Ceramics International xxx (xxxx) xxx–xxx

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

Mechanical and thermal behavior of kaolin/rice-husk ash matrix composites

reinforced with corrugated steel fibers
⁎
P.R. Santos, N.P. Stochero, E. Marangon, M.D. Tier
Universidade Federal do Pampa, Unipampa, PPEng Campus Alegrete, RS, Brazil

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

Keywords: Rice-husk silica (RHS), an industrial solid waste from rice processing, and corrugated galvanized steel fibers,
Composite materials were evaluated as alternative raw materials for the production of ceramic-matrix composites. Compositions
Kaolin clay containing kaolin clay (75–80 vol%), RHS (15–20 vol%), and corrugated galvanized steel fibers (1–2 vol%) were
Rice-husk silica homogenized (12 wt% moisture) and uniaxially pressed at 20 MPa to produce composite materials. The pro-
Corrugated galvanized steel fibers
duced composites were dried and fired up to 1300 °C in an oxidizing atmosphere, and then characterized in
Fracture energy
terms of their physical, microstructural, mechanical, and thermal properties. The results showed that materials
with 20 vol% RHS exhibited low porosity and high mechanical strength. Composites containing 2 vol% corru-
gated galvanized steel fibers exhibited the best performance with respect to fracture energy.

1. Introduction
Rice-husk ash (RHA) is generated during rice husk combustion and
it forms approximately 20% of the initial husk weight [1]. In Brazil, for
example, about 2.5 × 106 t of RHA is generated each year [2]. When
the silica content in RHA is greater than 92%, it is defined as rice-husk
silica (RHS) [1]. RHS has a large spectrum of applications across many
industrial fields such as electronics, civil construction, and chemical
and ceramic materials [3,4].
Many studies have demonstrated the efficiency of using RHS as a
silica precursor for ceramic production in order to improve their me-
chanical properties [5–8]. Sobrosa et al. [9] investigated the effect of
partial replacement of clay by RHS (5, 10, and 20 vol%) for the fabri-
cation of kaolin ceramics. The results showed that the use of RHS
promoted better mixture packing, and consequently, an increase in
mechanical resistance. However, the fabricated ceramics exhibited low
resistance to thermal shock.
According to Aveston et al. [10], the use of fiber reinforcement in
ceramic-matrix composites (CMCs) has led to significant improvements
in the mechanical and thermal properties of monolithic ceramics in
addition to a decrease in their crack propagation and brittleness. There
are several reports on the incorporation of particulate or layered me-
tallic constituents into ceramics; however, the most effective tough-
ening could only be achieved by the incorporation of a network of steel
fibers in the composites [11,12].
Several researchers [13–17] reported that for fracture to occur in
CMCs, it is necessary to apply very high loads as the fibers act like a
bridge to redistribute tension and reduce crack propagation, thus in-
creasing the strength of the material.
Stochero et al. [1] studied the effect of incorporating 20 vol% RHS
and 3, 6, and 9 vol% straight steel fibers in kaolin-ceramic matrices. The
use of steel fibers resulted in an increase in the ductility of the ceramics
due to their higher degree of deformation at the point of rupture but
they could not facilitate high loading levels after sample fracture; this is
probably due to the use of low volumetric fractions of short fibers.
According to Khabaz [18], increasing the adhesion efficiency be-
tween fibers and matrix by manipulating fiber parameters, such as the
aspect ratio (l/d), outer roughness, embedded length, and diameter,
might improve the mechanical properties of the produced composites.
It was reported that an increase in the total length of the fiber causes
unacceptable workability; therefore, two different types of fibers
(straight and corrugated) were tested. The results showed that the
corrugated fibers required greater effective stresses for fracture, which
proves that the bond strength between corrugated fibers and matrix is
greater than that between straight fibers and the matrix.
Therefore, CMCs reinforced with corrugated fibers can be used in a
large number of applications owing to their high ductility, toughness, and
strength. However, a critical factor in determining the effectiveness of fibers
in improving the mechanical performance of composites is fiber dispersion,
which describes fiber orientation as well as their location and arrangement
within the ceramic matrix. Applications involving multidirectionally ap-
plied stresses normally employ discontinuous fibers, which are randomly
oriented in the matrix material. However, better overall composite prop-
erties are realized when the fiber distribution is uniform [19].

⁎
Corresponding author.
E-mail address: marcotier@unipampa.edu.br (M.D. Tier).

https://doi.org/10.1016/j.ceramint.2018.05.034
Received 6 March 2018; Received in revised form 3 May 2018; Accepted 5 May 2018
0272-8842/ © 2018 Elsevier Ltd and Techna Group S.r.l. All rights reserved.

Please cite this article as: Santos, P.R., Ceramics International (2018), https://doi.org/10.1016/j.ceramint.2018.05.034
P.R. Santos et al. Ceramics International xxx (xxxx) xxx–xxx

Table 2
Characteristics of the galvanized steel fibers. Source: Astra Fibras
Metálicas.
Characteristic Average

Length (l; mm) 14

Diameter (d; mm) 0.5
Form factor (l/d) 28
Fusion point (°C) 1425–1510
Tensile strength at 870 °C (MPa) 46.9

Table 3
Sample nomenclature.
Mixture Abbreviation

100 vol% KC 100KC

85 vol% KC with 15 vol% RHS 85KC-15RHS
80 vol% KC with 20 vol% RHS 80KC-20RHS
84 vol% KC with 15 vol% RHS and 1 vol% galvanized steel fibers 84KC-15RHS-1F
83 vol% KC with 15 vol% RHS and 2 vol% galvanized steel fibers 83KC-15RHS-2F
Fig. 1. A simplified flowchart describing the fabrication of ceramics reinforced 79 vol% KC with 20 vol% RHS and 1 vol% galvanized steel fibers 79KC-20RHS-1F
with corrugated galvanized steel fibers. 78 vol% KC with 20 vol% RHS and 2 vol% galvanized steel fibers 78KC-20RHS-2F

On the basis of these observations, in this study, RHS and corru-

gated galvanized steel fibers were incorporated in a ceramic matrix.
The fiber orientation was random. Later, the mechanical strength and efficient packing; therefore, RHS contents of 15 and 20 vol% were used
ductility of the fabricated composites were analyzed. in this study.
Sieve analysis was conducted on KC and RHS to determine their
2. Materials and methods particle size distributions. The crystalline structure of RHS was ana-
lyzed using an X-ray diffractometer (XRD; Rigaku, Ultima IV) with Cu
The process for manufacturing CMCs reinforced with corrugated Kα radiation and operating voltage and current of 40 kV and 40 mA,
galvanized steel fibers is illustrated in Fig. 1; the details are described in respectively. The step size was 0.02°, while the incident time was 1 s.
the following sections.
2.2. Test sample manufacture and characterization
2.1. Raw material preparation and characterization
Test samples were manufactured according to the process described
The raw materials used for manufacturing CMCs were kaolin clay by Stochero et al. [1]. The raw materials were homogenized in a la-
(KC; Helager Indústria e Comércio Ltda - Brazil) containing approxi- boratory mixer with a moisture content of 12 wt% and uniaxially
mately 58 wt% SiO2 and 28 wt% Al2O3, RHS (Sílica Verde do Arroz pressed in a male/female mold at 20 MPa to obtain test parts with
Ltda) with 91 wt% SiO2 (as shown in Table 1), and corrugated galva- nominal dimensions of 150 mm × 30 mm × 20 mm. Natural drying
nized steel fibers (Astra Fibras Metálicas - Brazil). was allowed to occur at room temperature for 20 days in order to
Table 2 details the geometrical characteristics of the corrugated prevent accelerated moisture loss, which could create defects and im-
galvanized steel fibers as well as their fusion point and tensile strength. perfections, such as piece cambering. After 20 days, the samples were
Seven different samples were manufactured as summarized in dried in an oven at (105 ± 10) °C for 24 h. Subsequently, the CMCs
Table 3. Two different fiber volumes (1% and 2%) were incorporated in were subjected to a burning process in three steps in an electrical
the mixtures containing 15 or 20 vol% RHS. muffle-type furnace. In the first step, the sample was heated at a rate of
The RHS content was selected on the basis of Sobrosa et al.’s study 5 °C/min to 150 °C and held there for 10 min; in the second step, the
[9]. They reported that an increase in the volume fraction of RHS from temperature was increased to 500 °C at a heating rate of 3 °C/min and
5 vol% to 20 vol% resulted in a better mechanical strength due to more the sample was allowed to equilibrate at this temperature for 10 min; in
the final step, the temperature was increased at a rate of 5 °C/min to
1300 °C and the sample was allowed to equilibrate for 30 min. Subse-
quently, the furnace was turned off and the specimens were left to cool
Table 1
Chemical composition of KC and RHS. Source: Helager Industria e Comércio
down to room temperature naturally.
Ltda/Sílica Verde do Arroz Ltda. To evaluate the physical properties of the samples, porosity and
apparent mass density tests were conducted using a water bath with a
Constituent oxides KC (wt%) RHS (wt%)
digital thermostat and a hydrostatic balance, in accordance with the
SiO2 57.83 91.48 ISO 5017:2015 standard [20].
CaO 0.13 0.36 The mechanical properties of the samples were investigated in terms
MgO 0.36 0.32 of their tensile strength using compressive strength and three-point
Fe2O3 2.25 0.05
bending analyses. Their thermal properties were evaluated by thermal
Al2O3 27.52 ND
Na2O < 0.001 0.04 shock testing. All the measurements were repeated thrice to minimize
K2O 1.87 1.40 experimental errors.
TiO2 0.38 0.003 The compressive strengths of samples with nominal dimensions of
MnO < 0.01 0.32 27 mm × 25 mm × 17.5 mm were measured using an EMIC universal
SO3 – 0.15
testing machine (model DL 20000); the cross-head speed was set at
P2O5 – 0.45
Loss to fire 8.63 3.50 0.2 mm/min according to the ISO 10059–2:2014 standard [21]. The
samples were previously capped with an epoxy glue (Sikadur 32) on

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both sides in order to ensure homogeneous load transfer and to com-

pensate for any surface irregularities.
The flexural strength of test parts with nominal dimensions of
135 mm × 27 mm × 17.5 mm was evaluated by three-point bending
using a Shimadzu testing machine (model AGS-X); the cross-head speed
was set at 0.15 mm/min according to the ISO 5014:2012 standard [22].
Thermal shock resistance tests were performed according to the
NBR 13202:2015 standard [23]. In each cycle, the samples were heated
at 1200 °C for 10 min, after which they were immediately immersed in a
tank of water, where they remained for 5 min. The samples were then
removed from the tank and after 5 min at room temperature, they were
placed back in the furnace for a new cycle. This procedure was per-
formed until the test parts ruptured.
The morphology and microstructure of the fired samples were in-
vestigated by scanning electron microscopy (SEM; model XL 30
Philips).
Fig. 3. XRD pattern of rice-husk silica.
3. Results and discussion

3.1. Particle size distribution

The particle size distributions of kaolin clay and rice-husk silica are
shown in Fig. 2. Note that KC exhibited a smaller particle size (d10 =
0.001 μm < d50 = 0.006 μm < d90 = 0.03 μm) compared to RHS (d10
= 2.5 μm < d50 = 10.7 μm < d90 = 33.5 μm). According to Lam [24],
a combination of two or more particle size distributions may generate
bimodal distributions, i.e., distributions with more than one medium-
sized peak, which favors packing optimization by filling voids.

3.2. X-ray diffraction

Fig. 3 presents the XRD pattern of the as-received RHS. From the
pattern, it can be observed that a crystalline/amorphous phase struc-
ture is present; the halo ring located at 18° < 2θ < 30° is attributed to
amorphous silica and the peaks at 2θ = 21.89° and 36.02° are attrib-
uted to the crystalline cristobalite phase (JCPDS; 01–077-1317); this is
Fig. 4. Apparent bulk densities and porosities of the analyzed mixtures.
most probably related to contamination by the wind-blown sand of RHS
during the fluidization process [25,26].
cm³) of RHS is lower than that of kaolin clay (2.5 g/cm³). The decrease
in porosity is associated with better packing.
3.3. Density and porosity
All the samples containing fibers exhibited an increase in porosity.
According to Stochero et al. [1], this observation can be related to a
Fig. 4 shows the influence of the volume fraction of RHS and cor-
reduction in packing efficiency due to random fiber distribution.
rugated galvanized steel fibers on the apparent bulk density and por-
osity of CMCs. It can be observed that substituting KC with RHS led to a
reduction in density. This is probably because the specific mass (2.03 g/ 3.4. Mechanical and thermal properties

Fig. 5(a) shows the results of compressive strength analysis. It was

observed that the use of RHS induced a slight increase in the me-
chanical strength of the samples, with 0.27% and 1.47% increase re-
ported for 15 vol% and 20 vol% RHS-containing samples, respectively.
Therefore, RHS can be used without any loss of mechanical strength in
kaolin ceramics. This reduces the extraction/consumption of natural
raw materials and adds value to rice-husk ash. Fiber incorporation in
CMCs resulted in a large reduction in the strength due to an increase in
the porosity. However, fracture took place at higher energies as shown
in Fig. 5(b).
Fig. 6(a) presents the tensile strength results obtained by three-point
bending analysis. The average tensile strength changed from 19.5 MPa
in pure KC ceramics to 32.7 MPa in 15 vol% RHS, an increase of 39.5%,
and 33.3 MPa in 20 vol% RHS ceramics, an increase of 41.4%. The
samples 85KC-15RHS and 80KC-20RHS exhibited higher tensile
strengths during bending, which can probably be associated with the
reduction in apparent porosity. However, fracture occurred following a
complete fragile behavior as shown in Fig. 6(b).
Fig. 2. Particle size distribution curves of kaolin clay and rice-husk silica. On the other hand, the specimens with fibers underwent quasi-

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Fig. 5. (a) Compressive strength and (b) displacement versus load curves of different ceramic samples.

Fig. 6. (a) Tensile strength and (b) displacement versus load curves of different ceramic samples analyzed by three-point bending.

Table 4 The thermal shock test results are listed in Table 4. It can be inferred
Results of thermal shock resistance. that the ceramics produced from pure kaolin clay (100KC) and RHS
Mixture Average number Average number Average resistance to
substitution (85KC-15RHS and 80KC-20RHS) ruptured abruptly
of first crack of total break thermal shock without any prior signs of cracking. On the other hand, the ceramics
cycle (A) cycles (B) (r.t.s = A/B) containing 1 or 2 vol% steel fibers exhibited a larger interval between
the first chink and specimen rupture. Ceramics with 2 vol% fibers ex-
100KC 1.0 1.0 1.0
85KC-15RHS 1.0 1.0 1.0
hibited the best performance with respect to thermal shock resistance;
80KC-20RHS 1.0 1.0 1.0 this is especially true in the case of 83KC-15RHS-2F. These results are in
84KC-15RHS-1F 1.7 11.3 0.147 agreement with the compressive (Fig. 5) and tensile test (Fig. 6) results,
83KC-15RHS-2F 2.0 14.7 0.136 which suggested higher fracture energies for samples containing fibers.
79KC-20RHS-1F 1.7 10.3 0.161
It can be observed that rupture occurred at one of the extremities in
78KC-20RHS-2F 2.0 13.7 0.146
fiber-containing specimens, as shown in Fig. 7. According to Stochero
et al. [1], this behavior is related to the higher cooling rate at the edges
than at the center due to the larger area available for heat exchange.
fragile rupture, as shown in Fig. 6(b). The rupture load of 84KC-15RHS-
1F was 665 N with a residual load of about 55 N, while 83KC-15RHS-2F
exhibited a maximum load of 656 N and residual load of 249 N. 3.5. Microstructural analysis
Meanwhile, 79KC-20RHS-1F exhibited a rupture load of 765 N and
residual load of 163 N and 78KC-20RHS-2F was able to bear a max- Fig. 8 presents the SEM images of the specimens after tensile
imum load of 567 N and a residual load of 303 N. Thus, it can be strength testing by three-point bending. These micrographs were used
concluded that upon increasing the fiber content, the fracture energy of to analyze the bonding between fibers and ceramic matrix at the in-
the ceramics increased. terface.
It is worth mentioning that Stochero et al. [1] already reported that The micrographs show that the matrices were embedded with fibers
increasing the content of straight steel fibers from 3 vol% to 9 vol% and indicate the presence of voids (indicated by arrows) at the interface
increased the ductility of kaolin ceramics as the fibers behave like a between the fibers and matrix; these voids possibly contribute to fiber
bridge and redistribute tension. displacement. Furthermore, Fig. 8 suggests that the fibers have enough

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Fig. 7. Typical cases of cracking and rupture of samples: (a) 84KC-15RHS-1F, (b) 79KC-20RHS-1F, (c) 83KC-15RHS-2F, and (d) 78KC-20RHS-2F.
Fig. 8. Scanning electron micrographs of the (a) 83KC-15RHS-2F and (b) 78KC-20RHS-2F ceramics.
adhesion with the matrix to resist pull-out and hence promote stress
distribution.
4. Conclusions
Ceramic matrix composites containing rice-husk silica and corru-
gated galvanized steel fibers were manufactured by uniaxial pressing.
Their properties are suited for different engineering applications,
especially for those requiring a combination of good thermal stability
and mechanical strength.
By varying the process parameters, such as the contents of rice-husk
silica and corrugated galvanized steel fibers, it was possible to control
the microstructure of the produced ceramics and improve their me-
chanical and thermal properties.
The ceramic produced with 20 vol% RHS (80KC-20RHS) exhibited a
high packing density owing to a reduction in porosity; this in turn
slightly increased its mechanical strength.
Ceramic matrix composites with 2 vol% (78KC-20RHS-2F) corru-
gated galvanized steel fibers exhibited the best performance in terms of
mechanical strength due to their high degree of deformation at the
point of rupture; further, their resistance to thermal shock was higher
than that of kaolin ceramics containing 3 vol% straight steel fibers,
which were described in a previous study [1].
Acknowledgments
The authors thank Helager Indústria e Comércio Ltda – Brazil and
Sílica Verde do Arroz Ltda. of the Pilecco Nobre Group – Brazil for
providing the experimental materials. The authors also thank CNPq for
financial support through the Project 482225/2011-4.
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