Journal of Photochemistry and Photobiology 6 (2021) 100016

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Journal of Photochemistry and Photobiology

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Electrospun composite nanofibers prepared by varying concentrations of

TiO2 /ZnO solutions for photocatalytic applications
M.V. Someswararao a, R.S. Dubey b,∗, P.S.V. Subbarao c
a
Department of Physics, SRKR Engineering College, Bhimavaram, A.P., India
b
Department of Nanotechnology, Swarnandhra College of Engineering and Technology, Seetharamapuram, Narsapur, A.P., India
c
School Department of Physics, Andhra University, Visakhapatnam, A.P., India

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

Keywords: We present the electrospinning preparation and investigation of metal oxides TiO2 (T), ZnO (Z) and TiO2 /ZnO
TiO2 /ZnO nanofibers (TZ) composite nanofibers. For the fabrication of TZ composite nanofibers, different proportions of TiO2 /ZnO
Electrospinning process solutions (1:1, 1:2, 2:1 and 1:3) are preferred. X-ray diffraction (XRD) pattern of sample ‘T’ exhibited the mixed
X-ray diffraction
anatase and rutile phases while the wurtzite phase is examined in the sample ‘Z’. The field-emission scanning
Surface morphology
electron microscopy (FESEM) study evidenced the preparation of continuous and randomly oriented nanofibers
whereas the transmission electron microscopy (TEM) investigation endorsed the cylindrical morphology of the
TZ13-sample with mean diameter of 230 nm. The lattice d-spacing is estimated to be 0.289 nm corresponding to
the plane (100) of the hexagonal wurtzite ZnO while selected-area electron diffraction (SAED) analysis endorsed
the polycrystalline nature of the TZ13 composite nanofibers. Finally, photodegradation of the Eriochrome black
T dye was performed and the catalyst TZ13 showed about 85% photodegradation in 90 min as compared to
TZ11, TZ12 and TZ21. This boosted photocatalytic activity is ascribed to the synergetic effect of the TiO2 /ZnO
composite nanofibers with their distinct morphology.

1. Introduction
Titanium oxide (TiO2 ) and zinc oxide (ZnO) is the equally demanded
materials in several applications, for instance, batteries, sensors, photo-
catalytic/water splitting, dye-sensitized solar cells, antimicrobials etc.
[1-7]. TiO2 is abundant in nature, nontoxic, and easy to handle. The
anatase and rutile polymorphs of TiO2 are the well-recognized ones due
to their better stability as compared to their other forms. The anatase
and rutile TiO2 phases have 3.2 eV and 3.0 eV optical band gaps, respec-
tively. On the other hand, the ZnO material possesses better electrical
properties and investigated as the alternate choice in place of TiO2 due
to its almost similar band gap (3.37 eV) with its wurtzite hexagonal
phase structure. Therefore, both TiO2 and ZnO got demanded as the
photocatalysts [8-10]. Further, the composite semiconductor TiO2 /ZnO
materials are promising for the application of photodegradation owing
to the speed-up process of charge separation under the irradiation of
light. Therefore, TiO2 /ZnO hybrid nanomaterials in the form of parti-
cles, films, fibers etc. have been well-recognized for the photodegrada-
tion studies [11-14].
The fast, economic, and well-known approach for the preparation of
nanofibers based on mono, composite, or core-shell materials is an elec-
trospinning technique. Pei et al. reported the photodegradation study
∗
Corresponding author.
E-mail address: rag_pcw@yahoo.co.in (R.S. Dubey).
using electrospun TiO2 /ZnO nanofibers as the catalyst by tuning the
anatase/rutile ratio via calcination process at various temperatures.
Upon calcination at temperature 650 °C, the nanofibers sample con-
sisted of 48/52% of anatase/rutile crystallites and demonstrated the
better photodegradation of rhodamine B dye [15]. Yar et al. presented
the photodegradation study using catalysts based on electrospun poly-
acrylonitrile nanofibers decorated with TiO2 , ZnO, and TiO2 /ZnO com-
posite nanoparticles. The degradation of malachite green dye was per-
formed however, the hybrid nanofibers of TiO2 /ZnO/PAN evidenced the
photocatalytic activity two times greater than the bare PAN nanofibers
[16]. Baek et al. fabricated and investigated the various properties
of electrospun ZnO nanofibers. The choice of calcination temperature
showed a significant impact on the ZnO structure and endorsed the
improved morphology by increasing the diameter of the nanofibers at
higher calcination temperature [17]. Li et al. reported a recyclable ex-
periment of photodegradation study of electrospun TiO2 /ZnO compos-
ite nanofibers. They found improved photodegradation efficiency along
with the stability of the catalyst [18]. Araujo et al. demonstrated the
photodegradation study of rhodamine B dye using catalyst TiO2 /ZnO
hierarchical hetero nanostructures of nanorods prepared on electrospun
nanofibers. The morphological study revealed the three-dimensional ar-
rangement of ZnO nanorods on TiO2 nanoporous structure. These pre-
pared nanostructures demonstrated as the efficient photocatalyst, which
showed about 90% photodegradation of the dye within the 70 min
[19]. By varying the zinc acetate concentration, various composite fibers

https://doi.org/10.1016/j.jpap.2021.100016
Received 10 November 2020; Received in revised form 4 December 2020; Accepted 11 January 2021
Available online 18 January 2021
2666-4690/© 2021 The Author(s). 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/)
M.V. Someswararao, R.S. Dubey and P.S.V. Subbarao
Fig. 1. XRD patterns and FESEM images of TiO2 (T) and ZnO (Z) nanofibers.
were fabricated and characterized. Pei et al. explored the preparation
of TiO2 /ZnO nanofibers to study the photocatalytic activity. An opti-
mal quantity of the catalyst showed the increased photocatalytic re-
sponse of the composite fibers; as a result, enhanced-dye degradation
was noticed under visible light irradiation [20]. Liu et al. prepared
the core/shell (ZnO/TiO2 ) nanofibers for the photocatalytic applica-
tion. X-ray diffraction study exhibited the anatase and rutile phases
of TiO2 while the hexagonal wurtzite phase was noticed correspond-
ing to the ZnO. Comparatively, the core/shell (ZnO/TiO2 ) nanofibers
showed the red-shift regardless of the activation energy required for the
individual ZnO and TiO2 nanofibers. As a result, ZnO/TiO2 core-shell
nanofibers evidenced the enhanced photocatalytic activity along with
their recyclability [21]. To study the photocatalytic activity, Li et al.
presented a distinct experimental process for the preparation of het-
erojunction ZnO/TiO2 composite fibers. The approach was zinc plat-
ing on the electrospun TiO2 nanofibers and then heat treatment. As
a result of these processes, the photocatalytic activity of ZnO/TiO2
nanofibers was found reasonably better than the pure-TiO2 nanofibers
[22]. Kanjwal et al. reported the photocatalytic activity of hydrother-
mally treated electrospun ZnO/TiO2 nanofibers. The photocatalytic ac-
tivity of ZnO nanoparticles prepared by hydrothermal process, electro-
2
Journal of Photochemistry and Photobiology 6 (2021) 100016
spun TiO2 , ZnO/TiO2 composite nanofibers, and the hydrothermally
treated electrospun ZnO/TiO2 composite nanofibers were investigated
and compared. The hydrothermally treated ZnO/TiO2 nanofibers were
found to be more efficient, which could degrade the methyl red and rho-
damine B dyes within 90 and 105 min, respectively, as compared to 3 h
degradation time taken by the other three catalysts [23]. Liu et al. stud-
ied the TiO2 /ZnO composite nanofibers calcined at various tempera-
tures. Further, to improve the photocatalytic property, ZnO was blended
in TiO2 /ZnO composite nanofibers. As a result, the photodegradation of
rhodamine B and phenol were noticed to be 100 and 85%, respectively,
with the 15.76 wt% of ZnO content for the enhanced photocatalytic
response [24]. Park et al. explored the structural and electrical prop-
erties of the electrospun ZnO nanofibers. They reported the annealing
temperature as a significant factor for the improved crystallinity of ZnO
nanofibers. The electrical conductivity of ZnO nanofibers was observed
to be inversely proportional to the calcination temperature [25].
In this work, we present the study of TiO2 /ZnO composite nanofibers
prepared by varying the proportional ratios of TiO2 /ZnO solutions. No
similar study by varying the solution concentration has been reported
to the best of our knowledge. Further, we have performed the pho-
todegradation of the Eriochrome black T dye. The preparation of solu-
M.V. Someswararao, R.S. Dubey and P.S.V. Subbarao
Fig. 2. Surface morphology of TZ11 and TZ12 nanofibers.
tions and electrospinning process of nanofibers production is presented
in Section 2. The characterized results are discussed in Section 3. Finally,
Section 4 concludes the work.
2. Experimental approach
Titanium Tetraisopropoxide (TTIP, Sigma-Aldrich) and Zinc Ac-
etate Dehydrate (Zn(CH3COO)2•2HO, Merck) were used as the Ti and
Zn precursors respectively. Catalyst: Acetic Acid (Sdfine), polymer:
Polyvinyl Pyrolidone (PVP, Mw=1,300,000, Sigma-Aldrich) and the sol-
vent: Methanol (Fisher Scientific) were used. For the photodegradation
study, the Eriochrome Black T (EBT) dye was used.
For the preparation of TiO2 solution, 0.6 ml TTIP, 10 ml methanol
and 4 ml glacial acetic acid were mixed and stirred for 30 min. Later,
0.8 g PVP was added in the above solution under vigorous stirring which
was continued till the preparation of the transparent and enough viscous
solution. To obtain the ZnO solution, 1.2 g zinc acetate dehydrate was
dissolved in 10 ml methanol, followed by adding 4 ml acetic acid under
stirring. Later, 0.8 g PVP was added to the ZnO solution and stirred for
1 h to get enough viscous solution. After preparing both the solutions,
composite solutions of TiO2 and ZnO were prepared in the proportional
ratios 1:1, 1:2, 2:1, and 1:3. For all the electrospinning experiments,
the parameters like dc voltage, solution flow rate and the tip-collector
distance were 14 kV, 1 ml/h and 10 cm respectively. After preparation,
each sample was calcined at 600 °C for 1 h and named as TZ11, TZ12,
TZ21 and TZ13 corresponding to the 1:1, 1:2, 2:1 and 1:3 proportional
ratio of TiO2 :ZnO solutions.
The calcined nanofibers were characterized to investigate the phase
and crystallinity using X-ray Diffraction (XRD, Bruker AXS D8 Ad-
vance, Germany), the UV-vis absorbance using UV-Visible Spectropho-
tometer (UV 1800, Shimadzu, Japan), the surface morphology using
3
Journal of Photochemistry and Photobiology 6 (2021) 100016
Field-emission Scanning Electron Microscopy (FESEM, ZEISS, Germany)
and Transmission Electron Microscope (TEM, Tecnai G2 20 Twin FEI,
Netherlands).
The photocatalytic activities of electrospun nanofibers were per-
formed by evaluating the photodegradation of Eriochrome Black T (EBT)
dye under ultraviolet (UV) irradiation. The laboratory developed pho-
tocatalysis setup was consisting of four UV lamps assembled facing
each other from all the sides in a wood cabinet. Two exhaust fans
were arranged on the opposite sides to maintain the ambient temper-
ature in the cabinet due to the excessive heat generated by the UV
lamps. For the photodegradation studies, 0.1 g of respective electrospun
nanofibers/catalysts were mixed in EBT dye, and sonicated for 20 min.
Later, the prepared solutions were kept under UV irradiation for various
intervals of times and then UV–Vis absorbance was recorded.
3. Results and discussion
X-ray diffraction (XRD) study was performed to examine the phase
and crystallinity of TiO2 (T) and ZnO (Z) nanofibers as depicted in
Fig. 1(a). The XRD pattern of the T-sample shows the presence of two
crystallographic forms that are anatase (A) and rutile (R) indicating
the polycrystalline nature. The anatase peaks originated at Bragg angle
2Ɵ=25.2°, 36.9°, 37.8°, 48°, 53.8°, 55°, 62.1° and 68.7° were assigned
to the planes (101), (103), (004), (200), (105), (213) and (116) respec-
tively.
Similarly, the rutile peaks originated at 2Ɵ=27.4°, 41.2°, 44°, and
54.3° were assigned to the planes (110), (111), (210) (211) respectively.
The anatase and rutile peaks were found in good matching with the
JCPDS File No. 21–1272 and JCPDS File No. 21–1276, respectively. The
XRD pattern of Z-sample endorses the characteristic diffraction peaks of
ZnO crystallite originated at 2Ɵ=31.7°, 34.4°, 36.2°, 47.5°, 56.6°, 62.8°
M.V. Someswararao, R.S. Dubey and P.S.V. Subbarao
Fig. 3. Surface morphology of TZ21 and TZ13 nanofibers.
and 67.9° corresponding to the planes (100), (002), (101), (102), (110),
(103) and (112). The XRD pattern indicates the formation of the hexag-
onal wurtzite crystalline phase and coincides with the JCPDS File No.
36–1451. No other peaks were noticed in both the samples T, and Z
which endorsing the absence of impurities.
The morphology of the TiO2 and ZnO nanofibers were investigated
by FESEM, as shown in Figs. 1(b) and 2(c). The prepared nanofibers
of TiO2 and ZnO were found randomly aligned. Comparatively, TiO2
nanofibers possess a smoother surface than the ZnO nanofibers. Using
ImageJ tool, the mean diameter of the T and Z samples were observed
to be 169 nm and 209 nm respectively.
Fig. 2(a) and (b) depicts the FESEM images of composite TiO2 /ZnO
nanofibers (TZ11) prepared with the proportional ratio 1:1 of TiO2 :ZnO
solutions. Here, we can observe the preparation of smooth and aligned
nanofibers, as depicted in Fig. 2(a). A large scale FESEM image is
depicted in Fig. 2(b), which shows the well-aligned nanofibers along
with spherical nanoparticles in the sample TZ11. Comparatively, TZ12
nanofibers were noticed to be thinner and non-uniform as depicted in
Fig. 2(c). However, Fig. 2(d) endorses the presence of TiO2 and ZnO
nanoparticles arranged in a random direction. The diameters of TZ11
and TZ12 fibers were found to be in the range from 194 nm–379 nm
and 115 nm–240 nm, respectively. However, the average particle size
was estimated to be 11 nm and 11.3 nm corresponding to the fiber sam-
ples TZ11 and TZ12. Here, the double proportion of ZnO solution re-
sulted in the rough morphology of the fibers with randomly arranged
nanoparticles in the fiber form as referring to Fig. 2(b) and (d). With
the increased ZnO solution i.e. T:Z = 1:2 proportional ratio, we have
noticed rough nanofibers as depicted in Fig. 2(c) and (d).
Inversely with the sample TZ21, we can notice the preparation of
smoother nanofibers when the proportion of TiO2 solution was double
than the ZnO i.e. T:Z = 2:1 as shown in Fig. 3(a). A closer look at TZ21
4
Journal of Photochemistry and Photobiology 6 (2021) 100016
fiber morphology depicted in Fig. 3(b) endorses the compact packing of
the spherical nanoparticles. The diameter of TZ21 and TZ13 fibers and
nanoparticles were found to be in the range from 155 nm–284 nm and
332 nm–428 nm and 11 nm and 9.8 nm, respectively. As depicted in
Fig. 3(c), a distinct morphology of TZ13 nanofibers was noticed for the
case of proportional ratio, T:Z = 1:3. With a similar trend, as discussed
in Fig. 2(c), we can observe the formation of rough and well-aligned
nanofibers. It means the roughness of the fibers is enhanced with the
increased concentration of ZnO solution. However, the well packing of
the TiO2 and ZnO nanoparticles with a little porosity is observed in the
FESEM image, as shown in Fig. 3(d).
With the interest of distinct morphology observed in the TZ13 sam-
ple, we have performed the transmission electron microscopy (TEM)
measurement. Fig. 4(a) shows the cylindrical morphology of TZ13
nanofibers with a somewhat rough surface, as noticed in Fig. 3(c). As
compared to TZ11, TZ12, and TZ21 composite nanofibers, the diam-
eter of TZ13 sample is found to be increased in the range 184 nm–
464 nm with the increased proportion of ZnO solution as discussed in
Figs. 2 and 3. TEM result coincides with the FESEM observation and
the reported work [25]. As depicted in Fig. 4(b), the mean diameter
of the nanofiber is found to be around 230 nm, which is made-up of
grain-like nanocrystals of TiO2 and ZnO. Fig. 4(c) depicts the high-
resolution TEM (HR-TEM) image of TZ13 nanofibers while the d-space
imaging is shown in the inset of Fig. 4(c). The lattice d-spacing is found
to be 0.289 nm, which corresponds to the (100) plane of the hexag-
onal wurtzite ZnO structure as discussed later. The selected area elec-
tron diffraction (SAED) image shown in Fig. 4(d) endorses the polycrys-
talline nature of composite TZ13 nanofibers. To verify the crystallinity
of composite TZ13 nanofibers, XRD study was performed but not shown
here. The anatase TiO2 peaks was observed at 2Ɵ=25.2 o , 40.4 o , 48 o ,
and 53.8° along with the wurtzite ZnO peaks at 2Ɵ=31.7 o , 34.4 o , 36.2
M.V. Someswararao, R.S. Dubey and P.S.V. Subbarao
Fig. 4. TEM micrographs of TZ13 nanofibers with scale bar 500 nm (a) and 50 nm (b), HR-TEM with scale bar 5 nm (c) and SAED pattern (d).
o, 47.5 o , 56.6 o , 62.8 o , and 67.9 o . A peak at 2Ɵ=22.5° was also ob-
served, which might be associated with the polymer residual [26]. We
can recall that the XRD pattern of T-sample endorsed the mixed crys-
talline phases of the anatase and rutile, as shown in Fig. 1(a). How-
ever, in the XRD pattern of TZ13-sample only anatase phase of TiO2
and wurtzite ZnO peaks were noticed. More ZnO peaks in the XRD pat-
tern can be regarded as the increased ZnO concentration as compared
to TiO2 .
Depending on the ZnO concentration, the dominant peaks may vary,
as reported in the literature [25]. Therefore, the d-spacing obtained by
HR-TEM investigation represents the ZnO plane (100) of the hexagonal
wurtzite polycrystalline phase.
Using TZ11, TZ12, TZ21, and TZ13 composite fibers as the cata-
lysts, we have studied the photodegradation of the Eriochrome black
T (EBT) dye in aqueous under UV irradiation. Figs. 5(a), (b) and (c)
depicts the UV–Vis absorbance recorded after UV irradiation time of
30 min, 60 min and 90 min respectively. The appearance of two broad
absorption bands at wavelength 344 nm and 530 nm can be observed
which were associated with the ultraviolet and visible light absorp-
tion of the typical EBT dye. We can notice the reduced absorption
5
Journal of Photochemistry and Photobiology 6 (2021) 100016
with the increased UV irradiation time. Further, the samples TZ11,
TZ12 and TZ13 endorsed the dominant effect with the increased ZnO
concentration among the samples T and Z. However, the prominent
decrease in absorption is noticeable for the TZ13 sample under irra-
diation time of 30 min, 60 min and 90 min as compared to other
samples.
We have estimated the percentage of dye-degradation by using the
simple expression,% Degradation=(Ao -At )/Ao )∗ 100, where Ao is the ab-
sorbance at time t = 0 min and At is the absorbance after irradiation
time t (here, 30 min, 60 min, and 90 min). The value of Ao was recorded
by considering the maximum wavelengths corresponding to the UV and
Vis absorption bands.
Fig. 6 depicts the photodegradation percentage of EBT dye as a func-
tion of irradiation time by using the various catalyst samples of T, Z,
TZ11, TZ21, TZ11, TZ12, and TZ13.
The highest degradation percentage was observed for the compos-
ite nanofiber sample TZ13 of about 85.07% and 85.32% corresponding
to the ultraviolet and visible bands. As compared to ultraviolet band
absorption, we can notice the prominent decreased absorption in the
visible range. This improved photocatalytic activity is ascribed to the
M.V. Someswararao, R.S. Dubey and P.S.V. Subbarao
Fig. 5. UV–Vis absorbance of electrospun nanofibers after irradiation time of
30 min (a), 60 min (b) and 90 min (c).
Fig. 7. Photodegradation mechanism using electrospun nanofibers.
6
Journal of Photochemistry and Photobiology 6 (2021) 100016
Fig. 6. EBT dye-degradation of electrospun nanofibers as a function of irradia-
tion time.
synergetic effect of TiO2 /ZnO composite nanofibers having their dis-
tinct morphology.
Fig. 7 depicts the photodegradation mechanism of electrospun
nanofibers. After irradiating the UV light, the photoexcited electrons
get migrated from the conduction band of ZnO to the conduction band
of TiO2 . Simultaneously, the valence band holes of TiO2 get migrated
to the valance band of ZnO. With this process, the charge carriers, i.e.
electrons and holes, get separated and therefore, it boosted-ups the life-
time. Further, due to the reduction process, the electrons produce O2 .
from the O2 where the holes participate in the oxidation process which
yields the HO. from H2 O. As a result of the photoexcited separation of
electrons and holes, O2 .- radicals and holes get produced which felici-
tates in the enhancement of photodegradation mechanism.
Finally, we can notice that the O2.-, HO., and holes are the key fac-
tors in the photodegradation process of EBT dye. Under UV illumination,
M.V. Someswararao, R.S. Dubey and P.S.V. Subbarao
the semiconductor metal-oxides like TiO2 , ZnO etc. produce oxidized hy-
droxyl and oxy radicals due to the generation of the electron-hole pairs
and decomposes the organic materials.
4. Conclusions
Various metal oxides nanofibers fabricated and studied for their
structural and morphological properties. XRD pattern of pure-TiO2
showed the mixed anatase and rutile phases while the hexagonal
wurtzite phase examined in the pure-ZnO sample. Morphology studied
by FESEM evidenced the smooth, long, and randomly aligned nanofibers
in all the samples. However, a distinct morphology of TZ13 nanofibers
is attributed to the increased proportion of ZnO solution (T:Z = 1:3). The
sample ‘TZ13’ was found well-aligned with its mean diameter of 230 nm
with its surface roughness. TEM investigation endorsed the well-aligned
nanofibers with the lattice d-spacing around 0.289 nm, which was asso-
ciated with the (100) plane of the wurtzite hexagonal phase of ZnO. The
selected-area electron diffraction (SAED) analysis showed the polycrys-
talline nature of TZ13 nanofibers and coincided with the XRD result. Us-
ing various catalysts, the photodegradation of EBT dye was performed,
whereas the sample ‘TZ13’endorsed the highest photodegradation per-
centage as compared to others.
Declaration of Competing Interest
The authors declare that they have no competing interests.
Acknowledgements
Authors are thankful to Prof. M. A. More, Savitribai Phule Pune Uni-
versity, Pune (M.S.), India, for providing the accessibility of characteri-
zation facilities.
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