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Preparation method of Cp*Co(CO)I2-loaded cobalt-doped zinc oxide photoanode nano array

A nano-array and photoanode technology, applied in chemical instruments and methods, physical/chemical process catalysts, organic compounds/hydrides/coordination complex catalysts, etc., can solve problems such as no related reports, and achieve good electron transfer efficiency, good photoelectrochemical performance, and excellent photocatalytic performance

Active Publication Date: 2019-12-03
HENAN NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there is no relevant report on the research on cobalt-doped zinc oxide photoanodes supported by transition metal cobalt organic co-catalysts

Method used

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  • Preparation method of Cp*Co(CO)I2-loaded cobalt-doped zinc oxide photoanode nano array
  • Preparation method of Cp*Co(CO)I2-loaded cobalt-doped zinc oxide photoanode nano array
  • Preparation method of Cp*Co(CO)I2-loaded cobalt-doped zinc oxide photoanode nano array

Examples

Experimental program
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Effect test

Embodiment 1

[0020] Take 10~200μL of 10mM zinc acetate ethanol solution and drop-coat it on the cleaned FTO substrate, 2500~3500 rpm for 30 seconds. Transfer to a muffle furnace, heat up to 300° C. for 2.5 hours for calcination over 40 minutes to obtain a zinc oxide seed layer. Put the above substrate into a polytetrafluoroethylene autoclave, add 0.01M Zn(NO 3 ) 2 ·6H 2 O and 0.01M hexamethylenetetramine, 80mL mixed solution with a molar ratio of 1:1, were hydrothermally reacted at 90°C for 6h to obtain ZnO photoanode nanoarrays. Cobalt nitrate with a molar ratio of Co / Zn=1% was added to the hydrothermal reaction solution, and CZ1 photoanode nanoarrays were obtained under the same conditions. The prepared Co-ZnO photoanode nanoarrays were immersed in Cp*Co(CO)I at room temperature in the dark 2 N,N-dimethylformamide solution for 10h, and finally washed with ethanol and water to obtain Co / CZ1 photoanode nanoarrays.

Embodiment 2

[0022] Take 10~200μL of 10mM zinc acetate ethanol solution and drop-coat it on the cleaned FTO substrate, 2500~3500 rpm for 30 seconds. Transfer to a muffle furnace, heat up to 300° C. for 2.5 hours for calcination over 40 minutes to obtain a zinc oxide seed layer. Put the above substrate into a polytetrafluoroethylene autoclave, add 0.05M Zn(NO 3 ) 2 ·6H 2 O and 0.05M hexamethylenetetramine, 80mL mixed solution with a molar ratio of 1:1, were hydrothermally reacted at 90°C for 6h to obtain ZnO photoanode nanoarrays. Cobalt nitrate with a molar ratio of Co / Zn=3% was added to the hydrothermal reaction solution, and CZ3 photoanode nanoarrays were obtained under the same conditions. The prepared Co-ZnO photoanode nanoarrays were immersed in Cp*Co(CO)I at room temperature in the dark 2 N,N-dimethylformamide solution for 10h, and finally washed with ethanol and water to obtain Co / CZ3 photoanode nanoarrays.

Embodiment 3

[0024] Take 10~200μL of 10mM zinc acetate ethanol solution and drop-coat it on the cleaned FTO substrate, 2500~3500 rpm for 30 seconds. Transfer to a muffle furnace, heat up to 300° C. for 2.5 hours for calcination over 40 minutes to obtain a zinc oxide seed layer. Put the above substrate into a polytetrafluoroethylene autoclave, add 0.25M Zn(NO 3 ) 2 ·6H 2 O and 0.25M hexamethylenetetramine, 80mL mixed solution with a molar ratio of 1:1, were hydrothermally reacted at 90°C for 6h to obtain ZnO photoanode nanoarrays. Cobalt nitrate with a molar ratio of Co / Zn=5% was added to the hydrothermal reaction solution, and the CZ5 photoanode nanoarray was obtained under the same conditions. The prepared Co-ZnO photoanode nanoarrays were immersed in Cp*Co(CO)I at room temperature in the dark 2 N,N-dimethylformamide solution for 10 h, and finally rinsed with ethanol and water to obtain Co / CZ5 photoanode nanoarrays.

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Abstract

The invention discloses a preparation method of a Cp*Co(CO)I2-loaded cobalt-doped zinc oxide photoanode nano array. The preparation method comprises the following steps: putting a fluorine doped tin oxide (FTO) substrate containing a zinc oxide seed layer into a polytetrafluoroethylene high-pressure reaction kettle, adding a mixed solution of Zn(NO3)2.6H2O and hexamethylene tetramine, and performing a hydrothermal reaction at 90 DEG C for 5-10 hours to obtain a ZnO photoanode nano array; adding cobalt nitrate into the hydrothermal reaction liquid, and performing a hydrothermal reaction at 90 DEG C for 5-10 hours to obtain a Co-ZnO photoelectric anode nano array; and immersing the Co-ZnO photoelectric anode nano array in an N,N-dimethylformamide solution of Cp*Co(CO)I2 at room temperature under a dark condition for 6-10 hours, and finally carrying out washing with ethanol and water to obtain a target product. The Cp*Co(CO)I2 loaded cobalt-doped zinc oxide photoanode nano array preparedby the method not only can keep good zinc oxide array appearance, but also accelerates mobility of photo-generated electrons, has good stability, and finally exhibits excellent photoelectrochemical performance.

Description

technical field [0001] The invention belongs to the technical field of synthesis of nano-photoelectric materials, in particular to a transition metal cobalt organic molecular catalyst-pentamethylcyclopentadienyl cobalt diiodide (Cp*Co(CO)I 2 ) preparation method of cobalt-doped zinc oxide photoanode nano-array. Background technique [0002] With the development of science and technology and the progress of human civilization, energy issues have become increasingly prominent. The continuous consumption of non-renewable energy sources such as fossil fuels forces scientific researchers to continuously develop and utilize renewable energy sources. Solar photocatalytic water splitting technology has constructed a beautiful blueprint for the green, clean and sustainable development of human beings, but the slow water oxidation kinetics of photocatalytic performance, rapid photogenerated electron-hole recombination, and low electron migration rate hinder its large-scale applicatio...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C25B11/06C25B1/04B01J31/26
CPCC25B1/04B01J31/26C25B1/55C25B11/051C25B11/091B01J35/33B01J35/39Y02E60/36Y02P20/133
Inventor 崔佳宝陈俊霞潘楠楠姜聚慧娄向东
Owner HENAN NORMAL UNIV
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