Nano-Micro Letters

A Facile Self-assembly Synthesis of Hexagonal ZnO Nanosheet Filmsand Their Photoelectrochemical Properties

Bin Zhang1, Faze Wang1, Changqing Zhu1, Qiang Li1,

Jingnan Song1, Maojun Zheng1,2,*, Li Ma3, Wenzhong Shen1,2

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Nano-Micro Letters, April 2016, Volume 8, Issue 2, pp 137-142

First online: 15 October 2015 (Article)

DOI: 10.1007/s40820-015-0068-y

*Corresponding author. E-mail: mjzheng@sjtu.edu.cnFax: +86-021-54741040

 

Abstract

 


The schematic drawing of the experimental setup used for the fabrication of hexagonal ZnO nanosheet films.
Here, large-scale and uniform hexagonalzinc oxide (ZnO) nanosheet films were deposited onto indium tin oxide (ITO)-coated transparent conducting glass substrates via a facile galvanic displacement deposition process. Compared with other commonly used solution methods, this processavoids high temperature and electric poweras well as supporting agents to make it simple and cost-effective. The as-fabricated ZnO nanosheet films have uniform hexagonal wurtzite structure. The photoelectrochemical (PEC) cell based on ZnO nanosheet film/ITO photoelectrode was also fabricated and its performance was improved by optimizing the solution concentration. A higher photocurrent density of ~500 μAcm-2 under AM 1.5G simulated illumination of 100 mW cm-2 with zero bias potential (vs Ag/AgCl electrode) was obtained, which may ascribe to the increased surface-to-volume ratio of disordered ZnO nanosheet arrays.Our developed method may be used to deposit other oxide semiconductors, and the ZnO nanosheet film/ITO PEC cell can be used to design low-cost optoelectronic and photoelectrochemical devices.

 

Keywords

Zinc oxide;Nanosheet film; Self-assemble; Galvanic displacement method; Photoelectrochemical property

 

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Introduction

 

Over the past decades, there have been an increasing scientific interest in oxide semiconductors (such as TiO2, ZnO, Fe2O3, CuO, NiO and so on) [1-3], because of their numerous potential technological applications, including photovoltaic device [4], lithium ion battery [5], photocatalysis and optoelectronic device[6, 7]. Among the oxide semiconductors, ZnO as a prototypical n-type conducting oxidehas attracted considerable attentions for wide usages in piezoelectric device, ultraviolet optoelectronics detectors [8, 9], low-cost dye-sensitized solar cells [10], gas sensors [11, 12], photocatalysis and photoelectrochemical (PEC) devices [13, 14]. Most of these applications are based on the advantages of its abundance, low cost, non-toxicity, chemical stability and the possibility of growing ordered nanostructures, and strong exciton binding energy [15]. Especially, nanostructured ZnO exhibits enhanced performance and provided an ideal system to study the influence of surface effects and interface science on photoelectrochemical properties due to their large surface-to-volume ratios[16-18].

To date, ZnO and other nanostructured materials have been assembled and studied by various methods and means [19-22], including magnetron sputtering[23], chemical vapor deposition[24], hydrothermalprocess [25], electrochemical deposition [26-28], electroless deposition [29, 30], and other combination of methods [31]. Among all these techniques, electroless deposition presents several advantages such as low cost, large-scale deposition and low-temperature processing.Here, we explored a facile solution based galvanic displacement deposition technique to self-assembly synthesis uniform hexagonal ZnO nanosheet film on ITO glass substrate under ambient conditions. ZnO nanosheet film/ITO PEC cell andits photoelectrochemical property were also investigated.

 

Experimental Details

 

Synthesis of the ZnO nanosheet films

Compared with other common electrodeposition methods, an electroless deposition process was employed to fabricate ZnO nanosheets.A typical galvanic cell system with two half cell (A and B)was used to generate a current by coupling oxidation and reduction reactions in a spontaneous process, in which the A cell solution is 5-15 mM ZnSO4 and the B cell solution is 0.25 M NaOH. The two half cells were connected by a porous salt bridge that supplied ions to maintain charge neutrality during current flow. The galvanic cell deposition system is composed of Al sheet (99.99 % purity) and ITO conducting glass (sheet resistance of 10Ω cm-2), which acted as anode and cathode, respectively. The two electrodes were short-circuited externally through a metal copper wire. Before deposition, 4 cm × 2 cm Al sheet and ITO glass were respectively cleaned in acetone, ethanol and deionized water for 5 min. Then, the Al sheet was immerged into A cell solution and the ITO glass was immerged into B cell solution without stirring and oxygen gas bubbling at room temperature. In order to obtain higher crystal quality, the as-prepared sampleswere annealed at 550 °C for 60 min with the increasing rate of 10 °C min-1 in an air atmosphere.

Characterization

The surface morphology of the as-deposited ZnO nanosheet films were obtained by field emission scanning electron microscopy (FE-SEM; FEI Sirion 200, Holland). A D8 ADVANCE DA VINCI X-ray diffractometer (XRD, Bruker, German) was employed to verify the crystal structure of the samples using Cu Kα radiation (λ=0.15418 nm) with a scanning rate of 5°min-1. The photoluminescence (PL) spectrum of the as-resulting ZnO films were obtained using the Jobin Yvon LabRam HR 800 UV system with a 325nm laser at room temperature The UV-visble spectra of the ZnO samples were obtained through UV-Vis spectrophotometer (PerkinElmer Lambda 950, America).

PEC Cell Preparation and PEC Characterization

PEC cell was fabricated by placing a copper wire onto a bare portion of the ITO conducting substrate and securing with high purity silver conducting glue. Then, the part active area of ZnO nanosheet films were sealed with epoxy resin leaving an exposed working electrode surface area of 1 cm×1 cm. An electrochemical workstation (Princeton Applied Research, PARSTAT 4000, America) was used to study the photoelectrochemical property of the samples. The photoelectrochemical experiment was performed in a conventional three electrode, in which the resulting ZnO nanosheet film /ITO substrate acted as working electrode (illuminating area of 1 cm2 ), a platinum net (surface area of 1 cm2) as counter electrode, and an Ag/AgCl as reference electrode. The PEC experiments were carried out in a mixture solution of 0.35 M Na2S and 0.25M Na2SO3 under AM 1.5G (100 mW cm−2) simulated illumination, which was provided by a 300 W xenon lamp (Beijing Perfectlight Technology, PLS-SXE300C, China) equipped with a AM 1.5 filter. The illumination intensity was measured with a solar simulator spectroradiometer (EKO instrument, LS-100, Japan).

 

Results and Discussion

 

The schematic drawing of the experimental setup used for the fabrication ZnO nanosheet films was shown in Fig. 1. When the Al electrode,connected with the ITO glass externally,was dipped into the NaOH solution, Al3+ ions formed in the solution due to the dissolution ofAl foil.Then, the released electrons moved through the externally short-circuited path to the ITO electrode. At the same time, the electron prompted the basic electrochemical reduction ofoxygen (O2) in the aqueous solution,and thenleaded to the formation of OH ions on ITO substrate surface. Finally, the Zn2+ ions in the solution were attracted by the corresponding OH ions on the ITO surface, an intermediate Zn(OH)2formedand rapidly converted to ZnO. The growth mechanism of ZnO nanosheet filmhas similarelectrochemical reaction with the electrodeposition [32]. The reactions may be as followings:

The schematic drawing of the experimental setup used for the fabrication of hexagonal ZnO nanosheet films.

The schematic drawing of the experimental setup used for the fabrication of hexagonal ZnO nanosheet films.

Anode: Al0 (s) → Al3+ (aq) + 3e-

Cathode: O2 + 2H2O (aq) + 4e- → 4OH-

Zn2+ (aq) + 2OH- → Zn(OH)2→ ZnO (s) + H2O

In the process of nanosheet film formation, ZnO nanocrystals were primarily generatedand then they were self-assembled into ordered hexagon nanostructure. These staggered arrangement nanosheet formed ZnO film in the substrate surface finally. Actually, semiconductor self-assembly is a complex phenomenon that depends on the interplay of several physical factors and competing interactions of different nature. A thorough understanding of the self-assembly mechanism of nanocrystals to organize into ordered nanostructure is one of the key of future nanoscience [33].

Figure 2 shows FESEM images of the top and side view of the hexagonal ZnO nanosheet films grown on the ITO substrate at 5 and 10mM ZnSO4 aqueous solution for 2 h, and annealed at 550 °C for 1 h. One can see that the ZnO had quite perfect hexagon and large-scale irregular arrangement. The samplesshown in Fig. 2a and Fig. 2b were respectively grown at 5mM ZnSO4 solution and 10mM ZnSO4. It can be seen that the concentration of ZnSO4 aqueous solution plays an important role in the size and thickness of hexagonal ZnO nanosheets, as well as the surface-to-volume ratios.

FESEM images of the as-prepared hexagonal ZnO nanosheet films grown on the ITO coated glass substrate with different concentration ZnSO4.a 5mM and b 10mM, top view. c 10mM, side view.

FESEM images of the as-prepared hexagonal ZnO nanosheet films grown on the ITO coated glass substrate with different concentration ZnSO4.a 5mM and b 10mM, top view. c 10mM, side view.

Figure 3 showsXRD pattern of the hexagonal ZnO nanosheet films on ITO by electrolessdepositing at 7.5 mM ZnSO4 for 2 h under room temperature and post-annealingat 550 °C for 1 h in open air conditions. All diffraction peaks correspond to the standard diffraction of a hexagonal wurtzite ZnO crystal (JCPDS 36-1451) [34]. The major diffraction peaks have sharp features, corresponding to the (100), (002), (101), (102), (110), (103), and (112) planes, which is due to the disorder arrangement of ZnO nanosheets on the ITO. At the same time, the peaks from the ITO conducting substrates were observed as well.

XRD pattern of the as-annealed hexagonal ZnO nanosheet film at 550 C in open air conditions.

XRD pattern of the as-annealed hexagonal ZnO nanosheet film at 550 C in open air conditions.

Figure 4 exhibits the representative room temperature PL spectrum of the ZnO nanosheet films grown in 7.5mM ZnSO4 aqueous solution and annealed at 550 °C for 1 h. A laser with wavelength of 325 nm was used as the excitation source. The strong UV emission peak at about 390nm could be usually attributed to the free excitons emission from the wide band gap ZnO [35]. The lower broad peak around 500 nm is usually considered to be the recombination of a photogenerated hole with the single ionized charged state of the defect in ZnO and could be related to the surface oxygen vacancies of the ZnO because the ZnO nanosheet films have much high surface-to-volume ratios [36]. The PL spectrum result indicates that the as-prepared ZnO havefew defects[37]. The inset image in Fig. 4 showsthe UV-Vis absorption spectrum of this sample, indicating its band gap at nearly 3.25 eV. The band gap values of ZnO film was calculated by Tauc plot[38, 39].

Room temperature photoluminescence spectrum of the as-prepared ZnO nanosheet film. Excitation wavelength: 325 nm. The inset picture is the UV-Vis absorption spectrum of the same sample.

Room temperature photoluminescence spectrum of the as-prepared ZnO nanosheet film. Excitation wavelength: 325 nm. The inset picture is the UV-Vis absorption spectrum of the same sample.

The photoelectrochemical property of ZnO nanosheet thin film/ITO electrode was measured with an electrochemical workstation. All PEC measurement was carried out in a mixture solution of 0.35 M Na2S and 0.25M Na2SO3 under AM 1.5G (100 mW cm−2). Figure 5 showsthe photoelectrochemical property of ZnO nanosheet thin film/ITO electrode. Its photocurrent was investigated under a bias voltage of 0 V (vs Ag/AgCl) with a light on−off interval of 20 s, as shown in Fig. 5a. All PEC cell exhibits significant photoresponse under a bias voltage of 0 V (vs Ag/AgCl), but the sample fabricated at 7.5mM solution has superior characteristics with a higher photocurrent of 500μAcm-2. The photocurrent density of the photoelectrode varies with the different growth concentration ofZnSO4aqueous solution, which may be related to the resistance and surface-to-volume ratio of the samples that could affect the light absorption. Linear sweep voltammograms (LSV) curves were recorded for the 7.5mM sample in the dark and at 100 mW cm-2 (AM 1.5) with a scan rate of 10 mVs-1 in the applied potentials from -1 to +1 V (vs Ag/AgCl), as shown in Fig. 5b. The dark scan showsa very small current density in the range of 10 μAcm-2, whereas under light illuminationa pronounced photocurrent density was observed, implying efficient charge separation and transfer in this nanostructured ZnO. Figure 5c showsthe achronoamperometric plots of the Zno/ITO electrode for about 1 h, which indicated that the photoelectrochemical property was fairly stable under illumination. The photocurrent did not obviously decreased that is very important for the development of practical PEC cells.

The photoelectrochemical properties of the ZnO nanosheet thin film /ITO electrode. a Chronoamperometry measurements at zero bias potential (vs Ag/AgCl electrode) under chopped light illumination with a light on−off interval of 20 s. b LSV curves recorded for the 7.5 mM sample with a scan rate of 10 mV s-1 in the applied potentials from -1 to +1 V (vs Ag/AgCl ). c The J−T stability of electrode. All PEC experiments were carried out in a mixture solution of 0.35 M Na2S and 0.25 M Na2SO3 under AM 1.5 G (100 mW cm−2).

The photoelectrochemical properties of the ZnO nanosheet thin film /ITO electrode. a Chronoamperometry measurements at zero bias potential (vs Ag/AgCl electrode) under chopped light illumination with a light on−off interval of 20 s. b LSV curves recorded for the 7.5 mM sample with a scan rate of 10 mV s-1 in the applied potentials from -1 to +1 V (vs Ag/AgCl ). c The J−T stability of electrode. All PEC experiments were carried out in a mixture solution of 0.35 M Na2S and 0.25 M Na2SO3 under AM 1.5 G (100 mW cm−2).

In order to further understand the photoelectrochemical property of ZnO nanosheet films, the UV-Vis reflectance spectra were also measured by PerkinElmer Lambda 950 UV-Vis spectrophotometer. Figure 6 shows the UV-Vis reflection spectraof the ZnO nanosheet films grown at different concentration of ZnSO4. It can be seen thatthe 7.5mM sample had a maximumultraviolet absorption compared to other samples.The reflectance spectraresult was consistent with the photoelectrochemical result.These results clearly demonstrated that the PEC performancestrongly depended on the morphology of ZnO andcould be optimizedthrough controlling the material growth condition.

Reflectance spectra of ZnO sheet films on ITO glass grown at different concentration ZnSO4. a 5 mM, b 7.5 mM, c 10 mM, d 15 mM.

Reflectance spectra of ZnO sheet films on ITO glass grown at different concentration ZnSO4. a 5 mM, b 7.5 mM, c 10 mM, d 15 mM.

 

Conclusion

 

In this paper, we had presented a simple and highly efficient solution-based method to prepare large-scales hexagonal ZnO nanosheet films using a galvanic displacement reaction. The advantages of this solution-processing technique are its simplicity as well as it need not electric power and supporting agents. The hexagonal ZnO nanosheet films prepared by this method exhibited excellent PEC properties. These results indicatedthe ZnO nanosheet film could be applied in low cost, high-performance photoelectrochemical devices or other application fields.

 

Acknowledgments

 

We were grateful to Linna.Pang for assistance with PL spectrum. This work was supported by National Major Basic Research Project of 2012CB934302, National 863 Program 2011AA050518, the Natural Science Foundation of China (grant NO.11174197,11574203 and 61234005).

 

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References

 

[1] S.T. Kochuveedu, Y.H. Jang, D.H. Kim, A study on the mechanism for the interaction of light with noble metal-metal oxide semiconductor nanostructures for various photophysical applications. Chem. Soc. Rev. 42(21), 8467-8493 (2013). doi:10.1039/c3cs60043b

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[3] E. Comini, C. Baratto, G. Faglia, M. Ferroni, A. Vomiero, G. Sberveglieri, Quasi-one dimensional metal oxide semiconductors: Preparation, characterization and application as chemical sensors. Prog. Mater. Sci. 54(1), 1-67 (2009). doi:10.1016/j.pmatsci.2008.06.003

[4] M. Lira-Cantu, F.C. Krebs, Hybrid solar cells based on MEH-PPV and thin film semiconductor oxides (TiO2, Nb2O5, ZnO, CeO2 and CeO2–TiO2): Performance improvement during long-time irradiation. Sol. Energ. Mat. Sol. C90(14), 2076-2086 (2006). doi:10.1016/j.solmat.2006.02.007

[5] K.T. Park, F. Xia, S.W. Kim, S.B. Kim, T. Song, U. Paik, W.I. Park, Facile synthesis of ultrathin ZnO nanotubes with well-organized hexagonal nanowalls and sealed layouts: Applications for lithium ion battery anodes. J. Phys. Chem. C 117(2), 1037-1043 (2013). doi:10.1021/jp310428r

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Citation Information

Bin Zhang, Faze Wang, Changqing Zhu, Qiang Li, Jingnan Song, Maojun Zheng, Li Ma, Wenzhong Shen, A FacileSelf-assembly Synthesis of Hexagonal ZnO Nanosheet Filmsand Their Photoelectrochemical Properties. Nano-Micro Lett. April 2016, Volume 8, Issue 2, pp 137-142. http://dx.doi.org/10.1007/s40820-015-0068-y

History

Received: 13 July 2015 / Accepted: 23 September 2015


Additional Info

  • Type of Publishing: JOUR - Journal
  • Title:

    A FacileSelf-assembly Synthesis of Hexagonal ZnO Nanosheet Filmsand Their Photoelectrochemical Properties

  • Author: Bin Zhang, Faze Wang, Changqing Zhu, Qiang Li, Jingnan Song, Maojun Zheng, Li Ma, Wenzhong Shen
  • Year: 2015
  • Volume: 7
  • Issue: ?
  • Journal Name: Nano-Micro Letters
  • Publisher: OPEN ACCESS HOUSE SCIENCE & TECHNOLOGY
  • ISSN: 2150-5551
  • URL: http://dx.doi.org/10.1007/s40820-015-0068-y
  • Abstract:

    Here, large-scale and uniform hexagonalzinc oxide (ZnO) nanosheet films were deposited onto indium tin oxide (ITO)-coated transparent conducting glass substrates via a facile galvanic displacement deposition process. Compared with other commonly used solution methods, this processavoids high temperature and electric poweras well as supporting agents to make it simple and cost-effective. The as-fabricated ZnO nanosheet films have uniform hexagonal wurtzite structure. The photoelectrochemical (PEC) cell based on ZnO nanosheet film/ITO photoelectrode was also fabricated and its performance was improved by optimizing the solution concentration. A higher photocurrent density of ~500 μAcm-2 under AM 1.5G simulated illumination of 100 mW cm-2 with zero bias potential (vs Ag/AgCl electrode) was obtained, which may ascribe to the increased surface-to-volume ratio of disordered ZnO nanosheet arrays.Our developed method may be used to deposit other oxide semiconductors, and the ZnO nanosheet film/ITO PEC cell can be used to design low-cost optoelectronic and photoelectrochemical devices.

  • DOI: 10.1007/s40820-015-0068-y