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Titanium-doped alpha-iron oxide photo-anode, and preparation method and application thereof

A technology of iron oxide light and titanium doping, which is applied in the field of nanomaterial preparation and application, can solve the problems of increase in grain size, positive shift of photoelectrode initial potential, coarsening of iron oxide grains, etc., and achieve an increase in photocurrent Effect

Active Publication Date: 2016-08-10
THE NAT CENT FOR NANOSCI & TECH NCNST OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

One thing that needs special attention is that high-temperature annealing treatment is required in the process of preparing iron oxide photoanodes, but iron oxide grain coarsening will inevitably occur during the high-temperature process, which increases the grain size and inhibits the arrival of holes. Opportunity of the iron oxide surface, affecting the final efficiency of the iron oxide photoelectrode
Gratzel's group used SiO 2 layer to suppress the coarsening of iron oxide grains, and the crystal grain size is from 90-120nm (without using SiO 2 layer) is reduced to 30-40nm, and the effect of photocurrent improvement is remarkable, but on the one hand, SiO 2 The product made by the layer does not form effective ion doping, on the other hand, the photoelectrode initial potential has a positive shift phenomenon, which affects the final photoelectric performance.

Method used

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  • Titanium-doped alpha-iron oxide photo-anode, and preparation method and application thereof
  • Titanium-doped alpha-iron oxide photo-anode, and preparation method and application thereof
  • Titanium-doped alpha-iron oxide photo-anode, and preparation method and application thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0071] (1) Prepare the substrate used for preparing the titanium-doped α-iron oxide photoanode, cut it into a size of 2cm*4cm, and clean it with isopropanol, acetone, ethanol and water in sequence. After the FTO was cleaned and dried, the back-to-back and vertical inner substrate surface (FTO's SnO 2 Facing the lining wall) placed on the PTFE lining. Add 0.54058g FeCl to 20mL aqueous solution 3 ·6H 2 O, and 0.36036gNH 2 CONH 2 , stirred for 60min. The stirred solution was poured into the polytetrafluoroethylene lining, and then the polytetrafluoroethylene lining was placed in an autoclave and sealed, and heated at 70° C. for 6 hours in a blast drying oven. After hydrothermal treatment, a light yellow translucent β-FeOOH film grew on the FTO. The β-FeOOH film was cleaned with deionized water and dried with nitrogen.

[0072] (2) Take 100μL TiCl 4 Add 20mL ethanol solution to get TiCl 4 ethanol solution, take 10 μL TiCl 4 The ethanol solution was used as a spin coating ...

Embodiment 2

[0077](1) Prepare the substrate used for preparing the titanium-doped α-iron oxide photoanode, cut it into a size of 2cm*4cm, and clean it with isopropanol, acetone, ethanol and water in sequence. After the FTO was cleaned and dried, the back-to-back and vertical inner substrate surface (FTO's SnO 2 Facing the lining wall) placed on the PTFE lining. Add 0.54058g FeCl to 20mL aqueous solution 3 ·6H 2 O, and 0.36036gNH 2 CONH 2 , stirred for 60min. The stirred solution was poured into the polytetrafluoroethylene lining, and then the polytetrafluoroethylene lining was placed in an autoclave and sealed, and heated at 70° C. for 6 hours in a blast drying oven. After hydrothermal treatment, a light yellow translucent β-FeOOH film grew on the FTO. The β-FeOOH film was cleaned with deionized water and dried with nitrogen.

[0078] (2) Take 200μL TiCl 4 Add 20mL ethanol solution to get TiCl 4 ethanol solution, take 10 μL TiCl 4 The ethanol solution was used as a spin coating s...

Embodiment 3

[0083] (1) Prepare the substrate used for preparing the titanium-doped α-iron oxide photoanode, cut it into a size of 2cm*4cm, and clean it with isopropanol, acetone, ethanol and water in sequence. After the FTO was cleaned and dried, the back-to-back and vertical inner substrate surface (FTO's SnO 2 Facing the lining wall) placed on the PTFE lining. Add 5.4058g FeCl to 40mL aqueous solution 3 ·6H 2 O, and 3.6036g NH 2 CONH 2 , stirred for 50min. The stirred solution was poured into the polytetrafluoroethylene lining, and then the polytetrafluoroethylene lining was placed in an autoclave and sealed, and heated at 80° C. for 6.5 hours in a blast drying oven. After hydrothermal treatment, a light yellow translucent β-FeOOH film grew on the FTO. The β-FeOOH film was cleaned with deionized water and dried with nitrogen.

[0084] (2) Take 150μL TiCl 4 Add 20mL ethanol solution to get TiCl 4 ethanol solution, take 20 μL TiCl 4 The ethanol solution was used as a spin coating...

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Abstract

The invention discloses a titanium-doped alpha-iron oxide photo-anode, and a preparation method and an application thereof. The method comprises the steps: coating the surface of a beta-FeOOH membrane with a titanium source solution, forming a TiO2 layer during high temperature annealing, and inhibiting grain coarsening of alpha-iron oxide; at the same time, in the process, diffusing titanium ions to the interior of alpha-iron oxide crystal lattices to realize titanium doping; and after annealing, using a hydrogen peroxide aqueous solution to remove the TiO2 layer, and thus obtaining the titanium-doped alpha-iron oxide photo-anode. The photo-anode has small particle size which is 30 nm-40 nm; the maximum photocurrent density can reach 3.62 mA / cm<2> under a 300 W xenon lamp light source and at the bias of 1.23 V[RHE]; compared with a un-doped alpha-iron oxide photo-anode without introduction of the TiO2 layer, the photocurrent is increased by 5 times, and a positive shift phenomenon of initial potential is not generated.

Description

technical field [0001] The invention belongs to the field related to the preparation and application of nanomaterials, and relates to a titanium-doped α-iron oxide photoanode, its preparation method and application, in particular to a TiO 2 Preparation method of titanium-doped α-iron oxide photoanode, titanium-doped α-iron oxide photoanode and application thereof. Background technique [0002] Due to the increasing energy shortage and environmental pollution, the research on new energy has attracted extensive attention at home and abroad. The use of photoelectrochemical cell devices for hydrogen production from water splitting by solar energy is attracting more and more attention. Iron oxide (α-iron oxide) is a narrow bandgap, low-cost, and chemically stable semiconductor material, and is currently a popular choice for semiconductor materials used in photoanodes of photoelectrochemical cells. However, the short electron-hole pair lifetime and low minority charge carrier mo...

Claims

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Application Information

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IPC IPC(8): C04B35/26
CPCC04B35/26C04B2235/3232C04B2235/5454
Inventor 董天娇张凯宫建茹
Owner THE NAT CENT FOR NANOSCI & TECH NCNST OF CHINA
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