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Materials and Structures (2016) 49:2439–2454

DOI 10.1617/s11527-015-0659-6

ORIGINAL ARTICLE

New experimental methods for characterizing formation


and decay of foam bitumen
Biruk W. Hailesilassie . Martin Hugener .
Andrea Bieder . Manfred N. Partl

Received: 10 April 2015 / Accepted: 22 June 2015 / Published online: 8 July 2015
Ó RILEM 2015

Abstract Formation and decay of foam bitumen is a for obtaining information on the in situ surface
highly dynamic temperature dependent process which temperature of foam bitumen during the hot foaming
makes characterization difficult. In this research, new process. The result showed that the average surface
experimental tools were applied for characterizing the temperature of foam bitumen depends on the water
bitumen foam during the foaming process. Ultrasonic content of the bitumen and bubble size distribution,
sensors were used for accurately monitoring the 108 and 126 °C for 4 and 1 wt% (by weight) water
expansion and decay of foam bitumen as a function content respectively. The residual water content in the
of time. Assessment of foam bitumen viscosity was decaying foam bitumen was determined by thermo-
performed using high frequency torsional rheometer gravimetric analysis. The result demonstrated that
and in situ observation by X-ray radiography. A high- residual water content depends on the initial water
speed camera was applied for examining the foam content, and was found to be between 38 and 48 wt%
bitumen stream right at the nozzle revealing that foam of the initial water content of 4–6 wt%. Finally, X-ray
bitumen at a very early stage contains fragmented computed tomography was applied for examining the
pieces of irregular size rather resembling a liquid than decay of foam bitumen revealing that the bubbles of
foam. Moreover, infrared thermal images were taken foam bitumen remain trapped close to the surface of
the foam bitumen.

Electronic supplementary material The online version of Keywords Foam bitumen characterization  Process
this article (doi:10.1617/s11527-015-0659-6) contains supple- monitoring  X-ray analysis  Thermal properties
mentary material, which is available to authorized users.

B. W. Hailesilassie (&) A. Bieder


Infrastructure Engineering, Division of Highway and AmmannSchweiz AG, Eisenbahnstrasse 25,
Railway Engineering, School of Architecture and the 4901 Langenthal, Switzerland
Built Environment, Royal Institute of Technology (KTH), e-mail: andrea.bieder@ammann-group.com
100 44 Stockholm, Sweden
e-mail: biruk.hailesilassie@abe.kth.se M. N. Partl
KTH Stockholm, Division of Highway and Railway
M. Hugener Engineering, Director Road Engineering/Sealing
Road Engineering/Sealing Components, EMPA, Swiss Components, EMPA, Swiss Federal Laboratories for
Federal Laboratories for Material Science and Material Science and Technology, Ueberlandstrasse 129,
Technology, Ueberlandstrasse 129, 8600 Duebendorf, 8600 Duebendorf, Switzerland
Switzerland e-mail: manfred.Partl@empa.ch
e-mail: Martin.Hugener@empa.ch
2440 Materials and Structures (2016) 49:2439–2454

1 Introduction curve. Earlier, the FI parameter was considered as a


good indicator of the foam quality since it is calculated
Foam bitumen allows to construct asphalt pave- from the whole decay curve. However, it was found
ments at reduced temperature in terms of mixture that the FI concept cannot be applied for all types of
production, transport, laying and compaction [1]. bitumen. The half-life is not always decreasing with
Reducing production and compaction temperatures increasing ERm [8, 9]. Since half-life may increase or
by using warm mix asphalt (WMA) in place of hot decrease with increasing water content in the foam, it
mix asphalt (HMA) is environmentally beneficial is not a clear indicator for the stability of the foam
since it decreases fuel or energy consumption, bitumen. Moreover, the rheology and stability of the
reduces emissions of CO2 and reduces smoke from foam are mainly depending on the foam’s bubble size
mixing plant and improves working conditions at distribution and liquid volume fraction, i.e. the ratio of
the paving site [2, 3]. liquid volume to the total volume of the foam [10]. For
However, experience shows that foam asphalt determining the rate of bubble growth in dry foam
produced at lower temperature still requires improve- (liquid volume fraction\1–30 %), the bubble size and
ments to meet the requirements for heavy duty roads. shape are crucial since the foam bubbles can contain
Higher void content as compared to HMA and tetrahedral junctions and polyhedral faces. For wet
incomplete coating of large aggregates are main issues foam (liquid volume fraction [1–30 %) the influence
of enhancement. Foam bitumen is a mixture of air, of the bubble shape is less significant since the bubbles
water and bitumen. It is produced through injecting are expected to be more spherical [11]. Saleh [9] stated
small quantities of water, typically 1.0–6.0 % by that the optimum water content (WC) can be found
weight of the bitumen, into hot bitumen at a temper- from rotational viscosity measurement (using Brook-
ature 160–180 °C. The bitumen expands to about 5–15 field rotational viscometer). The water content that
times its original volume [4] forming a foam, which is produces the lowest average viscosity over a period of
highly efficient in wetting and coating the surface of 60 s is considered as optimum water content. This
fine particles [3]. When the foam collapses, most of the means, if two different bitumens have the same
water is lost as steam, leaving residual bitumen with viscosity but different expansion ratio and half-life,
properties similar to the original bitumen [5]. the mixing behavior of the foam bitumen can be
Foam bitumen can be characterized by different similar [9]. However the result could be in question,
parameters such as maximum expansion ratio (ERm), since the rate of foam collapse and the moisture
minimum viscosity, foaming index (FI) [3], coefficient content can influence the viscosity. Moreover, the
of foamability and half-life (s), which is defined as the instrument used for measuring the viscosity may
time that the expanded bitumen takes to settle to half distort the foam structure. In addition, locally deter-
its expanded volume [6]. The half-life is used to mining the foam viscosity after a certain time of decay
explain the stability of foam bitumen in general. The may not give a reliable result since foam bitumen
desirable design value of the half-life is difficult to contains a non-homogenous bubble size distribution
determine since it varies with the addition of water. within its bulk volume. Moreover, foaming bitumen is
The maximum expansion ratio (ERm = Vmax/Vo) is dynamic process with very quickly changing bubble
determined by the ratio of the volume of the expanded size distribution of the unstable foam. The coefficient
foam bitumen (Vmax) and the volume of the original of foamability is defined as the ratio of maximum
unfoamed bitumen (Vo). Both half-life (s) and ERm are expansion to the optimum water content at a given
still taken as main indicators of foam quality, in spite bitumen temperature. Lesueur et al. [12] stated that
of the fact that these parameters have no direct link to this coefficient is constant for a given bitumen type
the physical properties of bitumen in the foam. and independent of foaming temperature but relies on
Sufficient expansion of the bitumen is required for the type of nozzle used for foaming [12]. However, to
adequate coating of aggregates. Inadequate expansion the best knowledge of the authors, up to now no more
of foam bitumen lucks dispersion on the aggregate detailed work is available on how the foam bitumen is
during mixing [7]. The FI is the area under the curve of formed during the foaming process, how it changes
the expansion ratio vs. time. This parameter needs with time and which mechanisms are involved.
accurate measurement of the foam bitumen decay
Materials and Structures (2016) 49:2439–2454 2441

The main aim of this study is to investigate the [13]. In this study, measurement of foam bitumen
influence of water content and bitumen temperature on height over time during foam formation and decay was
foam bitumen. Foam bitumen characterizing param- improved experimentally by using ultra-sonic sensor
eters such as expansion ratio and half-life were technology (BaumerÒ standard ultra-sonic sensor). The
measured by accurately monitoring the foaming setup of the measurement is shown in Fig. 1a. The
process as a function of time. In addition, the residual repeatability of the ultra-sonic measurement technique
water content in the collapsed foam was determined. was compared with the conventional foam ruler
Moreover, the foam bitumen at the spraying nozzles measurement. Expansion ratio and half-life were
was observed for answering the question at what determined accurately by using an ultra-sonic sensor
moment foam bitumen is formed. for four different types of penetration grade bitumen as
characterized in Table 1. Foaming was conducted at
bitumen temperatures 160 and 180 °C with water
2 Experimental method contents of 1, 2, 4 and 6.6 wt% (by weight).
Foaming characterization can be affected by
Generally, expansion ratio and half-life are measured parameters such as bitumen type, grade and additive.
by placing a foam ruler next on the side of a container Special anti-foaming agents, such as silicon com-
filled with foam bitumen as shown in Fig. 1a. The half- pounds used in the refining process of bitumen may
life is determined with help of stopwatch. This affect the desired foaming characteristics [14, 15].
measurement is simple and practical. However, since Hence, gel-permeation chromatography (GPC) was
the result can be affected by the operators skill and used to assure that no polymer additives were present
experience, repeatability and accuracy are questionable in the bitumen. This method is commonly used to

Fig. 1 a Setup of foam bitumen expansion and decay measurement using ultra-sonic senor, b schematic of the high speed camera
setup, thermocouple arrangement, c setup one, d setup two
2442 Materials and Structures (2016) 49:2439–2454

Table 1 Penetration and softening point of the different types temperature at the tip of the nozzle. Spacing and order
of bitumen used for foaming of each thermocouple is depicted in Fig. 1c. In the
Bitumen type A B C D second setup, thermocouples were arranged in the
center and at the side of the vessel as presented in
Provider Nynas Grisard AG Nynas Shell Fig. 1d. The foam bitumen was produced with bitu-
Penetration (*0.1 mm) 81 51 64 51 men B (50/70 binder) at 160 °C with 2 and 4 wt% (by
Softening point (°C) 45.3 51.1 47.1 50.5 weight) water content. The vessel for capturing the
foam was at room temperature.
In addition to the thermocouples of the second setup
determine the composition of bitumen, detect possible in Fig. 1d, a Testo 885 thermal camera with image
inclusion of impurities, and separate polymer and resolution of 640 9 480 pixels and thermal sensitivity
asphalt components in polymer modified bitumen [16, \30 mK thermo was used for measuring the surface
17]. GPC was conducted using HPLC-pump Merck temperature of the foam.
655A-12 equipment, using eluent solvent the high Thermogravimetric analysis (TGA) records the
purity tetrahydrofuran. Diode array detector (DAD) weight changes in a sample with respect to temper-
was applied with a wave range of 210–290 nm, ature. Changes refer either to desorption of volatile
sampling rate 2/s and resolution 1.2 nm. components from the sample (negative weight
In order to study the state of foam bitumen (bitumen change) or to absorption of gaseous components from
A) when leaving the nozzle, a high-speed camera was the atmosphere surrounding the sample (positive
used. Two different setups were chosen for observing weight change). TGA is commonly used for analyzing
the foam bitumen at the four nozzles with 3 mm thermal degradation of cellulose, polymers and poly-
diameter openings. The first setup covered a field of mer modified bitumen, that occurs at several consec-
view (FOV) of 120.0 9 120.0 mm with a spatial utive stages [18, 19]. Research by Jenkins [3] shows
resolution of 2016 9 2016 pixels, corresponding to that at state of energy equilibrium the surface tension
*60 lm/pixel. The second setup focused on a FOV of effect in the foam bitumen can be ignored, since the
39.0 9 39.0 mm with a spatial resolution of energy loss from surface tension is an order of
2016 9 2016 pixels, corresponding to *19 lm/pixel. magnitude lower than from the pressure in the bubbles.
The bitumen temperature in both cases was 160 °C If all the foaming water is converted into vapor,
and the water content by weight of the bitumen was ideally, at least double of the actual measured
4 wt%. The pressure in the expansion chamber was set expansion ratio would occur. Therefore, less expan-
to *5 bar and the spraying rate to 100 g/s. During sion means that not all water was used or steam got lost
measurement, the images were captured at during the foaming of the bitumen [3]. In this paper
1280.41 Hz with 20 ls exposure time. The schematic TGA was applied to determine the residual water after
setup of the measurement is shown in Fig. 1b. The the decay of foam bitumen. TGA 209 F1 (NETZCH)
image plane of the high-speed camera was aligned and equipment was chosen in nitrogen atmosphere for
focused on the frontal surface of the foam bitumen heating the samples to the required temperature. The
stream. foam bitumen samples were taken with aluminum
It is well known that foam bitumen decays in a cans right after the foaming. On average, 93 ± 1.2 mg
highly dynamic and unstable process. The temperature of bitumen B (harder binder) was used for determining
of the foam can influence the viscosity of the foam and the water content. The foam bitumen was heated from
therefore the mixing and coating process. Hence, the 23 to 900 °C in three different steps: the first step
foam bitumen temperature was measured at specific consisted of a temperature increase from 23 to 110 °C
positions by using a series of thermocouples in two with 20 °C/min, the second step was a constant
different setups as shown in Fig. 1c and d. Simulta- temperature phase of 110 °C for 2 h and the third
neously the expansion and decay of the foam bitumen step was again an increase of temperature with 20 °C/
was measured with an ultra-sonic sensor. In the first min but from 100 to 900 °C. From the second step the
setup, three thermocouples were lined on the side of water released from the foam bitumen could be
the vessel that captured the foam. Two of them were measured whereas from the third step the amount of
placed on the bottom and one was used to measure the residues could be determined and as the temperature
Materials and Structures (2016) 49:2439–2454 2443

increases to 900 °C the bitumen completely decom- constant k, motion of mass x, frequency w, periodic
poses, which helps to detect presence of inclusion or force F0 and time t.
additives in the bitumen.
d2 x dx
Moreover to detect bubbles inside the decaying m þ c þ kx ¼ F0 eiwt : ð1Þ
foam, which possibly contains encapsulated water, 3D dt2 dt
X-ray computed tomography (CT) scan experiments The amplitude x0 of the oscillation can be written as
were conducted. 3D CT scanning conducted by Kutay follows
[20] with freezed foam bitumen sample using liquid
F0=k
nitrogen, it is reported that when using harder binder, x0 ¼ rffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi ð2Þ
  2  2  2
the amount of bubbles remain in the decay can reach 1  =w w þ 2nw =w0
up to 0.6 % by volume compared to 1.5 wt% (by
pffiffiffiffiffiffiffiffiffi
weight) initial water content used for foaming the where w0 ¼ k=m is the resonance frequency and the
bitumen. In this research, freezing technique was pffiffiffiffiffiffi
damping of the system reads n ¼ c= km.
attempted by using liquid nitrogen. However, during
The phase angle for the above forced damped
freezing the foam bitumen was collapsing. In addition,
oscillator equation is written as follows
cracks on the bitumen foam surface were observed 0 1
after freezing the foam bitumen. Therefore, CT 2n w=w 0
scanning was conducted without freezing the decaying / ¼ tan1 @ 2
A: ð3Þ
foam bitumen. Foam bitumen samples were taken 1  w w2
0
using 36 mm in diameter and 25 mm tall aluminum
As shown in Fig. 2a damping is inversely propor-
cans and stored at room temperature for about 4 h
tional to the slope of / (w) at resonance where
prior to X-ray CT scanning. For this experiment, a
w/w0 = 1. It follows from the frequency difference
20 keV cone beam was used, with covering a viewing
Dw between frequencies corresponding to phase angles
volume 41 9 41 9 41 mm. 1000 9 1000 9 1000
/ = p/2 ± D/. Figure 2b shows the amplitude x0 and
pixel volumes were scanned which corresponds to a
the change of phase angle /(w) as the damping factor n
spatial resolution of 41 lm.
increases from 0.1 to 2.0. The amplitude decreases with
In this study, a special high frequency torsional
increasing damping of the system.
rheometer (HFTR) shown in Sect. 3.5 was used to
monitor the viscosity of foam bitumen by applying
torsional vibrations at high frequencies. This HFTR
was already successfully used by Valtorta et al. [21] 3 Results and discussion
for measuring the change of viscoelastic properties of
asphalt plug joints on a motorway bridge. Moreover, 3.1 Expansion ratio and half-life
Dual [22] and Romoscanu et al. [23] used HFTR for
determining complex viscosity of fluids with Newto- The ultra-sonic sensor measurements were found
nian and viscoelastic properties. Valtorta and Mazza suitable for recording the history of the foam bitumen
[24] applied the HFTR for measuring the rheological during and after spraying until complete decay of the
properties of soft biological tissue. foam. The ultra-sonic sensor raw data are shown in
The measuring principle is as follows: when the Fig. 3a. They were smoothed with a moving average
fluid is brought into contact with HFTR, the oscillator filter according to in Eq. (4) by replacing each data
induces a shear flow with the fluid viscosity acting as point with the average of the neighboring data points
damping source for the oscillator. The dynamic defined within the span.
behavior of the fluid and the resonating oscillator is 1
quantified by the damping factor df and the resonant ys ðiÞ ¼ ðyði þ NÞ þ yði þ N  1Þ
2N þ 1 ð4Þ
frequency fres as explained in detail in references [22, þ    þ yði  NÞÞ
23].
The damping of the mechanical oscillator can be where ys is the smoothed data for the ith data point,
derived from Eq. 1 using a 1° of freedom damped N is the number of neighboring data points on either
oscillator with mass m, damping constant c, spring side of data point ys(i) and 2N ? 1 is the span. The
2444 Materials and Structures (2016) 49:2439–2454

Fig. 2 a Schematic of phase angle as a function of frequency, b amplitude and phase angle of a forced vibration with increasing
damping factor

(a) (b)

18 0.9
16 0.8 A
absorbition unit (AU)

0.7 B
expansion ratio (ER)

14
C
12 0.6
D
10 0.5

8 0.4
foam ruler
0.3
6 ultrasonic sensor
0.2
4
0.1
2
0
0 10 12 14 16 18 20 22 24
0 1 2 3 4 5 6 7
minutes
water content (%)
(c) (d)
Fig. 3 a Raw data of ultra-sonic sensor for 4 wt% WC c comparison of expansion ratio using foam ruler and ultra-sonic
compared to the smoothed data, b expansion and decay of foam sensor, d gel-permeation chromatogram of different types of
bitumen at different water content of bitumen B at 160 °C, bitumen
Materials and Structures (2016) 49:2439–2454 2445

span used in the analysis was 0.5 % of the total data with bitumen temperatures of 160 and 180 °C. In
points and data acquisition was made at 100 Hz for all general, the expansion ratio has increased with
measurements. increasing water content as indicated in Fig. 4a for
Measurement of the foam bitumen properties with all types of bitumen. Increasing the water content from
two ultra-sonic sensors from two different directions 1 to 2 wt% produced the highest expansion ratio
showed similar expansion and decay curves. There- increase compared to increases of water content from
fore, one ultra-sonic sensor was considered sufficient 2 to 4 wt% WC and from 4 to 6 wt%. Therefore
for measuring foam expansion height and decay over increasing the water content does not proportionally
time. Repeatability measurements with the ultra-sonic increase the expansion ratio. This can be related to the
sensors at 4 wt% water content were conducted, the increase of vapor pressure in the foam bubbles with
results from five experiments indicate that the max- increasing water content, which leads to fast coales-
imum expansion height of all repetitions was within cence of the bubbles during expansion of the foam
±0.5 cm of the average value 13.5 cm. bitumen.
Foamability of bitumen can be influenced by a Surface tension measurements by Jaroslaw and Jan,
number of factors, such as bitumen temperature, water showed that bitumen surface tension increases linearly
content, pressure under which the water and the with decreasing temperature [26]. Moreover, during
bitumen are injected in the expansion chamber and the foaming process, the temperature of the bitumen
presence of anti-foaming agent (silicon), bitumen decreases from the contact of bitumen with the
chemical composition related to origin of the binder foaming water at room temperature. Hence, the
[7, 25]. In this research, the influence of water content, surface tension can increase with the result that
bitumen temperature and bitumen type according to bubbles tend to merge quickly and create unstable
Table 1 (harder and softer binder) on the expansion foam. This can lead to less expansion of the foam
ratio and half-life was investigated. bitumen.
The expansion and decay curves depicted in Fig. 3b The results in Fig. 4b reveal that half-life is not a
for bitumen B result from the average of three tests. clear indicator for the stability of foam bitumen,
Similar foam decay curves were found for all water except for 1 wt% WC. It was observed that the soft
contents. The results of the ultra-sonic measurement binders, bitumen A and C are more stable compared to
are comparable to the foam ruler measurement as bitumen B and D at 1 wt% water content. In general,
presented in Fig. 3c. The advantage of using ultra- increasing the viscosity or using harder binder can
sonic sensor compared to foam ruler is that the increase the foam stability. Stable foam can also be
stability of the foam bitumen (half-life) can be achieved by slowing down the drainage process by
determined accurately whereas the accuracy of the increasing the bulk viscosity or by increasing the
foam ruler measurement depends on personal skill and surface elasticity of the liquid [27]. The reason for the
the precision can be questionable. For the ultra-sonic instability of the harder binder can be attributed to the
sensor measurement a minimum standard deviation of origin of binder which is related to chemical compo-
0.28 was found for the foam with a mean expansion sition, thus influencing the surface tension of bitumen.
ratio of 5.48 at 1.0 wt% water content. A maximum In order to investigate the influence of temperature
standard deviation of 0.5 was found for the foam with increase on foam bitumen, foaming experiments were
5 wt% water content and an expansion ratio of 13.79. conducted at 160 and 180 °C bitumen temperature in
The gel-permeation chromatography results in combination with different water contents as indicated
Fig. 3d shows comparable ultraviolet (UV) absorp- in Fig. 4. The resulting relative increase of expansion
tion, which is related to the molar mass of the bitumen. ratio due to a temperature increase from 160 to 180 °C
From this experiment, it is confirmed that bitumen A, for different water contents is presented in Fig. 4c. A
B, C and D are not modified by polymers. temperature increase by 20 °C improved the expan-
It was found that there was an instability problem of sion ratio of bitumen B (harder binder) by about
the foaming unit for water contents below 1 wt% and 40 ± 13 % and of bitumen A (softer binder) by
above 6.6 wt%. Expansion ratio and half-life were 17 ± 4 %. Hence, increasing the bitumen temperature
determined for the different types of bitumen shown in can significantly increase the expansion ratio of harder
Table 1, at 1, 2, 4, 6.6 wt% water content combined bitumen as compared to softer binder. This may be due
2446 Materials and Structures (2016) 49:2439–2454

60

expansion rao increase (% )


A
50
B
40
C
30

20

10

0
1 2 4 6.6
water content (%)

(a) (b) (c)


Fig. 4 Foaming parameters for different types of bitumen A, B, C, D: a expansion ratio, b half-life of different types of bitumen,
c expansion ratio increase by changing the bitumen temperature from 160 to 180 °C

to the fact that low viscosity means less resistance s) for the two phases to mix well in the expansion
against vapor pressure, leading to quick coalescence or chamber before leaving the nozzle. This raises the
disruption of bubbles particularly from softer binders. question, in which state water and bitumen are before
A similar decay mechanism has been reported in Ref. leaving the nozzle of the foam generator, specifically,
[28, 29] based on the X-ray radiograph images. On the what happens, when bitumen and water come in
other hand, in case of the hard bitumen, increasing the contact under high pressure (&5 bar) and a temper-
temperature reduces the viscosity and surface tension ature of 160 °C.
to an extent that creates favorable condition for
bubbles expansion. 3.3 Temperature measurement during foam
bitumen formation and decay
3.2 Observation of the foam bitumen stream
at the nozzle outlet with high-speed camera For thermocouple arrangement according to setup one
(Fig. 1c), the measured temperatures using thermo-
Bitumen A was used in this experiment to observe the couples for foam bitumen C at 2 wt% WC are shown
foam bitumen stream at the outlet of the foaming in Fig. 6. The maximum foam temperature profile is
nozzle. The time indicated in Fig. 5 is measured after constructed by connecting the maximum temperature
the spraying started. As shown in Fig. 5a the image envelope of each curve. The temperature measurement
taken with the first setup at 1.6 s reveals that the foam results from setup one in Fig. 6b indicate that the foam
flows in a stream when it comes out of the nozzle. temperature near to the nozzle tip is close to 150 °C
Water droplets were observed in the close-up of the for 2 wt% WC and 146 °C for 4 wt% WC. As
stream during spraying as depicted in Fig. 5b. This presented for setup two in Fig. 6c, the foam temper-
shows that the evaporation of the water droplets is not ature remains close to 100 °C for 4 wt% WC during
as fast and the foam is formed completely only the decay of the foam and above 116 °C for 2 wt%
afterwards and not as in the expansion chamber of the WC These results show clearly the influence of water
foam generator. With the second setup, shown in content on foam bitumen temperature during the
Fig. 5d, it was found that the liquid bitumen is decay. The difference in foam temperature curves of
fragmented into a number of small pieces. The the same water content in Fig. 6c can be related to
corresponding close-up in Fig. 5e reveals that the uneven distribution of water during the foaming
bitumen foam stream contains bitumen clusters when process, which leads to non-uniform temperature
the foam bitumen comes out of the nozzle. This can distribution in the foam bitumen as shown in Fig. 7.
indicate that the two phases, bitumen and water, are The thermal images for the surface temperature of
not mixed completely well in the expansion chamber. the foam bitumen during the decay after 7 and 12 s are
In addition, the spraying rate could be too high (100 g/ presented in Fig. 7. About 7 s after the start of
Materials and Structures (2016) 49:2439–2454 2447

Fig. 5 Foaming of bitumen A at the nozzle opening; first setup: c a foam stream at 2.1 s; second setup: d a close-up of the
a foam bitumen stream details at 4 wt% water content and bitumen foam stream, e observed bubble cluster, f a closer view
160 °C bitumen temperature, b a close-up of the stream at 1.6 s, of the foam stream at 2.1 s

spraying the maximum expansion of the foam is Table 2. The high amount of water (4 wt%) used for
reached and after 12 s most of the decay is over. foaming significantly reduces the minimum bitumen
Maximum peak temperature points on the thermal temperature after 7 s to 75 °C. According to Fig. 7b
images in Fig. 7b–e shows bubbles rising to the foam and d compared to Fig. 7c and e, foaming with 1 wt%
bitumen surface and exploding. This indicates that the WC produced a narrower range of surface tempera-
bubbles temperature inside the foam is close to 140 °C tures (139–100 °C) than foaming with 4 wt% WC
for 1 wt% WC and 125 °C for 4 wt% WC. The (125–75 °C). Moreover, the average temperature
average surface temperature for 1 wt% WC was found (Table 2) found from thermal images during decay
to be 126 and 121 °C at 7 and 12 s respectively as of the foam bitumen are comparable to thermocouples
shown in Table 2. The results in Table 2 are deter- temperature data shown in Fig. 6c.
mined by considering points every 0.6 mm in both The thermal images indicate that the distribution
directions (X and Y- axis) over a 60 mm by 60 mm of maximum and minimum peak temperature
surface size. In contrary to foam with 1 wt% water depends on the bubble size distribution. As demon-
content, the minimum temperature for 4 wt% strated in Ref. [28] and shown in Fig. 8f, the amount
increases with time, for instance at 12 s, as shown in of water used for foaming the bitumen influences
2448 Materials and Structures (2016) 49:2439–2454

Fig. 6 a Foam bitumen


temperature and expansion
ratio for bitumen C at
different positions 1–6
(setup one), and the
reconstructed maximum
time–temperature profile for
2 wt% water content,
reconstructed temperature
data and expansion ratio for
2 and 4 wt% water content
for bitumen C, b setup one,
c setup two

Fig. 7 a Schematic of foam bitumen decay curve, b–e surface temperature distribution for bitumen C; at t1 and t2 for 1 and 4 wt% WC

the bubble size distribution. For instance, for coarsening process. The foam bitumen bubbles are
bitumen C when foaming with 4 wt% WC, rear- larger when using 4 wt% WC compared to 1 wt%
rangement of bubbles over time occurs due to a WC as seen in the X-ray radiography measurements
Materials and Structures (2016) 49:2439–2454 2449

Table 2 Foam bitumen Water content, (wt%) 1 4


surface temperature data
found from the thermal Time, s (t1 and t2) t1 = 7 t2 = 12 t1 = 7 t2 = 12
images for bitumen C
Average temperature (°C) 126 122 108 105
Min temperature (°C) 116 102 75 90
Max temperature (°C) 139 132 125 120

presented in Fig. 8b and c. The bubbles are colored content (1 wt%), as presented in Fig. 7c and e. The
according to their size. The corresponding bubble original gray scale image is overlaid over the
area distribution for different water contents is segmented image in Fig. 8a, to show the possible
shown in Fig. 8d and e. Similarly, large areas of separation of the two phases, the liquid bitumen and
peak temperatures were found when using high the water vapor, using image analysis. More detail
water content (4 wt%) as compared to lower water information is presented in Ref. [28].

Fig. 8 a Foam bitumen


bubbles as seen from X-ray
image, b and c bubble
morphology at 7 s for 4 and
1 wt% water content
respectively, d and
e histogram for bubble area
distribution, f cumulative
area of bubbles vs. single
bubble area; all figures refer
to bitumen C
2450 Materials and Structures (2016) 49:2439–2454

3.4 Residual water in the foam bitumen decay reaches 300 °C; above this temperature the bitumen
starts to decompose according to Fig. 9b. The residual
Typical heat mass loss curves of TGA for three mass of bitumen after heating the bitumen at 900 °C is
repeated tests are depicted in Fig. 9a and b. The result close to 25 % in all cases of water content. The amount
shows that the repeatability of the TGA is good. In of water remaining in the decayed foam bitumen is
order to determine the residual water left in the about 38–48 % of the higher initial water contents of 4
decaying foam bitumen, TGA was performed for to 6 wt% (as shown in Fig. 9c and d), whereas foam
different water contents, 1, 4 and 6 wt%. Three decay in foam with less initial water content (1 wt%)
measurements were conducted for each foaming for foaming results in residual water content that is
experiment. TGA curves for the mass loss of the nearly 20 % of the initial water. As presented in Ref.
bitumen due to heating are presented in Fig. 9b. The [3]. This can be related to the latent heat energy of
results of TGA in Fig. 9a shows that the mass loss steam; theoretically, the normal expansion height
curves reach stable state within 4 h heating at 110 °C. doubles when all the foaming water evaporates.
This suggests that all the remaining water in the Hence, the whole initial water used for foaming is
bitumen has evaporated within this time period. not fully utilized for expanding the foam bitumen due
Moreover, when increasing the temperature from to loss of steam during the foaming process, as
110 to 900 °C at a rate of 20 °C/min, the change in commonly observed during the experiment. Another
bitumen mass is almost zero until the temperature reason may refer to the fact that not all the water

(a) (b)

2.5
residual weight of water

2
(%)

1.5

0.5

0
1 wt% 4 wt% 6 wt%
intial water content
(c) (d)
Fig. 9 a Heat mass loss curve as a function of time, b heat mass foam bitumen, d weight of water remained in the foam bitumen
loss and the rate of mass loss as a function temperature, decay for different initial water content (1, 4 and 6 wt%); all
c average value of TGA curve during water dissipation from the figures refer to bitumen C
Materials and Structures (2016) 49:2439–2454 2451

evaporates with small water droplets remaining in the the bottom of the foam capturing vessel, near to the
foam bitumen [3, 20]. This implies that the temper- sensor location of the HFTR. Then the HFTR is heated
ature of foam bitumen is not sufficient to evaporate all in an oven to the expected foam bitumen temperature at
the water used for foaming. As shown in Figs. 6 and 7, that location. Warming up the HFTR helps to reduce the
the temperature of the foam bitumen was higher when cooling effect in the foam bitumen when measuring the
using 1 wt% WC compared to the 4 wt% WC. This damping factor. The damping factor is measured by
indicates more energy is available to evaporate the placing the HFTR inside the foam bitumen close to the
water when using lower water content in the foam bottom of foam capturing vessel as shown in Fig. 11.
bitumen. Finally, the viscosity is calculated using the calibration
Moreover the X-ray CT scan image shown in curve shown in Fig. 12a. In order to observe closely the
Fig. 10 demonstrates the remaining bubbles trapped in foam bitumen bubbles surrounding the HFTR, X-ray
the foam bitumen after decay of 4 h. The initial water radiography was conducted during the foaming process
content used for foaming was 6 wt% and the bitumen in case of a foaming experiment with 4 % WC. The
temperature was 160 °C. Polydisperse bubbles were results are presented in Fig. 11.
observed in the decayed foam bitumen as shown in The calibration curve for calculating the viscosity
Fig. 10b. The histogram of bubble volume in Fig. 10c was determined from the average HFTR damping
indicates that the majority of the bubbles has a volume factors of fluids shown in Table 3. Three tests were
\0.5 mm3. The diameter of the trapped bubbles was conducted for each fluid. Then, the dynamic viscosi-
found to be 0.19–2.2 mm. The ratio of trapped bubbles ties of the fluids were measured three times using
to the total volume of the foam bitumen decay is Physica MCR 301 DSR (Anton Paar GmbH., Austria)
1.5 %. However, the TGA results for foaming the with 25 mm diameter parallel plates and a 1 mm gap.
bitumen at 6 wt% WC indicate that the percentage of The average dynamic viscosity results are shown in
residual water inside the trapped bubbles is higher as Table 3. The calibration curve fits well (R2 = 0.99) to
compared to the results from the CT scan. This a power function (Eq. 5) as presented in Fig. 12a. The
indicates that additional micro bubbles could be coefficients of Eq. 5 are, a = 500, b = 0.1191 and
trapped in the bitumen which could not be detected c = -599.9. Therefore, this equation was used to
with the X-ray CT scan since the resolution is limited calculate the viscosity from the measured foam
to 41 lm. bitumen damping factors.
g ¼ a nb þ c: ð5Þ
3.5 High frequency torsional rheometer
Three bitumen foaming tests were conducted as
The viscosity of the foam bitumen in this study is presented in Fig. 12b for estimating the repeatability
obtained as follows: First, the temperature of the foam of the damping factor measurements with HFTR.
bitumen is measured by placing a thermocouple close to Foaming of bitumen was conducted with bitumen E

50
total bubble volume (mmm )
3

45
40
35
30
25
20
15
10
5
0
0 1 2 3 4 5
single bubble volume (mm 3)

(a) (b) (c)


Fig. 10 a Bubbles as seen from the X-ray CT scan, b closer view of trapped bubbles in the foam bitumen decay, c foam bitumen bubble
volume distribution at 6 wt% WC; all figures refer to bitumen C
2452 Materials and Structures (2016) 49:2439–2454

Fig. 11 a X- ray radiography images of foam bitumen during HFTR measurement, b a close-up of the HFTR, c schematic of HFTR

Fig. 12 (a) calibration curve for viscosity, relationship between viscosity and damping factor (b) damping factor as a function of time
for bitumen E (c) viscosity of foam bitumen with time

which has a penetration of 168 (0.1 mm) and a was also measured with a thermocouple. The results
softening point of 40.9 °C. While measuring the are shown in Fig. 12b. The viscosity of foam bitumen
damping factor, the temperature of the foam bitumen B and E using the calibration curve according to Eq. 5
Materials and Structures (2016) 49:2439–2454 2453

Table 3 Measured average damping factor, resonance frequency and dynamic viscosity of fluids
Fluids Glycerol Polyethylene glycol Water

Damping factor 8.18 ± 0.08 5.92 ± 0.01 2.65 ± 0.03


Resonance frequency 6123.58 ± 0.01 6128.27 ± 0.07 6130.74 ± 0.05
Dynamic viscosity (mPa s) 81.1 60.0 1.00

is depicted in Fig. 12c. The foam formed from harder which resembled rather a liquid state than foam
bitumen B is more viscous compared to the softer and water droplets. This indicates that the mixing
bitumen E. In both cases, the viscosity increases and expansion of the bubbles in the expansion
during the foam bitumen decay over time. For certain chamber is not as fast as the spraying rate and the
mean bubble size dry foams are harder than wet ones foam is formed afterwards and not as assumed in
[27]. This means the gas volume fraction increases the expansion chamber of the foam generator.
with increasing shear modulus and, therefore, with 4. The temperature distribution on the surface of the
increasing viscosity [30, 31]. Hence, for decaying foam bitumen is non uniform, and the minimum to
foam bitumen the number of bubbles decreases with maximum temperature range is significant when
decreasing gas volume fraction. However, the tem- using high amount of water content (4 wt%).
perature of the foam bitumen drops quickly as shown Hence, the excess water for foaming can act as a
in Fig. 12b resulting in a viscosity increase. trigger for reducing the foam temperature locally
when in contact with bitumen during the foaming
process. In addition, the surface temperature of the
foam bitumen depends on the bubble size distri-
4 Summary and conclusions
bution. Thermal imaging revealed larger temper-
ature surface peaks with 4 wt% water content than
1. Characterization of foam bitumen nowadays with lower water content (1 wt%).
mainly consists in a visual estimation of foam 5. If water accumulates in the warm region of the
expansion by measuring the expansion height of foam bitumen (i.e. temperature \ 100 °C), then
the foam in an open container with a ruler. This residual water can accumulate in the foam bitumen.
kind of bitumen foam characterization was exper- Similarly, the thermogravimetric results confirmed
imentally improved using an ultra-sonic sensor that high residual water content (38–48 wt% of the
and applying moving average filtering for accu- initial water used for foaming) is found when using
rate monitoring of expansion and decay of the more than 1 wt% water for foaming. Therefore the
foam bitumen as a function of time. The ultra- amount of water used for foaming has an influence
sonic sensor measurement used for determining on the foam bitumen temperature and can influence
the foam bitumen expansion height is repeatable. the amount of residual water in the foam decay.
This technique also helps to obtain the half-life of This implies that the reason for improved com-
the foam bitumen in an accurate way. paction of foam asphalt mixture as the water
2. Foaming softer binder results in higher expansion content increases depends on the residual water, as
ratio compared to harder binder. The half-life does the water content increases ([1 %) the compaction
not give a clear indication about the stability of the improves. Whereas the mix performance decreases
foam, for initial water contents in the foam higher as the foaming water content increases [32].
than 1 %. 6. The HFTR is useful to measure the viscosity of the
3. From the high speed camera image, it was foam bitumen starting from spraying until the
discovered that, at the outlet of the nozzle bitumen foam decays completely. The viscosity of the
foam has not yet been completely formed. This foam bitumen increases as the foam bitumen
can lead to ‘‘delayed foaming’’ which depends on decay with time since the temperature of the foam
the origin of binder [3]. The ‘‘foam bitumen’’ decreases rapidly. This suggests that the mixing
stream showed fragmented pieces of irregular size need to start during the spraying of foam bitumen,
2454 Materials and Structures (2016) 49:2439–2454

before the foam viscosity start to increase during 14. Ramanujam JM, Jones D (2007) Characterization of foamed-
the foam decay. bitumen stabilisation. Int J Pavement Eng 8:111–122
15. Saleh MF (2006) Effect of aggregate gradation, mineral
fillers, bitumen grade, and source on mechanical properties
Acknowledgments The authors acknowledge the support of of foamed bitumen-stabilized mixes. Transp Res Record
Anton Demarmels, Ammann Construction Equipment 1952:90–100
(Ammann Schweiz AG, CH-4901 Langenthal, Switzerland). 16. Baumgardner GL, Masson J-F, Hardee JR, Menapace AM,
Jae Bong Lee and Peter Moonen from Building Science and Williams AG (2005) Polyphosphoric acid modified asphalt:
Technology laboratory EMPA. Group members of the Road proposed mechanisms. Presented at the Association of
Engineering/Sealing Components lab, EMPA (Federal Asphalt Paving Technologists, Hyatt Regency, Long Beach,
Laboratories for Material Science and Technology, California
Switzerland). Finally the Commission for Technology and 17. Negulescu I, Mohammad L, Daly W, Abadie C, Cueto R,
Innovation CTI, Switzerland and Ammann Schweiz AG, Daranga C, Glover I (2006) Chemical and rheological
Switzerland are greatly appreciated for financing the project. characterization of wet and dry aging of SBS copolymer
modified asphalt cements: laboratory and field evaluation.
Presented at the Journal of the Association of Asphalt
Paving Technologists from the Proceedings of the Technical
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