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 Road Materials and Pavement Design

ISSN: 1468-0629 (Print) 2164-7402 (Online) Journal homepage: http://www.tandfonline.com/loi/trmp20

Investigation on influence of nanoclay addition on

rheological performance of asphalt binder

Prabin Kumar Ashish, Dharamveer Singh & Siva Bohm

To cite this article: Prabin Kumar Ashish, Dharamveer Singh & Siva Bohm (2016): Investigation
on influence of nanoclay addition on rheological performance of asphalt binder, Road
Materials and Pavement Design, DOI: 10.1080/14680629.2016.1201522

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Road Materials and Pavement Design, 2016
http://dx.doi.org/10.1080/14680629.2016.1201522

Investigation on influence of nanoclay addition on rheological performance

of asphalt binder
Prabin Kumar Ashisha , Dharamveer Singha∗ and Siva Bohmb
a Department of Civil Engineering, Indian Institute of Technology Bombay, Mumbai, India; b Department of
Metallurgical Engineering and Materials Science, Indian Institute of Technology Bombay, Mumbai, India

(Received 14 December 2015; accepted 9 June 2016 )

Organo-modified nanoclay has got considerable attention in recent years to improve the per-
formance of asphalt binders. However, various aspects such as rutting performance using
Multiple Stress Creep Recovery (MSCR) test, fatigue performance using Linear Amplitude
Sweep (LAS) test and ageing resistivity potential using advanced rheological parameter are
still unexplored for better rheological characterisation. The present study deals with rutting,
ageing resistivity potential and fatigue performance of asphalt binder (AC-10) modified with
organo-modified nanoclay (CL-30B). Different percentages (0, 2, 4 and 6% by weight of
binder) of CL-30B were mixed with AC-10 using a high-shear mixer. Different rheologi-
cal studies, such as Brookfield viscosity, Superpave performance grading, time–temperature
sweep, MSCR and LAS tests, were conducted on CL-30B-modified asphalt binders. Effects of
CL-30B on performance were observed to be predominant in intermediate to high-temperature
range as obtained from the master curve. The ageing resistivity of asphalt binder increased
with the addition of CL-30B. The Superpave rutting parameter (G*/Sinδ) increased and
non-recoverable creep compliance (J nr ) estimated from MSCR decreased with inclusion of
CL-30B, indicating a better rutting performance of asphalt binders. The number of cycles
to fatigue estimated from the LAS test showed improvement in fatigue performance of
asphalt binder with addition of CL-30B. The high-temperature performance grade of CL-30B-
modified binder was found to be higher compared to virgin binder. The relationship between
J nr and G*/Sinδ, and recovery (R) and storage modulus (G ) parameters are presented in this
paper. In addition, ranking of asphalt binder based on various parameters (i.e. G*/Sinδ, AI,
J nr , R, N f ) is discussed in this paper.
Keywords: CL-30B; ageing index; rutting; recovery; fatigue life; Linear Amplitude Sweep

1. Introduction
The rutting, oxidation ageing and fatigue cracking of asphalt binders are major distresses
to asphaltic pavements. The rutting failure occurs under high temperature at which a binder
becomes soft and consequently unable to sustain heavy vehicular loads; therefore, a stiffer binder
is desired for a rut-resistant pavement. Stiffer or rut-resistant binders are produced by adding
different types of polymers or crumb rubber into a softer grade binder. These modifiers are
expensive and can pose storage stability due to phase separation at high temperature (Pamplona
et al., 2012). Recent research on addition of nanomaterial to asphaltic pavement application
shows that addition of nanomaterial may provide a system with high surface area, high functional
density, high strain resistance and higher catalytic effect which may help in addressing various
performance-related problems to asphaltic pavement (Teizer, Venugopal, Teizer, & Felkl, 2011).

*Corresponding author. Email: dvsingh@civil.iitb.ac.in

© 2016 Informa UK Limited, trading as Taylor & Francis Group

2 P.K. Ashish et al.

Previous research showed improvement in rutting performance of asphalt binder with addition of
organo-modified nanoclay evaluated based on Superpave rutting parameter (G*/Sinδ) (Golestani,
Nejad, & Galooyak, 2012; Hossain, Zaman, Hawa, & Saha, 2014; Jahromi, Ahmadi, Mortazavi,
& Vossough, 2011; Van de ven, Molenaar, Besamusca, & Noordergraaf, 2008; Yu, Feng, Zhang,
& Wu, 2009). However, limited studies have been conducted on rutting behaviour of nanoclay-
modified asphalt binder through advance characterisation tests, such as Multiple Stress Creep
Recovery (MSCR). The MSCR test can help in evaluating stress sensitivity of binder at differ-
ent stress levels, which is not possible under the test condition (i.e. test under linear viscoelastic
range) stipulated for estimating G*/Sinδ parameter. Another advantage of the MSCR test over
G*/Sinδ is an evaluation of elastic recovery at varying stress levels and to rank asphalt binders
for different traffic loading conditions based on vehicle speed and cumulative repetitions. The
MSCR test observed to have better correlation with the rutting potential of bituminous mixtures
(D’Angelo, Kluttz, Dongre, Stephens, & Zanzotto, 2007). The present study is an attempt to char-
acterise the rutting behaviour of asphalt binder containing organo-modified nanoclay through the
MSCR test and G*/Sinδ.
Similarly, oxidation of asphalt binder is one of the inevitable processes that takes place due
to evaporation of lighter molecular weight organic components. It is desirable to have a lower
oxidation rate for long-life pavements. Previous studies have shown improvement in oxidation
resistance of asphalt binder due to addition of organo-modified nanoclay materials (Jahromi &
Khodaii, 2009; Liu, Wu, Van de ven, Molenaar, & Besamusca, 2010; Mahdi, Muniandy, Yunus,
Hasham, & Aburkaba, 2013; Pamplona et al., 2012; Yu et al., 2009). This may be due to the
fact that organo-modified nanoclay increases the average mean path of lighter molecular weight
components in the asphalt binder system through their intercalation/exfoliation (Zhang, Zhang,
& Zhu, 2015). Also, organophilic nature of nanoclay improves the adhesion between inorganic
phase and asphalt matrix (Liu et al., 2010) which may play an important role in improving age-
ing resistivity potential. Normally, empirical approaches such as penetration, softening point, and
viscosity test are used for analysing ageing resistivity potential of asphalt binder. However, these
tests are unable to capture the wide range of temperature and frequency which a pavement expe-
riences in the field (Liu et al., 2010). The present study evaluates the oxidation ageing potential
of asphalt binder containing organo-modified nanoclay over a wide range of temperature and
frequency.
The fatigue failure is another serious concern for asphalt binder, particularly in the low to inter-
mediate temperature regions. Liu, Van de ven, Wu, Yu, and Molenaar (2011), Yu et al. (2009),
and Wu, Wang, and Jiesheng (2010) conducted research on the fatigue performance of binder
modified with organo-modified nanoclay and reported improvement in fatigue life. Contrary to
this, Jahromi et al. (2011), You et al. (2011), and Ghile (2006) reported decrease in fatigue life
of asphalt binder with the addition of organo-modified nanoclay. Therefore, additional research
work is needed in this direction for better understanding of fatigue behaviour of organo-modified
nanoclay binders with advanced rheological characterisation. Current Superpave fatigue param-
eter (G*Sinδ) is used for evaluating the fatigue performance of asphalt binder which is based
upon linear viscoelastic properties of asphalt binder and hence unable to capture actual damage
to asphalt binder beyond this range (Wen & Bahia, 2009). Thus, in order to capture the behaviour
beyond linear viscoelastic range, the present study utilises Linear Amplitude Sweep (LAS) test
which is based on the theory of viscoelastic continuum damage (VECD), to evaluate the fatigue
performance of asphalt binder with organo-modified nanoclay. The LAS test has shown fair
correlation with Long-Term Pavement Performance (LTPP) field fatigue cracking data (Hintz,
Velasquez, Johnson, & Bahia, 2011).
Overall, the literature review showed that application of organo-modified nanoclay can have a
potential for modification of asphalt binders for better pavement performance. However, limited
 Road Materials and Pavement Design 3

studies have been reported so far to characterise ageing, rutting and fatigue performance using
advanced rheological tests methods. Few studies are reported on change in mixing and com-
paction temperature, viscosity, performance grade and ranking of asphalt binder with addition
of nanoclay. The present study was undertaken to investigate the effects of organo-modified
nanoclay (CL-30B) on mixing and compaction temperature, high-temperature grading, age-
ing resistivity potential, rutting and fatigue behaviour of asphalt binder. It is expected that the
present research study would be helpful in enhancing further understanding on the performance
of nanoclay-modified asphalt in order to ensure a long-lasting pavement.

2. Objectives
Methodological steps to accomplish overall goal of the present research study are listed as
follows:

• Evaluate the effect of CL-30B on viscosity, mixing and compaction temperatures of asphalt
binder.
• Evaluate the effect of CL-30B on the rheological behaviour of asphalt binders using
temperature and frequency sweep tests.
• Evaluate the ageing resistivity potential of CL-30B-modified asphalt binders using
rheological performance parameter.
• Evaluate the rutting potential of CL-30B-modified asphalt binders using the Superpave
rutting parameter and MSCR test and develop a correlation between them, if any.
• Evaluate the fatigue performance of CL-30B-modified asphalt binders based on VECD
theory using the LAS test.
• Develop ranking for CL-30B-modified asphalt binder based upon various performance
parameters studied in the present research work.

3. Materials and experimental methodology

3.1. Materials
The present study uses a softer grade asphalt binder (AC-10) which is usually used for prepara-
tion of polymer- and crumb rubber-modified binders. The basic properties of AC-10 are given
in Table 1. A commercially available organo-modified nanoclay, CL-30B, was collected from
Southern clay Inc. The properties of CL-30B are listed in Table 2.

3.2. Preparation of nanomodified binder and experimental plan

A high shear mixer was used for mixing of CL-30B with virgin binder. Initially, the binder
was heated up to 155 ± 5°C and different percentages (i.e. 2, 4 and 6% by weight of binder)

Table 1. Basic rheological properties of AC-10.

Properties Values Standard code

Softening point (°C) 45 ASTM D36

Penetration 0.1 mm at 25°C 86 ASTM D5
Ductility at 25°C 79 ASTM D113
Absolute viscosity at 60°C Min. 800 ASTM D2170
Flash point (°C) Min. 220 ASTM D92
4 P.K. Ashish et al.

Table 2. Properties of CL-30Ba .

Modifier concentration Bulk density d001 spacing Chemical structure
Product name (meq/100 g clay) (gm/cm3 ) (A°) of surfactant

CL-® 30B 90 0.228263 18.5 NP-(CH2 -CH2 OH)2 (CH3 )-Tb

a Andrady (2008).
b T represents Tallow (C-14 ≈ 65%, C-16 ≈ 30%, and C-18 ≈ 5%).

Figure 1. Experimental flow chart.

of CL-30B were added gradually to it and mixed at a rotational speed of 4000 rpm for 2 hrs
to ensure complete dispersion of CL-30B. Virgin binder was also mixed at the same rotational
speed for 2 hrs without adding CL-30B to keep similar condition for all samples before testing
in order to investigate the effect of CL-30B. Thereafter, short-term and long-term ageing was
carried out in accordance with ASTM D1754-09 and ASTM D6521-13, respectively. Figure 1
shows the experimental plan for the present research work.

3.3. Dispersion characterisation using X-ray diffraction

The dispersion of CL-30B in asphalt binder was examined using the X-ray diffraction (XRD)
technique. This method quantitatively measures the interlayer spacing and determines the extent
of nanoclay dispersion in the asphalt binder. Bragg’s law of diffraction is used for determining
interlayer spacing between consecutive layers of clay mineral as given by Equation (1). Decrease
or increase in the interlayer spacing (d-spacing) determines the degree of dispersion of nanoclay
in the asphalt binder. For example, no d-spacing represents the immiscible, increase in d-spacing
represents intercalation and no distinct peak in diffractograms represents exfoliation of nanoclay
material (Hossain et al., 2014). The XRD test was conducted on pure CL-30B and CL-30B-
modified asphalt binder using PANalytical® (λ = 1.54 A°, Kα ratio = 0.5, voltage = 45 kv) at
the ambient temperature and pressure condition. The diffractograms for all samples were scanned
 Road Materials and Pavement Design 5

from 2° to 10° at a scan step size of 0.026° in the 2θ range.

nλ = 2d sin(θ ), (1)

where λ = wavelength of incident X-ray, d = interlayer spacing and θ = angle of incident.

3.4. Viscosity measurement

The viscosity of virgin and CL-30B-modified asphalt binders before short-term ageing was
measured at different temperatures (120°C, 135°C, 150°C, 165°C and 180°C) using Brookfield
viscometer as per ASTM D4402-15. The temperature of 120°C was selected in order to cap-
ture the lower range of compaction temperature, in case it is affected with addition of nanoclay.
Further, a viscosity value in the range between 170 ± 20 and 280 ± 30 mPa-sec was used to
determine mixing and compaction temperature range, respectively (AASHTO T312-04).

3.5. High-temperature performance grading

This test was carried out in order to evaluate the effect of CL-30B on high-temperature perfor-
mance grade based on limiting value of G*/Sinδ as 2.2 kPa for short-term aged binder as per
ASTM D7175-15.

3.6. Temperature and frequency sweep

The complex shear modulus and phase angle of short-term aged CL-30B modified asphalt
binders were measured at different temperatures (50°C, 60°C, 70°C, 80°C and 90°C) in the
frequency range of 0.1–100 rad/sec as per AASHTO 315. The complex shear modulus can be
mathematically represented as shown in Equation (2) (Airey, 1997).

σ σ0 σ0 σ0
G∗ (ω) = = eiδ = cos(δ) + i Sin(δ) = G (ω) + iG (ω), (2)
ε ε0 ε0 ε0

where G* = complex shear modulus, G = storage modulus, G = loss modulus, δ = phase
angle, ω = angular frequency, σ 0 = peak stress, and ε0 =peak strain.
Christensen, Anderson and Marasteanu (CAM) model was used in the present research study
to develop a master curve for complex modulus as represented in Equation (3) (Yusoff, Shaw, &
Airey, 2011; Yusoff, Jakarni, Nguyen, Hainin, & Airey, 2013).
  v w/v
ωc
|G∗ | = Gg 1 + , (3)
ωr

where Gg , ωc and ωr are glassy modulus, crossover frequency and reduced frequency respec-
tively, v = log2/R, where R is a rheological index which is defined as the ratio of glassy complex
shear modulus (Gg ) to the complex shear modulus (G*) at the crossover frequency. Rheological
index is an indicative parameter for spectrum width of master curve and considered as one of the
shape parameters of master curve. ‘w’ shows how fast or slow the complex modulus value will
converse to asymptote.
In this study, the authors found a lack of fitting of the CAM model while developing master
curve of phase angle (δ), particularly in the plateau zone. Hence, the Double-Logistic (DL) model
(Equation (4)) was used and found to have a good fitting with the observed data (Asgharzadeh,
6 P.K. Ashish et al.

Table 3. Rutting criteria based upon MSCR test.

Design ESALs (million) Speed (Kmph) J nr at 3.2 kPa (1/kPa) Designationa

< 10 and > 70 2–4 S

10–30 or 20–70 1–2 H
> 30 or < 20 0.5–1 V
> 30 and < 20 0–0.5 E
a S, H, V, and E represent standard, high, very high and extreme high grade, respectively.

Tabatabaee, Naderi, & Partl, 2013).

δ = δp − δp H (fred − fp )(1 − e−(Sr log(fred /fp )) ) + δL H (fp − fred )(1 − e−(sl log(fp /fred )) ),
2 2
(4)

where δ p represents the plateau phase angle, f red represents the reduced frequency and f p repre-
sents the frequency at which binder attains its plateau zone. H (f red − f p ) represents Heaviside
step function which is equal to 0, if f p is greater than f red and equal to 1, if f p is less than f red .
S r represents the slope of the master curve to the right of plateau zone. δ L stands for rise (or fall)
on left side of plateau. S l represents the slope of the master curve to the left side of plateau zone.

3.7. MSCR test

The MSCR test was conducted to study the rutting potential of CL-30B-modified asphalt binders
in accordance with AASHTO TP 70-13. Two different parameters, that is, J nr and recovery were
estimated as expressed in Equations (5) and (6), respectively:

εnr
Jnr = , (5)
σ

where J nr = non-recoverable creep compliance (1/kPa), εnr =non-recoverable strain at end of

rest period and σ = stress level applied (kPa) during creep phase.

ε1 − ε10
εr = × 100, (6)
ε1

where εr = % recovery, ε1 = strain at the end of 1 sec creep phase and ε10 = strain at the end of
10 sec creep phase.
For better performance, it is desirable to have lesser value of J nr and higher degree of recovery.
As per AASHTO MP-19, J nr value obtained at 3.2 kPa can be used to rank asphalt binders for
different traffic loading conditions (S, H, V, and E), as given in Table 3.

3.8. LAS test

In this test, initially a frequency sweep was carried out by applying constant strain amplitude
(0.1%) over a wide range of frequency (0.2–30 Hz) for finding undamaged material parameter
‘α’ followed by an amplitude sweep (0.1–30%) at a constant frequency of 10 Hz as per AASHTO
TP101-14. The parameter α is the inverse of slope between storage modulus and applied fre-
quency on logarithmic scale. Then, damage accumulation in the sample during the amplitude
sweep test was calculated using Equations (7)–(9). The AASHTO TP101-14 defines attainment
of maximum shear stress value during the amplitude sweep phase as a failure point. Finally,
 Road Materials and Pavement Design 7

different coefficients of fatigue life equation were calculated, as given in Equation (10):


N
D(t) ∼
= [π γ0 2 (Ci−1 − Ci )]α/(1+α) (ti − ti−1 )1/(1+α) , (7)
i=1

where D(t) = accumulated damage at any time period (t), Ct = G∗ (t)/G∗ (Initial) = integrity
parameter, γ 0 = applied strain (%), G* = complex modulus (MPa), and t = testing time
(second).
The relationship between integrity parameter and damage can be further fitted using power
law as follows:
Ct = C0 − C1 (D)C2 , (8)
where C0 , C1 and C2 are curve-fitting coefficients as derived from linearisation of the power law.
Further, damage value at failure (Df ) was further calculated as follows:
 1/C2
C0 − Cpeak stress
Df = , (9)
C1
Nf = A × (γmax )−B , (10)

where N f = no of load cycles to failure, A & B = regression parameters and γ max = expected
strain level (%).

4. Results and discussion

4.1. XRD pattern
Figure 2(a) represents the XRD pattern of CL-30B and asphalt binder modified with CL-30B.
Based upon Bragg’s law (Equation (1)), basal spacing (d001 ) was calculated for each sample. The
XRD results show a decrease in 2θ value with an increase in CL-30B content. No distinct peak
was observed for AC-10, indicating the non-crystalline nature for virgin binder. The characteris-
tic peak for CL-30B was observed at 2θ = 4.72° corresponding to a basal spacing of 18.67 A°.
The addition of 2% and 4% of CL-30B to asphalt binder shows a distinct peak at 2θ = 3.43° and
2θ = 2.99°, respectively, indicating intercalated structure of CL-30B with increased interlayer
spacing. Further increase in CL-30B content (6% by weight of asphalt binder) did not produce
distinct peak, showing exfoliation of CL-30B in modified binder. Figure 2(b) shows an increas-
ing trend of basal spacing with the increased amount of CL-30B. This increase in the interlayer
spacing resulted in the increase in the surface area of nanoclay modifier in the asphalt binder
system.

4.2. Brookfield viscosity

Figure 3 shows the effects of CL-30B on rotational viscosity of asphalt binder. It can be observed
that viscosity of asphalt binder increases with an increase in CL-30B content. Exfoliation of
CL-30B structure took place when CL-30B content increased from 4% to 6% (Figure 2) which
resulted in significant improvement in viscosity value. As per the Superpave criterion, the maxi-
mum limiting value of viscosity at 135°C is 3 Pa-sec. It can be observed that viscosity of different
percentages of CL-30B-modified binders is well below this limiting criterion, and hence the
addition of nanoclay does not hamper the workability criteria of binder. Further, mixing and
compaction temperatures of CL-30B-modified asphalt binders were estimated and summarised
8 P.K. Ashish et al.

(a)

(b)

Figure 2. XRD test results: (a) intensity versus angle and (b) basal spacing (d001 ) versus CL-30B content.

Figure 3. Rotational viscosity results obtained from Brookfield viscometer.

in Table 4. An increase in mixing and compaction temperatures with addition of CL-30B is evi-
dent from Table 4. Since CL-30B resulted into a higher viscosity, it is expected to have higher
mixing and compaction temperature. The observed value of mixing temperature is in the range
of 150–180°C which is in close approximation with AC-30 (150–165°C), AC-40 (160–170°C),
 Road Materials and Pavement Design 9

Table 4. Mixing and compaction temperature range of CL-30B modified binders.

Viscosity value Superpave
at 135°C criteria (Pa-sec) Mixing temp. Compaction
Sample (Pa-sec) @ 135°C range (°C) temp. range (°C)

AC-10 + 0%CL-30B 0.4 ≤3 Pass 151–157 140–145

AC-10 + 2%CL-30B 0.558 Pass 160–167 148–153
AC-10 + 4%CL-30B 0.775 Pass 166–173 154–159
AC-10 + 6%CL-30B 1.175 Pass 174–181 162–167

Figure 4. Variation of rut factor with temperature.

polymer-modified binder (PMB-40) (165–185°C) and crumb rubber-modified bitumen (CRMB-

60) (165–185°C) as recommended by the Ministry of Road Transport and Highways (MoRT&H,
2013). PMB-40 represents the polymer-modified bitumen with a penetration value from 30 to
50 mm at 25°C measured as per ASTM D5, whereas CRMB-60 represents the crumb rubber-
modified bitumen with minimum softening point value of 60°C measured as per ASTM D36.
However, compaction temperature for CL-30B-modified asphalt binder is on the higher side
than AC-30 ( > 140°C), AC-40 ( > 150°C), PMB-40 (115–155°C) and CRMB-60 (115–155°C),
as recommended by MoRT&H (2013).

4.3. High-temperature performance grade

Figure 4 shows the variation in the Superpave rutting factor value for short-term-aged CL-
30B-modified asphalt binders. An increase in the CL-30B content resulted in an increase in
G*/Sinδ, indicating improvement in rutting performance. A significant increase in G*/Sinδ was
observed for 6% CL-30B-modified binder compared to 2% and 4% modification levels. This may
be attributed to transformation of CL-30B structure from intercalated to exfoliated (Figure 2).
Change in performance grading (PG) can be observed where grade for 0%, 2%, 4% and 6%
CL-30B-modified binders are PG70, PG70, PG76 and PG82, whereas continuous grade was
observed to be 70°C, 72°C, 76°C and 82°C, respectively (Figure 4). It can also be observed that
though there is an increase in the rutting factor value when CL-30B content increased from 0%
to 2%, PG remained unchanged. As expected, the rutting factor decreased with an increase in
temperature. Also, a decrease in G*/Sinδ by an amount of 47–54% can be observed with every
performance grade bumping for all combinations.
10 P.K. Ashish et al.

(a)

(b)

Figure 5. Master curve for (a) complex modulus and (b) phase angle of CL-30B modified asphalt.

4.4. Time–temperature sweep test

4.4.1. Master curve
Figure 5(a) shows the master curve of complex modulus for short-term-aged CL-30B-modified
asphalt binders over a wide range of frequency at a reference temperature (60°C). It can be
observed that complex modulus increases with an increase in CL-30B content, indicating that
CL-30B-modified binders are more rut resistant compared to unmodified binder. This effect
seems to be predominant in the case of lower frequency (equivalent to high temperature) to inter-
mediate frequency range than at higher frequency (equivalent to low temperature) range where
slight improvement in complex modulus values was observed with CL-30B modification. Such
behaviour can be believed due to the fact that as the frequency of loading increases (or tempera-
ture decreases), nanoclay material plays lesser role in taking up the applied shear load compared
to a lower frequency (or higher temperature) range where nanoclay material starts bearing the
applied shear load. Similar observation has been reported by You et al. (2011) and Jahromi and
Khodaii (2009) for two different kinds of organo-modified nanoclay mixed with asphalt binders.
 Road Materials and Pavement Design 11

Figure 6. Cole–Cole diagram for CL-30B-modified asphalt.

Figure 5(b) shows the master curve for phase angle values. It can be seen that the phase
angle of asphalt binder decreases with an increase in CL-30B content, indicating improvement
in the elastic response of asphalt binder. It is expected that improved elastic response of CL-
30B-modified binder will provide better rutting performance compared to virgin binder. Further,
a similar phase angle in plateau zone can be observed for both virgin and CL-30B-modified
asphalt binder.

4.4.2. Cole–Cole diagram

The Cole–Cole diagram is a plot between storage (G ) and viscous modulus (G ) of asphalt
binder. This graph helps in finding out the relative change in storage modulus with respect to
viscous modulus value with overall change in complex modulus value (Airey, 1997). Also, Cole–
Cole diagram is used for validating the data obtained from the master curve (Akisetty, Gandhi,
Lee, & Amirkhanian, 2010). Viscoelastic properties of asphalt binder can be represented without
incorporating temperature or frequency as one of the axes using Cole–Cole diagram. Figure 6
represents the Cole–Cole diagram for CL-30B-modified asphalt binders. Single linear curve for
each combination of CL-30B-modified asphalt binder validates the data obtained from the master
curve. It is interesting to note that the slope of the curve shifted towards the storage modulus axis
with an increase in CL-30B content, showing relative improvement in elastic behaviour with the
addition of CL-30B. Such behaviour is expected to improve the rutting performance of virgin
asphalt binder with nanoclay modification.

4.5. Ageing resistivity potential

The ageing resistivity potential of CL-30-modified asphalt binders was evaluated by the esti-
mating ageing index (AI) based on the rutting factor parameter, as shown in Equation (11). A
higher value of AI represents a higher degree of susceptibility towards ageing and vice versa. It
should be noted that the AI value might change based on temperature and frequency. Therefore,
an attempt has been made in this paper to evaluate the AI value at different temperatures and
frequencies:

|G∗ / sin δaged |

AI = , (11)
|G∗ / sin δunaged |
12 P.K. Ashish et al.

(a)

(b)

Figure 7. Variation of AI at (a) different temperature (frequency = 10 rad/sec), and (b) different fre-
quency level (temperature = 60°C).

where |G*/Sinδ aged | and |G*/Sinδ unaged | are the rutting factor values of unaged and short-term-
aged binder, respectively.
Figure 7(a) represents the variation of AI with different temperatures at 10 rad/sec. The 10
rad/sec was selected, as it is a standard angular frequency recommended by Superpave to evaluate
the rutting potential of asphalt binder. The average value of three samples is reported while
calculating the AI values. Results shows that the AI value decreases with an increase in CL-30B
content, indicating that CL-30B can act as an antioxidant agent and may decrease the ageing rate
of binder in the field, and hence improved long-term performance. A similar trend was observed
at different temperatures. Such behaviour could be the result of CL-30B particles distribution in
asphalt binder which is providing hindrance as well as increasing the mean path length to be
travelled by lighter components of asphalt binder during the oxidation process (Liu et al., 2010;
Osman, Mittal, & Suter, 2007).
Figure 7(b) shows the variation in AI values with loading frequency (1–100 rad/sec) at a tem-
perature of 60°C. The highest value of AI for unmodified asphalt binder at a frequency of 10
rad/sec can be observed as 1.84 which decreased to 1.48 when the CL-30B modification level
increased to 6%, showing improvement in ageing resistivity of the binder with the addition of
 Road Materials and Pavement Design 13

(a)

(b)

Figure 8. Shear strain versus time from the MSCR test at (a) 0.1 kPa, and (b) 3.2 kPa.

nanoclay. Furthermore, as the frequency increases from 1 to 100 rad/sec, the AI value for all
the combination decreases by 10–20%. Such a decrease in AI value with an increase in loading
frequency shows a lesser degree of susceptibility to ageing at higher frequency level (or lower
temperature zone).

4.6. MSCR test

4.6.1. Strain response
Figure 8(a) and (b) shows the variation of applied shear strain during initial loading–unloading
period at standard stress levels of 0.1 and 3.2 kPa. As expected, the highest degree of strain was
found to be for virgin binder which further decreases with an addition of CL-30B content. Also,
the increase in shear strain value is evident with an increase in stress level.

4.6.2. Recovery and non-recoverable creep compliance

Figure 9(a) shows variation in recovery (R) value obtained from the MSCR test. It can be seen
that the addition of CL-30B increases the value of recovery. At 3.2 kPa stress level, an increase
in CL-30B from 0% to 6% resulted in an increase in R value from 0.60% to 9.29%. The AC-10
binder is a virgin binder with negligible R; however, the addition of higher percentage of CL-
30B exhibited improved elastic recovery of asphalt binders, indicating a better performance of
14 P.K. Ashish et al.

(a)

(b)

Figure 9. Effect of CL-30B on (a) elastic recovery and (b) non-recoverable creep compliance.

CL-30B-modified binders in terms of rutting and fatigue. A similar trend was observed at 0.1
kPa stress level where R value increased from 2.26% to 12.54% with an increase in CL-30B
content from 0% to 6%. This may be attributed to exfoliation of nanoclay at higher doses of
CL-30B which improved the compatibility between asphalt and nanoclay. Also, such exfoliation
results into increasing the ageing resistivity with an addition of CL-30B, as explained in previous
sections which helped in improving its recovery response.
Figure 9(b) shows the plot of J nr values obtained from the MSCR test. It can be seen that
the addition of CL-30B decreases the J nr value of asphalt binder. For example, at 3.2 kPa, the
addition of 0%, 2%, 4%, and 6% CL-30B showed J nr (kPa−1 ) values as 2.12, 1.84, 0.94 and 0.37,
respectively. It can be noted that the addition of 6% CL-30 resulted in a decrease in J nr value
from 2.12 to 0.37, which can be considered as significant improvement in rutting resistance. A
decrease in J nr may be attributed to intercalation and exfoliation of CL-30B, which leads to an
increase in stiffness value of the binder and hence improved rutting resistance.

4.6.3. Correlation between Superpave and MSCR parameters

The MSCR test determines J nr and R, while the Superpave standard test is conducted to esti-
mate G*/Sinδ of a binder. The J nr value can be used for ranking a binder for different traffic
loading conditions which is not possible with G*/Sinδ estimation alone (Table 3). Therefore,
 Road Materials and Pavement Design 15

(a)

(b)

Figure 10. Plot of (a) J nr_3.2 kPa versus G*/Sinδ, and (b) %R_3.2 kPa versus G at 64°C.

a relationship between G*/Sinδ and Jnr would be helpful for characterisation of rutting perfor-
mance for different classes of traffic loading by conducting PG test only. Figure 10(a) represents
the plot of J nr_3.2 kPa versus G*/Sinδ obtained at 64°C. A power–law relationship showed a better
correlation between J n and G*/Sinδ.
It is known that G measured during the Superpave PG test and R measured using the MSCR
test are indicative parameters for elastic response of asphalt binder. However, G cannot give
quantitative value of R at different stress levels through the PG test. Higher the value of recov-
ery is, better will be the elastic response of asphalt binder and hence improved performance in
fatigue. The present study develops a correlation between G obtained from the PG test and R
measured from the MSCR test. It is interesting to observe a linear relationship between G and
R, as shown in Figure 10(b).
It is to be noted that present relationships are based upon limited experimental data generated
during this research work which may not be generalised. Further research work is required in
order to reach more comprehensive relationship.

4.7. LAS test

Figure 11 represents the plot of shear stress versus shear strain obtained from amplitude strain
sweep test under strain controlled condition. All binder combinations showed considerable dam-
age at higher amplitude strain level. Also, the maximum shear stress value increased with an
16 P.K. Ashish et al.

Figure 11. Shear stress versus % strain in amplitude sweep test.

increase in CL-30B content, indicating an increase in load carrying capacity under shear action
with the addition of nanoclay into asphalt binder. The maximum shear stress value can be
observed at the applied amplitude strain level of 5% for all the binder combinations indicat-
ing a similar failure strain level irrespective of the CL-30B content. Also, all binders shows a
similar shear stress–strain pattern beyond amplitude strain level of 20% indicating redundancy
of amplitude sweep testing beyond this strain level as evident from Figure 11. Considering the
rate of damage in post peak region with an increasing amplitude strain level, the sample with 6%
CL-30B content exhibited the highest rate of damage followed by 4%, 2% and 0% CL-30B com-
binations. This may be attributed to the increase in stiffness value with the addition of CL-30B
to virgin binder.
Figure 12 shows the variation of number of load cycles to failure against applied amplitude
strain level. It shows significant improvement in fatigue life of asphalt binders with the addition
of CL-30B particularly in lower applied strain level. For example, at the strain level of 2%,
the number of load cycles to failures increased from 8582 to 51898 when the CL-30B content
increased from 0% to 6% indicating an increase in fatigue life by almost five times. It can be seen
that at higher strain level, effects of CL-30B on the fatigue behaviour of asphalt are diminishing.
Similar improvement in fatigue life with addition of nanoclay has been reported in the literature
based upon different parameters used for fatigue life assessment of asphalt binder (Liu et al.,
2011; Wu et al., 2010; Yu et al., 2009).
Earlier, a hypothesis was made regarding improvement in fatigue life of asphalt binder with
the addition of CL-30B based upon an increase in R value obtained through the MSCR test.
This hypothesis is found to be true, as a binder with 6% CL-30B exhibited the highest R value
(Figure 9(a)), and highest number of cycles to fatigue failures (Figure 12).

4.8. Ranking of binders based upon various performance parameters

Table 5 presents the performance ranking of CL-30B-modified asphalt binders based on the
following parameters: G*/Sinδ, J nr , R, AI, and number of cycles to fatigue failure from the
LAS test obtained through series of rheological studies conducted in the present research paper.
A higher value of G*/Sinδ, R and number of load cycles to fatigue failure is an indication of
a binder with better performance. Similarly, a lower value of J nr and AI are desirable for a
binder. The rank 1 of a binder indicates the best binder, while the rank 4 shows a comparatively
poorer binder. Previous sections showed that the addition of CL-30B provides increased rutting
 Road Materials and Pavement Design 17

Figure 12. Load cycle to failure versus % strain level applied.

Table 5. Ranking based upon various performance parameters.

Ranking based upon

AASHTO
Sample Code G*/Sinδ J nr AI %R Fatigue life MP-19 Ranking

AC-10 + 0%CL-30B 4 4 4 4 4 S
AC-10 + 2%CL-30B 3 3 3 3 3 H
AC-10 + 4%CL-30B 2 2 2 2 2 V
AC-10 + 6%CL-30B 1 1 1 1 1 E

resistance, better fatigue life, and lower oxidation ageing potential. It can be seen that a binder
with 0%, 2%, 4%, and 6% CL-30B was ranked as 4, 3, 2 and 1, indicating that binder with
6% CL-30B is superior compared to other binders. It is interesting to note that all considered
parameters shows a similar ranking (Table 5).
The AASHTO MP-19 suggests to grade a binder for different traffic loading conditions based
on J nr value estimated at 3.2 kPa from the MSCR test (Table 3). J nr represents the measure
for amount of residual strain left relative to the amount of stress applied in the specimen after
repeated creep and recovery. It can be seen that AC-10 binder is ranked suitable for ‘s’ traffic
loading condition which is a standard loading, while the addition of 2%, 4%, and 6% CL-30
B enhanced suitability of the binder for H, V, and E traffic loading conditions, indicating a
significant improvement in performance ranking of the binder.

5. Economics/cost consideration: a note

The CL-30B is organo-modified clay mineral which is rich in Montmorillonite (MMT) due to
their high Cation Exchange Capacity value. Clay available in western and central part of India
contains high amount of MMT and are available at very low cost. Such clay can be used for
development of organo-modified MMT. Currently in India, polymer-modified binder ( ≈ Rs
50,000 per MT), CRMB-60 ( ≈ Rs 41,000 per MT) or higher grade virgin binder, such as
AC-30/AC-40 ( ≈ Rs 33,000 per MT), is used particularly in higher temperature regions for
eliminating performance-related issues like rutting. Such binders are costlier than softer grade
18 P.K. Ashish et al.

asphalt binders, such as AC-10 ( ≈ Rs 27,000 per MT). This leads to an increase in the overall
cost of pavement construction. This research study shows promising results in terms of improve-
ment in performance. Also, other research shows a decrease in cost by approximately 22–33%
per metric tonne by using organo-modified clay compared to polymer-modified asphalt binder
(Hossain et al., 2014). This shows a significant decrease in cost and it will result in overall
cost saving. This gives the motivation for use of organo-modified clay developed from locally
available clay. This may lead to a decrease in material cost and hence overall cost of pavement
construction. Along with material cost, energy requirement during construction stage also needs
to be taken into consideration while carrying out cost analysis. An increase in mixing and com-
paction temperature can be observed as explained in Section 4.2 which will increase the energy
requirement and hence the overall cost of construction will increase. Hence, it is needed to carry
out life cycle cost analysis considering various associated aspects before making a concluding
remark in terms of cost.

6. Conclusions
This paper focuses on various rheological performance parameters of nanoclay (CL-30B)-
modified asphalt binder. The following conclusions can be drawn based upon results and
discussion above:

• Significant increase in mixing and compaction temperature of virgin asphalt binder was
observed with the addition of CL-30B particularly at higher doses of nanoclay. The mixing
temperature of nanoclay-modified asphalt binders was found to be comparable with that of
polymer-modified binder. However, compaction temperature of nanoclay-modified binder
was observed to be on higher side compared to that of polymer-modified binder.
• The addition of CL-30B to asphalt binder resulted in an increase in PG grade and
decrease in J nr (obtained through the MSCR test), indicating a better rut resistant of
nanoclay-modified binder compared to that of virgin binder. In addition, ranking of binder
for different traffic loading conditions based on J n in accordance with AASHTO MP-
19 showed that CL-30B-modified binder may be suitable for higher degree of ESALs
(equivalent standard axle load) compared to virgin binder.
• The mater curve of complex modulus showed significant improvement in stiffness value in
lower frequency (higher temperature) to intermediate frequency zone compared to higher
frequency (lower temperature) zone with CL-30B modification. This shows that the addi-
tion of nanoclay may play an important role in improving the performance of asphalt
binder under intermediate to high temperature condition.
• Addition of CL-30B to asphalt binder found to decrease its ageing potential estimated
using the AI index. A decrease in AI value was observed with an increase in loading
frequency value. Such decrease in AI shows a lesser degree of susceptibility to ageing at
higher loading frequency (or lower temperature zone).
• Nanoclay-modified binders exhibited higher R (obtained through the MSCR test) value
compared to virgin asphalt binder. It is expected that such improvement in recovery value
may enhance fatigue performance of a pavement.
• Fatigue behaviour of asphalt binder using the LAS test indicated that the number of load
cycle to failure increases with an increase in CL-30B content. The fatigue performance of
nanoclay-modified binder was found to be better than that of virgin binder.
• The ranking of CL-30B-modified asphalt binders found to be similar based on five param-
eters (G*/Sinδ, AI, J nr , R and N f ). It showed that a binder with 6% CL-30B is superior
followed by 4%, 2%, and 0% CL-30B-modified binders.
 Road Materials and Pavement Design 19

The present study characterises a binder with addition of CL-30B. It is recommended that
different organo-modified clays be tried to evaluate their performance on various source and types
of binders. Furthermore, the binder rheological tests can be validated by conducting mechanical
performance on asphalt mixtures.

Disclosure statement
No potential conflict of interest was reported by the authors.

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