materials

Article
Use of Recycled Fine Aggregates from C&DW for
Unbound Road Sub-Base
Luc Courard, Mélanie Rondeux, Zengfeng Zhao * and Frédéric Michel
Building Materials, Urban and Environmental Engineering, University of Liège, Allée de la découverte 9,
4000 Liège, Belgium; luc.courard@uliege.be (L.C.); m.rondeux@hotmail.com (M.R.); frederic.michel@uliege.be (F.M.)
* Correspondence: zengfeng.zhao@uliege.be; Tel.: +32-4366-5258




Received: 1 June 2020; Accepted: 3 July 2020; Published: 5 July 2020


Abstract: Fine recycled aggregates are produced in large quantities when crushing Construction and
Demolition Waste (C&DW). Even if coarse recycled aggregates are commonly used for road foundations,
fine particles are often rejected as they are considered detrimental for the long-term behaviour of
foundations. Physicochemical, mineralogical and mechanical characterizations (through X-ray diffraction,
X-ray fluorescence, the chloride and sulphate contents, Los Angeles abrasion, micro-Deval resistance
and static plate load tests) were performed on raw and treated fine recycled materials for understanding
both the effects of the preparation, the compaction and the freeze–thaw cycles on the properties and the
evolution of fine particles. Special attention was provided to the shape analysis of fines by means of image
analyser. The results showed that the main characteristic parameters to be considered are the sieving curve
and the proportion of grades. The mixes containing the highest quantity of fine particles, specifically lower
than 63 µm, usually inducing a higher water demand and a higher capillary rise. This can be explained
by specific surface and bluntness parameters which increase with the finer particles, inducing a higher
surface roughness and, consequently, a higher potential interaction with water. Compaction did not seem
to have a major effect on the production of fines (despite some breakdown occurred during compaction)
and on the shape of materials (the bluntness and convexity increased slightly, while the elongation values
remained similar after the compaction process). The static plate load tests showed that bearing capacity
is slightly lower than the specifications for the road foundation after compaction. However, the studied
material could meet the maximum criteria for secondary roads foundation construction on the wear
resistance criteria. Recycled aggregates from C&DW without sufficient quality could be blended with
other aggregates to enable their usage for upper-level road foundation.

Keywords: recycling; construction and demolition waste; recycled concrete aggregates; road sub-base;
fine; shape; compaction

1. Introduction
The durability of an aggregate used in a road structure can be defined as the capacity of the material
to be stored over time and to preserve its initial characteristics, in particular, its particle size distribution vs.
various stresses (since its treatment until the destruction of the road) [1,2]. This definition involves three
key concepts that should be specified, namely the conservation of the particle size distribution, the life
cycle of material and the defects by solicitations present within the material [3–5].
An unbound granular mixture is an assembly of grains of different sizes and nature that touch each
other at different points of the surface and are separated by intergranular spaces filled, with either free

Materials 2020, 13, 2994; doi:10.3390/ma13132994 www.mdpi.com/journal/materials

Materials 2020, 13, 2994 2 of 26

water or capillaries or air [6]. Each phase is characterized by distinct properties that influence the overall
behaviour of the material [7].
In the presence of stresses within the material, a part of the stresses is concentrated in the liquid
phase (in the form of interstitial pressure), whereas the other part is concentrated in the solid phase and,
in particular, in certain zones such as the contact points between grains, areas of weakness of the rock
(cracks, pores, etc.), or at the water–solid interface [8–10]. If these stresses grow, they can cause fractures
within the grains as well as their polishing, which results in their decomposition and the formation of
fine particles [11]. Therefore, this causes a change in the granular structure of the material that often
results in the loss of geotechnical characteristics [9,12], not only of the layer concerned but also of the entire
structure [13].
The conservation of the particle size distribution is therefore an important factor in the durability of
an aggregate [14,15]. This is why the majority of sustainability tests provide results in the form of fines
produced during these tests [16]. The presence of fines within a granular material can have several positive
or negative effects depending on the content on the following three parameters [17–21]:
(a) The compactness, the bearing capacity of the material as well as the resistance to the different types
of deformations: the fines tend to fill the intergranular spaces during the compacting operation [22,23].
This improves the density of the material and therefore its compactness. Therefore, from a certain content
(between 20–25% depending on the initial porosity of the coarse material), the addition of fines generates a
reverse phenomenon, namely a decrease in density [24]. The fines no longer occupy only the interstices
but they separate the large elements and the initial porosity of the material becomes more and more
important [25]. It should be noted that the specifications allow a fines content of up to 9% for load bearing
layers such as the foundation.
(b) Permeability: the fines present in the interstices reduce the permeability of the material by filling
the pores [24]. However, as long as their mass percentage remains moderate, the water continues to
circulate in the interstices without much problem. On the other hand, from a certain value (related to the
sieving curve of the material), the fines favour the accumulation of the water in the material rather than
the circulation of the latter. Thus, as already mentioned by Casagrande [26], the criterion concerning the
content of elements with a diameter of less than 20 µm should be less than 2%. Currently, on the basis of
the different experiments carried out since then and for practical reasons (the mechanical sieving stops at
63 µm), the majority of the specifications limit the content of fines (Ø < 63 or 80 µm) to a lower or equal
value to 7% for layers with draining role, such as the sub-foundation.
(c) Frost sensitivity: in case of frost, stationary water freezes more easily than moving water.
The transformation from liquid to solid state causes an increase in the volume (swelling). This swelling
is characterized either by an uplift of the upper structure or by an increase of stresses on the different
materials [27]. This therefore facilitates the breakage and the production of fines and accelerates the
phenomena of mechanical degradation of the material. A non-draining and therefore rich in fines structure
accelerates the propagation of frost and thaw fronts.
These considerations are of particular concern when using recycled concrete aggregates (RCA)
which are more and more used in road foundations [27,28]. RCA are composed of a mix of natural
aggregates and adherent hardened cement paste [29–32]. The latter is usually much more porous than
natural aggregates [33,34] and leads to a large water demand which makes RCA less easy to recycle
into concrete [1,35–37]. Properties of RCA such as water absorption and porosity can deeply influence
the fresh properties of concrete as well as mechanical properties and durability of concrete made with
RCA [16,38–41]. Over the past decades, many researchers have investigated the possibility of using C&DW
materials in the road base and sub-base [27,42–47]. They confirm that the properties of recycled aggregates
could influence the performances of unbound road layers [27,43,48–50].
Materials 2020, 13, 2994 3 of 26

Molenaar and van Niekerk [45] investigated the effects of gradation, composition and degree of
compaction on the mechanical characteristics. The results showed that crushed recycled concrete and
masonry rubble can be used to produce good quality road bases. The results indicated that the composition,
particle size and degree of compaction have a strong influence on the mechanical properties of recycled
materials, but the degree of compaction is the most important influencing factor. This was an important
conclusion for construction in practice, since the degree of compaction is much easier to realize and to
control than the other parameters.
Park [46] investigated the characteristics of RCA as base and sub-base materials. The results showed
that RCA can be used as alternative materials to crushed natural aggregates for roadways. The stability
and shear resistance of RCA in wet conditions were lower than in dry conditions, and the reduction rate
was comparable with that of natural aggregates. In addition, the deflection of the RCA section was similar
to that of natural aggregates section in the field.
Poon and Chan [47] presented the feasible use of RCA and crushed clay brick as unbound road
sub-base materials. The results demonstrated that the use of 100% of RCA decreased the maximum dry
density and increased the optimum moisture content of the sub-base materials compared to those of
natural sub-base materials. The California bearing ratio (CBR) value of sub-base using crushed clay brick
was lower than that with RCA. Nevertheless, the soaked CBR value for all recycled sub-bases were 30%
greater than that of the minimum strength requirement in Hong Kong.
Leite et al. [44] evaluated the composition and compaction influences on the mechanical behaviour of
road base and sub-base layers based on the C&DW materials. The CBR value and the resilient moduli
obtained with recycled C&DW materials were similar to those obtained with natural aggregate commonly
used in road construction.
Barbudo et al. [42] studied the relationship between different constituents of recycled aggregates and
their mechanical behaviour for the road application through a statistical analysis. The results showed
that the correct selection of materials and the removal of impurities in a plant with pre-screening and
double crushing are important to improve the quality of recycled aggregates. They concluded that recycled
aggregate can be used as sub-base materials in roadways.
Jiménez et al. [51] evaluated the behaviour and environmental impact of recycled aggregates from
selected C&DW in field conditions. The results demonstrated that both recycled aggregates (4/40 mm,
recycled concrete aggregate and recycled mix aggregate) were of good quality and met all limits. The static
plate load test showed an excellent bearing capacity in both structural layers. In addition, the use of
recycled aggregates in unpaved rural roads did not present a risk of environmental contamination to
ground and underground water.
Arulrajah et al. [11] investigated the possibility of using RCA, crushed brick (CB), reclaimed asphalt
pavement (RAP), waste excavation rock (WR) and recycled glass in unbound pavement base/sub-base
applications. RCA, CB and WR were found to meet the physical and shear strength requirements for
aggregates in pavement base/sub-base applications. RAP and recycled glass have to be blended with higher
quality aggregates to further enhance their physical and strength properties, particularly the Los Angeles
abrasion and California bearing ratio in order to meet road authority requirements.
Sangiorgi et al. [52] focused on the development of the stiffness of recycled materials during
construction, as well as how it modified over time. An experimental embankment with four sections
of different recycled materials was tested and fields were made from two structural layers, forming a
homogenous thickness of about 80 cm. The structural performance of the embankment was determined
using different types of lightweight deflectometers. The results showed that recycled aggregates performed
well when properly compacted and may showed some positive self-cementing properties.
Silva et al. [53] presented the representative case studies of several applications undertaken in
several countries worldwide, namely recycled aggregates in unbound in road and building constructions.
Materials 2020, 13, 2994 4 of 26

For some time now, there have been several real-scale road applications comprised of recycled aggregates,
the experience of which has indicated the material’s technical and economic viability.
Finally, some authors investigated the permeability of mixtures prepared with varying RCA
contents [13]. The results showed that the use of 75% RCA allowed permeability values closer to
those obtained in natural aggregates. However, the influence of fine particles into recycled aggregates on
the performance of road foundation is still limited [27,43,54], in particular the shape and grading during
the construction procedure and weathering ageing have not been previously reported [34,43].
This study focuses on the recycled fine C&DW specific characterization for exploring the effect
of recycled fine materials in road construction. The main objectives of this study are twofold: firstly,
the influence of treatment in recycling plants on the properties of recycled aggregates has been explored.
Afterwards, an experimental road foundation has been built and material has been excavated for analysing
the evolution of particles and materials induced by the construction process and environmental ageing.
In addition, special attention has been provided for the shape analysis of fines.

2. Materials
Recycled aggregates have been collected from FEREDECO, Fernelmont, Belgian recycling plants for
analysis and characterization [55]. Four types of samples were investigated, specifically fine particles.
(1) Raw materials (M84). Four raw materials (noted as M84A, M84B, M84C and M84D, respectively)
were directly collected from four different recycling sites. The quantity of each raw material was about
20 m3 and the origin of the raw material was unknown. A pre-treatment operation was necessary before
sampling. This operation consisted of eliminating the fraction greater than 100 mm by means of a comb
screen mounted on a mobile unit of treatment. In order to facilitate manual sorting on the different raw
samples, a sieving separation was first performed on each of them. The sample was fed on a conveyor
belt equipped with a magnetic pulley at its end which removed the ferrous metal elements from the
flow of material [56]. Then, a double pass was provided on a double-stage vibrating screen in order to
obtain four particle size fractions in order to carry out the visual characterization: fraction (+40 mm);
fraction (−40 + 16 mm); fraction (−16 + 4 mm); and fraction (−4 mm).
Four samples referenced M84Af to Df (these represent the fraction under 4 mm) were collected from
materials M84A to D, respectively.
(2) Recycled materials after treatment (M37). Four recycled materials (noted as M37A, M37B, M37C and
M37D, respectively) were produced by means of a crushing treatment of M84 samples (M84A, M84B,
M84C and M84D, respectively) after decontamination [56]. The main steps of a C&DW recycling facility
are as follows [57]:

(a) Scalping: pre-screening in order to separate fine particles and soil before crushing;
(b) Crushing (primary and eventually secondary);
(c) Iron extraction by electromagnetic strip;
(d) Manual extraction of impurities;
(e) Screening to the desired fraction.

Four samples referenced M37Af to Df (these represent the fraction under 4 mm) were collected from
materials M37A to D, respectively.
(3) Recycled materials after compaction (CRR11). Experimental road foundation (10 × 3 × 0.3 m) was
built with M37A (0/31.5 mm) and material was excavated after one week for analysing the evolution of
particles and materials induced by the construction process. The treated recycled material M37A was
spread by means of a blade over the entire surface of the board (over a thickness of around 30 cm) with the
incorporation of temperature sensors at different depths. The compaction of the layer using a BOMAG
Materials 2020, 13, 2994 5 of 26

BW 213D compactor (Bomag, Hamme, Belgium) according to the method commonly used on site by the
contractor, namely four passes with a low amplitude vibrating roller and two passes with a non-vibrating
roller in order to close the layer. CRR11f refers to the fraction lower than 4 mm from CRR11.
(4) Recycled materials after freeze–thaw cycles (CRR22). These materials were the same as CRR11
but were exposed outside without cover after 6 months’ natural environmental ageing and 17 recorded
freeze–thaw cycles (December 2014–May 2015, Belgian climate conditions). The lowest recorded freeze
and highest thaw temperature were −4 ◦ C and 12 ◦ C, respectively, according to the sensors on the layer’s
surface. CRR22f refers to the CRR22 fraction under 4 mm.

3. Experimental Methods
Bags of all studied materials (described in the section of materials) were collected (about 1 ton for
each sample) and representative samples (about 30 kg for each sample) were obtained by coning and
quartering. The physical characteristics including the density, the water content, the capacity of water
capture from atmospheric air as well as the particle size distribution were conducted on the representative
samples. The mineralogical and chemical compositions of the studied materials were investigated by
X-ray diffraction (XRD) and X-ray fluorescence (XRF), respectively. In addition, the chloride and sulphate
contents were investigated on these fines materials. The mechanical characterization was carried out by
means of Los Angeles (LA) abrasion, micro-Deval resistance and static plate load tests. The shape of the
studied materials was also performed by means of an image analyser. Table 1 presents the summary
of the experimental program conducted in this study. The detailed information has been given in the
following sections.

Table 1. Summary of the experimental program conducted in this study.

Properties of Samples Equipment or Technique Standard or Reference

Bulk density Balance –
Absolute density Helium pycnometer –
Constituents of recycled materials – EN 933-11 [58]
Particle size distribution Sieve analysis EN 933-1 [59]
Water content Balance EN 1097-5 [60]
Mineralogical composition XRD -
Chemical composition XRF [61]
LOI at 500 and 1000 ◦ C – EN 1744-1 [62]
Chloride content – EN 1744-1 [62]
Sulphate content – EN 1744-1 [62]
Micro-Deval coefficient – EN 1097-1 [63]
Los Angeles abrasion – EN 1097-2 [64]
Water content of the layer in situ Gamma densimeter [65]
Optimum moisture Modified Proctor Test [66]
Bearing capacity of the layer in situ Static plate load test CME 50.01 [67]
Shape analysis Occhio 500 Nano Image analyser and EPSON scanner [68]

3.1. Physical Characterization

The constituents of the raw materials M84 were measured according to the European standard EN
933-11 [58]. Each coarse fraction (larger than 40, 16/40 and 4/16 mm) of raw materials (M84A to M84D) was
evaluated on the representative samples after pre-drying in the oven of 60 ◦ C (about 3 kg). The constituents
of the total fraction of coarse aggregates (larger than 4 mm) were estimated on the basis of the constituents
and fraction distribution of each fraction.
The particle size distribution of the studied materials was determined using the European standard
EN 933-1 [59]. For determining grain size distribution and in order to avoid the loss of possible soluble
Materials 2020, 13, 2994 6 of 26

elements, the “dry” technique was selected, with the mesh sieves of 4, 2, 1, 0.5, 0.25, 0.125 and 0.063 mm,
respectively, superimposed on a vibrating table for 15 min (60 and 80 vibrations/s).
The representative samples were pre-dried in the oven at a temperature of 105 ◦ C. The bulk density (ρb )
was estimated by filling a graduated cylinder with a determined volume of dried samples (V). The mass
(m) of this known volume of matter allowed to calculate its bulk density (Equation (1)). The absolute
density of specimens (the mass of a particle divided by its volume, excluding open and closed pores) was
measured using helium pycnometer:
ρb = m/V (1)
Materials 2020, 13, x FOR PEER REVIEW 6 of 24
In order to measure the water content of the raw materials, the samples were stored in the laboratory at a
constant
close astemperature
possible to theand“natural”
hygrometry (21 ◦ C and
conditions). The60% relative
water humidity)
content for at
of samples least 1 month
reaching constant(asstate
close
atas
possible to the “natural” conditions). The water content of samples reaching constant
laboratory condition was determined using the European standard EN 1097-5 [60]. After the drying state at laboratory
condition
operationwas determined
in the oven at a using the European
temperature standard
of 105 °C, EN 1097-5 [60].
the representative Afterwere
samples the drying operation
placed in a closed in
the oven at a temperature of 105 ◦ C, the representative samples were placed in a closed box containing
box containing water (Figure 1) in order to determine their capacity of water capture from atmospheric
water (Figure
air (the 1) intemperature
external order to determine their capacity
and humidity were set of water
at 20 capture
± 3 °C and 60from atmospheric
± 10%). air (the
This original test isexternal
very
temperature and humidity were set at 20 ± 3 ◦ C and 60 ± 10%). This original test is very important with
important with regard to the behaviour of road foundation in case of freezing. Moreover, higher water
regard
captureto is
therelated
behaviour of roadamount
to a higher foundation inparticles.
of fine case of freezing.
The massMoreover,
variation higher water capture
of the samples is related
was regularly
toregistered.
a higher amount of fine particles. The mass variation of the samples was regularly registered.

(a) (b)
Figure
Figure 1. 1.Experimental
Experimental device
device forwater
for water capture
capture measurement
measurement from
from atmospheric
atmospheric airair water:
water: (a)(a) closed
closed box
inbox
the in the laboratory
laboratory with temperature
with temperature and humidity
and humidity set atset
20at±20
3 ◦±C3 and
°C and 6010%;
60 ± ± 10%;
and and
(b)(b)
thethe closed
closed box
box containing
containing the samples
the dried dried samples and water.
and water.

3.2.
3.2.Mineralogical
Mineralogicaland
andChemical
ChemicalCharacterization
Characterization
The mineralogical characterization
The mineralogical characterization waswasperformed by means
performed of X-ray
by means diffraction
of X-ray (XRD).(XRD).
diffraction The samples
The
were dried and milled before being subjected to X-ray diffractometers (PHILIPS PW-1130/90,
samples were dried and milled before being subjected to X-ray diffractometers (PHILIPS PW-1130/90, Philips,
Amsterdam, Netherlands).
Philips, Amsterdam, The positionThe
Netherlands). andposition
the relative
andintensity of the powder
the relative intensitydiffractogram
of the powder peaks
made it possible to determine the nature of the constituents. The semi-quantitative
diffractogram peaks made it possible to determine the nature of the constituents. The semi- analysis with X-ray
fluorescence
quantitative spectrometry
analysis with(spectrometer ARL 9400
X-ray fluorescence Sequential XRF
spectrometry XP, ThermoFisher,
(spectrometer ARL 9400 Waltham, MA,XRF
Sequential USA)
was
XP, ThermoFisher, Waltham, U.S.) was determined according to the protocol described by [61]: the of
determined according to the protocol described by [61]: the accuracy of the results is of the order
5% (presented asresults
an indication). The Losses On Ignition ◦ C, the chloride content
accuracy of the is of the order of 5% (presented as(LOI) at 500 andThe
an indication). 1000Losses On Ignition (LOI)
ofataggregate
500 and and
1000the
°C,sulphate content
the chloride (acidof
content soluble) of aggregate
aggregate were measured
and the sulphate contentusing
(acid the European
soluble) of
standard EN 1744-1 [62].
aggregate were measured using the European standard EN 1744-1 [62].

3.3. Mechanical Characterization

The resistance to wear of samples was determined by means of micro-Deval coefficient which
corresponds to the percentage of original sample reduced to a size smaller than 1.6 mm during rolling
[63]. The fraction of samples (10/14 mm) was tested with the addition of water. The drum within
samples (pre-dried in the oven at 105 °C, noted as Ma) and ball load (5000 ± 5 g) were rotated at a
speed of 100 ± 5 rounds per minute for 12,000 ± 10 revolutions. After the rotation, the materials were
Materials 2020, 13, 2994 7 of 26

3.3. Mechanical Characterization

The resistance to wear of samples was determined by means of micro-Deval coefficient which
corresponds to the percentage of original sample reduced to a size smaller than 1.6 mm during rolling [63].
The fraction of samples (10/14 mm) was tested with the addition of water. The drum within samples
(pre-dried in the oven at 105 ◦ C, noted as Ma ) and ball load (5000 ± 5 g) were rotated at a speed of
100 ± 5 rounds per minute for 12,000 ± 10 revolutions. After the rotation, the materials were collected and
washed carefully on the 1.6-mm sieve, and then dried in the oven at 105 ◦ C until constant mass (noted as
Mb ). The micro-Deval coefficient (MDE ) is calculated according to EN 1097-1 [63] as follows (Equation (2)):

MDE (%) = (Ma − Mb )/Ma × 100 (2)

The Los Angeles (LA) abrasion test of samples was measured according to the European standard
EN 1097-2 [64]. The LA abrasion test was carried out using aggregate sizes (10/14 mm fraction).
Aggregates (5000 g) were dried at 105 ◦ C for 24 h and then cooled to room temperature before placing in a
steel drum. The drum was rotating for 500 revolutions at a rate of 31–33 rev/min, along with nine steel
spheres (approximately 4840 g). After the 500 revolutions were complete, the crushed aggregate particles
were sieved through a 1.6 mm sieve. The amount of material passing the sieve, expressed as a percentage
of the original mass, is the LA abrasion resistance.
During the road foundation construction built with M37A (0/31.5 mm), the dry density and water
content of the layer were determined using a gamma densimeter at two different locations; this system is
widely used in France and Belgium for road construction control [65]. The results were compared with
the maximum dry density and optimum moisture obtained with the Modified Proctor Test [66] to verify
that the materials had been correctly set. To measure the bearing capacity of the layer, static plate load
tests were conducted in accordance with CME 50.01 [67]. The results of the plate load test are presented as
curves of applied contact pressure versus settlement. The bearing capacity Mi (M1 : 1st plate loading; M2 :
2nd plate loading) is determined by the Equation (3). A 309-mm diameter steel bearing plate was used for
this test. The compressibility coefficient (m) is determined by the ratio of M2 /M1 .
 
Mi = D × ∆p /∆s (3)

where D is the diameter of the plate (in cm); ∆p is the difference of applied contact pressure (in MPa); ∆s is
the difference of the settlement (in cm).

3.4. Shape Analysis

Static image analysis was performed by means of the Occhio 500 Nano image analyser (Figure 2,
Occhio, Liège, Belgium) and a high-resolution scanner EPSON V750PRO (Table 2, Epson, Tokyo, Japan) [68].
This instrument includes an integrated vacuum dispersion system and a high-quality optical component
which allows assessing size and shape of a set of dispersed particles. Few milligrams of particles were
dispersed onto a circular glass slide which is moved (in front of) above a collimated blue (490 nm) LED
backlighting. Pictures of individual particles were captured with a 1392 × 1040-pixel video camera fitted
with a telecentric lens. The system routinely determined the magnification through the imaging of a
calibrated grid. During this experiment, the working resolution was set up to 0.563 µm/pixel. The inscribed
disk diameter of each particle was calculated in real time to build particle size distribution curves weighted
by apparent volume (PSD-V’) [69], making the assumption that particles have identical densities and
flatness ratios, whatever their size.
 Materials
Materials 2020,
2020, 13,13,
2994x FOR PEER REVIEW 8 of 2426
8 of

1 − of the
Table 2. Performances ⁄ . used ℎfor shape analysis.
. test ℎdevices
where Ell.Width and Ell.Length
Size Range are the width and length
Nomenclature of the particle
Equipment on the inertia
Approximate ellipse
Pixel Size (µm)minor
and major axes, respectively. Elongation with default value of 1 if Ell.Length = 0.
>4 mm 4 EPSON scanner 21.2
2) Convexity
2–4 mm 2 EPSON scanner 21.2
1–2 mm 1 EPSON scanner 21.2
0.5–1 mm 0.5 Occhio 500 Nano 4.4
⁄
0.25–0.5 mm 0.25 Occhio 500 Nano 3.2
where Perimeter is the perimeter length calculated by multiplying 1 for each link between horizontal
0.125–0.25 mm 0.125 Occhio 500 Nano 2.2
0.063–0.125 mm +0.063 Occhio 500 Nano 1.4
and vertical pixels and √2 for other links. Convex Perimeter is the sum of the lengths of the convex
<0.063 mm −0.063 Occhio 500 Nano 0.9
perimeter segments. If the convex perimeter contains only three segments or less, Convex Perimeter =
1.
Particle image acquisition method proceeded by scanning the first 50,000 particles, ensuring that
3) areOcchio
particles scannedBluntness
at least once on the whole diameter of the glass slice. The accuracy associated to
The calculation of Size
the estimation of Particle the Distribution
Occhio Bluntness was
PSD-V’, based onasEric
expressed Pirard’s thesis;
the two-sided this parameter
95% confidence is
interval,
related
was to thebyvariability
computed of the
means of the particle
bootstrap calliper
method distribution
[69,70]. [71].the
Regarding The calliper
large numberis the distribution
of particle of
analysed,
rays
any of circles
further tangent
filtering wasto the outer
required to pixels
obtainand included
reliable in the particle. The bluntness values are shown
results.
in Figure 2.

(a) (b)
Figure 2.
Figure 2. Occhio
Occhio 500
500 Nano
Nano image
image analyser
analyser (a)
(a) and
and Occhio
Occhio Bluntness
Bluntness values
values (b)
(b) [71].
[71].

4. Results and Discussions

Raw materials (M84), recycled materials after treatment (M37) and recycled materials after compaction
(CRR11) were sieved and divided into eight different grades (Table 2).
4.1.The
Physical Characterization
selected discriminant parameters for shape analysis were [71]:
Mass distributions
(1) Elongation (from inertia of ellipse)
each fraction of raw material (M84) are shown in Table 3. Mass
distributions were calculated without considering the metal fraction (2 kg per ton). On the basis of
1 − Ell.Width/Ell.Length
visual observations, it can be concluded that all the raw materials are composed of many coarse
elements Ell.Width
where such and Ell.Length
as concrete are the
blocks and width
bricks; and length
however, the of
rawthematerials
particle on M84Athe inertia
to M84C ellipse minor
present a
and major axes, respectively. Elongation with default value of 1 if Ell.Length
brown colour, but a grey colour is presented for M84D. The raw material M84C presents the highest = 0.
(2)content of fine material (fraction smaller than 4 mm), which is due to the origin of C&DW. Table 3
Convexity
shows the classification of the components of different materials.
Perimeter/Convex Perimeter The raw material M84B offers the
highest
whereclay masonry
Perimeter content
is the (e.g.,length
perimeter brickscalculated
and tiles, by
Rb multiplying
= 57.1%) and1 for the each
lowestlinkcontent
between of horizontal
concrete
andand
unbound aggregate √ + Ru = 37.9%). On the contrary, the raw material 84C has the lowest clay
(Rc
vertical pixels and 2 for other links. Convex Perimeter is the sum of the lengths of the convex
masonry content
perimeter (Rb = 22.2%)
segments. and the
If the convex highest contains
perimeter content of concrete
only and unbound
three segments aggregate
or less, (Rc + Ru== 1.
Convex Perimeter
(3)72.0%),
Occhiowhich is within the requirement for type B recycled aggregates according to European
Bluntness
standard EN 12620 [72].
The calculation of the Occhio Bluntness was based on Eric Pirard’s thesis; this parameter is related to
Table 3. Classification
the variability of the particle of calliper
raw materials (M84A to[71].
distribution D) and recycled
The materials
calliper after treatment
is the distribution of(M37A
rays oftocircles
tangentD)toaccording
the outertopixels
EN 933-11 (Rc, Ru, Rb,
and included Ra, particle.
in the Rg, X andTheFI refer to percentages
bluntness values are of shown
concreteinproducts,
Figure 2.
unbound aggregate, clay masonry units, bituminous materials, glass, other non-floating materials and
volume percentage of floating material in %, respectively).

Mass Type of Constituents

Name of Materials Fraction
Percentage Rc Ru Rb Ra Rg X FI
M84A x > 40 mm 44.9 32.3 6.2 56.9 3.1 0.1 1.0 0.4
Materials 2020, 13, 2994 9 of 26

4. Results and Discussions

4.1. Physical Characterization

Mass distributions of each fraction of raw material (M84) are shown in Table 3. Mass distributions
were calculated without considering the metal fraction (2 kg per ton). On the basis of visual observations,
it can be concluded that all the raw materials are composed of many coarse elements such as concrete
blocks and bricks; however, the raw materials M84A to M84C present a brown colour, but a grey colour is
presented for M84D. The raw material M84C presents the highest content of fine material (fraction smaller
than 4 mm), which is due to the origin of C&DW. Table 3 shows the classification of the components of
different materials. The raw material M84B offers the highest clay masonry content (e.g., bricks and tiles,
Rb = 57.1%) and the lowest content of concrete and unbound aggregate (Rc + Ru = 37.9%). On the contrary,
the raw material 84C has the lowest clay masonry content (Rb = 22.2%) and the highest content of concrete
and unbound aggregate (Rc + Ru = 72.0%), which is within the requirement for type B recycled aggregates
according to European standard EN 12620 [72].
After the treatment in the recycling plant, the clay masonry content of all four recycled materials M37
decreased and all of them were finally within the requirement for type B recycled aggregates. The recycled
materials after treatment M37A has the lowest clay masonry content (Rb = 8.9%) and the highest content of
concrete and unbound aggregate (Rc + Ru = 88.0%). The recycling process including pre-screen, crushing,
sorting and decontamination (ferrous element, wood, plastic and paper) in four C&DW recycling facilities
can decrease the quantity of bricks and tiles present in the coarse fraction 4/30 mm. The quantity of fraction
0/4 mm, however, increases after the treatment (from 29.5% to 33.7% for M84A; from 21.9% to 26.5%
for M84B; from 28.6% to 36.5% for M84D) except for M37C, which means that the crushing process will
produce larger quantity of sand and filler fractions.
On the basis of visual observations, M84Bf to Df samples are dark brown while M84Af is light brown.
It is important to underline that, in view of the presence of condensed water on the bag in which the
samples were stored, all these powders seem to have an important absorption or adsorption capacity.
Figure 3 presents the distribution of the different fractions obtained during particle size separation for
each sample. Regarding the distribution of particle size fractions in the different samples, M84Af and Df
contain the highest content of fine particles (<250 µm). However, M84Df has the highest concentration of
particles with the fraction (0 to 125 µm). M84Af is essentially formed of fragments whose particle size is
between 125 and 500 µm. It is also in this sample that we find the least coarse elements (>2 mm). From a
sieving point of view, M84Bf and M84Cf are very similar. These two samples are also containing the
coarsest elements, essentially between 500 µm and 4 mm, and their cumulative refusal percentages are
systematically higher than those of the other two curves. The difference between the particle sizes of these
two samples is marked at the level of 250–500 µm, which is enriched in the fine fraction for M84Bf.
Figure 4 shows the sieving curves of recycled materials after treatment, compaction and freeze–thaw
cycles. After compaction process, the fine particle percentage (fraction 0/125 µm) slightly increased
according (curve CRR11f), which means that some breaking occurred during compaction. The materials
seem however to remain reasonably well graded through the compaction process. This is consistent with
the results of previous studies [30,44]. After the freeze–thaw cycles, the sieving curve of CRR22f sample
did not specifically reveal the formation of fines in larger amounts, which means that the freeze–thaw
cycles do not affect the particle size distribution for these recycled materials. During the freeze–thaw
cycles, the risk of damage could be due to the penetration of water into the particle pores upon freezing,
thus creating considerable tensile stresses that can break aggregate particle [43]. These recycled aggregates
showed good resistance to the freeze–thaw cycles.
Materials 2020, 13, 2994 10 of 26

Table 3. Classification of raw materials (M84A to D) and recycled materials after treatment (M37A to
D) according to EN 933-11 (Rc, Ru, Rb, Ra, Rg, X and FI refer to percentages of concrete products,
unbound aggregate, clay masonry units, bituminous materials, glass, other non-floating materials and
volume percentage of floating material in %, respectively).

Type of Constituents
Name of Materials Fraction Mass Percentage
Rc Ru Rb Ra Rg X FI
x > 40 mm 44.9 32.3 6.2 56.9 3.1 0.1 1.0 0.4
16 < x < 40 mm 18.2 47.9 11.0 32.9 2.4 0.9 4.4 0.7
M84A 4 < x < 16 mm 7.4 43.9 32.9 16.3 0.3 0.8 5.3 0.7
x < 4 mm 29.5 – – – – – – –
x > 4 mm 70.5 37.6 10.2 45.7 2.6 0.4 3.0 0.5
x > 40 mm 49.4 30.0 1.5 65.6 1.0 0.3 1.5 0.2
16 < x < 40 mm 21.4 38.4 3.9 52.1 1.7 1.9 1.7 0.4
M84B 4 <x < 16 mm 7.3 46.3 23.3 22.9 0.3 2.2 4.4 0.5
x < 4 mm 21.9 – – – – – – –
x > 4 mm 78.1 33.8 4.1 57.1 1.1 1.0 2.6 0.3
x > 40 mm 28.1 34.0 23.7 37.9 2.6 0.0 1.4 0.4
16 < x < 40 mm 23.9 49.5 26.4 16.4 5.3 0.2 2.3 0.2
M84C 4 < x < 16 mm 14.5 36.6 57.1 3.7 0.1 0.3 2.0 0.2
x < 4 mm 33.5 – – – – – – –
x > 4 mm 66.5 40.1 31.9 22.2 3.0 0.1 2.4 0.3
x > 40 mm 48.2 42.3 5.4 50.6 0.8 0.0 0.4 0.5
16 < x < 40 mm 16.1 44.4 2.6 47.2 1.1 0.5 3.7 0.7
M84D 4 < x < 16 mm 7.1 47.3 21.3 22.8 2.7 0.3 4.4 1.2
x < 4 mm 28.6 – – – – – – –
x > 4 mm 71.4 43.3 6.3 46.5 1.0 0.2 2.1 0.6
4 < x < 30 mm 66.3 43.7 44.3 8.9 1.5 0.0 1.1 0.5
M37A
x < 4 mm 33.7 – – – – – – –
4 < x < 30 mm 73.5 36.6 33.1 24.2 5.7 0.0 0.1 0.2
M37B
x < 4 mm 26.5 – – – – – – –
4 < x < 30 mm 73.1 49.2 22.2 25.2 0.9 0.0 2.3 0.1
M37C
x < 4 mm 26.9 – – – – – – –
4 < x < 30 mm 63.5 45.7 33.3 18.0 0.7 0.0 1.4 0.9
M37D
x < 4 mm 36.5 – – – – – – –
4 < x < 30 mm 70.5 41.3 24.6 32.1 1.3 0.1 0.3 0.3
CRR11
x < 4 mm 29.5 – – – – – – –

Table 4 presents the water content of the raw materials (M84Af to Df) after reaching the constant state
in the laboratory condition (21 ◦ C and 60% relative humidity). The water content of the sand fraction
of raw materials ranged from 11.9% to 14.7%. It revealed that the presence of fine particles is able to
physically attract water: the finer the particles, the higher water content. This is specifically the case for
M84Df, which has the highest content of fine particles under 63 microns.
 Materials 2020, 13, x FOR PEER REVIEW 10 of 24

curves.
Materials The
2020, 13,difference
2994between the particle sizes of these two samples is marked at the level of 250–
11 of 26
500 µm, which is enriched in the fine fraction for M84Bf.

30

M84Af M84Bf M84Cf M84Df

25

20
Fraction (%)

15

10

0
x< 63 µm 63 < x < 125 < x < 250 < x < 0.5 < x < 1 1 < x < 2 2<x<4 x > 4 mm
125µm 250 µm 500 µm mm mm mm
Materials 2020, 13, x3.FOR
Figure PEER REVIEW
Percentage of fractions obtained for the raw materials samples (M84Af to Df). 11 of 24
Figure 3. Percentage of fractions obtained for the raw materials samples (M84Af to Df).

Figure 4 shows the sieving curves of recycled materials after treatment, compaction and freeze–
thaw cycles. After compaction process, the fine particle percentage (fraction 0/125 µm) slightly
increased according (curve CRR11f), which means that some breaking occurred during compaction.
The materials seem however to remain reasonably well graded through the compaction process. This
is consistent with the results of previous studies [30,44]. After the freeze–thaw cycles, the sieving
curve of CRR22f sample did not specifically reveal the formation of fines in larger amounts, which
means that the freeze–thaw cycles do not affect the particle size distribution for these recycled
materials. During the freeze–thaw cycles, the risk of damage could be due to the penetration of water
into the particle pores upon freezing, thus creating considerable tensile stresses that can break
aggregate particle [43]. These recycled aggregates showed good resistance to the freeze–thaw cycles.

Figure 4. Particle size distribution of the sable fractions of the studied samples.
Figure 4. Particle size distribution of the sable fractions of the studied samples.

Table 4 presents the water content of the raw materials (M84Af to Df) after reaching the constant
state in the laboratory condition (21 °C and 60% relative humidity). The water content of the sand
fraction of raw materials ranged from 11.9% to 14.7%. It revealed that the presence of fine particles is
able to physically attract water: the finer the particles, the higher water content. This is specifically
the case for M84Df, which has the highest content of fine particles under 63 microns.
M84Df had the highest bulk density comparing with other three raw materials (the density of
Materials 2020, 13, 2994 12 of 26

Table 4. Physical properties of different samples.

Name of Materials Bulk Density (kg/m3 ) Absolute Density (kg/m3 ) Water Content (%)
M84Af 1018 – 11.9
M84Bf 1042 – 14.7
M84Cf 1021 – 12.9
M84Df 919 – 14.1
M37Af – 2676 3.8
M37Bf – 2649 6.1
M37Cf – 2648 8.8
M37Df – 2635 6.5
CRR11f – 2628 8.6
CRR22f – 2720 14.2

M84Df had the highest bulk density comparing with other three raw materials (the density of M84Df
was 919 kg/m3 , while it was 1042 kg/m3 for M84Bf in Table 4). It is difficult to draw conclusions from these
values without performing other types of measurements. Indeed, as previously stated, two parameters
(intrinsic density of the materials and packing density) intervene in this density, making the interpretation
difficult. However, the materials containing high water content and the finest particles content offered the
lowest bulk density (M84Df).
The mass variation of the samples at laboratory condition is shown in Figure 5. The result showed a
larger increase in mass over time for sample M84Df than for sample M84Cf. M84Df sample contains higher
amount of small particles, which can induce the creation of pores and favour capillary water absorption.
During the first week, the mass increase of the powders was the most consequent. This parameter still
increased in the following weeks, but, less importantly, the mass of the different samples continues to
progress but much more slowly. It is noteworthy that the results obtained are not correlated with the
previously calculated water content. In fact, the M84Bf sample, which has the highest value in terms of
humidity, has a lower mass gain vs the two other samples. Even more surprising, M84Af, which has a
relatively large mass gain, offers the lowest water content.
Physical properties of recycled materials after treatment (M37f) were broadly similar to those of
raw samples (M84f). However, higher absolute density of specimen collected after compaction (CRR11f)
and freeze–thaw cycles (CRR22f) could be correlated to higher fine content, even if the difference maybe
not discriminant.

4.2. Mineralogical and Chemical and Characterization

Tables 5 and 6 show the mineralogical and chemical compositions of the materials, respectively.
Powder diffractograms did not show significant differences between the four samples of raw materials.
They are, in fact, essentially composed of quartz and, in smaller proportions, of calcite, plagioclase and
potassium feldspars: cementitious components could also be present in the material and interfere with
interpretation. However, the presence of the minerals belonging to the group of clays in the M84Bf to Df
samples were observed, whereas M84Af did not seem to contain them. However, we must pay attention to
this last statement: the absence of peaks in clays in the latter may be due to the absence of these compounds
or their presence in too low levels to be detected. It indicated, incidentally, that no risk of swelling clay
effect had to be suspected.
 This parameter still increased in the following weeks, but, less importantly, the mass of the different
samples continues to progress but much more slowly. It is noteworthy that the results obtained are
not correlated with the previously calculated water content. In fact, the M84Bf sample, which has the
highest
Materials value
2020, in terms of humidity, has a lower mass gain vs the two other samples. Even more
13, 2994 13 of 26
surprising, M84Af, which has a relatively large mass gain, offers the lowest water content.

Figure 5. Capacity of water capture from atmospheric air of samples (M84Af to Df).
Figure 5. Capacity of water capture from atmospheric air of samples (M84Af to Df).
Table 5. Mineral composition of the different samples determined by XRD (%).
Physical properties of recycled materials after treatment (M37f) were broadly similar to those of
rawName
samples (M84f). However,
of Materials Calcite higher
Quartz absolute density
Plagioclases of specimen
Potassium collectedClay
Feldspars after compaction
Dolomite
(CRR11f)M84Af
and freeze–thaw12cycles (CRR22f)
68
could
7
be correlated 13
to higher fine content,
Not even if the
–
difference maybe not discriminant. detected
M84Bf 11 75 4 10 Detected –
M84Cf 14 71 7 8 Detected –
4.2. Mineralogical
M84Df
and Chemical
16
and Characterization
72 5 7 Detected –
Tables 5 and 6 show the mineralogical and chemical compositions of the materials, respectively.
M37Af 18 55 5 5 – 17
M37Bf 30 59 7 4 – 1
Powder diffractograms did not show significant differences between the four samples of raw
M37Cf 20 59 14 4 – 3
materials. They are, in fact,
M37Df 25 essentially
56 composed 4 of quartz and,9in smaller proportions,
– of 7calcite,
plagioclase and potassium feldspars: cementitious components could also be present in the Not
material
CRR11f 20 60 ≥3 16 –
and interfere with interpretation. However, the presence of the minerals belonging to the group of
detected
clays in CRR22f
the M84Bf to Df 17samples were Not
74 observed, 3 whereas M84Af6 did not seem –to contain them.
detected
However, we must pay attention to this last statement: the absence of peaks in clays in the latter may
be due to the absence of these compounds or their presence in too low levels to be detected. It
indicated, incidentally,
After treatment that no risk
in a recycling of swelling
plant, clay effect
the powder had to be (Table
diffractograms suspected.
5) did not show significant
Afterbetween
differences treatmentsamples,
in a recycling
except plant, the powder
for M37Af which diffractograms
contains many (Table 5) did compounds.
MgO-based not show
significant differences between samples, except for M37Af which contains many MgO-based
Fine materials are essentially composed of quartz (a little more for the sample taken after freeze–thaw)
compounds.
and, in smaller Fine materialsofare
proportions, essentially
calcite, composed
plagioclase and of quartz (afeldspars.
potassium little moreThefor the sample
high rate oftaken after
potassium
freeze–thaw) and, in smaller proportions, of calcite, plagioclase and potassium feldspars. The high
feldspars revealed the presence of large quantities of clay materials, specifically for CRR11f where
rate ofcontamination
possible potassium feldspars
duringrevealed
samplingthe presence ofFinally,
is envisaged. large quantities of clay materials,
X-ray fluorescence specifically
spectrometry allowed foran
CRR11f where
evaluation possible contamination
of the proportion of the differentduring sampling
compounds is envisaged.
present in the samplesFinally,
(TableX-ray
6) andfluorescence
confirmed a
spectrometry2 allowed an evaluation of the proportion of the different compounds presentproducts.
majority of SiO and CaO, which probably means a discriminant part of cementitious original in the
Materials 2020, 13, 2994 14 of 26

The compaction process and freeze–thaw cycles seem to have no effect on the mineral compositions
of materials.

Table 6. Chemical composition of the different samples determined by XRF (%).

Name of Materials M84Af M84Bf M84Cf M84Df CRR11f CRR22f

SiO2 70.00 60.59 59.87 60.20 60.62 64.19
TiO2 0.32 0.35 0.29 0.35 0.35 0.32
Al2 O3 4.47 6.44 5.19 6.58 6.44 6.43
Fe2 O3 2.31 3.10 3.69 2.93 2.89 2.75
MnO 0.05 0.12 0.26 0.06 0.06 0.06
MgO 0.74 0.85 1.25 0.74 0.97 0.97
CaO 9.71 12.38 13.95 10.08 12.35 11.87
Na2 O 0.17 0.13 0.14 0.16 0.11 0.14
K2 O 1.05 1.16 0.97 1.42 1.37 1.28
P2 O5 0.12 0.15 0.15 0.23 0.12 0.11
LOI 9.30 12.13 13.32 14.73 10.81 10.02
Total 98.25 97.39 99.09 97.47 96.09 98.14

Loss on ignition (LOI) at 500 ◦ C decreased for all raw materials after the treatment (Table 7).
The recycling process including pre-screen, crushing, sorting and decontamination (ferrous element, wood,
plastic and paper) in the four C&DW recycling facilities could improve the quality of recycled materials
by reducing the organic content. There was little difference between the samples, specifically at 1000 ◦ C
where it is possible to probably detect decomposition of calcite and magnesium carbonates [73].

Table 7. Chemical properties of different samples.

Name of Materials LOI at 500 ◦ C (%) LOI at 1000 ◦ C (%) SO4 2− Content (%) Cl− Content (%)
M84Af 5.18 8.96 1.568 0.024
M84Bf 4.5 12.30 1.786 0.024
M84Cf 3.46 13.53 0.618 0.016
M84Df 6.78 14.92 1.450 0.044
M37Af 2.25 17.76 0.617 0.020
M37Bf 2.60 12.72 0.722 0.028
M37Cf 2.12 10.01 0.541 0.020
M37Df 2.71 17.76 0.674 0.028
CRR11f 3.61 10.98 0.525 0.022
CRR22f 2.63 9.88 0.331 0.011

Chloride content of all studied materials is at a low level (Table 7). The chloride may often come from
de-icing salts sprayed during winter on civil engineering structures [36], even if in very small quantities in
the present specimens. After the treatment and compaction process the chlorides content remain low and
do not seem to be a risk for their use in cementitious mixtures. On the other hand, the risk of contact with
steel elements is unlikely at the level of base/sub-base road applications in which these recycled materials
are used.
The acid-soluble sulphate content values obtained for four raw materials decreased significantly
after the treatment. The origin of sulphates can be attributed to gypsum and plaster used in buildings.
After the treatment, all four samples were below the limits (0.8%) imposed according to Del Rey et al. [48].
It indicated that the decontamination of gypsum-based construction materials is efficient for all the four
recycling facilities. The solubility of sulphates should be restricted in road materials to guarantee the
Materials 2020, 13, 2994 15 of 26

dimensional stability of the section and to avoid potential adverse effect (expansive disruption) due to the
presence of sulphate near or in contact with concrete structure [74].
The investigations on raw fine materials do not reveal major differences, whatever the recycling plant
and the possible origin—building or civil engineering structures—of the materials: mostly containing SiO2 ,
with very low values of lime, sulphate, chlorides and inorganic materials, they mainly vary from sieving
curve and sieving grades. The investigations on fine materials after the treatment showed that the quality
of recycled aggregates (including the sulphate content, organic content) were improved. The removal of
impurities (such as organic matters, plastic, gypsum-base construction materials) and a pre-screening at
the beginning of the recycling process are very important, specifically for the quality and the quantity of
fine particles. Thus, the recycled aggregates from C&DW after treatment and good control can be used as
sub-base materials in road construction. In addition, the compaction process and freeze–thaw cycles seem
to have no or little effect on the mineral and chemical properties of the studied materials.

4.3. Mechanical Characterization

Table 8 shows the resistance to wear of samples determined by the micro-Deval coefficient and
LA abrasion resistance. An LA abrasion maximum value of 40 is normally adopted by road authority
specifications for road foundation construction [75]. The M37B and CRR11 sample meets these maximum
criteria, while the other samples are slightly above the limits. The micro-Deval coefficient maximum
values of 35 and 50 are required for primary roads (type I and IIa ) and secondary roads (type IIb and III),
respectively, according to road authority specifications for road foundation construction [75]. Three of the
four samples meet the maximum criteria for secondary roads foundation construction. This suggests that
the recycled aggregates from C&DW may have to be blended with other aggregates to enable its usage in
specific road foundation (for example for primary roads). After the compaction, the LA abrasion resistance
and micro-Deval value are slightly decreased, which means that the wear resistance of recycled aggregates
was slightly affected by the construction process. In addition, the freeze–thaw cycles seem to have no or
little effect on the wear resistance of studied materials.

Table 8. Micro-Deval resistance and LA abrasion resistance of different samples (%).

Name of Materials M37A M37B M37C M37D CRR11 CRR22

MDE 48 40 50.5 49 45.5 45.5
LA 42 39 42 46 39 42
MDE + LA 90 79 92.5 95 84.5 87.5

The optimum moisture content of M37A is obtained as 12% and the maximum dry density is
determined as 1.85 g/cm3 according to the laboratory Modified Proctor test. The results of gamma
densimeter (Table 9) show that the compaction degree varies from 83.13 to 90.06% of the optimum
laboratory Modified Proctor test condition. The compaction is therefore insufficient with regard to the
specifications for road foundation (95%). However, the compaction water content (Table 9) is lower than
the optimum moisture content obtained in laboratory (12%), which is possibly due to the lower compaction
degree on site than that of the laboratory condition. The compaction degree increases after 17 freeze–thaw
cycles (six months after the construction). The higher water content values after the freeze–thaw cycles
are obtained, which is possibly due to the rainwater penetration several days before test. To measure the
bearing capacity of the layer, static plate load tests has been carried out after the compaction. A bearing
capacity M1 of 33.2 MPa was obtained (Table 10), which is slightly lower than the specifications for the road
foundation (35 MPa) [75]. The compressibility coefficient m is relatively high (>2.5, Table 10). The bearing
capacity (M1 ) after freeze–thaw cycles is twice higher than that after its compaction. This could be due
lower than the optimum moisture content obtained in laboratory (12%), which is possibly due to the
lower compaction degree on site than that of the laboratory condition. The compaction degree
increases after 17 freeze–thaw cycles (six months after the construction). The higher water content
values after the freeze–thaw cycles are obtained, which is possibly due to the rainwater penetration
several
Materialsdays before
2020, 13, 2994 test. To measure the bearing capacity of the layer, static plate load tests has been 16 of 26
carried out after the compaction. A bearing capacity M1 of 33.2 MPa was obtained (Table 10), which
is slightly lower than the specifications for the road foundation (35 MPa) [75]. The compressibility
coefficient m is relatively
to self-cementing highof(>2.5,
properties Table 10).
fine fraction The bearing
of recycled capacity(unhydrated
aggregates (M1) after freeze–thaw
cement andcycles is
C2 S present
twice higher than that after its compaction. This could be due to self-cementing properties as
in the adherent mortar of fine RCA, especially the active fractions of 0–0.15 and 0.3–0.6 mm of reported
fine
fraction
by Poonofetrecycled
al. [76] andaggregates
Sangiorgi (unhydrated
et al. [52]). cement
Poon et and C2Sindicated
al. [76] present inthat
thethe
adherent mortar
grade, age andof fine of
amount
RCA, especially the active fractions of 0–0.15 and 0.3–0.6 mm as reported by Poon et al. [76] and
cementitious materials used in the original concrete would be the deciding factors on the self-cementing
Sangiorgi
propertiesetofal. [52]). Poon
sub-base et al.Furthermore,
materials. [76] indicated thethat
finethe grade,
particle age and (fraction
percentage amount of cementitious
0/0.125 mm) slightly
materials
increasedused
andin the original
some breakingconcrete
occurred would
duringbe the deciding factors
compaction: on theofself-cementing
the grading RCA has thusproperties
changed after
of sub-base materials. Furthermore, the fine particle percentage (fraction 0/0.125 mm) slightly
compaction process. The effects of the compaction effort and the rate of the compaction could favour the
increased and some
self-cementing breaking
properties occurred
of sub-base during compaction:
materials. the drainage
In addition, the grading of RCA
of the has thus
sub-base changedcould
materials
after compaction process. The effects of the compaction effort and the rate of the compaction could
also improve the bearing capacity of road foundation.
favour the self-cementing properties of sub-base materials. In addition, the drainage of the sub-base
Table 9. The results of gamma densimeter measurement of road foundation after the compaction (CRR11)
materials could also improve the bearing capacity of road foundation.
and freeze–thaw cycles (CRR22).
Table 9. The results of gamma
Afterdensimeter
Compactionmeasurement
(CRR11) of roadAfter
foundation after the
Freeze–Thaw compaction
Cycles (CRR22)
(CRR11) and freeze–thaw cycles (CRR22).
Depth from Surface (cm) −5 −15 −30 −5 −15 −30
Water content (%) After
10.45Compaction9.11 (CRR11) After 8.84 Freeze–Thaw
15.91 Cycles
14.36(CRR22)13.98
Depth from Surface
Compaction (cm)
degree (%) −5
83.13 −15
88.07 −30
90.06 −5
86.16 −15
91.49 −30 94.46
Water content (%) 10.45 9.11 8.84 15.91 14.36 13.98
Compaction degree (%) 83.13
Table 10. The 88.07
results of plate load test for90.06 86.16
CRR11 and CRR22. 91.49 94.46

Bearing Capacity M (MPa) Bearing Capacity M (MPa) Report m = M2 /M1

Table 10. The results of plate
1
load test for CRR11 and CRR22.
2

After compaction (CRR11) 33.2 110.4 3.3

After freeze–thaw cycles Bearing Capacity M1 (MPa) Bearing Capacity M2 (MPa) Report m = M2/M1
After compaction 68.733.2 181.8 3.3 2.65
(CRR22) (CRR11) 110.4
After freeze–thaw cycles (CRR22) 68.7 181.8 2.65

4.4. Shape Characterization

4.4. Shape Characterization
The results of shape analysis are presented from the coarsest to the finest particle size fraction, in
The results of shape analysis are presented from the coarsest to the finest particle size fraction,
graphical form. The legend is shown here below:
in graphical form. The legend is shown here below:

The samples (84Af, 84Bf, 84Cf and 84Df) contained small quantity of particles with a particle size
greaterThe samples
than 4 mm, (84Af, 84Bf,
while the 84Cf and
samples 84Df)
(37Af, contained
37Bf, small
37Cf, 37Df and quantity of particlesonly
CRR11f) contained withthea fraction
particle size
greater
lower than
than 4 mm,
4 mm while
(the theanalysis
shape samplesof (37Af, 37Bf,larger
particles 37Cf, than
37Df 4mm
and CRR11f)
is shown contained
in Figureonly theAppendix
A1 in fraction lower
than 4 mm (the shape analysis of particles larger than 4mm is shown in Figure A1 in Appendix
section). It should be noted that these analyses focused on only 63 to 130 particles, which is quite A). It
lowshould
be anoted
for that
precise these
shape analyses focused
characterization. Noon only 63 conclusion
definitive to 130 particles, which isbe
can therefore quite low for
inferred a precise
as regards shape
this
characterization. No
particle size fraction. definitive conclusion can therefore be inferred as regards this particle size fraction.
Between 500 and 4000 particles have been analysed, depending on the particle size: the larger the size,
the lower the number of analyses (Figures 6 and 7 and Figures A2–A6 in Appendix A).
An image treatment was applied on granular fraction 0.020–0.063 mm for removing particles smaller
than 0.020 mm (Figure A6 in Appendix A). Indeed, below this dimension, the number of pixels used in
the shape measurement is too small to obtain significant results. About 8000 particles were analysed for
each sample.
Significant differences in shape were observed for the nine samples in each of the granular fractions
tested. Most of the time, the trends were consistent for the same sample from one granular fraction to
another. The raw sample M84Cf contained globally more rounded particles than all the others, in particular
because of the coarse particles. However, for fines (<0.125 mm), raw sample M84Df had significantly
higher bluntness values. In the size fraction 0.125–0.25 mm, and to a lesser extent for the other fractions,
Materials 2020, 13, 2994 17 of 26

the difference between the raw samples M84 and the recycled samples after treatment M37 was particularly
visible. Raw fine materials (M84) globally offered higher bluntness but equal elongation and convexity
than recycled fine materials (M37). The recycling process, particularly the crushing process, could modify
theMaterials
particle2020,
Materials 2020,13,
shape13,xx[30].
FOR
FORPEER
PEER
No REVIEW
REVIEW
major differences between the four recycled samples (M37A to D) appeared. 16
16of
of24
24
After the compaction process, the values of Occhio bluntness and convexity increased slightly, while the
Between
elongation values500
Between 500 and
and4000
remained, 4000 particles
particles
despite somehave
have been
beenanalysed,
breakdownanalysed, depending
depending
that occurred on the
the particle
particle size:
oncompaction.
during size: the
thelarger
larger
the size, the lower the number of analyses (Figures 6, 7 and Figures A2–A6 in Appendix
the size, the lower the number of analyses (Figures 6, 7 and Figures A2–A6 in Appendix section). section).

Figure
Figure
Figure 6.6.Shape
6. Shape Shape analysis
analysis
analysis of
ofparticles
particles
of particles (0.125–0.25
(0.125–0.25
(0.125–0.25 mm)mm)
(84 (84
mm) (84refers
refers
refers to
toraw
to raw raw materials:
84A,84A,
materials:
materials: 84B,84B,
84A, 84C84C
84B, andand
84C and
84D
84D
refer to refer
M84Af, to M84Af,
M84Bf, M84Bf,
M84Cf andM84Cf
M84Df, and M84Df,
respectively;respectively;
37 refers to 37 refers
recycled to recycled
84D refer to M84Af, M84Bf, M84Cf and M84Df, respectively; 37 refers to recycled materials after
materials aftermaterials after
treatment: 37A,
37B,treatment:
treatment:
37C and 37D 37A,
37A, 37B,to37C
37B,
refer 37Cand
and37D
recycled 37Drefer to
torecycled
referafter
materials recycled materials
M37Af,after
materials
treatment aftertreatment
M37Bf, treatment M37Af,
M37Af,
M37Cf and M37Df,M37Bf,
M37Bf, M37Cf
M37Cf
respectively;
CRR and
and M37Df,
M37Df,
refers respectively;
respectively;
to recycled CRR
CRR
materials refers
refers
after to
torecycled
recycled
compaction: materials
materialsafter
CRR11f). aftercompaction:
compaction:CRR11f).
CRR11f).

Figure
Figure
Figure 7.7.Shape
7. Shape Shape analysis
analysis
analysis of
ofparticles
particles
of particles (0.063–0.125
(0.063–0.125
(0.063–0.125 mm) mm)
(84 (84
mm) (84refers
refers
refers to
toraw
to raw raw materials:
84A,84A,
materials:
materials: 84B,84B,
84A, 84C84C
84B, andand
84C and
84D
84D
refer to refer
M84Af, to M84Af,
M84Bf, M84Bf,
M84Cf andM84Cf
M84Df, and M84Df,
respectively;respectively;
37 refers to 37 refers
recycled to recycled
materials
84D refer to M84Af, M84Bf, M84Cf and M84Df, respectively; 37 refers to recycled materials afteraftermaterials
treatment:after
37A,
37B,treatment:
37C and 37D
treatment: 37A,
37A, 37B,
refer to37C
37B, 37Cand
and37D
recycled 37Drefer
materials to
torecycled
referafter materials
treatment
recycled M37Af,after
materials treatment
M37Bf,
after M37Af,
M37Cf and
treatment M37Bf,
M37Df,
M37Af, M37Cf
respectively;
M37Bf, M37Cf
CRR and M37Df,
refers to respectively;
recycled CRR
materials refers
after to recycled
compaction: materials
CRR11f). after compaction:
and M37Df, respectively; CRR refers to recycled materials after compaction: CRR11f). CRR11f).

An
An image
image treatment
treatment was
was applied
applied on
on granular
granular fraction
fraction 0.020–0.063
0.020–0.063 mmmm for
for removing
removing particles
particles
smaller than 0.020 mm (Figure A6 in Appendix section). Indeed, below this dimension,
smaller than 0.020 mm (Figure A6 in Appendix section). Indeed, below this dimension, the number the number
of
ofpixels
pixelsused
usedin
inthe
theshape
shapemeasurement
measurementisistoo
toosmall
smalltotoobtain
obtainsignificant
significantresults.
results.About
About8000
8000particles
particles
were analysed for each sample.
were analysed for each sample.
Significant
Significant differences
differences in
in shape
shape were
were observed
observed for
for the
the nine
nine samples
samples in
in each
each of
of the
the granular
granular
fractions
fractions tested. Most of the time, the trends were consistent for the same sample from onegranular
tested. Most of the time, the trends were consistent for the same sample from one granular
Materials 2020, 13, 2994 18 of 26

5. Conclusions
In this study, the effects of recycling process, compaction and freeze–thaw cycles on the properties of
recycled fine aggregates obtained from C&DW used for unbound sub-base were evaluated. In addition,
special attention was also provided for the shape analysis of fines. The following conclusions may
be reached from the present investigations concerning the analysis of properties of the fine particles
(under 4 mm) produced by recycling C&DW:

• The recycling process including pre-screening, crushing, sorting and decontamination (ferrous element,
wood, gypsum-based construction materials) could decrease the quantity of bricks and tiles present
in the coarse fraction 4/30 mm and slightly increase their quantity within a fine fraction. In particular,
the sulphate content could be limited by removing impurities and a pre-screening control at the
entrance of raw materials;
• Main discriminant parameter is the sieving curve and the proportion of grades. The mixes containing
the highest quantity of fine particles, specifically lower than 63 µm, usually induced a higher water
demand and a higher capillary rise. These fine particles represent a detrimental product for long term
unbounded foundations in road structures;
• Compaction did not seem to have a major effect on the production of fines (despite some breakdown that
occurred during compaction) and on the shape of materials. Mineralogy and chemical characteristics
remained globally similar after the compaction, which means no specific degradation of materials
with construction process. Freeze–thaw cycles had no measurable effect on the sieving distribution
of particles, specifically the production of fines, or the mineralogy and chemical characteristics
of materials;
• Bluntness was increasing with finer particles, which means higher surface roughness and higher
potential interaction with water. Raw fine materials globally offered higher bluntness but equal
elongation and convexity compared to recycled fine materials. After the compaction process,
the bluntness and convexity increased slightly, while the elongation values remained similar,
despite some breaking occurring during compaction;
• The LA abrasion resistance and micro-Deval coefficient values are slightly affected by the construction
process, while freeze–thaw cycles seem to have no or little effect on the wear resistance of the studied
materials. The material used for unbound road sub-base could meet the maximum criteria for
secondary roads foundation construction on the wear resistance criteria. The recycled aggregates
from C&DW without sufficient quality may have to be blended with other aggregates to enable their
usage in certain road foundation (for example, for high-quality primary roads). The static plate load
tests showed that bearing capacity is slightly lower than the specifications for the road foundation
after compaction. After 6 months’ drainage and freeze–thaw cycles, the bearing capacity of sub-base
materials is improved due to the self-cementing properties of fine RCA and the drainage of sub-base
materials. The long term behaviours of road sub-base using fine RCA in full-scale trails (e.g., after
several years’ daily traffic) could be interesting to be investigated in the future.

The most important parameter to be checked before using recycled materials as unbound base/sub-base
applications is definitely the content of particles finer than 63 µm that has to be strictly limited. This study
has been focused on the experimental analysis the effects of recycled fine aggregates from C&DW for the
unbound road sub-base. The theoretical modelling of the analysed parameters (especially the effects of
properties of recycled aggregates, the compaction process, and freeze–thaw cycles) on the properties of
unbound road sub-base could be interesting for the future study.
New processes for Construction and Demolition Waste treatment have been recently set up: washing
a grade lower than 4 mm allows to obtain a very good quality sand (as well as for coarser aggregates
Materials 2020, 13, 2994 19 of 26

which are also washed). These products can be actually used for a concrete skeleton and the production of
precast concrete products.

Author Contributions: Conceptualization, M.R. and L.C. Data curation, M.R. Formal analysis, Z.Z. Funding acquisition,
L.C. Investigation, M.R. Methodology, M.R. and Z.Z. Project administration, L.C. Resources, F.M. Supervision,
L.C. Validation, L.C., F.M. and Z.Z. Visualization, F.M. Writing—original draft, L.C. and Z.Z. Writing—review &
editing, L.C., Z.Z. and F.M. All authors have read and agreed to the published version of the manuscript.
Funding: This research is supported through the Government of Wallonia (DGO6) project APERROUT
(Convention 1217817) Amélioration des PErformances des Recyclés dans le domaine Routier par Optimisation
des Unités de TraitEment (Increasing Performances of Recycled Materials for Road Construction by means of Treatment
Unit Optimization).
Acknowledgments: The authors would like to thank the Government of Wallonia (DGO6) for financial support through
the project APERROUT (Convention 1217817) Amélioration des PErformances des Recyclés dans le domaine Routier
par Optimisation des Unités de TraitEment (Increasing Performances of Recycled Materials for Road Construction by
means of Treatment Unit Optimization). The authors would also like to thank the different participants of this project
for their contributions.
Conflicts of Interest: The authors declare no conflict of interest.

Acronyms
C&DW Construction and Demolition Waste
CB Crushed Brick
CBR California Bearing Ratio
CRR11 Recycled materials after compaction
CRR22 Recycled materials after freeze–thaw cycles
LA Los Angeles
LOI Loss On Ignition
M84 Raw materials
M37 Recycled materials after treatment
Particle Size Distribution curves weighted by apparent
PSD-V’
Volume
RAP Reclaimed Asphalt Pavement
RCA Recycled Concrete Aggregates
XRD X-ray Diffraction
XRF X-ray Fluorescence
WR Waste excavation Rock
Materials 2020, 13, 2994 20 of 26

Appendix A
Materials 2020, 13, x FOR PEER REVIEW 19 of 24
Materials 2020, 13, x FOR PEER REVIEW 19 of 24

Figure A1. Shape analysis of particles (>4 mm) (84A, 84B, 84C and 84D refer to raw materials M84Af,
Figure
Figure A1.Shape
A1. Shapeanalysis
analysisof
ofparticles
particles (>4
(>4 mm)
mm) (84A,
(84A,84B,
84B,84C
84Cand
and84D
84Drefer
refertoto
raw materials
raw M84Af,
materials M84Af,
M84Bf, M84Cf and M84Df, respectively).
M84Bf,
M84Bf, M84Cf
M84Cf and
and M84Df,
M84Df, respectively).
respectively).

Figure
Figure A2.A2. Shape
Shape analysis
analysis of particles
of particles (2–4(2–4
mm)mm) (84 refers
(84 refers to materials:
to raw raw materials:
84A, 84A, 84B,and
84B, 84C 84C84D
andrefer
84Dto
Figure A2. Shape analysis of particles (2–4 mm) (84 refers to raw materials: 84A, 84B, 84C and 84D
refer to
M84Af, M84Af,
M84Bf, M84Bf,
M84Cf M84Cf
and M84Df,andrespectively;
M84Df, respectively;
37 refers to37 recycled
refers to recycled
materialsmaterials after treatment:
after treatment: 37A, 37B,
refer to M84Af, M84Bf, M84Cf and M84Df, respectively; 37 refers to recycled materials after treatment:
37A,
37C and37B,
37D37C and
refer to 37D refermaterials
recycled to recycled materials
after afterM37Af,
treatment treatment M37Af,
M37Bf, M37Bf,
M37Cf and M37Cf
M37Df,and M37Df,
respectively;
37A, 37B, 37C and 37D refer to recycled materials after treatment M37Af, M37Bf, M37Cf and M37Df,
respectively;
CRR CRR refers
refers to recycled to recycled
materials materials after
after compaction: compaction: CRR11f).
CRR11f).
respectively; CRR refers to recycled materials after compaction: CRR11f).
Materials
Materials2020, 13,13,
2020, 2994
x FOR PEER REVIEW 21 24
20 of of 26
Materials 2020, 13, x FOR PEER REVIEW 20 of 24

Figure A3. Shape analysis of particles (1–2 mm).

Figure
FigureA3.
A3.Shape
Shapeanalysis
analysisofofparticles
particles(1–2
(1–2mm).
mm).

Figure
Figure A4.
A4. Shape
Shapeanalysis
analysisof
ofparticles
particles(0.5–1
(0.5–1mm).
mm).
Figure A4. Shape analysis of particles (0.5–1 mm).

Figure A5. Shape analysis of particles (0.25–0.5 mm).

Materials 2020, 13, 2994 22 of 26
Figure A4. Shape analysis of particles (0.5–1 mm).

Materials 2020, 13, x FOR PEER REVIEW 21 of 24

Figure
Figure A5.
A5. Shape
Shape analysis
analysis of
of particles
particles (0.25–0.5
(0.25–0.5 mm).
mm).

Figure
FigureA6.
A6.Shape
Shapeanalysis
analysisofofparticles
particles(0.020–0.063
(0.020–0.063mm).
mm).

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