Preparation method for electro-oxidation synthesis of one-dimensional nano-oxide structure

A nano-oxide and electro-oxidation technology, applied in the field of photoelectrolysis, can solve problems such as poor stability, easy to fall off, and difficult to control one-dimensional nanostructures, and achieve the effect of enhancing the binding force and enhancing the binding force

Active Publication Date: 2016-07-20
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

[0004] In order to overcome α-Fe 2 o 3 In the semiconductor film preparation process, the one-dimensional nanostructure is not easy to control, and has poor stability and easy to fall off. 2 o 3 A semiconductor photoanode provides a preparation method that can enhance the bonding force between the hematite film and the conductive substrate, maintain a one-dimensional nanostructure and easily control the film thickness

Method used

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  • Preparation method for electro-oxidation synthesis of one-dimensional nano-oxide structure
  • Preparation method for electro-oxidation synthesis of one-dimensional nano-oxide structure
  • Preparation method for electro-oxidation synthesis of one-dimensional nano-oxide structure

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Embodiment 1

[0034] Using 0.01M FeCl 2 ·5H 2 O was used as the electrolyte solution, and 1M HCl was used to adjust the pH of the solution to 4.1, and α-Fe was prepared using a three-electrode system at 75 °C 2 o 3photoelectrode. Among them, the stainless steel conductive substrate is used as the working electrode, the Pt sheet electrode is used as the counter electrode, the Ag / AgCl electrode (4MKCl solution) is used as the reference electrode, and the electrolyte is deionized water: ethylene glycol = 20:1. The optimized deposition electrode was tested under the condition of 1.4V. The deposition time is 2 min. After the deposition process was completed, the color of the deposited film sample changed from colorless to a layer of transparent yellow substance on the surface. Take out the working electrode and rinse it with deionized water, stir the sample in a solution containing tetraethyl orthosilicate for 1-4 hours, and then place it in a tube furnace for calcination. In the tube furna...

Embodiment 2

[0036] The difference from Example 1 is that in 0.05M FeSO 4 and 3M NH 4 Cl is used as the electrolyte, the pH value is 7.5, and the electrolyte solvent is deionized water:polyethylene glycol=1:1 under the condition of a voltage of 0.3V. Among them, FTO (conductive glass) is used as the working electrode, the Pt sheet electrode is used as the counter electrode, and the Ag / AgCl electrode (4MKCl solution) is used as the reference electrode. After the deposition process is completed, calcining is carried out in the same manner as in the previous example. One-dimensional α-Fe prepared by this method 2 o 3 The FESEM picture of the photoelectrode is as Figure 4 shown. It can be seen that the prepared iron oxide has a one-dimensional nanorod structure and grows vertically to the substrate.

Embodiment 3

[0038] The difference from Example 1 is that the working electrode is a Ti conductive substrate, the counter electrode is a graphite plate, Ag / AgCl (saturated KCl) is a reference electrode, and the electrolyte solvent is deionized water in different proportions: glycerol. Under the condition of applied voltage 1.0V, 70℃, with 0.1M FeCl 2 4H 2 O, pH=5.1 is the electrolyte solution, and the deposition time is 30min. After the deposition, the sample was sent into a tube furnace for high-temperature calcination at 800°C for 6 hours. α-Fe prepared in different ratios 2 o 3 The UV-visible absorption spectrum of the photoelectrode is as follows: Figure 5 As shown, it shows that the material has the ability to absorb solar energy and can be applied to the photoelectrolysis process.

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Abstract

The invention relates to a preparation method for one-dimensional nano-oxides in the field of photoelectrocatalysis. An electrochemical system is built with a Fe2+ precursor solution as an electrolyte solution, deionized water and polyols of different proportions as solvents, a conductive substrate as a working electrode, a Pt metal plate or a graphite plate as a counter electrode, and Ag/AgCl or a saturated calomel electrode as a reference electrode. A FeOOH thin film is prepared on a surface of conductive glass by means of electrodeposition; the thin film sample is dipped into a shape protective agent and then calcined into an alpha-Fe2O3 photoanode. Using such a method to prepare the photoanode, tight integration of the alpha-Fe2O3 photoanode thin film and the conductive substrate can be realized and the stability of the photoanode during photoelectrolysis is improved. Using the photoanode prepared by means of such a method during photoelectrolysis, accurate control over the thickness of the alpha-Fe2O3 photoanode thin film can be realized; thin films different in thickness can be deposited under different electric quantities by controlling the time of the current, thereby providing important basis for discussing the transfer mechanism of current carriers of a photoelectrolytic tank and the relation of optical characteristics to film thicknesses.

Description

technical field [0001] The invention relates to the field of photoelectrolysis, in particular to a method for preparing a photoanode with a one-dimensional nano-oxide structure used in a photoelectrolysis cell. Background technique [0002] The photoelectrolysis process is a process in which semiconductors absorb solar energy and convert and store energy into chemical energy. The most popular way to convert and store solar energy into chemical energy is to store solar energy into hydrogen through photoelectrolysis of water. This method is similar to photosynthesis in nature and is an ideal way to produce clean energy. The raw materials consumed in the process are reserves on the earth Abundant water resources. As a secondary energy source, hydrogen energy has been widely regarded as the most ideal pollution-free green energy in the new century, which has many advantages such as cleanness, high efficiency, safety, storability, and transportability. Compared with other photo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C25D11/34B82Y40/00B82Y30/00
Inventor 俞红梅付丽张长昆贾佳迟军邵志刚衣宝廉
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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