CN112725771A - Ti-based photo-anode, preparation method thereof and application thereof in preparing oxygen by photoelectrocatalysis total hydrolysis - Google Patents

Ti-based photo-anode, preparation method thereof and application thereof in preparing oxygen by photoelectrocatalysis total hydrolysis Download PDF

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CN112725771A
CN112725771A CN202110098698.5A CN202110098698A CN112725771A CN 112725771 A CN112725771 A CN 112725771A CN 202110098698 A CN202110098698 A CN 202110098698A CN 112725771 A CN112725771 A CN 112725771A
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titanium dioxide
anode
substrate
molecular catalyst
hydrothermal reaction
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CN112725771B (en
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王心晨
马一文
方元行
苏加鑫
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Fuzhou University
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
    • C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
    • C23C18/1204—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material inorganic material, e.g. non-oxide and non-metallic such as sulfides, nitrides based compounds
    • C23C18/1208—Oxides, e.g. ceramics
    • C23C18/1216—Metal oxides
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
    • C23C22/06—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6
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    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B1/00—Electrolytic production of inorganic compounds or non-metals
    • C25B1/01—Products
    • C25B1/02—Hydrogen or oxygen
    • C25B1/04—Hydrogen or oxygen by electrolysis of water
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    • Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis

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Abstract

The invention discloses a method for preparing a Ti-based photo-anode by a surface grafting technology, which is applied to a full hydrolysis reaction and belongs to the technical field of material preparation and photoelectrocatalysis. Titanium dioxide nanorods are used as a substrate, isopropyl titanate is used as a titanium source, 2, 5-dihydroxy terephthalic acid is used as a ligand, acetic acid is used as a solvent, a molecular catalyst containing Ti-oxo is grafted on the titanium dioxide in situ through a hydrothermal reaction, and the molecular catalyst is connected with the titanium dioxide substrate through a Ti-O bond. The photoelectric anode manufactured by the invention has proper energy band position, stronger light absorption capacity and charge transmission capacity, and the catalytic performance in neutral electrolyte is greatly improved compared with that of the titanium dioxide substrate. The method has the advantages of simple process, low cost and great application potential.

Description

Ti-based photo-anode, preparation method thereof and application thereof in preparing oxygen by photoelectrocatalysis total hydrolysis
Technical Field
The invention belongs to the technical field of material preparation and photoelectrocatalysis, and particularly relates to a Ti-based photoanode, a preparation method thereof and application thereof in preparing oxygen by photoelectrocatalysis full hydrolysis.
Background
The shortage of energy is one of the main problems of modern society, and the search for new energy is imminent. Among the many new energy sources, hydrogen is an attractive clean fuel at its high energy density. The photocatalytic hydrogen production by water decomposition is a promising hydrogen production method using sunlight as a reaction driving force and water as a reaction raw material, and the efficiency of photoelectrocatalysis is high because a low bias voltage is additionally applied (nature 1972, 5358 and 37). The cathode generates hydrogen, the anode generates oxygen, and the integral decomposition of water is realized. However, conventional metal semiconductor materials, which are often used for the photo-anode, have low photoelectric conversion efficiency due to a wide band gap and carrier recombination. The molecular catalyst developed in recent years has wide application prospect due to high activity and adjustability, and has great potential in the fields of solar energy water decomposition, carbon dioxide reduction and the like.
Molecular complexes of some metals are alternatives to metal oxides, and by adjusting the molecular composition, very high specific activities can be obtained. Some molecular catalysts also have the ability to absorb light, even visible light (nat. energy. 2019.4.290). In the photoelectrocatalytic system, light absorption is the first step and charge separation and transport is also necessary. However, complete contact is the primary condition for charge transport, and in essence, the advantages of molecular catalysts are maximized if they can be chemically bonded to the substrate in some way.
Disclosure of Invention
The invention aims to provide a method for preparing a photoanode by using a surface grafting technology and application of the photoanode to full water splitting. The molecular catalyst is grafted on the titanium dioxide nanorod substrate by a secondary in-situ method, and the molecular catalyst and the titanium dioxide substrate are connected by a Ti-O bond, so that the light absorption capacity is improved, the separation and transmission of charges are promoted, and the efficient photoelectrocatalysis water decomposition reaction in neutral electrolyte can be realized. The invention has the characteristics of simple process, low cost, high photocatalytic performance and the like, meets the actual production requirement and has larger application potential.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for preparing a Ti-based photo-anode by a surface grafting technology comprises the following steps: the titanium dioxide nano-rod is taken as a substrate, a molecular catalyst containing Ti-oxo is grafted on the titanium dioxide by a secondary in-situ growth method, the light absorption capacity of the synthesized photoelectrode is enhanced, the charge separation capacity is enhanced, and the photocurrent density is 2 times that of the titanium dioxide substrate.
A method for preparing a Ti-based photo-anode by a surface grafting technology comprises the following steps:
(1) the preparation method of the titanium dioxide nanorod substrate comprises the following steps:
1) SnO doped with fluorine2Conductive glass (FTO) was placed in a mixed solution containing 0.3ml of n-tetrabutyltitanate, 13ml of hydrochloric acid (37 wt%), and 15ml of deionized water, and subjected to hydrothermal reaction at 150 ℃ for 12 hours.
2) Calcining the product in air atmosphere at 550 ℃ for 2 hours to prepare the titanium dioxide nano rod with good crystallinity growing on the FTO.
(2) Grafting a molecular catalyst on a titanium dioxide nanorod substrate: placing a titanium dioxide nanorod substrate in a hydrothermal reaction kettle containing 0.25mmol of 2, 5-dihydroxy terephthalic acid, 0.25mmol of isopropyl titanate and 17ml of acetic acid, and performing hydrothermal reaction at 150 ℃ for 18 hours to obtain a Ti-based photo-anode; normally, one Ti atom is coordinated to six O atoms. In this Ti-based molecular catalyst, Ti atoms form an octahedral configuration molecular catalyst with six O atoms in the hydroxyl group and the carboxyl group. The long chain structure of tetrabutyl titanate makes it difficult to react with 2, 5-dihydroxy terephthalic acid to produce a Ti-containing molecular catalyst. The short chain structure of isopropyl titanate makes 2, 5-dihydroxy terephthalic acid easy to react with central Ti atom to produce molecular catalyst.
The invention has the following remarkable advantages: the Ti-oxo molecular catalyst is grafted on the titanium dioxide nano-rod by a preparation method of secondary hydrothermal in-situ growth. Because the two are similar in configuration and both contain titanium elements, titanium dioxide and the molecular catalyst can be connected through a chemical bond Ti-O, and the contact is good. The composite structure can improve the light absorption capacity of the photoelectrode, extend the absorption edge to more than 600 nm, promote the separation of electrons and holes, improve the reaction efficiency and improve the photocurrent by 1 time compared with the base titanium dioxide. The whole production process is simple and convenient, easy to control, low in energy consumption and low in cost, meets the actual production requirement, and is favorable for large-scale popularization.
Drawings
FIG. 1 is a transmission electron microscope photograph of Ti-oxo molecular catalyst grafted titanium dioxide nanorods obtained in example 2;
FIG. 2 is a graph of the UV-visible diffuse reflectance spectra of the materials obtained in example 1 (dashed line) and example 2 (solid line);
FIG. 3 is a graph of the oxygen signal of the X-ray photoelectron spectroscopy analysis of example 2;
FIG. 4 is a graph of the measured impedance of example 1 (square) and example 2 (circle);
FIG. 5 is a linear sweep voltammogram of example 1 (dashed line), example 2 (solid line), example 3 (dotted line);
FIG. 6 is a linear scanning voltammogram of examples 2 and 4.
Detailed Description
The following are several examples of the present invention to further illustrate the present invention, but the present invention is not limited thereto.
Example 1
FTO was placed in a mixed solution containing 0.3ml of n-tetrabutyltitanate, 13ml of hydrochloric acid and 15ml of deionized water, and subjected to a hydrothermal reaction at 150 ℃ for 12 hours. And calcining the sample in an air atmosphere at 550 ℃ for 2 hours to obtain the titanium dioxide nanorod with good crystallinity growing on the FTO.
Example 2
FTO was placed in a mixed solution containing 0.3ml of n-tetrabutyltitanate, 13ml of hydrochloric acid and 15ml of deionized water, and subjected to a hydrothermal reaction at 150 ℃ for 12 hours. And calcining the sample in an air atmosphere at 550 ℃ for 2 hours to obtain the titanium dioxide nanorod with good crystallinity growing on the FTO. Placing the titanium dioxide nanorod substrate in a hydrothermal reaction kettle containing 0.25mmol of 2, 5-dihydroxyterephthalic acid, 0.25mmol of isopropyl titanate and 17ml of acetic acid, and carrying out hydrothermal reaction at 150 ℃ for 18 hours to obtain the molecular catalyst grafted on the titanium dioxide nanorods.
Example 3
FTO was placed in a hydrothermal reaction kettle containing 0.25mmol of 2, 5-dihydroxyterephthalic acid, 0.25mmol of isopropyl titanate and 17ml of acetic acid and the molecular catalyst growing directly on FTO was prepared by hydrothermal reaction at 150 ℃ for 18 hours.
Example 4
FTO was placed in a mixed solution containing 0.3ml of n-tetrabutyltitanate, 13ml of hydrochloric acid and 15ml of deionized water, and subjected to a hydrothermal reaction at 150 ℃ for 12 hours. And calcining the sample in an air atmosphere at 550 ℃ for 2 hours to obtain the titanium dioxide nanorod with good crystallinity growing on the FTO. Placing the titanium dioxide nanorod substrate in a hydrothermal reaction kettle containing 0.25mmol of 2, 5-dihydroxyterephthalic acid, 0.25mmol of isopropyl titanate and 17ml of acetic acid, and performing hydrothermal reaction at 150 ℃ for 12 hours, 24 hours and 48 hours respectively to obtain the molecular catalyst grafted on the titanium dioxide nanorods.
FIG. 1 is a transmission electron microscope photograph of the Ti-oxo molecular catalyst grafted titanium dioxide nanorods obtained in example 2, from which it can be observed that the prepared molecular catalyst grows on the outer layer of the titanium dioxide nanorods, nucleating shell structure.
Fig. 2 is a graph of the uv-vis diffuse reflectance spectra of the samples obtained in example 1 and example 2. It can be observed from the figure that the absorption edge of the sample after grafting the molecular catalyst extends to 600 nm.
FIG. 3 is a graph of the oxygen signal of the X-ray photoelectron spectroscopy analysis of example 2. After grafting the molecular catalyst, the photoanode showed a signal of C — O bond, C = O bond, indicating that the molecular catalyst was complexed with titanium dioxide.
Fig. 4 is a graph of the measured impedance of example 1 and example 2. It can be seen from the figure that the impedance of the sample is obviously reduced after the molecular catalyst is grafted, and the charge transmission capability is enhanced.
FIG. 5 is a linear scanning voltammogram of examples 1, 2, and 3. The light source is AM 1.5G simulated sunlight, and the electrolyte is 0.2M Na2SO4And (3) solution. From the figure, it can be seen that the photocurrent after the molecular catalyst is grafted on the titanium dioxide nanorods is 2 times that of the original titanium dioxide nanorods; while the molecular catalyst grows directly on FTO, the photocurrent is very low.
FIG. 6 is a linear scanning voltammogram of examples 2 and 4. Under the irradiation of simulated sunlight by a light source AM 1.5G, the light is in 0.2M Na2SO4As can be seen from the graph, the photocurrent was highest when the secondary hydrothermal treatment was carried out for 18 hours.
The above description is only a preferred embodiment of the present invention, and all the changes of the precursor dosage ratio, the hydrothermal temperature and the calcination temperature made according to the claims of the present invention should be covered by the present invention.

Claims (9)

1. A preparation method of a Ti-based photo-anode is characterized by comprising the following steps: the Ti-oxo-containing molecular catalyst is grafted on the titanium dioxide nano-rod by using the titanium dioxide nano-rod as a substrate through a secondary hydrothermal in-situ growth method to obtain the Ti-based photo-anode.
2. The method of claim 1, wherein the Ti-based photoanode comprises: the method specifically comprises the following steps:
(1) preparing a titanium dioxide nanorod substrate: firstly, placing FTO in a mixed solution containing tetrabutyl titanate, hydrochloric acid and deionized water to carry out hydrothermal reaction, and then calcining a product to prepare a titanium dioxide nanorod growing on the FTO and having good crystallinity;
(2) surface grafting: and (2) placing the titanium dioxide nanorod substrate obtained in the step (1) in a hydrothermal reaction kettle containing 2, 5-dihydroxy terephthalic acid, isopropyl titanate and acetic acid for hydrothermal reaction, and grafting a Ti-oxo molecular catalyst on the titanium dioxide nanorod to obtain the Ti-based photo-anode.
3. The method of claim 2, wherein the Ti-based photoanode comprises: the volume of the tetrabutyl titanate in the mixed solution in the step (1) is 0.3ml, the volume of the hydrochloric acid is 13ml, and the volume of the deionized water is 15 ml.
4. The method of claim 2, wherein the Ti-based photoanode comprises: the temperature of the hydrothermal reaction in the step (1) is 150 ℃, and the reaction time is 12 h.
5. The method of claim 2, wherein the Ti-based photoanode comprises: the calcining conditions in the step (1) are as follows: calcining at 550 deg.C in air atmosphere for 2 h.
6. The method of claim 2, wherein the Ti-based photoanode comprises: the molar weight of the 2, 5-dihydroxy terephthalic acid in the step (2) is 0.25mmol, the molar weight of isopropyl titanate is 0.25mmol, and the volume of acetic acid is 17 ml.
7. The method of claim 2, wherein the Ti-based photoanode comprises: the temperature of the hydrothermal reaction in the step (2) is 150 ℃, and the reaction time is 18 h.
8. A Ti-based photoanode prepared by the method of any one of claims 1 to 7, wherein: the Ti-based photo-anode has a core-shell structure, the light absorption performance is enhanced, and the absorption band edge extends to more than 600 nm; the molecular catalyst of Ti-oxo is connected with the titanium dioxide substrate by Ti-O bonds, so that the charge separation and the transmission capability are enhanced.
9. Use of a Ti-based photoanode according to claim 8 in the preparation of oxygen by photoelectrocatalytic total hydrolysis.
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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2012024757A (en) * 2010-06-24 2012-02-09 Kyushu Univ Light hydrogen generation catalyst consisting of base metal complex and titanium dioxide
CN105312090A (en) * 2015-12-07 2016-02-10 福州大学 Preparation of (C5H5) Ru/TiO2 organic-inorganic hybrid photocatalyst
CN105540655A (en) * 2015-12-21 2016-05-04 河南师范大学 Three-dimensional dendritic structure TiO2 array preparation method
CN106548871A (en) * 2015-09-23 2017-03-29 湖南大学 The application of composite titania material and preparation method thereof, light anode and light anode
CN106757055A (en) * 2016-12-14 2017-05-31 中国科学院海洋研究所 A kind of method that hydro-thermal method prepares nanometer tube composite film light anode
CN108597886A (en) * 2018-04-28 2018-09-28 常州工程职业技术学院 A kind of organic solution and its application for modified oxidized iron light anode
CN110882725A (en) * 2019-12-06 2020-03-17 北京科技大学 Metal organic framework loaded titanium dioxide photocatalytic material and preparation method thereof

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2012024757A (en) * 2010-06-24 2012-02-09 Kyushu Univ Light hydrogen generation catalyst consisting of base metal complex and titanium dioxide
CN106548871A (en) * 2015-09-23 2017-03-29 湖南大学 The application of composite titania material and preparation method thereof, light anode and light anode
CN105312090A (en) * 2015-12-07 2016-02-10 福州大学 Preparation of (C5H5) Ru/TiO2 organic-inorganic hybrid photocatalyst
CN105540655A (en) * 2015-12-21 2016-05-04 河南师范大学 Three-dimensional dendritic structure TiO2 array preparation method
CN106757055A (en) * 2016-12-14 2017-05-31 中国科学院海洋研究所 A kind of method that hydro-thermal method prepares nanometer tube composite film light anode
CN108597886A (en) * 2018-04-28 2018-09-28 常州工程职业技术学院 A kind of organic solution and its application for modified oxidized iron light anode
CN110882725A (en) * 2019-12-06 2020-03-17 北京科技大学 Metal organic framework loaded titanium dioxide photocatalytic material and preparation method thereof

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