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Ceramics International
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SiC fiber reinforced geopolymer composites, part 2: Continuous SiC


fiber
Peigang He a,b,n, Dechang Jia a,b,n, Binyi Zheng a,b, Shu Yan a,b, Jingkun Yuan a,b,
Zhihua Yang a,b, Xiaoming Duan a,b, Jiahuan Xu c, Pengfei Wang d, Yu Zhou a,b
a
Institute for Advanced Ceramics, Harbin Institute of Technology, Harbin, China
b
School of Materials Science and Engineering, Harbin Institute of Technology, Harbin, China
c
School of Mathematics and Physics, Jiangsu University of Science and Technology, Zhenjiang, China
d
CAS Key Laboratory of Mechanical Behavior and Design of Materials, Department of Modern Mechanics, University of Science and Technology of China,
Hefei, China

art ic l e i nf o a b s t r a c t

Article history: In this paper, unidirectional SiC fiber (SiCf) reinforced geopolymer composites (SiCf/geopolymer) were
Received 4 April 2016 prepared and effects of fiber contents on the microstructure and mechanical properties of the composites
Received in revised form in different directions were investigated. The XRD results showed that addition of SiCf retarded geopo-
26 April 2016
lymerization process of geopolymer matrix by weakening the typical amorphous hump. SiCf in all the
Accepted 27 April 2016
composites were well infiltrated by geopolymer matrix, but microcracks which were perpendicular to
the fiber axial direction were noted in the interface area due to the thermal shrinkage of matrix during
Keywords: the curing process. With the increases in fiber contents, although Young's modulus of the composites
SiC fiber increased continuously, flexural strength, fracture toughness and work of fracture increased at first,
Geopolymer
reached their peak values and then decreased. And when fiber content was 20 vol%, the composites
Composites
showed the highest flexural strength, fracture toughness and work of fracture, which were 14.2, 15.2 and
Mechanical properties
Fracture behavior 81.6 times as high as those of pristine geopolymer, respectively, indicating significant strengthening and
toughening effects from SiCf. Meanwhile, SiCf/geopolymer composites failed in different failure modes in
the different directions, i.e., tensile failure mode in the x direction (in-plane and perpendicular to the
fiber axial direction) and shear failure mode in the z direction (laminate lay-up direction).
& 2016 Elsevier Ltd and Techna Group S.r.l. All rights reserved.

1. Introduction Recently, many studies have been carried out in order to im-
prove mechanical performance and crack tolerance of geopolymer
Geopolymer is a unique three-dimensional inorganic material materials. Typically, geopolymer based composites have been de-
that offers multiple valuable properties including easy-processing veloped with the presence of second phases, including graphene
and environmentally friendly nature, low CO2 emission, low den- [15–18], nanotube [19,20], particle [21–25], epoxy [5,26–28], short
sity, higher mechanical performance and anti-permeability than fiber [29–36] and continuous fiber [25,37–41]. Among them, fibers
traditional Portland cement, high melting point (1200–1600 °C) showed the best strengthening effect. Ranjbar et al. [42] reported
[1–9]. And thus it has been considered as a promising alternative that flexural strength of 3 wt% steel fiber reinforced geopolymer
to cement in the fields of infrastructure, hazard element en- based composite was more than 3 times as high as that of neat
capsulation, and heat resistant component, among others [10–14]. geopolymer; Assaedi et al. [43] prepared flax fabric reinforced
However, like other brittle materials such as cement and ceramic, geopolymer composites, and flexural strength, compressive
neat geopolymer materials showed disadvantages of both low strength, and fracture toughness were 411.1%, 369.1% and 350.0%
mechanical performance and catastrophic fracture behavior, higher than those of pure geopolymer, respectively; Lin et al. [31]
which were the insurmountable obstacle when they were applied prepared short carbon fiber reinforced geopolymer composites,
as structural components. and improved mechanical properties together with non-brittle
failure behavior were noticeable. In our previous research [38] we
n prepared continuous carbon fiber reinforced geopolymer compo-
Corresponding authors at: Institute for Advanced Ceramics, Harbin Institute of
Technology, Harbin, China. sites. Combined with the post high-temperature treatment, the
E-mail addresses: peiganghe@hit.edu.cn (P. He), dcjia@hit.edu.cn (D. Jia). resulted composites showed comparable mechanical performance

http://dx.doi.org/10.1016/j.ceramint.2016.04.168
0272-8842/& 2016 Elsevier Ltd and Techna Group S.r.l. All rights reserved.

Please cite this article as: P. He, et al., SiC fiber reinforced geopolymer composites, part 2: Continuous SiC fiber, Ceramics International
(2016), http://dx.doi.org/10.1016/j.ceramint.2016.04.168i
2 P. He et al. / Ceramics International ∎ (∎∎∎∎) ∎∎∎–∎∎∎

to advanced ceramic matrix composites such as Cf/SiO2 [44], Table 1


SiCf/SiC-Al2O3-Y2O3-CaO [45] and Cf/SiO2-Si3N4 [46] composites. Properties of SiC fiber.
Therefore, geopolymer technique provides an alternative route for
Brand Density Diameter Tensile Modulus Elongation (%)
the preparation of ceramic composites for potential high-tem- (g cm  3) (mm) strength (GPa)
perature applications. (GPa)
However, although carbon fiber can keep its superior proper-
SLFC1 2.36 137 0.5 1.5–1.6 1407 10 1.3–1.4
ties up to 2000 °C in protecting atmosphere, it is susceptible to be
oxidized to CO2 at a temperature as low as 500 °C in air, which
would be the worst disadvantage of the composites when exposed vacuum-bag technique after mechanical pressing. The fiber con-
to high temperature in air. SiC fiber showed similar mechanical tents are 10 vol%, 15 vol%, 20 vol% and 25 vol%.
performance as carbon fiber, but much higher oxidation resistance. The phases of composites after heat treatment were char-
It has been reported that SiC fiber can retain 80% room-tempera- acterized using an X-ray diffractometer (XRD: Rigaku, D/MAX-
ture strength even at 1200 °C in air, which makes it a prominent 2200VPC, Tokyo, Japan) with CuKa radiation at a scan rate of 4°/
high-temperature reinforcing candidate. min. Mechanical performance of the composites in the x direction
This paper will focus on the preparation of continuous SiC fiber (in-plane and perpendicular to fiber axial direction) and z direc-
reinforced geopolymer composites, together with an investigation tion (laminate lay-up direction) were investigated. Flexural
on the microstructure, interfacial state, mechanical properties and strength measurements were conducted on specimens
fracture behavior of the composites. Relevant studies were rarely (4 mm  3 mm  36 mm) using a three-point-bending fixture on
reported before. The high-temperature performance of the com- an Instron-500 testing machine with a span length of 30 mm at a
posites and comparison with carbon fiber reinforced geopolymer crosshead speed of 0.5 mm/min. Work of fracture was calculated
composites will be carried out in our future study. by the area between load curves and X axis in the load/displace-
ment curves till the load dropped to 90% of the maximum load. Six
specimens were tested under each test condition. Surface micro-
2. Materials and experiments graphs of the SiCf/geopolymer composites were observed by op-
tical microscope. Fractographs of the composites were observed by
Geopolymer resin with a composition of SiO2/Al2O3 ¼4, scanning electron microscopy.
K2O/SiO2 ¼0.25 and H2O/K2O¼ 11 (mole ratio) was obtained by
mixing metakaolin powder with potassium silicate solution. The
metakaolin was prepared by calcining kaolin at 800 °C for 3 h and 3. Results and discussion
the potassium silicate solution was prepared by dissolving amor-
phous silica (Shanghai Dixiang Indus, China) into KOH (Tianjin Fig. 2 shows the phase composition of SiC fiber, metakaolin,
Fuchen Indus., China) solution stirring for 48 h in order to dissolve geopolymer and SiCf/geopolymer composites. SiC fiber mainly
the silica completely. The particle size distribution of metakaolin is consisted of β-SiC, as shown in Fig. 2(a). Metakaolin showed
shown in Fig. 1, indicating that most particles are of 2–8 mm and characteristic amorphous hump between 22° and 24° (2θ), and
the average diameter of 4.44 mm. SiC fiber used in this study several reflections from quartz present introduced by the raw
(Sailifei Ceramic Fiber Co., Ltd., China) has a diameter of 13 mm and metakaolin. Post geopolymerization, the characteristic amorphous
an average tensile strength of 1.5–1.6 GPa, as shown in Table 1. SiC hump shifted to a higher position, 27–29° (2θ), which was a ty-
fiber was first treated at 370 °C in an air atmosphere for 2 h to pical feature as observed in other geopolymer materials. However,
remove the surface epoxy coating. The composite was prepared by with the addition of SiCf, typical amorphous hump in geopolymer
infiltrating geopolymer resin into the unidirectional continuous was weakened whereas hump between 22–24° became stronger
SiC fiber preform with the help of the ultrasonic vibration treat- than that in geopolymer, indicating SiCf retarded the geopoly-
ment, and stacked one by one to get a green sample with 16 layers. merization process of the matrix. Meanwhile, refraction peaks
To control fiber contents in the composites, the different me- corresponding to β-SiC were also weakened due to geopoly-
chanical pressure of 0.5, 1.0, 1.5 and 2 MPa, were applied to the merization.
green compact in a Hydraulic Machine. To remove the pores in the All the SiCf/geopolymer composites showed homogeneous
composites, degassing was applied at 70 °C for 24 h using a microstructure, and most fibers maintained unidirectional, as
shown in Fig. 3. The magnified microstructure in Fig. 4 showed
that the fiber bundles were infiltrated with porous geopolymer
matrix. Meanwhile, microcracks which were perpendicular to the
fiber axial direction were also noted. During curing process of the
SiCf/geopolymer composites, fiber maintained unchangeable, but
geopolymer matrix showed shrinkage due to both condensation of
-OH groups and evaporation of waters in macropores and capil-
laries. Therefore, matrix shrinkage in the axial direction was highly
hindered by the fibers, leading to the formation of the microcracks
in the matrix.
Fig. 5 shows flexural strength and Young's modulus of
SiCf/geopolymer composites in the x direction. It was noticed that
with the increase in fiber content flexural strength ramped up
first, reached the peak value when fiber content was 20 vol%, and
then decreased for the composite with a higher fiber content of
25 vol%. It should be pointed out that with 10 vol% fiber content,
the flexural strength of the corresponding composite was
147.5 MPa, which was 13.2 times as high as that of neat geopoly-
Fig. 1. Particle diameter distribution of metakaolin. mer, indicating a significant strengthening effect from SiC fibers.

Please cite this article as: P. He, et al., SiC fiber reinforced geopolymer composites, part 2: Continuous SiC fiber, Ceramics International
(2016), http://dx.doi.org/10.1016/j.ceramint.2016.04.168i
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Fig. 2. XRD patterns of SiC fiber (a), metakaolin, geopolymer and SiCf/KGP composites (b).

(a) (b)

400 m 400 m

(c) (d)

400 m 400 m

Fig. 3. Microstructure of SiCf/KGP composites with different fiber contents: (a) 10 vol%, (b) 15 vol%, (c) 20 vol% and (d) 25 vol%.

According to the strength mixing rule of composite, critical fiber Vfc =


σmu
content (Vfc) can be calculated according to the Eqs. (1)–(4), where σmu + σfu − σf′ (4)
smu, sfu, Δsf and σ′f , are the ultimate stress of matrix, ultimate
stress of fiber, additional fiber stress and fiber stress when matrix σmu
Vfc ≈
fractured, respectively; Vf and Vm are the volume contents of fiber σfu (5)
and matrix, respectively. In SiCf/geopolymer composite system, σfu ≫ σf ’ ≫ Δσf , effective
σ V Vfc can be calculated according to the Eq. (5), which implied that
Δσf = mu m the presence of high-performance fiber would enhance the
Vf (1)
strength of the composite. It explained the increase in flexural
Vf + Vm = 1 (2) strength when fiber contents were lower than 25 vol%. Within the
fiber content from 10 to 20 vol%, the flexural strength increased
slowly, from 147.5 MPa to 161.6 MPa, rising by 9.6%. The
Δσf = σfu−σf′ (3)
SiCf/geopolymer composite also showed higher flexural strength

Please cite this article as: P. He, et al., SiC fiber reinforced geopolymer composites, part 2: Continuous SiC fiber, Ceramics International
(2016), http://dx.doi.org/10.1016/j.ceramint.2016.04.168i
4 P. He et al. / Ceramics International ∎ (∎∎∎∎) ∎∎∎–∎∎∎

Fig. 4. Magnified microstructure of SiCf/KGP composites: (b) and (c) correspond to the areas B and C, respectively.

200 6 6000
30 1/2
Fracture toughness,MPa· m
-2
5 Work of fracture(J·m ) 5000

)
160 25

1/2
Flexural strength (MPa)

Fracture toughness (MPa· m


Young's modulus (GPa)

Work of fracture (J· m )


-2
4 4000
120 20

3 3000
15
80
2 2000
10
40
1 1000
5
0 0 0
0 5 10 15 20 25 0 10 15 20 25
Fiber content (vol %) Fiber content (vol %)

Fig. 5. Flexural strength and Young's modulus of SiCf/KGP composites in x Fig. 7. Fracture toughness and work of fracture of SiCf/KGP composites.
direction.

200
180 x direction
z direction
160
Flexural strength,(MPa)

140
120
100
80
60
40
20
0
0 10 20 25
Fiber content (vol %)
Fig. 6. Flexural strength of SiCf/KGP composites in x and z direction. Fig. 8. Stress and displacement curves of SiCf/KGP composites in x direction.

than Cf/geopolymer composite prepared through similar process matrix to the fiber during crack propagation. Therefore, at higher
[47], indicating a better interfacial state in SiCf/geopolymer than fiber content of 25 vol%, the possibility of both defects in-
that in Cf/geopolymer. However, when SiC fiber content was tensification and failure in load transferring would be higher, re-
25 vol%, the flexural strength showed a 17.5% drop to 133.3 MPa, sulting in the decrease in flexural strength.
compared to that of composites with 20 vol% fiber content. In the Young's modulus of the SiCf/geopolymer composites showed a
present investigation, higher fiber content indicated higher fiber- continuing rising trend with the increase in fiber content. Young's
matrix interfacial area, where defects such as microcracks and modulus can be calculated according to the Halpin-Tsai model as
micropores would gather as shown in Fig. 4. Meanwhile, with shown in Eqs. (6) and (7), where Ec, Ef and Em were Young's
respect to SiCf, geopolymer matrix was much weaker in strength, modulus of the composites, fiber and matrix; ξ was a parameter
and there might be not enough matrix to transfer the load from related to fiber morphology. Therefore, in this investigation,

Please cite this article as: P. He, et al., SiC fiber reinforced geopolymer composites, part 2: Continuous SiC fiber, Ceramics International
(2016), http://dx.doi.org/10.1016/j.ceramint.2016.04.168i
P. He et al. / Ceramics International ∎ (∎∎∎∎) ∎∎∎–∎∎∎ 5

Fig. 9. Images of bar specimens of SiCf/KGP composites in (a) x direction, (b) z direction, and (c) geopolymer matrix.

Fig. 10. Fractograph of SiCf/KGP composites in different directions. (a)–(c) x direction, (d)–(e) z direction.

Please cite this article as: P. He, et al., SiC fiber reinforced geopolymer composites, part 2: Continuous SiC fiber, Ceramics International
(2016), http://dx.doi.org/10.1016/j.ceramint.2016.04.168i
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modulus of SiC fiber (200 GPa) was much higher than that of geopolymer composite (SiCf/geopolymer) is prepared by a simple
matrix (8 GPa), resulting in the increase in modulus of composites ultrasonic-assisted slurry infiltration method. Effects of fiber con-
with fiber content. tent on the microstructure and mechanical properties of the
composites are studied. The results proved that with proper SiC
Ec 1 + ξηVf
= fiber content, the obtained SiCf/geopolymer composites showed
Em 1 + ξηVf (6)
greatly enhanced mechanical properties together with non-cata-
strophic fracture behavior. The main conclusions could be drawn
Ef /Em − 1 + ξηVf
η= as below:
Ef /Em + ξ (7)

Fig. 6 compared flexural strengths of SiCf/geopolymer compo- (1) The composites showed homogeneous microstructure and SiCf
sites in x and z directions. It can be noted that the composite were well infiltrated by geopolymer matrix. Meanwhile, mi-
showed anisotropic characteristic, i.e., higher flexural strength in crocracks in the interfacial area were observed, which was due
the x direction than that in z direction. But with the increase in to the thermal shrinkage of the matrix during the curing
fiber contents, the strength difference between two directions process.
decreased. In the z direction where fiber plies laid up, the gap (2) When fiber content was 20 vol%, the related composite
between two layers was the matrix-rich area, which was weak and showed the highest flexural strength, fracture toughness and
stress concentrated, leading to the strength decreasing in this di- work of fracture, which were 14.2, 15.2 and 81.6 times as high
rection. In this investigation, fiber content control was achieved as those of geopolymer matrix, respectively, indicating sig-
through applying different pressing stress. With increasing nificant strengthening and toughening effect from SiCf. All the
pressing stress, the gap between two layers (along z direction) SiCf/geopolymer composites showed non-brittle failure modes
decreased, and thus the strength difference between two direc- rather than the catastrophic failure as observed in neat geo-
tions became not evident. polymer. Meanwhile, the composites failed in tensile failure
Fig. 7 shows fracture toughness and work of fracture of mode in the x direction and shear failure mode in the z
SiCf/geopolymer composites, which showed similar trends to direction.
flexural strength. When fiber content was 20 vol%, the composite
exhibited the highest fracture toughness and work of fracture,
Acknowledgements
4.26 MPa m1/2 and 4421.4 J m  2, which were 15.2 and 81.6 times
as high as those of pristine geopolymer. The work of fracture of the
SiCf/geopolymer composites was much higher than monolithic This work was supported by the Fundamental Research Funds
ceramics such as alumina, silica, Si3N4 and ZrO2, and was com- for the Central Universities (Grant no. HITNSRIF20165), and the
parable with high-temperature sintered Cf/soda, Cf/LAS compo- National Natural Science Foundation of China (NSFC, Nos.
sites. This implied that geopolymer provides a low-cost route to 51372048, 51502052, 51321061 and 51225203).
prepare advanced composites of high reliability.
Fig. 8 shows typical stress-displacement curves of geopolymer
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(2016), http://dx.doi.org/10.1016/j.ceramint.2016.04.168i
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Please cite this article as: P. He, et al., SiC fiber reinforced geopolymer composites, part 2: Continuous SiC fiber, Ceramics International
(2016), http://dx.doi.org/10.1016/j.ceramint.2016.04.168i