Construction and Building Materials 264 (2020) 120685

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Construction and Building Materials

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

Adhesion between steel slag aggregates and bituminous binder based on

surface characteristics and mixture moisture resistance
Bárbara Luiza Riz de Moura a, Jamilla Emi Sudo Lutif Teixeira a,⇑, Renata Antoun Simão b,
Mahdieh Khedmati c, Yong-Rak Kim d, Patrício José Moreira Pires a
a
Civil Engineering Pos-Graduate Program, Universidade Federal do Espírito Santo, Vitória, ES, Brazil
b
Department of Metallurgical and Materials Engineering, Universidade Federal do Rio de Janeiro, Rio de Janeiro, Brazil
c
Whittier Research Center, University of Nebraska-Lincoln, Lincoln, NE, USA
d
Zachry Department of Civil & Environmental Engineering, Texas A&M University, College Station, TX, USA

h i g h l i g h t s

Binder-slag adhesion assessment based on small scale characterization.

Air-cooled blast furnace (ACBFS) slag and Linz-Donawitz (LD) slag were examined.

Chemical and surface energy characteristics affects binder-slag adhesion.

The AFM appeared as a promising method to evaluate binder-aggregate adhesion.

Small-scale surface characteristics agreed well with the large-scale observations.

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

Article history: Steel slag aggregates (SSA) have shown promising mechanical and physical properties for asphalt con-
Received 13 May 2020 crete application. However, SSA surface characteristics vary depending on the type of slag, which results
Received in revised form 12 August 2020 in different binder-SSA adhesion that affects moisture damage of asphalt mixtures containing SSA. This
Accepted 19 August 2020
study evaluated the adhesion in the binder-SSA system considering two typical types of slags (i.e. air-
Available online 22 September 2020
cooled blast furnace slag (ACBFS) and Linz-Donawitz steel slag (LD)) using various tests: morphological,
physical, chemical, and surface energy measurements. Also, the moisture damage susceptibility of
Keywords:
asphalt mixtures containing SSA were assessed based on two standard methods: ASTM D3625 and
Steel slag
Blast furnace slag
AASHTO T283. Test results showed strong influence of the SSA chemical composition and surface energy
Adhesion characteristics on the SSA-binder adhesion. LD showed a better adhesion with the asphalt binder than
Surface energy ACBFS due to its particular chemical and surface energy characteristics. The diminished adhesive bonding
Moisture damage from ACBFS could be improved with proper surface treatment using additives such as hydrated lime and
electrostatic precipitator powder, which change surface chemistry of ACBFS.
Ó 2020 Elsevier Ltd. All rights reserved.

1. Introduction
Industrial by-products from the steel industry have already
been studied and applied as infrastructure materials in the various
layers of pavement structures. Among the different types of slags
produced in the steelmaking process, it is highlighted herein the
⇑ Corresponding authors at: Centro Tecnológico, Dept. de Engenharia Civil
(CT-DEC). Universidade Federal do Espírito Santo (UFES). Av. Fernando Ferrari,
514 - CT I, Goiabeiras, CEP: 29060-970, Vitória, ES, Brazil.
E-mail addresses: barbaralrmoura@gmail.com (B.L.R. de Moura), jamilla.teixeira@
ufes.br (J.E.S.L Teixeira), renata@metalmat.ufrj.br (R.A. Simão), mahdieh.khedmati@
huskers.unl.edu (M. Khedmati), yong-rak.kim@tamu.edu (Y.-R. Kim), patricio.
pires@ufes.br (P.J.M. Pires).
use of air-cooled blast furnace slag (ACBFS, also referred as iron
slag) and Linz-Donawitz steel slag (LD). The former, obtained in
the initial steps of the process to produce molten iron, is a result
of reduced calcium carbonate which is associated with silicon
oxide, as well as other remaining process compounds such as alu-
minum and magnesium oxides. LD slag, on the contrary, is
obtained in the latter steps of the steel fabrication, and it is mainly
composed of calcium and iron oxides, followed by silicon, magne-
sium and manganese oxides [1,2]. The ACBFS has attractive proper-
ties for pavement application such as solidity, abrasion resistance
and high angle of friction, due to the angular shape, which justify
its application [3]. Similarly, LD has favorable characteristics such
as high stability, promising frictional properties and stripping

https://doi.org/10.1016/j.conbuildmat.2020.120685
0950-0618/Ó 2020 Elsevier Ltd. All rights reserved.
Bárbara Luiza Riz de Moura et al.
resistance [4,5]. However, those materials, when combined with
asphalt binder to produce asphalt mixtures, present significant
variances on the binder-aggregate surface adhesion, which subse-
quently affects the mixture’s moisture resistance. Chemically, the
types of steel slag aggregates (SSA) present changes in the percent-
ages of SiO2 and Fe2O3 [6]. These two oxides play an important role
in the asphalt binder and SSA adhesion. Thus, it is important to
identify the main differences among SSA that can notably affect
the overall asphalt mixture performance, in particular the moisture
damage resistance.
Related to the asphalt mixture performance, the adhesion can
be defined as the ability of the aggregate to be enveloped by the
asphalt binder, and it is usually dependent on the synergistic effect
of chemical interactions, physical adhesion and mechanical inter-
locking. A good binder-aggregate adhesion is essential to avoid
damage due to fatigue and moisture [7]. Cracks in this interface
are indicative of low adhesiveness between the compounds of
the bituminous mixtures. The interaction between binder and
aggregate is much more influenced by the surface characteristics
of the aggregates than by those of the binder. Aggregate with same
physical and mechanical characteristics may present variation in
adhesiveness due to differences in the chemical composition which
is relevant to the interaction forces formed between these materi-
als [8–11].
The cohesive (within the asphalt binder itself) and adhesive
interactions (at the binder-aggregate interface) are related to the
surface energy of the asphalt mixture components. The surface
energy concepts can be used to quantify the work of adhesion
between materials. The thermodynamic changes in the surface
energy are related to the disassociation of the bonded materials
and, consequently, the cracking potential in the asphalt composite
[12]. Zhou et al. [13] comment that SSA has greater interface
energy comparing to natural aggregates, such as basalt and ande-
site, when they are in association with asphalt binder, and SSA is
more susceptible to cohesive failure while the natural aggregates
are more prone to adhesive failures. Aguiar-Moya et al. [14] com-
ment that the work of adhesion generated in binder-aggregate
interface directly affects the resistance of asphalt mixture to mois-
ture damage because this parameter quantifies the ease with
which water can displace asphalt binder from the aggregate’s
surface.
Regarding the chemical composition, aggregates that are nega-
tively charged in the presence of water, such as silica-based aggre-
gates, have low adhesiveness to the asphalt binder [15]. In parallel,
those that present compounds such as iron, calcium, magnesium,
and aluminum, tend to have high affinity to the bituminous binder
[16]. Studies by Cala et al. [17,18] proposed a moisture damage
index based on an evaluation of aggregates with different litho-
graphs. They suggested that SiO2 is one of the compounds that
can contribute negatively to moisture damage, while other oxides
such as Al2O3, Fe2O3 and MgO are important compounds to mini-
mize such damage.
Existing studies demonstrate that the binder-aggregate interac-
tion is directly related to the small-scale chemical and thermody-
namic internal characteristics. Thus, better understanding of
those characteristics of SSA is essential for an adequate application.
As an attempt, this study aims to evaluate the adhesive character-
istics of the binder-slag system through different micro-surface
analyses in order to better understand the adhesion mechanisms
between SSA and asphalt binder. Resulting findings can help better
selection and engineering of SSA in asphalt mixtures if used as sup-
plemental recycled aggregates.
This study aims to identify the small-scale characteristics of two
different slags that might influence the binder-slag adhesion, con-
sidering the mechanical interlocking (physical adhesion), surface
free energy and work of adhesion (thermodynamic adhesion) and
2
Construction and Building Materials 264 (2020) 120685
chemical interactions between binder and SSA components.
Toward that end, two different types of SSA (i.e. ACBFS and LD)
were used and characterized using the following methods:

Laser scanning microscopy (LSM) for analysis of the surface
roughness and aggregate image measurement system (AIMS)
for shape properties (e.g. texture, angularity);

Contact angle measurements and atomic force microscopy
(AFM) test to investigate the free energy of the surface and
the adhesive work between binder and SSA, respectively;

X-ray fluorescence (XRF) test to identify the main oxides pre-
sented in each SSA; and

ASTM D3625 [19] which is empirical but can easily assess adhe-
sive bonding of binder to aggregates.
In addition, the moisture resistance of HMA mixtures with par-
tial replacement of natural aggregates by SSA was evaluated using
AASHTO T283-14 [20]. The HMA mixtures were designed using
75% of natural aggregates (NA) and 25% of SSA (either ACBFS or
LD). Also, additional HMA containing ACBFS were evaluated by
adding different additives, such as hydrated lime (HL), natural
aggregate passing #200 sieve (NA’), and two steel dust by-
products (FGD and EP).
2. Materials and methods
Fig. 1 shows a flowchart to summarize the selected materials
and the procedures presented in the study. The HMA mixtures
were named according to the type of slag used followed by the
type of filler addition.
2.1. Materials
Two different SSA (ACBFS and LD) were evaluated in this study.
Samples from those materials were obtained from a local steel
company. For the morphological testing methods and HMA pro-
duction, SSA particles were obtained after the company internal
crushing process, as shown in Fig. 2 (a and b). The SSA’s well-
distributed aggregate gradations with NMAS of 19 mm are pre-
sented in Fig. 3. For the thermodynamic analysis, cylindrical sam-
ples with about 23 mm in diameter as shown in Fig. 2 (c and d)
were extracted from large prismatic blocks of slag (approximately
100 mm  100 mm  200 mm). These samples were polished to
minimize the effects of aggregate roughness on the results.
In some experimental procedures employed in this study,
asphalt cement with a penetration grade of 50/70 was used. Table 1
presents its characterization, which is in accordance with ASTM
standard limits.
2.2. Binder-Slag adhesion methods
2.2.1. Morphological properties
a) Shape, angularity and texture by Aggregate Image Measurement
System (AIMS)
It is believed that mechanical interlocking is a mechanism of
physical adhesion that influences the ability of the aggregate to
be covered by asphalt cement. According to several studies, this
binder-aggregate adhesion mechanism is directly related to the
aggregate roughness [21]. Besides this property, other morpholog-
ical properties affect the asphalt mixture’s performance, such as
the aggregate’s shape and angularity.
To assess SSA’s morphology, AIMS equipment was used. It is
capable of obtaining different morphological properties of particles
through digital imaging technology. The equipment captures
images of reasonable number of aggregate particles in different
Bárbara Luiza Riz de Moura et al. Construction and Building Materials 264 (2020) 120685

Fig. 1. Flowchart of the experimental plan.

Fig. 2. ACBFS a) granular and c) cylindrical samples; LD b) granular and d) cylindrical samples.

100
90
80
70
Passing (%)

60
50
40
30
20
10
0
0.0001 0.001 0.01 0.1 1 10 100 1000

Particle size (mm)

ACBFS LD

Fig. 3. Particle size distribution curve of ACBFS and LD.

resolutions and angles of view providing an analysis of the shape,
angularity and texture in a short amount of time [22–24] and the
results were obtained according to AASHTO TP-81 [25]. Al Rousan
[26] proposed a classification system after gathering AIMS results
of 13 types of coarse aggregates and 5 types of fine aggregates with
known shape characteristics. For this study, ACBFS and LD samples
were evaluated using AIMS procedure and based on the results,
they were classified according to the classification established by
Al Rousan [26] and compared.
b) Roughness by Laser-Scanning Microscopy (LSM)
In addition to AIMS evaluation, the SSA surface roughness was
also assessed using LSM. This equipment is able to scan multiple
locations on the surface of a sample using a laser scanning micro-
scope. The microscope collects optical images and high-resolution
surface data by combining laser light with white light. The high-
resolution image of the sample is obtained by the reflection inten-
sity of the laser beams; thus, the topography is plotted by analyz-
ing the intensity of the return of the laser beam to the z position.
A statistical representation of the particle roughness, the root
mean square (RMS) roughness, was obtained by measuring the

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Bárbara Luiza Riz de Moura et al. Construction and Building Materials 264 (2020) 120685

Table 1
Asphalt binder characterization results.

Characteristics ASTM Method Specification Result Unit

Penetration D5 50 to 70 51 0.1 mm
Softening Point D 36 46 min 50 °C
Brookfield Viscosity 135° C-SP21 20 RPM D 4402 274 min 323 cP
Brookfield Viscosity 150 °C-SP21 D 4402 112 min 163 cP
Brookfield Viscosity 177 °C-SP21 D 4402 57 to 285 min 61 cP
RTFOT - Residual Penetration D5 55 min 61 %
RTFOT – Softening Point Increase D 36 8 max 5.0 °C
RTFOT - Ductility at 25 °C D 113 20 min >150 cm
RTFOT - % Weight Range D 2872 0.50 to 0.50 0.305 %
Ductility at 25 °C D 133 60 min >150 cm
Solubility in trichloroethylene D 2042 99.5 min 99.9 % mass
Flash Point D 92 235 min 344 °C
Thermal Suscetibility Index X 018 1.5 to 1.7 1.1 N/A
Relative Density at 20/4 °C D 70 (1) 1.011 N/A
Heating at 177 °C X 215 (2) (2) N/A

magnitude of a set of collected points in the surface and squaring
each number, then taking their average and the square root of
the average. The RMS roughness of the studied SSA was calculated
based on scanning measurements of five different areas (1430 mm
by 1000 mm) per sample. Three aggregate particles were scanned
for each type of SSA. The output data were also represented in a
3D topographic image.
2.2.2. Thermodynamic properties
a) Contact Angle Assessment
Wettability can be defined as the acceptance of a liquid to
spread over a solid surface. The wetting phenomena can be
observed when a drop of a liquid rests on a solid level surface
and interacts with it. The more spread the drop, the higher the sur-
face energy of the material’s interface. This concept has been
applied in many studies to verify the surface energy of the materi-
als [14,27–29]. A way to experimentally determine wetting is to
look at the contact angle (h), which is the angle connecting the
solid–liquid interface (Fig. 4a). It is established between the tan-
gent to a drop of liquid and the solid where the liquid was depos-
ited [30]. If h = 0°, the liquid completely wets the substrate. If 0°
< h < 90°, high wetting occurs. If 90° < h < 180°, low wetting occurs.
If h = 180°, the liquid does not wet the substrate at all.
Equation (1) (from the acid-base theory) is recognized as a ther-
modynamic equilibrium between materials and it relates the mea-
sured angle h to the surface energy components: nonpolar
component (cLW), acidic component (c+) and basic component
(c-). The S and L are related to the solid and liquid materials,
respectively.
qffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi qffiffiffiffiffiffiffiffiffiffiffi qffiffiffiffiffiffiffiffiffiffiffi
cL ð1 þ coshÞ ¼ 2 cLW
S cL þ 2
LW
cþS cL þ 2 cL cþS
In this study, an automated goniometer (Ramé-Hart, 100–50)
was used coupled with a CCD camera to obtain several images of
the drop of different liquids on SSA’s surface. The obtained images
are treated and the contact angles in the two ends of the drop are
measured. First, three probe liquids with known surface energies
and not capable of dissolving or chemically reacting with the
SSA, such as distilled water, glycerol (polar liquids) and diiodo-
methane (non-polar liquid), were used to quantify the SSA’s sur-
face free energy. Second, an asphalt binder drop was used to
verify the difference in wettability of the asphalt binder on differ-
ent SSA solid surfaces; similar analyses are found in [31–33]
(Fig. 4b). The binder was previously heated to 80 °C.
b) Atomic Force Microscopy (AFM)
The AFM has been used in many studies to extend the study of
the micro-rheological properties of asphalt binders, and to evalu-
ate the binder’s microstructural changes when subjected to load
[34–36]. Also, its scanning technique allows gathering information
about the substrate surface. AFM has recently become an interest-
ing alternative for the study of material’s adhesion [37]. AFM is
able to measure the fundamental attraction and retraction forces
between the material from the AFM tip and the selected substrate.
Each time the tip approximates and withdraws from a substrate,
instantaneous attraction and retraction forces are developed, as
illustrated in Fig. 5a [38,39]. As a result, and the deflective curve
is generated. This outcome curve allows the measurement of the
adhesive force between different materials with different atomic
compositions. The work of the adhesion force can be obtained by
calculating the area between the retraction curve and the x-axis
(Fig. 5b).
In this study, the AFM was employed to verify the adhesion
forces between binder and SSA aggregates. Thus, the slag aggre-
gates were considered, the substrate and two different procedures
were established. In the first one, polished slag samples were sub-
jected to a load applied by a silicon tip of undetermined elastic
constant - ranging between 20 and 80 kN/m and a frequency
ð1Þ
between 319 and 367 Hz. In the second procedure, a modified
AFM test was performed by covering another silicon tip of the
AFM with the same specifications by an asphalt binder film prior
to contact on the slag substrate. In this way, the work of adhesion
between binder-slag could be quantified.

Fig. 4. a) 2020 Ramé-Hart instrument co. image, b) Illustration of a drop of asphalt binder in the SSA surface and the surface free energy components.

4
Bárbara Luiza Riz de Moura et al.
Fig. 5. a) AFM resulting curves during the tip approximation and retraction from the substrate and b) Generic AFM curve with highlighted work of adhesion.
2.2.3. Chemical analysis by X-ray fluorescence (XRF)
To determine the main oxides components of the ACBFS and LD
samples, XRF analyses were performed in the SSA samples using a
WDS spectrometer and a Rh anode tube. Representative samples of
dry SSA containing difference particle sizes were crushed to obtain
XRF samples with particles passing in the n° 200 sieve (75 mm).
2.2.4. Visual observation according to ASTM D3625
The ASTM D3625 [19] is a rapid and commonly used procedure
to visualize the loss of adhesiveness in non-compacted asphalt
mixtures under the action of boiling water. For this study, initially
two samples of 250 g of SSA (LD and ACBFS) were mixed with
12.5 g of binder content (binder content of 5.0%). Since LD is denser
than ACBFS, a notable difference in the total volume of aggregates
was observed. Thus, a third LD sample (with the same volume of
aggregate particles used for ACBFS test) was also mixed with
12.5 g of asphalt binder and evaluated. After mixing the aggregates
with asphalt binder, each mixture was placed in a beaker contain-
ing 500 ml of distilled water and placed in an oven under a temper-
ature of 115 °C for 10 min. At the end of the process, the mixture
was drained and poured into a white ceramic container for the
visual analysis of adhesion loss between binder and SSA.
2.3. HMA moisture damage evaluation based on AASHTO T283
Initially, two asphalt mixtures were produced using 75% of nat-
ural aggregates and 25% of SSA, named HMA_ACBFS and HMA_LD,
according to the type of slag used in the mixture composition. The
aggregate gradation for both mixtures was kept the same and it
was based on the results from Teixeira et al. [4], representing a typ-
ical Superpave dense graded mixture. The optimum binder content
(5.14%) for the HMA_LD was also selected based on the referenced
study. For the HMA_ACBFS mixture, cylindrical Marshall com-
pacted samples with 75 blows on each side were produced with
different binder contents until a 4 ± 1% was obtained. Thus, the
optimum binder content for this mixture was found and equal to
5.84%.
In addition, the HMA_ACBFS received the addition of four chem-
ically different powders to improve its moisture resistance. The
selected powders were: 1) hydrated lime (HL), a typical additive
used to improve moisture resistance of asphalt mixtures; 2) fluid
gas desulfurization powder (FGD), a steel by-product powder with
high content of CaO, 3) electrostatic precipitator powder (EP),
another steel by-product powder that contains high percentages
of Fe2O3 in its composition, and 4) natural aggregate passing in
5
Construction and Building Materials 264 (2020) 120685
no. 200 sieve (NA’), included in the experimental plan to evaluate
the filling effect only since the granitic aggregate is mainly com-
posed of silicon oxide and it is not expected to improve the mois-
ture damage. Fig. 6 presents the studied HMA mixtures, including
the main differences on their composition.
The studied HMA were subjected to AASHTO T 283 procedure.
Six specimens of each mixture were compacted using Marshall
impactor to obtain cylindrical specimens with air voids of 7 ± 1%.
According to the AASHTO T 283 [20] procedure, three specimens
(conditioned set) were partially saturated, then submitted to a
freezing condition at 18 ± 3 °C and subsequently to a water bath
at 60 ± 1 °C before subjected to indirect tensile strength (ITS) test.
The other three specimens (dry set) were submitted to ITS without
conditioning. The ITS test was conducted at a 0.8 mm/s displace-
ment rate at 25 °C until the rupture and the tensile strength ratio
(TSR) (Equation (2)), which represents the fraction of tensile
strength remaining after moisture conditioning, was calculated.
S2
TSR ¼ ð2Þ
S1
S1: average tensile strength of the dry subset (kPa);
S2: average tensile strength of the conditioned subset (kPa).
3. Results and discussion
3.1. Morphology results
Table 2 shows the mean results obtained in AIMS and the clas-
sification according to the criteria established by Al Rousan [26]. It
can be noted that the morphological characteristics are very simi-
lar between both SSA. Considering the texture results, which is
assumed to be a characteristic that will greatly affect the mechan-
ical interlocking between the binder and the SSA, it can be seen
that either ACBFS or LD slags presented particles ranging from
smooth to high roughness. Considering these results, it is possible
to assume that the differences on the binder-slag adhesion behav-
ior were not related to their morphological properties.
3.2. RMS roughness
Fig. 7 shows representative 3D topographic image of each SSA.
The average RMS surface roughness was 41.60 ± 13.27 mm and
28.80 ± 9.07 mm, for ACBFS and LD samples, respectively. From
the presented values, the roughness of the ACBFS is notoriously
superior to the LD. Although the ACBFS presents higher values of
Bárbara Luiza Riz de Moura et al. Construction and Building Materials 264 (2020) 120685

Fig. 6. Studied HMA mixtures for moisture damage evaluation.

3.3. Contact angle results

Table 2
Aggregates classification according to Al Rousan [26]. The contact angles formed with each aggregate with the probe
Morphological Limit values ACBFS LD liquids are presented in Table 3. With these values, the surface free
Characteristic energies for the ACBFS and LD were calculated and equivalent to
2D Form < 6.5 (Circular) 45.7% 45.5% 34.65 ergs/cm2 and 36.75 ergs/cm2, respectively. For comparisons,
6.5 – 8.0 (Semi-Circular) 27.6% 26.2% Moraes, Velasquez and Bahia [40] found surface free energy values
8.0 – 10.5 (Semi-Elongated) 20.4% 24.6% of 19.3 and 31.3 ergs/cm2 for granite and limestone aggregates,
> 10.5 (Elongated) 6.3% 3.7% respectively. It can be observed that both SSA presented compara-
Angularity < 2100 (Rounded) 16.9% 22.0%
2100 – 4000 (Sub-Rounded) 58.4% 56.3%
ble values of surface free energy of those found for limestone
4000 – 5400 (Sub-Angular) 19.2% 16.9% aggregate samples, which implies a better adhesive characteristic.
> 5400 (Angular) 5.5% 4.6% However, the difference was not as significant between the two
Sphericity < 0.6 (Flat elongated) 10.2% 9.0% slags as it was expected.
0.6 – 0.7 (Low sphericity) 33.1% 23.6%
Table 3 also shows the values of contact angle between aggre-
0.7 – 0.8 (Moderate sphericity) 34.4% 37.1%
> 0.8 (High sphericity) 22.3% 30.2% gate and binder. As it can be seen, the results for ACBFS and LD
Texture < 165 (Polished) 5.4% 8.8% are similar, which corroborates with the surface energy results.
165 – 275 (Smooth) 24.9% 21.9% ACBFS presented slightly greater value of contact angle, denoting
275 – 350 (Low Roughness) 22.7% 17.2% a lower adhesiveness to the asphalt binder. Since LD is better
350 – 460 (Moderate 23.6% 27.3%
Roughness)
adhered by the binder, it was expected that the adhesion work
> 460 (High Roughness) 23.4% 24.7% for this type of slag would be considerably higher than of ACBFS,
resulting in contact angle values considerably lower than of ACBFS
ones. It is believed that this method could not properly identify dif-
ference in thermodynamic properties, especially, by the hetero-
roughness, this is not enough to guarantee a satisfactory adhesion. geneity of the composition of the material and the distribution of
According to Yoon and Tarrer [11], the physical properties of the pores on the surface [40,41].
aggregate - such as surface area and roughness - influence the ease
of bonding between binder and aggregate, but there is no strong 3.4. Work of adhesion
correlation between these factors. In their study, the authors con-
clude that the chemical and electrochemical properties are deter- As mentioned before, the work of adhesion was measured with
minants for the adhesiveness in the bituminous matrix. and without having the tip covered by asphalt, which means that

Fig. 7. 3D image of the surface in a) ACBFS and b) LD.

6
Bárbara Luiza Riz de Moura et al. Construction and Building Materials 264 (2020) 120685

Table 3
Contact angle values for each liquid for ACBFS and LD characterization and values of contact angle between asphalt binder and aggregates.

Substrate h(°)
Distilled water Glycerol Diiodomethane Asphalt binder
ACBFS 63.38 93.59 43.48 58.41 ± 0.11
LD 65.41 81.55 48.04 56.94 ± 0.06

Atraction Retraction Atraction Retraction

Deflective force [nN]

Deflective force [nN]

0.3 0.3
0.2 0.2 Interatomic interactions
0.1 0.1
0 0
-0.1 0 100 200 -0.1 0 50 100 150 200
-0.2 -0.2
Distance tip-sample [nm] Distance tip-sample [nm]
(a) (b)

Atraction Retraction
Atraction Retraction

Deflective force [nN]

Deflective force [nN]

0.3 0.3
0.2 Interatomic interactions
0.2
0.1 0.1
0 0
-0.1 0 50 100 150 200 -0.1 0 50 100 150 200
-0.2 -0.2
Distance tip-sample [nm] Distance tip-sample [nm]
(c) (d)
Fig. 8. Maps 1 - ACBFS work of adhesion for: a) tip without binder e b) tip with binder and LD work of adhesion for: c) tip without binder e d) tip with binder.

the results of the tip without the binder measure the interaction of
the aggregate with the silicon tip, while those of the binder tip
evaluate the interaction of the binder with the slag. In Fig. 8, the
average values of the maps 1 for the ACBFS and the LD, without
and with the binder, are presented. Fig. 9 shows the comparative
for all maps in the samples for the same tip, without and with
asphalt binder at the tip.
From Fig. 8, it can be noticed that when the tip is not covered by
asphalt, the retraction forces between silicon tips and the different
slags do not seem significant, and the pulling force is reduced
quickly. However, the tests performed with the tip covered by
asphalt (Fig. 8b and 8d), shows that the pulling force is not reduced
immediately as the tip-binder assembly moves away from the
aggregate. The calculated work of adhesion presented in Fig. 9 indi-
cates that the LD slag presented a higher interaction with the tip in
the three regions tested, in relation to the values of the ACBFS slag.
But what stands out in these results is the high values of the work
of adhesion for LD slag when tested with tip covered by asphalt
binder; the same does not occur for the ACBFS aggregate. Further-
more, it can be seen that the distances where the interatomic
bonds between binder and SSA components are different between
binder-ACBFS and binder-LD. For binder-LD, the interatomic inter-
actions start to occur at greater distances. Also, once the inter-
atomic adhesive forces are established, they need long distances
to be null again. This result reveals a stronger interaction between
LD SSA with the asphalt binder in comparison with ACBFS SSA .
3.5. Chemical composition
Table 4 presents the chemical composition of the ACBFS and LD
slag. It can be observed that ACBFS is rich in silicon, calcium and
aluminum oxides, presenting a binary basicity (BB = %CaO/%Si2O)
higher than 1, indicating that it is a basic compound. However,
7
the unsatisfactory bonding of EFRA to the binder indicates that
CaO and Al2O3 (important oxides that are related to good moisture
resistance of certain aggregates) are not able to overcome the neg-
ative effects of SiO2 on aggregate’s moisture resistance. Parallel to
this, LD slag is mainly composed of CaO and Fe2O3. It is possible to
evaluate the good adhesiveness of this aggregate due to the pres-
ence of Fe2O3 and the low content of SiO2, since calcium oxide con-
tent are similar on both SSA’s.
As already mentioned, and well known by experience, silica
aggregates have low adhesiveness to the asphalt binder. Corrobo-
rating with this, the works developed by Cala et al. [17–18] con-
cluded that felsic (silicon rich) aggregates have less resistance to
moisture damage than mafics, whose main composition is magne-
sium and iron and with low silicon content. According to the
authors, SiO2 is the main oxide responsible for damage due to
moisture. Also, other oxides, such as Al2O3, Fe2O3, MnO and MgO
- typical of mafic rocks - are important to avoid moisture damage
in asphalt mixtures.
In addition to SSA, the selected fillers added in HMA for mois-
ture damage evaluation were also subjected to XRF tests, and the
results are shown on Table 5. As expected, the FGD powder has a
high calcium content similarly to the HL and its application is jus-
tified by the action of basic fillers to increase the base component
and, consequently, the adhesion binder-aggregate of the mastic as
found by Arbabpour Bidgoli, Naderi and Moghadas Nejad [42]. The
EP powder has about 63% of iron content and the NA’ is mostly
composed of silicon oxide.
3.6. ASTM D3625 results
Fig. 10 shows the results from ASTM D3625. It is clear the visual
differences between the adhesion of asphalt binder with different
SSA’s. While LD showed great adhesion with the asphalt binder,
Bárbara Luiza Riz de Moura et al. Construction and Building Materials 264 (2020) 120685

Tip Tip with binder Tip Tip with binder

90

Work of Adhesion
90

Work of Adhesion
75 75

[10-19 J]

[10-19 J]
60 60
45 45
30 30
15 15
0 0
1 2 3 1 2 3 Map
Map

(a) (b)
Fig. 9. Work of adhesion for a) ACBFS e b) LD.

ACBFS notably presented unsatisfactory adhesion results, present-

Table 4 ing a considerable number of particles not completely covered by
Chemical composition of the studied slags by XRF. asphalt binder. This result confirms the low binder-EFRA adhesion
Oxides ACBFS (%) LD (%)
based on work of adhesion (thermodynamic adhesion) and chem-
ical interactions between binder and SSA components.
Na2O 0.28 0.17
MgO 5.20 5.00
Al2O3 9.30 4.90
3.7. HMA moisture damage results
SiO2 32.40 12.70
P2O5 0.10 1.30
SO3 4.50 0.16 Fig. 11 presents the obtained values for tensile strength for the
K2O 0.32 <0.10 conditioned and unconditioned groups – and the respective stan-
CaO 41.2 43.40
dard deviations - for all the mixtures and their respective TSR.
TiO2 0.49 0.36
MnO 0.55 3.20 According to many roadway agencies specifications, a minimum
Fe2O3 2.70 26.4 TSR of 70% is recommended.
SrO 0.11 0.10 From Fig. 11, only the HMA_ LD reached a TSR above 70% while
mixtures with ACBFS did not. These results corroborate with the
advanced surface adhesion tests, where LD presented a significant
amount of Fe2O3 and low percentage of SiO2 (compounds that are
related to positive and negative asphalt mixture moisture resis-
Table 5
tance, respectively) and improved work of adhesion and wettabil-
Chemical composition of the studied additives.
ity according to AFM and SFE results. Regarding the effects of
Oxide HL FGD EP NA’ additional fillers, the mixture with natural aggregate powder
Al2O3 0.41 <0.10 1.76 14.52 (HMA_ACBFS_NA’) behaved similarly to the reference mixture
CaO 66.83 56.40 12.14 7.46 (HMA_ACBFS), which indicates that the addition of a silicon-rich
Cr2O3 <0.01 <0.01 0.03 <0.01
filler did not contribute to resistance to moisture conditioning. Fur-
Fe2O3 0.16 0.12 62.94 8.82
K2O 0.19 0.04 0.33 3.56 thermore, it should be noted that the addition of any filler, just to
MgO 1.35 0.55 1.95 2.61 physically filling the asphalt mixture, does not guarantee a good
MnO <0.01 <0.01 0.53 0.12 performance against resistance to moisture damage.
Na2O <0.1 <0.1 <0.10 2.86 The mixture HMA_ACBFS_HL presented a TSR of 65%, showing
P2O5 0.17 0.17 0.08 2.35
SiO2 1.28 0.38 5.55 54.65
the improvement on the moisture resistance due to HL addition
TiO2 0.02 <0.01 0.15 1.63 (from 54% to 65%). The positive effect due to the addition of HL
ZrO2 <0.01 – – 0.13 on the mixture’s moisture resistance was expected, as other stud-
SO3 – 25.09 1.11 – ies showed similar results [21,43]. Although the addition of HL
ZnO – 0.02 0.08 –
improved the moisture resistance of asphalt mixture in compar-
ison with the mixture without any additive (i.e. HMA_ACBFS), it
did not reach the minimum recommended TSR value (i.e. 70%).

Fig. 10. ASTM D3625 - Boiling Test: a) LD (same vol. as ACBFS); b) LD (same mass as ACBFS), and c) ACBFS (250 g in mass and 94 cm3 in volume).

8
Bárbara Luiza Riz de Moura et al.
1.8
1.6
Tensile Strength (MPa) 1.4
1.2 54%
1.0
0.8
0.6
0.4
0.2
0.0
HMA_ACBFS
Positive effects on moisture resistance gain were observed with the
addition of EP powder (which is rich in Fe2O3). HL and EP powders
were more beneficial to the increase of moisture damage resis-
tance than other fillers. The mixture with FGD powder presented
a TSR of 58%. Although FGD presents a high content of CaO (as
HL), its effect was much less than HL. This could be related to
two aspects. First, the available free lime content in FGD might
be low. Dick et al. [44] showed that FGD free lime content can be
decreased when this material is stockpiled due to carbonation of
Ca(OH)2 by forming CaCO3 and ettringite and thaumasite forma-
tion. Second, the high content of SO3 in FGD could be a negative
factor. The two aspects require further investigation, which is in
progress by the authors.
4. Conclusions
This study evaluated the adhesion characteristics in the binder-
slag system through physical-geometrical-chemical surface char-
acterization to better understand the adhesion mechanisms that
may affect the asphalt mixture performance. From the test results,
the following conclusions can be drawn:

Considering the three mechanisms that contribute to binder-
aggregate adhesion, the physical adhesion (due to surface
roughness) was not predominant to explain the differences
found between SSA-binder systems. On the other hand, the bet-
ter bonding potential of LD was explained based on the chemi-
cal and surface energy measurements. This, although somewhat
indirect, indicates that the adhesion mechanism of slag aggre-
gates with asphalt binder is more influenced by aggregate sur-
face chemistry/energy than roughness.

The AFM appeared as a promising method to evaluate the inter-
atomic bonds between aggregates and binder, and it can be
used to quantify the work of adhesion between those materials.

Chemical composition along with other measurements indi-
cated that the high content of silica oxide approximates the
behavior of the iron slag (ACBFS) to that of a felsic rock, which
presents low adhesiveness to the binder. Parallel to this, iron
oxide seems important for the good adhesiveness of LD slag.

The observation from the small-scale surface characteristics
agreed well with the large scale observations from the mixture
tests: ASTM D3625 and AASHTO T283.

It was observed that the additives can affect moisture resis-
tance. In particular, HL and EP could improve moisture resis-
tance with ACBFS. This indicated the positive effects of CaO
and Fe2O3 on the asphalt mixture’s moisture damage
resistance.
Construction and Building Materials 264 (2020) 120685
Unconditioned Conditioned TSR
74% 80%
65% 63% 70%
58%
52% 60%
50%
TSR (%)
40%
30%
20%
10%
0%
HMA_ACBFS_HL HMA_ACBFS_FGD HMA_ACBFS_EP HMA_ACBFS_NA' HMA_LD
Fig. 11. Moisture induced damage results.

In general, it was shown that LD can potentially improve mois-
ture damage resistance of asphalt mixtures. However, other
performance tests need to be carried out to confirm the overall
effects of LD due to its expansive nature. ACBFS did not show
satisfactory adhesiveness to asphalt binder in this study. How-
ever, it can be engineered with proper antistripping agents, as
this study presented the effects of HL and EP.

This study showed that there is indeed much difference among
slags, and the differences affect bonding between slags and bin-
der due to surface characteristics. It is important to note that
properties of slags can vary due to the raw materials used and
the steel fabrication process. A careful application is thus
needed for practical purposes, and further studies to investigate
the case-specific challenges are necessary. The authors are cur-
rently working on follow-up studies and results will be pre-
sented when available.
CRediT authorship contribution statement
Bárbara Luiza Riz Moura: Conceptualization, Investigation,
Methodology, Validation, Formal analysis, Writing - original draft,
Writing - review & editing. Jamilla Emi Sudo Lutif Teixeira: Con-
ceptualization, Investigation, Methodology, Validation, Formal
analysis, Writing - original draft, Writing - review & editing, Fund-
ing acquisition. Renata Antoun Simão: Conceptualization,
Methodology, Validation, Formal analysis, Writing - original draft,
Writing - review & editing. Mahdieh Khedmati: Investigation, Val-
idation, Formal analysis, Writing - original draft, Writing - review &
editing. Yong-Rak Kim: Conceptualization, Validation, Writing -
original draft, Writing - review & editing. Patrício José Moreira
Pires: Conceptualization, Methodology, Validation, Writing - orig-
inal draft, Writing - review & editing, Funding acquisition.
Declaration of Competing Interest
The authors declare that they have no known competing finan-
cial interests or personal relationships that could have appeared
to influence the work reported in this paper.
Acknowledgements
This study was financed in part by ArcelorMittal Tubarão. The
second author also thanks the CAPES (Pos-Doctoral Program Grant
no. 88881.171157/2018-01) and CNPq (303845/2017-1) for the
scholarship grants. The authors also thank COPPE (UFRJ) and UFC
Federal Universities on the name of D.Sc. Thaisa Ferreira Macedo,
9
Bárbara Luiza Riz de Moura et al.
M.Sc. Mieka Arão and Ph.D. Verônica Castelo Branco, for their tech-
nical support on surface free energy and AIMS tests.
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