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z Catalysis
Synthesis of Core-Shell Au@TiO2@C Nanoparticles and Their
Photocatalytic Properties for the Degradation of
Rhodamine B Under Simulated-Solar Light
Xue-qin Wang,[a] Dong-ying Li,[a] Shi-peng Wang,[b] Fahad Azad,[c] and Shi-chen Su*[a]
A simple method to synthesize Au@TiO2@C core-shell sandwich
nanoparticles by hydrolysis and depositing carbon quantum
dots (CQDs) is reported. The photocatalytic activity of the
synthesized material was tested via degrading Rhodamine B
(RhB) under simulated-solar light irradiation. The degradation
rate was found in the following order: Au@TiO2@C > P25 >
Introduction
For the past few years, environment and energy challenges
have become most serious global problem. Semiconductor
(ZnO,[1–3] TiO2,[4–6] Fe2O3,[7] Ga2O3,[8,9] and so on) photocatalysis
has shown enormous potential for not only producing renew-
able energy but also eradicating harmful contaminants from
water. Titanium dioxide (TiO2) is a widely studied transition
metal oxides in the field of photocatalysis due to its superior
electronic and catalytic properties, outstanding chemical
stability and environment friendliness.[10,11] Though semicon-
ductor photocatalysis has achieved significant advancement,
but developing high quality green photocatalysts is still in
great demand. There are two main problems in TiO2 based
photocatalysts:[1,12,13] TiO2 is a wide-bandgap semiconductor
with a band gap of 3.2 eV, therefore, it produces photo-induced
electron and hole pairs only when stimulated by ultraviolet
light. Secondly, recombination rate of electron-hole pairs is
high due to small size of the nanoparticles, which leads to low
quantum efficiency. Therefore, in order to make full use of TiO2
in solving environmental and energy problems, further study
and modification of TiO2 is essential.
Over the past decades, a large number of researchers have
done a lot of work to enhance photocatalytic properties of
[a] X.-q. Wang, Dr. D.-y. Li, Prof. S.-c. Su
Institute of Semiconductor Science and Technology, South China Normal
University
Guangzhou 510631
E-mail: shichensu@scnu.edu.cn
[b] Prof. S.-p. Wang
Instituted of Applied Physics and Materials Engineering
University of Macau
Macau 999078, China
[c] Dr. F. Azad
School of Natural Sciences (SNS), National University of Science and
Technology (NUST),
H-12 Islamabad, Pakistan
Supporting information for this article is available on the WWW under
https://doi.org/10.1002/slct.202002713
ChemistrySelect 2020, 5, 10055 – 10059
Au@TiO2 > TiO2. The superior photocatalytic of Au@TiO2@C
was attributed to synergistic effect of Au and CQDs. The CQDs
layer coated outside benefits in improving absorption efficiency
of solar light host and separation of electron-holes pairs. The
Au core can accelerate transfer process of photo excitons which
can facilitate photocatalytic reaction.
TiO2,[14–16] such as fabricating mesoporous nanostructure,[17]
doping of inorganic elements and addition of narrower band
gap semiconductors (CoS,[18] CuO,[19] g-C3N4[20] etc.).One of the
promising strategies is to introduce noble metals into TiO2
nanoparticles such as, Au,[21] Ag[22] and Pt.[23] These noble metals
have superior optical and electrical and properties which can
enhance light absorption, if loaded on the surface of semi-
conductors, due to their surface plasma resonance (SPR) effect.
Awazu, K. and co-workers[24] reported a new phenomenon of
“plasmonic photocatalysis” by irradiating UV light on TiO2
grown on silica (SiO2) covered Ag nanoparticls showed a seven-
fold enhancement in degradation of methylene blue (MB) dye
as compared to the pure TiO2. Grabowska, E. et al.[25] synthe-
sized porous TiO2 microspheres using hydrothermal method
and then loaded noble metals by photo-chemical reduction on
the TiO2 surface. The noble metal loaded TiO2 microspheres
when irradiated with UV light showed excellent performance in
the degradation of phenol (aqueous phase). Wan and co-
workers[26] presented a method for the fabrication of single
atomic site catalysts by forming Ti Au Ti structure for enhanc-
ing catalytic properties of TiO2.
In addition to loading noble metals onto TiO2, the research
on carbon quantum dots in recent years also provides a new
idea for enhancing photocatalytic properties of TiO2. Since the
first demonstration of CQDs[27] in 2004, there has been
significant progress in the research of CQDs due to their
outstanding chemical and physical characteristics, such as
water solubility, non-toxicity and wavelength dependent
luminescence, which makes them a potential candidate for the
fields of tiny light emitting diodes (LED), biological imaging,
chemical sensing and photocatalysis.[28–31] Kumar, M. Sathish
et al.[32] achieved in situ growth of CQD/TiO2 nanostructure that
showed superior degradation of MB compared with commer-
cial TiO2-P25. Ruidi Liu and co-workers[33] successfully synthe-
sized TiO2/CQDs composite via solvothermal and in situ hydro-
thermal method for effective degradation of RhB in visible
light. TiO2 sensitized CQDs synthesized by Hu, Y. and co-
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workers[34] also showed excellent result by maintaining 99 %
removal efficiency under a fluorescent lamp.
Herein, we designed a feasible method to synthesis
Au@TiO2@C sandwich structure in order to make full use of
noble metals and CQDs. We prepared Au nanoparticles coated
with TiO2 via hydrolysis and deposited CQDs subsequently. The
characteristic of Au@TiO2@C nano-heterostucture and the
effect of Au and CQDs on the photocatalytic properties of TiO2
is studied in this paper.
Results and Discussion
The SEM images of TiO2 and Au@TiO2 prepared by hydrolysis
are shown in Figure 1(a) and (b). The size of TiO2 particles was
found to be in the range: 200–300 nm with some bigger
granules, whereas, Au@TiO2 particles exhibit a uniform diame-
ter of �110 nm. The introduction of Au during TiO2 growth
acted as nucleating agent. Figure 1(c) presents scanning trans-
mission electron microscopy (STEM) image of TiO2 indicating
big spherical structures which are further comprised of small
spherical nanoparticles. Inset in Figure 1(c) is the selected area
electron diffraction pattern of TiO2, revealing polycrystalline
nature of this sample. High-resolution transmission electron
microscope (HRTEM) image of Au@TiO2 is shown in Figure 1(d).
It showed that Au core of diameter �9 nm is coated with TiO2.
Moreover, two different kinds of lattice fringes, with d spacing
of �0.23 nm and �0.19 nm, were observed which can be
matched with (111) plane of face-centered cubic Au and (200)
plane of anatase TiO2,[35,36] respectively. The well-defined inter-
face depicts a strong interaction between Au core and TiO2
Figure 1. SEM images of (a) TiO2; (b) Au@TiO2; (c) STEM image of TiO2; (d)
HRTEM image of Au@TiO2; (e) STEM and (f) TEM images of Au@TiO2@C. The
inset in figure (c) is selected area electron diffraction pattern of TiO2.
ChemistrySelect 2020, 5, 10055 – 10059
shell. The STEM image in Figure 1(e) and TEM image in
Figure 1(f) show microstructure of Au@TiO2@C. Obviously, the
dark areas are regarded as Au cores, and the rest part presents
TiO2 and C shell. Moreover, the growth of C shell grown over
TiO2 can be clearly observed in Figure 1(f). These results
confirm successful fabrication of Au@TiO2@C sandwich nano-
structure by a simple hydrolysis method.
The crystal structures of the three samples (TiO2, Au@TiO2,
Au@TiO2@C) were further characterized by XRD and the result
are shown in Figure 2. The peak profiles of the three samples
are similar, to that of anatase TiO2. The peaks at 2q: 25.3°, 37.7°,
47.9°, 53.8° and 54.7°can be ascribed to the (101), (004), (200),
(105) and (211) planes of anatase TiO2,[37–39] whereas no
characteristic diffraction peaks of Au and C were detected. The
absence of Au and C peaks might be due to very low
concentration of these phases in the obtained compound. EDS
was employed to further explore presence of Au and C in the
synthesized samples. Figure 3. shows EDS spectra of Au@-
TiO2@C obtained at different encircled points in Figure 1(e). The
presence of corresponding peaks of Au and C and Ti confirms
their presence in synthesized Au@TiO2@C samples. It was also
observed that the mass % of Au diminishes from the center to
Figure 2. XRD patterns of TiO2, Au@TiO2 and Au@TiO2@C.
Figure 3. EDS images of Au@TiO2@C obtained at the point (a) 01, (b) 02 and
(c) 03 encircled region in Figure 1(e).
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ChemistrySelect doi.org/10.1002/slct.202002713
the edge of the nanoparticle while the content of C is
increasing gradually. The EDS results and structural information
revealed from TEM images confirm sandwitch structure of
Au@TiO2@C.
X-ray photo electron spectroscopy (XPS) was employed to
investigate chemical state of surface constituent elements in
Au@TiO2@C, Au@TiO2 and TiO2 samples. Figure 4(a) shows Ti-
2p3/2 and Ti-2p1/2 peaks in Au@TiO2@C, Au@TiO2 and TiO2. Ti-2p
peaks in Au@TiO2@C were observed at the binding energy of
458.6 eV (Ti-2p3/2 ) and 464.4 eV (Ti-2p1/2 ) indicating 4 +
oxidation state of Ti[40,41] in this sample. The binding energy of
these peaks were found 0.4 eV higher than that of Au@TiO2.
This increase in the binding energy of Ti-2p peaks indicates
increased coordination of Ti with carbon quantum dots[33,36] in
Au@TiO2@C. Figure 4(b) shows Au-4f peaks in Au@TiO2@C
located at 83.8 and 87.5 eV. These peaks correspond to the
splitting of 4f doublet of 3.7 eV in Au metal,[11,36,42] which
indicates metallic characteristic of Au. The ambiguous peaks of
Au were resulting by the thick shell of TiO2. Figure 4(c) presents
Gaussian fitted spectra for O-1s peaks at 529.8 eV which was
ascribed to oxygen sitting at lattice site (OL) in TiO2 in
Au@TiO2@C and Au@TiO2. The extra peak at 531.6 eV for
Au@TiO2@C was attributed to the oxygen vacancies (OV).[43]
Figure 4(d) shows C-1s peas in Au@TiO2@C. Three peaks with
binding energies of 284.8, 286.6 and 288.4 eV were assigned to
C C, C OH and C O bonds, respectively.[38,44] A small peak at
280.8 eV was also observed in C-1s spectra of Au@TiO2@C
which indicates formation of C Ti bond in this sample. This
formation of C Ti bond explains creation of oxygen vacancies
in Au@TiO2@C. These oxygen vacancies can essentially serve as
specific reaction sites for dye molecules in Au@TiO2@C, which
can improve the photocatalytic performance of TiO2, effectively.
Apart from carbon reacting with Ti in Au@TiO2@C, it implies
from TEM results that majority of carbon quantum dots coat
surface of TiO2 independently, which enhances the absorption
efficiency of solar light.
Figure 4. XPS spectrum of: (a) Ti-2p in TiO2, Au@TiO2 and Au@TiO2@C; (b) Au-
4f in Au@TiO2@C; (c) O-1s in Au@TiO2 and Au@TiO2@C; (d) C-1s in
Au@TiO2@C.
ChemistrySelect 2020, 5, 10055 – 10059
In order to study the effect of gold and CQDs on the optical
properties of TiO2, UV-vis absorbance spectra of samples are
preformed and the results shown in figure 5. Figure 5a showed
that both Au@TiO2 and Au@TiO2@C samples performed the
better absorption property compared to TiO2. The visible light
absorption of Au@TiO2@C was enhanced clearly. The band
gaps of semiconductors were calculated according to Kubelka-
Munk method,[45] as shown in figure 5b. The extrapolated band
gap energy of Au@TiO2 and Au@TiO2@C were 3.12 eV and
2.88 eV, respectively, both lower than that of pure TiO2
(3.40 eV), It indicates that the addition of gold and carbon
effectively reduces the band gap of TiO2.
The photocatalytic properties of the as-prepared samples
were estimated for the degradation of aqueous RhB under
simulated solar-light irradiation and compared with commercial
TiO2 (P25). The degradation rate shown in Figure 6(a) was
calculated by Eq. 1. Before studying photocatalysis, the solution
of RhB and photocatalysts was stirred in dark to reach
adsorption equilibrium. The values at 0 min in Figure 6(a) show
the adsorption activity of samples in dark. It can be seen that
the highest activity was observed in TiO2, which might be due
to porous structure of TiO2 poly-crystals. The degradation of
RhB without any photocatalysts was lowest and was barely
degraded. The photo-degradation efficiency of Au@TiO2@C was
found to be more than 90 % (within 2 hours) under simulated
solar-light, which is higher than P25 (62 %), Au@TiO2 (47 %) and
TiO2 (40 %). The photo-degradation reactions for all samples
(Au@TiO2@C, P25, Au@TiO2, TiO2) followed pseudo-first-order
kinetics with rate constants 0.0231, 0.0109, 0.0073 and
0.0044 min 1, data is shown in Figure 6(b). This can be
attributed to the synergistic effect of Au and C. The catalytic
efficiency of Au@TiO2@C showed a two-fold increase as
compared to commercial P25, and five-fold increase in case of
Figure 5. (a) UV-vis absorbance spectra; (b) plots of (αhv)1/2 versus hv(eV)
for TiO2, Au@TiO2 and Au@TiO2@C.
Figure 6. Photocatalytic performances of samples under simulated-solar
light: (a) degradation rate and(b) fitted curves for the kinetic traces of TiO2,
Au@TiO2, Au@TiO2@C, P25 and the blank control group.
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Table 1. Previous research of TiO2.

Composite Dosage Concentration of pollutants Pollutants Degradation time Effect

Au@ TiO2[11] 4 mg 5 ppm RhB 4h 98.1 %

CQDs/TiO2[33] – – MB 20 min 53 %
C-TiO2[36] 100 mg 10 mg L 1, 50 ml RhB 90 min 60 %
Au@r-GO/TiO2[36] 5 mg 2 × 10 5 mol L 1, 25 ml RhB 50 min 100 %
Au@ TiO2[46] 50 mg 2 × 10 5 mol L 1, 50 ml RhB 5h 100 %
TiO2@C[47] 50 mg 5 mg L 1, 50 ml RhB 12 min 100 %

pure TiO2. Table 1 shown the previous study on TiO2. There are
some articles reporting the application of C and gold in TiO2.
But Au@TiO2@C structure is rarely report. We can find that the
Au@TiO2@C prepared in this study is dominant compared with
these composites,
Figure 7 illustrates a proposed mechanism for Au@TiO2@C
nanoparticles for the degrading of RhB under solar-light. The
absorption wavelength spectrum of carbon quantum dots is
very wide for solar light, therefore, CQDs can generate
electron-hole pairs.[48] Moreover, Au cores can also accelerate
electron-hole transfer process. Therefore, doping of CQDs can
greatly improve the utilization ratio of photocatalysts. In
addition, the SPR effect of Au can also help in the optical
absorption. A schottky junction[46] exists in Au@TiO2@C
between Au and TiO2 because of the higher Fermi level of Au.
when light falls on the TiO2 spheres charges are separated due
to the Schottky junction at the interface of TiO2 and Au which
will reduce the charge recombination and therefore will lead to
enhanced photocatalytic activity. The photo-induced electrons
transfer from the conduction band of TiO2 to Au through their
contact interface.[49] This process helps in delayed recombina-
tion of photo excited electron-hole pairs, providing more action
sites. Previous research[47] at photodegradation show that OH
*
*
with H2O to form OH radicals. These radicals then react with
RhB to degrade it.
Conclusion
In summary, Au@TiO2@C sandwich nanoparticles have been
synthesized successfully by a feasible and simple method. The
degradation rate of RhB under simulated solar-light irradiation
was achieved to be �96 %. Two-fold enhancement in the
photocatalytic property of Au@TiO2@C was observed as
compared to commercially available P25 and five-fold for pure
TiO2. This increase in the photocatalytic properties from the
addition of Au and CQDs is due to improved light absorption
properties along with reduced recombination rate of electron-
hole pairs.
Supporting Information Summary
The preparation of samples and characterizations can be found
in Supporting Information.
Acknowledgements

and O2 were the primary reactive species. Scavenger analyses

*
conducted by Aditya Chauhan[50] comfirmed the idea that
photogenerated holes are the primary redox species followed
by hydroxyl radicals.The excited electrons can combine with
*
oxygen in water to yield O2 radicals while holes can combine
This work is supported by National Natural Science Foundation of
China (Grant No. 61574063, 11974122); Science and Technology
Program of Guangdong Province, China (Grant Nos.
2017A050506047); Guangzhou Science and Technology Project
(Grant Nos. 201904010399); Science and Technology Develop-
ment Fund (FDCT 084/2016/A2) from Macau SAR; Multi-Year
Research Grants (MYRG-00149-FST) from University of Macau.

Conflict of Interest
The authors declare no conflict of interest.

Keywords: Titanium · Catalysis · Au · core-shell structure ·

solar-light

Figure 7. Mechanism for the enhanced photocatalytic activity of Au@TiO2@C
for the degrading of RhB under solar light.
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Submitted: July 8, 2020
Accepted: August 16, 2020
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