Construction and Building Materials 251 (2020) 118851

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Construction and Building Materials

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

A study on fracture toughness of ultra-high toughness geopolymer

composites based on Double-K Criterion
Xiaomei Wan a,b,⇑, Chen Shen a, Penggang Wang a, Tiejun Zhao a,b, Yu Lu a
a
School of Civil Engineering, Qingdao University of Technology, Qingdao 266033, China
b
Cooperative Innovation Center of Engineering Construction and Safety in Shandong Blue Economic Zone, Qingdao University of Technology, Qingdao 266033, China

h i g h l i g h t s

An Ultra-high toughness geopolymer composites (UHTGC) were fabricated.

Both initial fracture toughness and unstable fracture toughness of UHTGC is improved.

The fracture energy of UHTGC is up to 77 times than that of specimens without fiber.

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

Article history: Ultra-high toughness geopolymer composites (UHTGC) were fabricated based on the matrix of binder
Received 14 July 2019 composed of alkali-activated fly-ash and granulated blast furnace slag and fiber of polyvinyl alcohol
Received in revised form 14 March 2020 (PVA) in this paper. The tensile behavior and fracture toughness of UHTGC are investigated on both macro
Accepted 21 March 2020
and micro scales experimentally and analyzed based on Double-K Criterion. With slag content of 20% and
Available online 11 April 2020
curing temperature 60 °C, the average strain of the composite under uniaxial tension load is more than
3% with pseudo-strain hardening behavior and multiple cracking. Both initial fracture toughness and
Keywords:
unstable fracture toughness of geopolymer is improved by adding PVA fibers. The fracture energy of
Fracture energy
Toughness
UHTGC is up to 77 times of that of mixes without fiber. The results of nanoindentation test verified that
Geopolymer the modulus of elasticity increases with curing temperature, while the fracture energy decreases slightly
Double-K Criterion with curing temperature.
Nanoindentation test Ó 2020 Elsevier Ltd. All rights reserved.
Sustainability

1. Introduction
Ultra-high toughness geopolymer composites (UHTGC) is a new
type of building material with sustainable and high performance. It
is a class of geopolymer-based materials typically reinforced by
polyvinyl alcohol (PVA) fibers. Owing to the advantages of high
strain capacity and tensile stress, UHTGC can be used to improve
the toughness of geopolymer matrix significantly, and to solve
the problems of pollution and high energy consumption caused
by traditional cement-based composites. Owing to its high tough-
ness and crack control ability, this material has the potential to
applied as repaired materials to structural members such as
beams, walls, columns, beam–column connections, and so on.
The design of UHTGC is similar to that of strain hardening
cement-based composites (SHCC) developed by V. C. Li and is
based on the principles of micromechanics and fracture mechanics
⇑ Corresponding author.
E-mail address: wanxiaomei1211@hotmail.com (X. Wan).
[1]. From the viewpoint of structural design, the strain hardening
behavior in tension and flexural toughness is often referred to as
the most relevant feature of UHTGC.
Similar with strain hardening geopolymer composite (SHGC),
firstly proposed by Ohno in 2014 [2], another predominant feature
of UHTGC is that it utilizes a large amount of industrial waste to
make it more suitable for the situation of global energy saving
and emission reduction. Ohno and Li et al. [3] studied the environ-
mental factors of EGC series. In the case of carbon equivalent emis-
sions, EGC materials show an excellent performance; global
warming indexes (GWI) of EGC is 56–65% of those of concrete
materials, and 30% less even when compared with the SHCC. The
carbon footprints of the PVA fiber are moderate, which offers an
advantage in the GWI reduction. For cost analysis, in the research
of Abdollahnejad et al. [4], the cost of 30% OPC + 70% FA is 1/3
lower than that of OPC due to the relatively low price of fly ash.
For EGC, PVA fiber and alkaline activator are the major contributors
to the total cost. Compared with the cost of SHCC, EGC needs addi-
tional alkaline activator. However, due to the absence of coarse

https://doi.org/10.1016/j.conbuildmat.2020.118851
0950-0618/Ó 2020 Elsevier Ltd. All rights reserved.
2 X. Wan et al. / Construction and Building Materials 251 (2020) 118851

Nomenclature

E Young’s modulus P load

Et initial modulus of elasticity a crack length
Etu modulus of elasticity for hardening stage a0 initial crack length
rnt initial crack stress ac critical equivalent crack length
e strain GF fracture energy
ent initial crack strain W work done by the external force
etu ultimate strain A cross-sectional area
a distance between the support and loading point h height of the specimen
b, B width and thickness of specimens Er modulus of reduction
m slope of the tangent to the straight-line portion of the v Poisson’s ratio
load-deflection curve WE elastic energy
rf flexural strength Afra maximum contact area
D displacement WP plastic work
l length of specimens WT total energy
K ini
Ic initial fracture toughness Vt total energy coefficient
K un
Ic unstable fracture toughness Ve elastic energy coefficient

aggregate in SHCC, it still needs a large amount of cement. There-
fore, the cost of the two materials is similar, but EGC is better than
SHCC in terms of embodied energy and carbon footprint.
UHTGC possess the similar basic characteristics as SHCC, such
as strain hardening and multiple micro-cracks. When UHTGC is
subjected to the axial tensile load, the first crack occurs at the place
where the defect size of the matrix is the largest. Then the fibers in
the UHTGC materials sustain the load, and the bridge stress is pro-
vided. The cracks in the matrix expand in a steady-state cracking
mode, that means the stress and deformation fields at the crack
tip remain unchanged during the crack development [5]. On the
basis of SHCC research, there are more and more theoretical stud-
ies on EGC recently. Ohno and V. C. Li et al. [2] found that the max-
imum crack width of SHGC is 117 mm and the average crack width
is 45 mm even at high tensile strain level (4.5%), which means
pseudo-strain hardening behavior and multiple micro-crack under
tension load are obtained for SHGC. Nematollahi, et al. [6,7] con-
cluded that in a certain range, the decrease of alkali/binder ratio
results in the increase of initial cracking strength, ultimate tensile
strength and tensile strain capacity of EGC. Both Na-based and K-
based alkali activated engineering geopolymer composites exhibit
strain hardening behavior.
In recent years, great attention has been paid to determining
the fracture toughness of materials such as rock and concrete. Frac-
ture toughness provides a criterion for interpreting their crack
resistance under different loads [8]. Furthermore, the degree of
crack propagation is determined by fracture toughness, which
has important significance for analyzing the performance of con-
crete [9,10]. In 1961, Kaplan [11] first integrated the fracture
mechanics theory into the research of concrete materials and

Table 1
Chemical composition of GBFS and FA.

Oxide (wt%) CaO SiO2 Al2O3 MgO TiO2 SO3 Fe2O3 MnO Na2O
GBFS 57.11 22.53 10.98 3.36 1.87 1.77 0.91 0.47 0.21
FA 8.59 39.99 25.43 0.62 2.17 1.26 16.93 0.19 0.54

Table 2
Properties of PVA fiber.
a
Fiber Nominal strength (MPa) Diameter (mm) Length (mm) Young’s modulus (GPa) Elongation (%) Oil coating (%)
REC15 PVA 1620 39 12 42.8 6.0 0.8
a
Apparent fiber strength is 1092 MPa.

Table 3
Mix proportions of UHTGC specimens.

Mix Binder Sand (wt%) Activator (wt%) Fiber (v/v %)

Fly ash (wt%) Slag (wt%)
M1 80 20 30 35 2
M2 80 20 30 35 0
M3 60 40 30 35 2
M4 80 40 30 35 0
M5 0 100 30 35 2
M6 0 100 30 35 0
 X. Wan et al. / Construction and Building Materials 251 (2020) 118851 3

(a)Dimension diagram of dumbbell specimen.

(b)Loading process of uniaxial tension test.

Fig. 3. Samples (a) and instrument (b) of nanoindentation test.
Fig. 1. Details of the uniaxial tension test.

(a) Iron sheet and triple mould for preparing notched beam

(b)Three-point bending test schematic of notched beams. (c) Loading process of three-point bending test for notched beams.

Fig. 2. Details of the three-point bending test.

4 X. Wan et al. / Construction and Building Materials 251 (2020) 118851

90
90
3
80 3
7 80
7
28
70 28
56 70
56
60
60
Stress (MPa)

Stress (MPa)
50
50

40
40

30
30

20
20

10
10

0
M1-20 M2-20 M3-20 M4-20 M5-20 M6-20 0
M1-60 M2-60 M3-60 M4-60 M5-60 M6-60
(a) Curing temperature is 20°C . (b) Curing temperature is 60°C.

90

3
80
7
70
28
56
60
Stress (MPa)

50

40

30

20

10

0
M1-80 M2-80 M3-80 M4-80 M5-80 M6-80
(c) Curing temperature is 80°C .

Fig. 4. Compressive strength of different mix proportions.

began to use the fracture mechanics method to determine the frac-
ture toughness parameters of concrete. In the subsequent research,
many fracture models have been proposed by scholars, such as Fic-
titious Crack Model (FCM) [12], Two-parameter Fracture Model
(TPFM) [13] and so on. Although these models can not reflect the
whole process characteristics of concrete fracture yet, they provide
a foundation for the later development of concrete fracture perfor-
mance. Xu et al. proposed a resistance curve KR based on crack
cohesion [14] and the Double-K Fracture Model [15], which solved
the problem of characterization of the whole process of concrete
fracture. According to the Double-K Fracture Model, two parame-
ters of initiation fracture toughnessK ini
Ic and unstability fracture
toughness K un
Ic are introduced to describe the process of concrete
crack propagation.
Many researchers have done a lot of research on the fracture
properties of fiber reinforced concrete based on different fracture
theories. Aliha et al. [16] studied the properties of fracture Mode
I and Mode III of fiber reinforced cementitious composites. It is
showed that the fiber reinforced cementitious composites exhibits
excellent post peak failure response and significant amount of
energy is required for overall breakage of composites. Rooholamini
et al. [17] found that based on three-point bending test results on
notched beam, fiber, cement, and water linearly affect the flexural
strength. Especially, fiber tended to influence the fracture energy
more significantly than flexural strength.
Due to the relatively late appearance of UHTGC, there is still a
lack of systematic research results on toughness and fracture
properties of UHTGC. Therefore, an ultra-high toughness
geopolymer composites (UHTGC) were fabricated and the
mechanical properties and fracture properties were studied in
this paper. The results of mechanical and fracture properties
are helpful to understand the behavior and optimize the design
of UHTGC. The tensile properties of UHTGC were tested experi-
mentally, and the strain–stress curves under tensile loads are
obtained. Different stages of stress–strain curve (elastic stage,
hardening stage and failure stage), and corresponding crack
 X. Wan et al. / Construction and Building Materials 251 (2020) 118851 5

5
5
M1-20-1 M3-20-1
4 M1-20-2 M3-20-2
4
M3-20-3
Stress (MPa)

Stress (MPa)
3
3

2 2

1 1

0 0
0 1 2 3 4 0 1 2 3 4
Strain (%) Strain (%)
(a) M1-20 (d) M3-20
5
5
M1-60-1 M3-60-1
M1-60-2 M3-60-2
4 4
M1-60-3 M3-60-3
Stress (MPa)

Stress (MPa)
3 3

2 2

1 1

0 0
0 1 2 3 4 0 1 2 3 4

Strain (%) Strain (%)

(b) M1-60 (e) M3-60

5 5
M1-80-1 M3-80-1
4
M1-80-2 M3-80-2
4
M1-80-3 M3-80-3
Stress (MPa)

Stress (MPa)

3 3

2 2

1 1

0 0
0 1 2 3 4 0 1 2 3 4
Strain (%) Strain (%)
(c) M1-80 (f) M3-80
Fig. 5. Strain-stress curves of specimens with different mix proportions under tensile load.

propagation are analyzed. Fracture toughness was evaluated by 2. Experimental program

four-point bending test and three-point bending test of notched
beam. The fracture toughness index of Mode I and fracture
energy were calculated based on double-K fracture criterion. In
addition to macro-test, the micro-mechanical properties of the
materials were characterized by nanoindentation test. And the
effects of the ratio of fly ash to slag and curing temperatures
on the mechanical and fracture properties of UHTGC are also dis-
cussed. Finally, the micro morphology and composition of
UHTGC were analyzed by SEM-EDS.
2.1. Materials
A Grade I fly ash (FA) and a S95 granulated blast furnace slag
(GBFS) were selected as binding materials, whose chemical compo-
sitions are given in Table 1. A mixture of water glass and sodium
hydroxide solution was prepared as alkaline activator. The modu-
lus of water glass mixture is 1.8, and the content of sodium oxide
is 9%. The water glass is provided by Qingdao Bay Solver Chemical
6 X. Wan et al. / Construction and Building Materials 251 (2020) 118851

5 5 min continually. After mixing, the mixtures were cast into dumb-
M5-20-1 bell moulds and 40 mm  40 mm  160 mm prism moulds. The size
4 M5-20-2 of the compression specimens which come from fractured prisms
M5-20-3 after bending test is equivalent to 40 mm  40 mm  40 mm.
Stress (MPa)

3
The specimens with moulds were then placed under different tem-
peratures (20 °C, 60 °C and 80 °C) for 12 h. Then the specimens were
demolded and cured in a cabinet with 65 ± 5% relative humidity and
2
20 ± 2 °C temperature until to 28 days.

1
2.3. Uniaxial tension tests
0
0 1 2 3 4 In order to obtain the stress–strain curves, dumbbell specimens
Strain (%) are selected to carry out direct tensile test according to Chinese
(g) M5-20 National Standard JC/T 2461-2018 [18] under external clamping
5 on the electronic tensile testing machine, SHIMADZU AG-IS, with
M5-60-1 the maximum load of 250kN and the loading rate of 0.05 mm/
M5-60-2 min. Dimensions of dumbbell-shaped specimens and loading mode
4
M5-60-3 for uniaxial tensile testing are presented in Fig. 1. LVDT is fastened
Stress (MPa)

to both sides of the test area and connected to the computer for
3
data acquisition. The tensile properties and strain hardening

0
0 1 2 3 4
Strain (%)
(h) M5-60
5
M5-80-1
4 M5-80-2
Stress (MPa)

0
0 1 2 3 4
Strain (%) (a) M1-20
(i) M5-80
Fig. 5 (continued)

Co., Ltd. The selected fine aggregates are quartz sand with a
maximum particle size of 600 mm. High modulus PVA fibers pro-
duced by KURARAY Co., Ltd are used. The properties are shown
in Table 2.
In the mix design, the influence of GBFS content in cementitious
materials and curing temperature is mainly considered. Six series
of UHTGC with different mix proportion were prepared, each mix
is cured in three kinds of temperature environment as 20 °C,
60 °C and 80 °C respectively. The mass ratio of alkaline solution
to cementitious material is 0.35. The mix proportions are shown
in Table 3.

2.2. Specimens fabrication

The cementitious materials and quartz sand were put into the
mixer and stirred for 2 min. Then the alkaline activator was added, (b) M1-60
and the mixture was stirred slowly for 2 min and stirred quickly for
1 min. Finally, the fiber was added, and the mixture were stirred for Fig. 6. Cracks distribution and cracks width.
 X. Wan et al. / Construction and Building Materials 251 (2020) 118851 7

(c) M1-80

(d) M3-60

Fig. 7. Bilinear Model Fitting.

behavior of specimens were analyzed based on the tensile stress-

strain curves obtained.

2.4. Four-point bending tests

Four-point bending tests with partly reference to the ASTM C

1018-97 [19] was conducted on the specimens with the size of
40 mm  40 mm  160 mm. The loading rate is 0.1 mm/min.
The deflection at the center of the specimen was measured by
means of a LVDT. The flexural toughness, elastic modulus, load-
deflection diagrams were analyzed accordingly.

2.5. Three-point bending tests of notched beam

(e) M5-60
In order to obtain the parameters for calculating fracture tough-
Fig. 6 (continued) ness and fracture energy, three-point bending tests of notched
beams were carried out on the specimens with the size of
8 X. Wan et al. / Construction and Building Materials 251 (2020) 118851

7 7

M1-20-1 M3-20-2
6 M1-20-2 6 M3-20-3
M1-20-3 M3-20-1
5 5

Load (kN)
Load (kN)

4 4

3 3

2 2

1 1

0 0
0 1 2 3 4 5 6 0 1 2 3 4 5 6
Deflection (mm)
Deflection (mm)
(a) M1-20 (d) M3-20
7
7
M3-60-1
M1-60-1
6 M3-60-2
6 M1-60-2
M3-60-3
M1-60-3
5
5
Load (kN)

4
Load (kN)

3
3

2
2

1
1

0 0
0 1 2 3 4 5 6 0 1 2 3 4 5 6

Deflection (mm) Deflection (mm)

(b) M1-60 (e) M3-60
7 7

M1-80-1 M3-80-1
6
M1-80-2 6 M3-80-2
M1-80-3 M3-80-3
5
5
Load (kN)

4
Load (kN)

3
3

2
2

1
1

0
0 1 2 3 4 5 6 0
0 1 2 3 4 5 6
Deflection (mm)
Deflection (mm)
(c) M1-80 (f) M3-80
Fig. 8. Load-deflection curve of specimens with 2% fiber content under four-point bending load.
 X. Wan et al. / Construction and Building Materials 251 (2020) 118851 9

7 40 mm  40 mm  160 mm with reserved notch of 20 mm in

M5-20-1 height and 1 mm in width in span center. The customized sheet
6 M5-20-2 iron which was fixed on the triple mold (for prism specimen of
40 mm  40 mm  160 mm) with glue was used to reserve the
5
notch for the specimens, as shown in Fig. 2(a). Three-point bending
tests were performed under the electronic universal testing
machine, SHIMADZU AG-IS, with the loading rate of 0.1 mm/min.
Load (kN)

4
In addition to measuring mid-span deflection by LVDT, the crack
opening of the specimen is measured by the clip extensometer at
3 the bottom. The loading details are shown in Fig. 2. P-CMOD curve
and load-deflection curve were obtained, and the fracture related
2 parameters were calculated accordingly. According to the research
of Aliha et al. [20–22], lower temperature will increase the mea-
1 sured fracture toughness. Therefore, the test was carried out in a
constant temperature laboratory to eliminate the interference of
0
ambient temperature on the results.
0 1 2 3 4 5 6
Deflection (mm) 2.6. Nanoindentation tests

(g) M5-20 The nanoindentation samples were prepared at the curing age
7 of 28 days. The prepared nanoindentation sample and loading pro-
cess are given in Fig. 3. The specimens were crushed into 10 mm
M5-60-1 pieces, soaked in alcohol for 24 h. After being dried, the samples
6 M5-60-2 were cold inlaid with epoxy resin and then grinded. The mesh
number of grinding papers is 800, 1500, 2000, 2500 and 3000 in
5 turn, and the grinded time is 1 min for each grind. After grinded,
the samples were polished by polishing suspension with fineness
of 3 mm and 1 mm. The polishing time is 5 min for each sample.
Load (kN)

4
The nanoindentation instrument is Nano Indenter G200 with a
3 triangular Berkovich diamond indenter with an angle of 65.03
between the center line and the conical surface. The duration of
2
loading is 10 s, the maximum compressive load is 500 mN, and
both loading and unloading rates are 20 mN/s. The center distance
between measuring point is not less than 200 mm.
1
The elastic modulus and hardness of nano-scale were obtained
by nanoindentation test, and the fracture toughness of nano-scale
0 was obtained by loading-unloading diagram.
0 1 2 3 4 5 6
Deflection (mm)
2.7. Microstructure analysis
(h) M5-60
The matrix samples were taken and crushed into flake and mor-
7 phological analysis was conducted under Field Emission Scanning
M5-80-1 Electron Microscope (FESEM, JSM-7500F). The elemental analysis
6 M5-80-2 was also done by Energy-dispersive X-ray spectroscopy (EDS, X-
M5-80-3 MaxN) technique. Surface scanning was used to measure the sub-
5 stances adhered on the fiber surface.

3. Results and discussion

Load (kN)

3.1. Compressive strength

3

The compressive strength of specimens was determined in

2
accordance with Chinese National Standard GB/T 17671-1999
[23]. The results of all mixes are shown in Fig. 4. It can be found
1 that the compressive strength of both UHTGC and geopolymer
mortar increases with the slag content generally. This is mainly
0 due to the low ability of water glass to dissociate the glass phase
0 1 2 3 4 5 6 of the fly ash, which leads to little C-(A)-S-H produced. However,
Deflection (mm) the increase of curing temperature is beneficial to the compressive
(i) M5-80 strength, especially for the early-age compressive strength. It also
can be observed that, fibers show positive effects on compressive
Fig. 8 (continued) strength overall.
10 X. Wan et al. / Construction and Building Materials 251 (2020) 118851

2.5 2.5

M2-20-1 M4-20-1
M2-20-2 M4-20-3
2.0 M2-20-3 2.0 M4-20-2

1.5 1.5

Load (kN)
Load (kN)

1.0 1.0

0.5
0.5

0.0
0.0 0.0 0.2 0.4 0.6 0.8 1.0
0.0 0.2 0.4 0.6 0.8 1.0
Deflection (mm)
Deflection (mm)
(d) M4-20
(a) M2-20
2.5
2.5

M2-60-1 M4-60-1
M2-60-2 2.0 M4-60-2
2.0 M2-60-3 M4-60-3

1.5
Load (kN)

1.5
Load (kN)

1.0
1.0

0.5
0.5

0.0
0.0 0.0 0.2 0.4 0.6 0.8 1.0
0.0 0.2 0.4 0.6 0.8 1.0
Deflection (mm)
Deflection (mm)

(b) M2-60 (e) M4-60

2.5
2.5
M4-80-1
M2-80-1
M4-80-2
M2-80-2
2.0 2.0 M4-80-3
M2-80-3

1.5 1.5
Load (kN)

Load (kN)

1.0 1.0

0.5
0.5

0.0
0.0 0.2 0.4 0.6 0.8 1.0 0.0
0.0 0.2 0.4 0.6 0.8 1.0
Deflection (mm)
Deflection (mm)
(c) M2-80 (f) M4-80
Fig. 9. Load-deflection curve of specimens without fiber under four-point bending load.
 X. Wan et al. / Construction and Building Materials 251 (2020) 118851 11

2.5 3.2. Strain hardening behavior and ductility

M6-20-1
M6-20-2 The strain–stress curves were obtained by uniaxial tension test
2.0 M6-20-3 as shown in Fig. 5. It was found that the strain of composites
decreased generally with the increase of slag content and curing
temperature. When the tensile strength is high enough, the fiber
1.5
failure mode is changed from pull-out to breaking. When slag con-
Load (kN)

tent is 20%, the strain of composite is enhanced except for the one
under the curing temperature of 20 °C. Other mixes show a lower
strain (from 0.5% to 2%), but still behave hardening performance.
1.0
Nevertheless, proper but not high slag content is benefit for the
strain hardening of UHTGC.
Additionally, as can be seen from the distribution of cracks dur-
0.5 ing loading and the size of cracks observed by a digital microscope
in Fig. 6, when the content of slag is 20%, many fine cracks appear
on the specimens. The width of these cracks is about 20–50 mm.
0.0 Especially when the curing temperature is 60 °C and 80 °C, the
0.0 0.2 0.4
multi-cracking mode is more obvious, the crack width and the
Deflection (mm) crack spacing are smaller, and the number of cracks is more than
50. This is consistent with the rule reflected by the stress–strain
(g) M6-20 curve, that is, the more cracks, the greater the strain.
2.5 Through stress–strain curves and crack development, it can be
M6-60-1 found that fly ash contributes to the increase of toughness and the
M6-60-2 formation of multi-cracking in composite materials. Fly ash is a kind
2.0 M6-60-3 of material with morphological effect, in which glass phase plays a
role of ball, enhances the fluidity of mortar and improves the com-
pactness of composite paste. The cracks develop more uniform,
instead of developing from the initial defect to the penetrating
1.5
Load (kN)

crack. Thus, the crack merged failure of specimens can be avoided.

Present tensile models mainly involve bilinear model and three
linear model. Bilinear model considering elastic stage and strain
1.0
hardening stage, proposed by Etsushi [24], while V. C. Li proposed
the three linear model [25]. Considering the experimental situation
of this study, the bilinear model is used to fit M1-60 in this paper.
0.5 The model formula is as follows:[24]


Et e ðe  ent Þ
re ¼ ð1Þ
0.0 rnt þ Etu ðe  ent Þ ðent < e < etu Þ
0.0 0.2 0.4
Deflection (mm) where Et is initial modulus of elasticity, Etu is modulus of elasticity
for hardening stage,rnt is initial crack stress, ent is initial crack
(h) M6-60
strain, etu is ultimate strain.
2.5 The fitting results are shown in the Fig. 7. From the fitting infor-
mation, the initial elastic modulus is about 9.9 GPa and the hard-
M6-80-1 ening stage elastic modulus is about 0.21 GPa. The fitting
M6-80-2
2.0 equation is as follows:
M6-80-3


99e ðe  0:0265Þ
re ¼ ð2Þ
2:48 þ 0:21ðe  0:0265Þ ð0:0265 < e < 3:05Þ
1.5
Load (kN)

3.3. Flexural properties

1.0
The load–deflection curves of specimens of all mixes during
four-point bending are shown in Figs. 8 and 9.
0.5 According to Fig. 8, with the increase of curing temperature, the
deflection of specimens under four-point bending load decreases
generally. It is unfavorable for the enhancement of deflection with
0.0 the increase of slag content. Both high curing temperature and high
0.0 0.2 0.4 slag content improve strength, while weaken toughness. The
Deflection (mm) deflection of the specimens with fibers is about 50 times that with-
(i) M6-80 out fibers. And the flexure strength is also greatly improved which
is consistent with the results of Daneshfar et al. [26]. The difference
Fig. 9 (continued) between load–deflection curves of specimens containing fibers and
12 X. Wan et al. / Construction and Building Materials 251 (2020) 118851

Table 4
Parameters of flexural properties.

Mix Initial crack Initial crack Initial crack Ultimate Ultimate Ultimate Young’s Standard deviations
load (kN) stress (MPa) strain (%) load (kN) stress (MPa) strain (%) modulus (GPa) of young’s modulus (GPa)
M1-20 2.6 6.1 0.08 4.4 10.3 1.2 8.6 0.36
M1-60 3.2 7.5 0.13 5.5 12.9 1.7 9.1 0.20
M1-80 3.4 7.9 0.14 5.6 13.1 1.6 11.4 0.56
M2-20 1.5 3.5 0.07 1.7 3.9 0.08 5.2 0.55
M2-60 1.7 3.9 0.04 1.8 4.2 0.07 8.2 0.25
M2-80 1.7 3.9 0.04 1.9 4.5 0.07 13.1 0.17
M3-20 3.1 7.5 0.13 5.6 13.1 1.7 13.3 0.47
M3-60 3.2 7.5 0.06 5.4 12.6 0.8 14.0 1.44
M3-80 3.6 8.4 0.07 5.4 12.6 0.9 24.0 1.33
M4-20 1.3 3.0 0.04 1.4 3.3 0.04 9.4 0.26
M4-60 1.4 3.3 0.02 1.9 4.5 0.05 17.2 0.61
M4-80 1.4 3.3 0.02 1.7 3.9 0.06 18.0 0.85
M5-20 3.0 7.0 0.07 6.1 14.3 1.8 12.4 0.61
M5-60 3.5 8.2 0.04 5.6 13.1 1.1 11.4 0.87
M5-80 3.6 8.4 0.12 5.7 13.3 0.8 13.7 0.31
M6-20 0.8 1.9 0.04 1.1 2.5 0.67 8.2 0.17
M6-60 1.2 2.8 0.002 1.3 3.0 0.01 13.1 0.36
M6-80 0.7 1.6 0.005 1.0 2.3 0.01 17.0 0.85

Note: Each group of data obtained from the average of three specimens.

those without fibers lies in the hardening stage. The failure mode
of specimens without fibers is a typical brittle fracture mode, while
the one of specimens with fibers is ductile failure. Meanwhile, due
to the bridging effect of fibers, the specimens behave multiple
cracks and hardening effect under four-point bending.
The flexural strength (rf ) and the Young’s modulus (E) based on
four-point bending test are calculated as:[27]
to higher initial crack strength, but the ultimate stress shows this
trend only when the content of slag is 20%. When the content of
slag is more than 40%, this rule becomes not obvious. The elastic
modulus of specimens with fiber is in the range of 8 to 24 GPa,
which is increased with curing temperature.
3.4. Double-K fracture analysis

3Pa The P-CMOD curve obtained from the three-point bending test
rf ¼ 3
ð3Þ
b of notched beams are presented in the Figs. 10 and 11. The initial
crack load can be determined by P-CMOD curve. The appearance
2
að3l  4a2 Þ of fracture process zone at crack tip of concrete leads to the nonlin-
E¼m 4
ð4Þ earity of the rising section of P-CMOD curve, and the turning point
4b
from linear to non-linear is defined as the initial cracking point,
where P is the load, l is the length of specimens, a is the distance and the corresponding load is the initial cracking loadðP ini ).
between the support and loading point, b is the width and thickness After the initial crack load is obtained, the initial fracture tough-
of specimens, m is the slope of the tangent to the straight-line por- nessðK ini
Ic Þ is calculated by Eq. (6) and (7).
tion of the load–deflection curve.
The strain e was calculated as Eq. (5): [27] 3Pini S pffiffiffiffiffi a0 
K ini
Ic ¼ a0 F 2 ð6Þ
2BD2 D
12bD
e¼ 2
ð5Þ a  h  2 i
3l  4a2 a  1:99  0
1  aD0 2:15  3:93 aD0 þ 2:7 aD0
0 D
F2 ¼   3 ð7Þ
where e is the tensile strain and D is the displacement recorded by D 1 þ 2 aD0 1  aD0 2
LVDT.
The results of first crack strength, ultimate flexural strength, where B is the thickness of the specimen, D is the height, a0 is the
peak stress and relative strain for all mix proportion are reported initial crack length, and S is the span.
in Table 4. The data in the table are obtained from the load–deflec- The specimens used in this paper are standard three-point
tion curve, and then the three groups of data are averaged (exclud- bending notched beams with span-height ratio of 4. The P and
ing the values with large deviations). CMOD relationship are given in the Tada stress intensity factor
From the results in Table 4, the initial crack stress of the speci- manual [28] as follows:
mens with fiber is 6–9 MPa and the ultimate stress is 10–15 MPa. 24Pa  a 
The initial crack stress and ultimate stress of the specimens with CMOD ¼ V2 ð8Þ
BDE D
fiber are 2–3 times of those without fiber. A significant advantage
of UHTGC is that it takes a relatively large deflection for the bend- a 2:28a  a 2  a 3 0:66
ing stress to increase from the initial crack stress to the ultimate V2 ¼ 0:76  þ 3:87  2:04 þ 2 ð9Þ
D D D D 1a
stress. It can be concluded that higher curing temperature leads D
 X. Wan et al. / Construction and Building Materials 251 (2020) 118851 13

0.6 0.6

M1-20 M2-20
M1-60 M2-60
0.5 0.5
M1-80 M2-80

0.4 0.4

P (kN)
P (kN)

0.3 0.3

0.2 0.2

0.1 0.1

0.0 0.0
0 1 2 3 4 0.0 0.1 0.2 0.3 0.4

CMOD (mm) CMOD (mm)

(a) M1 (a) M2
0.6
0.6
M4-20
M3-20 M4-60
M3-60 0.5
0.5 M4-80
M3-80
0.4
0.4
P (kN)

0.3
P (kN)

0.3

0.2
0.2

0.1
0.1

0.0
0.0 0.0 0.1 0.2 0.3 0.4
0 1 2 3 4
CMOD (mm)
CMOD (mm)
(b) M4
(b) M3 0.6
0.6
M6-20-1
M5-20
M6-60-1
M5-60 0.5
0.5 M6-80-1
M5-80

0.4
0.4
P (kN)

0.3
P (kN)

0.3

0.2
0.2

0.1
0.1

0.0
0.0 0.0 0.1 0.2 0.3 0.4
0 1 2 3 4
CMOD (mm)
CMOD (mm)
(c) M5 (c) M6
Fig. 10. P-CMOD curve of mixes with 2 % fiber content under three-point bending Fig. 11. P-CMOD curve of mixes without fiber under three-point bending load.
load.
14 X. Wan et al. / Construction and Building Materials 251 (2020) 118851

Table 5
Double-K fracture toughness parameter.

Mix CMODc (mm) ac (mm) Pini(N) Pmax (N) K ini

Ic (MPam
1/2
) Standard deviations K un
Ic (MPam
1/2
) Standard deviations
of K ini
Ic (MPam
1/2
) of K un
Ic (MPam
1/2
)

M1-20 0.74 22.86 89.70 109.92 0.12 0.03 0.17 0.02

M1-60 0.48 22.00 188.39 224.61 0.25 0.04 0.34 0.02
M1-80 0.35 21.74 134.31 163.36 0.24 0.02 0.51 0.03
M2-20 0.06 20.70 192.90 216.30 0.26 0.03 0.29 0.01
M2-60 0.11 20.12 240.82 265.91 0.32 0.02 0.35 0.02
M2-80 0.01 24.68 170.33 196.8 0.23 0.01 0.36 0.01
M3-20 0.47 25.67 180.00 224.48 0.26 0.04 0.55 0.05
M3-60 0.27 24.81 223.12 357.89 0.29 0.03 0.66 0.07
M3-80 0.39 27.13 265.85 363.83 0.35 0.02 0.83 0.02
M4-20 0.02 24.14 118.21 132.92 0.16 0.01 0.23 0.01
M4-60 0.01 22.43 173.75 194.22 0.23 0.01 0.30 0.03
M4-80 0.02 22.58 179.60 208.82 0.24 0.01 0.32 0.02
M5-20 0.52 29.72 199.33 309.85 0.27 0.01 0.94 0.02
M5-60 0.39 26.19 372.5 457.38 0.49 0.03 0.94 0.04
M5-80 0.28 25.54 258.57 330.22 0.34 0.01 0.64 0.01
M6-20 0.03 21.19 185.45 210.58 0.25 0.03 0.30 0.03
M6-60 0.03 20.18 209.39 231.98 0.28 0.02 0.31 0.01
M6-80 0.02 20.07 189.81 199.06 0.25 0.05 0.25 0.01

Note: Each group of data obtained from the average of three specimens.

Initial crack fracture toughness Table 6

1.0 Unstable fracture toughness Multiple linear regression analysis for kinking angle responses.

Independent Regression P-value t-value Standard

variable coefficient error
Fracture toughness(MPa*m )
1/2

0.8
Constant 3.480 0.620 0.512 6.800
x1 16.660 0.060 2.122 7.863
x2 8.107 0.326 1.032 7.863
0.6 x3 3.877 0.632 0.494 7.863
x4 7.597 0.356 0.967 7.863
x5 12.603 0.140 1.605 7.863

0.4
where E is the modulus of elasticity, a is the crack length, P is the
load corresponding to crack length a.
0.2 In the linear stage of P-CMOD curve, three elastic modulus val-
ues are obtained by substituting three points into Eq. (8). The aver-
age elastic modulus is defined as the elastic modulus (E) of the
0.0
specimen.
20 60 80 20 60 80 20 60 80 20 60 80 20 60 80 20 60 80
According to the linear progressive superposition hypothesis,
M1 M2 M3 M4 M5 M6 the P-CMOD curve is considered as a series of outsourcing lines
consisting of elastic points of specimens with the same material,
Fig. 12. Fracture toughness from P-CMOD curve.
the same size and different pre-cracking lengths. Thus, the linear

M1-20 M1-60 M1-80 M3-60 M5-60

Fig. 13. Crack trajectory envelope for different UHTGC specimens under applied loading.
 X. Wan et al. / Construction and Building Materials 251 (2020) 118851 15

0.6 0.3
M1-20 M2-20
M1-60 M2-60
0.5 M1-80 M2-80

0.4 0.2

Load (kN)
Load (kN)

0.3

0.1
0.2

0.1

0.0
0.0 0.0 0.2 0.4 0.6 0.8 1.0 1.2
0 1 2 3 4
Deflection (mm)
Deflection (mm)
(a) M2
(a) M1 0.3

0.6 M4-20
M4-60
M3-20
M4-80
0.5
M3-60
M3-80
0.2
0.4
Load (kN)
Load (kN)

0.3

0.1
0.2

0.1

0.0
0.0 0.0 0.2 0.4 0.6 0.8 1.0 1.2
0 1 2 3 4
Deflection (mm)
Deflection (mm)
(b) M3 (b) M4
0.3
0.6
M6-20
M5-20
M6-60
M5-60
0.5 M6-80
M5-80

0.2
0.4
Load (kN)
Load (kN)

0.3

0.1
0.2

0.1

0.0
0.0 0.0 0.2 0.4 0.6 0.8 1.0 1.2
0 1 2 3 4
Deflection (mm)
Deflection (mm)
(c) M6
(c) M5
Fig. 15. Load-deflection curves of mix proportions without fiber under three-point
Fig. 14. Load-deflection curves of 2% fiber content mix proportions under three- bending load.
point bending load.
16 X. Wan et al. / Construction and Building Materials 251 (2020) 118851

Table 7
Fracture energy parameter.

Mix W0 (Nm) W2 (Nm) W3 (Nm) W (Nm) GF(f) (Nmm2) Standard deviations of GF(f) (Nmm2) GF(f)/ GF
M1-20 0.73 0.011 0.75 1.491 1863.7 26.4 37.27
M1-60 0.83 0.007 0.91 1.747 2183.7 108.6 58.23
M1-80 0.91 0.007 0.62 1.537 1921.2 34.5 76.85
M2-20 0.04 – – 0.040 50.0 3.3 –
M2-60 0.03 – – 0.030 37.5 2.2 –
M2-80 0.02 – – 0.020 25.0 2.2 –
M3-20 0.34 0.007 0.31 0.657 821.2 29.4 21.90
M3-60 0.67 0.008 0.39 1.068 1335.0 31.0 53.40
M3-80 0.66 0.004 0.29 0.954 1192.5 96.4 47.70
M4-20 0.03 – – 0.030 37.5 2.0 –
M4-60 0.02 – – 0.020 25.0 1.6 –
M4-80 0.02 – – 0.020 25.0 1.0 –
M5-20 0.46 0.005 0.23 0.695 868.7 41.4 17.37
M5-60 0.59 0.005 0.21 0.805 1006.2 53.4 26.83
M5-80 0.58 0.004 0.15 0.734 917.5 13.5 73.40
M6-20 0.04 – – 0.040 50.0 3.2
M6-60 0.03 – – 0.030 37.5 1.8
M6-80 0.01 – – 0.010 12.5 1.0

Note: Each group of data obtained from the average of three specimens. GF(f)/ GF is the ratio of the fracture energy of the specimens with and without fibers.

2400
elastic method can be used to describe the complete fracture pro-
cess considering the non-linear characteristics. Under this assump-
tion, the critical equivalent crack length (ac ) can be calculated as
2000 Eq. (8). The instability fracture toughness can be obtained by
replacing the initial crack opening load (Pini) and the initial crack
Fracture energy (Nm*m )
-2

length (a0 ) in Eq. (6) with the maximum load ðP max ) and the critical
1600
equivalent crack length ðac Þ. The calculation results of fracture
toughness are shown in Table 5 and Fig. 12. The data in the table
1200 are obtained from the P-CMOD curve, and then the three groups
of data are averaged.
According to Table 5 and Fig. 12, the initial fracture toughness
800 and unstable fracture toughness of the specimens with PVA fiber
are higher than those without fiber, while the initial fracture
400
toughness and unstable fracture toughness of M1 specimens are
slightly lower than those of other mix proportions with fiber
(M3, M5). However, from the stress–strain curves under the tensile
0 load, M1 group shows the largest strain, and behaves obvious hard-
M1-20 M1-60 M1-80 M3-20 M3-60 M3-80 M5-20 M5-60 M5-80
ening effect. It is due to the initial crack toughness which is a char-
(a) With fiber acterization of the ability of concrete to resist cracks under load. It
2400 is closely related to the strength of matrix materials. Generally, the
60
data in Table 5 show that the critical crack length of specimens
50 with fiber is higher than that of the specimens without fiber, which
2000
40
indicates that the cracks of UHTGC undergo a longer period of
Fracture energy (N*m)

stable propagation before they begin to expand unstably.

1600 30 Fig. 13 presents the crack trajectory envelopes for different
20
specimens under Mode I applied loading. Through Photoshop, the
1200
gray level of the image is processed and the contrast of the image
10
is adjusted. According to the model established by Rooholamini
0
et al. [29], the kinking angle was analyzed by multiple regression
800 M2-20 M2-60 M2-80 M4-20 M4-60 M4-80 M6-20 M6-60 M6-80
analysis, and the effect of different factors on the kinking angle is
obtained. The model is defined as follows: [29]
400
X
5
h ¼ b0 þ bi xn ð10Þ
j¼1
0
M2-20 M2-60 M2-80 M4-20 M4-60 M4-80 M6-20 M6-60 M6-80
where is h the kink angle, b0,. . .. . ., b5 are the partial regression coef-
(b) Without fiber
ficients and xn are the independent input variables to the model as
Fig. 16. Calculated fracture energy of different mix proportions. follows:
 X. Wan et al. / Construction and Building Materials 251 (2020) 118851 17

Table 8
Fracture energy results of other researchers.

Author Fiber type Fiber dosage Specimens name Water/binder ratio Notch length/height Fracture energy
(activator/binder ratio) (Nmm2)
Siaw Foon Lee [34] Steel fiber 0.3%, volume FRC 0.3 0 214
Steel fiber 1%, volume FRC 0.3 0 269
Pavel Rovnanik [35] Carbon nanotube 0%, mass Nanotube reinforced AAS 0.4 0.3 35
Carbon nanotube 1%, mass Nanotube reinforced AAS 0.4 0.3 45
Shuling Gao [36] PVA fiber 2%, volume SHCC-F-2 0.45 0.5 1229
PVA fiber 2%, volume SHCC-FA-2 0.45 0.5 2155
Jifei Dai [37] Polypropylene fiber 2%, volume FRC-A11 0.46 0.5 608

20
500 M1-20
M1-60 Macroscopic experimental results
M1-80 Test results of nanoindentation
400
M3-60
M5-60 15

Elastic modulus (GPa)

Load (mN)

300

10
200

100 5

0
0 2000 4000 6000 8000 10000 12000 14000
0
Depth (nm) M1-20 M1-60 M1-80 M3-60 M5-60

Fig. 17. The load-depth curves of different mix proportions. Fig. 18. Elastic modulus of different mix proportions.

1 ifspecimenisM1  20 1 ifspecimenisM1  60
x1 ¼ x2 ¼ 400
0 otherwise 0 otherwise
Macroscopic expermental results (Without fibers)
Test results of nanoindentation

300
1 ifspecimenisM1  80 1 ifspecimenisM3  60
Fracture energy (Nm*m )

x3 ¼ x4 ¼
-2

0 otherwise 0 otherwise

200

1 ifspecimenisM5  60
x5 ¼
0 otherwise
100
The analysis results are listed in Table 6. As demonstrated in the
table, the curing temperature and FA/S ratio do not have significant
effects on the amount of h in a 95% confidence interval, and P-
values for the defined independent variables are more than 0.05,
0
which means that both curing temperature and FA/S ratio do not M2-20 M2-60 M2-80 M4-60 M6-60
have essential effects on the occurrence of the probable kinked
crack during its stable growth. Fig. 19. Fracture energy of different mix proportions from nanoindentation test .

Table 9
The parameter of micro fracture properties from nanoindentation test.

Mixture ID Elastic Standard deviations Fracture energy Standard deviations Fracture toughness Standard deviations of
modulus (GPa) of elastic modulus (Nmm2) of fracture energy 10-3(MPam2) fracture toughness
M1-20 8.1 0.26 215.3 12.87 41.7 1.73
M1-60 8.5 0.17 206.7 10.58 41.9 3.94
M1-80 11.8 1.31 186.4 10.04 47.6 4.38
M3-60 11.6 0.62 220.3 11.22 51.4 4.40
M5-60 11.7 1.14 282.5 10.25 58.2 2.92

Note: Each group of data obtained from the average of three specimens.
18 X. Wan et al. / Construction and Building Materials 251 (2020) 118851
M1-20
M3-60
Fig. 20. SEM micrographs at low magnification (37).
3.5. Fracture characteristics and parameters
Fracture energy GF is a fracture parameter based on virtual crack
model and considering the softening characteristics of concrete.
According to RILEM [30], the fracture energy can be calculated by
the load–deflection curve. The formula for calculating fracture
energy GF is as follows:
W W
GF ¼ ¼ ð11Þ
A tðh  a0 Þ
where W is the work done by the external force when the notched
beam fracture under three-point bending load. A is the cross-
sectional area, t is the thickness of beam, h is the height of the spec-
imen, a0 is the initial crack length. Considering the influence of self-
weight and support the work done by the external force, W is
divided into four parts: W0, W1, W2 and W3 as follows:
W ¼ W0 þ W1 þ W2 þ W3
W 2 ¼ DPA  d0 ¼ ð1=2ÞmgA  d0
where W 0 is the work done by the load, the value is the area under
the measured load–deflection curve. W 1 , W 2 and W 3 are the addi-
tional work taking into account the weight of the specimen, of
which W 1 is only about 0.16%-0.19% of W, negligible [31]. d0 is
the displacement corresponding to one third of the maximum load.
The value of W 3 depends on the area under the tail curve. The
power function is used to fit the tail curve first, and then the fitting
curve is used to calculate the integral. This method can effectively
eliminate the size effect [32,33]. The calculation formula is as
follows:
Z þ1
a
W3 ¼ adk dd ¼
d ðk  1Þdk1
0 that of SHCC studied by Gao [36]. Although the increase of slag
M1-60 M1-80
M5-60
P ¼ adk ð15Þ
where a and k are fitting coefficients.
Deflection-load curve of notched beam under three-point bend-
ing load as shown in Figs. 14 and 15. It can be observed that, the
flexural load of the specimens with fiber ranges from 0.15 kN to
0.6 kN, and the deflection is greater than 2 mm, which is signifi-
cantly different from brittle specimens without fibers. The deflec-
tion of the specimens without fiber is less than 0.5 mm (the
deflection corresponding to the reverse bending point). The flexu-
ral load of specimens without fiber is stable at about 0.1 kN to
0.25 kN.
The fracture energy parameters obtained from the load–deflec-
tion curve of notched beams under three-point bending load are
shown in Table 7. The result is the average of three sets of data.
The self-weight work of the specimens without fiber is too small,
so it is neglected. Fig. 16 is obtained from the data in Table 7. It
ð12Þ
can be found that the fracture energy of the specimens with fiber
is 17–77 times that of the specimens without fiber. For the fracture
ð13Þ
energy of non-fiber specimens, the increase of curing temperature
and slag content will lead to decrease of fracture energy. But for
specimens with 2% PVA fiber, the fracture energy increases with
the curing temperature enhanced from 20 °C to 60 °C, while
decreases with the curing temperature enhanced from 60 °C to
80 °C. With the increase of slag content, the fracture energy
decreases, which is consistent with the results of the specimens
without fiber. Higher curing temperature and slag content brings
higher bending strength, but also reduces ductility.
Table 8 presents the results of other researchers on the fracture
energy of similar materials. It is found that the effect of PVA fiber
on fracture energy is much higher than that of steel fiber and car-
ð14Þ bon nanofiber [34,35]. The fracture energy of M1 group is similar to
 X. Wan et al. / Construction and Building Materials 251 (2020) 118851 19

fiber
tiny cracks

fiber surface

micro-sphere

M1-20

scratched

peeled

M1-60

M1-80
Fig. 21. SEM micrographs of fiber and matrix interface and fiber surface of different specimens.

dosage in this paper leads to a significant decrease of fracture
energy, it is still similar to the result of polypropylene fiber rein-
forced geopolymer of Dai et al. [37].
3.6. Results of nanoindentation
According to the energy method [38–40], the parameters of the
specimen are calculated. Energy release rate at critical state Gc and
fracture toughness K IC are calculated by Eqs. (16) and (17).
Wc
Gc ¼
Afra
rffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi
E
K IC ¼ Gc ð17Þ
1  v2
where W c is fracture energy, Afra is maximum contact area, v is the
Poisson’s ratio of the tested material.
The load-depth curves obtained from nanoindentation are
shown in Fig. 17. The calculated elastic modulus, fracture energy
and fracture toughness are shown in Table 9. Furthermore, the
results of nanoindentation test are compared with those of
macro-indentation test, as shown in Figs. 18 and 19. It can be seen
ð16Þ that the nanoindentation results are in good agreement with the
macro-test results. With increase of curing temperature, the mod-
20 X. Wan et al. / Construction and Building Materials 251 (2020) 118851
M3-60
peeled
M5-60
Fig. 21 (continued)
ulus of elasticity increases while the fracture energy decreases
slightly. The fracture energy obtained by three-point bending of
notched beams is weaker than that obtained by nanoindentation
test. It is mainly due to the anticipated size of cracks in the test
of three-point bending notched beams, the damage in demoulding
and the errors in the test process, which will greatly reduce the
fracture energy obtained.
3.7. Microstructural analysis
The morphological images based on FESEM of specimens are
presented in Figs. 20 and 21. With low magnification, in M5-60,
the fibers is observed to be shorter, and there is obvious broke
down at the end of the fiber. In other images, the fiber is longer,
and the fiber surface looks smoother, which also shows that the
blend of fly ash improves the bonding performance between fiber
and matrix.
From Fig. 21, it can be observed that slag improves compactness
of the micro structure. However, there is more obvious gap at the
fiber/matrix interface in specimens with high content of slag. For
high content fly ash, the layer of hydration products attached to
the fiber surface in M1-20, M1-60 and M1-80 samples is loose.
There are many tiny cracks on the layer in M1-20 samples, which
shows that the bond strength between the products is lower. In
contrast, this layer on the fiber surface of M3-60 and M5-60 sam-
ple is denser. The surface of each sample is scraped to different
degrees, of which M5-60 has the most serious scrape of fiber,
which leads to the decrease of fiber diameter. The end of the fiber
becomes thinner, which will cause stress concentration and make
the fiber easier to break.
EDS of specimens is shown in Fig. 22 and Table 10. The com-
ponent of carbon element comes from fiber. Presence of Si and
Al indicate participation of aluminosilicate gel from fly ash and
slag. The Al/Si ratio the Ca/Si ratio and the Na/Si ratio are listed
in Table 10. As the content of slag increased from 20% to 100% in
the matrix, the main product is N-C-A-S-H rather than N-A-S-H.
The results are consistent with those of Lee et al. [41]. In addi-
tion, with the increase of slag content, the Ca/Si ratio in the
hydrated products increased, while Na/Si ratio decreased slightly
with the increase of Ca/Si ratio. For Al/Si ratio, the higher the
content of slag, the lower the Al/Si ratio is. Compared with
M1-60 and M1-80, it can be found that Ca/Si ratio and Al/Si ratio
increase with curing temperature, while Na/Si ratio is the
opposite.
 X. Wan et al. / Construction and Building Materials 251 (2020) 118851 21

tensile, four-point bending and three-point bending tests of

notched beams. The micro-mechanical properties and micro-
morphologic properties of FRGC were supplemented by nanoin-
dentation tests and FESEM-EDS. The following conclusions are
drawn.
When the slag content is 20%, the curing temperature  60 °C,
the average strain of the composite under uniaxial tension load is
more than 3%. The pseudo-strain hardening effect occurs, accom-
panied by multiple cracking. Increasing the content of slag is not
conducive to the increase of strain. The ductility first increases
and then decreases with the increase of curing temperature
generally.
For both initial fracture toughness and unstable fracture tough-
M1-60 ness, UHTGC is higher than the specimens without fiber. Before
unstable cracking, UHTGC undergo a stable significant deflection
during which the crack length expands continuously.
The fracture energy of UHTGC is 17–77 times of that of mixes
without fiber. The fracture energy of UHTGC increases first and
then decreases with the increase of curing temperature. For speci-
mens without fiber, the fracture energy decreases with curing
temperature.
The results of nanoindentation test verified that the modulus of
elasticity increases with curing temperature, while the fracture
energy decreases slightly with curing temperature, which are sim-
ilar to those of macro-scale mechanical test results.

CRediT authorship contribution statement

M1-80
Xiaomei Wan: Conceptualization, Methodology, Writing -
review & editing. Chen Shen: Data curation, Formal analysis, Writ-
ing - original draft. Penggang Wang: Investigation. Tiejun Zhao:
Supervision. Yu Lu: Investigation.

Declaration of Competing Interest

The authors declare that they have no known competing finan-

cial interests or personal relationships that could have appeared
to influence the work reported in this paper.

Acknowledgments
M5-60
The authors of this contribution gratefully acknowledge sup-
Fig. 22. EDS spectrums of fiber surface. port of the ongoing project of National Natural Science Foundation
of China (51878365, 51608286) and the Natural Science Founda-
tion of Shandong Province (ZR2017MEE040). Professor Zhijun
Table 10
Composition measured by EDS on the surface of the pulled-out fiber. DONG from Shenzhen Institute of Information Technology pro-
vided great help in nanoindentation test.
Element Weight %
M1-60 M1-80 M5-60
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O 37.93 56.42 42.79
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