CN106544693A - A kind of preparation of multilevel hierarchy ZnO@CoS membrane electrodes and its application in photoelectric decomposition water - Google Patents
A kind of preparation of multilevel hierarchy ZnO@CoS membrane electrodes and its application in photoelectric decomposition water Download PDFInfo
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Abstract
A kind of preparation of multilevel hierarchy ZnO@CoS membrane electrodes and its application in photoelectric decomposition water, belong to the technical field of energy conversion.The first step is applied by simple crystal seed and hydro-thermal reaction homoepitaxial ZnO nano-rod array in electro-conductive glass (FTO) substrate, second step is finally obtained ZnO@Co MOF composites in ZnO nanorod surface in situ growth metal-organic framework materials (Co MOF).ZnO@Co MOF vulcanizing treatments are obtained 3rd step the composite of multilevel hierarchy.ZnO@CoS have wider optical response signal, photoelectric catalytically active and chemical stability as optoelectronic pole, can be applicable to the storage of the new forms of energy such as photoelectric decomposition water and conversion equipment.
Description
Technical field
The invention belongs to the technical field of energy storage electrode material, technology is related to metal oxide, metal-organic framework materials
(MOFs) multilevel structure material constructed, is based particularly on ZnO nano-rod array, and further growth in situ Co-MOF simultaneously carries out sulphur
Change processes the derivative combination electrodes of the ZnO@CoS for obtaining.
Background technology
21 century, traditional non-renewable energy resources (coal, oil, natural gas) consume to be increasingly sharpened, and people are for novel environment friendly
The exploitation of sustainable energy is paid close attention to further.Wherein, to cause people as a kind of important clean energy resource increasing for solar energy
Research, at present with metal oxide semiconductor (TiO2, ZnO etc.) and sulfide (ZnS, CdS) be used for as optoelectronic pole material
Photoelectrocatalytioxidation oxidation system, and then effectively realize solar energy to electrical or chemical transformation of energy.This has valency mainly due to them
Lattice are excellent honest and clean, and synthetic method is simple and the advantages of environment-protecting asepsis.But such material its wider band structure is only to ultraviolet light
With response (ultraviolet light only accounts for the 5% of sunshine), visible ray is not almost absorbed, and then strongly limit its photoelectrocatalysis
Activity and transformation efficiency.Therefore, how to explore and develop visible absorption is high, catalysis activity is high and have good stability it is new
Photoelectric becomes the focus of people's research.
Metal-organic framework materials (MOFs) are constructed by coordination by metal ion or ion cluster and organic ligand
Reticulated porous structures.MOFs its own high-specific surface area and porosity, adjustable aperture and hole surface function, its absorption
The fields such as separation, catalysis, energy storage all have potential using value.In recent years, MOFs materials are gradually applied to electrification
Learn energy storage storage and conversion art, such as lithium ion battery, fuel cell and ultracapacitor etc..The portion that forefathers report simultaneously
Point MOFs can be effectively used for photoelectrocatalysis as optoelectronic pole material and decompose aqueous systems, but due to MOFs self-conductives it is poor with
And water stability is poor, avtive spot is caused to be lost in and catalysis activity decline.Therefore constructing MOFs derivatives improves its electric conductivity
Density of photocurrent and electricity conversion can be effectively improved with the problem of stability.
The content of the invention
Object of the present invention is to provide one kind grows the ZnO@with multilevel hierarchy in electro-conductive glass (FTO) substrate
CoS optoelectronic pole preparation methods.
A kind of multilevel hierarchy ZnO@Co-MOF composites, it is characterised in that multilevel hierarchy ZnO@Co-MOF composites
For core shell structure, wherein, central core layer is polygon nano-pillar ZnO, and outermost shell is born as Co-MOF skeletons；Outside core shell structure
Surface is axially stacked flower-like structure；Array structure of the multilevel hierarchy ZnO@Co-MOF composites for high-sequential.
ZnO@CoS composites, it is characterised in that multilevel hierarchy ZnO@Co-MOF composites are obtained by vulcanizing treatment
Multilevel hierarchy ZnO@CoS composites, the surface of multilevel hierarchy ZnO@CoS is that uniform honeycomb flower-like structure, i.e. outer layer are sky
Array structure of the CoS of heart polyhedral structure, the multilevel hierarchy ZnO@CoS composite for high-sequential.
The synthetic method of ZnO@CoS composites of the present invention, is broadly divided into three steps：The first step is passed through in FTO substrates
Hydro-thermal reaction grows uniform ZnO nanorod；Second step is in ZnO nanorod superficial growth Co-MOF systems by situ synthesis
Standby ZnO@Co-MOF；3rd step is that the ZnO@Co-MOF vulcanizing treatments that previous step synthesizes have been constructed the ZnO@CoS of multilevel hierarchy
Optoelectronic pole.
The synthetic method of the above-mentioned ZnO@CoS composites of the present invention, comprises the following steps：
The first step is pre-processed to FTO ultrasounds respectively with acetone, ethanol and water successively, raw in FTO substrates by hydro-thermal method
Long ZnO nanorod；
It is preferred that concrete grammar：Zinc acetate is dissolved in the zinc acetate ethanol solution that absolute ethyl alcohol prepares 5-10mM for which；By acetic acid
Zinc ethanol solution is spun on the FTO of pretreatment and obtains one layer of crystal seeding film, and then anneal at 300-400 DEG C obtains for 30 minutes
The FTO of growth ZnO crystal seeds；By the FTO obliques of growth ZnO crystal seeds in the polytetrafluoroethylene reaction kettle for reaction equipped with solution A, its
Middle solution A is the aqueous solution of the zinc nitrate and urotropine of same molar ratio, wherein nitric acid zinc concentration 30-60mM,
Reaction temperature 80-95 DEG C, reaction time 5-24 hour are subsequently cooled to room temperature, and obtained ZnO nanorod deionized water is rinsed
It is dried in atmosphere afterwards；
ZnO nanorod immersion mother liquor B is carried out hydro-thermal reaction by second step, and mother liquor B is 2-methylimidazole and six nitric hydrates
Cobalt is dissolved in water and gained in DMF mixed solvent, and wherein water and the volume ratio of DMF are 1:
1-1:5, preferably 1:5, and hydrothermal temperature is kept for 60-80 DEG C in moving into reactor, preferably 70 DEG C, time 0.5-3 hour is excellent
Select 2 hours.Ethanol washing after reaction obtains multilevel hierarchy ZnO@Co-MOF；Per 0.2-0.5g 2-methylimidazoles pair in mother liquor B
Answer 0.02-0.05g cabaltous nitrate hexahydrates correspondence 20ml water；
Thioacetamide is dissolved in ethanol and obtains solution C by the 3rd step, will be previous step synthetic ZnO@Co-MOF immersions molten
In liquid C, reaction temperature is 50-80 DEG C, preferably 70 DEG C, and the time is 0.5-2 hours, preferably 1 hour, with ethanol and going after reaction
Ion water washing finally gives ZnO CoS optoelectronic poles.
Preferably per 0.1-0.3g thioacetamides correspondence 20ml ethanol in solution C.
The composite of multilevel hierarchy ZnO@CoS can be further used for efficient photoelectricity treater catalysis point as the application of optoelectronic pole
Xie Shui.
The present invention is prepared for the ZnO@CoS multilevel hierarchy composites of regular pattern and orderly array.The optoelectronic pole
With wider optical response signal, photoelectric catalytically active and higher electronic transmission performance, decompose with excellent photoelectrocatalysis
Aqueous energy；Preparation method process is simple of the present invention, easy to implement, yield are high, prepare high performance electrode material beneficial to batch.
Description of the drawings
Fig. 1 is the ESEM schematic diagram of the ZnO.
Fig. 2 is the SEM schematic diagram of the ZnO@Co-MOF composites.
Fig. 3 is the SEM schematic diagram of the ZnO@CoS composites.
Fig. 4 is the performance schematic diagram of ZnO@CoS composite photoelectrocatalysis decomposition waters in embodiment 1.
Specific embodiment
With reference to embodiment, the invention will be further described, but the present invention is not limited to following examples.
Embodiment 1
The first step is pre-processed with acetone, second alcohol and water ultrasound respectively for 10 minutes to FTO glass, is prepared by simple hydro-thermal method
ZnO electrode.Concrete grammar：Zinc acetate is dissolved in the zinc acetate ethanol solution that absolute ethyl alcohol prepares 5mM for which.By above-mentioned solution spin coating
One layer of crystal seeding film is obtained on the FTO of pretreatment, is then annealed 30 minutes at 350 DEG C.Will be the FTO of growth ZnO crystal seeds oblique
Ride in the polytetrafluoroethylene reactor equipped with solution A, liquid A is the zinc nitrate and urotropine of same molar ratio
The aqueous solution, wherein nitric acid zinc concentration 30mM, 80 DEG C of reaction temperature, 5 hours reaction time.It is cooled to room temperature, obtained ZnO electrode
Deionized water is dried after rinsing in atmosphere.
ZnO nanorod immersion mother liquor B is carried out hydro-thermal reaction by second step, and mother liquor B is the 2-methylimidazole and 0.02g of 0.2g
Cabaltous nitrate hexahydrate be dissolved in 20ml water and DMF mixed solution, wherein water and DMF
Volume ratio is 1:5, and in moving into the reactor of 30ml, hydrothermal temperature is kept for 70 DEG C, time 2 h.After reaction, ethanol is washed
Wash and obtain multilevel hierarchy ZnO@Co-MOF.
0.3g thioacetamides are dissolved in 20ml ethanol and obtain solution C by the 3rd step, by previous step synthetic ZnO@Co-
In MOF immersion solution Cs, reaction temperature is 70 DEG C, and the time is 1 hour, washs final obtaining after reaction with ethanol and deionized water
To ZnO@CoS optoelectronic poles.
Embodiment 2
The first step is pre-processed with acetone, second alcohol and water ultrasound respectively for 10 minutes to FTO, obtains ZnO by simple hydro-thermal method
Electrode.Concrete grammar：Zinc acetate is dissolved in the zinc acetate ethanol solution that absolute ethyl alcohol prepares 10mM for which.Above-mentioned solution is spun to
One layer of crystal seeding film is obtained on the FTO of pretreatment, is then annealed 30 minutes at 350 DEG C.By the FTO obliques of growth ZnO crystal seeds
In the polytetrafluoroethylene reactor equipped with solution A, liquid A is the water of the zinc nitrate and urotropine of same molar ratio
Solution, wherein nitric acid zinc concentration 50mM, 95 DEG C of reaction temperature, 12 hours reaction time.It is cooled to room temperature, obtained ZnO electrode
Deionized water is dried after rinsing in atmosphere.
ZnO nanorod immersion mother liquor B is carried out hydro-thermal reaction by second step, and mother liquor B is 0.5g 2-methylimidazoles and 0.05g
Cabaltous nitrate hexahydrate is dissolved in 20ml water and DMF mixed solution, the wherein body of water and DMF
Product is than being 1:1, and hydrothermal temperature is kept for 80 DEG C, 1 hour in moving into the reactor of 30ml.Ethanol washing after reaction is obtained
Multilevel hierarchy ZnO@Co-MOF.
0.1g thioacetamides are dissolved in 20ml ethanol and obtain solution C by the 3rd step, by previous step synthetic ZnO@Co-
In MOF immersion solution Cs, reaction temperature is 80 DEG C, and the time is 2 hours, washs final obtaining after reaction with ethanol and deionized water
To ZnO@CoS optoelectronic poles.
The test result of the material obtained by above-described embodiment 1 is identical, specifically sees below：
(1) material morphology is characterized：
The ZnO electrode, a fritter of ZnO@Co-MOF and ZnO@CoS combination electrode materials are taken respectively, from Zeiss
SIGMA 500/VP model field emission scanning electron microscopes are characterized to which.Structure and morphology figure is shown in Fig. 1, Fig. 2, Fig. 3.
(2) material charge-discharge performance is characterized：
Light source model used herein is Beijing Bo Feilai Co., Ltds PLS-SXE300, and electro-chemical test instrument is Germany
ZAHNER electrochemical workstations.Fig. 4 is the dark and illumination condition (illumination in 0.5M metabisulfite solutions of ZnO@CoS combination electrodes
Radiation intensity is 150mW cm-2) volt-ampere linear polarisation curves.
Claims (8)
1. a kind of multilevel hierarchy ZnO@Co-MOF composites, it is characterised in that multilevel hierarchy ZnO@Co-MOF composites are
Core shell structure, wherein, central core layer is polygon nano-pillar ZnO, and outermost shell born as Co-MOF skeletons；The appearance of core shell structure
Face is axially stacked flower-like structure；Array structure of the multilevel hierarchy ZnO@Co-MOF composites for high-sequential.
2.ZnO@CoS composites, it is characterised in that multilevel hierarchy ZnO@Co-MOF composites obtain many by vulcanizing treatment
Level structure ZnO@CoS composites, the surface of multilevel hierarchy ZnO@CoS is hollow for uniform honeycomb flower-like structure, i.e. outer layer
Array structure of the CoS of polyhedral structure, the multilevel hierarchy ZnO@CoS composite for high-sequential.
3. the synthetic method of the ZnO@CoS composites described in claim 2, it is characterised in that comprise the following steps：
The first step is pre-processed to FTO ultrasounds respectively with acetone, ethanol and water successively, grows ZnO by hydro-thermal method in FTO substrates
Nanometer rods；
ZnO nanorod immersion mother liquor B is carried out hydro-thermal reaction by second step, and mother liquor B is that 2-methylimidazole and cabaltous nitrate hexahydrate are molten
The gained in water with DMF mixed solvent, wherein water are 1 with the volume ratio of DMF:1-1:
5, and in moving into reactor, hydrothermal temperature is kept for 60-80 DEG C, time 0.5-3 hour；Ethanol washing after reaction obtains many
Level structure ZnO@Co-MOF；Per 0.2-0.5g 2-methylimidazoles correspondence 0.02-0.05g cabaltous nitrate hexahydrate correspondences in mother liquor B
20ml water；
Thioacetamide is dissolved in ethanol and obtains solution C by the 3rd step, by previous step synthetic ZnO@Co-MOF immersion solution Cs
In, reaction temperature is 50-80 DEG C, and the time is 0.5-2 hours, is washed with ethanol and deionized water and finally give ZnO@after reaction
CoS optoelectronic poles；
Per 0.1-0.3g thioacetamides correspondence 20ml ethanol in solution C.
4. according to the method for claim 3, it is characterised in that the method for first step growing ZnO nanorod in FTO substrates：Its
Zinc acetate is dissolved in into the zinc acetate ethanol solution that absolute ethyl alcohol prepares 5-10mM；Zinc acetate ethanol solution is spun to into pretreatment
One layer of crystal seeding film is obtained on FTO, then annealing obtains the FTO for growing ZnO crystal seeds for 30 minutes at 300-400 DEG C；Will growth
In the polytetrafluoroethylene reaction kettle for reaction equipped with solution A, wherein solution A is same molar ratio to the FTO obliques of ZnO crystal seeds
The aqueous solution of zinc nitrate and urotropine, wherein nitric acid zinc concentration 30-60mM, reaction temperature 80-95 DEG C, reaction time
5-24 hours, are subsequently cooled to room temperature, and obtained ZnO nanorod deionized water is dried after rinsing in atmosphere.
5. according to the method for claim 3, it is characterised in that second step water is 1 with the volume ratio of DMF:5；
70 DEG C of hydrothermal temperature, time 2 h.
6. according to the method for claim 3, it is characterised in that three-step reaction temperature 70 C, time 2 h.
7. according to the application of the ZnO@CoS composites described in claim 2, as the application of optoelectronic pole.
8. according to the application of the ZnO@CoS composites described in claim 2, for efficient photoelectricity treater catalytic decomposition water.
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| CN107803207A (en) * | 2017-10-18 | 2018-03-16 | 中南大学 | A kind of carbon-based double metallic composite material, preparation and its application |
| CN107930670A (en) * | 2017-11-30 | 2018-04-20 | 中国石油大学(北京) | Heterogeneous catalysis material that a kind of self-cradling type is homogeneously changed and its preparation method and application |
| CN108439549A (en) * | 2018-04-03 | 2018-08-24 | 北京工业大学 | A kind of preparation of array structure transition metal selenides electrode and its application in electrolysis water |
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| CN110828785A (en) * | 2019-09-25 | 2020-02-21 | 肇庆市华师大光电产业研究院 | Preparation method of sodium ion battery cathode material of zinc-cobalt bimetallic sulfide |
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