Comparing The Field and Laboratory Curing Behavior of Cold Recycled Asphalt Mixtures For Binder Courses

materials
Article
Comparing the Field and Laboratory Curing
Behaviour of Cold Recycled Asphalt Mixtures for
Binder Courses
Gilda Ferrotti 1, * , Andrea Grilli 2 , Chiara Mignini 1 and Andrea Graziani 1
1 Department of Civil and Building Engineering and Architecture, Polytechnic University of Marche,
60131 Ancona, Italy; c.mignini@pm.univpm.it (C.M.); a.graziani@staff.univpm.it (A.G.)
2 Department of Economics, Science and Law, University of the Republic of San Marino,
47890 San Marino City, San Marino; andrea.grilli@unirsm.sm
* Correspondence: g.ferrotti@staff.univpm.it

Received: 21 September 2020; Accepted: 19 October 2020; Published: 22 October 2020
Abstract: The cold recycling of reclaimed asphalt (RA) for the rehabilitation of end-of-life pavements
is becoming very common. Cold recycled asphalt mixtures (CRAMs) are characterised by a curing
time, required to reach the material design mechanical performance. Since the laboratory simulation
of the long-term field curing is not yet a standardised procedure, a CRAM was laid as binder course
in a full-scale trial section that was monitored for more than two years. The comparison between field
curing and oven-curing in laboratory at 40 ◦ C was performed by carrying out indirect tensile stiffness
modulus (ITSM), indirect tensile strength (ITS) and complex modulus tests, as well as measurements
of the air voids content. The evolution of the ITSM as a function of the curing time (field/oven-curing)
was obtained for both gyratory specimens and cores taken from the trial section at different time
periods. Results showed that the material stiffness development can be accelerated with a small
effect on its long-term value if oven-curing is applied a few days/weeks after compaction. A linear
relationship was found between the ITS measured on the cores and their air voids content. Finally,
the complex modulus tests confirmed that CRAMs provide an intermediate behaviour between
asphalt concrete mixtures and cement-bound mixtures.
Keywords: cold recycling; curing; indirect tensile strength; indirect tensile modulus; reclaimed
asphalt; bituminous emulsion
1. Introduction
In the rehabilitation of end-of-life pavements, the focus on cold recycled materials (CRMs) is strongly
on the rise, allowing the reuse of reclaimed asphalt (RA) in a cost-effective and environmentally
friendly way [1].
The use of different binding agents (i.e., emulsified or foamed bitumen and cement) and their
dosages lead to the acquisition of different types of CRM [2], such as bitumen stabilised materials
(BSMs), cold recycled asphalt mixtures (CRAMs) and cement–bitumen treated materials (CBTMs) [3,4].
The CRM mechanical behaviour is strictly linked to its composition [5], providing mixtures with
properties ranging from those similar to unbound granular materials [6] to those of materials
characterised by an intermediate behaviour between cement-bound mixtures [3,7,8] and asphalt
concrete (AC). For this reason, several authors have characterised the mechanical behaviour of
CRAM by using the complex modulus [9–11]. For CRAMs and CBTMs, the combined effect of
bitumen and cement is very effective in terms of water sensitivity [7,8,12–14] and high-temperature
stability [12,13,15].
Materials 2020, 13, 4697; doi:10.3390/ma13214697 www.mdpi.com/journal/materials

Materials 2020, 13, 4697 2 of 19
The CRM composition in terms of RA content, is mainly related to the recycling technique [9,16,17].
Cold in-place recycling (CIR) is carried out directly at the jobsite and involves only the bituminous layers.
Therefore, the RA aggregate content may reach 100% of the aggregate blend. Full-depth reclamation
(FDR) [8,18] is also carried out at the jobsite and involves the full-depth of the pavements, including the
bituminous layers and the underlying granular or cemented layers. In this case, the RA content may be
reduced to about 30%. Cold central-plant recycling (CCPR) is carried out in a fixed or mobile plant,
where selected RA aggregate and virgin aggregate can be combined in the optimal way. The possibility
to better control the proportion of the mixture components during material production with CCPR
makes this technology able to produce high-performance CRMs for binder and base courses [17].
The selection of the most appropriate CRM composition and recycling technique depends on
several factors such as equipment and material availability, thickness and level of the pavement
degradation, as well as economic considerations. CRM reaches its design mechanical properties
in terms of strength and stiffness only after a specific curing period [19]. Depending on the CRM
composition, the curing process results from a combination of several mechanisms such as emulsion
breaking, moisture loss and hydration of cementitious compounds [4,7,20–22]. The curing in the field
is a gradual process which may require some weeks or even months and is affected by several factors
such as temperature, relative humidity, drainage conditions, and layer thickness [4,23]. Specifically,
higher temperatures accelerate the curing [23,24], whereas the influence of the relative humidity is
mainly linked to the presence of cement [25]. Indeed, a higher humidity promotes the formation of
cementitious bonds, thus increasing the material stiffness.
To investigate the long-term performance of the CRMs, the curing is usually accelerated in laboratory
by subjecting the specimens to oven-curing at a fixed temperature for several days. Many procedures
for curing acceleration exist [26]. The most widespread consists of oven-cure CRM specimens at 40 ◦ C
for 3 days immediately after compaction, even if it does not seem to guarantee the achievement of the
maximum mixture performance [27].
The main objective of this study was to compare the long-term behaviour of field-cured and
laboratory-cured CRAM mixtures. To this end, a trial section was carried out by applying, as binder
course, a CRAM produced in an asphalt plant (CCPR technique). Laboratory specimens were
compacted immediately after CRAM production and cores were taken from the trial section at several
time intervals (up to 796 days after construction). The evolution of the indirect tensile stiffness
modulus (ITSM) was studied in different curing conditions: oven-curing at 40 ◦ C, in the field and in a
combination of field and oven-curing. Moreover, the relationship between indirect tensile strength
(ITS) and air voids content was obtained. Finally, the rheological characterisation of the studied CRAM
was performed by measuring and modelling the complex modulus of field specimens.
2. Experimental Program
2.1. Materials and Mixture

The CRAM consists of RA aggregate, virgin river sand, mineral filler, bituminous emulsion,
cement and water.
The main characteristics of the RA aggregate and river sand are shown in Tables 1 and 2,
respectively. A mineral filler with high fineness (Table 3) was chosen to increase the fine content in the
blend and improve the bituminous mastic consistency.
Materials 2020, 13, 4697 3 of 19
Table 1. Reclaimed asphalt (RA) aggregate characteristics.
Parameter Standard Value

Aggregate size (mm) EN 933-1 [28] 16
Passing at 0.063 mm (%) EN 933-1 [28] 5.6
Flakiness index (%) EN 933-3 [29] 7.3
Shape index (%) EN 933-4 [30] 5.7
Crushed aggregate particle (%) EN 933-5 [31] 100
Sand Equivalent (%) EN 933-8 [32] 70.6
Resistance to fragmentation (%) EN 1097-2 [33] 17
Water absorption (%) EN 1097-6 [34] 1.3
Bitumen content to mixture (%) EN 12697-1 [35] 4.1
Table 2. Fine aggregate characteristics.

Fines content (%) EN 933-1 [28] 2.0
Sand equivalent (%) EN 933-8 [32] 81
Methylene blue (g/kg) EN 933-9 [36] 1.2
Density (Saturated surface dry) (Mg/m3 ) EN 1097-6 [34] 2.64
Loose bulk density (Mg/m3 ) EN 1097-3 [37] 1.56
Water absorption (%) EN 1097-6 [34] 1.0
Table 3. Filler characteristics.

Passing at 2 mm (%) EN 933-1 [28] 100
Passing at 0.125 mm (%) EN 933-1 [28] 98
Passing at 0.063 mm (%) EN 933-1 [28] 95
Methylene blue (g/kg) EN 933-9 [36] 3.5
Fineness (Blaine) (cm2 /g) EN 196-6 [38] 6500
An over-stabilised bituminous emulsion, designated as C60B10 (EN 13808 [39]) and a Portland
limestone cement, designated as CEM II/B-LL 32.5R (EN 197-1 [40]) were selected as co-binders.
Their main characteristics are shown in Tables 4 and 5.
Table 4. Portland cement characteristics.
Parameter Standard Value Specifications

Setting time (min) EN 196-3 [41] 140 >75
Fineness (Blaine) (cm2 /g) EN 196-6 [38] 4900 -
Strength after 2 days (MPa) EN 196-1 [42] 22 >10
Strength after 28 days (MPa) EN 196-1 [42] 42 ≥32.5
Table 5. Bituminous emulsion characteristics.
Parameter Standard Value Specification

pH value (pH) EN 12850 [43] 2.45 positive
Residual binder (%) EN 1431 [44] 59.8 60 ± 2
Storage stability (%) EN 1429 [45] 3 ≤10
Breaking value (–) EN 13075-1 [46] 190 >150
Mixing stability with cement (g) EN 12848 [47] <0.2 <2
Characteristic of bitumen (EN 13074 [48])
Penetration value (mm × 10−1 ) EN 1426 [49] 58 <100
Softening point (◦ C) EN 1427 [50] 47.8 >45
Materials 2020, 13, 4697 4 of 19
The mix design of the CRAMs employed in this research was carried out in accordance with
the specifications of the Republic of San Marino road agency [51]. The design aggregate blend was
obtained by combining 88% of RA aggregate, 10% of river sand and 2% of filler (Table 6 and Figure 1).
The design bituminous emulsion dosage, by dry aggregate mass, was 4.5% and 4.0% (2.7% and 2.4% of
residual bitumen) for the mixes employed for the binder and base courses, respectively. The design
cement dosage, by dry aggregate mass, was 2.0% and the total water content was 5.0% by dry aggregate
mass (including both the emulsion water and prewetting water). At the design composition, the CRAM
specimens compacted with a gyratory compactor at 100 gyrations had a dry density of 2.123 Mg/m3
(EN 12697-6 [52]) and an average indirect tensile strength (ITS) (EN 12697-23 [53]) value at 25 ◦ C of
0.41 MPa (curing for13,72
Materials 2020, h at
x FOR ◦ C).
40REVIEW
PEER 4 of 20
density of 2.123 Mg/m3 (EN 12697-6 [52]) and an average indirect tensile strength (ITS) (EN 12697-23
Table 6. Design gradation and specification limits.
[53]) value at 25 °C of 0.41 MPa (curing for 72 h at 40 °C).
Design Gradation
Sieve Size (mm) Table 6. Design gradation and specification
Specificationlimits.
Limits (% Passing)
(% Passing)
Design Gradation
Sieve
31.5 Size (mm) Specification Limits (% Passing)
(% 100
Passing) 100–100
20 31.5 99
100 90–100
100–100
16 20 96
99 90–100
14 16 93
96
12.5 14 88
93
10 12.5 79
88 50–80
8 10 71
79 50–80
6.3 8 62
71
5 6.3 54
62
4 5 46
54 30–55
2 4 33
46 20–40
30–55
0.5 2 19
33 10–25
20–40
0.25 0.5 19
16 10–25
0.063 0.25 16
5.1 3–8
0.063 5.1 3–8
100
90 Design gradation
80
Specification limits
70
Passing [%]
60
50
40
30
20
10
0
0.01 0.1 1 10 100
Sieve size [mm]
Figure 1.1.Design
Figure gradation.
Design gradation.
2.2. Trial Section

2.2. Trial Section
2.2.1. Mixing Plant
2.2.1. Mixing Plant
To produce the CRAM, a mix plant for cement treated mixtures was modified by adding an inlet
To produce the system
and storage CRAM, forathe
mix plant foremulsion
bituminous cement(Figure
treated
2). mixtures was
The emulsion is modified by adding
directly discharged at an inlet
and storage system
around for
55 °C the
into thebituminous emulsion (Figure
twin-shaft counter-rotating 2). The
mixer, almost emulsion iswith
simultaneously directly discharged at
aggregates,
◦ C into
around 55 filler, cement
theand water. Thecounter-rotating
twin-shaft mixing requires 20 smixer,
and afterwards
almost the cold mixture is transferred
simultaneously into
with aggregates, filler,
a storage bin before being discharged into waiting trucks. The capacity of the mixing plant is 200 t/h.
cement and water. The mixing requires 20 s and afterwards the cold mixture is transferred into a
storage bin before being discharged into waiting trucks. The capacity of the mixing plant is 200 t/h.
Materials 2020, 13, 4697 5 of 19
Materials 2020, 13, x FOR PEER REVIEW 5 of 20
Figure 2. Mixing plant for cold mixture production.

Figure
Figure 2. Mixing plant
2. Mixing plant for
for cold
cold mixture
mixture production.
production.
2.2.2.
2.2.2. Construction
Construction ofof theTrial
the TrialSection
Section
2.2.2. Construction of the Trial Section
The trial section was constructed adjacent to the mixing plant that is located in central-northern
The trial section was constructed adjacent to the mixing plant that is located in central-northern
Thewhere
Italy, trial section was constructed
a Mediterranean climateadjacent to the
is present. mixing
Since plant that
the curing is located
of CRAMs in central-northern
strongly depends on
Italy, where a Mediterranean climate is present. Since the curing of CRAMs strongly depends on
Italy, where
climatic a Mediterranean
conditions, the dailyclimate is present.
temperatures Since
and the the days
rainy curing of collected
were CRAMs strongly depends on
at a meteorological
climatic conditions, the daily temperatures and the rainy days were collected at a meteorological station
climatic
stationconditions,
35 km away thefrom
dailythetemperatures
mixing plant.and
They the
arerainy
showndays were collected
in Figure atfrom
3, starting a meteorological
the day of
35 km away from the mixing plant. They are shown in Figure 3, starting from the day of production
production
station 35 kmand awaylaying
from(24the
March 2018)
mixing until They
plant. about are
5 months
shownlater (31 August
in Figure 2018). from the day of
3, starting
and laying (24 March 2018) until about 5 months later (31 August 2018).
production and laying (24 March 2018) until about 5 months later (31 August 2018).
40
Rainy days Tmin Taverage Tmax
40 35
Rainy days Tmin Taverage Tmax
35 30
30 25
Temperature [°C]
25 20
Temperature [°C]
20 15
15 10
10 5 March April May June July August
0
5
March
0 April
20 40 May 60 80June 100 July
120 140 August160 180
0 Days from construction
0 20 40 60 80 100 120 140 160 180
Figure 3. Rainy days (vertical lines) and moving average (period = 7 days) of daily temperatures near
Figure 3. Rainy days (vertical lines) and moving
Days average (period = 7 days) of daily temperatures near
from construction
the plant.
the plant.
Figure
The 3. Rainy
trial days
section (vertical
(Figure 4),lines) and moving
detailly average
described (periodet=al.
by Grilli 7 days)
[54],ofconsists
daily temperatures near
of five subsections
theThe trial section (Figure 4), detailly described by Grilli et al. [54], consists of five subsections (A,
plant.
(A, B, C, D and E) characterised by different layers (Figure 5) and different compaction procedures
B, C, D and E) characterised by different layers (Figure 5) and different compaction procedures of the
of the
CRAMCRAMbinderbinder course
course (Table(TableBefore
7). Before construction, staticload
platetests
load tests18134
(DIN[55])
18134 [55])
The trial section (Figure 4),7). construction,
detailly described staticetplate
by Grilli al. [54], consists(DIN were
of five subsections (A,
were performed
performed on on
thethe subgrade
subgrade of of
all all subsections
subsections and and
the Ethe Ev1 modulus results are shown
v1 modulus results are shown in Figure 5.
in Figure 5.
B, C, D and E) characterised by different layers (Figure 5) and different compaction procedures of the
CRAM binder course (Table 7). Before construction, static plate load tests (DIN 18134 [55]) were
performed on the subgrade of all subsections and the Ev1 modulus results are shown in Figure 5.
the width of the layer in no more than four overlapping passes assuming that the overlap is not less
the width of the layer in no more than four overlapping passes assuming that the overlap is not less
than 20 cm.
than 20 cm.
All the Subsections were opened to traffic 4 days after construction. Traffic data were collected
All the Subsections were opened to traffic 4 days after construction. Traffic data were collected
for Subsection B, C and D. After two years from construction, Subsection B was subjected to heavy
for Subsection B, C and D. After two years from construction, Subsection B was subjected to heavy
traffic corresponding to about 270,000 cycles of 80 kN equivalent standard axle load (ESAL) whereas
traffic corresponding to about 270,000 cycles of 80 kN equivalent standard axle load (ESAL) whereas
Materials Subsections
2020, 13, 4697 C
Subsections
and D were subjected to about 70,000 ESAL. No distresses are visible on the
C and D were subjected to about 70,000 ESAL. No distresses are visible on the 6 of 19
Subsections.
Subsections.
Figure 4. Location of the five Subsections.

Subsection A Subsection B Subsection C Subsection D Subsection E

Subsection A Subsection B Subsection C Subsection D Subsection E
AC11: 4 cm AC11: 4 cm AC11: 4 cm Surface dressing Surface dressing
AC11: 4 cm
Tack coat AC11: 4 cm
Tack coat AC11: 4 cm
Tack coat Surface dressing Surface dressing
Tack coat Tack coat Tack coat
Binder course Binder course Binder course Binder course Binder course
Binder course Binder course Binder course Binder course Binder course
CRAM: 12 cm CRAM: 10 cm CRAM: 12 cm CRAM: 12 cm CRAM: 12 cm
CRAM: 12 cm CRAM: 10 cm CRAM: 12 cm CRAM: 12 cm CRAM: 12 cm
Prime coat Prime coat Prime coat Prime coat
Prime coat Prime coat Prime coat Prime coat
Ev1 = 103 MPa Ev1 = 102 MPa Ev1 = 143 MPa Ev1 = 115 MPa
Ev1 = 103 MPa Ev1 = 102 MPa Ev1 = 143 MPa Ev1 = 115 MPa
Base course
Base course
CRAM: 20 cm
CRAM: 20 cm
Prime coat
Prime coat
Ev1 = 163 MPa

Ev1 = 163 MPa
Figure Scheme
5. 5.
Figure Schemeof
of the Subsections
the Subsections composition.
composition.
Figure 5. Scheme of the Subsections composition.
Table 7. Compaction procedure of the cold recycled asphalt mixture (CRAM) binder course.
First Phase Second Phase Third Phase

Subsection
Rolle Type # Passes Rolle Type # Passes Rolle Type # Passes
A 9t SR 1 5 22t PR 2 10 9t SR 5
B 9t SR 5 22t PR 15 9t SR 5
C 22t PR 2 9t SR 5 22t PR 13
D 9t SR 3 22t PR 15
E 12t SR 3 22
1 Nine-ton steel-wheeled roller; 2 22-ton pneumatic-tired roller; 3 12-ton steel-wheeled roller.
Three types of structure were considered to simulate different maintenance activities provided by
the Republic of San Marino road agency:
• Subsections A (17 m long and 5 m wide) and C (25 m long and 4 m wide) represent a typical
intermediate maintenance work and consist in 12 cm of CRAM binder course and 4 cm of asphalt
concrete wearing course with maximum aggregate size of 11 mm (AC11);
• Subsection B (25 m long and 4 m wide) represents a typical deep maintenance work and consists
of 20 cm of CRAM base course, 10 cm of CRAM binder course and 4 cm of AC11 wearing course;
• Subsection D (15 m long and 4 m wide) and E (19 m long and 4 m wide) represent a typical
maintenance work for rural roads and consists of 12 cm of CRAM binder course and a
double-layered surface dressing.
In all subsections, a bituminous emulsion prime coat (1.00 kg/m2 of residual bitumen) was applied
above the subgrade and a bituminous emulsion tack coat (0.60 kg/m2 of residual bitumen), or a surface
treatment, was applied above the CRAM layer, immediately after construction.
Several compaction procedures, in terms of roller weight (9, 12 or 22 tons), roller type (steel or
pneumatic) and number of passes (back-forth movement), were considered for the CRAM binder
Table 7. Compaction procedure of the cold recycled asphalt mixture (CRAM) binder course.
Materials 2020, 13, 4697 First Phase Second Phase Third Phase 7 of 19
Subsection
Rolle Type # Passes Rolle Type # Passes Rolle Type # Passes
A 9t SR 1 5 22t PR 2 10 9t SR 5
B 9t SR 5 22t PR 15 9t SR 5
course to take into account
C different
22t PR construction
2 practices
9t SR (Table
5 722tand
PR Figure 13 6). The roller covered
the width of the layer inDno more9t than
SR four3 overlapping
22t PR passes
15 assuming that the overlap is not less
E 12t SR 3 22
than 20 cm. 1 Nine-ton steel-wheeled roller; 2 22-ton pneumatic-tired roller; 3 12-ton steel-wheeled roller.
Figure 6. Compaction of CRAM binder course of Subsection C by using the 22-ton pneumatic-tired
Figure 6. Compaction
roller.
of CRAM binder course of Subsection C by using the 22-ton pneumatic-tired roller.
All the Subsections were

2.3. Experimental opened to traffic 4 days after construction. Traffic data were collected
Program
for Subsection B, CInand D. After

this study, two
only the CRAMyears fromas construction,
applied Subsection
binder course (Figure B was
5) was tested. Duringsubjected
the to heavy
construction of the trial section, the loose mixture was immediately compacted with a gyratory
traffic corresponding to about 270,000 cycles of 80 kN equivalent standard axle load
compactor to produce four specimens with a diameter of 150 mm and a height, after 100 gyrations,
(ESAL) whereas
Subsections C and D were
of about 70 mm.subjected to section
After the trial aboutconstruction,
70,000 ESAL. Nowere
30 cores distresses
taken fromare
the visible onatthe Subsections.
subsections
several time intervals. As shown in Table 8, the cores were divided into groups, based on the coring
date. We highlight that Group 2 included cores taken from all subsections, while Subsection C was
2.3. Experimental Program
cored four times, from 23 to 796 days after construction.
The gyratory specimens (Group 0) and the core specimens of Groups 1.1 and 2 were oven-cured
In this study, only the CRAM applied as binder course (Figure 5) was tested. During the construction
in the laboratory at 40 °C and tested at different curing periods (Figure 7) for monitoring the evolution
of the trial section, the
of the loose
ITSM. mixture
At the end of thewas immediately
selected curing period,compacted with aongyratory
the ITS was measured compactor
all specimens. After to produce
four specimens testing,
with athediameter
volumetric characterisation of Group 0 and Group 2 specimens was performed 157 days
of 150 mm and a height, after 100 gyrations, of about 70 mm. After the
after construction, when most of (or all) the hydration had occurred, according to EN 12697-6 [52]
trial section construction, 30 cores
(Procedure C, i.e., were taken
sealed specimen method) from
and ENthe subsections
12697-8 [56]. at several time intervals. As shown
in Table 8, the cores Thewere
three cores of Group
divided 1.2 were
into cured atbased
groups, room temperature and subjected
on the coring date.to complex modulus that Group 2
We highlight
testing. The cores of Groups 3 and 4 were tested (ITSM and ITS) immediately after coring (Figure 7).
included cores taken Wefrom allthat
highlight subsections,
the humidity ofwhile Subsection
the CRAM Coven-curing
subjected to was cored andfour times, from
free evaporation (in 23 to 796 days
after construction.
laboratory) was totally different from the field, where evaporation is restricted as the mixture was
sealed between two bituminous layers (prime coat and tack coat/surface dressing).
Table 8. Coring plan.
Number of Specimens
Core
Coring Date Days from
Group Diameter Subsections
(mm/dd/yy) Construction
(mm) A B C D E
1.1 16 April 2018 23 150 - - 3 - -
1.2 16 April 2018 23 200 - 1 2 - -
2 5 June 2018 73 134 3 3 3 3 3
3 28 August 2018 157 134 - 3 3 - -
4 28 May 2018 796 134 - - 3 - -
The gyratory specimens (Group 0) and the core specimens of Groups 1.1 and 2 were oven-cured
in the laboratory at 40 ◦ C and tested at different curing periods (Figure 7) for monitoring the evolution
of the ITSM. At the end of the selected curing period, the ITS was measured on all specimens.
After testing, the volumetric characterisation of Group 0 and Group 2 specimens was performed
157 days after construction, when most of (or all) the hydration had occurred, according to EN
12697-6 [52] (Procedure C, i.e., sealed specimen method) and EN 12697-8 [56].
The three cores of Group 1.2 were cured at room temperature and subjected to complex modulus
testing. The cores of Groups 3 and 4 were tested (ITSM and ITS) immediately after coring (Figure 7).
Table 8. Coring plan.
Core Number of Specimens

Materials 2020, 13, 4697 Coring Date Days from 8 of 19
Group Diameter Subsections
(mm/dd/yy) Construction
(mm) A B C D E
1.1 16 April 2018 23 150 - - 3 - -
We highlight
1.2 that16the humidity
April 2018 of the CRAM
23 subjected
200 to oven-curing
- 1 2 and- free
- evaporation
2 5 June 2018 73 134 3 3 3 3 3
(in laboratory) was totally different from the field, where evaporation is restricted as the mixture was
3 28 August 2018 157 134 - 3 3 - -
sealed between4 two bituminous
28 May 2018layers (prime coat and tack 134
796 coat/surface
- dressing).
- 3 - -
ITSM ITSM + ITS Complex modulus

CORING
GROUP 4 CORING
GROUP 3 CORING
Oven-curing at 40 °C
GROUP 2 CORING
Curing at room temperature

GROUP 1.2
GROUP 1.1
GROUP 0
3 11 23 31 55 73 8393 157 194 796

Days from construction
Figure 7. 7.Experimental
Figure program.
Experimental program.
2.4. Testing Procedures

2.4. Testing Procedures
The ITSM test was carried out at 20 °C, according to EN 12697-26 (Annex C) [57]. The ITSM was
◦ C, according to EN 12697-26 (Annex C) [57]. The ITSM
The ITSM test was
measured carried
as average valueout
afterat
the20application of five load pulses with a rise time of 124 ms. Two
was measured as average
orthogonal diameters value after for
were tested the application
each of fiveand
cylindrical specimen load pulsesITSM
the average with
wasacalculated.
rise time of 124 ms.
The ITS test was carried out at 20 °C, according to EN 12697-23 [53]. The test allows the
Two orthogonal diameters were tested for each cylindrical specimen and the average ITSM was calculated.
calculation of the tensile strength ◦of a cylindrical specimen, loaded diametrically until its failure.
The ITS testThe was carried
complex out atwas
modulus 20 measured
C, according to EN
on cylindric 12697-23
specimens with[53]. The test
a diameter of 75allows
mm andthe a calculation
of the tensileheight
strength
of 140 of
mm, a obtained
cylindrical
with an specimen, loaded coring
additional horizontal diametrically
from cores ofuntil its1.2failure.
Group (Figure 8a).
The test was carried out with the asphalt mixtures performance tester (AMPT Pro). During the test,
The complex modulus was measured on cylindric specimens with a diameter of 75 mm and a
a strain amplitude of 30 microstrain was kept constant by applying a haversine compression load.
height of 140Three
mm,linear
obtained
variablewith an additional
differential transformershorizontal
(LVDT) placed coring from
120° apart cores
(Figure 8b)of Group
were used for 1.2 (Figure 8a).
The test wasmeasuring
carried the outaxialwith theonasphalt
strain the middlemixtures
part of theperformance
specimen, while tester (AMPT
a load cell Pro). During
was employed for the test,
axial stress measurement. Five temperatures (0, 10, 20, 35, 50 °C), five frequencies (0.1, 0.5, 1, 5, 10
a strain amplitude of 30 microstrain was kept constant by applying a haversine compression load.
Hz) and 20 loading cycles for each frequency were applied, allowing the determination of the stiffness
Three linearmodulus
variable differential
E0 and phase angle transformers
φ. (LVDT) placed 120◦ apart (Figure 8b) were used for
measuring the axial strain on the middle part of the specimen, while a load cell was employed for
axial stress measurement. Five temperatures (0, 10, 20, 35, 50 ◦ C), five frequencies (0.1, 0.5, 1, 5, 10 Hz)
and 20 loading cycles for each frequency were applied, allowing the determination of the stiffness
modulus E0 andMaterials
phase 13, x FORϕ.
angle
2020, PEER REVIEW 9 of 20
(a) (b)
Figure 8. (a) Horizontal coring from core of 200-mm diameter; (b) detail of the specimen mounted in
Figure 8. (a) Horizontal coring from core of 200-mm diameter; (b) detail of the specimen mounted in
the asphalt mixtures performance tester (AMPT Pro).
the asphalt mixtures performance tester (AMPT Pro).
3. Results and Discussion
3. Results and Discussion
3.1. Volumetric Characterisation
The bitumen content, recovered from the loose CRAM binder material after in-plant production,
3.1. Volumetric Characterisation
was equal to 5.9% with respect to the mixture mass. The air voids content of the CRAM specimens
The bitumenincluded in Group
content, 0 and Group
recovered from2 is the
shown in Table
loose 9 (average
CRAM value of
binder 2 or 3 replicates).
material The air
after in-plant production,
voids of Subsections A, B and C are similar (around 15.5%) and do not allow different site compaction
was equal to 5.9% with respect to the mixture mass. The air voids content of the CRAM
practices to be distinguished. Subsection D, where the least number of passes was carried out (Table specimens
included in Group 0 andtheGroup
7), provided 2 is
highest air shown
voids content in Table
(17.0%). 9 (average
On the value E,ofwhere
contrary, Subsection 2 oronly
3 replicates).
the 22- The air
ton steel roller was used, provided the lowest air voids content (14.1%).
Apparently, there is a correlation between the air voids of the cores and the number of roller
passes. However, we underline that other factors may have influenced the volumetric properties of
the specimens, such as the subgrade bearing capacity (existing base course or new CRAM base
course) and the post-compaction due to heavy vehicle circulation on the various subsections.
Gyratory specimens provided significantly lower air voids content (11.8%) than core specimens.
This suggests that the adopted compaction energy (100 gyrations), which was required by the
Materials 2020, 13, 4697 9 of 19
voids of Subsections A, B and C are similar (around 15.5%) and do not allow different site compaction
practices to be distinguished. Subsection D, where the least number of passes was carried out (Table 7),
provided the highest air voids content (17.0%). On the contrary, Subsection E, where only the 22-ton
steel roller was used, provided the lowest air voids content (14.1%).
Table 9. Air voids content of CRAM binder specimens of Group 0 and Group 2.
Air Voids Content

Specimens Max-Min
Average Value (%)
(%)
Gyratory 11.8 0.853
Subsection A 15.9 0.789
Subsection B 15.4 1.278
Subsection C 15.5 0.642
Subsection D 17.0 0.561
Subsection E 14.1 1.008
Apparently, there is a correlation between the air voids of the cores and the number of roller
passes. However, we underline that other factors may have influenced the volumetric properties of the
specimens, such as the subgrade bearing capacity (existing base course or new CRAM base course)
and the post-compaction due to heavy vehicle circulation on the various subsections.
Gyratory specimens provided significantly lower air voids content (11.8%) than core specimens.
This suggests that the adopted compaction energy (100 gyrations), which was required by the
construction specification
Materials 2020, 13, x[51], overestimates
FOR PEER REVIEW the actual field compaction effort provided
10 of 20 by the rollers.
The ITSM can be considered linearly dependent on the air voids in all the curing conditions.
3.2. Mechanical Results
Characterisation
from tests until 93 days after construction (73 days field + 20 days lab), indicate that the curing
did not affect the linear correlation between ITSM and air voids. Specifically, a 1% increase in air
3.2.1. ITSM Testvoids
Results
led to a reduction of ITSM of about 900 MPa. Results from tests after a 157-day curing time (73
days field + 84 days lab) kept an almost linear trend but with a higher sensibility to the air voids. This
Figure 9 shows thedue
is probably relationship between
to the replication ITSM
of the ITSM at the
tests on ◦ C and
20 same cores,air voids
which content
may have reducedofthe
cores of Group 2,
stiffness of the cores characterised by a higher air voids (Subsection D with 17% of air voids content).
at different curing conditions. Each point is the average value of three specimens (Table 8).
12000
10000
8000
ITSM @ 20 C [MPa]
6000
4000
73 days field ITSM = -934·Vv + 20154; R² = 0.92
2000 73 days field+10 days lab ITSM = -931·Vv + 21816; R² = 0.90

73 days field+20 days lab ITSM = -833·Vv + 21295; R² = 0.71
73 days field+84 days lab ITSM = -1548·Vv + 32874; R² = 0.91
0
13 14 15 16 17 18
Air voids content Vv [%]
Figure 9. Relationship betweenbetween

Figure 9. Relationship indirect tensile
indirect stiffness
tensile stiffness modulus
modulus (ITSM)
(ITSM) and and
air voids air voids
content of content of
specimens
specimens of Group 2 atof Group 2 at different
different curing curing times.
times.
Figure 10 shows the evolution of the average ITSM values over the curing time for gyratory
The ITSMspecimens
can be (Group
considered linearly
0) and core specimensdependent
of Group 2. Theon the air data
experimental voids
werein allthrough
fitted the curing
the conditions.
Results from tests until model
asymptotic 93 days afterbyconstruction
proposed (73 days field + 20 days lab), indicate that the curing
Graziani et al. [23,58]:
did not affect the linear correlation between ITSM and 𝑡 − 𝑡air
𝑖 voids. Specifically, a 1% increase in air voids
𝑦(𝑡) = 𝑦𝑖 + (𝑦𝑎 − 𝑦𝑖 ) (1)
led to a reduction of ITSM of about 900 MPa. Results (ℎ 𝑦 − 𝑡𝑖 ) +from𝑡𝑖tests
(𝑡 − ) after a 157-day curing time (73 days
where t (days) is the curing time, y(t) is the property under investigation (ITSM), ti is the curing time
when the property was measured for the first time (i.e., 3 or 73 days), yi is an intercept term that
represents the value of the properties at the time ti, ya is the long-term asymptotic value of y(t) and hy
(days) is a parameter representing a specific curing time. The parameter yi gives information on the
average rate of evolution of the material properties from the day of construction to ti.
The agreement between the measured data and the estimated regression curves is quite good,
as shown in Figure 10 and Table 10, where the estimated values of the regression parameters are
Materials 2020, 13, 4697 10 of 19
field + 84 days lab) kept an almost linear trend but with a higher sensibility to the air voids. This is
probably due to the replication of the ITSM tests on the same cores, which may have reduced the
stiffness of the cores characterised by a higher air voids (Subsection D with 17% of air voids content).
Figure 10 shows the evolution of the average ITSM values over the curing time for gyratory
specimens (Group 0) and core specimens of Group 2. The experimental data were fitted through the
asymptotic model proposed by Graziani et al. [23,58]:
t − ti
y(t) = yi + ( ya − yi ) (1)
(h y − ti ) + (t − ti )
where t (days) is the curing time, y(t) is the property under investigation (ITSM), ti is the curing time
when the property was measured for the first time (i.e., 3 or 73 days), yi is an intercept term that
represents the value of the properties at the time ti , ya is the long-term asymptotic value of y(t) and hy
(days) is a parameter representing a specific curing time. The parameter yi gives information on the
Materials 2020,
average rate13,
of xevolution
FOR PEER REVIEW
of the material properties from the day of construction to ti . 12 of 20
12000
12000
1200012000 12000 14.1%
1200012000
12000 14.1%14.1%
14.1%14.1%
15.4%
10000 14.1%14.1%14.1%
15.4% 15.4%
15.4% 15.4%
10000
1000010000 10000 11.8% 15.4%15.4%15.4%
1000010000
10000 11.8%
11.8%11.8% 11.8%
15.5% 11.8%11.8%11.8%
8000 15.5%
15.5%15.5% 15.5%
8000
8000 8000 8000
15.5%15.5%15.5%
ITSM @ 20 C [MPa]
15.9%
ITSM @ 20 C [MPa]
ITSM @ 20 C [MPa]
15.9%
C [MPa]
800080008000 15.9%
C [MPa]
15.9%15.9%
@ 20C [MPa]
15.9%15.9%15.9%
C [MPa]
ITSM @ 20 C [MPa]
17.0% 17.0%
17.0%17.0% 17.0%
6000 6000
6000 6000 6000 17.0%17.0%17.0%
600060006000
@ 20
@ 20
@ 20
Curing time [days]

ITSM
ITSM
4000
4000 4000 4000
ITSM
ITSM
4000 180 160

400040004000
140 120 100 80 60 40 20 0
gyratory
gyratory
gyratory
gyratory specimens
specimens
specimens ofcores
specimens corescores of of
cores Subsection
Subsection A A A Acorescores
of Subsection
Subsection ofcores of
cores
of Subsection
B BB B
of Subsection
Subsection
Subsection 0
gyratory specimens
gyratory ofspecimens
gyratory ofspecimens corescores
Mod. E of Subsection
of
cores of A A A corescores
Subsection
Subsection
Mod. D of Subsection
of
cores B B B
Subsection
of Subsection
Mod. C
ofcores
corescores cores
of Subsection
C C C Ccorescores
Subsection
Subsection
Subsection ofcoresof of
cores Subsection
of D D D Dcorescores
Subsection
Subsection
cores
of Subsection
of E EE E
Subsection
Subsection
Subsection
2000
2000 2000 2000
corescores
ofMod.
Subsection
of C C C corescores ofMod.
Subsection D D D corescores of Subsection E E E
ofSubsection
cores ofGC
Subsection of
coresSubsection
ofA
ofSubsection of
coresBSubsection
ofBSubsection
Mod. B Mod. A Mod. GC
2000 gyratory specimens
200020002000 Mod.Mod. cores
GC Mod.
GC GCSubsection A Mod.Mod. A coresMod.
A A Subsection B Mod.
Mod. BMod. Mod.
B 2000
Mod.Mod.
GC GC
Mod. GC
cores of Subsection E
Mod.C C Mod. Mod.
A A
Mod.
Mod.
D DA
cores of Subsection D Mod. Mod.
B B
Mod. B
cores of Subsection C
Mod.
E E
CMod.
Mod.Mod. C Mod.Mod.DMod. D EMod.
Mod.Mod. E
cores of Subsection
0 0 C0 0 Mod.Mod.cores Cof C
C Mod. Subsection D Mod.Mod.
cores of Subsection B cores
D Mod. D Dof SubsectionMod.
cores of Subsection A E Mod.
E Mod.E E
gyratory specimens
0 0 0 0 0 0 20
ITSM @ 20 C [MPa]
0 20 20 20 40 40 40 40 60 60 60 60 80 80 80 100 80 100100 100120 120120 120
140 140 140 140
160 160 160 160 180 180
180 180
0 4000
0 0 0 20 20 2040 40 4060 60 60Curing
Curing 80
80Curing
timeCuring80
time 100
time
[days] 100[days]
time
[days]
[days] 120 120 120
100 140 140 140 160 160 160 180 180 180
0 20 40 60 80 100 Curing 120
Curing time
Curing
time 140
[days]
time
[days] [days] 160 180
Curing time [days] 6000
17.0%
Figure 10. Measured

Figure 10. Measureddata
dataand model
and of the
model evolution
of the of ITSM
evolution over over
of ITSM curing time for
curing specimens
time of Group
for specimens of
15.9%
8000
0Group
(gyratory) and Group 2 (cores).
0 (gyratory) and Group 2 (cores).
15.5%
11.8%
10000
The agreement between the12000measured data and the estimated regression curves is quite good,
12000
12000
15.4%
14.1%
12000 10 and Table 10, where the estimated values of the regression parameters are
as shown in Figure 12000
reported along with the coefficient of determination R2 and the air voids.
10000
10000
10000
10000
Table 10. Estimated values of the regression parameters and air voids content of specimens of Group 0,
8000
8000
8000
Group 1.1, Group 2 and field curing.
8000
[MPa]
[MPa]
C [MPa]
ITSM @ 20 C [MPa]
t6000
i yi ya hy R2 Air Voids Content
Specimen Type 6000
6000
C
20 C
6000 (Days) (MPa) (MPa) (Days) (-) (%)

@
ITSM @ 20
@ 20
gyratory specimens 3 4668 9246 21 0.97 11.8

ITSM
ITSM
4000
4000
4000
cores of Sub. A-Group 2 73 5603 8730 81 0.85 15.9
4000
cores of Sub. B-Group 2 73 5807 10,412 84 0.75 15.4
cores of Sub. C-Group 2 73
2000
2000
2000 5625
Sub.C
Sub.C 87751.1
Sub.C- --Group
Group
Group 1.1
1.1 80Sub.
Sub. 0.85222
Sub.CCC- --Group
Group
Group 15.5
Sub.C
Sub.C
Sub.C- --field
field curing
fieldcuring
curing
cores of Sub.2000
D-Group 2 73 3815 6729 78 0.70 17.0
cores of Sub. E-Group 2 Sub.C -73
Group 1.1 Mod.
Mod.
6643 Group
Group
Mod.Sub.
Group 1.1
C -1.1
Group
1.1
11,375 2 92Mod.Mod.
Mod. Group
Group
Sub.C
Group 222 cured
- field
0.89 Mod.
Mod.
Mod. In-situ
In-situ
14.1 curing
In-situcuring
curing
cores of Sub. C-Group 1.1 23000 4139 8415 35 0.94 -
0
cores of Sub. C-field curing 23 000 100
100
100
3850 200
200
200
8001 300
300
30069 400 400
400 0.94500 500
500 600
600
600 - 700700
700 800
800
800 900
900
900
0 100 200 300 400 500 600 700 800 900
Curing
Curing time
Curingtime [days]
time[days]
[days]
Curing time [days]
Figure 11. Measured data and model of the evolution of ITSM over curing time for core specimens of
Subsection C: Group 1.1, Group 2 and field curing.
Table 10. Estimated values of the regression parameters and air voids content of specimens of Group
0, Group 1.1, Group 2 and field curing.
Materials 2020, 13, 4697 11 of 19
The gyratory specimens of Group 0 and the cores of Group 2 showed a different evolution of ITSM.
The gyratory specimens, oven-cured in laboratory at 40 ◦ C starting immediately after production,
showed a rapid increase in stiffness in the first days, with the ITSM reaching about 4500 MPa after 3
days and 7200 MPa after 21 days. At longer curing times, the stiffness increase slowed down, with the
ITSM reaching about 8200 MPa after 73 days and a long-term asymptotic value of 9246 MPa (Table 10).
For the cores, we have the first ITSM measurement after 73 days of field curing, with values
ranging from about 4000 (Subsection D) to 6500 MPa (Subsection E). At this curing time, the difference
in ITSM between cores and gyratory specimens, is due to differences in both volumetric properties
(the cores had higher voids) and curing conditions (oven-curing vs. field curing). The effect of air
Materials 2020, 13, x FOR PEER REVIEW
voids can be estimated using the experimental data reported in Figure 9. Specifically, with an air12 of 20
voids
content of 11.8% we can extrapolate an ITSM of about 9100 MPa after 73 days of field curing. Such
12000
value is even higher than the ITSM measured on the gyratory specimens. We can conclude that, in
12000
1200012000 12000 14.1%
these in-situ conditions (pavement 12000 stratigraphy,
1200012000
location and climate), field curing did not14.1% penalise
14.1% 14.1% 14.1%
15.4%
the stiffness evolution until 73 days.10000
10000 This tendency is confirmed in the long-term. In fact, 14.1% Figure
14.1%
15.4% 10
14.1%
15.4%
15.4%15.4%
1000010000 10000 11.8%
shows that the core specimens, which 10000
10000 were oven-cured at 40 ◦ C after extraction, had a rapid
10000 increase
15.4%15.4%15.4%
11.8%
11.8%11.8% 11.8%
15.5% 11.8%11.8%11.8%
in stiffness and reached an asymptotic
8000 value
8000
8000 8000 8000 of ITSM ranging from 6729 (Subsection D) to 11,37515.5% 15.5% 15.5%
15.5% MPa
15.5%15.5%15.5%
ITSM @ 20 C [MPa]
15.9%
ITSM @ 20 C [MPa]
ITSM @ 20 C [MPa]
15.9%
C [MPa]
800080008000 15.9%
C [MPa]
15.9%15.9%
(Subsection E). We observe that the asymptotic value of the gyratory specimens is comprised in this
@ 20C [MPa]
15.9%15.9%15.9%
C [MPa]
ITSM @ 20 C [MPa]
17.0% 17.0%
17.0%17.0% 17.0%
range, although6000 they had lower air voids.
6000
6000 6000 6000 17.0%17.0%17.0%
600060006000
@ 20
The field curing curve shown in Figure 11 depicts the ITSM evolution observed on core specimens
@ 20
@ 20
Curing time [days]

ITSM
ITSM
taken from Subsection C, from 23 4000to 796

4000 days after construction, when also field ageing, moisture
4000
4000
ITSM
ITSM
4000 400040004000
180 160 140 120 100 80 60 40 20 0
gyratory
gyratory
gyratory specimens
specimens corescores
specimens ofcores of
cores
of Subsection
A A A Acorescores
of Subsection
cores
of Subsection
B BB B
of Subsection
Subsection
damage and traffic induced stress influencedgyratory specimens Subsection Subsection 0
the
gyratory material
specimens
gyratory ofspecimens
gyratory performance.
ofspecimens corescores
of Subsection
of
cores These A Ameasurements
Subsection
of
Mod. E Subsection A corescores
of Subsection
of
cores reveal
B B B the
Subsection
Mod. Dof Subsection Mod. C
ofcores
corescores cores
of Subsection
C C C Ccorescores
Subsection
Subsection
Subsection ofcoresof of
cores Subsection
of D D D Dcorescores
Subsection
Subsection
cores
of Subsection
of E EE E
Subsection
Subsection
Subsection
2000
2000 2000 2000
actual stiffness evolution
2000
of the
gyratory material
specimens in the
coresfield.
200020002000 Mod. GC
ofMod.
cores
cores
Mod.
of
cores
GCof
Mod.
GC This
Subsection C trend
Subsection
ofGC
SubsectionC C cores
Subsection
A is
Mod. A compared
ofMod.
cores
Mod.
Subsection
of
cores
cores
Mod.
A A ofA
Mod. B
of D with
Subsection D D the
Subsection
Subsection B stiffness
corescores
of Subsection
of
cores
Mod.
Mod.
Mod. B
Mod. A
Mod.
B B evolution
E E E
Subsection
ofBSubsection Mod. GC
2000
Mod.Mod. GC
GCMod. Mod.Mod. A Mod.Mod. B
observed on cores taken 23 days (Group 1.1)Mod. and CMod.
Mod. 73
Mod.
C
GC
CdaysC (Group Mod.Mod.2DAMod.
cores of Subsection E Mod.
Sub. D AD
Mod.
D C) after construction B Mod. E B E and then
cores of Subsection D
EMod.
Mod.Mod. Mod.
E
cores of Subsection C
cores of Subsection
0 0 C0 0 Mod.Mod.cores Cof C
C Mod. Subsection D Mod.Mod. cores
D Mod.
cores of Subsection B D Dof SubsectionMod. E Mod.
E Mod.E E
cores of Subsection A gyratory specimens
oven-cured at 40 ◦ C. The measurements 0 0 0 0 0 0were fitted
40 40 using 60 60 the 80 model 80 described in 140
Equation (1)180and
ITSM @ 20 C [MPa]
0 20 20
20 20 40 40 60 60 80 80 100 100100 100
120 120120 120
140 140 140
160 160 160 160
180 180 180
0 4000
0 0 0 20 20 2040 40 4060 60 60Curing 80
80Curing 80
Curing 100
time 100[days]
time
[days] 120 120 120
100 140 140 140 160 160 160 180 180 180
the estimated values0 of the 20 regression 40 parameters 60 80are reported
Curing
100 Curing in
time
120
Curing
Table
Curing
time
time
[days]
time
[days]10.
140
[days]
time
[days] [days]
The core
160 specimens
180 taken
after 23 and 73 days and oven-cured at 40 ◦ C show Curing time a rapid
[days] increase in stiffness and, in the long term,
17.0%
6000
they are characterised by similar asymptotic values of ITSM: 8415 MPa and 8775 MPa, respectively.
Figure 10. Measured data and model of the evolution of ITSM over curing time for specimens of
15.9%
These values are only slightly higher than the asymptotic value which characterises the field cured
15.5%
8000
Group 0 (gyratory) and Group 2 (cores).

material, 8001 MPa. 11.8%
15.4%
10000
12000
12000
12000
14.1%
12000
12000
10000
10000
10000
10000
8000
8000
8000
8000
[MPa]
[MPa]
C [MPa]
ITSM @ 20 C [MPa]
6000
6000
6000
C
20 C
6000
@
ITSM @
ITSM 20
@ 20
ITSM
4000
4000
4000
4000
2000
2000
2000 Sub.C
Sub.C- --Group
Sub.C Group 1.1
Group1.1
1.1 Sub.
Sub.CCC- --Group
Sub. Group
Group222 Sub.C
Sub.C- --field
Sub.C field curing
fieldcuring
curing
2000
Sub.C - Group 1.1 Mod.
Mod. Group
Group
Mod.Sub.
Group 1.1
C -1.1
Group
1.1 2 Mod.
Mod. Group
Group
Sub.C
Mod. 222 cured
- field
Group Mod.
Mod. In-situ
Mod.In-situ curing
In-situcuring
curing
000
0 000 100
100
100 200
200
200 300
300
300 400
400
400 500
500
500 600
600
600 700
700
700 800
800
800 900
900
900
0 100 200 300 400 500 600 700 800 900
Curing
Curing time
Curingtime [days]
time[days]
[days]
Curing time [days]
Table 10. Estimated values of the regression parameters and air voids content of specimens of Group
0, Group 1.1, Group 2 and field curing.
ti yi ya hy R2 Air Voids Content

Specimen Type
(Days) (MPa) (MPa) (Days) (-) (%)
gyratory specimens 3 4668 9246 21 0.97 11.8
Materials 2020, 13, 4697 12 of 19
In summary, oven-curing with free evaporation and high temperature (40 ◦ C), a procedure
that is often used for accelerated curing in the laboratory, may lead to an underestimation of the
long-term stiffness of the mixture cured in the field with restricted evaporation (Figure 10). On the other
hand, if oven-curing is applied after a few days or weeks of field curing with restricted evaporation,
the long-term stiffness will not be affected (Figure 11). This is because the humidity of the material
subjected to oven-curing and free evaporation may be totally different from the field. Therefore,
the evolution of the cementitious and bituminous bonds will be different because humidity enhances
the former and penalises the latter.
These results suggest that the curing conditions immediately after compaction determine the
microstructure of the material (distribution and location of cementitious and bituminous bonds).
With immediate oven-curing and free evaporation (laboratory conditions), bituminous bonds are
favoured with respect to cementitious bonds, whereas if evaporation in restricted (field curing),
the cementitious bonds are favoured leading to a higher long-term stiffness. When oven-curing
is applied a few days/weeks after compaction (i.e., when the mixture microstructure is already
formed in sealed conditions), the stiffness development will be accelerated with a small effect on its
Materials 2020,
long-term 13, x FOR PEER REVIEW
value. 13 of 20
3.2.2.ITS
3.2.2. ITSResults
Results
Figure 12
Figure 12 shows the the results
resultsofofthetheITSITStests performed
tests performed on the corecore
on the specimens
specimensof Group 2, cured
of Group 2,
73 days in the field and then 84 days in laboratory at 40 °C, and ◦
on the gyratory
cured 73 days in the field and then 84 days in laboratory at 40 C, and on the gyratory specimens specimens cured 157
days in
cured 157laboratory at 40 °C. at
days in laboratory 40 ◦ C. relationship
A linear is found is
A linear relationship between the ITS of
found between thethe
ITScores and
of the their
cores air
and
voidsair
their content. Specifically,
voids content. a 3% increase
Specifically, in air voids
a 3% increase ledvoids
in air to approximately a halving aofhalving
led to approximately ITS (from 0.69
of ITS
to 0.38
(from 0.69MPa).
to 0.38This
MPa).trend
Thisshows that ifthat
trend shows hypothetical
if hypotheticalcorescores
with an an
with airairvoid
voidcontent
content of 11.8%
11.8%
(correspondingtoto
(corresponding thethe value
value obtained
obtained for gyratory
for the the gyratory specimens)
specimens) were considered,
were considered, the ITSthe ITSwould
value value
would be considerably higher than that provided by the gyratory specimens.
be considerably higher than that provided by the gyratory specimens. This confirms what was alreadyThis confirms what was
already observed
observed during ITSMduring ITSM
tests: the tests: the combination
combination of field andof field and laboratory
laboratory curing would curing would
lead lead to a
to a different
differentcompared
structure structure compared
to the soleto the sole
curing curing
in the at 40 ◦ C. at 40 °C.
in the laboratory
laboratory
0.9
0.8
0.7
ITS @ 20 C [MPa]
0.6
0.5
0.4
0.3
0.2 gyratory specimens

0.1 cores of Group 2 (all Subsections) ITS = -0.11·Vv + 2.26; R² = 0.98
0.0
11 12 13 14 15 16 17 18
Air voids content Vv [%]
Figure12.
Figure 12. Indirect tensile
tensile strength
strength(ITS)
(ITS)(with
(withmax
maxand
andmin
minerror bars)
error as as
bars) a function of air
a function voids,
of air 157
voids,
days
157 after
days construction.
after construction.
3.2.3.
3.2.3.Complex
ComplexModulus
Modulus
Figure
Figure13
13shows
showsthethecomplex
complexmodulus
modulusresults
resultsobtained
obtainedononcores
coresextracted
extractedfrom
fromSubsections
SubsectionsBB
(B10,
(B10, with air voids content of 14.3%) and C (C12 and C13, with air voids contents of 18.4%and
with air voids content of 14.3%) and C (C12 and C13, with air voids contents of 18.4% and 18.9%,
18.9%,
respectively). The results are plotted in the Black diagram (stiffness modulus 𝐸0 as a function of the
phase angle 𝜙–Figure 13a) and in the Cole–Cole diagram (loss modulus 𝐸2 as a function of storage
modulus 𝐸1 –Figure 13b).
Overall, the stiffness modulus was comprised between 9500 (B10, T = 0 °C, f = 10 Hz), and 1500
MPa (C12, T = 50 °C, f = 0.1 Hz). This range of variation is less than one order of magnitude, whereas,
Materials 2020, 13, 4697 13 of 19
respectively). The results are plotted in the Black diagram (stiffness modulus E0 as a function of the
phase angle φ–Figure 13a) and in the Cole–Cole diagram (loss modulus E2 as a function of storage
modulus
Materials E1 –Figure
2020, 13, x FOR 13b).
PEER REVIEW 14 of 20
1.E+05 1000
B10 C12 C13 B10 C12 C13
Stiffness modulus E0 (MPa)
Loss modulus E2 (MPa)

1.E+04
500
1.E+03
1.E+02 0
0.0 5.0 10.0 15.0 0 5000 10000
Phase angle f (degree) Storage modulus E1 (MPa)
(a) (b)
Figure 13. Measured values of E00 for
for CRAM:
CRAM: (a)
(a) Black
Black diagram;
diagram; (b)
(b) Cole–Cole
Cole–Cole diagram
diagram
Overall, the stiffness

Rheological modelling modulus was comprised
was carried out usingbetween
the model (B10, T = by
9500proposed 0 ◦ C, f = 10 Hz),
Graziani and
et al. 1500 MPa
[10,11] that
(C12, T = viscoelastic
combines 50 C, f = 0.1
◦
and Hz). This range
hysteretic of variation
dissipation is less than
mechanisms. The one order ofpart
viscoelastic magnitude, whereas,
is represented by
in the
the same temperature
Huet–Sayegh and frequency
(HS) model [62] while range,
the conventional
hysteretic part AC(HY)
mixtures normally show
is represented by aa time-
variability
and
of more than two orders ofphase
temperature-independent magnitude
angle (𝜙 [59]. Concurrently, the values of the phase angle were less
𝐻𝑌 ). The model, abbreviated HS-HY, is described by the
◦
than aboutequation:
10 . These reduced ranges of variability characterise the typical behaviour of cold recycled
following
mixtures where cement plays an important role in limiting the thermo-viscoelastic behaviour [60].
For each ∗ specimen,
𝐸𝑔 − 𝐸𝑒increase (or decrease) had the same effect on E∗ as the
𝐸𝐻𝑆−𝐻𝑌 (𝜔) = a[𝐸loading
𝑒 +
frequency
−𝑘 + (j𝜔𝜏)−ℎ
] ∙ exp(j𝜙𝐻𝑌 ) (2)
1 + 𝛿(j𝜔𝜏)
temperature decrease (or increase). This confirms the validity of the time-temperature superposition
principle (TTSP). In other terms, despite the concurrent presence of the residual bitumen from the
where the term in square brackets describes the HS model, and the term exp(j𝜙𝐻𝑌 ) represents a
emulsion and the aged bitumen of the RA aggregates, the tested CRAMs showed a thermo-rheologically
rotation in the complex plane (Figure 14). Physically, the phase angle 𝜙𝐻𝑌 accounts for the time-
simple behaviour. The master curves of the stiffness modulus and phase angle were obtained by fixing
independent (non-viscous) and temperature-independent dissipation phenomena which are present
the reference temperature T0 = 20 ◦ C and shifting the experimental data along the frequency axis until
during cyclic loading. The term hysteretic is normally used to indicate this type of dissipation
obtaining continuous curves. For each testing temperature T the amount of shifting, i.e., the shift factors
mechanism that may be attributed to the cementitious bonds or to internal friction phenomena
a0 (T ), was obtained through the closed form shifting (CFS) algorithm, consisting in the minimisation
[63,64].
of the area between two adjacent isothermal curves of E0 [61]. The same shift factors were used also
In Equation (2), j is the imaginary unit and 𝜔 is the angular frequency (𝜔 = 2𝜋𝑓). Ee is the
for shifting the ϕ values.
equilibrium value of 𝐸 ∗ (𝜔𝜏 → 0) and represents the purely elastic material response when the
Rheological modelling was carried out using the model proposed by Graziani et al. [10,11] that
bitumen is liquid, and its contribution to stiffness vanishes (high temperature/low frequency). For
combines viscoelastic and hysteretic dissipation mechanisms. The viscoelastic part is represented
AC mixtures this value represents the interlock between aggregates [65] and for CRAMs it also
by the Huet–Sayegh (HS) model [62] while the hysteretic part (HY) is represented by a time- and
accounts for the effect of cementitious bonds. Eg is the glassy value of 𝐸 ∗ (𝜔𝜏 → ∞) and represents
temperature-independent phase angle (φHY ). The model, abbreviated HS-HY, is described by the
the purely elastic material response when the bitumen is a glassy solid (low temperature/high
following equation:
frequency). Its value is mainly affected by the volumetric properties of the mixture [66].
The dimensionless parameters k, δ and h control E g the
− Eshape of the model in the low, intermediate
 
∗ e
and high temperature range EHS−HY (ω) Higher
[67]. = Ee +values of h and

−k k indicate
· exp(jφHY ) viscous dissipation

−h  that a higher
(2)
1 + δ(jωτ) + (jωτ)
component is present in the material response (with one indicating purely viscous behaviour). On
the other
where thehand,
term in lower
squarevalues of hdescribes
brackets and k indicate
the HSthat the material
model, response
and the term exp(jφ isHY
more elastic (with
) represents zero
a rotation
indicating purely
in the complex elastic
plane behaviour).
(Figure In general,
14). Physically, the physically
phase angleconsistent
φHY accountsvaluesforare
the0 time-independent
< k < h < 1, with k
characterising the low temperature/high frequency behaviour
(non-viscous) and temperature-independent dissipation phenomena which are present and h the high temperature/low
during cyclic
frequency behaviour.
loading. The term hysteretic is normally used to indicate this type of dissipation mechanism that may
The characteristic
be attributed time 𝜏 is abonds
to the cementitious function
or toofinternal
the testing temperature:
friction phenomena [63,64].
In Equation (2), j is the imaginary unit and ω is the angular frequency (ω = 2π f ). Ee is the
equilibrium value of E∗ ( ωτ → 0 ) and𝜏 represents
= 𝜏0 ⋅ 𝑎0 (𝑇)the purely elastic material response when
(3) the
bitumen is liquid, and its contribution to stiffness vanishes (high temperature/low frequency). For AC
where 𝜏0 is the characteristic time at the reference temperature. The value of 𝜏 does not affect the
shape of the master curves. In fact, since 𝜏 is a frequency multiplier, it only affects the position of the
master curve along the frequency axes. If 𝜏 increases, the E0 master curve shifts to the left indicating
a lower relaxation ability of the material. Higher values of 𝜏 have been correlated to higher degree
of bitumen aging and higher RA content, in both hot and cold mixtures [10,68–70].
Materials 2020, 13, 4697 14 of 19
mixtures this value represents the interlock between aggregates [65] and for CRAMs it also accounts
for the effect of cementitious bonds. Eg is the glassy value of E∗ ( ωτ → ∞ ) and represents the purely
elastic material response when the bitumen is a glassy solid (low temperature/high frequency). Its value
is mainly
Materials 2020, 13,affected by the
x FOR PEER volumetric properties of the mixture [66].
REVIEW 15 of 20
𝐸
𝐸 _
𝐸∗
𝐸 _
∅
𝐸 𝐸 𝐸
Figure 14. Comparison between the Huet–Sayegh (HS) and HS-HY model.
Figure 14. Comparison between the Huet–Sayegh (HS) and HS-HY model.
The dimensionless parameters k, δ and h control the shape of the model in the low, intermediate
Figure
and high15a shows therange
temperature master curves
[67]. superimposed
Higher values of h andtokthe experimental
indicate data
that a higher and the
viscous shift factors,
dissipation
whereas Table 11 summarises the model parameters. The E values of the three specimens
component is present in the material response (with one indicating purely viscous behaviour).
e are very
similar, confirming
On the that
other hand, they
lower wereofobtained
values from that
h and k indicate the the
same mixture
material (same
response aggregate
is more composition,
elastic (with zero
indicating purely elastic behaviour). In general, physically consistent values
same amount of cement). Very similar Eg values were obtained for C12 e C13 specimens whereas are 0 < k < h < 1, B10
with kprovided
specimen characterising the low
a higher temperature/high
value, probably duefrequency behaviour
to a lower and hcontent
air voids the high of
temperature/low
B10 (14,3%) with
frequency behaviour.
respect to C12 and C13 (18.4 and 18.9%, respectively).
The characteristic time τ is a function of the testing temperature:
Identical values of h and k were used for all specimens, obtaining an excellent fitting of the
experimental data. This indicates that whenτ 𝜔𝜏 = τ0→· a0 (high temperature/low frequency) and(3) 𝜔𝜏 →
0 (T )
∞ (low temperature/high frequency) the specimens showed the same viscoelastic dissipation
where τThe
behaviour. variability
0 is the of 𝜏time
characteristic may be reference
at the explained The value of τ does
by specimen-to-specimen
temperature. variability.
not affect the shape
of the master curves. In fact, since τ
The values of 𝜙 are comprised between 0.7° and 1.5°, whereas the measured
is a frequency multiplier, it only affects the position of the master
phase angle
curve
ranges along
from the11°
3° to frequency
(Figureaxes. If τ
15b). Itsincreases, the Ethe
means that 0 master 𝜙 /𝜙
ratiocurve shifts to thefrom
varies left indicating
less thana10%lower(high
relaxation ability
temperature/low of the material.
frequency) to aboutHigher
30%values
(high of τ have been correlated
temperature/low to higher
frequency). We degree
mayofconclude
bitumen that
aging and higher RA content, in both hot and cold mixtures [10,68–70].
the hysteretic dissipation component represents an important part of the material dissipation
Figure 15a shows the master curves superimposed to the experimental data and the shift factors,
behaviour and, more in general, the material is characterised by an intermediate behaviour between
whereas Table 11 summarises the model parameters. The Ee values of the three specimens are very
AC mixtures and cement-bound
similar, confirming mixtures.
that they were obtained from the same mixture (same aggregate composition,
same amount of cement). Very similar Eg values were obtained for C12 e C13 specimens whereas B10
specimen provided
1.E+05a higher value, probably due to a lower air voids content of B10 (14.3%) with respect
to C12 and C13 (18.4 and 18.9%, respectively).
B10 C12 C13 T = 20 °C
Identical values of h and k were used for all specimens, obtaining an excellent fitting of the
experimental data. This indicates that when ωτ → 0 (high temperature/low frequency) and ωτ → ∞
ffness modulus E0 (MPa)
(low temperature/high frequency) the specimens showed the same viscoelastic dissipation behaviour.
1.E+04
The variability of τ0 may be explained by specimen-to-specimen variability.
The values of φHY are comprised between 0.7◦ and 1.5◦ , whereas the measured phase angle ranges
from 3◦ to 11◦ (Figure 15b). Its means that the ratio φHY /φ varies from less than 10% (high temperature/low
1.E+03
Materials 2020, 13, 4697 15 of 19
frequency) to about 30% (high temperature/low frequency). We may conclude that the hysteretic dissipation
component represents an important part of the material dissipation behaviour and, more in general, the
material is characterised by an intermediate behaviour between AC mixtures and cement-bound mixtures.
1.E+05
Stiffness modulus E0 (MPa) B10 C12 C13 T = 20 °C
1.E+04
4
2
Log (shift factor)

1.E+03 0
-2
-4
-6
0 10 20 30 40 50
Temperature (°C)
1.E+02
1.E-07 1.E-04 1.E-01 1.E+02 1.E+05
Frequency fred (Hz)
(a)
15.0
T = 20 °C
B10 C12 C13
Phase angle φ (degree)
10.0
5.0
0.0
1.E-07 1.E-04 1.E-01 1.E+02 1.E+05
Frequency fred (Hz)
(b)
Figure curves
Figure 15. Master 15. Master
of curves
CRAMofat
CRAM at (a)
20 ◦ C: 20 °C: (a) stiffness
stiffness modulus
modulus E0 ;E(b)
0; (b) phase angle ϕ.
phase angle φ.
Table 11. Huet–Sayegh model parameters (Tref = 20 ◦ C).
Eg Ee k h δ log τ0 φHY
Specimen
(MPa) (MPa) - - - - (◦ )
B10 13,583 833 0.093 0.265 1.819 0.669 0.701
C12 7921 712 0.093 0.265 1.990 1.420 0.147
C13 7943 861 0.093 0.265 1.600 1.566 1.439
4. Conclusions
This study aimed at comparing the oven-curing in laboratory and the field curing of a CRAM mixture,
laid in a full-scale trial section. The CRAM was produced with the CCPR technique and applied as binder
course. Gyratory compacted specimens and cores taken from the pavement at different time intervals
were investigated for more than two years.
The results show that the air voids content strongly affects the mechanical properties of CRAMs.
Linear relationships link both ITSM and ITS to the air voids content, by showing that the production of
Materials 2020, 13, 4697 16 of 19
laboratory specimen with a correct air voids level is essential for estimating the mixture performance
in the field.
The evolution of the average ITSM values over the curing time was fitted with an asymptotic
model, which was in good agreement with the measured data. The differences in curing procedures
between laboratory and field caused differences in ITSM. This suggests that oven-curing with free
evaporation (laboratory) and sealed curing with restricted evaporation (field) led to the formation of a
different microstructure. Thus, when bitumen emulsion and cement are used as co-binders, laboratory
curing should be carried out both in sealed and unsealed condition to have a complete understanding
of the mixture potential behaviour in the field.
The complex modulus results confirmed the validity of the time-temperature superposition principle.
A rheological model, explicitly considering non-viscous dissipation, was adopted for analysing the
data and confirmed that CRAMs are characterised by an intermediate behaviour between AC and
cement-bound mixtures.
This study showed that an additional effort is necessary to find a more effective procedure for
producing CRAM specimens in laboratory, able to appropriately estimate the field material performance.
Author Contributions: Conceptualization, A.G. (Andrea Grilli); Methodology, A.G. (Andrea Graziani) and C.M.;
Formal Analysis, G.F. and A.G. (Andrea Graziani); Investigation, C.M.; Writing—Original Draft Preparation,
G.F.; Writing—Review & Editing, G.F., A.G. (Andrea Grilli), C.M. and A.G. (Andrea Graziani); Supervision,
A.G. (Andrea Graziani). All authors have read and agreed to the published version of the manuscript.
Funding: This research received no external funding.
Acknowledgments: The authors wish to thank the Impianti Cave Romagna s.r.l. for the support and collaboration
in managing and building the trial section and Valli Zabban S.p.A. for the support in the specific design and
qualification of the bituminous emulsion.
Conflicts of Interest: The authors declare no conflict of interest.
Acronyms
The following acronyms were used in the text
Definition Acronym
closed form shifting algorithm CFS
cold central-plant recycling CCPR
cold recycled asphalt mixture CRAM
cold recycled material CRM
cold in-place recycling CIR
full-depth reclamation FDR
Huet–Sayegh model HS
indirect tensile stiffness modulus ITSM
indirect tensile strength ITS
linear variable differential transformers LVDT
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Comparing The Field and Laboratory Curing Behavior of Cold Recycled Asphalt Mixtures For Binder Courses

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materials

Materials 2020, 13, 4697; doi:10.3390/ma13214697 www.mdpi.com/journal/materials

2.1. Materials and Mixture

Table 1. Reclaimed asphalt (RA) aggregate characteristics.

Parameter Standard Value

Table 2. Fine aggregate characteristics.

Parameter Standard Value

Table 3. Filler characteristics.

Parameter Standard Value

Table 4. Portland cement characteristics.

Parameter Standard Value Specifications

Table 5. Bituminous emulsion characteristics.

Parameter Standard Value Specification

2.2. Trial Section

Figure 2. Mixing plant for cold mixture production.

10 5 March April May June July August

Figure 4. Location of the five Subsections.

Subsection A Subsection B Subsection C Subsection D Subsection E

Ev1 = 163 MPa

First Phase Second Phase Third Phase

All the Subsections were

for Subsection B, CInand D. After

Table 8. Coring plan.

Core Number of Specimens

ITSM ITSM + ITS Complex modulus

Curing at room temperature

3 11 23 31 55 73 8393 157 194 796

2.4. Testing Procedures

Air Voids Content

2000 73 days field+10 days lab ITSM = -931·Vv + 21816; R² = 0.90

Figure 9. Relationship betweenbetween

Curing time [days]

4000 180 160

Figure 10. Measured

6000 (Days) (MPa) (MPa) (Days) (-) (%)

gyratory specimens 3 4668 9246 21 0.97 11.8

Curing time [days]

taken from Subsection C, from 23 4000to 796

Group 0 (gyratory) and Group 2 (cores).

ti yi ya hy R2 Air Voids Content

0.2 gyratory specimens

Loss modulus E2 (MPa)

Overall, the stiffness

Log (shift factor)

Table 11. Huet–Sayegh model parameters (Tref = 20 ◦ C).

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