Chinese Society of Pavement Engineering

International Journal of
Pavement Research and Technology
Journal homepage: www.springer.com/42947

Rheological investigation of asphalt binder modified with nanosilica

Faheem Sadiq Bhat, Mohammad Shafi Mir
Dept. of Civil Engineering National Institute of Technology, Srinagar J&K, India

Received 24 December 2019; received in revised form 1 July 2020; accepted 7 August 2020

Abstract

The study investigates the use of nanosilica as a potential binder modifier. Nanosilica can be produced from rice husk and silica fumes and therefore is
a cost-effective and environment-friendly modifier. Different percentages of nanosilica (0%, 0.5%, 1% and 3% by weight of asphalt binder) were added to
VG-10 binder in a high-speed mixer. The influence of temperature, strain rate and frequency on viscosity was evaluated. Different rheological tests like
time-temperature sweeps, Superpave rutting parameter (G*/sinδ), Multiple Stress Creep and Recovery (MSCR) Test, Creep tests, and Zero shear viscosity
(ZSV) tests were performed on base asphalt binder and nanosilica modified asphalt binders. The addition of nanosilica enhanced the rutting potential of the
asphalt binder. Fatigue evaluation using Linear Amplitude Sweep test showed that incorporation of nanosilica arrests the micro crack nucleation and therefore
enhanced the fatigue performance of asphalt binder. Nanosilica particles act as a potential heating barrier and protect the host polymeric chains of the asphalt
binder, thus improving its aging resistance. Nanosilica modified binders also showed an enhanced self-healing capability.

Keywords: Nanosilica; Shear thinning behaviour; Superpave rutting parameter; MSCR; ZSV; Self-healing; Linear amplitude sweep

1. Introduction a resistance against thermo-oxidative aging [13]. Aging resistance

of CL-30B nanoclay modified binders measured by means of
The pavements experience diverse kinds of distresses; amongst rheological aging index showed that addition of CL-30B nanoclay
which high-temperature rutting, intermediate temperature fatigue enhances the aging resistance of the asphalt binders [14]. The
and low temperature cracking are the most important from the addition of nanoclay significantly enhances the storage stability of
design standpoint of flexible pavements. The type and extent of the polymer modified asphalt binders [15]. Improvement in aging
these distresses are influenced by loading, axle configurations, and storage stability of asphalt binders was enhanced after the
temperature variations, mixture parameters and rheological addition of nanosilica [16]. A significant improvement in the aging
properties of the asphalt binders. There arises a need to overcome resistance of the SBS modified asphalt binder was observed after
various distresses to make the pavements more durable. There the addition of carbon nanotubes [17]. Carbon nanotube modified
have been continuous efforts to make pavements more durable asphalt binders showed an improvement in aging resistance and
against different types of failures by using diverse kinds of asphalt storage stability [18].
modifiers [1-6]. Besides the conventional modifiers, the use of Adding nanosilica to asphalt binder had a positive effect on the
different nanomaterials like nanoclays, nanotubes, nano alumina, physical and rheological properties of the asphalt binder. The
as asphalt binder modifiers is being explored [7-11]. High specific available literature has mostly concentrated on evaluating the
surface area, high functional density, and high strain resistance rutting resistance of the nanosilica modified asphalt binders by
make nanomaterials viable alternatives for binder modification utilizing Superpave (G*/sinδ) rutting parameter. Previous research
[12]. The addition of nano-sized additives improves the based on Superpave rutting parameter(G*/sinδ), showed that the
performance of the asphalt binder and overcomes the drawbacks addition of nanosilica enhanced the rutting resistance asphalt
of the conventional polymers such as phase separation problems, binders. The addition of nanosilica improves the storage modulus
storage instability problems, low resistance to heat, oxidation and and elasticity of the asphalt binder, besides an improvement in
higher costs. Organo-montmorillonite (OMMT) modified asphalt aging resistance [19]. It makes the asphalt binder stiff and
binders showed higher improves temperature susceptibility as shown by decrease in
penetration and increase in softening point. An enhancement in the
PG grade of the asphalt binder is also observed after the addition
* Corresponding author of nanosilica [20]. Nanosilica improves the self-healing capacity
E-mail address: [email protected] (F. S. Bhat). of the asphalt binders and mixes, therefore making the pavements
Peer review under responsibility of Chinese Society of Pavement more durable and lasting [21]. An improvement in the elastic
Engineering. behaviour of the asphalt binder leading to an improvement in
ISSN: 1997-1400 DOI: https://doi.org/ 10.1007/s42947-020-0327-2
Chinese Society of Pavement Engineering. Production and hosting by Springer Nature
2 F. S. Bhat and M. S. Mir / International Journal of Pavement Research and Technology xx (2020) xxx-xxx

fatigue resistance, rutting resistance and creep performance of the temperature, strain rate and frequency on rheological properties of
asphalt binder has also been reported. Indirect tensile strength the nanosilica modified asphalt binders. Based on the literature
significantly increases after the addition of nanosilica [22]. The review, it was found that nanosilica has been utilized in the range
resilient modulus, split tensile strength and fatigue life of the of 1 to 6% for asphalt binder modification [52]. Studies have
asphalt mixes improved after introduction of nanosilica, it also shown that using nanosilica in higher concentrations can have an
improved the moisture susceptibility [23]. The addition of adverse effect on the intermediate and low temperature
nanosilica slows down the oxidative process and thereby improves performance of asphalt binders [53]. Therefore, in this study, 0%,
the aging resistance of asphalt binders. An improvement in high 0.5%, 1%, and 3% nanosilica, by the weight of asphalt binder has
and intermediate temperature performance was observed but the been used. The maximum concentration of nanosilica used in this
low temperature performance did not show an improvement [24]. study was 3%, the maximum concentration was chosen on the
Introduction of nanosilica improves the permanent deformation basis of the study conducted by Leiva-Villacorta and Vargas-
characteristics of the asphalt binder. An improvement in the Nordcbeck 2019 [54]. They, in their study, evaluated the
intermediate and low temperature performance has also been seen performance of nanosilica modified asphalt binders at low,
[25]. Nanosilica forms an inorganic network in the asphalt binder intermediate and high temperatures and concluded that 3% content
as was confirmed by X-ray diffractometry and Scanning Electron was the optimum percentage of nanosilica to be used for asphalt
Microscopy. This leads to the crack arrests and improves the binder modification.
fatigue performance of the nanosilica modified asphalt binders
[26]. 2. Objectives and scope of the study
Although G*/sinδ is widely used to assess the rutting
performance of the asphalt binders, but this parameter does not The primary objective of this study was to evaluate the effect of
account for the delayed elastic response shown by modified nanosilica on various physical and rheological characteristics of
binders. G*/sinδ does not show good correlation with the rutting the asphalt binder. The sub-objectives are enlisted below:
performance of mixtures. So advanced characterization methods 1. Evaluate the effect of nanosilica on the viscosity of the
such as Multiple stress creep and recovery (MSCR) test, Zero shear asphalt binder in different temperature domains and shear
viscosity (ZSV), and creep tests may also be utilized to investigate rates.
the rutting potential of nanosilica modified binders [27-33]. 2. Investigate the effect of adding nanosilica on different
Employing ZSV, MSCR and creep tests can help in better rheological properties by means of time and temperature
evaluation of the rutting potential of nanosilica modified binders. sweep tests.
Zero-shear viscosity is a theoretical concept and is defined as the 3. Estimate the rutting potential of the nanosilica modified
viscosity measured when shear rate is approaching zero. The ZSV binders using the Superpave rutting parameter G*/sinδ,
concept is based on the fact that the purely dissipative viscous MSCR and creep tests.
component is solely responsible for the nonrecoverable 4. Evaluate the fatigue resistance of the control and nanosilica
deformation. ZSV is an indicator of stiffness of the binder and modifiers utilizing Linear Amplitude sweep.
permanent deformation under long-term loading [34]. Rutting of 5. Assess the aging resistance potential of the nanosilica
the asphalt mixes has been identified as a non-linear viscoelastic modified binders by means of a rheological parameter.
phenomenon, and therefore the measurements for binder rutting 6. Investigate the self-healing potential of the nanosilica
parameter in linear viscoelastic region will not relate well with modified binder by means of ductility test.
asphalt mixture rutting. The Superpave rutting parameter failed to
capture the true performance characteristics of modified binders, 3. Materials and experimental methodology
therefore to overcome the inadequacies of the existing rutting
parameter Multiple stress creep and recovery test was proposed 3.1. Materials
[35-37]. Different studies have shown this method to be applicable
for both unmodified and modified asphalt binders [38-40]. MSCR
A soft grade binder of viscosity grade VG-10 was used in the
test relates very well with the rutting performance of asphalt mixes
study as the base binder. The basic properties of the base asphalt
evaluated from different rut tests [41-47]. Fatigue distress has been
binder are enlisted in Table 1. Nanosilica used in the study as
evaluated using different approaches. Linear Amplitude sweep
modifier was supplied by Platonic Nanotech private limited. The
(LAS) test has been found to be most effective approach in
basic properties and elemental composition of nanosilica are listed
evaluating the fatigue distress. LAS test uses viscoelastic
in Table 2 and Table 3.
continuum damage approach for fatigue characterization of asphalt
binders [48-51]. Table 1
The authors found very limited literature discussing MSCR, Basic properties of the base binder.
ZSV, creep tests and linear amplitude sweep test for rutting and
fatigue evaluation of nanosilica modified asphalt binders, and Properties Standard Values Specification
therefore it is necessary to evaluate the performance of nanosilica code limit (minimum)
modified asphalt binders using these approaches. The present Penetration 0.1mm at 25° IS: 1203 89 80
study will be a good addition to the existing repository of Softening point (°C) IS: 1205 48 40
information about performance of nanosilica modified asphalt Ductility at 25°C IS: 1208 100+ 75
binders. Dynamic viscosity IS: 1206 1063 800
The addition of nanosilica affects rheological properties and the (Part II)
flow behaviour of the asphalt binder, and therefore it is important Kinematic viscosity IS: 1206 282 250
to study the change in behaviour at different temperatures and (Part III)
shear rates. The present study aims to examine the influence of
 F. S. Bhat and M. S. Mir / International Journal of Pavement Research and Technology xx (2020) xxx-xxx 3

Table 2 Table 3
Physical properties of nanosilica. Elemental composition of nanosilica particles.
Specification Value SiO2 Al Fe Mg Ca
Purity 99.50% 99.5% 0.02% 0.05% 0.1% 0.08%
Average size of the particle 30-50 nm
Specific surface area 200-250 m2/g 4.2. Physical characterization of the binders
Bulk density 0.10 g/cm3
True Density 2.5 g/cm3 The basic properties of base binder and nanosilica modified
Morphology Porous binder were evaluated, including penetration (IS: 1203), softening
point (IS: 1205) and ductility (IS: 1208) [57].
3.2. Sample preparation
4.3. Rheological characterization of the binders
The main challenge in the preparation of nanosilica modified
binders is the proper dispersion of nanosilica particles in the 4.3.1. Temperature and strain sweep
asphalt binder. The high shear mixing technique is effective in
dispersing nanosilica particles in the asphalt binder. Initially, the To investigate the variation in viscosity of base and nanosilica
control asphalt binder was heated to a temperature of 150+5°C, modified asphalt binders with change in temperature, a
and then nanosilica was added to the base binder in different temperature sweep was carried out in the temperature range of 60-
concentrations (0, 0.5, 1 and 3% by weight of the base binder) in a 135°C. Anton Paar MCR 102 Dynamic Shear Rheometer (DSR)
high-speed mixer. The highest concentration of nanosilica chosen with a parallel plate geometry of 25 mm diameter and a 1 mm gap
in the study was 3% by weight of the asphalt binder. The highest was used.
concentration of nanosilica was limited to 3%, based on a previous Shear rate dependency allows the flow behavior of the asphalt
study conducted by Leiva-Villacorta and Vargas-Nordcbeck 2019 binder under varying strain rates to be better understood [58,59].
[54]. Small quantities of nanosilica were added to the asphalt A shear rate sweep in the range of 0.1 to 100 1/s was carried out to
binder over a time period of 15 minutes to prevent the understand the behaviour of unmodified and modified asphalt
agglomeration of nanosilica particles. The temperature during the binders. The sweep was carried out at temperatures of 60°C, 100°C,
mixing process was maintained at 150+5°C by using a thermostat. and 135°C.
The high-speed mixer was maintained at the maximum rotational 4.3.2. Frequency sweep
speed of 3500 rpm for 2 hours. Samples from high-speed mixer
were taken after every 15 minutes and complex modulus was Frequency sweep test is one of the most common method for
evaluated, complex modulus values increased as the mixing time evaluating the rheological characteristics of the asphalt binder. The
increased, however; no change in complex modulus values was test was conducted within the LVE range to measure the
observed after mixing for 2 hours, and hence 2-hour mixing time viscoelastic parameters at different temperatures and frequencies.
was selected for preparation of nanosilica modified binders. The frequency sweep was carried at 0.1% strain rate and in the
The mixing was carried out in presence of oxygen at high frequency range of 0.1-100 rad/sec. The temperature was increased
temperature that accelerates the aging process. This leads to the from 40°C to 76°C, with 6°C increment.
stiffening of the asphalt binder and affects the rheological The dependence of complex modulus and phase angle on
properties of the asphalt binder. In order to remove any bias in the temperature and frequency or loading time can be shown in the
measurement of rheological properties that may incur due to aging form of isochronal and isothermal plots respectively [60].
of modified binder, the base asphalt was mixed under the same Black diagrams provide a useful tool in analyzing rheological
conditions without nanosilica to obtain the same set of conditions data for the identification of possible discrepancies in experimental
for all the samples before testing. results. It verifies the time-temperature equivalency, and thermo-
rheological simplicity [61]. The Black diagram is a plot between
3.3. Aging of asphalt binders complex modulus G* and phase angle δ obtained from a dynamic
test. A black diagram is independent of temperature and frequency
The base asphalt and modified asphalt binders were made to and allows all the oscillatory data to be reported in a single graph.
undergo short-term aging by conditioning in a Thin Film Oven A smooth curve in a black diagram indicates time-temperature
(TFO) at 163°C for 5 hours as per ASTM: D 1754 [55]. Long term equivalency. A disjointed curve indicates the breakdown of time-
aging of the asphalt binders was carried out in a pressure aging temperature equivalency, thus indicating a high degree of
vessel. The pressure aging vessel was maintained at a temperature modification [62].
100°C and 2.1 MPa pressure for 20 hours as per ASTM:D 6521 4.3.3. Rutting resistance using Superpave rutting parameter
[56].
Rutting resistance of the base asphalt and nanosilica modified
4. Test methods asphalt was evaluated by means of Superpave rutting parameter as
per ASTM-D7175-15 [63]. This parameter is used to determine the
high-temperature failure of the asphalt binder. As per the
4.1. Scanning electronic microscope
Superpave specifications, a binder is considered to fail when the
value of G*/sinδ drops below 1 kPa for the unaged binder. This
The SEM analysis was conducted to investigate the morphology test was performed on unaged binders using a dynamic shear
of the nanosilica powder and nanosilica modified asphalt binder. rheometer with a parallel plate geometry. The plate diameter was
The SEM images were captured using HITACHI-3600 SEM 25 mm and 1 mm gap was used. The test was carried out at a
device.
4 F. S. Bhat and M. S. Mir / International Journal of Pavement Research and Technology xx (2020) xxx-xxx

frequency of 10 rad/sec in the temperature range of 52°C to 76°C where, C(t) is the integrity parameter, C0, C1, and C2 are the curve
with 6°C temperature bumps. fitting parameters. C at peak shear stress is used to calculate failure
point Df by using the relation
4.3.4. Multiple stress creep and recovery
The MSCR test was performed on TFO-aged samples as per D = (5)
ASTM-D7405-15 [64]. The two parameters obtained from the
MSCR test are the average non-recoverable creep compliance (Jnr) Number of load cycles to failure Nf is calculated by using the
and the average percentage recovery. The test was done at standard equation,
stress levels of 0.1 kPa and 3.2 kPa. Non-recoverable creep
compliance is defined as the ratio between non-recoverable shear N = A(γ ) (6)
strain and shear stress applied during the loading cycle. Jnr is
capable to characterize stress dependence of modified binders as where, A and B are regression coefficients and
well as unmodified asphalt binders. The two parameters are ( )
specified in Eqs. 1 and 2 respectively. =( ;
( ) )×( )
B =2α
( ) =∑ (1)
= maximumst rainl evel
where, Jnr denotes non- recoverable creep compliance (1/kPa),
= residual strain at the end of the loading cycle; σ = Standard 4.4. Effect of nanosilica on ageing resistance
stress level of 0.1 kPa and 3.2 kPa.
Aging refers to the oxidative aging of the asphalt binders.
( )=∑ × 100 (2) Binders experience oxidation during the mixing and laying stage
and also during their service life. During this process of aging,
where, and denote strain at the end of the loading and some of the lighter and volatile components of the binder
recovery cycle, respectively. evaporate, making the binder brittle which can lead to pavement
deterioration. Therefore, binders with a lower degree of oxidation
4.3.5. Creep Test are sought after. The present study evaluates the aging resistance
of the unmodified and modified binders by means of rheological
Creep refers to the increase in deformation over time under
aging indices [66]. The aging index is given in Eq. 7.
sustained stress. The behavior of unmodified and modified asphalt
binders under sustained loading has been evaluated in this study. Ruttinga gingin dex = × 100 (7)
The stress of 100 Pa was applied for a loading period of 10 minutes
and the resulting strain at the end of loading period was measured.
The stress level in this study is same as used in the study conducted 4.5. Self-healing potential of nanosilica modified binder
by Anwar Parvez et al. 2014 [65] and also 100 Pa stress level is a
standard loading level for MSCR test [64]. The Self-healing phenomenon takes place at the molecular level
and is mainly affected by the Van der Waals forces and hydrogen
4.3.6. Linear Amplitude Sweep bonding molecules. Different types of additives can be added to
The fatigue evaluation of the control and nanosilica modified the asphalt binder to enhance the self-healing capacity of the
asphalt binders have been evaluated by utilizing LAS test as per asphalt binders. These materials include Ionomers, nanoparticles,
AASHTO TP 101. The test was performed at 25°C on a DSR with and super molecular rubber [67]. The self-healing phenomenon
an 8mm assembly and a gap of 2mm. LAS test consists of two takes place at the molecular levels, i.e. at the nano level. Therefore,
steps, in the first step, a frequency sweep test is conducted with modification of asphalt binder at the nano-level can help to
frequency varied from 0.2 to 30 Hz at 0.1% strain rate. The second improve the self-healing potential of the asphalt binders. In this
step consists of performing an amplitude sweep 0.1-30% at 10 Hz study, the self-healing potential of the nanosilica modified asphalt
frequency. The data from the frequency sweep test is used in the binders was evaluated by using a special ductility test. The
estimation of undamaged parameter α and consequently parameter methodology used to carry out the test was as given by Qui et al.
B. Amplitude sweep data is used to obtain the asphalt binders 2009 [67]. The ductility samples of nanosilica modified asphalt
damage property which can be written as, binders were prepared and then cut in the middle by using a sharp
knife. After cutting the samples, the specimens were placed on a
( ) ∑ [ ( )] ( ) (3) glass plate in a proper orientation. A small force was applied at the
ends of the briquettes for about 10 seconds. It was ensured that the
where, D(t) is the damage accumulation in the specimen; Ci = ratio two cut surfaces of the asphalt binder are properly in contact with
of complex modulus at any time (t) to the initial complex modulus each other. Finally, the samples were allowed to self-heal at room
= G*(t)/G* (initial); γo = applied strain level (%); α= inverse of the temperature for a period of 4 hours. After 4 hours of healing, self-
slope of the line plotted between log of storage modulus and log of healed nanosilica modified samples and base asphalt samples were
applied frequency. placed in a ductility machine, with the water bath maintained at a
The relationship between C(t) and D(t) is fitted using the power temperature of 5°C. The ductility test was performed at a
law: displacement rate of 5 cm/min. The healing percentage is
calculated as follows:
= ( )
% × 100 (8)
C(t) = C0 - C1 (D)C2 (4)
 F. S. Bhat and M. S. Mir / International Journal of Pavement Research and Technology xx (2020) xxx-xxx 5

where, % = self-healing percentage in ductility test; Table 4

% = length of the healed sample when it breaks; % Physical properties of nanosilica modified asphalt binder.
= length of the original ductility samples when it breaks; SiO2 Penetration Softening Ductility Penetration
concentration point index
5. Results and discussions (%) (mm) (°C) (mm)
0 92 52 >100 0.94
5.1. SEM analysis 0.5 78 60 86.4 2.22
1 61 66 71.2 2.55
Figs. 1 and 2 show SEM images of nanosilica and 3% nanosilica 3 54 72 68.3 3.33
modified asphalt binder. As is evident from Fig. 1, nanosilica
particles tend to agglomerate and form bundles of nanosilica PI = (9)
particles. In Fig. 2, no agglomeration of nanosilica particles can be
seen and thus the mixing technique used was successful in
5.3. Temperature and strain sweep
dispersing the nanosilica particles in the asphalt binder.
5.3.1. Temperature dependence of viscosity
5.2. Conventional binder tests
Viscosity is dependent on the force of cohesion. With an increase
As shown in Table 4, there is a decrease in the penetration of in temperature, the cohesive force decreases and hence the binder
asphalt binder with the addition of the nanosilica. The decrease in viscosity also decreases. Fig. 3 shows the effect of change in
penetration indicates the stiffening effect of the asphalt binder, and temperature on the viscosity of the unmodified and nanosilica
the stiffening increases with an increase in nanosilica modified asphalt binders. The results show a consistent increase in
concentration. The Softening point can be used as an indicator of the viscosity with an increase in the nanosilica content. The
temperature susceptibility of the asphalt binder. The addition of viscosity decreases with an increase in temperature for unmodified
nanosilica increased the softening point of the asphalt binder, as well as modified binders.
indicating an improvement in its temperature susceptibility.
5.3.2. Shear rate dependence
Ductility is a measure of elasticity of the asphalt binder. Ductility
test result values showed a decreasing trend after the addition of Asphalt binder is subjected to varying strain levels in bituminous
nanosilica. The stiffening effect of the nanosilica leads to a mix preparation and compaction stages. So, it becomes imperative
decrease in the ductility. The high specific surface area of the to investigate the effect of varying strain rates on the binder. Figs.
nanosilica enhances the interaction with the asphalt. 4, 5 and 6 show the effect of varying strain rates on the viscosity
Higher Penetration index indicates lower temperature of the binder at temperatures of 60°C, 100°C and 135°C. At 60°C,
susceptibility of the asphalt binder. Penetration index was the base binder shows Newtonian behavior up to a strain level of
calculated using Eq. (9) [68]. 10 1/s. The viscosity then starts to decrease with an increase in
strain rate indicating a shift towards non-Newtonian behaviour. As
the dosage of nanosilica is increased, the shear rate dependency
increases and the binder behaves as Newtonian fluid for a narrower
shear rate region. At 100°C, base binder and 0.5% nanosilica
modified binder show Newtonian behavior. 1% nanosilica
modified binder shows Newtonian behaviour up to a shear rate of
≈ 90 1/s, and 3% nanosilica modified binder showed Newtonian
behavior for a narrower strain region of ≈10 1/s. At 135°C, the
change in strain rate doesn’t affect the viscosity and thus the
unmodified and nanosilica modified binders show Newtonian
behaviour at this temperature.

0%
0.5%
Fig. 1. SEM images of nanosilica. 1%
3%
1000

100
Viscosity (Pa.s)

10

0.1
60 80 100 120 140 160
Tempearture (°C)

Fig. 2. SEM image of 3% nanosilica modified binder. Fig. 3. Temperature dependence of viscosity.
6 F. S. Bhat and M. S. Mir / International Journal of Pavement Research and Technology xx (2020) xxx-xxx
0%
0.5%
Table 5
10000
1%
3%
Carreau model parameters.
Binder (Pa.s) ∞ (Pa.s) γ (s-1) s
1000 Base 257.83 0 16.63 0.71
0.5% Nanosilica 1319.55 8.29 2.50 0.55
Viscosity (Pa.s)

1% Nanosilica 4169.73 20.65 1.45 0.66

100
3% Nanosilica 17146.74 40.68 0.34 0.57

0%
10 0% modelled
0.5%
0.5% modelled
1%
1% modelled
10000 3%
3% modelled
1
0.1 1 10 100
Strain Rate (1/s)
1000
Fig. 4. Strain rate sweep at 60°C.

Viscosity (Pa.s)
0%
0.5% 100
1%
3%

10
Viscosity (Pa.s)

10 1
0.1 1 10 100
Strain Rate (1/s)

Fig. 7. Model fitted curves.

∞
1
0.1 1 10 100
= ∞
+ (10)
Strain Rate (1/s)

Fig. 5. Strain rate sweep at 100°C. where, η∞ is infinite shear viscosity, η0 is zero shear viscosity, s is
the parameter related to the slope of the shear-thinning region and
0%
0.5% is the critical shear rate for the onset of shear thinning. The
10 1%
3% different carreau model parameters have been shown in Table 5.
In this model, a zero shear Newtonian plateau was assumed at the
beginning up until the critical shear rate is reached when the
shear thinning behaviour starts. With the increase of the shear rate,
Viscosity (Pa.s)

the viscosity gradually reached an infinite-shear Newtonian

1 plateau. The addition of nanosilica to the control binder caused a
significant increase in zero shear viscosity. A higher value of zero
shear viscosity at high temperature implies the fluidic nature of the
asphalt that would lead to a better coating of aggregates by asphalt
binder. The shear-thinning occurs due to the alignment of the
0.1
asphalt particles in the direction of the applied stress, which leads
0.1 1 10 100 to a decrease in the viscosity.
Strain Rate (1/s)

Fig. 6. Strain rate sweep at 135°C. 5.4. Time and temperature sweep tests

The shear-thinning behaviour of the nanosilica modified asphalt 5.4.1. Isochronal plot
binders can be modelled by using Carreau’s model, as shown in Eq. The Isochronal plot of complex modulus (G*) and phase angle
(10) [69-71]. Carreau’s model overcomes the drawbacks of power- at a frequency of 10 rad/sec is shown in Fig.8. The addition of
law model in very low and high shear rate regions. In Carreau’s nanosilica to the asphalt binder increases the complex modulus of
model, viscosity depends upon the shear rate. Carreau’s viscosity the binder. This increase can be observed in the entire temperature
model is useful in describing the flow behaviour of fluids in high domain. The establishment of the plateau region in the isochronal
shear rate region. This model is capable of describing both the plot suggests the high degree of modification that the binder has
shear thinning and shear thickening phenomenon. Carreau undergone [73]. The Phase angle of the binder increases with an
presented the rheological equations from molecular network increase in temperature and the nanosilica modified binders show
theories [72]. As can be seen from Fig.7, the model was found to lower phase angles as compared to the base binder. As the
have a good fit with the obtained results (with R2 equal to 0.9851, concentration of nanosilica increases, a significant decrease in the
0.9962, 0.9784 and 0.9682 for 0, 0.5, 1 and 3% respectively). phase angle is observed at lower as well as at higher temperatures.
 F. S. Bhat and M. S. Mir / International Journal of Pavement Research and Technology xx (2020) xxx-xxx 7
G* (0%)
G* (0.5%)
G* (1%)
improving the rutting resistance of the binders. This increase is
100
G* (3%)
δ (0%)
δ (0.5%)
more significant at higher frequencies and a plateau is formed
90 δ (1%)
δ (3%)
when the frequency is decreased. The phase angle of nanosilica
80 modified binders shows a decrease at low and high frequencies,
Complex Modulus G* (kPa)

80
implying that the modified binders are more elastic in nature.

Phase Angle (d)

60 70
5.4.3. Black diagram
60
40 The effect of the addition of nano nanosilica on the complex
50
modulus and phase angle has been shown in the form of the black
20
diagram as shown in Fig.10. As is evident from Fig.10, the
40 complex modulus and phase angle show a monotonic trend of
0
complex modulus increasing and phase angle decreasing.
30
35 40 45 50 55 60 65 70 75 80
Nanosilica modified asphalt binder has a smaller phase angle value
Temperature (°C) as compared to base asphalt binder for the same complex modulus.
As the measure of nanosilica is increased, the value of phase angle
Fig. 8. Isochronal plot for complex modulus and phase angle. decreased. This indicates an improvement in the elastic behaviour
of the asphalt binder and better rutting resistance.
The mechanism responsible for improvement in complex modulus
can be explained as follows. Incorporation of nanosilica in asphalt 5.5. Superpave rutting parameter
binder leads to the formation of a miscible system. The high
temperature and high-speed preparation aids in making it a To identify the improvement in the rutting resistivity of the
uniform and stable miscible system. The nanosilica particles binder after the addition of nanosilica, Superpave rutting
possess higher melting point as compared to the temperature used parameter (G*/sinδ) has been evaluated at different temperatures
during the mixing process, therefore it remains uniformly and presented in Fig.11. As can be seen in Fig. 11, there is an
dispersed in asphalt binder without dissolving in it. The uniform increase in G*/sinδ values with the addition of nanosilica at each
dispersion of nanosilica particles in the asphalt binder enhances the performance grade temperature. A significant improvement is
strength of the asphalt binder. The improvement in shear modulus observed at all the temperatures for a nanosilica content of 3%. The
can be explained by Orowan mechanism and Hall-Petch improvement in rutting is because when nanosilica is dispersed in
reinforcement mechanisms. According to Orowan mechanism the
addition of nanosilica restricts the motion of asphalt. This G*(0%)
G*(0.5%)

improves the load bearing capacity of the asphalt binder, leading G*(1%)
G*(3%)
90 δ(0%)

to enhancement in its shear complex modulus. Due to the smaller 100000 δ(0.5%)
δ(1%)
δ(3%)

size of the nanosilica particles the average distance between the

Complex Modulus G* (kPa)

particles decreases, thereby leading to an increase in the yield 85

10000
strength. The Orowan mechanism can be expressed using the

Phase Angle (d)

following equation. 80
1000
=
75

where, is the yield stress, µ is the shear modulus of matrix, b is 100

Burgers vector of matrix, and d is the average distance between the 70

particles.
10
According to Hall-Petch reinforcement there exists a mismatch 0.1 1 10 100
in atomic arrangement at the interface of asphalt binder and Frequency (rad/sec)
nanosilica. This mismatch in atomic arrangement disrupts the
dislocation movement of the asphalt binder by generating Fig. 9. Isothermal plot for complex modulus and phase angle.
repulsive stress fields. Higher the applied stress required to
0%
overcome the repulsive stress fields, higher the yield strength of 0.5%
1%
the asphalt binder. This leads to a decrease in the plastic 3%

10000
deformation of the asphalt binder. As per Hall-Petch equation, the
smaller size of nanosilica particles will generate higher phase
Complex Shear Modulus (G*)

interface that prevents the dislocation of the asphalt binder, and

thus improves its strength. Hall-Petch equation is shown as follows.

= + . 1000

where, σ is the yield strength of the material, k is a constant, d is

the particle size [74-78].
5.4.2. Isothermal plots
100
Frequency dependence of complex modulus and phase angle has 76 78 80 82 84 86 88
Phase Angle (δ)
been illustrated in Fig.9. A significant increase in the complex
modulus of nanosilica modified asphalt binders can be seen, thus Fig. 10. Black diagram.
8 F. S. Bhat and M. S. Mir / International Journal of Pavement Research and Technology xx (2020) xxx-xxx

asphalt binder, the nanosilica particles are glued to the surface of 5.6.1. Ranking of asphalt binders
the asphalt binder and a new structure of the nanosilica modified
As per AASHTO T350, non-recoverable creep compliance at 3.2
asphalt binders is formed. This new structure can absorb and
kPa can be used to determine the applicability of asphalt binder for
transfer more load coming onto the asphalt binder and therefore
a particular traffic level and load rate. Table 6 shows the different
improving the rutting resistance [24].
categories.
From the values of Jnr, it was found that control asphalt binder
5.6. Multiple stress creep and recovery test
with 0% nanosilica failed at 64°C as per AASHTO M332-14. 0.5%
nanosilica modified binder was found to be suitable for standard
The impact of nanosilica addition on non-recoverable traffic grade “S”. 1% nanosilica modified asphalt binder was found
compliance Jnr and recovery is shown in Fig.12. It can be seen that to be suitable for very heavy traffic grade “V”. 3% nanosilica
the Jnr decreases with the addition of nanosilica. The base asphalt modified binder was found to be suitable for extreme grade “E”.
had the highest value of Jnr value at both the stress levels. As the Thus, it may be concluded that addition of nano nanosilica
concentration of nanosilica is increased Jnr value showed a significantly enhances the traffic grading capacity of the asphalt
decreasing trend. Jnr showed the same trend for both the stress binder.
levels. The decrease in the Jnr value with the addition of nanosilica
may be attributed to the increased stiffness of the modified asphalt
5.7. Creep test
binder.
The addition of nanosilica enhances the elastic nature of the
Fig.13 shows the effect of creep loading on the strain values of
asphalt binder, which results in the improved recovery response.
base asphalt and nanosilica modified asphalt binders for a duration
As can be seen from Fig.12, the recovery of the asphalt binder
of 10 minutes at a temperature of 60°C. Strain shows a linear
increases with the addition of nanosilica. Nanosilica modified
variation with the loading time and the slope of the line can be used
binders showed a higher recovery response at both stress levels.
as a parameter to evaluate the effect of loading on the deformation
The improved recovery response of the nanosilica modified
of the binder. A line with a higher slope indicates a higher rate of
binders’ results in lesser strain accumulation in the binders and
deformation and line with a lower slope indicates a lower rate of
therefore enhances the rutting resistance.
deformation. The base binder curve has the highest slope amongst
0%
the curves. With the addition of nanosilica the slope of the curve
70
0.5% decreased as can be seen in Fig.13. The slope of the curve of the
1%
3% base binder was 41.57 s-1 and it decreased to 1.525 s-1 with 3%
60.89

60 nanosilica content. This is due to a lower accumulation of strain in

nanosilica modified binders. Thus, the addition of nanosilica to the
Superpave rutting parameter

50 asphalt binder improves its rutting resistance.

42.69
36.87
G*/sinδ (kPa)

40
5.8. Linear amplitude sweep
30.58
25.79

30
23.74

22.99

Fig.14 shows the effect of nanosilica on the fatigue performance

19.66
19.51

20
15.25

of asphalt binders at strain rates of 2.5% and 5%. The addition of

15.01

10.93
10.59

10 Table 6
7.8
6.53

5.71
2.73

Limiting values of Jnr for various traffic levels.

0.53

0.21
1.2

0
52 58 64 70 76
Jnr,3.2 kPa-1 Grade Traffic designation Load rate
Temperature (°C)
< 4.5 Standard (S) < 10 million ESAL >70 km/h
Fig. 11. Variation of Superpave rutting parameter with temperature. < 2.00 Heavy (H) 10-30 million ESAL 20-70 km/h
< 1.00 Very heavy (V) >30 million ESAL <20 km/h
Jnr at 0.1 kPa < 0.5 Extreme (E) >30 million ESAL <20 km/h
Jnr at 3.2 kPa
Recovery at 0.1 kPa
Recovery at 3.2 kPa
30 0%
0.5%
8 1%
Recovery at 0.1 kPa and 3.2 kPa

3%
25

10000
6
Jnr at 0.1 kPa and 3.2 kPa

20

15
Strain (%)

10 1000
2
5

0
0

100
0.0 0.5 1.0 1.5 2.0 2.5 3.0 100 200 300 400 500 600
Nanosilica content (%) Time (seconds)

Fig. 12. Variation of Jnr and recovery values at 0.1 kPa and 3.2 kPa Fig. 13. Variation of strain with Creep loading for different
stress levels for different nanosilica contents. nanosilica contents.
 F. S. Bhat and M. S. Mir / International Journal of Pavement Research and Technology xx (2020) xxx-xxx 9

2.5%
16311
200
5% 185.83
1.6E+4
180
1.4E+4
Number of Cycles to Failure (Nf)

160

Rutting Aging Index

1.2E+4 140

1E+4 120

7941
100
8E+3
6311 80
6E+3 60.62
60
4032
4E+3
40 39.27

2E+3 1794 20
874
1275 10.22
439
0 0
0% 0.5% 1% 3% 0 0.5 1 3

Nanosilica Content (%) Nanosilica Content (%)

Fig. 14. Load cycles to failure at strain levels of 2.5% and 5% for Fig. 15. Variation in rutting aging index with nanosilica content.
control and nanosilica modified asphalt binders.
90
82.48
nanosilica significantly enhances the fatigue life of the asphalt 80
75.67
binder. As is evident from the figure, addition of 3% nanosilica 70 69.25
64.41
increases the number of failure cycles to 16311 from 4032 for

Self Healing (%)

60
control binder. The nanosilica particles have high specific surface
50
area, and therefore have stronger interactions with different
40
functional groups within the asphalt binder. This leads to the
formation of a network within the asphalt binder that arrests the 30

growth of microcracks and thereby enhances the fatigue 20

performance. 10

0
0 0.5 1 3
5.9. Effect of nanosilica on aging resistance
Nanosilica Content (%)

Fig.15 shows the aging resistance of base asphalt binder and Fig. 16. Variation of ductility self-healing test for different
nanosilica modified asphalt binders. Results show that adding percentages of nanosilica.
nanosilica to the asphalt binder decreases the rutting aging index
of the binder. The improvement in aging due to the addition of temperature and frequency on the complex modulus and phase
nanosilica can be explained as follows. Asphalt being a polymer angle has been studied. The resistance to permanent deformation
system is susceptible to aging, which is initiated by thermal has been evaluated by means of Superpave rutting parameter,
scissions of carbon-carbon bonds associated with a transfer of MSCR, and creep tests. Linear amplitude sweep test was used for
hydrogen radical at the site of scission. When nanosilica is added fatigue characterization of asphalt binders. The ageing resistance
to the control binder, due to its low surface potential work, it can was evaluated by means of rutting ageing index. The following
migrate to the surface of the composite at higher temperatures and conclusions can be drawn from the study:
act as a potential heating barrier and protect the host polymeric 1. The addition of nanosilica increases the stiffness and
chains of the asphalt binder [24]. With an increase in the improves the elastic nature of the control binder.
nanosilica content, the oxidative process was found to slow down 2. The addition of nanosilica decreases the temperature
leading to a decrease in the aging resistance. For example, the susceptibility of the binder.
addition of 3% nanosilica decreased the rutting aging factor from 3. Nanosilica modified binders showed shear thinning
185.83 to 10.22. behaviour at certain temperatures. The base binder is a
Newtonian fluid at 135°C, 100°C and at 60°C. It showed
5.10. Self-healing potential of nanosilica modified binder Newtonian behaviour up to shear rate of 10/s. Nanosilica
modified binders show shear thinning behaviour at 60°C.
Fig.16 shows the variation in ductility self-healing values for Shear rate dependency increases with an increase in
base asphalt binder and nanosilica modified asphalt binders. The nanosilica content. Similar results are observed at a
ductility test carried out after the 4-hour healing period showed temperature of 100°C but to a lesser extent. The shear
that the base binder recovered by 64.41%. The binder recovery dependence of unmodified and Nanosilica modified binders
increases with incorporation of nanosilica particles in the asphalt vanishes at 135°C.
binder. 3% of nanosilica improved the recovery by 82.48%. Thus, 4. Complex modulus values increased and phase angle
it can be concluded that the addition of nanosilica helps in the self- decreased with the addition of nanosilica, and the same was
healing of the asphalt binder and hence in improving the service observed for the entire temperature and frequency range.
life of asphalt binders. 5. Nanosilica modified binders showed higher rutting
resistance as compared to the unmodified binder. Rutting
6. Conclusions resistance was evaluated by using different approaches like
G*/sinδ, MSCR, and creep tests. In all the approaches, it was
The study evaluated the effect of addition of nanosilica on the found that the use of nanosilica enhances the rutting potential
rheological properties of the asphalt binder. The effect of of the base binder.
10 F. S. Bhat and M. S. Mir / International Journal of Pavement Research and Technology xx (2020) xxx-xxx

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