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Materials: Mechanical Properties of Ultra-High Performance Concrete Before and After Exposure To High Temperatures

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Materials: Mechanical Properties of Ultra-High Performance Concrete Before and After Exposure To High Temperatures

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Saranyaleo
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materials

Article
Mechanical Properties of Ultra-High Performance
Concrete before and after Exposure
to High Temperatures
How-Ji Chen 1 , Yi-Lin Yu 1 and Chao-Wei Tang 2,3,4, *
1 Department of Civil Engineering, National Chung-Hsing University, No. 250, Kuo Kuang Road,
Taichung 402, Taiwan; hojichen@dragon.nchu.edu.tw (H.-J.C.); n0937699278@gmail.com (Y.-L.Y.)
2 Department of Civil Engineering & Geomatics, Cheng Shiu University, No. 840, Chengching Rd.,
Niaosong District, Kaohsiung 83347, Taiwan
3 Center for Environmental Toxin and Emerging-Contaminant Research, Cheng Shiu University, No. 840,
Chengching Rd., Niaosong District, Kaohsiung 83347, Taiwan
4 Super Micro Mass Research & Technology Center, Cheng Shiu University, No. 840, Chengching Rd.,
Niaosong District, Kaohsiung 83347, Taiwan
* Correspondence: tangcw@gcloud.csu.edu.tw; Tel.: +886-7-735-8800

Received: 14 January 2020; Accepted: 5 February 2020; Published: 7 February 2020 

Abstract: Compared with ordinary concrete, ultra-high performance concrete (UHPC) has excellent
toughness and better impact resistance. Under high temperatures, the microstructure and mechanical
properties of UHPC may seriously deteriorate. As such, we first explored the properties of UHPC with
a designed 28-day compressive strength of 120 MPa or higher in the fresh mix phase, and measured
its hardened mechanical properties at seven days. The test variables included: the type of cementing
material and the mixing ratio (silica ash, ultra-fine silicon powder), the type of fiber (steel fiber,
polypropylene fiber), and the fiber content (volume percentage). In addition to the UHPC of the
experimental group, pure concrete was used as the control group in the experiment; no fiber or
supplementary cementitious materials (silica ash, ultra-fine silicon powder) were added to enable
comparison and discussion and analysis. Then, the UHPC-1 specimens of the experimental group
were selected for further compressive, flexural, and splitting strength tests and SEM observations
after exposure to different target temperatures in an electric furnace. The test results show that at
room temperature, the 56-day compressive strength of the UHPC-1 mix was 155.8 MPa, which is
higher than the >150 MPa general compressive strength requirement for ultra-high-performance
concrete. The residual compressive strength, flexural strength, and splitting strength of the UHPC-1
specimen after exposure to 300, 400, and 500 ◦ C did not decrease significantly, and even increased due
to the drying effect of heating. However, when the temperature was 600 ◦ C, spalling occurred, so the
residual mechanical strength rapidly declined. SEM observations confirmed that polypropylene
fibers melted at high temperatures, thereby forming other channels that helped to reduce the internal
vapor pressure of the UHPC and maintain a certain residual strength.

Keywords: ultra-high performance concrete; residual mechanical properties; high temperature

1. Introduction
Ultra-high performance concrete (UHPC) is a cementitious composite characterized by
high compressive strength, typically greater than 120 MPa, specific durability, tensile ductility,
and toughness [1–5]. In the basic composition of UHPC, the aggregate is a filler and the binder reacts
with water to form a matrix with cementing ability and a lubricating effect. In addition to lubricating
the aggregate particles and providing proper workability, the matrix must fully solidify the aggregate

Materials 2020, 13, 770; doi:10.3390/ma13030770 www.mdpi.com/journal/materials


Materials 2020, 13, 770 2 of 17

particles to ensure the engineering properties of the hardened concrete. Considering the high strength
and durability requirements of UHPC, the packing density of the particles must be increased. To ensure
the sufficient strength of UHPC, silica fume and ultra-fine silica powder are often used in the matrix
composition to increase the packing density of the particle system, thereby increasing the strength of
the matrix. In addition to supplementary cementitious materials, a thickening agent is added, as is
a suitable amount of a superplasticizer to ensure the proper fluidity and viscosity of the prepared matrix.
Fibers are blended to increase the tensile and spalling resistance of the matrix. Because UHPC has
many advantages, its application has been increasing since the advent of its research and development.
For example, UHPC is now widely used in buildings, roads, bridges, and other structures. Among
them, the application in bridges is the most widespread [6].
Basically, the overall cost of a structure is directly related to the cross-sectional dimensions of the
structural members. The use of UHPC structural members reduces the cross-sectional dimensions and
provides additional useful space in the building [7]. UHPC blended with fibers has excellent crack
resistance and can suppress crack growth to reduce maintenance costs [8,9]. Although the cement content
required in UHPC is higher, the material cost is still lower than that of ordinary concrete members
requiring a larger cross-section. In addition, coarse aggregates are not used in UHPC and the amount
of fine aggregate can be reduced to 30% [10]. UHPC can reduce material costs by approximately 56%
compared with ordinary concrete, and energy consumption can be significantly reduced [11]. UHPC’s
high-strength properties allow for the design of thinner structures that reduce the weight of the structure
(less material used). This also reduces the amount of waste that will need to be dismantled in the future,
thereby reducing transportation requirements and mitigating environmental impacts [7]. The use of
by-products (such as fly ash and silica fume) instead of cement makes UHPC more sustainable [12]. Due to
their excellent durability, UHPC components require less maintenance costs, so their life cycle costs can be
reduced while providing longer service life [11]. Similarly, neighboring communities are not subject to
routine maintenance or replacement facility operations, having positive social effects. In UHPC, not all
cement has been hydrated. Therefore, the recycling of UHPC can be more effective because unhydrated
cement can be used for further reactions [12]. Notably, UHPC is less harmful to the environment, having
less of an impact on the ozone layer and producing fewer greenhouse gas emissions [13–18]. From this
point of view, UHPC has a better impact on the economy, society, and the environment, and its application
can lead to more sustainable construction.
Under the action of high temperature, the microstructure and properties of cement hydration
products change, which directly or indirectly changes the macroscopic properties of the substrate,
and affects the overall behavior of hardened concrete [19,20]. Due to the low porosity inside the UHPC,
the release of vapor pressure under fire and high temperature can be easily hindered. Therefore, UHPC
structures may be more susceptible to fire and high temperatures, resulting in tangible damage [21].
However, the use of polypropylene (PP) fibers can avoid comminuted damage or spalling [22–25].
The literature shows that the addition of 0.6% PP (volume ratio) can improve the fire resistance of
UHPC, preventing spalling [26,27]. This is attributed the PP, after melting at high temperatures,
providing an escape passage for the steam to release the accumulated pressure. However, on the
surface of the sample, 0.3 to 0.5 mm cracks were observed. In addition, due to the dehydration of
calcium silicate hydrates (C–S–H) colloid and the chemical decomposition and thermal expansion
damage of UHPC materials, the mechanical properties of UHPC degraded [21]. At a high temperature
of 1000 ◦ C, UHPC with 0.6% PP added demonstrated a weight loss of less than 9% [26]. The results of
Tai et al. [28] showed that the compressive strength of UHPC continued to increase with increasing
temperature to 300 ◦ C; however, once the temperature exceeded 300 ◦ C, the compressive strength
showed a downward trend. At high temperatures, the mechanical degradation of UHPC occurs mainly
due to the weakening of the internal microstructure [29]. However, the addition of steel fibers to UHPC
improved their behavior at elevated temperatures [28,29].
As mentioned above, UHPC is a more a sustainable material due to its improved durability, ecological
factors, economic benefits, and recycling capabilities for a variety of applications. As a result, the use of
Materials 2020, 13, 770 3 of 17

UHPC in infrastructure projects has increased in recent years. Fire damage is a special characteristic failure
mode of concrete structures because it has a considerable impact on the overall safety of the structure.
Basically, the failure of structural concrete in a fire varies depending on the nature of the fire, the loading
system, and the type of structure. The behavior of concrete during a fire mainly depends on its mix
proportions and constituents and is determined by complex physicochemical transformations occurring
in heating [30]. When exposed to high temperatures, ordinary-strength concrete and high-performance
concrete follow similar trends in microstructure, but UHPC behaves differently. When exposed to high
temperatures, UHPC is prone to explosive spalling due to its increased packing density. Therefore,
exploring the influence of high temperature and fire damage on UHPC is essential. As such, we aimed
to investigate the mechanical properties of UHPC before and after exposure to high temperatures.
We found effective methods to prevent UHPC from spalling while maintaining its fresh properties.
SEM observations of the UHPC specimens after exposure to different target temperatures in an electric
furnace were performed to understand changes in their microscopic properties.

2. Experimental Details

2.1. Materials
The materials used in the tests included cement, silica fume, ultra-fine silica powder, fine aggregate,
superplasticizer, viscous agent, steel fiber, and polypropylene fiber. A locally produced Type I Portland
cement with a specific gravity of 3.15 and a fineness of 3400 cm2 /g was used. The silica fume was
produced locally, with a specific gravity of 2.1 and a silicon dioxide content of 92.4%. The ultra-fine
silica powder was purchased from Dawei Stone Industry Co. (Jhubei, Taiwan). It had a specific gravity
of 2.73 and an average particle diameter of 0.075 to 0.225 µm. The fine aggregate contained two different
sizes of quartz sand (Type I and Type II). The physical properties and chemical composition of the fine
particles are shown in Table 1, and the particle size distribution is provided in Table 2. The mixing
ratio of the fine aggregate was 80% of Type I and 20% of Type II. Superplasticizers and viscous agent
were purchased from Dawei Stone Industry Co. (Jhubei, Taiwan) (in accordance with the Chinese
National Standards or the American Society for Testing Materials). The fibers used included steel and
polypropylene fibers, as shown in Figure 1. The basic properties of these two fibers are listed in Table 3.

Table 1. Physical properties and chemical composition of fine aggregates.

Physical Properties Chemical Composition


Type of
Quartz Sand Specific Gravity Water Absorption Rate
SiO2 (%) Fe2 O3 (%) Al2 O3 (%)
(S.S.D.) (%) (S.S.D.)
Type I 2.65 ≈0 99.82 0.014 0.033
Type II 2.65 ≈0 99.84 0.016 0.034
Notes: S.S.D., Saturated-Surface-Dry.

Table 2. Particle size distribution of fine aggregates.

Percentage Retained
Sieve No. Particle Size (%)
(ASTM E11-70) (µm)
Type I Type II
20 850 0.04 -
30 600 20.15 -
40 425 67.83 -
50 300 11.81 -
60 250 - 0.05
70 212 0.17 13.69
100 150 - 36.55
140 106 - 32.39
200 75 - 12.73
270 53 - 3.61
Materials 2020, 13, 770 4 of 17

Table 3. Basic properties of fibers.

Length Diameter Density Elastic Modulus Tensile Strength Melting Point


Type of Fiber
(mm) (mm) (g/cm3 ) (GPa) (MPa) (◦ C)
Steel Fibers 13 0.2 7.8 200 2000 -
Polypropylene
12 0.05 0.9 - 300 165
Fibers

Figure 1. Appearance of (a) steel fibers and (b) polypropylene fibers.

2.2. Mix Proportions and Casting of Specimens


Table 4 describes the mix design of the concrete used, including the control group and the
experimental group. The control group (Mix No. HPC-1) had no fiber or special cementitious materials
(silica fume and ultra-fine silica powder) for comparison and discussion. The experimental group had
five different UHPC mix proportions. In the experimental group, the four important parameters were:
the percentage of cement replaced by silica fume (SF), the percentage of cement replaced by ultra-fine
silica powder (SFP), the amount of steel fiber (volume percent), and the amount of polypropylene fiber
(volume percentage). Table 5 lists the percentage of these parameters used in the mix proportions of
the UHPC. The amounts of superplasticizers and viscous agent were 2.6% and 0.1% by weight of the
cementitious materials, respectively. The ratio of the weight of the fine aggregate to the weight of the
cementitious materials was maintained at 1.28 in both the control and the experimental groups.

Table 4. Mix proportions of concrete.

W C SF SFP SP VA PP Steel Fiber FA


Mix No. W/B
(kg/m3 ) (kg/m3 ) (kg/m3 ) (kg/m3 ) (kg/m3 ) (kg/m3 ) (kg/m3 ) (kg/m3 ) (kg/m3 )
HPC-1 0.195 196 1005 0 0 26 1 0 0 1286
UHPC-1 0.195 187 774 167 21 25 1 0.3 39 1231
UHPC-2 0.195 186 756 179 21 25 1 0.5 78 1223
UHPC-3 0.195 186 747 179 31 25 1 0.3 59 1225
UHPC-4 0.195 186 744 191 21 25 1 0.8 59 1223
UHPC-5 0.195 186 737 191 26 25 1 0.3 78 1220
Notes: HPC, high performance concrete; UHPC, ultra-high performance concrete; W/B, water-binder ratio; W, water;
C, cement; SF, silica fume; SFP, ultra-fine silica powder; S, superplasticizers; VA, viscous agent; PP, polypropylene
fiber; FA, fine aggregate.

Table 5. UHPC test parameters.

Parameter
Mix No. Percentage of Cement Percentage of Cement Amount of PP Amount of Steel Fiber
Replaced by SF (%) Replaced by SFP (%) (Volume Percent) (%) (Volume Percentage) (%)
UHPC-1 17.4 2.2 0.03 0.5
UHPC-2 18.7 2.2 0.06 1.0
UHPC-3 18.7 3.2 0.03 0.75
UHPC-4 20.0 2.2 0.09 0.75
UHPC-5 20.0 2.7 0.03 1.0

The concrete test proportions of each group were mixed using a forced single-shaft mixer, and the
mixing procedure was as follows:
Materials 2020, 13, 770 5 of 17

(1) Before mixing, the fine aggregates were treated in a dry state because their water absorption rate
approached zero.
(2) We placed the cementitious materials, aggregates, and fibers (steel fiber and polypropylene fiber)
into a mixing tank, and then dry blended uniformly for 5 min.
(3) We poured the water into the mixer. After mixing for about 1 min, we poured all the
superplasticizer and viscous agent into the mixture and mixed for another 4 min to produce
fresh concrete.

After the concrete mixture was uniformly mixed, the fresh properties of each mixture were
measured and recorded. Afterward, concrete specimens required for each test were cast and compacted
using an external vibrator to ensure that the specimens were sufficiently compacted. The compressive
strength and elastic modulus tests were conducted with cylindrical specimens with a diameter of
100 mm and a height of 200 mm. For the splitting strength test, we used a cylindrical specimen
with a diameter of 150 mm and a height of 300 mm. For the flexural strength test, a prism sample
360 mm long, 100 mm wide, and 100 mm thick was used. After casting, all the specimens were covered
with polyethylene sheets for 24 h overnight. The demolding operation was then conducted and each
specimen was placed in a laboratory water bath until the day before the mechanical test.

2.3. Test Methods and Instrumentation


The UHPC tests of unit weight, slump, slump flow, compressive strength, elastic modulus,
splitting tensile strength, and flexural strength were conducted according to the ASTM specifications
listed in Table 6 [31–37]. To study the effect of high temperature on the mechanical properties of UHPC,
the specimens were heated at the prescribed rate (2 ◦ C/min) until the temperature in the furnace
reached the target. After the target maximum temperature was reached, the furnace temperature was
maintained for 30 min to achieve better thermal stability of the entire specimen. Then, we turned off
the furnace power switch and cooled the sample to room temperature by opening the furnace door
before performing the residual strength test. A field emission scanning electron microscope (FE-SEM;
JEOL JSM-7401F, Tokyo, Japan) was used to observe the microscopic state of the concrete before and
after the high temperature to understand its changes. After the compressive strength test, the fractured
cylindrical specimens were retained for SEM observation. An appropriate number of fragments were
extracted from the cylindrical specimen and the hydration reaction of the fragments was stopped using
the methanol replacement method. These pieces were then placed in an oven at 105 ◦ C and dried for at
least 24 h before SEM observation.

Table 6. Concrete property test method.

Property Experimental Method


Unit weight ASTM C138
Slump ASTM C143
Slump flow ASTM C1611
Compressive strength ASTM C39
Elastic modulus ASTM C469
Splitting tensile strength ASTM C496
Flexural strength ASTM C78

3. Results and Discussion

3.1. Fresh Concrete Properties


The fresh properties of each concrete mixture are listed in Table 7. The table shows that the slump
value ranged from 250 to 262 mm. Both the control group and the experimental group had fairly good
workability. The HPC-1 mix of the control group had a slump flow of 690 mm, indicating very good
fluidity. For the experimental group, the slump flow of each mixture was lower than that of the control
group due to the incorporation of fibers, but they also had proper fluidity. Table 7 shows that the unit
Materials 2020, 13, 770 6 of 17

weight of the control group was 2318 kg/m3 . For the experimental group, the unit weight ranged from
2274 to 2316 kg/m3 . Overall, the unit weight ratio between the experimental group and the control
group ranged from 0.981 to 0.999, with no significant differences between each other.

Table 7. Results of fresh concrete properties.

Mix No. Slump (mm) Slump Flow (mm) Unit Weight (kg/m3 )
HPC-1 262 690 2318
UHPC-1 255 530 2263
UHPC-2 257 540 2316
UHPC-3 260 490 2274
UHPC-4 255 530 2288
UHPC-5 250 510 2308

3.2. Hardened Concrete Properties at Room Temperature


The seven-day results of the hardened properties of the control group and the experimental
group, including the compressive strength, elastic modulus, flexural strength, and splitting strength,
are shown in Table 8. The data in the table are the average of three specimens.

Table 8. Results of hardened concrete properties at room temperature.

7-day Experimental Results


Mix No.
0
fc (MPa) Ec (GPa) fr (MPa) fs (MPa)
HPC-1 81.6 (7.8) 32.3 6.6 (0.5) 4.4 (0.2)
UHPC-1 95.7 (11.2) 34.9 12.6 (1.4) 7.3 (0.9)
UHPC-2 107.0 (2.8) 37.2 15.1 (0.2) 9.6 (0.8)
UHPC-3 97.8 (7.9) 33.9 14.7 (0.3) 10.5 (0.3)
UHPC-4 95.6 (1.5) 35.4 12.2 (0.6) 8.9 (0.4)
UHPC-5 111.5 (3.3) 36.9 12.7 (1.4) 10.8 (0.1)
Note: fc ’, compressive strength; Ec , elastic modulus; fr , flexural strength; fs , splitting strength; data in parentheses
are standard deviation.

3.2.1. Compressive Strength of Concrete at Room Temperature


The use of pozzolanic material has a significant impact on the development of UHPC’s early
compressive strength, mainly depending on its type, addition amount, mineral composition, particle
shape and fineness, and pozzolanic activity. Table 8 shows that the control group had the lowest
seven-day compressive strength (81.6 MPa). In the experimental group, the seven-day compressive
strength of the UHPC mixtures was between 95.6 and 111.5 MPa. This result showed that the
incorporation of pozzolanic materials can enhance the early age compressive strength of UHPC, and the
percentage of improvement was between 17.2% and 36.6%. Table 9 shows the percentage of 28-day
compressive strength achieved by the UHPC mixture at seven days. For the UHPC-5 mix containing
large amounts of silica fume, its seven-day compressive strength was 89% of its 28-day compressive
strength. For the HPC-1 mix containing large amounts of cement, its seven-day compressive strength
was 91% of 28-day compressive strength.

Table 9. Development of compressive strength.


0 0 0 0
Mix No. fc−7d (MPa) fc−28d (MPa) fc−7d /fc−28d
HPC-1 81.6 (7.8) 90.0 (3.4) 0.91
UHPC-1 95.7 (11.2) 128.1 (5.4) 0.75
UHPC-2 107.0 (2.8) 127.0 (5.4) 0.84
UHPC-3 97.8 (7.9) 121.6 (14.9) 0.80
UHPC-4 95.6 (1.5) 123.6 (4.4) 0.77
UHPC-5 111.5 (3.3) 125.8 (6.8) 0.89
0
Note: fc−7d 0
, 7-day compressive strength; fc−28d , 28-day compressive strength; data in parentheses are standard deviation.
Materials 2020, 13, 770 7 of 17

3.2.2. Elastic Modulus of Concrete at Room Temperature


Figure 2 shows the stress–strain curve of each concrete mixture at seven days of age. Figure 2 shows
that the initial slope of the rising branch of the stress–strain curve exhibited a linear relationship before
reaching the maximum stress. The elastic modulus of the specimen obtained from the stress–strain
curve according to ASTM C469 is listed in Table 10. Table 10 shows that the seven-day elastic modulus
of the concrete mixture was between 32.3 and 37.2 GPa. The HPC-1 mixture had the lowest elastic
modulus (32.3 GPa) and the UHPC-2 mixture had the highest (37.2 GPa). However, in the experimental
group, we found no significant difference in the elastic modulus of the concrete mixtures. We also
found that the age of concrete at the time of the test did not significantly affect the elastic modulus.
Especially for the UHPC-2 and UHPC-3 mixtures, the elastic modulus at 7 and 28 days were almost
equal, as shown in Table 10, because the elastic modulus of concrete during the early stages develops
rapidly compared to compressive strength [38]. Myers also pointed out that about 90% or more of the
elastic modulus value is achieved within the first 24 h after casting [39].

Figure 2. Stress–strain curves of concrete.

Table 10. Development of elastic modulus.

Mix No. Ec-7D (GPa) Ec-28D (GPa) Ec-7D /Ec-28D


HPC-1 32.3 37.2 0.87
UHPC-1 34.9 39.5 0.88
UHPC-2 37.2 38.1 0.98
UHPC-3 33.9 34.0 1.00
UHPC-4 35.4 48.0 0.74
UHPC-5 36.9 44.8 0.82
Note: Ec-7D , 7-day elastic modulus; Ec-28D , 28-day elastic modulus.

3.2.3. Flexural Strength of Concrete at Room Temperature


The load versus midspan deflection curves for each group of concrete specimens are shown in
Figure 3. The load–displacement curve was linear in the region before the peak point. The control
group clearly exhibited brittle failure, as shown in Figure 3. In contrast, all test specimens of the
experimental group containing steel fiber showed greater load carrying capacity and better flexing
performance than the control group. In other words, the experimental specimens incorporating steel
fiber exhibited better toughness because the steel fibers in the experimental group specimens had the
ability to bridge cracks, as shown in Figure 4. As a result, the area under the load versus deflection
curve up to fracture (i.e., fracture toughness) of the experimental group was significantly better than
that of the control group. Table 8 shows that the seven-day flexural strength of the concrete mixtures
was between 6.6 and 15.1 MPa. The HPC-1 mix had the lowest flexural strength (6.6 MPa) and the
UHPC-2 mix had the highest (15.1 MPa). Overall, the flexural strength of the experimental group was
Materials 2020, 13, 770 8 of 17

1.85 to 2.29 times that of the control group. This shows that the steel fiber content is an important factor
affecting the flexural strength of concrete.

Figure 3. Load–deflection curves of concrete specimens.

Figure 4. Failure of the experimental group specimen in flexure test.

3.2.4. Splitting Strength of Concrete at Room Temperature


Regarding the splitting strength of concrete, the test results were between 4.4 and 10.8 MPa.
The HPC-1 mix had the lowest splitting strength (4.4 MPa) and UHPC-5 mix had the highest (10.8 MPa).
Overall, the splitting strength of the experimental group was 1.66 to 2.45 times that of the control group.
This shows that the steel fiber content is an important factor affecting the splitting strength of concrete.
Figure 5 shows that the control group exhibited brittle failure, and the experimental group maintained
its original appearance after reaching the ultimate load without much strain or deformation.

Figure 5. Comparison of splitting test results: (a) HPC-1, (b) UHPC-3, and (c) UHPC-5 specimens.

3.3. Test Results of Hardened Concrete Properties after Exposure to High Temperatures
To understand the influence of high temperature on the mechanical properties of UHPC,
the UHPC-1 specimens of the experimental group were selected for further compressive, flexural,
and splitting strength tests after exposure to high temperatures in an electric furnace. Generally, in the
fire test, the heating rate of the electric furnace had a strong influence. In this study, we first tried to
reach the target temperature (600 ◦ C) with heating rates of 15, 10, 5, and 2 ◦ C/min, and maintained
the furnace temperature for an additional hour. However, for all of the above cases, this resulted
Materials 2020, 13, 770 9 of 17

in specimen spalling, as shown in Figure 6a–d. In particular, the faster the heating rate, the more
severe the spalling. Therefore, we changed the heating rate to 2 ◦ C/min to reach the target temperature
(500 ◦ C) and held the temperature for 0.5 h, so that the specimen remained intact, as shown in
Figure 6e. The maximum fire damage temperature was divided into three types: 300, 400, and 500 ◦ C.
After reaching the target temperature, the temperature was held for 0.5 h. Then, the furnace was turned
off to allow the specimens to cool naturally to ambient temperature. The age of the UHPC-1 specimen
when subjected to high temperature fire damage was 56 days. Table 11 provides the results of the
compressive, flexural, and splitting strength tests at this age at room temperature. After heating the
UHPC-1 specimen to the target temperature for 0.5 h, it was naturally cooled in an electric furnace and
left for 24 h. After that, the post-fire compressive, flexural, and splitting strength tests were performed.
The test results are also listed in Table 11.

Figure 6. Rupture of the specimen after high temperature: (a) 15 ◦ C/min heating rate and target
temperature of 600 ◦ C, (b) 10 ◦ C/min heating rate and target temperature of 600 ◦ C, (c) 5 ◦ C/min heating
rate and target temperature of 600 ◦ C, (d) 2 ◦ C/min heating rate and target temperature of 600 ◦ C,
and (e) 2 ◦ C/min heating rate and target temperature of 500 ◦ C.

Table 11. Results of 56-day hardened concrete properties at room temperature.

Target Temperature fc 0 (MPa) fr (MPa) fs (MPa)


Room 155.8 (8.8) 13.0 (0.28) 9.8 (0.39)
300 ◦ C 157.0 (7.3) 13.3 (1.33) 9.9 (0.98)
400 ◦ C 156.5 (9.7) 13.1 (1.07) 9.2 (0.85)
500 ◦ C 155.0 (8.9) 10.3 (1.24) 9.2 (0.27)
Note: fc ’, compressive strength; fr , flexural strength; fs , splitting strength; data in parentheses are SD.

When the internal temperature of the electric furnace reached the target temperature, the internal
temperature of the concrete specimen gradually increased due to heat conduction. In this study,
two thermocouples were embedded in a concrete cylindrical specimen with a diameter of 10 cm and
a height of 20 cm. One of the thermocouples located at half the height was 3 cm from the surface of the
concrete specimen and the other at the core of the specimen was 5 cm from the surface of the concrete
specimen to measure the actual temperature inside the specimen. Based on these data, the relationship
between the internal temperature of the UHPC-1 specimen and the heating and cooling times of the
electric furnace was plotted. After reaching the maximum fire temperature, its holding time was 0.5 h,
and then the electric furnace was turned off. When the target temperatures were 300, 400, and 500 ◦ C,
the relationship curves between the internal temperature of the concrete specimen and the heating as
well as cooling time of the electric furnace were plotted, as shown in Figures 7–9. These figures shows
that a significant gap between the internal temperature of the specimen and the furnace temperature,
which was only about half that of the furnace temperature.
Materials 2020, 13, 770 10 of 17

Figure 7. Relationship between specimen internal temperature and time (target temperature = 300 ◦ C).

Figure 8. Relationship between specimen internal temperature and time (target temperature = 400 ◦ C).

Figure 9. Relationship between specimen internal temperature and time (target temperature = 500 ◦ C).

3.3.1. Compressive Strength of Concrete after Exposure to High Temperatures


The results of the 56-day compressive strength of the UHPC-1 specimen are shown in Table 11.
At room temperature, the 56-day compressive strength of the UHPC-1 specimen was 155.8 MPa,
which is higher than the general requirement for the compressive strength of UHPC to be greater than
150 MPa. Table 11 also lists the residual compressive strength of the UHPC-1 specimen after exposure
to different temperatures; the residual compressive strength of the UHPC-1 specimen after exposure to
300, 400, and 500 ◦ C was between 155 and 157 MPa. The relationship between the residual compressive
strength and the maximum fire temperature is shown in Figure 10a; the residual compressive strength
Materials 2020, 13, 770 11 of 17

of the UHPC-1 specimen after exposure to 300, 400, and 500 ◦ C did not decrease significantly, and even
increased. The strength of the specimen was slightly increased due to the drying effect of heating [40].
Although the furnace temperature was maintained for 0.5 h, the temperature inside the concrete
specimen was still lower than the target temperature. Under the action of high temperature drying,
the water vapor in the test specimen was easily released, which helped to improve the compressive
strength. Deshpande et al. [41] reported that a slight increase in residual strength compared to room
temperature strength may be related to favorable changes in microstructure at high temperatures
and inherent variability of concrete materials. At the target temperatures of 300, 400, and 500 ◦ C,
Figures 7–9 show that the maximum internal temperature of the concrete specimen was approximately
120, 180, and 250 ◦ C, respectively. The temperature difference between 3 and 5 cm from the surface
of the concrete specimen was not obvious. Therefore, fire damage had not caused the decay of the
concrete matrix. However, when the temperature was 600 ◦ C, the internal temperature of the concrete
specimen caused the concrete matrix to decay and spall, so the residual compressive strength dropped
sharply to zero. The loss of strength was mainly caused by physical changes at temperatures below
400 ◦ C. However, when the temperature exceeded 600 ◦ C, the decrease in strength was mainly due to
chemical degradation in hydrated products and aggregates, which is not directly related to the content
and type of fiber [41]. The relative compressive strength ratio is defined as the ratio of the strength after
exposure to the target high temperature to the original strength at room temperature. Figure 10b shows
that the relative residual compressive strength ratios after exposure to 300 and 400 ◦ C were both greater
than one. However, as the temperature reached 500 ◦ C, its relative compressive strength began to
decline; especially when the temperature was 600 ◦ C, the relative compressive strength ratio after fire
damage was zero.

Figure 10. Comparison of compressive strength before and after fire damage to the UHPC-1 specimen:
(a) residual compressive strength after high temperature; (b) relative compressive strength ratio.

3.3.2. Flexural Strength of Concrete after Exposure to High Temperatures


At room temperature, the 56-day flexural strength of the UHPC-1 specimen was 13 MPa, which was
significantly higher than that of ordinary concrete (Table 11). Table 11 also lists the residual flexural
strength of the UHPC-1 specimen after exposure to different temperatures. The residual flexural
strength of the UHPC-1 specimen after exposure to 300, 400, and 500 ◦ C was between 10.3 and
13.3 MPa. The relationship between the residual flexural strength and the fire temperature is depicted
in Figure 11a; the residual flexural strength of the UHPC-1 specimen after exposure to 300, 400,
and 500 ◦ C did not decrease significantly, and even increased. The strength of the specimen slightly
increased due to the drying effect of heating. However, when the target temperature was 600 ◦ C,
spalling occurred, so the residual flexural strength suddenly reduced to zero. Figure 11b also shows
that the relative residual flexural strength ratios after exposure to 300 and 400 ◦ C were all greater than
one. However, as the target temperature was 500 ◦ C, its residual flexural strength was significantly
reduced, and its relative flexural strength ratio after fire damage is 0.79; when the target temperature
was 600 ◦ C, its relative flexural strength was zero.
Materials 2020, 13, 770 12 of 17

Figure 11. Comparison of flexural strength before and after fire damage to the UHPC-1 specimen:
(a) residual flexural strength after high temperature; (b) relative flexural strength ratio.

3.3.3. Splitting Strength of Concrete after Exposure to High Temperatures


The results of the 56-day splitting strength of the UHPC-1 specimen are shown in Table 11.
At room temperature, the 56-day splitting strength of the UHPC-1 specimen was 9.8 MPa, which is
significantly higher than that of ordinary concrete. Table 11 also lists the residual splitting strength
of the UHPC-1 specimen after exposure to different temperatures. The residual splitting strength of
the UHPC-1 specimen after exposure to 300, 400, and 500 ◦ C was between 9.2 and 9.9 MPa, and the
relationship between the residual splitting strength and the target temperature is shown in Figure 12a;
the residual cleavage strength of the UHPC-1 specimen after 300, 400, and 500 ◦ C did not decrease
significantly, and even increased. However, when the temperature was 600 ◦ C, spalling occurred,
so the residual splitting strength was zero. Figure 12b shows that the relative splitting strength ratio
after exposure to 300 ◦ C was greater than one. However, as the target temperature reached 400 and
500 ◦ C, its residual splitting strength showed a decline. The relative splitting strength ratio after fire
damage was 0.94. When the target temperature was 600 ◦ C, the relative splitting strength ratio after
fire damage quickly dropped to zero.

Figure 12. Comparison of splitting strength before and after fire damage to the UHPC-1 specimen:
(a) residual splitting strength after high temperature; (b) relative splitting strength ratio.

3.3.4. SEM Observation before and after Exposure to High Temperatures


Figure 13 compares the morphological characteristics of the UHPC-1 specimen before and after
exposure to high temperatures. The micrographs captured from the core of the cylindrical specimens
revealed hydrated phases such as C–S–H gels. The addition of silica fume and ultra-fine silica powder
resulted in a much denser microstructure due to the pozzolanic reaction between supplementary
cementitious materials and cement hydration product (calcium hydroxide) (Figure 13). In Figure 13a,
the magnification is 50×, and the well-adhered aggregates in the UHPC matrix were uniformly
distributed. In addition, at room temperature, an excellent bond between the cementitious material
and the fine aggregate were observed in the test piece, and the formation of ettringite (Al2 O3 –Fe2 O3 –tri)
Materials 2020, 13, 770 13 of 17

and silicate was detected in the pores present. After exposure to high temperatures, the microstructure
and properties of the UHPC matrix changed with increasing temperature, as shown in Figure 13b.
Figure 13c shows that as the temperature increased, the bonding interface between the UHPC matrix
and the steel fibers gradually loosened. In particular, when the target temperature was 500 ◦ C, the steel
fibers were pulled out or broken after the peak loading Figure 14 shows that although the target
temperature had been raised to 500 ◦ C, typical acicular AFt crystals were still observed that withstood
the thermal aggression in a high-temperature environment.

Figure 13. Comparison of SEM observation before and after fire damage: (a) 50× (b) 100×, and
(c) 300× magnification.
Materials 2020, 13, 770 14 of 17

Figure 14. SEM observation after exposure to 500 ◦ C: (a) 300× and (b) 1500× magnification.

In general, when the temperature inside concrete reaches 105–200 ◦ C, C–S–H gels begin to lose
bound water and undergo chemical changes [19,20]. When the target temperature was 300–400 ◦ C,
the maximum internal temperature of the concrete specimen was approximately 180–200 ◦ C, as shown
in Figures 7 and 8. The test pieces in Figure 13 show that due to heating, a part of ettringite and C–S–H
gels were destroyed and dispersed. In addition, the formation of acicular ettringite was round and
cracks occurred due to thermal expansion and contraction. Notably, the cracks in the UHPC matrix
after exposure to 300 and 400 ◦ C, as shown in Figure 13, were narrower than those of the matrix at room
temperature. The reduction of crack width in the matrix after exposure to 300 C and 400 ◦ C is attributed
to the drying effect of heating that occurred under exposure temperatures. Therefore, the increase
in compressive strength of the UHPC-1 specimen can be improved up to 400 ◦ C. However, once the
internal temperature of the concrete was above 200 ◦ C, the decomposition of cement hydrate and the
decay of aggregate gradually occurred [19,20]. SEM observations of the UHPC-1 specimen exposed to
500 ◦ C exhibited that the microstructure of concrete had changed due to microcracks, voids, partial
C–S–H gels deterioration, and calcium hydroxide crystal deformation. When the target temperature
was 500 ◦ C, the maximum internal temperature of the concrete specimen was approximately 250 ◦ C,
as shown in Figure 9. At this temperature, most of the internal bound water of hydrates containing
Al2 O3 or Fe2 O3 was lost; about 20% of the bound water of C–S–H gels was also lost [19,20]. At the same
time, the polypropylene fibers in the test piece melted. Therefore, the holes left after the polypropylene
fibers melted can be observed in Figure 13. The size of these holes was consistent with the size of
the polypropylene fibers and had a certain depth. This result shows that polypropylene fibers melt
at high temperatures and a network of pores is created, helping to reduce internal vapor pressure
and maintaining a certain residual strength. In other words, the SEM observations confirmed that
the melting of the polypropylene fibers resulted in an increase in the permeability of the concrete
matrix, thereby releasing water vapor. This result is consistent with the findings of Dong et al. [23],
Hager et al. [24], and Wu et al. [25]. However, as the temperature increased further, cement hydrate
decomposition and aggregate decay was more serious. The difference in the thermal deformation
between the UHPC matrix and the aggregate caused stress concentration, so the strength of the concrete
began to decrease. As mentioned above, when the target temperature was 600 ◦ C, the number of cracks
increased and the cracks widened, which weakened the internal structure of the UHPC-1 specimen and
eventually reduced the compressive strength. From the above, SEM investigations produced evidence
of the various types of damage caused by exposure to fire.

4. Conclusions
In this study, we explored the mechanical properties of UHPC before and after exposure to
high temperatures. Based on the analysis and discussion of the test results, the results obtained are
summarized as follows. At room temperature, the 56-day compressive strength of the UHPC-1 mix
Materials 2020, 13, 770 15 of 17

was 155.8 MPa, which is higher than the general compressive strength requirement of 150 MPa for
UHPC. After the UHPC-1 specimen was exposed to 300, 400, and 500 ◦ C, the residual compressive
strength did not decrease significantly, and even increased. The strength of the specimen increased
slightly due to the drying effect of temperature rise. When the target temperatures were 300, 400,
and 500 ◦ C, the maximum internal temperature of the concrete specimen was about 120, 180, and 250 ◦ C,
respectively. Therefore, the fire damage did not cause the decay of the concrete matrix. However,
when the fire damage was 600 ◦ C, the internal temperature of the concrete specimen had caused the
concrete matrix to decay and spall. In terms of flexural strength, the 56-day strength of the UHPC-1
mix at room temperature was 13 MPa, which was significantly higher than that of ordinary concrete.
After the UHPC-1 specimen was exposed to 300, 400, and 500 ◦ C, the residual flexural strength did
not decrease significantly, and even increased slightly due to the drying effect of heating. The relative
residual flexural strength ratios after fire damage at 300 and 400 ◦ C were both greater than one.
However, as the target temperature of the fire damage reached 500 ◦ C, the residual flexural strength
of the UHPC-1 specimen decreased significantly, and its residual flexural strength ratio after fire
damage was 0.79. For the splitting strength, the 56-day splitting strength of the UHPC-1 mix at normal
temperature was 9.8 MPa, which is also significantly higher than that of ordinary concrete. After the
UHPC-1 specimen was exposed to 300, 400, and 500 ◦ C, the residual splitting strength did not decline
significantly, and even increased slightly due to the drying effect of heating. The relative residual
splitting strength ratio after fire damage at 300 ◦ C was greater than one. However, as the fire damage
temperature reached 400 and 500 ◦ C, the residual splitting strength declined, and the residual splitting
strength ratio after fire damage was 0.94. SEM observations confirmed that polypropylene fibers
melted at high temperatures, forming other channels that helped to reduce the internal vapor pressure
of UHPC and maintain a certain residual strength. However, the optimal amount of polypropylene
fiber needs to be further explored.

Author Contributions: Conceptualization, C.-W.T. and H.-J.C.; methodology, C.-W.T.; software, C.-W.T. and
H.-J.C.; validation, C.-W.T., H.-J.C. and Y.-L.Y.; formal analysis, C.-W.T., H.-J.C. and Y.-L.Y.; investigation, Y.-L.Y.;
resources, H.-J.C.; data curation, Y.-L.Y.; writing—original draft preparation, C.-W.T.; writing—review and editing,
C.-W.T.; visualization, C.-W.T., H.-J.C. and Y.-L.Y.; supervision, C.-W.T.; project administration, C.-W.T.; funding
acquisition, C.-W.T. All authors have read and agreed to the published version of the manuscript.
Funding: The research was funded by the Ministry of Science and Technology of Taiwan grant number
MOST 108-2221-E-230-003-MY2.
Acknowledgments: The authors sincerely thank the Ministry of Science and Technology of Taiwan for funding
this research work.
Conflicts of Interest: The author declares no conflict of interest.

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© 2020 by the authors. Licensee MDPI, Basel, Switzerland. This article is an open access
article distributed under the terms and conditions of the Creative Commons Attribution
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