.165 0.799
12 1 0.161 0.500 0.415 0.000 0.035 1.310 0.165 0.805
13 1 0.18 0.559 0.464 0.119 0.039 1.502 0.156 0.803
14 1 0.180 0.559 0.464 0.119 0.039 1.392 0.174 0.803
15 1 0.180 0.559 0.464 0.119 0.032 1.451 0.165 0.803
16 1 0.180 0.559 0.464 0.119 0.046 1.443 0.165 0.803
17 1 0.180 0.559 0.464 0.119 0.039 1.447 0.165 0.803
18 1 0.180 0.559 0.464 0.119 0.039 1.447 0.165 0.803
Note: w/b = water-to-binder ratio; a

Virtual packing density according to Larrard and Sedran.15
TESTING PROCEDURES
Mixing, Sample Preparation, and Curing
Type III cement, SF, limestone powder, RGP, MK (where appropriate), water, HRWR, and SS were mixed to-
gether in a mortar mixer according to the following procedure: First, all cementitious materials were dry-mixed
for about 10 minutes. Water that was previously premixed with superplasticizer was then added gradually and
mixed for another 5 minutes. Then, sand was also gradually incorporated and mixed for another 3 minutes.
Finally, the whole mixture was mixed for another 2 minutes. Cubes (50 × 50 × 50 mm) were formed for the
research to determine different-age compressive strength. To enhance the packing density of concrete, a vibrating
table was used after the cubes were cast. The samples were demolded approximately 24 hours after casting and
then cured in a moist room at 20°C until the day of the test.
Slump Flow Test

Once the mixing procedure was completed, the fresh properties of the RPC mixtures were measured to determine
the static slump flow diameter according to ASTM C1437, Standard Test Method for Flow of Hydraulic Cement
Mortar,47 by taking the spread diameter of the minislump cone in the flow-table test without being dropped,
filling the truncated conic mold with the concrete, and lifting it away. The Øm parameter was measured on spread
test and calculated according to equation (4), in which Øi is the mean value for each i of the four perpendicular
diameters, in mm:
X
∅m = 0.25 ∅i (4)
Compressive Strength
Concrete compression machine with a 1,000 kN capacity was used, following ASTM C109/C109M-20a, Standard
Test Method for Compressive Strength of Hydraulic Cement Mortars (Using 2-in. or [50-mm] Cube Specimens).48
For each age, i.e., 24 hours, 7 days, and 28 days, three samples were tested.

Results and Discussion

EXPERIMENTAL RESULTS
The experimental results are depicted in Table 7.
MAIN EFFECT PLOTS

To focus on the effect of the factor, a main effect plot of each factor for each response, isolating the influence of
each of the other factors. The main effect plots can be described as the mean response of each level factors con-
nected by the line. If the line presents a horizontal pattern, there is no main effect present. However, when the line
is a small deflection from horizontal it may significantly affect the response. The higher the slope in the line the
greater the magnitude of the main effect.49
Spread Flow
The main effect plot of each factor on spread flow is presented in figure 7.
As indicated in figure 7, it is clear that the inclusion of MK in the dosage causes a decrease in the slump
flow of concrete while the replacement ratio of MK increases (i.e., Factor A’s value decreases). The latter, which
can be linked to the accelerating effect of MK in the hydration process according to the values of pozzolanic activity
index at early ages, is shown in Table 2. Other reasons for the negative effect of MK on workability would be its high
amorphous SiO2/Al2O3 content (see Table 1 and fig. 5E) and its porous nonspherical particles (see fig. 4A).
Another explanation for this could be that, according to Restrepo Gutierrez, Restrepo Baena, and Tobón,50
the chemical reaction of reactive SiO2/Al2O3 MK content increases the temperature during the hydration process
of cement, making workability worse. However, isothermal calorimetry would be needed to confirm the latter in
our case of study.
It is noted that several studies have demonstrated that the inclusion of MK in a concrete requires more water
or superplasticizer to reach a determined workability.19,35,38,51–53
As expected, the water-to-binder ratio (Factor B) and superplasticizer content (Factor C) have a positive
effect in the spread flow value.
TABLE 7
Set point combinations and the corresponding experimental responses
f1d (MPa) f7d (MPa) f28d (MPa) Øm
N A B C Mean S.D. Mean S.D. Mean S.D. Mean S.D.
1 −1 −1 −1 58.01 1.51 97.88 6.84 139.54 5.55 100.00 0.00

2 1 −1 −1 43.77 2.93 93.99 2.70 139.40 10.43 126.25 12.50
3 −1 1 −1 57.87 1.87 97.33 5.77 129.11 8.52 102.50 5.00
4 1 1 −1 29.32 1.05 93.79 4.99 130.41 9.81 178.75 2.50
5 −1 −1 1 57.82 4.67 97.57 5.10 140.83 7.43 133.75 12.50
6 1 −1 1 22.78 1.03 92.63 3.76 140.74 11.01 218.75 2.50
7 −1 1 1 57.67 5.14 97.52 7.84 139.32 9.22 172.50 3.75
8 1 1 1 28.52 2.47 91.45 5.63 139.34 8.03 243.75 10.00
9 0 0 0 51.81 6.34 96.06 8.24 149.56 12.52 132.50 9.50
10 0 0 0 52.22 4.85 100.06 7.28 150.02 9.33 137.50 8.50
11 −1.7889 0 0 57.45 6.09 123.98 5.62 157.08 5.12 100.00 0.00
12 1.7889 0 0 54.29 5.36 110.52 3.35 158.84 8.89 260.00 12.50
13 0 −1.7889 0 55.89 3.78 115.63 5.99 155.74 7.72 115.00 0.50
14 0 1.7889 0 49.73 5.19 90.65 4.81 139.67 9.44 260.00 12.00
15 0 0 −1.7889 56.78 2.38 102.38 4.67 145.38 10.58 125.00 9.50
16 0 0 1.7889 51.65 4.41 90.54 5.52 154.42 7.54 170.00 8.50
17 0 0 0 52.01 5.17 98.06 9.03 149.79 8.78 135.00 6.50
18 0 0 0 53.11 3.53 102.06 4.21 151.90 12.21 136.25 8.50

FIG. 7 Main effect plot of each factor on slump flow.
One-Day Compressive Strength

The main effect plot of each factor on 1-day compressive strength is depicted in figure 8.
As depicted in figure 8, because of its high reactivity, MK provides significant enhancement in 1-day
compressive strength. As Factor A decreases (i.e., the amount of MK increases), the 1-day compressive strength
grows. The latter could be explained by the acceleration of portland cement hydration and the pozzolanic
reaction by MK with calcium hydroxide51,52 according to the values pozzolanic activity index at 1 day as shown
in Table 2.
The negative effect of the increase of water in the compressive strength is a well-known effect. Even the
negative effect of superplasticizers on early strength development has been proven by several researchers.54,55
The polycarboxylate forms a complex with Ca+2 ions liberated on the surface of the tobermorite gel (CSH)
or portlandite Ca(OH)2 crystal. At the beginning of the hydration process and in the presence of polycarboxylate,
only a low concentration of Ca+2 ions get into the solution, inhibiting the nucleation and growth of Ca-rich
species, whereby the hydration of silicates slows down (especially the alite phase).54 Therefore, the polycarbox-
ylate-based ether superplasticizer has a negative effect on the development of early age strength.20,54,56
Seven-Day Compressive Strength

Figure 9 presents the main effect plot of each factor at 7-day compressive strength.
As it can be observed, Factor A had a positive effect on the 7-day compressive strength of UHPC.
Nevertheless, Factors B and C had an adverse effect on this response.
FIG. 8 Main effect plot of each factor 1-day compressive strength.

FIG. 9 Main effect plot of each factor’s 7-day compressive strength.
Twenty-Eight-Day Compressive Strength

The main effect plot of each factor at 28-day compressive strength is presented in figure 10.
Contrary to what happens at the early ages of 1 and 7 days, the slope of the main effect plot of Factor A at 28-
day compressive strength has a positive sign; however, the line presents an almost horizontal pattern, which
indicates that Factor A does not appear to be significant.
It is important to highlight the fact that partial substitution of CEM III by MK does not enhance the virtual
packing density (see Table 5) because the cement mean particle size is slightly smaller than the MK particle. As
can be seen in Table 5, the virtual packing density of the mixtures with maximum (Run-11) and minimum (Run-
12) weight-by-weight substitution ratio are 0.799 and 0.805, respectively, which represents a very narrow range of
variation. Dense particle packing is the key principle for achieving high compressive strength in RPC.1,20,21,23,57
As can be seen in figure 10, Factor C has a positive effect on the compressive strength at 28 days, which can
be ascribed to the better dispersion of particles during the mixing procedure that enhances the real packing
density in concrete.58 The latter contrasts with the negative effect of this factor on the early strength of concrete,
which was previously explained.
RSM ANALYSIS
The adjusted polynomial regressions for each response according to equation (3) were used to elaborate the RSM
plots. To investigate the significance of those models, four ANOVA were performed. The results are given in
Table 8.
FIG. 10 Main effect plot of each factor’s 28-day compressive strength.

TABLE 8
Results for the developed regression models
Responses R2 RMSE F-Stat Lack-of-Fit Model p Value Shapiro p Value
Øm 0.933 3.62 53.96 4.12 <.0001 .189

f1d 0.923 2.06 16.78 2.72 <.0001 .268
f7d 0.965 2.54 24.61 3.09 <.0001 .172
f28d 0.926 1.34 21.52 1.72 <.0001 .175
Note: RMSE = root-mean-square error.
The significance of the model was determined by using both F-test and p value. The p values lower than
0.0001 were obtained for all the models, implying their significance. In addition, the analysis of results for
full regression models included the determination coefficient (R2), the root-mean-square error, the F Statistic
value, the lack-of-fit p value, the model p value, and the Shapiro–Wilk p value. The models presented a
high determination coefficient (R2) showing 93, 92, 96, and 93 % of the variability in the responses of
Øm, f1d, f7d, and f28d, respectively. This indicates the goodness-of-fit of the models used in the RSM. The
adequacy of the models was verified by performing a lack-of-fit test being that the desired result was an
insignificant lack-of-fit in all cases. In other words, the p values obtained by the ANOVA implied that
the lack-of-fit was insignificant compared with the pure error. In addition, the Shapiro–Wilk test showed
p > .05 in all cases.
Finally, the response surface plots, which represent the response as a function of the three factors by using the
fitted models, were created. These graphs offer an opportunity to analyze how certain factors and their relation-
ships affect the responses. The contour areas represent areas of equal response and can be visually filled with
different colors as response contours of Factors B and C while fixing Factor A at a given point. Therefore, for each
response, three plots were created, i.e., fixing Factor A at Points −1, 0, and 1.
Spread Flow
Figure 11 depicts the RSM plots for Øm response, for different fixed values of Factor A.
According to the European Federation of National Associations Representing Producers and Applicators of
Specialist Building Products for Concrete (EFNARC),59 a spread flow value from 240 to 260 mm is considered
adequate for a plain self-compacting concrete (SCC). It is noticeable that Factor A (i.e., MK content) is the most
significant factor regarding spread flow response. When Factor A is equal to or less than −1 (i.e., when MK
content is equal to or greater than 91.57 kg/m3), and according to figure 10 and Table 6, a SCC could not
be reached regardless of the values of Factors C and B.
As mentioned previously, the water-to-binder ratio (Factor B) and superplasticizer content (Factor C) have a
positive effect on the spread flow.
FIG. 11 RSM plots for Øm response, for different fixed values of Factor A.

One-Day Compressive Strength

Figure 12 presents the RSM plots for 1-day compressive strength response, for different fixed values of Factor A.
As shown in figure 12, the early compressive strength increases as the partial substitution of CEM III with
MK increases (i.e., Factor A decreases). According to Poon et al.,60 the higher initial reactivity of MK can be
attributed to its Al2O3 phases, which in our case represents 39.11 % of the MK as can be seen in Table 1.
Those Al2O3 phases would be involved in the formation of C2ASH8 (gehlenite) and a small amount of crystalline
C4AH13 phase.
Water-to-binder ratio (Factor B) and superplasticizer content (Factor C) have a negative effect on the 1-day
compressive strength, which is in agreement with the main effect plot analysis.
An interesting interaction between factors can be observed in figure 12. As the amount of cement increases
(Factor A increases) and Factor B decreases (i.e., water content decreases), the negative effect of polycarboxylate
(Factor C) on 1-day compressive strength increases.
Seven-Day Compressive Strength

Figure 13 shows the RSM plot of the effect of Factors B and C on the 7-day compressive strength for a fixed value
of Factor A. According to figure 13, Factor A has a positive effect on the 7-day compressive strength of RPC.
Nevertheless, Factors B and C have an adverse effect on 7-day compressive strength.
Twenty-Eight-Day Compressive Strength

Figure 14 depicts the contour plots for the 28-day compressive strength response, for different fixed values of
Factor A.
Contrary to what happened with early strength, by increasing the superplasticizer content and decreasing the
MK content (i.e., increasing the value of Factor A), the 28-day compressive strength rate increased. A possible
FIG. 12 RSM plots for 1-day compressive strength response for different fixed values of Factor A.

explanation of the latter could be found in the work of Khatib and Wild.61 They found that there is a decrease in
the porosity and the Ca(OH)2 content of MK-blended pastes and mortars up to 14 days. However, beyond 14 days,
the porosity and Ca(OH)2 levels increase. These phenomena were attributed to a critical change in the reaction
between MK and Ca(OH)2 at around 14 days, which involves the phase transformation of the reaction products,
that inhibits the reaction of MK with Ca(OH)2. Consequently, the strength enhancement produced by MK
reaches a maximum within the first 14 days and then declines.61 However, this hypothesis should be checked
by using a mercury intrusion porosimeter and a differential scanning calorimeter.
On the other hand, it is noted that the Ca(OH)2 content in a portland cement paste indicates the degree of
hydration of the cement, whereas the Ca(OH)2 consumption when using SCM is related to the degree of poz-
zolanic reaction.59,62 Regarding the latter Poon et al.,60 demonstrated that although a lower water-to-binder ratio
significantly reduces the degree of cement hydration, it has little effect on the degree of pozzolanic reaction of MK
at a 10 % replacement level. It may reduce the degree of pozzolanic reaction of MK at higher replacement levels.
As expected, Factor B has an adverse effect on the 28-day compressive strength. Finally, according to
figure 14, Factor C has a positive effect on the 28-day compressive strength of RPC, which was explained in
the previous section.
Conclusion
In this research, the effect of the partial substitution of CEM III 42.5 HE with MK in a previously optimized
mixture of reactive concrete powder with recycled glass and limestone powders was evaluated through a three-
factor CCD. In conclusion, the following observations can be drawn:
• The inclusion of MK in the dosage causes a decrease in the slump flow of concrete while the replacement
ratio of MK increases, which could be linked to the accelerating effect of MK in the hydration process, the
increase of the hydration process, and the porosity and water absorption of the MK particle.
• Under the EFNARC criteria, a plain SCC mixture could not be reached with values of MK over 91.57 kg/m3.
• The inclusion of MK highly and positively affects the 1-day and 7-day compressive strength because of the
acceleration of portland cement hydration and the pozzolanic reaction by MK with calcium hydroxide
(portlandite).
• For the 28-day compressive strength, the inclusion of MK has a slight negative effect on compressive
strength, as explained by both the pozzolanic index of MK at 28 days and the negligible decrease in
the packing density of concrete.
• Water-to-binder ratio has a positive effect on the slump flow but a negative effect on concrete strength at all
ages. The superplasticizer content has a positive effect on the slump flow.
• Regarding compressive strength the polycarboxylate-based ether superplasticizer slows down the hydration
of silicates and therefore has a negative effect on the development of early age strength. However, the

HRWR has a positive effect on the 28-day compressive strength because the particle dispersion was en-
hanced during the mixing procedure, which allows the finer particles to fill the gaps between the coarser
particles in the mixture, thereby increasing the real packing density of RPC.
Thus, the results obtained with the MK used in this study appear very promising for the manufacture of low-
cost UHPC with early high-strength needs without increasing the amount of costly SF. This could be an inter-
esting development for applications such as the connection of prefabricated elements for the accelerated bridge
construction methodology.
The perform of full factorial design for optimization represent the next research work in order to complete
the behavior knowledge of RPCs containing MK. The main objective of the optimization will be the development
of early high strength of RPC at lower cost. Other future works include the performance of thermogravimetric
analysis (TGA), isothermal calorimetry, and XRD to investigate the early hydration period and compare with the
statistical results of the present work.
ACKNOWLEDGMENTS
Special thanks to Cementos Argos SA. for donating most of the materials used in the research described herein.
The supply of recycled glass from Cristaleria Peldar SA, and the metakaolin from CORONA SA for this research is
highly appreciated. The writers would also like to acknowledge the support and suggestions of the Escuela
Colombiana de Ingeniería Julio Garavito and the Polytechnic University of Madrid (UPM).
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Advances in Civil Engineering Materials

doi:10.1520/ACEM20190224 / Vol. 9 / No. 1 / 2020 / available online at www.astm.org

Joaquín Abellán-García,1 María Alejandra Santofimio-Vargas,2 and