CN109913896A - A kind of preparation and application of the pucherite composite material of supported bi-metallic oxide nano-particles - Google Patents
A kind of preparation and application of the pucherite composite material of supported bi-metallic oxide nano-particles Download PDFInfo
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- CN109913896A CN109913896A CN201910154174.6A CN201910154174A CN109913896A CN 109913896 A CN109913896 A CN 109913896A CN 201910154174 A CN201910154174 A CN 201910154174A CN 109913896 A CN109913896 A CN 109913896A
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- 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
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- 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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- Y02P20/00—Technologies relating to chemical industry
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Abstract
It is by ZnCo the present invention provides a kind of preparation method of the pucherite composite material of supported bi-metallic oxide nano-particles2O4After black powder is fully ground, it is added to ultrasonic disperse in acetone and forms ZnCo2O4Acetone soln；Then with BiVO4Film makees cathode, using electrophoretic deposition, by ZnCo2O4Nanoparticle is successfully supported on BiVO4On film, so that ZnCo2O4/BiVO4Composite material forms n-n heterojunction structure, and such a construction increases the separative efficiencies of photo-generated carrier, and in BiVO4Area load water oxidation promoters ZnCo2O4Nanoparticle accelerates hole in the transmission of electrode and dielectric interface, improves BiVO4Photoelectricity water oxidation susceptibility, therefore as photo cathode material, for there is good water oxidation susceptibility in optical electro-chemistry water decomposition reaction.
Description
Technical field
The present invention relates to a kind of BiVO4Based composites are related to a kind of supported bi-metallic oxide nano-particles ZnCo2O4
BiVO4The preparation of composite material is reacted mainly as photo cathode material for optical electro-chemistry water decomposition.
Background technique
It seriously pollutes caused by use with fossil fuel and fossil fuel itself can not give birth to, people is forced to go out
It sends out a kind of and cleans reproducible new energy.Hydrogen Energy has energy height, pollution-free, sustainable advantage.Optical electro-chemistry water decomposition produces
Hydrogen is a kind of available production hydrogen mode.BiVO4It is a kind of common photo cathode material, has band gap width small, Ke Yili
The advantages of with sunlight, but its charge migration rate is low, and has slow water oxidation kinetics, limits BiVO4
Photoelectricity water oxidation susceptibility.
Summary of the invention
The purpose of the present invention is for BiVO in the prior art4Material there are the problem of, provide a kind of photoelectrochemical credit
Xie Shui composite material ZnCo of good performance2O4/BiVO4Preparation method.
One, composite material ZnCo2O4/BiVO4Preparation
(1) ZnCo2O4Preparation
By Zn (NO3)2.6H2O、Co(NO3)2.6H2O、NH4F、Co(NH2)2It is add to deionized water, stirring makes it completely dissolved
Afterwards, 120 DEG C ~ 130 DEG C hydro-thermal reaction 5 ~ 6 hours；It is cooled to room temperature after reaction, product, distilled water and second is collected by centrifugation
Alcohol washing, 60 DEG C in an oven ~ 70 DEG C drying 4 ~ 5 hours, obtain aubergine powder, aubergine powder be then placed in Muffle furnace
In at 400 DEG C ~ 450 DEG C calcine 2h ~ 3h, obtain black powder.Wherein Zn (NO3)2·6H2O:Co(NO3)2·6H2O:
NH4F:Co(NH2)2Molar ratio be 1:2:2:5.
(2) composite material ZnCo2O4/BiVO4Preparation
By ZnCo2O4After black powder is fully ground, being added in acetone and being ultrasonically treated 25 ~ 30min formation concentration is 0.7mg/
The ZnCo of mL ~ 0.8mg/mL2O4Acetone soln；Then with BiVO4Film makees cathode, using electrophoretic deposition, in 20V ~ 21V voltage
10 ~ 40s of lower deposition, so that ZnCo2O4Uniform load is in BiVO4Surface after the completion of deposition, is rinsed with distilled water and ethyl alcohol, is done
It is dry, form ZnCo2O4/BiVO4Composite material.
Two, ZnCo2O4/BiVO4The characterization of composite material
Fig. 1 is BiVO4SEM figure and ZnCo2O4/BiVO4SEM figure.As seen from Figure 1, the BiVO of above-mentioned synthesis4Film
For the worm shape structure of nanoporous, ZnCo2O4/BiVO4Composite material is the ball cactus shape structure being made of nanometer bead.
Fig. 2 is BiVO4TEM figure and ZnCo2O4/BiVO4TEM figure.From figure 2 it can be seen that BiVO4Film edge light
It is sliding, and ZnCo2O4/BiVO4There is nanometer small particle in film edge, these small particles are ZnCo2O4Nano particle.
Fig. 3 is FTO electro-conductive glass, BiVO4、ZnCo2O4、ZnCo2O4/BiVO4XRD diagram.It can be seen that FTO conduction glass
There is apparent SnO in glass2There is SnO at 27 degree and 38 degree or so in peak2Two strong diffraction maximums, the BiVO of synthesis4XRD
On there is BiVO4Characteristic diffraction peak, illustrate to have synthesized monoclinic phase BiVO4。ZnCo2O4The XRD characteristic diffraction peak and text of powder
The corresponding of middle report is offered, illustrates to have synthesized ZnCo2O4Nanoparticle, in ZnCo2O4/BiVO4Occurs BiVO in composite material4
Characteristic diffraction peak, almost without there is ZnCo2O4The peak of nanoparticle, this is because the ZnCo of load2O4The amount of nanoparticle
Less reason.
Three, BiVO4、ZnCo2O4/BiVO4The optical performance test of composite material
The optical property of all photo cathodes is assessed by test UV Diffuse Reflectance Spectroscopy.Fig. 4 is respectively BiVO4, composite wood
Expect ZnCo2O4/BiVO4UV Diffuse Reflectance Spectroscopy and band gap width figure.It can see from Fig. 4 a, BiVO4The absorption edge of film exists
498.9nm, corresponding band gap width are 2.42eV, ZnCo2O4/BiVO4Absorption edge in 528nm, corresponding band gap width is
2.27eV.When deposited ZnCo2O4After nanosphere, red shift is had occurred in absorption edge, and absorption intensity enhances.Composite material
Band gap width reduces, and lower energy can be absorbed, increase BiVO4To the utilization rate of sunlight.
Fig. 5 is BiVO4、ZnCo2O4/BiVO4Not special Schottky figure, as can be seen from Figure 5 pure BiVO4Mo Texiao
The slope of Te Jitu is positive, and illustrates BiVO4For n-type semiconductor, ZnCo2O4Not special Schottky figure slope be also it is positive, it is compound
Material ZnCo2O4/BiVO4N-n hetero-junctions is constituted, the separative efficiency of photo-generated carrier is improved.
Fig. 6 records pure BiVO4, ZnCo2O4/BiVO4LSV curve.Fig. 6 a, b show to load ZnCo2O4Afterwards, composite material
ZnCo2O4/BiVO4Performance and pure BiVO4Compared to all improving, wherein ZnCo obtained after deposition 35s2O4/BiVO4Composite wood
The performance of material is deposition ZnCo2O4Effect is best afterwards, BiVO4, ZnCo2O4/BiVO4(sedimentation time 35s) is in 1.23 V
Density of photocurrent respectively reaches 1.2mA cm when vs.RHE-2With 2.8 mA cm-2, with BiVO4(1.2mA cm-2) film compared to increase
2.3 times.By ZnCo2O4Deposit to BiVO4Surface on to form ZnCo2O4/BiVO4N-n hetero-junctions, it reduce photoproduction loads
Compound, the aqueous energy of raising optical electro-chemistry decomposition of stream.Fig. 6 c, d show the LSV curve under no illumination, BiVO4Film
Take-off potential is 2.4V, ZnCo2O4/BiVO4The take-off potential of composite material is 2V, composite material and pure BiVO4Compared to starting
Current potential is to movable cathode 0.4V.Illustrate overpotential of the composite material in water decomposition reaction than pure BiVO4It is small, water load oxidation
Co-catalyst ZnCo2O4After accelerate hole to electrode dielectric interface transmit.BiVO after addition hole trapping agents4And ZnCo2O4/
BiVO4Density of photocurrent all improve.
Fig. 7 is BiVO4The density of photocurrent figure of series of samples.From 7a it can be seen that deposited ZnCo2O4Afterwards, ZnCo2O4/
BiVO4Density of photocurrent ratio BiVO4Performance will be high.It can be seen that pure BiVO from Fig. 7 b4Density of photocurrent in 1.23 V
It is 1.2mA cm when vs.RHE-2, composite material ZnCo2O4/BiVO4The density of photocurrent of (deposition 35s) is in 1.23 V vs.RHE
When be 2.8mA cm-2And pure BiVO42.3 times are improved compared to density of photocurrent.Illustrate to load ZnCo2O4After improve BiVO4
Optical electro-chemistry water dispersible energy.
Fig. 8 is BiVO4And ZnCo2O4/BiVO4Electrochemical impedance spectrogram in the case where having light irradiation and unglazed irradiation.There is light
ZnCo under irradiation condition2O4/BiVO4Electrochemical impedance spectrogram arc diameter ratio BiVO4Want small, under non-illuminated conditions
ZnCo2O4/BiVO4Electrochemical impedance spectrogram camber ratio BiVO4Also want small.Illustrate to load ZnCo2O4Afterwards, photoproduction is accelerated
The transmission rate of charge.So that BiVO4PEC water dispersible can be more preferable.
In conclusion the present invention passes through electrophoretic deposition technique, by ZnCo2O4Nanoparticle is successfully supported on BiVO4Film
On, so that ZnCo2O4/BiVO4Composite material forms n-n heterojunction structure, and such a construction increases the separation of photo-generated carrier effects
Rate, and in BiVO4Area load water oxidation promoters ZnCo2O4Nanoparticle accelerates hole in electrode and dielectric circle
The transmission in face, improves BiVO4Photoelectricity water oxidation susceptibility be used for optical electro-chemistry water decomposition therefore as photo cathode material
There is good water oxidation susceptibility in reaction.
Detailed description of the invention
Fig. 1 is BiVO4SEM figure and ZnCo2O4/BiVO4SEM figure.
Fig. 2 is BiVO4TEM figure and ZnCo2O4/BiVO4TEM figure.
Fig. 3 is FTO electro-conductive glass, BiVO4、ZnCo2O4、ZnCo2O4/BiVO4XRD diagram.
Fig. 4 is respectively BiVO4, composite material ZnCo2O4/BiVO4UV Diffuse Reflectance Spectroscopy and band gap width figure.
Fig. 5 is BiVO4、ZnCo2O4/BiVO4Not special Schottky figure.
Fig. 6 records pure BiVO4, ZnCo2O4/BiVO4LSV curve.
Fig. 7 is BiVO4The density of photocurrent figure of series of samples.
Fig. 8 is BiVO4And ZnCo2O4/BiVO4Electrochemical impedance spectrogram in the case where having light irradiation and unglazed irradiation.
Specific embodiment
Below by specific embodiment to BiVO of the present invention4And ZnCo2O4/BiVO4The preparation of composite material is made furtherly
It is bright.
(1) preparation of BiOI film
It is electrodeposited in a three-electrode system, uses FTO substrate as working electrode, platinized platinum is used as to electrode, is saturated Ag/
AgCl carries out electro-deposition as reference electrode, by cyclic voltammetric electrodeposition process, and voltage is set as 0V ~ -0.13V, sweep speed
For 5mV/s, deposition is washed with distilled water and dehydrated alcohol after the completion, is then dried in air.
A. it is poured into the beaker of 100ml with the distilled water that graduated cylinder measures 40-60 mL, then weighs 3-3.5g potassium iodide,
Drug is slowly added into beaker under magnetic stirrer, stirring makes it completely dissolved, and forms colourless transparent solution；
B. nitric acid (HNO is used3) adjust potassium iodide aqueous solution pH value be 1.5 ~ 1.7；
C. 0.9 ~ 1g, five water bismuth nitrate (Bi (NO is weighed on balance3)3•5H2O it) is added in above-mentioned solution, stirs 30min, make it
It is completely dissolved, solution colour becomes orange red；
D. 0.4 ~ 0.5g 1,4-benzoquinone (C is weighed on balance6H4O2), under magnetic stirrer, 1,4-benzoquinone is added to
In 20mL-30mL dehydrated alcohol, stirring a period of time, it is completely dissolved 1,4-benzoquinone；
E. 1,4-benzoquinone ethanol solution is added dropwise to dropwise in the mixed solution of the potassium iodide and five water bismuth nitrates that are obtained in (c), so
After stir 30min, obtain the kermesinus electrolyte of deposition BiOI film.
(2) BiVO4The preparation of film
A. 0.1 ~ 0.15g vanadyl acetylacetonate (VO (acac) is weighed in the balance2), 2.5ml ~ 3ml dimethyl sulfoxide is added
(DMSO), then ultrasound 30min, makes it completely dissolved, obtains the dimethyl sulphoxide solution of vanadyl acetylacetonate；
B. the dimethyl sulphoxide solution that the vanadyl acetylacetonate of 100 μ L is measured with liquid-transfering gun, is added dropwise on BiOI film；
C. the BiOI film in vanadium source will be added dropwise, calcine 2 ~ 2.5h at 400 ~ 500 DEG C in Muffle furnace；It is down to room temperature to temperature, it will
BiVO4Film takes out；
D. by BiVO4Film immerses a period of time in NaOH solution, removes the excessive V in surface2O5, then dry with distilled water flushing
Only, it is put into baking oven and dries at 60 DEG C to get light yellow BiVO4Film.
(3) ZnCo2O4The preparation of powder
By 0.2g ~ 0.3gZn (NO3)2·6H2O, 0.5g ~ 0.6gCo (NO3)2·6H2O, 0.07g ~ 0.08g NH4F and 0.3g ~
0.4g urea is successively added in the distilled water of 35ml under magnetic stirring, makes it completely dissolved, is then placed in polytetrafluoroethylene (PTFE)
Reaction kettle in, control reaction temperature reacted 5 ~ 6 hours at 120 DEG C ~ 130 DEG C.Product distilled water and ethyl alcohol centrifugation, are washed
It washs, then keeps 5 ~ 6 hours at 60 DEG C in an oven, calcine 2h ~ 3h in Muffle furnace high temperature, form ZnCo2O4Black powder
End.
(4) ZnCo2O4/BiVO4The preparation of composite material
The acetone that 50ml is measured with graduated cylinder, then weighs 0.04g ~ 0.05gZnCo2O4Powder, by ZnCo2O4Powder is scattered in third
In ketone, ultrasonic 30min forms uniform ZnCo2O4Acetone soln, BiVO4Film makees cathode, by way of electrophoretic deposition, electricity
Pressure is set as 20V, sedimentation time 35s；After the completion of deposition, rinsed with distilled water and ethyl alcohol, it is dry, form ZnCo2O4/BiVO4
Film.
(5) ZnCo2O4/BiVO4Composite material is used for optical electro-chemistry water decomposition reaction test as photo cathode: 1.23
Density of photocurrent reaches 2.8 mA cm when V vs.RHE-2。
Claims (7)
1. a kind of preparation method of the pucherite composite material of supported bi-metallic oxide nano-particles, is by ZnCo2O4Black powder
After end is fully ground, it is added to ultrasonic disperse in acetone and forms ZnCo2O4Acetone soln；Then with BiVO4Film makees cathode, adopts
With electrophoretic deposition, 10 ~ 40s is deposited under 20V ~ 21V voltage, by ZnCo2O4Uniform load is in BiVO4Surface；After the completion of deposition,
It is rinsed with distilled water and ethyl alcohol, it is dry, form ZnCo2O4/BiVO4Composite material.
2. a kind of preparation method of the pucherite composite material of supported bi-metallic oxide nano-particles as described in claim 1,
It is characterized by: ZnCo2O4The ultrasonic disperse time being added in acetone is 25 ~ 30min.
3. a kind of preparation method of the pucherite composite material of supported bi-metallic oxide nano-particles as described in claim 1,
It is characterized by: made ZnCo2O4In acetone soln, ZnCo2O4Concentration be 0.7mg/mL ~ 0.8mg/mL.
4. a kind of preparation method of the pucherite composite material of supported bi-metallic oxide nano-particles as described in claim 1,
It is characterized by: the electrophoretic deposition is 10 ~ 40s of deposition under 20V ~ 21V voltage.
5. a kind of preparation method of the pucherite composite material of supported bi-metallic oxide nano-particles as described in claim 1,
It is characterized by: the ZnCo2O4The preparation of powder is by Zn (NO3)2·6H2O、Co(NO3)2·6H2O、NH4F、Co(NH2)2
Be add to deionized water, stirring make it completely dissolved after, 120 DEG C ~ 130 DEG C hydro-thermal reaction 5 ~ 6 hours；It drops after reaction
Warm to room temperature, product, distilled water and ethanol washing be collected by centrifugation, 60 DEG C in an oven ~ 70 DEG C drying 4 ~ 5 hours, obtain purplish red
Then aubergine powder is placed in Muffle furnace calcining 2h ~ 3h at 400 DEG C ~ 450 DEG C, obtains black powder by color powder.
6. a kind of preparation method of the pucherite composite material of supported bi-metallic oxide nano-particles as described in claim 1,
It is characterized by: Zn (NO3)2·6H2O:Co(NO3)2·6H2O:NH4F:Co(NH2)2Molar ratio be 1:2:2:5.
7. the pucherite composite material of the supported bi-metallic oxide nano-particles of method preparation as described in claim 1 is as light
Electric anode material is reacted for optical electro-chemistry water decomposition.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110923747A (en) * | 2019-12-09 | 2020-03-27 | 中国石油大学(华东) | Preparation method of bismuth ferrite photocatalytic film electrodeposition |
| CN112410819A (en) * | 2020-11-10 | 2021-02-26 | 北京化工大学 | Composite bismuth-based photoanode for photoelectrocatalytic decomposition of water and preparation method thereof |
| CN115055189A (en) * | 2022-06-28 | 2022-09-16 | 长安大学 | MCo 2 O 4 /MgO/BiVO 4 Composite photoelectric catalytic material and preparation method and application thereof |
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| CN107099818A (en) * | 2017-04-27 | 2017-08-29 | 西北师范大学 | The preparation and application of Ferrite/pucherite composite |
| CN108615616A (en) * | 2018-03-15 | 2018-10-02 | 江苏大学 | The Ni-based load ZnCo of hydro-thermal method synthetic foam2O4/ZnWO4Composite material and its application |
| CN108842169A (en) * | 2018-07-02 | 2018-11-20 | 西北师范大学 | A kind of metal oxide-loaded pucherite composite material and its preparation and application |
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| CN107099818A (en) * | 2017-04-27 | 2017-08-29 | 西北师范大学 | The preparation and application of Ferrite/pucherite composite |
| CN108615616A (en) * | 2018-03-15 | 2018-10-02 | 江苏大学 | The Ni-based load ZnCo of hydro-thermal method synthetic foam2O4/ZnWO4Composite material and its application |
| CN108842169A (en) * | 2018-07-02 | 2018-11-20 | 西北师范大学 | A kind of metal oxide-loaded pucherite composite material and its preparation and application |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110923747A (en) * | 2019-12-09 | 2020-03-27 | 中国石油大学(华东) | Preparation method of bismuth ferrite photocatalytic film electrodeposition |
| CN112410819A (en) * | 2020-11-10 | 2021-02-26 | 北京化工大学 | Composite bismuth-based photoanode for photoelectrocatalytic decomposition of water and preparation method thereof |
| CN115055189A (en) * | 2022-06-28 | 2022-09-16 | 长安大学 | MCo 2 O 4 /MgO/BiVO 4 Composite photoelectric catalytic material and preparation method and application thereof |
| CN115055189B (en) * | 2022-06-28 | 2023-08-08 | 长安大学 | MCo 2 O 4 /MgO/BiVO 4 Composite photoelectric catalytic material and preparation method and application thereof |
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Application publication date: 20190621 |