CN109402656A - A kind of preparation method of phosphatization cobalt modification molybdenum doping pucherite optoelectronic pole - Google Patents

A kind of preparation method of phosphatization cobalt modification molybdenum doping pucherite optoelectronic pole Download PDF

Info

Publication number
CN109402656A
CN109402656A CN201811540907.1A CN201811540907A CN109402656A CN 109402656 A CN109402656 A CN 109402656A CN 201811540907 A CN201811540907 A CN 201811540907A CN 109402656 A CN109402656 A CN 109402656A
Authority
CN
China
Prior art keywords
optoelectronic pole
pucherite
preparation
molybdenum
cobalt
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN201811540907.1A
Other languages
Chinese (zh)
Other versions
CN109402656B (en
Inventor
刘长海
罗恒
陈智栋
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Changzhou University
Original Assignee
Changzhou University
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Changzhou University filed Critical Changzhou University
Priority to CN201811540907.1A priority Critical patent/CN109402656B/en
Publication of CN109402656A publication Critical patent/CN109402656A/en
Application granted granted Critical
Publication of CN109402656B publication Critical patent/CN109402656B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • 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
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
    • C03C17/36—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
    • C03C17/36—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal
    • C03C17/3602—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal the metal being present as a layer
    • C03C17/3618—Coatings of type glass/inorganic compound/other inorganic layers, at least one layer being metallic
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
    • C03C17/36—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal
    • C03C17/3602—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal the metal being present as a layer
    • C03C17/3639—Multilayers containing at least two functional metal layers
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
    • C03C17/36—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal
    • C03C17/3602—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal the metal being present as a layer
    • C03C17/3649—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal the metal being present as a layer made of metals other than silver
    • 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
    • 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
    • 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
    • C25B11/091—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of at least one catalytic element and at least one catalytic compound; consisting of two or more catalytic elements or catalytic compounds
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2218/00—Methods for coating glass
    • C03C2218/10—Deposition methods
    • C03C2218/11—Deposition methods from solutions or suspensions
    • C03C2218/115—Deposition methods from solutions or suspensions electro-enhanced deposition
    • 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
    • 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
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/10—Process efficiency
    • Y02P20/133—Renewable energy sources, e.g. sunlight

Landscapes

  • Chemical & Material Sciences (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Metallurgy (AREA)
  • Electrochemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Inorganic Chemistry (AREA)
  • Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)
  • Hybrid Cells (AREA)
  • Electrodes For Compound Or Non-Metal Manufacture (AREA)
  • Photovoltaic Devices (AREA)

Abstract

The invention discloses a kind of preparation methods of phosphatization cobalt modification molybdenum doping pucherite optoelectronic pole, bismuth oxyiodide optoelectronic pole is first produced using sedimentation in conductive glass surface, in dropwise addition vanadium source and molybdenum source solution on bismuth oxyiodide optoelectronic pole, it obtains mixing molybdenum pucherite optoelectronic pole after annealing cleaning, again in three-electrode system by light assist in electrodeposition phosphatization cobalt in mixing molybdenum pucherite photoelectricity pole surface, up to made novel pucherite optoelectronic pole, the invention also discloses the compound molybdenum pucherite optoelectronic poles to decompose the application in water in photoelectrocatalysis.Optoelectronic pole produced by the present invention is used for photoelectrocatalysis hydrogen production by water decomposition, the concentration of carrier can effectively be increased by mixing molybdenum, increase photoelectric current, and electro-deposition cobalt phosphorus can effectively delay the recombination losses in optoelectronic pole, increase the service life of photo-generated carrier, promote optoelectronic pole surface oxygen evolution reaction, to improve the solar energy hydrogen transfer efficiency of semiconductor photoelectrode.

Description

A kind of preparation method of phosphatization cobalt modification molybdenum doping pucherite optoelectronic pole
Technical field
The invention belongs to optoelectronic materials technologies, and in particular to the system of kind phosphatization cobalt modification molybdenum doping pucherite optoelectronic pole Preparation Method and its application in photoelectrocatalysis decomposition water.
Background technique
In order to realize the strategy of sustainable development, the weight that renewable energy industry has become countries in the world is developed and utilized Want strategic objective.Wherein for solar energy as a kind of clean renewable energy, reserves are tens of thousands of times of other renewable energy； Solar energy hardly discharges greenhouse gases in use simultaneously, facilitates alleviation petroleum and largely uses caused environmental pollution And the environmental problems such as greenhouse effects for being promoted of fuel combustion, this allows solar energy to occupy importantly in renewable energy industry Position.
Semiconductor light sulfate ferroelectric functional material due to have photoconduction and photovoltaic effect, photoelectricity improper remark Mars inherently by Semiconductor material is determined by the behavioral trait for generating photo-generated carrier after the light excitation of enough energy, therefore is solar energy Using providing possibility.Chemical energy is converted solar energy into using semiconductor light sulfate ferroelectric functional material, is endangered for solving the current energy Machine and environmental problem have important research significance and practical value.
The photoelectric functional material mainly studied at present includes non-oxidic material and oxide material, non-oxidic material system Standby at high cost and photoetch phenomenon is serious, and the few pay close attention at present.Oxide material is since electrode is usually more stable, preparation Method is simple, low in cost, pays close attention to by people, is concentrated mainly on titanium dioxide, zinc oxide, iron oxide, pucherite etc..Wherein Pucherite (BiVO4) have the characteristics that rich reserves and fine in neutral solution stability, and it has relative to standard hydrogen The valence-band edge of electrode 2.4V can be used to that water, while its narrow band gap with 2.4eV is catalytically decomposed well, can absorb visible Light 516nm sunlight below.The theoretical photocatalytic water efficiency of pucherite is 9.2%, is equivalent to density of photocurrent 7.5mA cm-2, but It is the actual photocatalytic water efficiency of pucherite far below its theoretical efficiency, the current density of intrinsic pucherite optoelectronic pole is only 0.42mA cm-2As long as this has following three aspects to cause: up to 60~80% electricity caused by 1. electronics transport difference and surface defect are high Lotus is compound；2. oxygen Precipitation Kinetics process is slow；3. conduction band side is slightly below reversible hydrogen potential.
In terms of solving the problems, such as three above, researcher on the one hand from improving photo-generated carrier separative efficiency, By pucherite in conjunction with other semiconductors, on the other hand by sputtering method, hydrothermal synthesis method or light assist in electrodeposition method etc. in vanadium Sour bismuth surface modification co-catalyst.Therefore, photoproduction carrier concentration and the compound upper co-catalyst of electro-deposition are promoted by adulterating It will be expected to improve the density of photocurrent of pucherite, while promoting its photochemical catalyzing efficiency.
Summary of the invention
In order to promote pucherite optoelectronic pole photochemical catalyzing efficiency, the object of the present invention is to provide kind of a phosphatization cobalts to repair The preparation method for adoring molybdenum doping pucherite optoelectronic pole, the photoelectric current of optoelectronic pole is improved by cobalt phosphorus catalyst and doping molybdenum.
The present invention also provides kind of the preparation method of phosphatization cobalt modification molybdenum doping pucherite optoelectronic pole and light auxiliary electricity are heavy Product cobalt phosphorus modification mixes molybdenum pucherite optoelectronic pole and decomposes the application in water in photoelectrocatalysis.
To achieve the goals above, the technical solution adopted by the present invention are as follows:
The preparation method of kind phosphatization cobalt modification molybdenum doping pucherite optoelectronic pole, comprising the following steps:
(1) using electro-conductive glass as substrate, electrodeposition process produces bismuth oxyiodide optoelectronic pole；
(2) dimethyl sulfoxide of upper acetyl acetone and vanadyl acetylacetonate is added dropwise on the bismuth oxyiodide electrode obtained by step (1) Solution then heats to 400~500 DEG C, and constant temperature is kept for 1.5~2.5 hours, is cooled to room temperature, after aqueous slkali soaking, clearly It washes, dry, obtain mixing molybdenum pucherite optoelectronic pole；
(3) to mix molybdenum pucherite photoelectricity extremely working electrode obtained by step (2), platinized platinum is to electrode, and Ag/AgCl electrode is reference Electrode constitutes three-electrode system, is electricity with the aqueous solution containing 4~6mmol/L cobalt nitrate, 0.075~0.15mol/L sodium phosphate Xie Zhi is aided with simulated solar irradiation irradiation, uses potentiostatic method using 0.35~0.45V as constant potential, sedimentation time takes 120~140s Between, take out working electrode after to be deposited, it is washed, dry to get.
Preferably, in the dimethyl sulphoxide solution of acetyl acetone described in step (2) acetyl acetone concentration be 2~ 3mmol/L, and in the dimethyl sulphoxide solution of the vanadyl acetylacetonate vanadyl acetylacetonate concentration be 0.15~ 0.25mol/L。
Preferably, heating described in step (2), which refers to, is directly added dropwise to iodine oxygen for 150~400 μ L dimethyl sulphoxide solutions It heats up in Muffle furnace after changing bismuth surface, heating rate control is 1.5~3 DEG C/min.
Preferably, simulated solar irradiation described in step (3) irradiates, and is a sunlight (1.5AM) using intensity.
Preferably, the sedimentation time used in step (3) need to by cobalt phosphorus sedimentation time for 120 ~ 140 s after stop.
Molybdenum pucherite (CoPi/Mo/BiVO is mixed in the cobalt phosphorus modification being prepared using the above method4) optoelectronic pole.
The present invention is by BiVO4FTO conductive glass surface is grown into, and is doped molybdenum element while growth, then CoPi is attached to the surface of semiconductor BiVO4, forms uniform co-catalysis layer.Mo/BiVO is modified using CoPi4Optoelectronic pole is used In photoelectrocatalysis hydrogen production by water decomposition, can effectively delay photo-generated carrier self is compound, increase the density of photo-generated carrier, from And promote the evolution reaction of photoelectricity pole surface.
Detailed description of the invention
Fig. 1 is resulting CoPi/Mo/BiVO4The stereoscan photograph of optoelectronic pole；
Fig. 2 is resulting CoPi/Mo/BiVO4The high definition transmission electron microscope photo of optoelectronic pole；
Fig. 3 is resulting CoPi/Mo/BiVO4Optoelectronic pole and the linear sweep voltammetry curve of comparison electrode under light illumination；
Fig. 4 is resulting CoPi/Mo/BiVO4The not special Schottky curve and fitting a straight line of optoelectronic pole and comparison electrode.
Specific embodiment
In order to keep technical purpose of the invention, technical scheme and beneficial effects clearer, combined with specific embodiments below Further description of the technical solution of the present invention, but the embodiment is intended to explain the present invention, and should not be understood as to this The limitation of invention, in the examples where no specific technique or condition is specified, described technology or item according to the literature in the art Part is carried out according to product description.
A kind of preparation method of phosphatization cobalt modification molybdenum doping pucherite optoelectronic pole, comprising the following steps:
(1) using FTO electro-conductive glass as working electrode, platinized platinum is to electrode, and Ag/AgCl electrode (saturation KCl solution) is reference electricity Pole constitutes three-electrode system, is mixed using the acid solution containing bismuth nitrate and potassium iodide with the ethanol solution of 1,4-benzoquinone as electrolysis Liquid, the potentiostatic electrodeposition 180s with -0.1V(vs. Ag/AgCl), working electrode is taken out, is washed with deionized, and dry, Obtain bismuth oxyiodide optoelectronic pole；
(2) dimethyl sulphoxide solution of 400 μ L vanadyl acetylacetonates containing 0.2M and 2.5mM acetyl acetone is taken to be added dropwise in step (1) the bismuth oxyiodide surface of gained bismuth oxyiodide electrode, so that the dimethyl sulfoxide of acetyl acetone and vanadyl acetylacetonate is molten Liquid is uniformly paved in bismuth oxyiodide material surface, then is placed in Muffle furnace and is heated, and is warming up to 450 DEG C with the rate of 2 DEG C/min, perseverance Temperature is kept for 2 hours, and cooled to room temperature has been loaded Mo/BiVO4The electrode of film；Mo/BiVO will have been loaded4Film Electrode is placed in the NaOH aqueous solution of 1mol/L, is stirred 30 minutes, except the Mo/BiVO that unloads4The electrode surface of film it is residual Remaining V2O5, then it is washed with deionized, and dry, obtains Mo/BiVO4Electrode.
(3) to mix molybdenum pucherite photoelectricity extremely working electrode obtained by step (2), platinized platinum is to electrode, and Ag/AgCl electrode is Reference electrode constitutes three-electrode system, auxiliary using the aqueous solution containing 5mmol/L cobalt nitrate, 0.1mol/L sodium phosphate as electrolyte It is irradiated with the simulated solar irradiation of 1.5AM light intensity, uses potentiostatic method using 0.4V as constant potential, deposited charge amount is 0.07C, to heavy Working electrode is taken out after product, it is washed, dry to get CoPi/Mo/BiVO4Optoelectronic pole.
Wherein, step (1) described electrolyte is that the ethyl alcohol of acidic aqueous solution and 1,4-benzoquinone containing bismuth nitrate and potassium iodide is molten Liquid is mixed according to volume ratio 5:2；Wherein, the concentration of bismuth nitrate is in the acidic aqueous solution containing bismuth nitrate and potassium iodide 0.04M, potassium iodide concentration be 0.4M, the mixed solution PH of bismuth nitrate and potassium iodide is adjusted to using the dust technology of 5wt% 1.7, the concentration of 1,4-benzoquinone is 0.23M in the ethanol solution of 1,4-benzoquinone.
Fig. 1 is CoPi/Mo/BiVO4Tissue amplifies 30000 times of stereoscan photograph on optoelectronic pole, hence it is evident that as it can be seen that made Made of CoPi/Mo/BiVO4Tissue is bar-like structure, and size is more uniform, rod-like phase diameter 100~200nm it Between.Fig. 2 is CoPi/Mo/BiVO4The microstructure of tissue, hence it is evident that the CoPi in visible deposition is equably divided with intensive born of the same parents' shape Cloth mixes the surface of molybdenum pucherite in substrate.
In order to help to understand BiVO4With CoPi/Mo/BiVO4PhotoelectrocatalytiPerformance Performance difference, Fig. 3 is BiVO4、Mo/ BiVO4、CoPi/BiVO4And CoPi/Mo/BiVO4Linear sweep voltammetry curve under illumination condition, You Tuzhong it is found that 1.23V vs.RHE(0.6V vs.Ag/AgCl) under voltage, CoPi/Mo/BiVO4Photoelectric current be up to 2.38mA cm-2, it is 2.975 times of BiVO4 photoelectric current.
Enter pucherite matrix to verify molybdenum element and successfully adulterate during doping, tests BiVO4、Mo/BiVO4、 CoPi/BiVO4And CoPi/Mo/BiVO4The not special Schottky curve of optoelectronic pole, as a result as shown in Figure 4.As shown in Figure 4, it is doped with The optoelectronic pole photo-generated carrier density of molybdenum element is obviously bigger than undoped, the slope of not special Schottky curve matching straight line It is smaller.Photo-generated carrier density increases, it is meant that, the evolution reaction of effect bigger with the density of photocurrent under degree illumination It is more strong.
Finally, it is stated that the parameter of preparation complex light electrode can adjust in respective range in the present invention, it will be apparent that Flow increasing body, semiconductor material and co-catalyst dosage can make corresponding replacement and be modified.Above embodiments are only to say Bright technical solution of the present invention rather than limit, although having been retouched to the present invention by referring to the preferred embodiment of the present invention It states, it should be appreciated by those of ordinary skill in the art that various changes can be made to it in the form and details, The spirit and scope of the present invention limited without departing from the appended claims.

Claims (8)

1. a kind of preparation method of phosphatization cobalt modification molybdenum doping pucherite optoelectronic pole, which comprises the following steps:
Using electro-conductive glass as substrate, bismuth oxyiodide optoelectronic pole is produced by electrodeposition process；
The dimethyl sulfoxide that upper acetyl acetone and vanadyl acetylacetonate are added dropwise on the bismuth oxyiodide electrode obtained by step (1) is molten Liquid then heats to 450 DEG C, and constant temperature is kept for 1.5~2.5 hours, is cooled to room temperature, after aqueous slkali soaking, cleaning, drying, It obtains mixing molybdenum pucherite optoelectronic pole；
To mix molybdenum pucherite photoelectricity extremely working electrode obtained by step (2), platinized platinum is to electrode, and Ag/AgCl electrode is reference electricity Pole constitutes three-electrode system, to be electricity containing 4~6mmol/L Cobalt salts, the phosphatic aqueous solution of 0.075~0.15mol/L Xie Zhi is deposited, sedimentation time takes between 120~140s, after to be deposited under simulated solar irradiation irradiation using potentiostatic method Working electrode is taken out, modifies molybdenum doping pucherite optoelectronic pole through deionized water washing, drying to get phosphatization cobalt.
2. the preparation method of phosphatization cobalt modification molybdenum doping pucherite optoelectronic pole according to claim 1, it is characterised in that: step Suddenly the concentration of acetyl acetone is 2~3mmol/L in the dimethyl sulphoxide solution of acetyl acetone described in (2), and described The concentration of vanadyl acetylacetonate is 0.15~0.25mol/L in the dimethyl sulphoxide solution of vanadyl acetylacetonate.
3. the preparation method of phosphatization cobalt modification molybdenum doping pucherite optoelectronic pole according to claim 1, it is characterised in that: step Suddenly high-temperature process condition described in (2) is to keep the temperature 1.5 ~ 2.5 hours 450 DEG C in air atmosphere.
4. the preparation method of phosphatization cobalt modification molybdenum doping pucherite optoelectronic pole according to claim 1, it is characterised in that: step Suddenly the control of heating rate described in (2) is 1.5~3 DEG C/min.
5. the preparation method of phosphatization cobalt modification molybdenum doping pucherite optoelectronic pole according to claim 1, it is characterised in that: step Suddenly aqueous slkali described in (2) is one kind of sodium hydroxide or potassium hydroxide solution.
6. the preparation method of phosphatization cobalt modification molybdenum doping pucherite optoelectronic pole according to claim 1, it is characterised in that: step Suddenly Cobalt salts described in (3) are one of cobalt nitrate, cobaltous sulfate, cobalt chloride, and concentration is 4~6mmol/L.
7. the preparation method of phosphatization cobalt modification molybdenum doping pucherite optoelectronic pole according to claim 1, it is characterised in that: step Suddenly phosphate described in (3) is 0.075~0.15mol/L of one of sodium phosphate or potassium phosphate, and concentration is 4~6mmol/L.
8. the preparation method of phosphatization cobalt modification molybdenum doping pucherite optoelectronic pole according to claim 1, it is characterised in that: step Suddenly any current potential of the constant potential described in (3) between the V of 0.35 V ~ 0.45, sedimentation time are 120 ~ 140 s.
CN201811540907.1A 2018-12-17 2018-12-17 Preparation method of cobalt phosphide modified molybdenum-doped bismuth vanadate photoelectrode Active CN109402656B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201811540907.1A CN109402656B (en) 2018-12-17 2018-12-17 Preparation method of cobalt phosphide modified molybdenum-doped bismuth vanadate photoelectrode

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201811540907.1A CN109402656B (en) 2018-12-17 2018-12-17 Preparation method of cobalt phosphide modified molybdenum-doped bismuth vanadate photoelectrode

Publications (2)

Publication Number Publication Date
CN109402656A true CN109402656A (en) 2019-03-01
CN109402656B CN109402656B (en) 2021-01-29

Family

ID=65460423

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201811540907.1A Active CN109402656B (en) 2018-12-17 2018-12-17 Preparation method of cobalt phosphide modified molybdenum-doped bismuth vanadate photoelectrode

Country Status (1)

Country Link
CN (1) CN109402656B (en)

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109865525A (en) * 2019-03-05 2019-06-11 西北师范大学 A kind of preparation method of CoPi/Ag/ pucherite composite photoelectric anode material
CN110042407A (en) * 2019-03-15 2019-07-23 江苏大学 Cobalt phosphate-poly-dopamine-pucherite tri compound optoelectronic pole preparation method and application
CN110586130A (en) * 2019-10-12 2019-12-20 南京大学 Z-system visible light catalytic material based on crystal face energy level difference and hole trap synergistic effect and preparation method thereof
CN111302650A (en) * 2020-03-17 2020-06-19 吉林大学 Method for preparing bismuth vanadate photoelectric anode by spin coating of nanoparticle solution
CN111705333A (en) * 2020-05-19 2020-09-25 江苏大学 Ag-Pi/BiVO4Heterogeneous combination method and application thereof in photoelectrolysis water
CN114164448A (en) * 2021-10-31 2022-03-11 吉林大学 Heterogeneous nickel phosphide material and preparation method thereof
CN114250472A (en) * 2021-04-08 2022-03-29 台州学院 BiVO4CoP thin film electrode and preparation method and application thereof
CN114411168A (en) * 2022-01-24 2022-04-29 中国矿业大学 Cobalt-lanthanum co-doped visible light response BiVO4Photoelectrode and preparation method thereof
CN116854470A (en) * 2023-05-31 2023-10-10 四川省新材料研究中心 Doped modified bismuth vanadate material used as direct X-ray array imaging device and preparation method thereof

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112266045A (en) * 2020-09-21 2021-01-26 华南理工大学 Photoanode for retarding corrosion in photoelectrocatalysis wastewater treatment process by utilizing amorphous cobalt phosphate Co-Pi and preparation method and application thereof

Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109865525A (en) * 2019-03-05 2019-06-11 西北师范大学 A kind of preparation method of CoPi/Ag/ pucherite composite photoelectric anode material
CN110042407A (en) * 2019-03-15 2019-07-23 江苏大学 Cobalt phosphate-poly-dopamine-pucherite tri compound optoelectronic pole preparation method and application
CN110586130A (en) * 2019-10-12 2019-12-20 南京大学 Z-system visible light catalytic material based on crystal face energy level difference and hole trap synergistic effect and preparation method thereof
CN111302650A (en) * 2020-03-17 2020-06-19 吉林大学 Method for preparing bismuth vanadate photoelectric anode by spin coating of nanoparticle solution
CN111705333A (en) * 2020-05-19 2020-09-25 江苏大学 Ag-Pi/BiVO4Heterogeneous combination method and application thereof in photoelectrolysis water
CN114250472A (en) * 2021-04-08 2022-03-29 台州学院 BiVO4CoP thin film electrode and preparation method and application thereof
CN114164448A (en) * 2021-10-31 2022-03-11 吉林大学 Heterogeneous nickel phosphide material and preparation method thereof
CN114164448B (en) * 2021-10-31 2022-12-16 吉林大学 Heterogeneous nickel phosphide material and preparation method thereof
CN114411168A (en) * 2022-01-24 2022-04-29 中国矿业大学 Cobalt-lanthanum co-doped visible light response BiVO4Photoelectrode and preparation method thereof
CN114411168B (en) * 2022-01-24 2024-02-09 中国矿业大学 Cobalt-lanthanum co-doped visible light response BiVO 4 Photoelectrode and method for producing the same
CN116854470A (en) * 2023-05-31 2023-10-10 四川省新材料研究中心 Doped modified bismuth vanadate material used as direct X-ray array imaging device and preparation method thereof

Also Published As

Publication number Publication date
CN109402656B (en) 2021-01-29

Similar Documents

Publication Publication Date Title
CN109402656A (en) A kind of preparation method of phosphatization cobalt modification molybdenum doping pucherite optoelectronic pole
Khoomortezaei et al. Triple layer heterojunction WO3/BiVO4/BiFeO3 porous photoanode for efficient photoelectrochemical water splitting
Li et al. Photoelectrochemical splitting of natural seawater with α-Fe2O3/WO3 nanorod arrays
Tong et al. Cobalt-Phosphate modified TiO2/BiVO4 nanoarrays photoanode for efficient water splitting
Chen et al. Nano-architecture and material designs for water splitting photoelectrodes
CN106498372B (en) Light deposition prepares Bi/BiVO4The method of composite photoelectric anode material
Rodríguez-Gutiérrez et al. Photoelectrochemical water oxidation at FTO| WO3@ CuWO4 and FTO| WO3@ CuWO4| BiVO4 heterojunction systems: an IMPS analysis
Bashiri et al. Photoelectrochemical water splitting with tailored TiO2/SrTiO3@ g-C3N4 heterostructure nanorod in photoelectrochemical cell
CN108103525B (en) N doping carbon dots modify tungstic acid complex light electrode and preparation method thereof and decompose the application in water in photoelectrocatalysis
CN105803476B (en) The light anode of bismuth ferrite modification pucherite and preparation method and its application in photolysis water hydrogen
Li et al. Enhancement of photoelectrochemical response by Au modified in TiO2 nanorods
CN110047657A (en) A kind of compound preparation method for mixing molybdenum pucherite light anode of MIL series MOF
Yang et al. Enhanced photoelectrochemical water oxidation on WO3 nanoflake films by coupling with amorphous TiO2
CN108906080B (en) CdS/Cu2S/Co-based photoelectric catalytic material and preparation method thereof
Huang et al. TiO2-rutile/anatase homojunction with enhanced charge separation for photoelectrochemical water splitting
CN108193219B (en) Phosphorized copper modified titanic oxide optoelectronic pole and preparation method thereof and the application in photoelectrocatalysis decomposition water
Liu et al. Branched multiphase TiO2 with enhanced photoelectrochemical water splitting activity
Lv et al. Enhanced photoelectrochemical charge transfer on Mn-doped CdS/TiO2 nanotube arrays: The roles of organic substrates
Guo et al. Effective photocathodic protection for 304 stainless steel by PbS quantum dots modified TiO2 nanotubes
Wang et al. Construction of electron transport channels in type-I heterostructures of Bi2MoO6/BiVO4/g-C3N4 for improved charge carriers separation efficiency
CN107761127A (en) A kind of preparation method for the nanoporous pucherite analysis oxygen electrode that polyacid and phthalocyanine are modified jointly
CN108511198B (en) Ni-doped BiVO4Thin-film photoelectric anode, preparation method and application thereof
Burungale et al. Surface modification of p/n heterojunction based TiO2-Cu2O photoanode with a cobalt-phosphate (CoPi) co-catalyst for effective oxygen evolution reaction
Yin et al. Cascaded multiple-step hole transfer for enhancing photoelectrochemical water splitting
Ma et al. Interface modulation of BiVO4 based photoanode with Bi (III) Bi (V) O4 for enhanced solar water splitting

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant