Coatings 13 00474 v2

coatings
Article
Study on the Influence Factors of Dynamic Modulus and Phase
Angle of Dense Gradation Polyurethane Mixture
Haisheng Zhao 1,2 , Wensheng Zhang 3 , Shiping Cui 1 , Shijie Ma 1, * , Baoji Miao 3 , Enzhou Di 1 , Xiaoyan Wang 1 ,
Chunhua Su 1 , Jincheng Wei 1 and Shan Liu 1
1 Key Laboratory of Highway Maintain Technology Ministry of Communication, Jinan 250102, China
2 School of Highway, Chang’an University, Xi’an 710064, China
3 Wanhua Chemical Group Co., Ltd., Yantai 265599, China
* Correspondence: mashijie@sdjtky.cn; Tel.: +86-186-6016-3082
Abstract: Polyurethane (PU) mixture is a new pavement material with excellent pavement perfor-
mance, and most research was focused on the enhancement of pavement performance, but rarely
on the dynamic property. This paper studied the factors including gradation, aggregate type, PU
type, and PU content, which may influence the dynamic property of the PU mixture. Test results
showed that the PU mixture is a kind of linear viscoelastic material, its dynamic modulus and phase
angle changed with test temperature and loading frequency, the dynamic modulus would drop
by 40%~50% with the temperature raised from 5 ◦ C to 55 ◦ C. All of the factors could affect the
dynamic property of the PU mixture which was proved by the analysis of covariance. The effect of
gradation did not change with the increase of the nominal maximum aggregate size (NMAS), the
dynamic modulus of the PU mixture with limestone was higher than that of the PU mixture with
basalt, and the curing speed of PU could affect the ultimate stiffness of the PU mixture, and the
increase of the PU content did not help in the increase of the dynamic modulus of the PU mixture.
So, more consideration about the selection of gradation, aggregate type, PU type, and PU content
should be taken into the design of the PU mixture, which could produce the best pavement structure
combination and save more investment.
Keywords: polyurethane mixture; dynamic modulus; phase angle; covariance

Citation: Zhao, H.; Zhang, W.; Cui, S.;
Ma, S.; Miao, B.; Di, E.; Wang, X.; Su,
C.; Wei, J.; Liu, S. Study on the
Influence Factors of Dynamic
Modulus and Phase Angle of Dense 1. Introduction
Gradation Polyurethane Mixture. Asphalt mixtures have viscoelastic a property which is due to the combination of the
Coatings 2023, 13, 474. https:// viscoelastic asphalt binders and the aggregate skeleton [1,2]. At low temperatures, the
doi.org/10.3390/coatings13020474 asphalt binder is in rigid status, the asphalt mixture acts elastically, and the properties of
Academic Editor: Andrea Nobili the asphalt mixture are mainly subjected to the asphalt binder. The viscoelastic properties
of the asphalt mixture are more affected by the interlocking force between the aggregates
Received: 30 January 2023 than by the asphalt binder when the temperature rises (or frequency falls) because the
Revised: 12 February 2023
asphalt binder becomes soft and the asphalt mixture primarily exhibits a viscous behavior.
Accepted: 17 February 2023
Thus, the aggregate skeleton is primarily subject to the loading stress, as temperature (or
Published: 19 February 2023
frequency) increases [3]. At various temperatures, the viscoelastic behavior of the asphalt
mixture is impacted by the aggregate skeleton and asphalt binder.
In the Al−Khateeb model [4], the asphalt mixture is composed of three phases (asphalt
Copyright: © 2023 by the authors.
binder, aggregate, and air void) in parallel. From this perspective, the properties of the
Licensee MDPI, Basel, Switzerland. asphalt mixture must be influenced by the three phases, and numerous researchers have
This article is an open access article looked at the effects of the aggregate gradation and asphalt binder. Ali et al. [5] studied the
distributed under the terms and impact of temperature, frequency, and NMAS on the dynamic modulus and phase angle of
conditions of the Creative Commons eight kinds of asphalt mixture, including wearing and base course mixes, and test results
Attribution (CC BY) license (https:// showed that the test temperature and loading frequency could significantly influence the
creativecommons.org/licenses/by/ dynamic response of both wearing and base course mixes, but the NMAS factor had an in-
4.0/). significant effect. The study [6] identified that various factors including: aggregate, asphalt
Coatings 2023, 13, 474. https://doi.org/10.3390/coatings13020474 https://www.mdpi.com/journal/coatings

Coatings 2023, 13, 474 2 of 18
content, and reclaimed asphalt pavement (RAP) percentage had significant influence on
the dynamic response of asphalt mixtures, and the dynamic modulus of asphalt mixtures is
sensitive to the mix constituents. The study [7] reported that asphalt binder could signifi-
cantly affect the dynamic modulus of asphalt mixtures and concluded that the softer the
asphalt binder, the lower the dynamic modulus, and vice versa. This study [8] found that
binder grade, air voids, and RAP significantly influence the dynamic modulus of asphalt
mixtures. The research [9] concluded that the dynamic modulus of rubber asphalt mixture
was affected by factors, i.e., binder, mixture type, temperature, and loading frequency, and
temperature and loading frequency had a larger influence on the dynamic modulus of the
mixture than the binder, mixture type, etc. Hajibandeh and Shalaby [10] concluded that
the dynamic modulus of full-size (standard) and small-scale specimens were considerably
influenced by the aggregate gradation and specimen dimension.
The prediction equation employed in the mechanistic empirical pavement design
guide (MEPDG) to predict the dynamic modulus of asphalt mixture is a function of aggre-
gate gradation, effective binder content, binder properties, mix air voids, temperature, and
loading rate. The dynamic modulus of the asphalt mixture depends on many factors, e.g.,
aggregate gradation, binder type, aging, construction technology, and volumetric proper-
ties [11–15]. For example, Islam et al. [16] demonstrated how the rise in binder content and
air void will lead to an increase in the dynamic modulus of an asphalt mixture. According
to the research in [17,18], the dynamic modulus of the asphalt mixture is related to the
mixture gradation. Solatifar et al. and Su et al. [19,20] concluded that the laboratory-tested
dynamic modulus of the asphalt mixture is subjected to binder viscosity, binder content,
air voids, and gradation. According to Tan Hung et al. [21], porous asphalt mixtures with
fewer air voids exhibited higher dynamic modulus values.
The PU mixture is a complicated mixture that substitutes PU for asphalt binder, its
characteristic and mechanical behavior is not fully studied. Based on the above-mentioned
documents, many different variables could influence the dynamic modulus of the PU
mixture, and those influence variables are still awaiting identification and analysis. This
paper aimed at studying the dynamic response characteristics of different PU mixtures, and
analyzed the internal PU mixture variables that affect the PU mixture’s dynamic modulus
and phase angle. The PU content, PU type, aggregate type, and gradation were the variables
that were examined in this study. A statistical analysis of covariance was used to link the
changes in the mixture variables to the dynamic characteristic of the PU mixture, and the
most significant variables would be identified. The asphalt mixture performance tester was
adopted to measure the frequency sweep dynamic mechanical properties of different PU
mixtures at various test temperatures and loading frequencies.
2. Materials and Methods

2.1. Material and Gradation of PU Mixture
In this paper, four kinds of PU mixtures with dense gradation were adopted, donated
as, PUM−10, PUM−13, PUM−16, and PUM−20. Limestone and basalt aggregates were
chosen for the mixture design (Xingan Stone Co., Jinan, China). The particle passing
percent of the selected gradation was displayed in Figure 1, the X axis in Figure 1 was in
the 0.45 power scale, and the Y axis was in arithmetic scale.
In Figure 1, the letters L and B stand for the utilization of limestone aggregates and
basalt aggregates, respectively.
Three different types of polyurethane, traditional cure speed PU, slow cure speed
PU, and PU dyed with 6179H additive, were used for comparison. The traditional cure
speed PU means that the PU would be solidified after about 2−4 h under different cure
conditions, the slow cure speed PU means that the PU would be solidified after more than
4 h under the same cure conditions, compared with the traditional cure speed PU, and the
PU dyed with 6179H additive is the traditional cure speed PU with color additive. The
PU was provided by Wanhua Chemical Group Co., Ltd., (Yantai, China) and the PU is the
wet-set type which means that the PU would be solidified under wet conditions.
Coatings 2023, 13,
Coatings 2023, 13, x474
FOR PEER REVIEW 3 3ofof 19
18
110
100
90
80
70
Passing (%)
60
50
PUM−10/B
40
PUM−13/L
30 PUM−13/B−1
PUM−13/B−2
20
PUM−16/L
10 PUM−20/L
0
0.075 0.15 0.3 0.6 1.18 2.36 4.75 9.5 13.2 16 19 26.5
Sieve size (mm)
Figure
Figure 1.
1. The
The gradation
gradation results
results of
of the
the selected
selected dense
dense gradation.
gradation.
In Figureinformation
Mixture 1, the lettersisLsummarized
and B stand in forTable
the utilization of limestone
1. The indexes of the PUaggregates
with differentand
basalt aggregates, respectively.
cure speeds are shown in Table 2.
Three different types of polyurethane, traditional cure speed PU, slow cure speed
PU,
Tableand PUmixture
1. The dyed with 6179H
gradation additive,
design were used for comparison. The traditional cure
combinations.
speed PU means that the PU would be
Gradation solidified after about
Aggregate 2−4 h under different cure
PU Content
conditions,
Number
the Designation
slow cure speed PUType means thatTypethe PU would(%) be solidified after more than
PU Type
4 h under
1 the same
PUMcure
−10/Bconditions,PUMcompared
−10 with the traditional
Basalt 5.2 cureTraditional
speed PU, and
cure speedthe
PU dyed
2 with PUM
6179H additive
−13/B −2 isPUM
the −
traditional
13/2 cure speed PU5.2with color
Basalt additive.
Traditional cureThe
speedPU
3 PUM−13/L PUM−13 Limestone 5.2 Traditional cure speed
was provided
4
by Wanhua
PUM−16/L
Chemical
PUM−16
Group Co., Ltd.,
Limestone
(Yantai,
4.9
China) and the PU is
Traditional cure speed
the
wet-set
5 type which PUM− means
20/L that the PUMPU−20wouldLimestone
be solidified under
4.9 wet conditions.
Mixture
6 information
PUM −13/B−1/5.0is summarized
PUM−13/1 in TableBasalt1. The indexes
5 of theTraditional
PU withcure different
speed
7 PUM−13/B−1/5.6 PUM−13/1 Basalt 5.6 Traditional cure speed
cure 8speedsPUMare −
shown in TablePUM
13/B−1/5.3(T) 2. −13/1 Basalt 5.3 Traditional cure speed
9 PUM−13/B−1/S PUM−13/1 Basalt 5.3 Slow cure speed
Table 1. The mixture gradation design combinations. Stained with 6179H
10 PUM−13/B−2/H PUM−13−2 Basalt 5.2 additive and
Gradation Aggregate PU Content Traditional cure speed
Number Designation PU Type
B−1 and B−2 represent Type gradations,
different basalt aggregate Type S represents
(%)the slow cure speed PU, H represents
the traditional cure speed PU binder stained with 6179H additive, and T represents the traditional cure speed PU.
1 PUM−10/B PUM−10 Basalt 5.2 Traditional cure speed
Table 2 2. The index
PUM−13/B−2 PUM−13/2
of PU with different Basalt
cure speeds. 5.2 Traditional cure speed
3 PUM−13/L PUM−13 Limestone 5.2 Traditional cure speed
4 PUM−16/L
Index PUM−16 Limestone
Traditional Cure 4.9
Speed Traditional
Slow Curecure Speedspeed
5 Viscosity PUM−20/L
(25 C) (MPa·s) PUM−20 Limestone
◦ 1707 4.9 Traditional 1691cure speed
(30 ◦ C, 90% RH) (min)
6Dry timePUM−13/B−1/5.0 PUM−13/1 Basalt70 5 Traditional 83 cure speed
Tensile strength (MPa) 24.5 29.4
7 Breaking
PUM−13/B−1/5.6
elongation (%)
PUM−13/1 Basalt 212
5.6 Traditional 516
cure speed
8 PUM−13/B−1/5.3(T) PUM−13/1 Basalt 5.3 Traditional cure speed
9 PUM−13/B−1/S PUM−13/1 Basalt 5.3 Slow cure speed
2.2. Fabricated Specimens
Stained with 6179H
According to AASHTO: TP−62 (2009), the specimens were compacted using a Super-
10 PUM−13/B−2/H PUM−13−2 Basalt 5.2 additive and
pave gyratory compactor (SGC), and their dimensions were 170 mm in height and 150 mm
in diameter. The core specimens used for the dynamic modulus test were cored and sawed
B−1 and B−2 represent different basalt aggregate gradations, S represents the slow cure speed PU,
into the dimensions of 150 mm in height and 100 mm in diameter, as specified by AASHTO:
H represents the traditional cure speed PU binder stained with 6179H additive, and T represents
TP −79, after the specimens were constructed and cured (2010).
the traditional cure speed PU.
The fabricating course is shown as follows: (a) The aggregates and the filler should be
desiccant, and the PU mixture should be mixed at room temperature. Therefore, before
mixing, the aggregates and the filler had to be kept in a blown oven at 170 ◦ C for about 4 h,
Coatings 2023, 13, 474 4 of 18
then the aggregates and the filler were cooled to room temperature; (b) The PU mixture was
mixed for 90 s after the aggregates, filler, and PU binder were added in the correct order to
the mixing pot; (c) The PU mixture must be kept at room temperature (below 30 ◦ C) for
1.5 h before compaction; (d) The specimens must be compacted by SGC and compacted
100 times; (e) The specimens must be extracted after compaction, and the specimens were
cured for 5 days at 35 ◦ C and 70% RH.
Two replicates of each mixture type were fabricated. The volume index results of the
core specimens were listed in Table 3.
Table 3. The volume index results of the core specimens.
Designation γb γt Air Void (%)

PUM−10/B 2.451 2.574 4.75
PUM−13/B−2 2.419 2.592 6.7
PUM−13/L 2.4 2.523 4.9
PUM−16/L 2.379 2.535 6.15
PUM−20/L 2.412 2.528 4.6
PUM−13/B−1/5.0 2.495 2.661 6.25
PUM−13/B−1/5.6 2.476 2.638 6.15
PUM−13/B−1/5.3(T) 2.499 2.65 5.7
PUM−13/B−1/S 2.406 2.65 9.2
PUM−13/B−2/H 2.449 2.592 5.5
2.3. Dynamic Modulus Test

The asphalt mixture performance tester (AMPT) was adopted for dynamic modulus
testing according to the specification of AASHTO: TP−79 (2010). The loading waveform
was sinusoidal, and the control mode was the load-controlled uniaxial compression mode.
The amplitude of the loading wave was set to maintain the specimen’s strain between
75 and 125 uε, which is deemed just to keep the specimen within its viscoelastic range and
prevent specimen damage [22,23]. The test temperatures were 5 ◦ C, 15 ◦ C, 25 ◦ C, 35 ◦ C,
45 ◦ C, and 55 ◦ C, while the loading frequencies were set to 25, 20, 10, 5, 2, 1, 0.5, 0.2, and
0.1 Hz [24]. The results of the dynamic modulus and phase angle shown in this paper are
the average values of two replicates for each mixture.
2.4. Statistic Analysis

The SPSS software was used for analyzing the factors utilized in this paper. Addition-
ally, the analysis of covariance (ANCOVA) was used to evaluate the effects of gradation,
PU type, PU binder, and aggregate type on the dynamic modulus and phase angle. In the
statistical analysis [25,26], gradation, PU type, PU binder, and aggregate type were consid-
ered independent variables, whereas temperature and loading frequency were covariates.
The dynamic modulus and phase angle were regarded as dependent variables or responses.
The statistical analysis with a 5% level of significance (p-value) was used for the results
analyzed. When the p-value of any independent variables is less than 5% [27], it means that
the independent variable has a significant influence on the dependent variables.
3. Results
3.1. The Dynamic Modulus under Different Temperatures and Frequency
The dynamic modulus results of the PU mixture PUM−13 (fabricated with basalt
aggregate and traditional curing speed PU binder) at different test temperatures and
loading frequencies arere plotted in Figure 2a. The dynamic modulus of the different PU
mixtures at 15 ◦ C is shown in Figure 2b. The dynamic modulus results in this paper were
plotted on the normal scale [28].
The dynamic modulus results of the PU mixture PUM−13 (fabricated with basalt
gregate and traditional curing speed PU binder) at different test temperatures and load
frequencies arere plotted in Figure 2a. The dynamic modulus of the different PU mixtu
Coatings 2023, 13, 474 at 15 °C is shown in Figure 2b. The dynamic modulus results in this paper5 ofwere
18 plot
on the normal scale [28].
14,000 13,000
13,000
12,000
12,000
Dynamic Modulus (MPa)

11,000
11,000
10,000
10,000
9,000 9,000
8,000 8,000
7,000 PUM−13/B/T PUM−13/B/S

7,000 PUM−13/B/H PUM−13/B/T/5.0%
5℃ 35 ℃
6,000 PUM−13/B/T/5.6% PUM−13/B/T/5.3%
15 ℃ 45 ℃ PUM−13/L/T PUM−16/L/T
6,000
5,000 25 ℃ 55 ℃ PUM−20/L/T PUM−10/B/T
0 5 10 15 20 25 0 5 10 15 20 25
Loading Frequency (Hz) Loading Frequency (Hz)
(a) (b)
Figure 2. Dynamic
Figure modulus
2. Dynamic modulus ofofthe
thePU
PUmixtures. (a)PUM
mixtures. (a) PUM−13
−13 atat different
different testtest temperatures
temperatures and and lo
ing frequencies. (b) Different
loading frequencies. PU mixtures
(b) Different atat15
PU mixtures 15°C.
◦ C.
3.2. The Phase Angle under Different Temperatures and Loading Frequency
The phase angle results of PU mixture PUM−13 (fabricated with basalt aggregate and
tings 2023, 13, x FOR PEER REVIEW The phase
traditional angle
curing results
speed of PU at
PU binder) mixture
differentPUM−13 (fabricated
test temperatures with basalt
and loading aggregate
frequencies 6 ofa
traditional curing speed PU binder) at different test temperatures and loading frequenc
are plotted in Figure 3a. The dynamic modulus of different PU mixtures at 15 ◦ C is shown
in Figure 3b.
are plotted in Figure 3a. The dynamic modulus of different PU mixtures at 15 °C is sho
in Figure 3b.
9.0
10
8.5
5℃ 35 ℃ PUM−13/B/T PUM−13/B/S
9 8.0 PUM−13/B/H PUM−13/B/T/5.0%
15 ℃ 45 ℃
25 ℃ 55 ℃ 7.5 PUM−13/B/T/5.6% PUM−13/B/T/5.3%
Phase Angle (°)
PUM−13/L/T PUM−16/L/T
Phase Angle (°)
8
7.0 PUM−20/L/T PUM−10/B/T
7 6.5
6.0
6 5.5
5.0
5
4.5
4 4.0
0 5 10 15 20 25 0 5 10 15 20 25
(a) (b)
FigureFigure
3. The phase
3. The angle
phase angleofofthe
the PU mixtures.
PU mixtures. (a)(a)
PUMPUM−13 at different
−13 at different test temperatures
test temperatures and load
and loading
frequencies. (b) Different
frequencies. (b) DifferentPU
PUmixtures
mixtures atat1515C.°C.
◦
3.3. The Effect of Gradation on the Dynamic Modulus and Phase Angle
The dynamic modulus and phase angle results of the PU mixtures with the sam
aggregate type and different gradations at different test temperatures and loading f
quencies are plotted in Figures 4 and 5.
Coatings 2023, 13, 474 6 of 18
The dynamic modulus and phase angle results of the PU mixtures with the same ag-
gregate type and different gradations at different test temperatures and loading frequencies
are plotted in Figures 4 and 5.
3.4. The Effect of Aggregate Type on the Dynamic Modulus and Phase Angle
2023, 13, x FOR PEER REVIEW The dynamic modulus and phase angle results of the PU mixtures with the same gra-
dation and different aggregate types at different test temperatures and loading frequencies
are plotted in Figures 6 and 7.
13,000 12,000 12,000

Temp−5 ℃ Temp−15 ℃ Temp−25 ℃ PUM−13/B

14,000
12,000 11,000 11,000

13,000
10,000
11,000 10,000
12,000 9,000
10,000 9,000
11,000 8,000
9,000 8,000 7,000
10,000
PUM−13/B 8,000 6,000
7,000 5℃ 35 ℃
9,000
PUM−10/B 5,000 15 ℃ 45 ℃
7,000 6,000 25 ℃ 55 ℃
8,000 4,000
0 5 10 15 20 25 0 5 10 15 20 25 0 5 10 15 20 25
Loading Frequency (Hz) 0 5 10 15 20 25
15,000 Loading Frequency (Hz)
11,000 10,000
Temp−35 ℃ Temp−45 ℃ 9,000 Temp−55 ℃ 14,000 PUM−10/B
10,000
13,000
9,000
12,000
8,000
9,000 8,000
11,000
7,000
10,000
8,000
7,000 9,000
6,000 8,000
7,000 7,000
6,000
5,000 6,000
6,000
5,000 5,000
0 5 10 15 20 25 0 5 10 15 20 25 0 5 10 15 20 25 0 5 10 15 20 25
(a) (b)
14,000 12,000 11,000 12,000 14,000
PUM−20/L PUM−16/L
Temp−5 ℃ Temp−15 ℃ Temp−25 ℃ 13,000

11,000
13,000 11,000 10,000

10,000 12,000
12,000 11,000
10,000 9,000 9,000
10,000
8,000
11,000 9,000 8,000 9,000
7,000
8,000
10,000
8,000 7,000 6,000
7,000
PUM−20/L
9,000 5,000 6,000
PUM−16/L 7,000 6,000
4,000 5,000
8,000 PUM−13/L 6,000 5,000 3,000 4,000
0 5 10 15 20 25 0 5 10 15 20 25 0 5 10 15 20 25 0 5 10 15 20 25 0 5 10 15 20 25
10,000 9,000 13,000 PUM−13/L
Temp−35 ℃ Temp−45 ℃ 8,000 Temp−55 ℃
12,000
9,000 8,000
11,000
7,000
8,000
7,000 10,000 5℃ 35 ℃
6,000
7,000 9,000 15 ℃ 45 ℃
6,000
5,000 8,000 25 ℃ 55 ℃
6,000
5,000 7,000
5,000 4,000
6,000
4,000
4,000 3,000 5,000
0 5 10 15 20 25 0 5 10 15 20 25 0 5 10 15 20 25 0 5 10 15 20 25
(c) (d)
Figure Figure
4. The4. dynamic
The dynamic modulus
modulus of ofthe
the
PUPU mixtures
mixtures with thewith
samethe sametype
aggregate aggregate type and
and different
gradations. (a,b) Basalt aggregate, (c,d) Limestone aggregate.
6.0 7.0 8.0

6.0 7.5
5.5
6.5 5℃ 35 ℃
7.0
Angle (°)
PUM−13/B 5.5 15 ℃ 45 ℃
e Angle (°)
6.0 6.5
5.0 PUM−10/B 25 ℃ 55 ℃
6.0
5.5
5.0 5.5
4.5
6,000
5,000 7,000
5,000 4,000
6,000
4,000
4,000 3,000 5,000
0 5 10 15 20 25 0 5 10 15 20 25 0 5 10 15 20 25 0 5 10 15 20 25
(c) (d)
Coatings 2023, 13, 474 Figure 4. The dynamic modulus of the PU mixtures with the same aggregate type and
7 ofdifferent
18
6.0 7.0 8.0

6.0 7.5
5.5
6.5 5℃ 35 ℃
7.0
Phase Angle (°)

PUM−13/B 5.5 15 ℃ 45 ℃
Phase Angle (°)
6.0 6.5
5.0 PUM−10/B 25 ℃ 55 ℃
6.0
5.5
5.0 5.5
4.5
5.0 5.0
4.0 4.5 4.5
4.5
4.0
3.5 4.0 4.0 3.5
0 5 10 15 20 25 0 5 10 15 20 25 0 5 10 15 20 25
Loading Frequency (Hz) 0 5 10 15 20 25
8.0 Loading Frequency (Hz)
7.5 8.0 8.0
Temp−35 ℃ Temp−45 ℃ Temp−55 ℃ 7.5 PUM−10/B
7.0 7.5 7.5 7.0
7.0
Coatings 2023, 13,
6.5 x FOR PEER REVIEW 7.0 6.5 8 of 19
6.5 6.0
6.0 6.5
6.0 5.5
5.5 6.0
5.5 5.0
5.0 5.5 4.5
5.0
9 9 10 11 10
4.5 Temp−5 ℃ Tempe−15 ℃
5.0 Temp−25 ℃ 4.0 PUM−20/L PUM−16/L
Coatings 2023, 13, x FOR PEER REVIEW 8
4.5
8
9 10
3.5 9
8 of 19
4.0 4.0
PUM−20/L 4.5
0 5 10 15 20 25
Phase Angle (°)

0 5 10 15 20 25 0 5 10 15 20 25 80 5 10 15 20 25 9
PUM−16/L 8
Phase Angle (°)
7 PUM−13/L 7
(a) (b)
7 8
7
6 7
6 6
6
9 9 510 6 11 10
5
Temp−5 ℃ 5
Tempe−15 ℃ Temp−25 ℃ PUM−20/L PUM−16/L
5 5
49 10 9
8 8
4 PUM−20/L 4 3
Phase Angle (°)
4 4
0 5 10 15 20 25 0 5 10 15 20 25 8 0 5 10 15 20 25 90 5 10 15 20 25 0 5 10 15 20 25
PUM−16/L 8
Phase Angle (°)
Loading Frequency (Hz)

8 Loading Frequency (Hz)
7 PUM−13/L 7
7
10 11 11 9 7
Temp−35 ℃ Temp−45 ℃ 6 Temp−55 ℃ 7 PUM−13/L
6 6
10 8 6
9 10
5 6
5 59 7 5
8 9 5
8
4
5℃ 35 ℃
4 7
0 5 10 15 20 25
4
0 5 10 15 20 25
83
0 5 10 15 20 25
6 4 4 15 ℃ 45 ℃
7 0 5 10 15 20 25 0 5 10 15 20 25
6
7 5
Loading Frequency (Hz) 25 ℃ 55 ℃
6
10 11 11 9
5 Temp−35 ℃ 5 Temp−45 ℃ 6 Temp−55 ℃
4 PUM−13/L
10 8
9 10 3
4 4 5
0 5 10 15 20 25 0 5 10 15 20 25 0 5 10 15 20 25 0 5 10 15 20 25
9
8 9 7
8 (c) 5℃ 35 ℃ (d)
7 8 15 ℃ 45 ℃ 6
7
6 Figure 5. The phase

6
7 angle of the PU mixtures
5 with the same aggregate
25 ℃type and
55 different
℃ gradations.
5 (a,b) Basalt aggregate, (c,d) Limestone aggregate.
5
4
6
3
4 4 5
0 5 10 15 20 25 0 5 10 15 20 25 0 5 10 15 20 25 0 5 10 15 20 25
(c) (d)
The dynamic modulus and phase angle results of the PU mixtures with the same
Figure
Figure 5.5.The
gradation The phase
and angleofof
different
phase angle thePU
PUmixtures
aggregate
the mixtures with
types with
at thesame
same
different
the aggregate
test typeand
temperatures
aggregate type and different
and loading
different gradations.
fre-
gradations.
(a,b)
(a,b) Basalt
quencies
Basalt areaggregate, (c,d)
plotted(c,d)
aggregate, Limestone
in Figures 6 and
Limestone aggregate.
7.
aggregate.
14,000 3.4. The

12,000 Effect11,000
Temp−15 ℃
of Aggregate Type on12,000
the Dynamic Modulus and Phase Angle
PUM−13/B
Temp−5 ℃ Temp−25 ℃
The dynamic modulus and11,000

phase angle results of the PU mixtures with the same
13,000 11,000 10,000

10,000
12,000
gradation
10,000 and9,000
different aggregate
9,000types at different test temperatures and loading fre-
11,000
quencies are plotted in Figures 6 8,000
9,000
and 7.
10,000 8,000 7,000
PUM−13/B 8,000 6,000 5℃ 35 ℃
14,000
9,000 12,000 11,000 12,000
PUM−13/L
7,000
Temp−25 ℃ 5,000 PUM−13/B
15 ℃ 45 ℃
7,000
8,000
13,000 11,000 25 ℃ 55 ℃
0 5 11,000
10 15 20 25 0 5 10 15 20 2510,000 0 5 10 15 20 25 4,000
Loading Frequency (Hz) 10,000 0 5 10 15 20 25
10,000 10,000
9,000 9,000
14,000
9,000
Temp−55 ℃
PUM−13/L
11,000 13,000
8,000 8,000
9,000 9,000 12,000
8,000 8,000 7,000
10,000 11,000
7,000 10,000
8,000 PUM−13/B 8,000 6,000 5℃ 35 ℃
9,000 7,000 9,000
PUM−13/L 7,000 5,000 15 ℃ 45 ℃
7,000 7,000 6,000 8,000 25 ℃ 55 ℃
8,000
0 5 10 15 20 25 0 5 10 15 20 25 0 5 10 15 20 25 4,000
7,000
6,000 0 5 10 15 20 25
Loading Frequency (Hz) 6,000
6,000
5,000 5,000 Loading Frequency (Hz)
10,000 9,000 14,000
Temp−35 ℃ 5,000 Temp−45 ℃ Temp−55 ℃ 4,000 PUM−13/L
5,000 13,000
0 5 10 15 20 25 0 5 0 5 10
10 15 20 25 8,000 0 15 20 25 5 10 15 20 25
9,000 12,000
8,000
7,000
(a)
11,000
(b)
8,000 10,000
9,000
Figure 6. The dynamic modulus of the PU
7,000
mixtures with the same gradation and different aggregate
Figure 6. The dynamic modulus of the PU mixtures with the same gradation and different aggregate
8,000
7,000 6,000
types. (a) dynamic modulus under different 7,000 test temperatures, (b) dynamic modulus with different
6,000 types. (a) dynamic modulus under different test temperatures, (b) dynamic modulus with different
6,000 aggregate types.5,000 6,000
aggregate types. 5,000
5,000 4,000
5,000
0 5 10 15 20 25 0 5 10 15 20 25 0 5 10 15 20 25 0 5 10 15 20 25
(a) (b)
Figure 6. The dynamic modulus of the PU mixtures with the same gradation and different aggregate
types. (a) dynamic modulus under different test temperatures, (b) dynamic modulus with different
oatings 2023, 13, x FOR PEER REVIEW 9
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Coatings 2023, 13, 474 8 of 18
9 o
7.0 8.0 9.0 8.0
Temp−5 ℃ Temp−15 ℃ 8.5 Temp−25 ℃ PUM−13/B
6.5 7.5 7.5
8.0
7.0
PUM−13/B 7.0
Phase Angle (°)

6.0 7.5
Phase Angle (°)
7.0 8.0 9.0 8.06.5 5℃ 35 ℃

Temp−5 ℃
PUM−13/L 6.5 Temp−15 ℃ 8.5
7.0 Temp−25 ℃ PUM−13/B 15 ℃ 45 ℃
5.5 7.5 6.5 7.56.0
6.5
6.0 8.0 25 ℃ 55 ℃
5.0 7.0 6.0 7.05.5
Phase Angle (°)

6.0 PUM−13/B 7.5
Phase Angle (°)
5.5 5.5
7.0 6.55.0 5℃ 35 ℃
4.5 PUM−13/L 6.5
5.0 15 ℃ 45 ℃
5.5 5.0 6.5 6.04.5
6.0 4.5 25 ℃ 55 ℃
4.0 4.5 6.0 5.54.0
5.0 4.0
5.5 5.5
3.5 4.0 3.5 5.03.5
4.5 0 5 10 15 20 25 0 5 10 15 20 255.0 0 5 10 15 20 25
5.0
4.5 0 5 10 15 20 25
4.0
Loading Frequency (Hz) 4.5 10.0 Loading Frequency (Hz)
4.5 4.0
9.5 10.0 4.010.0 9.5
3.5 9.0 Temp−35 ℃ 4.09.5 Temp−45 ℃ 3.59.5 Temp−55 ℃ 3.59.0 PUM−13/L
0 5 10 15 20 25 0 5 10 15 20 25 0 5 10 15 20 25
9.0 8.5 0 5 10 15 20 25
8.5 9.0
Loading Frequency (Hz) 10.08.0 Loading Frequency (Hz)
8.0 8.5 8.5
9.5 10.0 8.0 10.0 9.57.5
7.5 Temp−35 ℃ Temp−45 ℃ 8.0
Temp−55 ℃ 9.07.0
PUM−13/L
9.0 9.5 7.5 9.5
7.0 7.5 8.56.5
8.5 9.0 7.0 9.0
6.5 8.5 6.5 7.0 8.06.0
8.0 8.5
6.0 8.0 6.0 6.5 7.55.5
7.5 8.0
5.5 7.5 5.5 6.0 7.05.0
7.0 7.5
5.0 7.0 5.0 5.5 6.54.5
6.5 7.0
4.5 6.5 4.5 5.0 6.04.0
6.0 6.5 5.5 0 5 10 15 20 25
4.0 6.0 4.0 4.5
5.5 0 5 10 15 20 25 0 5 10 15 20 256.0 0 5 10 15 20 25 5.0
5.5
5.0 5.0 5.5 4.5
4.5 4.5 5.0 (a) 4.0 (b)
4.0 4.0 4.5 0 5 10 15 20 25
0 5 10 15 20 25 0 5 10 15 20 25 0 5 10 15 20 25
Figure 7. The phase angle of the PU mixtures with the same gradation and different aggregate
(a) (a) phase angle under different test temperatures,(b)
types. (b) phase angle with different aggreg
types.
Figure 7. The phase angle of the PU mixtures with the same gradation and different aggregate
Figure 7. The phase angle of the PU mixtures with the same gradation and different aggregate types.
types.
(a)(a) phase
phase angle
angle underunder different
different test temperatures,
test temperatures, (b)with
(b) phase angle phase angleaggregate
different with different
types. aggrega
3.5. The Effect of the PU Type on the Dynamic Modulus and Phase Angle
types.
The dynamic modulus and phase angle results of the PU mixture with the same
The dynamic modulus and phase angle results of the PU mixture with the same
3.5. The Effect
dation and andof the PUPU
different Type on the Dynamic Modulus and Phase Angle
gradation different PUtypes atdifferent
types at different
testtest temperatures
temperatures and frequencies
and loading loading frequencie
are
plotted
The in
plotted inFigures
dynamic 88 and
Figuresmodulusand9.9. and phase angle results of the PU mixture with the same g
dation and different PU types at different test temperatures and loading frequencies
13,000
plotted in Figures
Temp−15 ℃
11,000
8 Temp−25
and 9.℃ 15,000
PUM−13/T
11,000
PUM−13/S
Temp−5 ℃ 12,000 14,000

12,000 10,000
10,000 13,000
11,000 9,000
11,000 12,000
13,000 9,000
11,000 15,000 11,000
10,000 Temp−15 ℃ PUM−13/T PUM−13/S
8,000
10,000 Temp−5 ℃ 12,000 Temp−25 ℃ 11,000
14,000
12,000 10,000
8,000
10,000 10,000 7,000
9,000 9,000 13,000
11,000 9,000 9,000
11,000 12,000 6,000
8,000 8,000 7,000
9,000 8,000
10,000 10,000 11,000 8,000
7,000 PUM−13/T 6,000 7,000 5,000
7,000 8,000 10,000
9,000 9,000 7,000
6,000 PUM−13/S 6,000
9,000
4,000
6,000 5,000 5,000
8,000 PUM−13/H8,000 7,000
8,000
6,000
3,000
5,000
0 5 10 15 20 25 0 5 10 15 20 25 0 5 10 15 20 25 0 5 10 15 20 25 5,000 0 5 10 15 20 25
7,000 PUM−13/T 7,000
6,000 PUM−13/S 6,000 4,000
PUM−13/H 6,000 5,000
Temp−55 ℃
13,000
5,000 PUM−13/H
5,000 Temp−35 ℃ 9,000 Temp−45 ℃ 3,000
9,0000 5 10 15 20 25 0 5 10 15 20 25 8,0000 5 10 15 20 25 12,000 0 5 10 15 20 25 0 5 10 15 20 25
8,000 7,000
Temp−55 ℃
10,000
13,000 PUM−13/H
9,000
7,000 Temp−35 ℃ 7,000
9,000
Temp−45 ℃ 5℃ 35 ℃
8,000
6,000 9,000
12,000
6,000 8,000
11,000
15 ℃ 45 ℃
8,000
6,000 8,000
7,000
5,000
5,000 7,000
10,000 25 ℃ 55 ℃
7,000
5,000
7,000 5℃ 35 ℃
6,000 6,000
9,000
4,000
4,000
6,000 5,000
8,000
15 ℃ 45 ℃
6,000
4,000
3,000
5,000
5,000
3,000 4,000
7,000 25 ℃ 55 ℃
0 5 10 15 20 25 0 5 10 15 20 25 0 5 10 15 20 25 0 5 10 15 20 25
5,000 6,000
4,000
4,000
4,000 (a) 5,000
(b)
3,000 3,000 4,000
0 5 10 15 20 25 0 5 10 15 20 25 0 5 10 15 20 25 0 5 10 15 20 25
Figure 8. The
Figure dynamic
8. The dynamicmodulus
modulus ofof the
thePU
PUmixtures
mixtures with
with the the
samesame gradation
gradation and different
and different PU PU
(a)
types. (a)(a)
types. dynamic
dynamic modulus under
modulus under different
different test temperatures, (b)dynamic
test temperatures,
(b) (b) dynamic modulus
modulus with differentwith diff
ent PU
PU8.types.
Figure types.
The dynamic modulus of the PU mixtures with the same gradation and different PU
types. (a) dynamic modulus under different test temperatures, (b) dynamic modulus with diffe
ent PU types.
Coatings 2023, 13, x FOR PEER REVIEW 1
oatings 2023, 13, x FOR PEER REVIEW 10

Coatings 2023, 13, 474 9 of 18
9 9 10 11 11
Temp−5 ℃ Temp−15 ℃ Temp−25 ℃ PUM−13/T PUM−13/S
9 10 10
9 8 9 8 10 11 11
℃ Temp−15 ℃ PUM−13/T PUM−13/S
Phase Angle (°)

Temp−5
PUM−13/T 8 Temp−25 ℃ 9
Phase Angle (°)
9 10 9
10
8 7 PUM−13/S
8 7 8
Phase Angle (°)

7
PUM−13/T
PUM−13/H 8 9 8
Phase Angle (°)
9
7 6 PUM−13/S 7 6 6
8
7
7 7
PUM−13/H 5 6 8
6 7
6 5 6 5 6
4 5 7
5 6
5 4 5 4 3 4 5
5 6
0 5 10 15 20 25 0 5 10 15 20 25
4 0 5 10 15 20 25 0 5 10 15 20 25 0 5 10 15 20 25
4
4 3 4 Loading Frequency (Hz) 5
010 5 10 15 20 25 011 5 10 15 20 25 011 5 10 15 20 25 110 5 10 15 20 25 0 5 10 15 20 25
Temp−35 ℃ Temp−45 ℃ PUM−13/H
Loading Frequency (Hz) Temp−55 ℃ Loading Frequency (Hz)
10 10
10 9 11 11 10 11
Temp−35 ℃ Temp−45 ℃ PUM−13/H
9 Temp−55 ℃ 9
8 10 9 10 5℃ 35 ℃
9 10
9
8
9
8 15 ℃ 45 ℃
8 7 9 8 5℃ 35 ℃
7 7 25 ℃ 55 ℃
6
8
7
8 15 ℃ 45 ℃
7 6 8 6
7 7 25 ℃ 55 ℃
6 5 5 7 6 5
6 6
4 4 5 4
5 0 5 10 15 20 25
5 0 5 10 15 20 6
25 0 5 10 15 20 25 5 0 5 10 15 20 25
4
0 5 10 15 20 25
4
0 5 10 (a)
15 20 25
5
0 5 10 15 20 25
4
0 5 10 15 20 25 (b)
(a) 9. The phase angle of the PU mixtures with the same
Figure (b) gradation and different PU typ
phase9.angle
Figure underangle
The phase different test
of the PUtemperatures,
mixtures with(b) phase
the sameangle with different
gradation PU types.
and different PU types.
Figure 9. The phase angle of the PU mixtures with the same gradation and different PU types.
phase angleangle
(a) phase under different
under test
different testtemperatures,
temperatures, (b)(b) phase
phase angle
angle with different
with different PU types.
PU types.
3.6. The Effect of the PU Content on the Dynamic Modulus and Phase Angle
3.6. TheThe dynamic
Effect of the PUmodulus
Content onandthephase
Dynamicangle resultsand
Modulus of Phase
the PU mixtures with the
Angle
The dynamic modulus and phase angle results of the PU mixtures with the same
gradation
gradation anddifferent
The dynamic
and different
PU PU
modulus contents
and
contents phase
at at angle
different
different test temperatures
results of the
test temperatures andPU and
mixtures
loading loading
with frequ
frequencies the s
ae plotted in Figures 10 and 11.
gradation and different PU contents at different test temperatures and loading frequen
15000
Temp-5 ℃ Temp-15 ℃ Temp-25 ℃ PUM-13/B/5.0 PUM-13/B/5.3
14000
14,000 12,000 11,000 14000
13000
13000
15000
Temp-5 ℃ Temp-15 ℃ Temp-25 ℃ PUM-13/B/5.0
12000
PUM-13/B/5.3
14000
14,00013,000 12,000 11,00010,000 14000
12000
11000
11,000 11000 13000

13000 10000
10000 12000
13,00012,000 12000 9000
11,000 10,0009,000 11000
9000 11000
10,000 8000
8000 10000
10000
12,00011,000 7000 9000
7000
PUM-13/B/5.0 9,0008,000 9000 6000
10,000 6000 8000
11,00010,000
PUM-13/B/5.3 9,000 8000
7000
5000
5000
7000 4000
PUM-13/B/5.6
PUM-13/B/5.0 6000
8,0007,000 6000 0 5 10 15 20 25 0 5 10 15 20 25
10,0009,000 0 PUM-13/B/5.3 9,000 Loading Frequency (Hz)
5000
5 10 15 20 25 0 5 10 15 20 25 0 5 10 15 20 25 5000
4000
PUM-13/B/5.6 13000 PUM-13/B/5.6
Loading Frequency (Hz) 7,000
0 5 10 15 20 25 0 5 10 15 20 25
12000
0 5
10,000 10 15 20 25 0 5 10 15 20 25 0 5
9,000 10 15 20 25
LoadingTemp-35 ℃ (Hz)
Frequency Temp-45 ℃ Temp-55 ℃ 13000 11000 PUM-13/B/5.6
9,000 12000 10000 5℃ 35 ℃
10,000 9,000
9,000 Temp-35 ℃ Temp-45 ℃ 8,000
Temp-55 ℃ 11000 9000 15 ℃ 45 ℃
9,000
8,000 10000 8000 5 ℃ 25 ℃ 35 ℃55 ℃
9,000 8,000
8,000 7,000 9000 7000 15 ℃ 45 ℃
8,000
7,000 8000 6000 25 ℃ 55 ℃
8,000 7,000
7,000 7000 5000
6,000
0 5 10 15 20 25
7,000 6000
6,000
7,000 5000
6,000 6,000
5,000 0 5 10 15 20 25
6,000
0 5 10 15 20 25 0 5 10 15 20 25 0 5 10 15 20 25
6,000
5,000
0 5 10 15 20 25 0 5 (a)
10 15 20 25 0 5 10 15 20 25 (b)
(a) 10.
Figure
Figure 10. The
Thedynamic
dynamic modulus
modulus of theofPU
the PU mixtures
mixtures (b) gradation
with
with the same the sameand
gradation
different PUand differ
contents. (a)
contents. (a) dynamic
dynamic modulus
modulus under
under differentdifferent test temperatures,
test temperatures, (b) dynamic
(b) dynamic modulus
Figure 10. The dynamic modulus of the PU mixtures with the same gradation and differen modulus
with different w
ferent PU
PU
(a) contents.
contents.
contents. dynamic modulus under different test temperatures, (b) dynamic modulus with
ferent PU contents.
oatings 2023, 13, x FOR PEER REVIEW
Coatings 2023, 13, 474 10 of 18
11
PUM-13/B/5.0 PUM-13/B/5.3

14,000
Temp-5 ℃ Temp-15 ℃ Temp-25 ℃ 14,000
14,000
12,000 11,000
12,000
13,000 12,000
11,000 10,000
10,000
12,000 10,000
9,000
10,000
8,000
11,000 8,000
PUM-13/B/5.0
8,000
10,000 PUM-13/B/5.3 9,000 6,000
6,000
PUM-13/B/5.6
7,000 4,000
9,000
0 5 10 15 20 25 0 5 10 15 20 25 0 5 10 15 20 25 0 5 10 15 20 25 0 5 10 15 20 25
10,000 9,000 PUM-13/B/5.6
Temp-35 ℃ Temp-45 ℃ Temp-55 ℃
9,000 12,000
9,000 8,000
8,000 10,000 5℃ 35 ℃
8,000 7,000 15 ℃ 45 ℃
7,000 8,000 25 ℃ 55 ℃
7,000
6,000
6,000
6,000
6,000
5,000
0 5 10 15 20 25 0 5 10 15 20 25 0 5 10 15 20 25 0 5 10 15 20 25
(a) (b)
Figure 11.11.
Figure TheThephase
phase angle
angle ofofthe
the PUPU mixtures
mixtures withwith the gradation
the same same gradation andPU
and different different
contents.PU cont
(a) phase angle
(a) phase angleunder different
under different testtest temperatures,
temperatures, (b) angle
(b) phase phase angle
with withPU
different different
contents.PU contents.
4. Discussion
4. Discussion
4.1. The Dynamic Modulus under Different Temperatures and Loading Frequency
4.1. TheFor
Dynamic Modulus under
all test temperatures, theDifferent Temperatures
dynamic modulus and Loading
monotonously Frequency
increased with the
increasing loading frequency and dropped as the test temperature increased [29], indicating
For all test temperatures, the dynamic modulus monotonously increased with
that the influence of the dynamic modulus provided by the PU binder weakened as the test
increasing
temperatureloading frequency
ascended. and dropped
This phenomenon as the
suggests thattest
the temperature
PU mixture mainly increased
exhibits[29], ind
ingelastic
that the influence
behavior of the dynamic
at low temperatures modulus
but shows viscous provided by the
behavior at high PU binder
temperatures. Thisweakene
the test temperature ascended. This phenomenon suggests that the PU mixture ma
study noted that the curves of PU mixture PUM − 13 tend to flatten out when the loading
exhibits elastic behavior at low temperatures but shows viscous behavior at high tem
frequency was higher than 10 Hz. This phenomenon indicated that the PU mixture’s
dynamic modulus was sensitive to low loading frequency, and the parameter and PU
atures.
binderThis
bothstudy noted
influenced thethat the curves
ultimate dynamicof PU mixture
modulus of the PU PUM−13
mixture.tend to flatten
This finding is out w
theconsistent
loading with frequency was of
the regularity higher than modulus
the dynamic 10 Hz. This phenomenon
of asphalt indicated
mixtures, as shown in [3],that the
mixture’s dynamicmodulus
that the dynamic modulus was
of the sensitive
asphalt mixture toincreases
low loading with thefrequency,
increase ofand the param
loading
and PU binder both influenced the ultimate dynamic modulus of the PU mixture.
frequency and decreases with the increase of test temperature.
At low temperatures, the PU mixture exhibits elastic behavior and is mainly subjected
finding is consistent with the regularity of the dynamic modulus of asphalt mixture
to PU binder, so when the temperature rises (or frequency drops), the PU binder softens and
shown
exhibits [3],
in thatbehavior,
viscous the dynamic
then leadsmodulus of the asphalt
to the increment of dynamic mixture
modulus. increases with the incr
At high temper-
of loading
atures, thefrequency
PU mixtureand decreases
mostly with the
exhibits viscous increase
behavior, and ofthetest temperature.
PU binder’s influence on
theAt low temperatures, the PU mixture exhibits elastic behavior
mixture is diminished while the interlocking force between aggregates in theand is mainly
mixture
is more pronounced. Thus, the phenomenon whereby the aggregate skeleton primarily
jected to PU binder, so when the temperature rises (or frequency drops), the PU bi
bears the loading stress becomes more apparent with additional increases in temperature
softens and exhibits
(or decreases viscous
in frequency), behavior,
which cause the then leads
decline to dynamic
of the the increment
modulusof[3,30].
dynamic
The mod
At dynamic
high temperatures,
modulus of PU mixturethe PUPUM mixture
−13 would mostly
drop by exhibits
40%~50% viscous
if the testbehavior,
temperatureand the
binder’s influence
was increased fromon the
5 ◦C mixture
to 55 is diminished while the interlocking force between
◦ C, and would drop by 20~35% if the loading frequency was
gregates
decreasedin the
frommixture
25 Hz to is
0.1more
Hz. Ali pronounced.
et al. [5] showed Thus,
that the phenomenon
the dynamic modulus whereby
of eight the ag
kinds of asphalt mixtures would drop by about 40% when the test temperature increased
gatefrom
skeleton primarily bears the loading stress becomes more apparent with additi
21.1 ◦ C to 37.8 ◦ C, and would drop by 67~80% if the loading frequency decreased
increases
from 25 inHztemperature
to 0.1 Hz. Compared(or decreases in frequency),
with the asphalt mixtures, the which cause
dynamic the decline
modulus of the of the
namic modulus
PU mixture was [3,30]. The to
less sensitive dynamic
temperature modulus of PU
and loading mixture PUM−13 would dro
frequency.
40%~50% if the test temperature was increased from 5 °C to 55 °C, and would dro
20~35% if the loading frequency was decreased from 25 Hz to 0.1 Hz. Ali et al.[5] sho
that the dynamic modulus of eight kinds of asphalt mixtures would drop by about
when the test temperature increased from 21.1 °C to 37.8 °C, and would drop by 67~
if the loading frequency decreased from 25 Hz to 0.1 Hz. Compared with the asphalt
Coatings 2023, 13, 474 11 of 18
As theoretically expected, it can be observed from Figure 2b that the dynamic modulus
of all PU mixtures was higher at lower temperatures or had a higher loading frequency,
which is the typical behavior of PU mixtures due to their viscoelastic nature.
In terms of variability in the test results, the coefficient of variation (COV) ranged
from 9 to 15%, the COV of dynamic modulus would increase with the rising of test
temperature, and the COV of different PU mixtures at the same test temperature had
no obvious significance. The COV of different PU mixtures would become higher at a
relatively low frequency.
Research indicates that the dynamic modulus of the asphalt mixture has a strong
correlation with its field rutting resistance [31]. In general, the asphalt mixture will be more
resistant to rutting (permanent deformation), the higher the dynamic modulus value [3].
From this aspect, this characteristic demonstrates that the PU mixture with PUM−10 grada-
tion and basalt aggregate had the strongest resistance to rutting (permanent deformation).
When linear viscoelastic material is subjected to dynamic loading, it presents a phe-
nomenon that the strain response lags behind the loading stress. The degree of this lag,
which manifests as a phase angle, was utilized to describe the linear viscoelastic material’s
viscoelastic properties. For a linear viscoelastic material, it is usual to expect that the
phase lag will increase as the frequency drops [32]. At all test temperatures, it is apparent
from Figure 3 that the phase lag grows as the loading frequency decreases. This trend in
the phase angle of PU mixture PUM−13 proved that the PU mixture is a kind of linear
viscoelastic material.
The linear viscoelastic material is more viscous the higher the phase angle value. There-
fore, a lower value denotes a more elastic behavior for the linear viscoelastic material [33].
From Figure 3a, it is observed that the phase angle grew as the test temperature rose, indi-
cating that the PU mixture would exhibit more viscous behavior at a higher temperature.
From Figure 3b, it can be inferred that PU mixture with different gradations, aggregate
types, and binder contents exhibited a variety of viscoelastic behaviors, and this means that
all of the aforementioned variables may have an impact on the viscoelastic behavior of the
PU mixture.
According to Witczak’s research, the dynamic modulus and the stiffness parameter
(E*/sin(δ)) of the asphalt mixture has a strong correlation with the rutting resistance of
asphalt pavement, and the stiffness parameter of the asphalt mixture can more accurately
reflect its rutting resistance at relatively high service temperatures [34]. In general, the
asphalt mixture is more resistant to rutting (permanent deformation), the greater the
stiffness parameter value [3]. It should be highlighted that the PU mixture with the basalt
aggregate and PUM−10 gradation had the highest stiffness parameter (E*/sin(δ)), or in
other words, the highest resistance to rutting.
From Figure 4b,d, the dynamic modulus of each PU mixture with a different aggregate
gradation dropped with an increase in test temperature and increased with an increase
in loading frequency. At all test temperatures and loading frequencies for basalt aggre-
gates, the dynamic modulus of PU mixture PUM−10 was greater than that of PU mixture
PUM−13, and the difference between those two PU mixtures changed slightly as the test
temperature and loading frequency changed. For limestone aggregates, the dynamic mod-
ulus of PU mixtures PUM−16 and PUM−13 were comparable, with PU mixture PUM−16
having a slightly higher dynamic modulus than PU mixture PUM−13. However, when the
test temperature rose, the difference between the two dynamic moduli became negligible.
They were both larger than PU mixture PUM−20 at all test temperatures and loading
frequencies, and the difference grew larger as the test temperature increased.
Coatings 2023, 13, 474 12 of 18
According to the discussion above, the dynamic modulus of the PU mixture with basalt
aggregates was not considerably impacted by the change in gradation. For the PU mixture
with limestone aggregates, the trend reversed. The dynamic modulus of PU mixtures did
not change with the change in the nominal maximum aggregate size of different gradations
in a simple form. This phenomenon indicated that each PU mixture should be tested before
application, and the structure combination should be selected carefully and based on the
demand of the project. For instance, the structure combination of PUM−13 gradation
(basalt aggregate) for the upper layer and PUM−16 gradation (limestone aggregate) for the
lower layer had a higher dynamic modulus than other combinations.
From Figure 5a, it can be inferred that the phase angle of PU mixtures PUM−13 and
PUM−10 were comparable, and the variation was negligible at low loading frequencies
(<5 Hz) and grew slightly as loading frequencies increased. As the loading frequency
increased, the phase angle of the PU mixture reduced. Figure 5b presented that the phase
angle was close under low temperatures (<35 ◦ C), and the variation grew as the test
temperature rose. The phase angle of the PU mixture with limestone aggregate ranked
as follows, PUM−20 > PUM−16 > PUM−13, and the difference became bigger with the
increase of test temperature, as shown in Figure 5c. According to Figure 5d, as the test
temperature rose, the phase angle of PU mixtures with limestone aggregates increased.
The gradation had a negligible impact on the phase angle of PU mixtures with basalt
aggregates, especially at low loading frequency (<5 Hz) and test temperature (<35 °C). With
a decrease in loading frequency and a rise in test temperature, the phase angle rose for PU
mixtures with limestone aggregates. So, the gradation could influence the viscoelasticity of
the PU mixture with limestone aggregate, and for the PU mixture with basalt aggregate,
but the influence was less evident for the PU mixture with basalt aggregate.
The dynamic modulus and phase angle results were analyzed statistically using the
analysis of covariance (ANCOVA). When the test temperature and loading frequency were
controlled, the statistical analysis aimed to determine if gradation appeared to have an
impact on the dynamic modulus and phase angle of the PU mixtures.
The response examined was the dynamic modulus and phase angle of the PU mixtures.
Independent variables included the three PU mixtures with limestone aggregates as fixed
factors (PUM−20/L, PUM−16/L, PUM−13/L gradation) and the two PU mixtures with
basalt aggregates as fixed factors (PUM−13/B, PUM−10/B gradation), respectively, and
two testing variables as covariates (temperature and loading frequency). The ANCOVA
results are summarized in Table 4 and detailed below. The determination of the conditions
under which samples are statistically different, was conducted using a 95% significance
level. The variables have statistically significant effects on the dynamic modulus and phase
angle if the computed p-value (i.e., significance level) is less than 0.05, otherwise, it can be
considered that the compared groups are statistically equivalent [35].
Table 4. Statistically significant effect of the aggregate gradation in the dynamic modulus and
phase angle.
Effect on Dynamic Effect on Phase

Aggregate Type Variables
Modulus Angle
Aggregate gradation Yes (p = 0.000) Yes (p = 0.000)
Temperature Yes (p = 0.000) Yes (p = 0.000)
Limestone
Loading frequency Yes (p = 0.000) Yes (p = 0.000)
Overall Yes (p = 0.000) Yes (p = 0.000)
Aggregate gradation Yes (p = 0.000) Yes (p = 0.002)
Basalt
Coatings 2023, 13, 474 13 of 18
The dynamic modulus and phase angle of the PU mixtures with various aggregate
gradations were significantly influenced by temperature and loading frequency as variables
because the p-values were less than 0.05 (p = 0.000), according to the significance values.
Therefore, the dynamic modulus and phase angle of the PU mixtures with different aggre-
gate gradations were significantly predicted by the temperature and loading frequency.
When the effects of temperature and loading frequency were taken into account, the
effect of aggregate gradation on the dynamic modulus and phase angle of the PU mixtures
was significant, with p = 0.000 and 0.002, respectively. The model as a whole was still
significant, therefore it is possible to conclude that these variables (aggregate gradation,
temperature, and loading frequency) significantly influence the dynamic modulus and
phase angle of the PU mixtures, as the p-value for the corrected model was less than 0.05
(p = 0.000).
Compared with the test results in [5], the NMAS had an insignificant influence on the
dynamic modulus and phase angle of eight kinds of asphalt mixtures, including wearing
and base course mixes.
From Figure 6, it is vital to obtain that the dynamic modulus of the PU mixtures with
basalt and limestone aggregates both increased with the rising of loading frequency and
decreased with the rising of test temperature. The dynamic modulus of the PU mixture
with limestone aggregate was larger than that of the PU mixture with basalt aggregate, and
the difference weakened with rising test temperature.
It can be learned from Figure 7 that the phase angle of the PU mixture with limestone
aggregate reduces with the rising loading frequency and increases with the increasing
test temperature. This trend contrasted with that of the PU mixture with basalt aggregate,
which was shown in Figure 5b. The phase angle of the PU mixture with limestone aggregate
was larger than that of the PU mixture with basalt aggregate, this trend means that the PU
mixture with limestone aggregates displayed more viscous properties than the PU mixture
with basalt aggregates, which indicated that the interlock of limestone aggregates was
weaker than that of basalt aggregates.
The limestone aggregate could enhance the dynamic modulus of the PU mixture
compared with the basalt aggregate, which did not comply with the anticipation. So, the
application of limestone in a PU mixture became more economical with higher resistance
to deformation. However, further criteria, such as sliding resistance, must be taken into
consideration when selecting the aggregate type for the upper layers.
In this section, the dynamic modulus of a PU mixture with PUM−13 gradation and
limestone was plotted against that of a PU mixture with PUM−13 gradation and basalt in
Figure 12. The plot displayed a nearly linear distribution of data along the line of equality
(LOE). The closer the data point is to the LOE, the effect of aggregate type on the dynamic
modulus of the PU mixture is less significant. So, the aggregate type could significantly
affect the dynamic modulus of the PU mixture.
How closely a fitting model’s unconstrained linear trend line matches the line of
equality is an indicator of its overall bias. In other words, it shows how the unconstrained
intercept and slope are close to 0 and 1, respectively. The closer the intercept is to 0 and the
slope is to 1, the lower the bias will be [36].
The equation (y = a*x + b) was used to fit the trend line of the data. The final equation
was y = 1.3211*x − 1248.42069 and the R2 was 0.99733. From the final equation, it can also
be concluded that the aggregate type may have an impact on the dynamic modulus of the
PU mixture.
The two PU mixtures with limestone and basalt acted as independent factors, while
two testing variables acted as covariates (temperature and loading frequency). The AN-
COVA results are presented in Table 5.
mixture with basalt aggregates, which indicated that the interlock of limestone aggregates
was weaker than that of basalt aggregates.
The limestone aggregate could enhance the dynamic modulus of the PU mixture
compared with the basalt aggregate, which did not comply with the anticipation. So, the
application of limestone in a PU mixture became more economical with higher resistance
Coatings 2023, 13, 474 14 of 18
to deformation. However, further criteria, such as sliding resistance, must be taken into
consideration when selecting the aggregate type for the upper layers.
14,000
Y = 1.3211*X − 1248.42069
12,000
R2 = 0.99733
10,000
PUM−13/L Line of equality
8,000
6,000
4,000
4,000 6,000 8,000 10,000 12,000 14,000
PUM−13/B
Figure 12.
Figure 12. The
The line
lineof
ofequality
equalityabout
aboutthe
thedynamic
dynamicmodulus
modulusofof
thethe
PUPU mixture
mixture with
with thethe same
same grada-
gradation
tion different
and and different aggregate
aggregate types.types.
TableIn this section,

5. Statistically the dynamic
significant effect modulus oftype
of aggregate a PUin mixture withmodulus
the dynamic PUM−13 andgradation and
phase angle.
limestone was plotted against that of a PU mixture with PUM−13 gradation and basalt in
Variables Effect on Dynamic Modulus Effect on Phase Angle
Fig. 12. The plot displayed a nearly linear distribution of data along the line of equality
Aggregate type Yes (p = 0.000) Yes (p = 0.000)
Looking at the significance values, the temperature and loading frequency as covari-
ates significantly affected the dynamic modulus and phase angle of the PU mixtures with
different aggregate types, because the p-values were less than 0.05 (p = 0.000).
Even when the effects of temperature and loading frequency were excluded, the effect
of aggregate types on the dynamic modulus and phase angle of the PU mixtures was
significant, with p = 0.000. Because the model as a whole was still significant and the
p-value for the corrected model was less than 0.05 (p = 0.000), it is possible to conclude that
these variables (aggregate type, temperature, and loading frequency) significantly affect
the dynamic modulus and phase angle of the PU mixtures.
From Figure 8, it can be observed from the plots that each of the PU mixtures with
different PU types followed the same trend mentioned above, which is that the dynamic
modulus would rise with an increase in loading frequency and fall with an increase in
test temperature. The dynamic modulus of the PU mixtures ranked as PUM−13/T >
PUM−13/H > PUM−13/S. Therefore, the PU type influenced the PU mixture’s dynamic
modulus.
The difference in PU type will influence the viscoelasticity of the PU mixture in the
same PU mixture with fixed gradation and aggregate type, which mostly reflects the change
of dynamic modulus and phase angle. In comparison to the PU mixture with the slow cure
speed PU binder, the PU mixture with the traditional cure speed PU binder had a greater
dynamic modulus. This also proved that different PU binders brought different viscoelastic
properties to the same mixture. The findings mentioned above demonstrate that the PU
binder was the source of the PU mixture’s viscoelastic property. The dynamic modulus of
the PU mixture might change depending on the type of PU employed, the phase angle of
the PU mixture only relied on the viscoelastic property of the PU binder.
It can be inferred from Figure 9 that the phase angle of PU mixtures with different
PU types followed the same trend mentioned above. According to Figure 9, the phase
angles of PUM−13/T and PUM−13/H were comparable, with the difference becoming
somewhat bigger as the temperature rose. They were both smaller than that of the PU
Coatings 2023, 13, 474 15 of 18
mixture PUM−13/S. Thus, the viscoelasticity of the PU mixture was not affected by the
6179H additive, but it was affected by the PU’s cure speed.
The three PU mixtures (PUM−13/T, PUM−13/S, and PUM−13/H) with different
PU types as fixed factors acted as independent variables, while two testing variables
(temperature and loading frequency) served as covariates. The ANCOVA results are
presented in Table 6 and are detailed below.
Table 6. Statistically significant effect of the PU type on the dynamic modulus and phase angle.

PU type Yes (p = 0.000) Yes (p = 0.000)
The dynamic modulus and phase angle of the PU mixtures with different PU types
were significantly influenced by temperature and loading frequency as covariates because
the p-values were less than 0.05 (p = 0.000), according to the significance values. Therefore,
the temperature and loading frequency were significant predictors of the dynamic modulus
and phase angle of the PU mixtures with different PU types.
The influence of the PU types on the dynamic modulus and phase angle of the PU
mixtures was significant, with p = 0.000, when the influences of temperature and loading
frequency were excluded from the calculation. Since the model, as a whole, was significant
and the p-value for the corrected model was less than 0.05 (p = 0.000), it can be inferred that
these variables (PU type, temperature, and loading frequency) significantly influence the
dynamic modulus and phase angle of the PU mixtures.
As can be seen from Figure 10, the dynamic modulus of the PU mixture with 5.6% PU
binder had the lowest value at low temperatures, the difference became insignificant as
the temperature rose. At high temperatures, the dynamic modulus of the PU mixture with
different PU binder contents had similar values. This could be explained by the fact that the
rising PU binder content did nothing to help the PU mixture’s dynamic modulus increase.
The dynamic modulus should be taken into consideration when determining the optimum
PU binder content. The dynamic modulus of the PU mixture with different PU binder
content followed the trend of the dynamic modulus decreasing with rising temperature
and increasing with growing loading frequency.
Depending on Figure 11, it can be seen that the phase angle of the PU mixture with
different PU binder contents increased as the test temperature rose, and dropped as the
loading frequency grew. The phase angle of the PU mixtures with 5.0% and 5.3% PU binder
were close and both higher than that of the PU mixture with 5.6% PU binder, this could be
attributed to the increasing PU content’s potential to aggravate strain response lag.
The three PU mixtures (5.6%, 5.3%, and 5.0%) with different PU content served as
fixed factors for the independent variables, and two testing variables (temperature and
loading frequency) served as covariates. The ANCOVA results are described below and
summarized in Table 7.
Table 7. Statistically significant effect of the PU content in the dynamic modulus and phase angle.

PU content No (p = 0.177) Yes (p = 0.000)
Coatings 2023, 13, 474 16 of 18
According to the significance values, the temperature and loading frequency as co-
variates significantly affected the dynamic modulus and phase angle of the PU mixtures
with different PU contents, because the p-values were less than 0.05 (p = 0.000). Therefore,
the temperature and loading frequency strongly predicted the dynamic modulus and the
phase angle of the PU mixtures with different PU contents.
The effect of PU contents on the dynamic modulus was non-significant with p = 0.177
even after the effects of temperature and loading frequency were excluded, but the ef-
fect on the phase angle was significant with a p-value of 0.000. The model as a whole
was significant and the p-value for the corrected model was less than 0.05 (p = 0.000), it
can be concluded that these variables (PU content, temperature, and loading frequency)
significantly influence the dynamic modulus and phase angle of the PU mixtures.
5. Conclusions
In this study, the PU mixtures with different gradations, aggregate type, PU type, and
PU content were subjected to a dynamic modulus test. The effect of gradation, aggregate
type, PU type, and PU content on the dynamic modulus and phase angle of the PU
mixtures were compared and discussed, and the statistical method of analysis of covariance
(ANCOVA) was introduced into the analysis of the effect of the different variables. Based
on the aforementioned discussion, we could draw the following conclusion:
(1) For PU mixtures, the dynamic modulus followed the trend that it would generally
be increased with the increasing loading frequency and decreased with the increasing test
temperature; however, the tendency was reversed for the phase angle. This regularity was
consistent with that of asphalt mixtures;
(2) The PU mixture is a kind of linear viscoelastic material which would exhibit elastic
properties at low temperatures and exhibit viscous properties at high temperatures;
(3) The PU mixture with PUM−10 gradation and basalt exhibited the greatest defor-
mation resistance;
(4) The dynamic modulus of the PU mixture would drop by 40%~50% if the test
temperature was increased from 5 ◦ C to 55 ◦ C, and drop by 67%~80% if the loading fre-
quency decreased from 25 Hz to 0.1 Hz. Compared with the asphalt mixtures, the dynamic
modulus of the PU mixture was less sensitive to temperature and loading frequency;
(5) The dynamic modulus and phase angle of the PU mixture were considerably
influenced by the gradation, and the influence trend did not follow the increase of nominal
maximum aggregate size. The structure combination should be selected carefully and
based on the demand of the project;
(6) The aggregate type affected the dynamic modulus and phase angle of the PU
mixture, and the dynamic modulus of the PU mixture with limestone was larger than
that of the PU mixture with basalt. The selection of aggregate type for the PU mixture,
particularly the upper layer, must be based on more factors, such as skidding resistance;
(7) The cure speed of the PU binder could also impact the dynamic modulus and phase
angle of the PU mixture, and further considerations, such as the construction window
period and ultimate stiffness, should be taken into account when choosing the PU type;
(8) The viscoelastic characteristic of the PU mixture may be greatly impacted by the
PU content. The dynamic modulus test should be taken into account when determining
the optimum PU binder content since the dynamic modulus and phase angle of the PU
mixture did not change linearly with the growing PU content and the rising PU content
did not help in the rise of stiffness of the PU mixture.
In this paper, the effect of gradation, aggregate type, PU type, and PU content was
compared and analyzed, but only the AC gradation and two kinds of aggregate types were
involved in this paper. It is still necessary to study more gradation types and aggregate
types. The impact of the variables on the changing trend of the dynamic modulus and
phase angle was discussed, and the effect on the master curve should be researched in
further study.
Coatings 2023, 13, 474 17 of 18
Author Contributions: Conceptualization, H.Z.; methodology, S.M. and B.M.; software, X.W.; valida-
tion, H.Z., X.W. and J.W.; formal analysis, H.Z.; investigation, H.Z. and S.C.; resources, W.Z., B.M.
and E.D.; data curation, H.Z., S.C., B.M., S.L. and E.D.; writing—original draft preparation, H.Z.;
writing—review and editing, S.M.; visualization, H.Z., S.C., C.S. and J.W.; supervision, S.M.; project
administration, W.Z. and S.M.; funding acquisition, W.Z.; All authors have read and agreed to the
published version of the manuscript.
Funding: This research received no external funding.
Institutional Review Board Statement: Not applicable.
Informed Consent Statement: Not applicable.
Data Availability Statement: The data that support the findings of this study are available on request
from the corresponding author, Shijie M, upon reasonable request.
Acknowledgments: We thank Guang Li for their assistance with experiments and valuable discussion.
Conflicts of Interest: The authors declare no conflict of interest.
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Keywords: polyurethane mixture; dynamic modulus; phase angle; covariance

Coatings 2023, 13, 474. https://doi.org/10.3390/coatings13020474 https://www.mdpi.com/journal/coatings

2. Materials and Methods

Table 3. The volume index results of the core specimens.

Designation γb γt Air Void (%)

2.3. Dynamic Modulus Test

2.4. Statistic Analysis

Dynamic Modulus (MPa)

7,000 PUM−13/B/T PUM−13/B/S

13,000 12,000 12,000

Dynamic Modulus (MPa)

12,000 11,000 11,000

Temp−5 ℃ Temp−15 ℃ Temp−25 ℃ 13,000

13,000 11,000 10,000

6.0 7.0 8.0

6.0 7.0 8.0

Phase Angle (°)

Phase Angle (°)

Loading Frequency (Hz)

6 Figure 5. The phase

14,000 3.4. The

The dynamic modulus and11,000

13,000 11,000 10,000

atings 2023, 13, x FOR PEER REVIEW

Phase Angle (°)

7.0 8.0 9.0 8.06.5 5℃ 35 ℃

Phase Angle (°)

Temp−5 ℃ 12,000 14,000

oatings 2023, 13, x FOR PEER REVIEW 10

Phase Angle (°)

Phase Angle (°)

11,000 11000 13000

Dynamic Modulus (MPa)

Effect on Dynamic Effect on Phase

PUM−13/L Line of equality

TableIn this section,

Variables Effect on Dynamic Modulus Effect on Phase Angle

Variables Effect on Dynamic Modulus Effect on Phase Angle

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