j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 3 ; 2 4 : 7 4 4 4 e7 4 6 1

Available online at www.sciencedirect.com

journal homepage: www.elsevier.com/locate/jmrt

Original Article

Properties of sustainable high-strength concrete

containing large quantities of industrial wastes,
nanosilica and recycled aggregates

Ibrahim Y. Hakeem a, Mohammad Alharthai a, Mohamed Amin b,

Abdullah M. Zeyad c, Bassam A. Tayeh d,*, Ibrahim Saad Agwa b,e
a
Department of Civil Engineering, College of Engineering, Najran University, Najran, Saudi Arabia
b
Civil and Architectural Constructions Department, Faculty of Technology and Education, Suez University, Egypt
c
Civil Engineering Department, Faculty of Engineering, Jazan University, Jazan, Saudi Arabia
d
Civil Engineering Department, Faculty of Engineering, Islamic University of Gaza, P.O. Box 108, Gaza Strip,
Palestine
e
Civil Engineering Department, El-Arish High Institute for Engineering and Technology, El-Arish, North Sinai, Egypt

article info abstract

Article history: This research aims to study the effect of adding nanosilica (NS) on the properties of sus-
Received 14 February 2023 tainable high-strength concrete (SHSC). The SHSC was produced using recycled aggregates
Accepted 5 May 2023 from concrete debris as a 100% alternative to coarse aggregate, and industrial waste was
Available online 9 May 2023 used as supplementary cementitious materials at 50% and 75% of Ordinary Portland
cement (OPC) weight. A total of 25 mixes, including control mix (The first mix was made as
Keywords: the reference by using only cement without replacement materals), binary mixes (OPC and
Nanosilica fly ash (FA)), ternary mixes (OPC, FA and ground-granulated blast-furnace slag (GGBS)) and
Sustainable concrete quaternary mixes (OPC, FA, GBFS and silica fume (SF)) were developed. The dosage of NS
Recycled aggregate was 0%, 1%, 3% and 5% by binder ratio. The fresh properties of SHSC were evaluated by
Industrial waste slump test, and the mechanical properties were assessed by testing the compressive
Quaternary blended cement strength, splitting tensile strength, flexural strength and modulus of elasticity. The
Transport properties transport properties were evaluated by water permeability, water sorptivity and chloride
Mechanical properties permeability tests. Results showed that compared with the reference mixture, the SHSC
containing 75% of the quaternary blends with 3% NS achieved enhanced mechanical
properties at 28 and 91 days, indicating that this mixture can achieve the highest sus-
tainability performance. The SHSC mixture containing 3% NS and 50% quaternary mixtures
achieved the highest performance of 80.7, 6.46 and 10.09 MPa for compressive strength,
split tensile strength and flexural strength, respectively, at 28 days. This SHSC mixture also
achieved water permeability; chloride permeability was 2.54
1011 (cm/sec) and 1370
coulombs at 28 days.
© 2023 The Author(s). Published by Elsevier B.V. This is an open access article under the CC
BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/).

* Corresponding author.
E-mail address: [email protected] (B.A. Tayeh).
https://doi.org/10.1016/j.jmrt.2023.05.050
2238-7854/© 2023 The Author(s). Published by Elsevier B.V. This is an open access article under the CC BY-NC-ND license (http://
creativecommons.org/licenses/by-nc-nd/4.0/).
 j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 3 ; 2 4 : 7 4 4 4 e7 4 6 1 7445

the sustainable development environment. These recom-

Nomenclature mendations include (1) increasing the reliance on supple-
mentary cementitious materials (SCMs) to reduce cement
Acronyms Definition consumption; (2) using industrial by-product waste as partial
NS Nanosilica or total substitutes for cement; (3) increasing the reliance on
SHSC Sustainable high-strength concrete recyclable materials, for example, using construction de-
OPC Ordinary Portland cement molition waste to produce aggregates; (4) improving the
FA Fly ash strength and durability of concrete (e.g. high-strength con-
GGBS Ground-granulated blast-furnace slag crete and high-performance concrete) to reduce material
SF Silica fume consumption and increase the operational life of concrete
SCMs Supplementary cementitious materials structures; (5) using treated wash water to produce and cure
XRD X-ray diffraction analysis concrete [13]. The sustainable production of concrete is
SEM Scanning electron microscope critical in reducing cement content, absorbing industrial
RCAs Recycled concrete aggregates waste and alleviating environmental and industrial burdens
SP Superplasticizer due to disposal costs and pollution problems [18,19]. Many
ITZ Interfacial transition zone industrial wastes have cementitious or pozzolanic proper-
ties, which encouraged researchers to use them as a partial
substitute for cement in quantities up to 75% by weight
[20e25]. FA is a by-product of coal combustion in coal power
plants. It mostly consists of SiO2 and possesses pozzolanic
1. Introduction properties that can react with Ca(OH)2 to make additional
binding products, such as CeSeH gel [26e29]. Therefore, FA is
Concrete is currently the most widely used product world- one of the most widely used industrial wastes in
wide because of the rapid global urban development in con- manufacturing raw cement or as a partial substitute for
struction, thereby increasing the demand for concrete [1,2]. cement in the cement concrete industry [30e32]. SF is an
In addition, the production cost of concrete is low, the com- industrial waste by-product of ferrosilicon alloy and silicon.
plex elements are easy to form, and the durability is high. The proportions of silica (SiO2) range from 90% to 99% by
Concrete production is mainly based on using Portland weight, and the surface area ranges from 13,000 m2/kg to
cement as a binder [3,4]. The annual global consumption of 30,000 m2/kg [33,34]. GBFS is a powder resulting from the
concrete is nearly 10 billion m3 meters. The production of grinding and softening of industrial waste (furnace slag) and
this amount requires approximately 3.8 Gt of cement, 17.5 Gt a by-product of smelting metal ores (e.g. iron, copper and
of aggregate and more than 2 Gt of water [5]. In 2018, global nickel). GBFS is mainly formed of SiO2, CaO and Al2O3. It also
cement production reached a record level of 4.1 Gt [6]. has the property of pozzolana, which enables it to react with
Therefore, the Portland cement industry consumes much cement hydration products. Nano silica (NS) or silica nano-
energy, as it needs high temperatures of up to 1450  C. The particles have an average diameter of 50 nm [35]. The nano-
consumption of nonrenewable natural resources, such as particles of NS are produced on a large scale through
limestone (CaCO3), and the process of burning limestone chemical synthesis [36]. NS can reach and fill the smallest
release CO2, which is added to the carbon dioxide produced pores and enhance the microstructure of concrete; it can
by the combustion of fossil fuels [7,8]. Producing one ton of react Ca(OH)2 to produce a CeSeH gel. Nanomaterials (e.g.
clinker emits more than 0.9 tons of carbon dioxide equiva- NS) in concrete production have recently gained importance
lent. According to environmental studies, cement production because of concrete's characteristics in the fresh and hard-
is responsible for 7%e10% of total global CO2 emissions [9,10]. ened stage [37]. Previous research indicates that using NS as a
Concrete production consumes natural resources, including partial substitute for 0%e6% cement enhances the strength
rocks for coarse and fine aggregate production. On the con- and durability of HSC. Moreover, the concrete combined with
trary, construction demolitions are carried out because of NS has a dense and compact microstructure with a minimal
urban development or deterioration. According to available amount of calcium hydroxide crystals [38e42]. In addition, a
statistics, Europe alone produces the equivalent of 859 number of studies examined the potential use of NS in
million tons of building demolition waste [11]. Construction various types of concrete. Aydin et al. [43] discovered that
demolition waste comprises 40% concrete, 30% tiles and ce- self-compacting concrete containing 2% NS, 0.08% nano-
ramics and 30% mixtures of other components [12]. Global carbon, and 40% FA performed better than NS-free admix-
industries produce huge amounts of other solid wastes as by- ture. Naniz and Mazloom [44]reported that replacing 3% of
products. These wastes can be harmful to humans and the the cement weight with NS improved the fresh and hardened
environment if not treated and deposited properly [13]. properties of concrete at various water-to-binder ratios. The
Various industries produce many kinds of solid wastes, such research conducted by Mohamed and Adamu [45] demon-
as fly ash (FA), silica fume (SF), granulated blast furnace slag strated that the use of 1%, 2%, and 3% NS as an alternative to
(GBFS) and metakaolin. These environmental problems have cement improved the microstructure, strength, and dura-
prompted researchers and scientists to look for other ways to bility of the concrete. It has been reported that some nano-
produce environmentally friendly and sustainable concrete particles helped optimize the CeSeH structure and improve
[14e17]. Several recommendations are made to produce the microstructure of both matrix and complex ITZs in RAC
sustainable concrete that complies with the requirements of [46,47]. Nanomaterials can suppress micro-cracks and
7446 j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 3 ; 2 4 : 7 4 4 4 e7 4 6 1

enhance contact between hydration products [48]. This is due

to the mechanism of action of NS in improving the properties 2. Experimental program
of concrete by accelerating the hydration rate when
compared to free-NS. NS significantly contributes to the 2.1. Materials
consumption of CH and thus the production of additional
CeSeH [49]. Nanomaterials also improve the dissolution of In this study, the OPC used was CEMI 52.5 N, with a specific
alumina phases and the precipitation of ettringite. The NS gravity of 3.17, and carried out as BS EN197/1e2011 [63]. The SF
also helps as a nucleation site for the creation of hydration utilized was made locally in Egypt., has a silica content of
products directly on their surfaces. The nucleation effect is 97.5%, a specific gravity of 2.15, a light grey colour and a spe-
more pronounced as particle size decreases [50]. However, as cific surface area of 20000 cm2/gm. As a high siliceous mate-
a result of its role in the clear early ages, the effect of nano- rial, the SF used follows the requirements of ASTM C1240 [64].
material nucleation decreased rapidly at late ages. On the FA is a byproduct produced by coal-fired power plants. FA
nanon scale, the NS is also important in the effect of packing comprises low calcium oxide and high silica and aluminium
and void filling [51,52]. As previously stated, the typical par- oxide contents, confirming it as a class F, based on ASTM
ticle size of nanomaterials ranges from 5 nm to 50 nm, which C618-12a [65]. The FA used has a specific gravity of 2.37, a light
is much smaller than the particle size of cement (10 m). Ul- grey colour and a particular surface area of 8150 cm2/gm. The
trafine nanoparticles can fill micro-voids and cracks in a GBFS from the steel industry wastes was got from rapid
matrix and improve its microstructure. This increases cooling by water (Helwan Steel factory, Cairo, Egypt). The
strength while decreasing permeability by obstructing fluid physical properties and chemical composition of OPC, SF, FA
paths or forcing them to tilt and turn around [47,53,54]. and GBFS are shown in Table 1. The NS was synthesised in the
The use of NS material in sustainable concrete with a high science laboratory of Beni Suef University, Egypt. NS is
replacement of cement content (up to 50% of the cement chemically prepared by using magnetic stirrer and adding HCl
weight) is essential to overcome low strength and delay in to sodium silicate solution (1000 ml) till reaching PH equal 8e9
setting time [55]. The interest in using multiblend cement has and NS gel is produced, then the steps are followed to obtain
increased because of the performance of the combination of pure silica as follow 1) distilled water is added and waiting till
more than two types of blends with cement. Ternary blends sedimentation, 2) filtration and repeat washing step several
(OPC with two or more SCMs) achieve high cement replace- times to get separate salt water and make sure by AgNO3 3)
ment ratios, enabling sustainable green concrete production drying silica in oven at 105  C, 4) finally particles are burnet at
[56]. Some previous studies revealed the importance of 600 0C for 2 h (1). The properties of NS are shown in Table 2.
ternary blends to reduce the cement content whilst main- The X-ray diffraction analysis (XRD) and scanning electron
taining the high performance of concrete [57]. The common microscope (SEM) images of NS are shown in Fig. 1.
ternary blend systems for sustainable concrete production The fine aggregate utilized in this study is Egyptian sand
include SF, FA or GGBS [58,59]. Multiple-blend systems have from the Belles region. It is a clean and rounded fine aggregate,
shown that the benefits of two or more blends can be exploi- measuring 0.15 mme4.75 mm. The maximum sizes of recy-
ted to overcome the low act of a binary or single-blend system. cled concrete aggregates (RCAs) are 4.75 and 19 mm. The RCAs
Therefore, compared with single alternatives, multiple-blend with 4.75/19 mm (see Fig. 2) grading were used in the experi-
systems (two or more blends) can improve operability and mental work; they were extracted from the failure and
environmental performance whilst maintaining high-level
strength and durability [60,61]. Rivera et al. reported that
ternary blended concrete shows a synergistic effect between Table 1 e Properties of OPC, FA, FA, GBFS, and SF.
blends, which improves compressive strength at later ages Properties OPC FA GBFS SF
[62]. Physical
However, studies focusing on the effect of quaternary and Specific gravity 3.14 2.32 2.61 2.14
pentagonal multiblend cement on sustainable high-strength Initial setting time (min) 60
concrete (SHSC) are limited. As far as we know, studies on Final setting time (min) 305 e e e
the effect of quaternary cement blends with NS at replace- Specific area (cm2/gm) 3540 7985 6250 19930
Color Grey Light Grey Yellow Light Grey
ment rates of up to 75% of the Ordinary Portland cement (OPC)
Chemical compositions (%)
weight on sustainable concrete containing coarse recycled SiO2 21.14 54.45 35.63 98.80
concrete aggregate (RCA) are lacking. Therefore, the novelty of Al2O3 4.75 27.36 12.78 0.13
this study lies in the investigation of the effect of adding 1%, Fe2O3 3.23 5.57 1.26 0.20
3% and 5% NS to a quaternary cement blend of CaO 62.91 5.95 40.10 0.14
OPC þ FA þ GBFS þ SF at substitution ratios of 50% and 75% of MgO 3.05 1.88 6.28 0.15
SO3 2.59 0.29 2.17 0.06
OPC weight on the SHSC containing 100% RCA. This study
K2O 0.76 1.84 0.39 0.10
explores the effect of adding 1%, 3% and 5% NS on the prop-
Na2O 0.58 0.93 0.25 0.06
erties of SHSC with binary (OPC þ FA), tertiary TiO2 0.18 0.75 0.81 0.02
(OPC þ FA þ GBFS) and quaternary (OPC þ FA þ GBFS þ SF) Cr2O3 0.05 e e e
cement blends. In this study, fresh and mechanical properties MnO 0.06 e e e
were tested at the ages of 1, 7, 28 and 91 days, and transport CI 0.03 e e e
properties were tested at 28 days. Loss on Ignition (LOI) 0.67 0.98 0.33 0.24
 j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 3 ; 2 4 : 7 4 4 4 e7 4 6 1 7447

researchers were considered to control the addition ratio of

Table 2 e The physical properties of NS.
nanomaterials. The suitable content of NS is 1% and 3%
Properties NS [79e82]. The dosage of NS was 0%, 1%, 3% and 5% by binder
Form Powder ratio. The RCA preparation employed in this study followed
Particle size 15 ± 5 nm the method proposed by Amin et al. and Guo et al. [83,84]. The
Color White present research focuses on fully replacing the RCAs, SCMs
Formula SiO2 (99.0%)
and OPC with a combination of FA, GBFS and SF. The SHSC
Molecular Weight 60.04 (g/mol)
mixtures with different combinations of variable percentages
Melting point 1620 ( C)
Boiling point 2250 ( C) of RCAs and other binding materials were prepared [84e86].
Density 2.2e2.5 (g/cm3) The replacement ratio of RCAs was 100%. The replacement
Specific gravity 2.25 levels of SCMs were 50% and 75% by weight of OPC. A total of
Water solubility Insoluble 25 mixes, including control mix (The first mix was made as the
reference by using only OPC without replacement materals),
crushing of the concrete [66e68] and classified as type 1 ag- binary mixes (OPC and FA), ternary mixes (OPC, FA and GBFS)
gregates in accordance to the standard of NF EN 933e11 [69]. and quaternary mixes (OPC, FA, GBFS and SF) were developed.
The RCAs were manually crushed into small sizes using a The design parameters and mix proportions of all mixes are
hammer. They were placed in the Los Angeles abrasion ma- summarised in Table 4.
chine with 12 steel balls, and the machine rotated until the
required particles were formed. The third step of the crushing 2.3. Specimen preparation
process was the sieving of the laboratory RCAs to maintain a
gradation similar to the natural coarse aggregate A rotary mixer was used to mix various materials for all mixes.
(NMAS ¼ 19 mm). The properties of aggregates in accordance The mixing of materials included four steps: In the first step, a
to ASTM C33/C33M  18 [70] and ECP 203e2017 [71]. Table 3 method for dispersing effective NS was used [81,87]. NS was
presents the physical and mechanical properties of aggre- added into the beaker with 50% water. The beaker was sub-
gates. Fig. 3 depicts the grading curve of the aggregates used. merged for 10 min in a water-filled ultrasonic device. In the
Both fine and coarse RCAs were used in saturated surface and second step, the fine and coarse aggregates and the OPC and
dry conditions. Superplasticiser (SP), which is commercially SCMs were added into the mixer and dry mixed for around
available, was used to improve the workability and consis- 3 min. In the third step, the NS with 50% of the water was
tency of fresh concrete. According to [41,42], the SP used in placed into the mixer and mixed for another 2 min. At the last
this study, with a specific gravity of 1.1 and a colour of clear step, the SP and the last 50% of the water were mixed. Then,
liquid, meets the requirements. Eight materials were used as they were added into the mixtures and mixed for 3 min until a
illustrated in Fig. 4 to develop SHSC. homogeneous mixture was obtained. For each mixture, the
mixing process was repeated. All concrete specimens were
2.2. Mix proportions cast in steel moulds and vibrated with a table vibrator. All
mould specimens were kept in a room with a temperature of
In the current study, twenty five mixes were designed (20 ± 2)  C and relative humidity of 95% for 24 h before being
accroding to absolut volume and presented in Table 4. The demoulded and cured in a room with the standard condition
control SHSC was considered to accomplish compressive until the day of testing per ASTM C192 [88].
strength at 28 days about 60 MPa with a large amount of
cement [72,73]. Based on, cementitious content of 500 kg/m3 2.4. Testing
was adopted to all mixes [74e76]. All the SHSC was prepared
with a water to binder (w/b) ratio of 0.25 and 3% of SP from the The ASTM C 143 [89] slump test was used to determine if fresh
binder ratio [77,78]. concrete was workable. Fig. 5 presents an illustration of some
The fine aggregate to coarse aggregate ratio was 40%:60%. tests conducted in the present study in addition to failure
In this study, the optimised mix ratios of numerous shape of concrete after test. The mechanical properties (i.e.

Fig. 1 e Nano silica used: a: XRD, and b: SEM.

7448 j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 3 ; 2 4 : 7 4 4 4 e7 4 6 1

Table 3 e Physical and mechanical properties of

aggregates.
Property Sand RCA
Specific gravity 2.65 2.70
Unit weight (kg/m3) 1670 1640
Fineness modulus 2.53 6.21
Water absorption (%) 0.76 4.26
Clay and fine materials (%) 1.14 1.23
Elongation index (%) e 18.3
Flakiness index (%) e 19.2
Impact value (%) e 17.1
Crushing value (%) e 15.2
Los Angles abrasion loss (%) e 21.5

the changes in the added NS (0.0%, 1.0%, 3.0% and 5.0%,

respectively, by weight of OPC). Therefore, when NS was used
to add OPC, the large specific surface area of the NS caused a
Fig. 2 e Recycled concrete aggregate used.
huge amount of water in the mixture to be absorbed by the NS
particles. The water for lubrication in the mixtures was
insufficient, and the particles in the mixture could not move
compressive strength, flexural strength, splitting tensile
freely, decreasing the workability of the concrete mixture
strength and modulus of elasticity) of the hardened SHSC
[96,97].
mixtures were determined. For each SHSC mix, three 100 mm
cubes were produced to determine cube compressive strength
3.2. Mechanical properties
at the ages of 1, 7, 28 and 91 days, according to BS EN 12390
[90]. The splitting tensile test was performed on a
3.2.1. Compressive strength
150
300 mm cylinder at 28 days according to ASTM C 496 [91].
The compressive strength results of the SHSC mixtures con-
The flexural strength test was executed on three beams with a
taining OPC/SCMs (C/SCMs) of 250/250 kg/m3 with 100% RCA
dimension of 500
100
100 mm at the age of 28 days, based
at 1, 7, 28 and 91 days are shown in Fig. 7. The results showed
on ASTM C 78 [26]. Furthermore, 150
300 mm cylinders were
the changes in the compressive strength of the SHSC concrete
used to determine the modulus of elasticity at 28 days ac-
samples due to the changing the ratios of materials used from
cording to ASTM C 469 [92].
FA, GBFS and SF. The reference mixture (500CN0) achieved a
The chloride penetration resistance at 28 days was also
compressive strength of 28.8, 53.2, 70.9 and 77.9 MPa at 1, 7, 28
determined on a 100
50 mm cylinder by using the test in the
and 91 days, respectively. In addition, the inclusion of FA as a
ASTM C 1202 [93]. The water sorptivity test was performed on
partial substitute at 50% of OPC weight decreased the
a 100
50 mm cylinder at 28 days based on the test described
compressive strength to 23, 47, 64 and 73.6 MPa at the test ages
in ASTM C1585 to determine the water absorption rate [94]. At
of 1, 7, 28 and 91 days, respectively. The results also showed
28 days, the water permeability test was performed on a
that compared with the mixture free of NS (250CFN0), the SHSC
150 mm 150 mm cylinder, based on BS EN 12390e8 [95].
mixtures with NS exhibited improved compressive strength at
all ages of the test. An increase in the percentage of NS in

3. Results and discussion

The test results of the slump, compressive strength, splitting

tensile strength, flexural strength and modulus of elasticity
are shown in Table 5.

3.1. Slump

The effect of NS and replacing OPC with FA, GBFS and SF on

the slump of fresh SHSC is presented in Fig. 6. Increasing the
OPC replacement content of FA, GBFS and SF led to a reduced
slump, which was high for the mixtures containing NS. The
slump results were obtained between 100% (500CN0) and
78.74% (125CFGSN5). The slump results of SHSC without NS
were 96.85%, 94.49%, 91.34%, 93.70%, 91.34% and 88.19% for
250
CFN0, 250CFGN0, 250CFGSN0, 125CFN0, 125CFGN0 and
125
CFGSN0, respectively. The slump results of the SHSC mix-
tures decreased by increasing the NS. For instance, the slump
values of 125CFGSN were 112, 109, 104 and 100 mm because of Fig. 3 e Grading curve of aggregates.
 j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 3 ; 2 4 : 7 4 4 4 e7 4 6 1 7449

Fig. 4 e Materials used in this study.

250
CFN0, 250CFN1, 250CFN3 and 250CFN5 mixtures increased the properties at the later ages of 28 and 91 days. Some re-
compressive strength to 64, 71.2, 76.1 and 72.1 MPa, respec- searchers indicated a synergistic interaction in the ternary
tively, at the test age of 28 days. Compared with the SHSC blended cement, which achieves positive results and reduces
mixtures with 1% and 5% NS, the SHSC mixture with 3% NS of cement content [62,98].
the cementitious weight achieved the highest compressive Compared with the mixture containing FA as a partial
strength (88.3 MPa at 90 days). Accordingly, the obtained re- replacement by 50% of OPC weight, the mixture with GBFS and
sults confirmed the positive role of adding the NS in enhans- FA as partial replacements by 50% of OPC weight exhibited a
ing the compressive strength at the early age (1 day) and late slight decrease in the compressive strength. On the contrary,
age (91 days). These results agreed with the previous studies including NS in addition to FA and GBFS contributed to an
indicating that the optimum proportions for the addition of improve in the compressive strength of the SHSC.
NS range from 1% to 6% of the weight of cementitious mate- The addition of Nan-Si improved the compressive strength
rials [38e40]. of the SHSC samples 250CFGN0, 250CFGN1, 250CFGN3 and
250
Compared with the single reaction of OPC and the binary CFGN5 to 60.2, 66.9, 71.5 and 68.1 MPa, respectively, at the
synergistic reaction of OPC and FA, the synergistic reaction of test age of 28 days. The improvement in compressive strength
the ternary mixtures of OPC, FA and NS improved strength caused by the addition of NS may be attributed to its

Table 4 e Proportions of sustainable HSC mixtures Kg per 1 m3.

Mixes OPC Sand RCA FA GBFS SF NS SP Water
500
CN0 500 752.4 1128.6 0 0 0 0 15 125
250
CFN0 250 722.3 1083.4 250 0 0 0 15 125
250
CFGN0 250 728.7 1093.0 125 125 0 0 15 125
250
CFGSN0 250 725.4 1088.2 100 100 50 0 15 125
125
CFN0 125 707.2 1060.8 375 0 0 0 15 125
125
CFGN0 125 716.8 1075.2 187.5 187.5 0 0 15 125
125
CFGSN0 125 712.0 1068.0 150 150 75 0 15 125
250
CFN1 250 719.9 1079.8 250 0 0 5 15 125
250
CFGN1 250 726.3 1089.4 125 125 0 5 15 125
250
CFGSN1 250 723.1 1084.6 100 100 50 5 15 125
125
CFN1 125 704.8 1057.2 375 0 0 5 15 125
125
CFGN1 125 714.5 1071.7 187.5 187.5 0 5 15 125
125
CFGSN1 125 709.6 1064.4 150 150 75 5 15 125
250
CFN3 250 715.2 1072.7 250 0 0 15 15 125
250
CFGN3 250 721.5 1082.3 125 125 0 15 15 125
250
CFGSN3 250 718.3 1077.5 100 100 50 15 15 125
125
CFN3 125 700.1 1050.1 375 0 0 15 15 125
125
CFGN3 125 709.7 1064.5 187.5 187.5 0 15 15 125
125
CFGSN3 125 704.9 1057.3 150 150 75 15 15 125
250
CFN5 250 710.4 1065.6 250 0 0 25 15 125
250
CFGN5 250 716.8 1075.1 125 125 0 25 15 125
250
CFGSN5 250 713.6 1070.3 100 100 50 25 15 125
125
CFN5 125 695.3 1042.9 375 0 0 25 15 125
125
CFGN5 125 704.9 1057.4 187.5 187.5 0 25 15 125
125
CFGSN5 125 700.1 1050.2 150 150 75 25 15 125
7450 j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 3 ; 2 4 : 7 4 4 4 e7 4 6 1

Fig. 5 e SUHPC test setup (a) Compression test (b) Failure shape of concrete cube after compression test (c) Indirect tensile
test (d) Failure shape of concrete cylinder after indirect tensile test (e) flexural test, and (d) Failure shape of concrete beam
after flexural test.

Table 5 e Fresh and hardened properties of sustainable HSC mixtures.

Mixes Slump (mm) Compressive Strength Splitting Tensile Flexural Strength (MPa) Modulus of Elasticity (GPa)
(MPa) Strength (MPa)
1day 7day 28day 91day 28day
500
CN0 127 28.8 53.2 70.9 77.9 6.39 9.43 36.80
250
CFN0 123 23.0 47.0 64.0 73.6 5.38 8.24 34.98
250
CFGN0 120 22.3 45.2 60.2 68.1 5.18 7.84 33.96
250
CFGSN0 116 24.4 49.5 66.7 77.6 5.47 8.47 35.69
125
CFN0 119 17.1 37.6 51.5 60.0 4.43 6.68 31.43
125
CFGN0 116 18.9 40.8 54.9 62.5 4.83 7.20 32.41
125
CFGSN0 112 20.4 44.7 60.6 70.8 5.10 7.76 34.03
250
CFN1 120 26.0 52.2 71.2 82.2 5.91 9.10 36.90
250
CFGN1 116 25.1 49.8 66.9 76.0 5.69 8.64 35.77
250
CFGSN1 113 27.6 55.3 74.5 87.1 6.09 9.39 37.73
125
CFN1 115 19.2 41.5 57.1 66.9 4.86 7.35 33.12
125
CFGN1 112 21.4 45.3 61.2 69.8 5.32 7.97 34.23
125
CFGSN1 109 23.0 49.7 67.4 79.0 5.60 8.56 35.92
250
CFN3 114 27.7 55.8 76.1 88.3 6.24 9.66 38.13
250
CFGN3 112 27.2 53.2 71.5 81.5 6.01 9.17 37.01
250
CFGSN3 108 30.3 59.9 80.7 94.7 6.46 10.09 39.27
125
CFN3 111 21.1 43.7 61.2 72.0 5.14 7.83 34.28
125
CFGN3 107 23.2 48.3 65.3 74.8 5.62 8.43 35.29
125
CFGSN3 104 24.9 52.9 72.1 84.7 5.91 9.09 37.16
250
CFN5 110 26.9 53.2 72.7 84.7 5.89 9.15 37.31
250
CFGN5 107 25.9 50.6 68.1 78.0 5.65 8.66 36.15
250
CFGSN5 103 28.6 56.5 76.2 90.0 6.04 9.45 38.14
125
CFN5 106 20.8 42.8 58.7 68.7 4.87 7.44 33.60
125
CFGN5 103 22.4 46.4 62.6 71.7 5.32 8.02 34.65
125
CFGSN5 100 23.9 50.6 69.0 81.2 5.64 8.63 36.25
 j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 3 ; 2 4 : 7 4 4 4 e7 4 6 1 7451

Slump (mm)

Mixes

Fig. 6 e Results of slump flow of all mixes.

ultrafineness, which leads to a wide diffusion within the interaction between the pozzolanic materials, thereby
cement matrix, clog capillary pores and nanopores, and to the achieving enhanced properties. The effect of the synergistic
rapid reaction with Ca(OH)2 in the early cement hydration interaction in quaternary blends is greater than that in ternary
times [99]. and binary blends [100,101]. This finding was shown in the
The compressive strength of the concrete containing qua- results of the present study. Compared with zero NS, the in-
ternary blends (OPC þ FA þ GBFS þ SF) by 50% of OPC weight clusion of NS (OPC þ FA þ GBFS þ SF þ NS) by 1%, 3% and 5% of
was higher than that of the ternary blends (OPC þ FA þ GBFS) the OPC weight to the quaternary blend improved the
and binary blends (OPC þ FA) by 50% of OPC weight at all ages. compressive strength of the SHSC mixture by 112%, 122% and
The increase in compressive strength of the SHSC containing 116%, respectively, at the test age of 91 days. The positive ef-
SF by 10% of OPC weight was attributed to the early reaction fect of NS involved rich reactive SiO2, and the average particle
with Ca(OH)2 to form additional CeSeH. The compressive size was often less than 50 nm. Accordingly, NS could improve
strength of the quaternary blend with SF at the early age of 1 the microstructure properties of the concrete matrix; this
day and later ages was higher than that of the ternary and finding is positively reflected in the mechanical and durability
binary concrete blends. The compressive strength results for properties [102].
samples 250CFGSN0, 250CFGN0 and 250CFN0 were 73.6, 68.1 The compressive strength results of the SHSC mixtures
and 77.6 MPa, respectively, at the test age of 91 days. Previous containing C/CS of 125/375 kg/m3 with 100% RCA at the test
research indicated that the inclusion of SF in the ternary or ages of 1, 7, 28 and 91 days are shown in Fig. 8. The results
quaternary blends causes a considerable synergistic showed that compared with the reference mixture (OPC),
Copmressive strength (MPa)

Mixes

Fig. 7 e Compressive strength of the SHSC containing 250 kg/m3 OPC.

7452 j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 3 ; 2 4 : 7 4 4 4 e7 4 6 1

Copmressive strength (MPa)

Mixes

Fig. 8 e Compressive strength of the SHSC containing 125 kg/m3 OPC.

binary (OPC þ FA), ternary (OPC þ FA þ GBFS), or quaternary ternary mixtures to enhance compressive strength at the
(OPC þ FA þ GBSF þ FS) cement blends with the replacement early and late ages [103,104].
rate of 75% of OPC weight exhibited a decreased compressive Fig. 9 shows the compressive strength results of the SHSC
strength at all test ages. Compared with the zero NS mixtures, mixtures with C/CS content of 125/375 and 250/250 kg/m3 at
the mixtures with NS exhibited an improved compressive the test age of 28 days. The results presented in Fig. 9 showed
strength. NS emhanced the compressive strength of the qua- that the lowest compressive strength of the SHSC was
ternary mixtures (OPC þ FA þ GBFS þ FS) compared with that observed in the binary blend (OPC þ FA), indicating a reduc-
of the reference mixture (OPC) at a later age of 91 days. The tion of 10% and 27% for the mixtures containing 250/250 and
compressive strength of 500CN0, 125CFGSN0, 125CFGSN1, 375/125C/CM, respectively, at the test age of 28 days. On the
125
CFGSN3 and 125CFGSN5 were 77.9, 70.8, 79, 84.7 and contrary, the highest compressive strength of the SHSC was
81.2 MPa, respectively, at the test age of 91 days. Compared achieved by the pentagonal blend (OPC þ FA þ GBSF þ
with incorporating other percentages of NS, incorporating NS SF þ NS), indicating an increase of 14% and 2% for the mix-
by 3% of OPC weight positively affected compressive strength. tures containing 250/250 and 375/125 kg/m3, respectively,
Compared with binary, ternary, or quaternary mixtures for at the test age of 28 days. These results supported the theory
the C/CM ratios of 250/250 and 125/375, the pentagonal blends of the synergistic interaction between alternative cement
(OPC þ FA þ GBFS þ SF þ NS) with NS achieved outstanding blends in SHSC. These alternative cement blends produced
performance. This finding agreed with several previous compressive strength higher than the compressive strength of
studies confirming the positive role of adding NS to binary or the reference mixture with 75% lower OPC content than the
Copmressive strength (MPa)

Mixes

Fig. 9 e Compressive strength of the SHSC at the test age of 28 days.

 j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 3 ; 2 4 : 7 4 4 4 e7 4 6 1 7453

Splitting tensile strength (MPa)

Mixes

Fig. 10 e Splitting tensile strength of the SHSC at the test age of 28 days.

pentagonal blends. Moreover, the synergistic reaction be- substitutes for OPC weight. The splitting tensile strength re-
tween the alternative cement blends achieved compressive sults of 500CN0, 250CFN0, 250CFGN0, 250CFGSN0, 125CFN0,
125
strength higher than the compressive strength of the refer- CFGN0 and 125CFGSN0 were 6.39, 5.38, 5.18, 5.47, 4.43, 4.83
ence mixture with 50% lower OPC content than the ternary, and 5.10 respectively. The results displayed that the addition
quaternary and pentagonal blends. These findings were of NS to SHSC mixtures improved splitting tensile strength. An
consistent with those of some researchers who reported a increase in the percentage of NS in 250CFGSN0, 250CFGSN1,
250
synergistic interaction between alternative cementitious CFGSN3 and 250CFGSN5 resulted in the splitting tensile
materials in ternary and quaternary blends; this interaction strength of 5.47, 6.09, 6.46 and 6.04 MPa, respectively. The
contributes to improving concrete mechanical and durability highest splitting tensile strength was attained by pentagonal
properties at a substitute rate of up to 75% of weight cement blend (50% OPC þ 20% FA þ 20% GBSF þ 10% SF þ 3% NS).
[105,106]. Compared with the reference mixture (500CN0), 250CFGSN3
achieved a splitting tensile strength that was slightly
3.2.2. Splitting tensile strength improved by 2%. These improvements were ascribed to the
The splitting tensile strength results of the SHSC mixtures strengthened binder matrix due to pozzolanic reactions.
containing 100% RCA with different SCMs at the test age of 28 Strengthening the ITZ between RCA and binder matrix could
days are shown in Fig. 10. The results showed the changes in also positively impact the splitting tensile strength of recycled
the splitting tensile strength of the SHSC concrete samples aggregate concrete (RAC). The trends of splitting tensile
due to using SCMs, such as FA, GBFS and SF, as partial strength and compressive strength of RAC with varying SCM
Flexural Strength (MPa)

Mixes

Fig. 11 e Flexural strength of the SHSC at the test age of 28 days.

7454 j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 3 ; 2 4 : 7 4 4 4 e7 4 6 1

Modulus of Elasticity (GPa)

Mixes

Fig. 12 e Modulus of elasticity of the SHSC at the test age of 28 days.

types had no considerable difference. The microstructural replacement levels. Increasing the OPC replacement content
(CeSeH) growths responsible for improving the compressive with SCMs (FA, GBFS and SF) reduced the flexural strength of
strength were also responsible for improving splitting tensile the mixtures without NS. For instance, compared with the
strength. Kou et al. [107] reported that no considerable dif- control mixture (500CN0), 250CFN0, 250CFGN0, 250CFGSN0,
125
ference exists in the trends of splitting tensile strength and CFN0, 125CFGN0 and 125CFGSN0 showed flexural strengths
compressive strength of RAC with varying SCM types. decreased by 12.6%, 16.86%, 10.18%, 23.64% and 17.70%,
respectively. The results also showed that adding NS to SHSC
3.2.3. Flexural strength mixtures improved flexural strength. NS had a high pozzo-
Fig. 11 shows the water flexural strength of the SHSC con- lanic activity, which could consume Ca(OH)2 to form addi-
taining 100% RCA and OPC substitutes of 50% and 75% OPC tional CeSeH. Fig. 11 shows that the SHSC had the highest
weight at the test age of 28 days. The flexural strength of the flexural strength when the NS content was 3%. Increasing the
control concrete containing 100% OPC at 28 days was 9.43 N/ NS content to 5% decreased the flexural strength. The reason
mm2. The flexural strength of the pentagonal blend (50% is that the excessive NS could not be effectively dispersed
OPC þ 20% FA þ20% GBSF þ 10% SF þ 3% NS) was higher than during the mixing of SHSC, thereby forming agglomerates. For
that of the other proportions. Compared with the control mix, instance, an increase in the percentage of NS in 250CFN0,
250 250
CFGSN3 exhibited a 7% increase in flexural strength. Flex- CFN1, 250CFN3 and 250CFN5 increased the flexural strength to
ural strength showed a behaviour similar to the behaviours of 8.24, 9.10, 9.66 and 9.151 N/mm2, respectively. Kong, Du, Wei,
compressive strength and splitting tensile strength at other Zhang, Yang and Shah [108] indicated that NS agglomerates
Water sorptivity coefficient (mm/s0.5)

Mixes

Fig. 13 e Water sorptivity resistance of the SHSC at the test age of 28 days.
 j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 3 ; 2 4 : 7 4 4 4 e7 4 6 1 7455

Water permeability x10-11(cm/sec)

Mixes

Fig. 14 e Water permeability resistance of the SHSC at the test age of 28 days.

absorb calcium ions and hydroxide ions in the solution to with FA did not affect the water sorptivity coefficient, which
form a pozzolan CeSeH gel. This gel does not function as a was at the same value of 0.08 (mm/sec0.5) for 500CN0 and
250
binder in the material. However, it prevents the cement- CFN0. The use of the ternary blends of OPC þ FA þ GBFS
hydrated CeSeH gel from penetrating the NS agglomerates. resulted in a growth in the value of the water sorptivity co-
This situation results in an interface transition zone between efficient by 2.5% and 5% for the substitution rates of 250/250
the NS agglomerates and the bulk paste, which reduces the and 125/375 (C/SCMs), respectively. The increase in the value
strength development effect of NS in cement-based materials. of the water sorptivity coefficient may be due to the effect of
In addition, excessive NS causes a large amount of CeSeH to cement dilution, particularly at the replacement rate of 75% of
form and wrap around the unhydrated cement during the OPC weight [109]. On the contrary, the quaternary mixture
early stage of cement hydration, limiting cement hydration to contributed positively to reducing the water sorptivity coeffi-
a certain extent. cient for the substitution ratios of 250/250 and 125/375 (C/
SCMs). The addition of NS to sustainable concrete mixes
3.2.4. Modulus of elasticity considerably reduced the water sorptivity coefficient. The
Fig. 12 shows the variation of modulus of elasticity of the SHSC addition of NS by 3% of OPC weight to the quaternary mixture
containing 100% RCA and SCMs, such as FA, GBFS and SF, as a (OPC þ FA þ GBFS þ SF) contributed to the highest decrease in
partial substitute of 50% and 75% OPC weight at the test age of the water sorptivity coefficient. The quaternary mixture
28 days. Modulus of elasticity showed a behaviour similar to (OPC þ FA þ GBFS þ SF) with 3% NS achieved low water
the behaviours of compressive strength, splitting tensile sorptivity coefficients. In particular, compared with the 500CN0
strength and flexural strength of mixtures with SCMs, such as mixture with 0.08 (mm/sec0.5), 125CFGFN3 and 250CFGFN3
FA, GBFS and SF, as partial substitutes. The modulus of elas- mixtures achieved 0.064 and 0.058 (mm/sec0.5), respectively.
ticity of 125CFN0 and 250CFGSN3 was between 31.43 and The improvement in the transport properties of SHSC may be
39.27 GPa. The results showed that replacing 75% of the OPC due to the effect of the pozzolanic properties and synergistic
weight with SCMs negatively affected the modulus of elasticity. interaction of the mixtures and the effect of filling [110,111].
Replacing 50% of the weight of OPC with SCMs slightly With regard to the high content of alternative cementitious
decreased the modulus of elasticity. The addition of NS to the materials at the rates of 50% and 75% of cement weight, the
SHSC mixture considerably increased the modulus of elasticity. synergistic reaction and filling are more effective than the
pozzolanic reaction because of the low cement content
3.3. Physical properties [112,113]. In addition, NS plays an important role in the filling
process because of its small particle size (nanoparticles).
3.3.1. Water sorptivity Thus, it can reach and close the smallest pores (capillary pores
Fig. 13 shows the water sorptivity resistance of the SHSC and nanopores). Moreover, sustainable concrete with highly
containing 100% RCA and OPC substitutes of 50% and 75% OPC efficient mechanical and transitional properties are produced
weight at the test age of 28 days. The results displayed that [113].
replacing 75% of the OPC weight with FA had a negative
impact on the water sorptivity resistance, with an increase of 3.3.2. Water permeability
8.7% compared with the water sorptivity resistance of the Fig. 14 shows the water permeability resistance of the SHSC
reference mixture. However, replacing 50% of the OPC weight containing cement substitutes of 50% and 75% OPC weight
7456 j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 3 ; 2 4 : 7 4 4 4 e7 4 6 1

with 100% RCA as coarse aggregate at the test age of 28 days. 3.3.3. Chloride permeability resistance
The results showed that replacing 50% and 75% of OPC weight Fig. 15 shows the chloride permeability resistance of the SHSC
with FA had a negative effect on the transport properties. In containing cement substitutes of 50% and 75% OPC weight and
particular, compared with the reference mixture, the SHSC 100% RCA as coarse aggregate at the test age of 28 days. The
with a high volume of replacement rates exhibited water behaviour of SHSC in resisting the chloride permeability with
permeability increased by 1.5% and 5%. The use of the ternary the resistance of water permeability matched with the
blends of OPC þ FA þ GBFS for substitution rates of 250/250 behaviour of the SHSC in resisting the water sorptivity. All of
and 125/375 (C/SCMs) increased the value of the water sorp- them were within the transport properties of concrete. The
tivity coefficient by 1.6% and 4%, respectively. The increase in results showed the positive effect of the quaternary cement
water permeability rates may be due to the effect dilution of blend of OPC þ FA þ GBFS þ SF, which achieved the highest
cement, particularly at the high replacement rates of 50% and level of chloride permeability for both replacement rates of
75% of cement weight [67]. On the contrary, the quaternary 50% and 75% of the OPC weight. The results proved that the
blend (OPC þ FA þ GBFS þ SF) contributed positively to synergistic reaction of the quaternary cement blend was bet-
reducing the water sorptivity coefficient for both substitution ter than that of the binary and ternary blends at the same
ratios (50% and 75%) of weight OPC. Moreover, adding NS to replacement rates. The results also showed the critical role of
quaternary blended concrete considerably reduced water adding NS in reducing the rate of chloride permeability in
permeability. The addition of NS by 3% of OPC weight to the SHSCs to the lowest level. Thus, the quaternary mixture plus
quaternary blended concrete (OPC þ FA þ GBFS þ SF) NS at 3% of the OPC weight was more advantageous than the
contributed to achieving the highest decrease in the water quaternary mixture without NS. Compared with the chlorine
permeability. The quaternary blends of OPC þ FA þ GBFS þ SF permeability value of the reference mixture (1418 coulomb),
with 3% NS achieved low water sorptivity coefficients. In the chlorine permeability values of 250CFGSN2 and 125CFGSN2
particular, compared with 3
1011(cm/sec) for the 500CN0 were decreased (1370 and 1381 coulombs, respectively). This
mixture, 2.67 and 2.54
1011(cm/sec) were achieved for the improvement might be attributed to the role of NS in
125
CFGFN3 and 250CFGFN3 mixture, respectively. The improving the microstructure of the cement matrix through
improvement in the transport properties of SHSC may be due the synergistic interaction and the pozzolanic interaction and
to the pozzolanic properties, synergistic interaction of the its role in packing/filling the nanopores. Thus, a dense cement
cementitious alternative blends and the filling effect [110,111]. matrix, which was slightly porous and permeable, was pro-
This scenario is evident in the quaternary mixtures compared duced. This finding was consistent with that of many re-
with the ternary and binary mixtures. The addition of NS searchers who studied the role of NS in the binary and ternary
played an important role in enhancing the synergistic inter- blends and its effect on the permeability of concrete
action and filling effect because of its high reactive SiO2 con- [114e116].
tent and small particle size (nanoparticles), which achieve
rapid interaction with cement hydration products, a syner- 3.4. Scanning electron microscopy (SEM) analysis
gistic reaction and the reaching and closing of the smallest
pores (capillary pores and nanopores). Thus, sustainable The SEM images of 250CFN0 and 250CFN3 pastes are shown in
concrete with highly efficient mechanical and transition Figs. 16 and 17. The improvement in the microstructure could
properties is produced [113]. be seen by comparing Fig. 16(a)e16(c) with Fig. 17(a)e17(c). The
Chloride permeability (coulomb)

Mixes

Fig. 15 e Chloride permeability resistance of the SHSC at the test age of 28 days.
 j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 3 ; 2 4 : 7 4 4 4 e7 4 6 1 7457

Fig. 16 e SEM images of the cement paste sample 250CFN0 Fig. 17 e SEM images of the cement paste sample 250CFN3,
(a) at magnification 1000 £, (b) at magnification 5000 £, (c) (a) at magnification 1000 £, (b) at magnification 5000 £, (c)
at magnification 20000 £. at magnification 20000 £.

microstructure of the OPC paste containing 3% NS was denser microstructure and ITZ between cement and aggregates
than that of the cement paste of the 250CFN0. The comparison contributed to the high density, low porosity and great
of both forms indicated that the black spots, indicative of strength in the cement paste. This improvement had a
pores/vacuoles, detected in 250CFN0 paste were fewer than considerable positive effect on the mechanical properties,
those detected in the paste containing 3% NS (250CFN0). This transferability and durability of the SHSC, as shown by the
observation suggested the formation of additional hydration results presented previously in this research. This finding was
products (CSH). Moreover, the addition of NS to the cement consistent with some studies indicating the positive effect of
paste improved the interfacial transition zone (ITZ) between adding NS to the cement paste to improve the microstructure
the aggregate and the cement matrix. Improving the and produce an additional gel [117,118].
7458 j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 3 ; 2 4 : 7 4 4 4 e7 4 6 1

General Research Funding program grant code (NU/DRP/SERC/

4. Conclusions 12/18).

In this conclusion, the effect of NS addition on SHSC

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