International Journal of Engineering & Technology, 7 (4.

7) (2018) 13-18

International Journal of Engineering & Technology

Website: www.sciencepubco.com/index.php/IJET

Research paper

Evaluation of Rheological Behavior of Bitumen Modified with

Nano Copper Oxide
G.H. Shafabakhsh1*, S.R.Sajadib 2
1
Professor, Faculty of Civil Engineering, Semnan University, Semnan, I. R. Iran
2
Phd Student, Faculty of Civil Engineering, Semnan University, Semnan, I. R. Iran
* Corresponding author: E-mail address: [email protected]

Abstract

Nowadays, one of the most challenging problems facing civil and transportation engineers, which consumes plenty of budgets (causes
large amount of cost) for maintenance of asphalt roads, is asphalt destructions. Lots of efforts are done in order to increase the resistance
and life span of asphalt, including development of bitumen properties. Bitumen is used broadly in road construction due to its appropriate
properties; however, it has some major deficiencies which may lead to destructions of asphalt pavements. Therefore different bitumen
modifications are implemented to achieve desired properties for different objectives, including (Such as) using rubber powder, waste
materials, various polymers, etc. Recently, researchers are turning to nanotechnology to improve bitumen properties. Conducted studies
on this topic (conducted research in this field) show that using modified bitumen by nanomaterial, increases the capacity of the pave-
ment’s load bearing and decreases probable cracks due to fatigue during the operation life of the pavement. In this study, Nano Copper
Oxide is used to develop rheological properties of bitumen. Nanoparticles have been added to bitumen with amount of 2.5, 3 and 5 per-
cent and then Dynamic Shear Rheometer (DSR) and Bending Beam Rheometer (BBR) experiments have been conducted to investigate
the effects of using nanoparticles in pure bitumen. Results show that adding Copper Oxide nanoparticles to bitumen improves the per-
formance of base bitumen, especially at middle and low temperatures.

Keywords: Nano Copper Oxide, Bitumen Modification, Rutting, Dynamic Shear Rheometer, Bending Beam Rheometer.

modification of bitumen properties. Researchers have used differ-

1. Introduction ent methods such as making use of various polymers. Adding
modifiers like nanomaterials to improve performance of the bitu-
Asphalt is now the first choice for highway construction for its men and asphalt mixture is getting popular in recent years. Nano-
various advantages like: smoothness, easiness, short period of composite is one of the most popular materials discovered for
construction and simple maintenance. [1] With the rapid develop- developing the properties of bitumen and asphalt mixture. [4]
ment of transportation systems and therefore increase of loading Nanotechnology includes techniques, setups and systems related
and passing traffic, Asphalt’s usage is getting broad and more to the nano scale. Nanotechnology is widely used in development
serious. of new generation of materials to improve the macroscopic prop-
Fracture in low temperature and fluidity in high temperature re- erties of them with more satisfying performance. This technology
spectively lead to cracks in pavement in low temperature and rut- is providing accessibility to smallest particles in civil engineering
ting in high temperature, which drops the quality and and is used in cases in which the dimensions of materials are in
pavement performance down. Rutting creates permanent defor- the range of 1 to 100 nanometers at least for one of the material
mation, so in any weather conditions, especially hot weather, it is dimensions. [5]
considered as one of the major destruction mechanisms in asphalt Bitumen modifiers are mainly used to develop the duration and
pavements, which can decrease the duration of service of pave- performance of asphalt mixture when pure bitumen cannot meet
ment and also hydroplaning when certain requirements in tough conditions. Different amounts and
water is trapped in cracks. Permanent deformations in top layers mixtures are used for enhancing the resistance against permanent
of asphalt grows when traffic load and wheel pressure increase. deformations, fatigue cracks, cracks created in low temperature,
[2] humidity damages, and aging. [6]
Performance, serviceability and durability of pavements depend In recent years, using nanomaterials for strengthening common
on conjunction and adherence between bitumen and surface of materials in pavement have gained popularity, due to its high effi-
aggregate in different conditions and the conjunction between ciency, being multipurpose, and long term performance. Exclusive
bitumen and surfaces of aggregates depends on their physical and mechanical and rheological properties of nanomaterials are useful
chemical properties. [3] for designing and manufacturing pavement materials. Dispersion
Destructions happened during operation life of pavement are of nanoparticles and chemical compatibility with bitumen matrix
mainly including rutting, permanent deformations, and cracks due are main challenges in development of bitumen nanocomposite
to fatigue. Inasmuch as treating and reconstruction of such defi- materials. Development of nanocomposite materials mainly de-
ciencies are costly, preventing these phenomena are a cheaper pends on betterment of the adherent of nanocomposite/bitumen
strategy. One of the approaches of prevention from destruction is
Copyright © 2016 Authors. This is an open access article distributed under the Creative Commons Attribution License, which permits unrestricted
use, distribution, and reproduction in any medium, provided the original work is properly cited.
14 International Journal of Engineering & Technology

matrix and homogeneous distribution of nanoparticles in bitumen 3. Research Necessity

matrix. [7]
Bitumen forms a small amount of volume and weight of asphalt
2. Research History mixture, but it plays an important role in performance of pavement
layers. Even though bitumen has various applications and useful
There has been a great deal of (extensive) research in applications properties in road construction industries, it has major deficiencies
of nanotechnology in asphalt mixture, some of which are reviewed which cause various damage in asphalt pavements. Among its
here: deficiencies are high sensitivity to temperature of bitumen and
Ghaffarpoor Jahromi investigated the effect of nano-clay upon asphalt pavement as a result, excessive softness in high tempera-
rheological properties of bitumen. Experiments conducted on bi- tures which leads to rutting, low elasticity in low temperatures
tumen samples showed (demonstrated) that bitumen modifier which leads to temperature asphalt cracks, and viscosity of bitu-
improves (causes a growth of) the stiffness and resistance against men that forms permanent and irreversible deformations in asphalt
aging. It is also concluded that elastic properties of modified bi- pavement and pavement fatigue under heavy traffic and load.
tumen by nano-clay are much more than base bitumen. [8] Considering these problems, researchers investigate modifying the
Assessment of properties of unaged bitumen modified with carbon rheological properties of bitumen. One of the novel methods in
nanoparticles which was carried out by Amirkhanian et al. showed this area, is modifying the bitumen using nanoparticles. Nanopar-
that adding carbon nanoparticles increases the viscosity of bitu- ticles, due to capability of offering completely (totally) new (dif-
men and it also has a remarkable effect on bitumen performance ferent) or developed properties, based on particular characteristics
degree. This research specified that bitumen containing 1% of (size, distribution, constitution, phase, etc.) in comparison with
nanoparticles has one more grade of the PG degree. [9] massive sizes of the same particles, and also minute size of parti-
Mobaraki et al. investigated rheology of the modified bitumen cles (1-100 Nm) and having very large specific surface, can have
with Aluminum Oxide nanoparticles and Acrylate Styrene Acry- significant effects on development of rheological properties of
lonhrtilrei (ASA) polymer. Modified bitumen with 3, 5 and 7 per- bitumen and asphalt pavement, though they are added in small
cent of each modifier (Nano Aluminum Oxide and ASA) were percent as modifiers to bitumen.
assessed. The results of the tests pointed out that the viscosity of Although nanotechnology is recently used in modifying and de-
the modified bitumen increased with more amount of modifiers veloping properties of bitumen and asphalt mixtures, significant
besides all the values of viscosity were in particular range. Base researches are conducted in recent years on nanomaterials perfor-
bitumen had the least amount of G* and G*/sinδ compared with mance in asphalt pavements. However, considering the wide range
modified bitumen and also the modified bitumen with 5% of Nano of nanoparticles that can be used in structure industry and infra-
Aluminum Oxide had the best functionality of resistance against structures, the effects of a good many of these particles in bitumen
rutting among all modified samples. Using Aluminum Oxide na- and asphalt mixture have not been investigated yet. One of these
noparticles generally displayed better results compared to using materials is Nano Copper Oxide which is investigated in this study
ASA polymer. [10] as bitumen modifier.
Sadeghnejhad et al. studied physical and rheological properties of
modified bitumen with various nanomaterials. Results indicated 4. Research Method
that adding 1.2% of Nano Silica and 0.9% of Nano Titanium Ox-
ide into bitumen leads to an upper resilience point compared to
This research is conducted aiming at modification of rheological
base bitumen. Also adding 1.2% of Nano Silica and 0.9% of Nano
properties of bitumen, and the modifier was Nano Copper Oxide.
Titanium Oxide into bitumen brought about the best result for
Nanoparticles in 2, 3.5 and 5 percent were added to bitumen by
shear modulus in 60-70 bitumen. The shear modulus of bitumen
high shear mixer and were aged for performance experiments.
with 1.2% of Nano Silica in comparison with bitumen with 0.9%
DSR and BBR experiments were conducted for evaluating rheo-
of Nano Titanium Oxide, is 10% greater. [11]
logical properties of modified bitumen with and without aging and
Moghaddasnejhad et al. conducted investigations on the effects of
the corresponding results were compared.
using Nano Calcium Carbonate on dynamic behavior of asphalt
mixture. Results identified that mixture made with Nano Calcium
Carbonate in comparison with the control mixture, has less poten- 4.1. Materials
tial for rutting and also increasing the amount of Nano Calcium
Carbonate up to 4% decreases the potential of rutting. Moreover, Materials used in these experiments consisted of bitumen and
the results reveals that using Nano Calcium Carbonate in asphalt Copper Oxide nanoparticles. Properties of each material were
mixture, boosts the fatigue duration, in 15°C temperature, by obtained by different experiments and are reported below.
41.4% and 55.8% respectively for mixtures with 2% and 4% of Bitumen
Nano Calcium Carbonate [12]. In this study, pure bitumen PG 64-16 made by Tehran Jay Oil
Besides, various researches focused on using nanoparticles in Refining Co. was used, and its physical properties are listed in
bitumen and asphalt mixture [13-15]; however, there is not much Table 1.
information about the effects of Nano Copper Oxide on bitumen.
Therefore, in this research Nano Copper Oxide is used as modifier
in pure bitumen and its effects are investigated.

Table 1:. Pure bitumen properties

Properties Values Test standard
Penetration (25 ̊ C, 100 g, 5 s,0.1 mm) 64 ASTM D5
Softening Point ( ̊ C) 49.8 ASTM D36
Ductility (cm, 25 ̊ C) >100 ASTM D1754
Flash point temperature ( ̊ C) 336 ASTM D99
Density (60 ̊ C , kg/m3) 1018 ASTM D70
Mass change (%) 0.003 ASTM D6
Thin film oven test (TFOT) Penetration ratio (%) 74.7 ASTM D6
Ductility (25 ̊ C, cm) >100 ASTM D113
Copper Oxide Nanoparticles In order to modify bitumen, Copper
Oxide nanoparticles produced by US Research Nanomaterials Co.
International Journal of Engineering & Technology 15

were used in this research. Properties of Copper Oxide nanoparti- nanoparticle.

cle are listed in Table 2. Figure 1 depicts FE-SEM image of this

Table 2:. Nano Copper Oxide Properties

Purity Size of Particles Specific Area True Density Shape Color
99% 40 nm 20 m2/gr 6.4 g/cm3 Approximately Spherical Black

plex modulus in bitumen materials, the value of total complex

shear modulus as well as elastic and viscos parts are evaluated.
Phase angle is time lag between the applied shear stress and the
result shear strain in degrees. G* is the total shear modulus, δ is

stress, γmax is the maximum shear strain, t is the time lag in se-
conds and f is the loading frequency (1.59 Hz) [16].

G*=max/γmax (1)

δ = 360×t×f (2)

Permanent deformation is controlled by limiting the value of

G*/sinδ in test’s temperature. The allowable values are 1.0 kPa
Figure 1:. FE-SEM image of Nano Copper Oxide (for unaged bitumen) and 2.2 kPa (for aged bitumen after RTFO
test). Cracks due to fatigue are controlled to values less than 5000
Preparation of Bitumen Samples kPa by limiting G*×sinδ (for aged bitumen by PAV). This method
In this research (study), PG 64-16 pure bitumen were prepared is suitable for temperatures between 5°C to 85°C in which the
and used for bitumen samples containing Nano Copper Oxide. value of G* is between 0.1 to 10000 kPa [17].
Nano Copper Oxide was used as modifier in bitumen. Copper Bending Beam Rheometer Test
Oxide nanoparticles in 2.00, 3.50 and 5.00 percent were mixed Bending Beam Rheometer (BBR) test is used for determining
with bitumen by high shear mixer in 160°C for 45 minutes with the low temperature efficiency of bitumen that is aged by PAV.
4000 rpm, in order to obtain a homogeneous mixture of bitumen This test is conducted according to AASHTO T313. Parameters
and nanoparticles. used for analyzing the results include creep stiffness S(t), the max-
imum of which is 300 MPa, and m value (the slope of stiffness
4.2. Experiments graph versus time), which its minimum is 0.300. They are deter-
mined with BBR software [18].
In this research, for evaluating modified bitumen, Rolling Thin
Film Oven Test (RTFOT), Pressure Aging Vessel (PAV), Dynam-
ic Shear Rheometer (DSR) and Bending Beam Rheometer (BBR) 5. Analysis and Results of Tests
are used, instructions of which are explained below.
4.2.1. Aging Tests Nano Copper Oxide was added to bitumen in 2, 3.5 and 5 percent
Aging of modified bitumen are done by using test on effect of of bitumen weight and rheological properties of modified bitumen
heat and air on thin film of moving bitumen (Rolling Thin Film were investigated. The reason for limiting the percentages up to
Oven Test, RTFOT) according to ASTM D1754 and Pressure 5% is that more usage amounts are not economically efficient.
Aging Vessel (PAV) test according to ASTM D6521. Test on The main goal of this research, besides investigating the perfor-
effect of heat and air on thin film of moving bitumen, simulates mance of modified bitumen with Nano Copper Oxide, is to deter-
short term aging in process of mixing with aggregate, while Pres- mine if there is any positive effect on the performance of pure
sure Aging Vessel test simulates long term aging in service dura- bitumen PG 64-16, in low and high temperatures, because of using
tion. these nanoparticles as modifier
Dynamic Shear Rheometer Test To this aim, Dynamic Shear Rheometer and Bending Beam Rhe-
The behavior of bitumen is a function of temperature and load- ometer tests were conducted on pure and modified bitumen sam-
ing time and an appropriate test for evaluating such materials ples, under unaged, short term aged and long term aged circum-
should be able to evaluate both mentioned(two) parameters. One stances.
of the advanced and widespread instruments for this aim, is Dy-
namic Shear Rheometer. By using this test one can measure fun- 5.1. DSR Test Results
damental rheological properties of bitumen including shear com-
plex modulus G* and phase angle δ in any temperature. These two G*/sinδ is obtained from Dynamic Shear Rheometer test as meas-
parameters describe elastic and viscos behavior of bitumen. Shear urement for evaluating of bitumen resistance against rutting. Larg-
complex modulus is a resistance criteria against deformation under er values of G*/sinδ means enhancement in bitumen resistance
shear stress cycles, which consists of two parts: elastic (reversible) against permanent deformations and rutting. Figure 2 illustrates
and viscos (irreversible). Phase angle is a criteria of elastic to vis- G*/sinδ resulted from DSR test, for pure bitumen and modified
cos deformation ratio. These two parameters are severely sensitive bitumen with Copper Oxide nanoparticles in 2, 3.5 and 5 percent-
to temperature and loading frequency. In high temperatures, bitu- ages, for unaged bitumen, in 64°C and 70°C.
men is similar to viscos fluids which are not able to return to their
initial states; in contrary, in low temperatures it (bitumen) behaves
like elastic materials which return to their initial state after unload-
ing.
Dynamic Shear Rheometer (DSR) test was conducted on bitumen
samples, for determining viscoelastic behavior, according to
ASTM D-7175. In this test, the value of dynamic shear complex
modulus (G*) and phase angle (δ) of the tested bitumen are meas-
ured according to equations (1) and (2). By measuring the com-
16 International Journal of Engineering & Technology

peratures. This parameter investigates the effect of fatigue destruc-

tion which generally is one of the important pavement damages in
moderate temperatures. Results of G*×sinδ obtained from DSR
test on pure and modified bitumen samples are shown in Figure 4.
A total descending manner in G*×sinδ parameter can be observed
because of increasing Nano Copper Oxide in base bitumen which
shows that rise in the amount of Nano Copper Oxide in bitumen
causes improvement in fatigue parameter in modified bitumen and
brings about better performance in middle temperature.

Figure 2:. Values of rutting measurements versus percentages of Nano

Copper Oxide in modified bitumen without aging (unaged bitumen)

G*/sinδ is more than 1.0 kPa for all modified bitumen, which
means using Copper Oxide nanoparticles for modifying bitumen,
did not lead to decline in the performance grade of base bitumen.
Results of this test in 64°C show that adding Nano Copper Oxide
to bitumen increases the G*/sinδ value. Among modified bitumen
samples, the one with 2 percent of Nano Copper Oxide had the
maximum increase, which was 82.6%. This explins that Copper
Oxide nanoparticles enhance stiffness and also stability of bitumen Figure 4:. Values of fatigue parameter versus percentage of Nano Copper
against deformation and rutting, in 64°C. Oxide in modified bitumen with long term aging
Test was also done in 70°C temperature for determining the effect
of adding Copper Oxide nanoparticles on development of bitumen According to Sharp, the value of fatigue parameter G*×sinδ for
performance in higher temperatures. As can be seen in figure 2, pure bitumen PG 64-16 in temperature of 28°C should be less than
none of modified bitumen in 70°C has G*/sinδ parameter greater 5000 kPa. (The results of the test for temperature of 28°C was
than 1.0 kPa. This shows that adding Nano Copper Oxide to bitu- very smaller than 5000 kPa. So only the results for 25°C and be-
men cannot develop performance of bitumen PG 64-16 in high yond that are showed.) From the results of DSR test one can ob-
temperature (70°C). serve that the value of fatigue parameter in 28°C for modified
In order to study the effect of short term aging (RTFO) of bitumen bitumen with Nano Copper Oxide is very smaller than 5000 kPa
on its rutting measurement, base bitumen and modified bitumen and this fact holds even for 25°C, which notifies better perfor-
aged by RTFO instrument, and then DSR test was conducted to mance and also elastic behavior of modified bitumen with nano-
evaluate properties of bitumen modified and aged by RTFO. Fig- particles. Moreover, the elastic behavior of modified bitumen with
ure 3 displays G*/sinδ values resulted from DSR test for short 5% nanoparticles up to 22°C, is in Sharp requirement range which
term aged bitumen. These results show that rutting measurement shows that modified bitumen with 5% Nano Copper Oxide has the
for modified bitumen in 64°C is above 2.2 kPa which is more than best fatigue parameter performance among bitumen samples.
sharp requirements. This test was also conducted in 70°C, but the
results were not in sharp requirement range (G*/sinδ > 2.2 kPa). 5.2. BBR Test Results
Considering total set of results obtained from DSR test for modi-
fied bitumen which were unaged and aged by RTFO, one can Bending Beam Rheometer test was conducted in temperatures -
conclude that modified bitumen with Nano Copper Oxide devel- 6°C and -12°C and values of S(t) and m for pure and modified
ops the rutting measurement (G*/sinδ) of pure bitumen PG 64-16 bitumen were evaluated in these temperatures. In bitumen, if the m
in its performance temperature (64°C), but does not lead to devel- value is greater than 0.300 and the value of creep stiffness is less
opment of base bitumen in high temperature (70°C). than 300 MPa, its performance in low temperatures is better con-
traction cracks are prevented. The greatest m value is desired be-
cause when the temperature falls, pavement begins to contract and
bitumen as a material with lower stiffness, responds to this phe-
nomenon. The decreased stiffness leads to smaller tensile stresses
in bitumen and the probability of low temperature cracks get low-
er.
According to Sharp, for PG 64-16 bitumen in temperature -6°C,
the value of S(t) should be less than 300 MPa and m value should
be greater than 0.300. S(t) results obtained from Bending Beam
Rheometer test are shown in Figure 5. Based on these results,
creep stiffness S(t) of all bitumen samples in temperatures -6°C
and -12°C are in desired range (less than 300 kPa). However, m
values (Figure 6) only for temperature of -6°C for all bitumen
samples are in desired range and in -12°C, this value just for mod-
Figure 3:. Values of rutting measurement versus percentages of Nano ified bitumen with 5% Nano Copper Oxide is above 0.300.
Copper Oxide in modified bitumen with short term aging

Bending Beam Rheometer test was also conducted according to

AASHTO T315, to evaluate dynamic viscoelastic properties (G*,
δ) of modified bitumen with long term aging (PAV) in middle
temperature. Sharp researchers defined a parameter as G*×sinδ≤
5000 kPa to determine performance of bitumen in middle tem-
International Journal of Engineering & Technology 17

belonged to modified bitumen with 5% nanoparticles which in

28°C, 25°C and 22°C were in Sharp desired range.
Bending Beam Rheometer test determined that values of S(t) as
well as m values for modified bitumen samples in -6°C are placed
in desired range of Sharp and rise in amount of nanoparticles im-
proves S(t) (with descending manner) and m values (with ascend-
ing manner) in bitumen modified with Copper Oxide nanoparti-
cles. Also the best results among bitumen samples were related to
modified bitumen with 5% Nano Copper Oxide that led to PG 64-
16 bitumen improvement into PG 64-22 bitumen performance
grade.
Noting(considering) method and material used in this research,
one can conclude that adding Nano Copper Oxide in pure bitumen
PG 64-16 in amount of 5% can develop the rutting measurement
in high temperature as well as in its performance grade tempera-
ture (64°C), and also improve fatigue parameter in middle temper-
Figure 5:. The values of creep stiffness S(t) versus percentage of Nano ature and gain acceptable resistance against cracks due to thermal
Copper Oxide in modified bitumen with long term aging stresses.
This result shows that bitumen with 5% nanoparticles is suitable
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