Materials Science & Engineering A 659 (2016) 158164

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Materials Science & Engineering A

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

Fabrication and characterization of laminated SiC composites

reinforced with graphene nanoplatelets
Karolina Pereira dos Santos Tonello n, Elisa Padovano, Claudio Badini, Sara Biamino,
Matteo Pavese, Paolo Fino
Politecnico di Torino, Dipartimento di Scienza Applicata e Tecnologia, Corso Duca degli Abruzzi 24, 10129 Torino, Italy

art ic l e i nf o

a b s t r a c t

Article history:
Received 20 November 2015
Received in revised form
16 February 2016
Accepted 16 February 2016
Available online 17 February 2016

Nanosized allotropes of carbon have been attracting a lot of attention recently, but despite the steady
growth of the number of scientic works on materials based on graphene family, there is still much to be
explored. These two-dimensional carbon materials, such as graphene nanoplatelets, multilayer graphene
or few layer graphene have emerged as a possible second phase for reinforcing ceramics, resulting in
remarkable properties of these composites. Typically, graphene ceramic matrix composites are prepared
by a colloidal or a powder route followed by pressure assisted sintering. Recently other traditional
ceramic processes, such as tape casting, were also successfully studied. The aim of this research is to
fabricate -SiC multi-layer composites containing 2, 4 and 8 vol% of graphene nanoplatelets (GNP) by
tape casting and study the effect of these additions on the mechanical behavior of the composites. In
order to achieve this purpose, samples were pressureless sintered and tested for density and mechanical
properties. The elastic modulus was measured by the impulse excitation of vibration method, the
hardness by Vickers indentation and fracture toughness using micro Vickers indentation and by threepoint bending applying the pre-cracked beam approach. Results showed that up to 4 vol%, the density
and mechanical properties were directly proportional to the amount of GNP added but showed a dramatic decrease for 8 vol% of GNP. Composites with 4 vol% of GNP had a 23% increment elastic modulus,
while the fracture toughness had a 34% increment compared to SiC tapes fabricated under the same
conditions. Higher amounts of GNP induces porosity in the samples, thus decreasing the mechanical
properties. This study, therefore, indicates that 4% is an optimal amount of GNP and suggests that excessive amounts of GNP are rather detrimental to the mechanical properties of silicon carbide ceramic
materials prepared by tape casting.
& 2016 Elsevier B.V. All rights reserved.

Keywords:
SiC
Graphene nanoplatelets
Composites
Tape casting

1. Introduction
Silicon carbide is one of the most used carbides, being applied
to a wide range of industrial applications for example, aerospace,
abrasive, electronics, wear resistance parts as ceramic seals and
bearings, and most recently for fuel cladding in nuclear ssion
reactors [14]. Its highly covalent bond between C and Si provides
excellent thermal and good mechanical properties at high temperature, good oxidation and thermal shock resistance [5,6] and is
the reason behind the use of silicon carbide in most of these applications. Despite these properties, the demand for superior
mechanical properties continues to grow. A classical solution to
this requirement is the development of ceramic composites [7],
but nowadays a multilevel approach is desirable [810], in order to
n

Corresponding author.
E-mail address: karolina.pereira@polito.it (K. Pereira dos Santos Tonello).

http://dx.doi.org/10.1016/j.msea.2016.02.050
0921-5093/& 2016 Elsevier B.V. All rights reserved.

take maximum advantage of the more efcient toughening mechanisms operating at different length scales. This is the case of
multilayer composites and biomimetic ceramics based on complex
architectures [11,12].
Nanometric carbon based materials have been successfully
applied as reinforcement phase for ceramics, one example being
carbon nanotubes [1,13,14]. More recently, graphene and other
two-dimensional carbon materials, such as graphene oxide (GO),
multilayer graphene (MLG), and graphene platelets (GPL) and
nanoplatelets (GNP), appeared as possible reinforcement phases
due to their excellent mechanical [15], thermal [16,17], and electric
[18] properties and are attracting widespread interest [1820].
Early works on graphene ceramic matrix composites have disclosed materials with outstanding properties [21], Ramires et al.
[22] obtained a 135% increase in fracture toughness for Si3N4
composites containing 4.3 vol% of rGO (reduced graphene oxide).
In the same way Walker et al. [23] reached 235% increase in
fracture toughness using 1.5 vol% of GPL in a Si3N4 matrix. Other

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159

examples of GCMC are equally impressive, such as the results

obtained by Nieto et al. [24] with sintering improving grain size
reduction and causing a 99% increase in fracture toughness of TaC
composites with only 5 vol% GNP. As well as the results obtained
by Porwal et al. [25] with 40% of fracture toughness increase with
the addition of 0.8 vol% of graphene in Si3N4. In all those cases the
toughening mechanisms of advanced composites are enhanced by
mechanisms typically associated with graphene related materials
(GNP, FLG, r-GO), such as, sheet bending and sheet sliding, which
ensures part of the properties improvement [21,23,26]. Despite
this perspective, there is a strong evidence of the limit for graphene additions, corresponding to the point where the mechanical
properties start to be negatively affected by the formation of an
interconnected graphene network [21,23,24,26], which must be
further studied.
Tape casting is one possible colloidal shaping technique for
these new composites, it allows the fabrication of relatively complex shapes and multilayer materials with a high up-scaling potential [2,27]. In order to reinforce these advantages the pressureless sintering is an attractive path, but until this moment few
researchers have focused on this technique, one reason is because
of the high temperature required for the sintering of covalent
ceramics, which could damage the graphene inclusions. [20,22
24,27] More work is needed on pressureless sintering of GCMC to
better understand the associated mechanisms and potential applications of this new composites class [23].
The purpose of this work is to develop and study SiC composites reinforced with GNP, produced by tape casting. In order to
achieve this purpose, the effect of increasing addition of GNP on
SiC matrix was studied. Starting with tape casting process and the
GNP dispersion. Then, the study of the densication and mechanical properties of laminated samples is discussed, together
with the GNP effect on these properties.

2. Experimental procedure
2.1. Composites production
A synthesis of processing and characterization steps can be
found in Fig. 1.
The starting materials used in this research were: Commercial
-SiC powder UF-15 (H.C. Starck) with reported average particle
size of d50 0.55 mm, used as ceramic matrix. Commercially
available graphene nanoplatelets (GNP) grade 3 (Cheap tubes)
with an average thickness of 8 nm (corresponding to 45 layers),
lateral size of 2 mm and reported surface area of 500700 m2/g,
according to the information provided by the manufacturer, was
used as reinforcement phase, Fig. 2. As sintering aid, it was chose
to add amorphous boron grade I (H.C. Starck) and graphite akes
(Alfa Aesar), with akes 710 mm wide.
The process started with the GNP dispersion in a double solvent system, composed of 39.4 wt% of ethanol (Fluka Analytical)
and 60.6 wt% butanol (Sigma-Aldrich), used as the tape casting
solvent. For the dispersion it was used an ultrasonic probe (Sonics
Vibra-cell), with 20 kHz frequency and sonication time of 15, 30,
45 and 60 min. The concentration of GNP in the solvent mixture
was 0.04 g ml  1 and polyvinyl butyral (PVB) resin B76 (Butvar)
was tested as a dispersant with 1:4 ratio with respect to GNP.
During sonication the suspension was cooled by a owing water
bath to avoid excessive heating and solvent evaporation.
Ceramic slurries were prepared by mixing the already dispersed GNP dispersion with SiC powder and menhaden sh oil
(MFO), selected as dispersant. To ensure a proper powder dispersion 12 h ball milling was performed. The next step was the addition of PVB, as a binder, and triethyleneglycol ester Bisoex 102

Fig. 1. Flow chart of composites production.

(PEG), as plasticizer. Ball milling was performed for further 24 h

[2,3]. After this process, the solid loading was 49% for all samples.
Composites were prepared with SiC, 1 wt% of boron as a sintering aid and an amount of GNP ranging from 2 vol% (SB2), 4 vol%
(SB4), and 8 vol% (SB8). A SiC composition without GNP, containing
1 wt% of B and 3 wt% of graphite akes as sintering aids was
processed for comparison (SBC) [2,3].
After homogenization, the slurries were degassed to remove air
bubbles. Tape casting was performed on a double blade tape
casting equipment, with a gap height of 1 mm at a speed of
100 mm/min over a Mylars lm. Tapes were left to dry naturally
and their quality was studied by visual examination, being considered suitable those ones with intact and smooth surfaces.
Samples were cut into rectangles of 50  60 mm, layers were glued
together with a mixture of PVA, ethanol, and water (1:10:10) and
left to dry for 12 h under a constant pressure, thereafter samples
were then cut into 12  50 mm bars. To completely remove the
polymers a burn-off step was carried out at 800 C in argon atmosphere. Samples were then pressureless sintered at 2200 C
with a 30 min isotherm, under argon atmosphere.

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P S 106 3(a/W )1/2

KIpb = g max 03/2

BW
2(1a/W )3/2

(1)

Where g is function of the ratio a/W for the three-point exure,

Pmax is the maximum load, S0 is the span, B is the sample width, W
the thickness and a is the crack length.
Microhardness tests were performed on the polished cross
section of the samples, with an applied load of 9.8 N and 15 s
holding time. Vickers hardness tester with 98 N load was used for
fracture toughness estimation by indentation method, on a, this
load was chosen because it generated sufciently long cracks for
reliable measurement. The KIC-IF was calculated using Anstis
equation [31].
1

E 2
P
KIC =0. 16 . 3

H
C0 2

(2)

Where E is the elastic modulus obtained by impulse excitation

method, H is the Vickers hardness, P is the applied load and C0
stands for radial crack length.
Microstructure characterization of green tapes, fracture surfaces and polished surfaces was realized using a eld emission
scanning electron microscope (FESEM) ZEISS (model Merlin 4248) with an operating voltage of 5 kV.

3. Results and discussion

3.1. Processing conditions

Fig. 2. (a) SEM micrograph and (b) Raman spectrum of as received GNP grade 3.

2.2. Characterization
The green density of the tapes was measured by geometrical
method. After sintering the bulk density was measured using Archimedes method with water as immersion media, according with
C373-88 (2006) ASTM standard test method [28]. Theoretical
densities were calculated based on the amount of SiC and GNP in
each composition using a volumetric mixture rule, considering the
densities of SiC as 3.21 g/cm3 and GNP as 2.20 g/cm3.
Rectangular samples with 42  4  3 mm size were used for the
elastic modulus determination, measured by the impulse excitation of vibration method using a grindosonic (model MK-5), the
tests were realized on samples suspended on nylon bers and the
modulus was calculated according with the equation proposed
ASTM e 1876-09 [29].
Three-point bending tests were used to measure exural
strength and fracture toughness. Tests were carried out using a
40 mm span and a crosshead speed of 0,1 mm/min on a computer
controlled universal testing machine Zwick/Roell (model SINTECH
10D) with a 1kN load cell.
Fracture toughness (KIpb) was measured using the pre-cracked
beam approach and calculated using Eq. (1). Samples were previously polished and Vickers indentation, performed with 98 N
load, was placed in the center of the bar, on the bottom surface, in
accordance with the recommendations found on ASTM C1421-10
[30].

The stability of the graphene dispersion plays an important role

in tape casting processing. The long milling cycles that followed
the ultrasonic step allowed shorter stabilization time. Preliminary
tests on GNP suspensions realized without dispersant reveals that
the mixture of ethanol and butanol have a poor GNP dispersibility
[32]. Adding PVB promotes the short-term stabilization of the
suspension, probably because of a steric impediment of the GNP. In
all cases, the amount of dispersed particles was proportional to the
sonication time. Based on that result the tape casting was performed using PVB as a previous dispersant and 45 mins sonication,
according with the procedure described in materials and methods.
3.2. Density and microstructure
Green samples were analyzed in order to observe the structure
and detect GNP. Fig. 3 presents the top surface of SiC with 4 vol%

Fig. 3. SEM images of a tape with 4 vol% GNP after polymer removal, with the
detail of GNP sheets.

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161

Fig. 4. Relative density as a function of GNP content.

GNP showing homogeneously distributed pores, compatible with

the green density, which was calculated from 55 to 60% of theoretical density. The insert in Fig. 3 presents a magnication
showing platelets with few graphene layers, with a small
transparency.
The bulk density of the sintered samples as a function of the
GNP quantity is displayed in Fig. 4. The SBC sample had over 97% of
theoretical density with the addition of B and C akes as sintering
aids. As the concentration of GNP increases, there is a gradual
decrease in bulk density, reaching its lowest value for SB8G
composite.
The presence of a native SiO2 lm on the particles reduces the
driving force for sintering the addition of reducing additives, such
as B, C or B4C is essential for solid state sintering of SiC. The effect
of boron and carbon as sintering aids was exhaustively studied,
[3335]. As the previous studies shown, the role of boron is to
increase the lattice or grain boundary diffusion coefcient [5,35],
in some studies it is also suggested that this effect helps to activate
densication mechanisms on later sintering stages [33,36]. However, the only addition of B is not enough to reach a fully dense SiC
by pressureless sintering. This sintering aid must be combined
with a more active phase, in this case it was used carbon. The
carbon role is to reduce the SiO2 lm formed on the SiC surface,
according to the Eq. (3).

SiO2 + C = SiC +2CO

(3)

As proposed by Clegg et al. [35] this reaction happens at lower

temperatures, before the reaction between SiC and SiO2 occurs,
and thus the formation of an interconnected pore channel, making
it critical to remove this oxide layer before the densication mechanism start. The carbon that did not react with SiO2 lm tends to
form localized inclusions on grain boundary which, in later sintering stages may hinders the densication by pinning mechanisms [33,35]. In this work the carbon needed as a sintering aid was
calculated in order to reduce the estimated 1.5 wt% O2 on SiC
surface, and for SBC the used value was 3 wt% [2,3,34,35]. X-ray
diffraction spectra, Fig. 5(a), were collected from sintered samples
ground in a vibratory mill. The identied crystalline phases were
SiC 6H, SiC 4H and graphite 2H, which is the graphite polytype
formed by hexagonal structured carbon layers, like graphene,
stacked in an ABAB sequence. To verify the presence of GNP after
the sintering process and to measure the integrity of nanoplatelets, a Raman spectrum was measured in the polished cross section of samples, Fig. 5(b).
The ID/IG ratio was near 0.42 for samples SB2G and SB4G, while
for the sample SB8G this value was 0.46. This result is indicative

Fig. 5. (a) XRD patterns of sintered composites, (b) Raman Spectrum of SiC-GNP
composites with D, G and 2D peaks of graphene.

that the colloidal process combined with the sintering temperature induced defects on the GNP, without a direct correlation with
the concentration added.
On the other part of the spectrum, the peaks near 2500 cm  1,
indicated a presence of graphite like structures which means that
cavitation and shear forces during the ultrasonication and the
milling cycles were insufcient to exfoliate the GNP.
3.3. Mechanical properties
The density and mechanical properties of composites are
summarized in Table 1. Elastic modulus was calculated with Reuss
model for all composites, considering 415 GPa as the value for pure
SiC [6] and 1 TPa for the value of graphene [37]. The theoretical
values obtained were respectively 419.9 GPa, 424.9 GPa, and
430.1 GPa. This increase on the elastic modulus was observed up to
4 vol% GNP content.
Although a SB2G sample elastic modulus was only 5% higher
compared to SBC sample SB4G had a 22% increase. Instead, the
composite SB8G showed a 13% decrease. This behavior was clearly
due to higher porosity, which in this case induced pore interconnection, largely overtaking the benets of GNP addition, Fig. 6.
On the other hand, micro hardness values of composites decreased on SB8G composites this drop indicated a behavior associated with the excessive GNP amount and consequently sample
porosity. During the micro hardness tests the contact zone

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Table 1
Density and mechanical properties of composites.
Sample

Relative
Density (%)

E
(GPa)

HV
(GPa)

s
(MPa)

KIc IF
(MPa m1/2)

Kisc
(MPa m1/2)

SBC
SB2G
SB4G
SB8G

98.9 7 1.1
96.9 7 0.3
97.8 7 0.4
89.2 7 3.7

345.3 7 11.9
362.9 7 6.2
424.37 23.8
210.4 7 23.5

25.1 74.7
24.472.9
25.6 72.4
18.3 74.0

285.4 7 30.1
288.8 7 36.3
317.0 7 30.3
297.7 7 30.2

2.9 7 0.5
2.4 7 0.3
3.17 1.1
2.5 7 0.6

4.2 7 1.3
5.17 1.9
6.6 7 0.9
6.9 7 1.3

Fig. 6. Elastic modulus of SiC/GNP composites as a function of porosity.

Fig. 7. SEM image of indentation on a SiC with 4 vol% GNP composite.

probably generates shear stress along GNP layers and on the interface between SiC grains and GNP, thus promoting deformation
due to sliding under indentation area [31].
Fracture toughness was measured using two distinct methods,
with Vickers indentation fracture (VIF) and pre-cracked bean on
exure test (PB). Values calculated using VIF were similar to what
is described in literature for monolithic SiC, approximately
3.0 MPa m1/2 [6], without an evident improvement in fracture
toughness associated to the reinforcement, Fig. 7.
At this point, it is important to emphasize that despite being an
easy method the indentation fracture probably it is not the most
accurate for this kind of composite. In this study, it must be because the effect of multilayer architecture was neglected during
the test and because the already discussed difculties of hardness
measure, here magnied by the higher load used for fracture test.
However, crack deviation mechanisms were observed on the
Vickers indentation, Fig. 7. Superior fracture toughness values
were observed when using the pre cracked bean method. The
introduction of weak interfaces provided by the multilayer

Fig. 8. SEM image of fracture surface sample (a) SB8G, with aligned GNP (b) GNP
mechanical solicitation; (c) SB4G with GNP on grain boundary.

K. Pereira dos Santos Tonello et al. / Materials Science & Engineering A 659 (2016) 158164

Fig. 9. Load/displacement curves of SiC/GNP composites.

architecture was one of the factors for this improvement, observed

in all samples.
During the current study the fracture toughness was over 50%
superior in all composites, these results are an evidence of GNP
toughening mechanisms Fig. 8.
As proposed in previous studies the toughening of graphene
ceramic composites must be due to the monolayer high strength,
that hinders crack propagation and forces crack deviation on the
interface [38].
Additionally, for a multilayer graphene material the interaction
of graphene layers changes fracture mechanisms [39] and the
weak interface between layer and matrix also introduces a path for
crack propagation. In this work the interface porosity and GNP pull
out were observed, Fig. 8(a) and (b).
The load-displacement curves are shown on Fig. 9. In this
curves it was observed the typical fracture behavior of multilayered materials, in composites SB2G and SB4G. The step-by-step
fracture enhances the reliability of laminated ceramics by dispersing fracture energy and avoid catastrophically breakage of the
samples. During this study, the interlayer glue made prior to debinding was not completely effective for composites SBC and
SB8G, which had a linear fracture behavior. Although this behavior,
the calculated work of fracture indicates that the main toughening
mechanisms were due to the GNP mechanisms and parallel
alignment to tape casting ow.
In the studied composites, there is the evidence that the GNP
network was detrimental for densication process and consequently for some of the mechanical properties of samples, in
special the elastic modulus, hardness. A limit of 4 vol% addition on
SiC composites seems to be the optimal amount to promote at the
same time good density and improved exural strength and
fracture toughness using the colloidal processing route followed
by tape casting.

4. Conclusions
In conclusion, a simple route to produce SiC tapes with graphene nanoplatelets was developed. The use of an ultrasonic
probe to disperse the GNP before the ball milling process was effective in promoting a well-dispersed second phase on the SiC
matrix, but it was ineffective for further exfoliation. The sintering
temperature used during these tests was not detrimental to the
GNP. The results obtained by the Raman and the XRD analysis of
the sintered samples showed no signicant degradation of the
second phase.

163

The density results provided evidence that the sintering process was directly affected by the amount of GNP. Samples containing up to 4 vol% of GNP showed more than 96% of theoretical
density, but above this concentration, the amount of GNP formed
an interconnected network which hinders the densication, as
veried on the sample SB8G. Consequently, the increased amount
of GNP also led to a reduction in the elastic modulus, hardness,
and bending strength of the sample.
To conclude, the observed improvement in fracture toughness
can be associated with GNP orientation and the modied fracture
toughening mechanisms. Typical of a multilayered graphene. The
results of this study suggests that the multilayered graphene is the
most suitable graphene-based materials to improve ceramic
toughness.
Additionally, in the present study SiC with 4 vol% of GNP seems
the be the most suitable composite for structural applications. The
combination of a higher elastic modulus (424.3 GPa) and improved
fracture toughness (6.6 MPa m) makes this composite a potential
candidate for extreme applications, for example thermal protection system for space vehicles.

Acknowledgement
K.P.S. Tonello thanks to CAPES - Programa Cincias sem Fronteiras (Brazil) for the concession of a fellowship for post-doctoral
research, process number 111-99-13.

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