Construction and Building Materials 239 (2020) 117827

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Construction and Building Materials

journal homepage: www.elsevier.com/locate/conbuildmat

The role of nanomaterials in reducing moisture damage of asphalt mixes

Seyed-Hamed Razavi, Amir Kavussi ⇑
Department of Civil and Environmental Engineering, Tarbiat Modares University, Tehran, Iran

h i g h l i g h t s

A cost-effective method for producing nano-hydrated lime is proposed using a planetary ball milling process.

The addition of nanomaterials reduces susceptibility of HMA mixes to moisture damage.

Among various nanomaterials, nano-hydrated lime contributed the most in increasing moisture damage resistance of HMA mixes.

a r t i c l e i n f o a b s t r a c t

Article history: Interest of researchers in using nanomaterials in asphalt mixes is increasing rapidly. In this research, the
Received 26 July 2019 effects of using various nanomaterials in asphalt mixes were investigated. In addition, the effects of two
Received in revised form 4 December 2019 different types of fillers at their conventional size and their nano-size in asphalt mixes were tested. Four
Accepted 6 December 2019
types of nanomaterials, namely nano-CaCO3, nano-hydrated lime, nano-bentonite and nano-silica, and
Available online 23 December 2019
two types of anti-stripping fillers, namely hydrated lime and CaCO3 were selected. Nano-hydrated lime
was produced using a planetary ball mill apparatus. In producing nano-hydrated lime, optimum combi-
Keywords:
nations of the main parameters that affect particle size reduction in milling process were determined
Tensile Strength Ratio (TSR)
Resilient modulus
applying trial and error procedure. Minimum particle size of the produced nano-hydrated lime was deter-
Modified asphalt mined using Scanning Electron Microscope (SEM) and Dynamic Light Scattering (DLS) tests. From these
Nano-sized filler tests, sizes of 125 and 208 nm were recorded, respectively.
Planetary Ball Mill Device With applying Field-Emission Scanning Electron Microscopy (FE-SEM) technique, homogenous distri-
Field-Emission Scanning Electron bution of the additives in a 60–70 bitumen binder was verified. Asphalt concrete mixes were prepared
Microscopy (FE-SEM) using the above additives and a siliceous type aggregate. Moisture damage of different mixes was eval-
Scanning Electron Microscope (SEM) uated applying modified Lottman test at different Freeze-Thaw (F-T) cycles. F-T cycles results indicated
X-ray diffraction spectrometer (XRD)
that Indirect Tensile Strength (ITS) values were reduced appreciably at the first cycle. In fact, it was
X-ray fluorescence (XRF)
shown that 4% nano-hydrated lime exhibited the most resistance against different F-T cycles. In addition,
Indirect Tensile Stiffness Modulus (ITSM) test was performed at 25 °C. From these tests, Tensile Strength
Ratio (TSR) and Index of Retained Resilient Modulus (IRMr) parameters were determined. Testing results
indicated that by adding 20% hydrated lime filler and 4% nano-hydrated lime to the binder, TSR values of
mixes increased to some 60%. In the case of using CaCO3 filler and nano-CaCO3, 60% increase in TSR, was
achieved when either 5% CaCO3 filler or 4% nano-CaCO3 were used. These results were validated perform-
ing resilient modulus test. IRMr of mixes containing 20% hydrated lime filler and 4% nano-hydrated lime
increased to 56% and 60%, respectively. IRMr values of asphalt mixes increased to 48% and 54% where 5%
CaCO3 filler and 4% nano-CaCO3 were added, respectively.
Ó 2019 Elsevier Ltd. All rights reserved.

1. Introduction asphalt from the aggregate particles, causing stripping distress

In wet weather conditions, dynamic traffic loading of vehicle
tires imparts moisture into pavement layers, creating pore water
pressure in asphalt layers. This will ultimately strip the film of
⇑ Corresponding author.
E-mail addresses: h.razavi@modares.ac.ir, se.hamed.razavi@gmail.com (S.-H.
Razavi), kavussia@modares.ac.ir (A. Kavussi).
[1]. Moisture damage is a complicated distress in bituminous pave-
ments that results in reduced stiffness and reduced structural
strength [2]. Researchers are looking to find methods for eliminat-
ing or reducing this problem [3]. Stiffness and moisture resistance
of Hot Mix Asphalt (HMA) is improved by addition of hydrated
lime [4].
In order to increase coating of aggregate particles, researchers
started to use nano-scale materials as new anti-stripping additives

https://doi.org/10.1016/j.conbuildmat.2019.117827
0950-0618/Ó 2019 Elsevier Ltd. All rights reserved.
2 S.-H. Razavi, A. Kavussi / Construction and Building Materials 239 (2020) 117827

in hot mix asphalt [5]. Nanomaterials due to their high surface area
and very low sizes (compared with the commonly used additives)
exhibit special features and unique characteristics to HMA mixes
[6]. International System of Units (SI) accounts nano as a prefix
to show 109 part of a unit and nanomaterials are conventionally
defined as materials having at least a dimension between 1 and
100 nm. Nevertheless, considering 100 nm as an upper limit for a
nanomaterial is not always accepted and still a matter of debate
[7]. There are two methods of producing nanomaterials, namely,
the top-down approach and the bottom-up approach. The top-
down approach consists of two methods. In the first, bigger struc-
tures are diminished in size until these reach to nano-scale. The
second approach consists of deconstruction into their composite
parts. The bottom-up approach is used where nanoparticles are
made from atomic or molecular fragments [8].
The addition of nano hydrophobic silane silica is a decent
method for reducing F-T cycle damage in asphalt pavements [9].
Results of ITS testing showed that mixtures containing nano-
silica, compared with control mixtures, depicted higher ITS values
[10]. Resilient Modulus (Mr) of asphalt mixtures improved as the
amount of nano-silica and hydrated lime were increased [11].
Using Zycosoil and lime slurry as additives enhanced resilient
modulus ratio and ITS of the mixtures [12]. Nano-clay, that is com-
posed of layered mineral silicates, is considered as an inexpensive
and abundant material. Nano-clay, based on its chemical composi-
tion and nanoparticle morphology, is classified into different
groups, including montmorillonite, bentonite, kaolinite, hectorite,
and halloysite [13]. Bentonite was used as nano-additive in bitumi-
nous concrete mixture and the result showed that mechanical per-
formance of mixes improved when 20% bentonite (by weight of
bitumen) was added [14].
Kavussi et al. [15] studied the effects of nano-clay and nano-
hydrated lime as additives on a continuously graded asphalt mix,
in order to reduce its moisture susceptibility. Result of their study
showed that addition of nano-hydrated lime at 5% (by weight of
asphalt binder) and nano-clay at 2%, increased TSR of asphalt mixes
by 52% and 49%, respectively. In another research, different per-
centages of nano-silica were added to asphalt mixtures and these
were tested against moisture susceptibility. They concluded that
the addition of 4% nano-silica (by weight of asphalt binder) was
the optimum content to reduce susceptibility of mixes to moisture
damage [16]. In ITS and ITSM tests, the addition of nano-silica at 6%
led to increase ITS and Mr values of 29% and 31%, respectively [17].
In another research, moisture resistance was tested on mixtures
containing limestone and siliceous aggregates, and two anti-
stripping agents (nano-organosilane and hydrated lime). Their
findings showed that using both anti-stripping additives, increased
adhesion bond between aggregate particles and bitumen [12]. A
study was performed on the impact of nano-CaCO3 on asphalt mix-
tures. In this study, different amounts of nano-CaCO3 and two
sources of aggregates were used. Multiple freeze–thaw cycles were
imparted and samples were subjected to Surface Free Energy (SFE)
and modified Lottman testing. Their findings showed that this
terials; while the role of nano-CaCO3 and nano-bentonite have not
been investigated in detail. In addition, in this research, nano-
hydrated lime was produced in laboratory from a conventional
hydrated lime filler using a rotary ball mill.
3. Experimental works
3.1. Materials
3.1.1. Asphalt binder and aggregates
A 60–70 penetration grade bitumen from Refinery of Tehran,
was used to prepare HMA mixes. Properties of the bitumen are
reported in Table 1. A siliceous aggregate type, with nominal max-
imum size of 12.5 mm, was used. Gradation was based on ASTM
Standard for dense aggregate gradation, as shown in Table 2 [20].
3.1.2. Additives
In order to investigate and compare the effects of various addi-
tives on moisture susceptibility of the HMA mix, the following
additives were utilized at different percentages:
a) A calcium carbonate filler (passing 75-mm sieve size) with
CaCO3 molecular formula
b) A hydrated lime filler (passing 75-mm sieve size)
c) Nano-hydrated lime of 125 nm size, produced using a rotary
ball mill.
d) Nano-calcium carbonate with CaCO3 molecular formula that
was designated as CAS registry number 471-34-1. This nano-
CaCO3 was manufactured by American Elements US Corpo-
rate Headquarters. Fig. 1 shows its SEM image.
e) Nano-silica with SiO2 molecular formula (i.e. silica fume),
that was produced by Evonik Industries AG – Germany. In
order to investigate practical size distribution of nanoparti-
cles, Transmission Electron Microscopy (TEM, EM 208 Phi-
lips) was performed. Fig. 2, shows a TEM image of the
nano-SiO2.
f) A Nano Clay, namely, bentonite with H2Al2O6 Si molecular
formula, produced by Sigma-Aldrich, USA, assigned with
designation CAS registry number 1302-78-9. The SEM (LEO
440i) image of this nanoparticle is shown in Fig. 3.
Characteristics of the nanomaterials are reported in Table 3.
Physical and geometrical properties of aggregate, hydrated lime
and CaCO3 fillers are reported in Table 4. By performing X-ray flu-
orescence (XRF) test, chemical properties of the fillers were deter-
mined (Table 5).
Table 1
Characteristics of the asphalt binder 60–70 penetration grade used in this research.
Properties Value Test Method

nanomaterial could be used as an additive to reduce water sensi- Penetration (100 g, 5 s, 25 °C), 0.1 mm 62 ASTM D5
tivity of HMA mixes [18]. Kavussi et al. [19] used locally manufac- Ductility (25 °C, 5 cm/min), cm 110 ASTM D113
Ring and ball softening point, °C 51 ASTM D36
tured nano-hydrated lime and nano-clay. The results of their
Specific gravity at 25 °C, g/cm3 1.016 ASTM D70
research indicated that using nanomaterials improved fatigue life Viscosity at 135 °C, cSt 292 ASTM D2170
of the nano-modified binders. Flash point, °C 269 ASTM D92-78

2. Research objectives Table 2

Gradation of the aggregates used.
The main purpose of this study was to investigate the effects of
Sieve (mm) 19 12.5 4.75 2.36 0.3 0.075
various nanomaterials in reducing moisture susceptibility of
Lower-Upper Limits 100 90–100 44–74 28–58 5–21 2–10
asphalt mixtures. Most of the previous research works had been
Passing (%) 100 95 55 35 15 6
limited to investigate the effects of some commonly used nanoma-
 S.-H. Razavi, A. Kavussi / Construction and Building Materials 239 (2020) 117827 3

Fig. 3. SEM image of nano-clay bentonite at 40 000 magnification.

Table 3
Properties of nanomaterials used in this study.

Properties Nano- Nano- Nano- Nano-

CaCO3 Silica Bentonite Hydrated
lime
Formula CaCO3 SiO2 H2Al2O6Si Ca(OH)2
Molecular Weight 100.09 60.08 180.1 74.09
(g/mol)
Appearance (Form) Powder Powder Powder Powder
Fig. 1. SEM image of nano-CaCO3 at 100 000 magnification.
Melting Point (°C) 825 1610 Decomposes 580
True Density (g/cm3) 2.93 2.4 2.35 2.24
Bulk Density (g/ml) 0.68 < 0:10 0.6–1.1 0.64
Average Particle 10–80 nm 11–  25; 000 125/208 nm
Size-APS (nm) 13 nm
Thickness of silicate – – 1–2 –
layers (nm)
Purity 99+% 99+% 99+% –
Specific Surface 30–60 200 500–750 25–50
Area-SSA (m2/g)
Color White White Light Tan to White
Brown
Morphology Cubic or Spherical Sheet Hexagonal
Hexagonal
SiO2 (%) – > 99 < 70 –

Table 4
Physical and geometrical properties of the fillers used in this research.

Properties Filler of the Hydrated lime filler CaCO3

aggregates filler
Retained on sieve 0 3.4 4.1
Fig. 2. TEM image of nano-SiO2. #200 (%)
Moisture (%) 2.01 0.41 0.06
pH value 6.9 12.4 9.5
Chemical name Granite Hydrated lime or calcium
According to previous research works, the amounts of nanopar-
calcium hydroxide carbonate
ticles which were used in asphalt mixes were between 1% and 8% Physical form Powder Powder Powder
by weight of binder. These amounts were enough to modify prop- Color Gray White White
erties of bituminous concrete mixes [18,21]. As the nanomaterials Shape of particle Angular Hexagonal Hexagonal
Molecular formula – Ca(OH)2 CaCO3
have very high surface area, in this research these were added first
Formula Weight (g/mol) – 74.09 100.09
to the control asphalt binder at 2% and 4% by weight of bitumen. In Melting/decomposition – 580 825
contrast to the nanomaterials and nano-fillers, conventional fillers, temperature (°C)
such as calcium carbonate (CaCO3) and hydrated lime (Ca(OH2)) fil- Bulk density (kg/cm3) 1009 481 961
lers were used as anti-stripping agents. These were used at the Specific gravity (g/cm3) 2.66 2.341 2.71
Specific Surface Area 1.79 4.82 3.28
amounts of 5, 10 and 20% (by weight of asphalt binder).
(m2/g)
Rigden voids (%) 38 62 34
3.2. Preparation of modified asphalt binders

In order to prepare modified asphalt binders, the aforemen- nanomaterials were used) was of great importance, a high shear
tioned percentages of additives were added to the neat asphalt bin- rate mixer, at high rotation rate and at high temperatures was uti-
der. As homogenous distribution of the additives (especially where lized. Mixing conditions, including mixing time, rotation speed and
4 S.-H. Razavi, A. Kavussi / Construction and Building Materials 239 (2020) 117827

Table 5 3.4. Laboratory tests

XRF testing results of the fillers.

Properties Filler of the Hydrated lime CaCO3 3.4.1. XRD test

aggregates filler filler One of the most important non-destructive tests that is per-
CaO (%) 1.704 68.939 64.805 formed to identify crystalline phases of materials is X-ray diffrac-
SiO2 (%) 69.102 1.212 0.654 tion spectrometer (XRD). X-rays are directed toward samples by
Al2O3 (%) 13.352 0.263 0.197 applying the voltage and reflected X-rays are gathered by the
Fe2O3 (%) 0.975 0.239 0.094
MgO (%) 1.025 0.711 3.426
detector. Results are usually reported in an XY plot; x-axis showing
Na2O (%) 1.061 – 0.05 the angle between the radiated and reflected X-ray and y-axis
MnO (%) 0.049 0.028 – depicting the counts of reflected X-ray. Compositions of the aggre-
Zr (%) – 0.004 – gates used in this study, as determined by XRD analysis (Explorer,
K2O (%) 2.257 0.117 0.029
G.N.R, Italy) are reported in Fig. 4. XRD pattern was measured using
P2O5 (%) 0.043 0.03 0.043
SO3 (%) 0.035 0.105 0.485 a scintillator detector over the 2h range of 5°–50°. X-ray source was
Cl (%) 0.013 0.029 0.035 a conventional X-ray tube with a Cu-Ka target operated at
Sr (%) 0.034 0.023 0.581 1.541874 Å, 40 kV and 30 mA.
Loss on ignition (L.O.I)*(%) 10.35 28.3 29.6 Regarding the XRD pattern in Fig. 4, it can be seen that main
*
L.O.I Method: sample put in furnace for 1 h at 950 °C. mineralogical constituents of the aggregate were Silicon Oxide
(SiO2) and magnesium calcium carbonate. In addition, most of
the peaks and the maximum peak value at 2 theta of 27° were
for silicon oxide. Therefore, as it can be seen in Fig. 4, the aggre-
Table 6 gates consisted of almost 70% SiO2. The main cause of this selection
Mixing conditions for preparing the modified binders.
was that siliceous aggregates are more susceptible to moisture
Additive Mixing damage due to their mineralogy and surface structure. In this case,
Time (min) Speed (rpm) Temperature (°C) the effectiveness of using anti-stripping additives will be more
CaCO3 Filler 25 3600 165
pronounced.
Nano-CaCO3 35 5200 160
Hydrated lime Filler 25 3600 165 3.4.2. FE-SEM test
Nano-hydrated lime 35 5200 160 FE-SEM is one of the useful tools for high resolution surface
Nano-silica 50 2600 160
imaging that characterizes nanomaterials and nanostructures in
Nano-clay (bentonite) 45 4000 160
asphalt mixes. In this study, in order to show the effects of mixing
time and to make sure of homogenous distribution of the additives,
mixing temperatures are reported in Table 6. In order to maintain FE-SEM (FEI-Nova Nano SEM 450) images were taken at different
the similar condition, the neat binder was stirred too applying mixing time and processing.
temperature 160 °C, time 35 min, and speed 4000 rpm as the aver-
age values from Table 6 results. 3.4.3. Production of nano-hydrated lime
The milling process that was adopted in this research was a top-
3.3. Mixture design down approach for producing nano-hydrated lime from hydrated
lime filler [23]. This technique has the advantage of using conven-
Optimum asphalt binder content of the mixture was deter- tional milling units to produce nano-size fillers. In fact, as for def-
mined based on Marshall Method with 75 blows on each side of inition, planetary rotary ball mills are low-cost laboratory units
the cylindrical samples for high traffic loading condition [22]. It that can reduce particle sizes into nano-size materials. In these
is necessary to mention that mixture design was performed using mills, a high centrifugal force is applied, achieving appropriate
the neat asphalt binder (i.e. without using any additives). There- mixing and homogenization of materials. Schematics of the mixing
fore, optimum binder contents of mixes were taken equal in all unit of a planetary rotary ball mill is shown in Fig. 5. The steel ball
mixtures, eliminating the role of binder contents in analysis of mill has two or four ball grinding containers that are mounted
the test data. eccentrically on a turn plate. Direction of the plate movement is
Two groups of Marshall specimens were fabricated. The first opposite to the grinding containers. When the plate spins, the con-
group consisted of samples having six bitumen contents and the tainer axis makes the planetary movement, and the balls and sam-
optimal asphalt binder was determined. The second group was fab- ples inside the containers are impacted strongly in high-speed
ricated at optimal binder content with the purpose of evaluating movement. Samples are then ultimately grounded into powder.
mechanistic properties of the HMA. With reference to Table 7, it Three types of milling methods are available, namely, dry mill,
can be seen that volumetric properties corresponding with the wet mill, and vacuum mill. Two or four grinding tanks can work
5% bitumen content met all the specification limits. This in the together. In order to perform the process a small amount of Process
graphs were found to be 5.1%. Control Agent (PCA) is introduced into the jar of the apparatus
together with powders and steel balls. PCAs create notable influ-
Table 7 ence on the particle size, likewise on the structural behavior and
Results of Marshall test (average of three samples). thermal stability of the milled powders, when compared with
milling synthetized materials without presence of a surfactant
Bitumen Air voids VMA* VFA* Marshall Marshall
content (%) content (%) (%) (%) stability (kN) flow (mm) [24].
In a research work, the effect of applying uniform size balls,
4.0 6.04 19.3 68.7 7.79 2.41
4.5 5.01 17.71 71.7 9.46 2.52 compared with different diameters balls, was investigated. The
5.0 4.12 15.46 73.4 10.54 2.64 results showed that producing CaCO3 in planetary ball mills will
5.5 3.85 15.51 75.2 9.75 2.7 be improved when uniform-size balls are used [25]. In this
6.0 3.25 15.97 79.6 9.45 2.81 research, nano-hydrated lime was manufactured, using a vertical
6.5 3.01 16.23 81.5 8.78 3.21
laboratory planetary ball mill set (Feritsch, Pulverisette 5 Classic
*
VMA: voids in mineral aggregate, VFA: voids filled with asphalt. Line-Germany). The main parameters that affected particle size
 S.-H. Razavi, A. Kavussi / Construction and Building Materials 239 (2020) 117827
Fig. 4. Result of XRD test on the aggregates.
Mill Jar
Support
Plate
Fig. 5. Schematic shape of the laboratory planetary ball mill.
reduction, consisted of rotation speed, milling time, size of balls,
medium of milling and Ball to Powder Ratio (BPR). These parame-
ters were optimized, applying trial and error method. Based on
previous studies, 2-Propanol material (at 5% by weight of hydrated
lime) was used as PCA. In addition, uniform steel balls and a 5:1
ratio as BPR were selected [15,19,26–29]. Hydrated lime filler
was milled for 9 h at 250 rpm speed. Using Dynamic Light Scatter-
ing (DLS, ZSP, Malvern Instruments Ltd., Worcestershire, UK) and
SEM (Leo 1450VP, Zeiss, Germany) machines. The average particle
size of this nanomaterial was measured at different milling times.
The diameter and weight of each of the uniform steel balls were
5 mm and 33 g, respectively.
3.4.4. Modified Lottman test
In order to evaluate water sensitivity of mixes, modified Lott-
man test (AASHTO T283) was performed [30]. In this research,
one, two, and three F-T cycles were applied on specimens to clearly
show resistance of various modified mixes against F-T cycles. Each
5
specimen was of 1002 mm diameter and 702 mm height. With
this purpose, for each mix composition, twelve specimens were
prepared consisting of four groups; each of three specimens (one
group for dry ones and other groups for one, two, and three F-T
cycles).
Marshall Hammer was used to compact the specimens. All sam-
ples contained air voids between 6.5% and 7.5%. Different trials
were made with Marshall Hammer in order to achieve the desired
air voids. Conditioned samples were subjected to moisture before
testing. In order to access the level of saturation (between 70%
and 80%), a vacuum of 10–26 inHg absolute pressure was applied.
The vacuum-saturated samples were then placed in freeze-thaw
condition (at 18 °C for 16 h and water bath at 60 °C for 24 h).
Samples were kept at 25  0.5 °C when ITS testing was performed
at the loading rate of 2 inch=min. Failure loads were recorded and
the average ITS values for both dry and wet samples were calcu-
lated. TSR was used as an index for evaluating moisture sensitivity
of the compacted asphalt samples. Calculations were made based
on equations in standard AASHTO T283 [30].
3.4.5. ITSM test
One of the major factors in analysis and design of asphalt pave-
ments is stiffness modulus (or resilient modulus) which indicates
the ability of asphalt layers to spread traffic loads on the underly-
ing layers. Resilient modulus is defined as the ratio of deviator
stress to recoverable strain of a sample under cyclic loading.
The resilient modulus is directly affected by loss of adhesion
and cohesion [31]. In order to investigate susceptibility of asphalt
mixtures to water damage, resilient modulus is more sensitive
than the tensile strength [32]. This non-destructive test was per-
formed according to ASTM D4123 procedure [33]. Using a Univer-
sal Testing Machine (UTM-14P), samples were tested at 25 °C by
applying a haversine loading waveshape consisting of 0.1-s loading
time and 0.9-s rest time and frequency of 1 Hz. Samples were kept
at the test temperature for 24 h in the temperature control cham-
ber before testing. The chamber was equipped with a reference
6 S.-H. Razavi, A. Kavussi / Construction and Building Materials 239 (2020) 117827
specimen containing two thermometers to measure and record the
core and skin temperatures. Each sample was tested twice, at a 90-
degree rotation, and the mean values of both tests were reported as
stiffness modulus. The load was induced along the vertical diamet-
ric axis of the cylindrical sample and two Linear Variable Differen-
tial Transducers (LVDTs) measured its horizontal deformation.
Specimens were preconditioned by initial load cycles; 75 precondi-
tioning pulses were applied to resilient deformations become
stable. Then 10 pulses of maximum loading were applied along
the diameter. Resilient modulus of samples was calculated by the
software connected to the test set up using the following equation:
Pð# þ 0:27Þ
Mr ¼
t  DH
where Mr is resilient modulus (MPa), P is cyclic load (N) that was
2500 N in this study, # is the Poisson’s ratio (assumed 0.35), t is
the specimen thickness (mm), and DH is the recoverable horizontal
deflection (mm).
3.4.6. Index of retained resilient modulus (IRMr) test
In order to evaluate moisture susceptibility of asphalt mixtures,
index of retained resilient modulus (IRMr) was defined as in Eq. (2)
below:
Mr of conditioned specimen
IRMr ¼  100
Mr of dry ðcontrolÞ specimen
where Mr is resilient modulus.
For conditioning test specimens in the determination of the
IRMr, Lottman procedure was employed. IRMr value of 70% was
taken as a minimum acceptable value to ensure good performance
(a) Nano-SiO2 modified asphalt-10 min mixing
(c) Nano-clay modified asphalt-5 min mixing
Fig. 6. FE-SEM images of nano-modified binders mixed at different mixing times.
against stripping of HMA mixtures [31]. IRMr is an indicative of
mix’s resistivity to moisture damage. The greater IRMr, the better
the mix resistance to damage. In this test, asphalt specimens with
diameter of 1002 mm and height of 552 mm were utilized.
4. Results and discussion
4.1. FE-SEM test results
Fig. 6 shows FE-SEM images of mixes at different mixing times.
These at magnification of 4000 times showed that when 2% nano-
silica were mixed with the binder, after 10 min the accumulated
ð1Þ nanomaterials could still be seen quite clearly; while these rarely
could be seen after 50 min of mixing. The 4% nano-bentonite mod-
ified binder when it was mixed for 5 min, was not homogenously
mixed with the binder. It was well-dispersed after 45 min of mix-
ing. With using this technique, it was confirmed that the adopted
circumstances were appropriate for mixing these nanomaterials
with the bitumen binder. A previous study revealed that by apply-
ing a mechanical mixer at 1500 rpm speed and a mixing tempera-
ture of 145 °C ± 5 °C, the optimum mixing time will be around
45 min for nano-silica and 60 min for nano-clay [34]. FE-SEM
images of Figs. 7 and 8 at two magnifications of 600 and 1200
times indicate that all the other additives were homogenously
ð2Þ mixed with bitumen.
4.2. Production of nano-hydrated lime results
Several methods are available to characterize Average Parti-
cle Size (APS) of nanomaterials. Each technique has its own
(b) Nano-SiO2 modified asphalt-50 min mixing
(d) Nano-clay modified asphalt-45 min mixing
 S.-H. Razavi, A. Kavussi / Construction and Building Materials 239 (2020) 117827 7

a-1) magnification of 600 times a-2) magnification of 1200 times

a) 2% nano-hydrated lime modified asphalt

b-1) magnification of 600 times b-2) magnification 1200 of times

b) 2% nano-CaCO3 modified asphalt
Fig. 7. FE-SEM images of nano-modified binders at different magnifications.

advantages and limitations. Therefore, a combination of at least
two methods, one of which should be a microscopic method, is
highly recommended [35].
During ball mill processing of nano-hydrated lime, the APS of
this material was determined at various milling times applying
SEM and DLS tests. The results are reported in Table 8. Since hydro-
dynamic diameters of the particles are measured in DLS test, in this
research, SEM test was performed to measure APS values beside
DLS test. Results of DLS and SEM tests indicated that APS values
of all samples in DLS technique were bigger than their SEM mea-
surements. The finest particle size was observed in sample that
was milled for 5 h in both techniques. According to SEM images
(analyzed by Image-J software) and DLS test, the minimum
achieved particle sizes were 125 and 208 nm, respectively. As it
can be seen from Fig. 9, morphology and size of the powders were
severely changed after 5 h ball-milling. With this processing, the
produced nanomaterial showed semi-spherical shape and consid-
erably smaller sizes than those that were produced after ball
milling for 1 and 3 h. Particle sizes did not exhibit a significant
change for 9 h of milling, compared with 7 h. The reason might
be that during ball mill processing, the fine materials experienced
cold welding (i.e. particle adhesion and sticking). Morphology and
microstructure of the milled powders changed with changing the
milling time. Considering SEM images of the samples before and
after ball mill processing, it was resulted that the flat and smooth
plates of hydrated lime particles were changed into semi-spherical
shape with high specific area.
Previous research work [15] indicated that APS of the produced
nano-hydrated lime was 281 nm, as determined with DLS tech-
nique. In the present work, APS of this material was produced in
smaller sizes than the above research. In addition to DLS, SEM test
as a microscopic technique was applied to measure APS values.
4.3. Modified Lottman test results
Greater ITS and TSR values indicate that the mix will have better
resistance to water damage. Figs. 10 and 11 show results of ITS and
TSR values of asphalt mixes containing various antistripping addi-
tives. With reference to these figures it can be seen that ITS and
TSR values of the modified mixes were greater than the neat mix.
Among the various samples, those containing 20% hydrated lime
filler, 5% CaCO3 filler, 2 and 4% of nano-hydrated lime and nano-
CaCO3 met the AASHTO T283 specification requirement of mini-
mum 80% TSR. As it can be seen in Fig. 11, the control mix did
not satisfy the specification requirement. This might be due to as
a result of using a siliceous aggregates type in this research. Slick
and smooth areas of siliceous aggregates make these more prone
to stripping. In determining adsorption characteristics and strip-
ping resistance, aggregates properties are much more influential
than asphalt properties [36]. The worst adhesion properties of silic-
eous aggregates, compared with limestone aggregates, were
proved by researchers [12,18]. The reason might be that in lime-
stone aggregates, both anionic and cationic surfactants are natu-
rally present in bonding between bitumen and calcium ions.
8 S.-H. Razavi, A. Kavussi / Construction and Building Materials 239 (2020) 117827

a-1) magnification of 600 times a-2) magnification of 1200 times

a) 10% hydrated-lime filler modified asphalt

b-1) magnification of 600 times b-2) magnification of 1200 times

b) 10% CaCO3 filler-modified asphalt
Fig. 8. FE-SEM images of hydrated lime and CaCO3 fillers modified binders at different magnifications.

Table 8 Regarding resistance to moisture damage, nano-hydrated lime

APS of hydrated lime in ball mill processing as determined with SEM and DLS
methods.
Ball milling time (h) APS* – SEM (nm)
0 1942
1 770
3 521
5 125
7 204
9 216
*
APS: Average Particle Size.
While in siliceous aggregates only cationic surfactants bond
strongly with silica atoms. As a consequence of this, on siliceous
aggregates, anionic surfactants are easily replaced by water [36].
The composition and surface chemistry of the aggregates influ-
ence strongly asphalt-aggregate interactions. Asphalt-aggregate
interactions are important in the adhesion of asphalt to aggregate
which is effective on moisture damage [36]. Surface modification
of the aggregates is one key aspect of hydrated lime modification.
Hydrated lime, by precipitation of calcium ions onto aggregate par-
ticles makes these prone to stick with bitumen and improve bond-
ing properties between these [37].
Interfacial tension is one of the most important factors that
affect coating of aggregate surface with asphalt. The role of nano-
materials is to reduce this factor, resulting in close contact
between aggregate particles and asphalt. This will improve resis-
tance of mixes to moisture damage.
and nano-CaCO3 exhibited better performance than nano-SiO2
and nano-bentonite. The reason may be attributed to chemical
APS – DLS (nm) properties and the shapes of these nanomaterials. Nano-hydrated
4059 lime and nano-CaCO3 consist of calcium oxide while nano-SiO2
1639 and nano-bentonite consist of silica. Also, as reported in Table 3,
967 nano-hydrated lime and nano-CaCO3 have hexagonal shape, but
208
309
nano-SiO2 and nano-bentonite have spherical and sheet particles,
324 respectively.
According to ITS and TSR results, nano-hydrated lime and nano-
CaCO3 showed almost similar behavior against water damage. This
fact might be associated with their similar properties. In fact, as it
can be seen from Table 3 both have almost equal Specific Surface
Area (SSA) and shape. These are important factors that affect the
adhesion of asphalt binder to aggregate.
Maximum TSR values, corresponded with 4% nano-hydrated
lime and 20% hydrated lime filler. The optimum values for CaCO3
filler and nano-CaCO3, resulted to be 5 and 4%, respectively. This
proved that the optimized TSR values were obtained at lower per-
centages when using nanomaterials (instead of their actual fillers).
This finding is in good agreement with findings of other research-
ers [15,38]. The reason might be attributed to physical properties
of these materials. SSA of these materials at the state of their
nano-sizes were greater than their filler sizes. According to the
Tables 3 and 4, SSA of nano-hydrated lime and hydrated lime filler
were 25–50 and 4.82 m2/g respectively. This property was 30–60
and 3.28 m2/g for nano-CaCO3 and CaCO3 filler, respectively. The
high specific surface area increases contact of material particles
 S.-H. Razavi, A. Kavussi / Construction and Building Materials 239 (2020) 117827 9

(a) 0 h (b) 1 h

(c) 3 h (d) 5 h

(e) 7 h (f) 9 h

Fig. 9. SEM images of hydrated lime after different ball milling times.

with the asphalt binder leading to stronger bond between them.
Hence, resistance to moisture damage will be improved.
As it can be seen in Fig. 10, with increasing hydrated lime and
CaCO3 fillers up to 10%, ITS in dry condition increased, while 20%
of these fillers resulted in reduced ITSdry values. The reason may
be attributed to the high amounts of these fillers in mixes. Hence,
agglomeration and improper dispersion of these materials resulted
in deteriorated performance of the modified bitumen [6,39].
The results of nano-CaCO3 were in agreement with the results
achieved in another research [18]. The results of nano-bentonite
additive showed that with increased amount of this nanomaterial,
TSR values reduced. The reason might be that bentonite consists of
a high percentage of silica. Hence, it accounts a hydrophilic mate-
rial. In addition, as it can be seen in Fig. 10 with increased nano-
bentonite content, ITSdry value increased, while ITSwet decreased,
resulting in reduced TSR value. A similar trend was observed in
nano-bentonite modified mixes [40].
As it can be seen in Fig. 11, with increased amount of nano-SiO2,
TSR values of mixes decreased. This can be attributed to the hydro-
philic properties of this nanomaterial. The trend of decreased TSR
values of nano-SiO2 modified mixes in this research was in contrast
with findings in previous research works [11,16,41], but depicts a
similar trend with the findings of another research [17]. The reason
for this can be attributed to the type of nano-silica used in this
study. There are two types of nano-silica: hydrophobic and
hydrophilic silica nanomaterials. Hydrophobic silica is obtained
10 S.-H. Razavi, A. Kavussi / Construction and Building Materials 239 (2020) 117827
ITS-Dry
1400
1200
1000
ITS (kPa)
800
600
400
200
0
control
5% HL
10% HL
20% HL
2% NHL
4% NHL
2% NL
Fig. 10. ITS testing results of mixes with and without additives at dry and wet conditions.
by surface modification of nano-silica in hydrophobic groups. In
this study nano-hydrophilic silica was used.
In fact, the addition of 20% (by weight of bitumen) of hydrated
lime filler and 4% nano-hydrated lime to the binder resulted in
increased TSR values of bituminous mixes by 60 and 61% respec-
tively. TSR values of asphalt mixes increased to 57 and 59% when
5% CaCO3 filler and 4% nano-CaCO3 were added, respectively.
ITS and TSR of mixes after conditioning under one, two, and
three F-T cycles are reported in Figs. 10 and 11. As it can be seen
in these figures, with increasing number of F-T cycles, ITS and
TSR values of the samples decreased. Similar observations were
reported by several researchers for the influence of increasing
the number of F-T cycles on ITS and TSR values of asphalt mixes
[18,42,43]. This trend could be attributed to loss of adhesion
between aggregate particles and binder and/or cohesion within
the bitumen binders. At all F-T cycles that were applied in this
research, ITS and TSR values of mixes containing additives were
greater than the control sample.
In order to investigate the decrease of ITS under different F-T
cycles, the percentage of drop in ITS values of control and modified
asphalt mixes are reported in Table 9. The reduction of ITS value
was much higher for control mixture than modified ones. As it
can be seen, the major reduction in ITS values occurred after
undergoing the first F-T cycle, then the rate of reduction decreased
for 2 and 3F-T cycles.
With comparing nano-silica and nano-bentonite for evaluation
of moisture damage of HMA, it can be concluded that nano-
bentonite is slightly more effective than nano-silica in improving
mixes to resist against moisture damage. Also, as reported in
Table 9, at the same amounts of additives the rate of reduction of
ITS values in nano-bentonite modified mixes under different F-T
cycles was less than nano-silica modified mixes. The reason might
be attributed to the physical and chemical properties of these
nanomaterials. As reported in Table 3, both nanomaterials were
consisted of silica, but nano-SiO2 had more silicon oxide than
nano-bentonite. Also, SSA of these nanomaterials was different
from each other. Nano-bentonite had greater SSA than nano-
silica. Therefore, it is expected that more interactions would occur
between nano-bentonite and binder and the moisture damage of
HMA will be improved. Moreover, shape of these nanomaterials
might influence the results. According to Figs. 2 and 3, and Table 3
1 cycle 2 cycle 3 cycle
10% L
20% L
5% L
2% NC
4% NC
4% NL
2% NS
4% NS
Mixtures
nano-silica had spherical shape while nano-bentonite particles
consisted of sheets with great SSA values.
These results show that mixtures containing anti-stripping
additives were highly enhanced against moisture damage. Among
these, the mix containing 4% nano-hydrated lime was more effec-
tive than the other specimens.
4.4. Resilient modulus test results
Findings of the resilient modulus test for dry and conditioned
HMA mixes at 25 °C are shown in Fig. 12. As it can be seen, the stiff-
ness modulus of modified samples is greater than the control mix.
Each additive contributes to stiffen the binder which results in
increased resilient modulus. In dry samples, the addition of
nano-additives up to 4% and anti-stripping fillers up to 10%, the
stiffness modulus increased. In contrast with adding 20% hydrated
lime or CaCO3 fillers the resilient modulus decreased. The reason
might be that the high amounts of these fillers caused agglomera-
tion, leading to a negative effect on performance of the modified
binder [6,39]. The reason for the increased Mr value in the dry sam-
ples containing high amounts of nanomaterials could be attributed
to very high surface area of nanoparticles. As a result of this, more
interaction might exist between bitumen and nanoparticles. In
fact, excessive absorption of the oils in asphalt cement, leads to
greater stiffness values [41].
Other researchers observed a similar trend of increased Mr in
dry condition for hydrated lime filler modified mixes [11]. The rea-
son for increased stiffness of hydrated lime filler might be that
hydrated lime has greater porosity than other mineral fillers. This
property differentiates hydrated lime from other fillers. Mineral fil-
lers generally have 30–34% air voids in dry compacted state (Rig-
den voids); while hydrated lime filler has this between 60 and
70% [37]. As reported in Table 4, hydrated lime filler had Rigden
voids of 62% which is greater than all the other fillers.
As it can be seen in Fig. 12, Mr in a dry state increased as a result
of increased nano-SiO2 content. This is similar to the results of
previous researches [16,41,44]. Among mixes, 4% nano-SiO2
resulted in mixes to have the most resilient modulus in dry condi-
tions; while in wet conditions weak performance was observed.
The reason for this fact is related to chemical properties of this
material.
 S.-H. Razavi, A. Kavussi / Construction and Building Materials 239 (2020) 117827 11

control 5% HL 10% HL 20% HL control 2% NHL 4% NHL

90 90
80 80
70 70

TSR (%)
TSR (%)

60 60
50 50
40 40
30 30
20 20
10 10
1 2 3 1 2 3
Number of F-T Cycles Number of F-T Cycles
a) Hydrated lime filler b) Nano-hydrated lime

control 5% L 10% L 20% L control 2% NL 4% NL

90 90
80 80
70 70
60

TSR (%)
60
TSR (%)

50 50
40 40
30 30
20 20
10 10
1 2 3 1 2 3
Number of F-T Cycles Number of F-T Cycles
c) CaCO3 filler d) Nano-CaCO3

control 2% NC 4% NC control 2% NS 4% NS
90 90
80 80
70 70
TSR (%)

TSR (%)

60 60
50 50
40 40
30 30
20 20
10 10
1 2 3 1 2 3
Number of F-T Cycles Number of F-T Cycles
e) Nano-Clay f) Nano-SiO2

Fig. 11. TSR testing results of mixes containing various additives at different F-T cycles.

Table 9
Percentage of changes in ITS values of mixes after different F-T cycles.

F-T cycles Mixture

control 5% HL 10%HL 20% HL 2%NHL 4%NHL 2%NL 4%NL 5%L 10%L 20%L 2%NC 4%NC 2%NS 4%NS
1 48.7 40.2 31.7 17.8 18.4 17.2 19.6 18.2 19.4 23.8 28.5 38.7 45.8 44.7 47.5
2 76.6 45.2 35.1 20.8 23.7 20.4 26.5 22.7 24.9 31.2 36.7 42.5 51.2 53.2 56.8
3 86.2 47.4 37.4 22.8 26.6 21.6 30.6 25.1 27.1 34.6 42 45.1 54.9 58.9 63.6

HL: Hydrated Lime, NHL: Nano-Hydrated Lime, L: CaCO3, NL: Nano CaCO3, NC: Nano Clay, NS: Nano SiO2.

Generally, for all mixes resilient modulus values were
decreased after F-T conditioning. However, this parameter was
profoundly enhanced when anti-stripping additives were used.
To investigate potential of mixtures to stripping, IRMr was used,
similar to what was performed in another research [12]. Resilient
modulus ratio (IRMr) results of samples are presented in Fig. 13.
Generally, IRMr values of the modified mixtures are greater than
the unmodified mixtures. Among the specimens, those containing
20% hydrated lime filler, 5% CaCO3 filler, 2 and 4% of nano-hydrated
lime and nano-CaCO3 met the required minimum 70% IRMr.
Among various additives, nano-CaCO3 and nano-hydrated lime
had higher IRMr values and showed better performance in resis-
tance to moisture damage than nano-bentonite and nano-SiO2
materials. This can be attributed to their chemical properties. As
it was mentioned before, nano-CaCO3 and nano-hydrated lime
consisted of calcium oxide while nano-bentonite and nano-SiO2
were of silica type.
As it can be seen in the results of resilient modulus of mixes,
nano-hydrated lime and nano-CaCO3 had greater Mr, compared
with hydrated lime and CaCO3 fillers at lower amounts. The reason
12 S.-H. Razavi, A. Kavussi / Construction and Building Materials 239 (2020) 117827

Dry Wet
3500

3000

2500
Mr (MPa)

2000

1500

1000

500

0
5% HL

2% NL

4% NL

10% L

20% L

2% NS

4% NS
5% L

2% NC

4% NC
control

2% NHL

4% NHL
10% HL

20% HL

Fig. 12. Resilient modulus of mixes containing various additives at dry and wet conditions.

90

80 75 76.9
73.9 71.9 74
71
70 66
63.1 62.1
55.1 57.1
60 53 54
50.9
48.1
50
IRMr (%)

40

30

20

10

0
5% HL

2% NL

4% NL
10% HL

20% HL

5% L

10% L

20% L
control

2% NS

4% NS
2% NC

4% NC
2% NHL

4% NHL

Fig. 13. IRMr results of mixes.

can be attributed to physical properties and nanostructure of these Table 10 reports the effects of anti-stripping additives on
materials. SSA property is related to the particle size of the filler. asphalt mixes. It reports the percentage of changes in Mr and IRMr
Hence, greater SSA values will be resulted in nanoscale particles. values of the modified specimens, compared with the control spec-
Therefore, it is expected that these materials absorb more the oily imen. As it can be seen, by adding 20% hydrated lime filler and 4%
components of the bitumen binder, making it stiffer. nano-hydrated lime to bitumen resulted in improving the IRMr

Table 10
Percentage of increase in Mr and IRMr values of the modified mixtures.

Mixture
Control 5% HL 10%HL 20% HL 2%NHL 4%NHL 2%NL 4%NL 5%L 10%L 20%L 2%NC 4%NC 2%NS 4%NS
Mr Dry 0 24.4 46.5 41.9 41.1 48.6 33.8 50.6 26.1 43.2 32.8 31 38.5 36.7 54.3
MrWet 0 42.5 92.1 121.3 116.8 137.6 100.1 131.9 86.1 96.5 71.3 55.4 52.5 53.5 63.4
IRMr 0 14.5 31.1 55.9 53.6 59.9 49.5 54 47.6 37.2 29 18.7 10.1 12.3 5.9

HL: Hydrated Lime, NHL: Nano-Hydrated Lime, L: CaCO3, NL: Nano CaCO3, NC: Nano Clay, NS: Nano SiO2.
 S.-H. Razavi, A. Kavussi / Construction and Building Materials 239 (2020) 117827
values of 56% and 60%, respectively. IRMr values of asphalt mixes
increased to 48% and 54% when 5% CaCO3 filler and 4% nano-
CaCO3 were added, respectively. Similar to TSR results, the mix
with 4% nano-hydrated lime had the highest IRMr value and
showed the most resistance to moisture damage.
More laboratory and field studies would be required to verify
the findings of this research before they can be applied in field
projects.
5. Conclusions
From the process of producing nano-hydrated lime from a con-
ventional hydrated lime filler, and with performing modified Lott-
man and resilient modulus tests of the modified HMA mixes
containing two types of fillers and four types of nanomaterials,
the following conclusions can be drawn:

A cost-effective method for producing nano-hydrated lime was
recognized using a planetary ball mill unit. At the optimum con-
dition, minimum particle sizes of nano-hydrated lime were 125
and 208 nm when SEM and DLS tests were performed,
respectively.

The optimum conditions for producing nano-hydrated lime
were consisted of 5 h of milling, using uniform steel balls,
applying 250 rpm rotation and a 5:1 ratio for the BPR.

FE-SEM images showed good dispersion of the additives in hot
bitumen binder when a high shear mixer was used, applying the
specified mixing conditions.

The addition of 20% hydrated lime filler and 4% nano-hydrated
lime to the binder promoted TSR values of bituminous mixes
by 60 and 61%, respectively. Also, with the addition of 5% CaCO3
filler and 4% nano-CaCO3, TSR values of bituminous mixes
increased by 57 and 59%, respectively.

With using anti-stripping additives, IRMr of mixes improved
appreciably. By adding 20% hydrated lime filler and 4% nano-
hydrated lime to bitumen, IRMr values of mixes enhanced by
56% and 60%, respectively. IRMr values of asphalt mixes
increased to 48% and 54% when 5% CaCO3 filler and 4% nano-
CaCO3 were added, respectively.

With adding nano-bentonite and nano-silica at greater levels
than the optimum amounts, ITSdry and Mrdry improved consid-
erably, while TSR and IRMr values decreased. This was attribu-
ted to hydrophilic property of these nanomaterials.

In order to increase water resistance of bituminous mixes,
application of nanomaterials at lower percentages is recom-
mended rather than using high amounts of conventional anti-
stripping fillers.

Among all materials tested, nano-hydrated lime improved resis-
tance of asphalt mixes against moisture damage the most.
CRediT authorship contribution statement
Seyed-Hamed Razavi: Conceptualization, Data curation, Formal
analysis, Investigation, Writing - original draft. Amir Kavussi: Con-
ceptualization, Supervision, Review & editing the manuscript.
Declaration of Competing Interest
The authors declare that they have no known competing finan-
cial interests or personal relationships that could have appeared
to influence the work reported in this paper.
13
Acknowledgments
Researchers would like to thank Dr. Nourolhoda Razavi and Dr.
Sajjad Janfaza for their support in providing nanomaterials and
analyzing DLS and SEM tests.
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