CN114645286A - Method for regulating and controlling epiphase oxygen vacancy of bismuth oxyhalide with high catalytic activity - Google Patents
Method for regulating and controlling epiphase oxygen vacancy of bismuth oxyhalide with high catalytic activity Download PDFInfo
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- CN114645286A CN114645286A CN202210325895.0A CN202210325895A CN114645286A CN 114645286 A CN114645286 A CN 114645286A CN 202210325895 A CN202210325895 A CN 202210325895A CN 114645286 A CN114645286 A CN 114645286A
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- 229910052797 bismuth Inorganic materials 0.000 title claims abstract description 31
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 title claims abstract description 31
- 238000000034 method Methods 0.000 title claims abstract description 31
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 title claims abstract description 27
- 229910052760 oxygen Inorganic materials 0.000 title claims abstract description 27
- 239000001301 oxygen Substances 0.000 title claims abstract description 27
- 230000001276 controlling effect Effects 0.000 title claims abstract description 22
- 230000001105 regulatory effect Effects 0.000 title claims abstract description 20
- 230000003197 catalytic effect Effects 0.000 title claims abstract description 17
- 239000000843 powder Substances 0.000 claims abstract description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 21
- 230000008569 process Effects 0.000 claims abstract description 10
- 239000007788 liquid Substances 0.000 claims abstract description 9
- 239000002253 acid Substances 0.000 claims abstract description 8
- 239000003513 alkali Substances 0.000 claims abstract description 8
- 239000003792 electrolyte Substances 0.000 claims abstract description 8
- 230000007935 neutral effect Effects 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 5
- 238000001914 filtration Methods 0.000 claims abstract description 5
- 239000002033 PVDF binder Substances 0.000 claims description 6
- 229920002981 polyvinylidene fluoride Polymers 0.000 claims description 6
- 239000004698 Polyethylene Substances 0.000 claims description 5
- 239000012153 distilled water Substances 0.000 claims description 5
- 239000003365 glass fiber Substances 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 4
- 230000005518 electrochemistry Effects 0.000 claims 1
- 230000001699 photocatalysis Effects 0.000 abstract description 7
- 239000011941 photocatalyst Substances 0.000 abstract description 3
- 238000007146 photocatalysis Methods 0.000 abstract description 2
- 238000002360 preparation method Methods 0.000 abstract description 2
- 239000003054 catalyst Substances 0.000 abstract 1
- 238000004140 cleaning Methods 0.000 abstract 1
- 230000000593 degrading effect Effects 0.000 abstract 1
- 239000002957 persistent organic pollutant Substances 0.000 abstract 1
- BWOROQSFKKODDR-UHFFFAOYSA-N oxobismuth;hydrochloride Chemical compound Cl.[Bi]=O BWOROQSFKKODDR-UHFFFAOYSA-N 0.000 description 11
- 238000002474 experimental method Methods 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 238000002848 electrochemical method Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000001362 electron spin resonance spectrum Methods 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 239000002440 industrial waste Substances 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000005067 remediation Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 description 1
- 229940043267 rhodamine b Drugs 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 230000004083 survival effect Effects 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- 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
- C25B1/24—Halogens or compounds thereof
- C25B1/26—Chlorine; Compounds thereof
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/06—Halogens; Compounds thereof
-
- B01J35/39—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
- B01J37/348—Electrochemical processes, e.g. electrochemical deposition or anodisation
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B15/00—Operating or servicing cells
- C25B15/02—Process control or regulation
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B15/00—Operating or servicing cells
- C25B15/02—Process control or regulation
- C25B15/023—Measuring, analysing or testing during electrolytic production
- C25B15/025—Measuring, analysing or testing during electrolytic production of electrolyte parameters
- C25B15/027—Temperature
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B15/00—Operating or servicing cells
- C25B15/02—Process control or regulation
- C25B15/023—Measuring, analysing or testing during electrolytic production
- C25B15/025—Measuring, analysing or testing during electrolytic production of electrolyte parameters
- C25B15/029—Concentration
- C25B15/031—Concentration pH
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B9/00—Cells or assemblies of cells; Constructional parts of cells; Assemblies of constructional parts, e.g. electrode-diaphragm assemblies; Process-related cell features
- C25B9/17—Cells comprising dimensionally-stable non-movable electrodes; Assemblies of constructional parts thereof
- C25B9/19—Cells comprising dimensionally-stable non-movable electrodes; Assemblies of constructional parts thereof with diaphragms
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
Abstract
A method for regulating and controlling an oxygen vacancy of an epiphase of bismuth oxyhalide with high catalytic activity. The invention adopts an electrochemical auxiliary method to treat the catalyst, and improves the concentration of the surface phase oxygen vacancy of the bismuth oxyhalide photocatalyst, thereby greatly improving the photocatalysis property for degrading organic pollutants. The method comprises the following steps: firstly, bismuth oxyhalide is put into an electrolytic cell containing water, and the electrolytic cell is separated by a diaphragm; secondly, adjusting the pH value of the electrolyte by acid (or alkali) under the stirring state; inserting the electrodes into the electrolytic cell, maintaining for a certain time in a constant voltage (or constant current) mode, and controlling the temperature of liquid in the electrolytic cell in the electrifying process; fourthly, filtering the powder obtained in the third step, cleaning the powder to be neutral, and drying the powder to obtain the bismuth oxyhalide powder rich in the high-concentration epiphase oxygen vacancy. The preparation method has the advantages of simplicity, low price, high concentration of the surface phase oxygen vacancy of the sample and the like.
Description
Technical Field
The invention relates to a method for regulating and controlling epiphase oxygen vacancies of bismuth oxyhalide by an electrochemical method.
Background
With the rapid development of science and technology and industry, the emergence of many new industries causes a great amount of industrial waste to be discharged into underground water, and seriously harms human health and the ecological environment of water resources depending on survival. The semiconductor photocatalysis technology using solar energy as a main energy source is considered to be one of the most ideal technical means for treating the current water pollution problem due to the characteristics of energy conservation, high efficiency, no secondary pollution and the like. However, with titanium dioxide (TiO)2) The traditional photocatalyst represented by the general formula has a limited spectral response range and low separation efficiency of a photon-generated carrier, so that the application of the photocatalytic technology in the field of environmental remediation is limited. Bismuth oxyhalide is considered to be one of the most promising new semiconductor photocatalysts due to its unique open layered structure and appropriate energy band structure. However, due to the large forbidden band width, the catalytic degradation efficiency of BiOCl under visible light is not ideal, and the photocatalytic performance of BiOCl needs to be improved. Introduction of oxygen vacancies into BiOCl materials is an effective method for improving their photocatalytic activity.
Disclosure of Invention
The invention provides a method for improving photocatalytic activity by regulating oxygen vacancies through an electrochemical method, aiming at finding a regulation and control process of bismuth oxyhalide epiphase oxygen vacancies to meet the requirement of improving photocatalytic performance.
1. A method for regulating and controlling epiphase oxygen vacancy of bismuth oxyhalide with high catalytic activity is carried out according to the following steps:
firstly, bismuth oxyhalide is put into the negative electrode side of an electrolytic cell containing water, and the electrolytic cell is separated by a diaphragm; the mass ratio of the bismuth oxyhalide to the water is 1: 1-10000, wherein the aperture of the electrolytic cell diaphragm is 3-1000000 nm, and the diaphragm can be made of PE, PVDF, glass fiber and the like;
secondly, adjusting the pH value of the electrolyte by acid (or alkali) in a stirring state, wherein the pH value range is 1-11;
inserting the electrode into an electrolytic cell, wherein the voltage range is 0.1-10000V in a constant voltage mode, the current range is 0.0001-10000 mA in a constant current mode, the power-on time is 1-100000000 s, and the temperature of liquid in the electrolytic cell is controlled to be 0-100 ℃ in the power-on process;
fourthly, after electrifying is finished, the powder obtained in the third step is filtered, washed for 1 to 8 times by using distilled water to be neutral at the temperature of between 30 and 150 DEG C
The bismuth oxyhalide powder regulated and controlled by the invention has the advantages of simple preparation method, low cost, high catalytic activity and the like.
Drawings
FIG. 1 is a photograph of a BiOCl scanning electron microscope prepared in experiment one;
FIG. 2 BiOCl phase analysis plot from experiment one;
FIG. 3 experiment one EPR spectrum of a BiOCl sample was prepared;
FIG. 4 is a graph of photocatalytic degradation of rhodamine B and CIP for a BiOCl sample prepared in experiment one;
Detailed Description
The technical solution of the present invention is not limited to the following specific embodiments, but includes any combination of the specific embodiments.
The first embodiment is as follows: the method for regulating and controlling the epiphase oxygen vacancy of the bismuth oxyhalide with high catalytic activity is carried out according to the following steps:
firstly, bismuth oxyhalide is put into the negative electrode side of an electrolytic cell containing water, and the electrolytic cell is separated by a diaphragm; the mass ratio of the bismuth oxyhalide to the water is 1: 1-10000, wherein the aperture of the electrolytic cell diaphragm is 3-1000000 nm, and the diaphragm can be made of PE, PVDF, glass fiber and the like;
secondly, adjusting the pH value of the electrolyte by acid (or alkali) in a stirring state, wherein the pH value range is 1-11;
inserting the electrode into an electrolytic cell, wherein the voltage range is 0.1-10000V in a constant voltage mode, the current range is 0.0001-10000 mA in a constant current mode, the power-on time is 1-100000000 s, and the temperature of liquid in the electrolytic cell is controlled to be 0-100 ℃ in the power-on process;
fourthly, after electrifying, filtering the powder obtained in the third step, washing the powder for 1 to 8 times by using distilled water to be neutral, and drying the powder at the temperature of between 30 and 150 ℃ to obtain the bismuth oxyhalide powder rich in the high-concentration epiphase oxygen vacancies.
The second embodiment is as follows: the difference between the first embodiment and the second embodiment is that the mass ratio of bismuth oxyhalide to water in the first step is 1: 10-8000, wherein the pore diameter of the diaphragm of the electrolytic cell is 3-1000000 nm, and the material of the diaphragm can be PE, PVDF, glass fiber, etc.
The third concrete implementation mode: the difference between the second embodiment and the first to second embodiments is that the pH of the electrolyte is adjusted by acid (or alkali) in the second step, and the pH range is 1 to 10.
The fourth concrete implementation mode: the present embodiment is different from the first to third embodiments in that the voltage range in the constant voltage mode in the third step is 0.1 to 8000V.
The fifth concrete implementation mode: the difference between this embodiment and the first to fourth embodiments is that in the third step, the current range in the constant current mode is 0.001 to 9000 mA.
The sixth specific implementation mode: the difference between the first embodiment and the fifth embodiment is that in the third step, the electrifying time is 10-80000000 s, and the temperature of the liquid in the electrolytic cell is controlled to be 0-100 ℃ in the electrifying process.
The seventh embodiment: the difference between the first embodiment and the sixth embodiment is that the temperature of the liquid in the electrolytic cell is controlled to be 0-90 ℃ in the electrifying process in the third step.
The following experiments are adopted to verify the effect of the invention:
experiment one:
a method for regulating and controlling BiOCl surface phase oxygen vacancies with high catalytic activity is carried out according to the following steps:
firstly, putting BiOCl into the negative electrode side of an electrolytic cell containing water, wherein the electrolytic cell is separated by a diaphragm; the mass ratio of BiOCl to water is 1:100, wherein the aperture of a diaphragm of the electrolytic cell is 200nm, and the diaphragm can be made of PE;
secondly, adjusting the pH value of the electrolyte by acid (or alkali) under the stirring state, wherein the pH value range is 7;
thirdly, inserting the electrode into the electrolytic cell, controlling the temperature of liquid in the electrolytic cell to be 25 ℃ in the electrifying process, wherein the voltage range is 300V under the constant voltage mode, the electrifying time is 19800 s;
fourthly, after electrifying is finished, filtering the powder obtained in the third step, washing the powder for 3 times by using distilled water to be neutral, and drying the powder at 50 ℃ to obtain the BiOCl powder rich in high-concentration surface phase oxygen vacancies.
Experiment two:
a method for regulating and controlling BiOBr surface phase oxygen vacancy with high catalytic activity is carried out according to the following steps:
firstly, placing BiOBr into the negative side of an electrolytic cell containing water, wherein the electrolytic cell is separated by a diaphragm; the mass ratio of BiOBr to water is 1:500, wherein the aperture of the diaphragm of the electrolytic cell is 500nm, and the diaphragm can be made of PVDF;
secondly, adjusting the pH value of the electrolyte by acid (or alkali) under the stirring state, wherein the pH value range is 6;
thirdly, inserting the electrode into an electrolytic cell, controlling the voltage range to be 0.02A in a constant current mode, controlling the electrifying time to be 28800s, and controlling the temperature of liquid in the electrolytic cell to be 20 ℃ in the electrifying process;
fourthly, after electrifying, filtering the powder obtained in the third step, washing the powder for 5 times by using distilled water to be neutral, and drying the powder at 50 ℃ to obtain the BiOBr powder rich in high-concentration surface phase oxygen vacancies.
Claims (8)
1. A method for regulating and controlling epiphase oxygen vacancy of bismuth oxyhalide with high catalytic activity is characterized in that the method for regulating and controlling the epiphase oxygen vacancy by adopting electrochemistry assistance is carried out according to the following steps:
firstly, bismuth oxyhalide is put into the negative electrode side of an electrolytic cell containing water, and the electrolytic cell is separated by a diaphragm; the mass ratio of the bismuth oxyhalide to the water is 1: 1-10000, wherein the aperture of the electrolytic cell diaphragm is 3-1000000 nm, and the diaphragm can be made of PE, PVDF, glass fiber and the like;
secondly, adjusting the pH value of the electrolyte by acid (or alkali) in a stirring state, wherein the pH value range is 1-11;
inserting the electrode into an electrolytic cell, wherein the voltage range is 0.1-10000V under a constant voltage mode, the current range is 0.0001-10000 mA under a constant current mode, the electrifying time is 1-100000000 s, and the temperature of liquid in the electrolytic cell is controlled to be 0-100 ℃ in the electrifying process;
fourthly, after electrifying, filtering the powder obtained in the third step, washing the powder for 1 to 8 times by using distilled water to be neutral, and drying the powder at the temperature of between 30 and 150 ℃ to obtain the bismuth oxyhalide powder rich in the high-concentration epiphase oxygen vacancies.
2. The method for regulating and controlling epiphase oxygen vacancy of bismuth oxyhalide with high catalytic activity as claimed in claim 1, wherein in the step one, bismuth oxyhalide is put into the negative electrode side of an electrolytic cell containing water, and the electrolytic cell is separated by a diaphragm.
3. The method for regulating and controlling the epiphase oxygen vacancy of the bismuth oxyhalide with high catalytic activity according to claim 1, wherein the mass ratio of the bismuth oxyhalide to water in the step one is 1: 1-10000.
4. The method for regulating and controlling epiphase oxygen vacancies of bismuth oxyhalide with high catalytic activity as claimed in claim 1, wherein in the step one, the two electrodes of the electrolytic cell are separated by a diaphragm, the aperture of the diaphragm is 3-1000000 nm, and the diaphragm can be made of PE, PVDF, glass fiber and the like.
5. The method for regulating and controlling the epiphase oxygen vacancy of the bismuth oxyhalide with high catalytic activity according to claim 1, wherein in the second step, the pH value of the electrolyte is regulated by acid (or alkali), and the pH value ranges from 1 to 11.
6. The method for regulating and controlling the epiphase oxygen vacancy of the bismuth oxyhalide with high catalytic activity according to claim 1, wherein in the third step, the voltage range is 0.1-10000V in a constant voltage mode.
7. The method for regulating and controlling the epiphase oxygen vacancy of the bismuth oxyhalide with high catalytic activity according to claim 1, wherein in the third step, the current range in the constant current mode is 0.0001 to 10000 mA.
8. The method for regulating and controlling the epiphase oxygen vacancy of the bismuth oxyhalide with high catalytic activity according to claim 1, wherein in the third step, the electrifying time is 1-100000000 s, and the temperature of the liquid in the electrolytic cell is controlled to be 0-100 ℃ in the electrifying process.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20150361566A1 (en) * | 2014-06-16 | 2015-12-17 | Wisconsin Alumni Research Foundation | Synthesis of high-surface-area nanoporous bivo4 electrodes |
| CN112958116A (en) * | 2021-02-22 | 2021-06-15 | 西南大学 | Bi2O2.33-CdS composite photocatalyst and preparation process thereof |
| CN113136602A (en) * | 2021-04-19 | 2021-07-20 | 西北师范大学 | Preparation and application of bismuth vanadate/Vo-FeNiOOH composite photo-anode |
| CN113690453A (en) * | 2020-05-18 | 2021-11-23 | 中国科学院上海硅酸盐研究所 | Mn (manganese)5O8Nano cage-shaped oxygen reduction electrocatalyst and preparation method thereof |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20150361566A1 (en) * | 2014-06-16 | 2015-12-17 | Wisconsin Alumni Research Foundation | Synthesis of high-surface-area nanoporous bivo4 electrodes |
| CN113690453A (en) * | 2020-05-18 | 2021-11-23 | 中国科学院上海硅酸盐研究所 | Mn (manganese)5O8Nano cage-shaped oxygen reduction electrocatalyst and preparation method thereof |
| CN112958116A (en) * | 2021-02-22 | 2021-06-15 | 西南大学 | Bi2O2.33-CdS composite photocatalyst and preparation process thereof |
| CN113136602A (en) * | 2021-04-19 | 2021-07-20 | 西北师范大学 | Preparation and application of bismuth vanadate/Vo-FeNiOOH composite photo-anode |
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