Ceramics International: Peng Zhang, Kexun Wang, Juan Wang, Jinjun Guo, Shaowei Hu, Yifeng Ling

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Ceramics International xxx (xxxx) xxx–xxx

Contents lists available at ScienceDirect

Ceramics International
journal homepage: www.elsevier.com/locate/ceramint

Mechanical properties and prediction of fracture parameters of geopolymer/


alkali-activated mortar modified with PVA fiber and nano-SiO2
Peng Zhanga, Kexun Wanga,∗, Juan Wanga,∗∗, Jinjun Guoa, Shaowei Hua,b, Yifeng Lingc
a
School of Water Conservancy Engineering, Zhengzhou University, Zhengzhou, 450001, China
b
College of Civil Engineering, Chongqing University, Chongqing, 400045, China
c
Department of Civil, Construction and Environmental Engineering, Iowa State University, Ames, IA, 50011, United States

A R T I C LE I N FO A B S T R A C T

Keywords: Properties of fly ash (FA) and metakaolin (MK) based geopolymer/alkali-activated mortar modified with poly-
Geopolymer/alkali-activated mortar vinyl alcohol (PVA) fiber and nano-SiO2, including workability, compressive strength, flexural performance,
Mechanical properties elastic modulus and fracture property were tested in this study. PVA fiber content varies from 0 to 1.2%. Nano-
Fracture parameters SiO2 content is 0 and 1%. Adaptive neuro-fuzzy interfacial systems (ANFIS) method was used to establish the
ANFIS
artificial intelligence (AI) model to predict the fracture parameters of geopolymer/alkali-activated mortars. The
inputs of ANFIS models include PVA fiber content, nano-SiO2 content, compressive strength, flexural strength,
elastic modulus, critical crack mouth opening displacement, crack load and peak load. The outputs of ANFIS
model include critical effective crack length, initiation fracture toughness, unstable fracture toughness, and
fracture energy. Experiment results showed that PVA fiber addition enhanced the mechanical properties espe-
cially the compressive strength and fracture performance, but decreased the workability. 0.8%–1.0% was con-
sidered as the optimal content of PVA fiber. Addition of 1% nano-SiO2 shows a slight improvement on both
workability and mechanical properties of the mortar no matter how much fiber is added. Based on the ANFIS
algorithm and 42 sets of experimental data, the trained models were proved to have high accuracy with root
mean square error (RMSE) under 0.15, mean absolute error (MAE) under 0.01, and coefficient of determination
(R2) over 0.85. The ANFIS model established in this study combined the fracture properties with the basic
mechanical properties of geopolymer/alkali-activated composites, which can provide a new method to assess the
fracture performance of geopolymer/alkali-activated mortars modified with PVA fiber and nano-SiO2 in the
future.

1. Introduction combination of the two is more capable of preparing geopolymer


mortar with high compressive strength [3,4]. FA or MA based geopo-
Due to the high early strength, excellent durability and low carbon lymer mortars activated by alkaline solution in which NaOH accounts
emission in the production process, geopolymers/alkali-activated bin- for 0.4–0.5 of activator have higher compressive strength [5,6]. Studies
ders and the composites have attracted increasing attention of scholars also showed that elastic modulus of geopolymer composites is generally
in the world. At present, researches on mechanical properties of geo- lower but the tensile strength and flexural strength is usually higher
polymer composites have been done from various perspectives. than that of the cement composites at the same compressive strength
Compressive strength of geopolymer composites was found to be closely level [7–10]. Furthermore, geopolymer composites were found to be
related to the type of source material and the composition of alkaline more brittle than cement composites [8,11]. Therefore, a growing
activator in addition to water-binder ratio and the aggregate content. number of studies on modified geopolymer composites have been done
FA is one of the industrial wastes and is considered as a raw material for in order to improve the mechanical properties of geopolymer compo-
green concrete preparation [1], and adding FA to cement composites sites, such as compressive strength, elastic modulus, especially the
can improve the fracture toughness of matrix [2]. Relevant studies flexural strength and fracture toughness, so as to meet the needs of
show that compared with other raw materials, FA or MK or a engineering practice. Adding fiber is the most effective way to improve


Corresponding author.
∗∗
Corresponding author.
E-mail addresses: zhangpeng@zzu.edu.cn (P. Zhang), wkx301@zzu.edu.cn (K. Wang), wangjuan@zzu.edu.cn (J. Wang), guojinjun@zzu.edu.cn (J. Guo),
hushaowei@cqu.edu.cn (S. Hu), yling@iastate.edu (Y. Ling).

https://doi.org/10.1016/j.ceramint.2020.05.074
Received 18 February 2020; Received in revised form 5 May 2020; Accepted 6 May 2020
0272-8842/ © 2020 Elsevier Ltd and Techna Group S.r.l. All rights reserved.

Please cite this article as: Peng Zhang, et al., Ceramics International, https://doi.org/10.1016/j.ceramint.2020.05.074
P. Zhang, et al. Ceramics International xxx (xxxx) xxx–xxx

the ductility and toughness of geopolymer composite, thus limiting the 2.2. Preparation of geopolymer mortars and specimens
propagation of cracks. Commonly used fibers in cement or geopolymer
composites are steel fibers [12], polypropylene (PP) fibers, carbon fiber, 2.2.1. Mix proportions
and glass fibers [13]. PVA fiber has high elastic modulus, tensile The water-binder ratio is set at 0.65, in which the water includes the
strength, acid resistance and alkali resistance, and is considered as a sum of water in alkaline activator and additional water. Binder-sand
suitable additive for geopolymer composites [13]. However, only a few ratio was set at 1.0. In the binder MK accounts for 70% of the total mass
fiber contents were set in most researches on PVA fiber modified geo- and FA accounted for 30%. Alkaline activator was made by mixing
polymer composites [14–17], which could not well indicate the trend of Na2SiO3 with NaOH and water. In the existing studies, the PVA fiber
properties with PVA fiber content. On the other hand, nano-particles volume fraction varied from 0.5% to 2, but the fraction gradient of fiber
modifying cement composites was becoming the potential improvement was usually small, which could not reflect the trend well [13]. In ac-
on mechanical properties [12,18]. The commonly used nano-additives cordance to Refs. [37,38], PVA fiber volume fraction was set at 0, 0.2%,
are nano-SiO2, nano-Al2O3, and nano-Fe2O3 [19,20]. The incorporation 0.4%, 0.6%, 0.8%, 1.0% and 1.2% of the mortar. In order to study
of nanomaterials is beneficial to enhance the mechanical properties and whether the addition of nano-SiO2 will affect the mechanical properties
durability of geopolymer composites. In particular, it has been shown of PVA fiber reinforced geopolymer mortar, nano-SiO2 mass fraction
that the introduction of nano-SiO2 to MK based geopolymer sample was set at 0 and 1.0% of the total amount of MK and FA. Mix propor-
results in higher strength, higher density and lower porosity than other tions are clearly showed in Table 4.
samples [21]. Based on the existing researches, this study focuses on the
mechanical properties of FA and MK based geopolymer mortar mixed 2.2.2. Preparation of geopolymer mortar
with variable fiber contents, as well as the effect of nano-SiO2 on PVA The dispersion uniformity of PVA fiber and nano-SiO2 in matrix was
fiber reinforced geopolymer mortar. the key point to prepare the mortar. As PVA fiber used in this in-
The author also noted that AI approaches had been increasingly vestigation exhibits good dispersibility, it can be added to the mixer
applied to solve complex engineering problems recently. AI based al- several times separately and stirred with longer mixing time. However,
gorithms have also been used to predict the performance of building when adding nano-SiO2, its activity and the influence on alkali con-
materials such as concrete and mortar [22–24]. However, through in- centration should be considered. Hence, nano-SiO2 was accessed to be
vestigation, a lot of studies worked on compressive strength prediction added to the mixture of water and superplasticizer, and after that ex-
of geopolymer composites using Artificial neural networks (ANN) isting solution was mixed with the binder. In general, the preparation of
[25–27], back-propagation neural network (BPNN) [28] and adaptive mortar followed the process shown in Fig. 1. The PVA fibers were added
neuro-fuzzy interfacial systems (ANFIS) methods [29–31], but few to the mixer in 2 batches separately and stirred well. Nano-SiO2 par-
studies involved in the fracture property analysis and prediction of ticles were dry mixed with geopolymer precursor for 2 min to ensure a
geopolymer or cement composites [32–34]. Besides, according to pre- uniform dispersion in matrix. The specimens used in the subsequent
vious studies, ANFIS shows better convergence, stability among several tests were demolded after 24 h and then placed in standard curing
methods [35,36]. In the researches on compressive strength prediction, condition according to GB/T50081-2019 [39], i.e. temperature of
a few input factors (3 or 4 in general) were considered in most re- 20 ± 3 °C and humidity above 95% for 28 days.
searches, which cannot fully reflect the reality. Therefore, based on
experimental data, ANFIS models with 8 input parameters were utilized 2.2.3. Specimens
to predict the fracture property in this article. In a comprehensive way, Three cube specimens with dimensions of
the input factors reflect the influence of the additive and the basic 70.7 mm × 70.7 mm × 70.7 mm for each group were used to study the
mechanical properties of geopolymer mortar on the fracture para- cubic compressive strength of geopolymer mortars. Moreover, 9 prisms
meters. This may be the first time to link the fracture property of with dimensions of 40 mm × 40 mm × 160 mm were prepared, 3 of
geopolymer composites to the basic mechanical properties by AI, and which were used for measuring the axial compressive strength, 3 for
will provide a new method for evaluating the fracture performance of elastic modulus measurement, and the other 3 for measuring the flex-
geopolymer composites in the future. ural strength as well as the compressive strength after bending. In ad-
dition, 5 beams in size of 100 mm × 100 mm × 400 mm with a precast
2. Experimental programs crack for each group were prepared for fracture performance test. The
depth of the precast crack is 40 mm.
2.1. Materials
2.3. Test methods
MK and first grade FA was used as the precursor of geopolymer.
Chemical composition of MK and FA were tabulated in Table 1. Physical 2.3.1. Slump flow
properties of FA and nano-SiO2 are shown in Table 2. PVA fiber was Due to the high fluidity of fresh geopolymer mortar, slump flow test
supplied by Kuraray Co. Ltd. Nano-SiO2 powder with 99.7% purity and was conducted to evaluate the workability of geopolymer mortars in
30 nm nominal diameter is used in this investigation. Properties of PVA order to investigate the effect of PVA fiber content and nano-SiO2 ad-
fiber are presented in Table 3. In addition, the efficient superplasticizer dition on the workability according to GB/T 50,080-2016 [40]. The
with 21% water reducing rate is used in this experiment. The fine ag- reported slump flow value was the average of the maximum and
gregate used in this study was extra-fine quartz sand with particle size minimum diameters after the mortar had collapsed.
of 75–120 μm. Alkaline solution was a mixture of sodium hydroxide
(NaOH) and sodium silicate (NaSiO3) to achieve a sodium oxide weight 2.3.2. Compressive strength test
ratio of 15%. The cubic compressive strength was obtained by compression tests
conducted in accordance to JGJ/T70-2009 [41]. Specimens were tested
Table 1 in an electro-hydraulic servo universal testing machine (600 kN).
Chemical constituents of MK and FA. Loading at a constant speed of 1.5 kN/s until the specimen failed, and
Chemical constituents (%) SiO2 Al2O3 Fe2O3 CaO + MgO K2O + Na2O
the failure load (Nu ) was recorded. Cubic compressive strength ( fcu ) was
calculated according to Eq. (1).
MK 54 43 ≤1.3 ≤0.8 ≤0.7
FA 52 18 6.5 12.4 4.3
Nu
fcu =
A (1)

2
P. Zhang, et al. Ceramics International xxx (xxxx) xxx–xxx

Table 2
Physical properties of FA and nano-SiO2.
FA Bulk density (g/cm3) Standard consistency (%) Water absorbing capacity (%) Specific gravity (g/cm3)
0.77 47.1 105 2.16
Nano-SiO2 Bulk density (g/cm3) Loss on ignition (%) Specific surface area (m2/g) pH
0.054 1.0 200 6

Table 3
Physical and mechanical properties of PVA fiber.
Wire diameter Nominal length Nominal tensile Elongation at break
(μm) (mm) strength (MPa) (%)

40 12 1560 6.5

where A is the area of bearing surface, which can be calculated as


70.7 mm × 70.7 mm.
The residual compressive strength after flexural test (R c ) and axial
compressive strength ( fcp ) were tested according to GB/T 7897-2008
[42]. Specimens were uniformly loaded at the speed of 2.4 kN/s to test
R c and 1 kN/s to test fcp by a 600 kN electro-hydraulic servo universal
testing machine. R c and fcp were calculated by Eq. (2) and Eq. (3), re-
spectively.
Fc
Rc =
A (2)

F
fcp =
A (3)

where Fc and F represent the failure loads in the two tests; A represents
the area of bearing surface, which can be calculated as
40 mm × 40 mm.

2.3.3. Flexural strength


The flexural strength (Rf ) was tested by a motorized bending tester Fig. 1. Preparation process of geopolymer mortar.
under the guidance of GB/T 7897-2008 [42]. Three-point bending test
were conducted under constantly loading at 50 N/s until the specimens testing machine. The loading pattern is shown in Fig. 2. In phase one,
broke. Rf was calculated by Eq. (4). The final result was the average of specimens were preloaded and unloaded repeatedly at 1 kN/s. The
three duplicates of each mix. fourth load started in phase two with the same speed; moreover, the
1.5Ff L initial load in phase two was set at 0.8 kN and it was holding for 30 s
Rf = = 0.234 × 10−2Ff after loading or unloading; strain was measured at the load holding
b3 (4)
stage until the difference between the two consecutive data was less
where Ff is the fracture load; L is the span of two supports (100 mm); b than 20 με. The strain gauges were pasted on center of the four flanks of
is the width of prism (4 mm). the prism, and were connected to a mortar elastic modulus measuring
instrument with a standard distance of 80 mm for strain collection. The
2.3.4. Elastic modulus elastic modulus (Em ) is calculated by Eq. (5). The average of three trial
Elastic modulus measured by GB/T 7897-2008 [42] refers to the results was reported as the final value.
secant modulus of loading at 40% of axial compressive strength. Spe-
cimens were tested by a 600 kN electro-hydraulic servo universal

Table 4
Mix proportions of geopolymer mortars.
MK (kg/m3) FA (kg/m3) Water (kg/m3) Na2SiO3 (kg/m3) NaOH (kg/m3) Quartz sand (kg/m3) PVA fiber (%) Nano-SiO2 (%) Superplasticizer (kg/m3)

429.5 184.1 106.2 445.4 71 613.6 0 0 3.07


429.5 184.1 106.2 445.4 71 613.6 0.2 0 3.07
429.5 184.1 106.2 445.4 71 613.6 0.4 0 3.07
429.5 184.1 106.2 445.4 71 613.6 0.6 0 3.07
429.5 184.1 106.2 445.4 71 613.6 0.8 0 3.07
429.5 184.1 106.2 445.4 71 613.6 1.0 0 3.07
429.5 184.1 106.2 445.4 71 613.6 1.2 0 3.07
425 182.2 106.2 445.4 71 613.6 0 1.0 3.07
425 182.2 106.2 445.4 71 613.6 0.2 1.0 3.07
425 182.2 106.2 445.4 71 613.6 0.4 1.0 3.07
425 182.2 106.2 445.4 71 613.6 0.6 1.0 3.07
425 182.2 106.2 445.4 71 613.6 0.8 1.0 3.07
425 182.2 106.2 445.4 71 613.6 1.0 1.0 3.07
425 182.2 106.2 445.4 71 613.6 1.2 1.0 3.07

3
P. Zhang, et al. Ceramics International xxx (xxxx) xxx–xxx

Fig. 2. Loading pattern of elastic modulus test.

Pa − P0 1.99 − α (1 − α )(2.15 − 3.93α + 2.7α 2) a


Em = f (α ) = ,α= 0
A (εa − ε0) (5) (1 + 2α )(1 − α )3/2 h (7)

where Pa represents the target load, which is 40% of the axial com- The load increased linearly and non-linearly in the P-CMOD curve.
pressive strength; P0 is the initial load; εa and ε0 are the corresponding The CMOD corresponding to Pmax is exactly the critical effective crack
strain, respectively. length (ac ), which can be expressed by Eq. (8), m.

2 bEVc
ac = (h + h 0)arctan − 0.1135 − h 0
2.3.5. Fracture properties π 32.6Pmax (8)
Three-point bending tests [43] were conducted by the same electro-
hydraulic servo universal testing machine which was used in the where h 0 is fixture thickness of the clamped extensometer (0.001 m); Vc
compressive strength test and elastic modulus test. An initial notch (μm) is the critical CMOD; Pmax (kN) is peak load; E (GPa) is the cal-
3 mm wide 40 mm long was precast in the middle of the beam bottom. culated elastic modulus, which can be calculated by Eq. (9).
Beam dimensions and the initial notch location are shown in Fig. 3.
1 ⎡ π a0 + h0 ⎞ ⎤
Loading rate was set at 0.05 mm/min, and the load on the specimen E= 3.7 + 32.6 tan2 ⎛ ⎜ ⎟

was obtained by a load transducer with a maximum range of 30 kN and bci ⎢


⎣ ⎝ 2 h + h0 ⎠ ⎥⎦ (9)
a precision of 1 N. The crack mouth opening displacement (CMOD) was
where ci (μm/kN) is the slope of the linear interval in the P-CMOD
tested by clamped extensometers. All data were collected by a static
curve.
strain test analysis system to obtain the fracture parameters. The frac-
In the last stage of fracture propagation, the cracks rapidly ex-
ture toughness should be the average of measured values of five spe-
panded and finally failed. In this case, unstable fracture toughness (KIcun )
cimens with the same proportion (measured values that differ from the
can be obtained by substituting critical effective crack length (ac ) and
average value by more than 15% should be omitted).
Fracture parameters including, initial fracture toughness (KIcini ), peak load (Pmax ), as Eq. 10 and 11 show.
critical effective crack length (ac ), unstable fracture toughness (KIcun ),
and fracture energy (G F ) were calculated on the basis of double-K KIcun =
(
1.5 Pmax +
m1 g
2 )
× 10−2 × 10−3S ac
f (α )
fracture model. The above parameters can be calculated by Eqs. 6–12 bh2 (10)
[44].
1.99 − α (1 − α )(2.15 − 3.93α + 2.7α 2) a
f (α ) = ,α= c
KIcini =
(
1.5 Pini +
m1 g
2
× )×
10−2 10−3S a0
f (α )
(1 + 2α )(1 − α )3/2 h (11)
bh2 (6)
According to double-K fracture theory, the fracture state can be
where KIcini (MPa∙m1/2) is initiation toughness; Pini (kN) represents the judged by comparing the strength factor of stress field at crack tip (K )
and the initiation fracture toughness (KIcini ) and the unstable fracture
cracking load, which is the load when P-CMOD curve turning linear to
toughness (KIcun ). When K < KIcini , cracks will not propagate; when
non-linear; m1 is the mass of the beam between two supports (5.5 kg); g
KIcini ≤ K < KIcun , cracks propagate stably; when K > KIcun , cracks propa-
is acceleration due to gravity (9.8 m/s2); S is the span between two
gate unstably. In practical engineering application, K = KIcini can serve
supports (0.3 m); a 0 is the initial notch length (0.04 m); b is the width of
as the criterion for crack propagation in principal structures;
beam (0.1 m); h is the height of beam (0.1 m); f (α ) is determined by
KIcini ≤ K < KIcun can serve as the warning signs to instability in principal
Eq. (7).
structures; K = KIcun can serve as the criterion for crack propagation in
ordinary structures.
According to the existing research results [45–47], fracture energy
was determined by Eq. (12) based on P-CMOD curve in this study.
1 Vc Vc
W0 + 8 mgS × ac
W0 + 0.0375mg × ac
GF = =
A b × (h − a0) (12)

where W0 (N∙m) is the area between P-CMOD curve and the X-axis; m
(kg) is sum of m1 (mass of the beam between two supports) and m2
(weight of the loading device on the beam); A (m2) is the area of the
Fig. 3. Shape of the notched beam. ligament.

4
P. Zhang, et al. Ceramics International xxx (xxxx) xxx–xxx

strengths as well as axial compressive strengths of mortar show the


same variation trend with PVA fiber content, whether nano-SiO2 was
added or not. This is different from the conclusion that PVA fiber has
little effect on compressive strength by Masi and Al-Majidi [17,52],
while consistent with Xu, Ekaputri, Park and Choi on the enhancement
of compressive strength by adding fiber [38,53–55]. The general
changing pattern of compressive strength with PVA fiber content is that
the strength first increases until the fiber content reaches 0.8% and then
begins to decline. The peak value of cubic compressive strength is
63.8 MPa and 60.4 MPa for fiber reinforced mortars with and without
nano-SiO2, increasing by 27.6% and 29.1% compared with control
groups, respectively. The initial promotion in cubic compressive
strength is on account of the restriction of PVA fiber on transverse ex-
pansion after specimens cracking, which leads to the increased ability
to resist the deformation. Increasing in axial compressive strength may
be attributed to the restriction of PVA fiber for specimen deformation
by taking some of the tensile stress when the specimen is subjected to
Fig. 4. Slump flow with different PVA fiber fractions. the axial load [56]. However, continuous increase of fiber content after
the optimum value will result in the reduction of compressive strengths;
this is different from previous studies on PVA reinforced geopolymer
3. Results and discussion
composites, where PVA showed continuous improvement on compres-
sive strength with content increasing. The possible reason for this
3.1. Workability
phenomenon is that excessive fiber will affect the uniformity of mortar,
and the voids formed by fiber clustering in matrix can decline the load
Fig. 4 shows the workability varying with PVA fiber and nano-SiO2
capacity. In general, for two series with different nano-SiO2 dosages,
content. Apparently, slump flow decreased by 26.4% with the fraction
there is a slight improvement in both cubic and axial compressive
variation of PVA fiber from 0 to 1.2%. The effect of adding fiber on the
strengths after introducing 1% nano-SiO2. This indication agrees with
workability of geopolymer mortar is consistent as that of cementitious
that nano-SiO2 has the positive effect on strength growth of cement-
materials [48]. The lower fluidity of geopolymer mortar with higher
based materials [18]. This is due to the pozzolanic activity of nano-
PVA fiber content is probably attributed to the increased density caused
SiO2, which leads to more aluminosilicate gels in mortar as a compli-
by the decreased porosity, as well as the reduction of free water caused
ment to the Si―O bonds [57]. Moreover, there is an optimal value of
by the hydrophilic behavior of PVA fibers. Moreover, the intensifying
PVA fiber content (0.8%) that enables compressive strengths reach the
entanglement of fibers could cause greater flow resistance of the mix-
highest when 1% nano-SiO2 is added. When a large amount of nano-
ture [49]. The result is consistent with previous studies [50,51]. The
SiO2 is added, the synergistic enhancement of compressive strength is
change of fiber content has the similar effect on workability of geopo-
obvious according to Xu et al. [55]. Therefore, it is feasible to increase
lymer mortars with and without nano-SiO2. With the variation gamut of
the content of nano-SiO2 to improve the PVA fiber reinforcing effect
PVA fiber content, the slump flow of geopolymer mortar with and
and enhance the strength of geopolymer composites in future study.
without nano-SiO2 decreased by 26.36% and 26.42%, respectively.
However, geopolymer mortars with 1.0% nano-SiO2 exhibited slightly
higher slump flow than those without nanoscale additives. 3.3. Flexural performance

3.3.1. Flexural strength


3.2. Compressive strength As shown in Fig. 6, within the considered range of fiber content in
this study, PVA fiber exhibits the promotion effect on flexural strength.
Fig. 5 shows compressive strength with different fiber contents of When only PVA is added to the geopolymer mortar, the flexural
geopolymer mortars with and without nano-SiO2. From Fig. 5 it can be strength increased by up to 68% as the fiber content increased. Com-
concluded that, same as the slump flow test results, cubic compressive pared to Xue's study [58], the flexural strength of geopolymer mortar in

Fig. 5. Compressive strength with different PVA fiber fractions. Fig. 6. Flexural strength with different PVA fiber fractions.

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P. Zhang, et al. Ceramics International xxx (xxxx) xxx–xxx

Fig. 7. Residual compressive strengths with different PVA fiber fractions. Fig. 8. Elastic modulus with different PVA fiber fractions.

this study is approximately 40% higher than PVA fiber reinforced ce- Therefore, the introduction of PVA fiber can indeed increase the
ment composites. This is due to the higher bonding strength between toughness and strength of mortar. However, excessive fiber will affect
PVA fiber and geopolymer mortar than that between PVA fiber and the uniformity of mortar and then affect the load capacity because of
cement matrix [59]. Similar to the effect on compressive strength, the the dense network structure. Hence, there is an optimal fiber content to
introduction of nano-SiO2 also has the positive effect on improving maximize the axial compressive strength and elastic modulus. More-
flexural strength, which is proved by Li et al. [60]. However, when over, the above two parameters of geopolymer mortar mixed with
considering the combined effect of fiber and nano additives, the en- nano-SiO2 are higher than those without nano-SiO2. This is due to the
hancement effect of nano-SiO2 on strength becomes weaker when the pozzolanic activity of nano-SiO2, which can be considered as a com-
PVA fiber content reaches 1.0%. The enhanced cracking resistance by pliment to the Si―O bonds, and it leads to more aluminosilicate gels in
adding PVA fiber comes from the nature of fiber, which has superior the mortar [57].
mechanical performances such as high strength and elastic modulus,
low elongation, etc.
3.5. Fracture properties

3.3.2. Residual compressive strength after flexural test The fracture behavior of geopolymer composites is usually char-
In order to investigate flexural properties of the modified geopo- acterized by sharp failure at the crack propagation stage [64], while the
lymer mortar, residual compressive strength of specimens after bending propagation of crack can be decelerated by the incorporation of fiber.
are also studied (Fig. 7). As with unbent specimens, the residual com- Peak loads of specimens and critical effective crack lengths with dif-
pressive strength first increased, and then decreased when PVA fiber ferent dosages of PVA fiber and nano-SiO2 are shown in Fig. 9 and
content exceeded a certain value. The peak residual compressive Fig. 10, respectively. It is clear that irrespective of nano-SiO2 addition,
strength appeared in the fiber content of 0.8%, no matter nano-SiO2 PVA fiber addition could considerably improve the carry capacity of
was added or not. For specimens with and without nano-SiO2, the geopolymer mortar. As shown in Fig. 9, the peak load first increases
maximum increases of residual compressive strength are 36.7% and significantly with the increase of PVA fiber content, then decreases
41.8%, respectively, which exhibits the higher increasing range than slightly when PVA content is over 1.0%. Differently, the inflection point
cubic compressive strength (compared with Fig. 5). In other words, it in Fig. 10 occurs at 0.4% and 0.6% fiber content. The critical effective
reflects the effect of fiber addition on improving the flexural strength. crack length increases abruptly after 0.4% fiber content and then re-
In addition, the enhancement effect of nano-SiO2 on residual com- mained basically unchanged after 0.6%, which indicates that the
pressive strength after flexural test is also shown in Fig. 7. At any fiber
content, a small amount of nano-SiO2 addition can improve the residual
compressive strength after flexural test, which proves that nano-SiO2
can also enhance the flexural properties of geopolymer mortar.

3.4. Elastic modulus

Fig. 8 reveals the relationship between elastic modulus with fiber


content. Compared to geopolymer mortar without any fiber in other
studies [61,62], geopolymer mortar modified with PVA fiber in this
study exhibits the 20%–130% higher elastic modulus. Similar to
changes in compressive strengths, both axial compressive strength and
elastic modulus first increase and then decrease with the variation of
PVA fiber content. Moreover, variation trend of the two parameters
with PVA fiber content are consistent whether adding nano-SiO2 or not.
This may be attributed to the restriction of PVA fiber for specimen
deformation by taking some of the tensile stress when the specimen is
subjected to the axial load [56]. Furthermore, the crack growth will
probably develop along the original direction rather than away from it
and will be restricted due to PVA fiber in disordered state [63]. Fig. 9. Peak loads with different PVA fiber fractions.

6
P. Zhang, et al. Ceramics International xxx (xxxx) xxx–xxx

toughness. However, the unstable fracture toughness increases sharply


after 0.4% fiber content, and then keeps growing until 1.0%. After the
surge, the difference between unstable fracture toughness and initiation
fracture toughness grows with the increase of PVA fiber content. The
variations of critical effective crack length and fracture toughness
consistently indicate that the stable crack propagation get longer, i.e.,
the stability of geopolymer mortar with cracks increase with PVA fiber
content. P-CMOD curve is shown in Fig. 12 and fracture energy calcu-
lated accordingly is shown in Fig. 13. It is clearly that the envelope area
under P-CMOD curve gets larger when PVA fiber content is higher, and
the fullest curve occurred when fiber content was 1.0%. Correspond-
ingly, as shown in Fig. 13, for both geopolymer mortars with and
without SiO2, the fracture energy of geopolymer mortar mixed with
PVA fiber is much higher than that without fiber. Fracture energy
measured in this study is about 10 times higher than geopolymer
mortars without fibers [66], and is about 5 times higher than that with
steel fibers in other studies [67]. The fracture energy gets higher when
PVA fiber ratio increases. However, the fracture energy decline sharply
Fig. 10. Critical effective crack lengths with different PVA fiber fractions.
when fiber content exceeds 1.0%. From Fig. 12 it can also be observed
that the curve snaps off in the descending phase for geopolymer mortar
stability of geopolymer mortar is distinctly improved when the PVA without fiber or nano-SiO2, while curves extend longer during the
fiber content is higher than 0.6%. descent for geopolymer mortars modified with PVA fiber and nano-
The variation of fracture toughness with PVA fiber content was SiO2. Especially for mortars with small fiber content and 1.0% nano-
shown in Fig. 11. From Fig. 11 it is revealed that, whether nano-SiO2 is SiO2, the lengthening effect of descending curve is particularly pro-
added or not, the addition of PVA fiber is beneficial to improve fracture nounced.
toughness of geopolymer mortars. Similar improvements of PVA fiber It can be concluded from the above phenomena, the introduction of
on KIcini and KIcun of cement mortar were studied [65]. To be specific, the PVA fiber could improve the fracture property of geopolymer mortars.
initiation fracture toughness increases slightly with PVA fiber content This is due to the cracking prevention and toughening effect of PVA
when it is lower than 0.4%, and it is close to the unstable fracture fiber. On the one hand, PVA fiber itself has high elastic modulus and
high tensile strength, which could disturb the internal stress of mortar
and will retard or deflect the crack expansion when mortar cracks. On
the other hand, when cracks have already occurred and continue to
expand, it is necessary to overcome the friction shear stress between
mortar and fiber surface, which in turn could impede the cracks de-
velopment; as fiber cross the cracks, the bridging effect could enhance
the toughness of geopolymer mortar as well. However, the fracture
parameters decrease with excessive PVA fiber (1.0%), as Figss. 9–13
show. This is due to the growing porosity caused by the cluster effect,
which lead to the decrease in mortar uniformity.
Similar to that of the cementitious composites [68], the effect of
nano-SiO2 on the fracture behavior of geopolymer mortar is also ob-
vious. According to Figss. 9–13, when geopolymer mortar is not mixed
with PVA fiber but modified with nano-SiO2, all the four fracture
parameters are improved in different degrees, which demonstrates the
improvement of nano-SiO2 for fracture property. From Fig. 10, it can be
observed that at first nano-SiO2 could improve the load capacity of PVA
fiber reinforced geopolymer mortar, but the improvement is not ob-
vious after PVA fiber content reaching 0.6%, which means that en-
hancing the load capacity of mortars mainly depends on PVA fiber ra-
ther than nano-SiO2. Moreover, as can be seen from Fig. 11, the
synergistic effect of PVA fiber and nano-SiO2 on unstable fracture
toughness is greater than that on initiation toughness when PVA fiber
content is more than 0.4%. The descending curve (Fig. 12) indicates the
remarkable effect of nano-SiO2 in improving toughness of the geopo-
lymer mortar with little or no PVA fiber. As to fracture energy (Fig. 13),
in addition to increasing the fracture energy of PVA fiber reinforced
geopolymer mortar, nano-SiO2 can also reduce the adverse effect of
excess fiber on fracture energy of mortar. This is attributed to the filling
effect of the nanoscale SiO2, which can increase the chain length of C-S-
H gel thus making the matrix more compact, so as to maximize the
improving effect of PVA fiber on fracture performance of mortar.
Based on the above four fracture parameters, it can be concluded
that the nano-SiO2 modified geopolymer mortar with fiber content of
1.0% has the best fracture performance.

Fig. 11. Fracture toughness with different PVA fiber fractions.

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P. Zhang, et al. Ceramics International xxx (xxxx) xxx–xxx

Fig. 12. P-CMOD curves.

network for estimating or approximating functions. In date, ANN has


been widely used to solve complex scientific problems. In recent years,
a considerable number of studies on predicting the mechanical prop-
erties of cement concrete or geopolymer composites by ANN were made
by researchers all over the world [23,24,69,70]. ANFIS, the combina-
tion of ANN and fuzzy logic, is a new type of adaptive neural network
which achieve the fuzzification, fuzzy inference and inverse fuzzifica-
tion using ANN [71]. Studies have shown that ANFIS has better pre-
diction ability than ANN [35,36]. ANFIS can not only be used to es-
tablish nonlinear mapping relations, but also shows better convergence,
stability and uniqueness of training results. Therefore, for fracture
properties affected by various factors such as materials, water to binder
ratio, specimen sizes, and geometric features [72,73], ANFIS can be
used to predict the fracture parameters.

4.1. Establishment and training of the ANFIS models

Fig. 13. Fracture energy with different PVA fiber fractions. The establishment of ANFIS model for fracture parameters predic-
tion of geopolymer mortar was carried out by the following steps: (1)
preparation of linearly normalized data for modeling, whose values are
between 0 and 1; (2) training the model by fuzzy inference system
based subtractive clustering algorithm, by which the natural groupings
of data can be identified; (3) validation of the model by evaluating
three statistical criteria: RMSE, MAE, and R2. These Quantitative in-
dicators are calculated by Eq. 13–15.
n
1
RMSE =
n
∑ (yi − yˆi )2
i=1 (13)
n
1
MAE =
n
∑ yi − yˆi
i=1 (14)
n
∑i = 1 (yi − yˆi )2
R2 = 1 − n
∑i = 1 (yi − y‾ )2 (15)

where yi is defined as the experimental value of the output, ŷi is the


predicted value of output, y‾ is the mean of yi , and n is the number of
samples.
In this study, eight factors including the basic mechanical properties
were considered to affect the fracture parameters. Hence, the input
Fig. 14. ANFIS model structure. parameters include PVA fiber content (%p), nano-SiO2 content (%n),
compressive strength ( fcu ), flexural strength (Rf ), elastic modulus (Em ),
4. ANFIS approaches for fracture parameters prediction critical crack mouth opening displacement (Vc ), crack load (Pini ) and
peak load (Pmax ). The output parameters are four fracture parameters,
ANN, one of the algorithms of machine learning, is a mathematical namely critical effective crack length (ac ), initial fracture toughness
model that mimics the structure and function of a biological neural (KIcini ), unstable fracture toughness (KIcun ), and fracture energy (G F ).
Totally, 40 sets of data (including three trials for each group) were

8
P. Zhang, et al. Ceramics International xxx (xxxx) xxx–xxx

Fig. 15. Predicted and experimental values of test datasets.

Table 5 In this ANFIS model, subtractive clustering algorithm was adopted to


Model evaluation parameters. generate the fuzzy inference system. The initial value of four para-
Output Statistical parameters Training epoch (to achieve the meters for this algorithm (range of influence, squash factor, accept
parameters minimum testing error) ratio, and reject ratio) were determined according to the selection
RSME MAE R2 method recommended by Zhang [71]. Considering the implement-
ability and prediction accuracy of the model, the four calculating
ac 0.13165 0.06258 0.85529 74
0.01021 0.00637 0.99867 6 parameters were adjusted to 1, 2, 0.5, and 0.15, respectively. The model
KIcini
structure consists of 8 input neurons, 2 hidden layers, and 1 output
KIcun 0.02002 0.01694 0.99676 23
GF 0.08846 0.06526 0.91239 9 neuron, as demonstrated in Fig. 14. This process was repeated 4 times
to get 4 ANFIS models for each output parameter.

collected for modeling, in which 30 sets were used for model training 4.2. Model evaluation
and 10 for testing.
The training has been done with Neuro-Fuzzy Designer by MATLAB. Training results of the 4 ANFIS model are very satisfied, in which

9
P. Zhang, et al. Ceramics International xxx (xxxx) xxx–xxx

the training error were all less than 5 × 10-5. Testing results, as illu- Declaration of competing interest
strated in Fig. 15, indicated that the values predicted by ANFIS model
agreed well with experimental values. RMSE, MAE, and R2 of four The authors declare that there is no conflict of interests in this
output parameters through ANFIS were listed in Table 5. Basically, the paper.
closer the values of RMSE and MAE are to 0, the better prediction ac-
curacy is; conversely, the closer R2 is to 1, the better fit regression of the Acknowledgements
model proposes [74,75]. Results demonstrated that it is feasible to
predict fracture parameters with conventional mechanical parameters The authors would like to acknowledge the financial support re-
of geopolymer mortar by ANFIS model. In addition, the ANFIS algo- ceived from National Natural Science Foundation of China (Grant No.
rithm possessed the excellent prediction ability for fracture parameters. 51678534, 51979251), Program for Innovative Research Team (in
Predicted outcomes in Fig. 15 and statistical parameters in Table 5 Science and Technology) in University of Henan Province
demonstrate the excellent suitability of the established ANFIS model for (20IRTSTHN009), CRSRI Open Research Program (Grant No.
four fracture parameters prediction of geopolymer mortars; the pre- CKWV2018477/KY) and Open Projects Funds of Dike Safety and
dicting results obtained by this method are of high accuracy. Further- Disaster Prevention Engineering Technology Research Center of
more, the prediction accuracy of KIcini and KIcun is higher than that of ac Chinese Ministry of Water Resources (Grant no. 2018006). We greatly
and G F . From the comparison of predicted results with experimental appreciate valuable comments and suggestions from the editor and
results and error analysis of the proposed ANFIS model, it could be reviewers.
easily concluded that, ANFIS algorithm is a promising tool for pre-
dicting the fracture parameters of geopolymer mortars modified with References
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