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Curing and temperature sensitivity of cement–bitumen

treated materials
a b a a
Fabrizio Cardone , Andrea Grilli , Maurizio Bocci & Andrea Graziani
a
Department of Civil and Building Engineering, and Architecture, Università Politecnica
delle Marche, Ancona, Italy
b
Department of Economics and Technology, University of the Republic of San Marino,
Republic of San Marino
Published online: 13 Oct 2014.

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To cite this article: Fabrizio Cardone, Andrea Grilli, Maurizio Bocci & Andrea Graziani (2015) Curing and temperature
sensitivity of cement–bitumen treated materials, International Journal of Pavement Engineering, 16:10, 868-880, DOI:
10.1080/10298436.2014.966710

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 International Journal of Pavement Engineering, 2015
Vol. 16, No. 10, 868–880, http://dx.doi.org/10.1080/10298436.2014.966710

Curing and temperature sensitivity of cement –bitumen treated materials

Fabrizio Cardonea, Andrea Grillib, Maurizio Boccia and Andrea Graziania*
a
Department of Civil and Building Engineering, and Architecture, Università Politecnica delle Marche, Ancona, Italy; bDepartment of
Economics and Technology, University of the Republic of San Marino, Republic of San Marino
(Received 26 June 2013; accepted 10 August 2014)

In the present study, the curing process of cement – bitumen treated materials (CBTM) was investigated by analysing the
influence of cement dosage and curing temperature on moisture loss and evolution of complex modulus. Moreover, the study
aimed to characterise the thermo-rheological behaviour of cured CBTM. Results showed that moisture loss by evaporation
controls the increase in stiffness of the mixtures. However, excessive evaporation can hinder the full potential of the cement
hydration process. Results also showed that the quantitative effects of curing time and loading frequency on stiffness can be
superposed. Similar to hot-mix asphalt, CBTM showed a viscoelastic and thermo-dependent response. In particular, results
suggested that at higher frequencies, the iso-thermal viscoelastic response is mainly affected by the aged binder whereas, at
lower frequencies, the response of the mixtures depended mainly on the behaviour of the fresh binder.
Downloaded by [Mr Pusjatan Bandung] at 02:35 27 August 2015

Keywords: cold recycling; cement – bitumen treated materials; curing; temperature sensitivity; complex modulus

Introduction dosage of bituminous binder. Usually, the RAP is blended

The growing social and political awareness about
environmental issues is moving towards the development
of low-energy and low-emission technologies for the
production and laying of bituminous mixtures. At the same
time, the limited availability of natural aggregates and the
increasing disposal costs of milled materials is supporting
the worldwide diffusion of recycling technologies for
pavement construction and rehabilitation (ARRA 2001,
EAPA 2008). In this context, cold recycling is becoming one
of the most attractive rehabilitation technologies because it
allows high-performance mixtures with low environmental
impact to be produced (Stroup-Gardiner 2011).
Basically, cold recycling consists of milling a
distressed bituminous pavement and combining the milled
material with one or more binding agents to produce a new
pavement layer without reheating. Bituminous binders
(paving grade bitumen or modified bitumen, either as foam
or emulsion), hydraulic binders (Portland cement,
hydrated lime and fly ash) and chemical additives
(recycling agents, rejuvenators) are employed to cover
the mechanical deficiencies of the cold recycled mixes and
to achieve the required structural and durability properties
(Kearney 1997, Stroup-Gardiner 2011).
A wide range of mixtures can be produced by cold
recycling techniques depending on the composition of the
recycled aggregate mix and the type and dosages of the
binding agents. In current practice, the term cold-recycled
asphalt mixture (CAM) indicates a mixture consisting of
reclaimed asphalt pavement (RAP) treated with a high
with virgin aggregate to meet grading requirements.
In most cases, bituminous emulsion or expanded (foamed)
bitumen is employed, while cementitious (hydraulic)
binders can also be added as ‘active’ fillers in order to
improve the short-term properties of the mix. The high
dosage of residual binder (fresh bitumen) and a ratio of
bituminous and cementitious binder normally greater than
one (B/C . 1), confers asphalt-like mechanical properties
like loading rate and temperature susceptibility to CAM
(Kim and Lee 2012, Stimilli et al. 2013).
The cold recycled mixture composition changes when
RAP is blended with reclaimed aggregates coming from
the underlying base or subbase layers, either unbounded or
hydraulically-bounded (Thompson et al. 2009, Bocci et al.
2011, 2014). As such, three main types of mixtures can be
distinguished: bitumen stabilised materials (BSM), cement
treated materials (CTM) and cement – bitumen treated
materials (CBTM).
BSM can be obtained with the addition of bituminous
binders, either as bitumen emulsion or foamed bitumen
(Asphalt Academy 2009). BSM are characterised by lower
bitumen dosage with respect to CAM and by a limited
dosage of active fillers. As a consequence, the mechanical
properties of BSM show a stress-dependent behaviour
with improved shear resistance if compared to unbound
granular materials (Fu and Harvey 2007).
CTM are produced using only cement as stabilising
agent and typically show brittle behaviour characterised
by the susceptibility to shrinkage cracking and a great

*Corresponding author. Email: a.graziani@univpm.it

q 2014 Taylor & Francis
 International Journal of Pavement Engineering
permanent deformation resistance (Xuan et al. 2012, Grilli
et al. 2013b).
CBTM are characterised by higher dosages of
cementitious binder with respect to BSM (generally
B/C # 1) which leads to an increase in stiffness and
strength properties (Grilli et al. 2012). From a mechanical
point of view, CBTM are stiffer and less prone to
permanent deformation as compared to BSM and show
reduced cracking susceptibility with respect to conven-
tional CTM (Bocci et al. 2011).
Regardless of aggregate nature, binder type and
dosage, a distinctive feature of cold recycled mixtures is
the requirement for a certain curing period to develop the
ultimate mechanical properties (strength and stiffness).
When both bituminous and cementitious binders are
employed, the curing process actually results from diverse
mechanisms: emulsion breaking, moisture loss and
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hydration of cementitious compounds (Asphalt Academy
2009, Kavussi and Modarres 2010, Bocci et al. 2011).
Controlling the breaking process is particularly
important when bitumen emulsion is employed because
it must occur after the completion of the mixing and
compaction phases. Afterwards, the presence of water
inside the cold recycled mixtures delays the attainment of
the ultimate mechanical properties. Moisture loss, by
means of drainage or evaporation, ensures mixture
hardening and bonding between the bituminous mortar
(i.e. fine aggregate particles bonded by the bituminous
binder) and the coarse aggregate skeleton.
Hydration of cementitious materials is linked to
various chemical and physical phenomena. Starting from
the early curing stages, it accelerates the emulsion
breaking process, increases the rate of bitumen coalesc-
ence and reduces the amount of evaporable water (Brown
and Needham 2000, Giuliani 2001). At low cement
content, the hydration products disperse inside the
bituminous mortar increasing its viscosity and improving
the resistance of the mixture to permanent deformations.
At higher cement content, the volume of hydration
products grows forming a stiffer matrix that connects
coarser aggregate particles (Garcia et al. 2013).
It is particularly important to remark that while the
curing process of bituminous binders, either emulsion or
foam, is strictly linked to moisture loss, the chemical
reactions that take place during the hydration of
cementitious binders require the presence of water and
do not entail any moisture loss.
Laboratory curing of cold recycled mixtures aims to
simulate field curing conditions while trying to accelerate
the attainment of ultimate properties (Jenkins and Moloto
2008). However, the factors that influence field curing are
extremely difficult to standardise and reproduce because
they are related to composition (binder types and dosage)
of the mixture, construction features (degree of compac-
tion, layer thickness, drainage conditions, construction
869
phases) and environmental factors (temperature, humidity,
wind). Therefore, a rational laboratory curing procedure
should: consider the relevant curing mechanisms which
arise from mixture composition (emulsion breaking/
moisture loss and cement hydration), define specimen
shape, dimensions and boundary conditions and control
curing temperature and relative humidity.
In the present laboratory study, the curing process of
CBTM is investigated by measuring the evolution of
moisture and stiffness. Specifically, uniaxial cyclic com-
pression tests (CCT) were carried out to measure complex
modulus at different curing ages. Our main objective was to
analyse the evolution of stiffness evolution of in CBTM
considering the influence of mixture and environmental
factors (cement dosage and curing temperature).
Another objective of the study was to characterise the
thermo-rheological behaviour of cured CBTM using the
procedure which is normally employed for hot-mix asphalt
(HMA). Therefore, complex modulus tests were performed
on 28-day cured mixtures and the results were analysed to
compare the effects of temperature and loading time.
Experimental programme
Materials
The samples of CBTM tested in this study were prepared
in the laboratory using RAP, virgin aggregate, bituminous
emulsion, Portland cement and water.
The RAP was sampled from a cold recycling jobsite
after milling the aged asphalt layers (Bocci et al. 2010).
Its average size distribution, obtained by wet sieving, is
reported in Figure 1. As can be observed, the maximum
size of the RAP particles is 32 mm, and the fine content is
low because the finer aggregate particles, including filler,
are bound to larger aggregate particles forming RAP
lumps. The average bitumen content of RAP was 4.6% by
aggregate weight (EN 12697-1), and the maximum size of
the extracted aggregate was 12 mm. The RAP was
designated as 32 RA 0/12 according to the European
100
0/4
6/12
75
12/20
Passing (%)
32 RA 0/12
50 CBTM mix
25
0
0.01 0.1 1 10 100
Sieve size (mm)
Figure 1. Gradation of virgin aggregates (0/4, 6/12, 12/20),
RAP (32 RA 0/12) and CBTM mixtures.
 870 F. Cardone et al.

Table 1. Main physical properties of the used aggregates. Table 2. Properties of bituminous emulsion and residual
bitumen.
Water absorption at
Material Particle density (Mg/m3) 24 h (%) Test
procedure Value
32 RA 0/12 2.50 0.5
12/20 (coarse) 2.69 0.9 Emulsion property
6/12 (coarse) 2.69 1.0 Polarity EN 1430 Positive
0/4 (fine) 2.73 1.8 Water content EN 1428 40%
pH EN 12850 3
Breaking value EN 13075-1 180
standard EN 13108-8. Two crushed coarse aggregate sizes, Settling tendency at 7 days EN 12847 8%
Mixing stability with cement EN 12848 2g
6/12 and 12/20, and a fine aggregate size, 0/4 having the
Residual binder property
same mineralogy (limestone) were blended with the RAP Penetration EN 1426 70 £ 1021 mm
in order to obtain the final mixture grading (Figure 1). The Softening point EN 1427 508C
main physical and geometrical properties of RAP and Fraass breaking point EN 12593 2 108C
virgin aggregate particles are summarised in Table 1.
The aggregate blend was prepared by mixing 50% of
RAP, 10% of 12/20, 5% of 6/12 and 35% of 0/4. These the laboratory (Tebaldi et al. 2014). The procedure adopted
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proportions were selected in order to meet the Italian
specification for a subbase course (Figure 1).
A cationic, slow-setting bituminous emulsion with a
60% nominal binder content was employed (Table 2). The
emulsion, designated as C60B5 according to the European
standard EN 13808, is specifically formulated for cold
recycling. In fact, it is characterised by high mixing stability
with cement (over-stabilised emulsion) and allows good
workability during the mixing and compaction phases. The
employed emulsion dosage was 3% by dry aggregate
weight, corresponding to 1.8% of residual (fresh) bitumen.
A Portland limestone cement type II/B-LL, strength
class 32.5 R (EN 197-1) was employed. Its composition is
a combination of clinker (65 – 79%) and limestone dust
(35 – 21%). Mixtures with two cement dosages (1% and
2% by dry aggregate weight) were produced and referred
to as M3B1C and M3B2C, respectively.
The mixing water content was 5% by dry aggregate
weight; this amount was determined in a preliminary mix-
design study and includes emulsion water and extra water
which is added to the fresh mix in order to improve
compactability (Grilli et al. 2012).
Specimen preparation
Before mixing and compaction, virgin aggregate and RAP
were dried at 1058C and 408C, respectively. The dry
aggregate blend was preliminarily mixed with a water
amount corresponding to the absorption of the constituent
particles. In order to obtain a homogeneous moisture, the wet
aggregate blend was stored in a sealed plastic bag for 12 h, at
room temperature. Afterwards, each blend was thoroughly
mixed, gradually adding water, cement and emulsion, in this
sequence. After mixing by hand for at least 2 min, a visual
evaluation was made to check for homogeneity and to verify
that emulsion breaking had not taken place.
Various types of compaction equipment are currently
employed for the preparation of cold-recycled specimens in
in the present study was developed in Italy, based on several
years of field experience (Santagata et al. 2009, Bocci et al.
2011, Grilli et al. 2012). In particular, specimens were
compacted by means of a shear gyratory compactor in a
100-mm diameter mould with a constant pressure of
600 kPa, a gyration speed of 30 rpm and a constant angle of
inclination of 1.258. For each specimen, the weight of the
loose mixture (about 2.4 kg) was adjusted to attain a bulk
density of about 2100 kg/m3 and a specimen height of
150 ^ 2 mm after 180 gyrations. After compaction, speci-
mens were sufficiently stable to allow immediate extrusion.
Curing procedure
The curing conditions were fixed and controlled to study
the evolution of the material properties as a physical
phenomenon. Compacted specimens were cured in a
climatic chamber at constant relative humidity (70 ^ 5%)
and at two curing temperatures (20 ^ 28C and 40 ^ 28C).
The relative humidity value was considered a reasonable
compromise in order to achieve curing of the bituminous
components, which is essentially based on moisture loss,
and the curing of cementitious components, which instead
requires a moist environment. The temperature of 208C
was considered a reference value, while the temperature of
408C was selected to obtain accelerated curing.
Complex modulus testing procedure
Complex modulus testing was conducted to measure the
stiffness evolution arising from the curing process and to
characterise the thermo-rheological behaviour of the
CBTM mixtures at their final curing stage (28 days).
Uniaxial CCTs were performed using a servo-
pneumatic testing equipment in control strain mode; a
sinusoidal (haversine) axial strain with 15 me amplitude
was applied at various frequencies. The deformation was
measured by means of two inductive transducers, fixed to
 International Journal of Pavement Engineering
Table 3. Complex modulus testing programme.
Temperature
Curing effect effect
Material codes M3B1C, M3B2C M3B1C, M3B2C
Curing temperatures (8C) 20, 40 20
Curing time (days) 1, 3, 7, 14, 21, 28
28
Testing temperatures (8C) 20 5, 20, 35, 50
Testing frequencies (Hz) 0.1, 0.3, 1, 3, 10, 0.1, 0.3, 1, 3, 10,
20 20
the lateral surface of the specimen 1808 apart; a 70-mm
measurement base was adopted to reduce end effects and
to provide a more accurate deformation reading. The test
procedure was adapted from those available for HMA
mixtures (EN 12697-26, AASHTO T 342-11). Although
higher strain amplitudes (up to 100 me) are currently
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applied to test HMA in the linear viscoelastic domain, a
reduced strain level was employed because the presence of
cementitious components may reduce the linearity field
and also in order to avoid specimen damage due to local
brittle behaviour, as observed in previous studies (Bocci et
al. 2011). The axial load was measured using a 20-kN load
cell.
A total of 110 test cycles were applied at each
frequency, and the last 10 cycles were analysed to
calculate the average amplitude of the sinusoidal strain
(10) and the corresponding amplitude of the sinusoidal
stress (s0). The complex modulus E* was calculated as
follows:
E* ¼ E0 expðjwÞ; ð1aÞ
s0
E0 ¼ ; ð1bÞ
10
w ¼ 2pf Dt; ð1cÞ
where E0 is the absolute value (norm) of the complex
modulus, also called the stiffness (or dynamic) modulus, w
is the phase (or loss) angle, f is the test frequency, j is the
imaginary unit ðj2 ¼ 21Þ, and Dt is the average time lag
between stress and strain over the analysed test cycles.
Summary of test programme
The complex modulus test programme is summarised in
Table 3. Two CBTM were analysed, characterised by 3%
emulsion dosage and two cement dosages: 1% and 2%
(coded M3B1C and M3B2C, respectively). For each
mixture, two series of six replicate specimens were
prepared. The first series was cured at 208C and the second
at 408C. For each series, four specimens were subjected to
CCT and two (control specimens) were used as reference
to check moisture loss due to evaporation.
871
100
80
Moisture loss (%)
60
40 M3B1C curing at 20°C
M3B1C curing at 40°C
20 M3B2C curing at 20°C
M3B2C curing at 40°C
0
0.1 1 10 100
Curing time (days)
Figure 2. Moisture loss by evaporation during the curing phase.
In order to evaluate the curing effect on stiffness, CCT
were carried out at 208C and six frequencies (0.1, 0.3, 1, 3,
10 and 20 Hz) at curing times of 1, 3, 7, 14, 21 and 28 days.
Specimens cured at 408C were conditioned for 4 h at 208C
before mechanical testing.
The thermo-rheological behaviour of the studied cold
recycled mixtures was analysed by performing CCT on the
specimen series cured at 208C for 28 days, at four
temperatures (58C, 208C, 358C and 508C) and six test
frequencies (0.1, 0.3, 1, 3, 10 and 20 Hz).
Results and discussion
Moisture loss
Moisture loss by evaporation was measured by weighing
the control specimens, and results are reported in Figure 2
where the curing time axis is in log scale. As can be
observed, moisture loss was particularly high in the first
hours and, after one curing day, exceeded 50% of the
initial water content for all specimens.
As expected, raising the curing temperature from 208C to
408C accelerated the rate of evaporation of both mixtures.
In particular, specimens cured at 408C reached an
equilibrium water content WEQ after 7 days, while specimens
cured at 208C required about 14 days. The value WEQ appears
to be influenced by the cement content of the mixture. In fact,
after 28 days of curing, mix M3B2C retained about 7% of the
initial water content, corresponding to WEQ ¼ 0.35%, while
mix M3B1C retained about 10% of the initial water content,
corresponding to WEQ ¼ 0.50%.
In order to analyse the moisture loss data, it should be
considered that the WEQ contains the water required by the
cement hydration process WHY that is not available for
evaporation. Part of WHY (about 23% of cement weight) is
chemically bound and becomes part of the calcium –
silicate– hydrate (C– S –H) gel; another part (about 19% of
cement weight) is adsorbed by the C – S –H nano-porosity
and can be removed only at extremely low relative
humidity values (below 50%) (Mehta and Monteiro 1993).
Therefore, the amount of water required by the hydration
 872 F. Cardone et al.

(a) 10000 (a) 10000

28 days 28 days
21 days

Stiffness modulus (MPa)

21 days
Stiffness modulus (MPa)

14 days 14 days
7 days 7 days
3 days 3 days
1 day 1 day

1 % cement - curing at 20°C 2 % cement - curing at 20°C

1000 1000
0.01 0.1 1 10 100 0.01 0.1 1 10 100

Frequency (Hz) Frequency (Hz)

(b) 10000 (b) 10000

28 days 28 days

Stiffness modulus (MPa)

21 days 21 days
Stiffness modulus (MPa)

14 days 14 days
7 days 7 days
3 days 3 days
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1 day 1 day

1 % cement - curing at 40°C 2 % cement - curing at 40°C

1000 1000
0.01 0.1 1 10 100 0.01 0.1 1 10 100

Frequency (Hz) Frequency (Hz)

Figure 3. Stiffness modulus E0 at 208C for M3B1C mixtures: Figure 4. Stiffness modulus E0 at 208C for M3B2C mixtures:
(a) curing at 208C and (b) curing at 408C. (a) curing at 208C and (b) curing at 408C.

For the M3B2C mixture, the estimated amount of

process can be estimated as
W HY ¼ ð0:23 þ 0:19Þakc0 ;
where a is the degree of hydration of the cement paste, c0
is the cement dosage relative to the dry aggregate weight
(1% for mix M3B1C, 2% for mix M3B2C) and k is the
fraction of Portland cement clinker in the cement (0.72
was assumed as the average value of the clinker content
range).
Considering a degree of hydration a ¼ 0.9, which may
be a reasonable assumption after 28 days of curing (Garcia
et al. 2013), Equation (2) gives: WHY ¼ 0.27% and
W HY ¼ 0.54% for mixtures M3B1C and M3B2C,
respectively.
This indicates that for the M3B1C mixture, the
measured equilibrium water content (WEQ ¼ 0.50%) still
contains a residual fraction of potentially evaporable water
(WEQ 2 WHY ¼ 0.23%); this residual amount may be
contained inside the larger-sized (capillary) pores of the
hydrated cement paste or inside the surface porosity of the
aggregates. Furthermore, the residual water amount may
form water bubbles inside the bituminous mortar, as shown
by Garcia et al. (2013), influencing the mechanical
behaviour of the mixture.
water required by hydration (WHY ¼ 0.54%) exceeded the
measured equilibrium water content (WEQ ¼ 0.35%). This
ð2Þ implies that the actual degree of hydration after 28 days
was well below the previously hypostasised value
(a ¼ 0.9). In fact, assuming that all the equilibrium
water content was employed in the hydration process
(WHY ¼ WEQ), Equation (2) would yield a degree of
hydration a ¼ 0.54, indicating that for the M3B2C
mixture moisture loss by evaporation stopped the
hydration process at about one-half of its potential.
Curing effects
Stiffness modulus
The stiffness modulus E0, measured at 208C and at curing
times starting from 1 to 28 days (average of four replicate
specimens), is reported in Figures 3 and 4, as a function of
test frequency, obtaining iso-curing curves. For each
curing period, stiffness increases with increasing test
frequency, at both curing temperatures. This typical
viscoelastic response, similar to the response of HMA (Di
Benedetto and de la Roche 1998), is generally measured
on cold recycled mixtures produced with both emulsion
(Kim and Lee 2012) and foamed bitumen (Van de Ven
 International Journal of Pavement Engineering 873

(a) 10000 The pattern of iso-curing modulus curves shown in

M3B1C curing at 20°C Figures 3 and 4 closely resembles the pattern of iso-
Stiffness modulus (MPa)

M3B1C curing at 40°C thermal stiffness values obtained in routine frequency

sweep tests on HMA. This suggests that the quantitative
effects of curing time and loading rate on E0 could be
superposed, and a unique master curve could be obtained
by selecting a reference curing time and shifting the iso-
curing values parallel to the frequency axis. This is
equivalent to defining a curing-reduced loading frequency
fr,c:
1000
1.0E–05 1.0E–03 1.0E–01 1.0E+01 1.0E+03
f
Curing-reduced frequency (Hz) f r;c ¼ ; ð3Þ
ac;R ðtc Þ
(b) 10000
M3BC2 curing at 20°C
where f is the actual test frequency and ac,R(tc) is a curing
Stiffness modulus (MPa)

M3BC2 curing at 40°C

shift factor whose value at each curing time tc depends on
the stiffness variation between tc and the reference curing
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1000
1.0E–05 1.0E–03 1.0E–01
Curing-reduced frequency (Hz)
Figure 5. Curing master curves of E0 at 208C at reference
curing time tc,R ¼ 28 days: (a) M3B1C mixtures and (b) M3B2C
mixtures.
et al. 2007). Fresh bituminous binder plays a major role in
the viscoelastic response, but the aged binder in the RA
also gives its contribution to the time- (and temperature)
dependent response (Grilli et al. 2013a).
Higher stiffness was measured with longer curing
times, regardless of the curing temperature. However, it
was observed that beyond 14 days the distance between
iso-curing lines tends to vanish, suggesting that stiffness is
approaching its ultimate value. This observation can be
directly related to the moisture loss trend of the mixtures
(Figure 2). In particular, it should be noted that all
mixtures showed a noticeable increase in stiffness between
7 and 14 days even if no significant moisture loss due to
evaporation occurred. This can be explained by cement
hydration that carried on using the residual water still
present inside the bituminous mortar or absorbed by the
surface porosity of aggregates.
time tc,R.
A similar approach, based on the definition of an age-
reduced time, has been used to characterise the creep and
relaxation response of polymeric and bituminous materials
subjected to physical ageing (Struik 1978, O’Connell and
McKenna 1997, Barbero and Julius 2004, Canestrari et al.
1.0E+01 1.0E+03
2013). The use of a shift function has also been proposed
to model the creep behaviour of ageing concrete (Bazant
and Wu 1974). In this perspective, the curing of CBTM
may be considered a sort of short-term ageing.
In the present study, a four-parameter sigmoidal
function was adopted to represent the curing master curve:
a
log E0 ðf r;c Þ ¼ d þ ; ð4Þ
1 þ exp ðb þ g log f r;c Þ
where a, b, d and g are shape parameters that were
estimated by the curve fitting of experimental data,
allowing a free variation of the curing shift factors.
Equation (4) is extensively employed to represent the
stiffness master curve of HMA (Pellinen et al. 2002)
obtained by superposing the effects of loading frequency
and temperature (time – temperature superposition prin-
ciple [TTSP]). It is worth noting that the TTSP is applied
with the implicit assumption that HMA is a non-ageing
material and that its rheological properties do not change
with time (e.g. binder ageing is fixed). In the present study,
the same mathematical procedure was applied to analyse
curing by superposing the effects of loading frequency and
curing time, fixing the loading temperature at 208C. The

Table 4. Shape parameters of the stiffness modulus curing master curve at 208C (reference curing time tc,R ¼ 28 days).

Mixture code Curing temperature (8C) d a b g R2

M3B1C 20 2.875 1.201 2 0.639 2 0.459 0.999
M3B1C 40 2.880 1.115 2 0.691 2 0.513 0.999
M3B2C 20 2.984 1.031 2 0.784 2 0.534 0.999
M3B2C 40 2.659 1.405 2 0.772 2 0.377 0.999
 874 F. Cardone et al.

M3B2C curing at 40°C M3B2C curing at 20°C M3B1C curing at 20°C

M3B1C curing at 40°C M3B1C curing at 20°C M3B1C curing at 40°C
(a) 4 M3B2C curing at 20°C
M3B2C curing at 40°C
4.0
Standardised residuals

3.0
0

2.0
–2

log ac,28
1.0
–4
3.0 3.2 3.4 3.6 3.8 4.0
Fitted values (log E0) 0.0
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M3B2C curing at 40°C M3B2C curing at 20°C

M3B1C curing at 40°C M3B1C curing at 20°C –1.0
1 10 100
(b) 4
Curing time (days)

Figure 7. Curing shift factors ac,28(tc) versus curing time tc.

Standardised residuals

0
–2
–4
–4 –2 0 2
Theoretical Quantiles
Figure 6. Residual analysis for the E0 curing master curve
models: (a) standardised residuals versus fitted values and (b) Q–
Q plot.
influence of test temperature on stiffness was separately
considered on the 28-day cured mixtures.
The stiffness modulus master curves at 208C and at the
reference curing time of 28 days are shown in Figure 5.
Excellent fitting of the experimental data was obtained
with Equation (3) (Table 4). The adequacy of the
sigmoidal model was checked with a residuals analysis.
Plotting the standardised residuals against the fitted values
of the independent variable (log E), it is observed that the
values show a random pattern and fall in the interval
(2 2, þ 2) (Figure 6(a)). Moreover, in the Q –Q plot
(Figure 6(b)), the residuals are distributed approximately
along the 458 reference line. These plots indicate that
residuals may be considered uncorrelated random
variables with normal distribution and therefore the
proposed model shows no severe inadequacies.
The logarithm of curing shift factors are plotted in
Figure 7 as a function of curing time (shifting function);
the values log ac,28(tc) are proportional to the horizontal
shift of the iso-curing lines on the log-frequency scale and
therefore may be used to measure the curing level at each
test frequency with respect to the 28 days condition.
From Figure 5, it can be observed that raising the
4
curing temperature from 208C to 408C, a lower stiffness is
obtained at 28-day curing, especially with 2% cement
content. A similar reduction in stiffness at long curing
times was also measured on CBTM by means of indirect
tensile tests (Bocci et al. 2011). This effect can be related
to the structural and morphological characteristics of the
hydrated cement. In particular, at higher curing tempera-
tures the density of the hardened cement can be less
uniform and have higher porosity (Verbeck and Helmuth
1969), leading to lower mechanical properties.
From Figure 7, it can be observed that at fixed cement
content lower shift factors were obtained when the curing
temperature was raised from 208C to 408C. This confirms
that higher temperature accelerated the curing process.
In fact, lower values of the curing shift factors (ac,28) at a
specific curing time (tc) indicate higher stiffness with
respect to the 28-day reference curing state, denoting a
higher curing level.
Starting from 14 days, the shifting functions tend to
overlap, indicating that in this second phase specimens
cured at 208C show a higher rate of stiffness increase. This
behaviour can be related to the amount of water present in
the mixture (Figure 2): at 408C evaporation is almost
 International Journal of Pavement Engineering 875

4.0 (a) 20.0

Phase angle (degree)

15.0
3.0

28 days
10.0 21 days
2.0 14 days
log ac,28

7 days
5.0 3 days
1.0 1 day 2 % cement - curing at 20°C

0.0
0.01 0.1 1 10 100
0.0 Frequency (Hz)
(b) 20.0

–1.0
50 60 70 80 90 100

Phase angle (degree)

15.0
Moisture loss (%)
Downloaded by [Mr Pusjatan Bandung] at 02:35 27 August 2015

28 days
10.0 21 days
M3B2C Curing at 40°C
14 days
y = –0.078x + 7.586 R2 = 0.950 7 days
M3B2C Curing at 20°C 5.0 3 days
y = –0.084x + 7.878 R2 = 0.982 1 day
2 % cement - curing at 40°C
M3B1C Curing at 40°C
0.0
y = –0.062x + 5.608 R2 = 0.969
0.01 0.1 1 10 100
M3B1C Curing at 20°C
y = –0.061x + 5.485 R2 = 0.994 Frequency (Hz)

Figure 9. Phase angle at 208C for M3B2C mixtures: (a) curing

Figure 8. Curing shift factors ac,28 versus moisture loss. at 208C and (b) curing at 408C.

complete after 7 days while at 208C some residual water is

still present in the mixture, allowing cement hydration to
proceed.
At a fixed curing temperature, higher shift factors were
obtained for the M3B2C mix compared to the M3B1C mix.
This indicates that cement addition resulted in a slower
increase of curing level, especially in the short term (1–
7 days). Beyond 14 days, the shifting functions tend to
overlap which indicates that in this phase specimens with a
higher cement content show a faster increase in curing level.
Additional information on the mechanisms that control
the curing process (evaporation and hydration) can be
obtained by plotting the curing shift factors versus
moisture loss by evaporation (Figure 8). As can be
observed, for M3B1C mixtures the relationship between
curing shift factors and moisture loss is almost perfectly
linear regardless of the curing temperature. This suggests
that the curing level, as measured by stiffness increase, is
controlled by the amount of moisture loss through
evaporation, whereas the curing temperature controls the
rate of curing level increase.
The development of stiffness for M3B2C mixtures is
analogous, as the increase can be basically explained by
the amount of moisture loss. However, at a fixed moisture
loss, M3B2C mixtures showed higher ac,28 values and
therefore lower curing level compared to the M3B1C
mixture. This indicates that the curing level of M3B2C
results from the combined effect of moisture loss and
cement hydration. In fact, when moisture content gets
closer to its equilibrium value, the curing shift factors
trend is no longer a function of moisture loss. At this point,
an increase in the curing level is not related to moisture
loss anymore but can be explained by cement hydration.
These findings suggest that an improved curing for
CBTM could be obtained by a two-phase procedure. In the
initial phase, environmental conditions should facilitate
moisture loss by evaporation to achieve curing of the
bituminous binder (low relative humidity); in the second
phase, once the equilibrium moisture value has been
reached, curing should aim to obtain the maximum degree
of hydration of the cementitious binder using the non-
evaporable water possibly present in the mixture or even
providing a moist environment. The relative duration of the
two phases should be related to environmental conditions
and to the initial moisture content of the CBTM, which is
usually established in order to obtain optimal compaction.
Phase angle
The phase angle (w) can be used to evaluate the balance
between the elastic and viscous response of CBTM and
 876 F. Cardone et al.

(a) 10000
Stiffness modulus (MPa)

Stiffness modulus
28 days
21 days
14 days F
7 days N
3 days
1 day

2 % cement - curing at 20°C Effect of curing time

1000 Effect of loading frequency
0 5 10 15 20
Phase angle (degree)
Phase angle
(b) 10000
Figure 11. Schematic representation of loading frequency and
curing time effects on E* components: increase in loading
Stiffness modulus (MPa)

frequency (F); increase in curing time (C); non-linearity effect

(N).
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28 days
21 days
14 days
7 days
3 days
1 day
2 % cement - curing at 40°C
1000
0 5 10
Phase angle (degree)
Figure 10. Black curves for M3B2C mixtures: (a) curing at
208C and (b) curing at 408C.
how such a balance is affected by curing. As an
example, iso-curing curves of w measured at 208C are
reported in Figure 9 for M3B2C (the same trend was
observed for M3B1C). For each curing period, the w
values decrease with increasing test frequency at both
curing temperatures. This behaviour is consistent with
the stiffness modulus variation and can be related to the
viscoelastic response of the fresh and aged bituminous
binder.
For each loading frequency, lower phase angles were
measured at longer curing times. In particular, it was
observed that beyond 7 days, curing the distance between
iso-curing curves tends to vanish similar to stiffness
modulus (Figure 4). Considering the observed moisture
loss trend (Figure 2), the higher viscous response of the
mixture at short curing times can be related to the presence
of water inside the mortar composed of fresh bitumen, fine
aggregate and cement, which binds the coarser aggregate
particles (virgin or recycled).
Similar to the stiffness modulus, an attempt was made
to superpose the effects of frequency and curing time for
the phase angle. However, the shape of the w iso-curing
lines clearly did not allow acceptable results to be obtained
(i.e. a unique master curve).
Overall viscoelastic response
The overall influence of curing on E* can be analysed in
the Black space where the stiffness modulus is plotted
versus the phase angle (Figure 10). As can be observed, a
15 20
unique curve cannot be obtained, indicating that it is not
possible to superpose the effects of load frequency and
curing time. As shown above, this is mainly due to the
phase angle and therefore to the viscous component of the
material response.
The combined effect of loading frequency and curing
on E0 and w is summarised in Figure 11. The dashed
curves represent the variability of E* with the load
frequency, that is the viscoelastic response which is due to
the fresh bituminous binder and the aged binder in the
RAP. On the other hand, the continuous lines indicate the
variability of E* with the curing age which is due only to
the curing-dependent mortar (fresh bituminous binder
and cement).
A stiffness increase can be obtained with higher test
frequencies (path F) or longer curing times (path C).
However, in the second case, the reduction in viscous
response is smaller (smaller phase angle reduction)
because it is related only to mortar curing.
From a phenomenological point of view, the effects of
curing (stiffness increase, phase angle reduction) may be
considered opposite to the effects of non-linearity (path N)
that results in stiffness reduction and a phase angle
increase (Gauthier et al. 2010). Opposite effects can be
explained by opposite physical phenomena: in the first
case, curing leads to the formation of stable micro-
structural bonds through the hardening of the fresh
bituminous phase and cement hydration; in the second
case, non-linearity occurring with large and/or repeated
strains, brings to a progressive destruction of supra-
molecular structures and networks (Gauthier et al. 2010).
 International Journal of Pavement Engineering 877

(a) 10000 100000

M3B2C
Stiffness modulus (MPa)

Stiffness modulus (MPa)

M3B1C
10000

1000 5 °C
20 °C
35 °C 1000
50°C

1 % cement
100 100
0.01 0.1 1 10 100 1.0E–06 1.0E–04 1.0E–02 1.0E+00 1.0E+02 1.0E+04

Frequency (Hz) Temperature-reduced frequency (Hz)

(b) 10000 Figure 13. Stiffness modulus master curves (curing for 28 days
at 208C), reference temperature T0 ¼ 208C.
Stiffness modulus (MPa)

stiffness variation between T and the reference temperature

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1000 5 °C
20 °C
35 °C
50°C
2 % cement
100
0.01 0.1
Frequency (Hz)
Figure 12. Stiffness modulus E0 after 28 days of curing at 208C:
(a) M3B1C mixtures and (b) M3B2C mixtures.
Temperature susceptibility
Stiffness modulus
The stiffness modulus of the studied CBTM measured
after 28 days of curing at 208C (average of the four
replicate specimens) is reported in Figure 12. Iso-thermal
curves at 58C, 208C, 358C and 508C show an increase in
stiffness with increasing test frequency and decreasing
temperature. This viscoelastic and thermo-dependent
response is analogous to the response of HMA mixtures.
Applying the TTSP, the stiffness modulus master curve
was obtained by fitting the experimental data using the
sigmoidal function described by Equation (4). In this case,
the temperature-reduced frequency is defined in the usual
way:
f r;T ¼ aT;R ðTÞf ;
where f is the actual test frequency and aT,R(T) is a shift
factor whose value, at each temperature T, depends on the
TR.
The stiffness modulus master curves at reference
temperature TR ¼ 208C are shown in Figure 13. Excellent
fitting of the experimental data was obtained with
Equation (4), allowing a free variation of the curing shift
factors. It can be noticed that by increasing the cement
1 10 100 content from 1% to 2%, the mixture stiffness increased
only moderately. This is also confirmed by the values of
the equilibrium (static) modulus Ee and glassy modulus Eg
obtained from the sigmoidal regression parameters.
In particular, the Eg values (10,307 and 14,270 MPa for
M3B1C and M3B2C, respectively) are low if compared to
the Eg values of conventional HMA. This can be related to
the partial aggregate bonding produced by the emulsified
bitumen and by the lower density of the mixtures. The
modest stiffening effect produced by the increase in
cement dosage is consistent with the low degree of
hydration that was previously estimated for the M3B2C
mixture. In addition, the shape of the two master curves is
similar (Figure 13) which results in similar values of the
shape parameters b and g (Table 5). This suggests that
cementitious bonds between the coarse aggregates do not
appear to influence the stiffness behaviour probably
because cement hydration products were incorporated into
the fresh bituminous matrix.
The logarithm of temperature shift factors, plotted in
Figure 14 as a function of test temperature, were fitted
using the Arrhenius relation:
ð5Þ
 
1 1
log a20 ðTÞ ¼ C 2 ; ð6Þ
T TR

Table 5. Shape parameters of the stiffness modulus master curve after 28 days of curing (reference temperature: T0 ¼ 208C).

Mixture code Curing temperature (8C) d a b g R2

M3B1C 20 2.652 1.360 2 1.066 2 0.472 0.999
M3B2C 20 2.498 1.656 2 0.943 2 0.380 0.999
 878 F. Cardone et al.

2.0 (a) 30000

M3B1C: C = 10980 °K

Stiffness modulus (MPa)

M3B2C: C = 10100 °K
Eg = 10307

0.0
log a20

3000 5 °C
20 °C
–2.0 35 °C
1 1 50 °C
log a20(T) = C –
T TR 1 % cement
–4.0 300
0 10 20 30 40 50 60 0 5 10 15 20

Temperature (°C) Phase angle (degree)

(b) 30000
Figure 14. Temperature shift factors.
Eg = 14270

Stiffness modulus (MPa)

where C (K) is a material constant that is related to the
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thermal sensitivity of the bituminous binder and

3000 5 °C
temperatures (T, TR) are expressed in K. The calculated
20 °C
C values were 10,980 and 10,110 K for M3B1C and 35 °C
M3B2C mixtures, respectively. These values are analo- 50 °C
gous to the values obtained from HMA (Di Benedetto and 2 % cement
De la Roche 1998, Pellinen et al. 2002) indicating that the 300
thermal sensitivity of the tested mixtures is the same as 0 5 10 15 20
that of HMA. Phase angle (degree)

Viscoelastic response
The influence of temperature on the viscoelastic behaviour
of the tested CBTM was analysed in the Black space
(Figure 15). As can be observed, the values of E0 and w
measured at different temperatures do not form a unique
curve indicating that as regards E*, it is not possible to
superpose the effects of load frequency and temperature.
Because the application of TTSP was acceptable for E0,
the thermo-rheologically complex behaviour of E* is due
to the phase angle and therefore to the viscous component
of the material response.
The analysis of the Black space plots shows that at
higher frequencies the iso-thermal E* curves become
almost flat and parallel, indicating that frequency variation
has a limited effect on E0 in this range. A similar pattern
was observed on E* iso-thermal Black curves obtained on
Figure 15. Black curves for mixtures cured for 28 days at 208C:
(a) M3B1C mixtures and (b) M3B2C mixtures. Eg values
estimated using Equation (4).
suggests that at lower frequencies, the response of the
mixtures, particularly their viscous component, arises
mainly from the fresh binder, while the RAP behaves only
as a ‘black’ aggregate.
These phenomenological considerations are further
illustrated in Figure 17. In the high-frequency range, a
stiffness increase can be obtained by increasing frequency
(path F0 ) or reducing temperature (path T0 ); however, in the
3.0E+04
T = 10°C
T = 20°C
3C-00RA T = 30°C
⏐E*⏐[MPa]

cement-bound mixtures containing high percentages of

RAP and no fresh bitumen (Figure 16, from Grilli et al. 3C-50RA
2013a). The outlined behaviour suggests that the iso-
thermal viscoelastic response of CBTM at high frequen- 3C-80RA
cies is mainly related to the response of the aged binder
contained in the RAP. On the other hand, temperature 3.0E+03
0 2 4 6 8 10 12
variations highlight the effect of the fresh binder; in fact,
an increase in temperature results in lower glassy values ϕ [°]

(intercept at w ¼ 0) of the modulus.

Figure 16. Iso-thermal E* Black curves obtained from cement-
At lower frequencies, the measured E* values tend to bound mixtures containing 3% cement: without RAP (3C-00RA);
overlap forming a unique envelope curve: the effect of 50% RAP (3C-50RA) and 80% RAP (3C-80RA) (from Grilli
temperature and frequency can be superposed. This et al. 2013a).
 International Journal of Pavement Engineering
T'
Stiffness modulus
F'
F'' ≡ T''
Effect of loading temperature
Effect of loading frequency
Phase angle
Figure 17. Analysis of E* Black curves for the studied
mixtures: increase in loading frequency (F0 and F00 ); increase in
temperature (T0 and T00 ).
Downloaded by [Mr Pusjatan Bandung] at 02:35 27 August 2015
second case, the reduction in the phase angle is smaller as
it is only due to the fresh binder. In the low-frequency
range, an increase in frequency (path F00 ) or a decrease in
temperature (path T00 ) has a similar quantitative effect
which indicates that the fresh binder controls the
viscoelastic response.
Conclusion
In the present study, the curing process of CBTM was
investigated by measuring moisture loss and complex
modulus, considering the influence of cement dosage and
curing temperature. In addition, the influence of tempera-
ture on the complex modulus of 28-day cured mixtures was
evaluated. Tests were carried out on laboratory compacted
specimens, considering a dosage of 3% of bituminous
emulsion and two cement dosages (1 –2%).
As regards moisture loss, the following conclusions
can be drawn:
. The moisture loss rate by evaporation increased
with an increase in curing temperature; in particular,
specimens cured at 208C reached a WEQ within
14 days, while specimens cured at 408C required
less than 7 days.
. Raising the cement dosage from 1% to 2% reduced
WEQ; for the M3B1C mixture, the WEQ value
suggests that complete cement hydration was
reached, whereas for the M3B2C mixture moisture
loss by evaporation stopped the hydration process at
about one-half of its potential.
As regards the curing effects on complex modulus E*,
the following conclusions can be drawn:
. The increase in stiffness modulus E0 due to curing
was mainly related to moisture loss and higher
temperature which accelerated the curing process.
879
. The quantitative effects of curing time and loading
frequency on E0 can be superposed, and a unique
master curve was obtained by selecting a reference
curing time and shifting the iso-curing values
parallel to the frequency axis (curing-reduced
frequency); a four-parameter sigmoidal function
was able to model the curing master curves at the
reference curing time of 28 days.
. The curing shift factors ac,R can be considered a
measure of the curing level; in particular, ac,R values
clearly highlight the role of moisture loss and
cement hydration in the curing level.
. When plotted on the Black diagram, the E* values
measured at different curing times do not form a
unique curve because of the viscous component (w)
of the material response; in particular, while test
frequency affects the response of both the aged
binder from RAP and the fresh binder from
emulsion, the curing process (moisture loss and
cement hydration) only affects the properties of the
fresh binder.
As regards the effects of temperature on E*, the
following conclusions can be drawn:
. Similar to HMA, CBTM exhibited a viscoelastic
and thermo-dependent response; the TTSP was
applied to obtain a master curve for the stiffness
modulus E0, and the temperature dependence of the
shift factors was analogous to that of HMA.
. The cement content had a moderate effect on
stiffness and on the temperature shift factors
confirming that the amount of cement hydration
products was very similar because of moisture loss
by evaporation.
. When plotted on the Black diagram, the E* values
suggest that at higher frequencies, the iso-thermal
viscoelastic response is mainly affected by the aged
binder, while at lower frequencies, the response of
the mixtures, in particular their viscous component,
arises mainly from the fresh binder, whereas the
RAP behaves only as a ‘black’ aggregate.
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