Preparation method for Au-ZnIn2S4 nanoarray electrode photocatalytic nitrogen fixation material

An au-znin2s4, nano-array technology, applied in catalyst activation/preparation, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems of low photoelectric performance, low catalytic performance, and low photoactive area, etc. To achieve the effect of loose preparation conditions, simple preparation and easy recovery

Active Publication Date: 2019-11-29
CHINA UNIV OF MINING & TECH
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Problems solved by technology

[0006] The purpose of the present invention is to provide a kind of Au-ZnIn 2 S 4 The preparation method of nano-array electrode photocatalytic nitrogen-fixing materials solves the problems of low photoactive area, low photoelectric performance and low catalytic performance in the field of photocatalysis in the current field of photocatalysis

Method used

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  • Preparation method for Au-ZnIn2S4 nanoarray electrode photocatalytic nitrogen fixation material
  • Preparation method for Au-ZnIn2S4 nanoarray electrode photocatalytic nitrogen fixation material
  • Preparation method for Au-ZnIn2S4 nanoarray electrode photocatalytic nitrogen fixation material

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preparation example Construction

[0042] Au-ZnIn 2 S 4 The preparation method of the nano-array is: based on ZnIn 2 S 4 Photodeposition of nano-Au particles on the surface of nano-array electrodes improves ZnIn 2 S 4 Photocatalytic nitrogen fixation performance; first, a layer of ZnIn was grown on FTO conductive glass by hydrothermal method 2 S 4 Nanosheet array with Au particles deposited on its surface by photodeposition; Au-ZnIn 2 S 4 The electrode sheet was fixed in methanol aqueous solution, and high-purity nitrogen gas was fed continuously, and the N 2 Convert to NH 3 , and then converted to NH 4+ ; Take the reaction solution and Nessler's reagent for color development, and determine the NH in the reaction solution 4+ Concentration, and then determine the photocatalytic nitrogen fixation performance of the material.

[0043] The Au-ZnIn 2 S 4 The preparation of nano-arrays, the specific steps are as follows:

[0044] Step 1. Utilize zinc nitrate Zn(NO 3 ) 2 ·6H 2 O, indium trichloride In...

Embodiment 1

[0070] Embodiment 1: ZnIn with 0.2mgAu 2 S 4 Nanoarray Surface Deposition.

[0071] 1. Add 20μl of 50mmol / L AuHCl 4 Dissolve in 100mL of pure water to obtain a solution containing 0.2mg of Au, and transfer the solution into a quartz electrolytic cell.

[0072] 2. Fix the electrode sheet with a polytetrafluoroethylene electrode clip, and immerse it in the middle solution, with ZnIn 2 S 4 The surface of the nanometer film faces the xenon lamp light source, and illuminates for 30 minutes in a magnetic stirring.

[0073] 3. Take out the electrode sheet, slowly rinse it with pure water for 3 minutes, and dry it in vacuum at 60°C for 6 hours to obtain an Au-ZnIn2S4 electrode sheet with 0.2 mg of Au photodeposited.

Embodiment 2

[0074] Embodiment 2: ZnIn with 0.4mgAu 2 S 4 Nanoarray Surface Deposition.

[0075] 1. Add 40μl of 50mmol / L AuHCl 4 Dissolve in 100mL of pure water to obtain a solution containing 0.4mg of Au, and transfer the solution into a quartz electrolytic cell.

[0076] 2. Fix the electrode sheet with a polytetrafluoroethylene electrode clip, and immerse it in the middle solution, with ZnIn 2 S 4 The surface of the nanometer film faces the xenon lamp light source, and illuminates for 30 minutes in a magnetic stirring.

[0077] 3. Take out the electrode sheet, rinse it slowly with pure water for 3 minutes, and dry it in vacuum at 60°C for 6 hours to obtain Au-ZnIn with 0.4 mg Au photodeposited 2 S 4 electrode sheet.

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Abstract

The invention discloses a preparation method for an Au-ZnIn2S4 nanoarray electrode photocatalytic nitrogen fixation material, belonging to the field of preparation and modification methods for photoelectrochemical catalytic materials. The preparation method comprises the following steps: based on a ZnIn2S4 nanoarray electrode, performing photodeposition of Au nanoparticles on the surface of the ZnIn2S4 nanoarray electrode so as to improve the photocatalytic nitrogen fixation performance of ZnIn2S4; growing a layer of a ZnIn2S4 nanosheet array on FTO conductive glass by adopting a hydrothermalmethod, and depositing Au particles on the surface of the ZnIn2S4 nanosheet array by adopting a photodeposition method so as to prepare an Au-ZnIn2S4 electrode; fixedly putting the Au-ZnIn2S4 electrode slice in an aqueous methanol solution, continuously introducing high-purity nitrogen, converting N2 into NH3 under the illumination of a xenon lamp, and then converting NH3 into NH4<+>; and mixing areaction solution with a Nessler's reagent for color development, and determining the concentration of NH4<+> in the reaction solution so as to further determine the photocatalytic nitrogen fixationperformance of the material. The method has the advantages of simple preparation, loose preparation conditions, no toxicity, and easy recovery and cyclic utilization of the material in the process ofapplication; since ZnIn2S4 is narrow in forbidden band width and can absorb visible light in a larger range, and Au also has strong absorption performance in a visible light range, the material is increased in the comprehensive utilization rate of visible light.

Description

technical field [0001] The invention relates to a method for preparing and modifying a photoelectrochemical catalytic material, especially an Au-ZnIn 2 S 4 A method for preparing a nano-array electrode photocatalytic nitrogen-fixing material. Background technique [0002] Ammonia is an essential raw material for the production of chemical industry, medicine, agriculture, etc. At present, the synthesis of ammonia in industrial production is still the traditional Haber method, the reaction temperature is mostly above 300°C, the pressure is above 100atm, and the reaction is carried out in the catalytic process of iron-based catalysts. H required for synthesis reactions 2 Mainly produced by the evaporative transformation of natural gas, maintaining the entire reaction process consumes 1-2% of the earth's fossil energy and causes a large amount of CO 2 emissions. From the perspective of reducing the consumption of non-renewable energy and reducing greenhouse gas emissions, t...

Claims

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Application Information

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IPC IPC(8): B01J27/04B01J37/10B01J37/34C23C18/14
CPCB01J27/04B01J37/10B01J37/341C23C18/14B01J35/23B01J35/33B01J35/39
Inventor 毛梁李坤顾修全蔡晓燕杨鼎
Owner CHINA UNIV OF MINING & TECH
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