Ultra-low-temperature growth of CdS quantum dots on g-C3N4 nanosheets and their photocatalytic performance

Article abstract of DOI:10.1039/c7dt04355d

CdS quantum dots deposited on carbon nitride (g-C₃N₄) nanosheets have been synthesized by ultra-low temperature (-60 °C) liquid phase precipitation reactions. The obtained CdS quantum dots were uniformly distributed on the surface of the g-C₃N₄ nanosheets with an average diameter of 5 nm. Correspondingly, CdS/g-C₃N₄ exhibits a highly enhanced photocatalytic performance.

Full text of DOI:10.1039/c7dt04355d

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Ultra-low-temperature growth of CdS quantum dots on g-C N4
3
nanosheets and their photocatalytic performance
Received 00th January 20xx,
Accepted 00th January 20xx
a
a
a
b
a
a
a
Ruoyu Zhang, Kai Huang, Hehe Wei, Dong Wang, Gang Ou, Naveed Hussain, Ziyun Huang,
c
a
Cheng Zhang and Hui Wu
DOI: 10.1039/x0xx00000x
www.rsc.org/
CdS quantum dots deposited on carbon nitride (g-C
3
N
4
)
temperature, k
B
is the Boltzmann constant, C
0
is the saturation
nanosheets have been synthesized by ultra-low temperature(-60 concentration of the solution, and C is the actual concentration of
) liquid phase precipitation reactions. The obtained CdS the reactants. In addition to the time dependence of the rate of
quantum dots were uniformly distributed on the surface of the g- conversion, the rate constant k is temperature dependent, usually
nanosheets with average diameter of 5 nm. Correspondingly, assumed to follow an Arrhenius relation of the form:
℃
3 4
C N
k ꢂ Aeꢃꢄꢅ/ꢆꢇ
(2)
the CdS/g-C
performance.
3
N
4
exhibits highly enhanced photocatalytic
Where T is the thermodynamic temperature, A is the pre-
exponential function and Ea is supposed to represent the activation
energy for the reaction. According to the equations (1) and (2), at
the certain concentration of the reactants, the nucleation of the
reaction products can be effectively suppressed by reducing the
The preparation of high-quality semiconductor nanocrystals,
particularly in quantum size (quantum dots, QDs), has become a
dominating research field, due to the unique size-dependent
1
-3
properties and well-defined electronic and optical properties. This
has attracted great attention in controlling the crystal structure of
10-12
temperature of the reactants.
In this work, we focus our attentions toward producing cadmium
sulfide (CdS) QD nanocrystals through controlling the reaction
temperature. CdS QDs have unique properties and adjustable band
4
semiconductor materials in both growth and nucleation. Hot
injection method and non-injection organic synthesis method are
the most common synthesis methods for semiconductor
gaps, making it widely applied to water pollution treatment and H
2
5
nanocrystal production. These methods usually require a heating
13-16
production.
However, shape control of high quality
process at specific reaction temperatures for semiconductor
nanocrystal growth. The heating process could stimulate reactive
precursors to nucleate nanoparticles and result in a coinstantaneous
homogeneous and stable semiconductor QDs from traditional
solution chemistry is extremely difficult, mainly because of the
difficulty in controlling the diffusion, aggregation and nucleation of
6
nucleation and growth.
17-20
the product molecule in the liquid phase.
One of the most
Usually, the QD formations contain the nucleation and growth
process. According to the classical nucleation, the necessary Gibbs
free energy of activation for nuclei formation (ΔG*) in a typical
efficient routes to solve these problems is to load cadmium sulfide
QDs onto graphitic carbon nitride (g-C
3
N
4
) nanosheets to form
g-C is metal-free
3 4
semiconductor, the photocatalyst activity of g-C N can be greatly
21, 22
stable 0D/2D nanocomposites.
3
N
4
a
7-9
solution synthesis can be described as follow:
3
2
1
6πγ ν
∆
G* =
2
(1)
enhanced via different methods, such as supporting various
materials as co-catalysts, such as carbon or metals, and forming
2T2ꢀln
C-C0
C0
ꢁ
3
k
B
23-25
composites with other semiconductors.
Interactions between
Where γ is the increase in the free energy per unit surface area of
the nucleus, ν is the molar volume of the nucleus, T is the
two moieties can make QDs more dispersive and stable, meanwhile
the accelerated charge facilitated can efficiently quench the
photoluminescence of QDs, thereby suppressing the recombination
2
6, 27
of photoexcited charge.
Herein, a CdS/g-C nanocomposite photocatalyst was fabricated
by an ultra-low temperature liquid phase precipitation reaction.
CdS/g-C nanocomposites were employed for visible-light-driven
.
3 4
N
3 4
N
photocatalytic hydrogen evolution and degradation for the organic
dye, Rhodamine B. The photostability of obtained photocatalysis
was significantly enhanced. A series of characterizations reveals that
CdS QDs with average diameter of 5 nm are uniformly scattered on
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g-C
nanocomposites could greatly improve the photocatalytic activity of
g-C nanosheets for hydrogen generation and degradation for
3
N
4
nanosheets. The obtained CdS content of 4.5wt% the g-C
3
N
4
3 4
g-C N nanosheets.
3 4
N
organic dye Rhodamine B.
The synthesis mechanism of CdS/g-C
3
N
4
is illustrated in Fig. 1. g-
precursor solutions. In
conventional precipitation synthesys methods, Na S solution is
3 4 2
C N nanosheets were dispersed into CdCl
2
slowly dropped into the CdCl
nanoparticles loading on g-C
2
precursor solutions. CdS
is then prepared by the
3 4
N
spontaneous nucleation and agglomeration of CdS nanocrystals, the
obtained material is room temperature (RT) CdS/g-C . In contrast,
we slowly dropped the Na S solution into CdCl precursors at -60℃,
3
N
4
2
2
CdS quantum dots supported on g-C N4 were obtained, and the
3
grown progress of CdS nanocrystals were suppressed at ultra-low-
temperature reaction progress.
The morphology of heterojunctions was investigated by
transmission electron microscopy analysis. As shown in TEM image
(Fig. 2a), it was clearly seen that the CdS QDs with an average size
of 5 nm (Fig. S1) were homogeneously dispersed on the lamellar
surface of g-C N . The HRTEM image further revealed that the
3
4
characteristic interplanar spacing of 0.336 nm matches the (111)
lattice planes of hawleyite CdS (Fig. 2b and Fig. 2d). As for the
control sample, CdS nanoparticles synthesized at 25℃ were
randomly accumulated on the surface of the g-C N nanosheets (Fig.
3
4
2
c). Furthermore, CdS nanoparticles showed larger size and a wider
size distribution compared with CdS QDs (Fig. 2d). Most of the CdS
nanoparticles had diameters from 20 to 50 nm (Fig. S2). The amount
of CdS QDs loading on g-C N nanosheets was 4.5% as measured by
Fig. 2. (a) TEM and (b) HRTEM images of CdS/g-C
HRTEM images of RT CdS/g-C
3 4
N . (c) TEM and (d)
3 4
N .
3
4
inductively coupled plasma ion emission spectroscopy (ICP/IES).
Clearly, the mentioned results strongly attested that the CdS QDs
show diffraction peaks of both CdS and g-C
characteristic peaks of CdS (26.7°) and g-C (27.4°) were very
close and overlap with each other. The peak width of the CdS/g-
3 4
at 44.1°and 52.2°, were smaller than that of RT CdS/g-C N ,
3 4
N , while the
had been homogeneously modified on the g-C N4 surface to
3
3 4
N
compose CdS/g-C N4 via the ultra-low temperature precipitation
3
approach.
C
3
N
4
The phase structure and composition of the samples were further
revealed by XRD, UV-vis spectra, and XPS, respectively. The XRD
patterns of the CdS/g-C N , RT CdS/g-C N and pure g-C N were
which indicated the crystalline size of CdS prepared at ultralow
temperature is smaller than that prepared at 25℃.
3
4
3
4
3 4
The optical properties of CdS/g-C
and CdS were further characterized by ultraviolet visible absorption
spectroscopy (UV-vis). The adhering of CdS to the g-C lead to an
3 4 3 4 3 4
N , RT CdS/g-C N , pure g-C N ,
shown in Fig. 3a. Two obvious diffraction peaks were displayed at
7.4°and 13.1°corresponding to pure g-C N , belonging to the
2
3
4
3 4
N
typical graphitic interlayer (002) peak and the in-plane structural
;
/
improvement in the whole investigated wavelength range (Fig. S3
and Fig. 3b). As shown in Figure S3 and Figure 3b, the pure CdS
exhibited an absorption edge at 521 nm with band gap of 2.38 eV,
packing motif (110).
The pure CdS displays three distinct
diffraction peaks at 26.7°, 44.1°and 52.2°respectively corresponding
to (111), (220), and (311) crystal planes of CdS (JCPDS No. 75-0581).
The XRD pattern of CdS/g-C N and RT CdS/g-C N nanocomposites
the pure g-C
gap of 2.79eV. The samples of CdS/g-C
absorption edges at 455 nm and 471 nm, which corresponded to
the band gaps of 2.72 eV and 2.63 eV. Thus, the CdS/g-C
nanocomposites exhibit hybrid absorption features of g-C and
3
N
4
exhibits an absorption edge at 444 nm with band
3
4
3 4
3
N
4
and RT CdS/g-C have
3 4
N
3 4
N
3 4
N
CdS, which contribute to efficiently produce photogenerated
electrons-holes.
3 4
The CdS/g-C N samples were further investigated by XPS. The XPS
peaks of Cd 3d and S 2p (Fig. S4) indicated the formation of CdS. The
energies of the main peaks of Cd 3d5/2 and 3d3/2 are found at 404.8
eV and 411.5 eV, respectively, which are consistent with those of Cd
2
8
3
d in CdS. The minor peak of S 2p at 161.6 eV and 162.8 eV is
closed to that of CdS, which is most possible from the elemental
2
9
3 4
sulfur, which was adsorbed on surface of g-C N .
Fig. 1. The schematic outline for the CdS nanoparticles deposited on
2
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nanosheets and CdS QDs. Photoelectrochemical measurements are
3 4 3 4 3 4
Fig. 3. (a) XRD pattern of g-C N , CdS/g-C N and RT CdS/g-C N . The
dark cyan line is the standard pattern of the CdS (JCPDS No. 75-
2
0
581). (b) (ahυ) versus hυ curve of CdS, g-C
CdS/g-C . The dashed lines are tangents of the curves. The
intersection value is the band gap.
3 4 3 4
N ,CdS/g-C N and RT
3 4
N
The recombination of the photo-generated electrons and holes
were investigated by photoluminescence (PL) spectra with an
excitation of 325 nm. The spectra of different samples had similar
3 4
shape emission peaks (Fig. S5). The pure g-C N sample exhibited an
intense emission peak at 455 nm, at the same time, the intensity of
this emission band dropped significantly for the composite samples
with CdS, which indicates a valid transfer of electron-hole pairs from
3
0
g-C
Photocatalytic H
nanocomposites was measured under visible light irradiation, and
.5wt% Pt was added as co-catalyst to cut dowm the overpotential
of H evolution. As shown in Fig. 4a and Fig. S6, the CdS QDs grown
at ultralow temperature on g-C nanosheets noticeably improved
the photocatalytic H evolution activity compared to pure g-C
More specifically, the CdS/g-C nanocomposites exhibited a H
2
3 4
N to CdS.
2
3 4
evolution activity of the synthesized CdS/g-C N
0
2
3
N
4
2
3 4
N .
Fig. 4. (a) Comparison of the visible light-driven photocatalytic
3
-
N
4
evolution H
b) Cycling tests of visible-light-driven photocatalytic evolution H
activity of CdS/g-C . (c) Comparison of the visible-light-driven
photocatalytic degradation RhB activity of CdS/g-C , RT CdS/g-
, g-C and CdS. (d) Cycling tests of visible-light-driven
photocatalytic degradation RhB activity of CdS/g-C . (e) The
transient photocurrent responses of CdS/g-C , RT CdS/g-C , g-
and CdS under visible-light irradiation. (f) Electrochemical
2 3 4 3 4 3 4
activity of CdS/g-C N , RT CdS/g-C N , g-C N and CdS.
1 -1
evolution rate of 4.967 mmol h g , which was more than 59 times
(
2
-1 -1
3 4
higher than pure g-C N (0.083 mmol h g ). Compared with the CdS
3 4
N
-
1
-1
-1 -1
(
0.997 mmol h g ) and RT CdS/g-C
nanocomposites displayed excellent photocatalytic for
hydrogen evolution. The stability test results of CdS/g-C were
shown in Fig. 4b, no distinct decrease of H evolution was observed
after a five-run test of photocatalytic H evolution. The XPS (Fig.S8)
and XRD (Fig.S9) of CdS/g-C after the H evolution stability test
3 4
N (1.72 mmol h g ), CdS/g-
3 4
N
3 4
C N
C
3
N
4
3 4
N
3 4
N
3 4
N
2
3
N
4
3 4
N
2
3 4
C N
3
N
4
2
impedance spectroscopy (EIS) of CdS/g-C
and CdS under visible-light irradiation.
3 4 3 4 3 4
N , RT CdS/g-C N , g-C N
were measured. No obvious changes in materials properties were
exhibited.
The photocatalytic activities of samples were also measured by RhB
photodegradation under visible light (λ＞ 420 nm). From Fig. 4c
and Fig. S7, the CdS/g-C N nanocomposites showed much higher
usually applied to research the excitation and transfer of
photogenerated charge carriers. Fig. 4e showed the transient
3
4
photodegradation efficiency (Dp =89.5%) than pure g-C N (Dp
3
4
photocurrent response of CdS/g-C
CdS. From the Fig. 4e, we can expressly figure out that the
photocurrent response of g-C is lower than other samples. The
photocurrent response of CdS/g-C was significantly higher than
of the RT CdS/g-C and CdS. The generation of the photocurrent is
3 4 3 4 3 4
N , RT CdS/g-C N , g-C N and
=
12.7%), CdS (Dp =40.6%) and RT CdS/g-C N4 (Dp =50.2%). This
3
demonstrates that the recombination of CdS QDs and g-C N can
3
4
3 4
N
tremendously improve the photodegradation efficiency. The cycling
3 4
N
test of photocatalytic degradation of RhB with CdS/g-C N4
3
3 4
N
nanocomposite was repeated five times (Figure 4d), displaying that
it possesses great stability and repeatability. The XPS (Fig.S10) and
XRD (Fig.S11) of CdS/g-C N after the RhB degradation stability test
31
mainly the result of photoinduced electrons diffusing to the ITO.
The transient photocurrent responses showed that the separation
efficiency of the photogenerated electrons and holes in the CdS/g-
3
4
were measured. No obvious changes in materials properties were
exhibited.
C
3
N
4
was markedly improved as a result of the synergistic effect
between CdS and g-C . The increasing of the photocurrent has
3 4
N
According to the mentioned experimental results, we confirm that
linear relationship with photocatalytic activity. Electrochemical
impedance spectroscopy (EIS) was also performed to characterize
charge carrier transportation. Fig.4f displayed that the impedance
the improvement of photocatalytic activity for CdS/g-C N4
3
nanocomposites are attributed to efficient interfacial transfer and
separation of photogenerated carriers between the g-C N4
3
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radius of the CdS/g-C
3
N
4
was smaller than that of RT CdS/g-C
3
N
4
, g- 11 Y. Xia, K. D. Gilroy, H. Peng and X. Xia, Chem., Int. Ed, 2017, 56,
0-95.
6
C
3
N
4
and CdS. which indicates the higher efficiency of photoinduced
1
1
1
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electron-hole pairs through an interfacial interaction between g-
32-34
C
3
N
4
and the CdS quantum dots
.
Fig. S12 showed the schematic illustration of the CdS/g-C
3 4
N
photocatalytic mechanism. Because of suitable match overlapping 15 H. Lin, Y. Li, H. Li and X. Wang, Nano Res. , 2017, 10, 1377-1392.
1
6 G. Yu, L. Geng, S. Wu, W. Yan and G. Liu, Nat. Commun. 2015,
band structures and similarly contacted interfaces, photoexcited
electrons in the CB of g-C can immediately move to the CB of
CdS. In the same time, photoexcited holes in the VB of CdS
spontaneously move to the VB of g-C . The mechanism of
5
1, 10676-10679.
3 4
N
1
7 H. Wang, S. Xu, C. Tsai, Y. Li, C. Liu, J. Zhao, Y. Liu, H. Yuan, F.
Abild-Pedersen, F. B. Prinz, J. K. Norskov and Y. Cui, Science,
2016, 354, 1031-1036.
3 4
N
hydrogen evolution over the composite material was presented in 18 J. M. Woods, Y. Jung, Y. Xie, W. Liu, Y. Liu, H. Wang and J. J. Cha,
ACS Nano, 2016, 10, 2004-2009.
2
Fig. S12a. As a consequence, L-ascrobic acid (H A) adhering on the
1
9 S. F. Tan, G. Lin, M. Bosman, U. Mirsaidov and C. A. Nijhuis, ACS
Nano, 2016, 10, 7689-7695.
0 R. Viswanatha, D. M. Battaglia, M. E. Curtis, T. D. Mishima, M. B.
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g-C
3 4
N surface can be oxidized by photoinduced holes. On the
surface of Pt nanoparticles, the separated electrons will have
2
+
2
enough time to induce H to H . Fig S12b showed the process of
degradation of RhB. The adsorbed dissolved oxygen could generate 21 Y. Xu, Z. Fu, S. Cao, Y. Chen and W. Fu, Catal.L Sci. Technol., 2017,
2
−
7, 587-595.
•O
free radicals, due to the photogenerated electrons transferred
2
2
2 X. Wang, J. Cheng, H. Yu and J. Yu, Dalton Trans., 2017, 46, 6417-
to the surface of composite. Meanwhile, active •OH radicals were
6
424.
+
produced by H
2
O splitting. When h moved from the VB of the g-
3 J. Liu, Y. Liu, N. Liu, Y. Han, X. Zhang, H. Huang, Y. Lifshitz, S. Lee,
J. Zhong and Z. Kang, Science, 2015, 347, 970-974.
+
3 4
C N
and CdS, both h and •OH free radicals can transform from RhB
into products.
24 W. Ong, L. Tan, Y. H. Ng, S. Yong and S. Chai, Chem. Rev., 2016,
16, 7159-7329.
1
Conclusions
2
5 S. Cao, Y. Yuan, J. Fang, M. M. Shahjamali, F. Y. C. Boey, J. Barber,
S. C. J. Loo and C. Xue, Int. J. Hydrogen Energy, 2013, 38, 1258-
In summary, a facile ultra-low-temperature reaction approach was
developed to synthesize CdS quantum dots supported on g-C
nanosheets. The resulting CdS/g-C
high photocatalytic performance for H
of RhB. The synthesized nanocomposites with 4.5wt% CdS quantum
3 4
N
1
266.
3 4
N nanocomposites exhibited 26 Y. Pan, T. Zhou, J. Han, J. Hong, Y. Wang, W. Zhang and R. Xu,
Catal. Sci. Technol., 2016, 6, 2206-2213.
2
production and degradation
2
2
7 I. Nikitskiy, S. Goossens, D. Kufer, T. Lasanta, G. Navickaite, F. H.
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-
1 -1
dots displayed a H
9 times higher than pure g-C
after 4 cycles. Meanwhile, CdS/g-C
2
evolution rate of 4.967 mmol h g , which was
5
3 4
N
and could retain over 90% activity
3 4
N nanocomposites displayed a 29 G. Liu, P. Niu, C. Sun, S. C. Smith, Z. Chen, G. Q. M. Lu and H.
degradation rate of 89.5% for RhB solution in 75 min and could
retain over 95% activity after 5 cycles. This study may inspire the
development an approach for the synthesis of CdS quantum dots
and their potential for photocatalystic applications.
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Conflicts of interest
33 Y. Wang, H. Wang, F. Chen, F. Cao, X. Zhao, S. Meng, Y. Cui, Appl.
Catal., B,, 2017 206, 417-425.
There are no conflicts to declare
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