Results in Physics 14 (2019) 102390

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Results in Physics
journal homepage: www.elsevier.com/locate/rinp

Experimental studies of TiO2 nanoparticles synthesized by sol-gel and T

solvothermal routes for DSSCs application
⁎
R.S. Dubeya, , Katta Venkata Krishnamurthyb, Shyam Singhc
a
Advanced Research Laboratory for Nanomaterials and Devices, Department of Nanotechnology, Swarnandhra College of Engineering and Technology, Seetharampuram,
Narsapur, A.P., India
b
Department of Chemistry, S.M.B.T.A.V. & S.N. Degree College, Veeravasaram, A.P., India
c
Department of Physics, University of Namibia, Windhoek, Namibia

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

Keywords: This paper presents the synthesis and characterization of TiO2 nanoparticles prepared by the sol–gel (SG) and
TiO2 nanoparticles solvothermal (ST) methods. The crystallinity and phase identification examined by the X-ray diffraction (XRD)
Sol-gel method evidenced the pure-anatase TiO2 nanocrystals without any impurities. The scanning electron microscopy (SEM)
Solvothermal method analysis showed the preparation of spherical-shape TiO2 nanoparticles while energy-dispersive X-ray spectro-
Dye-sensitized solar cells
scopy (EDS) study endorsed the elemental compositions of Ti and O. Transmission electron microscopy (TEM)
Cell efficiency
investigation evidenced the mesoporous microspheres of TiO2 nanoparticles with their average size 119 nm. By
UV–vis spectroscopy study, the optical band gaps were estimated to be 2.9 and 3.2 eV corresponding to the
samples SG and ST. Furthermore, both SG and ST samples were employed as the photoanode materials for the
dye-sensitized solar cells (DSSCs) however, ST based DSSC endorsed the enhanced photovoltaic performance.

Introduction properties of the nanoparticles. As the precipitates derived by the sol-

gel process is amorphous in nature therefore, calcination at adequate
Titanium dioxide (TiO2) is the most demanded photoanode material temperature is required in order to attain the crystallinity of the sample.
in dye-sensitized solar cells (DSSCs) including its potential applications Furthermore, calcination at a higher temperature may promote the
in water treatment, pigments, self-cleaning surfaces, biosensors, che- phase transformation due to agglomeration of the particles and the
mical sensors, biodiesel production and so on [1–7]. The main attrac- growth on the grain boundaries.
tion of TiO2 is its non-toxicity, easy handling, and inexpensive pro- The anatase and rutile crystalline phases of TiO2 are mainly de-
duction. In spite of several synthesis methods, the sol-gel and manded for the industrial applications as compared to other phases
solvothermal processes are the easiest ways to synthesize TiO2 nano- such as brookite and the TiO2 (B) monoclinic. The energy band gap
particles with their tailor-ability to attain the required optical and values of the anatase and rutile crystalline phases are 3.2 and 3.0 eV
physical properties. The solvothermal synthesis method is ideal for the respectively. As the anatase-TiO2 has its high electrons mobility
preparation of nanomaterials and has the controllability to prepare the therefore, it is employed as the photoanode material in dye-sensitized
various forms of the nanostructures i.e. nanoparticles/nanorods/nano- solar cells (DSSCs). The choice of the anatase-TiO2 evidenced the rea-
tubes etc. The process parameters to attain these kinds of nanos- sonable enhancement in the cell efficiency [8]. Furthermore, the mixed
tructures are the reaction temperature, reaction time, autoclave pres- phases of the anatase-rutile have also been employed in the DSSCs [9].
sure and the solvent type. Further, the particles morphology and The rutile phase nanoparticles can be prepared by the thermal treat-
crystallinity can also be tailored with the chemical composition, solu- ment at higher temperature beyond 400 °C [10]. Ahn et al. investigated
tion pH and the aging time. This method produces the fine particles the photovoltaic performance of the dye-sensitized solar cells by em-
with their unique physical properties as compared to other chemical ploying the photoanodes based on multiwalled carbon nanotubes em-
routes. An analogy to solvothermal synthesis, the sol-gel method is easy bedded with TiO2 nanowires prepared via electrospinning and the
due to its low-temperature and pressure process. Depending upon the calcination process. The composition of 5 wt% of the multiwalled
chemistry of the precursor and synthesis conditions, this method pro- carbon nanotubes with TiO2 nanowires was reported the enhanced cell
vides the flexibility to tune the compositional and microstructural efficiency due to the enhanced electron-transfer mechanism with the

⁎
Corresponding author.
E-mail address: rag_pcw@yahoo.co.in (R.S. Dubey).

https://doi.org/10.1016/j.rinp.2019.102390
Received 20 April 2019; Received in revised form 26 May 2019; Accepted 26 May 2019
Available online 31 May 2019
2211-3797/ © 2019 The Authors. Published by Elsevier B.V. This is an open access article under the CC BY-NC-ND license
(http://creativecommons.org/licenses/BY-NC-ND/4.0/).
R.S. Dubey, et al. Results in Physics 14 (2019) 102390

reduced charge recombination [11]. Liu et al. manipulated the position as sample ‘ST’.
of the scattering (S) layer in the DSSCs and investigated the photo-
voltaic performance. The scattering layer of rutile-TiO2 nanoparticles Fabrication of dye-sensitized solar cells
with its thickness 5 μm was placed on the FTO plate followed by double
layers of anatase-TiO2 (T) films of thicknesses 5 μm each (STT), in-be- The prepared nanoparticles samples, SG and ST were used to pre-
tween the two TiO2 films (TST) and after the preparation of double pare TiO2 pastes by following a few simple steps. First, 0.15 g TiO2
layer of anatase-TiO2 films (TTS). In this investigation, the scattering particles were mixed in 0.25 ml ethanol followed by adding 0.25 ml
layer placed on TiO2 (STT configuration) showed the weak usage of the acetic acid and 0.25 ml of PVP. The solution was mixed in a mortar till
incident light but improved the electron collection efficiency. However, the preparation of TiO2 slurry. The fluorine-doped TiO2 (FTO) glasses
TTS configuration was supported to a strong incident light harvesting were cut in the size 1 cm2 then ultrasonically cleaned in ethanol and
but reduced the electron collection efficiency. Further, the application acetone simultaneously for 15 min. Further, by doctor blade method,
of scattering layer in-between two transparent TiO2 films (TTS config- the TiO2 pastes were rolled-on to prepare the photoanodes. The effec-
uration) showed the better electron collection efficiency with 7 % cell tive active area of the DSSCs was 0.25 cm2. After coating TiO2 pastes on
efficiency [12]. Tong et al. synthesized the mesoporous microspheres of FTO glasses, these were dried on hot-plate for 15 min at temperature
anatase-TiO2 by the hydrolysis of titanium butoxide in butanol. The 60 °C and finally kept for sintering in the muffle furnace at temperature
synthesized TiO2 microspheres diameter was 0.5 μm with the nano- 500 °C for 30 min. Later, the photoanodes were washed in ethanol and
particles size about 10 nm. By hydrothermal process, the aggregated soaked in the dye solution for 12 h. After soaking photoanodes in dye,
TiO2 particles with their random shapes were obtained. The crystal- these were washed in ethanol and deionized water. For the counter
linity of TiO2 particles was found to be good with the pre- and post- electrode, the platinum paste was rolled on the FTO glasses using doctor
calcination treatment. The solar cell efficiency using the photoanode blade method. Finally, the solar cells were assembled while the elec-
based on the aggregated TiO2 nanoparticles was better than the TiO2 trolyte was injected in between the photoanode and the counter elec-
sphere based photoanode [13]. Metal-doped TiO2 nanoparticles showed trode.
the great improvement in the DSSCs performance Sakthivel et al. de-
monstrated the synthesis of silver-doped TiO2 nanoparticles by che- Characterization of TiO2 nanoparticles and DSSCs performance
mical reduction process. The prepared nanoparticles of anatase-rutile
crystalline phases showed the improved light absorption in the visible The prepared nanoparticles (SG and ST) were characterized for the
region with a red-shift of its absorption edge and as much as 1.55 % cell investigations of their phase and crystallinity using X-ray Diffraction
efficiency was obtained [14]. (D8 Advance Bruker AXS, Germany), the optical measurements using
This paper presents the synthesis and characterization of TiO2 na- UV–Visible Spectrophotometer (UV 1800, Shimadzu, Japan), the sur-
noparticles prepared by the sol-gel and solvothermal methods. Using face morphology measurements using Scanning Electron Microscopy
the prepared nanoparticles, DSSC’s photoanodes are prepared and (Leica Cambridge 440 Microscope, UK) and Transmission Electron
photovoltaic performance is evaluated. The detailed procedure of na- Microscope (Tecnai G2 20 Twin FEI, Netherlands). The performance of
noparticles synthesis and the DSSC fabrication are presented in Section the DSSCs was investigated by using Sun Simulator attached assembled
“Experimental”. The various properties of the synthesized particles and with a power source (Keithley 2420) and LED light source with an il-
the photovoltaic performances of DSSCs have been discussed in Section lumination of 80 mW/cm2.
“Results and Discussion”. Finally, Section “Conclusions” concludes the
paper. Results and discussion

Experimental XRD investigations were done to examine the crystal structure and
phase constitution of the prepared powder samples. Fig. 1 shows the
Chemicals XRD patterns of SG and ST samples recorded in 2θ range of 20–80°.
Fig. 1(a) and (b) exhibits the pure-anatase phases with the dominant
Titanium isopropoxide (TTIP, Ti[OCH(CH3)2]4) with purity 97 % peaks at 25° and 48° without the presence of any impurities. The
(Sigma-Aldrich) was preferred as the titanium precursor. Acetic acid
glacial (CH3COOH) was used as the catalyst supplied by SDFine.
Ethanol with purity 99.99 % and de-ionized water were used as the
solvents. All the chemicals were used without any further purification.
For the DSSCs fabrication, Ruthenizer 535-bis TBA, Iodolyte HI-30, and
Plastisol T were procured from Solaronix.

Syntheses of TiO2 nanoparticles

For the comparative study, we have synthesized the TiO2 nano-

particles by the sol–gel (SG) and solvothermal (ST) methods. For the
sol-gel process, 150 ml ethanol was mixed with 10 ml deionized water
under constant stirring. Further, 9 ml TTIP was mixed in the above
solution under constant stirring while maintaining the temperature at
85 °C using paraffin oil bath upto 4 h. After forming the gel, it was dried
in the hot-air oven at temperature 60 °C. The calcination was performed
for 3 h at 400 °C and the prepared sample was named as ‘SG’. With the
same above chemical compositions, another solution was prepared for
the solvothermal process which was transferred into teflon lined auto-
clave followed by the hydrolysis process. The autoclave was placed in
the hot-air oven for 2 h at temperature 200 °C. Later, the sample was
collected from the autoclave and washed with ethanol. Finally, after
drying at 80 °C for 1 h the collected particles were grinded and named Fig. 1. X-ray diffraction patterns of powder samples SG (fig. a) and ST (fig. b).

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R.S. Dubey, et al. Results in Physics 14 (2019) 102390

diffraction peaks were found to be consistent with the reflections of diffraction (SEAD) image shown in Fig. 4(d) endorses the polycrystal-
anatase phase and are indexed in accordance with File No. 96-152-6932 line nature of the pure-anatase TiO2 nanoparticles.
using Match software. The indexed planes endorse the pure tetragonal Fig. 4 depicts the morphology of ST sample prepared by the sol-
anatase phase of TiO2 with the octahedral and trigonal planar co- vothermal process. The agglomeration of TiO2 nanoparticles can be
ordination geometry. observed in Fig. 4(a) whereas the closer observation reveals the for-
Based on the dominant diffractions peaks corresponding to the mation of microspheres as shown in Fig. 4(b). Fig. 4(c) confirms the
(1 0 1) plane as shown in Fig. 1(a) and (b) the crystallite sizes were mesoporous microspheres made-up of TiO2 nanoparticles. The nano-
estimated by using Scherrer’s formula which is represented as, particles are in spherical shape with their average size 13.4 nm. These
d = kλ /βcosθ where β is the full-width at half-maximum of the dif- nanoparticles are arranged in the microsphere form with the average
fraction peaks, λ is the X-ray wavelength (nm) and θ is the diffraction size 119 nm. The microsphere morphology investigated by TEM coin-
angle. The estimated crystallite sizes were found to be 13 and 11 nm cides with the SEM analysis as shown in Fig. 2(b). The concentric rings
corresponding to the SG and ST samples respectively. Furthermore, the in SAED pattern as shown in Fig. 2(d) confirms the polycrystalline
diffraction peaks were found to be slightly wider for the sample ST nature of TiO2 nanoparticles. The morphology of the nanomaterials
which evidenced the smaller crystallite size as compared to the SG strongly depends on the solvothermal process conditions. Comparing
sample. Our XRD results coincide with the work reported on the with the sol-gel technique, the solvothermal method yields not only a
synthesis of catalyst particles derived by the sol-gel and solvothermal large surface area of the nanomaterials but also a high crystallinity. By
approaches. Comparatively, the broader diffraction peaks corre- comparing the morphologies of both the samples, we can observe the
sponding to the solvothermal derived sample was attributed to the mesoporous structure in the sample ST while the agglomerated nano-
presence of the smaller crystallite size. In other words, the sample particles in the SG sample. A similar trend was reported by Wanna-
prepared by the sol-gel method evidenced the sharp X-ray diffraction borworn et al. in a comparative study of solvothermal and sol-gel-de-
peaks corresponding to a larger crystallite size [15]. Accordingly, we rived nanocrystalline catalysts. The nanoparticles prepared by the
can observe the variation in the crystallite sizes in the order SG > ST solvothermal method exhibited the porous structure with a slight ag-
that is 13 nm > 11 nm. glomeration as compared to more agglomerated and irregular shape
Fig. 2 depicts the scanning electron microscopy (SEM) images of the particles prepared by the sol-gel method [15]. Wu et al. adopted the sol-
synthesized TiO2 nanoparticles. The SG sample shows the agglomera- hydrothermal approach for the synthesis of titania nanoparticles and
tion of the nanoparticles as shown in Fig. 2(a). reported the non-agglomerated and uniform morphology of the anatase
The similar trend of agglomeration of spherical particles can also be TiO2. Furthermore, in the presence of various acid solvents like HCl,
observed in the SEM image of the sample ST as depicted in Fig. 2(b). For HNO3, HAc and H2SO4 the rutile titania was also synthesized [16]. Wei
both the samples, EDS spectra were recorded and shown in Fig. 2 (right et al. synthesized the crystalline mesoporous anatase-TiO2 nano-
side along the SEM images). The presence of the elemental composi- particles by the solvothermal method. This kind of morphology was
tions of Ti and O peaks were endorsed in both the samples. associated with the use of CTAB as the surfactant which was helpful for
Fig. 3 illustrates the TEM images of the SG sample prepared by sol- the reduced agglomeration and the size of the nanoparticles with an
gel process. We can observe the homogeneous distribution of the increased surface area [17].
spherical-shape TiO2 nanoparticles from lower resolution to a higher The optical absorption of the prepared samples was studied by
resolution as depicted in Fig. 3(a)–(c). The average size of the particles UV–Vis measurement as depicted in Fig. 5. Usually, the position of the
was observed to be 13 nm which coincides with the crystallite size absorption edge (i.e. blue-/red-shift) corresponds to the particles size.
calculated by the Scherrer’s formula. The selected area electron Using Tauc relation, the estimated optical band gaps were found to be

Fig. 2. SEM images and EDS spectra of samples SG (fig. a) and ST (fig. b).

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R.S. Dubey, et al. Results in Physics 14 (2019) 102390

Fig. 3. TEM micrographs of sample SG at resolution 200 nm (fig. a), 100 nm (fig. b), 50 nm (fig. c) and SAED pattern (fig. d).

2.9 and 3.2 eV corresponding to the samples SG and ST as shown in the This enhancement in efficiency can be attributed to the mesoporous
inset of Fig. 5(a) and (b) respectively. The increase in crystallite size microspheres of TiO2 nanoparticles which could yield the larger surface
yields low band gap value as it is noticed for the sample SG as compared area for the dye adsorption. The obtained photovoltaic parameters are
to ST. summarized in Table 1.
Typically, the measurement of the current density in accordance the DSSC based on TiO2 nanoparticles prepared by the solvothermal
applied voltage under light illumination yields the solar efficiency. For method endorses the enhanced cell efficiency due to the formation of
the solar cell characteristics, the short-circuit ( Jsc ), the open circuit mesoporous TiO2 spheres as evidenced in the TEM micrographs shown
voltage (Voc ) and the fill factor (FF ) are the main parameters. The short- in Fig. 4(b). The mesoporous morphology of the particles is more fa-
circuit ( Jsc ) is the current when the net voltage is zero while the open vorable in DSSCs as it possesses lower contact resistance among the
circuit voltage (Voc ) is the voltage when net the current is zero. The fill TiO2 nanoparticles therefore, responsible for the enhanced cell effi-
factor (FF ) is the representation of the squareness of the curve asso- ciency.
ciated with the resistance in the solar cell. The fill factor equation is
expressed as FF = Pmax / Jsc × Voc which is affected by the parasitic re- Conclusions
sistances. Depending upon the high or low magnitude of the voltages,
the series or shunt resistances fluctuate. These analyses can be extracted In this work, synthesis and characterization of TiO2 nanoparticles
from the I-V curve under the dark condition. Under dark condition, the using sol-gel and solvothermal methods have been carried out. XRD
solar cell shows the ideal-diode characteristics while fluctuation re- analyses showed the presence of pure-anatase TiO2 with their crystallite
sembles the leakage current. Using SG and ST samples, two slurries sizes 13 and 11 nm corresponding to the samples SG and ST. SEM
were prepared to fabricate the dye-sensitized solar cells which are measurementconfirmed the spherical-shape nanoparticles while the
named as SC-SG and SC-ST. Fig. 6 depicts the current density-voltage sample SG was found agglomerated. TEM investigation evidenced the
characteristics of the prepared DSSCs. From Fig. 6(a), we can observe mesoporous TiO2 microspheres in the sample ST while EDS study en-
the photovoltaic performance of the SC-SG which shows its efficiency dorsed the elemental peaks of Ti and O. The optical band gap of the
1.57 %, open circuit voltage 0.62 V, short-circuit current 3.9 mA/cm2 sample SG was noticed to be lower than the ST which coincides with the
and 0.5 fill factor. increased crystallite size. Furthermore, dye-sensitized solar cell based
As compared to SC-SG device, SC-ST shows the upward-shift of the on ST sample evidenced the better performance with its cell efficiency
short-circuit current density as shown in Fig. 6(b) and accordingly, the 2.17 % and short-circuit current density 3.9 mA/cm2. This improvement
enhanced cell efficiency can be observed. The obtained SC-ST’s para- could be attributed to the mesoporous morphology prepared by the
metrical values were found to be 2.17 % efficiency, 0.64 V open-circuit solvothermal approach. Further, performance can be improved by fol-
voltage, 3.9 mA/cm2 short-circuit current density and 0.7 fill factor. lowing the standard method of DSSC’s photoanode preparation.

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R.S. Dubey, et al. Results in Physics 14 (2019) 102390

Fig. 4. TEM micrographs of sample ST at resolution 200 nm (fig. a), enlarged image (fig. b), 50 nm (fig. c) and SAED pattern (fig. d).

Fig. 5. UV–vis absorption of TiO2 samples SG (fig.a) and ST (fig.b) with inset images of Tauc plots.

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R.S. Dubey, et al. Results in Physics 14 (2019) 102390

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