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 applied
sciences
Article
The Properties and Durability of Self-Leveling and Thixotropic
Mortars with Recycled Sand
Sebastiano Candamano 1, *, Francesco Tassone 2 , Ivan Iacobini 1 , Fortunato Crea 1 and Piero De Fazio 3






Citation: Candamano, S.; Tassone, F.;
Iacobini, I.; Crea, F.; De Fazio, P. The
Properties and Durability of
Self-Leveling and Thixotropic
Mortars with Recycled Sand. Appl.
Sci. 2022, 12, 2732. https://doi.org/
10.3390/app12052732
Academic Editor: Asterios Bakolas
Received: 24 January 2022
Accepted: 4 March 2022
Published: 7 March 2022
Publisher’s Note: MDPI stays neutral
with regard to jurisdictional claims in
published maps and institutional affil-
iations.
Copyright: © 2022 by the authors.
Licensee MDPI, Basel, Switzerland.
This article is an open access article
distributed under the terms and
conditions of the Creative Commons
Attribution (CC BY) license (https://
creativecommons.org/licenses/by/
4.0/).
Appl. Sci. 2022, 12, 2732. https://doi.org/10.3390/app12052732
1 Department of Mechanical, Energy and Management Engineering, University of Calabria, 87036 Rende, Italy;
iacobini.ivan@gmail.com (I.I.); f.crea@unical.it (F.C.)
2 Personal Factory S.p.A., 89822 Simbario, Italy; francesco.tassone@isolmix.com
3 Department of Energy Technology, DTE SAEN, Centro Ricerca ENEA Trisaia, 75026 Rotondella, Italy;
piero.defazio@enea.it
* Correspondence: sebastiano.candamano@unical.it
Featured Application: In the present work, the authors investigated the properties and durabil-
ity of mortars produced by replacing 100% of natural sand with recycled aggregate. The mix
was tuned to produce self-leveling and thixotropic mortars that can find application in creating
smooth and level surface/floor and in restoration.
Abstract: In recent decades, relevant environmental and economic reasons have driven an increasing
interest in using a large amount of recycled aggregate in replacement of natural ones to produce mor-
tar and concrete. The present study aims to investigate the effect of substituting 100% of natural sand
with recycled aggregate on fresh properties, mechanical properties, and the durability of a thixotropic
and a self-leveling mortar. Recycled aggregate was characterized using X-ray diffractometry and
energy-dispersive X-ray spectroscopy. Its morphology was investigated using scanning electron
microscopy and automated morphological imaging. Recycled aggregate mortars showed a moderate
decline in initial workability, as well as higher shrinkage and porosity than the control ones. The com-
pressive strength of self-leveling mortars produced with recycled aggregate was only 6% lower than
mortars produced with natural sand. The gap increased to 40% in the case of thixotropic mortars. The
self-leveling recycled aggregate mortar showed equivalent resistance to freeze–thaw cycles and better
sulfate resistance than the control one. The thixotropic recycled aggregate mortar showed comparable
sulphate resistance and only slightly lower resistance to freeze–thaw cycles than the control one.
Their capacity to relief stresses, due to hydraulic pressures and the formation of expansive products,
arises from their higher porosity. Thermal stability of the prepared mortars, after a curing period of
90 days, up to 700 ◦ C, was also investigated. A significant decrease in ultrasonic pulse velocity is
observed in the 200–400 ◦ C interval for all the mortars, due to the dehydration–dehydroxylation of
calcium silicate hydrate. The overall decline in the strength of both the recycled aggregate mortars
was comparable to the control ones. The results reported in the present investigation suggest that
the selection of high-quality recycled aggregate helps to obtain good-quality mortars when a large
amount of natural sand is replaced.
Keywords: recycled aggregate mortar; mechanical properties; high temperature; sulphate resistance;
freeze–thaw resistance
1. Introduction
The construction industry consumes around 40% of all extracted natural resources,
produces large amount of waste from building demolition, and consumes a lot of energy [1].
Several approaches have been carried out to mitigate the environmental impact of con-
struction practices, such as investigating on more sustainable binders [2,3] and reusing
demolition waste [4,5]. The generation of construction and demolition waste (C&DW)
comprises the largest waste stream in the European Union (EU). It totaled 374 million
https://www.mdpi.com/journal/applsci
Appl. Sci. 2022, 12, 2732 2 of 26

tons in the EU in 2016, excluding excavated soil [6]. Their management is driven by the
increasingly environmental concerns about the over-exploitation of aggregates from quar-
ries or rivers, landfill shortages, and rising transportation and landfill costs. Construction
and demolition represent a priority area in the EU according to the Circular Economy
Action Plan (EC 2015) for closing the loop, and EU countries set a 70% recovery target of
C&DW within 2020 [6]. While most EU countries are on track to meet or exceeded the
recovery target of 2020, it should be emphasized that most of the recovery practices result
in a down-cycling [6]. They are actually based on low-value backfilling operations, such
as filling holes on construction sites and low-grade recovery (involving the use of recy-
cled and crushed cement or stones (aggregates) in road construction). The revised Waste
Framework Directive (WFD 2008/98/EC, amended 2018/851) encourages measures which
promote and implement selective demolition and sorting systems for C&DW in order to
enable the removal and safe handling of hazardous substances and to facilitate reuse and
high-quality recycling. Analyses of the costs and benefits of reusing demolition waste as
recycled aggregates have been published in recent years, not only involving economic con-
siderations but also environmental benefits. Tam [7] reported that the long-term net benefit
of producing coarse recycled concrete aggregate (CRCA) from waste concrete was positive
with a value of USD 22,334,116 per year, while that of crushed coarse natural aggregate
(CNA) had a negative net value of USD −31,841,109 per year. Hameed [8] reported cost
savings of 63.13% for recycled aggregate concrete (RAC) produced from the recycling of
concrete waste to make fresh concrete at the same demolition site, rather than producing
conventional concrete made with CNA. According to Ohemeng et al. [9], the long-term
cost of producing one ton of coarse recycled concrete aggregate is about 40% less than that
for coarse natural aggregate. Furthermore, they calculated that the environmental benefit
of producing one ton of recycled concrete aggregate was approximately 97% higher than
that for natural aggregate.
Marius Dan Gavriletea [10] and Leal Filho [11] summarized the major environmental
impacts and consequences of sand exploitation based on the analysis of existing literature
associated with this issue. The very high volume of sand being currently extracted has a
serious negative impact on rivers, deltas, and coastal and marine ecosystems, such as the
loss of land through river or coastal erosion, the lowering of water levels, and the loss of
sediment supply, thus damaging fauna and flora at significant levels.
However, technical and commercial barriers for circular concrete recycling can be
summarized as follows:
• A lack of quality/purity in recycled materials;
• A lack of national instructions for recycling in new concrete in some countries;
• Low replacement rates in low-grade concrete allowed by Standards;
• A lack of documented information available regarding the origins of waste;
• Variable quality of feedstock;
• Contamination risks;
• A lack of trust of end-users in the quality/purity of recycled materials;
• The low price of virgin materials;
• The processing costs of demolition waste to secure high-quality material for recycling.
Different levers can be implemented to make the C&DW recycling an economically
attractive option that includes levies on virgin materials, taxes on landfilling waste, and
agreements and commitments between stakeholders in the value chain [6].
Specifically, to make the recycled aggregates competitive with virgin materials, it is
crucial to increase their market value and manufacture products that perform as well as
those made with virgin materials, or at least meet high-performance and durability criteria.
The amount of recycled materials in cementitious composites and their applications is
regulated by national standards. Furthermore, up to 20 percent substitution of virgin
aggregates is allowed in new concrete because it does not damage the durability and
the resistance of the cementitious materials. More than 50 percent substitution of virgin
aggregates is only suitable for certain applications [12].
Appl. Sci. 2022, 12, 2732 3 of 26

The possibility of using higher replacement rates of recycled aggregate from building
demolition in concrete would represent a key step in increasing its high-quality recycling,
due to the huge volumes of concrete yearly produced and being the fine and coarse
aggregate accounting for 60–75% of concrete total volume [13–15]. Therefore, the scientific
community has sought to close the gap in knowledge related to the topic. Attributing the
loss of fresh and hardened state properties of RAC to the higher porosity of sorted RA
has been met with unanimous consensus due to its inherent defects, such as the existing
of additional interfacial transition zones (ITZ) [16–18]. These pores absorb water during
mixing and have any load carrying capacity in the cured concrete. They also reduce the
durability of RAC, because channels facilitate the penetration of detrimental substances,
such as chloride ion and carbon dioxide, which both promote the corrosion of steel rebar
and sulphate ion.
The mechanical properties and long-term performance of RAC can be improved by
enhancing the properties of the ITZ to facilitate the reuse of RCA in construction projects.
In the most recent papers, three group of approaches have been proposed and investigated:
(1) Reduction in the recycled aggregate porosity:
• Accelerated carbonation. The old mortar layer on the RAs contains a high
amount of calcium hydroxide and calcium silicate hydrate. The method involves
a carbonation reaction with CO2 under the presence of water. The corresponding
carbonated products show a volume expansion and partially occupy or even
close the porosity of the RAs [19,20].
• Biodeposition. The biodeposition is defined as microbial carbonate precipitation
that can be achieved by ureolytic bacteria B. Megaterium [21] and B. Sphaeri-
cus [22]. The concrete pores can be filled with the insoluble calcium carbonate.
• The addition of pozzolana. Silica fume (SF), fly ash (FA), and nano-SiO2 (NAS)
have been investigated for RA modification throughout the literature [23,24]. In
this case, the pores are filled by the calcium silicate hydrate (C-S-H) gel produced
by the pozzolana reaction with Ca(OH)2 .
• The addition of nanoparticles. Nanoparticles have much smaller size than cement
grains. They not only act as filler in the ITZ, pores, or cracks, thus reducing the
porosity, but also participate to the hydration process of the cement as nucleation
centers for the crystallization [25,26].
• Polymer emulsions. When polymer emulsion is applied to RA, the polymer
molecules can fill up the pores and cracks in the RA, especially in the attached
mortar and the ITZ and the aggregate surfaces can be sealed [27,28]
(2) Reduction in the old mortar layer on recycled aggregate surface:
• Acid treatment. Pre-soaking of recycled concrete aggregate in HCl, H2 SO4 ,
HNO3 , and (CH3 COOH) solution at room temperature for programmed time
reduces or removes the old mortar layer, as the alkaline mortar can be dissolved
in acid solutions [29,30].
• Thermal treatment. The heating of the recycled concrete causes the dehydration
of old cement stone, which leads to the separation of old mortar layer from the
aggregate particles [31].
(3) Property improvement without recycled aggregate modification:
• The mixing approach. This involves an atypical mixing of concrete compo-
nents [32]. In the two-stage mixing approach (TSMA), the mixing water is
divided into two portions. In the sand enveloped mixing approach (SEMA), sand
and 75% of water are mixed at first, and then the cement is added. After further
mixing, the remaining water and coarse aggregate are added. The aim of the
approach is to generate a thin cement slurry on the surface of recycled concrete
aggregate during the first water addition that covers pores and cracks of the
recycled concrete aggregates.
Appl. Sci. 2022, 12, 2732 4 of 26

• The addition of fiber. The addition of short monofilament fibers in RAC is aimed
to control the cracks opening and propagation by the “fibre bridge effect”, thus
overcoming the brittle failure mode of the RAC and increasing its tensile and
flexural strength [33]
The effect of the above-mentioned different approaches on the RAC properties has
been investigated in terms of fresh properties (workability), physical and chemical proper-
ties (i.e., density, carbonation depth, and chloride ion penetration), mechanical properties
(i.e., compressive, flexural, and splitting tensile strength as well as elastic modulus), and
long-term performance (i.e., freezing-thawing resistance, alkali-silica reaction resistance,
and creep and dry shrinkage). The bio-deposition significantly improves the elastic mod-
ulus and compressive strength of the final RAC. Specifically, the compressive strength
increased by about 16% and 10% for RAC using recycled concrete aggregate and recycled
mixed aggregate, respectively [34]. However, the bacterial culture medium may affect the
concrete hydration process and long-term performance [21]. Shi et al. [23] studied the im-
provement in compressive strength of recycled concrete aggregate constituent RAC through
adding pozzolanic materials SF, FA, and NAS (pozzolana to cement ratio is 0.13). Increases
in the compressive strength of RAC modified with SF, FA, and NAS were 55.2%, 39.4%,
and 17.6%, respectively, over 28 days, i.e., higher compared with that of RAC without any
modification. A small amount of nanoparticles can significantly improve RCA properties,
but they can also increase the cost of concrete production. Furthermore, the dispersion of
the nanoparticles in the composition is a critical issue and the proposed lab methods have
limitations given the massive production of concrete [25]. The increases in compressive
strength after 28 days for HCl, HNO3 , and H2 SO4 treatment were 34.6%, 25.3%, and 17.6%
for a 100% RA replacement ratio, respectively. However, they are dangerous, expensive,
and far from eco-friendly. Furthermore, they can deteriorate concrete and promote the
corrosion of steel rebar. The mixing approach is considered a practical method [35] because
it can be easily implemented, it has low costs, and it can lead to a significant strength
enhancement (up to 20%) of the RAC compressive strength. Katkhuda et al. [36] applied
chopped basalt fibers in RAC with a 20% replacement ratio with recycled concrete ag-
gregate. Increasing the weight fibers content from 0% to 1.5% on cement increased the
splitting tensile strength and flexural strength by 40% and 61%, respectively. However,
the incorporation of fibers could reduce the workability of fresh RAC, especially when
they have a high aspect ratio [36,37]. Larbi et al. [38] reported that heating the recycled
concrete aggregate to maximum 800 ◦ C for 2 h can remove most of the attached old mortar;
however, this treatment has a high-energy consumption. Kou et al. [39], using recycled
concrete aggregates soaked in 10% PVA solution for 24 h, reduced the water absorption of
recycled aggregate concrete by approximately 70.0%.
Other than the above-mentioned technical and production process limitations, social
aspects, such as a public awareness and acceptance of the products from recycled mate-
rials by public, prevent their actual massive use or commercialization [40]. The practical
application of RAC is still limited and its use in structural application is even more so [16].
According to the authors, cementitious products based on recycled aggregate for non-
structural application could achievebetter acceptance by public in the status quo. Several
papers have been recently published on this topic. Restuccia et al. [41] investigated the
effect of washing and sieving the recycled aggregate on the properties of a mortar produced
according to standard UNI EN 196-1. Da Silva Neto et al. [42] studied the influence of the
mortar fine recycled aggregate ratio and the mixing sequence on the behavior of mortars
using modified Brazilian standard NBR 7215 and two-stage mixing approach (TSMA),
while Katz et al. [43] investigated the effects on the fresh and hardened properties of a
rendering mortar at different replacement ratios. Roque et al. [44] presented a study of
incorporation at 0%, 20%, 50%, and 100% (by volume) of demolition waste aggregate
(CDW) in rendering mortars and evaluated their workability, mechanical strength, water
absorption, shrinkage, open porosity, and durability. Mora-Ortiz et al. [45] evaluated the
performance of masonry mortar manufactured by replacing natural sand with pre-wetted
Appl. Sci. 2022, 12, 2732 5 of 26

recycled fine aggregate (RFA) and using a commercial plasticizer. In all the aforementioned
works, the performance of the cement mortars with recycled aggregate was investigated
only as a function of the percentage of replacement or of the mixing approach method
used. In few cases, a plasticizer was used to adjust the workability. A higher percentage
of recycled aggregate lead to lower workability and mechanical properties, partially com-
pensated by adopting the different mixing methods. However, the performance, fresh and
hardened properties, and durability of most of the commercial mortars and concrete are
achieved or altered by adding chemical admixtures. The type and amount of the used
chemicals depend on the specific application of concrete and mortars. Chemical admixtures
also alter physical, chemical, and surface chemical properties of the mortars’ components.
Therefore, they reasonably affect the performance of recycled aggregate mortar. Based on
the aforementioned information, authors evaluated the fresh and hardened properties and
the durability of two commercial products, a self-leveling and a thixotropic mortar, whose
mix design includes two specific chemical admixtures kits. They compared the results with
those obtained when their mix design was modified by replacing the 100% the natural sand
with recycled aggregate.
Self-leveling mortars (SLMs) are building materials with the property of leveling by
gravity. They can be used over a subfloor before the installation of floors as underlayment
to smoothen out any surface and correct the irregularities that the concrete could have [46].
Their high fluidity, good flatness, high compressive strength, and thin leveling layer also
make them ideal for finished flooring in large supermarkets, shopping malls, parking lots,
factory workshops, and warehouses. Cements, fine aggregates, mineral fillers, and chemical
admixtures compose conventional SLMs [47]. Portland cement (PC) is commonly used as
binder. However, SLMs that contain it struggle to meet the early strength requirements and
show cracks and curls that commonly appear at the corners and perimeter. The low early
strength and serious drying shrinkage of PC are responsible of the behavior [48]. In order
to avoid the aforementioned issues, binary or ternary cementitious systems containing PC,
calcium aluminate cement (CAC) or sulphoaluminate cement (SAC), and calcium sulfate
(CS) are used [47]. The chemical admixtures (water reducer, retarder, early strength agent,
and stabilizer) represent another significant factor that can influence their performance
and properties by prolonging the setting time and increasing the fluidity of SLMs. An
essential additive component of mortar as a floor material is the redispersible powder
(RP). This is prepared by spray-drying or other process of polymer emulsion. A very
small amount of RP can deeply affect the properties and performance of SLMs. When the
powder mixes with water, the polymer emulsion can significantly improve the fluidity, the
wear resistance and flexural strength, the bond strength, the impact resistance, and the
flexibility of self-leveling mortar [49,50]. However, an excessive amount of RP can reduce
the compressive strength of SLMs [50]
Thixotropic mortars are commonly used for non-structural and structural restoring and
smoothing of concrete. Their elastic modulus, drying shrinkage, and chemical permeability
and compatibility with the damaged concrete must be taken into account. Cement-based
or polymer-modified repair materials can be used [51]. The former includes grout, mortar,
or concrete (containing Portland cement, aluminous cement, or silicate cement). They
are characterized by properties similar to those of the original concrete, thus assuring
a high compatibility. However, they cannot overcome the drawbacks of the original
concrete, such as permeability, which can lead to cracking carbonization, rebar corrosion,
and drying shrinkage, which can affect bonding strength and, thus, the overall efficacy
of repairs. The latter consists of mortars that contain polymers, such as redispersible
polymer powder. This improves the bonding strength of repairing mortar to the substrate,
fills in capillary pores, enhances the freeze–thaw resistance, improve resistance to water
and chemicals, and reduces surface cracking [51]. They also provide a protective film
on the surfaces of aggregates, and form a link with the hydration products of cement.
Furthermore, the addition of cellulose ethers provides high viscosity, air incorporation, and
water retention [52]. These factors also prevent an excessive loss of water into the substrate,
Appl. Sci. 2022, 12, x FOR PEER REVIEW 6 of 26

Appl. Sci. 2022, 12, 2732

surfaces of aggregates, and form a link with the hydration products of cement. Further- 6 of 26
more, the addition of cellulose ethers provides high viscosity, air incorporation, and water
retention [52]. These factors also prevent an excessive loss of water into the substrate,
which could cause failures in the mechanism of adhesion and improve the sag resistance
which could cause
of the mortar. failures inofthe
The viscosity themechanism of adhesion
cellulose ether solution and improve the
is responsible sag thickening
of the resistance
of the mortar. The viscosity of the cellulose ether
effect of cellulose ether on cement-based materials. solution is responsible of the thickening
effect of cellulose ether on cement-based materials.
In the present investigation, a self-leveling mortar and a thixotropic mortar contain-
In the present investigation, a self-leveling mortar and a thixotropic mortar containing
ing 100% of recycled aggregate and specific chemical admixtures kits were produced.
100% of recycled aggregate and specific chemical admixtures kits were produced. Their
Their fresh and hardened state properties, such as workability, porosity, compressive and
fresh and hardened state properties, such as workability, porosity, compressive and flexural
flexural strengths, and drying shrinkage, were evaluated. Freeze–thaw, sulphate, and
strengths, and drying shrinkage, were evaluated. Freeze–thaw, sulphate, and thermal
thermal resistance of the prepared mortars were also investigated in order to assess their
resistance of the prepared mortars were also investigated in order to assess their durability.
durability. Self-leveling and thixotropic mortar have the same mix design but that con-
Self-leveling and thixotropic mortar have the same mix design but that containing natural
taining natural sand was used as a control group.
sand was used as a control group.
2. Materials
2. Materials and
and Methods
Methods
2.1. Materials
2.1. Materials
Cement of type
Cement type CEMCEMII/A-LL
II/A-LL42.5 42.5RRwas used
was used to manufacture
to manufacture mortars.
mortars.ThisThis
was waspro-
duced in accordance
produced in accordance with standard
with standard UNI ENEN
UNI 197-1.
197-1.TheThecement
cementparticle sizesize
particle distribution,
distribu-
basedbased
tion, on volume
on volume distribution, is: D50
distribution, = 19.84
is: D50 μm; µm;
= 19.84 D90 D90
= 36.11 μm;µm;
= 36.11 D10D10 = 8.414
= 8.414μm.µm. Its
main
Its components,
main components, in terms of oxides
in terms werewere
of oxides SiO2 SiO= 18.61
2 = wt%;
18.61 Fe
wt%;
2O 3 =
Fe 2.87
O
2 3 wt%;
= 2.87Al O
wt%;
2 3 =
Al
4.38O
2 3 =
wt%; 4.38CaOwt%;
= CaO
60.60 =
wt%;60.60
MgO wt%;= MgO
3.16 wt%;= 3.16
K 2 O wt%;
= 0.79 K O
wt%;
2 = 0.79
Na 2 Owt%;
= 0.35;NaMnO
2 O ==0.35;
0.17
MnO
wt%; =SO 0.17 wt%;wt%;
3 = 2.83 SO3 TiO
= 2.83
2 = wt%;
0.2 wt%.TiO2 = 0.2 wt%.
AA natural siliceous
siliceoussand sandwas wasusedused ininthethe experimental
experimental campaign
campaign to produce
to produce the
the con-
control mortars.
trol mortars. TheThe recycled
recycled aggregate
aggregate camecamefromfrom thethe demolition
demolition of of a buildingused
a building usedasasa
awarehouse.
warehouse.The Thedemolition
demolitionwaste wastewas wasthen
then sorted
sorted by by obtaining approximately 60 m m33,
mainly
mainly consisting
consisting of of bricks,
bricks, lime
lime and
and cementitious
cementitious mortars,mortars, andandconcrete.
concrete. High-quality
High-quality
aggregates were then produced by dry grinding
aggregates were then produced by dry grinding and sieving. and sieving.
Scanning
Scanningelectron
electronmicroscopy
microscopyenergy-dispersive
energy-dispersive X-ray analysis
X-ray analysis waswasused to investigate
used to investi-
the morphology and elemental composition of the sands.
gate the morphology and elemental composition of the sands. Analyses were carriedAnalyses were carried out without
the
withhelp
the of a computer-controlled
help of a computer-controlled field field
emission Phenom
emission ProX,ProX,
Phenom equipped withwith
equipped an energy-
an en-
dispersive X-rayX-ray
ergy-dispersive (EDX)(EDX)spectrometer
spectrometer(Deben, Suffolk,
(Deben, UK).UK).
Suffolk, Before SEMSEM
Before observation,
observation,the
samples were sputtered with gold to stop their non-conductive
the samples were sputtered with gold to stop their non-conductive surfaces from changing, surfaces from changing,
and
and images
images werewere acquired
acquiredat at2020kV.
kV.TheThecounting
countingtime timeforforthe
theEDXEDXanalysis
analysiswas was120120s.s.
Shape,
Shape, surface texture, and mineralogical composition of sands can markedly affect the
surface texture, and mineralogical composition of sands can markedly affect the
fresh
fresh and
and hardened
hardened state state properties
propertiesof ofthe
theproduced
producedmortars mortarsand andtheir
their durability
durability [53–55].
[53–55]. In
In Figure
Figure 1, the
1, the SEMSEM analysis
analysis of recycled
of recycled aggregate
aggregate (RS)(RS)andand natural
natural sand sand
(NS)(NS) are reported.
are reported.

Figure 1.
Figure 1. SEM
SEM analysis
analysis of
of recycled
recycled sand
sand (A)
(A) and
and natural
natural sand
sand(B).
(B).

Natural
Naturalsand
sand (Figure
(Figure1B)
1B) is
is characterized
characterizedbyby angular
angularand
and rough
roughgrains.
grains. Recycled
Recycled sand
sand
contains
containsgrains
grainswith
withirregular shape
irregular andand
shape sharply cut edges
sharply and some
cut edges of grains
and some show cracks
of grains show
throughout their microstructure
cracks throughout (Figures(Figures
their microstructure 1A and1A2). and
Their
2).formation is promoted
Their formation by the
is promoted
crushing process at the interfacial transition zone (ITZ) of concretes and mortars used as
starting materials to produce RS, as reported by other authors [56,57].
 Natural sand 57.8 11.7 1.9 2.7 17.5 5.2 3.1 0.2
Recycled sand 27.6 9.3 2.0 0.4 52.5 6.1 2.0 0.4
* Obtained by energy-dispersive X-ray analysis (EDX).

Appl. Sci. 2022, 12, 2732 In Figure 2, the EDX mapping analysis of recycled sand is reported, revealing
7 of 26 the
heterogeneity of composition among grains.

2. SEM-(left)
Figure 2.
Figure SEM-(left)and
andenergy-dispersive X-ray
energy-dispersive mapping
X-ray analysis
mapping (right)(right)
analysis of recycled sand. sand.
of recycled

Natural sand is mainly composed by a silica, with other elements indicating the
Automated morphological imaging was carried out using Morphologi-G3 (MAL-
presence impurities (Table 1). The main elements found in the recycled aggregates (Table 1)
VERN). This
are silicon, was used
calcium, to investigate
aluminium, theoriginating
and iron, recycled particles’ shape; thecompounds
from cementitious circle equivalent
(CE) diameter,
(concretes definedand
and mortars) as bricks.
the diameter of a circle with the same area as the 2D image of
the particle [58]; and the high sensitivity circularity (HS circularity) defined as:
Table 1. The average composition of used sands in terms of oxides *.
HS circularity = 4πA/P2
Chemical Composition [%wt] SiO Al O K O Na O CaO FeO MgO SO
where A2 is the particle
2 3
area2
and P is2 its perimeter [58]. HS circularity has values 3
in the
Natural sand 57.8 11.7 1.9 2.7 17.5 5.2 3.1
range 0–1. A perfect circle has a circularity of 1, while a ‘spiky’ or irregular object has a 0.2
Recycled sand 27.6 9.3 2.0 0.4 52.5 6.1 2.0 0.4
circularity value closer to 0. Representative results are reported in Figure 3.
* Obtained by energy-dispersive X-ray analysis (EDX).
The calculated HS circularity for RS, based on the analysis of more than 500,000 par-
ticles was 0.8. Recycled sand was analyzed by X-Ray diffractometry using a Rigaku Min-
In Figure 2, the EDX mapping analysis of recycled sand is reported, revealing the
iFlex 600 X-ray
heterogeneity diffractometer
of composition among(Rigaku
grains.Corporation, Tokyo, Japan) with CuKα (wave-
length of 1.5406morphological
Automated Å) radiation imaging
generated wasat 20 mA
carried outand 40Morphologi-G3
using KV. This was (MALVERN).
scanned at 0.02 2θ
step
This at
wasa rate
usedofto1°/min between
investigate 5°and particles’
the recycled 50° (2θ angle range).
shape; Theequivalent
the circle obtained(CE)
X-Ray diffraction
diame-
pattern is shown
ter, defined in Figure
as the diameter of 4.
a circle with the same area as the 2D image of the particle [58];
and the high sensitivity circularity (HS circularity) defined as:

HS circularity = 4πA/P2

where A is the particle area and P is its perimeter [58]. HS circularity has values in the
range 0–1. A perfect circle has a circularity of 1, while a ‘spiky’ or irregular object has a
circularity value closer to 0. Representative results are reported in Figure 3.
The calculated HS circularity for RS, based on the analysis of more than 500,000 parti-
cles was 0.8. Recycled sand was analyzed by X-Ray diffractometry using a Rigaku MiniFlex
600 X-ray diffractometer (Rigaku Corporation, Tokyo, Japan) with CuKα (wavelength of
1.5406 Å) radiation generated at 20 mA and 40 KV. This was scanned at 0.02 2θ step at a
rate of 1◦ /min between 5◦ and 50◦ (2θ angle range). The obtained X-Ray diffraction pattern
is shown in Figure 4.
Appl. Sci.
Sci. 2022,
2022, 12,
12, x2732
FOR PEER REVIEW 8 8ofof 26
26
Appl. Sci. 2022, 12, x FOR PEER REVIEW 8 of 26

Particle
Figure3.3.Particle
Figure images
images andand CE diameters
CE diameters [μm][µm]
of RS of RS as obtained
as obtained by automated
by automated morphological
morphological imaging.
imaging.
Figure 3. Particle images and CE diameters [μm] of RS as obtained by automated morphological imaging.
*
* + C-S-H (∆)
laumontite
C-S-H (∆) (□)
+ microcline
laumontite(◊)(□)
muscovite
microcline(+)
[a.u.]

(◊)
quartz (*) (+)
muscovite
[a.u.]

calcite (●)
quartz (*)
Intensity

∆ portlandite
calcite (●) (○)
●
Intensity

∆ portlandite (○)
●

+
◊ ◊○
* +
◊ ◊○ ●
+ * ◊ ● * ●●
○ ●∆ ● ◊●
□ + + ◊ ●◊ ◊ ++ ○ ++*● ** * +* ○● ●
∆ + ○
◊ ●∆ ●
● ◊ ◊ ●
□ + + ◊ ◊ ++ ○ ++* * * +* ○ ●
∆
10 20 30 40 50
10 20 30 40 50
2θ
2θ
Figure 4. X-Ray diffraction pattern of recycled sand.
Figure 4. X-Ray diffraction pattern of recycled sand.
Figure 4. X-Ray diffraction pattern of recycled sand.
The main crystalline phases of the recycled sand are silicates, such as quartz (PDF
The
The main
9000776), main crystalline
microcline phases
phases of
(PDF 00-900-5308),
crystalline of the recycled
thecalcite (PDF
recycled sand are
are silicates,
7022027),
sand such
such as
portlandite
silicates, as quartz
(PDF (PDF
1000045),
quartz (PDF
9000776),
muscovite microcline (PDF
(PDF 00-900-6329),
9000776), microcline 00-900-5308),
and laumontite
(PDF 00-900-5308), calcite (PDF
calcite(PDF 7022027),
(PDFR0601141). portlandite (PDF
Significant (PDF
7022027), portlandite 1000045),
peaks1000045),
indicat-
muscovite
ing
muscovite (PDF
(PDF00-900-6329),
the presence of and
andlaumontite
calcium hydroxide
00-900-6329), and, its(PDF
laumontite (PDFR0601141).
carbonated form,
R0601141). Significant peaks
calcite are
Significant indicating
observed.
peaks The
indicat-
the
peakspresence of
ofpresence calcium
the quartz hydroxide and, its carbonated form, calcite are observed. The peaks
ing the ofand feldspars
calcium are attributed
hydroxide and, its to the natural
carbonated sandcalcite
form, and aggregates
are observed. used in
The
of the
the quartz and feldspars
manufacturing of the are attributed
original concrete to the
and natural
mortar. sand andcan
Muscovite aggregates
be used to
associated in the
the
peaks of the quartz and feldspars are attributed to the natural sand and aggregates used in
manufacturing
presence of bricksofand
the ceramics.
original concrete
It concrete andto
is difficult mortar. Muscovite can be associated to the
the manufacturing of the original and clearly
mortar.distinguish
Muscovite the cancrystalline hydrated
be associated to the
presence of bricks and ceramics. It is difficult to clearly distinguish the crystalline hydrated
calcium
presencesilicate phases
of bricks and as their peaks
ceramics. overlap to
It is difficult with the peaks
clearly of calcite
distinguish the and feldspars;
crystalline how-
hydrated
calcium silicate phases as their peaks overlap with the peaks of calcite and feldspars;
ever, thesilicate
calcium detection of calcium
phases as theirhydroxide
peaks overlap is related to their
with the peaksoccurrence. Thefeldspars;
of calcite and results are in
how-
however, the detection of calcium hydroxide is related to their occurrence. The results are
agreement with theofchemical
ever, the detection calciumcomposition
hydroxide isreported
related tointheir
Table 1; they areThe
occurrence. congruent
results arewithin
in agreement with the chemical composition reported in Table 1; they are congruent with
the mineralogical composition of the parent materials (concrete, mortar,
agreement with the chemical composition reported in Table 1; they are congruent with and bricks) used
the mineralogical composition of the parent materials (concrete, mortar, and bricks) used
for
thetheir production
mineralogical and they are
composition of consistent
the parentwith other(concrete,
materials publishedmortar,
studiesand
[59–63].
bricks) used
for their production and they are consistent with other published studies [59–63].
Natural
for their and recycled
production sands
and they areinconsistent
a saturated surface
with otherdry (s.s.d.) condition
published were used to
studies [59–63].
Natural and recycled sands in a saturated surface dry (s.s.d.) condition were used to
produce mortars.
Natural and This prevents
recycled sandsthem
in a from absorbing
saturated surfacethedry
free(s.s.d.)
watercondition
that lendswere
workability
used to
produce mortars. This prevents them from absorbing the free water that lends workability
produce mortars. This prevents them from absorbing the free water that lends workability
Appl. Sci. 2022, 12, x FOR PEER REVIEW 9 of 26
Appl. Sci. 2022, 12, 2732 9 of 26

to the mix [64,65]. The same particle size distribution curve, reported in Figure 5, was used
to the mix [64,65]. The same particle size distribution curve, reported in Figure 5, was used
for both the sands.
for both the sands.

100

Cumulative mass passing (%) 80

60

40

20

0
0.0 0.5 1.0 1.5 2.0 2.5 3.0
Sieve size (mm)
Figure 5. The grain size distribution curve of the natural and recycled aggregate.
aggregate.

By observing
observingthe thegranulometric
granulometriccurve
curveof of
thethe
aggregate, it can
aggregate, it be
canhighlighted that close
be highlighted that
attention
close was used
attention was to prevent
used fines used
to prevent finesinused
the production of mortars.
in the production It is well
of mortars. It known
is well
that fines
known from
that finesrecycled aggregate
from recycled have ahave
aggregate considerable negative
a considerable impact
negative on mortars
impact and
on mortars
concrete
and rheology.
concrete This is
rheology. caused
This by their
is caused by tendency to agglomerate
their tendency when water
to agglomerate when is added
water is
to the mix, as different small forces (such as capillary and electrostatic charges,
added to the mix, as different small forces (such as capillary and electrostatic charges, or or van der
Waals
van der forces)
Waalsarise [66–68].
forces) arise Furthermore, they show
[66–68]. Furthermore, some
they showhydraulic activity and
some hydraulic a rough
activity and
asurface
roughthat determine
surface a high water
that determine absorption
a high capacity capacity
water absorption [67]. [67].

2.2. Methods
2.2. Methods
Thixotropic and
Thixotropic and self-leveling mortars, with
self-leveling mortars, with natural
natural and and recycled
recycled aggregates,
aggregates, were
were
produced using a water/cement ratio equal to 0.52 and a sand/binder ratio equal to 2.28.
produced using a water/cement ratio equal to 0.52 and a sand/binder ratio equal to 2.28.
Two chemical kits, especially those designed for producing self-leveling and thixotropic
Two chemical kits, especially those designed for producing self-leveling and thixotropic
mortars, were provided by Personal Factory s.p.a. and used in the experimental campaign.
mortars, were provided by Personal Factory s.p.a. and used in the experimental campaign.
The chemical kit was equal to the 5 wt% of the overall admixture. In Figure 6, the mix
The chemical kit was equal to the 5 wt% of the overall admixture. In Figure 6, the mix
design of the four types of mortars is reported.
design of the four types of mortars is reported.
The mixing protocol establishes that water and cement are initially blended for 30 s.
Mixture proportions of mortars (kg/m3) are reported in Table 2.
The chemical compound is then added and a further 30 s of blending is carried out. Natural
The mixing protocol establishes that water and cement are initially blended for 30 s.
or recycled sand is then added in 30 s under mixing, followed by 1 more minute of mixing
The chemical compound is then added and a further 30 s of blending is carried out. Nat-
time. The admixture rests for 1 min and 30 s and, finally, it is mixed again for 1 min before
ural or recycled sand is then added in 30 s under mixing, followed by 1 more minute of
starting the tests.
mixing time. The admixture rests for 1 min and 30 s and, finally, it is mixed again for 1
For each type of mortar, the nomenclature used is classified as follows: the first two
min before
letters startingto
correspond the tests.
the origin of the aggregate, i.e., natural aggregate (NS) or recycled
For each
aggregate type
(RS); theoflast
mortar, the nomenclature
two letters used of
refer to the type is classified as thixotropic
mortar, i.e., follows: the(RX)
first and
two
letters correspond
self-leveling (PX). to the origin of the aggregate, i.e., natural aggregate (NS) or recycled
aggregate (RS);
At zero timethe lastmixing,
after two letters refer to theoftype
the workability of mortar,
freshly preparedi.e.,mortars
thixotropic (RX) and
was evaluated
self-leveling (PX).
using the flow table and according to EN 1015-3 [69].
Several specimens, with a dimension of 40 mm × 40 mm × 160 mm, were produced
according to EN 1015-11:2001 [70] and stored in a climatic chamber at 20 ± 3 ◦ C and
RH 90 ± 3% for certain cure ages. Compressive and flexural strengths, drying shrinkage,
and open and total porosities were measured, according to relevant standard reported in
Table 3. The drying shrinkage was measured on specimens stored in a dry environment
(20 ◦ C, RH 60%).
Appl. Sci.
Appl. Sci. 2022,
2022, 12,
12, 2732
x FOR PEER REVIEW 10
10 of 26
of 26

Figure 6. The
Figure 6. The mix
mix design
design of
of thixotropic
thixotropic and
and self-leveling
self-leveling mortars.
mortars.
3
TableMixture proportions
2. The mixture of mortars
proportions (kg/m
of mortars ) are
(kg/m 3). reported in Table 2.

Cement
Table 2. The mixture Natural
proportions Sand (kg/m
of mortars Recycled
3 ). Sand Water Chemical Kit
[kg] [kg] [kg] [kg] [kg]
Cement Natural Sand Recycled Sand Water Chemical Kit
NSRX 539.3 1227.3 - 279.0 93
[kg] [kg] [kg] [kg] [kg]
RSRX 496.0 - 1128.7 256.6 85.5
NSRX 539.3 1227.3 - 279.0 93
NRPX 539.3 1227.3 - 279.0 93
RSRX 496.0 - 1128.7 256.6 85.5
RSRX
NRPX 496.0
539.3 -
1227.3 1128.7
- 256.6
279.0 85.5
93
RSRX 496.0 - 1128.7 256.6 85.5
At zero time after mixing, the workability of freshly prepared mortars was evaluated
using the flow table and according to EN 1015-3 [69].
Table 3. Tests, shape and size of the specimens, curing time, and applied standards.
Several specimens, with a dimension of 40 mm × 40 mm × 160 mm, were produced
according to EN 1015-11:2001
Specimen [70] and stored in a climatic
Specimen Test Time chamber at 20 ± 3 °C and RH 90
Test ± 3% for certain cure ages. Compressive and flexural strengths, Standard
drying shrinkage, and open
Shape Dimensions [cm] [Days/Months/Cycles]
Workability
and total -porosities were measured, -
according to relevant -
standard reported in Table 3. The
UNI EN 1015-3 [69]
Flexural strength dryingPrisms
shrinkage was measured 4 × 4on× specimens
16 stored
2, 7, in
28,a90
dry environment
days EN(20 °C, RH
1015-11 60%).
[70]
Compressive strength Post bending test pieces 4×4×8 2, 7, 28, 90 days EN 1015-11 [70]
Drying shrinkage Table 3. Tests, shape and size of
Prisms 4 ×the
4×specimens,
16 curing
2, time,
7, 28, and applied standards.
90 days EN 12617-4 [71]
Open/total porosity Prisms 4 × 4 × 16 28th curing day UNI 11060:2003 [72]
Thermal cycles resistance Specimen
Prisms 4 × 4Specimen
× 16 Test
- Time -
Test Standard
Sulphate resistance Shape
Prisms 4Dimensions
× 4 × 16 [cm] [days/months/cycles]
6 months UNI 8019 [73]
Freeze–thaw resistance
Workability Prisms - 4 × 4 × 16- 300 cycles
- UNIUNI
EN7087 [74] [69].
1015-3
Flexural strength Prisms 4 × 4 × 16 2, 7, 28, 90 days EN 1015-11 [70]
Compressive strength Post
The resistance of the prepared mortars to freeze–thaw cycles wasEN
bending test pieces 4 × 4 × 8 2, 7, 28, 90 days 1015-11
tested [70]
according
Drying shrinkage Prisms
to the relevant standard reported 4 ×in4 ×Table
16 3, after2,a7,curing
28, 90 period
days of 28 EN 12617-4
days. [71]
Saturated
Open/total porosity specimens Prisms 4 × 4 × 16 cycle test28th
were placed in the freeze–thaw curing
machine day the UNI
under 11060:2003
condition [72]
of freezing
Thermal cycles resistance temperature of −20 ◦ C and thawing
Prisms 4 × 4 temperature
× 16 of 5 ◦ C.-Each cycle consisted of: -
Sulphate resistance Prisms
(a) a cooling phase, in which the 4 ×temperature
4 × 16 moved6from 5 ◦ C (±2 ◦ C) to
months UNI
−20 ◦ C ([73]
8019 ±2 ◦ C)
Freeze–thaw resistance Prisms rate of 5 ◦ C/h4(×±40.5
at a constant ◦ C/h);
× 16 300 cycles UNI 7087 [74]
(b) a constant phase in which the temperature was kept constant at −20 ◦ C (±2 ◦ C) for
The
two resistance
hours; of the prepared mortars to freeze–thaw cycles was tested according to
(c) a heating
the relevant phase inreported
standard which the temperature
in Table 3, after returns 5 ◦ C (±
a curingtoperiod ◦ C)
of228 at the
days. same velocity
Saturated spec-
imensaswere
step.placed in the freeze–thaw cycle test machine under the condition of freezing
temperature of −20 °C and thawing temperature of 5 °C. Each cycle consisted of:
 (a) a cooling phase, in which the temperature moved from 5 °C (±2 °C) to −20 °C (±2 °C)
at a constant rate of 5 °C/h (±0.5 °C/h);
(b) a constant phase in which the temperature was kept constant at −20 °C (±2 °C) for
two hours;
Appl. Sci. 2022, 12, 2732 11 of 26
(c) a heating phase in which the temperature returns to 5 °C (±2 °C) at the same velocity
as step.
Mechanical properties and weight loss of specimens after 6 month of exposure to
Mechanical
sulphate solutionsproperties and weight loss of specimens after 6 month of exposure to
were measured.
sulphate
The solutions
resistancewere
of themeasured.
prepared mortars to sulphate was tested according to the rele-
vant The resistance
standard of theinprepared
reported Table 3, mortars to sulphate
after a curing was
period of tested
28 daysaccording to the
by soaking relevant
specimens
standard reported in Table 3, after a curing period of 28 days by soaking
in a solution containing 10% by weight of MgSO4. The sulphate solution was replaced specimens in a
solution containing
every 2 months. 10% by weight of MgSO 4 . The sulphate solution was replaced every
2 months.
The specimens’ flexural and compressive strengths after 300 freeze–thaw cycles and
their The specimens’
weight flexural
loss versus the and compressive
number strengths
of freeze–thaw after expressed
cycles, 300 freeze–thaw cycles and
as a percentage,
their weight
were measured. loss versus the number of freeze–thaw cycles, expressed as a percentage,
wereThe
measured.
thermal stability of the prepared mortars was also investigated by exposing the
prismatic thermal
The specimens,stability
after aofcuring
the prepared
period ofmortars
90 days,was also investigated
at temperatures from by100exposing
°C up◦to
the prismatic
700 °C in steps specimens,
of 100 °C after
in a a curing
muffle period
furnace. of
Each90 days,
thermal at temperatures
cycle consisted from
of a 100 C
soaking
up to 700 ◦ C in steps of 100 ◦ C in a muffle furnace. Each thermal cycle consisted of a
period of 12 h followed by a cooling period of 24 h. The degradation of mechanical prop-
soaking period of 12 h followed by a cooling period of 24 h. The degradation of mechanical
erties was evaluated by the non-destructive ultrasonic reflection technique. The mortars’
properties was evaluated by the non-destructive ultrasonic reflection technique. The
compressive and flexural strengths, after all thermal cycles, were also measured and com-
mortars’ compressive and flexural strengths, after all thermal cycles, were also measured
pared with those obtained with the untreated ones.
and compared with those obtained with the untreated ones.
3.
3. Results
Results and
and Discussion
Discussion
In Figure 7, the workability
In Figure 7, the workability of
of the
the prepared
prepared mortars
mortars is
is reported.
reported.

250
Spread Diameter [mm]

200

150

100

50

0
NSRX RSRX NRPX RSPX
Figure 7. Spreading of thixotropic and self-leveling mortars produced with natural and recycled
Figure 7. Spreading of thixotropic and self-leveling mortars produced with natural and recycled
aggregate.
aggregate.

Both self-leveling and thixotropic mortars produced with RS show only a moderate
Both self-leveling and thixotropic mortars produced with RS show only a moderate
decline in initial workability with respect to control mortars. It can be also observed that
decline in initial workability with respect to control mortars. It can be also observed that the
the decline in spreading value is lower in the case of the thixotropic mortar. As reported by
decline in spreading value is lower in the case of the thixotropic mortar. As reported by
many authors, several factors affect the workability of these types of mortars. A significant
many authors, several factors affect the workability of these types of mortars. A significant
role is played by the RS content, the degree of saturation, the kinetics of water absorption,
role is played by the RS content, the degree of saturation, the kinetics of water absorption,
and the surface texture [53,54]. The chemical kit also has a pivotal role in defining their
and the surface texture [53,54]. The chemical kit also has a pivotal role in defining their fresh
fresh state properties. When dry surface saturated aggregate is used, as in the present
state properties. When dry surface saturated aggregate is used, as in the present investiga-
investigation, the more irregular and rougher surface of RS offers a higher resistance to the
tion, the moremovements,
inter-particle irregular and rougherparticles’
promotes surface of RS offers a and
interlocking, higher resistance
requires moreto the inter-
water to be
particle movements, promotes particles’ interlocking, and requires more water to be
wetted [75]. The presence of adherent cement paste on aggregate, due to its porosity, alsowetted
affects the workability [67]. The resin and surfactant included in the chemical kit of both
the types of mortars limited the loss of workability by a ball bearing action and a dispersing
effect, respectively. The higher amount of cellulose ethers (CE) in the chemical compound
of the thixotropic mortars, used as viscosity enhancing and water retention additive to
prevent the rapid loss of water by suction, hinders the wettability of the surface of recycled
aggregate, thus lowering the gap in the initial mortar workability between NSRX and RSRX
 [75].
[75]. The
The presence
presence of of adherent
adherent cement
cement paste
paste on
on aggregate,
aggregate, duedue toto its
its porosity,
porosity, also also affects
affects
the
the workability [67]. The resin and surfactant included in the chemical kit of both the
workability [67]. The resin and surfactant included in the chemical kit of both the types
types
of
of mortars
mortars limited
limited thethe loss
loss ofof workability
workability by by aa ball
ball bearing
bearing action
action and
and aa dispersing
dispersing effect,
effect,
Appl. Sci. 2022, 12, 2732 respectively.
respectively. TheThe higher
higher amount
amount of of cellulose
cellulose ethers
ethers (CE)
(CE) in
in the
the chemical
chemical compound
compound of ofof
12 the
the
26
thixotropic mortars, used as viscosity enhancing and water retention additive
thixotropic mortars, used as viscosity enhancing and water retention additive to prevent the to prevent the
rapid
rapid loss
loss of
of water
water byby suction,
suction, hinders
hinders thethe wettability
wettability of
of the
the surface
surface of of recycled
recycled aggregate,
aggregate,
thus
thus lowering the gap in the initial mortar workability between NSRX and RSRX mortars.
mortars. The chemical kit used for self-leveling mortars, characterized by a highermortars.
lowering the gap in the initial mortar workability between NSRX and RSRX amount
The
The chemical
chemicalkit
of surfactant kitused
and used for
forself-leveling
a lower amount of mortars,
self-leveling mortars,characterized
cellulose, enhances theby
characterized by aahigher
higheramount
wettability amount of
of recycledofsurfac-
surfac-
sand
tant
tant and a lower
and thus
surface, a lower amount
amount of
decreasing of cellulose,
thecellulose, enhances the
enhances the
initial workability wettability
wettability
in the of recycled
of recycled
RSPX mortar. sand surface,
8 and 9,thus
sand surface,
In Figures thus
the
decreasing
decreasing
evolution of the
the initial
initial workability
compressiveworkability in
in the
and flexural RSPX
RSPX mortar.
thestrengths of theIn
mortar. In Figures 88 and
and 9,
Figuresmortars
prepared the
the evolution
9,with evolution
curing time of
of
compressive
compressive and flexural strengths of the prepared mortars with curing
is reported. and flexural strengths of the prepared mortars with curing time is reported. time is reported.

40
40
NSPX
NSPX
35
[MPa]

35 RSPX
strength[MPa]

RSPX
NSRX
NSRX
30
30 RSRX
RSRX
Compressivestrength

25
25
20
20
Compressive

15
15
10
10
55

00
22 77 28
28 90
90
Time
Time [days]
[days]
Compressive strength vs.
Figure 8.Compressive
Figure vs. curingdays.
days.
Figure8.
8. Compressivestrength
strength vs.curing
curing days.

10
10
NSPX
NSPX
RSPX
RSPX
[MPa]

NSRX
strength[MPa]

NSRX
RSRX
RSRX
Flexuralstrength

55
Flexural

00
22 77 28
28 90
90
Time
Time [days]
[days]
Figure
Figure9.
Figure 9.Flexural
9. Flexuralstrength
Flexural strengthvs.
strength vs.curing
vs. curingdays.
curing days.
days.

The compressive and flexural strengths of thixotropic (RSRX) and self-leveling (RSPX)
mortars are lower than those of the corresponding control mortars made with siliceous sand.
However, RSRX and RSPX show different behaviors, in terms of the extent of compressive
strength decrease. The thixotropic RSRX mortar shows a compressive strength 15% lower
than the reference mortar after two days of curing. The gap increases to around 40% after
seven curing days and then remains stable for a longer curing time. The self-leveling
RSPX mortar shows a limited compressive strength gap compared to the control mortar,
varying from 11% to 6% with curing time. As reported by several investigations [76–80],
Appl. Sci. 2022, 12, 2732 13 of 26

the reduction in mechanical properties in mortars produced using recycled aggregate can
be caused by:
• the poorer mechanical properties of recycled sand in comparison to the natural sand
used;
• the higher porosity of recycled sand;
• the presence of adherent cement paste on aggregate;
• the moisture conditions of aggregate;
• a weaker interfacial transition zone (ITZ).
As evidenced in Figures 1A and 2, the recycled sand, mainly composed by particles of
mortar and concrete, shows micro-cracks occurring at the weaker interfacial transition zone
(ITZ) because of the crushing process. They modestly participate, through the so-called
“ceiling effect” [56], to lower the strength of the RSRX and RSPX mortars, in comparison to
those with natural aggregates [81,82].
The chemical kit has an important role in explaining the different behavior of the two
type of mortars with recycled sand.
It contains sulphoaluminate cement in the case of the thixotropic mortars, which has
been partially replaced by metakaolin in the mix used to produce the self-leveling mortars.
Sulphoaluminate cement (CSA cement), used to provide a shorter setting time [83,84]
and to lower the overall shrinkage, reacts according the following reaction:

3CaO·1Al2 O3 ·6H2 O + 3(CaSO4 ·2H2 O) + 19H2 O = 3CaO·1Al2 O3 ·3CaSO4 ·31H2 O (1)

The main hydration product of CSA cement is AFt (cf. Equation (1)). Its generation
process requires a high amount of water.
Metakaolin reacts with the calcium hydroxide produced by the cement hydration
reaction, which already exists in both the adherent cement paste on recycled aggregate and
the recycled aggregate itself, as highlighted by X-Ray diffraction analysis (Figure 4). The
pozzolanic reaction produces calcium silicate hydrate, thus increasing the density of the
matrix especially the transition zone area between recycled aggregates and cement mortar
and filling the porosity and the cracks of recycled aggregates, as revealed by Torkittikul
and Chaipanich [85] and Zhao et al. [66].
The use of cellulose ethers (CE) and sulphoaluminate cement in the mix design of RSRX
leads to an initial water retention, followed by faster consumption which produces expan-
sive Aft. The addition of calcium formate reduces set times and improves early strengths
by accelerating C-S-H formation. It is useful in repair systems, but further contributes to
the fast water consumption. As an overall consequence, the wettability of adherent cement
paste on recycled aggregate is partially hindered, the micro-cracks occurring in recycled
aggregate can widen, the porosity increases, and mechanical performances decline.
In the chemical compound used for RSPX, the calcium formate is replaced by lithium
carbonate, commonly used in the production of the self-leveling system, which only
promotes fast setting. The partial replacement of sulphoaluminate cement with metakaolin
leads to the reduced formation of expansive Aft and the densification of the transition zone
in the recycled aggregates and between the cement paste and the recycled aggregate [85].
Therefore, the pore structure is improved, enhancing the mechanical performances, as
reported in Figures 8 and 9.
The porosity of the produced mortars was measured to validate the proposed explana-
tion. Porosity is defined as the fraction of the total volume that is occupied by pores. It can
be further classified into open porosity and closed porosity [86]. The difference between
them is the interconnection of pores. The measure porosities are reported in Table 4.
 The porosity of the produced mortars was measured to validate the proposed expla-
nation. Porosity is defined as the fraction of the total volume that is occupied by pores. It
Appl. Sci. 2022, 12, 2732 can be further classified into open porosity and closed porosity [86]. The difference between
14 of 26
them is the interconnection of pores. The measure porosities are reported in Table 4.

Table 4. Open and total porosity of tested mortars.

Table 4. Open and total porosity of tested mortars.
Mixes Open Porosity (%) Total Porosity (%)
Mixes Open Porosity (%) Total Porosity (%)
NSPX 17.3% 25.8%
NSPX 17.3% 25.8%
RSPXRSPX 20.3% 20.3%
32.6%32.6%
NSRXNSRX 20.5% 20.5% 28.8%28.8%
RSRXRSRX 23.5% 23.5% 35.56%35.56%

The
The higher
higher porosity
porosity of of the
the NSRX
NSRX thanthan NSPX
NSPX can can be
be attributed
attributed toto the
the entrapped
entrapped air air
due to the lower workability of the thixotropic mortar that can promote
due to the lower workability of the thixotropic mortar that can promote air entrapping. air entrapping.
The
The RSRX
RSRX and
and RSPX
RSPX mortars
mortars show
show higher
higher open
open andand total
total porosities
porosities than
than NSRX
NSRX and and NRPX
NRPX
mortars, used as the control. Furthermore, the RSRX mortar has higher
mortars, used as the control. Furthermore, the RSRX mortar has higher porosity than RSPX. porosity than
RSPX. The obtained results are consistent with the measured mortars’
The obtained results are consistent with the measured mortars’ mechanical performances mechanical perfor-
mances
because,because, as expected,
as expected, greater porosity
greater porosity is associated
is associated with lower with lower strengths.
strengths.
The
The drying
drying shrinkage
shrinkageof ofthe
theprepared
preparedmortars
mortarsoveroverearly curing
early curingtime
timeis reported
is reported in
Figure 10.10.
in Figure All All
specimens
specimens experienced
experienced a continuous
a continuous increase in shrinkage
increase during
in shrinkage the test
during the
period, withwith
test period, a fairly rapid
a fairly growth
rapid during
growth the first
during curing
the first curingdays, followed
days, followedby aby slower in-
a slower
crease. Compared to the control mortars NSPX and NSRX,
increase. Compared to the control mortars NSPX and NSRX, the RSPX and RSRX the RSPX and RSRX mortars
show a shrinkage increase of 13.5% and 23.1%, respectively, after 28 days of curing. curing. As
expected, greater porosity leads total larger drying shrinkage. Similar Similar results
results are reported
in scientific literature by Mao et al. [87]. The frost resistance of mortars produced using
recycled aggregate
aggregatehas hasbeen
beeninvestigated
investigated ininrecent papers
recent paperswith divergent
with divergentresults that that
results can
be
canaddressed
be addressedto both the variability
to both of the
the variability of quality of the
the quality of recycled aggregate
the recycled and and
aggregate the dif-
the
ferent employed
different employed methods
methods [88–92]. In order
[88–92]. to further
In order contribute
to further to scientific
contribute literature,
to scientific the
literature,
prepared mortars
the prepared mortars were
weretested to to
tested freezing
freezing and
andthawing
thawingresistance.
resistance.Mechanical
Mechanical properties
properties
measured after
were measured after300300freeze–thaw
freeze–thaw(F-T) (F-T)cycles,
cycles,using
using the
the properties
properties of of mortars
mortars after
after 90
90 days
days of curing,
of curing, corresponding
corresponding withwith Figures
Figures 11 11
andand
12.12.

1200

1000
Shrinkage [με]

800

600

400 NSRX
RSRX
RSPX
200 NSPX

0
0 5 10 15 20 25 30
Time [days]

Figure 10.
Figure The mortars’
10. The mortars’ drying
drying shrinkage
shrinkage vs.
vs. curing
curing days.
days.
Appl. Sci.
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FOR PEER
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26

50
50
Ref.
Ref. 90d
90d

[MPa]
After
After 300
300 freeze-thaw
freeze-thaw cycles

strength [MPa]
cycles
40
40

Compressive strength
30
30
Compressive
20
20

10
10

00
NSPX
NSPX RSPX
RSPX NSRX
NSRX RSRX
RSRX

Figure 11.
Figure 11. The
The mortars’ compressive strength
mortars’ compressive strength after
after 300
300 F-T
F-T cycles.
cycles.

10
10
Ref.
Ref. 90d
90d
After
After 300
300 freeze-thaw
freeze-thaw cycles
cycles
[MPa]
strength [MPa]
Flexural strength

55
Flexural

00
NSPX
NSPX RSPX
RSPX NSRX
NSRX RSRX
RSRX
Figure 12. The mortars’ flexural strength after 300 F-T cycles.
Figure
Figure 12.
12. The
The mortars’
mortars’ flexural
flexural strength
strength after
after 300
300 F-T
F-T cycles.
cycles.
The final variation in the weight and mechanical performances is reported in Table 5.
The final variation in the weight and mechanical performances is reported in Table 5.
Table 5. The weight and mechanical properties variation after freeze–thaw cycles and sulphate attack.
Table
Table 5.5. The
The weight
weight and
and mechanical
mechanical properties
properties variation
variation after
after freeze–thaw
freeze–thaw cycles
cycles and
and sulphate
sulphate
attack.
attack. Attack (6 Months)
Sulphate Freeze–Thaw Cycles (300 Cycles)
Mixes ∆ Weight ∆ Flexural ∆ Compressive
Sulphate Attack (6 Months) Penetration ∆ Weight ∆ Flexural
Freeze–Thaw ∆ Compressive
Cycles (300 Cycles)
Mixes (%)
Δ WeightStrength (%) Strength (%) [cm] (%)
Δ Flexural Δ Compressive Penetration Δ Weight Strength (%)
Δ Flexural Strength (%)
Δ Compressive
Δ Weight Δ Flexural
Δ Compressive Penetration Δ Weight Δ Flexural Δ Compressive
NSPX −16.9%(%) −
Strength
63.0% (%) −80.6% (%)
Strength [cm]
1.5 −(%)
1.0% −9.6%(%)
Strength −10.0%(%)
Strength
RSPX
NSPX −15.8%
−16.9% −55.1%
−63.0% −79.3%
−80.6% 1.7
1.5 − 1.0%
−1.0% − 11.6%
−9.6% −10.4%
−10.0%
NSRX −12.5% −69.4% −86.1% 1.1 −1.7% −9.7% −9.8%
RSPX
RSRX
−15.8%
−11.7% −55.1%
−61.8% −79.3%
−77.1% 1.7
1.2
−1.0%
− 1.2%
−11.6%
−14.0% −10.4%
−18.1%
NSRX −12.5% −69.4% −86.1% 1.1 −1.7% −9.7% −9.8%
RSRX −11.7% −61.8% −77.1% 1.2 −1.2% −14.0% −18.1%
The freezing and thawing resistance of RSPX is similar to that of the control mortar.
The greater porosity
The freezing andthat arisesresistance
thawing from the ofincorporation of the
RSPX is similar to recycled
that of theaggregate favors
control mortar.
the dissipation
The of hydraulic
greater porosity pressures.
that arises from theOnly when the voids
incorporation system
of the is soaggregate
recycled developed that
favors
a significant decline in the initial mechanical properties can be determined,
the dissipation of hydraulic pressures. Only when the voids system is so developed that as for RSRX
amortar, a slightly
significant reduced
decline in theresistance to F-T cycles
initial mechanical is observed.
properties can beThe present investigation
determined, as for RSRX
outcome confirms some previously reported findings [92–97].
mortar, a slightly reduced resistance to F-T cycles is observed. The present investigation
A sulphate
outcome confirms attack
someispreviously
also a major concernfindings
reported for the durability
[92–97]. of construction. Sulphate-
rich environments expose mortar and concrete to expansion and degradation due to the
A sulphate attack is also a major concern for the durability of construction. Sulphate-rich
formation of ettringite. It causes high internal stresses, leading to an extended cracking
environments expose mortar and concrete to expansion and degradation due to the formation
pattern [98,99].
of ettringite. It causes high internal stresses, leading to an extended cracking pattern [98,99].
Appl.
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26

The
The literature
literature regarding
regarding recycled
recycled aggregate
aggregate mortar
mortar and
and concrete
concrete performance
performance against
against
external sulphate attack (ESA) is not conclusive. This is mainly due to
external sulphate attack (ESA) is not conclusive. This is mainly due to the several param-the several pa-
rameters involved in ESA. Kazmi et al. [30] replaced the coarse fraction of
eters involved in ESA. Kazmi et al. [30] replaced the coarse fraction of concrete with recy-concrete with
recycled aggregate
cled aggregate and and
testedtested specimens
specimens after after 60 days
60 days of immersion
of immersion in sulfate
in sulfate solution.
solution. They
They reported a lower resistance of recycled aggregate concrete (RSC)
reported a lower resistance of recycled aggregate concrete (RSC) compared to the controlcompared to the
control one in
one in light of light of the sulphate
the sulphate attack, causing
attack, causing strengthstrength
losses oflosses of around
around 26% and26%20%,and 20%,
respec-
respectively. They attributed
tively. They attributed the findings
the findings to theto the higher
higher porosity
porosity and water
and water absorption
absorption of
of RSC,
RSC, leading to higher sulphate ion penetration. However, some studies
leading to higher sulphate ion penetration. However, some studies present a similar or present a similar
or even better performance for RSC than for natural aggregate mortar and concrete (NSC).
even better performance for RSC than for natural aggregate mortar and concrete (NSC).
Dhir et al. [100] reported that the exposure to a sulphate solution has a negative effect only
Dhir et al. [100] reported that the exposure to a sulphate solution has a negative effect only
for RSC with replacement ratios higher than 30%. Bulatovic et al. [101] reported that RSC
for RSC with replacement ratios higher than 30%. Bulatovic et al. [101] reported that RSC
with 100% replacement shows worse performance than NSC against ESA only when a high
with 100% replacement shows worse performance than NSC against ESA only when a
water-cement ratio (w/c = 0.55) and a non-sulphate-resistant cement were used.
high water-cement ratio (w/c = 0.55) and a non-sulphate-resistant cement were used.
Since the scientific community has reached no consensus by now, the prepared mortars
Since the scientific community has reached no consensus by now, the prepared mor-
have been tested for sulphate attack.
tars have been tested for sulphate attack.
After an immersion period of 6 months, all the mortars experience a significant loss
After an immersion period of 6 months, all the mortars experience a significant loss
of mechanical properties (see Figures 13 and 14) that is explained by following reactions
of mechanical properties (see Figures 13 and 14) that is explained by following reactions
[102,103]:
[102,103]:
• the formation of gypsum (calcium sulphate dihydrate), leading to softening and loss
• theconcrete
of formation of gypsum (calcium sulphate dihydrate), leading to softening and loss
strength:
of concrete strength:
Ca(OH)2 + Na2 SO4 ·10H2 O = CaSO4 ·2H2 O + 2NaOH + 8H2 O (2)
Ca(OH)2 + Na2SO4⋅10H2O = CaSO4⋅2H2O + 2NaOH + 8H2O (2)
• The higher amount of gypsum converts tricalcium aluminate (C3A) in the mortars
• The higher amount of gypsum converts tricalcium aluminate (C3A) in the mortars to
to ettringite (calcium aluminate trisulphate). The expansive reaction leads to high
ettringite (calcium aluminate trisulphate). The expansive reaction leads to high inter-
internal stresses and cracking:
nal stresses and cracking:
3CaO·1Al2 O3 + 26H2 O + 3(CaSO4 ·2H2 O) = 3CaO·1Al2 O3 ·3CaSO4 ·32H2 O (3)
3CaO⋅1Al2O3 + 26H2O + 3(CaSO4⋅2H2O) = 3CaO⋅1Al2O3⋅3CaSO4⋅32H2O (3)

50
Ref. 90d
After sulphate attack
Compressive strength [MPa]

40

30

20

10

0
NSPX RSPX NSRX RSRX
Figure 13. The mortars’ compressive strength after 6 months of immersion in sodium sulphate
Figure 13. The mortars’ compressive strength after 6 months of immersion in sodium sulphate solution.
solution.
Appl. Sci. 2022, 12, x FOR PEER REVIEW 17 of 26
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Appl.Sci. 2022,12,
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x FOR PEER REVIEW 17 of 26
17 26

10
Ref. 90d
10
After90d
Ref. sulphate attack

[MPa]
After sulphate attack

strength [MPa]
strength 5
5
Flexural
Flexural

0
NSPX RSPX NSRX RSRX
0
NSPX
Figure 14. The RSPX
mortars’ flexural NSRX
strength after RSRX
6 months of immersion in in sodium sulphate solution.
Figure 14. The mortars’ flexural
Figure 14. flexural strength
strengthafter
after66months
monthsofofimmersion
immersionininininsodium
sodiumsulphate
sulphate solution.
solution.
Notably, RSPX and NSPX showed a similar loss of compressive strength (Table 5),
whereasNotably,
RSRXRSPX
Notably, mortar
RSPX and
and NSPX
NSPXashowed
showed aa similar
similar loss
better performance
showed loss of
of compressive
than the control mortar
compressive strength
strength (Table
(Table 5),
(NSRX). 5),
whereas The RSRX
recycledmortar showed
aggregate a
usedbetter
in performance
the present than
campaign
whereas RSRX mortar showed a better performance than the control mortar (NSRX). the control
is mainlymortar (NSRX).
composed by ce-
The
Therecycled
mentitious compounds
recycled aggregate
aggregate used
(concretes
used in in
the
and present
themortars),campaign
present as wellisas
campaign mainly composed
materials
is mainly of by cementi-
ceramic
composed origin
by ce-
tious compounds
(brick), as evidenced
mentitious compounds (concretes and
by (concretes
EXD and X-Ray mortars), as well
analyses.as
and mortars), as materials
Therefore, of ceramic
mortars produced
well as materials origin
of ceramic (brick),
with the
origin
as evidenced
recycled
(brick), by EXDcontain
asaggregate
evidenced and
by EXDX-Ray
more
and analyses.
Portland
X-Ray Therefore, mortars produced
cementTherefore,
analyses. hydration products
mortars with
which
produced the can
recycled
withreact
the
aggregate
with contain
external more
sulfate. Portland
Furthermore, cement
as hydration
reported in products
Table 4,
recycled aggregate contain more Portland cement hydration products which can react which
RSPX can
and react
RSRX with
mortarsexternal
show
sulfate.
increased Furthermore,
with external overall
sulfate. as reported
porosities that in
Furthermore, Table
favor and4, RSPX
as reported inand
accelerate
TableRSRX
the mortars
4, ESA
RSPX andshow
kinetics.
RSRX Theincreased
obtained
mortars over-
showre-
all porosities
sults, thus, that
cannot favor
be and accelerate
explained based the
on ESA
only kinetics.
these The obtained
considerations
increased overall porosities that favor and accelerate the ESA kinetics. The obtained re- results,
and thus,
further cannot
contribu-
be explained
tions
sults, based
participate
thus, cannot onexplained
to be
defineonly these
the considerations
observed
based behavior.
on only theseandconsiderations
furthertocontributions
According authors,andbecause participate
further ESA to
dam-
contribu-
define the observed
age isparticipate
tions mainly due behavior.
to to According
the formation
define the observed to authors,
of expansive because
products in
behavior. According ESA damage
toconfined is mainly
pores, greater
authors, because due
ESA dam- to
po-
the formation
rosity of
can helpdue expansive
to to
reduce products
the internal in confined pores,
restrictionproducts greater porosity
of mortarintoconfined can
deform pores, help to
and decrease reducethe
age is mainly the formation of expansive greater po-
the internalinternal
generated restriction of mortar
stresses. The to deform
capacity of and decrease
mortar and the generated
concrete produced internal
with stresses.
recycled
rosity can help to reduce the internal restriction of mortar to deform and decrease the
The capacity
aggregate toof mortar
relief and concrete
stresses produced with recycled aggregate to relief stresses due
generated internal stresses.dueTheto their
capacity high porosity
of mortar andhasconcrete
been also reported
produced by Santillán
with recycled
to their high
et al. [104] to porosity
and Boudali has been
et al. also
[105]. reported by Santillán et al. [104] and Boudali et al. [105].
aggregate relief stresses due to their high porosity has been also reported by Santillán
Figure 1515shows the cross-section ofof
specimens exposed to to
sulphate attack post bending
et al.Figure
[104] and shows
Boudali theetcross-section
al. [105]. specimens exposed sulphate attack post bend-
test and
ing test after
and using
after BaCl
using +KMnO
2 2+KMnO
BaCl solutions [106] to measure the sulphate
4 4 solutions [106] to measure the sulphate penetration penetration
Figure 15 shows the cross-section of specimens exposed to sulphate attack post bend-
depth
depth (Table 5).
ing test(Table 5). using BaCl2+KMnO4 solutions [106] to measure the sulphate penetration
and after
depth (Table 5).

Figure15.
Figure 15.Sulphate
Sulphatepenetration
penetrationdepth
depthinintested
testedmortars,
mortars,using BaCl2++ KMnO
using BaCl KMnO4 solutions
solutions and
and after
after66
2 4
months
Figure of Sulphate
15. immersion in a sodium
penetration sulphate
depth in solution.
tested mortars,using BaCl + KMnO solutions and after 6
months of immersion in a sodium sulphate solution. 2 4

months of immersion in a sodium sulphate solution.

Appl. Sci. 2022, 12, 2732 18 of 26

Recycled aggregate mortars show greater ion penetration depth than the control
ones (Table 5). This can be explained by their higher open porosity. Interestingly, self-
leveling mortars show higher sulphate ion penetration depths than the more porous
thixotropic mortars. An important role in the observed behaviour can be attributed
Appl. Sci. 2022, 12, x FOR PEER REVIEW to
18 of 26
a different efficiency in the redispersible powder dispersion. During mixing, polymer
particles firstly disperse in the cement paste. As cement hydration proceeds and capillary
water is consumed, the polymer particles flocculate to form a close-packed layer on the
Recycled aggregate mortars show greater ion penetration depth than the control ones
surfaces of capillary pores that can also effectively block the transportation of invasion ions
(Table 5). This can be explained by their higher open porosity. Interestingly, self-leveling
based on the continuity polymer network [27]. The continuity polymer network depends
mortars show higher sulphate ion penetration depths than the more porous thixotropic
on the amount and dispersion of the redispersible powder.
mortars. An important role in the observed behaviour can be attributed to a different ef-
The exposure of cementitious materials to high temperatures, as it occurs during a fire,
ficiency in the redispersible powder dispersion. During mixing, polymer particles firstly
deteriorates their mechanical properties and affects their durability. The main causes of this
disperse
decline can in be
theascribed
cementto paste. As cement hydration
the decomposition of hydrates,proceeds and capillary
the coarsening water
of porous is con-
structure,
sumed, the polymer particles flocculate to form a close-packed
thermal cracking induced by water vapor pressure, and thermal mismatches [107,108]. The layer on the surfaces of
capillary pores that can
last two mechanisms also effectively
considerably dependblockonthe
thetransportation
type of aggregateof invasion
used in ions based
mortars on
[109].
the continuity polymer network [27]. The continuity polymer
Therefore, the thermal degradation characteristics of the prepared recycled aggregate network depends on the
amount
mortars and anddispersion
the control ofones
the redispersible powder.
were investigated by exposing the prismatic specimens,
after a curing period of 90 days, up to 700 to
The exposure of cementitious materials ◦ Chigh temperatures,
in steps of 100 ◦ Cas initaoccurs
muffleduring
furnace. a
fire, deteriorates their mechanical properties and affects their durability.
Each thermal cycle consisted of a soaking period of 12 h followed by a cooling period of The main causes
of
24this decline
h. The can be ascribed
degradation of the to the decomposition
physical and mechanical of hydrates, thewas
properties coarsening
evaluatedof porous
by the
structure, thermal
non-destructive cracking reflection
ultrasonic induced by water vapor
technique (Figurepressure,
16) andand thermal
weight lossmismatches
(Figure 17).
[107,108].
UltrasonicThe last two mechanisms
non-destructive considerably
testing (NDT-UT) dependestimate
techniques on the type of aggregate
the quality usedand
of mortar in
mortars [109]. Therefore, the thermal degradation characteristics of
concrete by measuring the propagation velocity of the ultrasonic wave [110]. Its magnitude the prepared recycled
aggregate
depends on mortars and the density
the material’s control ones
or thewere
poreinvestigated
volume fraction; by exposing theclosely
thus, it is prismatic spec-
related to
imens, after a curing
their mechanical period and
properties of 90modulus
days, upof toelasticity
700 °C in[2]. steps of 100 °C in a muffle furnace.
Each Thethermal cycle consisted
propagation velocities of aofsoaking period of
the ultrasonic 12 hmeasured
wave followed by on aspecimens
cooling period
at room of
24 h. The degradation
temperature and reported of the physical
in Figure andconsistent
16 are mechanical withproperties
porosity andwasmechanical
evaluated proper-
by the
non-destructive
ties of the prepared ultrasonic
mortars.reflection technique
In particular, (Figure 16)
a 5% difference and weight
between NSPXloss and (Figure
RSPX and 17).a
Ultrasonic non-destructive testing (NDT-UT) techniques estimate
14% difference between NSRX and RSRX propagation pulse velocities (UPV) have been the quality of mortar
and
found.concrete
As theby measuringincreases
temperature the propagation
(Figure velocity
16), all theof mortar
the ultrasonic
experiencewave [110]. Its in
a decrease mag-
the
nitude depends
propagation on the
velocity as amaterial’s
consequence density orthermally
of the the pore induced
volume damage.
fraction; Four
thus, temperature
it is closely
related
intervals tocan
their bemechanical
distinguished.properties and modulus of elasticity [2].

4500
NSPX
RSPX
4000 NSRX
RSRX
3500
Velocity [ms−1]

3000

2500

2000

1500

1000

500
0 100 200 300 400 500 600 700 800
Temperature [°C]
Figure 16.
Figure Propagation velocities
16. Propagation velocities of
of ultrasonic
ultrasonic pulse
pulse vs.
vs. temperature
temperature for
for the
the tested
tested mortars.
mortars.
Appl.
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26

550
NSPX
RSPX
NSRX
RSRX
500

Weight [g]
450

400

350
0 100 200 300 400 500 600 700 800
Temperature [°C]
Figure17.
Figure Weightof
17.Weight ofspecimens
specimensvs.
vs.temperature
temperaturefor
forthe
thetested
testedmortars.
mortars.

Interval 25–100 ◦ C: the integrity of the specimen structure is close to that at room
The propagation velocities of the ultrasonic wave measured on specimens at room
temperature. At these temperatures, the free water or capillary water inside the concrete are
temperature and reported in Figure 16 are consistent with porosity and mechanical prop-
heated to evaporate and form water vapors. NSPX and NSRX mortars show a decrease in
erties of the prepared mortars. In particular, a 5% difference between NSPX and RSPX and
weight of 0.2% and 2%, respectively, which is lower than that of the corresponding mortars
a 14% difference between NSRX and RSRX propagation pulse velocities (UPV) have been
produced with recycled aggregate equal to 1.2% (RSPX) and 4.4% (RSRX) (Figure 17).
found. As the temperature increases (Figure 16), all the mortar experience a decrease in
This can be ascribed to the greater difficulty for water vapors to escape in more densely
the propagation velocity as a consequence of the thermally induced damage. Four tem-
structured mortars [107]. The steeper decrease in UPV measured for RSPX (around 13%)
perature
and RSRX intervals can be distinguished.
(9.3%) mortars can be explained by the greater ease of water vapor to escape in
mortars that are more°C:
Interval 25–100 the integrity
porous and of theoffine-cracks
the specimen structure
to develop, is close
under vapor to pressure,
that at room from
temperature. At these temperatures, the free
original defect of the recycled aggregate at pore boundaries.water or capillary water inside the concrete
are heated to evaporate
Interval 100–400 ◦ C: andtheform water water
capillary vapors. NSPX and
continues to NSRX mortars
evaporate. show
Resins a decrease
used as addi-
in weight of 0.2% and 2%, respectively, which is lower than that
tive are thermally degraded. Furthermore, several reactions occur in the cement matrix. of the corresponding
mortars
Ettringiteproduced
(AFt) is with recycled
thermally aggregate [110];
decomposed equal the
to 1.2% (RSPX) and 4.4% (RSRX) (Figure
dehydration–dehydroxylation of cal-
17). This can be ascribed to the greater difficulty
cium silicate hydrate (C–S–H gel) cause the loss of crystal water and for water vapors to escape
an increase in more
in structural
densely
porosity.structured
The loss ofmortars
bonded[107].waterThe steeper
results in andecrease
increasedinweightUPV measured
loss for all for
the RSPX
tested
(around
mortars,13%)largerand forRSRX (9.3%)
mortars mortarswith
produced can be explained
recycled by the greater
aggregate (5.6% for ease of water
RSPX va-
vs. 3.5%
por
for to
NRPXescapeandin10.4%
mortarsfor that
RSRX are
vs.more
9.8%porous and of
for NRSX). Thisthefinding
fine-cracks
can be toexplained
develop, underby the
vapor pressure,
following from original defect of the recycled aggregate at pore boundaries.
processes:
• Interval 100–400 °C: the capillary water
The dehydration–dehydroxylation continues
of calcium to hydrate
silicate evaporate. Resins
(C–S–H used
gel) as addi-
in RSPX and
tive are thermally degraded. Furthermore, several reactions occur
RSRX mortars not only involves the cement matrix, but also the recycled aggregate, in the cement matrix.
Ettringite
mainly(AFt) is thermally
composed decomposed
by concrete rubble.[110]; the dehydration–dehydroxylation of cal-
cium
• The higher amount of water vaporthe
silicate hydrate (C–S–H gel) cause loss of crystal
produced waterescape
can easily and an inincrease
the more inporous
struc-
tural structures
porosity. The loss of bonded water results
of mortars produced with recycled aggregate. in an increased weight loss for all the
tested mortars, larger for mortars produced with recycled aggregate (5.6% for RSPX vs.
In this temperature range, a significant decrease in UPV is observed for all the mortars.
3.5% for NRPX and 10.4% for RSRX vs. 9.8% for NRSX). This finding can be explained by
However, it is steeper for mortars produced with natural sand (28.9% for RSPX vs. 36.9%
the following processes:
for NRPX and 30.8% for RSRX vs. 37.1% for NRSX). This can be ascribed to their denser
•structure
The dehydration–dehydroxylation
which hinders the migration of ofwater
calcium silicate
vapors thathydrate (C–S–H
are blocked andgel) in RSPX
accumulated
and
in the RSRX
pores. Themortars not vapor
increased only involves
pressurethe on cement matrix, but
pore boundaries also the
favors the formation
recycled aggre-
of fine
gate,
cracks. mainly composed by concrete rubble.
• The higher
Interval amount
400–500 ◦ C:of
thewater vaporofproduced
reactions can easily escape in the
dehydration–dehydroxylation more porous
of calcium silicate
structures of mortars produced with recycled aggregate.
hydrate (C–S–H gel) continue, and most of the calcium hydroxide (CH) decomposes into
calcium oxide
In this (CaO) [111,112].
temperature range, The overall processes
a significant decreaselead in UPVto anisincrease
observed infor
weight loss
all the and
mor-
the formation of cracks in the mortar which determine a further
tars. However, it is steeper for mortars produced with natural sand (28.9% for RSPX vs.lowering of measured UPV.
No relevant
36.9% for NRPX deviations
and 30.8% in theforbehavior
RSRX vs. of 37.1%
mortars forare observed
NRSX). This can be ascribed to their
 denser
denser structure
structure whichwhich hinders
hinders the the migration
migration of of water
water vapors
vapors thatthat are
are blocked
blocked and and accu-
accu-
mulated
mulated in in the
the pores.
pores. The The increased
increased vaporvapor pressure
pressure on on pore
pore boundaries
boundaries favorsfavors thethe for-
for-
mation
mation of of fine
fine cracks.
cracks.
Interval
Interval 400–500
400–500 °C: °C: the
the reactions
reactions of of dehydration–dehydroxylation
dehydration–dehydroxylation of of calcium
calcium silicate
silicate
hydrate
hydrate (C–S–H
(C–S–H gel) gel) continue,
continue, and and most
most of
of the
the calcium
calcium hydroxide
hydroxide (CH) (CH) decomposes
decomposes into into
Appl. Sci. 2022, 12, 2732 calcium
calcium oxide
oxide (CaO)
(CaO) [111,112].
[111,112]. TheThe overall
overall processes
processes lead lead to
to an
an increase
increase in in weight
weight loss
loss and
20 of 26
and
the
the formation
formation of of cracks
cracks in in the
the mortar
mortar which
which determine
determine aa further
further lowering
lowering of of measured
measured
UPV.
UPV. No No relevant
relevant deviations
deviations in in the
the behavior
behavior of of mortars
mortars areare observed
observed
Interval
Interval 500–700
500–700 °C: ◦ C:the
°C: thereactions
the reactionsof
reactions ofdehydration–dehydroxylation
of dehydration–dehydroxylation of
dehydration–dehydroxylation of calcium
calcium silicate
silicate
hydrate (C–S–H
hydrate (C–S–H
(C–S–Hgel) gel) involves
gel)involves
involvesthethe inner
theinner
innerregion
region
region of specimens.
of of
specimens.
specimens. At about
At about 570 °C,
570 570
At about ◦
the
°C, the α/β
thetran-
C,α/β tran-
α/β
sition
sition in
in the
transition thein siliceous
siliceous
the siliceous aggregates
aggregates
aggregates occurs
occurs with its
its related
withwith
occurs related sudden
sudden
its related volumetric
suddenvolumetric
volumetric expansion
expansion
expan-
[113].
[113]. At
At about
sion [113]. At 650
about 650
about°C,
°C,650 the ◦thermal
the thermal decomposition
decomposition
C, the thermal of
of calcium
decompositioncalcium ofcarbonate
carbonate (CaCO
(CaCO33)) produced
calcium carbonate produced
(CaCO3 )
carbon
carbon
produced dioxide
dioxide
carbon (CO
(CO 22)) starts
dioxide starts
(CO[112].
[112].
2 ) The
The
starts thermal
thermal
[112]. expansion
Theexpansion
thermal mismatch
mismatch
expansion between
between
mismatch the
the different
different
between the
minerals
different of
minerals of the
the natural
minerals natural
of the and
and recycled
recycled
natural andaggregate
recycled and
aggregate and cement
cement
aggregate andmatrix,
matrix,
cementthe thermal
thematrix,
thermalthe expansion
expansion
thermal
anisotropy
anisotropy within
within individual
expansion anisotropy within minerals,
individual minerals,
individual and
and the
the thermal
minerals,thermal
and thedecomposition
decomposition of
of several
thermal decompositionseveral compo-
compo-
of sev-
nents of
of the
the mortars
eral components
nents mortars of theand stress
stress concentration
andmortars due
due to to water
and stress concentration
concentration waterduevapor
vapor to reduce
reduce the
the compactness
water vapor reduce the
compactness
of all
all the
the mortars.
compactness
of of all the mortars.
mortars.
The
The residual
residual mechanical properties
mechanical properties
propertiesof of mortars
ofmortars
mortarsafterafter the
afterthe thermal
thethermal
thermal cycles
cycles
cycles are
are
are reported
reported
reported in
Figures
in
in Figures
Figures 1818 and
18 and
and19.19.
19.

10
10
Ref.
Ref. 90d
90d
After
After thermal
thermal cycles
cycles
Flexural strength [MPa]

55

00
NSPX
NSPX RSPX
RSPX NSRX
NSRX RSRX
RSRX
Figure
Figure 18.
18. Flexural
Flexural strength
strength vs.
vs. temperature
temperature for
for the
the tested
tested mortars.
mortars.

50
50
Ref.
Ref. 90d
90d
After
After thermal
thermal cycles
Compressive strength [MPa]

cycles
40
40

30
30

20
20

10
10

00
NSPX
NSPX RSPX
RSPX NSRX
NSRX RSRX
RSRX
Figure 19.
Figure Compressive strength
19. Compressive strength vs.
vs. temperature
temperature for
for the
the tested
tested mortars.
mortars.

Table 6 summarizes the variations in the weight and mechanical properties after
thermal cycles.
The reduction in mechanical performances of the tested mortars containing 100% RS
after exposure to thermal cycles up to 700 ◦ C is comparable to that obtained for the control
mortars, thus supporting the findings of Sarhat et al. [114] and Khaliq and Taimur [115].
Appl. Sci. 2022, 12, 2732 21 of 26

Table 6. Variations in the weight and mechanical properties after thermal cycles.

Mixes ∆ Weight (%) ∆ Compressive Strength (%) ∆ Flexural Strength (%)

NSPX −5.5% −49.9% −52.1%
RSPX −8.7% −61.5% −55.6%
NSRX −14.9% −21.8% −44.4%
RSRX −19.2% −19.0% −40.7%

4. Conclusions
In this study, authors produced self-leveling and thixotropic mortars using 100%wt
of recycled aggregate. Their physical and mechanical properties and their durability
were investigated and compared with the control mortars. The following outcomes are
stated below.
• The use of pre-saturated RS prevented the absorption of free water during the mixing.
The workability of RSRX and RSPX mortars was 6% and 12% lower than that of the
control mixes, respectively.
• The thixotropic and self-leveling mortars produced with recycled aggregate showed
porosities of 35.6% and 32.6%, respectively. The higher porosity affected both their
drying shrinkage behaviour and mechanical properties. In particular, RSRX mortars
showed an increase of 23.1% in the drying shrinkage and a loss of about 40% in the
compressive strength compared to the control mortar. RSPX mortar showed a loss of
about 6% in the compressive strength and an increase of 13.5% in the drying shrinkage
with respect to the control mix. The variation in properties was more pronounced in
the thixotropic mortars, where the chemical additives contributed to the fast water
consumption that partially hindered the wettability of adherent cement paste on
recycled aggregate.
• After 300 freeze–thaw (F-T) cycles, RSRX and RSPX mortars, respectively, lost 11.6%
and 14% of their initial compressive strength. Their greater porosity favours the
dissipation of hydraulic pressures, resulting in a freezing and thawing resistance that
is comparable to that of the control mortars, which experienced a loss of strength of
about 10%.
• After a period of 6 months under sulphate attack, the self-leveling and thixotropic
mortars with recycled aggregate showed a loss of compressive strength of about 55%
and 62% respectively. Conversely, the decrease in the corresponding control mixes was
63% and 69%, respectively. The greater extent of porosity in RSRX and RSPX mortars,
even favouring the ESA kinetics, reduces the internal restriction of mortar to deform
and the generated internal stresses due to the formation of expansive products.
• The decline in the mortars’ compressive strength containing recycled aggregate, after
exposure at high temperatures up to 700 ◦ C, is about 55% for RSPX and 19% for RSRX.
This is comparable to that of the control mixes. In the 100–400 ◦ C temperature range,
a significant decrease in UPV, equal to 28.9% for RSPX, 36.9% for NRPX, 30.8% for
RSRX, and 37.1% for NRSX, is observed and can be attributed to the dehydration–
dehydroxylation of calcium silicate hydrate. Furthermore, a steeper decrease in UPV
was measured in the 20–100 ◦ C interval for mortars with recycled aggregate. This can
be explained by the greater ease of water vapour to escape in mortars that are more
porous and of the fine-cracks to develop, under vapour pressure, from the original
defect of the recycled aggregate at the pore boundaries.
The present investigation shows that the use of high-quality and purity-recycled
aggregates, obtained by selective demolition, can help to produce mortars with acceptable
properties and durability, even when a high amount of natural sand is replaced.
Authors believe that a further tuning of the additives types and amount, the pre-
treatment of the recycled aggregate to reduce the ceiling effect, and the partial replacement
of Portland cement with pozzolanic powders could further improve the performance of the
investigated mortars.
Appl. Sci. 2022, 12, 2732 22 of 26

Author Contributions: Conceptualization, S.C., F.T. and F.C.; Data curation, S.C. and F.T.; Formal
analysis, F.C. and P.D.F.; Investigation, S.C. and I.I.; Methodology, S.C., F.T. and I.I.; Validation, F.C.
and P.D.F.; Writing—original draft, S.C.; All authors have read and agreed to the published version of
the manuscript.
Funding: The ECOFIBAR project-PON 01_01522, funded by the Italian government, partially sup-
ported this work.
Conflicts of Interest: The authors declare no conflict of interest.

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