Construction and Building Materials 319 (2022) 126120

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Construction and Building Materials

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Evaluation on long-term performance of emulsified asphalt cold recycled

mixture incorporating fly ash by mechanistic and
microscopic characterization
Quan Li a, Chongzheng Zhu b, Henglong Zhang a, b, *, Shuai Zhang a, b
a
Hunan Provincial Engineering Research Center for Construction Solid Wastes Recycling, Hunan Yunzhong Recycling Technology Co., Ltd, Changsha 410205, China
b
Key Laboratory for Green & Advanced Civil Engineering Materials and Application Technology of Hunan Province, College of Civil Engineering, Hunan University,
Changsha 410082, China

A R T I C L E I N F O A B S T R A C T

Keywords: In this paper, the long-term performance of emulsified asphalt cold recycled mixture (CRME) incorporating fly
Emulsified asphalt cold recycled mixture ash was investigated. The dosages of fly ash included 0.75%, 1.5% and 3.0%, and the long-term service con­
Fly ash ditions of CRME were simulated by curing in an oven at 60 ◦ C for different ages. Mechanical performance of
Mechanical performance
CRME under different curing ages were obtained through indirect tensile strength (ITS), Marshall stability, low-
Microstructure
Long-term service conditions
temperature ITS and freeze-thaw ITS tests, and the microstructures were characterized by optical microscope, X-
ray diffraction (XRD) and environmental scanning electron microscopy (ESEM) tests. The results show that, as
the curing age increases, the ITS, flow value, and low-temperature indirect tensile strain of CRME with fly ash
increase first and then decrease, while the Marshall stability and freeze–thaw ITS ratio (TSR) always show a
gradual increase trend. By comparing the CRME with cement, the CRME with fly ash throughout the long-term
curing process exhibits the higher ITS and low-temperature anti-cracking performance and the lower high-
temperature stability and water stability. Optical microscope, XRD and ESEM analysis indicate that the disso­
lution of fly ash particles and the demulsification of asphalt emulsion particles occur simultaneously during the
curing ages. After a certain curing age, a dense structure composed of asphalt binders, dissolved and undissolved
fly ash particles is formed. Also, the fly ash replacing cement in CRME can effectively reduce the energy con­
sumption and carbon emission.

1. Introduction
Efficient recycling for reclaimed asphalt pavement (RAP) can not
only solve the serious adverse effect of RAP on environment, but also
save natural resources and costs of road repairing or rebuilding [1].
Emulsified asphalt cold recycling as one of recycling technologies has
lots of advantages of low energy consumption, less emissions of harmful
gases and high utilization rate of RAP materials [2,3]. But the low early
strength is mainly shortcoming which delays traffic opening [4].
Therefore, cement as conventional additive is usually added in the
emulsified asphalt cold recycled mixture (CRME) to enhance its early
strength [5–7]. Besides, some other additives (e.g. fly ash, lime and rice
husk ash) are also used for CRME [8–11].
Fly ash is the main waste products from thermal power plants and
made up primarily of Al2O3, SiO2, Fe2O3, CaO and so on, which is
deemed a major source of air pollution for a long time. Although there
were some studies on the influence of fly ash on cold recycled mixture
without emulsified asphalt [12–14], only a few researches were con­
ducted on the effect of fly ash on CRME. Behnood et al found that adding
fly ash could improve the indirect tensile strength (ITS) and Marshall
stability (MS) of CRME, while reduce the permanent deformation [11].
Modarres and Ayar also pointed out that coal waste ash (CWA, similar to
type F or N fly ash) could augment the MS, ITS and resilient modulus of
CRME. Besides, lime could act as a complement of CWA to further
enhance the mechanical properties and water stability of CRME [8].
They also found that CWA could increase fatigue life of CRME. More­
over, the CRME with CWA had longer fatigue life at higher strain levels
of 200με compared with ordinary Portland cement [15]. Furthermore,

* Corresponding author at: Key Laboratory for Green & Advanced Civil Engineering Materials and Application Technology of Hunan Province, College of Civil
Engineering, Hunan University, Changsha 410082, China.
E-mail address: hlzhang@hnu.edu.cn (H. Zhang).

https://doi.org/10.1016/j.conbuildmat.2021.126120
Received 22 October 2021; Received in revised form 13 December 2021; Accepted 14 December 2021
Available online 27 December 2021
0950-0618/© 2021 Elsevier Ltd. All rights reserved.
Q. Li et al. Construction and Building Materials 319 (2022) 126120

they using field emission scanning electron microscopy demonstrated Table 1

that a combination of coal waste ash and cement kiln dust could change Properties of asphalt emulsion.
the structure of CRME from a porous and discontinuous matrix to an Properties Asphalt emulsion Standards
integrated structure [16].
Emulsifier content (%) 2.5 –
However, on the one hand, the interaction mechanism between fly Residue by distillation (%) 63.8 JTG E20-2011T0651
ash and emulsified asphalt in CRME is not clear at present. On the other Storage stability at 1d (%) 0.7 JTG E20-2011T0655
hand, the influence of fly ash on long-term performance is not also Storage stability at 5ds (%) 3.7 JTG E20-2011T0655
involved, and the feasibility of fly ash replacing cement in CRME under Penetration of residue, 25 ℃ (0.1 mm) 59 JTG E20-2011T0604
Ductility of residue, 15 ℃ (cm) 63.3 JTG E20-2011T0605
long-term service condition needs to be discussed. Therefore, the Weight specific surface area (m2/kg) 2118.0 –
research on these two aspects is vital to broaden the application of fly D10 (μm) 1.82 –
ash in CRME, as well as reduce carbon emissions from cement produc­ D50 (μm) 3.73 –
tion [17]. D90 (μm) 6.65 –
Besides, the curing process, including curing temperature, curing
time and curing humidity, has important influence on the performance
Table 3 and Fig. 3, it can be determined that the particle size of fly ash A
of CRME [3,6]. The increased curing temperature can accelerate the
is bigger than that of fly ash B.
hydration rate of cement and the demulsification rate of asphalt emul­
sion, thus the early strength of CRME is enhanced. As the curing time
2.1.3. Aggregates
increase, the moisture loss and strength of CRME is also enhanced. Refer
Reclaimed asphalt pavement (RAP) materials included RAP-1
to the research of Peter E. Sebaaly et al, asphalt emulsion cold in-place
(0–4.75 mm), RAP-2 (4.75–9.5 mm), RAP-3 (9.5–16 mm) and RAP-4
recycled mixtures could be evaluated at three curing stages: initial
(16–26.5 mm). Technical indicators of old asphalt recovered in RAP
curing stage (25 ◦ C for 15 h in the mold), final curing stage (60 ◦ C for 3
were as follows: penetration (25℃) 3.6 mm, softening point 55.3℃,
days after extruding out of the mold) and long-term curing stage (60 ◦ C
ductility (15℃) 9.2 cm. The interface friction among aggregates was
for 30 days after extruding out of the mold) [18]. Therefore, in this
optimized by introducing virgin coarse limestone aggregate (9.5–19
study, specimens were cured in an oven at 60 ◦ C for different ages to
mm). Mineral filler was obtained through grinding and processing
simulate the long-term service conditions of CRME, and the longest age
limestone. Their gradations were presented in Table 4.
was 30 days.
This research investigated the long-term performance of CRME
2.2. Mixture design
incorporating fly ash, and discussed the interaction mechanism between
fly ash and emulsified asphalt. The dosages of fly ash included 0.75%,
Initially, based on our previous research [19,20], the gradation of
1.5% and 3.0% by weight of RAP, virgin aggregate and mineral filler.
CRME was determined according to a regulated grading range, as listed
Mechanical performance of CRME under different curing ages were
in Table 5. The corresponding mix formula was as follows: RAP-1 (35%),
measured through ITS, MS, low-temperature ITS and freeze–thaw ITS
RAP-2 (24%), RAP-3 (18%), RAP-4 (7%), virgin aggregate (12%),
tests. Besides, the microstructures were characterized by optical mi­
mineral filler (4%).
croscope, X-ray diffraction (XRD) and environmental scanning electron
Next, preparation process of CRME are as follows: Firstly, both the
microscopy (ESEM) tests. Finally, economical, energy consumption and
coarse virgin aggregate, RAP-3 and RAP-4 were put in mixing pot, 1/
carbon emission assessments on fly ash replacing cement in CRME were
5–1/4 water (for wetting these aggregates) and 1/3 asphalt emulsion
conducted.
were also added in mixing pot, then the mixture was mixed for 60 s;
After that, the remaining water was used to wet RAP-1 and RAP-2 by
2. Materials and experiments
hand mixing, then this wetting fine RAP aggregate and the remaining
asphalt emulsion were also put in mixing pot and mixed for 60 s; Finally,
2.1. Materials
both cement and mineral filler were added in mixing pot and mixed for
60 s, the obtained mixture was CRME.
2.1.1. Asphalt emulsion
Finally, the mix design of CRME were determined by the modified
Cationic slow-setting emulsified asphalt was prepared with virgin
Marshall design method in the light of the Chinese specification (JTG/T
asphalt 70# and cationic emulsifier by employing a colloidal mill. The
5521-2019). The optimum asphalt emulsion content (OEC) and the
preparation process was as follows. Firstly, the water solution was
optimum water content (OWC) were determined to 4.60 % and 3.83%
configured through mixing water, cationic emulsifier and hydrochloric
by weight of virgin aggregate, RAP and mineral filler, respectively.
acid (HCl) with a glass rod. The weights of water, cationic emulsifier and
In addition, the selected contents of fly ash (A or B) included 0.75%,
HCl were 204 g, 15 g and 3 g, respectively. The HCl solution with 36%–
1.5% and 3.0% by weight of virgin aggregate, RAP and mineral filler.
38% concentration was used to adjust the pH value of water solution to
For comparison, the CRME with 1.5% cement or without additives was
2. Subsequently, the water solution was added in the colloidal mill and
also prepared.
its temperature was controlled at 60 ± 5℃. Finally, the colloid mill
began to work, and the molten asphalt (378 g) under 140 ± 5℃ was also
2.3. Air void test
added in the colloidal mill. After about 1.5 min, the prepared emulsified
asphalt was obtained. The basic properties of emulsified asphalt were
For calculating the air void of CRME specimens, the bulk densities
listed in Table 1.
(ρb) and the theoretical maximum densities (ρm) of specimens were
obtained in the light of saturated surface dry method (JTG E20-2011T
2.1.2. Additives
0705) and vacuum method (JTG E20-2011T 0711), respectively, as
Two types of fly ash (A and B) were adopted in this research, and P.O
seen in formula (1).
42.5 Portland cement (PC) as a conventional additive was used for
comparison with the fly ashes. The chemical composition of cement and Air void =
ρm − ρb
× 100% (1)
fly ashes were tested by X-ray fluorescence spectrometer (XRF), as ρm
illustrated in Table 2. The particle sizes of cement and fly ashes were
obtained by laser diffraction particle size analyzer, as listed in Table 3. 2.4. Indirect tensile strength (ITS) test
The micro morphology of fly ashes was characterized by environmental
scanning electron microscopy (ESEM), as shown in Fig. 1. According to ITS test was conducted using Marshall specimen. The molding

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Q. Li et al. Construction and Building Materials 319 (2022) 126120

Table 2
Chemical composition of cement and fly ashes.
Composition SiO2 Fe2O3 Al2O3 SO3 MgO CaO Na2O K2 O TiO2

Percentage (wt%) Fly ash A 47.58 4.77 38.72 0.92 0.47 2.90 0.51 0.97 1.91
Fly ash B 49.10 4.31 37.79 0.92 0.61 2.85 0.69 0.92 1.61
Cement 18.52 4.00 4.01 3.24 1.70 66.41 0.29 0.55 0.39

2.6. Low-temperature ITS test

Table 3
Particle size test results of cement and fly ashes.
The low-temperature ITS test of CRME specimens was conducted
Physical properties Fly ash A Fly ash B Cement according to the Chinese specification (JTG E20-2011T 0716). Four
Weight specific surface area (m2/kg) 497.2 984.9 648.9 specimens for parallel test were used. Before testing, the specimens were
D10 (μm) 5.97 3.00 4.65 immersed in a − 10 ◦ C temperature ethyl alcohol bath for 1.5 h. The test
D50 (μm) 18.75 9.08 13.62 temperature was − 10 ± 0.5 ◦ C and the loading rate was 1 mm/min.
D90 (μm) 44.84 19.18 29.10

2.7. Freeze-thaw ITS test

procedure of Marshall specimen was as follows: Firstly, the CRMEs after
mixing were added in Marshall mould and compacted 50 times on both
The freeze–thaw ITS test of CRME specimens was conducted ac­
sides using Marshall compaction apparatus, then the sample together
cording to the Chinese specification (JTG E20-2011 T 0729). Eight
with mould was side placed in a constant temperature oven at 60 ◦ C, and
specimens for conducting the freeze–thaw ITS test was divided into
the curing time was generally not less than 40 h; After that, the specimen
group 1 and group 2. The specimens in both groups were immersed in a
was taken out of the oven and immediately compacted 25 times on both
water bath at 25 ◦ C for 2 h before ITS test. Besides, the specimens of
sides; Finally, the specimen together with mould was placed on the
group 2 were firstly treated by vacuum saturation with 97.3–98.7 kPa
ground and cooled at room temperature for at least 12 h, and then
for 15 min, and put in plastic bags together with 10 mL water. Subse­
demolded. The dimension and height of Marshall specimen were 101.6
quently, the bags were placed in a − 18 ◦ C refrigerator for 16 h. Finally,
± 0.2 mm and 63.5 ± 1.3 mm, respectively.
the specimens were removed from the bags and placed in a 60 ◦ C water
The indirect tensile strength (ITS) of CRME specimens was obtained
bath for 24 h. The specimens before and after freeze–thaw were tested
in the light of the Chinese specification (JTG E20-2011 T 0716). Four
under 25 ◦ C temperature and 50 mm/min loading rate. The ITS (RT)
specimens for parallel test were used. Before testing, the specimens were
ratio of group 2 to group 1, TSR (%), was calculated in accordance with
immersed in a 15 ◦ C temperature water bath for 2 h. The test temper­
the formula (3).
ature was 15 ± 0.5 ◦ C and the loading rate was 50 mm/min. ITS was
calculated in accordance with formula (2). TSR =
RT2
× 100% (3)
RT1
ITS = 0.006287PT /h (2)
where, RT2 and RT1 represent the ITS of the specimen in group 2 (MPa)
where, PT and h signify the tested peak load (N) and the specimen height and the ITS of the sample in group 1 (MPa), respectively.
(mm), separately.

2.8. Simulation method of long-term service conditions of CRME

2.5. Marshall stability test
The Marshall stability test of CRME specimens was conducted ac­
cording to the Chinese specification (JTG E20-2011T 0709). Four
specimens for parallel test were used. Before testing, the specimens were
immersed in a 60 ◦ C temperature water bath for 40 min. The test tem­
perature was 60 ± 1 ◦ C and the loading rate was 50 mm/min.
For simulating the mechanical performance evolution of CRME
under long-term service conditions, the research of Peter E. Sebaaly et al
was referenced [18]. Specimens were extruded out of the mold and
cured in an oven at 60 ◦ C for 0, 3, 7,10, 20 and 30 days. After different
curing ages, the specimens were removed from oven and cooled at
ambient temperature for the next tests.

Fig. 1. ESEM images of fly ashes a) Fly ash A, b) Fly ash B.

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Q. Li et al. Construction and Building Materials 319 (2022) 126120

Fig. 2. Dynamic microscopic images of fly ash B in AE (1000 times magnification) under 25℃. a) 2 min; b) 10 min; c) 20 min; d) 45 min.

Fig. 3. Dynamic microscopic images of fly ash B in AE (400 times magnification) under 60℃. a) 2 min; b) 10 min; c) 20 min; d) 45 min.

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Q. Li et al. Construction and Building Materials 319 (2022) 126120

Table 4 latter tend to be gray or grayish-white.

Gradations of RAP materials, virgin aggregate and mineral filler. Fig. 2 shows that the dynamic microscopic images (1000 times
Sieve RAP- RAP- RAP- RAP- Virgin Mineral magnification) of fly ash in AE under 25℃ from 2 min to 45 min. As seen
(mm) 1 2 3 4 aggregate filler in Fig. 2a (2 min) to Fig. 2c (20 min), some AE particles are gradually
26.50 100.0 100.0 100.0 100.0 100.0 100.0 adsorbed on the surface of fly ash particles. After 45 min (as shown in
19.00 100.0 100.0 100.0 27.9 59.5 100.0 Fig. 2d), on the one hand the shell of fly ash particles is dissolved and
16.00 100.0 100.0 100.0 2.4 31.1 100.0 fuses each other, on the other hand these adsorbed AE particles break
13.20 100.0 100.0 78.3 0.3 11.0 100.0 and then adhere to the surface of fly ash particles. Some explanations are
9.50 100.0 100.0 5.0 0.3 0.3 100.0
4.75 100.0 8.6 0.2 0.3 0.3 100.0
as follows: In the preparation process of AE, hydrochloric acid (HCl) is
2.36 51.9 0.4 0.2 0.3 0.3 100.0 added for adjusting the pH value of water solution to 2, and it is
1.18 23.4 0.4 0.2 0.3 0.3 100.0 determined by short range pH test strips that pH value of the prepared
0.60 8.1 0.4 0.2 0.3 0.3 100.0 AE is 2; Thus, the HCl in AE can react with the substances (e.g. CaO,
0.30 1.5 0.4 0.2 0.3 0.3 100.0
Al2O3, Fe2O3) on the surface of fly ash particles, which can result in a
0.15 0.9 0.4 0.2 0.3 0.3 100.0
0.075 0.1 0.1 0.0 0.0 0.0 82.1 rough surface of fly ash particles and then enhance their adsorbability
[21–23]. Besides, as the HCl is reacted, the AE particles become insta­
bility and easier to break. For cationic emulsifier, the higher H+ con­
centration in water solution can enhance the protonation degree of
Table 5
active (hydrophilic) groups in emulsifier molecules, which in turn leads
Gradation of CRME.
to the high emulsifying activity and improves the dispersion effect of
Sieve (mm) CRME Upper limit Lower limit
asphalt. However, as the HCl is reacted, the H+ concentration reduces,
26.50 100.0 100.0 100.0 which can decrease the protonation degree of hydrophilic groups in
19.00 90.1 100.0 90.0 emulsifier molecules. Then the activity of emulsifier declines and the
16.00 84.9 94.0 80.0
emulsifying effect of emulsifier becomes worse.
13.20 78.4 82.0 64.0
9.50 63.9 74.0 50.0 As shown in Fig. 3, the similar phenomenon can be found when the
4.75 41.2 56.0 30.0 tested temperature is 60℃ and the magnification is 400 times. In Fig. 3a
2.36 22.3 43.0 15.0 (2 min) and Fig. 3b (10 min), it can be observed that some AE particles
1.18 12.4 32.0 10.0
are adsorbed on the surface of fly ash particles. After 20 min (as seen in
0.60 7.0 22.0 6.0
0.30 4.7 15.0 3.0 Fig. 3c), demulsification occurs in nearly all the adsorbed AE particles,
0.15 4.5 11.0 2.0 in the meantime, dissolution happens in partially of fly ash shell, and
0.075 3.4 5.0 1.0 then a structure composed of asphalt binder, dissolved and undissolved
fly ash is formed. As shown in Fig. 3d, from 20 min to 45 min, the
microscopic image is nearly unchanged. It indicates that the elevated
2.9. Optical microscope test
temperature (from 25℃ to 60℃) accelerates the evolution of AE and fly
ash.
The transillumination mode of a fluorescence microscope (DYF-
680LED, Shanghai Dianying Optical Instrument Co., LTD) was used to
observe the dynamic behavior of asphalt emulsion or fly ash in asphalt 3.2. X-ray diffraction (XRD) analysis
emulsion. The magnification was 400 times.
The XRD results of the fly ash B and the mixtures containing AE,
2.10. X-ray diffraction (XRD) test mineral filler and fly ash B under different curing ages (1 day and 2 days)
are illustrated in Fig. 4. The peaks at 35.3◦ and 40.9◦ in the diffracto­
XRD test was performed using an automated multipurpose X-ray grams for all samples represent the hematite (Fe2O3) and the mullite
diffractometer (Rigaku SmartLab SE) to examine the change of crystal­ ((Al2O3)1.136(SiO2)0.728 [24]. It can be found that, as the curing ages
line structures of the mixtures (asphalt emulsion-mineral filler or asphalt increase (from 1 day to 2 days), the intensity of the two peaks becomes
emulsion-mineral filler-fly ash) after different curing conditions. In the relatively weaker. This might be attributed to that some hematites and
preparation process of the mixtures sample, the ratio of asphalt emul­ mullites are decreasing with increasing curing ages. Considering that
sion, fly ash, mineral filler and water is 3.1:1:2.7:2.6 is adopted, which is
the same as their ratio in the CRME with 1.5% fly ash. The test was
performed with 2θ value of 10◦ ~80◦ , a step size of 0.004◦ , and a scan­
ning speed of 5◦ /min.

2.11. Environmental scanning electron microscopy (ESEM) test

Microstructure of the CRME with 1.5% fly ash under different curing
ages was characterized with a model Quanta 200 ESEM from FEI Cor­
poration (America). In this test, a smooth surface of the specimens was
shaped firstly. Subsequently, the smooth surface was coated with gold.

3. Results and discussion

3.1. Optical microscope analysis

Dynamic microscopic images of fly ash (B) in asphalt emulsion (AE)

were illustrated in Fig. 2 and Fig. 3, and the weight ratio of water, AE
and fly ash is 40:1:1. Although both AE particles and fly ash particles are
spherical, the former tend to be tan under optical microscope, while the Fig. 4. XRD patterns of the mixtures containing AE, mineral filler and fly ash B.

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Q. Li et al. Construction and Building Materials 319 (2022) 126120

hematites are mainly distributed in the shell of fly ash particle [21], the
dissolution of fly ash particle shell occurs. This result is consistent with
the optical microscope analysis.
3.3. Environmental scanning electron microscopy (ESEM) analysis
Fig. 5 presents the microstructure of the CRME with 1.5% fly ash B
under different curing ages. As illustrated in Fig. 5 a) and b), after 1 day
curing, although part of fly ash particles dissolves and part of AE breaks,
a lot of undissolved particles are retained. The structure composed by

Fig. 5. ESEM images of the CRME with 1.5% fly ash B under different curing ages. a) and b) 1 day, c) and d) 2 days, e) and f) 5 days, g) and h) 30 days.

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Q. Li et al. Construction and Building Materials 319 (2022) 126120

asphalt binders, dissolved and undissolved fly ash particles is loosely

bound. After 2 days curing (as shown in Fig. 5 c) and d)), as the disso­
lution of fly ash particles and the demulsification of AE particles goes on,
the structure becomes relatively dense. Furthermore, after 5 days curing
(as shown in Fig. 5 e) and f)), the number of asphalt binders further
increases, and a continuous and dense structure is formed by the asphalt
binders, dissolved and undissolved fly ash particles. After 30 days curing
(as seen in Fig. 5 g) and h)), there is no obvious difference compared
with 5 days curing. It suggests that, for the CRME with 1.5% fly ash B,
the change in asphalt emulsion and fly ash is not intense.

3.4. Air void

Fig. 6 shows that the influence of fly ash types (A and B) and dosages
(0.75%, 1.5% and 3%) on air void of CRME. In Fig. 6, C + AE, FA + AE
and FB + AE represent the CRMEs with cement, fly ash A and fly ash B,
separately. It can be observed that, with the dosages of fly ash
increasing, the air void of CRME decreases. Additionally, except for the
CRME with 0.75% fly ash A, other CRMEs with fly ash show the lower air
void value than the CRME with 1.5% cement. It means that two types fly
ash has the better fill effect than cement. Moreover, compare with fly ash
A, the CRME with fly ash B shows the lower air void under same dosages,
which is attributed to the smaller particle size for fly ash B [25].
Air void of CRME with 1.5% fly ash B or cement during long-term
curing is shown in Fig. 7. For fly ash B and cement, as the curing time
goes on, the air void of CRME first increases and then decreases. These
reasons are as follows: Under 60℃ high temperature curing early stage,
due to the evaporation of water, most of air void is left; after a extent of
time, the water can be evaporated becomes more and more scarce, but
the asphalt binder from breaking of emulsified asphalt become flow
state under 60℃, which can fill in some air void; at the same time, there
is one possible reason that some RAP particles consisted of smaller RAP
particles or even old asphalt mortar can gradually disperse due to the
long-term effect of 60℃ high temperature, as a result the air void in
CRME begins to decrease.
By comparing cement and fly ash B, the CRME with cement has the
highest air void when the curing time is 3 days, while the highest air
void of CRME with fly ash B appears when the curing time is 7 days. On
the one hand, the cement can react with water, and the volume of hy­
drated products is smaller than the total volume of the reacted water and
cement. On the other hand, the initial air void of CRME with cement is
bigger than CRME with fly ash B, thus the evaporated speed of water in
CRME with cement is faster.
Fig. 7. Air void of CRME with fly ash B or cement during long-term curing.
3.5. Indirect tensile strength
Indirect tensile strength (ITS) of CRMEs with fly ash A and B under
different curing ages are presented in Fig. 8 and Fig. 9, respectively. As
illustrated in Fig. 8, when the curing age doesn’t exceed 20 days, the ITS
of all CRMEs increases as the curing age increases. For the CRME
without additive (AE), the increase in ITS is mainly ascribed to loss of
water and demulsification of asphalt emulsion, in turn, more and more
asphalt binders are involved in adhesion between aggregates. In terms of
the CRME with cement, the enhancement in ITS is caused by the
demulsification of asphalt emulsion, the hydration of cement and the
mutual effect between them [20]. With regard to the CRME with fly ash,
based on the optical microscope, XRD and ESEM analysis, the increase in
ITS should be relevant to the demulsification of asphalt emulsion, the
dissolution of fly ash shell and the mutual effect between them. How­
ever, except for the CRME without additive (AE), a decrease occurs in
the CRMEs with cement or fly ash A when the curing age exceeds 20
days. Refer to our previous research [20], the temperature 60℃ could
cause aging of asphalt binder after 10 days curing to some extent.
Meanwhile, as we know, aging can make asphalt binder hard and brittle
[26–28]. Although aging has a negative effect on the cohesion of asphalt
binder, it can increase the adhesion between asphalt and aggregate
[29,30]. Thus, the following hypothesis is provided: the aging degree of
asphalt binder after a certain day curing has no adverse influence on the
ITS and even enhances the ITS of CRME without additive due to the

Fig. 8. Indirect tensile strength of CRMEs with fly ash A during long-
Fig. 6. Air void of CRMEs with cement or fly ash. term curing.

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Q. Li et al.
Fig. 9. Indirect tensile strength of CRMEs with fly ash B during long-
term curing.
increased adhesion; however, this aging degree might weak the struc­
ture made up of hydration products and asphalt binders or the structure
composed by dissolved fly ashes, undissolved fly ashes and asphalt
binders because of the decreased cohesion, and then cause the decrease
in ITS of CRME with cement or fly ash. But this hypothesis needs to be
demonstrated in the further research.
As illustrated in Fig. 8 and Fig. 9, regardless of the types, the ITS of
CRME with fly ash shows an obvious augment when the dosages increase
from 0.75% to 1.5%. However, the higher dosages (3%) don’t further
enhance the ITS and even show unfavorable effect to some extent. It
indicates that a proper fly ash dosage is importance in order to enhance
ITS of CRME. In this research, 1.5% dosages are recommended irre­
spectively of fly ash types. Moreover, compare with fly ash A, the CRME
with fly ash B has the higher ITS under same dosages, which is attributed
to the better fill effect of fly ash B [25,31].
Besides, as seen in Fig. 8 and Fig. 9, it can be found that the CRME
with 1.5% fly ash A or B shows higher ITS value than the CRME with
1.5% cement under same curing ages. For fly ash A and B, the biggest
increase amplitudes are 13% (after 10 days curing) and 43% (after 7
days curing), respectively. The analysis is as follows: the cement or its
hydration products can act as “reinforced function” in CRME; for the fly
ash B, the dissolved or undissolved particles also can play “reinforced
function” role in CRME at lower temperature (e.g. 15℃); moreover, the
CRME with fly ash is denser than the CRME with cement.
3.6. Marshall stability
High temperature stability of CRME is evaluated using Marshall
stability test at 60℃, the test results are shown in Fig. 10. As seen in
Fig. 10. Marshall stability test results of CRME with fly ash B or cement during long-term curing a) Marshall stability, b) Flow value.
8
Construction and Building Materials 319 (2022) 126120
Fig. 10a), as the curing time increases, the Marshall stability value of
CRME with fly ash also increase, indicating the increased high-
temperature bearing capacity. But the flow value of CRME with fly
ash first increases and then decreases, which is supposed to be related
with the change in air void. In addition, the Marshall stability values of
CRME with fly ash B are obviously lower than those of CRME with
cement during the whole long-term curing, which indicates that CRME
with fly ash has lower high-temperature bearing capacity. It can be
explained as follows: for the CRME with cement, the cement hydrated
products and asphalt binder can form partially continuous network [32],
under 60℃ high temperature, the continuous hydrated products can
effectively retard the movement of asphalt binder; for the CRME with fly
ash B, although the fly ash shows better fill effect and the fly ash par­
ticles or its dissolved substances has “reinforced function” in CRME
under lower temperature (e.g. 15℃), under high temperature (e.g.
60℃) the asphalt binder becomes soft and the separated fly ash particles
can not keep the “reinforced function”, thus the movement of asphalt
binder can not be restricted.
3.7. Low-temperature anti-cracking performance
The low-temperature anti-cracking performance of CRME is evalu­
ated by indirect tensile test at − 10℃, the results are shown in Fig. 11. As
seen in Fig. 11a), it can be found that, with the increasing of curing time,
the ITS of CRME with fly ash B or cement shows the increasing trend.
Moreover, during the whole curing, the CRME with fly ash B has the
higher ITS than the CRME with cement.
In addition, as seen in Fig. 11b), for the CRME with cement, the in­
direct tensile strain first decreases and then (after 10 days) keeps
essentially unchanged. This is because hydration products of cement and
demulsification of asphalt emulsion occur in the first 10 days, which
increased the tensile strength of CRME at low temperatures. However,
the stiffness of cement hydration products is much higher than that of
asphalt binders, the increase in hydration products weakens the ability
of CRME to resist low-temperature deformation; and during the curing
process, a large number of voids are left in CRME due to the evaporation
of water, which also has an adverse effect on the low temperature anti-
cracking performance. For the CRME with fly ash B, its indirect tensile
strain first increases and then decreases, the reason is the same with the
change in ITS under 15℃. Besides, in the whole curing process, the
CRME with fly ash B shows the higher indirect tensile strain than the
CRME with cement, which is attributed the lower air void for the former.
3.8. Water stability
The water stability of CRME is evaluated using freeze–thaw indirect
tensile test, and the results are shown in Fig. 12. As seen in Fig. 12,
during the whole curing, the tensile strength ratio (TSR) of CRME with
fly ash B stays increasing trend, while that of CRME with cement climb
Q. Li et al. Construction and Building Materials 319 (2022) 126120

Fig. 11. Low-temperature ITS test results of CRME with fly ash B or cement during long-term curing a) Indirect tensile strength, b) Indirect tensile strain.

Table 6
Economic analysis of the considered cold recycling mixtures.
Material Unit Content / CRME with CRME
price / (%) cement/ with fly
(¥/t) (¥/t) ash/ (¥/t)

Raw materials Asphalt 4479 4.6 285.7 282.5

cost / (¥ emulsion
(CNY) / t) Portland 410 1.5
cement
Fly ash 200 1.5
RAP 62 84
Natural 120 12
aggregate
Mineral 170 4
filler
Water 5 3.8
Mixing cost / Labor cost 0.56 0.56
(¥/t) Machinery cost 17.85 17.85
Total cost / (¥/t) 304.11 300.91

Fig. 12. Freeze-thaw ITS test results of CRME with fly ash B or cement during
long-term curing.
up and then decline. Additionally, the latter shows the obvious higher
TSR than the former.
For CRME with cement, cement hydration can produce hydrated
calcium silicate gel (C-S-H) in the interface area of asphalt mortar and
aggregate to increase the adhesion, and the cement hydration can also
consume tiny water droplets in the interface area. Both them will be
conducive to improve the water stability of the cold recycled mixture.
But for the CRME with fly ash B, it does not have the above-mentioned
characteristics of cement, and the asphalt emulsion is not completely
demulsified at early stage of curing, so it exhibits poor water stability.
3.9. Economic, energy consumption and carbon emission assessments
The economic analysis (including raw materials cost and mixing
cost) of the CRME with cement or fly ash is illustrated in Table 6 [33]. As
seen in Table 6, the total costs of the CRME with cement or fly ash are
304.11 ¥/t and 300.91 ¥/t, respectively. It manifests that the difference
in costing for the two CRMEs is very small. In addition, the corre­
sponding energy consumption and carbon (CO2) emission are listed in
Table 7 [34]. By comparing the CRME with cement and the CRME with
fly ash, it can be found that the energy consumption and CO2 equiva­
lence of the latter is obviously lower than those of the former, and the
reduction magnitudes are 15.6% and 48.2%, respectively. It indicates
that the fly ash replacing cement in CRME can effectively reduce the
energy consumption and CO2 emission.
4. Conclusions
This research investigated the evolution in microstructures and
CNY-Chinese Yuan.
mechanical performance of CRME with fly ash under long-term service
conditions. Based on the tested results, the following conclusions can be
drawn:
(1) The ITS of CRME with fly ash can decrease when the long-term
curing time reaches a certain point, and the turning point is relevant
to the types and dosages of fly ash. Regardless of fly ash types, a proper
dosage is importance for enhancing ITS of CRME, and 1.5% dosages are
recommended in this research.
(2) The ITS of the CRME with fly ash (A or B) is higher than that of
the CRME with cement during long-term curing. For fly ash A and B, the
biggest increase amplitudes are 13% (after 10 days curing) and 43%
(after 7 days curing), respectively.
(3) As the curing age increases, the air void, flow value, and low-
temperature indirect tensile strain of CRME with fly ash increase first
and then decrease, while the Marshall stability and TSR always show a
gradual increase trend. By comparing the CRME with cement, the CRME
with fly ash throughout the long-term curing process exhibits the higher
low-temperature anti-cracking performance and the lower high-
temperature stability and water stability.
(4) Optical microscope analysis indicates that, after adding fly ash in
asphalt emulsion, the shell of some fly ash particles is gradually dis­
solved and fuses each other, as well as the demulsification of asphalt
emulsion particles is accelerated. Then, a structure composed of asphalt
binder, dissolved and undissolved fly ash is formed.
(5) XRD and ESEM results analysis also demonstrate that the disso­
lution of fly ash particles and the demulsification of asphalt emulsion
particles occur simultaneously during the curing ages. For the CRME
with 1.5% fly ash B, from 1 day to 5 days curing, a denser microstructure
made up of the asphalt binders, dissolved and undissolved fly ash par­
ticles is gradually formed. However, from 5 days to 30 days, the change

9
Q. Li et al. Construction and Building Materials 319 (2022) 126120

becomes very small.

CO2 equivalence / (kg/t)

(6) The fly ash replacing cement in CRME can effectively reduce the
energy consumption and CO2 emission, the reduction magnitudes are
15.6% and 48.2%, respectively.

CRediT authorship contribution statement

14.17
13.5

0.67
Quan Li: Writing – original draft. Chongzheng Zhu: Data curation,
Methodology. Henglong Zhang: Supervision. Shuai Zhang: Writing –
Energy consumption / (MJ/t)

review & editing.

CRME with fly ash

Declaration of Competing Interest

The authors declare that they have no known competing financial

210.98
201.9

interests or personal relationships that could have appeared to influence

9.08

the work reported in this paper.

CO2 equivalence / (kg/t)

Acknowledgements

This work was supported by the Huxiang Youth Talent Program of

Hunan Province (grant number 2019RS2052), the Transportation Sci­
ence and Technology Development and Innovation Project of Hunan
27.37
26.7

0.67

Province (grant number 201805), the Science and Technology Planning

Project of Hunan Province (grant numbers 2019GK5004, 2018TP2038).
The authors gratefully acknowledge their financial support.
Energy consumption/ (MJ/t)

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