CN109280937A - A kind of preparation of ZIF-67/ pucherite composite material and application as photo cathode material - Google Patents

A kind of preparation of ZIF-67/ pucherite composite material and application as photo cathode material Download PDF

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CN109280937A
CN109280937A CN201811425263.1A CN201811425263A CN109280937A CN 109280937 A CN109280937 A CN 109280937A CN 201811425263 A CN201811425263 A CN 201811425263A CN 109280937 A CN109280937 A CN 109280937A
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zif
bivo
composite material
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pucherite
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CN109280937B (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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    • 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
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    • 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
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    • 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

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Abstract

It is by 2-methylimidazole and Co (NO the invention discloses a kind of preparation of ZIF-67/ pucherite composite material3)2·6H2O is dissolved in n,N-Dimethylformamide-distilled water, then by BiVO4Film, which is placed in one, impregnates one section of hour；Then washed completely with distilled water, ethyl alcohol, it is dry to get.ZIF-67 is successfully loaded to BiVO by the method for in-situ deposition by the present invention4Surface forms stable ZIF-67/BiVO4Thin-film material.Under high bias, ZIF-67/BiVO4Composite material is than pure/BiVO4There is higher photoelectric current；The introducing of ZIF-67 extends the service life of carrier well simultaneously, also improves BiVO4PhotoelectrocatalytiPerformance Performance.It is accordingly tested by photoelectric current and photoelectricity injection efficiency calculates, it was demonstrated that the composite photoelectric is great excellent PhotoelectrocatalytiPerformance Performance, is used for optical anode material, can effectively improve hydrogen generation efficiency.

Description

The preparation of a kind of ZIF-67/ pucherite composite material and as photo cathode material Using
Technical field
The present invention relates to a kind of preparation of pucherite combination electrode film more particularly to a kind of ZIF-67/BiVO4Photoelectrocatalysis The preparation method of composite material is decomposed in the reaction for producing hydrogen mainly as photo cathode material with light electro-chemical water.
Background technique
Currently, the problems such as largely resulting in Global climate change and environmental degradation using fossil fuel.And it all these asks Topic has become the major impetus accelerated from using renewable energy to clean energy resource.Therefore this is maximum renewable for solar energy The utilization of the energy has obtained extensive concern, and in widely available various solar energy conversion options, it is reacted using photoelectrolysis Decomposing water with solar energy and to generate hydrogen be one of most promising technology.Up to the present, many semiconductor materials are had studied Material is widely used in photoelectricity as light anode, especially binary metal oxide and produces hydrogen field.However because of these materials Unstable chemcial property, electron-hole pair are easy compound, it is seen that light absorpting ability is weak, electron-hole pair migration velocity slowly etc. because Element limits them in the application in optical electro-chemistry field.Even if improving its performance by various modifications, but incident photon is converted Efficiency is still lower.
In terms of optical electro-chemistry water decomposition produces hydrogen, numerous semiconductor materials are having excellent table as optical anode material It is existing, such as TiO2、Cds、Fe2O3And WO3, therefore be concerned.And in numerous welcome materials, BiVO4Show its uniqueness Performance, it is a kind of thin pillar (Eg=2.4 ~ 2.5 eV) n-type semiconductor, have excellent visible light absorption capacity, it is adjustable Electronic structure, the preparation of good stability and low cost.However, its PEC capacity is relatively poor, such as chemical stability shakiness Fixed, photo-generated carrier quick compound and weakly visible light absorption limits it and further goes to utilize it.
A large amount of research has solved BiVO in recent years4Electron-hole pair is in conjunction with low with solar conversion efficiency Problem.Generally speaking, BiVO4Photoelectrochemical behaviour a degree of raising has been obtained by various methods.Universal Method includes: ion doping, Morphological control and WO3、ZnFeO4, graphene oxide, BiOI form hetero-junctions, load produces oxygen and helps and urges Agent Co3O4,NiO,FeOOH,NiOOH；Or in surface depositing noble metal nanoparticle Ag, Au etc..
Metal organic framework (MOFs) is a kind of emerging porous material, due to the function of its structure abundant and multiplicity Property, it is stored in gas, separation, there is potential application in terms of catalysis and chemical sensitisation.Although having many advantages, many MOF's Using finally being limited by their stability under severe conditions.Therefore, the present invention combines pucherite and MOFs, system A kind of standby MOFs/ pucherite photoelectrocatalysis composite material is BiVO4Photoelectrochemical behaviour propose a kind of new plan Slightly.
Summary of the invention
The object of the present invention is to provide a kind of preparation methods of ZIF-67/ pucherite photoelectrocatalysis composite material；
It is another object of the present invention to the photoelectrochemical behaviours to ZIF-67/ pucherite photoelectrocatalysis composite material to study.
One, ZIF-67/BiVO4The preparation of photo cathode
By 2-methylimidazole and Co (NO3) 2·6H2O is dissolved in N,N-dimethylformamide-with the mass ratio of 1:0.1 ~ 1:0.2 It distills in water mixed solution, stirs 20 ~ 30 minutes；By BiVO4Film is placed in mixed solution, and it is small that 1 ~ 2 is impregnated at 50 ~ 70 DEG C When；It is successively washed completely with distilled water, ethyl alcohol, vacuum drying is at 50 ~ 80 DEG C to get MOFs/BiVO4Photo cathode material.
In n,N-Dimethylformamide-distillation water mixed solution, the volume ratio of n,N-Dimethylformamide and distilled water is 3:1~5:1。
Two, ZIF-67/BiVO4The structure of photo cathode
Fig. 1 is the electron-microscope scanning figure of optoelectronic pole.Wherein a, b are the porous BiVO under different amplification4Film.C is ZIF-67/ BiVO4Combination electrode.By Fig. 1, it is clear that in pure BiVO4Uniform unbodied ZIF-67 has been loaded on film.Card Bright ZIF-67 has successfully been loaded on BiVO4 film.
Fig. 2 is BiVO4And ZIF-67/BiVO4The XRD diagram of film.BiVO4All diffraction maximums be shown to be monoclinic crystal, and There is no the diffraction maximum of other impurity peaks and other crystal phases to occur, shows the BiVO of monocline crystal phase4It successfully prepares.Other diffraction maximums It is tetragonal phase SnO2 diffraction maximum in FTO (JCPDS. No. 41-1445) substrate.The diffraction maximum of ZIF-67 exists after light reaction 27.14 DEG C of appearance, the weaker reason of diffraction maximum is that ZIF-67 is supported on BiVO4Amount on film is seldom.
Fig. 3 is BiVO4With ZIF-67/BiVO4The UV-Vis DRS figure of combination electrode.As shown, BiVO4's For ABSORPTION EDGE substantially in 500nm or so, this is consistent with the document of report, illustrates BiVO4Response is visible light.As load ZIF-67 After nano particle, BiVO4The absorption intensity of light is enhanced, and slight Red Shift Phenomena also has occurred in ABSORPTION EDGE, therewith Forbidden bandwidth will also reduce.Allow for ZIF-67/BiVO4Electrode more visible lights can be absorbed so that optical property more It is good.
Fig. 4 is BiVO4 and ZIF-67/BiVO4Electrode linear scan.BiVO4With ZIF-67/ BiVO4The photoelectricity of electrode Analog light source of the catalytic water oxidation susceptibility in AM 1.5G, the 0.5M Na of pH 6.862SO4It is tested in solution.It was found that unglazed According to when BiVO4Film is almost without electric current.And in the voltage range entirely tested, load the ZIF-67 of ZIF-67 nano particle / BiVO4The electric current of electrode is higher than BiVO4The electric current of electrode.In the 1.23 V vs.RHE of normal potential of water oxygen, ZIF-67/ BiVO4The photoelectric current of electrode is 3.16mA/cm2, it is BiVO4The theoretical photocurrent values that (1.33v) semiconductor is generated as anode 2.4 times.And support materials are in 100 mW/cm2Under AM 1.5G light source, almost primary current 12 times (0.80 mA/ cm2).Meanwhile with BiVO4Electrode is compared, ZIF-67/BiVO4The water oxygen initial potential of electrode becomes 0.38V from 0.61 V, This shows that ZIF-67 is a kind of excellent water oxidation promoters.
Fig. 5 is BiVO4With ZIF-67/ BiVO4Time current curve figure at 0.6V and 1.0V.5 it can be known by figure, no By being ZIF-67/BiVO under which bias4The density of photocurrent of electrode is all higher than pure BiVO4Electrode.This be mainly because BiVO is enriched in for photohole4The compound again of a large amount of electron-hole pair has occurred in film surface.And work as ZIF-67 nanoparticle Son is carried on BiVO4Behind surface, the situation that can efficiently reduce accumulation occurs, to enhance carrier during water oxygen In conjunction with extending the service life of carrier, improve the efficiency of light quantum.Finally enhance PhotoelectrocatalytiPerformance Performance.Further Prove ZIF-67/BiVO4Combination electrode is excellent optical anode material.
Fig. 6 is the BiVO when excitation wavelength is 350nm4With ZIF-67/BiVO4The photoluminescence figure of light anode.From Fig. 6 It can be seen that ZIF-67/BiVO4The pure BiVO of fluorescence intensity ratio4Film wants weak.Show ZIF-67/BiVO4Light induced electron- Hole has higher photo-quantum efficiency to more easily separated.
Fig. 7 is BiVO4 and ZIF-67/BiVO4The charge injection efficiency figure of light anode.The charge injection efficiency of electrode is Assessment participates in the important parameter of the hole ratio of reaction.Within the system, charge injection efficiency can be by by electrode catalyst oxygen The electric current of change is divided by electrode catalyst Na2SO3The electric current of oxidation obtains.As shown in fig. 7, ZIF-67/BiVO4Electrode has highest Charge injection efficiency, show after loading ZIF-67 reach electrode surface hole reactivity it is higher.ZIF-67 / BiVO4The charge injection efficiency of electrode reaches 65%.
In conclusion ZIF-67 is successfully loaded to BiVO by the method for in-situ deposition by the present invention4Surface is formed steady Fixed ZIF-67/BiVO4Thin-film material.(> 0.6 V vs. Ag/AgCl), ZIF-67/BiVO under high bias4Composite wood Material is than pure/BiVO4There is higher photoelectric current.The introducing of ZIF-67 extends the service life of carrier well simultaneously, also improves BiVO4PhotoelectrocatalytiPerformance Performance.It is accordingly tested by photoelectric current and photoelectricity injection efficiency calculates, it was demonstrated that composite photoelectric is great to be had Excellent PhotoelectrocatalytiPerformance Performance.ZIF-67/BiVO4Composite material is directly used in optical anode material, can effectively capture light, reduces Charge transfer resistance, accelerates the fast transferring of carrier, to inhibit the compound of electron hole pair, can effectively improve and produce hydrogen effect Rate.
Detailed description of the invention
Fig. 1 is (a-b) BiVO4(c) ZIF-67/BiVO4The electron-microscope scanning figure of optoelectronic pole.
Fig. 2 is the XRD diagram of BiVO4 and ZIF-67/BiVO4 optoelectronic pole.
Fig. 3 is BiVO4 and ZIF-67/BiVO4 UV-vis DRS figure.
Fig. 4 is the linear scan of BiVO4 and ZIF-67/BiVO4. electrode.
Fig. 5 is the i-t circulation A in different biass) 0.6 V and (B) 1.0 V vsAg/AgCl (0.35 M KCl) be bent Line.
Fig. 6 is the photoluminescence figure of BiVO4 and ZIF-67/BiVO4..
Fig. 7 is the charge injection efficiency figure of BiVO4 and ZIF-67/BiVO4..
Specific embodiment
Exist below by specific embodiment to the preparation of ZIF-67/BiVO4 composite material of the present invention and as photo cathode The application that water decomposition produces hydrogen is described further.
(1) prepared by BiVO4de: is prepared according to Kim and Choi seminar electro-deposition combination heat-treating methods.Specifically Step: BiOI nanometer sheet is prepared by electrodeposition process with CHI 660D electrochemical workstation first.With acetone/isopropanol/distillation For the FTO glass that water (volume ratio: 1:1:1) was cleaned by ultrasonic as working electrode, Ag/AgCl (3.5 M KCl) electrode is ginseng Than electrode, Pt electrode is to electrode.With 6M HNO350 mL0.4 M KI pH value of solution are adjusted to 1.5 ~ 1.7, add 0.970 g Bi(NO3)3•5H2O is until dissolution, solution colour become orange red.Then 0.498 g 1,4- benzoquinones of 20ml is slowly added dropwise Ethanol solution stirs several minutes, and solution becomes blood red again.Electro-deposition is scanned with cyclic voltammetry, voltage: -0.13-0 V is swept Speed: 5 mV/ s.The BiOI film of acquisition is washed with distilled water.Then, 0.1 mL, 0.2 M vanadyl acetylacetonate-dimethyl is sub- Sulfolane solution micro syringe drips on the BiOI film prepared, rises to 450 DEG C in Muffle furnace with 2 DEG C/min rate and forges Burn 2h.Extra V2O5It is impregnated and is eliminated with 1 M NaOH with bismuth oxide etc., leave the vanadic acid bismuth thin film of gilvous.Finally obtain BiVO4Electrode is washed with distilled water natural drying.
(2) ZIF-67/BiVO4Preparation: take 2-methylimidazole (0.1g) and Co (NO3) 2·6H2O(0.0125g), dissolve In 16mL N,N-dimethylformamide and distilled water (DMF:H2O=3:1, V:V) mixed solution in, stir 30 minutes；It will be upper State the BiVO of preparation4It is placed in above-mentioned mixed solution, is impregnated 2 hours at 70 DEG C；It is washed completely with distilled water and ethyl alcohol, 60 3 hours are dried in vacuo at DEG C to get ZIF-67/BiVO4Composite material.
(3) ZIF-67/BiVO4Composite material is applied directly as photo cathode and produces hydrogen reaction in optical electro-chemistry water decomposition In, hydrogen generation efficiency 92.6%.

Claims (5)

1. a kind of preparation method of ZIF-67/ pucherite composite material, being will be by 2-methylimidazole and Co (NO3) 2·6H2O dissolution In n,N-Dimethylformamide-distillation water mixed solution, stir 20 ~ 30 minutes；Again by BiVO4Electrode film is placed in mixed solution In, it is impregnated 1 ~ 2 hour at 50 ~ 70 DEG C；Successively washed completely with distilled water, ethyl alcohol, it is dry to get MOFs/BiVO4Composite wood Expect material.
2. a kind of preparation method of ZIF-67/ pucherite composite material as described in claim 1, it is characterised in that: 2- methyl miaow Azoles and Co (NO3) 2·6H2The mass ratio of O is 1:0.1 ~ 1:0.2.
3. a kind of preparation method of ZIF-67/ pucherite composite material as described in claim 1, it is characterised in that: N, N- diformazan In base formamide-distillation water mixed solution, the volume ratio of n,N-Dimethylformamide and distilled water is 3:1 ~ 5:1.
4. a kind of preparation method of ZIF-67/ pucherite composite material as described in claim 1, it is characterised in that: drying be It is dried in vacuo at 50 ~ 80 DEG C.
5. application of the ZIF-67/ pucherite composite material of method preparation as described in claim 1 as photo cathode material.
CN201811425263.1A 2018-11-27 2018-11-27 Preparation of ZIF-67/bismuth vanadate composite material and application of composite material as photoelectric anode material Active CN109280937B (en)

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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
CN110180529A (en) * 2019-05-23 2019-08-30 北京科技大学 A kind of preparation method of MOF as precursor synthesis catalysis material
CN110408951A (en) * 2019-07-15 2019-11-05 江苏大学 A kind of Cu-MOF/BiVO4The preparation method and application of complex light electrode
CN110983362A (en) * 2019-12-19 2020-04-10 湖南大学 MOFs-coated OV-BiVO4Composite photo-anode and preparation method and application thereof
CN112210787A (en) * 2020-09-28 2021-01-12 西南石油大学 Preparation method of metal organic framework material coating on surface of nano-structure substrate
CN113130776A (en) * 2019-12-30 2021-07-16 Tcl集团股份有限公司 Quantum dot light-emitting diode and preparation method thereof
CN113818043A (en) * 2021-10-18 2021-12-21 台州学院 Bismuth vanadate-metal organic complex composite photoelectrode and preparation method and application thereof

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Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN110180529A (en) * 2019-05-23 2019-08-30 北京科技大学 A kind of preparation method of MOF as precursor synthesis catalysis material
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
CN110408951A (en) * 2019-07-15 2019-11-05 江苏大学 A kind of Cu-MOF/BiVO4The preparation method and application of complex light electrode
CN110408951B (en) * 2019-07-15 2021-05-25 江苏大学 Cu-MOF/BiVO4Preparation method and application of composite photoelectrode
CN110983362A (en) * 2019-12-19 2020-04-10 湖南大学 MOFs-coated OV-BiVO4Composite photo-anode and preparation method and application thereof
CN110983362B (en) * 2019-12-19 2021-05-28 湖南大学 MOFs-coated OV-BiVO4Composite photo-anode and preparation method and application thereof
CN113130776A (en) * 2019-12-30 2021-07-16 Tcl集团股份有限公司 Quantum dot light-emitting diode and preparation method 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
CN112210787A (en) * 2020-09-28 2021-01-12 西南石油大学 Preparation method of metal organic framework material coating on surface of nano-structure substrate
CN113818043A (en) * 2021-10-18 2021-12-21 台州学院 Bismuth vanadate-metal organic complex composite photoelectrode and preparation method and application thereof

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