applied

sciences
Article
Influence of the Microwave Heating Time on the
Self-Healing Properties of Asphalt Mixtures
Jose Norambuena-Contreras and Irene Gonzalez-Torre *
LabMAT, Department of Civil and Environmental Engineering, University of Bío-Bío,
Concepción 4051381, Chile; jnorambuena@ubiobio.cl
* Correspondence: irenegon@ubiobio.cl; Tel.: +56-41-311-1175

Received: 21 August 2017; Accepted: 20 September 2017; Published: 18 October 2017

Featured Application: A new generation of advanced self-healing asphalt pavements is coming.

The asphalt mixture presented in this study could be potentially used to build long-life roads
with crack-healing properties through electromagnetic heating, e.g., induction and microwaves.

Abstract: This paper aims to evaluate the influence of the microwave heating time on the self-healing
properties of fibre-reinforced asphalt mixtures. To this purpose, self-healing properties of dense
asphalt mixtures with four different percentages of steel wool fibres were evaluated as the three-point
bending strength before and after healing via microwave heating at four different heating times.
Furthermore, the thermal behaviour of asphalt mixtures during microwave heating was also
evaluated. With the aim of quantifying the efficiency of the repair process, ten damage-healing
cycles were done in the test samples. In addition, self-healing results were compared with the fibre
spatial distribution inside asphalt samples evaluated by CT-scans. Crack-size change on asphalt
samples during healing cycles was also evaluated through optical microscopy. It was found that the
heating time is the most influential variable on the healing level reached by the asphalt mixtures
tested by microwave radiation. CT-Scans results proved that fibre spatial distribution into the asphalt
mixtures play an important role in the asphalt healing level. Finally, it was concluded that 40 s was
the optimum heating time to reach the highest healing levels with the lowest damage on the asphalt
samples, and that heating times over 30 s can seal the cracks, thus achieving the self-healing of asphalt
mixtures via microwave heating.

Keywords: self-healing; asphalt mixture; metallic fibres; microwave heating; heating time

1. Introduction
Asphalt mixtures are composite materials made of aggregates and bitumen. They are widely
used in the pavement industry around the world. However, mechanical resistance and durability of
asphalt mixtures can be reduced due to their permanent exposure to traffic loading and environmental
conditions [1]. Ageing [2], moisture damage [3] and thermal cracking [4] are the main factors that affect
the durability of asphalt pavements. With the aim of improving the behaviour of flexible pavements
against these factors, different types of fibres can be added to the asphalt mixtures [5], such as: cellulose
and mineral fibres [6]; polymeric fibres like polypropylene and polyester [7]; and steel wool and other
waste fibres [8]. In particular, due to the higher tensile strength of metallic fibres compared with asphalt
mixtures they can improve the tensile resistance and cohesive force when added to the mixture [5].
Additionally, these fibres can help to prevent the origin and propagation of cracks [9]. Also, asphalt
mixtures with metallic fibres are known for presenting improved resistance, fatigue and ductility
characteristics [10]. Therefore, asphalt mixtures reinforced with metallic fibres can have good resistance
to ageing, moisture damage and cracking [11].

Appl. Sci. 2017, 7, 1076; doi:10.3390/app7101076 www.mdpi.com/journal/applsci

Appl. Sci. 2017, 7, 1076 2 of 15

Moreover, metallic fibres can be added to asphalt mixtures with the aim of increasing their
thermal and electrical conductivity [12]. Hence, metallic fibres have been used to develop new flexible
pavements with energetic [13] and self-healing purposes via heating processes by electromagnetic
induction [12,14–17] or microwave radiation [17–20]. It is known that asphalt pavements have
self-healing properties when they reach high temperatures during summer, when the cracks in the
road can be closed by themselves [12]. This is due to the fact that the bitumen viscosity is related with
the temperature, and consequently when the bitumen reaches a temperature threshold (between 30 ◦ C
and 70 ◦ C) it can flow by capillarity through the micro-cracks opened in the pavement [21].
There are currently different heating technologies that can accelerate the healing process of
asphalt mixtures. One of them is the electromagnetic induction heating [22]. This method consists on
adding ferrous materials (like metallic fibres) to the asphalt mixture and exposing it to an alternating
electromagnetic field with a frequency of Kilohertz [23], using an induction heating device. This process
induces an electrical current in the ferrous particles increasing their temperature due to the Joules
principle. Thus, the thermal energy disperses in the asphalt mixture and increases the temperature of
the bitumen [24].
A second technique is microwave heating [17], where asphalt mixtures are exposed to an
alternating electromagnetic field with a frequency in the order of Megahertz [20], using an
electromagnetic radiation device like a microwave. Microwave heating affects the bitumen, producing
a change in the orientation of polar molecules, which results in internal friction and an increase of
the mixture temperature [25]. Additionally, when ferrous materials are added to the mixtures, they
can reflect the microwave radiation and accelerate the temperature increase procedure [25]. In this
context, metallic fibres can be used to increase the heating rates of asphalt mixtures considering that
they can absorb more thermal energy than the aggregates and bitumen [19]. For all the above, fibres
addition can have influence on the mechanical and self-healing properties of the new asphalt mixtures,
although it is still not clear how this influence is produced.
The main objective of this study is to evaluate the influence of the microwave heating time on the
self-healing behaviour of asphalt mixtures. With this purpose, four different asphalt mixtures have
been studied under laboratory conditions, using the same aggregates gradation and bitumen content,
but varying the amount of fibres added to the mixture: 2%, 4%, 6% and 8% by total volume of bitumen.
Self-healing properties of asphalt mixtures have been measured using the three-point bending test
before and after microwave healing at four different heating times: 10 s, 20 s, 30 s and 40 s, during
ten cracking-healing cycles.
Finally, the main results of this research concluded that the heating time is the most influential
variable on the healing level reached by the asphalt mixtures tested by microwave radiation, over the
effect of the amount of fibres. Besides, CT-Scan results proved that fibre spatial distribution into the
asphalt mixtures play an important role in the asphalt healing level.
Furthermore, it was concluded that the optimum microwave heating time is 40 s, to reach the
highest healing levels with the lowest damage on the asphalt. In short, the study of the crack-sizes
revealed that heating times over 30 s can also seal the cracks, thus achieving the self-healing of asphalt
mixtures via microwave heating.

2. Materials and Methods

2.1. Materials
A standard IV-A-12 dense asphalt mixture was used in this research, since it is the mainly used
in asphalt pavement building in Chile [1]. Table 1 shows the composition and specifications of the
materials that form the asphalt mixture used. Fluvial type aggregates were used, and they were
classified in three fractions: coarse aggregate or gravel (size between 5 and 12.5 mm), fine aggregates
or sand (size between 0.08 and 2.5 mm), and filler (size < 0.08 mm). Bitumen used was a CA24 type,
according to Chilean Specifications. The penetration grade of the CA24 bitumen used for mixture
Appl. Sci. 2017, 7, 1076 3 of 15

preparation was 80/100 mm at 25 ◦ C. In addition, metallic fibres made from low-carbon steel were
added to the asphalt mixtures. The length of the fibres was measured using an optical microscope,
as the average value of 120 fibres randomly selected from the total sample, and the diameter was
measured in 10 fibres using a digital calibrated micrometre. Resulting in an average diameter of
0.157 mm with an average aspect ratio of 30 and an initial length in the range of 2–8 mm.
Finally, four different percentages of fibres were added to the asphalt mixtures: 2%, 4%, 6%
and 8%, by total volume of bitumen (see Table 1). Hence, 5 different types of asphalt mixtures were
manufactured: 1 reference mixture without fibres and 4 asphalt mixtures with fibres, using the same
aggregates gradation and bitumen content but varying the amount of fibres added to the mixture.

Table 1. Composition of the asphalt mixtures used in the study.

Cumulative Mass
Sieve Size (mm) Mass (g) Density (g/cm3 )
(% Retained)
12.5 16 176
10 29 143 2.779
5 53 264
Aggregates
2.5 69 176
0.63 86 187
0.315 90 44 2.721
0.16 93 33
0.08 95 19
<0.08 100 58 2.814
Type Amount (%mass/Aggr.) Mass (g) Density (g/cm3 )
Bitumen
CA24 5.3 58.3 1.039
Amount Length Range/
Mass (g) Density (g/cm3 )
(% vol./Bitumen) Avg. Diameter (mm)
2 8
Steel Wool Fibres
4 16
2–8/0.157 7.180
6 24
8 32

2.2. Test Specimens Preparation

A total of 40 Marshall specimens were manufactured using the following procedure:

• Before the mixing process, the aggregates were heated during 24 h at 150 ◦ C, while the bitumen
and the fibres were heated at 150 ◦ C during 2 h.
• Raw materials were added to the mixer in a specific order: bitumen and fibres, coarse aggregate,
fine aggregate and at last, filler.
• Raw materials were mixed in a metallic bowl during approximately 3.5 min at a speed of 100 rpm
and keeping a constant temperature of 150 ◦ C.
• After mixing, asphalt mixtures were poured into a previously heated Marshall mould (10 cm
diameter, 6 cm height) and compacted using a Marshall hammer applying 75 blows on each face.
• Marshall specimens were left to cool at ambient temperature during 24 h and then extracted from
the mould.

After manufacturing, bulk density and air void content of all Marshall specimens were determined.
Finally, each Marshall specimen was sawed into 4 semi-circular samples obtaining 160 semi-circular
samples in total (with dimensions 10 cm diameter, 5 cm height and 2.5 cm thickness), 80 of which
were used in the heating tests, while the other 80 were used in the crack-healing cycles. In both cases,
4 samples for each mixture type and heating time were tested.
Appl. Sci. 2017, 7, 1076 4 of 15

2.3. Asphalt Heating by Microwave Radiation

With the aim of knowing the temperatures reached by the asphalt mixtures, and their
heating-cooling behaviour when submitted to microwave radiation, semi-circular specimens of asphalt
mixture with and without fibres were heated in a microwave oven during four different heating times
Appl. Sci. 2017, 7, 1076
(10 s, 20 s, 30 s and 40 s). All the heating tests were carried out using a microwave oven with4 700 of 14
W
Appl. Sci. 2017, 7, 1076 4 of 14
power, and a working frequency of 2.45 GHz that corresponds to a wavelength of 120 mm [20]. In total,
power, and a working frequency of 2.45 GHz that corresponds to a wavelength of 120 mm [20]. In
◦ C (see Figure
80 power,
samples were tested, starting at of
approximately that20 1a). The temperature mm variation
total, 80 and a working
samples were frequency
tested, starting 2.45atGHz corresponds
approximately 20 °Cto(see a wavelength
Figure 1a).ofThe
120 temperature
[20]. In
on total,
the surface
80 on of
samples the samples
were tested, was measured using a thermographic camera PCI PI160 connected
variation the surface of the starting
samples at wasapproximately
measured using 20 °C (see Figure 1a).camera
a thermographic The temperature
PCI PI160
toconnected
avariation
computer. on Acomputer.
to athe real-time
surface A ofvideo record
the samples
real-time of
videowasthe surface
of thetemperature
measured
record using was obtained
surfacea temperature
thermographic withPCI
wascamera
obtained PIwith
Connect
PI160PI
software.
connected The video
to a register
computer. Astarted just
real-time after
video the heating
record of theended
surface(and the microwave
temperature
Connect software. The video register started just after the heating ended (and the microwave door was door
obtained was opened,
with PI
see
was Figure
Connect 1a),
opened, andFigure
software.
see its
The duration
video
1a), and was
register variable
startedwas
its duration depending
after theon
just variable the cooling
heating
depending ended time
(and
on the (required
timeto
the microwave
cooling reach
doorthe
(required
initial temperature of ◦
20temperature
C) ofand
eachitsasphalt sample. Additionally, the surface temperature onsurface
7 points
towas opened,
reach the see Figure
initial 1a), ofduration
20 °C) was variable
of each depending
asphalt sample. on Additionally,
the cooling time
the(required
to reach
distributed the
on theinitial
front temperature
surface of of
the 20 °C)
samples of each
was also asphalt
real-time sample. Additionally,
measured.
temperature on 7 points distributed on the front surface of the samples was also real-time measured. Thus, the
the surface
maximum
temperature
surface
Thus, on 7 points
temperature
the maximum was distributed
calculated
surface as
temperatureonthe
theaverage
frontcalculated
was surface
valueofof the
as allsamples
thethe was
measured
average also
value real-time
points
of all of measured.
the
the sample in
measured
the Thus,
moment
points the maximum
of thewhen
sample thein surface
highest
the moment temperature
temperatures
when the was
were calculated
registered
highest as the average
(see Figure
temperatures value
were1b). of all the measured
registered (see Figure 1b).
points of the sample in the moment when the highest temperatures were registered (see Figure 1b).

(a) (b)
(a) (b)
Figure1.1.(a)
(a)Microwave
Microwaveheating
heatingtest;
test;and
and(b)
(b)surface
surface temperaturemeasurement
measurement points,example
example foran
Figure
Figure 1. (a) Microwave heating test; and (b) surfacetemperature
temperature measurementpoints,
points, examplefor
for
an asphalt
asphalt mixturemixture with
with with4%
4% of4% of fibres
fibres heated
heated during
during 30 s.
30 s.30 s.
an asphalt mixture of fibres heated during
2.4. Flexural Strength of the Test Samples
2.4.2.4.
Flexural Strength
Flexural Strengthofofthe
theTest
TestSamples
Samples
Flexural strength of asphalt mixtures was measured in semi-circular samples using the three-
Flexural
Flexuralstrength
strengthof asphalt mixtures
of asphalt was
mixtures measured
was measured in semi-circular
in semi-circularsamples using
samples thethe
using three-point
three-
point bending test (see Figure 2). With the purpose of locating the initial point of cracking, a notch of
bending test (seetest
point bending Figure
(see2). With2).the
Figure purpose
With of locating
the purpose the initial
of locating pointpoint
the initial of cracking, a notch
of cracking, of 4 of
a notch mm
4 mm thickness and 10 mm height was made centered in the bottom side of the samples, and oriented
4 mm thickness
thickness and 10 mmand 10 mm height
height was madewas made centered
centered in thein bottom
the bottom
sideside of the
of the samples,and
samples, andoriented
oriented in
in the load direction (see Figure 2b). Moreover, all the samples were pre-conditioned at a temperature
theinload
the load direction
direction (see (see
FigureFigure
2b).2b). Moreover,
Moreover, all all
thethe samples
samples were
were pre-conditionedatataatemperature
pre-conditioned temperature of
of −20 °C during 24 h before testing, to ensure that a brittle fracture was produced.
−20of ◦−20 °C during
C during 24 h24before
h before testing,
testing, to ensure
to ensure that
that a brittle
a brittle fracturewas
fracture wasproduced.
produced.

(a) (b)
(a) (b)
Figure 2. (a) Three-point bending test on asphalt mixture semi-circular samples; and (b) schematic
Figure 2. (a) Three-point bending test on asphalt mixture semi-circular samples; and (b) schematic
Figure 2. (a) Three-point
representation bending
of the broken test on asphalt mixture semi-circular samples; and (b) schematic
test sample.
representation of the broken test sample.
representation of the broken test sample.
To
Tododothe
the flexural
flexural tests,
tests, the
the semi-circular
semi-circular samples
samples at at −20
−20 °C
°C were
were placed
placed on
on two
two cylindrical
cylindrical
supports
supportsseparated
separated80 80mm,
mm,andandthen
then aa vertical
vertical load
load at
at aa speed
speed ofof 0.5
0.5 mm/min
mm/min was was applied centered
applied centered
on the top part of the samples using a loading actuator (see Figure 2a,b). The equipment
on the top part of the samples using a loading actuator (see Figure 2a,b). The equipment used was used was aa
CONTROLS Multispeed static universal testing machine, with a load cell of 50 kN
CONTROLS Multispeed static universal testing machine, with a load cell of 50 kN and controlled byand controlled by
computer (see Figure 2a).
computer (see Figure 2a).
Appl. Sci. 2017, 7, 1076 5 of 15

To do the flexural tests, the semi-circular samples at −20 ◦ C were placed on two cylindrical
supports separated 80 mm, and then a vertical load at a speed of 0.5 mm/min was applied centered
on the top part of the samples using a loading actuator (see Figure 2a,b). The equipment used was a
CONTROLS Multispeed static universal testing machine, with a load cell of 50 kN and controlled by
computer (see Figure 2a).

2.5. Self-Healing Level of Asphalt Mixtures by Microwave Heating

The evaluation of the self-healing level of asphalt mixtures with fibres using microwave heating
has been carried out according to the following methodology [17]: first, each sample was submitted to
a three-point bending test (see Section 2.4) at −20 ◦ C, until it breaks in two parts. After this, the broken
samples were conditioned during 2 h at a temperature of 20 ◦ C, until the surface moisture due to
defrosting was completely dried. Then, the two parts of the sample were put together and heated
using microwave radiation during four different heating times (10 s, 20 s, 30 s and 40 s). After heating,
the samples were left to cool at ambient temperature to later be conditioned at a temperature of −20 ◦ C
during 24 h and submitted again to the three-point bending test, thus completing a cracking-healing
cycle. Hence, the healing level reached by each tested sample (HL) can be defined as the quotient
between the maximum force resisted by the sample initially tested (Fi ) and the maximum force resisted
by the sample after the healing process (Fr ).

Fr
HL = (1)
Fi

Finally, to quantify the efficiency of the healing methodology, 10 cracking-healing cycles were
carried out for each asphalt sample.

2.6. X-ray Computed Microtomography

With the aim of evaluating the spatial distribution of the fibres inside the asphalt mixture
specimens, X-ray micro computed tomography was employed. With this purpose, cylindrical
samples of approximately 25 mm in diameter and 12 mm in height were cut from sections of
semi-circular asphalt samples. The X-ray micro-tomography scans were obtained using a Bruker
SkyScan 1272 scanner. The scanner was operated at 100 kV and 100 µA and images were reconstructed
at a spatial resolution of 26.8 µm (voxel side). Thus, classification of voxels as phases present in
the mixture (i.e., voids, bitumen, aggregate and fibres) was achieved by segmenting based on voxel
intensity values, which are proportional to average density of the specimen within the volume mapped
by each voxel. Finally, reconstructions of the spatial distribution of the fibres were prepared by
segmenting the materials found in a specific volume, based on simple thresholding [26]. The software
used for the reconstruction of the CT scans images was ImageJ® .

2.7. Morphological Study of the Cracks before and after Healing

To qualitatively evaluate the effect of the heating time on the healing level of the asphalt
mixtures, the width of cracks has been measured by taking photographs of a square area with sides of
approximately 1 cm (see Figure 3), under an optical microscope Leica EZ4 with 35× magnification.
After the flexural test, the crack width of all samples was calculated as the average value of four
measurements equidistantly distributed along the image. In addition, the crack width was also
measured after healing by microwave heating at different times in all the tested samples, using the
same procedure. The software used for the crack-size measurements by optical images was ImageJ® .
 mixtures, the width of cracks has been measured by taking photographs of a square area with sides
of approximately 1 cm (see Figure 3), under an optical microscope Leica EZ4 with 35× magnification.
After the flexural test, the crack width of all samples was calculated as the average value of four
measurements equidistantly distributed along the image. In addition, the crack width was also
measured after healing by microwave heating at different times in all the tested samples, using the
Appl.
same Sci.procedure.
2017, 7, 1076 The software used for the crack-size measurements by optical images was ImageJ
6 of®15
.

Figure 3. Schematic diagram of the measurement of the crack size before and after microwave heating.
Figure 3. Schematic diagram of the measurement of the crack size before and after microwave heating.

3. Results and Discussion

3.1. Influence of Heating Time on the Thermal Behaviour of Asphalt Mixtures with Fibres
Table 2 shows the average results of the heating-cooling test of asphalt mixtures. The values
presented in this Table are: Tmax , maximum surface temperature reached by the samples; and CT,
cooling time until the samples reached the temperature before heating (20 ◦ C).
Regarding to heating of asphalt mixtures, it can be observed that the surface temperature of
the samples (Tmax in Table 2) increased with the increase of the microwave heating time, and that
this temperature was higher in samples with higher fibres contents. Thus, samples heated during
40 s registered the highest temperatures, followed by samples heated during 30 s, 20 s and 10 s,
respectively. Additionally, it can be seen that asphalt mixtures with 6% of fibres registered the highest
surface temperatures, followed by mixtures with 4%, 8%, 2% and 0%, in that order (reaching surface
temperatures of 98.86 ◦ C, 87.41 ◦ C, 78.71 ◦ C, 59.76 ◦ C and 50.46 ◦ C, respectively) when they were
heated during 40 s. Also, a similar trend was observed with the other three heating times.
Moreover, using short heating times (10 and 20 s), asphalt mixtures with different contents of
fibres presented similar temperature increases (see Table 2). For example, samples with 0% and 8% of
fibres registered temperature increases of 7.91 ◦ C and 10.33 ◦ C respectively, when they were heated
during 10 s. However, in the case of using long heating times (30 and 40 s), the asphalt mixtures with
different contents of fibres registered big differences regarding to their temperature increase, with the
same microwave heating time. Specifically, samples with 2% and 6% of fibres presented an increase on
their surface temperature of 39.76 ◦ C and 78.86 ◦ C respectively, when they were heated during 40 s.
This reveals that 10 s and 20 s are too short heating times to induce a significant heating of the fibres
that can distribute the temperature through the asphalt mixture and melt the bitumen, resulting in
those similar temperature increases in the samples regardless their fibre content.
Therefore, it does not seem likely that asphalt mixtures can heal their cracks using heating times
of 10 s and 20 s, due to the fact that the bitumen did not reach the temperature threshold required to
reduce its viscosity and flow through the cracks opened in the pavement, sealing it [21].

Table 2. Average results of the heating-cooling test on asphalt mixtures.

Microwave Heating Time (s)

Fibres Content 10 20 30 40
(% vol. Bitumen) Tmax CT Tmax CT Tmax CT Tmax CT
(◦ C) (min) (◦ C) (min) (◦ C) (min) (◦ C) (min)
2% 28.11 55 40.76 60 47.33 63 59.76 56
4% 28.13 55 45.56 81 64.90 85 87.41 54
6% 29.19 63 55.71 90 65.30 87 98.86 63
8% 30.33 65 47.19 88 61.93 81 78.71 92
Ref. 0% 27.91 48 40.08 22 45.26 52 50.46 44
Appl. Sci. 2017, 7, 1076 7 of 15

Furthermore, in view of the results presented in Table 2, it can be concluded that asphalt mixtures
with higher contents of fibres reached, in general, the highest surface temperatures. Nevertheless,
in the case of the samples with 8% of fibres, they did not register the highest surface temperature
values. This was attributed to the bad distribution of the fibres inside the asphalt mixtures with 8% of
fibres, which generates located heating in certain zones of the samples with presence of fibre clusters,
see Figures 4d and 5d, respectively. Then, the located heating is distributed to the rest of the sample,
as it can be observed in the sample with 2% of fibres, see Figure 4a. Thus, samples with 6% (Figure 4c),
and 4% (Figure 4b) of fibres reached the highest surface temperatures (Table 2) for the heating time of
40 s, since they present a better distribution of the fibres in the asphalt mixture matrix. This result can
also be seen in the CT-Scan images shown in Figure 5a–d.
Additionally, Table 3 presents the results of bulk density and air voids content of the asphalt
mixtures with different fibres content. As it can be observed, bulk density slightly decreased with the
Appl. Sci. 2017, 7, 1076 7 of 14
increase of fibres, while the air voids content increased with the increase of the amount of fibres
Appl. Sci. 2017, 7, 1076
added
7 of 14
toadded
the mixture. Therefore,
to the mixture. the heatthe
Therefore, distribution in thein
heat distribution samples with with
the samples a high content
a high of air
content of voids is not
air voids
the
is optimum
added
not theto the (see Figure
mixture.
optimum 4d), which
Therefore,
(see is attributed
thewhich
Figure 4d), to
heat distribution the heat
is attributedinto
the dissipation
samples
the through
with a high
heat dissipation the air
contentthe
through voids
of air inside
air voids
voids
these
insideasphalt
is not the
these mixtures.
optimum
asphalt (see Figure 4d), which is attributed to the heat dissipation through the air voids
mixtures.
inside these asphalt mixtures.

(a) (b) (c) (d)

(a) (b) (c) (d)
Figure 4. Thermographic images of asphalt mixtures with different fibre content after 40 s of
Figure 4. Thermographic images of asphalt mixtures with different fibre content after 40 s of microwave
Figure 4. Thermographic
microwave images
heating: mixtures of 2%;
with (a) asphalt mixtures
(b) 4%; with
(c) 6%;(d) 8%different fibrefibres.
of steel wool content after 40 s of
heating: mixtures with (a) 2%; (b) 4%; (c) 6%;(d) 8% of steel wool fibres.
microwave heating: mixtures with (a) 2%; (b) 4%; (c) 6%;(d) 8% of steel wool fibres.
Conversely,regarding
Conversely, regardingthe
thecooling
coolingresults
resultsshown
shownininTable
Table2,2,ititcan
canbe
beobserved
observedthatthatiningeneral
generalthe
Conversely, regarding the cooling results shown in Table 2, it can be observed
the longest cooling times were recorded after the heating times of 20 s and 30 s. In contrast, that in general
the
longest cooling times were recorded after the heating times of 20 s and 30 s. In contrast, the shortest
the longest cooling times were recorded after the heating times of 20 s and 30 s.
shortest cooling times were registered after 10 s and 40 s of heating. Additionally, these results areIn contrast, the
cooling
shortesttimes weretimes
cooling registered
were after 10 s and
registered after 4010s sofand
heating.
40 s Additionally,
of heating. these results
Additionally, theseareresults
relatedare
with
related with the temperatures reached by the samples. Thus, samples without fibres reached lower
the temperatures
related with the reached by thereached
samples. Thus, samples without fibres reached lower temperatures
temperatures andtemperatures
consequently neededby the samples.
a shorter time toThus, samples
cool down, without
while fibres
samples reached
with 6% andlower
8%
and consequently
temperatures needed
andthe a shorter
consequently time
needed to cool down,
a shorter time while samples with 6% and 8% of fibres reached
of fibres reached highest surface temperatures and to
tookcool down,
longer while
times to samples
cool down.with 6% and 8%
theofhighest surfacethe
fibres reached temperatures andtemperatures
highest surface took longer times to cool
and took down.
longer times to cool down.
2% fibres 4% fibres 6% fibres 8% fibres
2% fibres 4% fibres 6% fibres 8% fibres

Cluster
(a) (b) (c) Cluster (d)
(a) (b) (c) (d)
Figure 5. CT-scan 3D reconstructions of fibre spatial distribution inside asphalt mixture samples with
Figure 5. fibre
different CT-scan 3D reconstructions
contents: of fibre
(a) 2%; (b) 4%; 6%;spatial
(d) 8%distribution inside asphalt mixture
boxsamples with
Figure 5. CT-scan 3D reconstructions of(c)
fibre spatial of steel wool
distribution fibres.
inside Bounding
asphalt mixture dimensions
samples with
different fibre
are 25 × fibre
25 × 12contents: (a) 2%; (b)
mm, approximately. 4%; (c) 6%; (d) 8% of steel wool fibres. Bounding box dimensions
different contents: (a) 2%; (b) 4%; (c) 6%; (d) 8% of steel wool fibres. Bounding box dimensions
are 25 × 25 × 12 mm, approximately.
are 25 × 25 × 12 mm, approximately.
Finally, it can be deduced from Table 2 that, from a practical point of view, the best solution is
Finally,
to heat
Finally, it itcan
the samplescan be deduced
bewith from
4% or from
deduced 6% Table
fibres22during
ofTable that, from
that, 40 s.aaThis
from practical pointthese
pointofofview,
is because
practical the best
samples
view, solutionthe
thepresented
best is
solution is
to heat the samples with 4% or 6% of fibres during
also, 40 s. This
lastisisbecause these63samples
min topresented the
tohighest
heat thesurface
samples temperature
with 4% or increases
6% of fibresand, during they
40 s. This 54 min and
because these samples cool down,
presented the
highest surface
respectively. temperature inincreases and,thealso, they lastobtained
54 minwith
and 63 min of
to 10
cool down,
highest surfaceThese times areincreases
temperature the range
and,ofalso, cooling
they last times
54 min and 63 mina to heating
cool down, s.respectively.
Besides,
respectively.
regarding These times are in the range of the cooling times obtained with a heating of 10 s. Besides,
These times the
are application
in the rangeofofthese asphalt times
the cooling mixtures in road
obtained pavements,
with a heatingthey
of 10could be microwave
s. Besides, regarding
regarding
heated the application
during of these
40 s, reaching surfaceasphalt mixturesover
temperatures in road
85 °C,pavements,
implying they could
that the be microwave
traffic should be
heated during
stopped during40 s, reaching surface
approximately temperatures
1 h to heal the cracks over 85 °C, to
and return implying thattemperature.
the service the traffic should be
stopped during approximately 1 h to heal the cracks and return to the service temperature.
Table 3. Bulk density and air void content of asphalt mixtures (Average ± Stand. Deviation).
Table 3. Bulk density and air void content of asphalt mixtures (Average ± Stand. Deviation).
Fibres Content Bulk Density Air Voids
Appl. Sci. 2017, 7, 1076 8 of 15

the application of these asphalt mixtures in road pavements, they could be microwave heated during
40 s, reaching surface temperatures over 85 ◦ C, implying that the traffic should be stopped during
approximately 1 h to heal the cracks and return to the service temperature.

Table 3. Bulk density and air void content of asphalt mixtures (Average ± Stand. Deviation).

Fibres Content
Bulk Density (g/cm3 ) Air Voids Content (%)
(% vol. Bitumen)
2% 2.33 ± 0.02 7.45 ± 0.98
4% 2.32 ± 0.02 8.70 ± 0.98
6% 2.31 ± 0.02 9.64 ± 0.92
8% 2.28 ± 0.03 11.43 ± 0.97

Appl. Sci. 2017, 7, 1076 Ref. 0% 2.35 ± 0.02 6.70 ± 0.85 8 of 14

3.2. Influence
Influence of Fibres and Heating Time on the Asphalt Self-Healing Properties
Properties
Figure 6a–d shows the results of the healing levels reached by the asphalt mixtures with fibres
depending on the number
number of healing
healing cycles,
cycles, using
using microwave
microwave heating
heating atat 44 different
different times:
times: 1010 s,s, 20
20 s,s,
30 s and
and 40
40 s.
s. In
Inthese
theseFigures,
Figures,ititcancanbebeobserved
observedthat
thatmicrowave
microwave heating
heating helps
helps toto the
the partial
partial resistance
resistance
recovery of cracked asphalt mixtures with fibres. fibres. In addition, it can be observed
observed that the healing
healing levels
levels
reached by the mixtures increased with the increase of the microwave heating time. Thus, the highest
healing levels
levels reached
reachedby bythe thesamples
samples areare
thethe obtained
obtained using
using 40 s40
as sthe
as heating
the heating
time,time, followed
followed by those by
those obtained
obtained using using 30s s,and
30 s, 20 20 10
s and 10 s, respectively
s, respectively (see Figure
(see Figure 6). This6).was
This was produced
produced becausebecause
the longer the
longer the heating
the heating time, thetime,
higher thethe
higher the temperature
temperature reached byreached by the(see
the samples samples
Table (see Tableallowed
2), which 2), which to
allowed to reach
reach higher higher
healing healing levels.
levels.

1.0 2% fibres 1.0 2% fibres

4% fibres 4% fibres
6% fibres 6% fibres
0.8 8% fibres 0.8 8% fibres
Healing level at 10s

Healing level at 20s

0.6 0.6

0.4 0.4

0.2 0.2

0.0 0.0
1 2 3 4 5 6 7 8 9 10 1 2 3 4 5 6 7 8 9 10
Microwave healing cycles Microwave healing cycles

(a) (b)
1.0 2% fibres 1.0 2% fibres
4% fibres 4% fibres
6% fibres 6% fibres
0.8 0.8
8% fibres 8% fibres
Healing level at 40s
Healing level at 30s

0.6 0.6

0.4 0.4

0.2 0.2

0.0 0.0
1 2 3 4 5 6 7 8 9 10 1 2 3 4 5 6 7 8 9 10
Microwave healing cycles Microwave healing cycles

(c) (d)
Figure
Figure 6.
6. Healing
Healing levels
levels of
of asphalt
asphalt mixtures
mixtures with
with different
different content
content of
of fibres,
fibres, depending
depending on on the
the number
number
of healing cycles, heated in a microwave at 4 different times: (a) 10 s; (b) 20 s; (c) 30 s and (d)
of healing cycles, heated in a microwave at 4 different times: (a) 10 s; (b) 20 s; (c) 30 s and (d) 40 40 s.
s.

Additionally, it can be seen that in the cases of short heating times (10 and 20 s), the number of
healing cycles has not a significant influence on the healing level of the samples. For example, in the
case of 20 s heating times (see Figure 6b), samples with 6% of fibres reached healing levels of 38% and
29% after the first and tenth cycles, respectively. In contrast, with longer heating times (30 and 40 s),
it can be observed that the healing levels reduced with the increase of the number of healing cycles.
 Appl. Sci. 2017, 7, 1076 9 of 15

Additionally, it can be seen that in the cases of short heating times (10 and 20 s), the number of
healing cycles has not a significant influence on the healing level of the samples. For example, in the
case of 20 s heating times (see Figure 6b), samples with 6% of fibres reached healing levels of 38% and
29% after the first and tenth cycles, respectively. In contrast, with longer heating times (30 and 40 s),
it can be observed that the healing levels reduced with the increase of the number of healing cycles.
In the case of samples with 4% of fibres heated 40 s (see Figure 6d), healing levels of 93% and 49% are
reached after the first and tenth healing cycles, respectively. The variation can be attributed to the high
temperatures reached by the asphalt samples when heated for long times (see Table 2).
This behaviour was also observed in previous researches [17] that demonstrated that microwave
heating can change the internal structure of asphalt mixtures, modifying the aggregates position
inside the samples and thus changing the air void content distribution of the mixtures. In this way,
the mechanical resistance of asphalt mixtures and consequently their healing levels are reduced after
each cycle. In addition, using these heating times (30 and 40 s), the bitumen can also be damaged in
each cycle (see Figure 7).
Furthermore, in cases of long heating times it can be observed that healing levels also depend
Appl. Sci. 2017, 7, 1076 9 of 14
on the fibres content added to the asphalt mixtures. In general, mixtures with 6% and 2% of fibres
registeredthe
registered thehighest
highesthealing
healinglevels
levelsininthe
thecase
caseofof3030s sheating
heating(see
(seeFigure
Figure6c),
6c),followed
followedby bymixtures
mixtures
with 4% and 8% of fibres, respectively. Therefore, higher healing levels are not necessary attributedto
with 4% and 8% of fibres, respectively. Therefore, higher healing levels are not necessary attributed
tohigher
highermechanical
mechanical resistance
resistanceandand
higher fibres
higher contents,
fibres as canasbecan
contents, deduced from the
be deduced obtained
from results of
the obtained
the maximum flexural force (force initially resisted by the samples before submitted
results of the maximum flexural force (force initially resisted by the samples before submitted to to cracking-healing
cycles) in Figurecycles)
cracking-healing 8a. Thisinresult
Figurecan8a.
beThis
due to the temperature
result can be due reached by the samples
to the temperature whenby
reached heated
the
during 30 s (see Table 2). Thus, the samples that reached high temperatures
samples when heated during 30 s (see Table 2). Thus, the samples that reached high temperatures (6% of fibres) presented
high
(6% of healing levels (60%
fibres) presented on average).
high healing levels (60% on average).

(a) (b) (c) (d)

Figure
Figure7.7.Optical
Opticalmicroscope
microscopeimages
imagesofofthe
thecrack
crackproduced
producedononananasphalt
asphaltsample
samplewithwith4%
4%ofoffibres,
fibres,inin
different
different stages of the cyclic healing process: (a) before healing; (b) after the 2nd healing cycle; (c)after
stages of the cyclic healing process: (a) before healing; (b) after the 2nd healing cycle; (c) after
the
the5th
5thhealing
healingcycle;
cycle;(d)
(d)after
afterthe
the10th
10thhealing
healingcycle.
cycle.Image
Imagedimensions
dimensionsare are8 8× ×
1010
mm,
mm,approximately.
approximately.

InInaddition,
addition,mixtures
mixtureswith with2%2%andand4% 4%ofoffibres,
fibres,registered
registeredsimilar
similarvalues
valueson ontheir
theirhealing
healinglevels
levels
(55%
(55%on onaverage),
average),which
whichcancanbeberelated
relatedwith
withthethefact
factthat
thattheir
theirair
airvoid
voidcontent
contentand andfibres
fibresdistribution
distribution
inside
insidethem
them areare
similar.
similar.Finally, mixtures
Finally, mixtureswithwith
8% of 8%fibres presented
of fibres the lowest
presented healinghealing
the lowest levels (40%
levels
on average)
(40% after microwave
on average) heatingheating
after microwave during during
30 s. This 30can be mainly
s. This can be attributed to the fact
mainly attributed to that higher
the fact that
fibres
higher content produceproduce
fibres content higher higher
air voidair contents in the
void contents mixtures,
in the mixtures,thatthat
consequently
consequently produced
produceda a
decrease
decreaseon ontheir
theirflexural
flexuralresistance
resistance(see(seeFigure
Figure8a),
8a),and
andananincrease
increaseon onthetheformation
formationofoffibrefibreclusters
clusters
(see
(seeFigures
Figures4d4dandand5d),
5d),which
whichmeans
meansthatthatthe
theuse
useofofasphalt
asphaltmixtures
mixtureswithwithelevated
elevatedcontents
contentsofoffibres
fibres
isisnot
notrecommended.
recommended.
Moreover,
Moreover,analysing
analysingthe theerror
errorbars
barsobtained
obtainedfrom fromthe thehealing
healinglevel
levelresults
results(see
(seeFigure
Figure6),6),ititcan
can
bebeobserved
observedthat,that,regardless
regardlessthe thehealing
healingcycle,
cycle,thethevariability
variabilityofofthe theresults
resultsobtained
obtainedfrom fromsamples
samples
with
withdifferent
differentfibres
fibrescontent
contentwas wassimilar
similarforforall
allthe
theheating
heatingtimes.
times.ThisThissuggests
suggeststhat thatthere
thereisisnot
nota a
significant difference between healing levels of asphalt mixtures with different
significant difference between healing levels of asphalt mixtures with different fibre contents. However, fibre contents.
However, the influence
the influence of content
of the fibres the fibres oncontent on the
the healing healing
levels levels
reached by reached
the asphaltby the asphalt
mixtures hasmixtures
not been
has not been proved. Due to that, the Cycle Reduction Ratio (CRR) has been
proved. Due to that, the Cycle Reduction Ratio (CRR) has been defined in this study with the purpose defined in this study
with the purpose of evaluating if an increase on the fibres content has an effect on the healing level
of asphalt mixtures, according to the following Equation:
‫ܮܪ‬௜
‫ ܴܴܥ‬ൌ ൤ ൨ (2)
‫ܮܪ‬௠௔௫ ௡

where n is the studied healing cycle, HLi is the healing level of an asphalt sample with i% of fibres
Appl. Sci. 2017, 7, 1076 10 of 15

of evaluating if an increase on the fibres content has an effect on the healing level of asphalt mixtures,
according to the following Equation:
 
HLi
CRR = (2)
HLmax n

where n is the studied healing cycle, HLi is the healing level of an asphalt sample with i% of fibres and
HLmax is the maximum healing level within the cycle n (considered as the average healing level obtained
from the samples with the fibres content that reach the maximum value). This ratio represents the
variation of the healing level of asphalt mixtures within a specific cycle, with different fibres contents.
With the aim of demonstrating that the difference between CRR values is due to the scatter of
the results (see Figure 6), the Weibull probability of all CRR data has been calculated and presented
versus the data percentiles in a probability-probability plot, see Figure 8b. This probability function
was used considering that the cyclical process of cracking-healing fits to a fracture process of materials,
idealized by means of a damage function of Weibull type [26]. Figure 8b represents all the CRR data
regardless the healing cycle and fibres content, for all the studied heating times. The results show
that CRR values are aligned to a straight line with a slope 1:1, thus fitting to the Weibull distribution
function. This
Appl. Sci. 2017, means that the differences between healing levels reached by the asphalt mixtures
7, 1076 10 of 14
within a specific cycle can be attributed to statistical variations, which implies that the maximum
maximum
healing healing
levels levels
in a cycle areinnot
a statistically
cycle are not statistically
significant andsignificant and that
that these values are these values are
not produced not
by the
producedof
influence bythe
thefibres
influence
or theofnumber
the fibres
of or the number
cycle. of cycle.
Consequently, Consequently,
it can it can
be stated that the be stated that
variable that has
the
variable that
influence hashealing
on the influence on is
level the healing
the heatinglevel is the heating time.
time.

3.5 1

3.0 0.9
Maximum flexural force (kN)

0.8
Weibull Probability

2.5
0.7

2.0 0.6
0.5
1.5 10s
0.4 20s
0% fibres
1.0 2% fibres 0.3 30s
4% fibres R² = 0.8675 40s
6% fibres 0.2
0.5 8% fibres Line 1:1
0.1
Lineal (average)
0.0 0
4 6 8 10 12 14 0 0.2 0.4 0.6 0.8 1
Air voids content (%) Probability ((i-0.5)/n)
(a) (b)
Figure 8.
Figure 8. (a)
(a) Maximum
Maximum flexural
flexural force
force versus
versus the
the air
air void
void content
content of
of asphalt
asphalt mixtures
mixtures with
with different
different
fibres content;
fibres content; (b)
(b) Weibull
Weibullprobability-probability
probability-probabilityplot
plotfor
forall
allCycle
CycleReduction
ReductionRatio
Ratiodata.
data.

Besides, the goodness of fit of the CRR data series to the Weibull Weibull distribution
distribution function
function can be
observed in
observed in Figure
Figure 8b,
8b,for
forthe
thedifferent
differentheating
heatingtimes.
times.InInthis
thiscontext,
context,it itcan
canbebe stated
stated that
that thethe better
better is
is the
the data
data fitting,
fitting, the
the higherisisthe
higher theinfluence
influenceofofheating
heatingtimetimeon onthe
thehealing
healing levels
levels of asphalt mixtures.
mixtures.
As can
As can be
be seen,
seen, CRR
CRR data corresponding to 30 s and 40 s heating times fit better to the probability
distribution function,
distribution function,while
while CRR CRRdatadata corresponding
corresponding to 10to 10 20
s and s and 20 s times
s heating heating
are times are more
more dispersed,
dispersed,
see see Figure
Figure 8b. On the 8b.oneOn the the
hand, one worse
hand, fitting
the worse fitting
to the to the
Weibull Weibull distribution
distribution function offunction
CRR data of
CRR data corresponding
corresponding to heating to heating
times of 10times
s andof2010 s iss related
and 20 withs is related
the high with the and
scatter highrandomness
scatter and
randomness
of of healing
healing levels levels
of asphalt of asphalt
mixtures mixtures
heated duringheated
shortduring
times. short
On the times.
otherOn the other
hand, in thehand, in
case of
the casesamples
asphalt of asphalt samples
heated heated
during 30 s during
and 40 s, 30they
s and 40 s,
have they have
enough time enough
to increasetimetheir
to increase their
temperature
temperature
and distributeand distribute
it. Based it. Based
on these on itthese
results, results, it
is necessary to is necessary
define to define
an optimum an optimum
heating time of heating
asphalt
time of asphalt
mixtures mixtures radiation.
via microwave via microwave radiation.
In this context, Figure 9 presents the healing levels of asphalt mixtures with 4% of fibres, at 7
different heating times (from 10 s to 100 s). In this Figure, the heating times of 60 s, 80 s and 100 s
have been obtained from a previous work of Norambuena-Contreras and García [17]. As it can be
seen in Figure 9 there are 2 possible optimum times, 40 s and 100 s, since they allow asphalt mixtures
to obtain the highest healing levels. However, heating time of 100 s was discarded against 40 s due
Appl. Sci. 2017, 7, 1076 11 of 15

In this context, Figure 9 presents the healing levels of asphalt mixtures with 4% of fibres,
at 7 different heating times (from 10 s to 100 s). In this Figure, the heating times of 60 s, 80 s and 100 s
have been obtained from a previous work of Norambuena-Contreras and García [17]. As it can be seen
in Figure 9 there are 2 possible optimum times, 40 s and 100 s, since they allow asphalt mixtures to
obtain the highest healing levels. However, heating time of 100 s was discarded against 40 s due to
the fact that heating asphalt mixtures by microwave during 100 s melted the bitumen, thus damaging
the composite material. In addition, the effect of heating the samples during 100 s can be observed in
Figure 9, as the reduction on the healing levels after each healing cycle. Therefore, it can be stated that
Appl. Sci. 2017, 7, 1076 11 of 14
using a 700 W microwave with a working frequency of 2.45 GHz, the optimum heating time is 40 s.

1.0 10s 20s 30s 40s 60s 80s 100s

Healing level (4% fibres)

0.8

0.6

0.4

0.2

0.0
1 2 3 4 5
Microwave healing cycles

Figure 9. Healing levels of asphalt mixtures with 4% of fibres, depending on the heating time (includes
Figure 9. Healing levels of asphalt mixtures with 4% of fibres, depending on the heating time
results of healing level at 60 s, 80 s and 100 s from the previous research of Norambuena-Contreras and
(includes results of healing level at 60 s, 80 s and 100 s from the previous research of Norambuena-
García [17]).
Contreras and García [17]).

3.3. Crack-Size of
3.3. Crack-Size of Asphalt
Asphalt Samples
Samples Healed
Healed by
by Microwave
Microwave Radiation
Radiation
Figure
Figure 10a 10a shows
shows the the frequency
frequency histogram
histogram for for the
the average
average crack
crack size
size measured
measured using using an an optical
optical
microscope
microscope of of all
all the
thesemi-circular
semi-circularsamplessamplesafter afterthe
the first
first three-point
three-point bending
bending test.
test. It can It can be seen
be seen that
that the average size of the open cracks before healing is 0.431 mm, and
the average size of the open cracks before healing is 0.431 mm, and that the values ranged from 0.141 that the values ranged from
0.141
mm and mm0.781
and mm.0.781Additionally,
mm. Additionally, with thewith aimtheof aim
knowingof knowing if the amount
if the amount of fibresofadded
fibres toadded to
asphalt
asphalt
mixtures mixtures
have anhave an influence
influence on the on thesize,
crack cracka size, a probability
probability analysis analysis
has been has developed.
been developed. In thisInway,
this
way, Figure 10b presents the Normal probability-probability plot for all
Figure 10b presents the Normal probability-probability plot for all the crack size data obtained from the crack size data obtained
from the samples
the samples regardless
regardless theirtheir amount
amount of fibres
of fibres added
added to to
thethemixtures.
mixtures.It Itcancanbe be seen
seen that
that the
the
relationship
relationship between the Normal probability and the data percentiles align in a straight line with aa
between the Normal probability and the data percentiles align in a straight line with
1:1
1:1 slope,
slope, which
which means
means that that it
it can
can be concluded that
be concluded that the amount of
the amount fibres added
of fibres added to the asphalt
to the asphalt mixture
mixture
has
has not
not aa significant
significant influence
influence on on the
the size
size ofof the
the cracks
cracks produced
produced in in the
the semi-circular
semi-circular samples
samples by by the
the
three-point bending
three-point bending test. test.
Moreover,
Moreover, FigureFigure 11a 11a shows
shows the the box-plot
box-plot graphgraph of of the
the crack
crack sizesize measured
measured in in all
all the
the samples
samples
before
before (shown
(shown as as 00 s)
s) and
and after
after healing
healing byby microwave
microwave heatingheating at at different
different times
times (10(10 s,s, 20
20 s,
s, 30
30 ss and
and
40 s), regardless the amount of fibres added to the mixtures. Observing
40 s), regardless the amount of fibres added to the mixtures. Observing this Figure, it can be this Figure, it can be concluded
that the longer
concluded thatisthe
thelonger
heating time,
is the the smaller
heating time, theare the crackare
smaller sizes
themeasured
crack sizesonmeasured
the samples. on the In samples.
addition,
with shorterwith
In addition, heating times
shorter (10 s times
heating and 20(10s),s and
the measured cracks presented
20 s), the measured more dispersed
cracks presented values,
more dispersed
that
values, that can be related with the dispersion of the healing level results, see Figure 6a,b. In thiscrack
can be related with the dispersion of the healing level results, see Figure 6a,b. In this way, way,
sizes
crack measured
sizes measuredon theonhealed samples
the healed ranged
samples fromfrom
ranged 0.0350.035
mm mm to 0.38 mm,mm,
to 0.38 andandfrom from0.032 mm
0.032 mmto
0.206 mm, in the case of samples heated during 10 s and 20 s, respectively.
to 0.206 mm, in the case of samples heated during 10 s and 20 s, respectively. While samples heated While samples heated
during
during 30 30 ssand
and40 40s spresented
presentedcrack crackapertures
apertures ranged
ranged fromfrom0.018 mmmm
0.018 to 0.072 mm,mm,
to 0.072 and and fromfrom
0.0140.014
mm
to
mm 0.058 mm, mm,
to 0.058 respectively.
respectively.
Furthermore, a crack has been considered healed when its aperture after healing is half of the
minimum aperture measured before healing, which is under 0.07 mm. In view of that, it can be
concluded that only the cracks of the samples heated during 30 s and 40 s were healed, which
reaffirms the results obtained from the measurements of the self-healing levels of asphalt mixtures,
see Figure 6c,d. In contrast, although samples heated during 10 s and 20 s can heal some of their
Appl. Sci. 2017, 7, 1076 12 of 15

Furthermore, a crack has been considered healed when its aperture after healing is half of the
minimum aperture measured before healing, which is under 0.07 mm. In view of that, it can be
concluded that only the cracks of the samples heated during 30 s and 40 s were healed, which reaffirms
the results obtained from the measurements of the self-healing levels of asphalt mixtures,
see Figure 6c,d. In contrast, although samples heated during 10 s and 20 s can heal some of their cracks,
they are more likely to obtain wide crack sizes, not being able to heal most of the open cracks and
Appl. Sci. 2017, 7, 1076 12 of 14
consequently
Appl. Sci. 2017, 7,losing
1076 a high percentage of the initial mechanical resistance, see Figure 11b. 12 of 14

25 1
25 1
Average = 0.431
Average
Mode ==0.386
0.431
Mode = 0.386 Crack initial size
Variance = 0.025 0.8 Crack initial size
20 Variance
20 Std. Dev.= =0.025 0.8

Probability
0.161

NormalProbability
Std.
CV Dev. = 0.161
= 0.373
CV = 0.373
Frequency
Frequency

15 0.6
15 0.6

10 0.4

Normal
10 0.4
y = 0.974x + 0.0225
y = 0.974x + 0.0225
R² = 0.983
5 0.2 R² = 0.983
5 0.2

0 0
0 0
<0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 >0.8 0 0.2 0.4 0.6 0.8 1
<0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 >0.8 0 0.2 0.4 0.6 0.8 1
Crack initial size (mm) Probability ((i-0.5/n))
Crack initial size (mm) Probability ((i-0.5/n))
(a) (b)
(a) (b)
Figure 10. (a) Frequency histogram and statistical parameters of the crack initial size data; and (b)
Figure
Figure10. (a)Frequency
10. (a) Frequency histogram
histogram and statistical
and statistical parameters
parameters of the
of the crack crack
initial sizeinitial size(b)
data; and data;
Normal probability-probability plot for the crack sizes.
Normal
and probability-probability
(b) Normal plot for the
probability-probability plotcrack sizes.
for the crack sizes.

0.8 Maximum
0.8 Maximum
0.7 Third quartile
0.7 Third quartile
0.6 Median
0.6 Median
(mm)
size(mm)

0.5 First quartile

0.5 First quartile
0.4
Cracksize

Minimum
0.4 Minimum
0.3
Crack

0.3
0.2
0.2
0.1
0.1
0
0
0 10 20 30 40
0 10 20 30 40
Heating time by microwave (s)
Heating time by microwave (s)
(a) (b)
(a) (b)
Figure 11. (a) Box plot representation of the crack size before healing (heating time = 0 s) and after
Figure 11. (a) Box plot representation of the crack size before healing (heating time = 0 s) and after
Figure 11.of (a)
healing Box mixture
asphalt plot representation of the heating
samples at different crack size before
times; healing
(b) Optical (heating
images time = asphalt
of a cracked 0 s) and
healing of asphalt mixture samples at different heating times; (b) Optical images of a cracked asphalt
after
sample before and after heating by microwave radiation at 40 s (Image dimensions are 8 × 10cracked
healing of asphalt mixture samples at different heating times; (b) Optical images of a mm,
sample before and after heating by microwave radiation at 40 s (Image dimensions are 8 × 10 mm,
asphalt sample before and after heating by microwave radiation at 40 s (Image dimensions are
approximately).
approximately).
8 × 10 mm, approximately).
4. Conclusions
4. Conclusions
4. Conclusions
This paper has studied the effect of the microwave heating time on the self-healing properties of
This paper has studied the effect of the microwave heating time on the self-healing properties of
asphalt
This mixtures
paper containing
hascontaining
studied the metallic
effect offibres. To do this, an experimental
the microwave study including heating- of
asphalt mixtures metallic fibres. To do this, heating time on the
an experimental self-healing
study includingproperties
heating-
cooling
asphalt tests and
mixtures cracking-healing
containing metallic cyclic
fibres.tests
To was
do carried
this, an out on asphalt
experimental mixtures
study with heating-cooling
including four different
cooling tests and cracking-healing cyclic tests was carried out on asphalt mixtures with four different
contents
tests of steel wool fibres,
and cracking-healing evaluating
cyclic tests was the (1) thermal behaviour under microwave heating; (2) self-
contents of steel wool fibres, evaluating thecarried out on
(1) thermal asphalt mixtures
behaviour with fourheating;
under microwave different
(2)contents
self-
healing properties at different heating times; and (3) crack-sizes in the asphalt mixtures before and
healing properties at different heating times; and (3) crack-sizes in the asphalt mixtures before and
after healing. The main conclusions of this article are summarised as follows:
after healing. The main conclusions of this article are summarised as follows:
• It was proved that the longer the microwave heating time and the higher the amount of fibres,
• It was proved that the longer the microwave heating time and the higher the amount of fibres,
the higher the reached temperatures. However, the influence of the metallic fibres amount on
the higher the reached temperatures. However, the influence of the metallic fibres amount on
the asphalt mixtures heating occurs in the case of long times (30 s and 40 s).
the asphalt mixtures heating occurs in the case of long times (30 s and 40 s).
Appl. Sci. 2017, 7, 1076 13 of 15

of steel wool fibres, evaluating the (1) thermal behaviour under microwave heating; (2) self-healing
properties at different heating times; and (3) crack-sizes in the asphalt mixtures before and after healing.
The main conclusions of this article are summarised as follows:

• It was proved that the longer the microwave heating time and the higher the amount of fibres,
the higher the reached temperatures. However, the influence of the metallic fibres amount on the
asphalt mixtures heating occurs in the case of long times (30 s and 40 s).
• Additionally, it was found that asphalt mixtures with 6% of fibres reached the highest surface
temperatures followed by mixtures with 4% of fibres, while mixtures with 8% of fibres presented
difficulties during heating due to the bad distribution of the fibres, proved by CT scans analysis.
• In addition, cooling times after heating the asphalt mixtures during 40 s are in the range of those
obtained with a heating of 10 s (between 54 min and 63 min). Consequently, the best solution is
to heat the samples with 4% or 6% of fibres during 40 s, thus achieving that the application of
these asphalt mixtures in road pavements should imply that they could be microwave heated
during 40 s, implying that the traffic should be stopped for approximately 1 h to heal the cracks
and return to the service temperature.
• Moreover, it was found that the healing level of the asphalt mixtures increased with the increase
of the microwave heating time, due to the higher temperatures reached by the samples when
heated longer times. However, using long heating times (30 s and 40 s), the mechanical resistance
of asphalt mixtures and consequently their healing levels were reduced after each healing cycle.
• It was also found that the temperature achieved as a result of the heating time is the most
influential variable on the self-healing properties of asphalt mixtures, while the fibres amount did
not have a significant influence on the healing levels of asphalt mixtures.
• In addition, based in the results of this and previous research, it was concluded that the optimum
microwave heating time is 40 s, since the highest healing levels are reached without an early
damage of the bitumen.
• Finally, the probability analysis of the morphological study of the cracks revealed that the presence
of fibres did not have influence on the obtained crack-size. Additionally, in view of the crack-sizes
obtained with the different microwave heating times, it was demonstrated that the cracks can be
sealed using long heating times (30 s and 40 s), consequently achieving the self-healing of asphalt
mixtures via microwave heating.

The results contained in this paper are part of a research about self-healing asphalt mixtures
including metallic waste materials that is being developed in Chile. The second part of the study,
currently under development, is the evaluation of the effect of adding different metallic waste to asphalt
mixtures, e.g., steel shavings, analysing their self-healing properties under microwave radiation.

Acknowledgments: The authors want to thank the financial support given by the National Commission
for Scientific & Technological Research (CONICYT) from the Government of Chile, through the Research
Project FONDECYT Initiation 2014 No. 11140103. In addition, the authors would also like to acknowledge
the experimental help provided by Eng. José L. Concha from LabMAT and the bachelor student Manuel Riffo,
from the Department of Civil and Environmental Engineering, both from the University of Bío-Bío. Finally,
the authors also want to thank Ricardo Serpell from PUC-Chile for his help with the CT-Scan tests.
Author Contributions: José Norambuena-Contreras is the Principal Investigator of the Project
(FONDECYT Initiation 2014 No. 11140103), and was responsible of all the research presented in this
paper. His work was specially focused on the data analysis and manuscript writing. Irene Gonzalez-Torre is part
of the technical staff involved in the Research Project. Her work included carrying out the experimental tests,
data collection and test result analysis.
Conflicts of Interest: The authors declare no conflict of interest. The founding sponsors had no role in the design
of the study; in the collection, analyses, or interpretation of data; in the writing of the manuscript, and in the
decision to publish the results.
Appl. Sci. 2017, 7, 1076 14 of 15

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