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The table of contents entry

CdS/ZnS-RGO hybrids: An innovative CdS/ZnS-RGO hybrid has been synthesized

Journal of Materials Chemistry A Accepted Manuscript

via a facile one-pot hydrothermal method. The further introduction of Au
nanoaparticles enables the final composite with the advantages of heterostructured
semiconductor/semiconductor junction benefiting the hole transfer and noble metal as
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well as graphene favorable for electron transportation.

ToC figure
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COMMUNICATION

An Innovative Au-CdS/ZnS-RGO Architecture for Efficiently

Photocatalytic Hydrogen Evolution
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Received 00th January 20xx,

Accepted 00th January 20xx Shuangshuang Kai,a Baojuan Xi,a Xiaolei Liu,b Lin Ju,b Peng Wang,*b Zhengyu Feng,a Xiaojian Maa
and Shenglin Xiong*a
DOI: 10.1039/x0xx00000x

www.rsc.org/

It has been a challenge to design a novel structure for effectively The integration of multiple components into a nano-assembly
improving the efficiency of carriers’ separation and transfer. has recently intrigued gigantic interests due to either synergistic
Herein, CdS/ZnS heterostructure with tunable Cd/Zn ratio was performance or multifunctional features resulting from the
engineered on reduced graphene oxide (RGO) by a one-pot construction of interfaces of heterostructres in fields of no matter
6
hydrothermal method, followed by in-situ formation of Au catalysis or energy conversion/storage. Correspondingly, several
nanocrystals, which combines the strong electron capture ability strategies have been developed to engineer such heterostructures
of noble metal and transfer capability of graphene. The CdS/ZnS- to enhance the photocatalytic performance. Appropriate
RGO architecture was featured by the anisotropic growth of ZnS cocatalysts are picked out to load, including noble metals (Pt, Au,
7 8
nanoparticles on CdS nanorod tip. Relying on the low lattice etc.) and transition metal compounds (oxides such as NiOx and
9 10 11
mismatch, the epitaxial growth of ZnS on CdS as well as CdS on CoOx, sulphides such as MoS2 and WS2 and phosphides such as
12 13
graphene was realized, which rendered the immediate contact of Ni2P and FeP ). Advantageously, cocatalysts can enable the
interfaces between different phases. Due to the three features in spatial separation of electron-hole pairs and favorably facilitate the
one structure including CdS/ZnS, noble metal and graphene, Au- proton reduction. Recently, carbon-based materials, such as carbon
14 15 16
CdS/ZnS-RGO heterostructure offers an excellent photocatalytic nanotubes, graphene, and g-C3N4 were emerging a new class
−1 −1
H2 evolution rate as high as 9.96 mmol h g under visible-light of cocatalysts. Alternatively, hybridizations with other
irradiation and a photocatalytic stability over 30 h. The result semiconductors form semiconductor/semiconductor
17 18 19
confirms the efficient separation and transfer of photogenerated heterojunctions, such as CdS-TiO2, CdS-ZnO, ZnS-CdS(-Cu2-xS),
20
electrons and holes. CdxZn1-xS and so on. In type-I core–shell quantum dots, the
photogenerated electrons can be transported from core to shell
The clean hydrogen can be sustainably obtained from water resulting from electron tunneling. Type-II heterojunctions can
splitting over Photocatalysis and photoelectriccatalysis by the render the transfer of opposite charges towards two sides of
1
consumption of solar energy, which will resolve the global energy structures, allowing for the efficient electron–hole separation.
shortage and environmental pollution issues. But a lot of widely- Considering the availability and versatility, the combination of these
2 3
studied photocatalysts, like TiO2 and ZnS, almost respond to structural functionalities is one system is able to provide an
ultraviolet light. Therefore, the key is to search for photocatalysts alternative strategy for photocatalysts of hydrogen production.
applicable that can’t only harvest visible light but also separate
Herein, the epitaxial growth of ZnS on CdS and CdS on RGO was
photogenerated charge carriers efficiently. CdS is a promising
realized by one-pot hydrothermal treatment to attain CdS/ZnS-RGO
candidate due to the advantages of appropriate band gap (2.4 eV)
heterostructures. Specifically, multi-branched CdS nanorods rooted
favorable for absorption to visible light and suitable conduction
4 on RGO sheets and followed by the anisotropic growth of ZnS
band (CB, -0.52 eV) position for H2 production from water.
nanoparticles (NPs) on the top tip. This is the first time to report the
However, it suffers from several problems such as the fast
epitaxial growth of three phases in one step. Facilely via controlling
recombination of photo-induced electron-hole pairs and bad
5 the molar ratio of Cd and Zn source, CdS/ZnS heterostructures can
photostability caused by photocorrosion.
be tuned in terms of chemical composition and microstructures,
from multi-branched nanorods, densely-stacked cauliflower-like
a.
Key Laboratory for Colloid and Interface, Ministry of Education, School of clusters, and final to hollow hemispheres. After the introduction of
Chemistry and Chemical Engineering, Shandong University, Jinan, 250100, P.R. Au nanocrystals, Au-CdS/ZnS-RGO exhibited enhanced
China, E-mail: chexsl@sdu.edu.cn
b.
State Key Lab of Crystal Material, Shandong University, Jinan, 250100, P.R. China
photocatalytic activity over hydrogen production by virtue of the
E-mail: pengwangicm@sdu.edu.cn effect of excellent ability of Au and graphene to transfer and
† Electronic Supplementary Information (ESI) available. See 6
capture electrons and the effective interface of ZnS/CdS.
DOI: 10.1039/x0xx00000x

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The stepwise synthesis of heterostructures composed of Au in Fig. S4 (ESI†) while ZnS nanoparticle aggregates pack more
nanoparticles anchored on CdS/ZnS-RGO (Au-CdS/ZnS-RGO) is densely and grow bigger, resembling the cauliflowers up against a
schemed in Fig. 1A. Typically, GO suspension was mixed with Cd and bigger head. And finally when Zn source was added alone, Cd0Zn1.0
Zn sources. As a result of the negative surface property of GO (ZnS) hemispheric bowls were tightly inverted on the graphene

Journal of Materials Chemistry A Accepted Manuscript

sheets covered by oxygen-involved groups, Cd and Zn cations were sheets in Fig. S5G-I (ESI†). Transmission electron microscopy (TEM)
readily to be absorbed (Fig. S1A, Energy-dispersive X-ray (EDX) image describes the dramatic hollow structure of Cd0Zn1.0G2. The
displaying a much higher content of Cd and Zn than S) (process i). red circles marked in each panels give the good demonstration of
2+
As decomposition of thiourea (TU), Cd ions firstly reacted into CdS immediate growth of these heterostructures on RGO sheets. X-ray
crystals on RGO sheets because of the lower solubility product of diffraction (XRD) patterns in Fig. S6 (ESI†) demonstrate hexagonal
CdS than ZnS (in Fig. S1B-C) (process ii). CdS heterogeneously wurtzite-type CdS (h-CdS, JCPDS No. 41-1049) for Cd1.0Zn0G2 and
nucleated on the surface of RGO sheets, where less energy was cubic ZnS (c-ZnS, JCPDS No. 65-0309) for Cd0Zn1.0G2 alongside the
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required to overcome the solid-liquid interface barrier than coexistence of the two phases for other CdxZn1-xG2 (0<x<1) samples,
homogeneous nucleation from liquid phase. By the structural whose chemical composition was detected by EDX spectra in Fig. S7
direction of diethylenetriamine (DETA), CdS nanorod bunches (ESI†).
formed, followed by the anisotropic growth of ZnS nanoparticles on
the nanorod tip (process iii) (see Fig. S1D-F, ESI†). Till now, the
heterojunction of CdS stem with ZnS nanocrystals on tips was
prepared on RGO sheets, which has been the first time to realize
the formation of such heterojunctions via the one-pot route. At last,
Au nanoparticles were anchored on the surface of CdS/ZnS
heterojunctions (process iv). The detailed growth mechanism was
discussed and proposed in Figure S1-3.

Fig. 2 Characterization of Au2-Cd0.5Zn0.5G2 heterostructures. (A,B)

Different magnification TEM images, (C) HAADF-STEM image, (D)
Fig. 1 Schematic diagram of the formation procedure of Au- HRTEM image of one single nanorod, (E-G) line scan signal, HAADF-
CdS/ZnS-RGO heterostructures. STEM and elemental mapping images of one typical rodlike
structure. Scale bars, 500 nm (A, C), 10 nm (B, F, G), and 5 nm (D).
Here, the heterostructured CdS/ZnS-RGO composites (CdxZn1-xGy
the scale bar in (G) also applies to (H-K).
where x and y equal mole of Cd source and volume of GO
suspension applied, respectively) could be tuned in terms of When beginning with CdS/ZnS-RGO heterostructures, quaternary
configuration and chemical composition by changing the molar Au-CdS/ZnS-RGO composites (Auz-CdxZn1-xGy and z is the mass of
ratio of raw Cd and Zn source. With keeping 2 mL GO suspension HAuCl4·4H2O applied for Au preparation) can be constructed. Taking
unchanged, in case of only Cd source, a high yield of multi-branched Cd0.5Zn0.5G2 as an example for anchoring Au nanoparticles, Fig. 2
Cd1.0Zn0 (CdS) uniformly distributed on graphene sheets in Fig. S4A displays the structural details Au2-Cd0.5Zn0.5G2. The negatively-
(ESI†). Fig. S4B-C (ESI†) clearly demonstrate the feature of charged surface of graphene sheets, as mentioned above, favorably
-
multinanorods obliquely anchoring on surface of graphene just like repelled AuCl4 ions to approach, resulting in the exceptional
grass growing on the ground. Grass-like CdS consists of several immobilization onto ZnS/CdS surface. TEM image in Fig. 2A presents
nanorods with 80-100 nm long. With increasing Zn source to 0.3 the multibranched structures of ZnS/CdS consistent with the above
mmol and reducing Cd source to 0.7 mmol, the obtained field-emission scanning electron microscopy (FESEM) results and
Cd0.7Zn0.3G2 retained the multi-branched CdS structure on RGO that no remarkable Au nanocrystals are visible except rare discrete
sheets with few ZnS nanoparticles on the rod tips in Fig. S4D-F ones. Fig. 2B clearly gives the impression of small NPs with size of 4-
(ESI†). Continuously increasing Zn source to 0.5 mmol, ZnS 7 nm attached around nanorods, further monitored by high-angle
nanoparticles grew bigger on tips in final Cd0.5Zn0.5G2 structure, annular dark-field scanning TEM (HAADF-STEM) image in Fig. 2C.
clearly demonstrated by Fig. S4G-I (ESI†). When the amount of Zn XRD coupled with EDX data in Fig. S8-9 (ESI†) clearly demonstrate
source reached 0.7 and 0.8 mmol, Cd0.3Zn0.7G2 and Cd0.2Zn0.8G2 the presence of face-centered-cubic (fcc)-Au in Au2-Cd0.5Zn0.5G2. No
samples exhibited similar morphology in Fig. S5A-F (ESI†). CdS visible diffraction peaks of Au are observed for Au1-Cd0.5Zn0.5G2 due
nanorods became shorter caused by the lower Cd source than those to the low amount of Au NPs. In order to make clear the junction of

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CdS/ZnS, the HRTEM investigation of Au2-Cd0.5Zn0.5G2 was done. The recombination of photo-induced electron-hole pairs. By setting x =
domain marked by black circle in Fig. S10 (ESI†) shows the lattice 0.3 get the optimal Cd/Zn ratio, pristine Cd0.3Zn0.7G0 without RGO
−1 −1
spacing of 0.238 nm corresponding to (111) planes of fcc-Au phase. just reaches 1.34 mmol h g (Fig. S13A, ESI†). When the volume
Well-defined lattice structure is observed, displaying the good of GO increased to 1 mL, the hydrogen evolution rate of Cd0.3Zn0.7G1
−1 −1

Journal of Materials Chemistry A Accepted Manuscript

crystallinity of the sample. As shown in Fig. 2D, the spacing of 0.330 was enhanced to 3.60 mmol h g , twice higher than that of
and 0.309 nm results from (0002) of h-CdS and (111) of c-ZnS, Cd0.3Zn0.7G0. In case of 2 mL, Cd0.3Zn0.7G2 reaches the highest
−1 −1
respectively. The line scan spectrum of the TEM image in Fig. 2E hydrogen production rate of 4.48 mmol h g . Continual increase
testifies the Zn element mainly concentrating on the tip and Cd to 3 and 5 mL gives rise to the degraded activity. RGO exhibits
distributing on the stem, implying the heterostructure of ZnS/CdS. excellent electron transportation ability, favorably accelerating the
The HAADF-STEM and corresponding elemental mappings are electron separation from hole, but excessive amount of RGO will
shown in Fig. 2F-K, proving the homogeneous distribution of shielding the incident light and even cover the active site of
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respective elements in Au2-Cd0.3Zn0.7G2 and consistent with the photocatalyst.

FESEM/TEM observations, whose X-ray photoelectron spectroscopy
The amount of Au also exerts remarkable effect on the activity of
(XPS) analysis is present in Fig. S11 (ESI†). Based on the
products (see Fig. S13B, ESI†). With Z=2, Au2-Cd0.3Zn0.7G2 exhibited a
crystallographic relationship, CdS nanorods are growing −1 −1
highest rate of 9.96 mmol h g , comparable to many study about
preferentially along [0001]h axis, parallel to [111]c of c-ZnS. Fig.
the CdS-related photocatalyst (See Table S1, ESI†). As cocatalyst,
3A,B shows the projected atomic arrangement of crystal planes of
metallic Au is well-known electron collector and hole thus
(111)c for c-ZnS and (0002)h for h-CdS, displaying a similar
accumulates on surface of photocatalysts, realizing the separation
configuration. The spacings of the adjacent Cd atoms along [1000]h
of charge carriers. The long-term stability is also a principal factor to
and Zn atoms along [110]c are 4.140 and 3.825 Å with an
evaluate the photocatalysts. As shown in Fig. 4A, the long cycling
insignificant lattice mismatch of 7.6%, contributive to the epitaxial
behavior of several samples was tested. After continually producing
growth of (111) planes of c-ZnS on (0002) planes of h-CdS matrix in
hydrogen for 5 h, hydrogen was removed from the reaction system
Fig. 3C. By calculation based on the density function theory, the
by bubbling with high-purity N2 for 20 minutes and then the
isosurfaces of electron density near the interface of CdS/ZnS
photocatalyst was recycled. It’s remarkable to observe the stability
structure can be clearly observed (see Fig. 3D), showing a token of
during the 6 cycles lasting for 30 h, indicating the excellent lifetime
chemical bonding formation. The growth mode of c-CdS crystal on
of these as-fabricated heterostructured samples, especially Au2-
graphene is displayed along c axis in Fig. 3E,F.
Cd0.3Zn0.7G2. The excellence was mainly attributed to the timely
transferring of photogenerated charge carriers by coefficient noble-
metal Au and graphene. Moreover, the photocorrosion of CdS was
efficiently retarded.

In addition, it was found that fresh Cd0.3Zn0.7 displays the same

hydrogen production rate in initial 3 h in Fig. S13C (ESI†). However,
after the initial 1 h photocatalysis of Cd0.3Zn0.7G2, the rate is
dramatically enhanced in the second and tend to stabilize for the
third hour. That’s to say, as photocatalysis reaction proceeded, the
catalytic activity of Cd0.3Zn0.7G2 became higher. The similar
phenomenon was also observed in other pairs of CdxZny and
CdxZnyG2 (Fig. S13D, ESI†). To unveil the reason, Raman spectra
Fig. 3 (A,B) The projected atomic arrangement on (0002)h for h-CdS were detected in Fig. S14 (ESI†). Before photocatalysis, fresh
and (111)c for c-ZnS. (C,D) The side view of ZnS growth on CdS. (E,F) Cd0.3Zn0.7G2 has an ID/IG value of 1.18, which increased to 1.28 after
the projected and side scheme for growth model of h-CdS on cycling for 30 h, showing more defects existing due to further
19b,21
graphene. S, yellow; Cd, purple; Zn, grey; C, green. reduction of the RGO sheets. In the first two hours, the
photogenerated electrons partially reduced the remaining
For evaluation of performance of the samples prepared,
functional groups of graphene, favoring photogenerated carrier
photocatalytic hydrogen evolution tests were carried out using 0.35
charges to separate and contributing to the enhancement of H2
M Na2S and 0.25 M Na2SO3 as hole scavenger in water under
production rate in the initial 3 h.
irradiation of visible light (λ > 420 nm). We have explored the
variable relationship between H2 production rate and the Cd/Zn The UV-vis diffuse reflectance spectra of the related samples are
ratio in a series of CdxZn1-xG2 structures as shown in Fig. S12, where compared in Fig. 4B. The pure Cd1.0Zn0 displays a shoulder around
CdS/ZnS heterostructures exhibit improved H2 production rate 515 nm corresponding to the band gap of 2.41 eV. After integration
compared to pure Cd1.0Zn0G2 and Cd0Zn1.0G2. And Cd0.3Zn0.7G2 with ZnS, the absorption edge (shoulder) of heterostructure
shows a maximum hydrogen production rate of 4.50 mmol h−1 g−1, Cd0.3Zn0.7 exhibits an obvious blue shift to 480 nm corresponding to
which indicates the optimal content of ZnS in the heterostructures. bandgap of 2.59 eV, characteristic of type I heterojunction. After
As indicated by ZnS basically having no ability for hydrogen combination with graphene, Cd1.0Zn0G2 and Cd0.3Zn0.7G2 show
evolution under visible-light, the performance improvement dramatically-improved absorption intensity in visible light range,
demonstrated the significant roles of CdS and ZnS in inhibiting the suggesting the good light harvesting ability. PL spectra in Fig. 4C
give the similar trend that the peak of Cd1.0Zn0 at 570 nm is higher

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than Cd0.3Zn0.7 at 540 nm. Moreover, the PL peaks of Cd1.0Zn0G2 and

Cd0.3Zn0.7G2 exhibit almost unchanged position compared with the
counterparts before combination with graphene, but decreases
remarkably in intensity. The phenomenon displays that the

Journal of Materials Chemistry A Accepted Manuscript

recombination of photoexcited holes and electrons is well inhibited.
Further introduction of Au to the heterostructures makes the PL
peak of Au2-Cd0.3Zn0.7G2 drastically quenched, whose absorption is
enhanced during the whole visible light range in line with the result
given by the UV-vis diffuse reflectance spectra above. The
observation reasonably suggests that noble metal Au and graphene
cooperate to effectively suppress photogenerated electron-hole
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recombination. In addition, the electrochemical impedance

spectroscopy (EIS) commonly used to explore the charge transfer
processes from the electrolyte to electrode and the contact
interface of them, which also utilized to investigate the separation
efficiency of electron-hole pairs. In Figure S15 the Au2-Cd0.3Zn0.7G2
and Cd0.3Zn0.7G2 give significantly smaller semicircles compared with
Cd0.3Zn0.7, which indicates more efficient charge transfer over the
Au2-Cd0.3Zn0.7G2 and Cd0.3Zn0.7G2, especially the Au2-Cd0.3Zn0.7G2.
The EIS measurements consistent well with the hydrogen
production rate in our work.
The high H2 evolution rate of Au2-Cd0.3Zn0.7G2 can be explained by
the mechanism in Fig. 4D. In general, the transfer of photoinduced
charges follows type I heterojunction owing to the band structure Fig. 4 (A) The long-term cycling stability of H2 production over Cd0.3Zn0.7,
of natural valence band (VB) and conduction band (CB) of CdS and Cd0.3Zn0.7G2 and Au2-Cd0.3Zn0.7G2 for 30 h, (B,C) UV-vis diffuse
ZnS. But the obvious enhancement of H2 evolution rate implies the reflectance and PL spectra of Cd1.0Zn0, Cd0.3Zn0.7, Cd1.0Zn0G2, Cd0.3Zn0.7G2,
efficient separation of photogenerated charge carriers, similar with and Au2-Cd0.3Zn0.7G2. D) Schematic description of the photocatalytic
the results of previous reports about CdS/ZnS.7b,16,19a,22 Many evolution of H2.
intrinsic defects present in ZnS crystal include zinc vacancies (VZn),
sulfur vacancies (VS) and interstitial sulfur (IS) localized above the VB
of both ZnS and CdS. They work as acceptor states for holes in
Conclusions
CdS,23 which provides the effective hole transfer mechanism. On In summary, we firstly developed a facile one-pot hydrothermal
the other hand, the electrons on CB of CdS after photoinduction are method for preparing CdS/ZnS heterostructure on RGO sheets
immediately transported to the electron collector of Au due to the which provide abundant functional groups and large specific surface
deeper potential wells.7a Thus, Au NPs become electrons-enriched area for nucleation and growth of CdS crystals. The further
where the reduction of H+ to H2 can take place. Simultaneously, introduction of Au nanoaparticles enables the final composite a
electrons also can transfer to RGO sheets due to the lower potential composite with the advantages of heterostructured
of graphene/graphene- (-0.08 V)24 than CdS (-0.52 V). Hence, the semiconductor/semiconductor junction benefiting the hole transfer
graphene sheets not only act as electron collector but as and noble metal as well as graphene favorable for electron
transporter because of its excellent conductivity. The co-efficiency transportation. Some structural factors including the content of ZnS,
of Au coupled with RGO greatly accelerates electrons to move away Au and RGO have been explored for investigating the H2 evolution
from CdS and thus effectively prevents the recombination of activity. Au2-Cd0.3Zn0.7G2 shows a highest H2 production rate 9.96
−1 −1
electrons and holes. Therefore, great promotion of the separation mmol h g without visible decay more than 30 h. The composite
of photogenerated charge carriers distinctly benefits the H2 works well together to improve the separation and transfer
production activity. efficiencies of charge carriers, which can be demonstrated by PL
results. The multi-component structures are combined with several
favorable carriers’ separation strategies in one system, which can
be extended to other fields.

Conflicts of interest
There are no conflicts to declare.

Acknowledgements

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This work was supported by the National Natural Science Fund 23 W. Becker, A. Bard, J. Phys. Chem., 1983, 87, 4888.
of China (21371108). P. Wang acknowledges support from the 24 X. Wang, L. Zhi, K. Mullen, Nano Lett., 2008, 8, 323.
Recruitment Program of Gloabal Experts.

Journal of Materials Chemistry A Accepted Manuscript

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