Applied Surface Science 378 (2016) 8–14

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Applied Surface Science

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

Facile synthesis of silicon carbide-titanium dioxide semiconducting

nanocomposite using pulsed laser ablation technique and its
performance in photovoltaic dye sensitized solar cell and
photocatalytic water purification
M.A. Gondal a,∗ , A.M. Ilyas a , Umair Baig a,b
a
Laser Research Group, Physics Department & Center of Excellence in Nanotechnology, King Fahd University of Petroleum and Minerals, Dhahran 31261,
Saudi Arabia
b
Center of Excellence for Scientific Research Collaboration with MIT, King Fahd University of Petroleum and Minerals, Dhahran 31261, Saudi Arabia

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

Article history: Separation of photo-generated charge carriers (electron and holes) is a major approach to improve the
Received 11 January 2016 photovoltaic and photocatalytic performance of metal oxide semiconductors. For harsh environment like
Received in revised form 12 March 2016 high temperature applications, ceramic like silicon carbide is very prominent. In this work, 10%, 20% and
Accepted 17 March 2016
40% by weight of pre-oxidized silicon carbide was coupled with titanium dioxide (TiO2 ) to form nanocom-
Available online 19 March 2016
posite semiconductor via elegant pulsed laser ablation in liquid technique using second harmonic 532 nm
wavelength of neodymium-doped yttrium aluminium garnet (Nd-YAG) laser. In addition, the effect of
Keywords:
silicon carbide concentration on the performance of silicon carbide-titanium dioxide nanocomposite as
Silicon carbide-titanium dioxide
nanocomposite photo-anode in dye sensitized solar cell and as photocatalyst in photodegradation of methyl orange dye
Dye sensitized solar cells in water was also studied. The result obtained shows that photo-conversion efficiency of the dye sen-
Photo-conversion sitized solar cell was improved from 0.6% to 1.65% and the percentage of methyl orange dye removed
Pulsed laser ablation in liquid was enhanced from 22% to 77% at 24 min under ultraviolet–visible solar spectrum in the nanocompos-
ite with 10% weight of silicon carbide. This remarkable performance enhancement could be due to the
improvement in electron transfer phenomenon by the presence of silicon carbide on titanium dioxide.
© 2016 Elsevier B.V. All rights reserved.

1. Introduction been widely applied in electronic, environmental and optical fields

[2,3]. However, it has certain drawbacks such as its wide band gap
Socio-economic development of any nation is based on ample (3.2 eV that correspond to 388 nm) that makes it to only absorb
supply of clean water and clean energy which are essential for a UV light which is only 4% of the total solar radiations limiting its
good living standard. Global atmospheric pollution caused by gen- ability to efficiently use wide range of solar energy (UV–visible-IR)
eration of energy from burning of fossil fuel is debated a lot due and high recombination rate of photo-generated electron-hole pair
to climate change. Due to these reasons, researchers as well pol- [4]. In order to overcome this problem, TiO2 is doped with metal
icy makers are looking for alternative clean energy sources. In this and non-metal, coupled with other metal oxide semiconductors [5],
context, the use of solar energy conversion devices like dye sensi- carbon based materials [6] and polymeric materials [7] or sensitized
tized solar cells which are cheap, bio-friendly and easy to fabricate with dyes. Silicon carbide (SiC) is a non-oxide high temperature
with no emission are under great consideration. The pollutants like ceramic with a wide band gap (2.0 eV ≤ Eg ≤ 7.0 eV) [8]. It is used for
heavy metals, dyes, surfactants and micro-organisms from indus- devices under harsh environments and possess excellent electrical,
trial waste contaminated water also pose great threat to humanity. mechanical and thermal properties such as toughness, high elas-
The process used for water purification and dye sensitized solar cell, tic modulus, hardness and fracture strength, high resistivity, good
photo-catalyst like TiO2 has become prominent in decades because thermal and chemical stability, low density and thermal expan-
it is cheap, non-toxic, light and chemically stable [1]. Thus, it has sion co-efficient [6]. The following properties have been achieved
by using SiC with metal oxide semiconductors like ZrO2 [9], Al2 O3
[10,11], TiO2 [12] and MgO [13]: brittleness is compensated, sin-
∗ Corresponding author. tering temperature is lowered. In addition, it has also been used
E-mail address: magondal@kfupm.edu.sa (M.A. Gondal). as scattering layer in dye sensitized solar cells to increase optical

http://dx.doi.org/10.1016/j.apsusc.2016.03.135
0169-4332/© 2016 Elsevier B.V. All rights reserved.
 M.A. Gondal et al. / Applied Surface Science 378 (2016) 8–14 9

path [14] and in photocatalytic applications to improve separation

of photo-generated charge carriers [15,16]. Moreover, micro-sized
SiC are used to reinforce ceramics, alloys and metals for tribio-
logical and structural applications. Semiconductor coupling has
been confirmed useful towards obtaining better charge separa-
tion, improved charge carrier lifetime and improved charge transfer
interface [17,18].
In this work, a fast, simple and green optical technique [19]
known as pulsed laser ablation in liquid (PLAL) capable of break-
ing and making bonds is applied in combining the micron sized SiC
with TiO2 nanoparticles to form a SiC–TiO2 nanocomposite. PLAL
has been applied recently in synthesis of semiconductor nanocrys-
tals such as chalcogenides like CdSe [20] and Oxide semiconductors
like TiO2 [21,22], CuO [23,24] and ZnO [25,26] without produc-
ing bi-products and its capability of generating high temperature
and pressure useful in sintering SiC under ambient conditions. Fig 1. XRD pattern of TiO2 , 6H-SiC, T-SiC-10, T-SiC-20 and T-SiC-40.
The synthesized SiC–TiO2 nanocomposites with different percent-
age weight of SiC were applied for photodegradation of methyl
2.3. Photo-catalytic studies
orange (MO) dye and as photo-anode in the dye-sensitized solar
cell. In addition, the effect of SiC concentration on the performance
Photocatalytic activities of synthesized nanocomposite were
nanocomposite is also investigated.
evaluated as follows. The photodegradation of methyl orange (MO)
was conducted under a 500 W Xenon lamp (Oriel, USA). In a typical
2. Experimental photodegradation experiment, a 0.05 g of photocatalyst was mixed
with 100 ml of MO solution. In order to ensure adsorption equi-
2.1. Synthesis of TiO2 -SiC binary nanocomposite librium between the nanocomposite and MO, the suspension was
kept under stirring in the dark for 30 min. The mixture was fur-
The preparation of silicon carbide (SiC) used in this work has ther exposed to UV–vis light. The suspensions were collected and
been reported in our previous work [27]. The SiC was calcined in centrifuged (4000 rpm, 2 min) to remove the photo-catalyst parti-
air at 1200 ◦ C such that SiO2 layer is formed on the surface of the SiC. cles at regular time intervals of 12 min. The degradation of MO was
This was conducted to prevent further oxidation of SiC [28] when determined at 460 nm by UV–vis spectroscopy.
used during the synthesis of the nanocomposite. The nanoparti-
cles (TiO2 and SiC) in powder form were mixed at diffrent mass 2.4. Dye sensitized solar cell fabrication
ratios in deionized water. The mixture was sonicated and placed in
a PLAL setup. The mass of SiC was varied while the mass of TiO2 The nanocomposite solution with a mass concentration of
was kept constant. The obtained composite is denoted as T-SiC-k, 3 g/dm3 was prepared in ethylene glycol. The solution was soni-
where k (k = 10, 20, 40) represents the percentage weight of SiC in cated and then drop casted on an FTO glass substrate placed in an
the nanocomposite.The Nd-YAG laser (532 nm wavelength) applied oven at ∼70 ◦ C. The thin film was further annealed at ∼450 ◦ C for
in the synthesis process was kept at the laser energy = 350 mJ/pulse 30 min. The obtained thin film cooled to ∼100 ◦ C was immersed for
with a laser pulse duration of 6 ns and repetition rate of 10 Hz for 10 min in 0.27 mM of N719 dye prepared in ethanol solution. The
35 min. After the ablation, the resulting colloids were collected and 0.25 cm2 area thin film with dye molecules adsorbed to its surface
dried in oven at 200 ◦ C for 40 min. was bonded with a commercial Pt coated counter electrode. The
internal space of the cell was filled with the I2 based electrolyte
2.2. Characterization (component: CMI, LiI, I2 , TBP, AN).

The crystallization studies of the as-prepared nanocomposite 3. Results and discussion

were carried out using X-ray diffraction (XRD, Bruker advance-D8
diffractometer) with Cu-K␣ radiation. The UV–vis absorption spec- The XRD of SiC, TiO2, and SiC–TiO2 nanocomposite is depicted
tra of synthesized nanocomposite were acquired with Jasco 670 in Fig. 1. The indexed XRD pattern of SiC indicates that it has hexag-
double beam spectrophotometer. FTIR spectra were acquired on a onal phase (6H-SiC) with lattice parameters of a = 0.308 nm and
Nicolet 6700 FT-IR spectrometer (Thermo Electron Corp.) The sam- c = 1.509 nm (JCPDS No. 29-1128) [27,29,30]. Although SiO2 peak
ples were prepared for FTIR studies by mixing 0.5 mg of each of appears at 2␪ = 29.14◦ which is indexed to (040) plane but this
the samples with 98 mg of dry KBr homogeneously to make pel- peak disappears in all the TiO2 -SiC nanocomposite due to its low
lets of 6.95 mm diameter and 0.44 mm thick. The morphology of intensity as compared with SiC and TiO2 peaks. The indexed TiO2
the samples was obtained using Lyra TESCAN Field emission elec- nanoparticle with anatase phase (JCPDS 211272) appears in all the
tron microscope (FE-SEM). FEI Titan 80-300CT TEM instrument was nanocomposites. The presence of SiC improves the crystallinity of
employed to obtain the Transmission electron microscope (TEM) TiO2 due to decrease in the roughness of the nanocomposites XRD
image of the synthesized composite. A potentiostat (PGSTAT302N, pattern. However, in the synthesized TiO2 -SiC nanocomposites, it
Metrohm Autolab B.V., Netherlands) in combination with 500 W was observed that the number of SiC peaks indexed with (101),
Xenon Lamp (Oriel, USA) equipped with 8 mW cm−2 light intensity (103), (110) and (202) planes appears in the nanocomposites. The
was used to obtain the photocurrent-voltage (I–V) curve of the dye intensity of the peaks increases as the concentration of SiC increases
sensitized solar cell with the NOVA software. The electrochemi- in the T-SiC nanocomposites and they became well pronounced in
cal impedance spectroscopy (EIS) measurement was done using the TiO2 -SiC-40 nanocomposite. Also observed is the perfect over-
a potentiostat that scans the DSSC from frequency of 0.05 Hz to lap between the (004) plane of TiO2 and (103) plane of SiC which
50 kHz under Xenon lamp illumination at open circuit voltage and explains there is interaction between the lattice of TiO2 and SiC in
all the measurements were carried out with the NOVA software. the nanocomposites.
10 M.A. Gondal et al. / Applied Surface Science 378 (2016) 8–14

Fig. 3. FTIR spectrum of TiO2 , 6H-SiC, T-SiC-10, T-SiC-20 and T-SiC-40.

of free water which appears in TiO2 and all the synthesized T-SiC
nanocomposite due to presence of SiO2 .
The morphology of 6H-SiC integrated TiO2 is shown in Fig. 4.
The FE-SEM image depicted in Fig. 4(a) appears to be a wool
containing aggregates of particles which are clearly known to be
6H-SiC formed within the crystals of TiO2 . This can be described
as reinforcement of TiO2 NPs with 6H-SiC in surface coupled semi-
Fig. 2. (a) Absorbance spectra. (b) Tauc plot of TiO2 , 6H-SiC, T-SiC-10, T-SiC-20 and conductors of the nanocomposite. In order to confirm the image
T-SiC-40. obtained in FE-SEM image, the TEM image is also depicted in
Fig. 4(b) which also shows the presence of large particles integrated
The absorption spectra and the corresponding Tauc plot of 6H- within populated smaller particles. The larger particles known
SiC, TiO2 NPs and synthesized TiO2 -SiC nanocomposites (T-SiC-10, to be 6H-SiC have a lower concentration than the smaller par-
T-SiC-20 and T-SiC-40) are depicted in Fig. 2(a) and 2(b) respec- ticles known as TiO2 NPs because a low percentage weight of
tively. The SiC has a strong absorption in the deep UV–region at the 6H-SiC (∼10%) is present in the synthesized T-SiC-10 nanocom-
absorption edge of 260 nm with a band gap of ∼3.9 eV. However, the posite. Therefore, a perfect integration of 6H-SiC into the surface of
band gap of 3.17 eV is reported for the SiC in our previous work [27]. TiO2 NPs was well accomplished during the pulsed laser ablation
Therefore the broadened band gap is due to the presence of SiO2 process.
created on the surface of SiC after calcination. The TiO2 nanoparti- XPS analysis was performed to investigate the chemical state
cle has strong absorption at 324 nm with a band gap of ∼3.32 eV. of T-SiC-10 nanocomposite. The high resolution of Ti 2p spec-
The T-SiC-10, T-SiC-20 and T-SiC-40 nanocomposites show absorp- trum demonstrated two peaks at 458.9 eV (Ti 2p3/2 ) and 464.4 eV
tion peak at 322, 320 and 315 nm which correspond to a band gap (Ti 2p1/2 ) which confirms the existence of titanium. The Ti 2p3/2
of 3.4, 3.42 and 3.46 eV respectively. Therefore, compared to TiO2 , shown in Fig. 5(a) was deconvoluted into two peaks at 455.9 eV
there is a blue shift in the absorption peak due to the effect of deep and 458.0 eV which represents TiO [33] and TiO2 [34] respectively.
absorption edge of SiC on absorption peak of TiO2 . The Si 2p spectrum shown in Fig. 5(b) was fitted into three char-
Fig. 3 shows the FTIR spectra of TiO2 , 6H-SiC, and T-SiC acteristic peaks of Silicon state at 101.1 eV, 101.9 eV and 102.8 eV
nanocomposite. At 790 cm−1 is a strong peak which corresponds to which correspond to SiC [35], SiC-O [36] and TiO2 -SiO2 [37] respec-
Si-C bond stretching mode [31]. This stretching mode present in all tively. The O1s peaks shown in Fig. 5(b) was deconvoluted into two
the synthesized T-SiC nanocomposite enhanced the TiO2 stretching gaussian peaks at 529.1 eV and 531.7 eV which are signatures of
mode at this region. The 1104 cm−1 band assigned to the asym- oxygen states in metal oxide (TiO2 and SiO2 ) and carbonates [38].
metric Si-O-Si stretching vibration was also observed for the bond The high-resolution spectrum of C1s spectrum in Fig. 5(d) shows
between the silicon in 6H-SiC and oxygen in TiO2 NPs. Also around three small fraction peaks at 283.4 eV, 285.0 eV and 287.2 eV which
this region is the C H2 bond within SiCH2 wagging mode because are associated with carbide (SiC) [39], C C and C with O bond [38].
1104 cm−1 is broadened in all the synthesized T-SiC nanocomposite This explains that, a small percentage of SiO2 and SiC O was incor-
(T-SiC-10, T-SiC-20 and T-SiC-40). The presence of the 1380 cm−1 porated in the nanocomposite and there is exchange of elements
peak correspond to Ti-O-Ti bond in TiO2 [32] is observed in the between 6H-SiC and TiO2 during the ablation process.
T-SiC-10 nanocomposite, but absent in such as T-SiC-20 and T-
SiC-10 nanocomposite. This is because the quantity of 6H-SiC in 3.1. Photovoltaic performance of SiC–TiO2 nanocomposites
the T-SiC-10 nanocomposite is very small, less than 12%, for TiO2
bond to appear and become dominant. The band that appear at The current density–voltage (I–V) curves of TiO2 and synthe-
1633 cm−1 was assigned to the bending vibration of the O H bond sized TiO2 -SiC nanocomposite are as shown in Fig. 6. Table 1
of chemisorbed water during laser ablation and the broadband summarized photovoltaic parameters obtained from the DSSCs
around 3377 cm−1 was due to the stretching mode of the O H bond such as the Open circuit voltage (Voc), Short circuit current den-
 M.A. Gondal et al. / Applied Surface Science 378 (2016) 8–14 11

Fig. 4. (a) FE-SEM image and (b) TEM of T-SiC-10 nanocomposite.

Fig. 5. XPS spectral analysis of T-SiC nanocomposite showing deconvoluted peaks in the high resolution of the elements present (Ti, Si, O and C).

Table 1
Parameters of the DSSCs with TiO2 , T-SiC-10, T-SiC-20 and T-SiC-40.

JSC (mA/cm2 ) Voc (V) FF (%) ␩ (%) Rct (k)

TiO2 0.852 0.1787 0.2932 0.56 0.46

T-SiC-10 0.844 0.3951 0.3969 1.65 0.18
T-SiC-20 1.232 0.2949 0.2748 1.25 0.29
T-SiC-40 0.444 0.0884 0.2355 0.12 0.47
12 M.A. Gondal et al. / Applied Surface Science 378 (2016) 8–14

Fig. 6. J–V curve of TiO2 , 6H-SiC, T-SiC-10, T-SiC-20 and T-SiC-40 based DSSC.

Fig. 8. Photo-degradation of MO (a) T-SiC-10, T-SiC-20 and T-SiC-40, (b) TiO2 , 6H-SiC
and T-SiC-10.

T-SiC-10, T-SiC-20, and T-SiC-40 are 463 , 181.6 , 292.3  and

Fig. 7. Nyquist plot of TiO2 , 6H-SiC, T-SiC-10, T-SiC-20 and T-SiC-40 based DSSC.
465  respectively as listed in Table 1. Hence, the Rct values reduce
the concentration of 6H-SiC reduces from 40 wt.% to 10 wt.%. This
sity (Jsc), Fill factor and Photoconversion efficiency. It was observed indicates that a faster recombination occurs in T-SiC-40 nanocom-
that the Voc of the nanocomposite reduces as the quantity of 6H- posite due to the fact that electron gets retarded when oxidation
SiC increases. The Jsc of the T-SiC-10 is equal to that of TiO2 as resistance is too high due to the presence of high quantity of 6H-SiC.
the quantity of 6H-SiC is very small (<12%) in the matrix of the The charge transfer resistance changes accordingly with VOC values
nanocomposite and the T-SiC-20 shows a higher Jsc. This might and the efficiency of the DSSC. Hence, The T-SiC-40 shows the low-
be because the quantity of 6H-SiC is high enough to improve the est efficiency of 0.12% and T-SiC-10 shows the highest efficiency of
pore size of TiO2 . T-SiC-40 nanocomposite shows a relatively very 1.65% which is more than that of TiO2 because
low Voc and Jsc as compared to TiO2 . This might be because the
percentage of 6H-SiC is too high therefore reducing electron drift (i) The 6H-SiC introduced into TiO2 matrix has excellent oxidation
from the valence band to conduction band in the nanocompos- and corrosion resistance [40,41]. However, when the concen-
ite. The efficiency increases gradually from 0.55% to 1.65% when tration of 6H-SiC is too high it can cause electron retardation
10 wt% of SiC was introduced into TiO2 and then decreases to 0.12% in TiO2 matrix which is the case of T-SiC-40 showing low per-
when 40 wt% of SiC was present. The T-SiC-40 shows the lowest formance.
efficiency of 0.12%. This means excessive SiC has led to decreased (ii) 6H-SiC in micron size is used as a starting material. Therefore,
Jsc, Voc, and the efficiency. This can be attributed to increase after pulsed laser ablation, 6H-SiC in the nanocomposite has
in recombination of photogenerated electron and holes at the T- reduced in size that enhances its catalytic activity [42–46].
SiC/dye/electrolyte interfaces. To further investigate the charge (iii) The TiO2 nanoparticles are reinforced by SiC in the nanocom-
recombination process, electrochemical impedance spectroscopic posite matrix [47].
(EIS) measurements were conducted under constant illumination
under a bias of their relative open circuit voltage. Fig. 7 presents the 3.2. Photocatalytic performance of SiC–TiO2 nanocomposites
Nyquist plots and the corresponding simplified equivalent circuit
for the DSSCs, respectively. The diameters of the large semicircles The photocatalytic performance of SiC–TiO2 composites via
observed in the Nyquist plot can be used to measure the charge methyl orange photodegradation experiments under UV–vis light
transfer resistance (Rct) in TiO2 and all the TiO2 -SiC nanocomposite. irradiation. Before photo-irradiation, the samples are kept in the
Since TiO2 and all the T-SiC nanocomposite have the same interface solution for 30 min so that adsorption equilibrium can be reached.
with the counter electrode/electrolyte in the DSSC, therefore, all The photocatalytic activity of the composite catalyst is shown in
other resistance observed that can be observed remain the same. Fig. 8(a). Stability of MO dye was confirmed when the MO dye
The Rct values from the photoelectrode synthesized from TiO2 , is exposed to the solar irradiation without a catalyst. The T-SiC-
 M.A. Gondal et al. / Applied Surface Science 378 (2016) 8–14 13

nanocomposites. The synthesized silicon carbide-titanium dioxide

nanocomposites with different percentage weight of silicon car-
bide were applied for removal of methyl orange dye from water
and as a photo-anode in the dye-sensitized solar cell (DSSC). The
impregnation of silicon carbide into titanium dioxide enhanced
the performance of titanium dioxide in dye-sensitized solar cell
by a factor of 3 and in removal of methyl orange dye by 3.5. This
enhancement could be due to better conduction of electrons by
presence of silicon carbide in titanium dioxide and thus reduction
in recombination of electron hole pair. In addition, the effect of sil-
icon carbide concentration on the performance of nanocomposite
was also investigated.

Acknowledgements

The authors would like to thank Laser Research Group (LRG),

Physics Department, King Fahd University of Petroleum and Min-
erals (KFUPM), Saudi Arabia for the financial support through the
project # RG 1311-1. Authors are also thankful to Mr. T.A. Fasasi for
technical help during the experiment.

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