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Preparation method of silicon/nickel-cobalt-iron photo-anode

A nickel-cobalt-iron and photoanode technology, which is applied in the direction of electrodes, electrolytic components, energy input, etc., can solve the problems of difficult to prepare large-area films, affect film formation, and slow deposition rate, and achieve rapid large-scale preparation and accelerate hydrogen production. The generation, protective corrosion passivation effect

Pending Publication Date: 2022-04-01
XI AN JIAOTONG UNIV +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, these methods have more or less shortcomings. For example, the laser pulse deposition method is not easy to prepare a large-area film, and it is difficult to realize industrial production; the deposition rate of the atomic layer deposition method is too slow, and the thickness of ten cycles can only reach the nanometer level. There is no effective deposition process for materials such as silicon germanium; the gas plasma in the magnetron sputtering process is not stable, which affects the formation of the film; the electron beam evaporation method may cause secondary damage caused by high-energy electrons Secondary electrons may ionize residual gas molecules and may also cause pollution

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  • Preparation method of silicon/nickel-cobalt-iron photo-anode

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preparation example Construction

[0047] A method for preparing a silicon / nickel-cobalt-iron photoanode, comprising the following steps:

[0048] S1. Dissolve nickel sulfate, cobalt sulfate, ferrous sulfate, boric acid and surfactant in deionized water, purging and stirring, and wait until completely dissolved to obtain an electrodeposition solution;

[0049] S2. Immerse the packaged silicon photoanode in the electrodeposition solution configured in step S1, and conduct electrodeposition under the constant current mode of the electrochemical workstation (and the deposition voltage does not reach the reduction potential of each metal ion), to obtain the target product silicon / Nickel-cobalt-iron photoanode.

[0050] Specifically, the specific process of the step S1 is: A mol NiSO 4 , B mol CoSO 4 , C mol FeSO 4 Dissolve in 100mL deionized water to get NiSO 4 、CoSO 4 , FeSO 4 A mixed solution of deionized water, A+B+C=0.01mol (A: 0.002~0.009mol; B: 0.0005~0.004mol; C: 0.0005~0.004mol), was purged and stirr...

Embodiment 1

[0065] 1) 0.002mol NiSO 4 , 0.004mol CoSO 4 , 0.004mol FeSO 4 Dissolve in 100mL deionized water to get NiSO 4 、CoSO 4 , FeSO 4 deionized water mixed solution, nitrogen or argon purging and stirring for 10 minutes;

[0066] 2) Put the sealed silicon photoanode (working electrode), silver / silver chloride electrode (reference electrode) and platinum electrode (counter electrode) into the deionized water mixed solution 3cm below the liquid surface;

[0067] 3) When performing electrodeposition, set the electrochemical workstation to constant current mode, and the current density is 1mA cm -2 , the deposition time is 1000s, and the deposition temperature is 20°C. After electrodeposition, the silicon / nickel-cobalt-iron photoanode was rinsed with deionized water for 30 seconds to obtain the target product. Electrochemical deposition of silicon / nickel-cobalt-iron photoanodes figure 1 As shown, the cyclic voltammogram of the prepared silicon / nickel-cobalt-iron photoanode is as ...

Embodiment 2

[0069] 1) 0.005mol NiSO 4 , 0.0025mol CoSO 4 , 0.0025mol FeSO 4 Dissolve in 100mL deionized water to get NiSO 4 、CoSO 4 , FeSO 4 deionized water mixed solution, nitrogen or argon purging and stirring for 10 minutes;

[0070] 2) Put the sealed silicon photoanode (working electrode), silver / silver chloride electrode (reference electrode) and platinum electrode (counter electrode) into the deionized water mixed solution 3cm below the liquid surface;

[0071] 3) When performing electrodeposition, set the electrochemical workstation to constant current mode, and the current density is 1mA cm -2 , the deposition time is 1000s, and the deposition temperature is 20°C. After electrodeposition, the silicon / nickel-cobalt-iron photoanode was rinsed with deionized water for 30 seconds to obtain the target product. Electrochemical deposition of silicon / nickel-cobalt-iron photoanodes image 3 As shown, the cyclic voltammogram of the prepared silicon / nickel-cobalt-iron photoanode is a...

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Abstract

The invention discloses a silicon / nickel-cobalt-iron photo-anode preparation method, nickel sulfate, cobalt sulfate and ferrous sulfate are dissolved in deionized water to form a uniformly mixed electro-deposition solution, inert gas is used for maintaining the existence of iron elements in the solution in the form of ferrous ions, and in the under-potential deposition process, the content of the ferrous ions in the solution is reduced; divalent nickel-cobalt-iron elements form a compact nickel-cobalt-iron alloy film on the surface of a silicon electrode, a silicon anode is effectively protected to avoid corrosion and passivation, the outermost layer of the nickel-cobalt-iron alloy film is oxidized to generate a complex nickel-cobalt-iron (hydrogen) oxide at the initial stage of photoelectric water decomposition, and the photoelectric water decomposition efficiency is improved. More surface active sites are provided for photoelectrochemical water decomposition to accelerate the photoelectrochemical water decomposition process so as to accelerate the generation of hydrogen, the silicon / nickel-cobalt-iron photo-anode synthesized by the method can be prepared on a large scale in a controllable, repeatable and rapid manner by using the existing electro-deposition equipment in a factory, and the method is suitable for industrial production. And no toxic chemical reagent is added in the whole synthesis process, the conditions are mild, and no pollution is caused.

Description

technical field [0001] The application belongs to the field of electrode materials, and in particular relates to a method for preparing a silicon / nickel-cobalt-iron photoanode. Background technique [0002] Compared with other semiconductor photocatalysts, silicon is very abundant on the earth, easy to obtain and low in price. In addition, its 1.12eV bandgap width matches the sunlight spectrum very well, and it can obtain good photoresponse in visible light and even far infrared light region. , which is conducive to the realization of efficient utilization of solar energy, has been widely used in the photovoltaic industry, and has great potential application value in the field of new photoelectric catalysis technologies. [0003] However, the "pinning effect" of silicon itself leads to the slow charge transfer kinetics on its surface, which limits the separation and transfer of photogenerated carriers; and as a photoanode reacts in alkaline solution, its surface is extremely...

Claims

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Application Information

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IPC IPC(8): C25B11/04C25B1/04
CPCY02E60/36Y02P20/133
Inventor 沈少华孔婷婷何凌云
Owner XI AN JIAOTONG UNIV
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