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Effects of Calcium Carbonate Nanoparticles and Fly Ash on Mechanical and

Permeability Properties of Concrete

Article · November 2018

DOI: 10.1520/ACEM20180066

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 Advances in Civil Engineering Materials

doi:10.1520/ACEM20180066 / Vol. 7 / No. 1 / 2018 / available online at www.astm.org

Fereidoon Moghadas Nejad,1 Morteza Tolouei,2 Hossein Nazari,3 and Ali Naderan3

Effects of Calcium Carbonate

Nanoparticles and Fly Ash on Mechanical
and Permeability Properties of Concrete

Reference
Nejad, F. M., Tolouei, M., Nazari, H., and Naderan, A., “Effects of Calcium Carbonate
Nanoparticles and Fly Ash on Mechanical and Permeability Properties of Concrete,” Advances in
Civil Engineering Materials, Vol. 7, No. 1, 2018, pp. 651–668, https://doi.org/10.1520/
ACEM20180066. ISSN 2379-1357

ABSTRACT
Manuscript received June 8, 2018; The use of additives to supplement or replace cement in concrete is a well-studied
accepted for publication October
topic. The use of fibers, polymers, minerals, and even nanomaterials has been
10, 2018; published online
November 27, 2018. considered for improving concrete properties such as permeability and strength,
1
and these issues are constantly under investigation. In this study, the mechanical
Department of Civil and
Environmental Engineering, properties and permeability of concrete containing calcium carbonate (CaCO3)
Amirkabir University of nanoparticles and fly ash are investigated. For this purpose, concrete specimens
Technology, Hafez Ave.,
Tehran 1591634311, Islamic
with different proportions of nanoparticles and fly ash were prepared and aged
Republic of Iran for 7 days and 28 days to investigate the mechanical properties via compressive
2
Department of Civil Engineering,
strength tests, tensile strength tests, and flexural strength tests under three-point
Science and Research Branch, loading and also to study the permeability properties via full water absorption
Islamic Azad University, PO Box
tests and the testing of penetration depth under water pressure. To determine
14515-775, Tehran 1477893855,
Islamic Republic of Iran the distribution of nanoparticles and their size and microstructure, scanning
(Corresponding author), e-mail: electron microscopy (SEM) images were obtained, and energy-dispersive X-ray
morteza.tolouei@srbiau.ac.ir,
https://orcid.org/0000-
spectroscopy (EDS) and X-ray diffraction (XRD) analyses were performed. The
0002-3481-3945 results show the positive effect of CaCO3 nanoparticles in filling concrete pores,
3
Department of Civil Engineering,
which leads to increased strength and reduced permeability. In general, the SEM
Science and Research Branch, images and EDS and XRD analyses showed that there was a good correlation
Islamic Azad University,
between the materials used in the concrete and also that the nanoparticles were
Tehran 1477893855, Islamic
Republic of Iran appropriately distributed in the concrete samples.

Copyright © 2018 by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959 651
652 NEJAD ET AL. ON CONCRETE

Keywords
concrete, mechanical properties, permeability properties, calcium carbonate nanoparticles, fly ash

Introduction
In the preparation of concrete, different types of cement, pozzolana, slag, furnaces, sulfur,
additives, polymers, fibers, etc., may be used [1–7]. Generally, for testing the mechanical
properties, compressive strength tests, tensile strength tests, and flexural strength tests are
used, and for testing the permeability properties, water penetration depth tests and water
absorption tests are used [8–16]. Many additives have been used to improve the mechani-
cal properties and the permeability of concrete, and each of these additives has its own
unique effect. Fly ash and various nanoparticles are among the additives that have been
used in the last few years [9,11,12,15–26]. Fly ash is a by-product of industrial processes,
and the use of a high volume of fly ash in concrete raises challenges relating to sustain-
ability [16]. Chemically, fly ash has pozzolanic activity attributed to the presence of silica
(SiO2) and alumina (Al2O3) [16]. These substances react with calcium hydroxide (CH)
during hydration to form calcium silicate hydrate (CSH) and calcium aluminate hydrate
(CAH) [16,27,28]. These two substances are effective in forming a denser matrix with
higher strength and less permeability, which enhances the resistance of the concrete to
deleterious phenomena such as sulfate attack and alkali silica reaction [29–31]. The
amount of cement replaced by fly ash is, in practice, limited to 15–20 % of the total mass
of cement material [16,32,33]. Most research on nanotechnology in concrete science in-
volves SiO2 nanoparticles [19,34–38], ferric oxide (Fe2O3) nanoparticles [39–42], titanium
oxide (TiO2) nanoparticles [17,43–47], Al2O3 nanoparticles [48–51], carbon nanotubes
[52–56], calcium carbonate (CaCO3) nanoparticles [11,15,16,21,52–57], and clay nanopar-
ticles [56,58,59]. It has been shown and observed that the addition of 5 % (total weight of
cement materials) Al2O3 nanoparticles increases the elastic modulus by about 143 % at the
age of 28 days [60]. The effects of these nanoparticles on the elastic modulus and the
compressive strength are different. Using 3 % (total weight of cementitious materials) and
5 % (total weight of cementitious materials) of Al2O3 nanoparticles reduces the strength at
28 days, but using 7 % (total weight of cementitious materials) causes a relative increase in
strength [60]. Clay nanoparticles include tetrahedrons of orthosilicate (SiO4), which are
bonded to alumina hexagonal plates in various ways. The most notable are the montmo-
rillonite smectites, which have two layers of tetrahedrons surrounded by an octahedral
hearth layer. In the study, 0.6 % and 0.4 % optimal percentages of the total weight of
cementitious materials were added, and the compressive strength of the concrete increased
by 13.24 %, while the permeability coefficient was reduced by 49.95 % [61]. Duan et al.
examined the effect of using TiO2 nanoparticles on the compressive strength of concrete
and found that the use of 5 % (total weight of cementitious materials) of these nanopar-
ticles resulted in an increase in the concrete strength at 28 days [62]. Mohamed (2016)
studied the effect of using nanoclay and nanosilica on the compressive and flexural
strength of concrete and revealed that the use of these nanomaterials resulted in increased
compressive strength and flexural strength [63]. Jalal, Ramezanianpour, and Pool exam-
ined the effect of using fly ash and TiO2 nanoparticles on the mechanical properties of
high-strength concrete. It was found that the use of up to 4 % (total weight of cementitious
materials) by weight of these substances resulted in increased durability and compressive
strength in the concrete [64]. Salemi and Behfarnia (2013) explored the effect of using

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NEJAD ET AL. ON CONCRETE 653

nanosilica in a concrete pavement containing fibers and concluded that 5 % nanosilica

(total weight of cementitious materials) could increase the compressive strength of the
concrete by up to 30 % [65]. In 2015, Du, Du, and Liu reviewed the effect of using nano-
silica on the durability of concrete and found that using 0.3 % nanosilica (total weight of
cementitious materials) resulted in an increase in concrete durability [66]. Research con-
ducted on concrete incorporating CaCO3 nanoparticles also shows the positive effect of
these nanoparticles on the concrete properties [11,15,16,21,57]. The investigation by
Shaikh and Supit (2014) showed that the high-volume fly ash (HVFA) concretes contain-
ing 1 % CaCO3 nanoparticles have reasonably higher compressive strength, lower volume
of permeable voids and porosity, and higher resistance to water sorptivity, chloride per-
meability, and chloride ion diffusivity than the counterpart HVFA concretes [16]. It is also
revealed that the addition of CaCO3 nanoparticles not only led to a much denser micro-
structure in the HVFA matrix but also changed the formation of hydration products, and
hence, contributed to the improvement of the early-age compressive strength and durabil-
ity properties of HVFA concretes [16]. Because the effects of these nanoparticles are well
known, different properties of the concrete are evaluated in each study. In this study, using
tests for mechanical properties and permeability properties, the effects of CaCO3 nano-
particles on concrete without fly ash and concrete with fly ash, at 7 days and 28 days, were
investigated. X-ray diffraction (XRD) and scanning electron microscopy (SEM) experi-
ments were also undertaken to investigate the presence of nanoparticles and the structure
of the nanoparticles in concrete.

Experimental Program
MATERIALS AND MIX PROPORTIONS
The cement used in this study is portland Type 2, according to the ASTM C150-07 stan-
dard, Standard Specification for Portland Cement [67]. Class F fly ash was used according
to the ASTM C618 standard, Standard Specification for Coal Fly Ash and Raw or Calcined
Natural Pozzolan for Use in Concrete [68]. Table 1 shows the chemical and physical char-
acteristics of cement and fly ash. The nanoparticle used in this study was CaCO3, and
Table 2 presents the characteristics of this nanoparticle. In Fig. 1, the XRD analyses of
cement, fly ash, and CaCO3 nanoparticles are shown. As shown in Fig. 1, in the CaCO3
nanoparticles analysis, calcite had the highest intensity at 28° position [°2Theta] and
the most compositions. In the fly ash analysis, the quartz had the highest intensity at
26° position [°2Theta] and the most compositions. In the fly ash analysis, the composition
of quartz (SiO2) at 26° position [°2Theta] had the highest intensity. In the cement, most of
the CS and CaCO3 compounds were observed. Natural aggregates with a maximum ag-
gregate size of 25 mm were used. A superplasticizer (superlubricant) was also used. This
superplasticizer is based on modified polycarboxylates. It has a green color, an anionic
liquid state with a pH value of about 7, and a specific gravity of about 1.1 kg/L.
In order to prepare the concrete samples, the mixture designs shown in Table 3 were
used. The mixtures design method is based on the ACI 211 standard, Standard Practice for
Selecting Proportions for Normal, Heavyweight, and Mass Concrete [69]. According to
Table 3, eight concrete mixtures were prepared with a water–cement ratio of 0.36; a total
cement, fly ash, and nano-CaCO3 content of 400 kg/m3; and a soft-sand modulus of 2.6. The
concrete was prepared using a laboratory concrete drum mixer or rotary mixer, according to
previous research [70]. Cement, fly ash, and aggregates (in Saturated surface dry (SSD)

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654 NEJAD ET AL. ON CONCRETE

TABLE 1
Chemical composition and physical tests of cement and fly ash.

Cement

Chemical Analysis (%) Min. Max Fly Ash

SiO2 21 22.5 70.7

Al2O3 4.7 5.5 20.7
Fe2O3 3.8 4.2 3.9
CaO 63 65 1.13
MgO 1.5 2.2 0.77
SO3 1.5 2.5 –
K2O 0.45 0.65 1.09
Na2O 0.45 0.65 0.26
TiO2 – – 0.92
P2O5 – – 0.15
MnO – – 0.05
Loss of ignition 1 2 0.7
Autoclave Expansion 0.05 0.15 –
Setting Time (min) Initial 100 160 –
Final 180 240
Fineness, cm2/g Blaine Test >2,900 –
Fineness, % – 99
Relative Density – 2.35

Note: CaO = calcium oxide; MgO = magnesium oxide; SO3 = sulfur oxide; K2O = potassium oxide; Na2O = sodium
oxide; P2O5 = phosphorus pentoxide; MnO = manganese (II) oxide.

TABLE 2
Physical properties of CaCO3 nanoparticles.

Properties CaCO3 Nanoparticle

Morphology Cubic or hexagonal

Color White
pH Not applicable
Bulk Density, g/mL 0.68
True Density, g/cm3 2.93
Specific surface area, m2/g 30–60
Average particle size, nm 10–45
Purity, % 99.9
Melting Point, °C 825
Boiling point, °C Decomposes
Molecular weight, g/mol 100.09

condition) were added dry to the mixer and mixed for 2 min, and then the water and super-
plasticizer were added and mixed for a further 2 min. To prevent agglomeration, the nano-
particles were added to water and manually stirred for 2 min. The prepared solution of
nanoparticles was added with the water to the mixer and mixed with the other materials
for 3 min. Finally, the concrete mixes were placed in laboratory molds for curing and testing.
For curing, samples were in the water tub until the break age. It should be noted that from
each mix of concrete in accordance with Table 3 for each experiment, three samples were
made, and an average of their results is presented in the results and discussion section.

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NEJAD ET AL. ON CONCRETE 655

FIG. 1
XRD patterns of cement, fly ash, CaCO3 Nanoparticles fly ash Cement
and CaCO3 nanoparticles. 40,000
C C = Calcite (CaCO3)
35,000 Q = Quartz (SiO2) M = Mullite H = Hematite
CS = Calcium Silicate CA = Calcite L = Larnite
30,000 Q

Intensity (Counts)
25,000
C C C
C C
20,000 C
M Q
15,000 H

10,000
CS CS
5,000
CS
L CA CS CS
0
10 15 20 25 30 35 40 45 50 55 60 65 70 75 80

Position [°2Theta]

TABLE 3
Mix proportions of concrete.

Mix ID Cement,kg/m3 Fly ash,kg/m3 Nano-CaCO3, kg/m3 Sand, kg/m3 Coarse Aggregate, kg/m3 Water, kg/m3 Superplasticizer,kg/m3

PCa 400 – – 1,161 846 147 3.3

N0.5b 398 – 2 1,161 846 147 3.3
N0.7c 397.2 – 2.8 1,161 846 147 3.3
N1.0d 396 – 4 1,161 846 147 3.3
Fe 320 80 – 1,161 846 147 3.3
FN0.5f 318 80 2 1,161 846 147 3.3
FN0.7g 317.2 80 2.8 1,161 846 147 3.3
FN1.0h 316 80 4 1,161 846 147 3.3

Note: a Without fly ash and without nano-CaCO3; b Without fly ash and with 0.5 % nano-CaCO3; c Without fly ash and with 0.7 % nano-CaCO3; d Without fly ash
and with 1 % nano-CaCO3; e With fly ash and without nano-CaCO3; f With fly ash and with 0.5 % nano-CaCO3; g With fly ash and with 0.7 % nano-CaCO3; h With
fly ash and with 1 % nano-CaCO3.

TEST PROCEDURE
Mechanical Properties
Mechanical tests were performed on the concrete specimens at 7 days and 28 days. The
compressive strength test was performed on 15 by 15 by 15-cm cubic samples according to
BS 1881-116, Testing Concrete Part 116: Method for Determination of Compressive Strength
of Concrete Cubes [71]. Tensile strength tests were performed on 30 by 15-cm cylindrical
specimens according to the ASTM C496/C496M standard, Standard Test Method for
Splitting Tensile Strength of Cylindrical Concrete Specimens [72]. In addition, flexural
strength tests were performed on concrete beams with dimensions of 600 mm in length,
100 mm in width, and 60 mm in height, in accordance with the ASTM C293/C293M
standard, Standard Test Method for Flexural Strength of Concrete (Using Simple Beam with
Third-Point Loading) [73]. For each mixing plan presented in Table 3, a total of six cubic
samples, six cylindrical samples, and six beams were prepared. The compressive strength,
tensile strength, and flexural strength final results at the ages of 7 days and 28 days were
obtained from the average strength of the samples.

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656 NEJAD ET AL. ON CONCRETE

Permeability Properties
The permeability tests, like the mechanical tests, were performed on the concrete spec-
imens at 7 days and 28 days. The test for the depth of penetration of water under pressure
was performed on 15 by 15 by 15-cm concrete specimens in accordance with BS EN
12390-8, Testing Hardened Concrete: Depth of Penetration of Water Under Pressure [74].
In this experiment, the surface of the concrete is cleaned from the grooves in the sample
frame so that the water entry point (test surface) is placed at the bottom. A water pressure
of 500 ± 50 kPa (5.1 ± 0.51 kg/cm2) was applied to the sample surface. The pressure was
constant for 72 ± 2 h. During this period, the sample and the apparatus were regularly
inspected to control water leakage, and the water pressure remained constant. Then,
the sample was removed from the apparatus. In the perpendicular position on the surface
under the test of water penetration, samples were pressured and split with the help of a rod.
The wet parts of the samples were marked with a marker, and the maximum penetration
depth recorded using calipers. The determination of the void percentage for water absorp-
tion was performed on 10 by 10 by 10-cm cubic samples according to the ASTM C642
standard, Standard Test Method for Density, Absorption, and Voids in Hardened Concrete
[75]. This test was performed in three steps: drying, saturation, and boiling of samples.
First, the sample was dried in an oven at 100–110°C for 24 h. After being removed from the
oven, the samples were equilibrated to 20–25°C, and the mass of the samples was calcu-
lated again. The samples were placed for the second time in the oven, again for 24 h, and
the mass was determined. This continued until the difference in mass was less than 0.5 %.
In the second step, the concrete samples were immersed in water for 48 h at 21°C, and then
for a further 24 h, until the difference in mass was less than 0.5 %. The saturation mass was
determined with a dry specimen surface. In the third step, the samples were boiled in a
drinking-water reservoir for 5 h until the temperature reached 20–25°C. Finally, having
obtained the masses and the relationships according to the ASTM C642 [75], we examined
the results.

Microstructural Evaluation
SEM and Field-Emission SEM
Pieces of the samples with the PC, F, N0.5, and N1.0 identifiers (the control sample with-
out fly ash or nanoparticles; sample containing only fly ash; sample with 0.5 % total weight
of cement materials CaCO3 nanoparticles; and the sample with 1 % total weight of cement
materials CaCO3 nanoparticles; respectively) were examined using SEM and field-
emission scanning electron microscopy (FE-SEM). These pieces of concrete were coated
with a very thin layer (1.5–3 nm) of gold and placed on the page for photography.
Subsequently, the microstructure of the samples was observed and examined. The purpose
of these images was to examine and evaluate the microscopic structure, measure the di-
mensions of the nanoparticles, and determine the chemical composition and particle size
distribution of the elements with energy-dispersive X-ray spectroscopy (EDS).

XRD
As in the study by Shaikh and Supit [16], small fragments of samples were ground man-
ually to prepare the powder sample for XRD analysis. The samples selected for the XRD
test were those with the F and FN1.0 (with fly ash and CaCO3 nanoparticles) identifiers at
28 days. The XRD patterns were obtained using an X’Pert PRO MPD (λ = 1.54 Å, Kα
ratio = 0.5, voltage = 40 kV) from PANalytical B.V., Netherlands, with CuKα radiation.
The diffraction patterns were recorded in the 2θ range of 10° to 80°, with a step of 0.025°.

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NEJAD ET AL. ON CONCRETE 657

FIG. 2
Compressive strength results of 60
different concrete at 7 and

Compressive Strength (MPa)

28 days. 50

40

30

20

10

0
PC F N0.5 N0.7 N1.0 FN0.5 FN0.7 FN1.0
7 days 21.60 23.70 41.64 39.27 36.24 33.65 31.12 29.40
28 days 34.67 36.34 53.57 50.91 47.69 44.86 41.34 39.74

Results and Discussion

MECHANICAL PROPERTIES
According to Fig. 2, the N0.5 sample with 41.64 MPa at 7 days and 53.57 MPa at 28 days
has the highest average compressive strength compared with the other samples. This
shows the effect of the CaCO3 nanoparticles in increasing the compressive strength and
improving the concrete mix. In general, the effect of CaCO3 nanoparticles in increasing the
compressive strength of the lower and upper ages of the samples was observed to be greater
than the effect of the fly ash during the first 28 days. This indicates a high-level and suitable
effect for CaCO3 nanoparticles in concrete mixing. The increased compressive strength of
concrete containing nanoparticles showed that nanoparticles accelerate the water-repellent
reaction and densify the microstructure of the matrix [76]. As shown in Fig. 2, the com-
pressive strength of the control sample (PC) and of Sample F, which contains only fly ash,
was less than that of the other specimens. According to Samples N0.5, N0.7, and N1.0, the
addition of CaCO3 nanoparticles decreases the compressive strength. It is concluded that
the sample containing 0.5 % (total weight of cementitious materials) CaCO3 nanoparticles
had the optimum proportion for increasing compressive strength. The compressive
strength of the FN0.5, FN0.7, and FN1.0 samples with fly ash and CaCO3 nanoparticles
was lower than that of N0.5, N0.7, and N1.0 with only CaCO3 nanoparticles. The reduced
effect of CaCO3 nanoparticles could be due to the effect of SiO2 on fly ash and its reaction
with CaCO3 nanoparticles. Chemically, the compressive strength of the samples compared
with the control sample (PC) at 7 days and 28 days shows that the fly ash exhibits poz-
zolanic activity because of the SiO2 and Al2O3. These substances react with CH during
cement hydration and form CSH and CAH, which contribute to the formation of a dense
matrix with higher strength and lower permeability [16,27,28]. Hydration products are
considered to be an important factor in accelerating the pozzolanic reaction and leading
to a strong composition with both fly ash and nanoparticles [19,77–79]. Furthermore,
chemically, the CaCO3 nanoparticles increased the reaction rate of tricalcium aluminate
(C3A) to form a carbon–aluminate complex, and hence, hydration products increase com-
pressive strength [16,80,81]. In addition, they react with tricalcium silicate (C3S) and ac-
celerate the hardening and development of initial strength in concrete [16,20,82]. As a
result of the formation of a larger volume of hydration materials, an increase in the amount

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658 NEJAD ET AL. ON CONCRETE

FIG. 3
Split tensile strength results of 5.0
different concrete at 7 and 4.5

Split Tensile Strength (MPa)

28 days. 4.0
3.5
3.0
2.5
2.0
1.5
1.0
0.5
0.0
PC F N0.5 N0.7 N1.0 FN0.5 FN0.7 FN1.0
7 days 2.30 2.35 3.55 3.25 3.14 2.95 2.80 2.71
28 days 3.25 3.35 4.45 4.35 4.10 3.85 3.70 3.56

of water absorption compensates for the effect of the dilution of the bonded materials and
therefore, results in a higher initial strength [16,83]. Moreover, the lower compressive
strength of concretes with a higher CaCO3 nanoparticle content (N1.0) can be attributed
to poor dispersion because of the agglomeration of CaCO3 nanoparticles in the wet mix
and the van der Waals forces in the cement [16].
As shown in Fig. 3, the addition of CaCO3 nanoparticles and fly ash to the concrete
also leads to an increase in tensile strength at both 7 days and 28 days. With an increase in
the proportion of CaCO3 nanoparticles as an additive in concrete both without fly ash and
with fly ash, tensile strength decreases. The N0.5 sample with a value of 3.55 MPa at the age
of 7 days and a value of 4.45 MPa at the age of 28 days had the highest tensile strength. This
indicates the positive effect of CaCO3 nanoparticles on the tensile strength. According to
Fig. 3, the fly ash (F sample) has little effect on the tensile strength. The fly ash had the
greatest impact when mixed with CaCO3 nanoparticles. This is because there is more SiO2
in the fly ash.
Fig. 4 shows that samples with CaCO3 nanoparticles and fly ash have a better
three-point flexural strength at the ages of 7 days and 28 days compared with the control

FIG. 4
Flexural strength results of 7
different concrete at 7 and
6
Flexural Strength (MPa)

28 days.
5

0
PC F N0.5 N0.7 N1.0 FN0.5 FN0.7 FN1.0
7 days 3.91 4.11 5.36 4.96 4.87 4.65 4.54 4.43
28 days 4.67 4.89 6.78 6.52 6.26 5.95 5.72 5.51

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NEJAD ET AL. ON CONCRETE 659

sample (PC). CaCO3 nanoparticles at 0.5 % (total weight of cementitious materials) had
the greatest effect on increasing the three-point flexural strength. Samples containing both
fly ash and CaCO3 nanoparticles have more flexural strength than the control sample (PC)
and samples with fly ash only (F) because the fly ash contains high levels of silicate and
aluminate, which react with the CaCO3 nanoparticles to produce additional hydration
products in the concrete. Therefore, the effect is to improve the flexural strength properties
at the ages of 7 days and 28 days [16]. It can be concluded that the addition of CaCO3
nanoparticles is effective in increasing the flexural strength of the samples. However, the
flexural strength decreases when the proportion of nanoparticles increases. As the pro-
portion increases, the flexural strength decreases because nanoparticles tend to aggregate
when the mixture contains a high proportion. This aggregation forms weak regions and
thus, prevents the formation of homogeneous hydrated microstructures, leading to a de-
crease in strength [16,77].

PERMEABILITY PROPERTIES
As shown in Fig. 5, with increased aging, the water absorption of the samples is reduced
for all mixing designs. In the PC sample, the water absorption for the samples at 7 days and
28 day was 6.87 % and 4.1 %, respectively. Lower water absorption in older specimens is
due to the increasing hydration reaction of the cement in these specimens. This reaction is
more advanced in the older samples, and therefore, the pores of the samples are filled with
hydrated products and so absorb less water. Water absorption decreases as a result of the
intensification of the hydration process, the intensification of the consumption of CH, and
the formation of new CSH gels that fill the spaces that would otherwise be filled with water,
reducing the porosity of the concrete [16]. In general, the addition of CaCO3 nanoparticles
was effective in reducing the porosity of the samples and hence, reducing the water ab-
sorption of the samples. As shown in Fig. 5, the N1.0 sample, i.e., 1 % (total weight of
cementitious materials) CaCO3 nanoparticles, had the greatest effect in reducing the ab-
sorption of water from the primary (7 days) and secondary (28 days) concrete samples.
Furthermore, in samples with fly ash, an increase in the nanoparticle proportion led to a
decrease in the water absorption of the concrete. It can be concluded that, among the
studied systems, the optimal proportion of CaCO3 nanoparticles is about 1 % (total weight

FIG. 5
Water absorption results of 8
different concrete at 7 and
7
28 days.
Water absorption (%)

6
5
4
3
2
1
0
PC F N0.5 N0.7 N1.0 FN0.5 FN0.7 FN1.0
7 days 6.87 5.48 5.58 5.55 4.94 5.94 5.81 5.36
28 days 4.10 3.26 3.50 3.38 3.00 3.87 3.85 3.18

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660 NEJAD ET AL. ON CONCRETE

FIG. 6
Water penetration depth results 35
of different concrete at 7 and

Water penetration depth (mm)

30
28 days.
25

20

15

10

0
PC F N0.5 N0.7 N1.0 FN0.5 FN0.7 FN1.0
7 days 32.00 15.80 13.60 12.00 9.8 26.50 24.30 11.60
28 days 29.10 12.60 11.30 9.70 7.4 24.80 21.60 9.20

of cement materials) for water absorption in concrete samples with fly ash and without
fly ash.
According to Fig. 6, in the control concrete (PC), the penetration depth for the sam-
ples at 7 days and 28 days was 32 % and 29.1 % (maximum), respectively. As shown in
Fig. 6, the porosity of all the concrete samples reduced with increasing age. Sample N0.7,
at 7.4 and 9.8 mm (28 days and 7 days, respectively), had the lowest penetration depth
compared with other specimens. As a result, the porosity of this sample was lower.
Therefore, it can be concluded that the addition of CaCO3 nanoparticles is effective in
reducing the porosity of the sample and decreasing the penetration depth of water in
the sample. The optimum proportion of CaCO3 nanoparticles in the samples containing
fly ash was 1 % (total weight of cement materials). By combining CaCO3 nanoparticles
with fly ash, the acceleration of the hydration process can be increased. This is due to the
consumption of CH and the formation of a new CSH gel. The addition of nano-CaCO3
also led to a densification of the microstructure and reduction of the concrete pores [16].
According to Fig. 6, changes in the penetration depth of samples compared with the con-
trol sample (PC) indicate that all specimens have a reduced penetration depth and poros-
ity. This is most marked in Sample N1.0. After N1.0, Samples FN1.0 and N0.7 at 67 % and
61 % (28 days), respectively, had the highest degree of penetration depth reduction and
porosity reduction.

MICROSTRUCTURAL EVALUATION
As discussed in the previous section, electron microscope observations were used to ex-
amine the proper distribution of fly ash and nanoparticles in concrete, to investigate the
hydration reaction and formation of cement structures, and also to observe the particle
size. In this section, PC, F, N0.5, and FN1.0 samples were examined using an electron
microscope. Fig. 7 shows micrograph images of the PC sample, (i.e., the sample without
fly ash or CaCO3 nanoparticles), the F specimen, (i.e., the sample with fly ash) and the FN1
sample (with fly ash and CaCO3 nanoparticles). Constituent elements after cement hy-
dration include the desired elements, such as CH and CSH, and undesirable elements,
such as holes and pores and Ettringite [84]. In Fig. 7a, the undesirable elements, such
as holes and pores, are more than those in Fig. 7b and c. According to Fig. 7b and c,
when using fly ash and CaCO3 nanoparticles, samples become denser, and the concrete

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NEJAD ET AL. ON CONCRETE 661

FIG. 7
SEM images of (a) control
specimens (sample without fly
ash and CaCO3 nanoparticles),
(b) a sample containing fly ash,
and (c) a sample containing fly
ash and 1 % CaCO3
nanoparticles.

porosity decreases. This is because fly ash reacts with CH during cement hydration to form
a supersaturated CSH, which then forms a denser matrix, resulting in higher strength and
better permeability. In the Fig. 7c, the nucleation is performed around the nanoscale. In
fact, the the nanoparticles accelerates the hydration of the cement, generates more desired
products, and decreases the pores of the concrete. In addition, the sponge-like parts were
in solid form, which is also due to the CSH. This is the most desirable hydration product
and the main cause of the increase in strength and decrease in permeability of cement
compounds.
Because the FE-SEM is equipped with EDS microanalysis, it is possible to identify the
smallest quantities of phases and elements. As shown in Fig. 8a, a part of Sample FN0.5
(i.e., the sample with 0.5 % total weight of cement materials CaCO3 nanoparticles) was sub-
jected to EDS analysis, the result of which is shown in Fig. 8b. The device indicated the
presence of CaCO3 nanoparticles with an estimated size of 29.33 nm. The EDS spectrum
chart (Fig. 8b) is plotted based on the amount of energy received from each energy level (Kα
or Kβ). Each of the peaks of the graph is assigned to a particular atom, and peaks of greater
height indicate a greater concentration of that element in the sample. As shown in the Fig. 8,
Si has the highest concentration because of the presence of fly ash. After Si, O, Ca, and C are
shown to be much more concentrated than other elements, and the technique can confirm

FIG. 8
Micrograph and EDS analysis of
concrete with 0.5 % CaCO3
nanoparticle content (a) EDS
region and (b) EDS spectrum.

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662 NEJAD ET AL. ON CONCRETE

FIG. 9
XRD analysis for concrete with 14,000
fly ash (F) and concrete with fly Q
F FN1
ash and 1 % nano-CaCO3 (FN1). 12,000

10,000 CH = Calcium Hydroxide

Intensity (Counts)
CS = Calcium Silicate
8,000 Q = Quartz (SiO2)

6,000 CH
Q
4,000
CH
CS CH CS
2,000 CH CH
CH
0
0 10 20 30 40 50 60 70 80 90
Position [°2Theta]

the addition of CaCO3 nanoparticles to the concrete. The symbols α and β are related to the
transition between the L and K levels or between the M and K levels.
Fig. 9 shows the XRD analysis of the concrete sample with fly ash (F) and the sample
with fly ash and 1 % (total weight of cementitious materials) nano-CaCO3 (FN1) at the age
of 28 days. In Fig. 9, the horizontal axis is the 2θ angle (in degrees), and the vertical axis is
the linear intensity (in terms of counts). Regarding Fig. 9 for both samples, peak intensity
Q for SiO2 at 26.5° is the highest. Because of the addition of CaCO3 nanoparticles, the
intensities of the CH and CS peaks decrease, which indicates a reaction with this material.
The nanoparticles react with CH, cement, and fly ash, which can lead to significant in-
creases in strength and can reduce water absorption and reduce the penetration depth of
the samples, compared with the samples without nanoparticles.

Conclusion
This study investigated the effects of nano-CaCO3 and fly ash on the mechanical and per-
meability properties of concretes. The following conclusions can be drawn.

• The results of mechanical property tests (compressive strength, tensile strength, and
flexural strength) showed that samples containing CaCO3 nanoparticles had the
greatest improvement in mechanical properties in the primary (7 days) and secon-
dary (28 days) concrete samples. The chemical reaction of the nanoparticles with the
elements in the concrete results in increased strength. The use of fly ash in concrete
led to a slight improvement in the mechanical properties of the concrete, but adding
CaCO3 nanoparticles to samples with fly ash increased the strength. On the other
hand, an increase in the proportion of nanoparticles leads to a decrease in strength.
According to the results, 0.5 % CaCO3 nanoparticles can be considered as an opti-
mum proportion for improving the mechanical properties of concrete.
• According to the results obtained from the concrete permeability tests (water ab-
sorption test and penetration depth test), CaCO3 nanoparticles had a significant
effect in improving the concrete properties. In the water absorption test and the
water penetration depth test, the control sample (without nanoparticles and without
fly ash) had the highest water absorption, penetration depth, and porosity. In sam-
ples without fly ash and with fly ash, the addition of CaCO3 nanoparticles at 1 %

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NEJAD ET AL. ON CONCRETE 663

(total weight of cementitious materials) had the greatest effect on reducing water
absorption and led to the lowest water penetration depth for both primary and sec-
ondary ages. This modification and improvement of permeability properties could
be due to the consolidation of the microstructure and the correction of the concrete
pore space.
• The results of the SEM observations show that CaCO3 nanoparticles are well dis-
tributed in the concrete sample, which increases the effect of nucleation on the
hydration process, hence, reducing the porosity of the concrete. The results of the
EDS analysis show high concentrations of Si because of the presence of cement. In
addition, the concentrations of Ca and O were significant. XRD results confirm the
presence of CaCO3 nanoparticles in the concrete, showing the reaction of these
nanoparticles with CH, cement, and fly ash, leading to the increased strength
and improved permeability properties of the samples, compared with the samples
without nanoparticles.

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