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Construction and Building Materials 231 (2020) 117186

Contents lists available at ScienceDirect

Construction and Building Materials


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

The thermoregulation effect of microencapsulated phase-change


materials in an asphalt mixture
Biao Ma a, Sha-sha Chen a,⇑, Yu-zheng Ren b, Xue-yan Zhou c
a
Key Laboratory for Special Area Highway Engineering of Ministry of Education, Chang’an University, Xi’an, Shaanxi 710064, China
b
CCCC First Highway Consultants Co., LTD, Xi’an, Shaanxi 710075, China
c
School of Modern Posts & Institute of Posts, Xi’an University of Posts & Telecommunications, Xi’an, Shaanxi 710064, China

h i g h l i g h t s

 The latent heat storage capacity of the micro-PCM was referred to by use of the Ch.
 Thermoregulation effect of three types of micro-PCMs were compared.
 The high dosage of micro-PCMs improved the thermal properties of asphalt mixture.

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

Article history: Temperature plays an important role in the long-term performance and service life of pavement. With
Received 14 February 2019 the large-scale use of asphalt pavement, the paving industry is now more interested in the related pave-
Received in revised form 18 September ment distress generated by temperature. Against this background, this paper presents the test results for
2019
pure microencapsulated phase change materials (micro-PCMs), as well as asphalt mixtures containing
Accepted 6 October 2019
Available online 14 October 2019
micro-PCMs, with the aim of reducing the temperature difference. The latent heat storage capacity of
pure micro-PCMs was evaluated by the T-history method, and Ch was proposed to characterize their
latent heat storage capacity. Outdoor experiments were performed to observe the temperature change
Keywords:
Road engineering
behavior of seven asphalt mixture specimens manufactured by the wheel-grind method. Two specimens
Asphalt pavement were mixed with 5°C micro-PCMs, with micro-PCM contents of 0.3% and 0.5% respectively, substituting
Micro-PCM the equivalent amount of mineral filler. Another two specimens were mixed with 0 °C micro-PCMs, with
Latent heat storage capacity micro-PCM contents of 0.3% and 0.5%. Two other specimens were mixed with 5 °C micro-PCMs, with
Thermoregulation micro-PCM contents of 0.3% and 0.5%. The results show that the thermoregulation ranges of different
micro-PCMs differ. As the micro-PCM content increases, the temperature difference between the ordinary
AC-13 asphalt mixture and AC-13 mixed with micro-PCMs increases. The use of 5 °C micro-PCMs in an
asphalt mixture can significantly improve its thermal behavior.
Ó 2019 Elsevier Ltd. All rights reserved.

1. Introduction produce fatigue cracking under prolonged temperature distress.


When the temperature suddenly drops, asphalt pavement cracks
The functional and structural performance of asphalt pavement due to a failure to rapidly release the internal stress [8,9]. From
is significantly related to its temperature [1]. Additionally, temper- autumn to winter, the road is often covered in snow or frost. The
ature is the main factor affecting asphalt pavement road perfor- presence of a frost layer provides poor skid resistance on asphalt
mance [2–4]. Temperature variations within the pavement pavement. This can cause traffic accident rates to rise significantly
structure contribute in many different ways to the distress and and low vehicle speeds that reduce automobile trip efficiency. All
possible failure of that structure [5]. During a hot summer, an of these directly affect the travelling safety and durability of
increase in the moving vehicle load decreases the asphalt mixture’s asphalt pavement. Therefore, how to improve asphalt pavement’s
modulus, leading to large deflections and the jostle, piling up, wave high-temperature rut resistance, low-temperature anti-cracking
and rut of the facing layer [6,7]. In addition, pavement can easily performance and anti-frost capability should be studied.
To date, solar energy seems to be the cheapest and most envi-
ronmentally friendly form of clean energy. However, solar energy
⇑ Corresponding author.
is only available during the day. Hence, its application requires
E-mail address: 13468844299@163.com (S.-s. Chen).

https://doi.org/10.1016/j.conbuildmat.2019.117186
0950-0618/Ó 2019 Elsevier Ltd. All rights reserved.
2 B. Ma et al. / Construction and Building Materials 231 (2020) 117186

an efficient system for thermal energy storage so that the excess thermoregulation as an example. A PCM provides a thermoregula-
heat collected during daylight hours may be stored for later use tion effect on an asphalt mixture, which originates from the latent
[10]. Efficient and economical heat storage is the key to the effec- heat exchanged during crystallization. PCMs solidify during the
tive and widespread utilization of solar energy for low- long and cold winter and then release heat into the pavement sur-
temperature thermal applications. Phase change materials (PCMs) roundings when the surface temperature decreases to the PCMs’
take advantage of the latent heat that can be stored or released phase change temperature, which can ensure the asphalt pave-
from a material over a narrow temperature range [11]. They can ment temperature is higher than the low temperature distress
absorb thermal energy as they transform from solid to liquid, temperature for a prolonged time. Thus, a pavement structure’s
and release it when returning to a solid [12]. The volume and ther- low-temperature adaptability can be improved by micro-PCM
mal conductivity of PCMs changes during the phase transforma- addition.
tion. PCMs have the potential for use in asphalt pavement. As is To understand how micro-PCMs regulate the temperature of
well known, hot-mix asphalt mixtures are always associated with asphalt pavement, a series of tests were conducted to choose the
high temperature during the mixing process. In addition, aggre- most suitable phase change material. For this study, the latent heat
gates and stones rub against each other during the concrete mixing storage capacity test was used to explore the heat transfer charac-
process. And, PCMs leak easily during the melting process [13]. One teristic and heat capacity of micro-PCMs. The thermoregulation
question that needs to be asked, however, is whether PCMs can be effect test was conducted on three types of micro-PCMs to ascer-
encapsulated effectively, in case they leak during mixing. To tain the temperature change regulation of micro-PCM-mixed
address the problem, the PCM needs to be stored in a carrier. In asphalt pavement.
microencapsulation, PCMs are coated with polymeric materials
[14], yielding microencapsulated phase-change materials (micro-
PCMs). 2. Materials
An increasing number of studies have addressed PCMs. Ma et al.
[15] used a membrane layer to encapsulate the PCM to prepare a 2.1. Micro-PCM preparation
composite shape-stabilized phase change material (CPCM). The
proper proportion for CPCM preparation was determined by a The PCM in this study was n-tetradecane with a flash point of
scanning electronic microscope, a differential scanning calorimeter 122 °C and a density of 0.767 g/cm3. The substrate was silica with
and an orthogonal test. In their another related study [16], four dif- granules in millimicron form. Ethyl cellulose (EC) functioned as the
ferent kinds of CPCMs were prepared using pure PCM, silica pow- membrane material and ethyl alcohol (CH3CH2OH) as an organic
der absorbed PCM, floating bead absorbed PCM and activated solvent for EC to cover the PCM. Dioctyl sebacate was used as a
carbon absorbed PCM as raw materials. The results showed that plasticizer. All aqueous solutions were prepared using distilled
compared to the other three CPCMs, the CPCM with activated car- water.
bon absorbed PCM as a raw material had a better high- First, silica (as carrier material) and the PCM (n-tetradecane)
temperature stability and could meet the use demands for asphalt were mixed uniformly in a vacuum pump so that the n-
mixtures. Taking the initiative to solve the asphalt pavement tem- tetradecane was fully adsorbed by the silica. Then, a shape-
perature problems, Si et al. [17] proposed three different CPCM stabilized PCM was prepared. Second, ethyl cellulose was dissolved
thermoregulation types for use in asphalt pavement. Their study into anhydrous ethanol to prepare the gelatinous solution. Third, a
proposed composite mass proportions for different thermoregula- mixture of shape-stabilized PCMs and dispersing agent was mixed
tion types and the corresponding enthalpy values. However, previ- with the gelatinous solution. Finally, the mixture was placed into a
ous studies tend to ignore a CPCM’s inherent physical properties. coating pan. The final dry powder was the micro-PCM, as shown in
Recently, using a heat exchange system and a data acquisition sys- Fig. 1(a). Fig. 1(b) shows that the PCMs were well encapsulated.
tem, Ma et al. [18] determined the specific heat capacity of CPCM
and asphalt mixtures mixed with CPCM, intuitively reflecting 2.2. Micro-PCM DSC results
CPCM’s thermoregulation mechanism in asphalt mixtures. Using
PCM as the main component of an unsaturated organic acid and The initial phase change temperature of the main micro-PCM
a polypropylene carrier, Ma et al. [19] successfully prepared road used in this study was approximately 5 °C, which is hereafter
temperature-adjustment material (RTM). The results showed that called the 5 °C micro-PCM. For instance, 5°C micro-PCM indicates
an asphalt mixture with RTM could actively adjust the working that the initial phase change temperature of the material is 5°C.
temperature with a damping effect and enhance the asphalt mix- The differential scanning calorimetry (DSC) curves of the 5 °C
ture’s temperature resistance capacity. Wei and Ma [20] summa- micro-PCM are shown in Fig. 2. During the exothermic process,
rized the latest research progress on micro-PCMs worldwide. In the initial phase change temperature and final phase change tem-
addition, the chemical methods for micro-PCM preparation were perature were 4.84 °C and –18.64 °C, respectively, and the com-
introduced and the performance of micro-PCMs was analyzed. pensation power peak appeared at 1.04 °C. The exothermic
Future development directions for micro-PCMs were also pro- enthalpy was 94.20 J/g. During the endothermic process, the initial
posed. Memon et al. [21] incorporated paraffin into porous light- phase change temperature and final phase change temperature
weight aggregates (LWAs) through vacuum impregnation. were 12.81 °C and 28.82 °C, respectively, and the compensation
Although PCMs have been widely used in the construction, mil- power peak appeared at approximately 13.02 °C. The endothermic
itary, textile and agricultural fields, their application for roads is enthalpy was 92.29 J/g.
still in the exploratory research stage [22]. Therefore, the purpose
of this study was to analyze the thermoregulation of a micro-PCM,
as well as its influence on the asphalt mixture. The PCM ther- 3. Experimental methods
moregulation effect is a dynamic process that allows an asphalt
mixture containing PCMs to slow the speed of its internal temper- 3.1. Latent heat storage capacity test
ature change when directly exposed to cold or hot weather condi-
tions. This process depends on the latent heat absorption or release Many approaches have been used to characterize the thermo-
that occurs when the PCM undergoes a phase change from solid to physical properties of PCMs, among which the T-history method
liquid, liquid to gas or vice-versa. Consider low-temperature has been widely adopted in many studies due to its convenient
B. Ma et al. / Construction and Building Materials 231 (2020) 117186 3

Fig. 1. Micro-PCM powder and its SEM image.

Fig. 2. DSC test results of 5 °C micro-PCM.

operation and high precision [23]. Thus, the T-history method was Pure water
adopted in this research. 35
Pure water mixed with micro-PCMs

30
3.1.1. Test theory
Two glass bottles, A and B, were filled with the same mass of 25
water. Bottle A contained some PCMs, while bottle B did not.
20
1. Temperature sensors were installed in the two bottles, and then
they were placed into an environmentally controlled box until
15
they reached the same temperature.
2. A certain quantity of hot water was successively and quickly
poured into two identical insulation barrels, and temperature 10

sensors were immersed in the two water baths.


3. The glass bottles were removed from the environmentally con- 5
trolled box and put into the two insulation barrels.
18:09:00 18:15:00 18:21:00 18:27:00 18:33:00 18:39:00 18:45:00 18:51:00
4. The two insulation barrels were put into the environmentally
controlled box, and the box was set to a fixed temperature. Time

Fig. 3. The temperature curves of pure water and pure water with micro-PCMs
Each of the insulation barrels filled with water served as water during heating.
baths. There was a temperature difference between the glass bot-
tles and the insulation barrels at step three. The temperature For the pure water mixed with micro-PCMs, the temperature
changes (Fig. 3) of the two insulation barrels in the environmen- increased gradually, reaching its maximum at 31 °C. The pure
tally controlled box were recorded using temperature sensors. water reached its maximum during the same period. The initial
4 B. Ma et al. / Construction and Building Materials 231 (2020) 117186

temperature conditions of the two insulation barrels were the


same. However, there is hysteresis between the curves for pure
water and pure water with micro-PCMs. The reason for this behavior
is that the micro-PCMs underwent a solid-to-liquid phase transi-
tion during the heating process.
According to the theory of latent heat, the total amount of heat
(QM) absorbed by the pure water with micro-PCMs during heating
is composed of the latent heat (QL), the sensible heat (QS) and the
lost heat (QC). However, the total amount of heat (QNM) absorbed
by the pure water in bottle B consists of only the sensible heat
(QNS) and the lost heat (QNC). The amount of heat can be calculated
as:
Q NM ¼ Q NS þ Q NC ð1Þ
Fig. 5. The glass bottle placed into the insulation barrel.
QM ¼ QS þ QC þ QL ð2Þ
During the latent heat storage capacity test, the two insulation tion estimation of the micro-PCM during a typical T-history
barrels were put into the same environmentally controlled box. method. Considering that the micro-PCM stores or releases more
Therefore, the total heat values, QNM and QM, are the same, and heat around its phase change temperature, temperature ranges of
the heat loss values, QNC and QC, are equal. By subtracting Eq. (1) 45–50 °C and 0–8 °C were chosen as the heat exchange tempera-
from Eq. (2), the heat stored by the micro-PCMs in the form of ture ranges for the heating and cooling processes, respectively.
latent heat is shown in Eq. (3).
(1) The heating process
Q L ¼ Q NS  Q S ð3Þ
The relationship between the heat and temperature is shown in 1. Two glass bottles, A and B, were filled with the same mass of
Eq. (4). water (240 g), and m g of micro-PCMs were added to bottle A.
2. After inserting temperature sensors, both bottles were properly
Q ¼ cmDT ð4Þ
sealed (Fig. 4).
In Eq. (4), Q is the quantity of heat, c is the specific heat capacity, 3. The two glass bottles were placed into a refrigerator set to a cer-
m is the material mass and DT represents the temperature differ- tain temperature for 40 min.
ence during a certain time duration. The values of QNS and QS can 4. Two insulation barrels were placed in an environmentally con-
be calculated based on Eq. (4). To keep the following derivation trolled box set to 50 °C for 10 min.
simple, it is assumed that the specific heat capacity of the pure 5. The insulation barrels were removed from the environmentally
water and the pure water mixed with micro-PCMs was the same. controlled box. Then, 1550 g of hot water (50 °C) was poured
The value of QL can then be expressed by Eq. (5). into each insulation barrel, which were equipped with temper-
ature sensors. Every combination of barrel and temperature
Q L ¼ Q NS  Q S ¼ cmðDT n  DT Þ ð5Þ
sensor was tested.
In Eq. (5), m is the mass of water, DTn represents the tempera- 6. Bottle A and bottle B were removed from the refrigerator and
ture difference of the pure water during a certain time range and put into the two barrels, which were then covered with cotton
DT represents the temperature difference of the water in bottle A and capped as quickly as possible (Figs. 5 and 6).
during the same time range. 7. The two insulation barrels were placed into the environmen-
tally controlled box; data were extracted after 40 min (Fig. 7).
3.1.2. Thermoregulation ability
Because the phase-change peak temperature and phase-change (2) The cooling process
enthalpy of the micro-PCMs are different in the exothermic and
endothermic processes, both heating and cooling process tests The procedure for the cooling process test was similar to the
were conducted to provide the data required for the thermoregula- heating process test. However, the initial temperature conditions
were different.

1. Two insulation barrels containing 1550 g of pure water were


placed into a refrigerator for one hour.
2. Two glass bottles, A and B, were filled with the same mass of
water (240 g), and m g of micro-PCMs were added into bottle A.
3. Both glass bottles were placed into a 50 °C water bath and
allowed to heat until the water temperature inside reached
50 °C.
4. After the temperature sensors were put in place, both bottles
were properly sealed.
5. The insulation barrels were removed from the refrigerator, and
temperature sensors were installed in the two insulation
barrels.
6. Bottle A and bottle B were removed from the water bath and
each put into one of the two barrels. The two insulation barrels
were covered with cotton and capped as quickly as possible.
7. The two insulation barrels were placed into the environmen-
Fig. 4. Glass bottle A and glass bottle B with temperature sensors. tally controlled box, and data were extracted after 40 min.
B. Ma et al. / Construction and Building Materials 231 (2020) 117186 5

specimen (Fig. 9). The ambient temperature data was obtained by


placing a temperature sensor in the air. The placement of the seven
rut specimens are shown in Fig. 10.

4. Results and analysis

4.1. Micro-PCM latent heat storage capacity

A latent heat storage capacity test is very inexpensive and mea-


sures the temperature of a sample and a reference material, such as
water, easily over time. This single measurement can be used to
calculate the latent heat storage capacity of a micro-PCM. It is
Fig. 6. Sealed insulation barrels. based on recording temperature versus time curves of the micro-
PCMs, with water as a reference. The latent heat absorbed or
released by the micro-PCM can be calculated based on Eq. (5).
Therefore, in this research, heat storage capacity is described by
Ch in J°C/g. To be more specific, Ch represents the heat absorbed
or released by a micro-PCM per unit mass versus the temperature
of water. The measured value extracted from one test is shown in
Fig. 11, in which water temperature is plotted on the horizontal
axis and the latent heat of micro-PCMs is plotted on the vertical
axis. After fitting the curves as shown in Fig. 11, the value of Ch
can be obtained by calculating the coordinate curve integral.

Z T2  
QL
Ch ¼ dT ð6Þ
T1 m
In Eq. (6), QL is the quantity of latent heat, m is the micro-PCM’s
mass and T1 and T2 represent the initial and final water tempera-
Fig. 7. Insulation barrels placed in the environmentally controlled box.
tures, respectively, during the heating or cooling process. In addi-
tion, Chh represents the latent heat storage capacity during the
heating process, while Chc represents the latent heat storage capac-
3.2. Thermoregulation effect test
ity during the cooling process. The test results are shown in
Table 1.
3.2.1. Test equipment
The value of Ch during the heating and cooling processes are dif-
The test equipment included an asphalt mixture mixer, a rut
ferent, as shown in Table 1. This is because the energy released or
meter, and a temperature measuring system (Fig. 8).
absorbed by the micro-PCMs were different during the phase tran-
sition process. Figs. 12 and 13 show there is a linear relationship
3.2.2. Test plan between Ch and the mass of micro-PCMs used in the test. However,
To investigate the thermoregulation effect of micro-PCMs in an Ch was an inherent property of the micro-PCM. Thus, the value of
asphalt mixture, the AC-13 asphalt mixture was used in this test. Ch should approach a fixed value based on the large number of data
The AC-13 asphalt content was 4.9% by weight of aggregate. The samples. The mean value of Ch can be viewed as the fixed value.
thermoregulation effect has a strong relationship with the asphalt
mixture’s micro-PCM mass ratio. Therefore, in order to provide sat-
isfactory road performance, it is necessary to increase the micro- 4.2. Thermoregulation effect analysis
PCM mass ratio as much as possible. Asphalt mixture specimens
were manufactured by the wheel rolling method with a height of 4.2.1. Temperature recorded versus time
10 cm. There were seven specimens with different micro-PCM The temperature changes of seven specimens over time are
mass ratios from three different thermoregulation types. Two rut shown in Fig. 14. The details of the seven rut specimens were intro-
specimens were mixed with 5°C micro-PCMs with mass ratios duced in Section 3.2.2, Test plan. As is shown in Fig. 14, the temper-
of 0.3% and 0.5%. Similarly, two rut specimens were mixed with ature change behaviors of the seven rut specimens were similar.
0 °C micro-PCMs with mass ratios of 0.3% and 0.5%. Two other Notably, there were some temperature differences between the
rut specimens were mixed with 5 °C micro-PCMs with mass ratios control and the other six rut specimens. Specifically, the tempera-
of 0.3% and 0.5%. The other specimen that did not contain micro- ture difference between the 5 °C micro-PCM and the control was
PCMs was used as the control group. In addition, temperature sen- the largest. This result reflects that micro-PCMs of different types
sors were installed in the center as well as the surface of each rut have a certain thermoregulation effect on an asphalt mixture.

Fig. 8. Temperature measuring system.


6 B. Ma et al. / Construction and Building Materials 231 (2020) 117186

900

800

Chh /(J* /g)


700

600

Fig. 9. Rut sample embedded with temperature sensors. 500

400
20 22 24 26 28 30 32
Micro-PCM mass /g

Fig. 12. Heat storage capacity versus mass of the micro-PCM during the heating
process.

1000

900

800
Chc /(J* /g)

Fig. 10. Outdoor modeling test.

700
2
y = -43.56412x +3119.4624x-54275.24344
Fitting curve 600
1600

1400 500

1200
400
1000 20 22 24 26 28 30 32
Micro-PCM mass /g
Heat /J

800

600 Fig. 13. Heat storage capacity versus mass of the micro-PCM during the cooling
process.
400

200

-200
30 32 34 36 38 40 42
Temperature/°C

Fig. 11. Latent heat of micro-PCMs versus water temperature.

Table 1
Chh and Chc values with different micro-PCM mass.

Mass (g) Chh (J°C/g) Chc (J°C/g)


30 854 980
25 513 607
20 409 471
Means 592 686

4.2.2. Temperature difference analysis


Fig. 15 shows the temperature difference between the
experimental specimens and the control specimen. The experi-
mental specimens include six asphalt mixture specimens with dif-
ferent micro-PCM contents. The reason for the temperature
difference between the rut specimens is that micro-PCMs undergo
a phase change transition from solid to liquid or vice versa during Fig. 14. The rut samples’ internal temperatures over time.
B. Ma et al. / Construction and Building Materials 231 (2020) 117186 7

Fig. 17. 0.3% Micro-PCM mass ratio.


Fig. 15. Temperature difference between the experimental and control specimens
over time.

this process. When the ambient temperature decreases, PCMs


solidify and thus release heat into the pavement surroundings,
which influences the temperature change of the asphalt pavement.
It is obvious that the mass ratio and type of micro-PCM have signif-
icant influences on the temperature differences. The specimens
mixed with 5 °C micro-PCMs have the biggest temperature differ-
ence values. The specimen with the 0.5% mass ratio micro-PCM has
a bigger temperature difference compared with the specimen
mixed with 5 °C micro-PCM.

4.2.3. Analysis of different micro-PCM types


To study the affected factor, micro-PCM thermoregulation
types, the temperature differences of the three rut specimens with
the same micro-PCM mass ratio were recorded in Figs. 16 and 17.
The temperature difference trends of the three samples were basi-
cally identical. Fig. 16 shows that a distinct trough of 5 °C micro-
PCMs appears at 12:25:00, right behind the troughs of 0 °C and
5°C micro-PCMs. That means the thermoregulation range of dif- Fig. 18. Different mass ratios of 5°C micro-PCM.
ferent micro-PCMs were different. Meanwhile, the temperature
difference of the 5 °C micro-PCM reaches its maximum at approx-
imately 1.5 °C. At that point, the environment temperature was
approximately 7 °C and the temperature of the specimen not
mixed with micro-PCMs was 8.9 °C. According to the DSC result,
the initial and final phase change temperatures of the 5 °C micro-
PCMs were 4.84 °C and –18.64 °C, respectively. Therefore, 5 °C
micro-PCMs can respond to the temperature change effectively
when the environment temperature changes within the range of
0–10 °C.

Fig. 19. Different mass ratio of 0 °C micro-PCM.

4.2.4. Analysis of different micro-PCM mass ratios


To study the affecting factor, the mass ratio of micro-PCMs, the
temperature difference of the two specimens mixed with the same
type of micro-PCMs were recorded in Figs. 18–20. The ambient
temperature rises and then falls successively. The temperature dif-
Fig. 16. 0.5% Micro-PCM mass ratio. ference change trends of the two samples were basically the same
8 B. Ma et al. / Construction and Building Materials 231 (2020) 117186

Acknowledgments

The writers wish to acknowledge the financial support of this


research by the ‘‘Twelfth five-year’’ National Science and Technol-
ogy Support Plan (No. 2014BAG05B04), the Construction Science
and Technology Project of Ministry of Transport of China (No.
2013 318 490 010), the Central University program (No.
310821151010), the Transportation Industry High-Level Technical
Personnel Training project (No. 2018019) and the Special Project
Education Department of Shaanxi Provincial Government (No.
19JK0801)

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The authors declare that they have no known competing finan-
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cial interests or personal relationships that could have appeared
to influence the work reported in this paper.

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