CN102220615B - Method for preparing CdS/ZnO nanotube array photoelectrode - Google Patents

Method for preparing CdS/ZnO nanotube array photoelectrode Download PDF

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CN102220615B
CN102220615B CN2011101248570A CN201110124857A CN102220615B CN 102220615 B CN102220615 B CN 102220615B CN 2011101248570 A CN2011101248570 A CN 2011101248570A CN 201110124857 A CN201110124857 A CN 201110124857A CN 102220615 B CN102220615 B CN 102220615B
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zno
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CN102220615A (en
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师文生
齐小鹏
佘广为
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Technical Institute of Physics and Chemistry of CAS
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Abstract

The invention belongs to the technical field of semi-conductor nanometer material application, in particular to a method for preparing CdS/ZnO nanotube array photoelectrode. The method takes conductive glass loaded with a ZnO nanotube array as a work electrode, platinum sheets as a counter electrode, saturated calomel electrode as a reference electrode, and dimethyl sulfoxide solution containing S powder and CdCl2 as electrolyte; and the CdS/ZnO nanotube array photoelectrode is prepared by applying constant current between the work electrode and the counter electrode so as to electro-chemically deposit a CdS film on the ZnO nanotube. The CdS/ZnO nanotube array photoelectrode has an excellent performance in the field of hydrogen production through photoelectrical chemical decomposition water.

Description

The method for preparing CdS/ZnO nano-tube array optoelectronic pole
Technical field
The invention belongs to the semiconductor nano material applied technical field, relate in particular to the method that a kind of Applied Electrochemistry technology prepares CdS/ZnO nano-tube array optoelectronic pole.
Background technology
ZnO is a kind of good photoelectrocatalysimaterial material, has advantages such as photoresponse is good, carrier mobility is high, with low cost, has in fields such as photovoltaic device, senser element, conductor photocatalysis widely to use.Advantages such as the One-Dimensional ZnO nanostructure is big owing to its specific surface area, reflection preventing ability good, the photo-generated carrier capacity gauge is good show excellent performance (Nano Lett., 2009,9,2331.) in photoelectrochemistry hydrogen production by water decomposition field.As a kind of wide band gap semiconducter (3.34eV), the maximum limitation of ZnO optoelectronic pole is that its photoresponse wave band at ultraviolet region, causes it can only utilize 4～5% solar energy.CdS is a kind of narrow gap semiconductor, has good photoresponse ability at visible light wave range, in photocatalytic degradation pollutent, hydrogen production by water decomposition (Nano Lett., 2010,10,1088.), photoelectrochemical cell field by sufficient research.It is reported; The composite structure that CdS and ZnO form can form second type of heterojunction structure, and this energy band structure can help the right separation in light induced electron-hole in the electrode materials, thereby has reduced the spontaneous compound of photo-generated carrier; Raising is to the utilization ratio (Chem.Commun. of photo-generated carrier; 2009,23,3452.).Even so, because being compounded in the very short time of photo-generated carrier takes place, still the photo-generated carrier of quite a few falls through recombination losses, thereby the ZnO/CdS system also has very big room for promotion on performance.
The ZnO nanotube has been proved in area of solar cell can play good carrier collecting action (J.Phys.Chem.A; 2009,113,4015.); But, also be not studied in the matrix material optoelectronic pole system that especially ZnO/CdS forms in the photolysis water hydrogen field.Simultaneously, the preparation of CdS photoactive layer at present also has deficiencies such as loaded down with trivial details such as preparation technology, that preparation time is long, and CdS contacts still with the electricity of ZnO and has much room for improvement.Therefore; Applying nano pipe array improves the collection to photo-generated carrier as the characters and appearances of ZnO material; Improve CdS/ZnO electricity contact at the interface with electrochemical method as the preparation means of CdS photoactive layer, can improve the photoelectrochemical behaviour of ZnO/CdS optoelectronic pole greatly.
Summary of the invention
The method that the purpose of this invention is to provide a kind of CdS/ZnO of preparation nano-tube array optoelectronic pole.
Applied Electrochemistry of the present invention technology, with the conductive glass that is loaded with the ZnO nano-tube array as working electrode, with platinized platinum as counter electrode, with SCE as reference electrode; To contain S powder and CdCl 2Dimethyl sulphoxide solution as electrolytic solution, through to applying constant current between described working electrode and the counter electrode, electrochemical deposition goes out the CdS film on the ZnO nanotube, thereby makes CdS/ZnO nano-tube array optoelectronic pole.This CdS/ZnO nano-tube array optoelectronic pole shows excellent performance in photoelectrochemistry hydrogen production by water decomposition field.
The method of the CdS/ZnO of preparation nano-tube array optoelectronic pole of the present invention may further comprise the steps:
(1) preparation of ZnO nano-tube array: containing 5mM Zn (Ac) 2The temperature of (zinc acetate) and 0.1M KCl is in 85 ℃ the deionized water solution, as working electrode, as counter electrode, to form three-electrode system with SCE as reference electrode with platinized platinum with clean conductive glass; Described working electrode is applied-constant voltage of 1.0V (with respect to SCE), on described conductive glass, obtain the ZnO nanometer stick array; Having the conductive glass substrate of ZnO nanometer stick array to be soaked in the temperature that contains 0.2M KOH growth is in 85 ℃ the deionized water solution (preferably soaking about 1 hour), because KOH makes the ZnO nano-tube array to the selective etch effect of ZnO;
(2) galvanic deposit of CdS: containing S powder and CdCl 2Dimethyl sulphoxide solution in, the ZnO nano-tube array for preparing with step (1) as counter electrode, is formed three-electrode system with SCE as reference electrode with platinized platinum as working electrode; Through to applying constant current between described working electrode and the counter electrode, on described ZnO nanotube, deposit the CdS film, described working electrode is taken out from solution, clean, with rare gas element (like exsiccant N 2) dry up, obtain described CdS/ZnO nano-tube array optoelectronic pole.
In order to improve between the CdS particle; And CdS contacts with electricity between the ZnO, can further carry out the post-processed of optoelectronic pole to the CdS/ZnO nano-tube array optoelectronic pole that obtains: the CdS/ZnO nano-tube array optoelectronic pole that step (2) is prepared in retort furnace in 350 ℃ of high temperature annealings 1 hour.
Described conductive glass is ito glass or FTO glass.
Described S powder and the CdCl of containing of step (2) 2The temperature of dimethyl sulphoxide solution be 75～95 ℃.
Described S powder and the CdCl of containing of step (2) 2Dimethyl sulphoxide solution in the concentration of S powder be 0.01～0.2M, CdCl 2Concentration be 0.005～0.02M.
Step (2) is described to be 1～4mA/cm to the electric current that applies between working electrode and the counter electrode 2
The described cleaning of step (2) is that to use temperature successively be 85 ℃ dimethyl sulphoxide solution, acetone soln, deionized water rinsing.
CdS/ZnO nano-tube array optoelectronic pole of the present invention, its meliority is: be because nano-tube array to the excellent antireflective effect of incident light, can improve the absorption of optoelectronic pole to luminous energy on the one hand; Be because the size (40nm) of ZnO nanotube tube wall more approaches minority carrier (hole) diffusion length of (perhaps less than) ZnO material on the other hand, thereby can improve collection most photo-generated carriers (electronics).
Description of drawings
Fig. 1. the scanning electron microscope diagram sheet of the ZnO nanometer stick array of the embodiment of the invention 1 preparation.
Fig. 2. the scanning electron microscope diagram sheet of the ZnO nano-tube array of the embodiment of the invention 1 preparation.
Fig. 3. the scanning electron microscope diagram sheet of the CdS/ZnO nano-tube array of the embodiment of the invention 1 preparation.
Fig. 4. the scanning electron microscope diagram sheet of the CdS/ZnO nano-tube array of the embodiment of the invention 2 preparations.
Fig. 5. the scanning electron microscope diagram sheet of the CdS/ZnO nano-tube array of the embodiment of the invention 3 preparations.
Fig. 6. the scanning electron microscope diagram sheet of the CdS/ZnO nanometer stick array of Comparative Examples preparation.
Fig. 7. the CdS/ZnO nanotube transmission electron micrograph of the embodiment of the invention 3 preparations.
Fig. 8. the ZnO nano-tube array (ZNT) of the embodiment of the invention 1 preparation, the X-ray diffraction spectrum before and after the annealing of the CdS/ZnO nano-tube array of embodiment 3 preparations.
Fig. 9. the ZnO nano-tube array (ZNT) of the embodiment of the invention 1 preparation, the CdS/ZnO nano-tube array (CdS/ZNT) of embodiment 3 preparations, the uv-visible absorption spectroscopy of the CdS/ZnO nanometer stick array (CdS/ZNR) of Comparative Examples preparation.
Figure 10. in the embodiment of the invention 4; ZnO nano-tube array (ZNT) to the embodiment of the invention 1 preparation; The CdS/ZnO nano-tube array (CdS/ZNT) of embodiment 3 preparations, the photoelectrochemistry hydrogen manufacturing test that the CdS/ZnO nanometer stick array (CdS/ZNR) of Comparative Examples preparation carries out.
Embodiment
Embodiment 1.
Containing 5mM Zn (Ac) 2With the temperature of 0.1M KCl be in 85 ℃ the deionized water solution, as working electrode, as counter electrode, form three-electrode system as reference electrode with the FTO glass that cleans up with SCE with platinized platinum; To described working electrode apply-1.0V (with respect to SCE), total time are 1 hour constant voltage, on described ito glass, prepare the ZnO nanometer stick array, the scanning electron microscope diagram sheet is as shown in Figure 1; There is the ito glass substrate of ZnO nanometer stick array to be soaked in the temperature that contains 0.2M KOH growth and is in 85 ℃ the deionized water solution 1 hour, makes the ZnO nano-tube array that the scanning electron microscope diagram sheet is as shown in Figure 2.As the S powder that contains 0.01M of electrolytic solution and the CdCl of 0.005M 2Temperature be in 75 ℃ the dimethyl sulphoxide solution, as working electrode, as counter electrode, form three-electrode system as reference electrode with the ZnO nano-tube array for preparing with SCE with platinized platinum; Between described working electrode and described counter electrode, apply 1mA/cm 2, total time is 15 minutes continuous current, on described ZnO nanotube, deposits the CdS film, obtains CdS/ZnO nano-tube array optoelectronic pole.
The CdS/ZnO nano-tube array optoelectronic pole for preparing is taken out from electrolytic solution, and using temperature successively is 85 ℃ of dimethyl sulphoxide solutions, acetone soln, deionized water rinsing; Use exsiccant N then 2Dry up, in retort furnace, carry out 350 ℃ high temperature annealing 1 hour, the scanning electron microscope diagram sheet of gained CdS/ZnO nano-tube array is as shown in Figure 3.
Embodiment 2.
Containing 5mM Zn (Ac) 2With the temperature of 0.1M KCl be in 85 ℃ the deionized water solution, as working electrode, as counter electrode, form three-electrode system as reference electrode with the ito glass that cleans up with SCE with platinized platinum; Described working electrode is applied-1.0V (with respect to SCE), and total time is 1 hour a constant voltage, on described ito glass, prepares the ZnO nanometer stick array; Having the ito glass substrate of ZnO nanometer stick array to be soaked in the temperature that contains 0.2M KOH growth is in 85 ℃ the deionized water solution 1 hour, makes the ZnO nano-tube array.As the S powder that contains 0.2M of electrolytic solution and the CdCl of 0.02M 2Temperature be in 85 ℃ the dimethyl sulphoxide solution, as working electrode, as counter electrode, form three-electrode system as reference electrode with the ZnO nano-tube array for preparing with SCE with platinized platinum; Between described working electrode and described counter electrode, apply 4mA/cm 2, total time is 5 minutes a continuous current, on described ZnO nanotube, deposits the CdS film, obtains CdS/ZnO nano-tube array optoelectronic pole.
The CdS/ZnO nano-tube array optoelectronic pole for preparing is taken out from electrolytic solution, and using temperature successively is 85 ℃ of dimethyl sulphoxide solutions, acetone soln, deionized water rinsing; Use exsiccant N then 2Dry up, in retort furnace, carry out 350 ℃ high temperature annealing 1 hour, the scanning electron microscope diagram sheet of gained CdS/ZnO nano-tube array is as shown in Figure 4.
Embodiment 3.
Containing 5mM Zn (Ac) 2With the temperature of 0.1M KCl be in 85 ℃ the deionized water solution, as working electrode, as counter electrode, form three-electrode system as reference electrode with the ito glass that cleans up with SCE with platinized platinum; Described working electrode is applied-1.0V (with respect to SCE), and total time is 1 hour a constant voltage, on described ito glass, prepares the ZnO nanometer stick array; Having the ito glass substrate of ZnO nanometer stick array to be soaked in the temperature that contains 0.2M KOH growth is in 85 ℃ the deionized water solution 1 hour, makes the ZnO nano-tube array.As the S powder that contains 0.1M of electrolytic solution and the CdCl of 0.01M 2Temperature be in 95 ℃ the dimethyl sulphoxide solution, as working electrode, as counter electrode, form three-electrode system as reference electrode with the ZnO nano-tube array for preparing with SCE with platinized platinum; Between described working electrode and described counter electrode, apply 2mA/cm 2, total time is 5 minutes a continuous current, on described ZnO nanotube, deposits the CdS film, obtains CdS/ZnO nano-tube array optoelectronic pole.
The CdS/ZnO nano-tube array optoelectronic pole for preparing is taken out from electrolytic solution, and using temperature successively is 85 ℃ of dimethyl sulphoxide solutions, acetone soln, deionized water rinsing; Use exsiccant N then 2Dry up, in retort furnace, carry out 350 ℃ high temperature annealing 1 hour, the scanning electron microscope diagram sheet of gained CdS/ZnO nano-tube array is as shown in Figure 5; The transmission electron micrograph of CdS/ZnO nanotube is as shown in Figure 7; X-ray diffraction spectrum before and after the annealing of CdS/ZnO nano-tube array is shown in Fig. 8 institute.
Comparative Examples
Containing 5mM Zn (Ac) 2With the temperature of 0.1M KCl be in 85 ℃ the deionized water solution, as working electrode, as counter electrode, form three-electrode system as reference electrode with the ito glass that cleans up with SCE with platinized platinum; Described working electrode is applied-1.0V (with respect to SCE), and total time is 1 hour a constant voltage, on described ito glass, prepares the ZnO nanometer stick array.As the S powder that contains 0.1M of electrolytic solution and the CdCl of 0.01M 2Temperature be in 95 ℃ the dimethyl sulphoxide solution, as working electrode, as counter electrode, form three-electrode system as reference electrode with the ZnO nanometer stick array for preparing with SCE with platinized platinum; Between described working electrode and described counter electrode, apply 2mA/cm 2, total time is 5 minutes a continuous current, on described ZnO nanometer rod, deposits the CdS film, obtains CdS/ZnO nanometer stick array optoelectronic pole.
The CdS/ZnO nanometer stick array optoelectronic pole for preparing is taken out from electrolytic solution, and using temperature successively is 85 ℃ dimethyl sulphoxide solution, acetone soln, deionized water rinsing; Use exsiccant N then 2Dry up, in retort furnace, carry out 350 ℃ high temperature annealing 1 hour, the scanning electron microscope diagram sheet of gained CdS/ZnO nanometer stick array is as shown in Figure 6.
Embodiment 4.
Photoelectrochemistry hydrogen manufacturing test: as a comparison with the ZnO nano-tube array that do not deposit CdS, CdS/ZnO nanometer stick array.Test condition: to contain 1M NaS 2Deionized water solution as electrolytic solution, be 100mW/cm with intensity 2The xenon lamp directional light that sees through AM 1.5 spectral filters as light source; With platinized platinum as counter electrode; SCE is as reference electrode; The blank ZnO nano-tube array (ZNT) for preparing with embodiment 1 respectively, the CdS/ZnO nano-tube array among the embodiment 3, the CdS/ZnO nanometer stick array in the Comparative Examples are made the voltage-to-current curved scanning as working electrode, and voltage sweep speed is 10mV/s.Fig. 9 is the uv-visible absorption spectrum of three different samples, can be found out by Fig. 9, compares with the blank ZnO nano-tube array of embodiment 1 preparation, and the CdS/ZnO nano-tube array among the embodiment 3 strengthens in the absorption of visible light wave range to light greatly; And for the CdS/ZnO nanometer stick array in the Comparative Examples, the CdS/ZnO nano-tube array has better optical absorption.Figure 10 is the photoelectrochemical behaviour test curve of three different samples; Can be found out by Figure 10: the CdS/ZnO nano-tube array optoelectronic pole among the embodiment 3 has high photoelectrochemistry electric current than the CdS/ZnO nanometer stick array optoelectronic pole in the Comparative Examples; Both are in 0 voltage (with respect to SCE), and electric current is respectively 14.27mA/cm 2, 7.27mA/cm 2, show that CdS/ZnO nano-tube array optoelectronic pole has better photoelectrochemistry hydrogen manufacturing performance.

Claims (4)

1. a method for preparing CdS/ZnO nano-tube array optoelectronic pole is characterized in that, described method may further comprise the steps:
(1) preparation of ZnO nano-tube array: containing 5mM Zn (Ac) 2With the temperature of 0.1M KCl be in 85 ℃ the deionized water solution, as working electrode, as counter electrode, form three-electrode system as reference electrode with clean conductive glass with SCE with platinized platinum; Described working electrode is applied-constant voltage of 1.0V, on described conductive glass, obtain the ZnO nanometer stick array; Having the conductive glass substrate of ZnO nanometer stick array to be soaked in the temperature that contains 0.2M KOH growth is in 85 ℃ the deionized water solution, makes the ZnO nano-tube array;
(2) galvanic deposit of CdS: containing S powder and CdCl 2Dimethyl sulphoxide solution in, the ZnO nano-tube array for preparing with step (1) as counter electrode, is formed three-electrode system with SCE as reference electrode with platinized platinum as working electrode; Through to applying constant current between described working electrode and the counter electrode; On described ZnO nanotube, deposit the CdS film, described working electrode is taken out from solution, clean; Dry up with rare gas element, obtain described CdS/ZnO nano-tube array optoelectronic pole;
Described S powder and the CdCl of containing of step (2) 2The temperature of dimethyl sulphoxide solution be 75～95 ℃;
Described S powder and the CdCl of containing of step (2) 2Dimethyl sulphoxide solution in the concentration of S powder be 0.01～0.2M, CdCl 2Concentration be 0.005～0.02M;
Step (2) is described to be 1～4mA/cm to the electric current that applies between working electrode and the counter electrode 2
2. method according to claim 1 is characterized in that: described conductive glass is ito glass or FTO glass.
3. method according to claim 1 is characterized in that: the described cleaning of step (2) is that to use temperature successively be 85 ℃ dimethyl sulphoxide solution, acetone soln, deionized water rinsing.
4. method according to claim 1 is characterized in that: the CdS/ZnO nano-tube array optoelectronic pole that step (2) prepares was annealed 1 hour in 350 ℃ in retort furnace.
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