1 s2.0 S0950061819306105 Main
1 s2.0 S0950061819306105 Main
h i g h l i g h t s
Effect of fineness on tensile stress is less apparent than that on strain capacity.
Strain capacity with different fineness fly ash shows a tendency in certain condition.
High calcium-content do not make tensile properties greater at all ages.
High calcium-content will make compressive properties more excellent as age increases.
a r t i c l e i n f o a b s t r a c t
Article history: As a new green material, ECC has received extensive attention all over the world because of its potent
Received 19 October 2018 ability of crack width controlling, excellent behavior of flexural toughness, and fatigue durability. The
Received in revised form 9 March 2019 use of high volume fly ash as a partial replacement of cement reduces environmental pollution and con-
Accepted 11 March 2019
serves natural resources. This paper presents the experimental results to find out the effect of fineness
Available online 16 March 2019
and calcium content of fly ash on the mechanical properties of ECC. Four different types of fly ash were
used and a series of mechanical tests, including cube compressive strength, uniaxial direct tensile, three-
Keywords:
point bending and single-crack tension tensile were conducted in this paper. The results indicate that
Engineered Cementitious Composites (ECC)
Fly ash
between tensile strain properties and fly ash fineness, there is not just a simply linear relationship.
Ductility Fineness is not the determining factor for ECC’s compression performance, but the activity of fly ash.
Strength Fly ash with the higher calcium content did not make the tensile properties of ECCs greater at all ages,
Fineness but make compressive performance better.
Calcium content Ó 2019 Elsevier Ltd. All rights reserved.
https://doi.org/10.1016/j.conbuildmat.2019.03.129
0950-0618/Ó 2019 Elsevier Ltd. All rights reserved.
L.-l. Kan et al. / Construction and Building Materials 209 (2019) 476–484 477
strength [14–16]. Over the years, many studies found that the were added slowly and mixed for 4 min to ensure the good dispersion. The fresh
mixture was cast into molds and demolded after 24 h and cured in the standard
incorporation of FA and other supplementary cementitious materi-
curing box at 20 ± 1 °C temperature and 95 ± 5% humidity prior to testing.
als can dramatically improve the bonding performance between
fiber and matrix interface, cause the filling of the spaces, increase
2.2. Uniaxial direct tensile test
compactness, help achieve expansion of more micro-cracks and
greatly improve the ductility and toughness [17–21]. Nevertheless, Dog-bone shaped specimen (Fig. 1) recommended by the Japan Society of Civil
previous studies indicated that the workability properties of ECC Engineers [32] was adopted for standardized tension test. After curing at designed
mixtures were affected due to the variability of FA. Tosunfelekoglu ages, a LDS-5 type electro-servo machine was applied to specimens using a quasi-
static loading speed of 0.3 mm/min. Two sets of LVDTs (Linear Variable Displace-
et al. [22] examined the effects of FA type, FA/cement ratio and ment Transducers) installed on each specimen monitoring extensions within the
water/cement ratio on fresh and hardened properties of ECC. As a gauge length of about 80 mm.
result of the tests performed, it was seen that physical and chem-
ical properties of FA, directly affect the performance of composites 2.3. Compressive strength test
both in fresh and hardened state and class F FA was found more
advantageous in producing ECC compared to class C FA employed A set of cube specimens with dimension of 50 mm for each mixture in accor-
dance with ASTM C109 were used in compressive strength test. The test was carried
in this study. Yu et al. [23] attempted to improve the compressive out by using a WDW-300 electronic universal testing machine.
strength and maintain the excellent tensile characteristics of ECC.
They found that ECC could achieve a compressive strength of 2.4. Tests for assurance of high ductility
49.4 MPa at 7 days and 69.2 MPa at 28 days, with the correspond-
ing ultimate tensile strain more than 3.5% at 28 days, under the Three-point bending tests were conducted on notched beams based on ASTM
appropriate fly ash content. Sßahmaran et al. [24] produced ECC E399 [33]. The sample was made without fiber, after curing for 28 days, and a
30 mm depth notch was cut before testing. The notch size of the specimen and test
mixtures to discuss the influence of the high volumes of FA and
setup is shown in Fig. 2.
fibers on the cyclic freeze–thaw resistance and microstructure of For single-crack tensile tests, a crack with 6.5 mm length, 2 mm depth and
the ECC. It was observed that both ECC mixtures with high volumes width less than 0.6 mm crack [34] was notched in the center position of dog-
of FA remained durable, and showed a tensile strain capacity of bone specimens after curing for 28 days. Fig. 3 shows the schematic dimension of
notched dog-bone specimen for single crack tension test.
more than 2% even after 300 freezing and thawing cycles. Further-
In 1992, Li and Kanda proposed the energy and strength criterion for the mate-
more, they concluded that the addition of micro PVA fiber to the rial to achieve tensile strain-hardening, only if these two criterions are meet, the
ECC matrix substantially improved its frost resistance. material has stable saturated multiple micro-cracking behavior under tensile load
FA is also considered as a beneficial ingredient for long-term [35]. In addition, based on the micromechanics theory, fiber bridging complemen-
strength development of ECC due to its pozzolanic properties, tary energy J0b and matrix fracture energy Jtip are closely related to the pseudo
strain-hardening process of ECC. In 1999, the ratio J0b /Jtip has been suggested by
and promotes self-healing behavior due to tighter crack width
Kanda and Li as an index (PSH Index) for quantifying the robustness of tensile duc-
and a higher amount of unhydrated cementitious material avail- tility in ECC [36–37]. Fig. 4 [36] shows a typical stress-strain curve for strain-
able for further hydration [25–27]. In the previous studies, Zhang hardening composite, hatched area represents Jb0 , shaded area represents matrix
et al. [28] produced three ECC mixtures proportions with different toughness.
volumes of FA to investigate the mechanical properties and self- Three-point bending and single-crack tension test were carried out to obtain Jtip
and Jb0 , respectively. Based on the data recorded in three-point bending test, frac-
healing behavior of ECC. From the study, it was observed that ture toughness Km and Jtip were derived according to Ref. [35,38].
ECC mixture with FA/cement ratios of 4.0, by weight revealed the Then, on the basis of results from the single-crack tension test, specific peak
best self-healing behavior. Based on tests under two different heal- stress roc and corresponding crack opening displacement doc were obtained. Com-
ing conditions, Sß ahmaran [29] indicated that micro-cracked ECC plementary energy J0b is computed according to Eq. (1).
mixtures could still obtain considerable tensile stress and strain Z doc
and restore almost the original stiffness, which showed excellent Jtip J0b ¼ roc doc rðdÞdd ð1Þ
0
self-healing behavior. Therefore, FA plays a very important role
on mechanical properties of ECC and the impact of FA cannot be
underestimated and is worthy of investigation. However, the pre- 3. Results and discussion
vious studies on the influence of FA on the performance of ECC
are largely focused on the volume, the factors such as fineness 3.1. Effect of fineness
and calcium content of FA has received limited attention.
Consequently, in this paper, to contribute to the achievement of Adding 1 g grinding aid (SikaGrind 700), FA-1 was milled by
sustainable development, series of comprehensive experimental planetary ball mill machine for 5 min, 10 min and 15 min, respec-
studies were conducted to figure out the effect of fineness and cal- tively. Then the specimens were divided into group A, B, and C. The
cium content of FA on the mechanical performance of ECC. fineness and particle size distribution are detailed plotted in Fig. 5
and Table 3, respectively. It can be seen from Fig. 5 that along with
the increment of grinding time, the peak of particle size graph line
2. Materials and methods gradually moves toward Y axis, that is to say, the particle size
becomes finer. In addition, while the specific surface areas of group
2.1. Materials and preparation
A, B and C are 646.9 m2/kg, 750.4 m2/kg and 850.1 m2/kg in turn, it
According to ASTM C618 requirements, four kinds of FA originated from differ- can be concluded that the specific surface area increases with an
ent power plants, Class F FA (FA-1, FA-2, FA-3) and Class C FA (FA-4); Type II ordi- increment in grinding time.
nary Portland cement; polyvinyl alcohol (PVA) fibers; a polycarboxylate-based
high-range water-reducing admixture (HRWRA) were used for the preparation of
3.1.1. Tensile properties
ECC. In addition, 0.1% by weight of thickener (methyl cellulose) was added for the
fiber dispersion [30]. The chemical compositions of cement and different types of The uniaxial tensile stress-strain curves of ECC with FA-1 having
FA obtained by XRF are reported in Table 1. In order to reduce the binding effect different finenesses are illustrated in Fig. 6 for different ages.
between the fiber and the matrix interface due to the strongly hydrophilic nature Effects of fineness of FA on the tensile properties of ECC are
of PVA fibers, the surface of the fiber is treated with oil (1.2%, by weight) [31]. reported in Table 4. It could be seen that whether it was 7 days
Representative proportions for ECC mixtures are presented in Table 2.
All mixtures were prepared based on Table 2 in a 5 L-capacity mixer. The raw
or 28 days, the curve of group B was farthest from Y-axis, and
materials and thickener were mixed together for 2 min. Then, HRWRA and water the group C was between A and B. This showed that the overall ten-
were added and mixed to reach a moderate fluidity of matrix. Finally, PVA fibers sile properties of group B were better than other two groups.
478 L.-l. Kan et al. / Construction and Building Materials 209 (2019) 476–484
Table 1
Chemical compositions of cement and different types of fly ash.
Table 2 It was clear that the tensile strain capacity did not increase with
Mixture design proportion of ECC specimen. the increase of fineness. At the age of 28 days, the tensile strain
Components (kg/m3) capacity of group B was the largest which reached 4.35 ± 0.24%, fol-
Cement Sand FA Water HRWRa MCb Fiber
lowed by group C, 3.53 ± 0.48%, and the least was group A,
3.12 ± 0.52%. Group B was 1.23% higher than group A, and the dif-
346.33 346.33 808.10 346.33 10.17 1.88 24.29
ference between the two groups’ surface areas was about 100 m2/
a
HRWR: High Range Water Reducer. kg. When the surface area of group B was increased by 100 m2/kg,
b
MC: Thickener (Methyl cellulose). the ultimate tensile strain capacity was reduced from the maxi-
mum to the minimum, and the difference was 0.82% while tensile
stress showed no significant difference. Compared with the speci-
mens of 7 days, it was also observed that the increase of fineness
did not increase the strain capacity. Additionally, the ductility of
medium-fineness-FA specimen was the best, and the difference
between the tensile stress of specimens was not as obvious as
the ductility. Based on the distribution of cracks, it should be noted
that the uniform cracking performance was consistent with the
ductility performance. Cracks’ distribution of group B with inter-
mediate fineness was more uniform, and the number of cracks
was more than that the other two groups. Therefore, the effect of
fineness of FA on the ductility of ECC was by no means monoto-
nous and simply linear.
Fig. 2. (a) Geometry of notched beam (Note: all dimensions are in mm) and (b) Three-point bending test set up.
L.-l. Kan et al. / Construction and Building Materials 209 (2019) 476–484 479
Fig. 3. Schematic dimension for single-crack tension tensile test (Note: all dimensions are in mm).
4 Group B (10 min) group B specimens were better, and the behavior of multiple
Group C (15 min) micro-cracking was also more apparent. Table 6 indicated that
group B was higher than the other two groups in both fracture
3 toughness Km and fracture Energy Jtip, which the Km was
0.40 ± 0.01 MPam1/2 and Jtip was 9.96 ± 0.11 Jm2. Table 7 also
showed that the complementary energy J0b of group B was also
2 reached 1246 ± 173.29 Jm2 which was the highest among groups,
enabled the PSH index J0b /Jtip exceeded 100.
It is known that J0b is the reflection of crack bridging capacity
1 provided by fibers, and a relatively lower Jtip to a higher J0b pro-
motes flat crack propagation which leads to more cracks. There-
fore, it is illustrated that PSH index J0b /Jtip remains the precise
0 relation with tensile capacity, and still acceptable as a criterion
0.1 1 10 100 to quantify the tensile ductility of ECC. This further indicated that
the relationship between fineness and the high ductility of ECC is
Diameter( m)
not strictly linear. The fineness of FA could be changed to achieve
Fig. 5. Particle size distribution of FA-1 under different grinding time. more stable saturated multiple micro-cracking behaviors of ECC,
and the ductility could also be improved appropriately.
Table 3
Fineness features of three groups of FA-1.
3.2. Effect of calcium content
Group A B C
Three kinds of FA (FA-2, FA-3 and FA-4) were divided into three
Mean diameter (lm) 9.738 7.507 5.830 groups according to different amount of calcium contents. The XRD
Specific surface area (m2kg1) 646.9 750.4 850.1 results are illustrated in Fig. 8.
3.0 3.0
A-7days (a) 1 A-28days (b) 1
2.5 2 2.5 2
3 3
Stress (MPa)
Stress (MPa)
2.0 2.0
1.5 1.5
1.0 1.0
0.5 0.5
0 0
0 1 2 3 4 5 6 0 1 2 3 4 5 6
Strain (%) Strain (%)
3.0
B-7days (c) 1 2.5 B-28days (d) 1
2.5 2 2
3 3
2.0
2.0
Stress (MPa)
Stress (MPa)
1.5
1.5
1.0
1.0
0.5 0.5
0 0
0 1 2 3 4 5 6 0 1 2 3 4 5 6
Strain (%) Strain (%)
3.0 3.0
C-7days (e) 1 C-28days (f) 1
2 2.5 2
2.5
3 3
2.0
Stress (MPa)
2.0
Stress (MPa)
1.5 1.5
1.0 1.0
0.5 0.5
0 0
0 1 2 3 4 5 6 0 1 2 3 4 5 6
Strain (%) Strain (%)
Fig. 6. Uniaxial tensile stress–strain curves of ECC with different fineness FA at 7 and 28 days ages.
Table 4 Table 5
Tensile properties of ECC specimens with different fineness FA-1. Effect of FA-1 with different fineness on the
compressive properties of ECC at 28 days.
Mixture Ultimate tensile stress (MPa) Tensile strain capacity (%)
Mixture Compressive strength (MPa)
A-7d 2.39 ± 0.27 4.26 ± 0.26
A-28d 2.32 ± 0.28 3.12 ± 0.52 A 45.4 ± 1.67
B-7d 2.44 ± 0.10 4.94 ± 0.31 B 35.8 ± 0.82
B-28d 2.28 ± 0.08 4.35 ± 0.24 C 32.0 ± 1.07
C-7d 2.20 ± 0.09 4.16 ± 0.39
C-28d 2.23 ± 0.26 3.53 ± 0.48
minimum was the FA-4 which was 3.27 ± 0.23 MPa. Therefore,
the early strength of the ECC would not be greater with the
3.03 ± 0.41%. However, the effect of different calcium content on increase of calcium content.
ultimate tensile stress was not significant, and the maximum of According to the Fernéndez-Jiménez’s microanalysis of the pre-
tensile stress at 7 days was FA-2 which was 3.73 ± 0.22 MPa. The vious study [42], it was observed that the active Si/Al ratio of gel
L.-l. Kan et al. / Construction and Building Materials 209 (2019) 476–484 481
Table 6
Fracture toughness of ECC with different fineness FA-1.
Mixture Mass (kg) Peak load (kN) Fracture toughness Km (MPam1/2) Fracture Energy Jtip(Jm2)
A 1.86 ± 0.02 0.37 ± 0.03 0.36 ± 0.03 7.97 ± 1.30
B 1.79 ± 0.05 0.42 ± 0.01 0.40 ± 0.01 9.96 ± 0.11
C 1.84 ± 0.02 0.35 ± 0.06 0.34 ± 0.05 8.01 ± 1.79
Table 7
Test results of single-crack tension test for ECC with different fineness FA-1.
Mixture Peak stress roc (MPa) Crack opening doc (mm) Fiber bridging complementary energy J0b (Jm2) PSH index J 0b =Jtip
4.5 Table 8
Effect of FA with different calcium content on the tensile properties of ECC.
4.0 C
Curing Mixture Ultimate tensile stress Tensile strain capacity
age (MPa) (%)
3.5
7d FA-2 3.73 ± 0.22 3.84 ± 0.24
FA-3 3.30 ± 0.02 4.31 ± 0.64
3.0
Stress (MPa)
FA-2 tent of SiO2 in FA. It was noted that Ca2+ could reduce the chemical
FA-3 6 7d
28d
150d
5
FA-4
Stress (MPa)
10 20 30 40 50 60 70
3
2-Theta (°)
1
product was related to the development of the strength of cement-
based system. When the Si/Al ratio in the gel was close to 1.8, there
would be a balance between Si and Al which was favorable for 0
FA-2 FA-3 FA-4
quick setting and early strength. Based on XRF analysis, the Si/Al
ratio of FA-2 was 1.527 which was closest to 1.8, whereas FA-3 Fig. 9. Comparison of ultimate stress of ECC with different calcium content FA at
was 1.273 which was farthest from 1.8. Furthermore, because the different ages.
482 L.-l. Kan et al. / Construction and Building Materials 209 (2019) 476–484
bond strength of the gel products, and if the amount of Si in the gel and strain capacity of specimens at different age are shown in
was low when the alkali is activated, the bond strength of the low- Fig. 9 and Fig. 10, respectively.
silica gel would be weakened and some gel products of low degree It can be demonstrated that the ultimate tensile stress of spec-
of polymerization would be formed at the same time, which would imens increased with age, while the strain capacity had a different
lead to the decline of the strength of the whole matrix. The SiO2 level of decrement and deterioration of ductility. The changes were
content of FA-3 was the highest which was 51.7%, while the FA-2 most significant in group FA-2, while the tensile strain capacity at
was 42.3% and the FA-4 was the least, only 35.4%. 28 days decreased by 50% compared with that at 7 days. In conse-
In terms of ultimate strain capacity, the above studies found quence, it can be considered that the effect of strength develop-
that the particle size of FA in group B was 7.507 lm, and the duc- ment of group FA-3 on ductility was weaker and the
tility was the best among the three groups. The particle size of the performance was more stable compared to the other two groups.
FA-3 used in this experiment was 7.654 lm, which was closest to And it can also be clearly seen that at the same age, the strain
group B, and the ductility was also the best. It was proved again capacity of group FA-3 was the highest. In conclusion, through
that the ductility of the ECC was not changed with the fineness the comparison of three groups after curing at different ages, the
of FA monotonously but had an optimum particle size within a cer- best of cracking performance and tensile properties was group
tain value range. Results of comparison of ultimate tensile stress FA-3, followed by group FA-2, and the worst was group FA-4.
3d
3.2.3. The assurance of high ductility
7d
40 28d Three-point bending test results are showed in Table 9. The
Compressive Strength (MPa)
Table 9
Fracture toughness of ECC with different calcium content FA.
Sample Mass (kg) Peak load (kN) Fracture toughness Km (MPam1/2) Fracture energy Jtip(Jm2)
FA-2 1.85 ± 0.01 0.45 ± 0.05 0.42 ± 0.04 11.99 ± 2.28
FA-3 1.83 ± 0.01 0.49 ± 0.02 0.44 ± 0.01 17.43 ± 0.97
FA-4 1.85 ± 0.03 0.51 ± 0.04 0.46 ± 0.03 13.92 ± 1.72
L.-l. Kan et al. / Construction and Building Materials 209 (2019) 476–484 483
Table 10
Test results of single-crack tension test with different calcium content FA.
Mixture Peak stress roc (MPa) Crack opening doc (mm) Fiber bridging complementary energy J0b (Jm2) PSH index J 0b =Jtip
6 Conflicts of interest
[23] J. Yu, C.K.Y. Leung, Strength improvement of strain-hardening cementitious [33] E399–12, Standard test method for linear-elastic plane-strain fracture
composites with ultrahigh-volume fly ash, J. Mater. Civil. Eng. 29 (9) (2017) 1– toughness KIC of metallic materials, ASTM International, West
8. Conshohocken (PA), 2012.
[24] M. Sß ahmaran, E. Ozbay, H.E. Yucel, et al., Frost resistance and microstructure of [34] K.Q. Yu, Y.C. Wang, J.T. Yu, et al., A strain-hardening cementitious composites
Engineered Cementitious Composites: influence of fly ash and micro poly- with the tensile capacity up to 8%, Constr. Build. Mater. 137 (2017) 410–419.
vinyl-alcohol fiber, Cem. Concr. Comp. 34 (2) (2012) 156–165. [35] S. Xu, H.W. Reinhardt, Determination of double-K criterion for crack
[25] E. Ozbay, M. Sß ahmaran, M. Lachemi, et al., Self-healing of microcracks in high- propagation in quasi-brittle fracture, Part II: Analytical evaluating and
volume fly-ash-incorporated Engineered Cementitious Composites, ACI Mater. practical measuring methods for three-point bending notched beams, Int. J.
J. 110 (1) (2013) 33–44. Fracture 98 (2) (1999) 151–177.
[26] M. S ß ahmaran, G. Yıldırım, G. Aras, et al., Self-Healing of cementitious [36] T. Kanda, New micromechanics design theory for pseudostrain hardening
composites to reduce high CO2 emissions, ACI Mater. J. 114 (1) (2017) 93–104. cementitious composite, J. Eng. Mech. ASCE 125 (4) (1999) 373–381.
[27] G. Yıldırım, A.H. Khiavi, S. Yesßilmen, et al., Self-healing performance of aged [37] V.C. Li, C.K.Y. Leung, Theory of steady state and multiple cracking of random
cementitious composites, Cem. Concr. Comp. 87 (2018) 172–186. discontineous fiber reinforced brittle matrix composites, J. Eng. Mech. ASCE
[28] Z.G. Zhang, S.Z. Qian, H. Ma, Investigating mechanical properties and self- 118 (11) (1992) 2246–2264.
healing behavior of micro-cracked ECC with different volume of fly ash, Constr. [38] V.C. Li, Performance driven design of fiber reinforced cementitious composites,
Build. Mater. 52 (2014) 17–23. in: Proceedings of Rilem International Symposium on Fiber Reinforced
[29] M. S ß ahmaran, V.C. Li, Durability of mechanically loaded engineered Concrete, 1992, pp. 12–30.
cementitious composites under highly alkaline environments, Cem. Concr. [39] S. Wang, V.C. Li, Engineered Cementitious Composites with high volume fly
Comp. 30 (2) (2008) 72–81. ash, ACI Mater. J. 104 (3) (2007) 233–241.
[30] S. Chen, R. He, Y. Li, et al., Influence of thickeners on cement paste structure [40] M.D. Lepech, V.C. Li, R.E. Robertson, et al., Design of green Engineered
and performance of engineered cementitious composites, J. Wuhan. Univ. Cementitious Composites for improved sustainability, ACI Mater. J. 105 (6)
Technol. Mater. 28 (2) (2013) 285–290. (2008) 567–575.
[31] Z.G. Zhang, Q. Zhang, Matrix tailoring of Engineered Cementitious Composites [41] V.C. Li, S. Wang, C. Wu, Tensile strain-hardening behavior of PVA-ECC, ACI
(ECC) with non-oil-coated, low tensile strength PVA fiber, Constr. Build. Mater. Mater. J. 98 (6) (2001) 483–492.
161 (2018) 420–431. [42] A. Fernández-Jiménez, A. Palomo, I. Sobrados, et al., The role played by the
[32] JSCE, Recommendations for design and construction of high performance fiber reactive alumina content in the alkaline activation of fly ashes, Micropor.
reinforced cement composites with multiple fine cracks, Japan Society of Civil Mesopor. Mater. 91 (1) (2006) 111–119.
Engineers, Tokyo, 2008, 1–16.