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C for 6h. The black product was collected and washed repeat-
edly using distilled water and ethanol, and was then dried under
vacuum at 60
) correspond to the
(001) reection of graphite oxide [28]. The diffraction peaks of
grapheneCdS (x =0, curve a) are well indexed to a pure cubic
wurtzite CdS phase (JCPDS No. 42-1411) with the three prominent
diffraction peaks corresponding to (111), (220) and (311) planes.
In addition, the diffraction peaks of grapheneZn
x
Cd
1x
S hybrid
materials (x =0.20.8, curve be) correspond to cubic wurtzite
structure of CdS. It can also be found that the increment of Zn
composition (x) in grapheneZn
x
Cd
1x
S leads to positional shifts
of the diffraction peaks toward higher scattering angles, indicat-
ing the decrease in lattice spacing for Zn
x
Cd
1x
S alloyed QDs,
which results from the replacement of some cadmium atoms in
CdS by zinc atom with smaller radius [10]. The continuous peak
shift clearly indicates no separated phase and nucleation of ZnS or
CdS nanoparticles in the formation of grapheneZn
x
Cd
1x
S alloyed
QDs [29]. When x increased to 1.0 (grapheneZnS), the diffraction
peaks (curve f) agree with the crystal lattice values of ZnS phase
(JCPDS No. 77-2100). Moreover, the broadening of the diffraction
peaks is ascribed to the small crystallite size of the nanoparticles.
Besides, no diffraction peaks of GO and graphene can be found in
grapheneZn
x
Cd
1x
S, indicating the lowamount andrelatively low
diffraction intensity of graphene.
The morphology and size of grapheneZn
0.8
Cd
0.2
S
were depicted by TEM and HRTEM. The TEM image of
grapheneZn
0.8
Cd
0.2
S shown in Fig. 2A indicates that Zn
0.8
Cd
0.2
S
QDs are attached and spread uniformly on the graphene sheets.
As shown in Fig. 2B, the HRTEM image of grapheneZn
0.8
Cd
0.2
S
reveals that the average diameter is around 4nm. The lattice
F. Xu et al. / Sensors and Actuators B 203 (2014) 8994 91
Fig. 2. (A) TEMimage, (B) HRTEMimageof grapheneZn
0.8
Cd
0.2
SalloyedQDs; (C) TEMimageof Zn
0.8
Cd
0.2
SalloyedQDs; (D) FTIRspectra of GO(a) and(b) grapheneZn
0.8
Cd
0.2
S
alloyed QDs.
fringes with interplanar distance of 0.32nm can be assigned to
the (111) plane of cubic CdS. For comparison, pure Zn
0.8
Cd
0.2
S QDs
prepared through the same method without GO agglomerate and
stack randomly together (Fig. 2C). Therefore, it can be supposed
that the reduction of GO and the deposition of Zn
0.8
Cd
0.2
S QDs on
graphene occur simultaneously. Accompanied with the reduction
of GO, graphene sheet plays an important role as support material
in assisting the growth and dispersion of the Zn
0.8
Cd
0.2
S QDs on
graphene surface. In the meantime, the Zn
0.8
Cd
0.2
S decoration
helps to prevent the aggregation of graphene sheets. Fig. 2D shows
the Fourier transform infrared spectroscopy (FTIR) of GO and
grapheneZn
0.8
Cd
0.2
S QDs in the range of 4000500cm
1
. The
characteristic bands of GO are observed at 3400cm
1
(stretching
vibration of OH groups), 1717cm
1
(C O vibration of COOH),
and 1623cm
1
(epoxide groups and skeletal ring vibrations). For
grapheneZn
0.8
Cd
0.2
S QDs, the representative adsorption bands
of GO nearly disappeared, and other peaks of oxygen-containing
functional groups (such as C O, at 1717cm
1
) reduced sig-
nicantly. The results indicate that GO is reduced to graphene.
Simultaneously, the skeletal vibration absorption peak of graphene
is observed at 1550cm
1
, conrming the recovery of the sp
2
hybrid carbon skeleton [30,31].
The UVvis diffuse reectance spectra (DRS) and energy band
gap (E
g
) values of grapheneZn
x
Cd
1x
S are displayed in Fig. 3. It
can be seen that the grapheneZn
x
Cd
1x
S has intense absorption
bands with steep edges in the visible light region, which indicates
that the visible light absorption is ascribed to the transition from
the valence band to conduction band but not to the transition
from the impurity levels to the conduction band [32]. Moreover,
the E
g
value is calculated from the equation of (ahv)
2
=C(hv E
g
),
where hv is the photon energy, A is the absorption coefcient, and
C is a constant. The E
g
of grapheneZn
x
Cd
1x
S (x =00.8) calcu-
lated from the UVvis DRS increased from 2.3eV (x =0) to 2.7eV
(x =0.8), indicating the band gap depends on the Zn:Cd ratio. As x
increased to 1.0, the band gap increased to 3.6eV. Moreover, the
band gap of grapheneCdS (2.3eV) and grapheneZnS (3.6eV) are
narrower than those of CdS and ZnS nanoparticles. The results indi-
cate the formation of a chemical bond between Zn
x
Cd
1x
S QDs and
graphene [33].
3.2. Photoelectrochemical measurements
The photocurrent of grapheneZn
x
Cd
1x
S QDs/ITO electrodes
withdifferent Zn:Cd ratio measured at 0.2Vis shownin Fig. 4A. The
photocurrent of Zn
x
Cd
1x
Sgraphene increases when x increases
from 0 to 0.2, and the photocurrent experiences a slight drop at
0.4 and 0.6. Interesting, the photocurrent reaches to the highest
as x equals 0.8. However, when x increases to 1.0 (grapheneZnS),
the photocurrent decreases abruptly and reaches lowest value. The
different photoelectrochemical activities of grapheneZn
x
Cd
1x
S
Fig. 3. UVvis DRS of grapheneZnxCd
1x
S alloyed QDs with x values of 0 (a), 0.2
(b), 0.4 (c), 0.6 (d), 0.8 (e), and 1.0 (f). The inset is the calculated band gap of
grapheneZnxCd
1x
S alloyed QDs.
92 F. Xu et al. / Sensors and Actuators B 203 (2014) 8994
Fig. 4. (A) Photocurrent density and (B) EIS of grapheneZnxCd
1x
S/ITO (x =01.0) electrode with applied voltage of 0.2V in 0.1 MPBS (pH 7); (C) photocurrent density of
grapheneZn
0.8
Cd
0.2
S/ITO electrode with different graphene dosage; (D) time based photocurrent response of grapheneZn
0.8
Cd
0.2
S/ITO electrode in 0.1MPBS under visible
irradiation repeated every 15s.
should be attributed to the different band gap and electron injec-
tion ability. The conduction band of grapheneZn
x
Cd
1x
S consists
of hybridized Zn 4s4p with Cd 5s5p. The position of conduction
band becomes more positive with the increment of Zn, which is
advantageous to enhance the electron injection ability and disad-
vantageous for visible light absorption [34]. So, a balance between
the increment of visible light absorptionandelectroninjectionabil-
ity could be achieved [35]. The highest photocurrent intensity of
grapheneZn
0.8
Cd
0.2
S alloyed QDs results from its optimum band
gap and electron injection ability. The results indicate that when
x is 0.8, the grapheneZn
x
Cd
1x
S/ITO photoelectrode exhibits the
best photoelectrochemical activities, whichis the most appropriate
windowmaterial for photoelectrochemical cell.
Fig. 4B shows the electrochemical impedance spectroscopy
(EIS) of grapheneZn
x
Cd
1x
S/ITOphotoelectrode whichcarried out
using K
3
Fe(CN)
6
/K
4
Fe(CN)
6
as a redox probe. As x increases from
0 to 0.2, the resistance increases, and then decreases when x
increases to 0.4. Further, when x increases to 0.6 and 0.8, resis-
tance decreases and reaches the smallest value when x is 0.8. The
resistance reaches the highest value when x is 1.0. The results are
consistent with the results reported in Fig. 4A. The results prove
that grapheneZn
0.8
Cd
0.2
S exhibits the smallest resistance, which
is essential to gain rather high photoelectrochemical activities.
Fig. 4C is the photocurrent of grapheneZn
0.8
Cd
0.2
S QDs with
different dosage of graphene. As the dosage of GO increases from
0 to 2mg, photocurrent increases from 2.8 to 8.9A/cm
2
, and
decreases to 5.5A/cm
2
as the dosage of GO increases fur-
ther to 3 and 5mg. At a rather lower ratio of GO, photocurrent
increases with the increment of GO because the introduction of
graphene facilitates the electron transport efciently and sup-
presses the recombination of electronhole pairs. On the contrary,
graphene has strong light adsorption which can shield active sites
of Zn
0.8
Cd
0.2
S surface, and then decreases the light absorption due
to the shielding effect [36].
Fig. 4D shows the photoelectrochemical stability of
grapheneZn
0.8
Cd
0.2
S/ITO electrode. The photocurrent was
repeatedly measured at 15s intervals under simulated solar
irradiation, and the photocurrent response intensity did not show
obvious change after 600s. The results indicate that the photo-
current of grapheneZn
0.8
Cd
0.2
S/ITO electrode is very stable and
suitable for the construction of PEC sensor.
3.3. Photoelectrochemical detection of Cu
2+
Given the excellent photocurrent response,
grapheneZn
0.8
Cd
0.2
S QDs are ideal candidate materials for
photoelectrochemical sensing of Cu
2+
, which is an essential ele-
ment for many living organisms but toxic at high concentrations.
Fig. 5A is the photocurrent of grapheneZn
0.8
Cd
0.2
S/ITO electrode
with existence of Cu
2+
. The photocurrent response gradually
decreased with the increment of Cu
2+
concentration. Based on
this, a novel and sensitive PEC sensor is developed. A good linear
relationship is found (Fig. 5B) between the photocurrent decrease
(I
0
I) and the concentration of Cu
2+
ranges from 1mol dm
3
to
120mol dm
3
, which is beyond the upper guideline levels for
copper in drinking water legislated by various governments (the
EUstandard is 30mol dm
3
) [37,38]. I
0
and I are the photocurrent
intensities of the grapheneZn
0.8
Cd
0.2
S nanocomposites in the
absence and presence of Cu
2+
, respectively. The linear regression
equation was (I
0
I) (A) =0.0725+0.234C Cu
2+
(mol dm
3
)
with a correlation coefcient of 0.9992. The detection limit is
6nmol dm
3
at a signal-to-noise (S/N) ratio of 3. The results are
satised compared with uorescent sensor and surface plasmon
resonance (SPR) sensor [3942].
The possible mechanism for the determination of Cu
2+
via PEC
method is shown in Fig. 5C. When there is no Cu
2+
, photogenera-
ted electrons transfer from valence band (VB) to the conduction
band (CB) of Zn
0.8
Cd
0.2
S QDs under visible irradiation. Then,
F. Xu et al. / Sensors and Actuators B 203 (2014) 8994 93
Fig. 5. (A) Photocurrent intensity of grapheneZn
0.8
Cd
0.2
S/ITO electrode in the presence of different Cu
2+
concentrations: 0M (a), 1M (b), 10M (c), 30M (d), 60M
(e), 100M(f), 120M(g); (B) plot of (I
0
I) versus Cu
2+
concentration on grapheneZn
0.8
Cd
0.2
S/ITO electrode.
photogeneratedelectrons intheCBtransfer tographeneandthento
ITO, which is energetically favorable process [43,44]. When Cu
2+
is
added, Cu
2+
can be bind with S
2
and be reduced to Cu
+
under irra-
diation. Conclusively, Cu
x
S (x =1, 2) formed on Zn
0.8
Cd
0.2
S surface
due to the chemical displacement of surface Cd
2+
by Cu
2+
and Cu
+
resulting fromthe lower solubility of Cu
x
S than that of Zn
0.8
Cd
0.2
S.
Moreover, the formation of Cu
x
S on the Zn
0.8
Cd
0.2
S surface gen-
erates a lower energy level that provides effective recombination
centers of photogenerated carriers. Therefore, the photocurrent
intensity of grapheneZn
0.8
Cd
0.2
S decreases withexistence of Cu
2+
.
EDS spectra shown in Fig. 5D proves the existence of Cu on
grapheneZn
0.8
Cd
0.2
S/ITO electrode.
The selectivity of the grapheneZn
0.8
Cd
0.2
S/ITO electrode is
investigated by measuring PEC response of other metal ions
Fig. 6. Photocurrent intensityof grapheneZn
0.8
Cd
0.2
S/ITOelectrodeinthepresence
of 30Mof various metal ions.
(Na
+
, K
+
, Ca
2+
, Mg
2+
, Mn
2+
, Hg
+
, Ba
2+
, Fe
2+
, Co
2+
, Ni
2+
, Pb
2+
, Ag
+
)
with concentration of 30M on the photocurrent intensity of
grapheneZn
0.8
Cd
0.2
S/ITO electrode. As shown in Fig. 6, only
weaker current changes can be induced for other metal ions. The
results indicate that the PEC sensor is much more sensitive to
Cu
2+
than other metal ions, proving high selectivity in detec-
ting Cu
2+
. Thus, based on the sensitive and selective effect of
Cu
2+
on the photocurrent intensity of grapheneZn
0.8
Cd
0.2
S/ITO
electrode, a sensitive photoelectrochemical Cu
2+
sensor is
developed.
4. Conclusions
In summary, grapheneZn
x
Cd
1x
S QDs (x =01) were pre-
paredvia one-stephydrothermal method. The experimental results
proved grapheneZn
0.8
Cd
0.2
S QDs exhibited the highest photo-
current density with graphene dosage of 2mg at an applied voltage
of 0.2V. Then, grapheneZn
0.8
Cd
0.2
S/ITO electrode was used as
PEC sensing platform to detect Cu
2+
. The PEC sensor exhibited
good selectivity and linear relationship from 1M to 120M
with detection limit of 6.5nM at a signal-to-noise (S/N) ratio of
3. The grapheneZn
0.8
Cd
0.2
S QDs also show promising applica-
tions intheelds of photoelectrochemical sensingandphotovoltaic
cell.
Acknowledgments
This work was supported by the Natural Science Foundation of
China (Nos. 61176004, 61204078, U1304505), Program for Inno-
vative Research Team (in Science and Technology) in University
of Henan Province (No. 13IRTSTHN026), and the Key Project of
94 F. Xu et al. / Sensors and Actuators B 203 (2014) 8994
Science and Technology of Henan Province (Nos. 122102210561,
13A150517, 14A150002).
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Biographies
Fang Xuhas beenanassociatedprofessor of School of Chemistry andChemical Engi-
neering, Henan Normal University, China since 2013. She received a Ph.D. degree
in School of Materials Science and Engineering from University of Science and
Technology Beijing. The main research interests of Fang Xu are the synthesis and
photoelectrochemical properties of semiconductor micro/nanomaterials, carbon-
based composite, etc.
DandanBai is anMS candidateintheSchool of ChemistryandChemical Engineering,
Henan Normal University, China. Her main research interests are the synthesis of
graphene-based quantumdots and the application in photoelectrochemical sensor.
Shuyan Han is a bachelor candidate in the School of Chemistry and Chemical
Engineering, Henan Normal University, China. Her main research interests are the
synthesis and characterization of graphene-based composite.
DapengWuis anassociatedprofessor inthe School of Chemistry andChemical Engi-
neering, Henan Normal University, PR China. He received a Ph.D. degree in School of
Chemistry and Chemical Engineering, Henan Normal University. His main research
interests are the design and fabrication of materials in nanoscale for the application
in energy conversion and storage.
Zhiyong Gao is an associated professor in the School of Chemistry and Chemical
Engineering, Henan Normal University, PR China. He received a Ph.D. degree from
Xiamen University. His main research interests are the uorescence and electro-
chemical properties of carbon quantumdots, metal oxide, etc.
Kai Jiang is a professor in the School of Chemistry and Chemical Engineering, Henan
Normal University, PRChina. The mainresearchinterests of Prof. Jiang are solar cells,
and green synthesis of nanomaterials.