Construction and Building Materials 250 (2020) 118808

Contents lists available at ScienceDirect

Construction and Building Materials

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

The mechanical evaluation of cold asphalt emulsion mixtures using a

new cementitious material comprising ground-granulated blast-furnace
slag and a calcium carbide residue
Anmar Dulaimi a,b,c,⇑, Hayder Kamil Shanbara d, Ali Al-Rifaie d
a
College of Engineering, University of Warith Al-Anbiyaa, Karbala, Iraq
b
Ministry of Education, Karbala, Iraq
c
Department of Civil Engineering, Liverpool John Moores University, Liverpool, UK
d
Department of Civil Engineering, College of Engineering, Al-Muthanna University, Samawah, Iraq

h i g h l i g h t s

 CCR and GGBS were used as filler materials in cold asphalt emulsion mixtures (CAEMs).
 CCR improved the indirect stiffness modulus of the CAEMs.
 The impact of CCR-activated-GGBS on the performance of the CAEM’s was examined.
 The microstructures of the BBF paste specimens were observed.
 Fatigue life and permanent deformation were investigated.

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

Article history: Cold asphalt emulsion mixtures (CAEMs) can be said to produce a reduced environmental impact and
Received 17 October 2019 lower energy consumption in comparison to hot mix asphalt (HMA). They are also safer to use as there
Received in revised form 31 January 2020 is no heating involved in the production and application of such mixtures. However, CAEMs are described
Accepted 20 March 2020
as inferior to traditional HMA because of weak early strength and the length of curing time required to
reach their full strength. As such, this piece of research aimed to develop new, CAEMs, a binary blended
filler (BBF), made from ground-granulated blast-furnace slag (GGBS) and calcium carbide residue (CCR),
Keywords:
as an alternative to traditional limestone filler (LF) in such mixtures. The new BBF mixture was compared
Cold asphalt emulsion mixture
Calcium carbide residue
to a mixture containing LF and with a control HMA. A significant improvement was reported in indirect
Close graded surface course mixture tensile stiffness modulus (ITSM) when using CCR as the activator of GGBS. Early strength in terms of
Indirect tensile stiffness modulus ITSM, was improved due to the activation of GGBS by the CCR. Scanning electron microscopy (SEM) anal-
Microstructure ysis revealed that when added to GGBS, the CCR lead to considerable changes in the microstructure of
components of the mix during the curing period. This confirmed the generation of the cementitious prod-
ucts ettringite, Portlandite and C-S-H gel. It is anticipated that the requirement for uninterrupted curing
in the case of conventional CAEMs, will be eliminated through use of this new BBF mixture.
Ó 2020 Elsevier Ltd. All rights reserved.

1. Introduction tures. Health and safety issues are generated as a result of the high
temperatures, fumes and dust produced during HMA manufacture.
The relatively high working temperature of hot mix asphalt Consequently, such issues are considered as additional negative
(HMA), leads to the consumption of large quantities of fuel neces- aspects of the use of HMA. As such, the motivations to finding sub-
sary to heat the bitumen and aggregates to manufacture such mix- stitutes to HMA are to reduce construction costs and emissions of
carbon associated with its’ production.
Using cold mix asphalts (CMA) produce several advantages over
⇑ Corresponding author at: College of Engineering, University of Warith Al- the use of HMA. Triggered by economic benefits, CMA is currently
Anbiyaa, Karbala, Iraq.
considered to have a positive impact on the environment [1,2]. Road
E-mail addresses: A.F.Dulaimi@ljmu.ac.uk, a.f.dulaimi@uowa.edu.iq, anmarfale-
h@yahoo.com (A. Dulaimi), hayder.shanbara@mu.edu.iq (H.K. Shanbara), ali.alri-
pavement construction using CMA has subsequently acquired
faie@mu.edu.iq (A. Al-Rifaie). increasing attention around the world. In 2008, Turkey produced

https://doi.org/10.1016/j.conbuildmat.2020.118808
0950-0618/Ó 2020 Elsevier Ltd. All rights reserved.
2 A. Dulaimi et al. / Construction and Building Materials 250 (2020) 118808

approximately 3.5 million tonnes of CMA, while France manufac- Peethamparan [25]. The CKD-GGBS blend offered a substantial
tured around 2 million tonnes [3,4]. However, the use of CMA in compressive strength after 2 days curing at high temperature,
the UK is still limited to base and subbase courses of structural layers with a water-to-binder ratio of 0.40. CKD was found to be an out-
[5–7]. standing activator for pozzolanic materials as it has a high alkali
Cold asphalt emulsion mixtures (CAEMs) contain bitumen and sulfate content [26].
emulsion as a binder and can be considered the most common type Calcium carbide residue (CCR) is a waste material generated
of CMA. CAEMs offer many advantages which are very attractive from the production of acetylene gas (C2H2) through the hydrolysis
concerning the environment, the economy and safety, but these of calcium carbide (CaC2). However, due to the high alkalinity of
mixtures suffer from deficits in important mechanical properties, carbide lime, different environmental problems are created when
making them inferior to HMA. In consequence, its use has been it is disposed of in landfill. Because it is a high alkaline material,
restricted to footways reinstatement work and low/medium traf- this makes it appropriate for the activation of GGBS by enhancing
ficked roads [8–12]. early age reactivity in similar way to CKD [27,28]. CCR could there-
To address this, hydraulic binders have been widely utilized to fore provide the environment needed to activate latent hydraulic
produce CAEMs with an acceptable performance, this normally materials like GGBS. There is no shortage of CCR as for example,
involving the use of Ordinary Portland Cement (OPC). The incorpo- in 2014, roughly 1,423,000 tonnes of waste CCR was produced
ration of cement into CAEMs is one of the most important tech- worldwide, this generated from the manufacture of about half mil-
niques to reduce the disadvantages associated with CAEMs in lion tonnes of acetylene gas. The amount of CCR produced is esti-
terms of its mechanical properties [13]. Emulsified asphalt, Port- mated to increase by 3% in 2020 [29].
land Cement and graded aggregates, produce cement emulsified A limited number of studies have been performed to examine
asphalt concrete, a composite material [14]. Fang et al. [15] carried the use of waste and by-products to improve the performance of
out a study to accelerate improvements in the mechanical proper- CAEMs. The shortcomings of CAEMs and the advantages of includ-
ties of cement bitumen emulsion asphalt (CBEA) by incorporating ing two waste materials, namely CCR and GGBS, of specific interest.
rapid-hardening cement as a filler replacement in 3 percentages: This study is an approach to enhance CAEMs under normal curing
0%, 3% and 6%, by weight of dry aggregate. Their findings showed so that they have similar properties to those of traditional HMA.
that the two types of bitumen emulsions used, cationic and anio- This is in direct contrast to previous research which seeks to
nic, could influence the rate of early hydration of the cement. How- improve CAEMs by using cement. In the current research, the sub-
ever, after a few days, the bitumen emulsions were found to have stitution of limestone filler by GGBS and CCR, has improved the
no substantial effect on the overall degree of hydration. performance of CAEMs by the generation of cementitious hydrated
The increasing accumulation of industrial by-products and solid products via the use of activating materials. This offers a positive
waste is creating an alarming level of severe environmental and impact on sustainability by decreasing waste materials.
economic issues around the world. Because of this, the develop- Both SEM and XRD, advanced techniques for the assessment of
ment of the properties of CAEMs through the use of various by- microstructures, are used to understand the internal structure and
product and waste materials i.e. fly ash [16–18], construction and microstructure of the CAEMs. The materials used for the manufac-
demolition waste material and recycled asphalt pavement, has ture of the CAEMs were granite aggregate, cationic bitumen emul-
been gaining in popularity. Ellis et al. [19] found that adding sion, water and two supplementary cementitious materials,
ground granulated blast furnace slag (GGBS) to bitumen emulsion namely GGBS and CCR, these used as a replacement for limestone
mixtures, led to improved long-term, mechanical performance in filler.
comparison to reference mixtures. The substitution of the mineral
filler with fly ash (FA) was the reason for this enhancement.
2. Materials and method
Modarres and Ayar [20] performed research using coal ash on cold
recycled asphalt material. While a positive impact on resistance to
2.1. Aggregate
water damage could not be achieved, its mechanical properties
were improved. A binary blended filler material developed by
The properties of the crushed granite aggregates used in both
Dulaimi et al. [21], using a fluid catalytic cracking catalyst and high
the CAEMs and HMA, are shown in Table 1. A close-graded, surface
calcium fly ash, improved the microstructural integrity in a new,
coarse gradation of 14 mm, complying with BS EN specifications,
fast-curing CMA. Recently, GGBS, activated by hydrated lime, was
was selected in accordance with BS EN 933-1 [30], as shown in
used in an asphalt emulsion mixture (AEM) by Du [22] as a
Fig. 1. This aggregate is considered durable, has a suitable shape,
replacement for conventional limestone filler, the findings showing
is hard and clean, resists permanent deformation and produces
that AEM with GGBS and hydrated lime can be used a substitute of
an acceptable level of skid resistance. It is the most conventional
OPC for pavement base courses.
aggregate used in the manufacture of bituminous mixtures [31].
Bijen [23] found that GGBS which is rich in lime content, is a
latent hydraulic cement which only requires to be activated. GGBS
is a by-product of iron and steel-making, obtained from a blast fur- 2.2. Bitumen emulsion and asphalt
nace in water or steam, to produce a glassy, granular product that
is then ground into a fine powder after drying. As the initial hydra- To achieve the most effective bond between the aggregate par-
tion of GGBS is much slower in comparison to Portland cement, ticles, cationic, slow-setting bitumen emulsion (C50B4) was
activators such as alkalis, Portland cement, or lime are used to Table 1
speed up said reaction [24]. GGBS requires an activator when it Physical characteristics of the granite aggregate.
is used as a sole binder in concrete in order to improve its reactiv-
Material Property Result
ity by attacking the glassy structure [25].
The use of GGBS as a supplementary cementitious material can Coarse aggregate Bulk particle density, Mg/m3 2.60
Apparent particle density, Mg/m3 2.65
only occur in a high alkaline environment, this environment the Water absorption, % 0.7
result of cement hydration. This will dissolve the glassy structure Fine aggregate Bulk particle density, Mg/m3 2.53
of the coating, exposing the anhydrous surface for additional Apparent particle density, Mg/m3 2.64
hydration. A non-conventional binding material comprising GGBS Water absorption, % 1.5
Limestone filler Particle density, Mg/m3 2.56
and cement kiln dust (CKD), was studied by Chaunsali and
 A. Dulaimi et al. / Construction and Building Materials 250 (2020) 118808 3

Fig. 1. Gradation of the AC 14 mm close graded surface course.

selected as the binder for all the CAEMs [10,32]. This bitumen Table 3
emulsion consists of 50% base bitumen with a penetration grade Properties of 40/60 and 100/150 penetration grade biyumens.
of 40/60. It was provided by Jobling Purser, Newcastle, UK, and Bituminous binder 40/60 Bituminous binder 100/150
called Cold Asphalt Binder (CAB50). The reason for selecting this Property Value Property Value
emulsion was because of its high stability and adhesion. Its prop-
Appearance Black Appearance Black
erties are shown in Table 2.
Penetration at 25 °C, 0.1 mm 49 Penetration at 25 °C, 0.1 mm 142
For comparison purposes, two HMA have been included in this Softening point, °C 51.5 Softening point, °C 43.5
research. These mixtures comprise the same type and gradation of Density, g/cm3 1.02 Density, g/cm3 1.04
aggregate as used in the CAEMs. Two standard bitumen grades, soft
grade penetration (100/150) and hard grade penetration (40/60),
supplied by NYNAS, were used to manufacture the HMA. Table 3 magnesium and sodium in its structure, as shown in Table 4. These
details the characteristics of the binders. results are consistent with the chemical compositions analysed by
Chaunsali and Peethamparan [25]. While the main oxides in CCR
2.3. Selected fillers are lime and silica, these results are consistent with those of Han-
jitsuwan et al. [33]. CCR comprises a substantial quantity of cal-
In this research, three filler materials were used: conventional cium oxide making it attractive for use as a promoter like OPC
limestone filler (LF) supplied by Francis Flower, UK as BS EN [28]. This chemical composition of CCR makes it a potential mate-
13,043 grade; ground granulated blast furnace slag (GGBS) pro- rial for the activation of GGBS. The chemical composition of the LF
vided by Hanson, UK, this used as a replacement to the LF, and cal- indicates it was mainly composed of CaO and SiO2. Although LF has
cium carbide residue (CCR), applied as an activator in different a high content of CaO (77.82%), it is considered an inert material
percentages (obtained from BOC, UK & Ireland). The CCR was in meaning that no hydration happens when in contact with water
the form of large, wet blocks which had to be broken into small as CaO exists in a non-hydrated state.
pieces and oven dried at 110 °C for 1 day. The resultant lumps were A Rigaku Miniflex diffractometer was used to examine the X-ray
then ground using a mechanical grinder under low-energy, inten- diffraction (XRD) and thus the mineralogy of the fillers. Fig. 2 dis-
sive, dry agitation, applying a pestle and mortar for a short period plays the diffraction patterns of the GGBS, CCR and LF. GGBS has an
of time (15 min) to prevent particle agglomeration which is harm- amorphous nature with a halo between the 25° and 35° (2h°)
ful to the quality of the ground CCR. range, while the CCR contains Portlandite and calcite as its main
Chemical analysis of the GGBS via X-ray fluorescence technique components, but with no indication of the existence of amorphous
(XRF) using a Shimadzu EDX 720, energy dispersive, X-ray fluores-
cence spectrometer, indicated the presence of lime, alumina, silica,
Table 4
Comparative chemical properties of the fillers.
Table 2
Properties of bitumen emulsion. Chemical composition GGBS CCR LF
CaO, % 40.35 81.84 77.82
Description (C50B4) bitumen emulsion
SiO2, % 37.23 14.08 17.21
Type Cationic Al2O3, % 5.73 0.90 0.00
Appearance Black to dark brown liquid MgO, % 4.22 0.77 0.89
Base bitumen, 1/10 mm 40–60 Fe2O3, % 0.01 0.00 0.00
Bitumen content, % 50 SO3, % 0.00 0.77 0.01
Particle surface electric charge Positive K2O, % 0.00 0.20 0.35
Viscosity – Efflux time 4 mm at at 50 °C, sec 15–70 TiO2, % 0.63 0.12 0.19
Boiling Point, °C 100 Na2O, % 0.00 1.32 2.27
4 A. Dulaimi et al. / Construction and Building Materials 250 (2020) 118808

phases. The presence of these alkalis in the CCR will accelerate the 2.4. Manufacturing of samples
reactivity of the GGBS. The powder XRD pattern of the LF, is com-
posed of calcite and quartz. The CAEMs samples have been created according to the Mar-
Scanning electron microscopy (SEM) images of all the fillers, shall Method for Emulsified Asphalt Aggregate Cold Mixture
taken by a Quanta 200, are shown in Fig. 3. The samples were Design (MS-14) [34], a method adopted by the Asphalt Institute.
coated with a thin layer of gold to increase conductivity, using an Pre-wetting of the aggregate is essential, the optimum proportion
auto fine sputter coater. It can be seen that the GGBS particles of pre-wetting water consistent with a satisfactory coating. This
are comprised mainly of particles that are irregularly shaped, while pre-wetting water is essential for the lubrication of the aggregates
CCR particles are agglomerated, this in common with the research and the activation of the surface charges on aggregate particles
published by Hanjitsuwan et al. [28]. All the LF particles are irreg- prior to adding bitumen emulsion [35]. The optimum emulsion
ular in shape with a rough texture and sharp angles. content has been found using indirect tensile stiffness modulus
The particle size distribution (PSD) of the GGBS powder reveals (ITSM) tests, the optimum total liquid content at compaction iden-
that around 90% of the particles are smaller than 40 lm, while the tified using the mix density test. From these results, it was found
dominant particle size of the CCR almost falls below 25 lm. The that the optimum bitumen emulsion content was 12.5%, the pre-
fineness of the CCR particles plays an important role regarding wetting water content 3%. Mixing was carried out using a Hobart
hydration rates when exposed to water. The average grain size mixer. All the mixture components, aggregate, fillers and pre-
(D50) of the CCR ground for 15 min, was approximately 24.6 lm. wetting water, were added and mixed at a minimal speed for
The PSD of the limestone powder was examined, 90% of the parti- one minute. Through the next half minute of mixing and at a con-
cles passing through a sieve size 80 lm, as shown in Fig. 4. stant rate, the bitumen emulsion was introduced. Mixing contin-
The pH of the aqueous GGBS solution was found to be 11.6, ued for another 2 min at the same speed. Thereafter, the
while the CCR was 13.1, this helping to accelerate the mixtures were poured into steel moulds and quickly compacted
breaking of the bitumen emulsion in the CAEMs. The pH for the using a Marshall hammer to apply 50 blows on each surface of
LF was 9.39. the samples. Finally, all samples were left inside their moulds for

Fig. 2. Powder XRD pattern of (a) GGBS, (b) CCR and (c) LF.
 A. Dulaimi et al. / Construction and Building Materials 250 (2020) 118808 5

Fig. 3. SEM images of the fillers.

Fig. 4. Particle size distribution of the fillers.

24 h before de-moulding, a hydraulic de-moulding jack used to mixture with a soft bitumen 100/150 pen. The second is a harden
extrude them. bitumen 40/60 pen, used throughout the experimental work, with
The results of the CAEMs have been compared with two types of the same type and gradation of aggregate according to the stan-
HMA, the first a standard AC 14 mm close-graded, surface course dard PD 6691:2010 [36] and with 5.1% optimum binder content
6 A. Dulaimi et al. / Construction and Building Materials 250 (2020) 118808

by aggregate weight. The mixing temperatures for the 100/150 and

40/60 AC 14 surface courses were 150 to 160 °C and 160 to 170 °C,
respectively. The compaction method and the number of blows
applied to the HMA were the same as for the CAEMs. Table 5 shows
the proportions of all mixtures by percentage of Marshall samples.

2.5. Laboratory testing programme

2.5.1. ITSM test

The ability of different pavement layers to distribute traffic
loads to the layers beneath, was tested using the ITSM test, this
used by many researchers [12,37–39]. All CAEMs samples were
mixed and prepared at room temperature, a minimum of five dif-
ferent specimens of each mix prepared. The CAEMs specimens
were kept in their steel moulds in the lab at ambient temperature
(20 ± 1 °C). Following this, all the samples were kept at the same
temperature for the recommended curing period and tested at 3,
7, 14, 28 and 56 days. Room temperature was adopted as the nor-
mal curing temperature for all the prepared mixtures when testing
for ITSM. This regime was followed in order to mimic the manufac-
ture, laying and compaction of CAEMs on site, and also to prevent
early bitumen ageing [40,41]. Testing was performed at 20⁰C fol- Fig. 5. ITSM apparatus.
lowing BS EN 12697-26 [42] guidelines, using a Cooper Research
Technology HYD 25 testing machine (Fig. 5). A transient peak hor-
izontal deformation of 5 mm was achieved by applying an impul- 21 days by which point a constant mass was reached. It was
sive stress for 124 ± 4 ms as a rise time. Five test pulses were reported by Thanaya [10] that samples could achieve their con-
applied to the samples after ten conditioning pulses. The average stant mass by placing them into an oven at 40 °C for 2 weeks cur-
stiffness values of two different measurements on the diameters ing. However, curing at ambient temperature was adopted
of each cylindrical specimen were calculated. meaning that ageing of the bitumen will be avoided [48,49]. The
GGBS replaced the conventional mineral limestone filler at 6% slab samples were then subjected to a wheel track test where a sin-
by total weight of the dry aggregate. CCR was used as an activator gle wheel was applied to the surface of the slab as shown in Fig. 6.
by replacing 1%, 2%, 3%, 4%, 5% and 6% of GGBS by dry aggregate Table 6 outlines the test conditions.
weight, to generate a binary blended cementitious filler made from
GGBS and CCR.
2.5.3. Fatigue test
An asphalt beam fatigue test was performed using a four-point
2.5.2. Wheel-tracking test beam-bending schematic. This method evaluates the behaviour of
Rutting is one of the most significant and widespread failure bituminous mixtures under fatigue loading, in accordance with BS
modes in flexible pavements, particularly in areas suffering from EN 12697-24 [50]. Dulaimi et al. [21] and Al-Hdabi et al. [51] used
seasonal elevated temperatures [43]. Permanent deformations of the same four-point beam-bending test to evaluate the fatigue
all mixtures were performed at 60 °C following BS EN 12697-22 resistance of CAEMs. A strain control mode was used in this test,
[44], using a wheel track machine type HYCZ-5. The same wheel by which prismatic beams were subject to strain levels of 150 le
track test as adopted by numerous researchers, was adopted to and 200 le. Sinusoidal repeated loading waves at a frequency of
appraise the resistance to permanent deformation of the CAEMs 10 Hz, were applied at a controlled room temperature of
[17,31,35,45,46]. The test was performed to simulate, as much as 20 ± 1 °C. Fatigue life was observed during the test period and
possible, field conditions to find the failure mechanisms of the
CAEMs under controlled conditions.
Prior to testing, the loose mixtures were compacted in a steel
mould, under a roller compactor, in accordance to the standard
procedure in BS EN 12697-33 [47], resulting in slabs measuring
400  305  50 mm. These slabs were kept in their moulds for
1 day at a lab temperature of 20 °C. Following this, they were cured
for another 1 day at 40 °C then left to cure at lab temperatures for

Table 5
Specifics of mix proportions.

Mixture types Filler types Bitumen emulsion, %

LF mix 6% LF 12.5%
G6 mix 6% GGBS 12.5%
G5C1 mix 5% GGBS + 1% CCR 12.5%
G4C2 mix 4% GGBS + 2% CCR 12.5%
G3C3 mix 3% GGBS + 3% CCR 12.5%
G2C4 mix 2% GGBS + 4% CCR 12.5%
G1C5 mix 1% GGBS + 5% CCR 12.5%
C5 mix 6% CCR 12.5%
HMA 40/60 6% LF 5.1% bitumen 40/60
HMA 100/150 6% LF 5.1% bitumen 100/150
Fig. 6. Wheel-tracking test equipment.
 A. Dulaimi et al. / Construction and Building Materials 250 (2020) 118808 7

Table 6 the specimens were dried in a vacuum pump to remove any evap-
Wheel track test conditions. orable moisture. They were then mounted onto aluminum stubs
Item Range using double-sided, adhesive carbon disks, an auto-fine sputter
Tire of outside diameter, mm 200–205 coater used to coat the fracture surface specimens with gold. The
Tire width, mm 50 ± 5 paste specimens were used to identify differences in the
Trolley travel distance, mm 230 ± 10 microstructure of the materials at various curing ages.
Trolley travel speed, time/min 42 ± 1
Contact pressure, MPa 0.7 ± 0.05
Poisson’s ratio 0.35 3. Results and discussion
No. of conditioning cycles 5
No. of test cycles 10,000
Test temperature, °C 60
3.1. ITSM development
Compaction Roller compactor
Specimen temperature conditioning 12 hours before testing Fig. 8 details the average ITSM for five samples of each of the
CAEMs, at 3 days normal curing. The mixes were prepared with
LF and with GGBS and CCR in different percentages. It can be seen
determined in terms of number of load applications (N cycle), that both the control LF mixture and the GGBS mixture, display low
when the stiffness modulus of the specimens had decreased to strength during their early life, the performance in terms of ITSM
50% of their initial rate, measured in the first 100th load applica- poor compared to both traditional hot asphalt mixtures.
tion. The total length, width and height of the prismatic specimens The second step in the development of the new CAEMs in this
were 400 mm, 50 mm and 50 mm, respectively. Three duplicated study was to substitute the GGBS with different contents of CCR;
beam specimens were examined for each mixture, the average 0, 1, 2, 3, 4, 5 and 6% of the total weight of the dry aggregate. A sig-
value determined. nificant improvement was achieved by adding CCR in that 4% GGBS
and 2% CCR (G4C2 mixture), gave the optimum ITSM. As such, this
2.5.4. Water sensitivity test new binary blended filler (BBF), has been produced as it has
Asphalt mixtures become sensitive in the presence of water, cementitious properties. A maximum ITSM of 1678 MPa, this 9
this playing a major role in flexible pavement failure. Water in times more than the ITSM of the LF mixture, was achieved by the
asphalt pavements means that the bitumen will not adhere to BBF at three days normal curing.
the aggregate, this causing damage to flexible pavements, com- Fig. 9 shows that the ITSM increased significantly for the BBF
monly known as stripping. In this study, the water sensitivity of mixture across all curing times, the LF mixture having an inferior
the bituminous mixtures was assessed following the British Stan- ITSM in comparison to the other mixtures. The GGBS mixture alone
dard EN 12697-12 [52]. Using this method, the effects of water sat- (without CCR), produced a slight improvement in ITSM but the cur-
uration of the bituminous mixtures on variations in tensile rent research shows that using CCR as an activator can contribute
strength of said mixtures were examined. Two groups of cylindri- to improvements in the hydration process, leading to substantial
cal test specimens were prepared and conditioned. Group one (dry) enhancement in ITSM values.
was left dry at lab temperature, while group two (wet) was soaked From Fig. 10, it can be seen that the ITSM of the G4C2 mixture
and placed in water at an elevated conditioning temperature of exceeded that of HMA 100/150 within 3 days normal curing, mean-
40 °C. ing that using 4% GGBS and 2% CCR as a filler reduces the curing
At the end of the preparation and compaction stages, the dry period on site, this in turn, leading to more acceptance of the use
specimens were placed on a flat surface at lab temperature for of CAEM’s in pavement construction. As a point of comparison,
7 days. The wet group specimens were put into a water bath at the LF mixture failed to reach this ITSM value throughout the cur-
20 °C for 4 days, the water level 25 mm above the top surface of ing period.
the specimens. They were placed inside a vacuum container filled As stated above, the mixture containing 4% GGBS and 2% CCR
with potable water up to 25 mm above the top of the specimens, at (G4C2), had a better ITSM value in comparison to HMA 100/150
lab temperature, for 10 min at a pressure of 6.7 kPa. They were at 3 days of age. This significant improvement in ITSM was
kept submerged in the water for an extra 30 min after gradually achieved by the generation of hydration products, this attributed
letting atmospheric pressure into the vacuum container. The spec- to the role of CCR which provides the environment required to acti-
imens were then transferred to the water bath for 72 h at 40 °C. vate the latent hydraulic material – GGBS. An adequate early con-
After the conditioning processes, the ITSM of each of the two centration of alkali has a significant effect on GGBS activation and
groups was determined. The indirect tensile stiffness ratio (ITSR) initial hydration. The addition of CCR works as this activator, the
was calculated and stated as a percentage of the ITSM of the wet
group compared to that of the dry group. The ITSR of asphalt mix-
tures indicates their water damage resistance and measures how
sensitive such mixtures are to water. A higher ITSR value indicates
a better resistance to moisture because there is no reduction in
strength due to the impact of water saturation.

2.6. Microstructure examination

Scanning electron microscopy (SEM) is a high-resolution, imag-

ing method. Through this technique, the morphology of an object
can be examined as well as its internal microstructure. The
microstructure of the BBF fractured surface paste specimens
(Fig. 7), was observed using an electron beam from a scanning elec-
tron microscope type ‘Inspect S’, with an accelerating voltage
10 kV. Fragments (specimens) at ages 3 and 28 days were taken
from the center of the paste samples. Before the SEM observation, Fig. 7. Samples taken for SEM examination.
8 A. Dulaimi et al. / Construction and Building Materials 250 (2020) 118808

Fig. 8. ITSM optimization for the BBF after 3 days curing.

Fig. 9. ITSM at normal curing.

dissolution and breaking of the glassy phase of the pozzolanic 3.2. Wheel tracking test results
material improved due to an increase in the pH of the hydration
medium. The presence of CCR in the CAEMs accelerated the break- A wheel tracking device is used mainly to determine rutting in
ing of the cationic bitumen emulsion as it increased the pH because bituminous mixtures at 60 °C, following BS EN 12697-22 [44].
of the alkaline nature of the material (pH = 13.1). The average ITSM Fig. 11 shows the depth of rutting of various bituminous slabs in
value for each of the five samples, was examined for each mixture. terms of number of applied load repetitions. The BBF mixture
With respect to the air voids in both the CAEMs and HMA, it was (G4C2) shows an improved performance in wheel tracking, while
observed that when the ITSM for the G4C2 mixture increased, the weakest performance was that of the LF mixture. The mixture
there was an enhancement in air voids. The air voids reduced from comprising 6% BBF, performed positively, resisting rutting and dis-
10.12% (for the LF mixture) to 8.92% (for the G4C2 mixture) by playing a longer surface life under a moving wheel load, as com-
increasing the CCR content in the G4C2 from 0% to 2%. CCR, with pared to the other mixtures.
its high alkalinity, accelerates the breaking of the bitumen emul-
sion which leads to free water in the mix prior to compacting. As 3.3. Fatigue results
a result of this, the compactability of the G4C2 improves. The air
voids of HMA 100/150 and HMA 40/60, are 4.65% and 3.84%, The fatigue characteristics of both the improved and traditional
respectively. CAEMs, in addition to two different HMA mixtures, were evaluated
 A. Dulaimi et al. / Construction and Building Materials 250 (2020) 118808 9

Fig. 10. ITSM after 3 days normal curing.

Fig. 11. Wheel track results.

through a four-point beam-bending test. Fig. 12 presents the con- be included in bituminous mixes and to predict long-term suscep-
ventional definition of fatigue distress at which the mixture stiff- tibility to stripping itself. In general, the higher the SMR value, the
ness modulus at specific cycles, dropped to half of its initial more water damage resistance. The results of SMR and ITSM for the
value. The mixture that can tolerate the maximum number of conditioned and dried mixtures, are shown in Fig. 13. The SMR of
cycles is expected to perform better than others with reference the improved specimen (G4C2), is higher than all the control spec-
to resistance to fatigue cracking. The control cold mix asphalt mix- imens (hot and cold). The enhancement in the bond between the
ture (LF), had the lowest fatigue life, followed by both hot mix aggregates and bitumen of the modified mixture has increased
asphalt mixtures. The modified cold asphalt emulsion mixture its tensile strength in wet conditions. As such, the development
(G4C2), tolerated the highest number of cycles and was ranked of the ITSM in saturated conditions in the modified specimens,
the best mixture with the longest fatigue life for both strain levels can be attributed to the enhanced cohesion and adhesion created
of 150 le and 200 le. after adding BBF, the new cementitious filler.

3.4. Water damage results 3.5. SEM observation

Water damage in asphalt mixtures creates a loss of serviceabil- The morphology of the microstructure of the fractured surface
ity due to the existence of moisture. The results of the current of the BBF paste samples at 3 and 28 days, is shown in Fig. 14.
study may help to establish which anti-stripping modifiers should The BBF particles started reacting at 3 days of age, the microstruc-
10 A. Dulaimi et al. / Construction and Building Materials 250 (2020) 118808

Fig. 12. Fatigue results.

Fig. 13. Water damage resistance results.

ture comprised of C-S-H gel and Portlandite with ettringite needle C-S-H gel. Looking at the SEM observation at 28 days, the develop-
crystals. A dense material has been created by these hydration ment of strength and the binding properties in the GGBS-CCR are
products, this responsible for the improvement in its mechanical due to the generation of Portlandite and C-S-H gel, most of the
properties. There are no intact particles in the BBF, major crystalli- ettringite generated at an early age. This means that ettringite is
sation happening in its early life, the surface of the BBF covered by responsible for some of the early strength developed in the
C-S-H gel, Portlandite and ettringite needles. It was reported by Shi GGBS-CCR, any further strength enhancement mainly attributed
and Day [53] that the generation of early reaction products and to the generation of Portlandite and C-S-H gel.
dissolution of slag in alkali-activated slag, are due to the primary The enhancement in the microstructure of G4C2 might be
pH of the activating median. In the current research, ettringite another reason for the improvement in air voids. The existence of
appeared in vacant areas during early hydration, CCR activating hydration products such as Ettringite, produced as a result of the
the GGBS leading to the precipitation of these needle crystals. This use of GGBS and CCR in the capillary voids of BBF, reduces porosity
ettringite, in addition to the formation of C-S-H gel and Portlandite, by decreasing both the pore size and their continuity, this resulting
aids stiffness improvement at an early stage [54,55]. in an enhancement of the volumetric properties meaning that the
At 28 days, the structure of the BBF was much denser and more movement of water into the mixture will be prevented. These find-
compact, crystalline products present in the sample. The alkali ings are consistent with those obtained by Nassar et al. [56] and
activation created by the CCR, increased the formation of more Dulaimi et al. [57].
 A. Dulaimi et al. / Construction and Building Materials 250 (2020) 118808 11

Fig. 14. Morphology details of microstructures: (a) and (b) morphology of BBF at 3 days, (c) and (d) morphology of BBF at 28 days.

4. Conclusions behind the increased stiffness over time. The formation of

needle-like ettringite, Portlandite and C-S-H gel as the prod-
The following conclusions are drawn as follows: ucts of BBF hydration, were found to significantly increase
the ITSM.
1. In terms of stiffness modulus and the rutting resistance of 5. The modified specimens containing a BBF additive, performed
CAEMs, the use of GGBS and CCR as a filler, can improve perfor- better in terms of moisture sensitivity compared to all other
mance. The stiffness modulus of said improved mixtures, control specimens. The increase in the amount of SMR in mod-
increased approximately 9 times more than the control LF mix- ified CAEM’s, can be attributed to the increase in bonds between
ture after 3 days of curing. aggregates and the bitumen emulsion.
2. The BBF mixture has an improved stiffness modulus, 6. Incorporating BBF into CAEMs appears to increase its fatigue
comparable to traditional HMA 100/150-pen, after approxi- life by about 3.5 and 9 times for strain levels 150 le and
mately 3 days of curing. This can help to remove the restrictions 200 le, respectively, in comparison to the traditional mixture
imposed by the pavement industry on the use of CAEMs with LF.
concerning the long curing period required for such mixtures. 7. Replacing traditional limestone filler with BBF will offer sus-
3. The addition of CCR was found to have an accelerating influence tainable advantages including a positive effect on the environ-
on the hydration of GGBS, as evaluated by the ITSM test and ment, the solution of problems related to carbon emissions in
confirmed by the SEM observation. the manufacture process and also problems related to the need
4. BBF was observed to produce considerably better proportions to maintain a suitable temperature during transportation and
of hydrated crystals, SEM analysis explaining the reasons the laying process for HMA.
12 A. Dulaimi et al. / Construction and Building Materials 250 (2020) 118808

[19] C. Ellis, B. Zhao, J. Barnes, N. Jones, Properties of GGBS-Bitumen emulsion

CRediT authorship contribution statement systems with recycled aggregates, Road Mater. Pavement Des. 5 (3) (2004)
373–383.
Anmar Dulaimi: Supervision, Resources, Project administra- [20] A. Modarres, P. Ayar, Comparing the mechanical properties of cold recycled
mixture containing coal waste additive and ordinary Portland cement, Int. J.
tion, Conceptualization, Methodology, Writing - original draft, Pavement Eng. (2016) 1–14.
Writing - review & editing, Investigation, Formal analysis, [21] A. Dulaimi, H. Al Nageim, F. Ruddock, L. Seton, New developments with cold
Validation. Hayder Kamil Shanbara: Conceptualization, asphalt concrete binder course mixtures containing binary blended
cementitious filler (BBCF), Constr. Build. Mater. 124 (2016) 414–423.
Resources, Methodology, Writing - original draft, Writing - review [22] S. Du, Mechanical properties and reaction characteristics of asphalt emulsion
& editing, Validation, Resources, Investigation, Formal analysis. mixture with activated ground granulated blast-furnace slag, Constr. Build.
Ali Al-Rifaie: Visualization, Writing - original draft, Writing - Mater. 187 (2018) 439–447.
[23] J. Bijen, Benefits of slag and fly ash, Constr. Build. Mater. 10 (5) (1996) 309–
review & editing, Methodology, Investigation, Formal analysis,
314.
Validation. [24] E. Özbay, M. Erdemir, H.I. _ Durmusß, Utilization and efficiency of ground
granulated blast furnace slag on concrete properties–a review, Constr. Build.
Mater. 105 (2016) 423–434.
Declaration of Competing Interest [25] P. Chaunsali, S. Peethamparan, Evolution of strength, microstructure and
mineralogical composition of a CKD–GGBFS binder, Cem. Concr. Res. 41 (2)
The authors declare that they have no known competing finan- (2011) 197–208.
[26] M.S. Konsta-Gdoutos, S.P. Shah, Hydration and properties of novel blended
cial interests or personal relationships that could have appeared cements based on cement kiln dust and blast furnace slag, Cem. Concr. Res. 33
to influence the work reported in this paper. (8) (2003) 1269–1276.
[27] M. Sadique, E. Coakley, The influence of physico-chemical properties of fly ash
and CKD on strength generation of high-volume fly ash concrete, Adv. Cem.
Acknowledgements Res. 28 (9) (2016) 595–605.
[28] S. Hanjitsuwan, T. Phoo-ngernkham, N. Damrongwiriyanupap, Comparative
The authors are grateful for the co-operation of Jobling Purser, study using Portland cement and calcium carbide residue as a promoter in
bottom ash geopolymer mortar, Constr. Build. Mater. 133 (2017)
BOC UK & Ireland, and to Hanson and Francis Flower who donated 128–134.
bitumen emulsion, CCR, GGBS and limestone filler to achieve the [29] Market Research Store, Acetylene gas market for chemical production, welding
current study. & cutting and other applications: Global industry perspective, comprehensive
analysis and forecast, 2014–2020. Market Research Store Rep., Deerfield Beach,
FL, 110, 2015.
References [30] European Committee for Standardization, BS EN 933-1:2012: Tests for
geometrical properties of aggregates-Part 1: Determination of particle size
distribution-Sieving method, British Standards Institution, London, UK, 2012.
[1] H.K. Shanbara, F. Ruddock, W. Atherton, Stresses and strains distribution of a
[31] H.K. Shanbara, F. Ruddock, W. Atherton, Predicting the rutting behaviour of
developed cold bituminous emulsion mixture using finite element analysis,
natural fibre-reinforced cold mix asphalt using the finite element method,
Sci. Technol. Behind Nanoemulsions (2018) 9.
Constr. Build. Mater. 167 (2018) 907–917.
[2] H.K. Shanbara, A. Shubbar, F. Ruddock, W. Atherton, Characterizing the Rutting
[32] A. Nikolaides, A new design method for dense cold mixtures, in: J.G. Cabrera, J.
Behaviour of Reinforced Cold Mix Asphalt with Natural and Synthetic Fibres
R. Dixon (Eds.), Proceedings of the first European symposium on performance
Using Finite Element Analysis, in: Advances in Structural Engineering and
and durability of bituminous materials. University of Leeds, E & FN Spon,
Rehabilitation, Springer, 2020, pp. 221–227.
London, 1994, p. 259.
[3] B. Gómez-Meijide, I. Pérez, Effects of the use of construction and demolition
[33] S. Hanjitsuwan, T. Phoo-ngernkham, L.-Y. Li, N. Damrongwiriyanupap, P.
waste aggregates in cold asphalt mixtures, Constr. Build. Mater. 51 (2014)
Chindaprasirt, Strength development and durability of alkali-activated fly ash
267–277.
mortar with calcium carbide residue as additive, Constr. Build. Mater. 162
[4] EAPA. Asphalt in Figures. Available from: http://www.asefma.es/wp-content/
(2018) 714–723.
uploads/2015/12/AIF_eapa_2014.pdf, 2014 (19th December 2016).
[34] Asphalt Institute, Asphalt cold mix manual, manual series no. 14(MS-14), third
[5] D. Needham, Developments in Bitumen Emulsion Mixtures for Roads,
ed., Lexington, KY 40512-4052, USA, 1989.
University of Nottingham, Nottingham, UK, 1996.
[35] C.K. Ojum, The Design and Optimisation of Cold Asphalt Emulsion Mixtures,
[6] H.A. Khalid, O.K. Monney, Moisture damage potential of cold asphalt, Int. J.
University of Nottingham, Nottingham, UK, 2015.
Pavement Eng. 10 (5) (2009) 311–318.
[36] European Committee for Standardization, PD 6691: Guidance on the use of BS
[7] I.N.A. Thanaya, J.P. Forth, S.E. Zoorob, A laboratory study on cold-mix, cold-lay
EN 13108 Bituminous mixtures – Material specifications, British Standards
emulsion mixtures. Proc. ICE – Trans. 162 (1) (2009) 47–55.
Institution, London, UK, 2015.
[8] D. Leech, Cold Asphalt Materials for Use in the Structural Layers of Roads.
[37] A. Dulaimi, H. Al Nageim, K. Hashim, F. Ruddock, L. Seton, Investigation into
Project Report 75, Transport Research Laboratory, Berks, U.K., 1994.
the Stiffness Improvement, Microstructure and Environmental Impact of A
[9] J. Read, D. Whiteoak, The Shell Bitumen Handbook - Fifth Edition, London, UK,
Novel Fast-Curing Cold Bituminous Emulsion Mixture, in: Eurasphalt &
2003.
Eurobitume Congress, Prague, Czech Republic, 2016.
[10] I.N. A. Thanaya, Improving the performance of cold bituminous emulsion
[38] A. Dulaimi, H. Al Nageim, F. Ruddoc,k L. Seton, Microanalysis of Alkali-
mixtures incorporating waste materials, University of Leeds, UK, 2003.
Activated Binary Blended Cementitious Filler in a Novel Cold Binder Course
[11] A. Dulaimi, H.A. Nageim, F. Ruddock, L. Seton, Laboratory studies to examine
Mixture, in: The 38th International Conference on Cement Microscopy, Lyon,
the properties of a novel cold-asphalt concrete binder course mixture
France, 2016.
containing binary blended cementitious filler, J. Mater. Civ. Eng. 29 (9)
[39] H.K. Shanbara, F. Ruddock, W. Atherton, A viscoplastic model for permanent
(2017) 04017139.
deformation prediction of reinforced cold mix asphalt, Constr. Build. Mater.
[12] H.K. Shanbara, F. Ruddock, W. Atherton, A laboratory study of high-
186 (2018) 287–302.
performance cold mix asphalt mixtures reinforced with natural and
[40] H.A. Khalid, O.K. Monney, Moisture damage potential of cold asphalt, Int. J.
synthetic fibres, Constr. Build. Mater. 172 (2018) 166–175.
Pavement Eng. 10 (2009) 311.
[13] A. Dulaimi, H. Al Nageim, F. Ruddock, L. Seton, Assessment the Performance of
[41] C. Ojum, K. Kuna, N.H. Thom, G. Airey, An investigation into the effects of
Cold Bituminous Emulsion Mixtures with Cement and Supplementary
accelerated curing on Cold Recycled Bituminous Mixes, in: International
Cementitious Material for Binder Course Mixture, in: The 38th International
Conference on Asphalt Pavements, ISAP, 2014, pp. 1177–1188.
Conference on Cement Microscopy, Lyon, France, 2016.
[42] European Committee for Standardization, BS EN 12697: Part 26. Bituminous
[14] Fu. Jun, Xiaoqiang Zhang, F. Wang, The meso structure and strain distribution
mixtures-test methods for hot mix asphalt- stiffness. London, British
analysis of cement emulsified asphalt concrete, Int. J. Pavement Res. Technol. 8
Standards Institution, UK, 2012.
(3) (2015).
[43] H.K. Shanbara, F. Ruddock, W. Atherton, Rutting prediction of a reinforced cold
[15] X. Fang, A. Garcia, F. Winnefeld, M.N. Partl, P. Lura, Impact of rapid-hardening
bituminous emulsion mixture using finite element modelling, Procedia Eng.
cements on mechanical properties of cement bitumen emulsion asphalt,
164 (2016) 222–229.
Mater. Struct. 49 (1) (2016) 487–498.
[44] European Committee for Standardization, BS EN 12697: Part 22. Bituminous
[16] A. Dulaimi, H. Al Nageim, F. Ruddock, L. Seton, A novel cold asphalt concrete
mixtures -Test methods for hot mix asphalt - Wheel tracking test methods for
mixture for heavily trafficked binder course, Int. J. Civ., Environ., Struct.,
hot mix asphalt London, British Standards Institution, UK, 2003.
Constr. Architect. Eng. 9 (15) (2015) 734–738.
[45] A. Dulaimi, H.A. Nageim, F. Ruddock, L. Seton, Laboratory studies to examine
[17] A. Dulaimi, H. Al Nageim, F. Ruddock, L. Seton, Performance analysis of a cold
the properties of a novel cold-asphalt concrete binder course mixture
asphalt concrete binder course containing high-calcium fly ash utilizing waste
containing binary blended cementitious filler, J. Mater. Civ. Eng. 29 (9) (2017).
material, J. Mater. Civ. Eng. 0 (0) (2017).
[46] H.K. Shanbara, F. Ruddock, W. Atherton, Improving the mechanical properties
[18] S. Al-Merzah, S. Al-Busaltan, H.A. Nageim, Characterizing cold bituminous
of cold mix asphalt mixtures reinforced by natural and synthetic fibers,
emulsion mixtures comprised of palm leaf ash, J. Mater. Civ. Eng. 31 (6) (2019).
Airfield Highway Pavements (2017) 102.
04019069.
 A. Dulaimi et al. / Construction and Building Materials 250 (2020) 118808 13

[47] European Committee for Standardization, BS EN 12697: Part 33.Bituminous sensitivity of bituminous specimens, British Standard Institution, London,
mixtures - Test methods for hot mix asphalt - Specimen prepared by roller UK, 2008.
compactor. London, British Standards Institution, UK , 2003. [53] C. Shi, R.L. Day, A calorimetric study of early hydration of alkali-slag cements,
[48] F. Cardone, A. Grilli, M. Bocci, A. Graziani, Curing and temperature sensitivity Cem. Concr. Res. 25 (6) (1995) 1333–1346.
of cement–bitumen treated materials, Int. J. Pavement Eng. 16 (10) (2014) [54] A. Xu, S. Sarkar, Microstructural study of gypsum activated fly-ashhydration in
868–880. cement paste, Cement Concr. Res. 21 (6) (1991) 1137–1147.
[49] K. Kuna, Mix design considerations and performance characteristics of foamed [55] C.S. Poon, S.C. Kou, L. Lam, Z.S. Lin, Activation of fly/cement systems using
bitumen mixtures (FBMs), University of Nottingham, United Kingdom, 2015. calcium sulfate anhydrite (CaSO4), Cem. Concr. Res. 31 (6) (2001) 873–881.
[50] European Committee for Standardization, BS EN 12697-24. Bituminous [56] A.I. Nassar, M.K. Mohammed, N. Thom, T. Parry, Mechanical, durability and
mixtures-Test methods for hot mix asphalt- Part 24: Resistance to fatigue. microstructure properties of Cold Asphalt Emulsion Mixtures with different
London, British Standard Institution, UK, 2012. types of filler, Constr. Build. Mater. 114 (2016) 352–363.
[51] A. Al-Hdabi, H. Al Nageim, L. Seton, Performance of gap graded cold asphalt [57] A. Dulaimi, H. Al Nageim, F. Ruddock, L. Seton, High performance cold asphalt
containing cement treated filler, Constr. Build. Mater. 69 (2014) 362–369. concrete mixture for binder course using alkali-activated binary blended
[52] European Committee for Standardization, BS EN 12697: Part 12. Bituminous cementitious filler, Constr. Build. Mater. 141 (2017) 160–170.
mixtures-test methods for hot mix asphalt-determination of the water