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Method for preparing iron oxide photoanode under combined action of oxalic acid and tetrabutyl titanate

A tetrabutyl titanate and co-acting technology, which is applied in the field of preparation of iron oxide photoanode, can solve the problems of small hole diffusion length, complicated operation, poor electrical conductivity, etc., so as to improve the photoelectric performance, simple operation steps and high performance. boosted effect

Active Publication Date: 2020-12-04
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, α-Fe 2 o 3 There are also many disadvantages: poor conductivity, slow surface reaction rate, small hole diffusion length, etc.
Most of the methods reported in the literature to control morphology are complicated to operate and have high requirements on the environment and conditions.

Method used

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  • Method for preparing iron oxide photoanode under combined action of oxalic acid and tetrabutyl titanate
  • Method for preparing iron oxide photoanode under combined action of oxalic acid and tetrabutyl titanate
  • Method for preparing iron oxide photoanode under combined action of oxalic acid and tetrabutyl titanate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] α-Fe 2 o 3 The preparation method of the photoanode is as follows:

[0023] (1) Clean the FTO substrate in an ultrasonic bath with detergent, deionized water, acetone and ethanol for 20 minutes, and then dry it with nitrogen flow. Then standard double electrodes were used, with FTO as the working electrode and platinum sheet as the counter electrode. 4 ·7H 2 O concentration is 36g·L -1 , (NH 4 ) 2 SO 4 The concentration is 22g·L -1 In the electrolytic solution, the Fe film formed on the surface of the FTO substrate was obtained by depositing at a current of 5mA for 180s by the constant current method.

[0024] (2) Wash the Fe film with ethanol, air-dry it, anneal it in argon at 750 °C for 10 min, and cool it naturally to room temperature at a heating rate of 10 °C / min to obtain α-Fe 2 o 3 Photoanode.

Embodiment 2

[0026] Fe 2 o 3 -H 2 C 2 o 4 The preparation method of photoanode comprises the steps:

[0027] (1) is consistent with step (1) in embodiment 1;

[0028] (2) with 50wt% H 2 O in 0.3mol / L oxalic acid ethanol solution soaked at 60°C for 20min to obtain FeC 2 o 4 membrane;

[0029] (3) FeC in step (2) 2 o 4 Membrane is washed with ethanol, after air drying, carries out annealing treatment, and the annealing treatment condition is identical with the step (2) in the specific example 1, namely annealing in argon at 750 DEG C for 10min, heating rate is 10 DEG C / min, naturally cooling to room temperature, Fe 2o 3 -H 2 C 2 o 4 Photoanode.

Embodiment 3

[0031] Fe 2 o 3 -The preparation method of TBT photoanode comprises the steps:

[0032] (1) is consistent with step (1) in embodiment 1;

[0033] (2) Immerse the Fe film prepared in step (1) in the mixed solution of tetrabutyl titanate ethanol solution and concentrated hydrochloric acid, soak for 30s, and perform ultrasonic treatment during the soaking process to ensure that tetrabutyl titanate is evenly attached to the surface of the Fe film. The concentration of tetrabutyl titanate ethanol solution is 0.01mol / L, the mass concentration of concentrated hydrochloric acid is 36%, the volume of ethanol in the mixed solution is 4.95mL, the volume of concentrated HCI is 42 μL, and the volume of tetrabutyl titanate is 17 μL.

[0034] (3) Washing the Fe film after soaking in step (2) with ethanol, after air drying, heat treatment, the heat treatment conditions are the same as the step (2) in Example 1, that is, annealing in argon for 10min at 750°C, The heating rate is 10°C / min, a...

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Abstract

The invention relates to a method for preparing an iron oxide photoanode under the combined action of oxalic acid and tetrabutyl titanate. The method comprises the following steps: carrying out simpleelectrodeposition to obtain an an iron film, soaking the iron film in an oxalic acid (H2C2O4) ethanol solution while heating, carrying out ultrasonic soaking with tetrabutyl titanate (TBT), and carrying out annealing treatment to obtain the Fe2O3-H2C2O4+TBT photoanode. Due to oxalic acid and tetrabutyl titanate, the specific surface area of ferric oxide is increased, electron hole recombination is reduced, and the photoelectric property of ferric oxide is improved. Under AM1.5 standard test conditions, the photocurrent density can reach 0.59 mA cm<2> at 1.23 V relative to a reversible hydrogen electrode. Different from a reported method, the method of the invention has the advantages that raw materials are cheap and easy to obtain, the whole photoelectrode preparation process is fast, andlarge-batch preparation is easy. Different from a conventional method for controlling morphology, the method of the invention is completed by simple impregnation and chemical reaction.

Description

technical field [0001] The present invention relates to Fe in the photoelectrochemical process in solar energy utilization 2 o 3 A structure of a photoanode and a preparation method thereof, specifically a preparation method of an iron oxide photoanode in which oxalic acid and tetrabutyl titanate act together. Background technique [0002] With the improvement of people's living standards, people's demand for energy continues to increase, resulting in an increasingly serious shortage of energy resources. Traditional fossil energy is not only non-renewable energy, but also produces a lot of pollution. As a result, attention is being turned to solar energy, an inexhaustible natural resource. The photoelectrochemical splitting of water to produce hydrogen is the most promising way for humans to use solar energy as a clean energy source in the future. Among various semiconductors, iron oxide (α-Fe 2 o 3 ) not only has the characteristics of natural abundance, low cost, and...

Claims

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Application Information

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IPC IPC(8): H01G9/20H01G9/042
CPCH01G9/2027Y02E10/542
Inventor 陈智栋田大香李龙珠刘长海王世颖王文昌
Owner CHANGZHOU UNIV
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