Measurement 93 (2016) 359–371

Contents lists available at ScienceDirect

Measurement
journal homepage: www.elsevier.com/locate/measurement

Evaluation of mechanical properties of nano-clay modified asphalt

mixtures
Erol Iskender
Karadeniz Technical University, Faculty of Technology, Civil Engineering Department, 61830 Trabzon, Turkey

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

Article history: This study aimed to investigate the performance of nano-clay modified asphalt mixtures. This study
Received 25 November 2015 aimed to investigate the performance of nano-clay modified asphalt mixtures. Three different nano-
Received in revised form 9 July 2016 clay materials were selected and each modifier was used with three different concentrations (2%-3.5%-
Accepted 11 July 2016
5%) as substituted for filler.
Available online 12 July 2016
Modified Lottman including hot water conditioning (conditioning 1) and cold water conditioning (con-
ditioning 2) systems were used. Models of water damage were used on half of the identical compacted
Keywords:
samples. Cracking, stripping and rutting evaluations were realized with AASHTO T 283 Modified
Asphalt mixtures
Stripping
Lottman Test and repeated creep tests (RCT) with Nottingham asphalt tester (NAT). Indirect tensile
Rutting strength (ITS) tests were realized with control and two types of conditioning systems but RCT were
Cracking applied with control and Lottman water damage procedure. Nano-clay materials increased rutting resis-
Nano-clay materials tance of samples with Lottman water damage conditioning method. 2%, 3.5% and 5% nano-clay modified
Modified Lottman Test mixtures were found as more rutting resistance than the conventional mixtures according to the AASHTO
T283 conditioning. Indirect tensile strength tests were realized with Lottman moisture damage condi-
tioning model. Higher tensile strength values were obtained with 2% and 3% nano-clay modified asphalt
mixtures denotes that higher internal friction. Stripping damage of the modified mixtures was interro-
gated with the ratios of tensile strength concept. In the ratios of tensile strength, 2% each of three
nano-clay modified mixtures gives higher ratios. Stripping resistance of the 2% nano-clay mixtures was
found as higher than the control conditioned samples based on Modified Lottman Test. It is thought that
nano-clay modifiers can be successfully used in view of higher stripping, rutting and cracking resistance
with low ratio as 2%. Stripping resistance increased with increasing nano-clay concentrations in view of
conditioning 2. As a result of the mechanical test approaches 2% nano-clay content is thought as a suit-
able ratio in context with stripping, rutting and cracking optimization.
Ó 2016 Elsevier Ltd. All rights reserved.

1. Introduction Nano-technology is a highly creative and promising technique

Rutting and fatigue cracking distresses occur mainly before the
service life of pavement. The minimizing of the problems would be
more economical for recovery, while reconstructing defects would
involve more costs. One of the methods is to modify the properties
of asphalt cement for avoiding failure. Various methods, such as
the use of different polymers types, were employed. Using
additives such as nano-materials to improve asphalt cement and
mixture performance has recently become more popular.
Nano-composites are among used materials for improving asphalt
mixture properties [1–4].
E-mail addresses: eroliskender@gmail.com, eiskender@ktu.edu.tr
for the materials industry. Nano-materials find widespread use in
many applications around the world. The Scientific Committee on
Emerging and Newly Identified Health Risks defines nano-
materials as a type of material with an outer structure consisting
of one or multiple outer dimensions; an internal structure consist-
ing one or more dimensions in the order of 6100 nm; and whose
properties differ from those exhibited by comparable materials
lacking nano-features. Portland cement with non-materials is
being used by many researchers. In recent times, nano-materials
have also begun to find use in asphalt pavement mixtures. Nano-
technology is being used to develop new materials, devices and
systems by modifying and fashioning them at a molecular level.
There are various different types of nano-materials available, with
each type offering different opportunities for modifying and
improving asphalt mixtures. Examples of nano-materials that can

http://dx.doi.org/10.1016/j.measurement.2016.07.045
0263-2241/Ó 2016 Elsevier Ltd. All rights reserved.
360 E. Iskender / Measurement 93 (2016) 359–371

be used in asphalt applications include nano-tubes, nano-fibres, 2. Materials and methods

polymerized powders, nano-sized plastic powders, nano-
hydrated lime, nano-silica, and nano-clay [5].
Clays can be used for nano-clay production as additive materi-
als. Some are aluminosilicates revealing sheet-like structures.
Besides this the layered silicate structures mostly include vermi-
culite, kaolinite and montmorillonite appertain to the smectite
group clays. The thicknesses of layers are generally in the environs
of 1 nm. Likewise the aspect ratios are usually in the 100–1500 nm
range and hence fairly high. With the bitumen modification, the
nano-clay’s discs - or layers - need to be modified and separated
through the application of surface treatment. Separating the nan-
oclay layers greatly enhances the its active surface area, which
reaches between 700 and 800 m2/g with this process. With this
process a strong and extensive interaction between the asphalt
binder and nano-clay develop. Layered silicate can be intercalated
or exfoliated in polymer modified bitumen when their scales are
nanometric. This polymer chains can intercalate between the clay
discs/layers, causing the nano-clay to spread and disperse at a
nano-metric level across the polymer matrix. In the conclusions
polymer additives enhances mechanical, barrier and thermal char-
acteristics [6].
Nanomaterials such as nanoclay, nano hydrated lime, and nano
carbon have significant effects in improving the engineering prop-
erties of asphalt binders and mixtures. Many benefits or promising
potential of nanoclay materials are concerned with when it was
modified with base bitumen for flexible pavement applications.
This material has also been used as a secondary modifier to further
develop the performance properties of SBS-modified binder [7].
Nano-clay modifications result in considerable improvement in
the characteristics of bituminous binders and mixtures; however,
further studies need to be conducted before these modifications
can be used at larger scales [8]. The main reason for the necessity
to conduct further studies before applying these modifications in
real settings stems mainly from the limited amount of information
on how they actually reduce fatigue and increase rutting resistance
in asphalt mixtures. Similar studies have been performed in China
on asphalt modified with nano-calcium carbonate (nano-CaCO3)
[9,10], which determined that nano-CaCO3 can improve asphalt’s
temperature resistance (which is normally rather low) and rutting
resistance. The asphalt and nano-CaCO3 mixture results in a
system of steady and uniform composition that ameliorates
asphalt’s susceptibility to temperature. Despite such observations,
there is still limited understanding of the mechanisms through
which such nano-modification change the behavior and properties
of asphalt.
The effects of layered silicate in asphalt binder were evaluated
and a paucity of studies has been made on nano-composite modi-
fied asphalt cement and mixture. For example kaolinite clay has
been used for improving storage stability issue in polymer modi-
fied asphalt. Although kaolinite clay could increase this issue
because of its micrometric scale, no other improvements have been
observed for physical and mechanical properties [11,12]. Closi-
te_15A and Nano-fill-15 nano-clay materials were evaluated with
asphalt binder and mixtures. Nano-clay additives increased the
stiffness, indirect tensile strength, resilient modulus, Marshall Sta-
bility and improved the rutting resistance of the modified mix-
tures. But, fatigue strength decreased at low temperatures [13].
Aggregate combination, bituminous binder and three different
nano-clay A-B-C materials were used in experimental stages. Stone
mastic asphalt gradation was chosen and 19 mm maximum aggre-
gate size was used. Grain size distribution values were presented in
Table 1. Granulometry curve was presented in Fig. 1.
Aggregate material is basalt in view of mineralogy-petrography.
Basalt aggregate properties were given in Table 2. Basalt aggre-
gates were evaluated and described based on rock petrography
and mineralogical tests. Chemical analyses were performed for
the main oxides. The mineralogical composition of the basalt was
also determined through chemical analyses, and then confirmed
with material selection. Table 3 shows the evaluated basalt aggre-
gate’s chemical composition.
AC 50–70 penetration bituminous binder was used. Bitumen
properties were illustrated in Table 4 and the cellulose fiber used
as a preventive filtration material for SMA design characteristics
were given in Table 5.
In addition, nano-clay materials were added to improve the
asphalt mixture’s mechanical properties. Three different types of
nano-clay were employed. Nano-clay materials were produced
from bentonite clays supplied from various regions of Turkey. Used
bentonite clays for production of nano-clay A, nano-clay B and
nano-clay C were obtained respectively from Eskisßehir-Kütahya,
Eskisßehir and Çanakkale regions. Bentonites were dried and grinded
nanometric levels. Firstly, bentonites were activated with Na and
thus Ca-Bentonites converted to Na-activated bentonites. Na-
activated bentonites were purified with centrifuge. It was carried
out surface modification with quaternary ammonium salts under
the specified reaction conditions. Used organic modifiers were
given in Table 6. Also XRF, XRD and SEM methods were performed.
Chemical analysis results were given in Table 7 and XRD patterns
and SEM images of nano-clays were presented in Figs. 2–7.
Figs. 2 and 4 show that the distance between the layers varies
between 34 Å and 37 Å. Nano-clay A showed biggest interlayer dis-
tance while nano-clay C has the smallest value. Sieve analysis was
done to all nano-clay types and gradation curves showed in Figs. 8–
10. Nano-clay A has the largest surface area. Despite having the
highest SiO2 nano-clay C has the smallest surface area (2151 m2/kg).
When the polymer is unable to penetrate between the silicate
sheets, a phase-separated composite is constituted, and the prop-
erties stay in the same range for traditional micro-composites. In
an intercalated structure, where a single extended polymer chain
can penetrate between the silicate layers, a well-ordered multi-
layer morphology results with alternating polymeric and inorganic
layers. Silicate layers are completely and uniformly dispersed in a
continuous polymer matrix and so an exfoliated or delaminated
structure is obtained. Intercalated and exfoliated structures are
mostly desirable for improving the material performance [15].
Table 1
Used SMA gradations and fraction proportions.
Sieve size Percentage Fraction Board in Turkey
passing percentage (SMA Type 1-A)
inch mm Lower Upper
limit (%) limit (%)

Water sensitivity and tensile strength concepts were studied with 3/4 19.0 100 Coarse aggregate, 100 100
nano-clay and carbon microfiber modification. Nano-clay agents 1/2 12.5 92.7 70.9% 90 100
3/8 9.5 63.5 50 75
improved mechanical strength of the asphalt mixtures. 1.5%
nano-clay modification showed higher tensile strength and the No. 4 4.75 29.1 Fine aggregate, 25 40
No. 10 2.00 21.6 18.7% 20 30
moisture susceptibility performance [14].
No. 40 0.42 14.8 12 22
This study aimed to investigate cracking, stripping and rutting No. 80 0.177 12.4 9 17
resistance of nano-clay modified asphalt mixtures containing dif- No. 200 0.075 10.4 Filler, 10.4% 8 12
ferent type nano-clay materials and concentrations (2%-3.5%-5%).
 E. Iskender / Measurement 93 (2016) 359–371 361

100 Table 4
SMA 1-A upper limit for Turkey Test results for asphalt cement (AC 50–70).
90
Used SMA gradation Properties Test method Unit Value Board in
80 Turkey
SMA 1-A lover limit for Turkey
70 Specific gravity TS EN 15326 gr/cm3 1.025
(25 °C)
Percentage Passing, %

60 Softening point (°C) TS EN 1427 °C 52 46–54

Flash point TS EN ISO 2592 °C 240 P230
50 (Cleveland)
Penetration (25 °C) TS EN 1426 0.1 mm 63 50–70
40
Solubility TS EN 12592 % 99.6 P99
30

20
Table 5
10 Conventional properties of cellulose fiber.

0 Properties Value
0.01 0.10 1.00 10.00 100.00
Cellulose content, % 66.7
Sieve Size, mm Bitumen content, % 33.3
Inflammability temperature, °C 500
Fig. 1. Gradation curve for SMA mixture. Apparent density, g/l 480–530
Average particle thickness, mm 4±1
Average particle size, mm 2–8
Table 2 Physical shape Cylindrical dollop
Properties of used basalt aggregate.

Properties Test Value Specification

limit in Table 6
Turkey Used organic modifiers.

Specific gravity (coarse agg.) ASTM C 127 Nano-clay Organic modifier

Bulk 2.684
Nano-clay A Dimethyl, dehydrogenated tallow, quaternary ammonium
Apparent 2.744
Nano-clay B Methyl, tallow, bis 2 hydroxyethyl quaternary ammonium
Specific gravity (fine agg.) ASTM C 128
Nano-clay C Dimethyl, benzyl, hydrogenated tallow, quaternary
Bulk 2.656
ammonium
Apparent 2.754
Specific gravity (filler) 2.821
Los Angeles abrasion (%) ASTM C-131 12 Max 25
Flakiness index (%) BS 812 (Part 105) 14 Max 25
Stripping resistance ASTM D-1664 35–40 Table 7
(no additive) (%) Chemical analysis results of nano-clays.
Stripping resistance ASTM D-1664 80–85 Min 60
(with agent) (%) Compound Name Nano-clay A Nano-clay B Nano-clay C
Water absorption (%) ASTM C-127 0.81 Max 2 Conclusion (%) Conclusion (%) Conclusion (%)
Soundness in NaSO4 (%) ASTM C-88 0.92 Max 8
Al2O3 8.394 8.715 9.512
Plasticity index for sandy TS 1900 non-plastic Non-plastic
CaO 0.1531 0.3955 0.3327
aggregate
Cl 0.4869 0.4578 0.3386
CuO 0.007995 0.009166 –
Fe2O3 0.5189 0.4875 0.5078
Ga2O3 – 0.003557 0.002838
Table 3 GeO2 0.003939 – –
Chemical analysis results of used aggregate. K2O 0.1672 0.2896 0.2807
MgO 2.174 2.089 2.152
Components, % Formula Sample 1 Sample 2
MnO 0.01927 0.03464 0.03035
Silicium dioxide SiO2 57.28 59.41 Na2O 0.2342 0.2422 0.2802
Aluminum oxide Al2O3 13.58 13.44 Nb2O5 0.005885 0.004946 0.003544
Ferrous oxide Fe2O3 6.75 6.72 NiO 0.01105 0.01358 0.01560
Calcium oxide CaO 5.25 4.49 P2O5 0.008532 – 0.01367
Magnesium oxide MgO 3.41 3.75 PbO – 0.006113 0.005431
Sulfur trioxide SO3 0.00 0.00 Rb2O 0.002243 0.004387 0.004348
Sodium oxide Na2O 1.95 1.68 SO3 0.04875 0.03358 0.03586
Potassium oxide K2O 1.78 2.63 SiO2 42.99 49.15 51.17
Chlorine Cl 0.0216 0.0260 SrO – 0.006886 0.005726
Loss on heating 4.68 3.01 TiO2 0.04296 0.04347 0.05033
Calcium carbonate + Magnesium CaCO3 + MgCO3 5.30 2.80 ZnO 0.007696 0.008811 0.009018
carbonate ZrO2 0.004362 0.0000 0.0000
LOI 44.72 38.00 35.25

When the polymer penetrates between the adjacent layers of

the nanoclay, the gallery spacing is increased and the consisting
morphology is an intercalated structure system. An exfoliated mor-
phology occurs when the clay platelets are extensively delami-
nated and completely separated due to thorough polymer
penetration by various dispersion techniques. In combination with
nanoclay, couplings agents, such as silane, are used to disperse the
nanoclay in a stable manner. Also, silane coupling agents have been
observed to develop the bonding of nano-clay to the polymer
matrix [16].
Besides conventional mixtures three different mixture
alternatives modified with nano-clay materials were studied.
Nano-clays were used as substituted for filler. Filler content was
decreased by weight of total dry aggregate at 2%, 3.5%, 5% ratios
and nano-clays were added as 2%, 3.5%, and 5% proportions in dry
362 E. Iskender / Measurement 93 (2016) 359–371

Fig. 2. X-ray diffraction of nano-clay A.

Fig. 3. X-ray diffraction of nano-clay B.

aggregate mixtures. Marshall Design was performed and design
results were illustrated in Table 8. The designs were in accordance
with the specifications of the Turkish Board [17].
In the laboratory frame design, one group of conventional and
nine groups of nano-clay modified samples were produced. It also
worked with conditioned samples as well as unconditioned sam-
ples. It underwent two different conditioning systems. Condition-
ing system 1 was based on Lottman water damage model. In
conditioning 1 system, vacuum saturation was firstly applied to
specimens at levels ranging from 70% to 80%. The samples were
maintained for 30 min at 0.9 bar pressure vacuum cabin. The sam-
ples saturated with vacuum were then maintained for 16 h inside a
18 °C computer-controlled freezer, before being immersed for
24 h in a 60 °C water bath.
Conditioning system 2 covers cold water conditioning system.
Samples were kept in waterlogged canister. The canister was placed
in a computer controlled conditioning cabinet. Alternating 12-h
periods of +25 °C and 25 °C were sequentially applied for 10 times.
In this conditioning system, vacuum saturation was not performed.
The ‘‘Resistance of Compacted Bituminous Mixture to Moisture
Induced Damage” (AASHTO T283) is a widely used and effective
procedure for forming hot mix asphalt with susceptibility to mois-
ture. This procedure is largely similar to the Lottman test method
and brings for a few changes and differences. One of these excep-
tions is that the samples continue to be saturated with vacuum
until the level of water saturation reaches 70–80%-the original
Lottman method, on the other side, requires that a set time of
30 min is achieved [18].
The Superpave system used the AASHTO T283 method to deter-
mine the level of potential moisture damage. This procedure is
mostly similar to the Lottman procedure, save for a few changes
and differences. Lately AASHTO T283 has also become a widely
employed test procedure to assess the moisture damage perfor-
mance of asphalt mixtures. However, certain agencies have
reported issues regarding the correlation of field observations with
laboratory-based results [18].
The repeated load creep test, the indirect tensile strength test,
and the Marshall Stability test were performed to compacted
 E. Iskender / Measurement 93 (2016) 359–371
Fig. 4. X-ray diffraction of nano-clay C.
Fig. 5. SEM image of nano-clay A.
Fig. 6. SEM image of nano-clay B.
identical samples prepared at optimum bitumen content. Both
control and conditioned samples were used for these three tests.
3. Moisture damage evaluation
Moisture damage is the most important mechanism for asphalt
mixture degradation. Problem associated with moisture damage
363
Fig. 7. SEM image of nano-clay C.
can be examined based on the damage ratios observed in various
water damage models.
Moisture susceptibility of the compacted specimens was evalu-
ated upon determining Tensile Strength Ratio (TSR) of the samples
from the following equation F2/F1 where F2 is the average ITS of the
wet specimens and F1 is the average ITS of the dry specimens. A
minimum of 0.8 in TSR is required in order to prevent failure [19].
In this research stability and indirect tensile strength ratios
were used for evaluating moisture damage. Mixture specific grav-
ities decreased with nano-clay concentrations such as 3.5% and 5%
ratios (Fig. 11). Higher and lower specific gravity values can be
obtained with 2% nano-clay ratio.
Moisture damage investigation was applied with stability tests
and indirect tensile strength tests under the Lottman conditioning
(cond.1). Stability and flow properties and damage ratio values
were shown in Table 9 and Fig. 12. Modified mixtures with 2%
nano-clay concentrations for A-B-C additives gave higher resis-
tance values in context with stripping damage. Based on Marshall
damage ratios 2% nano-clay content is preferable ratio in view of
stripping. Increasing of nano-clay content from 2% to 3.5–5% den-
sity values decreased and damage ratio decreased.
Indirect tensile strength test results were presented in Table 10
and Fig. 13. Tensile strength ratios were obtained with conditioned
value and control unconditioned value. In comparison with Mar-
shall Stability ratios indirect tensile strength ratios gave higher
364 E. Iskender / Measurement 93 (2016) 359–371

100 Size % Volume Size % Volume

90 (nm) under (nm) under
80 0.01 0 25 89.26
70 0.05 0 30 92.35

% Volume under
60 0.1 0 32 93.41
50 0.5 2.12 38 95.99
40
1 9.59 40 96.66
2 26.28 45 97.98
30
2.7 35.78 50 98.86
20
Nanoclay A 5 55.34 52 99.12
10
7.5 66.38 60 99.78
0 10 73.04 63 99.87
0.01 0.1 1 10 100
15 80.73 74 100
Size (nm)
20 85.5 Surface area: 2512 m2/kg

Fig. 8. Size distribution of nano-clay A material.

100 Size % Volume Size % Volume

90 (nm) under (nm) under
80 0.01 0 25 97.55
% Volume under

70 0.05 0 30 98.87
60 0.1 0 32 99.2
50 0.5 2.44 38 99.79
40 1 7.97 40 99.87
30 2 21.17 45 99.99
20
2.7 30.85 50 100
Nanoclay B 5 55.88 52 100
10
7.5 71.77 60 100
0
0.01 0.1 1 10 100 10 81.02 63 100
Size (nm) 15 90.58 74 100
20 95.13 Surface area: 2435 m2/kg

Fig. 9. Size distribution of nano-clay B material.

100 Size % Volume Size % Volume

(nm) under (nm) under
80 0.01 0 25 93.86
0.05 0 30 96.66
% Volume under

60 0.1 0 32 97.45
0.5 2.4 38 98.99
40 1 7.04 40 99.31
2 17.03 45 99.79
20 2.7 24.77 50 99.95
Nanoclay C 5 46.84 52 99.99
7.5 62.25 60 100
0
0.01 0.1 1 10 100 10 71.8 63 100
Size (nm) 15 82.92 74 100
20 89.52 Surface area: 2151 m2/kg

Fig. 10. Size distribution of nano-clay C material.

Table 8
Marshall design test results.
resembles this situation [19]. In this research indirect tensile
strength results were also found lower than the Marshall Stability
Design parameter Value Board in Turkey ratios. Nine mixtures belong to total ten mixtures gave lower dam-
Min. Max. age ratios in context with stripping approach.
Compaction amount, blows 50 50 50 Resistance to water damage was alternatively evaluated with
Bulk specific gravity, Gmb 2.433 – – another water damage conditioning (cond. 2) model. Table 11
Marshall Stability, kg 1200 – – and Fig. 14 give strength values and ratios. In this conditioning
Air voids, Pa, % 3.0 2 4
model higher ratios were found with increasing of nano-clay con-
Void filled with asphalt, Vf, % 81.4 – –
Flow, F, 1/100 in. 3.1 – – centrations. Because of lower specific gravity values for high nano-
Asphalt cement, Wa 6.10 5.8 – clay content mixtures with 2% nano-clay ratio were taken as more
Voids in mineral aggregate, % 16.1 16 – harmonious ratio.
Schellenberg binder drainage test, % 0.19 – 0.3
The performance of polymer modified asphalt with nano-silica
particle additives was evaluated. PMA (PG-76) was mixed with
0%, 2% and 4% of nano-silica relative to asphalt binder weight.
value or else higher stripping resistance for nano-clay modified Dynamic creep, resilient modulus and moisture susceptibility tests
mixtures at the 2% nano-clay concentrations. In an another were performed to evaluate the performance of PMA with nano-
research the asphalt mixture specimens’ indirect tensile strength silica additive under different conditions of moisture susceptibility
ratios were determined to lower than the Marshall Stability ratios and aging. The nano-silica particles reduced the water damage
 E. Iskender / Measurement 93 (2016) 359–371 365

Air Void (%)

3

100

80
Voids with filled
asphalt (%)

60

40

20

22

20
Voids in Mineral
Aggregate (%)

18

16

14

12

10

2.48
Density (gr/cm3)

2.44

2.40

2.36

2.32
Control Nanoclay Nanoclay Nanoclay Nanoclay Nanoclay Nanoclay Nanoclay Nanoclay Nanoclay
A 2% B 2% C 2% A 3.5% B 3.5% C 3.5% A 5% B 5% C 5%
Mixture Type

Fig. 11. Air void, VFA, VMA and density variation of mixtures due to nano-clay percentage.

Table 9 of adding nano-silica. Adding nano-silica at a concentration of 4%

Stability and flow test results of conditioned and unconditioned samples.
appears to have resulted in the highest level of improvement for
Uncond. Cond. 1 mixtures Stability ratio the asphalt binder [5].
mixtures (cond. stability/ Comparative rheological tests for bitumen and mechanical tests
control uncond.
Stability, Flow, Stability, Flow,
stability)
for asphalt mixtures with unmodified and nano-clay modified
kN mm kN mm bitumen were also performed. Nano-clay had the effect of improv-
Control 52.825 0.55 42.175 1.695 0.80 ing the asphalt mixtures’ indirect tensile strength, resilient modu-
Nanoclay A 2% 53.94 0.49 50.61 1.42 0.96 lus and stability [13].
Nanoclay A 3.5% 55.775 0.475 50.015 2.12 0.95
The performance of the nano-composite modified bitumen was
Nanoclay A 5% 52.855 0.545 48.025 1.77 0.91
Nanoclay B 2% 56.09 0.805 46.705 2.09 0.88 also investigated. The physical, mechanical and rheological
Nanoclay B 3.5% 55.09 0.68 46.325 2.28 0.88 properties of conventional bitumen, and bitumen modified with
Nanoclay B 5% 55.175 1.095 37.775 0.72 nano-composite have been compared. Nano-composite could
Nanoclay C 2% 55.25 0.605 46.625 1.97 0.88
improve the physical, rheological behaviors and the stability of
Nanoclay C 3.5% 53.09 0.97 44.23 1.11 0.84
Nanoclay C 5% 51.525 0.935 41.23 1.375 0.78
the bitumen [20].
The benefits associated with using different levels of SBS and
nano-SiO2 powder in mixtures of pavement asphalt were evaluated
as well. Different ratios of nano-SiO2 powder and SBS were used to
susceptibility, while increasing the asphalt mixtures’ overall develop five different formulations of bitumen; both unmodified
strength and resistance. Rutting resistance and fatigue were also and modified bitumen were then used to prepare the Marshall
improved by the addition of nano-silica particles to the PMA. The Samples. Based on the test results, the best performance was
aging index indicated that the oxidative aging susceptibility – observed in asphalt mixtures with 1% nano-SiO2 powder and 5%
and especially long-term aging – decreased significantly as a result SBS [21].
366 E. Iskender / Measurement 93 (2016) 359–371

70
Uncond. Cond. 1
60

50

Stability (kN)
40

30

20

10

0
Control Nanoclay Nanoclay Nanoclay Nanoclay Nanoclay Nanoclay Nanoclay Nanoclay Nanoclay
A 2% A 3.5% A 5% B 2% B 3.5% B 5% C 2% C 3.5% C 5%
Mixture Type

Fig. 12. Marshall Stability values of mixtures.

Table 10
Test results for the indirect tensile strength of conditioned and unconditioned mixtures (cond. 1 was applied and tested at 25 °C).

Unconditioned samples Conditioned samples Uncond. tensile Cond. 1 tensile Percent increase in tensile Tensile strength ratio
strength strength strength according to cond. (cond./control
S1 S2 S3 S1 S2 S3
(average), kN (average), kN control mixture, % uncond.)
Control 12.20 10.90 11.54 7.68 9.03 8.20 11.55 8.31 0.72
Nanoclay A 2% 12.00 14.57 12.99 12.06 13.68 13.31 13.19 13.02 56.8 1.13
Nanoclay A 3.5% 13.64 14.10 13.86 10.59 9.38 9.64 13.87 9.87 18.8 0.94
Nanoclay A 5% 12.05 10.50 13.29 8.08 8.80 8.32 11.95 8.40 1.1 0.78
Nanoclay B 2% 12.38 13.20 12.77 11.20 10.67 10.72 12.78 10.86 30.8 0.85
Nanoclay B 3.5% 13.81 14.16 13.63 9.76 9.57 10.17 13.87 9.83 18.3 0.85
Nanoclay B 5% 11.35 11.68 10.78 6.89 5.60 6.44 11.27 6.31 24.1 0.68
Nanoclay C 2% 10.82 9.86 10.05 9.51 8.73 8.86 10.24 9.03 8.7 0.73
Nanoclay C 3.5% 9.27 10.23 10.31 7.07 8.25 8.11 9.94 7.81 6.0 0.55
Nanoclay C 5% 10.04 9.33 9.49 6.45 6.16 6.28 9.62 6.30 24.2 0.55

16
Uncond. Cond. 1
Indirect Tensile Strength (kN)

14
12
10
8
6
4
2
0
Control Nanoclay Nanoclay Nanoclay Nanoclay Nanoclay Nanoclay Nanoclay Nanoclay Nanoclay
A 2% B 2% C 2% A 3.5% B 3.5% C 3.5% A 5% B 5% C 5%
Mixture Type

Fig. 13. Indirect tensile strength values of mixtures for cond. 1 (25 °C).

Tests were also performed to evaluate the effect of nano-clay
addition on asphalt mixtures’ long-term performance. Within the
frame of indirect tensile tests, stress levels at 200, 300, 400 and
500 kPa were applied to cylindrical specimens consisting of
unmodified and modified bitumen. Test results revealed that add-
ing 1% nano-clay resulted in a noticeable increase in the asphalt
mixtures’ fatigue life [22].
Surface science methods were used to investigate the nano-
clay-modified asphalt binders’ susceptibility to moisture. Two
grades of nano-clay (Cloisite 15A and Cloisite 11B) with different
ratios were mixed with the PG 64-22OK binder. SAXD data indi-
cated that adding 4% and 6% (relative to binder weight) of Cloisite
11B, formed exfoliated structures in modified asphalt binders.
Moisture susceptibility results also suggested that, among the dif-
ferent binder and aggregate ratios, 6% Cloisite 11B and 4% Cloisite
15A were the ratios that exhibited the largest adhesive energy [23].
Some characteristics of asphalt binders and asphalt mixtures
can be improved with nanoclay modifications but anyway more
research is required for applying on a large scale. The major reason
for this is that while the nanoclay increased the rutting resistance
little is known about how it mitigates the fatigue problem of
asphalt. In China, similar research has been conducted on nano cal-
cium carbonate (nano-CaCO3) modified asphalt and illustrated that
the nano-CaCO3 can enhance asphalt’s rutting-resistance as well as
improve its low-temperature toughness. The mixture of nano-
CaCO3 and asphalt forms a uniform-steady system which improves
 E. Iskender / Measurement 93 (2016) 359–371 367

Table 11
Test results for the indirect tensile strength of conditioned and unconditioned mixtures (cond. 2 was applied and tested at 15 °C).

Unconditioned samples Conditioned samples Uncond. Tensile Cond. 1 tensile Percent increase in Tensile strength
strength (average), strength tensile strength according ratio (cond./uncond.)
S1 S2 S3 S1 S2 S3
kN (average), kN to cond. control mixture, %
Control 29.26 28.61 31.62 15.26 16.35 17.54 25.00 16.38 0.66
Nanoclay A 2% 21.00 24.87 26.56 17.37 18.35 18.94 24.14 18.22 11.2 0.75
Nanoclay A 3.5% 21.17 21.50 19.77 18.97 16.55 16.06 20.81 17.19 4.9 0.83
Nanoclay A 5% 16.67 19.51 17.75 16.56 15.91 15.59 17.98 16.02 -2.2 0.89
Nanoclay B 2% 20.93 21.65 22.72 16.32 17.65 15.76 21.77 16.58 1.2 0.76
Nanoclay B 3.5% 17.47 18.29 19.87 11.83 16.64 17.99 18.54 15.49 -5.5 0.84
Nanoclay B 5% 15.53 12.33 14.22 12.14 13.72 10.79 14.03 12.22 -25.4 0.87
Nanoclay C 2% 25.01 25.30 26.57 19.32 17.03 19.03 25.63 18.46 12.7 0.72
Nanoclay C 3.5% 22.87 21.02 26.47 16.15 14.99 18.00 23.45 16.38 0.0 0.70
Nanoclay C 5% 19.95 18.17 20.79 17.84 16.29 17.92 19.64 17.35 5.9 0.88

30
Uncond. Cond. 2
25
Tensile Strength (kN)

20

15

10

0
Control Nanoclay Nanoclay Nanoclay Nanoclay Nanoclay Nanoclay Nanoclay Nanoclay Nanoclay
A 2% B 2% C 2% A 3.5% B 3.5% C 3.5% A 5% B 5% C 5%
Mixture Type

Fig. 14. Indirect tensile strength values of samples for cond. 2 (15 °C).

temperature susceptibility of asphalt at high temperatures.
However, the mechanism of asphalt material behavior with this
modification is not well understood [16].
It was conducted preliminary tests, blending small percentages
of nanoclay-composites into virgin asphalt with aim of producing
a binder that is less susceptible to permanent deformation and
low-temperature cracking. The study is to significantly reduce the
temperature sensitivity of the bituminous binder at service temper-
atures while sustaining workability at construction temperatures.
Nano-modified asphalt may potentially improve the rutting, crack
and fatigue resistance of asphalt mixtures [24].
Nanoclay and/or carbon microfiber modified asphalt mixtures
were evaluated with indirect tensile strength tests in a modified
AASHTO T283 test method. Hot-mixed asphalt samples were dam-
aged in either water or deicing solutions of various concentrations
and were then exposed to seven freeze–thaw cycles. The addition
of nano-clay and carbon microfiber would improve a mixture’s
water susceptibility performance or decrease the moisture damage
potential in most cases. As the nanoclay dosage increased the ten-
sile strength of unconditioned asphalt mix samples decreased, but
increased for samples conditioned in water. In general, asphalt
mixtures modified with 1.5% nano-clay appear to offer high tensile
strengths and less susceptibility to water or deicers [14].
Nanoclays can be effectively used as a modifying agent to
improve the mechanical properties of asphalt binders. Nanoclays
A and B improved the G⁄ and viscosity. Nanoclay B binder had more
pronounced improvements in G⁄ and viscosity than Nanoclay.
According to the direct tension test indicates that Nanoclay A
asphalt has better low-temperature cracking resistance than the
Nanoclay B asphalt. The blending procedure is crucial in achieving
well distributed nanoclay asphalt. The ongoing research will
focus on the low-temperature cracking performance and fatigue
resistance of the nanoclay-modified binder as well as the asphalt
concrete mixtures made with nanoclay-modified asphalt [16].
4. Rutting evaluation
Repeated creep test was applied with Umatta test apparatus in
Nottingham asphalt tester (NAT). Table 12 illustrates interested
test parameters used in repeated creep test.
Repeated creep tests were performed to control and nano-clay
modified mixtures for Lottman conditioning (cond. 1). Figs. 15–17
illustrate creep curves for A-B-C nano-clay modified asphalt mix-
tures for control and conditioned mixtures.
Under the modified Lottman water damage model all nano-clay
modified mixtures showed higher resistance compared to the con-
ditioned mixtures. Rutting resistance was found higher the control
mixtures for modified mixtures. As a general approach such nano-
clay concentrations can be leaded higher and lower flow rutting
resistance but in each case higher resistance are concerned with
control mixtures. Estimating reliable nano-clay content is very
important in view of rutting evaluation. Nearly 50% lower perma-
nent deformation can be calculated with selected nano-clay
concentrations.
Repeated creep test was also done with unconditioned control
and modified mixtures. In the passive condition or else no damage
condition as it shown in Figs. 18–20 conflicting results are sub-
jected. Modified mixtures can give lower resistance but in the
damage conditions this resistance trend is found as expected.
Nano-clay modifiers reveal its efficiency under the water damage
mechanisms like in the field condition.
Stability to flow ratio is called Marshall Quotient (MQ) and may
be used as an indicator for rutting investigation. In this research
MQ values were calculated and illustrated in Fig. 21. Controversial
368 E. Iskender / Measurement 93 (2016) 359–371

Table 12 1.1
Repeated creep test parameters.

Test parameters Values 1.0

Temperature 40 °C
0.9
Conditioning stress 10 kPa.
Conditioning stress time 2 min
0.8

Permanent Deformation (mm)

Test stress 100 kPa
Loading period 1000 ms
Time loaded 500 ms 0.7
Time unloaded 500 ms
Pulse number 21,600
0.6

0.5
1.1
0.4
1.0
0.3 Control
0.9 Nanoclay C 2%
0.2 Nanoclay C 3.5%
0.8 Nanoclay C 5%
Permanent Deformation (mm)

0.1
0 5000 10000 15000 20000
0.7
Pulse Count
0.6
Fig. 17. Rutting potential of nano-clay C modified mixtures for cond. 1.

0.5

1.0
0.4
Control

0.3 Control Nanoclay A 2%

Nanoclay A 2% 0.9
Nanoclay A 3.5%
0.2 Nanoclay A 3.5% Nanoclay A 5%
Nanoclay A 5%
0.8
Permanent Deformation (mm)

0.1
0 5000 10000 15000 20000
Pulse Count
0.7
Fig. 15. Rutting potential of nano-clay A modified mixtures for cond. 1.

0.6
1.1

1.0 0.5

0.9
0.4
Permanent Deformation (mm)

0.8

0.7
0.3
0 5000 10000 15000 20000
0.6 Pulse Count

0.5 Fig. 18. Rutting potential of nano-clay A modified mixture (uncond. mixtures).

0.4
MQ has a more completed effect on the rutting potential than
0.3 Control the other variables. This ratio indicates the stiffness of the mixture
Nanoclay B 2% as well as the minimum flow necessary; it may thus serve to pre-
0.2 Nanoclay B 3.5% vent the use of embrittlement-susceptible mixtures. Previous stud-
Nanoclay B 5% ies indicated that higher MQ levels are associated with higher
0.1 mixture stiffness and a higher spread/distribution of applied loads.
0 5000 10000 15000 20000
Pulse Count Therefore, higher MQ values provide asphalt pavements the exhibit
greater resistance to lasting deformations [25]. However, studies in
Fig. 16. Rutting potential of nano-clay B modified mixtures for cond. 1. the literature provide different results and conclusions regarding
high MQ levels’ effect on asphalt mixture rutting resistance. [26].
It has been described that in asphalt mixtures consisting of poly-
results were found in view of MQ values. MQ values conflict with mer modifiers, MQ levels may not serve as accurate illustration
repeated creep test. It was understood that MQ approach is not a of the level of permanent deformation [27].
reliable approach for nano-clay modified asphalt mixture rutting Using nanoclay modified asphalt as nano-composites has the
phenomena. effect of increasing aging resistance [28]. It was previously
 E. Iskender / Measurement 93 (2016) 359–371 369

1.0 Adding 2–4% nano-silica relative to the weight of asphalt has

the effect of decreasing rutting depth by nearly a half. Moreover,
it has been determined that nano-material-modified asphalt mix-
0.9 tures’ rut depths are lower than those of control mixtures, with
smaller rutting depths being observed when higher levels of
nano-materials are used in the mixtures. However, there are only
0.8 a limited number of studies on nano-material-modified asphalt
Permanent Deformation (mm)

mixtures compared to studies on binder modification through

the addition of nano-materials [16,33].
0.7 80/100 asphalt cement was modified with 1, 2, and 3% chemical
warm mix asphalt (WMA) additive and 4% nano-clay respectively.
WMA mixture performance was compared with hot-mix asphalt
0.6 (HMA). Apart from the insignificant low resilient modulus value
obtained with the WMA mixtures, the modified WMA mixtures
performed incredibly well in the way of moisture susceptibility,
0.5 rutting, and permanent deformation when compared with
Control
conventional HMA. Nanoclay and chemical WMA additive could
be effectively used as WMA modifiers. Indirect tensile fatigue test
Nanoclay B 2%
0.4 indicated that the number of cycles to cause failure of WMA
Nanoclay B 3.5% mixtures were not significantly different when compared with
Nanoclay B 5% the HMA. However, the number of cycles to cause failure
0.3 increased significantly for WMA with NCMB B4% when compacted
0 5000 10000 15000 20000
at 135 °C [7].
Pulse Count
Nano, polymer and nanocomposite modified asphalt mixtures
Fig. 19. Rutting potential of nano-clay B modified mixture (uncond. mixtures). were produced. Tensile strength, resilient modulus and rutting
tests were employed for the control and modified mixtures.
Nano-clay can enhance physical and rheological properties of the
1.0 PMA binder mixtures as well as its storage stability. Tensile
Control strength and resilient modulus and also improved rutting resis-
Nanoclay C 2% tance over conventional asphalt concrete were obtained [34].
0.9 Physical and mechanical properties of bituminous binder could
Nanoclay C 3.5%
also be improved with modification with nanoclay modification.
Nanoclay C 5% Stiffness, storage stability, rutting resistance, thermal cracking
0.8 resistance, and aging resistance properties of the mixtures were
Permanent Deformation (mm)

also significantly improved. After modification, the asphalt binders

0.7
0.6
0.5
0.4
0.3
0 5000 10000
Pulse Count
Fig. 20. Rutting potential of nano-clay C modified mixture (uncond. mixtures).
determined that increasing nano-clay content decreases modified
asphalt’s storage stability [29]. Nano-clay modifications improve
tend to improve the rheological properties of the binders by
decreasing the phase angle (improves elasticity), and by providing
higher levels of stiffness in comparison conventional asphalt. These
nano-clay modifications can consequently reduce the effect of aging
as well [30]. Certain studies have determined that a 2% of nano-clay
content in asphalt can increase shear (complex) moduli by up to
184% [16], which illustrates that rutting resistance of the asphalt
has been considerably increased by the addition of the nano-clay.
These materials are commonly used secondary modifier to increase
the performance SBS-modified asphalt even further [31,32].
were named Nanoclay A modified asphalt binder (NCMB A), Nan-
oclay B modified asphalt binder (NCMB B), and chemical WMA
modified asphalt binder (CWAA). The rheological characteristics
of the binders were evaluated with the rotational viscosity,
dynamic shear rheometer, and bending beam rheometer tests.
NCMB B and CWAA significantly decreased mixing and compaction
temperatures. However, only NCMB B showed a significant
increase in rutting and fatigue resistance when compared with
base bitumen [35].
Rutting, fatigue and moisture damage performance of nanoclay
(CL-30B) modified asphalts with newly adopted test methods were
evaluated. Incorporating of CL-30B enhances fatigue life of a bitu-
minous binder. It was shown potential of CL-30B to enhance vari-
ous rheological performance of a binder for better and long lasting
15000 20000 pavements [36].
Improvement in fatigue life of asphalt binder with addition of
nanoclay evaluated using Superpave fatigue parameter was
obtained [37]. Contrary to this observed reduction in fatigue life
of binders with addition nanoclay evaluated using Superpave fati-
gue parameter was found [8,38]. Fatigue life of nanoclay modified
asphalt mixture depends on temperature [39]. Improvement in
fatigue life of nanoclay modified mixture was observed at 25 °C,
while reduced fatigue life was found at 5 °C compared to control
mix [36].
Nanoclay adding to the bitumen improved the resistance to
deformation and viscosity of the modified bitumen mixtures. Also
using nanoclay have good impact to improve low temperature
cracking. Modified bitumen with nanoclay material shows excel-
lent fatigue resistance. Addition of nano-particles to bitumen have
effective role for the bitumen used in hot climate area. That means
the modified asphalt with nano-clay can resist rutting [40].
370
140
120
Stability / Flow (kN/mm)
100
80
60
40
20
0
Control Nanoclay Nanoclay Nanoclay Nanoclay Nanoclay Nanoclay Nanoclay Nanoclay Nanoclay
A 2% A 3.5% A 5%
Fig. 21. Stability/flow ratios of conditioned and unconditioned mixtures.
5. Conclusions and recommendations
This study investigated the usability of nano-clay materials pro-
duced from different sources as modifiers in asphalt mixtures.
Three types of nano-clay products were prepared and used at three
different ratios of 2%, 3.5%, and 5%. These nano-clay materials were
used as substitute of filler material. Different water damage condi-
tioning systems were selected and applied to half of the identical
samples. Indirect tension strength tests and repeated creep tests
were studied. Marshall Stability values were obtained. AASHTO T
283 moisture cohesion tests were used evaluating efficiency of
selected additives. Based on the study results, following state-
ments and conclusions can be drawn:
 Nano-clays have been used as modifiers in asphalt mixtures
through various different methods. In this study, it was
observed that nano-clay materials can be used instead of min-
eral fillers.
 Increasing ratios of nano-clay materials in the mixtures led to a
decrease in the mixture density. However, a 2% nano-clay ratio
was not associated with a significant change in density.
 Mixtures with nano-clay modification exhibited higher water
damage resistance. Nano-clay modification of 2% was found to
be effective against water damage. In water damage assess-
ment, nano-clay materials have revealed some more effective
results. It is thought that this condition resulted from finer
grinding size according to filler gradation. During water damage
assessments/tests, indirect tensile strength ratios were found to
be smaller than the Marshall Stability ratios. Evaluating mois-
ture damage problem conflicting results can be obtained with
different test methods. For this reason moisture damage prob-
lem is complex. Because of the lower damage ratios belongs
to indirect tension strength test additive ratio contents must
be selected with a true approach.
 It is considered that the grinding size of nano-clay materials in fil-
ler gradation distribution and hence surface area of nano-clays
have a positive effect on the performance of asphalt modification.
 According to the AASHTO T283 water damage conditioning
regime, moisture damaged samples showed a higher rutting
resistance increment depending on the ratio and type of nano-
clay additive. Nanoclay modified mixtures showed 50% greater
rutting resistance than the control mixtures as an average.
 Although unconditioned samples showed some contradictory
results, they generally exhibited an increase in rutting resis-
tance. However, it is believed that conditioning the mixtures
according to conditions encountered during actual application
and use will better illustrate the effectiveness of nano-clays.
E. Iskender / Measurement 93 (2016) 359–371
Uncond.
Conditioned 1
B 2% B 3.5% B 5% C 2% C 3.5% C 5%
Mixture Type
 The use of nano-clays in asphalt mixtures is a current topic,
with various ongoing studies being conducted on this subject.
These studies generally investigate the effects of certain
nano-clay materials on asphalt mixtures or asphaltic binders.
However, it would be more beneficial if future studies focus
on concepts such as the addition method of the nano-clays,
the mixing speed, the mixing duration and temperature, and
the compaction temperature.
Acknowledgements
This investigation is a part of the research supported by
Karadeniz Technical University (KTU), Scientific Research Projects
Unit (Project Number: 9542). The author would like to thank
KTU – Turkey for providing the financial support to perform this
study and Dr. Atakan AKSOY for giving consultation. The author
is also gratefully acknowledged to Eczacıbasßı ESAN Company for
their material supports and test facilities.
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