CN112899721A - Three-dimensional ZnO/CdS nano-array electrode and preparation method thereof - Google Patents
Three-dimensional ZnO/CdS nano-array electrode and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a three-dimensional ZnO/CdS nano-array electrode and a preparation method thereof, which comprises the following steps: step one, selecting and plating F: SnO2The glass plate of the conductive layer is used as a substrate; placing the substrate into a mixed solution of zinc acetate and hexamethyltetramine for sealing hydrothermal treatment, and calcining the substrate after the hydrothermal treatment to obtain a ZnO nanorod array; putting the ZnO nanorod array into a mixed solution of cadmium chloride and thiourea, sealing the mixed solution, performing hydrothermal treatment, adding triethanolamine serving as a surfactant into the mixed solution of the cadmium chloride and the thiourea, and adjusting the pH value by using ammonia water to enable the mixed solution of the cadmium chloride and the thiourea to be clear and transparent; and calcining the ZnO nanorod array subjected to the hydrothermal treatment, and washing the calcined ZnO nanorod array to obtain the three-dimensional ZnO/CdS nano-array electrode. The preparation method comprisesThe three-dimensional ZnO/CdS nano-array electrode with high light energy absorption rate, high surface reaction rate and high light energy conversion efficiency is obtained.
Description
Technical Field
The invention belongs to the technical field of new energy materials, and particularly relates to a three-dimensional ZnO/CdS nano array electrode and a preparation method thereof.
Background
At present, fossil energy is in shortage, environmental pollution is increasingly serious, and the preparation of hydrogen by decomposing water through a photoelectrode is concerned widely. However, the traditional one-dimensional photoelectric material has a relatively small surface area, so that the rapid reaction cannot be realized, and the wide application of the photoelectric material is limited.
Disclosure of Invention
In order to solve the technical problems, the invention designs a three-dimensional ZnO/CdS nano array electrode and a preparation method thereof.
In order to solve the technical problems, the invention adopts the following technical scheme on one hand:
a preparation method of a three-dimensional ZnO/CdS nano-array electrode comprises the following steps:
step one, selecting and plating F: SnO2The glass plate of the conductive layer is used as a substrate;
placing the substrate into a mixed solution of zinc acetate and hexamethyltetramine for sealing hydrothermal treatment, and calcining the substrate after the hydrothermal treatment to obtain a ZnO nanorod array;
putting the ZnO nanorod array into a mixed solution of cadmium chloride and thiourea, sealing the mixed solution, performing hydrothermal treatment, adding triethanolamine serving as a surfactant into the mixed solution of the cadmium chloride and the thiourea, and adjusting the pH value by using ammonia water to enable the mixed solution of the cadmium chloride and the thiourea to be clear and transparent; and calcining the ZnO nanorod array subjected to the hydrothermal treatment, and washing the calcined ZnO nanorod array to obtain the three-dimensional ZnO/CdS nano-array electrode.
Further, in the first step, the substrate is pretreated, wherein the pretreatment is to put the substrate into a mixed solution of deionized water, acetone and ethanol, and clean the substrate by ultrasonic cleaning.
Further, the substrate is a glass plate of 5cm × 3 cm.
Further, in the second step, the temperature of the sealing water is 90 ℃, and the heating time is 6 h.
Further, in the second step, the calcining temperature is 400 ℃, and the calcining time is 1 h.
Further, in the second step, the mixed solution of zinc acetate and hexamethylenetetramine is a mixed solution prepared by deionized water, and the concentrations of the zinc acetate and the hexamethylenetetramine in the mixed solution are both 0.05 mol/L.
Further, in the third step, the sealing water heating temperature is 80 ℃, and the heating time is 2 hours.
Further, in the third step, the calcining temperature is 400 ℃, the calcining time is 1h, and the calcining environment is nitrogen atmosphere.
Further, in the third step, the concentration of the cadmium chloride in the mixed solution of the cadmium chloride and the thiourea is 0.02mol/L, and the concentration of the thiourea is 0.06 mol/L.
On the other hand, the invention also discloses:
a three-dimensional ZnO/CdS nano-array electrode is prepared by any one of the preparation methods of the three-dimensional ZnO/CdS nano-array electrode, and the energy conversion efficiency of the electrode is 2.25% under an external voltage of-0.15V.
The three-dimensional ZnO/CdS nano-array electrode and the preparation method thereof have the following beneficial effects:
(1) the invention provides a three-dimensional ZnO/CdS nano-array electrode and a preparation method thereof, wherein the preparation method can change the specific surface area of a ZnO/CdS nano-array and obtain the ZnO/CdS nano-array electrode with high light energy absorption rate, high surface reaction rate and high light energy conversion efficiency; the three-dimensional ZnO/CdS nano array electrode has high energy conversion efficiency which reaches 2.25 percent and is two times of the one-dimensional ZnO/CdS nano array electrode and five times of the one-dimensional ZnO nano array electrode.
(2) According to the three-dimensional ZnO/CdS nano array electrode, CdS in a flaky structure wraps the surface of ZnO, so that the contact area of a photoelectric film and electrolyte is greatly increased, and further, the reaction active sites of photo-generated holes and solution are increased.
(3) In the invention, the CdS is in a sheet structure, so that the photo-generated holes can reach the CdS surface and react with the electrolyte only by a very short transmission distance, thereby greatly accelerating the consumption rate of the photo-generated holes and improving the collection efficiency of photo-generated electrons.
Drawings
FIG. 1: the invention discloses a flow chart of a preparation method of a three-dimensional ZnO/CdS nano array electrode in an embodiment;
FIG. 2: the preparation process of the three-dimensional ZnO/CdS nano-array electrode in the embodiment of the invention is schematically shown;
FIG. 3: the X-ray diffraction contrast map of the three-dimensional ZnO/CdS nano array electrode in the embodiment of the invention and the X-ray diffraction contrast map of the ZnO nanorod array electrode and the one-dimensional ZnO/CdS nano array electrode in the prior art;
FIG. 4: the light energy absorption spectrum comparison graph of the three-dimensional ZnO/CdS nano array electrode in the embodiment of the invention and the ZnO nanorod array electrode and the one-dimensional ZnO/CdS nano array electrode in the prior art;
FIG. 5: the photoelectric conversion efficiency of the three-dimensional ZnO/CdS nano array electrode in the embodiment of the invention is compared with that of a ZnO nanorod array electrode and a one-dimensional ZnO/CdS nano array electrode in the prior art under illumination;
FIG. 6: the microstructure and the charge transfer schematic diagram of the three-dimensional ZnO/CdS nano array electrode in the embodiment of the invention are shown.
Detailed Description
The invention will be further explained with reference to the accompanying drawings:
fig. 1 to 6 show a specific embodiment of a three-dimensional ZnO/CdS nano-array electrode and a method for preparing the same according to the present invention. Fig. 1 to 2 are schematic views of a flow and a process of a method for preparing a three-dimensional ZnO/CdS nano-array electrode according to the present embodiment; FIGS. 3 to 5 are graphs comparing the performance of the three-dimensional ZnO/CdS nano-array electrode of the present embodiment with that of the prior art ZnO nano-rod array electrode and one-dimensional ZnO/CdS nano-array electrode; fig. 6 is a microstructure and charge transfer schematic diagram of the three-dimensional ZnO/CdS nano-array electrode in the present embodiment.
As shown in fig. 1 to 2, the method for preparing a three-dimensional ZnO/CdS nano-array electrode according to the present embodiment includes the following steps:
step one, selecting and plating F: SnO2The glass plate of the conductive layer is used as a substrate;
placing the substrate into a mixed solution of zinc acetate and hexamethyltetramine for sealing hydrothermal treatment, and calcining the substrate after the hydrothermal treatment to obtain a ZnO nanorod array;
putting the ZnO nanorod array into a mixed solution of cadmium chloride and thiourea, sealing the mixed solution, performing hydrothermal treatment, adding triethanolamine serving as a surfactant into the mixed solution of the cadmium chloride and the thiourea, and adjusting the pH value by using ammonia water to enable the mixed solution of the cadmium chloride and the thiourea to be clear and transparent; and calcining the ZnO nanorod array subjected to the hydrothermal treatment, and washing the calcined ZnO nanorod array to obtain the three-dimensional ZnO/CdS nano-array electrode.
Preferably, in the step one, the substrate is pretreated, and the pretreatment is to put the substrate into a mixed solution of deionized water, acetone and ethanol, and clean the substrate by ultrasonic cleaning.
Preferably, the substrate is a 5cm by 3cm glass plate.
Preferably, in the second step, the temperature of the sealing water is 90 ℃, and the heating time is 6 h.
Preferably, in the second step, the calcining temperature is 400 ℃ and the calcining time is 1 h.
Preferably, in the second step, the mixed solution of zinc acetate and hexamethylenetetramine is a mixed solution with a concentration of 0.05mol/L prepared by deionized water.
Preferably, in the third step, the sealing hydrothermal temperature is 80 ℃, and the heating time is 2 hours.
Preferably, in the third step, the calcining temperature is 400 ℃, the calcining time is 1h, and the calcining environment is a nitrogen atmosphere.
Preferably, in the third step, the concentration of the cadmium chloride in the mixed solution of the cadmium chloride and the thiourea is 0.02mol/L, and the concentration of the thiourea is 0.06 mol/L.
The specific embodiment is as follows:
firstly, putting a substrate into a mixed solution of deionized water, acetone and ethanol for cleaning for later use; wherein, the substrate is coated with F: SnO2A glass plate (FTO) of the conducting layer, wherein the length multiplied by the width of the glass plate is 5cm multiplied by 3cm, the FTO is put into a mixed solution of deionized water, acetone and ethanol, and the FTO is cleaned by ultrasonic;
step two, preparing a mixed solution of zinc acetate and hexamethylenetetramine, putting a cleaned substrate (FTO) into 80mL of the mixed solution, sealing at 90 ℃ for 6 hours, and carrying out hydrothermal treatment; after the water heating is finished, taking out the substrate, washing the substrate, calcining the substrate for 1 hour at 400 ℃, taking out the substrate, and washing the substrate for later use to obtain a ZnO nanorod array; wherein the mixed solution of zinc acetate and hexamethylenetetramine is prepared by deionized water, and the concentrations of the zinc acetate and the hexamethylenetetramine in the mixed solution are both 0.05 mol/L;
thirdly, preparing a mixed solution of cadmium chloride and thiourea, taking 80mL of the mixed solution, and adding 2.5mL of Triethanolamine (TEA), wherein the volume percentage content of the triethanolamine is 3%; and ammonia water is used for adjusting the pH value to ensure that the mixture is clear and transparent; putting the prepared ZnO nanorod array into the clear solution, sealing for 2 hours at 80 ℃ and carrying out hydrothermal treatment; after the water heating is finished, taking out and washing the ZnO nanorod array, calcining for 1h at 400 ℃ in a nitrogen atmosphere, and then taking out and washing to obtain a three-dimensional ZnO/CdS nano array electrode; wherein, in the mixed solution of the cadmium chloride and the thiourea, the concentration of the cadmium chloride is 0.02mol/L, and the concentration of the thiourea is 0.06 mol/L.
As shown in fig. 6, the three-dimensional ZnO/CdS nano-array electrode in the present embodiment is manufactured by the above manufacturing method, and the energy conversion efficiency of the electrode is 2.25% at an applied voltage of-0.15V.
The three-dimensional ZnO/CdS nano-array electrode obtained in this example was subjected to X-ray diffraction, optical energy absorption, and photoelectric conversion efficiency under illumination, and the test results are shown in fig. 3, 4, and 5.
The invention provides a three-dimensional ZnO/CdS nano-array electrode and a preparation method thereof, the preparation method can change the specific surface area of a ZnO/CdS nano-array, obtain a ZnO/CdS nano-array photoelectrode with high light energy absorption rate, high surface reaction rate and high light energy conversion efficiency, and realize the high-efficiency conversion and utilization of solar energy; the three-dimensional ZnO/CdS nano array electrode has high energy conversion efficiency which reaches 2.25 percent and is two times of the one-dimensional ZnO/CdS nano array electrode and five times of the one-dimensional ZnO nano array electrode.
According to the three-dimensional ZnO/CdS nano array electrode, CdS in a flaky structure wraps the surface of ZnO, so that the contact area of a photoelectric film and electrolyte is greatly increased, and further, the reaction active sites of photo-generated holes and solution are increased.
In the invention, the CdS is in a sheet structure, so that the photo-generated holes can reach the CdS surface and react with the electrolyte only by a very short transmission distance, thereby greatly accelerating the consumption rate of the photo-generated holes and improving the collection efficiency of photo-generated electrons.
The invention is described above with reference to the accompanying drawings, it is obvious that the implementation of the invention is not limited in the above manner, and it is within the scope of the invention to adopt various modifications of the inventive method concept and solution, or to apply the inventive concept and solution directly to other applications without modification.
Claims (10)
1. A preparation method of a three-dimensional ZnO/CdS nano-array electrode is characterized by comprising the following steps:
step one, selecting and plating F: SnO2The glass plate of the conductive layer is used as a substrate;
placing the substrate into a mixed solution of zinc acetate and hexamethyltetramine for sealing hydrothermal treatment, and calcining the substrate after the hydrothermal treatment to obtain a ZnO nanorod array;
putting the ZnO nanorod array into a mixed solution of cadmium chloride and thiourea, sealing the mixed solution, performing hydrothermal treatment, adding triethanolamine serving as a surfactant into the mixed solution of the cadmium chloride and the thiourea, and adjusting the pH value by using ammonia water to enable the mixed solution of the cadmium chloride and the thiourea to be clear and transparent; and calcining the ZnO nanorod array subjected to the hydrothermal treatment, and washing the calcined ZnO nanorod array to obtain the three-dimensional ZnO/CdS nano-array electrode.
2. The method for preparing the three-dimensional ZnO/CdS nano-array electrode as claimed in claim 1, wherein in the first step, the substrate is pretreated by putting the substrate into a mixed solution of deionized water, acetone and ethanol, and cleaning the substrate with ultrasound.
3. The method for preparing a three-dimensional ZnO/CdS nano-array electrode as defined in claim 1 or 2, wherein the substrate is a 5cm x 3cm glass plate.
4. The method for preparing the three-dimensional ZnO/CdS nano-array electrode as claimed in claim 1, wherein in the second step, the temperature of the sealing water is 90 ℃ and the heating time is 6 h.
5. The method for preparing the three-dimensional ZnO/CdS nano-array electrode as claimed in claim 1, wherein in the second step, the calcination temperature is 400 ℃ and the calcination time is 1 h.
6. The method for preparing the three-dimensional ZnO/CdS nano-array electrode as claimed in claim 1, wherein in the second step, the mixed solution of zinc acetate and hexamethylenetetramine is prepared by deionized water, and the concentrations of the zinc acetate and the hexamethylenetetramine in the mixed solution are both 0.05 mol/L.
7. The method for preparing the three-dimensional ZnO/CdS nano-array electrode as claimed in claim 1, wherein in the third step, the sealing hydrothermal temperature is 80 ℃ and the heating time is 2 h.
8. The method for preparing the three-dimensional ZnO/CdS nano-array electrode as claimed in claim 1, wherein in the third step, the calcining temperature is 400 ℃, the calcining time is 1h, and the calcining environment is nitrogen atmosphere.
9. The method for preparing the three-dimensional ZnO/CdS nano-array electrode as claimed in claim 1, wherein in the third step, the concentration of cadmium chloride is 0.02mol/L and the concentration of thiourea is 0.06mol/L in the mixed solution of cadmium chloride and thiourea.
10. A three-dimensional ZnO/CdS nano-array electrode, characterized in that the electrode is manufactured by the method for manufacturing a three-dimensional ZnO/CdS nano-array electrode according to any one of claims 1 to 9, and the energy conversion efficiency of the electrode is 2.25% under an applied voltage of-0.15V.
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