CN110923747A - Preparation method of bismuth ferrite photocatalytic film electrodeposition - Google Patents
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Abstract
The invention discloses a preparation method of bismuth ferrite photocatalytic film electrodeposition. The method comprises the following steps: 1) pretreating FTO; 2) dissolving bismuth nitrate pentahydrate and potassium iodide in water, adding rare earth salt ions, and adjusting the pH value with nitric acid; 3) dissolving p-benzoquinone in ethanol; 4) mixing the two, and carrying out electrochemical deposition to obtain a thin film electrode; 5) and (4) dripping dimethyl sulfoxide dissolved with ferrous acetylacetonate into the film electrode obtained in the step (4), and performing high-temperature heat treatment in a vacuum tube furnace to obtain the bismuth ferrite film. The preparation method is simple and easy to realize, has low requirements on the size and the shape of the bottom electrode, uniform film quality, large specific surface area, accurate stoichiometric ratio, excellent photocatalytic performance and high water photolysis efficiency, and is easy to carry out doping modification research.
Description
Technical Field
The invention relates to the technical field of film preparation, in particular to a preparation method of bismuth ferrite photocatalytic film electrodeposition.
Background
With the rapid development of social economy, energy shortage and environmental pollution are two major and troublesome problems facing the current human society, and the direct utilization of solar energy to solve the global energy and pollution problems is increasingly paid more attention by human beings. The photocatalytic reaction can convert solar energy into high-density electric energy and chemical energy, and can be directly used in the fields of air purification, sewage treatment, hydrogen production and the like. Therefore, photocatalysis has great potential in solving the problems of energy shortage and environmental pollution in the current society.
The bismuth ferrite material is one of important functional materials, has the forbidden band width of only 2.16eV, has the advantage of obvious narrow band gap compared with other photocatalytic materials, and can directly utilize visible light to complete the photocatalytic process. Meanwhile, due to the excellent characteristics of ferroelectricity, dielectric, pyroelectricity, piezoelectricity and the like, the bismuth ferrite material has an important position and an extremely high application value in the aspects of solid devices such as a memory, an infrared detector, an acoustic surface wave, an integrated photoelectric device and the like, and along with the trend of research heat of the ferroelectric material, the bismuth ferrite material is more and more favored as a novel photocatalyst material.
The sol-gel method is the most general method for preparing bismuth ferrite film materials, and in the process of synthesizing the bismuth ferrite film by using the sol-gel method, a plurality of factors determining the appearance and performance of the film are provided, in the process of colloidally configuring, the selection and proportion of the solvent mainly affect the structure and performance of the film, and if the difference of the crystal structure between the film and the bottom electrode is larger, the lattice mismatch coefficient is larger, so that larger contact surface stress exists between the film and the bottom electrode, and the film is cracked or even falls off. The microwave drying method is one of the better film drying methods at present. The annealing temperature mainly affects the degree of crystallization of the film. In general, the higher the temperature, the larger the film grains, the higher the crystallization level of the film, however, the higher the temperature may increase the number of defects inside the material.
The invention relates to a preparation method of bismuth ferrite photocatalytic film electrodeposition, which is simple and easy to realize, has low requirements on the size and the shape of a bottom electrode, uniform film quality, large specific surface area, accurate stoichiometric ratio, excellent photocatalytic performance and high water photolysis efficiency, and is easy to carry out doping modification research.
Disclosure of Invention
The invention aims to provide a preparation method of bismuth ferrite photocatalytic film electrodeposition.
The method comprises the following steps:
1) cleaning conductive glass FTO (2cm x 2cm), ultrasonic cleaning for 10-50min by using deionized water and acetone in sequence, and then ultrasonic cleaning for 10-60min by using a mixed solution with a volume ratio of 1:1:1 (deionized water, acetone and isopropanol);
2) dissolving 0.01-1M pentahydrate bismuth nitrate and 0.1-1M potassium iodide in 50ml of deionized water, adding rare earth salt ions RE, adding nitric acid to adjust the pH value to 1.0-4.0, and uniformly stirring to obtain a solution A;
3) dissolving 0.1-1M p-benzoquinone in 20ml of ethanol, and stirring for a few minutes to obtain a solution B;
4) and mixing the solution A and the solution B to obtain an electrodeposition solution, performing electrodeposition by adopting a three-electrode method under a CHI760E electrochemical workstation, wherein FTO is used as a working electrode, Ag/AgCl is used as a reference electrode, and a platinum wire is used as a counter electrode. Depositing for 1-60min under the constant potential of-1V to 0.5V vs (Ag/AgCl), and washing with deionized water to obtain a thin film electrode;
5) dissolving 0.1-1M ferrous acetylacetonate in 5ml dimethyl sulfoxide, uniformly stirring to obtain solution C, dripping 0.1-0.5ml of solution C on the obtained film electrode, carrying out heat treatment in a tubular furnace, and keeping the temperature at 400-700 ℃ for 1-5 h.
The rare earth salt ion is one of nitrate, sulfate and chloride salt, the molar concentration of RE is 0.001-0.3M, and the RE element is one or more of La, Ce, Pr, Nd, Sm, Gd, Tb, Dy, Ho, Yb and Y.
The invention has the following advantages: (1) the invention adopts cheap and easily available raw materials for preparation, the preparation conditions are simple and easy to realize, and the preparation period is short. (2) The invention has low requirements on the size and the shape of the bottom electrode, uniform film quality, large specific surface area, accurate chemical metering ratio, excellent photocatalytic performance and high water photolysis efficiency, and is easy to carry out doping modification research.
Detailed Description
1) Cleaning conductive glass FTO (2cm x 2cm), ultrasonic cleaning for 10-50min by using deionized water and acetone in sequence, and then ultrasonic cleaning for 10-60min by using a mixed solution with a volume ratio of 1:1:1 (deionized water, acetone and isopropanol);
2) dissolving 0.01-1M pentahydrate bismuth nitrate and 0.1-1M potassium iodide in 50ml of deionized water, adding rare earth salt ions RE, adding nitric acid to adjust the pH value to 1.0-4.0, and uniformly stirring to obtain a solution A;
3) dissolving 0.1-1M p-benzoquinone in 20ml of ethanol, and stirring for a few minutes to obtain a solution B;
4) and mixing the solution A and the solution B to obtain an electrodeposition solution, performing electrodeposition by adopting a three-electrode method under a CHI760E electrochemical workstation, wherein FTO is used as a working electrode, Ag/AgCl is used as a reference electrode, and a platinum wire is used as a counter electrode. Depositing for 1-60min under the constant potential of-1V to 0.5V vs (Ag/AgCl), and washing with deionized water to obtain a thin film electrode;
5) dissolving 0.1-1M ferrous acetylacetonate in 5ml dimethyl sulfoxide, uniformly stirring to obtain solution C, dripping 0.1-0.5ml of solution C on the obtained film electrode, carrying out heat treatment in a tubular furnace, and keeping the temperature at 400-700 ℃ for 1-5 h.
The rare earth salt ion is one of nitrate, sulfate and chloride salt, the molar concentration of RE is 0.001-0.3M, and the RE element is one or more of La, Ce, Pr, Nd, Sm, Gd, Tb, Dy, Ho, Yb and Y.
Example 1
1) Cleaning the conductive glass FTO, sequentially adopting liquid detergent, water, deionized water and acetone to perform ultrasonic cleaning for 10min, and then adopting a mixed solution with a volume ratio of 1:1:1 (deionized water, acetone and isopropanol) to perform ultrasonic cleaning for 60 min;
2) dissolving 0.04M pentahydrate bismuth nitrate and 0.4M potassium iodide in 50ml deionized water, and adding 0.01M rare earth nitrate ion La3+Then adding nitric acid to adjust the PH value to 2, and uniformly stirring to obtain a solution A;
3) dissolving 0.23M p-benzoquinone in 20ml ethanol, and stirring for a few minutes to obtain a solution B;
4) and mixing the solution A and the solution B to obtain an electrodeposition solution, performing electrodeposition by adopting a three-electrode method, wherein FTO is used as a working electrode, Ag/AgCl is used as a reference electrode, and a platinum wire is used as a counter electrode. Depositing for 5min under the constant potential of-0.1V vs (Ag/AgCl), and washing with deionized water to obtain a thin film electrode;
5) dissolving 0.1M ferrous acetylacetonate in 5ml dimethyl sulfoxide, uniformly stirring to obtain a solution C, dropwise adding 0.1ml of the solution C on the obtained film electrode, carrying out heat treatment in a tubular furnace, keeping the temperature at 450 ℃ for 2h, and increasing the temperature at the rate of 2 ℃/min to obtain the bismuth ferrite film with uniform and stable quality, wherein the film has good photocatalytic performance, and the degradation rate of a pollutant methyl orange can reach 90% per hour per square centimeter.
Example 2
1) Cleaning the conductive glass FTO, sequentially adopting liquid detergent, water, deionized water and acetone to perform ultrasonic cleaning for 10min, and then adopting a mixed solution with a volume ratio of 1:1:1 (deionized water, acetone and isopropanol) to perform ultrasonic cleaning for 60 min;
2) 0.04M bismuth nitrate pentahydrate and 0.4M potassium iodide were dissolved in 50ml deionized water, and 0.005M rare earth nitrate ion Yb was added3+Then adding nitric acid to adjust the PH value to 2, and uniformly stirring to obtain a solution A;
3) dissolving 0.23M p-benzoquinone in 20ml ethanol, and stirring for a few minutes to obtain a solution B;
4) and mixing the solution A and the solution B to obtain an electrodeposition solution, performing electrodeposition by adopting a three-electrode method, wherein FTO is used as a working electrode, Ag/AgCl is used as a reference electrode, and a platinum wire is used as a counter electrode. Depositing for 10min under the constant potential of-0.5V vs (Ag/AgCl), and washing with deionized water to obtain a thin film electrode;
5) dissolving 0.2M ferrous acetylacetonate in 5ml dimethyl sulfoxide, uniformly stirring to obtain a solution C, dropwise adding 0.1ml of the solution C on the obtained film electrode, carrying out heat treatment in a tubular furnace, keeping the temperature at 500 ℃ for 2h, and increasing the temperature at the rate of 2 ℃/min to obtain the bismuth ferrite film with uniform and stable quality, wherein the film has good photocatalytic performance, and the degradation rate of a pollutant methyl orange can reach 93% per hour per square centimeter.
Example 3
1) Cleaning the conductive glass FTO;
2) dissolving 0.2M pentahydrate bismuth nitrate and 0.6M potassium iodide in 50ml deionized water, and adding 0.1M rare earth nitrate ion Y3+0.05M of rare earth nitrate ion Nd3+Then adding nitric acid to adjust the pH to 1, and homogenizingStirring to obtain a solution A;
3) dissolving 0.5M p-benzoquinone in 20ml of ethanol, and stirring for a few minutes to obtain a solution B;
4) and mixing the solution A and the solution B to obtain an electrodeposition solution, performing electrodeposition by adopting a three-electrode method, wherein FTO is used as a working electrode, Ag/AgCl is used as a reference electrode, and a platinum wire is used as a counter electrode. Depositing for 30min under the constant potential of 0.3V vs (Ag/AgCl), and washing with deionized water to obtain a thin film electrode;
5) dissolving 0.6M ferrous acetylacetonate in 5ml dimethyl sulfoxide, uniformly stirring to obtain solution C, dripping 0.2ml of solution C on the obtained film electrode, carrying out heat treatment in a tubular furnace, and keeping the temperature at 550 ℃ for 2 hours to obtain a bismuth ferrite film with uniform and stable quality, wherein the photocurrent of the film can reach 0.9mA/cm under the irradiation of standard sunlight2。
Example 4
1) Cleaning the conductive glass FTO;
2) dissolving 0.2M pentahydrate bismuth nitrate and 0.6M potassium iodide in 50ml deionized water, and adding 0.1M rare earth nitrate ion Y3+0.05M of rare earth nitrate ion Nd3+Then adding nitric acid to adjust the PH value to 1, and uniformly stirring to obtain a solution A;
3) dissolving 0.5M p-benzoquinone in 20ml of ethanol, and stirring for a few minutes to obtain a solution B;
4) and mixing the solution A and the solution B to obtain an electrodeposition solution, performing electrodeposition by adopting a three-electrode method, wherein FTO is used as a working electrode, Ag/AgCl is used as a reference electrode, and a platinum wire is used as a counter electrode. Depositing for 30min under the constant potential of 0.3V vs (Ag/AgCl), and washing with deionized water to obtain a thin film electrode;
5) dissolving 0.6M ferrous acetylacetonate in 5ml dimethyl sulfoxide, uniformly stirring to obtain solution C, dripping 0.2ml of solution C on the obtained film electrode, carrying out heat treatment in a tubular furnace, and keeping the temperature at 550 ℃ for 2 hours to obtain a bismuth ferrite film with uniform and stable quality, wherein the photocurrent of the film can reach 0.9mA/cm under the irradiation of standard sunlight2。
Example 5
1) Cleaning the conductive glass FTO;
2) mixing 0.3M pentahydrateBismuth nitrate and 0.3M potassium iodide were dissolved in 100ml of deionized water, and 0.05M of rare earth nitrate ion Ce was added3+Then adding nitric acid to adjust the PH value to 1, and uniformly stirring to obtain a solution A;
3) dissolving 0.2M p-benzoquinone in 20ml of ethanol, and stirring for a few minutes to obtain a solution B;
4) mixing the solution A and the solution B to be used as an electrodeposition solution, performing electrodeposition by adopting a three-electrode method, depositing for 15min under the constant potential of-0.8V vs (Ag/AgCl), and washing with deionized water to obtain a film electrode;
5) dissolving 0.2M ferrous acetylacetonate in 5ml dimethyl sulfoxide, uniformly stirring to obtain solution C, dripping 0.2ml solution C on the above-mentioned obtained film electrode, making heat treatment in tubular furnace, heat-insulating at 550 deg.C for 1 hr to obtain the bismuth ferrite film with uniform and stable quality, under the irradiation of standard sunlight, the photocurrent of said film can be up to 1.3mA/cm2。
Claims (6)
1. A preparation method of bismuth ferrite photocatalytic film electrodeposition is characterized by comprising the following steps:
1) cleaning FTO conductive glass;
2) dissolving bismuth nitrate pentahydrate and potassium iodide in deionized water, adding rare earth salt ions RE, adding nitric acid to adjust the pH value to 1.0-4.0, and uniformly stirring to obtain a solution A;
3) dissolving p-benzoquinone in ethanol, wherein the molar concentration of the benzoquinone is 0.1-1M, and stirring for 5-50 minutes to obtain a solution B;
4) mixing the solution A and the solution B to obtain an electrodeposition solution, performing electrodeposition by adopting a three-electrode method, and washing by using deionized water to obtain a deposited layer;
5) dissolving ferrous acetylacetonate in dimethyl sulfoxide, uniformly stirring to obtain a solution C, dripping 0.1-0.5ml of solution C on the above-mentioned settled layer, then making heat treatment at 400-700 deg.C for 1-5 hr in tubular furnace.
2. The method for preparing the bismuth ferrite photocatalytic film electrodeposition according to claim 1, wherein in the step 1), the FTO is cleaned by sequentially adopting deionized water and acetone for ultrasonic cleaning for 10-50min, and then adopting a mixed solution with a volume ratio of 1:1:1 (deionized water, acetone and isopropanol) for ultrasonic cleaning for 10-60 min.
3. The method according to claim 1, wherein in step 2), the molar concentration of bismuth nitrate pentahydrate is 0.01-1M, and the molar concentration of potassium iodide is 0.1-1M.
4. The method for preparing bismuth ferrite photocatalytic film electrodeposition according to claim 1, wherein in step 2), the rare earth salt ion is one of nitrate, sulfate and chloride salt, the molar concentration of the rare earth salt ion RE is 0.001-0.3M, and RE is one or more of La, Ce, Pr, Nd, Sm, Gd, Tb, Dy, Ho, Yb and Y elements.
5. The method for preparing the bismuth ferrite photocatalytic film through electrodeposition according to claim 1, wherein in the step 4), the three-electrode method is adopted for electrodeposition, wherein FTO is used as a working electrode, Ag/AgCl is used as a reference electrode, a platinum wire is used as a counter electrode, and the working electrode is subjected to electrodeposition for 1-60min at a constant potential of-1V to 0.5V vs (Ag/AgCl).
6. The method according to claim 1, wherein the bismuth ferrite photocatalytic film is uniform and has an available surface area ranging from 1 cm to 100 cm2。
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116371415A (en) * | 2023-04-14 | 2023-07-04 | 哈尔滨工程大学 | Preparation method of cerium doped material for improving catalytic performance of bismuth ferrite |
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