CN109280937B - Preparation of ZIF-67/bismuth vanadate composite material and application of composite material as photoelectric anode material - Google Patents

Preparation of ZIF-67/bismuth vanadate composite material and application of composite material as photoelectric anode material Download PDF

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CN109280937B
CN109280937B CN201811425263.1A CN201811425263A CN109280937B CN 109280937 B CN109280937 B CN 109280937B CN 201811425263 A CN201811425263 A CN 201811425263A CN 109280937 B CN109280937 B CN 109280937B
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bivo
zif
composite material
distilled water
bismuth vanadate
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CN109280937A (en
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王其召
周诗仟
佘厚德
王磊
黄静伟
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Northwest Normal University
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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
    • C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
    • C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
    • C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
    • 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
    • C25B1/02—Hydrogen or oxygen
    • C25B1/04—Hydrogen or oxygen by electrolysis of water
    • 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
    • C25B1/50—Processes
    • C25B1/55—Photoelectrolysis
    • 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
    • C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
    • C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
    • C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
    • C25B11/055—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the substrate or carrier material
    • C25B11/057—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the substrate or carrier material consisting of a single element or compound
    • 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
    • C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
    • C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
    • C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
    • C25B11/073—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material
    • C25B11/075—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of a single catalytic element or catalytic compound
    • 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

The invention discloses a preparation method of a ZIF-67/bismuth vanadate composite material, which is prepared by mixing 2-methylimidazole and Co (NO)3)2·6H2Dissolving O in N, N-dimethylformamide-distilled water, and adding BiVO4Soaking the film in the solution for a period of time; then completely washing with distilled water and ethanol, and drying to obtain the final product. The invention successfully loads ZIF-67 to BiVO by an in-situ deposition method4Surface to form stable ZIF-67/BiVO4A film material. Under high bias, ZIF-67/BiVO4Composite material pureness/BiVO4Higher photocurrent; meanwhile, the introduction of ZIF-67 well prolongs the service life of a current carrier and improves BiVO4The photocatalytic performance of (a). Through photocurrent corresponding test and photoelectric injection efficiency calculation, the composite photoelectrode is proved to have excellent photoelectric catalytic performance, and can effectively improve the hydrogen production efficiency when being used as a photoanode material.

Description

Preparation of ZIF-67/bismuth vanadate composite material and application of composite material as photoelectric anode material
Technical Field
The invention relates to preparation of a bismuth vanadate composite electrode film, in particular to ZIF-67/BiVO4The preparation method of the photoelectrocatalysis composite material is mainly used as a photoelectrochemistry anode material in the reaction of hydrogen production by water decomposition.
Background
At present, the use of fossil fuels in large quantities causes problems such as global climate change and environmental deterioration. All of these issues have been the primary driving force to accelerate the use of renewable energy sources to clean energy sources. The use of solar energy, the largest renewable energy source, has thus received widespread attention, and among the various solar energy conversion options widely available, the solar energy decomposition of water and the production of hydrogen using the photo-electrolytic reaction is one of the most promising technologies. So far, many semiconductor materials have been studied as photoanodes, and particularly binary metal oxides are widely applied to the field of hydrogen production by photoelectricity. However, due to unstable chemical properties of these materials, electron-hole pairs are easy to recombine, the visible light absorption capability is weak, and the migration speed of the electron-hole pairs is slow, which limits their applications in the field of photoelectrochemistry. Even though their performance is improved by various modifications, the incident photon conversion efficiency is still low.
In the aspect of photoelectrochemical water decomposition and hydrogen production, a plurality of semiconductor materials have excellent performance as photoanode materials, such as TiO2、Cds、Fe2O3And WO3And is therefore of great interest. Among the many popular materials, BiVO4The crystal structure shows unique performance, is a narrow energy gap (Eg = 2.4-2.5 eV) n-type semiconductor, and has excellent visible light absorption capacity, adjustable electronic structure, good stability and low-cost preparation. However, their PEC capacity is relatively poor, as chemical stability is unstable, rapid recombination of photogenerated carriers and weak visible light absorption limit their further exploitation.
BiVO has been solved by a great deal of research in recent years4Electron-hole pair recombination and low solar energy conversion efficiency. Overall, BiVO4Has been improved to some extent by various methods. The general method comprises the following steps: ion doping, morphology control, and WO3、ZnFeO4Graphene oxide and BiOI form a heterojunction, and an oxygen generation promoter Co is loaded3O4NiO, FeOOH, NiOOH; or depositing noble metal nano particles Ag, Au and the like on the surface.
Metal Organic Frameworks (MOFs) are an emerging class of porous materials with potential applications in gas storage, separation, catalysis and chemical sensing due to their abundant structure and diverse functionality. Despite many advantages, the applications of many MOFs are ultimately limited by their stability under harsh conditions. Therefore, the invention combines bismuth vanadate and MOFs to prepare the MOFs/bismuth vanadate photoelectrocatalysis composite material which is BiVO4The improvement of photoelectrochemical properties of (a) suggests a new strategy.
Disclosure of Invention
The invention aims to provide a preparation method of a ZIF-67/bismuth vanadate photoelectrocatalysis composite material;
the invention also aims to research the photoelectrochemical properties of the ZIF-67/bismuth vanadate photoelectrocatalysis composite material.
ZIF-67/BiVO4Preparation of a photoanode
2-methylimidazole and Co (NO)3) 2·6H2Dissolving O in the mixed solution of N, N-dimethylformamide and distilled water in a mass ratio of 1: 0.1-1: 0.2, and stirring for 20-30 minutes; BiVO (bismuth oxide) is added4Placing the membrane in the mixed solution, and soaking for 1-2 hours at 50-70 ℃; completely washing the mixture by using distilled water and ethanol in sequence, and drying the washed mixture in vacuum at the temperature of 50-80 ℃ to obtain the MOFs/BiVO4A photo-anode material.
In the mixed solution of N, N-dimethylformamide and distilled water, the volume ratio of the N, N-dimethylformamide to the distilled water is 3: 1-5: 1.
II, ZIF-67/BiVO4Structure of photoelectric anode
FIG. 1 is an electron microscope scan of a photoelectrode. Wherein a and b are porous BiVO under different magnification4A film. c is ZIF-67/BiVO4And (3) a composite electrode. As can be clearly seen from FIG. 1, in pure BiVO4The film was loaded with uniform amorphous ZIF-67. The successful loading of ZIF-67 on BiVO4 film was demonstrated.
FIG. 2 is BiVO4And ZIF-67/BiVO4XRD pattern of the film. BiVO4Shows monoclinic crystal and no other impurity peaks and diffraction peaks of other crystal phases appear, showing BiVO of monoclinic crystal phase4Has been successfully prepared. The other diffraction peak is a tetragonal SnO2 diffraction peak on FTO (JCPDS. number 41-1445) substrate. The reason why the diffraction peak of ZIF-67 appears at 27.14 ℃ after the photoreaction is that the ZIF-67 is loaded on BiVO4The amount on the film is small.
FIG. 3 is BiVO4And ZIF-67/BiVO4Ultraviolet-visible diffuse reflectance pattern of the composite electrode. BiVO as shown in the figure4The absorption edge of (A) is approximately 500nm, which is consistent with the reported literature, and indicates BiVO4The response is to visible light. When the ZIF-67 nano-particles are loaded, BiVO4The absorption intensity of light is enhanced, and the absorption edge also generates a slight red shift phenomenon,the forbidden bandwidth will also decrease accordingly. Make ZIF-67/BiVO4The electrode can absorb more visible light and thus make the light performance better.
FIG. 4 shows BiVO4 and ZIF-67/BiVO4Is scanned linearly. BiVO4And ZIF-67/BiVO4The photoelectrocatalytic water oxidation performance of the electrode is in a simulated light source of AM 1.5G, 0.5M Na with pH of 6.862SO4The test was performed in solution. BiVO in the absence of illumination4The film has little current. While the ZIF-67/BiVO loaded with ZIF-67 nanoparticles is in the whole voltage range tested4The current of the electrode is higher than BiVO4The current of the electrodes. ZIF-67/BiVO at standard potential of water oxidation of 1.23V vs. RHE4The photocurrent of the electrode was 3.16mA/cm2Is BiVO4(1.33 v) semiconductor as anode produced a value of 2.4 times the theoretical photocurrent. And the loading material is 100 mW/cm2Almost 12 times (0.80 mA/cm) of the original current under an AM 1.5G light source2). Simultaneously, with BiVO4Electrode comparison, ZIF-67/BiVO4The initial potential for water oxidation at the electrode was changed from 0.61V to 0.38V, indicating that ZIF-67 is an excellent promoter for water oxidation.
FIG. 5 is BiVO4And ZIF-67/BiVO4Time-current plots at 0.6V and 1.0V. As can be seen from FIG. 5, under any bias, ZIF-67/BiVO4The photocurrent density of the electrode is higher than that of pure BiVO4And an electrode. This is mainly because the photogenerated holes are concentrated in BiVO4A large number of electron-hole pair recombinations occur at the surface of the film. When the ZIF-67 nano-particles are loaded on BiVO4After the surface, the accumulation condition can be effectively reduced, so that the recombination of current carriers in the water oxidation process is enhanced, the service life of the current carriers is prolonged, and the efficiency of light quanta is improved. Finally, the photoelectrocatalysis performance is enhanced. Further proves that ZIF-67/BiVO4The composite electrode is an excellent photo-anode material.
FIG. 6 is BiVO at an excitation wavelength of 350nm4And ZIF-67/BiVO4Photoluminescence of photoanodes. As can be seen from FIG. 6, ZIF-67/BiVO4Fluorescence intensity ratio ofBiVO (b)4The film is weak. Indicating ZIF-67/BiVO4The photogenerated electron-hole pairs are easier to separate, and therefore have higher photon efficiency.
FIG. 7 is BiVO4 and ZIF-67/BiVO4Charge injection efficiency of the photo-anode. The charge injection efficiency of the electrode is an important parameter for evaluating the proportion of holes participating in the reaction. In this system, the charge injection efficiency can be determined by dividing the current for electrode-catalyzed oxidation by the electrode-catalyzed Na2SO3An oxidizing current. As shown in FIG. 7, ZIF-67/BiVO4The electrode has the highest charge injection efficiency, which indicates that the hole reaction activity reaching the surface of the electrode after loading the ZIF-67 is higher. ZIF-67/BiVO4The charge injection efficiency of the electrode reaches 65%.
In conclusion, the ZIF-67 is successfully loaded to BiVO by the in-situ deposition method4Surface to form stable ZIF-67/BiVO4A film material. At high bias voltage (> 0.6 V vs. Ag/AgCl），ZIF-67/BiVO4Composite material pureness/BiVO4There is a higher photocurrent. Meanwhile, the introduction of ZIF-67 well prolongs the service life of a current carrier and improves BiVO4The photocatalytic performance of (a). The composite photoelectrode is proved to have excellent photoelectrocatalysis performance through corresponding test of photocurrent and calculation of photoelectricity injection efficiency. ZIF-67/BiVO4The composite material is directly used for a photo-anode material, can effectively capture light, reduce charge transfer resistance and accelerate the rapid migration of current carriers, thereby inhibiting the recombination of electron hole pairs and effectively improving the hydrogen production efficiency.
Drawings
FIG. 1 shows (a-b) BiVO4And (c) ZIF-67/BiVO4Electron microscope scan of photoelectrode.
FIG. 2 is an XRD pattern of the BiVO4 and ZIF-67/BiVO4 photoelectrode.
FIG. 3 is a UV-visible diffuse reflectance plot of BiVO4 and ZIF-67/BiVO4.
FIG. 4 is BiVO4 and ZIF-67/BiVO4.
FIG. 5 is a plot of i-t cycles A) 0.6V and (B) 1.0V vsAg/AgCl (0.35M KCl) at different biases.
FIG. 6 is a photoluminescence map of BiVO4 and ZIF-67/BiVO4.
FIG. 7 is a plot of the charge injection efficiency of BiVO4 and ZIF-67/BiVO4.
Detailed Description
The preparation of the ZIF-67/BiVO4 composite material and the application thereof as a photoelectrode in water decomposition hydrogen production are further explained by the following specific examples.
(1) Preparation of BiVO 4: is prepared according to the Kim and Choi project group electrodeposition combined heat treatment method. The method comprises the following specific steps: firstly, preparing the BiOI nano-sheet by an electrodeposition method through a CHI 660D electrochemical workstation. FTO glass ultrasonically cleaned by acetone/isopropanol/distilled water (volume ratio: 1:1: 1) is used as a working electrode, an Ag/AgCl (3.5M KCl) electrode is used as a reference electrode, and a Pt electrode is used as a counter electrode. With 6M HNO3Adjusting the pH value of 50 mL0.4M KI solution to 1.5-1.7, and then adding 0.970 g Bi (NO)3)3•5H2O until dissolved, the solution turned orange-red in color. Then 20ml of 0.498 g 1, 4-benzoquinone ethanol solution is slowly added dropwise and stirred for several minutes, and the solution turns into a blood red color again. Electrodeposition was scanned using cyclic voltammetry, voltage: -0.13-0V, sweep rate: 5 mV/s. The obtained BiOI film was washed with distilled water. Subsequently, 0.1 mL of a 0.2M vanadyl acetylacetonate-dimethyl sulfoxide solution was dropped onto the prepared BiOI film using a micro-syringe and calcined in a muffle furnace at a rate of 2 ℃/min up to 450 ℃ for 2 hours. Redundant V2O5And bismuth oxide, etc. were removed by soaking in 1M NaOH, leaving a pure yellow bismuth vanadate film. BiVO finally obtained4The electrode was washed with distilled water and dried naturally.
（2）ZIF-67/BiVO4The preparation of (1): taking 2-methylimidazole (0.1 g) and Co (NO)3) 2·6H2O (0.0125 g), dissolved in 16mL of N, N-dimethylformamide and distilled water (DMF: H)2Stirring for 30 minutes in a mixed solution of O-3: 1 and V) to obtain a solution; BiVO prepared by the method4Soaking in the mixed solution at 70 deg.C for 2 hr; completely washing with distilled water and ethanol, and vacuum drying at 60 deg.C for 3 hr to obtain ZIF-67/BiVO4A composite material.
（3）ZIF-67/BiVO4The composite material is directly used as a photoelectric anode and applied to the photoelectrochemistry water decomposition hydrogen production reaction, and the hydrogen production efficiency is 92.6%.

Claims (4)

1. A ZIF-67/bismuth vanadate composite material is prepared by mixing 2-methylimidazole and Co (NO)3) 2·6H2Dissolving O in the mixed solution of N, N-dimethylformamide and distilled water, and stirring for 20-30 minutes; then BiVO is added4Placing the electrode film in the mixed solution, and soaking for 1-2 hours at 50-70 ℃; completely washing with distilled water and ethanol in sequence, and drying to obtain MOFs/BiVO4A composite material; 2-methylimidazole with Co (NO)3) 2·6H2The mass ratio of O is 1: 0.1-1: 0.2.
2. The method of claim 1, wherein the ZIF-67/bismuth vanadate composite material is prepared by: in the mixed solution of N, N-dimethylformamide and distilled water, the volume ratio of the N, N-dimethylformamide to the distilled water is 3: 1-5: 1.
3. The method of claim 1, wherein the ZIF-67/bismuth vanadate composite material is prepared by: the drying is vacuum drying at 50-80 ℃.
4. The use of the ZIF-67/bismuth vanadate composite material prepared by the method of claim 1 as a photoanode material.
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CN109876867A (en) * 2019-03-05 2019-06-14 西北师范大学 A kind of preparation method of bimetallic-organic backbone/pucherite composite photoelectric anode material
CN110047657A (en) * 2019-04-02 2019-07-23 常州大学 A kind of compound preparation method for mixing molybdenum pucherite light anode of MIL series MOF
CN110180529B (en) * 2019-05-23 2020-10-13 北京科技大学 Preparation method for synthesizing photocatalytic material by using MOF as precursor
CN110408951B (en) * 2019-07-15 2021-05-25 江苏大学 Cu-MOF/BiVO4Preparation method and application of composite photoelectrode
CN110983362B (en) * 2019-12-19 2021-05-28 湖南大学 MOFs-coated OV-BiVO4Composite photo-anode and preparation method and application thereof
CN113130776B (en) * 2019-12-30 2022-05-24 Tcl科技集团股份有限公司 Quantum dot light-emitting diode and preparation method thereof
CN112210787B (en) * 2020-09-28 2022-01-14 西南石油大学 Preparation method of metal organic framework material coating on surface of nano-structure substrate
CN113818043B (en) * 2021-10-18 2022-08-30 台州学院 Bismuth vanadate-metal organic complex composite photoelectrode and preparation method and application thereof

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US20170175276A1 (en) * 2015-12-18 2017-06-22 Board Of Regents, The University Of Texas System Nanostructured electrodes and methods of making and use thereof
CN106498372B (en) * 2016-11-01 2019-01-22 西北师范大学 Light deposition prepares Bi/BiVO4The method of composite photoelectric anode material
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