Construction and Building Materials 165 (2018) 93–103

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Construction and Building Materials

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Review

Influence of nano- and micro-silica additions on the durability

of a high-performance self-compacting concrete
Jordi Massana a,⇑, Encarnación Reyes b, Jesús Bernal c, Néstor León b, Elvira Sánchez-Espinosa a
a
Dpto. de Ingeniería Agroforestal, E.T.S.I. Agronómica, Alimentaria y Biosistemas, Universidad Politécnica de Madrid, Av. Complutense s/n, 28040 Madrid, Spain
b
Dpto. Ingeniería Civil: Construcción, E.T.S.I. de Caminos, Canales y Puertos, Universidad Politécnica de Madrid, C/ Profesor Aranguren 3, 28040 Madrid, Spain
c
Escuela de Ingeniería Mazatlán, Universidad Autónoma de Sinaloa, México, Mexico

h i g h l i g h t s g r a p h i c a l a b s t r a c t

The effects of a binary and ternary

mixture with nSi and mSi on HPSCC
were examined.

The use SP produced bubbles directly
proportional to the nSi quantity
incorporated.

The ternary mixture 2.5%/2.5% of nSi
and mS was the highest compressive
strength.

Generally ternary mixtures show the
greater resistance to the carbonation.

Usually ternary mixtures show the
greater resistance to freeze-thaw
cycles.

a r t i c l e i n f o a b s t r a c t

Article history: The main purpose of the research is to examine the effects of binary and ternary mixtures of nSi and mSi
Received 3 July 2017 on the durability of a high-performance self-compacting concrete (HPSCC). Compressive strength at 28
Received in revised form 5 November 2017 days, accelerated carbonation processes after 60 and 200 days of exposure to CO2, resistance to freeze-
Accepted 11 December 2017
thaw cycles and capillary suction coefficient, were analyzed. In addition, microstructural characterization
Available online 10 January 2018
was carried out by Mercury Intrusion Porosimetry (MIP). Ten blends were manufactured: one without
additions as control, three with 2.5%, 5% and 7.5% of nSi, three more with 2.5%, 5% and 7.5% of mSi and
Keywords:
three using both admixtures, with 2.5%/2.5%, 5%/2.5% and 2.5%/5%, of nSi and mSi, respectively. The high-
High-performance self-compacting concrete
Microsilica
est compressive strength is achieved in the ternary admixture with 2.5%/2.5%. A wider particle size dis-
Nanosilica tribution creates a low porosity, improves packing density, decreases water demand in comparison with
Durability mixtures with the same amount of total addition using only nSi, provides higher compressive strength
Accelerated carbonation and an improved durable performance. The porous network in mixtures with nSi involved a smaller pore
Freeze-thaw cycles diameter with respect to control, proportional to the amount of nSi. In concretes with mSi, there was a
lower total porosity with an average pore size similar to the reference concrete. In ternary mixtures,
the porous network presented concretes with a smaller average pore size and a smaller total porosity.
This produced concretes with a high compactness and improved durability properties, with a lower cap-
illary absorption and a lower susceptibility to carbonation and freeze-thaw cycles. The low capillary

⇑ Corresponding author.
E-mail addresses: jordi.massana@upm.es (J. Massana), encarnacion.reyes@upm.es (E. Reyes), jmbernalc@uas.edu.mx (J. Bernal), elvira.sanchez.espinosa@upm.es
(E. Sánchez-Espinosa).

https://doi.org/10.1016/j.conbuildmat.2017.12.100
0950-0618/Ó 2017 Elsevier Ltd. All rights reserved.
94 J. Massana et al. / Construction and Building Materials 165 (2018) 93–103

absorption deduced in this type of concrete might prevent the penetration of aggressive agents afflic-
tively and hence, increases the life span of concrete structures in aggressive environments.
Ó 2017 Elsevier Ltd. All rights reserved.

Contents

1. Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 94
2. Experimental study . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 95
2.1. Materials used and mixture proportioning . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 95
2.2. Test program . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 96
3. Results and discussions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 97
3.1. Mechanical properties. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 97
3.2. Microstructural characterisation by Mercury Intrusion Porosimetry (MIP). . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 98
3.3. Durability properties . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 99
3.3.1. Carbonation depth . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 99
3.3.2. Freeze-thaw resistance. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 100
3.3.3. Capillary absorption . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 101
4. Conclusions. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 102
Acknowledgements . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 102
References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 102

1. Introduction no segregation, coarse aggregate blocking or bleeding. These work-

In designing a concrete structure, one of the most important
properties to be considered, in addition to have an adequate
mechanical strength, is durability. Durable concrete must resist
any chemical, physical or biological process that tends to damage
it during the service life of the structure.
There are several aggressive agents and environmental condi-
tions that can significantly affect reinforced concrete structures
or precast concrete elements, and to date there are many unre-
solved issues regarding the physical and chemical durability of
concrete, in particular when additions or by-products are used
[1]. This study focuses on two of the most important and frequent
actions: freeze-thaw cycles and carbonation of a high-performance
self-compacting concrete with nano and micro silica additions.
Damage due to the freeze-thaw action can occur when concrete
pores are fully saturated or close to saturation, since during the
process of freezing, water volume increases around 9%. If there is
insufficient space in the concrete to control this expansion, damage
can occur. Such damage can be both internal (specifically, micro-
structural damage generated by micro-cracking) and external (loss
of material by peel) [2]. Another agent that can cause significant
damage is CO2 from the atmosphere which can penetrate the con-
crete pores and reacts with calcium hydroxide. This creates cal-
cium carbonate which then progressively reduces concrete or
cement paste alkalinity. This phenomenon is the known process
of carbonation. If the pH value of concrete reaches 9.5 or lower,
the alkalinity of the media is insufficient to keep the protective
oxide coat of reinforcing steel bars in a passive manner. Therefore,
under the action of both moisture and oxygen, a steel corrosion
process can be initiated which leads to concrete prone to develop-
ing a generalised corrosion [3]. Hence, in order to guarantee a good
durability of precast, as well as on site concrete elements regarding
the two above-mentioned damaging processes it is necessary to
use high-performance concrete to prolong concrete service life.
Self-compacting concrete (SCC) has been used for more than 20
years both in civil engineering and in building works. The main
property of this type of concrete is its high workability [4,5]. This
allows placement, under its own weight, without the usual vibrat-
ing compaction requirements, in densely reinforced and congested
structures and/or with complex geometries. Additionally, it shows
ability properties are mainly due to the high content of fine aggre-
gates, a reduced content and size of coarse aggregates and the
action of superplasticizer admixtures that provides the fluidity
required for placement on site [6]. Moreover, SCC allows the final
cost of the structural element to be reduced and concrete produc-
tivity to be improved. At the same time, good mechanical proper-
ties, durability and uniformity of the hardened material can be
achieved. Such advantages increase the use of SCC in several pro-
jects. Moreover, the high workability of SCC reduces the produc-
tion costs and maintenance of equipment, which is particularly
relevant in the prefabrication industry. In order to obtain an ade-
quate flowability in fresh state, the use of a high amount of cement,
mineral admixtures and superplasticizer is often required, as the
water/cement ratio is low. Special care should be taken in ensuring
the required workability when additions or by-products are used
in the concrete mixture [7].
According to the experts for specialised construction and con-
crete systems, SCCs can be classified in three classes in terms of
the flowability, measured by the slump-flow test [6]. The slump-
flow classes defined are the following:
SF1 (550–650 mm) is appropriate for unreinforced or slightly
reinforced concrete structures that are cast from the top with free
displacement from the delivery point (e.g. housing slabs).
SF2 (660–750 mm) is suitable for many normal applications
(e.g. columns and walls).
SF3 (760–850 mm) is typically produced with a small maxi-
mum size of aggregates (fewer than 16 mm) and used for vertical
applications in congested structures, structures with complex
shapes, or for filling areas under formwork.
Shi et al. [8], proposed different methods to design a SCC mix-
ture. In their published research, they suggest use different meth-
ods according to the properties required. A high-performance
self-compacting concrete (HPSCC) is understood to be a self-
compacting concrete with both high-compressive strength and
durability properties. In general, such a HPSCC is obtained through
high cement contents and a low water/cement ratio, which can be
improved by the use of inactive or active additions to the mixture.
Nepomuceno et al. [9] proposed a methodology to design SCC mix-
tures. For this purpose, they obtained correlations between param-
eters of the properties of the fresh-state and hardened concrete.
 J. Massana et al. / Construction and Building Materials 165 (2018) 93–103 95

Jalal et al. [10] replaced a Portland cement fraction with differ- This work is a part of a more extensive research [30]. The main
ent fractions of pozzolanic mineral additions. However, there have purpose of the extensive research is to study the effects of binary
been many other studies published that examine use of inactive and ternary mixtures of nSi and mSi when incorporated, in differ-
and active mineral additions [10–19]. The main objective of the ent proportions, during HPSCC mixture preparation. In doing so,
use of these additions, and in particular of nano and micro- several standard tests were carried out during concrete fresh state
particles, in mortars and concretes is to improve the strength and to evaluate the self-compacting properties of the mixtures.
durability properties of the final material. Undoubtedly the design of self-compacting mixes with these addi-
There are several nano-particles that have been studied (mainly tions is a challenge due to the loss of workability, and in this work
silica, titanium, aluminium and iron oxides) [20]. However silica it has been possible using appropriate dosages and compatible
oxide with nanometric or micrometric particle-size, is the most chemical admixtures. Additionally, compressive strength, resis-
used particle in concrete. This is because the addition of nano- tance to freeze-thaw cycles and accelerated carbonation-process
silica (nSi), or micro-silica (mSi) presents high pozzolanic activity properties were evaluated in the hardened state of concrete. Once
[21–23]. This pozzolanic activity can facilitate the crystal nucle- the durability properties were obtained and analysed in the HPSCC
ation of hydrated cement apart from the effect of filler and chem- mixtures, optimisation of chemical admixtures’ dosages for struc-
ical reactivity [15]. Theoretically, these effects become more tural element fabrication with a high sustainability could be
remarkable as the smaller the particle size is, that is to say, the big- possible.
ger the specific surface is. There are numerous studies that com-
pare the effects between additions of nSi and mSi [10,24,25].
2. Experimental study
Although both additions can react with calcium hydroxide or port-
landite (Ca(OH)2), it is the nSi that generates the greatest amount
2.1. Materials used and mixture proportioning
of CSH gel and, therefore, improves the concrete mechanical
strength at early stages [14,16,26,27] at the same time as densify-
In this study, the cement used was a CEM I 52.5 R (CP), accord-
ing the cementitious matrix [28]. In addition, the size and the
ing to EN 197-1. Table 1 presents the chemical composition and
amount of portlandite crystals are significantly reduced, as the
physical properties of cementitious materials used. The mineral
crystals cluster within the small pores of the cement paste. Addi-
admixtures used were nSi and mSi. The first was dispersed in
tions of nSi and mSi also produce an increase over the amount of
water, under the trade name of LevasilÒ 200/40%, with 40% of solid
hydration products [16], improving the cement durability proper-
by weight, a specific surface area of 200 m2 g1 and a particle size
ties since they are more compact and diminishing penetration of
of approximately 15 nm (see Table 1). The mSi used was Elkem
aggressive agents [27]. In order to achieve a better packing of the
MicrosilicaÒ MS 940 U, a material composed of nonporous amor-
microstructure, the mixtures should have a continuous particle
phous spheres of SiO2 with submicron size and small agglomerates,
size distribution of the material used for concrete production. In
with a specific surface area of 15–30 m2 g1 and particle size of
2012, Jalal et al. [25] analysed the mechanical and rheological
approximately 0.15 mm (see Table 1). Even when some of the
properties of a HPSCC that incorporated nSi, mSi and ternary mix-
spheres can be found in individual way, the majority tend to form
tures. Water absorption, electrical resistivity and the penetration
agglomerates of primary particles with a size range between 0.1
of chloride ions were also compared for the case of nSi, mSi and
and 1micron.
ternary mixture additions. They concluded that the more refined
The additives employed were the following: as superplasticizer
pore structure of the concrete containing admixtures could lead
(SP), SIKA ViscoCreteÒ 5720 based in polycarboxylate polymers
to enhancement of strength and the durability properties of HPSCC
and SIKA StabilizerÒ 4R (MV) which permits the viscosity of con-
specimens, especially at longer ages. Jalal et al. [10] analysed
crete to be controlled, with a constant amount in all mixtures of
the effects of nSi, mSi and fly ash and their combinations on
0.15% by weight of cement (wt%).
rheological properties, water absorption, capillary absorption and
The aggregates used in the mixtures were: 1160 kg/m3 of river
chloride penetration resistance of HPSCC. In this study, the results
sand (A) of less than 4 mm and fineness modulus 3.30, 585 kg/m3
also showed that mechanical and transport properties improved in
of gravel (G) rolled from 6 to 12 mm and 100 kg/m3 of limestone
the mixtures containing admixtures, especially blend of silica
filler (LF) with a granulometry in accordance with UNE 12620:
nanoparticles and silica fume. Gesoglu et al. [29] studied the effect
2003 + A1: 2009 and with a maximum diameter of 63 lm. All the
of using binary and ternary blends of nSi and mSi on the mechan-
SCCs were made by using a water-to-cementitious material ratio
ical properties of low-binder ultra-high performance cementitious
(w/cm) of 0.36 and 450 kg of cement. Table 2 shows the 10 dosages
composites (UHPCs). The mixtures of UHPC containing nSi and mSi
designed. For the above, the additions of nSi and mSi were used in
showed better mechanical behaviour than concretes containing
different percentages in reference to cement weight. It is important
only nSi. However, there are few published works that evaluate
to mention that additions (nSi and mSi) were not used as a cement
the effects of nSi, mSi and ternary combinations on durability prop-
replacement, but as an additional cementitious material. Regarding
erties of HPSCC, such us freeze-thaw and carbonation-process
the HPSCC dosages, three were made with 2.5%, 5% and 7.5% of nSi,
resistance which are very important for concrete structures in
which were identified as [nSi]-2.5; [nSi]-5 and [nSi]-7.5, respec-
some aggressive environments. For example freeze-thaw resis-
tively. Three more were made with 2.5%, 5% and 7.5% of mSi, which
tance is considered as fundamental for the precast, as well as on
were identified as [mSi]-2.5; [mSi]-5 and [mSi]-7.5, with the
site, structural elements used in natural environments with fre-
remaining three being made by using both admixtures (ternary
quent frost action, such as high-mountain environments.
mixtures), nSi and mSi, with percentages of 2.5%/2.5%, 5%/2.5%

Table 1
Properties of Portland cement (CP) and mineral additions (nSi, mSi).

SiO2 Al2O3 Fe2O3 CaO MgO SO3 K2O Na2O Loss on ignition (%) Density (gcm3) Specific Surface area (m2g1)
CP 19.20 6.07 1.70 63.41 2.56 3.38 0.2 0.33 2.09 3.5 0.42
nSi 99.90 – – – – – – – 0.10 1.29 200
mSi 94 – – – – – – – – 0.7 30
96 J. Massana et al. / Construction and Building Materials 165 (2018) 93–103

Table 2
Mixture proportions for the HPSCC studied.

Material (kg/m3) HPSCC [nSi]-2.5 [nSi]-5 [nSi]-7.5 [mSi]-2.5 [mSi]-5 [mSi]-7.5 [nmSi]-2.5/2.5 [nmSi]-5/2.5 [nmSi]-2.5/5
nSi – 11.25 22.5 33.75 – – – 11.25 22.5 11.25
2.5% 5% 7.5% 2.5% 5% 2.5%
mSi – – – – 11.25 22.5 33.75 11.25 11.25 22.5
2.5% 5% 7.5% 2.5% 2.5% 5%
water 162 166 170.1 174.1 166 170.1 174.1 170.1 174.1 174.1
SP (%) 2 3.30 4 6 2.30 2.50 2.70 3.60 4.80 3.90

Table 3
Results of self-compacting tests.

Tests HPSCC [nSi]-2.5 [nSi]-5 [nSi]-7.5 [mSi]-2.5 [mSi]-5 [mSi]-7.5 [nmSi]-2.5/2.5 [nmSi]-5/2.5 [nmSi]-2.5/5
df (mm) 650 720 635 565 787 817 795 685 675 752
TV (s) 8 11 13 17 10 7 5 12 12 10
Cbl 0.98 0.96 0.81 0.85 0.95 0.95 1 0.89 0.97 0.97
Slump-flow class SF1 SF2 SF1 SF1 SF3 SF3 SF3 SF2 SF2 SF2

and 2.5%/5%, respectively (identified as [nmSi]-2.5/2.5; [nmSi]-
5/2.5; [nmSi]-2.5/5). In order to obtain reference values to compare
the results, a HPSCC without mineral additions was designed. The
only cementitious material was CEM I 52.5 R.
The following tests were performed to determine the self-
compacting of the blends: slump-flow diameter [df (mm)],
V-funnel flow time [TV (s)], and L-box height ratio [Cbl] [6,31].
The values obtained in the tests are shown in Table 3.
According to EFNARC classification [6], in this work, mixtures
with additions of mSi are classified as SF3, ternary mixtures as
SF2, mixtures with 5 wt% and 7.5 wt% of nSi as SF1 and the mixture
with 2.5 wt% of nSi as SF2. Thus, the addition of nSi decreased the
settlement flow diameter as such an addition increased. This indi-
cates a lower docility of the mixture, even though there is an
increase of up to 6 wt% in the amount of SP, higher than that rec-
ommended by the Spanish Standards, Instrucción Española del
Hormigón Estructural (in English: Structural Concrete Instruction)
EHE-08 [31]. Consequently, this suggests that the percentage of
nSi, in binary mixtures, to obtain an acceptable slump flow should
not exceed 2.5 wt%. This is in agreement with research published
by Ghafari et al. [16], which limits the percentage to 3 wt%. How-
ever, Güneyisi et al. [32] obtain SF2 mixtures with up to 6 wt% of
nSi. The difference may be due to the higher amount of cement
and superplasticizer in mixtures with nSi used in their case.
None of the mixtures presented segregation or bleeding, despite
having high amounts of SP and even, for the mixture [nSi]-7.5 (6 wt
%), higher than that established by the previously mentioned EHE-
08 [30], which limits its use to 5 wt%. A high amount of SP additive
produces significant bubbling directly proportional to the aggre-
gate amount [33,34]. These bubbles can give rise to the formation
of non-interconnected pores in the hardened material, which can
compromise the resistant characteristics of this concrete. In order
to avoid this phenomenon, together with the polycarboxylate,
use of a condensed polyethylene that acts as a defoamer is recom-
mended [25].
2.2. Test program
A total of 40 specimens with a diameter of 100 mm and a height
of 200 mm were made. The moulds were removed 24 h after cast-
ing and then placed in a curing chamber at a temperature of 20 ± 2
°C and a relative humidity of 95 ± 5% until testing, according to
UNE-EN 12390-2: 2009.
The mechanical properties were evaluated by examining
compressive strength test at the age of 28 days, according to
UNE-EN-12390-3:2009.
It is important to note that the maximum size of aggregates was
lower than 12 mm; this permitted use of a specimen with a diam-
eter of 100 mm and height of 200 mm in the compressive strength
test [3,31]. An Ibertest press, with a maximum capacity of 1500 kN,
was used to carry out the test. The speed test was of 0.2 MPa/s until
reaching 40% of compressive strength.
Microstructural characterization was carried out by Mercury
Intrusion Porosimetry (MIP). The pore-size distribution and total
porosity were evaluated. In order to perform the test, two layers
of 60 mm and 20 mm were cut, respectively, with the external
layer of the concrete specimen being discarded. In such a test,
the specimen of 60 mm was used. From this, two cylinders with
a diameter of 10 mm and a height of 20 mm were extracted from
the central and peripheral areas. The MIP was carried out according
to ASTM D4404-84 (2004), with the equipment used being a
Micromeritics Autopore IV 9500 with a maximum pressure of
33,000 psi and range of 5 nm and 180 mm.
Lastly, the durability properties were evaluated by performing
accelerated carbonation tests, capillary absorption and resistance
to freeze-thaw cycles. The carbonation accelerated test was carried
out according to UNE-EN 13295:2005. In order to determine the
carbonation depth, a specimen with a diameter of 100 mm and
height of 200 mm was used. The specimens were cured in a cham-
ber with a relative humidity >95% for 28 days. They were then
placed in a hermetic chamber with a relative humidity of 75 ± 5%
and temperature of 20 ± 2 °C with a controlled content of carbon
dioxide of 4.7 ± 2.5%. After 56 days, the specimens were cut and
sprayed with phenolphthalein to determine carbonation depth.
The test for the freeze-thaw resistance of concrete was carried
out according to UNE-CEN/TS 12390-9:2008 and capillary suction,
de-icing agent and freeze-thaw (CDF) test by the alternative
method. In this case, it was necessary to prepare five specimens
for each mixture, with dimensions of 150 mm  150 mm  70
mm. These specimens were demoulded after 24 h and cured under
water for six days; after that time they were placed in a curing
chamber with a temperature of 20 ± 2 °C and relative humidity of
70 ± 5% until the age of 24 days. The specimens were then prepared
by covering the side surfaces with epoxy resin until a layer thick-
ness of 0.8 mm was obtained. For the test, a DYCOMETAL CCK-
40/100 climate chamber was used. The freeze-thaw cycles were
of 12 h with a temperature range from 20 °C to +20 °C. In order
to determine the freeze-thaw resistance of the HPSCCs, the loss
of mass by peel was measured after 6, 14 and 28 cycles.
The absorption test was carried out according to UNE
83982:2008, for which two specimens with a diameter of 100
mm and height of 50 mm were used. The specimens were prepared
 J. Massana et al. / Construction and Building Materials 165 (2018) 93–103 97

Table 4
Means for compressive strength at 28 days by mixture with 95% LSD intervals.

Mixture Count Mean Lower limit Upper limit

a
HPSCC 3 62.46 60.74 64.17
[mSi]-2.5 3 63.79a 62.08 65.51
[mSi]-5 3 65.01a,b 63.30 66.72
[mSi]-7.5 3 68.86c,d 67.15 70.57
[nSi]-2.5 3 65.73a,b,c 64.02 67.44
[nSi]-5 3 68.37b,c,d 66.66 70.08
[nSi]-7.5 3 70.35c,d 68.64 72.06
[nmSi]-2.5/2.5 3 82.17e 80.46 83.89
[nmSi]-2.5/5 3 69.26c,d 67.54 70.97
[nmSi]-5/2.5 3 71.15c,d 69.44 72.86
Total 30 68.72
Standard error of the mean (SEM) 1.16
a-e
Superscripts (a-e) indicates homogeneous groups.

according to UNE 83966:2008. Capillary absorption was obtained

by measuring the weight increase of the specimens at 0, 5, 10, 15
and 30 min, and at 1, 2, 3, 4, 6 and 24 h and each 24 h up to 18
days.

3. Results and discussions

3.1. Mechanical properties

Table 4 shows the means for compressive strength at 28 days by

mixture with 95% Least Significant Difference (LSD) intervals.
Values with different superscripts (a, b, c and d) indicate significant
differences between them. It also shows the standard error of each
mean, which is a measure of its sampling variability. The rightmost
two columns show 95% confidence intervals for each of the means.
Table 4 also shows how the compressive strengths in concrete
with additions are significantly higher than those of the reference
concrete, except in the mixture with 2.5 wt% mSi. In this propor- Fig. 2. Frequency distribution of the pores in binary mixtures with mSi at 7 days of
tion, the addition of mSi had no influence on the strength. Only curing.
from 5 wt% mSi with respect to this property a significant effect
can be observed. In mixtures with nSi, the increase in compressive
strength is more noticeable. Gesoglu et al. [29] showed that the
effect of 1 wt% addition of nSi is almost equal to, or close to, 10
wt% of mSi at 90 days. This is due to the hydration reactions and
to the pozzolanic activity of the active additions in general. In

Fig. 3. Frequency distribution of the pores in ternary mixtures with mSi and nSi at
7 days of curing.

particular, for mixtures with an addition of nSi, these can facilitate

the nucleation of hydrated cement crystals which makes them
Fig. 1. Frequency distribution of the pores in binary mixtures with nSi at 7 days of more active [15,27]. As for the amount of addition, Ghafari et al.
curing. [16] confirm that the optimum amount of cement replacement
98 J. Massana et al. / Construction and Building Materials 165 (2018) 93–103
Fig. 4. Frequency distribution of the pores in binary mixtures with nSi at 28 days of
curing.
Fig. 5. Frequency distribution of the pores in binary mixtures with mSi at 28 days
of curing.
by nSi in cement paste to achieve the highest compressive strength
was 3 wt%. However, in this work, the increase in compressive
strength continues up to 7.5 wt% addition of nSi, with a value of
70.35 MPa. This mixture does not show significant differences with
the ternary mixtures, except with HPSCC [nmSi]-2.5/2.5, in which
the maximum value of compressive strength (82.17 MPa) is
obtained. This may be because there is a better packaging in the
case of using ternary mixtures [10,25,35]. In spite of this, the
results of compressive strength provided by this work are lower
than those obtained by Jalal et al. [25], which acquire concrete of
80 MPa of compressive strength with 2 wt% of replacement for
nSi at 28 days. Similar values are reported by Yu et al. [36] that
obtain ultra-high strength concrete with compressive strength of
88 MPa at 28 days with a 4 wt% addition of nSi and with high
superplasticizer (SP) contents, although these concretes were rein-
forced with steel fibres. The differences between the results
obtained in this work and of Jalal et al. [25] may be due to the for-
mation of air bubbles inside the hardened concrete. Yu et al. [36]
tested high-performance concretes with contents of nSi between
Fig. 6. Frequency distribution of the pores in ternary mixtures with mSi and nSi at
28 days of curing.
Fig. 7. Frequency distribution of the pores in binary mixtures with mSi at 90 days of
curing.
1 wt% and 5 wt% and with a constant amount of SP. They obtained
an exponential increase in the content of entrained air as the
amount of nSi became greater, despite the use of SP based on poly-
carboxylates. This type of SP produces pores of smaller diameter to
the ones in the case of SP based on lignosulfonates or naphthalenes
[34].
3.2. Microstructural characterisation by Mercury Intrusion
Porosimetry (MIP)
Figs. 1–3 show the frequency distribution of the pores for the
mixtures studied, at seven days of curing.
Figs. 4–6 show frequency distribution of the pores for the mix-
tures studied, at 28 days of curing.
Figs. 7–9, show the frequency distribution of the pores for the
mixtures studied, at 90 days of curing.
Table 5 shows total porosity, macro and micro pores percent-
ages and critical pore diameters values for all mixtures. In this
 J. Massana et al. / Construction and Building Materials 165 (2018) 93–103
Fig. 8. Frequency distribution of the pores in binary mixtures with nSi at 90 days of
curing.
Fig. 9. Frequency distribution of the pores in ternary mixtures with mSi and nSi at
90 days of curing.
work macro pores are considered those with a diameter larger than
50 nm in width according to IUPAC, 1984 [37].
The figures of frequency distribution of the pores show that the
use of nSi and mSi could have a positive effect on modifying the
internal pore structure at all ages and in all mixtures as compared
to the reference mixture (HPSCC). Specifically, in mixtures with
mSi, there is a slight refinement of the pore structure at seven days,
which evolves with a decrease in the number of pores at 28 days
and continues to decrease until reaching 90 days. It is noteworthy
that, in Fig. 7, a clear reduction in the number of pores (see total
porosity in Table 5) is observed that might be because a filling
effect of the addition, though the critical pore-size diameter is
increased. In Fig. 8, a different behaviour is observed. The nSi
causes a reduction in the critical pore diameter with 5 wt% and
7.5 wt% addiction mainly; though it is associated with a slight
decrease in the amount of total pores (observe micropores percent-
age in Table 5). In addition, there is a displacement of the pore-size
distribution diagram to the left. This effect might be caused by an
99
enhancement of the hydration process due to the high pozzolanic
activity of nSi addition regarding to its great surface/volume ratio.
This might cause the formation of higher amount of CSH gels and
gel pores, reducing the critical pore diameter. Both behaviours
occur at all ages and they are most significant at 90 days of curing.
In ternary mixtures overlap behaviour was deduced. This beha-
viour might be influenced by an enhanced hydration process due
to the presence of nSi addition, and the final packing efficiency
related to the continuity particle size distribution of the compo-
nents that intervene in the ternary mixture (see micropores
percentage and critical pore diameters in Table 5). For example,
at 28 and 90 days of curing, such an overlap is clearly noticeable
(see Fig. 9). There are both a refinement of the pore structure
and a smaller intruded volume. Fig. 10 shows frequency distribu-
tion of the pores of the mixtures with 5 wt% of nSi, mSi and
nmSi-2.5/2.5 wt%.
It can be seen that nSi reduces pore size and this result is con-
firmed by several investigations [16,28,32,38,39], while mSi
reduces the amount of pores without reducing the critical pore
diameter. The ternary mixture in Fig. 10 reduces both the amount
of pores and the critical pore diameter as compared with reference
mixture. This result is consistent with the maximum value of com-
pressive strength obtained for this mixture at 28 days. Nazari and
Riahi [33] studied the effect of different amounts of nSi when
incorporated into an SCC. They observed a refinement of the pore
structure, while Romero [2] specified only a decrease in pore size.
The high values of compressive strength obtained in the mix-
tures with additions of both nSi and mSi might be related to the
distribution and size of the pores and to the densification of the
matrix. The hydration process might be enhanced by the high
pozzolanic activity of nSi addition regarding to its great surface/
volume ratio and the final packing efficiency might be improved
by the continuity particle size distribution of the components in
the mixture. Both of these effects could improve the compactness
of the material, which would translate into higher mechanical
strength and lower porosity.
Fig. 11 shows values of total porosity of mixtures studied at 7,
28 and 90 days of curing.
Porosity is reduced over the curing time in every mixture with
mSi. Total porosity is low for mixtures with mSi, with extreme val-
ues between 9.09 and 5.67 for [mSi]-5–7 and 90 days respectively.
This behaviour might be attributed to the mSi addition ability to
only reduce the pores with large critical pore diameter. Total
porosity values are inconclusive in the mixtures with nSi, although
the tendency is to a reduction with curing time. However, amount
of micro-pores in all the mixtures with this addition is greater than
the one obtained by the mixtures with mSi. Ternary mixtures have
a range of total porosity values between 9.65 and 7 days in the
mixture [nmSi]-5/2.5 and 7.13 at 28 days in the mixture [nmSi]-
2.5/5, value held at 90 days. In these, the critical pore size is similar
to the mixtures with nSi.
It is worth noting that mixtures with nSi demanded particularly
high amount of SP. This produces a large number of bubbles in
fresh state, many of which remain retained inside the mixture in
hardened state. The presence of air voids inside the material might
exert influence in the mechanical and durability behaviour of the
material. Nevertheless, these spherical bubbles are not intercon-
nected neither accessible from the outside, so cannot be character-
ized by MIP.
3.3. Durability properties
3.3.1. Carbonation depth
The results obtained revealed that the concrete produced show
no any depth of carbonation after 60 days of exposure to CO2
which is the normalized time according to UNE-EN 13295:2005.
100 J. Massana et al. / Construction and Building Materials 165 (2018) 93–103

Table 5
Percentage of macro and micro pore and critical pore diameters values for all mixtures.

Mixes Days Total Porosity (%) Macro-pores (Ø > 50 nm) Micro-pores (Ø < 50 nm) Critical pore diameters (lm)
HPSCC 7 9.24 24.02 75.98 0.010
28 9.31 16.83 83.17 0.008
90 8.68 27.88 72.12 0.015
[nSi]-2.5 7 9.91 13.32 86.68 0.091
28 8.10 23.49 76.51 0.012
90 8.32 25.54 74.46 0.010
[nSi]-5 7 8.34 8.60 91.40 0.007
28 9.03 13.05 86.95 0.007
90 8.07 13.33 86.67 0.007
[nSi]-7.5 7 9.98 8.49 91.51 0.006
28 7.43 11.87 88.13 0.007
90 8.34 27.71 72.29 0.008
[mSi]-2.5 7 9.00 15.31 84.69 0.008
28 7.15 21.63 78.37 0.010
90 6.86 38.60 61.40 0.019
[mSi]-5 7 9.09 15.07 84.93 0.009
28 6.97 27.03 72.97 0.010
90 5.67 43.15 56.85 0.032
[mSi]-7.5 7 8.36 18.88 81.12 0.009
28 7.34 16.32 83.68 0.008
90 5.92 36.08 63.92 0.018
[nmSi]-2.5/2.5 7 9.18 15.96 84.04 0.008
28 7.36 21.40 78.60 0.007
90 8.40 25.56 74.44 0.009
[nmSi]-5/2.5 7 9.65 10.87 89.13 0.007
28 8.61 14.08 85.92 0.007
90 7.38 15.26 84.74 0.050
[nmSi]-2.5/5 7 8.83 9.34 90.66 0.007
28 7.13 12.73 87.27 0.007
90 7.14 27.13 72.87 0.009

Service life calculation could be adopted using an equation pro-

vided by EHE [31]

t ¼ d  K 2
2
c ð1Þ

t: time expressed in years

d: carbonation depth in mm
Kc: carbonation coefficient

According to this model, if a carbonation depth of 1 mm after

Fig. 10. Frequency distribution of the pores of the mixtures with 5 wt% nSi, 5 wt%
mSi and 2.5/2.5 wt% nSi/mSi at 90 days of curing.
Fig. 12 shows the surface of concrete specimens treated with phe-
nolphthalein solution after 200 days of exposure to CO2.
None of the concretes studied exhibited carbonation.
Mohammed et al. [14] obtained similar results by subjecting SCC
specimens with mSi to accelerated carbonation after 28 days of
curing. They claimed that the addition of mSi could have a positive
effect on modifying the internal pore structure of SCC, especially at
the micro scale level, while it had a negative effect on the connec-
tivity of the capillary pores after a complete carbonation.
365 days of exposure to CO2 is achieved, the carbonation coeffi-
cient Kc would be 1 and the time required to reach a carbonation
depth of 20 mm in the concretes studied (the minimum cover to
the reinforcement in EHE-08 [31] would be 400 years. Therefore,
based on the results of the accelerated carbonation test obtained
in this work and the above assumption, the estimated service life
for a concrete produced would be even longer, given that the prop-
agation time to initiate corrosion should be added.
3.3.2. Freeze-thaw resistance
The expected freeze-thaw resistance of the concretes with
admixtures studied is marked as improved in comparison with
the reference concrete. Table 6 shows the loss of material mass
due to scaling per unit surface after 6, 14 and 28 cycles. As shown
in Table 6 the amount of scaling per unit surface area due to 6 and
14 freeze-thaw cycles are not very significant. Table 7 shows the
percentage of increase in loss of material mass due to scaling
regarding the reference concrete after 28 cycles.
As can be observed, the concretes with nSi showed significant
differences with respect to the reference concrete, reducing the
loss of material by up to 92.38% in the case of the mix with 7.5
 J. Massana et al. / Construction and Building Materials 165 (2018) 93–103 101

Fig. 11. Total porosity of studied mixtures at 7, 28 and 90 days of curing.

Fig. 12. Result of carbonation test after 200 days of exposure to CO2.

Table 6 influenced by the amount of superplasticizer added to the mixture.

Loss of material mass per unit surface area due to scaling after 6, 14 and 28 freeze- SP might produce a large quantity of bubbles inside the concrete,
thaw cycles. which may show a similar behaviour to the air voids formation
Cycles (n) Sn (kgm2) produced by an air-entrainment additive. The formation of uncon-
nected spherical small size air bubbles allow the water embedded
6 14 28
inside to expand when it freezes without causing interstitial
HPSCC 0.004 0.047 0.506
pressure inside the material [19,40].
[nSi]-2.5 0.014 0.037 0.186
[nSi]-5 0.008 0.024 0.086
[nSi]-7.5 0.004 0.011 0.039
[mSi]-2.5 0.006 0.122 0.423 3.3.3. Capillary absorption
[mSi]-5 0.006 0.052 0.237 Fig. 13 shows the capillary suction coefficient of concretes stud-
[mSi]-7.5 0.007 0.046 0.171 ied at 28 days of curing.
[nmSi]-2.5/2.5 0.005 0.013 0.086
It is worth noting that this parameter is proportional to the loss
[nmSi]-5/2.5 0.001 0.006 0.072
[nmSi]-2.5/5 0.002 0.014 0.092 of material due to scaling found in the freeze-thaw test (see
Table 5). This means that the concrete with nSi addition absorbs
the lower amount of water, and therefore the mixtures with the
wt% of nSi. In the case of concretes with mSi, while there was a lower quantity of ice during freezing can be maintained. As a con-
reduction of the loss of material it was to a lesser extent as sequence, these mixtures will be subjected to less internal tensile
compared with nSi addition. Lastly, the concretes with nSi and stresses, resulting less micro-cracking and loss of material weight.
mSi combination showed a behaviour influenced by the nSi addi- This result is in agreement with those obtained by Leung et al. [35].
tion only, presenting less scaling as the amount of nSi was greater. However, in their work they used fly ash and silica fumes which
This excellent result against freeze-thaw cycles was possibly also significantly reduced the surface water suction of SCC.

Table 7
Percentage of increase of loss of material mass due to scaling at 28 cycles respect to the reference concrete.

[nSi]-2,5 [nSi]-5 [nSi]-7,5 [mSi]-2,5 [mSi]-5 [mSi]-7,5 [nmSi]-2,5/2,5 [nmSi]-5/2,5 [nmSi]-2,5/5

63.27 82.91 92.38 16.30 53.05 66.11 82.95 85.76 81.81
102 J. Massana et al. / Construction and Building Materials 165 (2018) 93–103
Fig. 13. Capillary suction coefficient in concrete studied at 28 days.
4. Conclusions
All the mixtures studied complied with the requirements to
be classified as HPSCCs, only by controlling the quantity of super-
plasticizer additive. In addition, it was deduced that the quantity
of nSi and the demand of the superplasticizer additive are
proportional. However, the use of superplasticizer additive pro-
duces bubbles directly proportional to the additive quantity
incorporated. These bubbles are voids inside the mass that could
cause concentration of stresses that would lead to a loss of
mechanical strength.
The use of mineral admixtures of both mSi and nSi increases
the compressive strength of SCCs: the greater the admixture
quantity, the greater the compressive strength. However, the
increment is larger when nSi is used. Moreover, it is possible
to ascertain that the highest compressive strength is achieved
when the self-compacting compounds have a continuous
particle size distribution from the smallest particle size, addition,
to the largest one, coarse aggregate. In this paper, such a condi-
tion is improved by the use of nSi and mSi in ternary mixtures.
This wider particle size distribution creates a low porosity,
improves packing density (and thus compactness), decreases
water demand in comparison with mixtures with the same
amount of total addition using only nSi and, therefore, provides
higher compressive strength and an improved durability
performance.
The use of nSi, or the combination of nSi and mSi in the mix-
tures studied produced concretes with a high compactness and,
therefore, improved durability properties. This leads to less suscep-
tibility to carbonation, freeze-thaw cycles and a lower capillary
absorption that might prevent the penetration of aggressive
agents, leading to increase life span of concrete produced.
The improvement in mechanical and durability behaviour
achieved with nSi is related to the pore refinement due to the poz-
zolanic reaction and the packing effect. The pore size reduction
was proportional to the amount of nSi. In the case of concretes
with mSi, the microstructure produced had a lower total porosity
with an average pore size similar to the reference concrete without
addition. Lastly, in ternary mixtures the pores network obtained is
a result of the combination of both effects, producing concretes
with a small average pore size, proportional to the amount of
nSi, and with a smaller total porosity proportional to the amount
of mSi.
Acknowledgements
The authors wish to express their gratitude to the Ministerio de
Ciencia y Tecnología (Spain), project MAT2013_48009_C4_4_P for
financial support received.
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