materials
Article
Full Characterization of Self-Compacting Concrete Containing
Recycled Aggregates and Limestone
Meriem Guessoum, Fouad Boukhelf *
Citation: Guessoum, M.; Boukhelf, F.;
Khadraoui, F. Full Characterization of
Self-Compacting Concrete
Containing Recycled Aggregates and
Limestone. Materials 2023, 16, 5842.
https://doi.org/10.3390/
ma16175842
Academic Editors: Ruizhe Si
and Shuaicheng Guo
Received: 30 June 2023
Revised: 19 August 2023
Accepted: 23 August 2023
Published: 26 August 2023
Copyright: © 2023 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/).
Materials 2023, 16, 5842. https://doi.org/10.3390/ma16175842
and Fouzia Khadraoui
Builders Ecole d’Ingénieurs, Builders Lab, ComUE NU (Communauté Universitaire de Normandie Université),
1 Rue Pierre et Marie Curie, 14610 Epron, France; meriem.guessoum@builders-ingenieurs.fr (M.G.);
fouzia.khadraoui-mehir@builders-ingenieurs.fr (F.K.)
* Correspondence: fouad.boukhelf@builders-ingenieurs.fr; Tel.: +33-231463200
Abstract: This work deals with the study of self-compacting concretes (SCCs) containing recycled
aggregates (RAs) recovered from demolition waste and limestone filler as a partial replacement
for natural aggregates (NAs) and cement, respectively. Four mix designs were developed and
characterized in both the fresh and hardened states. In the fresh state, the properties studied
included slump, sieve stability, and t500 viscosity. In the hardened state, the properties studied were
compressive strength and porosity at 15 h and 28 days, thermogravimetric analysis, and durability
tests involving freeze–thaw cycles and accelerated carbonation. The results indicate the RAs lead to
a decrease in slump flow. However, the substitution rate of aggregate replacement does not affect
the compressive strength. This can be attributed to the optimized mix design, resulting in all SCC
mixtures achieving the same compressive strength class of 30–35 MPa. As for the durability tests, the
incorporation of recycled aggregates modifies the behavior of the concrete during freeze–thaw cycles.
Throughout the 300 freeze–thaw cycles, all concrete mixtures exhibited a mass loss accompanied by a
slight strain increase, but the materials remained visually intact. Additionally, the carbonation depth
is strongly influenced by the rate of aggregate replacement due to changes in the microstructure,
particularly in porosity.
Keywords: recycled concrete aggregates; limestone; self-compacting concrete; fresh properties;
durability
1. Introduction
Concrete is the most widely used construction material globally, with an annual pro-
duction exceeding 10 billion m3 [1]. In terms of regional consumption, Europe stands
out with an annual consumption of concrete surpassing 620 million m3 . This highlights
the significant demand for concrete in construction activities throughout the continent.
Specifically, in France, the production of concrete amounts to over 21 million tons per year.
This substantial production volume contributes to the country’s construction industry, gen-
erating a considerable sales revenue of 19 billion euros, according to the French Federation
of the Concrete Industry [2].
However, despite its advantageous qualities in terms of mechanical strength, durabil-
ity, and cost-effectiveness, concrete has significant drawbacks related to its composition
and manufacturing processes. The concrete industry is known for its high energy consump-
tion and adverse environmental impact, particularly in terms of greenhouse gas (GHG)
emissions. It is estimated that the production of concrete contributes to 5.2% of global
GHG emissions. One of the main contributors to these emissions is cement production,
which alone accounts for 52% of the total emissions associated with concrete. In France, for
instance, the production of one ton of cement emits an average of 0.62 tons of CO2 eq [3].
Another concerning aspect is the extensive use of concrete in construction, which
has additional negative consequences for the environment. One such consequence is the
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Materials 2023, 16, 5842 2 of 13

depletion of non-renewable natural resources, particularly sand and gravel, which are
essential components of concrete production [4]. The extraction of these resources can lead
to habitat destruction, erosion of riverbanks, and disruption of ecosystems. In concrete,
aggregates are the most important part, accounting for around 3/4 of the total volume
of the concrete mix [5]. The demand for aggregates tends to increase with the growing
demand for concrete. In this context, the use of recycled aggregates in the manufacture of
concrete is a method of circular economy that meets the needs of sustainable construction
while preserving the environment [6,7].
In addition to its contribution to global warming, the blatant use of concrete leads to
a shortage of non-biodegradable natural resources, namely sand and gravel, which are
essential for its manufacture [4]. Furthermore, the demolition of concrete at the end of
its life generates considerable quantities of waste occupying large surfaces. This waste
represents about 36% of the total waste produced on earth [8]. The environmental impact
of the concrete industry extends beyond carbon emissions and resource depletion. The
indiscriminate use of concrete results in significant amounts of waste when buildings or
infrastructure reach the end of their lifespan. In the United States, concrete waste has
significantly increased from 50 million tons in 1980 to 548 million tons in 2015 [9]. In
China, this amount exceeds 1500 million tons [10]. In Europe, approximately 850 million
tons of concrete waste is produced each year, accounting for about 31% of the total waste
production in the European Union [11] and about 36% of the total waste produced on
earth [8].
Nowadays, the use of recycled aggregate in the manufacture of new concrete is
becoming increasingly widely practiced. Recycled aggregate is obtained by processing
concrete waste, demolishing structures, or reclaiming materials from other sources. The
main advantage of using recycled aggregate is that it reduces the amount of construction
waste sent to waste disposal sites, thus helping to preserve the environment. In addition,
its use reduces the demand for natural materials, such as virgin aggregates extracted from
quarries, thus helping to preserve natural resources. Although recycled aggregate may have
slightly different particle sizes and properties compared to natural aggregates, it can be
adapted and used effectively in the manufacture of concrete. Studies and research have been
carried out to determine the appropriate proportions of recycled aggregate to use in each
type of concrete, considering the required mechanical properties [12,13]. The use of recycled
aggregate in new concrete does not compromise the quality and performance of the final
material. In fact, it has been demonstrated that concretes containing recycled aggregate can
perform comparably to, or even better than, traditional concretes with natural aggregates.
Moreover, the use of these recycled materials can contribute to obtaining environmental
certifications for construction projects by reducing the overall carbon footprint [14]. In order
to address these problems, the use of recycled aggregate and alternative binders in concrete
mix designs is necessary and constitutes an unavoidable solution [15]. The path towards
the production of concrete that is more respectful of the environment and less polluting
for the planet will be confronted with several important challenges, including rheological
and mechanical performances, durability, and adaptability to the intended application.
However, the use of recycled aggregates in the development of self-compacting concrete
(SCC) is justified and technically feasible [16–18], although it is imperative to adjust the
mix design each time due to the irregularity of the intrinsic characteristics of recycled
aggregates. For this replacement to be effective, it is necessary to remedy the adverse
effect of old mortar on SCC containing recycled aggregates. Potential aggregate treatment
methods have been investigated to promote the maximum use of recycled aggregates [19].
Nevertheless, it is necessary to monitor changes in mechanical strength and durability over
time. To this end, indirect estimation of these properties through non-destructive testing is
now possible [18].
Several current studies aim to find the appropriate mix design of low-carbon self-
compacting concretes based on recycled gravel, obtained by adding a superplasticizer
whose excess can lead to segregation and by incorporating mineralogical additives and
Materials 2023, 16, 5842 3 of 13

recycled aggregate at relatively high rates [20], without the latter adversely affecting the
mechanical and rheological performance of the concrete [21]. Therefore, extensive research
and testing are required to optimize the mix design of low-carbon self-compacting concretes
based on recycled aggregate [22]. This includes the careful addition of a superplasticizer
to prevent segregation and the incorporation of mineral additives and recycled aggregate
at high rates without compromising the mechanical and rheological properties of the
concrete [23–25].
In fact, limestone fillers are widely used in the production of SCC [14]. Limestone
fillers, also known as fine limestone powders, are fine materials that can partially replace
cement or traditional fillers (such as silica fillers) in the composition of SCC. Limestone
fillers offer several advantages in SCC. Firstly, they help to improve the workability of
the mix [26], enabling better particle distribution and filling of voids [27]. This facilitates
concrete placement without the need for vibration, reducing construction time and, thus,
labor costs. Limestone fillers also have a beneficial effect on the mechanical properties of
concrete [28].
To address the environmental issues associated with concrete production, the use of
recycled gravel and alternative binders in concrete mix designs is indeed a necessary and
viable solution. This approach helps to reduce the need for natural aggregates, as well as the
depletion of natural resources and the carbon footprint. However, implementing these changes
in concrete production does come with several significant challenges, namely rheological and
mechanical performances, durability, and adaptability to the intended application.

2. Materials and Methods

Experiments were carried out to investigate the partial or total replacement effect of
aggregates by those resulting from the demolition of old buildings. The use of recycled
aggregates would affect fresh and hardened properties of SCC. For all mix designs, cement
(CEM I-52.5 R) provided by AALBORG® (Rochefort, France) was replaced with limestone
filler produced by Omya® (Noisy le Roi—Yvelines, France) with a mass replacement ratio
of 35%. Sand and coarse natural aggregates are classified as 0/4 and 4/12.5, respectively.
Recycled aggregates are classified as 4/14, and their property classification is type 1 accord-
ing to EN 206-1 [29]. Figure 1 presents the particle size analysis curve for the aggregates
used. It can be seen that recycled aggregates are coarser than natural ones but contain fine
material derived from the dust of the old cementitious matrix of the old concrete. Table 1
provides the amounts in kg/m3 of the different constituents of the SCC. In fact, in the case
of self-compacting concrete, the volume of binder paste should be around 40% of the total
volume, to the detriment of the volume of aggregates.
Following the steps presented in Figure 2, The raw materials were prepared and
weighed before dry mixing for 1 min. After that, water and admixture were added,
respectively. Indeed, the target concrete class was C30/37 with a consistency of SF2. Four
concrete mix designs were studied: a reference concrete with natural aggregates (NAs) and
three concretes incorporating recycled aggregates (RAs). The substitution rates of NA by
RA are 20, 50, and 100%. These are noted 0%RA, 20%RA, 50%RA, and 100%RA, respectively.
The aggregates were stored under ambient conditions (Temperature T = 20 ◦ C and relative
humidity RH = 50%). All concretes were manufactured at a temperature of 23 ◦ C. The
11 cm × 22 cm cylindrical specimens were demolded 24 h after production and stored at
T = 20 ◦ C and RH = 95%. A total of 28 specimens for each mix design were made to study the
property evolution at a hardened state in the laboratory for 15 h and 28 d. In order to assess
the RA effects, the different concrete compositions were characterized in terms of slump
flow, segregation strength, and t500 according to the European standard EN 12350-8 [30],
critical sieve stability according to the European standard EN 12350-11 [31], compressive
strength according to the French standard NF EN 12390-3 [32], thermogravimetric analysis
(TGA) and its derived factor (dTG), and water absorption and porosity according to AFPC-
AFREM [33].
 with standard XP P18-458 [35]. After 7, 28, and 70 days of carbonation, the prisms melted
in the transverse direction. Immediately after splitting, the surface was wiped clean, and
phenolphthalein solution was sprayed on, allowing the pH of the surface to be measured.
Phenolphthalein is colorless at a pH below 8.2, corresponding to a change in microstruc-
ture, particularly portlandite phase, which becomes carbonated and generates a calcite
Materials 2023, 16, 5842 4 of 13
phase, and deep pink at a pH above 9.9. In general, 12 depth measurements, i.e., the col-
orless part, were taken for each sample.

100
Sand NA RA
90
80

Percentage passing (%)

70
60
50
40
30
20
10
0
0.01 0.1 1 10 100
Particle size (mm)
Figure1.
Figure 1. Particle
Particle size
size analysis
analysis curve.
curve.

Table1.1.Mix
Table Mixdesign
designof
ofSCC
SCCstudied
studied(kg/m
(kg/m33).).

0%RA 0%RA 20%RA 20%RA 50%RA50%RA

100%RA
100%RA
Sand 0/4 786 786 786 786
Sand 0/4 786 786 786 786
Natural aggregate
Natural aggregate 4/12.5 726 726 580.8 580.8 361 361 --
4/12.5
Recycled aggregate 4/14 - 145.2 361 726
Recycled aggregate
Blanc CEM I-52.5 R - 320 145.2 320 361 320 726
320
4/14
Limestone
Blanc CEM I-52.5 R 320 160 320 160 320 160 160
320
Limestonewater
Efficient 160 161.81 160 161.81 160 161.81 179
160
Efficient
Totalwater
water 161.81 168 161.81 168 161.81 168 179
185.19
Total water
Superplasticizer 168 4.8 168 4.8 168 4.8 185.19
4.8
Superplasticizer
Set accelerator 4.8 3.80 4.8 3.80 4.8 3.80 4.8
3.805 of
Materials 2023, 16, x FOR PEER REVIEW 13
SetWater-repellent
accelerator 3.80 0.78 3.80 0.78 3.80 0.78 3.80
0.78
Water-repellent 0.78 0.78 0.78 0.78

Figure2.2.Specimen
Figure Specimenpreparation.
preparation.

From the
3. Results anddurability test point of view, the extreme freeze–thaw test was carried out
Discussion
on 3 test specimens
3.1. Fresh State measuring 10 cm × 10 cm × 40 cm for each mix design according to

Figure 3 illustrates the slump flow results 15 and 45 min after mixing for the studied
SCC. The findings indicate that the variation in workability at 15 min after mixing was not
significant for the SCC based on RA compared to the reference SCC (0%RA). This conser-
vation of workability can be attributed to the presence of superplasticizers in the different
 Manufacturing of self-compacting
- concretes

1 2 3 4

Materials 2023, 16, 5842 5 of 13

Raw materials Dry mixing (1 min) Admixtures and water Fresh concrete
Samples preparation

the European Specimen

standard NF P 18-424 [34]. The test specimens were placed in a freezing
chamber, allowing casting 300 cycles of temperature variation
Storage for 24h to be reproduced at a freezing
rate of 6 ◦ C/h until −18 ◦ C was reached. The freeze
20 °C and 95% RH period was maintained for 30 min,
followed by a programmed thaw period of 30 min at 9 ◦ C with a 45 min rise time. Test
specimens were recovered every 30 cycles after thawing, wiped dry, and stored at room
Water cure
temperature for 90 min. Two measurements were carried out, the first measuring specimen
strain
Figureand the second
2. Specimen mass loss. In addition, concrete carbonation depth was measured on
preparation.
7 cm × 7 cm × 28 cm prismatic specimens placed in a carbon incubator with a regulated
3. Results
CO of 3%, a temperature of 23 ◦ C and a relative humidity of 60%, in
and Discussion
2 concentration
accordance with standard XP P18-458 [35]. After 7, 28, and 70 days of carbonation, the
3.1. Fresh State
prisms melted in the transverse direction. Immediately after splitting, the surface was
Figure 3 illustrates the slump flow results 15 and 45 min after mixing for the studied
wiped clean, and phenolphthalein solution was sprayed on, allowing the pH of the surface
SCC. The findings indicate that the variation in workability at 15 min after mixing was not
to be measured. Phenolphthalein is colorless at a pH below 8.2, corresponding to a change
significant for the SCC based on RA compared to the reference SCC (0%RA). This conser-
in microstructure, particularly portlandite phase, which becomes carbonated and generates
vation of workability can be attributed to the presence of superplasticizers in the different
a calcite phase, and deep pink at a pH above 9.9. In general, 12 depth measurements,
SCC mix designs. However, a significant change in workability occurs at 45 min after mix-
i.e., the colorless part, were taken for each sample.
ing was observed for the SCC completely formulated with RA (100%RA). The use of RA
changed
3. Resultstheandrheological
Discussionproperties and extended the workability maintenance period.
3.1. Fresh State case of 100%RA, the SCC lost its fluidity. This change can be explained by
Whereas, in the
the presence of fines from old concrete, which increases the water demand and adversely
Figure 3 illustrates the slump flow results 15 and 45 min after mixing for the studied
affects workability 45 min after mixing.
SCC. The findings indicate that the variation in workability at 15 min after mixing was
As for viscosity, measured by the time it takes for the slump flow to reach a diameter
not significant for the SCC based on RA compared to the reference SCC (0%RA). This
of 500 mm (t500) and depicted in Figure 4, an increase in the slump flow time was ob-
conservation of workability can be attributed to the presence of superplasticizers in the
served with the rise in RA replacement rate. This increase is a consequence of RA being
different SCC mix designs. However, a significant change in workability occurs at 45 min
less mobile
after mixingdue wastoobserved
the decrease in paste
for the SCCcontent
completely[36]. formulated
In particular,with the 100%RA mix design
RA (100%RA). The
loses its workability and ceases to flow. This can be attributed to
use of RA changed the rheological properties and extended the workability maintenance the presence of excess
fine material
period. in theinRA,
Whereas, theleading
case ofto100%RA,
a higher water
the SCC demand
lost its[15]. This higher
fluidity. water demand
This change can be
is associated with the increased water absorption observed when the
explained by the presence of fines from old concrete, which increases the water demand RA replacement ratio
is raised [36,37].
and adversely affects workability 45 min after mixing.

90
78 76
80 75 73.5 75
71 72
70
Slump flow (cm)

60

50 15 min
40
45 min
30
22
20

10

0
0%RA 20%RA 50%RA 100%RA
Substitution rate

Figure3.
Figure 3. Slump
Slumpflow
flowof
ofSCC
SCCstudied.
studied.

As for viscosity, measured by the time it takes for the slump flow to reach a diameter
of 500 mm (t500) and depicted in Figure 4, an increase in the slump flow time was observed
with the rise in RA replacement rate. This increase is a consequence of RA being less
mobile due to the decrease in paste content [36]. In particular, the 100%RA mix design
loses its workability and ceases to flow. This can be attributed to the presence of excess fine
material in the RA, leading to a higher water demand [15]. This higher water demand is
Materials 2023, 16, 5842 6 of 13

Materials 2023, 16, x FOR PEER REVIEW 6 of 13

Materials 2023, 16, x FOR PEER REVIEW 6 of 13
associated with the increased water absorption observed when the RA replacement ratio is
raised [36,37].
12
12 10.63
10.63
10
10

8
(s) 8 6.56
6.56
Time(s)

6 5.03 5.28 15 min

6 4.88 5.28
Time

5.03 4.88 15 min

3.91
4 3.91 45 min
4 45 min
2.49
2.49
2
2
0
0 0
0
0%RA 20%RA 50%RA 100%RA
0%RA 20%RA 50%RA 100%RA
Substitution rate
Substitution rate
Figure 4. Viscosity of SCC studied.
Figure4.
Figure 4. Viscosity
Viscosity of
ofSCC
SCCstudied.
studied.

Figure 5 shows an assessment of the segregation resistance determined by measuring

Figure
Figure55 shows
shows anan assessment
assessment ofof the
the segregation
segregation resistance
resistance determined
determined by by measuring
measuring
the amount of laitance passed through a 5 mm sieve. The results obtained by the sieve
the
the amount
amount of of laitance
laitance passed
passed through
through aa 55 mm
mmsieve.
sieve. The
The results
results obtained
obtained byby the
the sieve
sieve
stability test qualify the 0%RA and 100%RA as stable concretes, the percentage of laitance
stability
stability test
test qualify
qualify thethe 0%RA
0%RA andand 100%RA
100%RA as as stable
stable concretes,
concretes, thethe percentage
percentage ofof laitance
laitance
being lowerthan
being than 15%, which expresses a good segregation stability for these two con-
beinglower
lower than15%, 15%,which
whichexpresses
expressesa good segregation
a good segregationstability for these
stability two concretes.
for these two con-
cretes.
Contrary Contrary to
to the 20%RA the 20%RA and
and 50%RA, 50%RA, which
which represent represent critical
critical stability, stability,
expressed expressed
a laitanceaa
cretes. Contrary to the 20%RA and 50%RA, which represent critical stability, expressed
laitance exceeding
exceeding 15%.
15%. This15%. This
can This can be attributed
be attributed to the granular
to the granular discontinuity
discontinuity between
between between
RA and NARA
laitance exceeding can be attributed to the granular discontinuity RA
and
used NA used
in these in these two mix designs. In agreement with the literature, the segregation
and NA usedtwo mix designs.
in these In agreement
two mix designs. with thewith
In agreement literature, the segregation
the literature, tended
the segregation
tended
to to decrease
decrease with the with the increased
increased substitution
substitution rate. Thisrate.
is Thistoisthe
due due to the
high high
water water ab-
absorption
tended to decrease with the increased substitution rate. This is due to the high water ab-
sorption capacity
capacity of RA material
with fine material [36,37].
sorptionof RA with
capacity of fine
RA with fine[36,37].
material [36,37].
21
21
18
(%)

18
percentage(%)

15
15
Passingpercentage

12
12
9
9
Passing

6
6
3
3
0
0
0%RA 20%RA 50%RA 100%RA
0%RA 20%RA 50%RA 100%RA
Substitution rate
Substitution rate
Figure5.5. Sieve
Figure Sieve stability
stabilityof
ofSCC
SCCstudied.
studied.
Figure 5. Sieve stability of SCC studied.
3.2.
3.2. Hardened
Hardened State
State
3.2. Hardened State
The
The water-accessible porosity
water-accessible porosity and
and water
water absorption
absorption results
results at
at 28
28 days
days are
arepresented
presented
in The water-accessible
Figure 6. An increase porosity
in porosityand water
and waterabsorption
absorption results
with atthe
28 increase
days are of presented
the sub-
RA
in Figure 6. An increase in porosity and water absorption with the increase of the RA
in Figure 6. An
substitution rateincrease
was in porosity
observed. and the
Indeed, water absorption
porous structure withof the
the increase
SCC of the
based on RA was
RA sub-
stitution rate was observed. Indeed, the porous structure of the SCC based on RA was
stitutiontorate
related was observed. Indeed, thetransition
porous structure of the SCC based on RAnew was
related to thethe presence
presence of
of an
an interfacial
interfacial transition zone
zone (ITZ)
(ITZ) between
between thethe old
old and
and new
related
mortars, to the presence of an interfacial transition zone (ITZ) between the old and new
mortars,according
accordingtotowhat
whatisisfound
foundininthe
theliterature
literature[38].
[38].InIngeneral,
general, concrete
concreteconsists
consistsof of
a
mortars,
blend of according cement,
aggregate, to what and
is found inwith
water, the literature
each of [38].components
these In general, concrete consists
contributing to theof
a blend of aggregate, cement, and water, with each of these components contributing to
a blend of aggregate, cement, and water, with each of these components contributing to
the strength and durability of the building material. However, the presence of distinct
the strength and durability of the building material. However, the presence of distinct
elements and their interactions results in the formation of an interfacial transition zone
elements and their interactions results in the formation of an interfacial transition zone
 failures occur at the ITZ due to its limited capacity for stress transmission [41].
In standard concrete, a single ITZ exists, positioned between mortar and natural
coarse aggregate. However, when incorporating recycled aggregate sourced from con-
struction and demolition waste, a three-phase composite emerged. This composite in-
Materials 2023, 16, 5842 cludes aged natural aggregate, the associated cement mortar, and the previous ITZs 7 ofbe-
13
tween these materials. Consequently, the integration of recycled aggregate introduces at
least two distinct types of ITZs into the concrete matrix [42]. These new ITZs can be further
categorized
strength and into two groups:
durability the ITZ material.
of the building between old and new
However, themortar,
presenceand the ITZelements
of distinct between
the aged
and aggregate surface
their interactions resultsand newformation
in the mortar, as ofwell as the pre-existing
an interfacial transitionITZ zonebetween the
(ITZ) [39].
original aggregate and its attached aged mortar.
This ITZ represents the most vulnerable connection between cement mortar and coarse
In addition,
aggregates. due toathe
It occupies consistency
range of 20–40% required in the fresh
of the overall state,
volume the 100%RA contained
of cementitious material,
typically measuring around 40 µm in thickness [40]. The ITZ has a of
more water than the other mix designs due to the high absorption recycled impact
significant aggregate,on
as shown
the in Table
mechanical and1 [15]. This canqualities
long-lasting lead to the
offormation
solidified of voids inOften,
concrete. the cementitious matrix
concrete failures
and inefficient
occur at the ITZpacking
due to itsof limited
the binder particles
capacity with the
for stress aggregates[41].
transmission [43].

25.0

Water absorption (%) Porosity (%)

20.0 18.3
17.7
15.7
Magnitude (%)

14.5
15.0

10.0 8.4 8.8

6.7 7.4

5.0

0.0
0%RA 20%RA 50%RA 100%RA

Substitution rate
Figure6.6. Porosity
Figure Porosityand
andwater
waterabsorption
absorptionof
ofSCC
SCCstudied.
studied.

In standard
Figure concrete,
7 presents theacompressive
single ITZ exists, positioned
strength valuesbetween mortar
at 15 h and 28 dand natural In
of curing. coarse
gen-
aggregate. However,
eral, concretes reach when incorporating
a strength higher thanrecycled
22 MPa aggregate
after 15 sourced fromThis
h of curing. construction and
high strength
demolition
is the resultwaste,
of theause
three-phase
of 52.5 R composite emerged.
cement, which has aThis composite
short-term rapidincludes aged in
hardening, natural
addi-
aggregate,
tion to thetheuseassociated
of limestonecement mortar,
fillers and the previous
that close ITZsalso
pores. It was between thesethat
observed materials.
all the
Consequently,
SCCs made with RA had better compressive strength than the natural SCC (0%RA),types
the integration of recycled aggregate introduces at least two distinct even
of
at ITZs intoage.
an early the concrete
Indeed, the matrix [42]. Theseofnew
incorporation RA,ITZs
evencan behigh
with further categorized
percentages intoSCCs,
in the two
groups:
improved thetheir
ITZmechanical
between old and new mortar,
performance. andmix
The SCC thedesigns
ITZ between
with RA thehad
aged aggregate
a higher com-
surface
pressive and new
than NA mortar,
becauseas well as the pre-existing
the recycled aggregate’s ITZ between
physical themechanical
and original aggregate and
characteris-
its attached aged mortar.
tics improved upon interlocking with the cementitious matrix [44]. In fact, the RA used
was In addition,
type 1, which due to the
comes consistency
from required
old concrete in the fresh
and contains state, the
no plastic, 100%RAmasonry,
gypsum, contained or
more water
glass waste. than the other mix designs due to the high absorption of recycled aggregate, as
shown in Table 1 [15]. This can lead to the formation of voids in the cementitious matrix
and inefficient packing of the binder particles with the aggregates [43].
Figure 7 presents the compressive strength values at 15 h and 28 d of curing. In general,
concretes reach a strength higher than 22 MPa after 15 h of curing. This high strength is the
result of the use of 52.5 R cement, which has a short-term rapid hardening, in addition to
the use of limestone fillers that close the pores. It was also observed that all the SCCs made
with RA had better compressive strength than the natural SCC (0%RA), even at an early age.
Indeed, the incorporation of RA, even with high percentages in the SCCs, improved their
mechanical performance. The SCC mix designs with RA had a higher compressive than
NA because the recycled aggregate’s physical and mechanical characteristics improved
upon interlocking with the cementitious matrix [44]. In fact, the RA used was type 1, which
comes from old concrete and contains no plastic, gypsum, masonry, or glass waste.
, x FOR PEER REVIEW
Materials 2023, 16, 5842 8 of 13 8 of 13

15 hours 28 days
40
34.75 35.30
Compressive strength (MPa)

34.28
35 31.98
30
24.72
25 22.86 22.89 23.11

20
15
10
5
0
0% RA 20% RA 50% RA 100% RA

Substitution rate
Figure 7. Compressive strength
Figure at 15 h and
7. Compressive 28 datof
strength 15studied
h and 28 concretes.
d of studied concretes.

In order to discussIn order to discuss thestrength

the mechanical mechanical strength
results, results, thermogravimetric
thermogravimetric size analysis
size analysis
was carried out on all concrete at 15 h and 28 d of curing. The results shown in Figure 8
was carried out on all concrete at 15 h and 28 d of curing. The results shown in Figure 8
indicate the presence of three phases. The first is attributed to the departure of (absorbed)
indicate the presence
wateroffrom
three
thephases. The of
constitution first is attributed
certain hydrates such to the departure
as C-S-H of (absorbed)
and ettringite AFt at 100 to
◦
water from the constitution of certain hydrates such as C-S-H and
130 C. The second is linked to the dehydration of the water chemically ettringite AFt at 100 to
bound with the
130 °C. The second is linked
portlandite to the2 )dehydration
(Ca(OH) at a temperature ofofthe water400
between and 480 ◦ C,bound
chemically with
and the last the to the
relates
decarbonation of the calcite ◦ C [45]. Furthermore,
portlandite (Ca(OH) 2) at a temperature ofphase
between(CaCO 4003 ) at
andbetween
480 °C, 750and
andthe
850 last relates to
a variation in hydrate quantities was observed for samples tested at 15 h and 28 d. This
the decarbonation of the calcite phase (CaCO3) at between 750 and 850 °C [45]. Further-
variation is explained by the kinetics of the hydration process of cement and limestone
more, a variation fillers.
in hydrate
These quantities was observed
concretes contain less of thefor samplesphase
portlandite tested at more
and 15 h calcite
and 28asd.a result
This variation is explained
of the additionby of
the kineticsfillers,
limestone of the hydration
which are veryprocess of cement
rich in CaCO and lime-
3 [46]. The findings show
stone fillers. These
thatconcretes
RA has no contain less
effect on theof the portlandite
hydration process inphase terms and
of CSHmoregel calcite
formed,asettringite,
a
portlandite,
result of the addition and calcite.
of limestone This
fillers, is dueare
which to the
very quality
rich inof the
CaCO recycled
3 [46].aggregates,
The findings which are
show that RA hastype 1 according
no effect on thetohydration
EN 206-1 [29] and contain
process in terms onlyofold
CSHconcretes.
gel formed, ettringite,
portlandite, and calcite. This is due to the quality of the recycled aggregates, which are
3.3. Durability
type 1 according 3.3.1.
to ENFreeze–Thaw
206-1 [29] and contain only old concretes.
Results
Figure 9 shows a quasi-linear increase in strain with freeze–thaw cycles for the 0%RA
material and a non-linear increase for other mix designs. In addition, the maximum strain
was 0.55, 0.8, 0.85, and 1.2 mm/m for 0%GR, 20%GR, 50%GR, and 100%GR, respectively.
From the mass loss point of view, the expansionary behavior of the concrete samples in
response to freeze–thaw cycles led to a weakening and cracking of the surface material,
resulting in a mass loss (cf. Figure 10). All these results are in accordance with those for
porosity. In fact, freeze–thaw behavior was improved by replacing part of the cement with
limestone fillers, as demonstrated by Zeng et al. [46].

3.3.2. Accelerated Carbonation

The accelerated carbonation results in Figure 11 show that the rate of CO2 penetration
was proportional to the exposition time [47]. This is explained by the synthesis process
between the cementitious matrix and the absorbed CO2 , which reduces the pH of the pore
solution [48], resulting in the formation of the calcite phase (CaCO3 ) to the detriment of
the calcium silicate hydrate (CSH), the portlandite phase (Ca(OH)2 ), and calcium oxide
Materials 2023,16,
Materials2023, 16,5842
x FOR PEER REVIEW 99 of
of 13
13

100 (CaO), as shown by [49]. 5.00Moreover,100 all mix designs had the same CO2 uptake at 7 days 5.00 of
0%RA 20%RA
exposition. After that, 4.00 the carbonation depth increased with the replacement rate4.00 of the
90 recycled aggregates. In general, the90
accelerated carbonation results were in accordance
3.00 3.00with
those for porosity related to the ITZ. Indeed, CO penetrates through the concrete’s2.00pore

dTG(%/min)

dTG(%/min)
80 2.00 80 2
TGA (%)

TGA (%)
network and reacts with1.00the concrete’s old and new cementitious matrix [50]. Furthermore, 1.00
70 the carbonation rate of 0.00 the concretes 70 studied was calculated in accordance with standard 0.00
FD P 18-480 [51] and showed -1.00
−1.00 a rate of 1.8 mm/day0.5 for all SCCs based on RA, (20%RA, -1.00
−1.00
60 60 0.5 for the reference concrete (0%RA), which, for
50%RA, and 100%RA) and −2.00 0.96 mm/day
-2.00 -2.00
−2.00
50 our mix designs, can be-3.00 used in a carbonation
−3.00 50 exposure class of XC4 according to EN −3.00206-
-3.00
Materials02023,150
16, x FOR
300 PEER
450 REVIEW
600
1 [29].750 This
900change
1050 may
1200 be related to the0 150 that
fact 300RA containing
450 600 750 cementitious
old 900 1050 1200 9 of in
matrix 13
Temperature (°C) Temperature (°C)
its interface comes from the already carbonated concrete of old building materials [52].
TGA_15hours TGA_28days dTG_15hours dTG_28days TGA_15hours TGA_28days dTG_15hours dTG_28days

100
100 5.00 100 5.00
50%RA 5.00
0%RA
100 100%RA 5.00
20%RA
4.00
4.00 4.00
4.00
90
90 90
90
3.00
3.00 3.00
3.00
dTG(%/min)

dTG(%/min)
2.00 dTG(%/min) 2.00

dTG(%/min)
80 2.00 80 2.00
(%)

(%)
80 80
TGA(%)

TGA(%)
1.00
1.00 1.00
1.00
TGA

70
TGA 70
70 0.00
0.00 70 0.00
0.00
-1.00
−1.00
-1.00
−1.00 -1.00
−1.00
-1.00
−1.00
60
60 60
60
-2.00
−2.00
-2.00 -2.00
−2.00
-2.00
−2.00 −2.00
50
50 -3.00
−3.00
-3.00
−3.00 50
50 -3.00
−3.00
-3.00
−3.00
00 150
150 300
300 450
450 600
600 750
750 900
900 1050
1050 1200
1200 00 150
150 300
300 450
450 600
600 750
750 900
900 1050
1050 1200
1200
Temperature(°
Temperature (°C)
C) Temperature(°
Temperature (°C)
C)
TGA_15hours
TGA_15hours TGA_28days
TGA_28days dTG_15hours
dTG_15hours dTG_28days
dTG_28days TGA_15hours
TGA_15hours TGA_28days
TGA_28days dTG_15hours
dTG_15hours dTG_28days
dTG_28days

100
Figure 8. TGA and dTG 5.00
50%RA at 15 h and 100
28 d of SCC studied. 100%RA
5.00

4.00 4.00
90 90
3.00 3.00
3.3. Durability
dTG(%/min)

dTG(%/min)
80 2.00 80 2.00
TGA (%)

TGA (%)

3.3.1. Freeze–Thaw Results

1.00 1.00
70 Figure 9 shows a 0.00 quasi-linear70increase in strain with freeze–thaw cycles for the 0%RA
0.00
material and a non-linear −1.00 increase for other mix designs. In addition, the maximum
-1.00 strain
-1.00
−1.00
60 60
was 0.55, 0.8, 0.85, and-2.00 1.2 mm/m for 0%GR, 20%GR, 50%GR, and 100%GR, respectively.
−2.00 -2.00
−2.00
50 From the mass loss point −3.00 of view,
-3.00 50 the expansionary behavior of the concrete samples -3.00
−3.00 in
0 150 300 450 600 response
750 900 1050 1200
to freeze–thaw cycles led 0to a 150
weakening300 450 600
and cracking 750 of900 1050
the surface 1200
material,
Temperature (°C) Temperature (°C)
TGA_15hours TGA_28days
resulting in a mass
dTG_15hours
loss (cf. Figure 10).
dTG_28days
All these results
TGA_15hours
are in accordance
TGA_28days dTG_15hours
with those for
dTG_28days
porosity. In fact, freeze–thaw behavior was improved by replacing part of the cement with
limestone
Figure 8. TGA fillers, as demonstrated
and dTG at 15 h and 28 d byofZeng et al. [46].
SCC studied.

3.3. Durability
1.2
3.3.1. Freeze–Thaw Results
1
Strain (mm/m)

Figure 9 shows a quasi-linear increase in strain with freeze–thaw cycles for the 0%RA
material0.8
and a non-linear increase for other mix designs. In addition, the maximum strain
0.60.8, 0.85, and 1.2 mm/m for 0%GR, 20%GR, 50%GR, and 100%GR, respectively.
was 0.55,
From the mass loss point of view, the expansionary behavior of the concrete samples in
0.4
response to freeze–thaw cycles led to a weakening and cracking of the surface material,
0.2in a mass loss (cf. Figure 10). All these results are in accordance with those for
resulting
porosity. 0In fact, freeze–thaw behavior was improved by replacing part of the cement with
limestone fillers,
0 as demonstrated
50 by Zeng et al.
100 150[46]. 200 250 300
Cycles (Days)
1.2
0%RA 20%RA 50%RA 100%RA
1
Strain (mm/m)

0.8
Figure9.9.Strain
Figure Straindue
dueto
tothe
thefreeze–thaw
freeze–thawcycles
cyclesof
oftested
testedconcretes.
concretes.
0.6
0.4
0.2
0
 0 50 100 150 200 250 300
Cycles (Days)
0%RA 20%RA 50%RA 100%RA

Figure 10. Mass loss due to the freeze–thaw of tested concretes.

Materials 2023,16,
Materials2023, 16,5842
x FOR PEER REVIEW 10 of 13
10 13

3.3.2. Accelerated Carbonation

The accelerated carbonation results in Figure 11 show that the rate of CO2 penetration
4.5
was proportional to the exposition time [47]. This is explained by the synthesis process
between 4 the cementitious matrix and the absorbed CO2, which reduces the pH of the pore
solution
3.5 [48], resulting in the formation of the calcite phase (CaCO3) to the detriment of

Mass loss (%)

the calcium
3 silicate hydrate (CSH), the portlandite phase (Ca(OH)2), and calcium oxide
(CaO),
2.5as shown by [49]. Moreover, all mix designs had the same CO2 uptake at 7 days of
exposition.
2
After that, the carbonation depth increased with the replacement rate of the
recycled aggregates. In general, the accelerated carbonation results were in accordance
1.5
with those for porosity related to the ITZ. Indeed, CO2 penetrates through the concrete’s
1
pore network and reacts with the concrete’s old and new cementitious matrix [50]. Fur-
0.5
thermore, the carbonation rate of the concretes studied was calculated in accordance with
0
standard FD P 18-480 [51] and showed a rate of 1.8 mm/day0.5 for all SCCs based on RA,
0 50 100 150 200 250 300
(20%RA, 50%RA, and 100%RA) and 0.96 mm/day0.5 for the reference concrete (0%RA),
Cycles (Days)
which, for our mix designs, can be used in a carbonation exposure class of XC4 according
0%RA 20%RA 50%RA
to EN 206-1 [29]. This change may be related to the fact that RA100%RA
containing old cementi-
tious matrix in its interface comes from the already carbonated concrete of old building
Figure 10. Mass
materials
Figure 10. Mass loss due
[52].loss due to
to the
the freeze–thaw
freeze–thawof
oftested
testedconcretes.
concretes.

3.3.2. Accelerated Carbonation

0%RA 20%RA 50%RA 100%RA
The
25 accelerated carbonation results in Figure 11 show that the rate of CO2 penetration
was proportional to the exposition time [47]. This is explained by the synthesis process
between the cementitious matrix and the absorbed CO2, which reduces the pH of the pore
20 [48], resulting in the formation of the calcite phase (CaCO3) to the detriment of
solution
the calcium silicate hydrate (CSH), the portlandite phase (Ca(OH)2), and calcium oxide
(CaO),15 as shown by [49]. Moreover, all mix designs had the same CO2 uptake at 7 days of
Depth (mm)

exposition. After that, the carbonation depth increased with the replacement rate of the
recycled aggregates. In general, the accelerated carbonation results were in accordance
with 10
those for porosity related to the ITZ. Indeed, CO2 penetrates through the concrete’s
pore network and reacts with the concrete’s old and new cementitious matrix [50]. Fur-
thermore,
5
the carbonation rate of the concretes studied was calculated in accordance with
standard FD P 18-480 [51] and showed a rate of 1.8 mm/day0.5 for all SCCs based on RA,
(20%RA, 50%RA, and 100%RA) and 0.96 mm/day0.5 for the reference concrete (0%RA),
which,0 for our mix designs, can be used in a carbonation exposure class of XC4 according
7 28 70
to EN 206-1 [29]. This change may be related to the fact that RA containing
Time (Days) old cementi-
tious matrix in its interface comes from the already carbonated concrete of old building
Figure11.
11.Carbonation
materials
Figure Carbonation
[52]. depthof
depth oftested
testedconcretes.
concretes.

4. Conclusions
0%RA 20%RA 50%RA 100%RA
This
25 study is part of an environmental transition process aimed at reducing the
carbon footprint associated with construction materials and addressing the issue of non-
biodegradable waste occupying vast landfill areas. The focus of this research was on
20
investigating the properties of self-compacting concretes containing 35% limestone and
recycled aggregates in both fresh and hardened states, including slump flow, t500 viscosity,
sieve 15stability, porosity and water absorption, mechanical strength, thermogravimetric
Depth (mm)

analysis, freeze–thaw, and accelerated carbonation. The results obtained are encouraging
and align with the specified requirements and intended applications. The findings are
10 as follows:
outlined
• The use of recycled aggregates reduces the time required to maintain consistency due
to5 the fine particles present in the aggregates and their significant water absorption.
• The sieve stability of the 20%RA and 50%RA self-compacting concretes was greatly
modified by the granular discontinuity, in contrast to homogeneous aggregate mix
0
designs such as 0%RA and 100%RA.
7 28 70
• The recycled aggregates do not affect
Time either
(Days) the mechanical compressive strength or
the binder hydration, as demonstrated by TG analyses.
Figure 11. Carbonation depth of tested concretes.
Materials 2023, 16, 5842 11 of 13

• The self-compacting concretes tested exhibit good freeze–thaw resistance, and the
difference between them is strongly related to the porosity. The 0%RA presents a
quasi-linear behavior, and this increases with the higher replacement rate by 45%, 54%,
and 110% for 20%RA, 50%RA, and 100%RA, respectively.
• The developed self-compacting concretes have a carbonation rate of 0.96 mm/day0.5
for the 0%RA and about 1.8 mm/day0.5 for the other mix designs.
The comprehensive experimental characterization campaign presented in this work
and the resulting findings constitute valuable additions to the database on self-compacting
concretes. Another study will be carried out on the application of these materials in a
demonstrator building.

Author Contributions: Conceptualization, M.G. and F.B.; methodology, M.G. and F.B.; validation, F.B.
and F.K.; formal analysis, F.B.; investigation, F.B.; resources, F.B. and F.K.; data curation, M.G. and F.B.;
writing—original draft preparation, M.G. and F.B.; writing—review and editing, F.K.; visualization,
F.B. and F.K.; supervision, F.B. and F.K.; project administration, F.B. and F.K.; funding acquisition, F.B.
and F.K. All authors have read and agreed to the published version of the manuscript.
Funding: This research received no external funding.
Institutional Review Board Statement: Not applicable.
Informed Consent Statement: Not applicable.
Data Availability Statement: The experimental and computational data presented in the present
paper is available from the corresponding author upon request.
Acknowledgments: Authors thank the agency of Environmental transition ADEME for financing
the research through the BFIeP project.
Conflicts of Interest: The authors declare no conflict of interest.

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