Construction and Building Materials 191 (2018) 1221–1229

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Construction and Building Materials

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Thermal and mechanical evaluations of asphalt emulsions and mixtures

for microsurfacing
Shuguang Hou a, Chen Chen b,⇑, Junhui Zhang c, Huajie Shen a, Fan Gu b
a
College of Transportation Science and Engineering, Nanjing Tech University, Nanjing, Jiangsu 210009, China
b
National Center for Asphalt Technology, Auburn University, 277 Technology Parkway, Auburn, AL 36830, United States
c
National Engineering, Laboratory of Highway Maintenance Technology, Changsha University of Science & Technology, Changsha, Hunan 410004, China

h i g h l i g h t s

2

There is a linear relationship between the D and storage stability.

DSC is used to evaluate the thermal stability of asphalt emulsions.

A linear relationship exists between |DH| and equilibration time of mortar viscosity.

Mixtures properties are dramatically affected by materials proportion and temperature.

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

Article history: In this study, four different emulsifiers were used to prepare asphalt emulsions. The effects of emulsifiers
Received 18 June 2018 on emulsion stability were investigated using the storage stability test, laser particle size analyzer (LPSA),
Received in revised form 13 October 2018 and differential scanning calorimetry (DSC). Furthermore, aggregate (0.15–0.3 mm) was mixed with
Accepted 15 October 2018
asphalt emulsions to obtain emulsified asphalt mortar. The Brookfield rotational viscometer (BRV) was
employed to determine the mortar viscosity and equilibration time. According to the laboratory results,
the storage stability of asphalt emulsions were in agreement with the corresponding particle size and
Keywords:
specific surface area. There was a linear relationship between the square of particle size and storage sta-
Microsurfacing
Asphalt emulsions
bility. In addition, the QA-emulsifier-prepared asphalt emulsion yielded the smallest particle size and
Thermal stability greatest specific surface area. This indicated the QA asphalt emulsion had the highest storage stability,
WTAT which was followed by AA, XA, and IM asphalt emulsion, respectively. The DSC results showed that
the enthalpy change displayed a linear relationship with the equilibration time. It was also demonstrated
that the XA asphalt emulsion had the highest thermal stability, which was followed by AA, IM, and QA
asphalt emulsion, respectively. This implied that there was no consistent ranking between storage stabil-
ity and thermal stability. Finally, the AA asphalt emulsion was selected to prepare microsurfacing mix-
tures. The performance tests results indicated that aggregate gradation, aggregate temperature,
additional water content, cement content and sand equivalent affected the mixing time and demulsifica-
tion time dramatically. The wet-track abrasion test (WTAT) results demonstrated that mixtures with
higher asphalt emulsion content and sand equivalent tended to have a higher early strength and a lower
moisture susceptibility.
Ó 2018 Elsevier Ltd. All rights reserved.

1. Introduction
Emulsions are defined as a dispersion of small liquid droplets
into another liquid. Standard asphalt emulsions are considered as
a dispersion of asphalt droplets into water, including 40–75%
asphalt, 0.1–2.5% emulsifier, and 25–60% water [1–3]. The applica-
⇑ Corresponding author.
E-mail addresses: houshuguang@njtech.edu.cn (S. Hou), czc0105@auburn.edu
(C. Chen), zjhseu@csust.edu.cn (J. Zhang), fzg0014@auburn.edu (F. Gu).
tion of asphalt emulsions began in the early 20th century, and 5–
10% asphalt used in pavements was the emulsified product [1,3].
Compared with asphalt binder, the viscosity of asphalt emulsions
were significantly lower, which allowed the application of asphalt
emulsion in lower temperatures [1]. Meanwhile, the commonly
recognized advantages of using asphalt emulsions also included
the lower energy requirements, environmental benefits, and safer
construction [1,3–4]. In the past decades, asphalt emulsions were
widely used in tack coat, chip-sealing, microsurfacing mixtures,

https://doi.org/10.1016/j.conbuildmat.2018.10.091
0950-0618/Ó 2018 Elsevier Ltd. All rights reserved.
1222 S. Hou et al. / Construction and Building Materials 191 (2018) 1221–1229
stabilization of galvanic sludge, cement mortar and concrete [1,4–
7].
Asphalt binder and emulsifier are the main components in
asphalt emulsions, which play an important role in the properties
of asphalt emulsions. It is well known that asphalt binder consists
of asphaltenes, resins, aromatics, and saturated compounds [8–9].
Al-Sabagh et al. [10] demonstrated that resins and aromatic com-
pounds could stabilize the colloidal structure of asphalt emulsions,
but asphaltenes and saturated compounds had negative effects on
the stability of asphalt emulsions. Similar findings were also
obtained by Jada and Salou [11] and Sleem-ur-Rahman and Dwi-
vedi [12]. To improve the thermal and mechanical properties of
asphalt emulsions, polymer-modified asphalt was utilized to
replace unmodified asphalt for using in chip seal, slurry seal, and
microsurfacing mixtures [1,3,13–14]. Emulsifiers are surfactants,
and the molecular formula contains both hydrophilic and
hydrophobic function groups. Based on the charge of primary func-
tion groups, emulsifiers are commonly classified into anionic,
cationic, and nonionic types [1]. Hydrophilic-lipophilic balance
(HLB) value is usually utilized to evaluate the hydrophilic or lipo-
philic degree of emulsifiers, which dramatically affects the stability
of asphalt emulsions [1,2,15].
Many experimental studies have been conducted to investigate
the stability of asphalt emulsions, and several test methods are
commonly used to assess the stability, including rheology tests,
particle size measurement, optical microscope, and traditional
storage stability test [1–2,15–19]. In general, asphalt emulsions
with smaller droplet size were expected to have higher stability
than those with greater size [17–18]. The existing studies mainly
focused on the storage stability of asphalt emulsions. However,
asphalt emulsions are typically thermodynamically unstable col-
loidal system, and temperature significantly affects their stability
[2,18,20]. Differential scanning calorimetry (DSC) is a thermo-
analytical technique which is used to characterize the thermal
transition of materials when temperature changes. Furthermore,
DSC was commonly used to characterize the stability and kinetics
of emulsions [21–23]. In this study, DSC was applied to investigate
the thermal stability and temperature susceptibility of asphalt
emulsions through measuring enthalpy change and critical tem-
peratures. In addition, the correlations between different stability
tests were also explored.
Microsurfacing is a thin asphalt emulsion mixture layer
designed for medium or heavy traffic application. This technique
is commonly used to improve pavement surface friction character-
istics and remove rutting [1,24]. In recent years, most of the studies
about microsurfacing mixtures focused on the construction and
mix design, particularly to the determination of optimal dosage
of asphalt emulsions [1,14,24–27]. Although microsurfacing pro-
vided excellent smoothness and friction performance in the field
[14,27], the understanding of the influence factors on mixture per-
formance was limited. Thus, this study investigated the influence
of different factors on the performances of microsurfacing mix-
tures, including mixing time, demulsification time and wet-track
abrasion.
In general, the objectives of this study include: (1) characterize
the thermal stability and temperature susceptibility of asphalt
emulsions, (2) explore the correlations between different stability
tests, and (3) investigate the influence of different factors on the
performances of microsurfacing mixtures properties.
2. Experimental design
The experimental plan was presented in Fig. 1, which included asphalt emulsion
and microsurfacing mixture. For asphalt emulsion, one virgin binder and four
different emulsifiers were utilized to prepare asphalt emulsions with a specific
procedure. The stability of asphalt emulsions was characterized with storage
stability test, laser particle size analyzer (LPSA), and DSC. In addition, aggregate
(0.15–0.30 mm) was mixed with asphalt emulsions to obtain emulsified asphalt
mortar, and the viscosity changes were recorded during the mixing process. Subse-
quently, microsurfacing mixtures were prepared with the selected asphalt emul-
sion, and mixing time test, demulsification time test, and WTAT were employed
to evaluate mixture properties. The effects of a variety of factors on the performance
of microsurfacing mixtures were investigated, which included aggregate tempera-
ture, aggregate gradation, sand equivalent, cement content, asphalt emulsion
content, and additional water content.
2.1. Materials
2.1.1. Virgin asphalt and emulsifiers
The 70 # virgin binder was used to prepare asphalt emulsion, and the properties
of virgin binder were determined in accordance with Standard Test Methods of
Bitumen and Bituminous Mixtures for Highway Engineering (JTG E20-2011) [28],
which were shown in Table 1.
Four different cationic emulsifiers were utilized to prepare asphalt emulsions,
including Quaternary ammomium salt (QA), Imidazolinium (IM), Acid amides
(AA), and Xylonamide (XA), and the physicochemical properties were presented
in Table 2.
2.1.2. Aggregate
Three aggregate gradations were utilized to prepare microsurfacing mixtures,
including coarse gradation, middle gradation, and fine gradation, which were
shown in Tables 3–5.
2.2. Preparation of asphalt emulsions
As for the manufacture procedure of asphalt emulsions, several important
parameters should be considered, including asphalt heating, dispersing phase
preparation, dispersed phase preparation, emulsifying equipment, and storage
[1,29]. In this study, asphalt emulsions were prepared with following three steps:
(1) disperse emulsifiers into warm water (60–65 °C) to produce soap solution, (2)
adjust the solution pH to 2 with acid (HCl), and (3) homogenize 60% virgin asphalt
(140 °C) and 40% soap solution (60–65 °C, pH = 2) through high-speed colloid
milling. The preparation process was shown in Fig. 2. The dosage of emulsifiers
was 2%.
2.3. Asphalt emulsion tests
2.3.1. Laser particle size analyzer
The asphalt emulsions were oil in water (O/W) emulsions, and the small asphalt
particles (droplets) distributed in water. In this study, particle size distribution of
emulsion droplets were characterized by the LDSA. The asphalt emulsions were
placed into a standard glassy cell, and the laser was applied to measure the particle
size with continuous stirring during the process. Median particle size (D50) and
specific surface area were determined after testing, and emulsions with a smaller
size and higher specific surface area had higher stability than those with a bigger
size and lower specific surface area.
2.3.2. Storage stability
According to JTG E20-2011 T 0655 [28], the 1-day storage stability of asphalt
emulsions was measured. The asphalt emulsions were placed into a standard exper-
imental tube, and the tube was settled for 24 h at an ambient temperature. The
storage stability was defined as the solid content difference between the upper
and lower layers, which is shown in Eq. (1). Asphalt emulsions with lower P value
are expected to be more stable than those with higher P value.
P ¼ SA  SB ð1Þ
where: P is storage stability, SA is the solid content of lower layer, and SB is the solid
content of upper layer.
2.3.3. Differential scanning calorimetry
DSC is a thermo-analytical technique which is used to characterize the thermal
transition of materials when temperature changes. DSC plot of heat flow per gram
of material versus temperature is generated, and the upward peaks and downward
peaks indicate exothermic and endothermic process, respectively. Meanwhile, the
area of peak represents change in enthalpy (DH). The stability of asphalt emulsions
is temperature-dependent, and the distribution of emulsion droplets is stable and
uniform at a low temperature. However, the emulsion droplets will absorb heat
with the increasing of temperature, resulting in particle agglomeration, known as
demulsification. Thus, DSC was performed to characterize the thermal transition
during the demulsification process, which indicated the thermal stability of asphalt
emulsions.
In this study, DSC was conducted between 60 and 100 °C through a DSC 204
differential thermal analyzer. For each asphalt emulsion, 5–10 mg samples were
tested with a 5 °C/min heating rate and 20 mol/min Nitrogen flow rate. The
enthalpy change (DH) and critical temperatures (Onset, Peak, and End tempera-
tures) can be determined with the output plot. The enthalpy change and critical
 S. Hou et al. / Construction and Building Materials 191 (2018) 1221–1229 1223

Fig. 1. Experimental plan.

Table 1 Table 4
Properties of 70# virgin binder. Coarse aggregate properties.

Test parameters Test results Method Test Parameters Test Results Criteria

25 °C Penetration (0.1 mm) 64 T 0604 Gsa 2.737 2.50

Penetration Index 1.39 – Toughness (%) 17.8 28
Softening Point (°C) 48.5 T 0606 Soundness (%) 8.5 12
Density (g/cm3) 1.027 T 0603 Flat or Elongated Particles (%) 9.1 15
10 °C Ductility (cm) 113.4 T 0605
15 °C Ductility (cm) >150 T 0605

Table 5
Fine aggregate properties.
Table 2
Test parameters Test results Criteria
Physicochemical properties of four cationic emulsifiers.
Gsa 2.740 2.50
AA XA QA IM
Sand Equivalence (%) 76 60
Active Content (%) 60  45 60 60 Soundness (>0.30 mm) (%) 9.6 12
pH (1% water solution) 7–9 10–12 7–9 7–9
Solubility (1:100 acid solution) 100% 100% 100% 100%

temperatures of samples were determined by the equipment software, and the
specific analyzed procedures were explained by Menczel and Prime [30]. In general,
the DSC peak includes descended and ascended parts, and each part can be divided
into slowly-changing and rapidly-changing phases. The corresponding tempera-
tures at the intersection of the fitted lines that characterize two phases represents
onset and end temperatures. In addition, the enthalpy change is defined as the inte-
grated peak area, as shown in Fig. 3.
In general, two complex peaks could be observed in the output plots, and both
peaks were downward, which indicated the endothermic process occurred. The first
peak shown around 0 °C indicated the ice melting caused by the water in the
asphalt emulsions. Meanwhile, the second peak represented the demulsification
of asphalt emulsions, and the DH and critical temperatures varied with different
emulsifiers. Asphalt emulsion with a higher absolute DH value ((|DH|)) required
more energy for demulsification process, which implied that asphalt emulsion
had a higher thermal stability. Furthermore, the onset temperature showed when
the demulsification started, and the O/W structures of asphalt emulsions were

Table 3
Aggregate gradation.

Passing Percentage (%)

9.5 mm 4.75 mm 2.36 mm 1.18 mm 0.6 mm 0.3 mm 0.15 mm 0.075 mm
Fine 100 90 70 50 34 25 18 15
Middle 100 80 58 39 27 19 13 10
Coarse 100 70 45 28 19 12 7 5
1224 S. Hou et al. / Construction and Building Materials 191 (2018) 1221–1229
Fig. 2. Preparation of asphalt emulsions.
1
End: 69.5 °C
0 changes between original specimen and worn specimen, shown as following.
-1
DSC (mW/mg)
-2 Complex Peak:
Onset: 39.3 °C H: -743.4 J/g
-3 Width: 27.8 °C
Height: 5.054
-4
-5
Peak: 63.6 °C
-6
-50 -30 -10 10 30 50 70 90
Temperature (°C)
Fig. 3. DSC output of asphalt emulsions with IM.
almost destroyed at peak temperature. This indicated that the demulsification
would terminate soon after peak temperature. Technically, asphalt emulsions with
lower critical temperatures were more susceptible to temperature.
2.4. Emulsified asphalt mortar viscosity test
The viscosity of asphalt emulsions is usually stable at a constant temperature,
but the demulsification will initiate and then accelerate when blended with aggre-
gate. Meanwhile, more and more asphalt droplets will be released with the acceler-
ation of demulsification, which resulted in the increase of viscosity. Thus, the
change in mortar viscosity is capable of quantifying the demulsification process
of asphalt emulsions.
In this study, 60% aggregate (0.15–0.3 mm) was mixed with 40% asphalt emul-
sions to obtain emulsified asphalt mortar, and the viscosity changes were measured
with BRV at an ambient temperature. Note that the rotational speed was 50 rpm,
and the mortar viscosity was recorded every minute.
2.5. Microsurfacing mixture tests
Asphalt emulsions with AA emulsifier and aggregate gradation of MS-3 were
selected to prepare microsurfacing mixtures.
2.5.1. Mixing time and demulsification time
Mixing and demulsification time are important indicators for pavement con-
struction, which indicate the operation time before demulsification. In this study,
the mixing and demulsification time of microsurfacing mixtures were measured
in accordance with JTG E20-T 0757 and T 0753 [28], respectively. The materials
of control microsurfacing mixtures used for determining the mixing and demulsifi-
cation time consisted of 85.5% aggregate, 8.5% asphalt emulsion prepared with 2%
AA emulsifier, and 6% additional water. Meanwhile, the aggregate temperature
and sand equivalent of control mixture were 20 °C and 80%, respectively, and the
aggregate gradation is the middle gradation shown in Table 3.
2.5.2. Wet-Track abrasion test
WTAT test is commonly used to evaluate the wearing qualities and long-term
moisture susceptibility of slurry or microsurfacing mixtures under wet conditions,
and to determine the minimum emulsified asphalt content of slurry or microsurfac-
ing mixtures. In this study, this test was conducted in accordance with JTG E20-T
0752 [28], and the test procedures are summarized: (1) prepare microsurfacing
mixtures with designed components, and place mixtures into the specified mold,
(2) after the removal of the mold, cure the specimen at 60 °C oven for 16 h, (3) Place
the cured specimen into the 25 °C water bath for 1 h, then setup the specimen
under the abrasion head to conduct the test. WTAT value was defined as the mass
WTAT ¼ ðma  mb Þ=A ð2Þ
where: WTAT is the abrasion value, g/m2; ma is the mass of original specimen; mb is
the mass of worn specimen; A is the abrasion area, m2 (0.034 m2).
The materials of control microsurfacing mixtures used for determining WTAT
value consisted of 84.7% aggregate, 8.5% asphalt emulsions prepared with 2% AA
emulsifier, 5.9% additional water, and 0.9% cement. Meanwhile, the aggregate tem-
perature and sand equivalent of control mixture were 20 °C and 80%, respectively,
and the aggregate gradation is the middle gradation shown in Table 3.
110 3. Test results and data analysis
This section investigates the effects of emulsifier types on the
properties of asphalt emulsions and mortar based on the results
of storage stability, LPSA, DSC, and changes in mortar viscosity.
According to the analysis of results, asphalt emulsion produced
with AA emulsifier was selected to prepare microsurfacing mix-
tures with middle gradation. Furthermore, the mixing time, demul-
sification time and WTAT were measured to evaluate the effects of
several influence factors, including aggregate gradation, sand
equivalent, additional water content, cement content, binder con-
tent, and aggregate temperature.
3.1. Effects of emulsifier types on the properties of asphalt emulsions
3.1.1. LPSA results
Fig. 4 presents the particle size and specific surface area results
of initial and 1-day stored asphalt emulsions produced with four
different emulsifiers. As shown in Fig. 4(a), for all four asphalt emul-
sions, the particle size of asphalt emulsions consistently increased
after 1-day storage, which indicated the agglomeration of asphalt
droplets occurred during the storage. The increase in particle size
for all four asphalt emulsions varied from 0.1 mm to 1.7 mm.
The specific surface area results were displayed in Fig. 4(b), and
initial asphalt emulsions showed greater specific surface area than
those emulsions after 1-day storage as expected, which also in
agreement with particle size results. The decrease in specific sur-
face area for all four asphalt emulsions varied from 3 m2/Kg to
49 m2/Kg. In general, asphalt emulsion prepared with QA emulsi-
fier yielded the smallest particle size and greatest specific surface
area, which indicated the highest storage stability, followed by
asphalt emulsions prepared with AA, XA, and IM, respectively.
3.1.2. Storage stability results
Fig. 5 presents the storage stability test results of four asphalt
emulsions produced with different emulsifiers. The storage stabil-
ity test results were in agreement with particle size results in Fig. 4
(a), asphalt emulsion prepared with QA yielded the smallest stor-
age stability value, which indicated the highest storage stability,
followed by asphalt emulsions prepared with AA, XA, and IM,
respectively.
 S. Hou et al. / Construction and Building Materials 191 (2018) 1221–1229 1225

Initial Size Size after 1 day During the storage stability test, the internal and external phase
12.0 are virgin asphalt and water, respectively. Additionally, the Dq, g,
9.7 and g are constant values when the test is performed at a constant
Particle Size (µm)

ambient temperature. Thus, the precipitation rate of asphalt dro-

9.0 8.0
plets is proportional to the square of particle size. The storage sta-
5.8 5.9 bility value (P) results were plotted against the corresponding
6.0 particle size square (D2), as shown in Fig. 6. Fig. 6 indicated that
3.9 4.1 3.8
3.3 there was a linear relationship between P and D2, and the regres-
3.0 sion coefficient (i.e., R2) was greater than 0.97. In addition, the
regression results complied with the Stoke’s law, which can be
0.0 used to evaluate or predict the storage stability of asphalt emul-
AA XA QA IM sions based on the corresponding particle size results.
Emulsifier Type
(a) 3.1.3. DSC results
As mentioned previously, two complex peaks could be observed
Initial Area Area after 1 day in the DSC output plots, caused by ice melting and demulsification
1200.0 of asphalt emulsions, respectively. The |DH| and critical tempera-
Specific Surface Area(m2/Kg)

tures results of second complex peak for four asphalt emulsions

918 were presented in Fig. 7. As shown in Fig. 7(a), asphalt emulsion
839 836 869
900.0
prepared with XA emulsifier yielded the greatest |DH|, which sug-
577 574 gested the highest thermal stability, followed by asphalt emulsions
600.0 prepared with emulsifier AA, IM, and QA. Fig. 7(b) presents the crit-
397
353 ical temperatures of all four asphalt emulsions, including onset,
300.0 peak, and end temperatures. For all four asphalt emulsions, the
temperature interval of demulsification was approximately 31 °C,
0.0 defined as the temperature difference between onset and end
AA XA QA IM point. In addition, the temperature difference between peak and
Emulsifier Type end is approximately 5 °C for all emulsions, which implied the
(b) demulsification process would terminate soon after peak tempera-
ture. Furthermore, asphalt emulsions with higher onset tempera-
Fig. 4. LPSA results of asphalt emulsions with different emulsifiers; (a) particle size, ture were expected to have higher peak and end temperatures.
(b) specific surface area. According to Fig. 7(b), asphalt emulsion prepared with AA yielded
the highest critical temperatures, which indicated lowest temper-
ature susceptibility, followed by asphalt emulsions prepared with
3.0
emulsifier XA, QA, and IM. In general, no consistent ranking was
2.35 found between storage stability and thermal stability for the four
Storage Stability (%)

asphalt emulsions, and this may be attributed to the differences

2.0 of temperature susceptibility.

1.08 3.2. Effects of emulsifier types on the mortar viscosity

1.0 0.76
0.62 Fig. 8 presents the viscosity results of mortar prepared with
singe-size aggregate and four different asphalt emulsions. As
shown in Fig. 8, the changes in mortar viscosity for four asphalt
0.0 emulsions generally contained increasing stage and steady stage,
AA XA QA IM
and the final mortar viscosities varied from 2000 to 2400 mPa.s.
Emulsifier Type
In addition, the equilibration time (t) was defined as the time
Fig. 5. Storage stability results of asphalt emulsions with different emulsifiers. needed to reach the maximum viscosity. The equilibration time
for different mortars varied from 11 to 17 min, which was in agree-

Technically, the storage stability test is a process in which

asphalt droplets coalesce and precipitate, thus, asphalt emulsions 3
with higher storage stability are expected to have less solid content
difference between upper layer and bottom layer. According to P = 0.03 (D2) + 0.21
Storage Stability (%)

Stoke’s law [31], the precipitation rate of a single droplet is affected R2 = 0.97
2
by particle size, viscosity of external continuous phase, and the
density difference between internal and external phase, which is
presented by Equation (3).
1
2r 2 Dq
t¼ g ð3Þ
9g

where: t is the precipitation rate; r is the particle size of droplet; 0

Dq is the density difference between internal and external phase; 0 10 20 30 40
D2 (µm2)
50 60 70
g is shear viscosity of external continuous phase; g is the gravita-
tion constant. Fig. 6. Correlations between storage stability and particle size.
1226 S. Hou et al. / Construction and Building Materials 191 (2018) 1221–1229

1,200 1100
1051

| H| = 65.18 (t) - 92.92

900
755.2 743.4 R² = 0.92
900
663.7

| H| (J/g)
| H| (J/g)

600

700
300

0 500
AA XA QA IM 10 12 14 16 18
Emulsifier Type Equilibration Time (min)
(a)
Fig. 9. Correlations between |DH| and equilibration time of mortar viscosity.

Onset Peak End

120 be attributed to the differences of temperature susceptibility. How-
Critical Temperatures (°C)

ever, both storage stability and thermal stability of asphalt emul-

88.4 92.8 sions prepared with AA emulsifier ranked second among all four
90
76 80.2 71.9 asphalt emulsions, and the corresponding temperature susceptibil-
67 69.5
60.5 63.6 ity was the lowest. Therefore, asphalt emulsions prepared with AA
60 51.9 emulsifier was selected to prepare microsurfacing mixtures.
40.1 39.3

30 3.3.1. Mixing time and demulsification time

Appropriate mixing and demulsification time play an important
0 role in the production and construction of microsurfacing mix-
AA XA QA IM tures. Meanwhile, they affect the mixture performance. Although
Emulsifier Type many influence factors could affect the mixing and demulsification
(b) time during construction, five factors were considered in this
study, including aggregate gradation, aggregate temperature, addi-
Fig. 7. DSC Results of Asphalt Emulsions with Different Emulsifiers; (a) |DH|, (b)
tional water content, cement content, and sand equivalent. Fig. 10
Critical Temperatures.
presents the effects of five influence factors on mixing and demul-
sification time.
3000
As shown in Fig. 10(a), the mixtures with coarser gradation had
longer mixing and demulsification time than those with finer gra-
dation. Both mixing time and demulsification time of mixtures
2500
with coarse gradation were approximately three times as long as
Viscosity (mPa.s)

those with fine gradation. Since the aggregates with finer gradation
2000 had greater specific surface area, they would result in higher and
Equilibration Time

quicker water absorption, which would further decrease the mix-

1500
1000
11
500
0 5 10
Fig. 8. Viscosity results of mortar with different emulsifiers.
ment with the results of |DH|. Furthermore, the equilibration times
were plotted versus the corresponding |DH|, as shown in Fig. 9.
Fig. 9 indicated that there was a linear relationship between t
and |DH|, and the regression coefficient (i.e., R2) was greater than
0.92. In general, asphalt emulsion with a higher |DH| was expected
to take a longer time to achieve steady mortar viscosity, and this
regression results could be applied to characterize the demulsifica-
tion of asphalt emulsion when mixed with aggregate.
3.3. Influence factors of the properties of microsurfacing mixtures
According to the results of asphalt emulsions tests and mortar
viscosity, no consistent ranking was found between storage stabil-
ity and thermal stability for the four asphalt emulsions, which may
AA ing time and demulsification time. Fig. 10(b) displays the effects
XA of aggregate temperature on mixing and demulsification time. As
QA expected, mixtures prepared with higher temperature aggregates
13 14 17 tended to yield shorter mixing and demulsification time, and the
IM
decrease of time was observed when temperature was greater than
15 20 25 30 35 25 °C. Higher aggregate temperatures may accelerate the evapora-
Time (min) tion of water, which explained the above trend.
As shown in Fig. 10(c) and (d), both mixing time and demulsifi-
cation time of mixtures were approximately positive linear
relationship with additional water content and sand equivalent,
respectively. The increasing additional water could protect the
O/W structure of emulsions and delay the demulsification process
through extending the water absorption of aggregate, which
implied longer mixing time and demulsification time. In addition,
the mixtures with lower sand equivalent tended to contain more
fine dust or claylike material, which could absorb more water
and accelerate the demulsification of asphalt emulsions [32].
Fig. 10(e) presents the mixing time and demulsification time
results of mixtures with varied cement content. Mixtures with
more cement, which is a super fine hydrophilic material, tended
to absorb more water, and then accelerate the demulsification,
resulting in longer demulsification time. Meanwhile, the effect of
cement content on mixing time was slightly complex, and the
mixing time of mixtures extended with the increase of cement
and achieved the maximum value with the 0.8% dosage. At the
 S. Hou et al. / Construction and Building Materials 191 (2018) 1221–1229 1227

Mixing Time Demulsification Time Mixing Time Demulsification Time

Demulsification Time (Miin)

300 80 250 40

Demulsification Time (Min)

Mixing Time (s)

Mixing Time (s)

200 30
200 60
150 20
100 40
100 10

0 20 50 0
Fine Middle Coarse 15 20 25 30 35 40 45 50
Aggregate Gradation Aggregate Temperature (°C)

(a) (b)

Mixing Time Demulsification Time Mixing Time Demulsification Time

Demulsification Time (Min)

400 60 250 40

Demulsification Time (Min)

Mixing Time (s)

Mixing Time (s)

300 200 30
40
150
200 20
100
20
100 50 10

0 0 0 0
3 4 5 6 7 8 9 50 60 70 80
Additional Water Content (%) Sand Equivalent (%)

(c) (d)
Mixing Time Demulsification Time
Demulsification Time (Min)
250 40
Mixing Time (s)

200 30

150 20

100 10

50 0
0 1 2 3 4 5
Cement Content (%)
(e)
Fig. 10. Influence factors of mixing time and demulsification time; (a) aggregate gradation, (b) aggregate temperature, (c) additional water content, (d) sand equivalent, (e)
cement content.

1300
1200

1000
WTAT(g/m2)

WTAT(g/m2)

900

600 700

300 400
6 7 8 9 10 11 50 60 70 80
Asphlat Emulsions Content (%) Sand Equivalent (%)

(a) (b)
Fig. 11. Influence factors of WTAT; (a) asphalt emulsions content, (b) sand equivalent.
1228 S. Hou et al. / Construction and Building Materials 191 (2018) 1221–1229
beginning, the use of moderate cement could absorb water and
produce cement paste film around aggregate, which can lubricate
the mixtures and extend the mixing time. However, excess cement
would absorb abundant water and result in the demulsification,
which indicated shorter mixing time.
In general, all influence factors discussed above have significant
influences on mixing time and demulsification time of microsur-
facing mixtures, which should be paid more attention during
construction.
3.3.2. WTAT results
WTAT was used to evaluate the early strength and moisture sus-
ceptibility of microsurfacing mixtures, and two influence factors
were discussed in this section, including asphalt emulsion content
and sand equivalent. Fig. 11 presents the effects of two influence fac-
tors on WTAT results, and WTAT showed a decreasing trend with the
increasing asphalt emulsion content and sand equivalent. As shown
in Fig. 11(a), WTAT decreased dramatically with the increasing
asphalt emulsion content when the dosage was less than 8.5%, then
the amplitude of variation decreased. Similar trend was observed in
Fig. 11(b), and the turning point of sand equivalent was around 70%.
As discussed previously, the mixtures with lower sand equivalent
tended to contain more fine dust or claylike material, which could
have a negative effect on the bonding between asphalt and aggre-
gate. Meanwhile, the increasing emulsion content contributed more
asphalt binder, resulting in better bonding between aggregate and
binder. Therefore, mixtures with higher asphalt emulsion content
and sand equivalent tended to have higher early strength and lower
moisture susceptibility, resulting in lower WTAT.
4. Conclusions and recommendations
In this study, four different cationic emulsifiers were utilized to
prepare asphalt emulsions, and their effects on the storage stability
and thermal stability were investigated. Meanwhile, the influences
of emulsifier types on the changes in mortar viscosity were inves-
tigated and their correlations with corresponding |DH| were deter-
mined. In addition, the effects of a variety of factors on the
performance of microsurfacing mixtures were evaluated, including
mixing time, demulsification time, and WTAT. According to the
results of this study, the following conclusion were obtained:

Fresh asphalt emulsions tended to have smaller particle size
and greater specific surface area. Asphalt emulsion prepared
with QA emulsifier yielded the smallest particle size and great-
est specific surface area, which indicated the highest storage
stability, followed by asphalt emulsions prepared with AA, XA,
and IM, respectively.

The storage stability test results were in agreement with parti-
cle size and specific surface area results, and there was a linear
relationship between square of particle size and storage stabil-
ity results.

Asphalt emulsion prepared with XA emulsifier yielded the high-
est thermal stability, and no consistent ranking was found
between storage stability and thermal stability.

The changes in mortar viscosity for four asphalt emulsions gen-
erally contained increasing stage and steady stage, and a linear
relationship between t and |DH| was observed.

All influence factors discussed above have significant effects on
mixing time and demulsification time of microsurfacing mix-
tures, including aggregate gradation, aggregate temperature,
additional water content, cement content, and sand equivalent.

Mixtures with higher asphalt emulsion content and sand equiv-
alent tended to have higher early strength and lower moisture
susceptibility.
The effects of emulsifier types on the asphalt emulsions proper-
ties were investigated based on one dosage level (2%), which was
recommended by the producer and commonly applied in the real
constructions. Thus, the effects of multiple dosage levels need to
be evaluated in the future research. In addition, only one virgin
binder type was used in this study, and there is a need to evaluate
the effects of emulsifier types on different binder types in the fur-
ther study. Note that the correlations between different test
parameters were obtained based on limited samples, and more test
results were required to determine the range of applicability.
Therefore, these correlations cannot be directly applied to other
asphalt emulsions until the determination of applicability range.
Furthermore, there is a need to evaluate the effects of more influ-
ence factors on WTAT and other mixture properties.
Conflicts of interest
The authors declare that they have no conflict of interests in this
study.
Acknowledgement
This work was primarily conducted in Nanjing Tech University
under the financial support by Natural Science Foundation of China
(51108237), and the remaining work was completed by the
authors at National Center for Asphalt Technology at Auburn
University and Changsha University of Science & Technology under
the financial support by Open Fund of National Engineering Labo-
ratory of Highway Maintenance Technology at Changsha Univer-
sity of Science & Technology (KFJ170104).
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