www.seipub.

org/sceaStudyofCivilEngineeringandArchitecture(SCEA)Volume3,2014

TheImprovementofBitumenPropertiesby
AddingNanoSilica
FarhadZafari1,MohammadRahi2,NazaninMoshtagh3,HosseinNazockdast4
HeadofResearchandDevelopmentDepartment,PasargadCompany,Tehran,Iran

PolymerEngineeringDepartment,AmirkabirUniversityofTechnology,Tehran,Iran

2,3

AssociatedProfessor,PolymerEngineeringDepartment,AmirkabirUniversityofTechnology,Tehran,Iran

farhad_zafari@yahoo.com;2mohamadrahi@yahoo.com;3nazanin.moshtaq@gmail.com;4nazdast@aut.ac.ir
1

Abstract
Asphalt oxidative aging is one of the prevalent causes of
pavementdistresseswhichincreasepavementsusceptibility
to fatigue andlow temperature cracking. This phenomenon
is mainly studied through oxidation kinetics and through
evaluating oxygen diffusivity rate into asphalt binders.
Whileoxidativeaginginpavementisinevitable,application
of antiaging additives shown to be an effective method in
delayingoxidativeaging.Assuchthispaperinvestigatesthe
meritofapplicationofnanosilicaasanantiagingadditive.
To do so, different percentages of nanosilica was added to
neat asphalt binder. Asphalt binder was then exposed to
short term oxidative aging using a rolling thin film oven
(RTFO). To study the change in the chemical, rheological
andmorphologicalpropertiesofasphaltbindersinpresence
of nanosilica, the Superpave tests, Fourier transform
infrared spectroscopy (FTIR) as well as SEM imaging were
conducted. The FTIR study shows that nanosilica can
improve the aging resistance of the asphalt binder as
reflectedinlowerlevelofcarboxylicacids(observedat1400
1440cm1)andsulfoxide(observedat~1050cm1)innano
silicamodifiedspecimencomparedtothoseinnonmodified
specimens. Carboxylic acids occur naturally in asphalt;
however its concentration has been known to be increased
significantly due to oxidative aging. This in turn reduces
oxidation aging in modified asphalt. In addition, it was
foundthatpresenceofnanosilicasignificantlyincreasesthe
complex modulus (G*) and complex viscosity (*) of the
asphaltbinder.Thisinturnimprovespavementresistanceto
rutting. It was concluded that introduction of nanosilica to
asphalt binder can improve the antiaging property, rutting
performanceandrheologicalpropertiesofasphaltbinder.
Keywords
Nanosilica;NanoModifiedAsphalt;Rheology;Aging

Introduction
Thechemicalcompositionofasphaltisquitecomplex,
therefore,researchersmainlyusepercentagesofSARA
(Saturates, Asphaltene, Resin and Aromatic) to
compare various asphalt binder produced from
different origins. Composition of each asphalt binder

62

is typically grouped into two categories: asphaltenes

and maltenes. The latter can be further subdivided
into saturates, aromatics and resins (Petersen, 1984).
However,asphaltscolloidalsystemmaychangewhen
it is exposed to oxygen at elevated temperature
causing oxidative during asphalt production and
service life. Aging has been known to be one of the
principal factors expediting asphalt pavements
deterioration (Lu and Isacsson, 1998). The occurrence
of asphalt binder aging is further expedited by
thermaloxidation during storage, mixing, transport
and placing and compaction; this in turn negatively
affects asphalt binder rheological properties causing
pavement to be more susceptible to low temperature
cracking(LuandIsacsson,2002;GawelandBaginska,
2004). While pavement oxidative aging is inevitable,
therehavebeenmanystudiestobetterunderstandthe
oxidation mechanisms as well as to develop new
methods and additives to delay oxidative aging.
Among those additives are various resins, rubbers,
polymers, sulphur, metal complexes, fibres, chemical
agents and nano materials. The use of nanomaterials
has seen a tremendous development in recent years
mainly due to their surface properties and their
effectiveness in altering hierarchical structure of
compositematerials(Youetal.,2011;Yaoetal.,2012b;
Onochieetal.,2013;Fini,2013).Ithasbeenshownthat
introduction of certain nanomaterials into asphalt
binder could offer a significant improvement in
asphaltphysicalandrheologicalpropertiesleadingto
development of nano modified asphalt with superior
performance. As such nanotechnology has been
gradually incorporated into the field of modified
asphalt with various kinds of nanomaterials being
usedtomodifyasphaltinrecentyears.Nanosilicahas
been widely used in polymers and asphalt binder as
inorganicfillertoimprovethepropertiesofpolymeric
andbituminousmaterials(Zhouetal.,1999;Huetal.,
2004;Chengetal.,2006;LiuandPan,2007).Overthe

StudyofCivilEngineeringandArchitecture(SCEA)Volume3,2014www.seipub.org/scea

last 10 years, nanosilica has served as a promising

material for designing and preparing new functional
materialsbecauseofitshighsurfaceareaandstability
(Senffetal.,2009;ZhangandIslam,2012;Kongetal.,
2012; Singh et al., 2013). The shape and dimension of
thesilicaparticlesareverydesirableforapplicationin
asphalt binder mainly because the surface area of
interaction is much higher than that of conventional
fillers. By dispersing nanosilica into asphalt matrix
one can create polymeric nanocomposites with
enhanced mechanical behavior, thermal and gas
barrierproperties(LeBaronetal.,1999;SinhaRayand
Okamoto, 2003; Yao et al., 2012a). Therefore, in this
study,thenanosilicawasusedtomodifytheasphalt
binder. Nanosilica was added into the neat asphalt
binderatconcentrationsof2%,4%and6%byweight
ofthebaseasphaltbinder.Rheological,chemicaland
morphological characterization of neat and modified
asphalt binder was conducted to evaluate the
performance of nanosilica modified asphalt binder.
Following sections of the paper is devoted to
description of materials and test methods including
materials and sample preparation, aging procedure,
dynamic rheological characterization and Fourier
transforminfraredspectroscopy(FTIR).Theresultsof
Physical properties of asphalt binder, dynamic
rheological characterization and Fourier Transform
Infrared Spectroscopy (FTIR) are presented in section
3. Dynamic rheological properties of asphalt binders
are investigated based on three approaches including
frequencysweep,temperaturesweepandshearcreep.
Finally, the merit of application of nanosilica to
improve antiaging properties of asphalt binder is
discussed.

Whentheasphalttemperaturereachedto180o98C,
specified amount of nanosilica was added to the
can and mixing for two hours. Using this
procedure one neat sample and three nanosilica
modifiedasphalt(NSMA)sampleswereproduced.
For simplicity in referring to each sample, they
were named using following abbreviation: NEAT,
NSMA2%, NSMA4% and NSMA6%. To ensure
nanosilicaparticlesaredisperseduniformlywithin
the asphalt matrix. The Scanning Electron
Microscopy (SEM) images of asphalt were mainly
usedtounderstandthemicrostructuralchangesof
modified samples and to evaluate the matrix
structure such as the physical dispersion of nano
silica particles (Kavussi and Barghabani, 2014). As
can be clearly seen in FIGURE 1, nanosilica
particlesarewelldispersedintheasphaltmatrix.

(a)

MaterialsandTestMethods
This section will describe various materials used in
thisstudyaswellasthesourcesofeachmaterialand
itspreparationmethod.
1)

(b)

MaterialsandSamplePreparation

The base asphalt used in this study was AC 60/70

Pen grade.Asphalt binder was then blended with
2%, 4% and 6% nanosilica acquired through
Neutrino Corporation located in Tehran, Iran. The
quantityofeachadditivewasselectedbyweightof
based asphalt binder. The mixing was conducted
using an IKAbench top high shear mixer at 4000
rpm for 2 hours. To conduct the mixing, an
aluminium can was filled with 250 260 g of
asphalt and placed in a thermoelectric heater.

(c)
FIGURE1SEMMICROSTRUCTUREIMAGESOFNANOSILICA,
NEATANDNANOSILICAMODIFIEDASPHALTAT18000X
MAGNIFICATION,(A)NSMA2%,(B)NSMA4%AND
(C)NSMA6%

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2)

AgingProcedure

TABLE1CONVENTIONALPROPERTIESOFNEATANDNANOSILICA
MODIFIEDASPHALTBINDERS

All asphalt binder samples were aged by rolling

thin film oven test (RTFOT) (ASTM D287285) in
order to simulate the hot mixing process during
plantproduction.
DynamicRheologicalCharacterization
Dynamic Shear Rheometer (DSR) MCR101 from
Austria Anton Paar Company was used in this study
to measure complex modulus and complex viscosity.
The repeated shear creep test with a loading and
recoveryperiodwasconductedoneachspecimen.The
creeptestsweredoneundertwofixedshearstressesof
100and3200Pafor10cycleswith1sloadingtimeand
9sofrecoverytimeat50C.
FourierTransformInfraredSpectroscopy(FTIR)

Sample
NEAT
NSMA2%
NSMA4%
NSMA6%

2)

Penetration Softening
(mm)
point(oC)
58
47
56
50.5
50
54.1
43
58

Ductility
(cm)
>150
93
53
27

Elastic
recovery(%)
12
16
19
23

StorageStability

The storage stability results are listedin TABLE2.

The difference between the softening points was
usedtoevaluatestabilityofthemodifiedsamples.
The stability was deemed acceptable if the
difference between the softening point of samples
takenfromthetopandthebottomofthespecimen
waslessthan2.5C.
TABLE2STORAGESTABILITYOFNEATANDNANOSILICAMODIFIED
ASPHALTBINDERS

Fourier Transform Infrared Spectroscopy (FTIR)

spectra were recorded by Jasco IRT 3000 FTIR
spectrometer. Infrared spectra can be utilized in
organic structure determination by identifying
interatomic bonds in chemical compounds. Chemical
bonds in different environments will absorb varying
intensitiesandatvaryingfrequencies.Thefrequencies
atwhichthereareabsorptionsofIRradiationreferred
toaspeakscanbecorrelateddirectlytobondswithin
the materials chemical structure. Each interatomic
bond may vibrate in several different motions
(stretchingorbending).Stretchingabsorptionsusually
producestrongerpeaksthanbending.
Results and discussion
PhysicalPropertiesofAsphaltBinder
1)

BasicPhysicalProperties

The effect of nanosilica modification on the

conventional 128 asphalt binder rheological
properties can be seen in TABLE 1. It can be
observedthatthereisadecreaseinpenetrationand
anincreaseinthesofteningpointwhennanosilica
was introduced to the asphalt binder. It was
observed that all nanomodified asphalt samples
had lower penetration and higher softening point
than control asphalt. This in turn can lead to
improvement in the asphalt binder stiffness and
flexibility. However, the result of ductility test
showeda declining trendin the presence of nano
silica.Thiscanbeattributedtothepresenceofhigh
specific surface area in nanosilica which leads to
increaseofasphaltabsorption.

64

Sample
NEAT
NSMA2%
NSMA4%
NSMA6%

Top
47.8
52.5
57.3
61.9

SofteningPoint(oC)
Bottom
SPtopSPBottom
47.8
0
52.4
0.1
57.6
0.3
91.6
0.6

TABLE2showsthesofteningpointsofthetopand
bottomspecimensandthedifferencebetweenthese
twotemperatures.AscanbeobservedfromTABLE
2, the differences between the top and bottom
softening points in all samples are less than 2.5C.
This indicates that nanosilica modified specimens
have appropriate storage stability. Therefore
addition of nanosilica into asphalt will not
negatively affect storage stability of the modified
samples.
DynamicRheologicalCharacterization
1)

FrequencySweep

The relationship between frequency and

temperature established by the TimeTemperature
Superposition Principle (TTSP); this principle
allows rheological properties of asphalt binders to
beestimatedoveranextendedfrequencyrange.In
FIGURE2,complexmodulus(G*)andphaseangle
() values are presented in the form of black
diagrams. Black diagrams provide a useful tool in
analyzing rheological data for the identification of
possiblediscrepanciesinexperimentalresults,and
for the verification of time temperature
equivalencyinthermorheologicalsimplematerials
(Airey,2002).Blackdiagramcurvescorresponding
toallasphaltbindershavemonotonictrend.Ascan

StudyofCivilEngineeringandArchitecture(SCEA)Volume3,2014www.seipub.org/scea

be clearly seen, the samples with higher

concentration of nanosilica have lower complex
modulus at higher phase angle and higher
complex modulus at smaller phase angle. The
RTFOagingslightlyshiftsallcurvestowardlower
phaseangle,thusindicatingachangeinrheological
behaviour. In addition, comparison of Black
diagram for RTFO aged and unaged samples
shows that specimens with high concentration of
nanosilicaarelesssusceptibletooxidativeaging.

silicaconcentration.Ananosilicamodifiedasphalt
binderwithhighviscositycanleadtodevelopment
ofathickerfilmsurroundingtheaggregateswhich
increases the cohesive strength. This in turn can
promotepavementdurability.

(a)

(a)

(b)
FIGURE3THEISOCHRONALPLOTSOFCOMPLEXVISCOSITY
VERSUSTEMPERATUREAT10RAD/S,(A)UNAGEDNEAT
ANDMODIFIEDASPHALTBINDERAND(B)AGEDNEATAND
MODIFIEDASPHALTBINDER.

(b)
FIGURE2THEBLACKDIAGRAMOFASPHALTBINDERSAT30
C,(A)UNAGEDNEATANDMODIFIEDASPHALTBINDER
AND(B)AGEDNEATANDMODIFIEDASPHALTBINDER

2)

TemperatureSweep

The values for the complex viscosity, complex

modulus and phase angle of the nanosilica
modified samples as a function of the nanosilica
concentrationandtemperatureat10rad/s(1.59Hz)
areshowninFIGURES35.
As it can be seen (FIGURE 3), asphalt complex
viscosity increases with the increases in the nano

(a)

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(b)
FIGURE4THEISOCHRONALPLOTSOFCOMPLEXMODULUS
VERSUSTEMPERATUREAT10RAD/S,(A)UNAGEDNEAT
ANDMODIFIEDASPHALTBINDERAND(B)AGEDNEATAND
MODIFIEDASPHALTBINDER

FIGURE 4 indicates that the complex modulus of

allmodifiedsampleswerehigherthanthoseofthe
neatasphaltbinder.Inaddition,itcanbeseenthat
phase angles of modified asphalt binder were all
lowerthanthoseofbaseasphaltbinder.

Consequently, the modified asphalt binders were

more elastic than neat asphalt binder and could
enhance the asphalt rutting resistance. To further
investigate asphalt performance in terms of
permanent deformation (rutting); Superpave
ruttingparameter(G*/sin)wasmeasuredforboth
modified and nonmodified specimens. Rutting is
defined as the progressive accumulation of
permanent deformation of each layer of the
pavement structure under repetitive loading
(Tayfur et al., 2007). FIGURE 6 shows the G*/sin
versus temperature curves for (a) before and (b)
after RTFO aging. The G*/sin values were
calculatedforthetemperaturesrangingfrom30to
90C. The results show that introduction of nano
silica to the neat asphalt binder significantly
increased the rutting parameter G*/sin; this in
turn can enhance pavement resistance to
permanent deformation. This can further allow
extending the high temperature range within
whichasphaltbindercouldbeused.

(a)

(a)

(b)

(b)

FIGURE5THEISOCHRONALPLOTSOFPHASEANGLEVERSUS
TEMPERATUREAT10RAD/S,(A)UNAGEDNEATAND
MODIFIEDASPHALTBINDERAND(B)AGEDNEATAND
MODIFIEDASPHALTBINDER

FIGURE6THEISOCHRONALPLOTSOFG*/SINVERSUS
TEMPERATUREAT10RAD/S,(A)UNAGEDNEATAND
MODIFIEDASPHALTBINDERAND(B)AGEDNEATAND
MODIFIEDASPHALTBINDER

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3)

ShearCreep

FourierTransformInfraredSpectroscopy(FTIR)

Theresultsofcreeptestat50Chavebeenshown
in FIGURE 7. At each loading cycle, the loading
and recovery time was equal to 1 s and 9 s,
respectively and loading cycles repeated for 20
times(10 cycles with 100Pa loading and10 cycles
with 3200 Pa loading). Instantaneous elastic strain
ofasphaltdevelopedduringtheloadingstage,and
the viscoelastic strain of asphalt was calculated as
the total creep strain accumulated at the time of
unloading. The instantaneouselastic strain of
asphalt disappeared after unloading, and the
delayed elastic strain recovered gradually (Wang,
2011). The unrecoverable viscoelastic strain is the
permanentstrain(Wangetal.,2011).Analysisofthe
data indicates that increasing the nanosilica
content and aging in RTFO have noticeable effect
on reducing the level of permanent strain. As
shown in FIGURE7 the trend is consistent among
various cycles. However, the level of total
permanentstrainincreasesasthenumberofcycles
increases.

The FTIR results show that nanosilica can improve

the aging resistance of the bitumen as reflected in
lowerlevelofcarboxylicacids(observedat14001440
cm1relatedtoOHband)andsulfoxide(observedat
~1050 cm1) in nanosilica modified specimen
compared to those in nonmodified specimens. Even
though carboxylic acids naturally exist in asphalt, its
concentration increases significantly due to oxidative
aging(FIGURE8).Tofurtherquantifythe
effect of nanosilica on reducing asphalt oxidative
aging, carbonyl index was calculated for both nano
silica modified and nonmodified specimens before
and after RTFO aging. As shown in TABLE 3, the
carbonyl index of aged nanosilica modified asphalt
binder decreases as the percentage of nanosilica
increases. Therefore, the nanosilica can be a
promising candidate for delaying oxidative aging of
asphaltbinder.
TABLE3.CARBONYLINDEXOFAGEDANDUNAGEDMODIFIEDBITUMEN

Unaged
neatbitumen
bitumen+2%
nanosilica
bitumen+2%
nanosilica
bitumen+2%
nanosilica

C=O(1690cm1)
0.082
0.044
0.039
0.052

Aged
neatbitumen
bitumen+2%
nanosilica
bitumen+2%
nanosilica
bitumen+2%
nanosilica

C=O(1690cm1)
0.095
0.055
0.041
0.031

(a)

FIGURE8FTIRSPECTRAANALYSISOFNEATANDMODIFIED
ASPHALTBINDER(A)UNAGEDASPHALTBINDERSAND(B)
AGEDASPHALTBINDERS

(b)
FIGURE7THERESULTSOFCREEPTESTFORUNMODIFIED
ANDMODIFIEDSAMPLESAT50C,(A)UNAGEDNEATAND
MODIFIEDASPHALTBINDERAND(B)AGEDNEATAND
MODIFIEDASPHALTBINDER

Conclusion
This paper investigates the merit of application of
nanosilicainasphaltbinderasanantiagingadditive.
To investigate the effectiveness of the nanosilica in
reducingasphaltaging,differentpercentagesofnano

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silica were added to neat asphalt binder. Asphalt

binderwasthenexposedtoshorttermoxidativeaging
using a rolling thin film oven (RTFO). To study the
changeinthechemical,rheologicalandmorphological
propertiesofasphaltbindersinpresenceofnanosilica,
the Superpave tests and Fourier transform infrared
spectroscopy (FTIR) were conducted. Rheological
characterizationofmodifiedandnonmodifiedasphalt
binder showed introduction of nanosilica enhances
therheologicalpropertiesofneatbinderbyincreasing
its storage modulus and elasticity. This in turn can
lead to improvement of pavement rutting resistance.
Furthermore, the FTIR spectrums showed that
introduction of nanosilica can delay the oxidative
aging process; this was reflected in the reduction of
therateofcarboxylformationafteragingasmeasured
bycarbonylindex.Therefore,thestudyconcludedthat
nanosilicacanbeapromisingcandidatetobeusedas
an antiaging additive in asphalt while enhancing
asphaltruttingresistance.

Kavussi, A. Barghabani, P.(2014). The influence of nano

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ACKNOWLEDGMENT

The research was carried out in the department of

polymer engineering, Amirkabir University of
Technology(AUT).

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EngineeringAspects,148(3),199211.

Farhad Zafari Born in Tehran, 1989, Graduate Student,

Department of Polymer Engineering(2012), Amirkabir
University of Technology (Tehran Polytechnic), Hafez
Avenue,Tehran,Iran
Mohammad Rahi Born in Tehran, 1980. BSc Polymer
Engineering (2004); MSc Polymer Engineering (2006)
Amirkabir University of Technology (Tehran Polytechnic),
HafezAvenue,Tehran,Iran
Nazanin Moshtagh Born in Mashhad, 1992, BSc Polymer
Engineering Student Amirkabir University of Technology
(TehranPolytechnic),HafezAvenue,Tehran,Iran
Hossein Nazokdast Born in Tehran, 1950, Associate
Professor, Department of Polymer Engineering, Amirkabir
University of Technology (Tehran Polytechnic), Hafez
Avenue,Tehran,Iran

69