Mech Time-Depend Mater

DOI 10.1007/s11043-016-9300-5
O R I G I N A L A RT I C L E

Black curves and creep behaviour of crumb rubber

modified binders containing warm mix asphalt additives

Juan Gallego1 · Ana María Rodríguez-Alloza2 ·

Felice Giuliani3

Received: 25 February 2016 / Accepted: 3 March 2016

© Springer Science+Business Media Dordrecht 2016

Abstract Warm mix asphalt (WMA) is a new research topic in the field of road pavement
materials. This technology allows lower energy consumption and greenhouse gas (GHG)
emissions by reducing compaction and placement temperatures of the asphalt mixtures.
However, this technology is still under study, and the influence of the WMA additives has yet
to be investigated thoroughly and clearly identified, especially in the case of crumb rubber
modified (CRM) binders.
In order to study the effect that different types and quantities of organic waxes have on
the high and intermediate temperature properties of 15 % and 20 % CRM binders, a dynamic
shear rheometer (DSR) was used. Using Black diagrams, the rheological behaviour of the
binders for the defined range of test temperature and frequency are summarised in a single
diagram. In this way, a preliminary evaluation of the rheological behaviour in the extended
domain of time and temperature can be attained as well as the effectiveness of the time–
temperature superposition principle (TTSP) on the materials under study. Creep tests were
also performed in order to evaluate the differences regarding mechanical response due to the
addition of rubber and WMA additives, and particularly the ability to recover the strain at
high temperatures.
The results of this study reveal that these binders do not conform to the Time Temperature
Superposition Principle (TTSP) and their rheological behaviour is strongly affected by the
interaction of waxes and bituminous matrix and thus generally exhibited a higher elasticity
compared to the corresponding control binder. The creep test results carried out proved
the enhancement of elasticity and the resistance to permanent deformation produced by the
addition of waxes. The WMA additives significantly lower the maximum deformation when
compared to the control binders and slightly increased their elastic recovery.

B J. Gallego
juan.gallego@upm.es
1 Department of Civil Engineering: Transport, Technical University of Madrid (UPM), C/ Profesor
Aranguren 3, 28040 Madrid, Spain
2 Department of Civil Engineering: Construction, Infrastructure and Transport, Technical University
of Madrid (UPM), C/ Alfonso XII 3, 28014 Madrid, Spain
3 Department of Civil and Environmental Engineering and Architecture, University of Parma, Parco
Area delle Scienze, 181/A, 43124 Parma, Italy
 Mech Time-Depend Mater

Keywords Road materials · Pavement · Crumb rubber · Warm mix asphalt · Additive ·
Dynamic shear rheometer (DSR) · Phase angle · Black curves · Creep tests

1 Introduction

Although hot mix asphalt (HMA) pavements containing crumb-rubber modified (CRM)
binders offer an improved resistance to rutting, fatigue and thermal cracking and other ben-
efits (Huang et al. 2002; Shen et al. 2005), these mixtures present one major drawback: the
manufacturing temperature is higher compared to conventional asphalt mixtures and, there-
fore, greater amounts of greenhouse gas (GHG) emissions are produced. Warm mix asphalt
(WMA) technology offers a solution to this drawback thanks to the use of additives which
are able to guarantee lower viscosity of bitumen at mix production temperatures and, there-
fore, the energy consumption and the GHG emissions can be reduced (Hurley and Prowell
2005). Hence, asphalt mixtures containing CRM binders and also those with a higher con-
tent of rubber, denominated asphalt rubber (AR) mixtures with WMA additives might be an
excellent, environmentally-friendly material for road construction.
The influence of organic additives on CRM binders has not been identified in great detail
(Rodríguez-Alloza et al. 2013, 2014) although some studies have been carried out on organic
additives in bitumen focused on the crystallisation properties (Lu et al. 2005; Redelius et al.
2002), the determination of the wax content (Edward and Isacsson 2005; Lu et al. 2008), the
chemical structure (Lu and Redelius 2006; Rossi et al. 2013), and their influence on bitumen
and asphalt performance (Chambrion et al. 1996; Cowley and Fisher 2002; Edwards and
Redelius 2003; Petersson et al. 2008; Polacco et al. 2012).
The physical properties of bitumen can be measured characterising the rheological be-
haviour of the material. The stiffness of bitumen is time dependent and the rheology of
bitumen is defined by its stress–strain–time–temperature response.
Frequently, the basic rheological characteristics of bitumen in road pavement design have
been characterised performing different empirical tests like the softening point which has
been used to predict the high temperature performance and permanent deformation prop-
erties. The test used to predict low temperature behaviour was the Fraass breaking point
and ductility test which provides information about the cohesive properties. The penetration
and softening point tests are almost completely empirical and therefore do not characterise
the viscoelastic behaviour of bitumen. Viscosity tests do not yet provide information on the
time dependence of bitumen. These tests are therefore unable to describe the viscoelastic
properties needed for a complete rheological characterisation.
Modified binders cannot be accurately characterised by these conventional tests as the
modification considerably alters the rheological properties. This in turn has led to rheolog-
ical properties of bitumen to be determined using a dynamic shear rheometer (DSR). The
data provided from this test may be presented in different forms including isothermal and
isochronal plots which are rheological parameters versus loading time at specific tempera-
tures and versus temperature at specific loading times.
Master curves present the interrelationship between temperature and frequency, and the
principle used to produce this curve and relate the equivalency between time and tempera-
ture is the time–temperature superposition principle (TTSP). When bitumen exhibits a sim-
ple rheological behaviour, it is said to be “thermo-rheologically simple” and this occurs
with conventional unmodified bitumen. However, this thermo-rheological simplicity is not
encountered in the case of modified bitumen.
Mech Time-Depend Mater

In this study, Black diagrams are presented as they do not require manipulation of the
rheological data and they provide a quick and robust method. A Black diagram is a graph
of the magnitude of the complex modulus (G∗ ) versus the phase angle (δ) obtained with a
dynamic test. In these diagrams the frequency and the temperature are eliminated from the
plot, allowing the dynamic data to be presented in a unique plot without the need to perform
TTSP manipulations. A smooth curve in a Black diagram is an indicator of time–temperature
equivalency. A disjointed curve indicates a breakdown of TTSP and the presence of either
a high wax content bitumen, a highly asphaltene structured bitumen or a highly polymer
modified bitumen (Lesueur et al. 1996; Planche et al. 2002).
Creep tests were also performed to complete the rheological description of the materials.
These tests can be static or repeated for a fixed number of cycles in order to evaluate the
resistance to non-reversible deformation and the existence of elastic recovery properties of
asphalts under traffic conditions. These tests were carried out to evaluate the differences
in the mechanical response due to the addition of rubber and WMA additives, especially
regarding the ability to recover the strain at high temperatures. The static methodology with
reduced application time was considered to be the most adequate. Static tests involve the
imposition of a step change in stress and the observation of the subsequent development in
time of the strain; the stress level applied is constant and can be also increased for successive
tests.
The increasing shear stress enables the evaluation of the binders mechanical behaviour
and their comparison; the resistance to non-reversible deformation is identified as the binders
ability to contrast the propagation of the viscous flow and their behaviour can then be de-
scribed by separating the delayed elastic phenomena from the effective residual deformation
(Giuliani and Merusi 2010). When the material shows a completely Newtonian behaviour,
there is no elastic recovery. With the addition of modifiers, the elastic properties can be
improved and the delayed elastic component becomes more relevant. This depends on the
capacity of the binders to store and release energy when a load is applied and then removed,
which determines the consequent binders ability to recover from the strain developed during
the creep phase. On the basis of this concept, the discrimination between what is actually
lost and what is storage and recoverable (in a deferred time) is a consequence of the ac-
cumulation of non-reversible deformation and of the distribution of the delayed elastic and
essential viscous components in binders mechanical response.
Consequently, the topic of this article is the evaluation of the mechanical behaviour of
CRM binders containing WMA additives. The addition of the WMA additives is indeed
potentially beneficial for lowering manufacturing temperatures of CRM binders. As a result,
it is necessary not only to control the rheological variations of these types of binders and
avoid compromising the asphalt mixtures workability but also to identify the elastic response
and resistance to permanent deformations in order to obtain the best pavement design.

2 Materials and test program

The following sections describe the materials used throughout the whole investigation.

2.1 Virgin binder

The virgin binder used in this study is a 50/70 penetration grade bitumen. It is widely used
to produce asphalt mixtures at conventional temperatures. Table 1 summarizes the basic
 Mech Time-Depend Mater

Table 1 Characteristics of the

50/70 virgin binder Properties Unit Test results

Penetration (25 °C) 0.1 mm 55.4

Softening point °C 51.1

Composition Unit Test results

Asphaltenes (%) 13.8

Saturates (%) 9.7
Naphthene-aromatic (%) 48.5
Aromatic-polar (%) 28.0

Table 2 Gradation of crumb

rubber Sieve (mm) (UNE 933-2) Accumulated (%)

2.0 100
1.5 100
1.0 100
0.50 94.1
0.250 23.7
0.125 3.7
0.063 0.4

Table 3 Thermogravimetric
analysis of crumb rubber TGA Rubber

Plasticizer + additives (%) 4.67

Polymer (rubber) (%) 57.41
Carbon black (%) 32.22
Ash (%) 6.02

specifications of the virgin binder. The penetration grade was assessed according to UNE-
EN 1426 (Bitumen and bituminous binders—Determination of needle penetration) while the
Softening Point was measured according to UNE-EN 1427:2007 (Bitumen and bituminous
binders—Determination of the softening point—Ring and ball method). The bitumen was
also subjected to a fractionation analysis as specified in the NLT 373/94 standard.

2.2 Crumb rubber modifier

The crumb rubber modifier was manufactured by mechanical grinding at ambient tempera-
ture (50 % from truck tyres and 50 % from car tyres) and to ensure consistency, only one
batch of crumb rubber was used in this study. The gradation of the crumb rubber is provided
in Table 2 and the thermo-gravimetric analysis in Table 3, both provided by the supplier.

2.3 WMA additives

The WMA technologies can be classified in three groups: organic additives, chemical addi-
tives and foaming processes. In this study, only one organic additive was chosen in order to
Mech Time-Depend Mater

Table 4 Binders name and their

composition Binder name Bitumen/Rubber (%) Additive (%) Additive name

B 100/0 0 –

B15 85/15 0 –
B15 + 2S 85/15 2 Sasobit
B15 + 4S 85/15 4 Sasobit
B15 + 2L 85/15 2 Licomont BS 100
B15 + 4L 85/15 4 Licomont BS 100

B20 80/20 0 –
B20 + 2S 80/20 2 Sasobit
B20 + 4S 80/20 4 Sasobit
B20 + 2L 80/20 2 Licomont BS 100
B20 + 4L 80/20 4 Licomont BS 100

undertake a thorough research on this specific technology and thus evaluate the performance
of the different existing additives as well as carrying out a comparative study.
The WMA additives used in this study were Sasobit® and Licomont BS 100® . Sasobit®
is a Fischer–Tropsch (F-T) wax which is produced by treating hot coal with steam in the
presence of a catalyst. It is a long-chain aliphatic hydrocarbon wax with the melting range
between 85 °C and 115 °C, high viscosity at lower temperatures and low viscosity at higher
temperatures. Licomont BS 100® is a fatty acid amide manufactured synthetically by re-
acting amines with fatty acids which melts between 141 °C and 146 °C (D’Angelo et al.
2008).
The study of the binders included a rheological characterisation at high and intermediate
temperatures. 15 % and 20 % weight of rubber was added to the 50/70 net bitumen in order
to obtain the CRM binders. The dosage rates of the WMA additives referred to the bitumen
weight were 2 % and 4 %. All the binders and the names referred to hereafter are listed in
Table 4.
The binders labelled B, B15 and B20 will be referred to as control binders as they do not
contain WMA additives.

2.4 Preparation of CRM binders containing WMA additives

An oil bath with a maximum temperature of 225 °C, a mixer with a maximum velocity of
15,000 rpm, fitted with a propeller agitator and a one-litre metal container for mixing was
used for the preparation of the binders. The oil bath has a temperature probe which can be
introduced into the mixing receptacle, allowing the temperature of the binder to be controlled
with a precision of ± 1 °C. A bitumen sample of 750 g was heated at 140 °C and then
placed in the oil bath. WMA additives were carefully added to the bitumen and the blends
were subsequently mixed for 15 minutes at 4000 rpm, ensuring that the additive was properly
incorporated into the binder. The blend was then heated to 185 °C, and the crumb rubber was
added. The mixture was blended for 30 minutes at 2000 rpm then for another 30 minutes at
900 rpm at a constant temperature of 185 °C. Reheating and homogenisation were carefully
carried out at a controlled temperature in order to obtain reproducible results (Anderson
et al. 2000). Special attention was then paid to the thermal history and storage conditions
of the test samples before testing (1 h at 25 °C ± 0.5 °C) because of their influence on
rheological measurements (Soenen et al. 2006).
 Mech Time-Depend Mater

Table 5 Temperature shear

stress couple Test T a (°C) Shear stress (Pa)

−10 40,000
0 20,000
10 10,000
20 5000
30 2000
40 1000
50 500
60 200
70 100
80 50

2.5 Rheological tests

Frequency sweeps performed at different temperatures provide information about the trend
of the complex modulus and the phase angle in function of frequency: they are dynamic
tests which consist in the application of a fixed shear stress at a constant temperature while
the angular frequency changes between 1 and 100 rad/s.
The shear stress applied depends on the test temperature and must belong to the linear
region for the analysed binder: in order to obtain significant results, shear stresses defined
in the literature for similar tests were assumed and confirmed by the results of stress sweep
tests. It was decided to establish the change from linear to non-linear region when the storage
modulus G decreases 5 % in relation to its initial value, according to SHRP Superpave. The
chosen test temperatures and shear stresses, listed in Table 5, were kept the same for all the
binders.
The frequency sweeps were completed from 1 to 10 Hz in the temperature range between
−10 °C and 80 °C at 10 °C intervals. The plate–plate configuration, 25 mm diameter and
2 mm gap sample geometry was used.
The frequency sweeps were carried out inside the linear viscoelastic region of the studied
asphalts. The change of the plate’s geometry, from 8 mm diameter to 25 mm diameter, was
completed between 20 °C and 30 °C, as recommended in the literature, in order to obtain
results which best fit the real trend (CEN 2006) limiting the measurement error of the sensor
due to the influence of the torsional stiffness of the sample at low temperatures.
Regarding the creep tests, the strain curves obtained for different materials at different
stress levels are not comparable in the same diagram because they depend on the shear stress
applied, and the comparison is therefore only valid for the same shear stress value. The tests
methodology is divided in two phases: a first phase where the shear stress is applied on
the specimen for a time period of 10 seconds and a second phase where the shear stress is
removed but the strain is still recorded for the next 30 seconds, in order to evaluate the elastic
recovery of the binders. The tests are carried out using the DSR in the stress-controlled
mode. Table 6 summarizes the test set.
Tests were repeated at a temperature of 40 °C, which represent the current conditions of
exposure of a road pavement. The results obtained are described in the following sections.
Even though the tests were made at three different shear stresses (100, 1000 and 10,000 Pa),
it was decided to plot the results at 100 Pa exclusively and in one figure to simplify and
avoid repetitive results. All the rheometrical measurements were repeated three times for
each sample.
Mech Time-Depend Mater

Table 6 Creep test set

Phase Duration [s] Point of measure Measurement
numbers [−] point [s]

1 creep 10 20 0.5
2 recovery 30 60 0.5

Fig. 1 Black curves for different control binders

3 Results and discussion

3.1 Black curves

All the frequency sweep tests and related Black curves showed in the paper are representa-
tive of three independent experiments that offered the same results.
Figure 1 demonstrates that with higher rubber content, the Black curves lose their smooth
trends. In fact, it can be observed that there are “waves” and discontinuities in the diagrams
for B15 and B20. As previously explained, this is associated with the changes in the mi-
crostructures within the binders.
The CRM binders show an inflection, which indicates the changes in the behaviour
closely due to the presence of crumb rubber. Although the values still remain continu-
ous with one another, based on the results shown, we should admit that the TTSP is not
respected. It may also be observed that, as the rubber content increases, the phase angle
becomes lower, attributing higher elasticity to the CRM binders and, at the same time, de-
formations become less time-dependent, highlighting a rubbery plateau.
Figures 2, 3 and 4 show the Black curves for binders with 15 % rubber. Figures 5, 6
and 7 show the Black curves for 20 % CRM binders, presenting the influence of each WMA
additive with increasing contents. At lower temperatures even modified binders present high
stiffness, and the behaviour tends to be similar to the bituminous binder.
 Mech Time-Depend Mater

Fig. 2 Black curves of B15 with Sasobit®

Fig. 3 Black curves of B15 with Licomont BS 100®

Binders with 15 % CRM and 20 % CRM, in particular, show a predominant solid-like be-
haviour due to the creation of an internal network between rubber particles and asphaltenes.
The rubber particles are indeed relevant in number, and when they swell by absorbing the
Mech Time-Depend Mater

Fig. 4 Black curves for different 15 % CRM binders

Fig. 5 Black curves of B20 with Sasobit®

aromatic oils and the light bitumen fraction, they interact with the asphaltenes giving a
rubbery behaviour to the blend.
Regarding both additives, it can be observed that as the content of wax increases, the
trend of Black curves does not change after the CRM modification, and they do not lose
 Mech Time-Depend Mater

Fig. 6 Black curves of B20 with Licomont BS 100®

Fig. 7 Black curves for different 20 % CRM binders

their smooth trends. The addition of the WMA additives also decreases the phase angle,
and so these binders exhibit a higher elasticity compared to the control binders B15 and
B20. In the case of Sasobit® , the reduction of the phase angle at the high temperatures is
inferior.
Mech Time-Depend Mater

Fig. 8 Creep tests for different control binders at 40 °C

This behaviour can be explained by the different microcrystalline structure of organic

additives and the reduced melting range of amide groups with intervals between 120 °C
and 155 °C (Licomont BS 100® ) compared to paraffinic chains that have a melting range
detectable at 40 °C (Sasobit® ).
The presence of the wax enhances the highly structured blend matrix because it crys-
tallises and increases the cohesion between particles. It determines a shift from sol-type to
gel-type behaviour of the bituminous binders. The explanation of this behaviour should in-
clude not only the chemistry of the wax molecules but also the shape and dimension of the
crystals (Polacco et al. 2012).
At high temperatures, when the bituminous matrix becomes liquid, the wax crystals and
asphaltene are able to move and re-arrange, forming a better structured network. This con-
firms the solid-like behaviour observed in the Black diagrams, offering the marked shape of
Black curves especially when 4 % of Licomont BS 100® was added.
Sasobit® and Licomont BS 100® have different melting temperatures and different resid-
ual crystallinity after being mixed with the bitumen. This is directly reflected in the crystal
content and therefore in the rheological effects. However, we already observed that the in-
applicability of the TTSP is not necessarily due to the wax melting, but primarily related to
changes in the structures built by the solid phase inside the bituminous matrix.

3.2 Creep-recovery test at 40 °C

All the creep-recovery tests shown in the paper are representative of three independent ex-
periments that gave the same results.
Figure 8 shows the strain versus time diagram for the control binders when a 100 Pa
shear stress is applied at 40 °C.
In Table 7, the values of the final strain ratio (γr ), the maximum strain value (γmax ) and
the elastic recovery ratio (γr /γmax ) are presented for the control binders.
As may be observed, the addition of rubber to the base bitumen improves the elastic
component behaviour of the binders. The strain is much lower for the binders containing
rubber, and they show a more significant elastic recovery ratio. The difference between the
elastic recovery of the B15 and B20 is insignificant at this temperature. As for the base
 Mech Time-Depend Mater

Table 7 Elastic recovery ratios

for control binders at 40 °C Binder γr [%] γmax [%] γr /γmax [–]

B 7.4 8.1 0.91

B15 0.2 0.7 0.31
B20 0.1 0.3 0.33

Fig. 9 Creep tests for 15 % CRM binders with WMA additives at 40 °C

Table 8 Elastic recovery ratios

for 15 % CRM binders at 40 °C Binder γr [%] γmax [%] γr /γmax [–]

B15 0.2 0.7 0.31

B15 + 2S 0.2 0.5 0.31
B15 + 4S 0.0 0.2 0.24
B15 + 2L 0.2 0.5 0.37
B15 + 4L 0.1 0.3 0.26

bitumen, almost all the deformation energy is dissipated in internal friction or it is used to
deform the liquid matrix of the bitumen and mainly produces a non-reversible flow.
The diagram of strain as a function of time was also plotted for the CRM binders with the
selected WMA additives in order to evaluate the changes of the resistance to non-reversible
deformation due to the addition of waxes. In Fig. 9, the creep tests for 15 % CRM binders
can be observed, and in Table 8, their respective elastic recovery ratios are listed.
It may be noted that with the addition of the waxes, the maximum deformation becomes
lower compared to the control binder B15. With the addition of 4 % of any of the waxes, the
highest level of elastic recovery is achieved.
Figure 10 shows the diagrams of strain as a function of time for the 20 % CRM binders
with WMA additives, and Table 9 provides the summaries of the final and maximum strain
value as well as the elastic recovery ratios.
It can be observed that the addition of the waxes shifts the values towards zero and
increases the elastic component compared to the control binder B20. The addition of 4 %
Mech Time-Depend Mater

Fig. 10 Creep tests for 20 % CRM binders at 40 °C

Table 9 Elastic recovery ratios

for 20 % CRM binders at 40 °C Binder γr [%] γmax [%] γr /γmax [–]

B20 0.1 0.3 0.33

B20 + 2S 0.0 0.2 0.23
B20 + 4S 0.0 0.1 0.28
B20 + 2L 0.1 0.2 0.21
B20 + 4L 0.1 0.2 0.31

Sasobit® provides a higher elastic recovery compared to the binder with 4 % Licomont BS
100® (Table 9). In terms of maximum strain ratio, the binder with 4 % Licomont BS 100®
presents the lowest value.

4 Conclusions

A dynamic shear rheometer (DSR) was used to investigate the effect of different types and
quantities of WMA additives on the high and intermediate temperature properties of 15 %
and 20 % CRM binders.
A preliminary evaluation of the rheological behaviour in the extended domain of time
and temperature was attained with the Black diagrams as the rheological behaviour of the
binders for the defined range of test temperature and frequency were summarised in a single
diagram. Creep-recovery tests were also performed in order to evaluate the differences of the
mechanical response due to the addition of rubber and WMA additives, especially regarding
the ability to recover the strain at high temperatures.
From these test results, the following conclusions were drawn for the binders created:
Black curves did not show the standard smooth trend, and the presence of rubber and
wax caused the formation of inflections and disjoint features. This is in line with the fact
that these binders to not conform the Time Temperature Superposition Principle TTSP. The
 Mech Time-Depend Mater

inapplicability of the TTSP is not necessarily due to the wax melting, but is mainly related
to changes in the structures built by the solid phase inside the bituminous matrix.
The creep test results carried out to determine the recovery from a creep loading, con-
firmed once more the improvement of the elasticity and the resistance to permanent defor-
mation produced by the addition of the waxes.
With the increased content of rubber, the deformations are lower; this implies that the
CRM binders are less deformable and have a better resistance to non-reversible deforma-
tions. The presence of the rubber particles in the binder leads to stronger elastic properties
and shifted the liquid-like behaviour of the base bitumen towards a more predominant solid-
like behaviour. The WMA additives significantly lowered the maximum deformation and
increased the elastic recovery when compared to the control binders and will have a signifi-
cant improvement regarding resistance to permanent deformations in road pavements.

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