materials

Article
Performance Degradation and Microscopic Analysis
of Lightweight Aggregate Concrete after Exposure to
High Temperature
Weijing Yao 1,2,3, * , Jianyong Pang 1,2,3 and Yushan Liu 1
1 School of Civil Engineering and Architecture, Anhui University of Science and Technology,
Huainan 232001, China; pangjyong@163.com (J.P.); liuyushan1997@126.com (Y.L.)
2 Engineering Research Centre of Underground Mine Construction, Ministry of Education,
Huainan 232001, China
3 State Key Laboratory of Mining Response and Disaster Prevention and Control in Deep Mine,
Anhui University of Science and Technology, Huainan 232001, China
* Correspondence: yaoweijing0713@163.com




Received: 2 February 2020; Accepted: 24 March 2020; Published: 28 March 2020


Abstract: This study analyses the deterioration of mechanical properties in lightweight concrete after
exposure to room temperature (20 ◦ C) and high temperature, i.e., up to 1000 ◦ C, including changes in
visual appearance, loss of mass, and compressive strength. All-lightweight shale ceramsite aggregate
concrete (ALWAC) and semi-lightweight shale ceramsite aggregate concrete (SLWAC) are prepared
using an absolute volume method to analyse the relationships between relative ultrasonic pulse
velocity, loss rate of compressive strength, damage degree, and temperature levels. Our results show
that, under high temperature, the lightweight aggregate ceramsite concrete performs better compared
to normal concrete. After exposure to 1000 ◦ C, the ALWAC shows a strength loss of no more than
80%, while the normal concrete loses its bearing capacity, with a similar strength loss as the SLWAC.
Furthermore, the relative ultrasonic pulse velocity and damage degree are used to evaluate the effects
of high temperature on the concretes, including the voids and cracks on the surface and inside of the
specimens, which induces the deterioration of mechanical properties and contributes to the thermal
decomposition of the cementing system and the loss of cohesion at the aggregate interface. Based on
internal structure analyses, the results from this study confirm that the lightweight aggregate concrete
shows a high residual compressive strength after exposure to the high temperature.

Keywords: lightweight shale ceramsite concrete; high temperature; ultrasonic testing; performance
deterioration; microstructure

1. Introduction
Lightweight aggregate, mixed with concrete to form lightweight aggregate concrete, has been
widely used in building insulation walls, tall buildings, and bridge construction [1,2]. Compared
to the normal aggregate, the lightweight aggregate has the characteristics of lower weight, porous
surface, and strong water absorption, providing lower bulk density and large moisture content, which
not only achieves the internal curing effect and enhances the interface structure density, but also
reduces the occurrence of burst in the fire. Ceramsite is a kind of lightweight porous aggregate, added
into concrete. Currently, shale ceramsite lightweight aggregate concrete has been broadly used as
the lightweight aggregate concrete [3,4]. However, when concrete structures are subjected to high
temperature disasters, such as fire, concrete can deteriorate for a variety of reasons. Indeed, exposure
to fire and high temperature often cause serious deterioration of concrete performance. Therefore,
manufacturing high-heat-resistant concrete with high performance is considered as an important

Materials 2020, 13, 1566; doi:10.3390/ma13071566 www.mdpi.com/journal/materials

Materials 2020, 13, 1566 2 of 15

direction for future development [5,6]. This study is motivated by the laboratory test method to reveal
the degradation process of lightweight shale ceramsite concrete from room temperature (about 20 ◦ C),
to the high temperature, up to 1000 ◦ C with an interval of 100 ◦ C, which is used to simulate the
deterioration process of concrete in a high temperature environment, subjected to fire in a short time
(usually 2–3 h).
The high temperature characteristics of ceramsite concrete have been widely researched. For
instance, Zhou et al. analysed the residual strength, appearance characteristics, and microstructure
of all-lightweight concrete after experiencing high temperature [7]. Jiang et al. designed a series of
tests to analyse the high temperature characteristics of shale ceramsite with different mixing ratios,
at different temperatures [8]. He [9] and Guo et al. [10] suggested that the high temperature burst
resistance of the lightweight aggregate concrete was improved by applying an aggregate surface
covered treatment. Yoon et al. validated the excellent performance of concrete which consists of a
clay-ash-based artificial lightweight aggregate by comparing its high temperature properties against
granite-based aggregate concrete [11]. Go et al. studied the fire-resistance properties of a reinforced
lightweight aggregate concrete wall and concluded the lightweight aggregate walls maintained a
superior structure behaviour after exposure to the high temperature [12]. Current literature review
suggests that the lightweight aggregate concrete can maintain a complete structure after exposing
to the high temperature, while, the internal structure suffers from different degrees of deterioration.
However, the quantitative methods have not been used to indicate the internal damage degree of
deterioration. Currently, ultrasonic non-destructive testing method is considered as a convenient, fast,
reliable, and reproducible method for evaluating internal damage [13,14]. However, so far, limited
studies have focused on the application of the ultrasonic method for evaluating the performance of
lightweight aggregate concrete after exposure to the high temperature.
Furthermore, in recent studies, many modern laboratory methods have been used to reveal
concrete deterioration mechanism after exposure to high temperature [15,16]. For instance, X-ray
computed tomography (X-ray CT) and scanning electron microscopy (SEM) are applied to observe
the internal structure of concrete specimens after exposure to high temperature, which can disclose
fractal characteristics of fragmentation changing with temperature [17]. Moreover, SEM and energy
dispersive spectrometer (EDS) analysis are performed to analyse internal structure properties of
lightweight concrete after exposed to high temperatures [18]. In addition, nuclear magnetic resonance
and SEM techniques are combined to observe the spectrum distribution, pore size distribution, and
flaw development of concrete after exposure to high temperature [19]. A current literature review
suggests that, at present, SEM has been widely used to study the microstructure of concrete. Also,
the microscopic composition of the interface between aggregate and cementitious materials as well
as the interaction between components are considered as significant factors to further improve the
performance of materials [20]. The results from relative studies suggest new pores and channels
appeared in the concrete, in response to the high temperature. Indeed, as the temperature increased,
cement paste and hydration products became looser and adhesion between the aggregate and slurry
weakened, causing occurrence of macroscopic crack [21–24]. However, the mechanisms behind the
deterioration of concrete performance, internal damages, and microstructure changes after exposure to
high temperature have not been studied in depth. The lightweight aggregate concrete is significantly
different from normal concrete because the strong water absorbing force of the lightweight aggregate
may help to reduce the porosity and increase the micro-hardness of the interfacial transition zone [25,26].
So far, few studies have focused on the change of the interfacial transition zone in the concrete, after
exposure to high temperature. Therefore, the current study focuses on the relationship between the
mechanical properties deterioration, damage degree, and microstructure changes of the lightweight
aggregate concrete.
This study aims to (1) investigate the performance of all-lightweight and semi-lightweight shale
ceramsite concrete under high temperature, (2) analyse the strength loss rate of the lightweight
aggregate concrete after exposure to various temperatures, (3) investigate the microstructural changes
 Materials 2020, 13, x FOR PEER REVIEW 3 of 16

Materials 2020, 13, 1566 3 of 15

changes of the interfacial transition zone, using SEM, and (4) explore the mechanism of degradation
of the lightweight aggregate concrete after exposure to high temperature.
of the interfacial transition zone, using SEM, and (4) explore the mechanism of degradation of the
2. Materialsaggregate
lightweight and Methods
concrete after exposure to high temperature.

2.1.Materials
2. Raw Materials
and Methods
Cement and fly ash are used as cementitious materials. The cement, used in this study, is made
2.1. Raw Materials
of Huainan Bagongshan P·C 42.5 composite Portland cement (Huainan, China), with 3-day and 28-
Cement and fly
day compressive ash areofused
strength 29.9as cementitious
MPa materials.
and 47.7 MPa, The cement,
respectively. The used in is
fly ash this study,Ⅰ, is
Grade made of
produced
Huainan
by Huainan Pingwei Power Plant (Huainan, China). Furthermore, fine sand is used as 28-day
Bagongshan P·C 42.5 composite Portland cement (Huainan, China), with 3-day and a fine
compressive
aggregate, with strength of 29.9modulus
a fineness MPa andof 47.7
2.8.MPa, respectively.
Coarse aggregate,The fly ash
used is Grade
in this study,I, produced
includes theby
Huainan
lightweightPingwei Power
aggregate Plant
and (Huainan,
limestone China).
gravel, bothFurthermore, fine sand
with a continuous is used asofa 5–15
gradation fine aggregate,
mm. The
with a fineness
lightweight modulusisofshale
aggregate 2.8. Coarse aggregate,
ceramsite, usedby
produced in this study,
Anhui includes
Jinrui the lightweight
Building aggregate
Materials (Huainan,
and limestone
China). gravel,
The basic both with parameters
performance a continuousofgradation
the shale of 5–15 mm.
ceramsite areThe lightweight
presented aggregate
in Table is shale
1. Moreover,
ceramsite, produced by Anhui Jinrui Building Materials (Huainan, China). The basic
the water-reducing admixture, used in this study, is produced by Shanxi Qinfen Building Materials performance
parameters of the China).
Factory (Weinan, shale ceramsite are presented in Table 1. Moreover, the water-reducing admixture,
used in this study, is produced by Shanxi Qinfen Building Materials Factory (Weinan, China).
Table 1. Physical properties of shale ceramsite.
Table 1. Physical properties of shale ceramsite.
Particle Bulk Apparent Cylinder 1 h Water Silt
Performance SizeParticle Density
Bulk Density
Apparent Compressive
Cylinder 1Absorption
h Water Shape Silt Content
Performance(mm)Size (kg/m Density
3) Density
(kg/m 3) Compressive
Strength (MPa) Absorption
(by mass) (%) Shape Content (%)
(mm) (kg/m3 ) (kg/m3 ) Strength (MPa) (by mass) (%) (%)
Shale Ordinary
Shale 5–15 415 769 ≥2.5 9.5–12.0 Ordinary ≤1.6
ceramsite 5–15 415 769 ≥2.5 9.5–12.0 type ≤1.6
ceramsite type

Shale ceramsite is a kind of artificial porous lightweight aggregate, in which the outer surface
has aShale
coarseceramsite
ceramic is a kind ofwith
structure, artificial porous
visible openlightweight aggregate,
pores and cracks [27].in which
After the outerthe
dissection, surface has
core has
aa coarse ceramic structure, with visible open pores and cracks [27]. After dissection, the
large aperture with spherical holes, forming a passage with a clear network structure (Figure 1). core has a large
aperture
Because of with
thisspherical holes, forming
special structure, a passage
some cement with
paste a clear network
penetrates structure
the lightweight (Figure 1).
aggregate, Because
during the
of thismixing
fresh specialstage.
structure,
Duringsomethecement pastestage,
hardening penetrates the lightweight
the cement hydrationaggregate, during humidity
and the relative the fresh
mixing stage.
inside the During
material arethe hardening
reduced, and stage, the cement
the moisture hydration
stored inside theand the relative
ceramsite humidity
is released to inside the
internally
material
maintainare thereduced, and the
surrounding moisture
cement stored
paste andinside the ceramsitecement
the surrounding is released to internally
matrix becomesmaintain
denser andthe
surrounding cement
more uniform [28]. paste and the surrounding cement matrix becomes denser and more uniform [28].

(a) (b)
Figure 1. Micro-structures of shale ceramsite: (a) Shell, (b) Core.

2.2. Mix Design

2.2. Mix Design
According to JGJ55-2011 “Normal Concrete Mix Design Specification” [29] and JGJ51-2002
According to JGJ55-2011 “Normal Concrete Mix Design Specification” [29] and JGJ51-2002
“Lightweight Aggregate Concrete Technical Regulations” in China [30], the absolute volume method
“Lightweight Aggregate Concrete Technical Regulations” in China [30], the absolute volume method
is used to design all-lightweight and semi-lightweight aggregate concretes. The volume sand rate is
is used to design all-lightweight and semi-lightweight aggregate concretes. The volume sand rate is
40% and five types of concrete are designed, including NC, LC-100, LC-75, LC-50, and LC-25. The NC
40% and five types of concrete are designed, including NC, LC-100, LC-75, LC-50, and LC-25. The
is normal concrete, while the LC-100 represents all-lightweight shale ceramsite aggregate concrete.
Materials 2020, 13, x FOR PEER REVIEW 4 of 16

NC is normal concrete, while the LC-100 represents all-lightweight shale ceramsite aggregate
concrete. The LC-75, LC-50, and LC-25 are the semi-lightweight shale ceramsite aggregate concrete
Materials 2020, 13, 1566 4 of 15
in which the ceramsite, with a volume 75%, 50%, and 25%, respectively, is used instead of coarse
aggregate gravel. Following Kong and Yu [25], before the preparation of concrete, the ceramsite is
treated
The LC-75,withLC-50,
water and
absorption for the
LC-25 are 1 h,semi-lightweight
which can form internal curing effect.
shale ceramsite The concrete
aggregate concrete mix ratio
in which
of
theeach group iswith
ceramsite, presented in Table
a volume 75%,250%,
and the
andbasic
25%,performance
respectively,test results
is used are demonstrated
instead in Table
of coarse aggregate
3.
gravel. Following Kong and Yu [25], before the preparation of concrete, the ceramsite is treated with
water absorption for 1 h, which can form internal curing effect. The concrete mix ratio of each group is
presented in Table 2 and the basicTable 2. Mix proportions
performance of are
test results concrete.
demonstrated in Table 3.
Binding Material Coarse Aggregate Water
Table 2. Mix proportions of concrete. Water
Number Shale Sand Water Cement
Cement Fly Ash Gravel Reducer
Binding Material
Ceramsite
Coarse Aggregate
Ratio
Water Water Cement
Number
NC 421 47 856.00 Shale Ceramsite
- Sand
856.00 Water
177.84 4.68 1:0.38
Cement Fly Ash Gravel Reducer Ratio
LC-25
NC
421
421 47
47 835.06
856.00
77.92
-
702.54
856.00
168.48
177.84
4.68
4.68
1:0.36
1:0.38
LC-50
LC-25 421
421 4747 565.03
835.06 158.00
77.92 712.28
702.54 159.12
168.48 4.68
4.68 1:0.34
1:0.36
LC-75
LC-50 421
421 4747 286.37
565.03 240.24
158.00 722.01
712.28 149.76
159.12 4.68
4.68 1:0.32
1:0.34
LC-75
LC-100 421
421 4747 286.37- 240.24
324.64 722.01
731.74 149.76
140.40 4.68
4.68 1:0.32
1:0.30
LC-100 421 47 - 324.64 731.74 140.40 4.68 1:0.30

Table 3. Performances of different types of concrete.

Table 3. Performances of different types of concrete.
Compressive 28-day 28-day 28-day
Workability Compressive Strength
Workability Strength (MPa) Apparent
28-day Moisture
28-day Thermal
28-day Thermal
Number
Number (MPa)
Slump Slump Flow Density
Apparent Content
Moisture Conductivity
Conductivity
Slump Slump Flow 3-day 28-day28-dayDensity (kg/m3
(mm)
(mm) (mm)(mm)
3-day (kg/m3) ) Content
(%)(%) (W/(m·K))
(W/(m·K))
NC 175 350 14.83 38.65 2272.00 1.10 1.65
NC 175 350 14.83 38.65 2272.00 1.10 1.65
LC-25
LC-25 125125 300 300 14.29 14.29 30.6730.67 2167.30
2167.30 2.64
2.64 1.54
1.54
LC-50
LC-50 95 95 260 260 14.85 14.85 24.5124.51 2056.48
2056.48 3.01
3.01 1.32
1.32
LC-75
LC-75 75 75 240 240 15.06 15.06 24.3324.33 1913.00
1913.00 4.30
4.30 1.15
1.15
LC-100
LC-100 50 50 200 200 11.03 11.03 14.1514.15 1679.33
1679.33 5.29
5.29 0.95
0.95

As shown in Table 3, with the increase of ceramsite replacement

replacement rate,
rate, the
the concrete
concrete strength,
strength,
apparent density, thermal conductivity,
conductivity, slump,
slump, and slump flow decrease to some extent. Meanwhile,
Meanwhile,
the moisture
moisture content
contentimproves,
improves,reflecting
reflectingthe
theinternal
internal curing
curing effect
effect of ceramsite
of ceramsite pre-wetting.
pre-wetting. When
When the
the replacement
replacement rate exceeds
rate exceeds 50%,apparent
50%, the the apparent
densitydensity meets
meets the the requirements
requirements of lightweight
of lightweight concrete
concrete below
below 1950 3 , thekg/m
kg/m1950 3, the thermal conductivity of the LC-100 is 42.4% lower than that of the
thermal conductivity of the LC-100 is 42.4% lower than that of the NC, and
NC, and the compressive
compressive strength
strength reduces reduces by 63.4%.
by 63.4%.

Experimental Design
2.3. Experimental Design
Following Kong
Following Kong and
and Yu [25], the lightweight aggregate was soaked in water for 1 h, before
hour, the
before
preparation of concrete (Figure 2). Concrete test specimens with size of 100 mm × 100 mm × 100
the preparation of concrete (Figure 2). Concrete test specimens with size of 100 mm × 100 mm × 100 mm
(L × (L
mm W××WH) were
× H) cured
were forfor
cured 28 28
days, under
days, curing
under curingconditions
conditionswith
withrelative
relativehumidity of≥95%
humidityof ≥95% and
◦ C [31].
temperature of 20 ±± 22 °C [31].

Figure 2. Forming
Forming process
process of concrete.

Before the
the high
hightemperature
temperaturetreatment,
treatment,allallthe
the test
test specimens
specimens were
were dried
dried in aindrying
a drying baker
baker at
at 105
◦
5 °C
±105 ± 5forC24for 24eliminate
h to h to eliminate the influence
the influence of moisture
of moisture contentcontent and toexcessive
and to avoid avoid excessive
moisturemoisture
content
content causing burst during heating [31]. The test specimens were heated using a chamber electric
resistance furnace, with target temperature of 100, 200, 300, 400, 500, 600, 700, 800, 900, and 1000 ◦ C, and
a heating rate of 10 to 15 ◦ C/min. Reaching to the target temperature, the temperature was kept constant
Materials 2020, 13, x FOR PEER REVIEW 5 of 16

causing burst during heating [31]. The test specimens were heated using a chamber electric resistance
Materials 2020, 13, 1566 5 of 15
furnace, with target temperature of 100, 200, 300, 400, 500, 600, 700, 800, 900, and 1000 °C, and a
heating rate of 10 to 15 °C/min. Reaching to the target temperature, the temperature was kept constant
for 22hhtoto ensure
ensure achieving
achieving the the
samesame temperature
temperature for thefor the furnace
furnace and theand the parts
internal internal parts
of test of test
specimen.
specimen.
When When the temperature
the temperature of furnace
of furnace dropped about 100to◦ C,
to dropped about 100 °C, the were
the specimens specimens wereand
taken out taken
left out
for
and
48 h,left for measuring
before 48 h, beforevarious
measuring various
properties properties
[8–11]. [8–11]. Subsequently,
Subsequently, after eachthe
after each temperature, temperature,
ultrasonic
the ultrasonic
pulse velocity of pulse velocity of was
the specimens the specimens
measured usingwas measured
a non-metal using a non-metal
ultrasonic ultrasonic
test meter (NM-4B, testBeijing
meter
(NM-4B, Beijing
Koncrete EngineeringKoncrete
TestingEngineering
Technology Testing Technology
Company, Beijing,Company,
China). Two Beijing, China).
relative Two relative
measuring points
measuring
were arrangedpoints were
in each arranged
specimen in each specimen
to calculate the mean value to calculate the meanfrequency
[32]. Ultrasonic value [32].
wasUltrasonic
set up to
frequency
50 kHz andwas theset up to 50
emission kHz and
voltage wasthe emission
500 V, with voltage was 500
the sampling V, with
period theµs.
of 0.4 sampling
After theperiod of 0.4
ultrasonic
µs. After the ultrasonic
measurement, measurement,
the compression the(CSS-YAN3000,
failure test compression failure test (CSS-YAN3000,
Changchun Testing Machine Changchun
Research
Testing Machine
Institute, Changchun, Research
China) Institute, Changchun,
was carried out andChina) was carried
the relative outcompressive
residual and the relative
strengthresidual
was
compressive
calculated strength
based was
on the calculated
ratio based on the
of the compressive ratio ofof
strength theeach
compressive
specimenstrength
after highoftemperature
each specimen to
afterdryness.
the high temperature
Finally, theto the dryness.
samples Finally, the
were selected from samples
the crushedwere specimen
selected from the crushed
to analyse specimen
the microscopic
to analyse the
morphology ofmicroscopic
the interfacial morphology of the
transition zone interfacial
(S-3400N, transition
Hitachi zoneTokyo,
Limited, (S-3400N, Hitachi
Japan), Limited,
by evaluating
Tokyo,
the Japan),
joints by evaluating
of cement matrix, thethe joints of cement
lightweight aggregate, matrix,
and the lightweight
cement aggregate,
matrix. Figure and cement
3 represents the
matrix. Figure
schematic 3 represents
diagram of the testtheprocedure,
schematic including
diagram ofthe thedrying
test procedure,
baker (HK, including
Qinzhuothe drying baker
Environmental
(HK, Qinzhuo
Equipment Environmental
Testing EquipmentChina)
Company, Dongguan, Testing andCompany,
chamberDongguan, China)furnace
electric resistance and chamber
(KSW, electric
Beijing
resistance furnace (KSW, Beijing Kewei
Kewei Yongxing Instrument Company, Beijing, China). Yongxing Instrument Company, Beijing, China).

Figure 3. Test procedure.

3. Results and Discussion

3. Results and Discussion
3.1. Visual Appearance after High Temperature
3.1. Visual Appearance after High Temperature
Figure 4 demonstrates the visual appearance changes in the NC and LC-100 specimens after
Figure 4 demonstrates the visual appearance changes in the NC and LC-100 specimens after
exposure to the high temperature. As can be observed in the figure, below 800 ◦ C, similar changes are
exposure to the high temperature. As can be observed in the figure, below 800 °C, similar changes
observed in the appearance of test specimens. As the temperature increases, the colours of each group
are observed in the appearance of test specimens. As the temperature increases, the colours of each
of samples gradually convert from blue-grey to light grey and become cream-coloured at 1000 ◦ C
group of samples gradually convert from blue-grey to light grey and become cream-coloured at 1000
(Figure 4). Between 20 and 300 ◦ C, no significant changes occur in the specimens’ appearance. At this
°C (Figure 4). Between 20 and 300 °C, no significant changes occur in the specimens’ appearance. At
stage, the samples have a crisp knocking sound and no crack is observed over their surface. Between
this stage, the samples have a crisp knocking sound and no crack is observed over their surface.
300 and 500 ◦ C, the specimens’ colours darken, showing a shade of brownish colour, with a gentle
Between 300 and 500 °C, the specimens’ colours darken, showing a shade of brownish colour, with a
knocking sound. After 600 ◦ C, obvious cracks begin to appear, also, the specimens’ colours change to
gentle knocking sound. After 600 °C, obvious cracks begin to appear, also, the specimens’ colours
greyish-white, with a low knocking sound. At 800 ◦ C, the specimens’ colours become yellowish-white
change to greyish-white, with a low knocking sound. At 800 °C, the specimens’ colours become
and continuous long cracks are observed over the samples’ surfaces. These results are consistent with
yellowish-white and continuous long cracks are observed over the samples’ surfaces. These results
those ofJiang et al. [8], He et al. [9], Guo et al. [10], Gong et al. [13,32], and Ma et al. [33].
are consistent with those◦ ofJiang et al. [8], He et al. [9], Guo et al. [10], Gong et al. [13,32], and Ma et
However, after 900 C and above, coarse crack, peeling, and scaling are observed only in the NC
al. [33].
specimen. Subsequently, after 48 h, the internal cracks penetrate the surface, resulting in a severe
break of the specimen (Figure 4a). Moreover, the sample has an overall loose structure (Figure 4a).
In contrast, the all-lightweight ceramsite aggregate concrete, i.e., the LC-100, shows the advantage
of high temperature resistance (Figure 4b). After 1000 ◦ C, the integrity of the specimen is still good
and there are obvious peeling, scaling, and surface crack. For semi-lightweight ceramsite aggregate
concrete, with the reduction of ceramsite replacement rate, high temperature degradation gradually
 20℃ 200℃ 400℃ 20℃ 200℃ 400℃

Materials 2020, 13, 1566 6 of 15

600℃ 800℃ 1000℃ 600℃ 800℃ 1000℃

deepens, hence, similar effects are observed in samples LC-25 and NC. Indeed, gravel softened after
being subjected to the high temperature, causing serious strength loss, high temperature degradation,
and broken
Materials interface
2020, 13, withREVIEW
x FOR PEER the cement matrix [33,34]. 6 of 16
(a) (b)
Figure 4. Appearance changes of concrete specimens after exposure to high temperature: (a) NC; (b)
20℃
LC-100. 200℃ 400℃ 20℃ 200℃ 400℃

However, after 900 °C and above, coarse crack, peeling, and scaling are observed only in the NC
specimen. Subsequently, after 48 hours, the internal cracks penetrate the surface, resulting in a severe
break of the specimen (Figure 4a). Moreover, the sample has an overall loose structure (Figure 4a). In
contrast,600℃ 800℃ ceramsite
the all-lightweight 1000℃ 800℃ shows1000℃
600℃ i.e., the LC-100,
aggregate concrete, the advantage of
high temperature resistance (Figure 4b). After 1000 °C, the integrity of the specimen is still good and
there are obvious peeling, scaling, and surface crack. For semi-lightweight ceramsite aggregate
concrete, with the reduction of ceramsite replacement rate, high temperature degradation gradually
(a)
deepens, hence, similar effects are observed in samples LC-25 and NC. Indeed, (b) gravel softened after
beingFigure
subjected to the high
4. Appearance temperature,
Appearancechanges causing
changesofofconcrete serious
concretespecimens
specimens strength
after
after loss,
exposure
exposure high
to high
to high temperature(a)degradation,
temperature:
temperature: (a) NC;
NC; (b)
and broken
(b) interface
LC-100.
LC-100. with the cement matrix [33,34].

3.2. Mass
3.2. Mass Loss after
Loss
However, after Exposure
afterExposure to High
to
900 °C and High Temperature
Temperature
above, coarse crack, peeling, and scaling are observed only in the NC
specimen.
The Subsequently,
The mass
massloss of each
loss after 48 hours,
raw material
of each raw theconcrete
and
material internal cracks penetrate
specimens
and concrete the after
surface,
after exposure
specimens resulting
toexposure
different toindifferent
a severe
temperatures
break
are of the specimen
presented
temperatures in Figure
are (Figure
5. in4a).
presented Moreover,
Figure 5. the sample has an overall loose structure (Figure 4a). In
contrast, the all-lightweight ceramsite aggregate concrete, i.e., the LC-100, shows the advantage of
high temperature
100 resistance (Figure 4b). After 1000 °C, 100
the integrity of the specimen is still good and
there are obvious peeling, scaling, and surface crack. For semi-lightweight ceramsite aggregate
95
90with the reduction of ceramsite replacement rate, high temperature degradation gradually
concrete,
Mass fraction/%
Mass fraction/%

deepens, hence, similar effects are observed in samples 90 LC-25 and NC. Indeed, gravel softened after
80
being subjected to the high temperature, causing serious85 strengthNC
loss, high temperature degradation,
and broken interface with the cement matrix [33,34]. LC-25
Cement fly ash specimen
70 80 LC-50
Gravel
3.2. Mass Loss after
SandExposure to High Temperature LC-75
75
60 Shale ceramsite LC-100
The mass loss of each raw material and concrete specimens after exposure to different
70
0 100
temperatures are200 300 400 500
presented 600 700 5.
in Figure 800 900 1000 0 100 200 300 400 500 600 700 800 900 1000
Temperature/℃ Temperature/℃
100 100
(a) (b)
Mass 95 high temperature: (a) Raw materials;
Figure
90 5.5.Mass loss loss of materials
of materials after exposure
after exposure to
to high temperature: (a) Raw materials; (b) Concrete
Mass fraction/%
Mass fraction/%

(b) Concrete specimens.

specimens. 90
80 NC
3.2.1. Raw Materials Mass Loss after Exposure to the High 85 Temperature
3.2.1. Raw Materials Mass Loss after Exposure to the High Temperature
LC-25
The70cementCement
fly ash flytest
ash specimen
specimen (10% fly ash content)80 shows a large mass loss rate below 600 ◦ C,
LC-50
The cementGravelfly ash test specimen (10% fly ash content) shows a large mass loss rate below 600
followed by a gentle decrease. The mass loss after exposure toLC-75 1000 ◦ C is nearly 20% (Figure 5a).
°C, followed by a gentle decrease. The mass loss after exposure
Sand
75 to 1000 °C is nearly 20% (Figure 5a).
Since the main component
60main Shale ceramsiteof the cement after hydration is C-S-HLC-100(hydrated calcium silicate) gelation,
Since the component of the cement after hydration is C-S-H (hydrated calcium silicate) gelation,
below 600 ◦ C, the crystallization water, free water, and C-S-H 70 gelled adsorption water inside the test
below 6000 °C, 100the
200crystallization
300 400 500 600water, free
700 800 900water,
1000 and C-S-H gelled
0 100 200 300adsorption
400 500 600water inside
700 800 the test
900 1000
specimen are largely lost, resulted in a significant decrease in mass. Above 600 ◦ C, the C-S-H begin to
lost, resulted in a significant decrease in mass. Above 600 °C, the C-S-H begin
specimen are largelyTemperature/℃
significantly decompose. However, the decomposition mass loss is small. Temperature/℃
Therefore, the mass loss
to significantly decompose. However, the decomposition mass loss is small. Therefore, the mass loss
(a)
rate of the cement fly ash sample decreases significantly with the increase (b) of temperature and then
stabilizes
Figureto5.80%
Mass(Figure
loss of 5a).
materials after exposure to high temperature: (a) Raw materials; (b) Concrete
The mass of gravel remains unchanged below 600 ◦ C. Between 600 and 800 ◦ C, the mass loss is
specimens.
about 5%. Above 900 ◦ C, the mass loss decreases sharply, reaching 40% after exposure to 1000 ◦ C
3.2.1.
(FigureRaw5a).Materials Mass Loss
After exposure after Exposure
to high to the
temperature, theHigh
massTemperature
loss of sand is small. Indeed, the main
The cement fly ash test specimen (10% fly ash content) shows a large mass loss rate below 600
°C, followed by a gentle decrease. The mass loss after exposure to 1000 °C is nearly 20% (Figure 5a).
Since the main component of the cement after hydration is C-S-H (hydrated calcium silicate) gelation,
below 600 °C, the crystallization water, free water, and C-S-H gelled adsorption water inside the test
specimen are largely lost, resulted in a significant decrease in mass. Above 600 °C, the C-S-H begin
to significantly decompose. However, the decomposition mass loss is small. Therefore, the mass loss
Materials 2020, 13, x FOR PEER REVIEW 7 of 16

rate of the cement fly ash sample decreases significantly with the increase of temperature and then
stabilizes to 80% (Figure 5a).
The
Materials mass
2020, of gravel remains unchanged below 600 °C. Between 600 and 800 °C, the mass loss
13, 1566 is
7 of 15
about 5%. Above 900 °C, the mass loss decreases sharply, reaching 40% after exposure to 1000 °C
(Figure 5a). After exposure to high temperature, the mass loss of sand is small. Indeed, the main
component ◦ C, resulting in a
component of of gravel
gravel isis CaCO
CaCO33,, which
which decomposes
decomposes intointo CaO
CaO and
and CO
CO22 atat 600
600 to
to 820
820 °C, resulting in a
significant
significant mass
mass reduction
reduction [35].
[35].
The shaleceramsite
The shale ceramsiteshowsshowsnonomass
mass loss
loss after
after exposure
exposure to the
to the highhigh temperature.
temperature. Indeed,Indeed, the
the shale
shale ceramsite is produced by high temperature sintering of shale, where the
ceramsite is produced by high temperature sintering of shale, where the temperature of the sintering temperature of the
sintering process1000
process exceeds exceeds 1000 ◦ C. Comparing
°C. Comparing the appearance
the appearance of gravel andof shale
gravel and shale
ceramsite at ceramsite at the
the temperature
temperature of 1000 ◦ C, the gravel’s colourfrom
changes from bluish-white to snow-white
of 1000 °C, the gravel’s colour changes bluish-white to snow-white and the and the strength
strength loss is
loss is considerable (Figure 6a,b). In contrast, the ceramsite changes from brown
considerable (Figure 6a,b). In contrast, the ceramsite changes from brown to red in color, while to red in color, while
the
the sample
sample is still
is still intact
intact andandthe the strength
strength lossloss is small,
is small, indicating
indicating highhigh temperature
temperature resistance
resistance property
property of
of the ceramsite (Figure
the ceramsite (Figure 6c,d). 6c,d).

(a) (b) (c) (d)

Figure 6. Appearance
Appearance changes of gravel and ceramsite exposure to high temperature of 1000 °C:
ceramsite after exposure ◦ C:

(a) Gravel (20 °C);

◦ C); (b) Gravel (1000 °C);
◦ C); (c) Shale ceramsite (20 °C);
◦ C); (d) Shale ceramsite (1000 °C).
◦ C).

3.2.2. Concrete Specimens

3.2.2. Concrete Specimens Mass
Mass Loss
Loss after
after Exposure
Exposure to
to High
High Temperature
Temperature
From
From Figure
Figure5b,
5b,the
themass
massloss
losstrend
trend of of
each concrete
each concretespecimen
specimenis consistent, afterafter
is consistent, exposure to high
exposure to
temperature. Mass loss is controlled in 5% and 10% below 200 ◦ C and above 600 ◦ C, respectively. For
high temperature. Mass loss is controlled in 5% and 10% below 200 °C and above 600 °C, respectively.
this temperature
For this interval,
temperature the mass
interval, loss is
the mass mainly
loss caused
is mainly by the
caused byloss
theof cement
loss binderbinder
of cement and the
andmass
the
further decreases after exceeding 600 ◦ C. For the NC, the mass decreases significantly above 800 ◦ C,
mass further decreases after exceeding 600 °C. For the NC, the mass decreases significantly above 800
and mass loss loss
reaches 27.01% afterafter
exposure to 1000 ◦ C. For the LC-100, the mass loss curve is gentle
°C, and mass reaches 27.01% exposure to 1000 °C. For the LC-100, the mass loss curve is
after exceeding 600 ◦ C, reaching 11.56% after exposure to 1000 ◦ C. For semi-lightweight ceramsite
gentle after exceeding 600 °C, reaching 11.56% after exposure to 1000 °C. For semi-lightweight
aggregate
ceramsite concrete,
aggregatethe mass loss
concrete, gradually
the mass loss increases as the
gradually replacement
increases as therate decreases. rate
replacement Afterdecreases.
exposure
to 1000 ◦ C, the mass losses of the LC-75, LC-50, and LC-25 are 14.14%, 15.60%, and 18.87%, respectively.
After exposure to 1000 °C, the mass losses of the LC-75, LC-50, and LC-25 are 14.14%, 15.60%, and
The latterrespectively.
18.87%, suggests theThehighlatter
temperature
suggestsresistance
the high advantage
temperature of ceramsite,
resistance compared
advantagetoofgravel.
ceramsite,
compared to gravel.
3.3. Strength Loss after Exposure to High Temperature
3.3. Strength Loss after
The relative Exposure
residual to High Temperature
compressive strength of each concrete specimen after exposure to high
temperature are presented in Figure 7. Below 400 ◦ C, the relative residual compressive strength of
The relative residual compressive strength of each concrete specimen after exposure to high
various types of concrete changes, slightly. Moreover, under different degrees, from 100 ◦ C to 400 ◦ C,
temperature are presented in Figure 7. Below 400 °C, the relative residual compressive strength of
the strength increases, resulting in a maximum growth of about 20%. Indeed, the concrete is heated
various types of concrete changes, slightly. Moreover, under different degrees, from 100 °C to 400 °C,
from normal temperature to a secondary hydration reaction of “high temperature curing” at 400 ◦ C,
the strength increases, resulting in a maximum growth of about 20%. Indeed, the concrete is heated
which resulted in an increase in strength, similar to “steam curing” [36]. Water is evaporated from gel
from normal temperature to a secondary hydration reaction of “high temperature curing” at 400 °C,
pores by high temperature heating, but the dense concrete structure makes water different for overflow.
which resulted in an increase in strength, similar to “steam curing” [36]. Water is evaporated from
Furthermore, the crystallization water escapes inside the concrete and the concrete pore structure
gel pores by high temperature heating, but the dense concrete structure makes water different for
does not change significantly. As a result, the hydration with unhydrated cement paste continues
overflow. Furthermore, the crystallization water escapes inside the concrete and the concrete pore
to increase the strength of the cement matrix. These results are in line with the findings of recently
structure does not change significantly. As a result, the hydration with unhydrated cement paste
conducted research in this field [37–39]. Above 500 ◦ C, the compressive strength decreases sharply,
continues to increase the strength of the cement matrix. These results are in line with the findings of
because the internal pore structure of the concrete is severely roughened at 500–800 ◦ C, the C-S-H gel
recently conducted research in this field [37–39]. Above 500 °C, the compressive strength decreases
is severely dehydrated, losing the effect of cementation. Therefore, the crack expands and penetrates
sharply, because the internal pore structure of the concrete is severely roughened at 500–800 °C, the
by the cement shrinkage and gravel softening and expansion. These changes are also reflected in the
microscopic analyses (see Section 3.6). After experiencing a high temperature of 900–1000 ◦ C, the
compressive strength and bearing capacity are greatly lost.
Materials 2020, 13, x FOR PEER REVIEW 8 of 16

C-S-H gel is severely dehydrated, losing the effect of cementation. Therefore, the crack expands and
penetrates by the cement shrinkage and gravel softening and expansion. These changes are also
reflected in the microscopic analyses (see section 3.6). After experiencing a high temperature of8900–
Materials 2020, 13, 1566 of 15
1000 °C, the compressive strength and bearing capacity are greatly lost.

125

compressive strength/%
100

Relative residual
75

50 NC
LC-25
LC-50
25 LC-75
LC-100
0
0 100 200 300 400 500 600 700 800 900 1000
Temperature/℃
Figure 7.
Figure Relativeresidual
7. Relative residual compressive
compressive strength
strength of
of concrete
concrete after exposure to high temperature.

In addition,
In addition, asas it
it can
can be
be seen
seen from
from Figure
Figure 7,7, the
the strength
strength loss
loss rate
rate of
of the
the NC
NC after
after treatment
treatment at
at
1000 ◦ C is 88.5%, while the LC-100 shows a strength loss rate of 71.7%, after experiencing a high
1000 °C is 88.5%, while the LC-100 shows a strength loss rate of 71.7%, after experiencing a high
temperature of of 1000 ◦ C. The reason is that the performance of shale ceramsite changes slightly, after
1000 °C.
temperature The reason is that the performance of shale ceramsite changes slightly, after
exposure to high temperature
exposure to high temperature and and the
the strength
strength loss
loss of
of the
the lightweight
lightweight aggregate
aggregate concrete
concrete is
is mainly
mainly
caused by high temperature damage of the cement gel. For the samples LC-75,
caused by high temperature damage of the cement gel. For the samples LC-75, LC-50, and LC-25, LC-50, and LC-25,
similar to
to the
the NC,
NC, when
when the the temperature
temperature is is lower
lower than
than 400 ◦
400 °C,
C, the
the strength
strength increases
increases slightly.
slightly. After
After
similar
exposure to the high temperature of 500–1000 ◦ C, the test specimen shows a serious strength loss.
exposure to the high temperature of 500–1000 °C, the test specimen shows a serious strength loss.
Indeed, the
Indeed, the semi-lightweight
semi-lightweight ceramsite
ceramsite aggregate
aggregate concrete
concrete contains
contains both
both calcareous
calcareous gravel
gravel and
and shale
shale
ceramsite. The
ceramsite. Thecalcareous
calcareous gravel andand
gravel cement gel aregel
cement botharedecomposed by high temperature
both decomposed destruction,
by high temperature
resulting in a loss of cementation and affecting the overall strength.
destruction, resulting in a loss of cementation and affecting the overall strength.
3.4. Internal Damage after Exposure to High Temperature
3.4. Internal Damage after Exposure to High Temperature
Ultrasonic testing is performed to evaluate the internal damage of concrete specimens after
Ultrasonic testing is performed to evaluate the internal damage of concrete specimens after
exposure to high temperature. Following Gong et al. (2018) and Gong and Zhang (2019), the relative
exposure to high temperature. Following Gong et al. (2018) and Gong and Zhang (2019), the relative
ultrasonic pulse velocity and damage degree are used as evaluation parameters to eliminate the
ultrasonic pulse velocity and damage degree are used as evaluation parameters to eliminate the
influence of aggregate type, particle size, cement type, and dosage on the ultrasonic propagation
influence of aggregate type, particle size, cement type, and dosage on the ultrasonic propagation
characteristics [32,40], as follows:
characteristics [32,40], as follows:
vR = vT /v0 (1)
𝑣 = 𝑣 /𝑣 2 (1)
D = 1 − (vT /v0 ) (2)

where, vR is relative ultrasonic pulse velocity, 𝐷 = v1T −is ultrasonic

𝑣 /𝑣 pulse velocity after exposure to high (2)
temperature
where, (m/s), v0ultrasonic
vR is relative is ultrasonic pulse
pulse velocity
velocity, vTbefore exposure
is ultrasonic to high
pulse temperature
velocity (m/s), and
after exposure D is
to high
damage degree.
temperature (m/s), v0 is ultrasonic pulse velocity before exposure to high temperature (m/s), and D is
Figure
damage degree.8 represents the processed data. The regression fitting was performed using a suitable
function and the fitting the
Figure 8 represents results are shown
processed data. in
TheTable 4. Based
regression on was
fitting our performed
results, theusing
two ultrasonic
a suitable
parameters
function andofthe
the fitting
main frequency
results areand the amplitude
shown in Table 4.ofBasedthe concrete
on ourspecimens after
results, the twoexposure to
ultrasonic
different temperatures are somehow similar, indicating that these two types parameters
parameters of the main frequency and the amplitude of the concrete specimens after exposure to are unsuitable
for evaluating
different and analysing
temperatures are the performance
somehow changes
similar, of concrete
indicating that after
theseexposure
two typesto high temperature.
parameters are
This is consistent with the conclusions of the relevant research [32,40,41].
unsuitable for evaluating and analysing the performance changes of concrete after exposure to high
As can beThis
temperature. seenisinconsistent
Figure 8, the relative
with ultrasonic pulse
the conclusions of thevelocity
relevant and damage
research degree of each concrete
[32,40,41].
specimen have a good correlation with the heating temperature. As the heating temperature increases,
the relative ultrasonic pulse velocity gradually decreases, and damage degree increases continuously,
indicating that the internal damage of the test specimen accumulates at high temperatures [14]. It
can be seen from the fitting results that the fitting effect of each concrete is good, indicating that it is
reasonable and feasible to evaluate the internal damage of concrete after exposure to high temperature
using ultrasonic parameters (Table 4). In addition, with the ceramsite addition decreasing of LC-100,
LC-75, LC-50, and LC-25, the fitting formula is closer to NC.
Materials 2020, 13, 1566 9 of 15
Materials 2020, 13, x FOR PEER REVIEW 9 of 16

Relvative ultrasonic pulse velocity 1.2

1.0

1.0 0.8

Damage degree
0.8 0.6

0.6 0.4
NC Fitted line
0.4 NC Fitted line LC-25 Fitted line
LC-25 Fitted line 0.2
LC-50 Fitted line
LC-50 Fitted line LC-75 Fitted line
0.2 LC-75 Fitted line 0.0 LC-100 Fitted line
LC-100 Fitted line
0.0 0 100 200 300 400 500 600 700 800 900 1000
0 100 200 300 400 500 600 700 800 900 1000
Temperature/℃ Temperature/℃
(a) (b)
Figure 8. Relationship between ultrasonic parameters and temperature of concrete: (a) Relationship
between relative ultrasonic pulse velocity and temperature; (b) Relationship between damage degree
and temperature.

Table 4. Fitting results of ultrasonic parameter and temperature of concrete.

Table 4. Fitting results of ultrasonic parameter and temperature of concrete.

Number
Relative
Relative Ultrasonic
Ultrasonic Pulse
Pulse Velocity
Velocity vRvR2 Damage
Damage DD 2
Degree
Degree
Number Fitting Formula R Fitting Formula R 2
Fitting Formula R2 Fitting Formula R
0.58
NC T.
vR = −22.15𝑇1000 + 1.33 0.98 D = 1.64T0.13 − 2.97 0.97
NC
LC-25 𝑣 v ==−22.15 T0.66 + 1.33
−11.751000
0.98
0.96 D = 1.64T0.13 − 2.97
D = 0.39T0.26 − 1.38
0.97
0.94
R 1000 + 1.29
1.03
LC-50 T
vR = −0.83 𝑇1000 . + 1.13 0.98 D = 0.05T0.51 − 0.56 0.97
LC-25
LC-75 𝑣 v= −11.75
= −8.83 T 0.69
+
+ 1.29
1.28 0.96
0.98 D D== 0.34T 0.26 − 1.38
0.39T0.28 − 1.35 0.94
0.97
R 1000
1000
0.69
LC-100 T
vR = −7.77 1000 + 1.24 0.95 D = 0.07T 0.45 − 0.64 0.93
𝑇 .
LC-50
Note: 𝑣 = −0.83
vR represents relative + 1.13
ultrasonic pulse 0.98 damage D
velocity; D represents = 0.05T
degree;
0.51 − 0.56 temperature.
T represents 0.97
1000
𝑇 .
+ 1.28
LC-75 0.98 𝑣 = −8.83
D = 0.34T0.28 − 1.35 0.97
1000
3.5. The Relationship between Internal Damage and Strength Loss
𝑇 .
LC-100
According 𝑣 =7,
to Figure −7.77 + 1.24specimens
the concrete 0.95 D = 0.07T
show a slight 0.45 − 0.64
increase in strength0.93
due to
1000
“high temperature curing” within 400 ◦ C and the ultrasonic propagation is affected by many factors. The
Note: vR represents relative ultrasonic pulse velocity; D represents damage degree; T represents temperature
relative ultrasonic pulse velocity and damage degree continue to increase with the heating temperature,
which fails to reflect this change. Therefore, discussing the relationship between relative ultrasonic
As can be seen in Figure 8, the relative ultrasonic pulse velocity and damage degree of each
pulse velocity, damage degree, and strength loss, we do not consider the impact of this segment. The
concrete specimen have a good correlation with the heating temperature. ◦As the heating temperature
fitting effect is optimal after deducting the temperature range of 100–200 C.
increases, the relative ultrasonic pulse velocity gradually decreases, and damage degree increases
Figure 9 shows
continuously, the relationship
indicating betweendamage
that the internal the relative ultrasonic
of the pulse velocity,
test specimen damageat
accumulates degree,
high
and the compressive strength loss rate of each concrete specimen. The appropriate
temperatures [14]. It can be seen from the fitting results that the fitting effect of each functions
concrete are
is used
good,
for regression
indicating thatanalysis (Table 5).and
it is reasonable Based on the
feasible results, the
to evaluate thecorrelation coefficient
internal damage R2 is greater
of concrete after than 0.90,
exposure
and the temperature
to high fitting result is good,
using indicating
ultrasonic that the non-destructive
parameters testing method
(Table 4). In addition, with theis feasible
ceramsiteto addition
evaluate
the compressive strength loss rate with the relative ultrasonic pulse and
decreasing of LC-100, LC-75, LC-50, and LC-25, the fitting formula is closer to NC. damage degree. In addition,
similar to the fitting relationship between the ultrasonic parameters and heating temperature, with
decreasing ceramsite
3.5. The Relationship content
between in theDamage
Internal semi-lightweight
and Strengthaggregate
Loss concrete, the fitting relationship is
closer to the NC.
According to Figure 7, the concrete specimens show a slight increase in strength due to “high
temperature curing” within 400 °C and the ultrasonic propagation is affected by many factors. The
relative ultrasonic pulse velocity and damage degree continue to increase with the heating
temperature, which fails to reflect this change. Therefore, discussing the relationship between relative
ultrasonic pulse velocity, damage degree, and strength loss, we do not consider the impact of this
segment. The fitting effect is optimal after deducting the temperature range of 100–200 °C.
Figure 9 shows the relationship between the relative ultrasonic pulse velocity, damage degree,
and the compressive strength loss rate of each concrete specimen. The appropriate functions are used
for regression analysis (Table 5). Based on the results, the correlation coefficient R2 is greater than
0.90, and the fitting result is good, indicating that the non-destructive testing method is feasible to
evaluate the compressive strength loss rate with the relative ultrasonic pulse and damage degree. In
addition, similar to the fitting relationship between the ultrasonic parameters and heating
temperature,
Materials 2020, 13,with
1566 decreasing ceramsite content in the semi-lightweight aggregate concrete, 10 ofthe
15
fitting relationship is closer to the NC.

Compressive strength loss rate/%

Compressive strength loss rate/%

100 100
NC Fitted line
NC Fitted line
80 LC-25 Fitted line 80 LC-25 Fitted line
LC-50 Fitted line LC-50 Fitted line
60 LC-75 Fitted line 60 LC-75 Fitted line
LC-100 Fitted line LC-100 Fitted line
40 40

20 20

0 0

-20 -20

0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1.0
Relative ultrasonic pulse velocity Damage degree
(a) (b)
Figure 9. Relationship between ultrasonic parameters and compressive strength loss rate of concrete
temperature: (a) Relationship between relative ultrasonic pulse velocity and
after exposure to high temperature:
compressive strength loss rate; (b) Relationship between damage degree and compressive strength
loss rate.

Table 5. Fitting results between ultrasonic parameter and compressive strength loss rate of concrete
Table 5. Fitting results between ultrasonic parameter and compressive strength loss rate of concrete
after exposure to high temperature.
after exposure to high temperature.
Relative Ultrasonic Pulse Velocity vR Damage Degree D
Number Relative Ultrasonic Pulse Velocity v2R Damage Degree D
Number Fitting formula R Fitting Formula R2
Fitting formula R2 Fitting Formula R2
Ct = −79.49lnvR − 46.53
CCt t==0.24e
NC 0.93 6.32D − 24.36
0.24e6.32D 0.92
NC Ct = −79.49lnvR − 46.53 0.93 − 24.36 0.92
LC-25 Ct = −79.66lnvR − 41.65 0.98 Ct = 0.35e5.99D5.99D − 24.63 0.97
LC-25
LC-50
Ct = −79.66lnvR − 41.65
Ct = −73.20lnvR − 30.24
0.98
0.94
CCt ==0.35e
0.68e 5.27D−−24.63
18.34
0.97
0.96
t
LC-50
LC-75 CCt t== −84.01lnv
−73.20lnvRR−−21.81
30.24 0.94
0.96 CCt t==0.68e
6.51e3.06D−−18.34
5.27D
25.57 0.96
0.97
LC-75
LC-100 CCt t== −88.15lnv
−84.01lnvRR−−24.15
21.81 0.96
0.97 CCt =t= 6.51e
0.75e3.06D −−
5.35D 25.57
9.00 0.97
0.99
LC-100 C t = −88.15lnv R − 24.15 0.97 C t = 0.75e 5.35D − 9.00 0.99
Note: vR represents relative ultrasonic pulse velocity; D represents damage degree; Ct represents compressive
Note:strength loss rate.relative ultrasonic pulse velocity; D represents damage degree; Ct represents compressive
vR represents
strength loss rate.
3.6. Microscopic Analysis
3.6. Microscopic Analysis
3.6.1. Analysis of High Temperature Degradation Process of Cement Paste
3.6.1.Figure
Analysis 10 of High Temperature
demonstrates DegradationofProcess
the microstructure the NCofcement
CementpastePasteafter exposure to different
temperatures.
Figure 10Under normal temperature,
demonstrates the cement
the microstructure hydration
of the pastepaste
NC cement is tightly
aftercombined,
exposurethe to structure
different
is complete and different phases are dense and continuous. Furthermore,
temperatures. Under normal temperature, the cement hydration paste is tightly combined, the crystal water and thea
large amount of gel are existed at this stage.are
After exposing to temperature of 200–400 ◦
structure is complete and different phases dense and continuous. Furthermore, theC, no obvious
crystal water
changes in the microstructure are observed. However, the internal free water
and a large amount of gel are existed at this stage. After exposing to temperature of 200–400 °C, no and capillary water
vaporize and evaporate.
obvious changes Moreover, the C-S-H
in the microstructure gel adsorption
are observed. waterthe
However, is lost, promoting
internal cement
free water andhydration
capillary
reaction to formand
water vaporize “high temperature
evaporate. curing”.
Moreover, the Hence, theadsorption
C-S-H gel compressive strength
water is promoting
is lost, improved. cement
Above
600 ◦ C, a large amount of water is lost and lots of pores appear on the gelled surface. Furthermore, the
hydration reaction to form “high temperature curing”. Hence, the compressive strength is improved.
gel is decomposed,
Above 600 °C, a large the structure
amount of ofthe cement
water paste
is lost is destroyed,
and lots of poresthe appear
structureonis the
loose and slack.
gelled At
surface.
this temperature,
Furthermore, thethe
gelmacroscopic
is decomposed, performance shows
the structure ofwhitening
the cement ofpaste
the specimen and cracks
is destroyed, appear on
the structure is
the surface. At 800–1000 ◦ C, further decomposition and generation of loose and porous materials result
loose and slack. At this temperature, the macroscopic performance shows whitening of the specimen
in
andthe appearance
cracks appearof onathe
large number
surface. Atof long and
800–1000 wide
°C, cracks
further on the surface
decomposition andof generation
the specimens. Afterand
of loose 48
h, the specimens are damaged and peeled off and a large amount of coarse aggregate are peeled off
from the cement paste, and the interface adhesion force is attenuated or even lost. The compressive
strength decreases by more than 70% after treatment of 800 ◦ C and the bearing capacity is basically lost
after exposure to 1000 ◦ C [42,43].
porous materials result in the appearance of a large number of long and wide cracks on the surface
of the specimens. After 48 h, the specimens are damaged and peeled off and a large amount of coarse
aggregate are peeled off from the cement paste, and the interface adhesion force is attenuated or even
lost. 2020, 13, 1566 strength decreases by more than 70% after treatment of 800 °C and the bearing
The compressive
Materials 11 of 15
capacity is basically lost after exposure to 1000 °C [42,43].

(a) (b)

(c) (d)

(e) (f)
Figure
Figure 10.10. Micro-structures
Micro-structures of cement
of cement matrix
matrix of NC
of NC after
after exposure
exposure to different
to different temperature:
temperature: (a) (a) 20 ◦ C,
20 °C,
◦ ◦ ◦ ◦ ◦
(b)(b) °C, (c)
200200 C, (c) °C, (d)
400400 C, (d) °C, (e)
600600 C, (e) °C, (f)
800800 C, 1000 °C. C.
(f) 1000

3.6.2. Analysis of High Temperature Degradation in Transition Zone of the Lightweight

3.6.2. AnalysisConcrete
Aggregate of High Temperature Degradation in Transition Zone of the Lightweight Aggregate
Concrete
Figure 11 shows the evolution process of high temperature degradation in the interface transition
Figure
zone of the11LC-100.
showsAt the evolution
normal process the
temperature, of ceramsite
high temperature
is bondeddegradation
with cement in the interface
matrix, the cement
transition
matrix structure is dense, and no defects, such as cracks and holes, are existed over thematrix,
zone of the LC-100. At normal temperature, the ceramsite is bonded with cement surfaces.
theHowever,
cement matrix
above structure is dense,
400 ◦ C, a great waterand nooccurs
loss defects,
insuch as crackszone,
the interface and causing
holes, are
theexisted over the
stratification and
surfaces. However, above 400 °C, a great water loss occurs in the interface zone, causing
looseness of the cement paste. However, no obvious signs of hole defects are observed and the bonding the
stratification and looseness
between ceramsite of thematrix
and cement cementremains
paste. However,
very strong. no The
obvious signs ofmeshing
mechanical hole defects are is
structure
observed and the bonding between ceramsite and cement matrix remains very
undamaged and the macroscopic performance is slightly improved. The compressive strength of the strong. The
specimen increases by 13.8% at 200 ◦ C. Above 600 ◦ C, the cement paste is decomposed and destroyed,
resulting in appearance of obvious cracks, holes, and interpenetration. After exposure to 800–1000 ◦ C,
the cement paste is loose and the adhesion to the ceramsite is weakened or even disappeared, resulting
in a serious loss of macro strength. The strength loss was 60.1% at 800 ◦ C and 71.7% at 1000 ◦ C.
mechanical meshing structure is undamaged and the macroscopic performance is slightly improved.
The compressive strength of the specimen increases by 13.8% at 200 °C. Above 600 °C, the cement
paste is decomposed and destroyed, resulting in appearance of obvious cracks, holes, and
interpenetration. After exposure to 800–1000 °C, the cement paste is loose and the adhesion to the
ceramsite is weakened
Materials 2020, 13, 1566 or even disappeared, resulting in a serious loss of macro strength. The strength
12 of 15
loss was 60.1% at 800 °C and 71.7% at 1000 °C.

(a) (b)

(c) (d)

(e) (f)
Figure
Figure 11.11. Micro-structures
Micro-structures of interfacial
of interfacial transition
transition zonezoneof of LC-100
LC-100 after
after exposure
exposure to to different
different
◦ C, (b) 200 ◦ C, (c) 400 ◦ C, (d) 600 ◦ C, (e) 800 ◦ C, (f) 1000 ◦ C.
temperature: (a) 20 °C, (b) 200 °C, (c) 400 °C, (d) 600 °C, (e) 800 °C, (f) 1000 °C.
temperature: (a) 20

Ceramsite
Ceramsite is is
anan excellent
excellent high
high temperature
temperature resistance
resistance material.
material. Microscopic
Microscopic characteristics
characteristics of of
shell and core ◦ ◦
shell and core atat
thetheroom
roomtemperature
temperature(i.e., 20°C)
(i.e.,20 C) (Figure
(Figure 1)
1) and
and after
after treatment
treatment of 1000 °C
of1000 C (Figure
(Figure12)
12) suggests that after exposure to high temperature, some defects, such as holes, are observed in in
suggests that after exposure to high temperature, some defects, such as holes, are observed thethe
porous ceramic material in the outer shell, however, the internal structure remains intact (Figure 12).12).
porous ceramic material in the outer shell, however, the internal structure remains intact (Figure
Therefore,
Therefore, thethe strength
strength loss
loss of of
thethe lightweight
lightweight aggregate
aggregate concrete
concrete after
after exposure
exposure to to high
high temperature
temperature
is mainly due to the weakening of cement paste and the loss of interfacial adhesion. Because of of
is mainly due to the weakening of cement paste and the loss of interfacial adhesion. Because thethe
integrity
integrity of of ceramsite,
ceramsite, nono softeningand
softening anddecomposition
decompositionofofcalcareous
calcareousaggregate
aggregate occur
occur inin the
the samples.
samples. In
the macroscopic view, the specimen is complete, with no peeling and lack of corners. This also explains
why the high-temperature strength loss of the lightweight aggregate concrete is better compared to
the NC.
Materials 2020, 13, x FOR PEER REVIEW 13 of 16

In the macroscopic
Materials 2020, 13, 1566 view, the specimen is complete, with no peeling and lack of corners. This
13 also
of 15
explains why the high-temperature strength loss of the lightweight aggregate concrete is better
compared to the NC.

(a) (b)
◦ C:
Micro-structures of shale ceramsite after exposure to 1000 °C:
Figure 12. Micro-structures (a) Shell; (b) Core.

4. Conclusions
4. Conclusions
Compared to
Compared to the
the normal
normal concrete,
concrete, thethe all-lightweight
all-lightweight shale shale ceramsite
ceramsite aggregate
aggregate concrete
concrete has has aa
great advantage,
great advantage, due due to its high temperature performance. Based on our experimental
to its high temperature performance. Based on our experimental research, after research, after
exposure to 1000 ◦ C, the all-lightweight shale ceramsite aggregate concrete specimen remains intact,
exposure to 1000 °C, the all-lightweight shale ceramsite aggregate concrete specimen remains intact,
without any
without any damage
damageand andpeeling.
peeling.Under
Underthis thistemperature,
temperature, thethe
mass
mass andandcompressive
compressive strength
strengthlossloss
are
11.56% and 71.7%, respectively, while under the same temperature, these
are 11.56% and 71.7%, respectively, while under the same temperature, these values for the normal values for the normal concrete
are 27.01%
concrete and
are 88.5%,and
27.01% respectively. Furthermore,Furthermore,
88.5%, respectively. the strength loss the rate of the loss
strength semi-lightweight
rate of the semi- shale
lightweight shale ceramsite aggregate concrete is similar to the normal concrete, because ofhigh
ceramsite aggregate concrete is similar to the normal concrete, because of the multiple effects of the
temperature softening of calcareous gravel, high temperature decomposition,
multiple effects of high temperature softening of calcareous gravel, high temperature decomposition, and decomposition of the
cement
and paste. In contrast,
decomposition of the thecement
ceramsite lightweight
paste. aggregate
In contrast, the is an excellent
ceramsite high temperature
lightweight aggregate resistant
is an
material, resulting in a limited loss of mass and strength after exposure
excellent high temperature resistant material, resulting in a limited loss of mass and strength after to the high temperature.
A comparative
exposure to the high analysis
temperature. of the relationship between relative ultrasonic pulse velocity, damage
degree, heating temperature,
A comparative analysis ofand the compressive
relationship betweenstrength relative
loss rateultrasonic
suggest that pulsewith increasing
velocity, damage the
heating temperature, the relative ultrasonic pulse velocity decreases
degree, heating temperature, and compressive strength loss rate suggest that with increasing the gradually, while the damage
degree and
heating the compressive
temperature, strength
the relative loss ratepulse
ultrasonic increase. The decreases
velocity fitting effect of the regression
gradually, while the formula
damage is
good, suggesting that it is reasonable and feasible to use relative ultrasonic
degree and the compressive strength loss rate increase. The fitting effect of the regression formula is pulse velocity and damage
degreesuggesting
good, as evaluation thatparameters
it is reasonable to judge the performance
and feasible to use relative degradation
ultrasonic ofpulse
concrete afterand
velocity exposure
damage to
high temperature.
degree as evaluation parameters to judge the performance degradation of concrete after exposure to
high Microscopic
temperature.analysis of the interfacial transition zone between the cement paste and the lightweight
aggregate after exposure
Microscopic analysis to of
different temperatures
the interfacial show that
transition zone as the temperature
between the cementincreases,
pastetheand
cement
the
gel is loosened
lightweight and dispersed
aggregate after from compaction
exposure and the
to different bond strengthshow
temperatures with thethataggregate is gradually
as the temperature
lost, resulting
increases, in loss of
the cement gelmacroscopic
is loosened and strength.
dispersedHowever, the lightweight
from compaction and theaggregate ceramsite
bond strength withis not
the
significantly damaged after exposure to high temperature, suggesting
aggregate is gradually lost, resulting in loss of macroscopic strength. However, the lightweight its excellent high temperature
resistant property,
aggregate ceramsitewhich is notissignificantly
the main reason damagedthat theafterresidual
exposure strength
to highoftemperature,
the lightweight aggregate
suggesting its
concrete is higher than that of normal concrete after exposure to the high
excellent high temperature resistant property, which is the main reason that the residual strength of temperature.
In addition,
the lightweight throughconcrete
aggregate experimental
is higher research,
than that it can be concluded
of normal concrete thatafter there
exposureis anto objective
the high
relationship
temperature. between the deterioration of mechanical properties, damage degree, and microstructure
changes of the lightweight
In addition, through aggregate
experimentalconcrete. After undergoing
research, different degrees
it can be concluded that thereof high temperature,
is an objective
the cement hydrates are thermally decomposed, causing voids and cracks
relationship between the deterioration of mechanical properties, damage degree, and microstructure on the surface and inside of
the concrete specimen, which is the primary reason for the deterioration
changes of the lightweight aggregate concrete. After undergoing different degrees of high of mechanical properties and
the increase ofthe
temperature, damage
cementdegree.hydrates are thermally decomposed, causing voids and cracks on the surface
and
Authorinside of the concrete
Contributions: specimen, which
Conceptualization, W.Y.;ismethodology,
the primary W.Y.;
reason for the
formal deterioration
analysis, W.Y. andof mechanical
Y.L.; resources,
properties and the increase of damage degree.
J.P.; data curation, W.Y.; writing—original draft preparation, W.Y.; writing—review and editing, W.Y. and Y.L.;
supervision, J.P.; project administration, J.P.; funding acquisition, W.Y. and J.P. All authors have read and agreed to
the published version of the manuscript.
Materials 2020, 13, 1566 14 of 15

Funding: This research was funded by the Funding Project of Anhui University of Science and Technology
(Grant Number QN2019115), Introduced Talent Research Funding of Anhui University of Science and Technology
(Grant Number 13190022).
Conflicts of Interest: The authors declare that there are no conflicts of interest regarding the publication of
this paper.

References
1. Wu, T.; Liu, X.; Wang, N.N.; Xing, G.; Liu, B. Experimental study on shear behavior flexural members made
of high-strength lightweight aggregate concrete. China Civ. Eng. J. 2014, 47, 40–48.
2. Ting, T.Z.H.; Rahman, M.E.; Lau, H.H.; Ting, M.Z.Y. Recent development and perspective of lightweight
aggregates based self-compacting concrete. Constr. Build. Mater. 2019, 201, 763–777. [CrossRef]
3. Zhang, D.X.; Yang, W.J. Experimental research on bond behaviors between shale ceramsite lightweight
aggregate concrete and bars through pullout tests. J. Mater. Civ. Eng. 2015, 27, 06014030. [CrossRef]
4. Huang, J.K.; Pang, J.Y.; Liu, G.C.; Mo, Y.X.; Jiang, P.W.; Su, Q. A new heat insulation shotcrete mixed with
basalt and plant fibers. Adv. Civ. Eng. 2019, 2019, 6376807. [CrossRef]
5. Peng, G.F.; Niu, X.J.; Cheng, K. Research on fire resistance of ultra-high-performance concrete: A review.
Mater. Rev. A Rev. Pap. 2017, 31, 17–23.
6. Tanyildizi, H.; Coskun, A. The effect of high temperature on compressive strength and splitting tensile
strength of structural lightweight concrete containing fly ash. Constr. Build. Mater. 2008, 22, 2269–2275.
[CrossRef]
7. Zhou, M.Z.; Sun, Q.X.; Cao, W.Z.; Xue, H.R.; Qiao, H.X. The light-wide concrete performance and its
microscopic analysis after high temperature. Build. Sci. 2009, 25, 30–33.
8. Jiang, Y.C.; Huo, D.; Teng, H.W.; Qiao, Y. Study on performance of shale ceramsite concrete after exposure to
high temperature. J. Build. Mater. 2013, 16, 888–893.
9. He, K.C.; Guo, R.X.; Ma, Q.M.; Yan, F.; Lin, Z.W.; Sun, Y.L. Experimental research on high temperature
resistance of modified lightweight concrete after exposure to elevated temperatures. Adv. Mater. Sci. Eng.
2016, 2016, 5972570. [CrossRef]
10. Guo, R.X.; He, K.C.; Ma, Q.M.; Yan, F.; Lin, Z.W.; Sun, Y.L. Compressive properties and microstructure of
modified lightweight aggregate concrete after exposure to elevated temperatures. J. Build. Mater. 2017, 20,
333–338.
11. Yoon, M.; Kim, G.; Choe, G.C.; Lee, Y.; Lee, T. Effect of coarse aggregate type and loading level on the high
temperature properties of concrete. Constr. Build. Mater. 2015, 78, 26–33. [CrossRef]
12. Go, C.-G.; Tang, J.-R.; Chi, J.-H.; Chen, C.-T.; Huang, Y.-L. Fire-resistance property of reinforced lightweight
aggregate concrete wall. Constr. Build. Mater. 2012, 30, 725–733. [CrossRef]
13. Gong, J.Q.; Deng, G.Q.; Shan, B. Performance evaluation of RPC exposed to high temperature combining
ultrasonic test: A case study. Constr. Build. Mater. 2017, 157, 194–202. [CrossRef]
14. Lin, Y.; Hsiao, C.; Yang, H.; Lin, Y.-F. The effect of post-fire-curing on strength–velocity relationship for
nondestructive assessment of fire-damaged concrete strength. Fire Saf. J. 2011, 46, 178–185. [CrossRef]
15. Thomas, C.; Rico, J.; Tamayo, P.; Ballester, F.; Setién, J.; Polanco, J.A. Effect of elevated temperature on the
mechanical properties and microstructure of heavy-weight magnetite concrete with steel fibers. Cem. Concr.
Compos. 2019, 103, 80–88. [CrossRef]
16. Ma, Q.M.; Guo, R.X.; Zhao, Z.M.; Lin, Z.W.; He, K.C. Mechanical properties of concrete at high temperature-A
review. Constr. Build. Mater. 2015, 93, 371–383. [CrossRef]
17. Zhao, X.; Xu, S.L.; Li, Q.H. Fractal characteristics of fire-damaged ultra high toughtness cementitious
composite after impact loading. China Civ. Eng. J. 2019, 52, 44–55.
18. Bideci, Ö.S. The effect of high temperature on lightweight concretes produced with colemanite coated pumice
aggregates. Constr. Build. Mater. 2016, 113, 631–640. [CrossRef]
19. Xue, W.P.; Liu, X.Y.; Yao, Z.S.; Cheng, H.; Li, H.P. Effect of different damage sources on pore structure of
basalt fiber reinforced concrete. Acta Mater. Compos. Sin. 2020, 37, 1–8. [CrossRef]
20. Wu, Z.W.; Lian, H.Z. High Performance Concrete; China Railway Press: Beijing, China, 1999.
21. Zhao, D.F.; Gao, H.J.; Jia, P.H.; Wen, H.; Yang, J.H. Performance degradation of high strength concrete (HSC)
after different-high-temperature history. J. Vib. Shock 2018, 37, 240–248.
Materials 2020, 13, 1566 15 of 15

22. Shaikh, F.U.A.; Taweel, M. Compressive strength and failure behaviour of fibre reinforced concrete at elevated
temperatures. Adv. Concr. Constr. 2015, 3, 283–293. [CrossRef]
23. Heap, M.J.; Lavallée, Y.; Laumann, A.; Hess, K.U.; Meredith, P.G.; Dingwell, D.B.; Huismann, S.; Weise, F.
The influence of thermal-stressing (up to 1000 ◦ C) on the physical, mechanical, and chemical properties of
siliceous-aggregate, high-strength concrete. Constr. Build. Mater. 2013, 42, 248–265. [CrossRef]
24. Zheng, W.Z.; Li, H.Y.; Wang, Y. Compressive behaviour of hybrid fiber-reinforced reactive powder concrete
after high temperature. Mater. Des. 2012, 41, 403–409. [CrossRef]
25. Kong, L.J.; Du, Y.B. Effect of lightweight aggregate and the interfacial transition zone on the durability of
concrete based on grey correlation. Indian J. Eng. Mater. Sci. 2015, 22, 111–119.
26. Hu, S.G.; Wang, F.Z.; Ding, Q.J. Interface structure between lightweight aggregate and cement paste. J. Chin.
Ceram. Soc. 2005, 33, 713–717.
27. Zhuang, Y.-Z.; Chen, C.-Y.; Ji, T. Effect of shale ceramsite type on the tensile creep of lightweight aggregate
concrete. Constr. Build. Mater. 2013, 46, 13–18. [CrossRef]
28. Ji, T.; Zheng, D.-D.; Chen, X.-F.; Lin, X.-J.; Wu, H.-C. Effect of prewetting degree of ceramsite on the early-age
autogenous shrinkage of lightweight aggregate concrete. Constr. Build. Mater. 2015, 98, 102–111. [CrossRef]
29. Specification for Mix Proportion Design of Ordinary Concrete JGJ55-2011; China Architecture and Building Press:
Beijing, China, 2011.
30. Lightweight Aggregate Concrete Technical Regulations JGJ51-2002; China Architecture and Building Press: Beijing,
China, 2002.
31. Standard for Test Methods of Concrete Physical and Mechanical Properties GB/T 50081-2019; China Architecture
and Building Press: Beijing, China, 2019.
32. Gong, J.Q.; Deng, G.Q.; Shan, B. Ultrasonic test and microscopic analysis of reactive powder concrete exposed
to high temperature. J. Hunan Univ. Nat. Sci. 2018, 45, 68–76.
33. Ma, Q.M.; Guo, R.X.; He, K.C.; Du, H.Y.; Lin, Z.W.; Yan, F.; Zhao, Z.M.; Bai, Y. Performance of modified
lightweight aggregate concrete after exposure to high temperatures. Mag. Concr. Res. 2018, 70, 1243–1255.
[CrossRef]
34. Peng, G.F.; Jiang, Y.C.; Li, B.H.; Zhang, J.; Shi, Y.X. Effect of high temperature on normal-strength
high-performance concrete. Mater. Res. Innov. 2014, 18, S2-290–S2-293. [CrossRef]
35. Varona, F.B.; Baeza, F.J.; Bru, D.; Ivorra, S. Influence of high temperature on the mechanical properties of
hybrid fibre reinforced normal and high strength concrete. Constr. Build. Mater. 2018, 159, 73–82. [CrossRef]
36. Zeng, X.P.; Wu, B.; Jiang, S.; Deng, X.R. The analysis for the calcium carbonate at high temperatures.
Guangdong Chem. Ind. 2010, 37, 70–72.
37. Long, G.C.; Yang, J.G.; Xie, Y.J. The mechanical characteristics of steam-cured high strength concrete
incorporating with lightweight aggregate. Constr. Build. Mater. 2017, 136, 456–464. [CrossRef]
38. Peng, G.F.; Yang, J.; Shi, Y.X. Experimental study on residula mechanical properties of ultra-high performance
concrete exposed to high temperature. China Civ. Eng. J. 2017, 50, 73–79.
39. Xing, Z.; Beaucour, A.-L.; Hebert, R.; Noumowe, A.; Ledsert, B. Influence of nature of aggregates on the
behaviour of concrete subjected to elevated temperature. Cem. Concr. Res. 2011, 41, 392–402. [CrossRef]
40. Gong, J.Q.; Zhang, W.J. The effects of pozzolanic powder on foam concrete pore structure and frost resistance.
Constr. Build. Mater. 2019, 208, 135–143. [CrossRef]
41. de Oliveira Dias, A.R.; Amancio, F.A.; de Carvalho Rafael, M.F.; Bezerra Cabral, A.E. Study of propagation of
ultrasonic pulses in concrete exposed at high temperatures. Proced. Struct. Integr. 2018, 11, 84–90. [CrossRef]
42. Huang, Z.Y.; Padmaja, K.; Li, S.; Liew, J.Y.R. Mechanical properties and microstructure of ultra-lightweight
cement composites with fly ash cenospheres after exposure to high temperatures. Constr. Build. Mater. 2018,
164, 760–774. [CrossRef]
43. Peng, G.F.; Huang, Z.S. Change in microstructure of hardened cement paste subjected to elevated temperatures.
Constr. Build. Mater. 2008, 22, 593–599. [CrossRef]

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