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Materials Science and Engineering A 497 (2008) 181–185

Contents lists available at ScienceDirect

Materials Science and Engineering A


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

Effects of fiber length on mechanical properties and fracture behavior


of short carbon fiber reinforced geopolymer matrix composites
Tiesong Lin, Dechang Jia ∗ , Peigang He, Meirong Wang, Defu Liang
Institute for Advanced Ceramics, Harbin Institute of Technology, Harbin 150001, People’s Republic of China

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

Article history: A kind of sheet-like carbon fiber preform was developed using short fibers (2, 7 and 12 mm, respectively)
Received 4 February 2008 as starting materials and used to strengthen a geopolymer. Mechanical properties, fracture behavior,
Received in revised form 26 June 2008 microstructure and toughening mechanisms of the as-prepared composites were investigated by three-
Accepted 26 June 2008
point bending test, optical microscope and scanning electron microscopy. The results show that the short
carbon fibers disperse uniformly in geopolymer matrix. The Cf /geopolymer composites exhibit apparently
Keywords:
improved mechanical properties and an obvious noncatastrophic failure behavior. The composite rein-
Geopolymer
forced by the carbon fibers of 7 mm in length shows a maximum flexural strength as well as the highest
Composites
Short carbon fiber
work of facture, which are nearly 5 times and more than 2 orders higher than that of the geopolymer
Sheet-like preform matrix, respectively. The predominant strengthening and toughening mechanisms are attributed to the
Mechanical properties apparent fiber bridging and pulling-out effect based on the weak fiber/matrix interface as well as the
Fracture behavior sheet-like carbon fiber preform.
© 2008 Elsevier B.V. All rights reserved.

1. Introduction sion and excellent electrical properties [10], and have been used in
fabrication of the geopolymer mold in order to facilitate heat trans-
In recent years, geopolymer materials have attracted much more fer and stability of molds [11]. However, the mechanical properties
attention due to their low density, low cost, low curing/hardening and fracture behavior of short carbon fibers reinforced geopolymer
temperatures, environmentally friendly nature and excellent ther- matrix composites have not been reported yet.
mal stability at high temperatures [1–4]. Geopolymer materials At present, single or twin screw extruding [7,8,12] and high-
were regarded as the most promising substitute for aircraft com- speed mechanical mixing methods [9] are popular to mix short
posites and cabin interior applications instead of polymer materials fibers into matrix. However, the shear stresses exerted by screw
in a research program by U.S. Federal Aviation Administration or vane usually result in aggregation or fracture of fibers [12–14],
(F.A.A.) [5]. However, the poor mechanical properties of geopoly- which is unfavorable to obtain reasonable microstructure and
mer materials usually result in catastrophic failure during service, excellent mechanical properties. So, new methods for obtaining
which is a well-known impediment to their wide applications [6]. homogeneous distribution of intact fibers within matrix are very
Short fibers are effective reinforcements in strengthening and necessary.
toughening geopolymer materials. It was reported that short In this paper, we developed a kind of sheet-like short carbon
polyvinyl alcohol (PVA) fibers reinforced geopolymer composites fiber preform with the help of the ultrasonic scattering treat-
showed a good flexural strength and reasonable toughness [7,8]; the ment for reinforcing geopolymer matrix. In addition, effects of the
addition of short basalt fibers reduced the strength of composites, starting short carbon fiber length (2, 7 and 12 mm, respectively)
but the work of fracture of composites was drastically increased [9]. on the mechanical properties, fracture behavior and toughening
Zhao et al. [6] recently reported that incorporation of 10 vol.% short mechanisms of the as-prepared composites were systematically
Nextel 610 fibers could increase the flexural strength of geopolymer investigated.
matrix by 224%.
Short carbon fibers have advantages over other kinds of fibers
2. Experimental
because of their high modulus, high strength, low thermal expan-

The geopolymer resin used here has a composition with


SiO2 /Al2 O3 = 4, K2 O/SiO2 = 0.3 and H2 O/K2 O = 11 (mole ratio), as
∗ Corresponding author. Tel.: +86 451 86418792; fax: +86 451 86414291. described in a literature [15]. Kaolin powder (4.08 ␮m in aver-
E-mail address: dechangjia@yahoo.com.cn (D. Jia). age diameter) was calcined at 800 ◦ C for 2 h to obtain metakaolin

0921-5093/$ – see front matter © 2008 Elsevier B.V. All rights reserved.
doi:10.1016/j.msea.2008.06.040
182 T. Lin et al. / Materials Science and Engineering A 497 (2008) 181–185

Table 1
The chemical compositions of metakaolin (wt.%)

SiO2 Al2 O3 Fe2 O3 CaO CuO TiO2 SrO K2 O P2 O5 SO3 ZrO2 PbO Ga2 O3 ZnO

51.906 40.404 0.921 0.113 0.018 0.763 0.011 0.455 0.155 0.103 0.034 0.074 0.003 0.052

powder. The chemical compositions of the metakaolin are given load. Six specimens were tested under each test condition. Sur-
in Table 1. And its main phase is amorphous with a characteristic face micrographs of the Cf /geopolymer composites were observed
hump centered at about ∼28◦ in 2Â and its minor phase is quartz. A by optical microscope. Fracture surfaces of the composites were
typical processing route for geopolymer resin is as follows: a potas- observed by scanning electron microscopy.
sium silicate solution was made by dissolving silica sol into a KOH
solution with a magnetic stirrer. The metakaolin powder was then
added to the potassium silicate solution and mixed for 30 min with 3. Results and discussion
a high-shear mixer.
Starting short carbon fibers used for preparing preforms have It is known that the starting short carbon fibers possess a high
a diameter of 6–8 ␮m and an average length of 2, 7 and 12 mm, aspect ratio (330–2000), so they tend to twist during mixing. In this
respectively. They were first separated by an ultrasonic vibrator in experiment, the short carbon fiber preform preparation method
ethanol, then filtered out by a wire sieve to get sheet-like short with the help of the ultrasonic scattering treatment can effectively
carbon fiber preforms (as shown in Fig. 1) with a thickness in the prevent fibers from too much aggregation as indicated in Fig. 1. As a
range of 0.15–0.2 mm. The as-prepared preforms were impregnated result, the short carbon fibers have a relatively uniform distribution
with geopolymer resin in a plastic container and laid together one in geopolymer matrix for all the cases as shown in Fig. 3.
by one to get a stack consisting of 30 layer preforms. In order to The bar specimens of the Cf /geopolymer composites deform
avoid the formation of small pores between the sheet preforms significantly but without breaking completely even after a three-
during the lamination, a vacuum-bag technique was used at 80 ◦ C point bending test (Fig. 4(b)), suggesting a noncatastrophic fracture
for 48 h, followed by curing at 120 ◦ C for 24 h. The volume fraction of behavior. In contrast, the geopolymer matrix shows a typical brit-
short carbon fibers in the as-prepared composites is about 3.5 vol.%. tle failure mode (Fig. 4(a)). The apparent failure difference between
Fabrication process of Cf /geopolymer composites is illustrated in the composites and the matrix can also be clearly seen from their
Fig. 2. corresponding load/displacement curves as shown in Fig. 5. The
Flexural strength measurements were conducted on specimens low fracture energy of geopolymer matrix results in an apparent
(4 mm × 3 mm × 36 mm) using a three-point-bending fixture on an catastrophic failure. In comparison, the Cf /geopolymer compos-
Instron-500 testing machine with a span length of 30 mm at a ites all exhibit a non-linear elastic increase of load until the
crosshead speed of 0.5 mm/min. All flexural bars were machined maximum load was reached, then the load gradually decreases
with the tensile surface perpendicular to the direction of lamina- with increasing displacement, which is a typical pseudoplastic-
tion. Load-displacement curves were recorded. Work of fracture ity behavior. The higher fracture energy of the composite shows
was calculated by the area between load curves and X axis in the a progressive fracture behavior rather than a catastrophic behavior
load/displacement curves till the load drops to 90% of the maximum through the propagation of cracks proceeding in a progres-

Fig. 1. Optical images of as-prepared sheet-like short carbon fiber preforms with (a) 2 mm, (b) 7 mm and (c) 12 mm starting short carbon fibers in length, respectively.

Fig. 2. Fabrication process of short carbon fiber reinforced geopolymer matrix composites.
T. Lin et al. / Materials Science and Engineering A 497 (2008) 181–185 183

Fig. 4. Images of bar specimens of (a) geopolymer matrix and (b) Cf /geopolymer
composites after a three-point bending test.

Fig. 5. Load/displacement curves for (a) geopolymer matrix and the Cf /geopolymer
composites with starting fibers having an average length of (b) 2 mm, (c) 7 mm and
(d) 12 mm, respectively.

ture of the composites shows a similar trend as that of the flexural


strength. Incorporation of the preforms with 7 mm starting short
carbon fibers increases the work of fracture of geopolymer matrix
from 54.2 to 6435.3 J/m2 (nearly 118 times increase), indicating that
the composite reinforced by the stacked sheet-like short carbon
fiber preform can also absorb much energy to avoid the catastrophic
fracture behavior probably due to the friction between fibers and

Fig. 3. Micrographs of the surface of Cf /geopolymer composites with starting fibers


having an average length of (a) 2 mm, (b) 7 mm and (c) 12 mm, respectively.

sive and controlled manner with increasing displacement of the


crosshead [16].
The flexural strength and work of fracture of the composites
vs starting fiber length are shown in Fig. 6. The flexural strength
of the Cf /geopolymer composites increases with the increase of
the starting carbon fiber length from 2 to 7 mm. The addition of
short carbon fiber increases the geopolymer matrix strength from
16.8 to 91.3 MPa (4.4 times higher), which is regarded as a great
strengthening effect for such a low volume percentage (3.5%) of
short carbon fibers. However, the strengthening effect of fibers
unexpectedly lowers a little with a further increase in the start-
ing fiber length from 7 to 12 mm, and 84.6 MPa is obtained for the Fig. 6. Variation of flexural strength and work of fracture of geopolymer matrix and
composite with 12 mm starting fiber in length. The work of frac- Cf /geopolymer composites vs starting fiber length.
184 T. Lin et al. / Materials Science and Engineering A 497 (2008) 181–185

Fig. 7. High (a) and low (b) magnified scanning electron microscopy micrographs Fig. 8. Scanning electron microscopy micrographs of perpendicular (a) and parallel
of the tensile side of Cf /geopolymer composites after flexural strength tests. (b) to the fracture surface of Cf /geopolymer composites.

loading process. The fiber/matrix interfacial debonding and fiber


geopolymer matrix during fiber pulling-out. Therefore, geopoly-
pulling-out can consume much higher fracture energy and thus
mer matrix composites reinforced with stacked sheet-like preforms
prevent catastrophic failure during service.
of short carbon fibers exhibit an obvious noncatastrophic fracture
Typical fracture surfaces of the obtained composites after flex-
behavior.
ural strength tests are shown in Fig. 8. Lots of fiber pulling-outs
The increase in strength with increasing starting fiber length
are found because the bonding strength of fiber/matrix is relatively
from 2 to 7 mm might be attributed to the fact that the extent of
weak as shown from the clean surface of the pulling-out fibers and
load transmission is a function of fiber length and the magnitude of
the strength of carbon fibers is far higher than that of geopolymer
fiber/matrix interfacial cohesion. Longer fibers impart more restric-
matrix. The pulling-out length is so large that it ensures substan-
tion on deformation, whereas shorter fibers create friction due to
tially effective toughening effect from carbon fibers and therefore
the increased number of fiber ends [17]. In this paper, both the flex-
prevents catastrophic fracture of the composites. In addition, a lot of
ural strength and work of fracture show maximum value for the
cracks (Fig. 8(a)) distribute in the geopolymer matrix on the fracture
composites with 7 mm starting short carbon fibers. It is possible
surfaces of the obtained composites. These cracks are generated
that the interaction between carbon fibers and geopolymer matrix
because lots of fibers are pulled out from the geopolymer matrix in
reaches its maximum degree at this fiber length, and the effects of
different direction during testing to failure. And they are helpful to
fiber length decrease with longer fibers probably because of fiber
obtain higher work of facture value and make the composites show
entanglement [17]. The mechanical properties of Cf /geopolymer
the pseudoplasticity behavior.
composites indicate that 7 mm starting fiber length seems to be
the critical fiber length that is essential for the production of better
reinforcement in Cf /geopolymer composites. 4. Conclusions
The toughening mechanisms of Cf /geopolymer composites can
be deduced from the observations of the tensile side and frac- The geopolymer matrix composites were reinforced with a
ture surface of specimens. A lot of cracks formed on the surface of kind of sheet-like short carbon fiber preform prepared with the
tensile side of composite beam as shown in Fig. 7(a). They are gen- help of the ultrasonic scattering treatment, which exhibit excel-
erated with nearly homogeneous spacing and propagate relatively lent mechanical properties. The composites with 7 mm starting
perpendicular to the direction of tensile force. There is a high dis- short carbon fiber length show the maximum flexural strength and
tribution density of cracks on tensile surface of composites, which work of fracture values, which are increased by 4.4 times and 118
can consume a lot of energy and make the composites show the times, respectively, compared to that of the geopolymer matrix.
pseudoplasticity behavior. In addition, many holes formed on the The Cf /geopolymer composites show a typical pseudoplasticity
surface of tensile side of the composites beam, as shown in Fig. 7(a behavior rather than brittle failure mode as shown of geopolymer
and b). They are resulted from the fiber/matrix interfacial debond- matrix. The main strengthening and toughening mechanisms are
ing and fiber “pulling-out” from the geopolymer matrix during the attributed to the fiber bridging and pulling-out.
T. Lin et al. / Materials Science and Engineering A 497 (2008) 181–185 185

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