CN106222685A - A kind of WO of photoelectrocatalysis water decomposition3the preparation method of LDH laminated film - Google Patents
A kind of WO of photoelectrocatalysis water decomposition3the preparation method of LDH laminated film Download PDFInfo
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- CN106222685A CN106222685A CN201610698073.1A CN201610698073A CN106222685A CN 106222685 A CN106222685 A CN 106222685A CN 201610698073 A CN201610698073 A CN 201610698073A CN 106222685 A CN106222685 A CN 106222685A
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- 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
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- C—CHEMISTRY; METALLURGY
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- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B9/00—Cells or assemblies of cells; Constructional parts of cells; Assemblies of constructional parts, e.g. electrode-diaphragm assemblies; Process-related cell features
- C25B9/70—Assemblies comprising two or more cells
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
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- C25B1/55—Photoelectrolysis
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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
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Abstract
The present invention relates to the WO of a kind of photoelectrocatalysis water decomposition3LDH(Layered double hydroxide, layered double-hydroxide) preparation method of laminated film, comprise the steps of soluble in water to ammonium tungstate and concentrated hydrochloric acid, transfer in autoclave liner after stirring, insert electro-conductive glass FTO good for pretreatment, then solvent thermal reaction is carried out, naturally cool to room temperature, by electro-conductive glass washing, after drying, in air atmosphere, 450 550 DEG C of heat treatment at least 1 h, obtain WO3Thin film；Again with WO3Thin film be the aqueous solution of working electrode, nickel nitrate and ferric nitrate be electrolyte, at WO3Film surface galvanostatic deposition NiFe LDH, finally obtains WO3LDH laminated film；The product that the present invention prepares is higher than electricity conversion, and photooxidation water take-off potential is low, has broad application prospects in fields such as photocatalytic degradation, photoelectrocatalysis water decomposition, artificial photosynthesis, light auxiliary energy storage batteries.
Description
Technical field
The present invention relates to field of inorganic nonmetallic material, the WO of a kind of photoelectrocatalysis water decomposition3-LDH
The preparation method of (Layered double hydroxide) laminated film.
Background technology
Last century 70, increasing environmental pollution and energy shortage problem have allowed it was recognized that the two is dived
Global crisis.For the sustainable development of human society, the pollution-free technology of development environment close friend and alternative cleaning
The energy is extremely the most urgent.Among numerous environmental protections and renewable energy source item, utilize the quasiconductor of natural daylight energy
Photocatalysis technology has become one of the most promising technology.1972, Japanese scholars Fujishima and Honda reported first
At TiO2Research [the A. Fujishima and K. Honda. Photolysis-of electrode surface photoelectric decomposition water
decomposition of water at the surface of an irradiated semiconductor. Nature,
1972,238,37-38.], this is considered to have the event of milestone significance, has greatly promoted and has urged based on photocatalysis/photoelectricity
The research of the light energy switch technology of change technology.Unfortunately, the forbidden band of titanium dioxide is wider (3-3.2 eV), and can utilize arrives
Reach the solar energy of earth surface less than 5%(ultraviolet light, λ < 400 nm) so that it is preferable catalysis material can not be become.At present,
Numerous studies all concentrate on to respond at visible light wave range (400 < λ < 800 nm) and have the narrow band gap of highlight catalytic active and partly lead
[A. B. Murphy, P. R. F. Barnes, L. K. Randeniya, I. C. Plumb, I. E. on body material
Grey, M. D. Horne and J. A. Glasscock. Efficiency of solar water splitting
using semiconductor electrodes. Int. J. Hydrogen Energy, 2006, 31, 1999-
2017.], such as WO3、Fe2O3、BiVO4Deng oxide, CdS, Cu2ZnSnS4Sulfides, the nitrogen oxides such as TaON, ZnGaON, with
And nonmetallic compound g-C3N4.
WO3It is a kind of N-shaped semiconductor material with wide forbidden band with good physical and chemical stability, by filling up the low of electronics
Can valence band (valence band, VB) and empty higher energy conduction band (conduction band, CB) composition.With other photocatalyst
Comparing, the energy gap of Tungstic anhydride. is narrower, can have preferably absorption at visible-range, can well utilize in sunlight
Visible ray resource.If but only use Tungstic anhydride. quasiconductor, exist easily by photoetch, photo-catalysis capability instability
Etc. defect, so this area expands substantial amounts of research around how improving Tungstic anhydride. photo-catalysis capability, it is proposed that many changes
Property means, reduce its energy gap with this, increase the ability of strong light absorption, also to promote its light induced electron and hole simultaneously
Separation efficiency, reduces the combined efficiency of electronics and hole, promotes catalytic capability.Common method has WO3With other quasiconductor
Material (TiO2、ZnO、BiVO4) be combined, but these methods all can not reduce WO3The overpotential of light electroxidation water.
Layered double-hydroxide LDH(Layered double hydroxide) be a kind of moisture resolve oxygen co-catalysis
Agent, can effectively reduce the overpotential of analysis oxygen, can constitute hetero-junctions with other semi-conducting materials the most again thus improve electronics
The separating power in hole.At present, WO is utilized3Formation WO is combined with layered double-hydroxide LDH3The skill of-LDH laminated film
Art, there is not been reported.
Summary of the invention
For the problems referred to above, the present invention provides one to have efficient photoelectricity treater catalytic water capacity of decomposition WO3-LDH(Layered
Double hydroxide) preparation method of laminated film, the method is achieved in that
(1) take the tungstic acid that mass fraction is 0.017 g/ml, regulate pH=1, be placed in 40 DEG C of environment stir to being formed colourless
Clear solution, is then transferred in the polytetrafluoroethyllining lining of autoclave；
(2) by FTO electro-conductive glass oblique cutting good for pretreatment in inner liner of reaction kettle, solution did not had glass, and conducting surface is downward；
(3) it is tamping reactor to put into baking oven carries out solvent thermal reaction, be placed in 160 ~ 200 DEG C of environment and react at least 1h, from
So it is cooled to room temperature；Take out FTO electro-conductive glass, be dried with after deionized water, absolute ethanol washing 40 ~ 100 DEG C successively, obtain light greenish blue
Color thin film；
(4) by electro-conductive glass under air atmosphere is protected, it is placed in heat treatment at least 1h in 450 ~ 550 DEG C of environment, it is thus achieved that long have WO3
FTO electro-conductive glass；
(5) three-electrode system is used, with WO3Thin film be the aqueous solution of working electrode, nickel nitrate and ferric nitrate be electrolyte,
WO3Film surface galvanostatic deposition NiFe-LDH, is passed through constant current-0.10 mA/cm2, electro-deposition 50 ~ 400 s, i.e. obtain WO3-
LDH laminated film.
Further, the WO of photoelectrocatalysis water decomposition of the present invention3In the preparation method of-LDH laminated film, pretreatment
Step is: electro-conductive glass is cut into the small pieces of 3 cm x 1.5 cm, uses acetone, deionized water, dehydrated alcohol ultrasonic clearly respectively
Wash (power of ultrasonic cleaning is 100 W) 30 min, and cleaned electro-conductive glass is placed in dehydrated alcohol preservation, before using
Dry up with hair-dryer.
Further, the WO of photoelectrocatalysis water decomposition of the present invention3In the preparation method of-LDH laminated film, step
(5) aqueous solution of described nickel nitrate and ferric nitrate obtains by the following method: by 2.181 g Ni (NO3)2·6H2O and
1.784 g Fe(NO3)3·9H2O adds in 100mL water, i.e. obtains described solution.
Further, the WO of photoelectrocatalysis water decomposition of the present invention3In the preparation method of-LDH laminated film, step
(1) described regulation pH=1, refers to that the HCl solution so that concentration is 6 mol/L regulates pH=1.
Further, the WO of photoelectrocatalysis water decomposition of the present invention3In the preparation method of-LDH laminated film, step
(5) described three-electrode system refers to, has WO with long3FTO electro-conductive glass be working electrode, Pt sheet is to electrode, saturated calomel
The system that electrode is formed by reference electrode.
The present invention is by WO3Formation WO is combined with layered double-hydroxide LDH3-LDH laminated film, light induced electron is with empty
The separation efficiency in cave is high, and oxygen evolution potential is low, so that its catalytic capability is remarkably enhanced.The WO that the present invention obtains3-
The photooxidation water decomposition electric current density of LDH laminated film is much larger than pure WO3, and take-off potential is lower demonstrate preferably application before
Scape.
Accompanying drawing explanation
Fig. 1 is the WO prepared by the embodiment of the present invention 13The electron scanning micrograph of-LDH laminated film.
Fig. 2 is the WO prepared by the embodiment of the present invention 13The transmission electron microscope photo of-LDH laminated film.
Fig. 3 is the WO prepared by the embodiment of the present invention 13WO prepared by thin film and embodiment 43The XPS of-LDH laminated film
Collection of illustrative plates.
Fig. 4 is the WO prepared by the embodiment of the present invention 13WO prepared by thin film and embodiment 43The light of-LDH laminated film
Current curve.
Fig. 5 is the WO prepared by the embodiment of the present invention 43The electron scanning micrograph of thin film.
Fig. 6 is the pure WO not depositing LDH3The electron scanning micrograph of thin film.
Detailed description of the invention
Embodiment relates to reagent and equipment source:
Ammonium tungstate, analytical pure AR, purchased from Chemical Reagent Co., Ltd., Sinopharm Group；
Acetone, dehydrated alcohol, hydrochloric acid, six water nickel nitrates, nine water ferric nitrates and anhydrous sodium sulfate are analytical pure AR, purchased from Nanjing
Chemical reagent company limited；
FTO electro-conductive glass: Pilkington product, thickness 2.2mm, resistance 7 ohm, light transmittance 80%；
Autoclave: in triumphant sub-KH-50, enclosure material is 304 rustless steels, and inner bag is politef；
Electrochemical workstation: Shanghai Chen Hua Instrument Ltd., CHI660A；
Scanning electron microscope: Japan Hitachi company S-4800, accelerating potential is 10kV；
Transmission electron microscope: FEI company's T ecnai G2, accelerating potential is 200kV；
X-ray photoelectron power spectrum (XPS): PHI 5000 VersaProbe electron spectrometer.
Described in embodiment, pretreated FTO electro-conductive glass is obtained by: FTO electro-conductive glass is cut out 3 cm x
The small pieces of 1.5 cm, use acetone, deionized water and dehydrated alcohol ultrasonic cleaning FTO electro-conductive glass 30min(ultrasonic cleaning respectively
Power is 100 W), the FTO electro-conductive glass after cleaning is placed in dehydrated alcohol preservation, uses front hair dryer (about 60 ~ 80
DEG C) dry up.
Embodiment 1
(1) ammonium tungstate weighing 0.5 g is dissolved in 30 ml water, with 6 mol/L HCl solution regulation pH value of solution=1, at 40 DEG C
Solution, until forming colourless transparent solution, is transferred in the polytetrafluoroethyllining lining of 50 ml autoclaves by stirring afterwards；
(2) by pretreated FTO electro-conductive glass sheet oblique cutting inside inner liner of reaction kettle, make conducting surface down；
(3) reactor is sealed tightly put into baking oven carries out solvent thermal reaction, 180 DEG C of thermal response 5 h, naturally cool to room temperature,
By electro-conductive glass through deionized water, absolute ethanol washing dried in 40 DEG C, obtain nattierblue thin film；
(4) there is the electro-conductive glass of thin film under air atmosphere is protected by long, 500 DEG C of isothermal holding 2 h, obtain the WO of yellow3Thin
Film.
(5) three-electrode system is used, specific as follows: long have WO3FTO electro-conductive glass be working electrode, Pt sheet is to electricity
Pole, saturated calomel electrode are reference electrode, and electrolyte contains 2.181 g Ni (NO3)2·6H2O and 1.784 g Fe (NO3)3·
9H2O, and 100 mL water, at WO3Film surface is with-0.10 mA/cm2Electric current density galvanostatic deposition NiFe-LDH, electricity is heavy
The long-pending time is that 200 s finally obtain WO3-LDH laminated film.
The WO that the present embodiment obtains3-LDH laminated film stereoscan photograph is shown in Fig. 1, it is seen that the WO of preparation3-LDH THIN COMPOSITE
Film is by bar-shaped WO3Granule and lamellar LDH composition.
This laminated film transmission electron microscope is shown in Fig. 2, and as shown in Figure 2, the product of synthesis is for crystallizing good WO3With covering at table
The LDH material composition in face.
The Elemental redistribution of this laminated film constituency scanning electron microscope is as it is shown on figure 3, in Fig. 3, A is the shape of the embodiment 1 chosen
Looks figure, B-E is respectively the scattergram of this region W, O, Ni, Fe element, it is seen that element W, O, Fe, Ni are evenly distributed in thin film
In.
Embodiment 2
(1) ammonium tungstate weighing 0.5 g is dissolved in 30 ml water, with the pH=1 of 6 mol/L HCl regulation solution, stirs at 40 DEG C
Mixing until forming colourless transparent solution, being transferred to afterwards in the polytetrafluoroethyllining lining of 50 ml autoclaves；
(2) by pretreated FTO electro-conductive glass sheet oblique cutting inside inner liner of reaction kettle, make conducting surface down；
(3) reactor is sealed tightly put into baking oven carries out solvent thermal reaction, 160 DEG C of reaction 1 h, naturally cool to room temperature, will
It is dried that electro-conductive glass sequentially passes through deionized water, absolute ethanol washing 60 DEG C, obtains nattierblue thin film；
(4) length of gained has the electro-conductive glass of thin film under air atmosphere is protected, and 450 DEG C of heat treatments are incubated 1 h, obtain yellow
WO3Thin film.
(5) using three-electrode system, long have WO3FTO electro-conductive glass be working electrode, Pt sheet is to electrode, saturated sweet
Mercury electrode is reference electrode, and electrolyte contains 2.181 g Ni (NO3)2·6H2O and 1.784 g Fe (NO3)3·9H2O, and 100
ML water, at WO3Film surface is with-0.10 mA/cm2Electric current density galvanostatic deposition NiFe-LDH, electrodeposition time is 50 s,
Finally obtain WO3-LDH laminated film.
Embodiment 3
(1) ammonium tungstate weighing 0.5 g is dissolved in 30 ml water, with the pH to 1 of 6 mol/L HCl solution regulation solution, at 40 DEG C
Lower stirring, until forming colourless transparent solution, is transferred in the polytetrafluoroethyllining lining of 50 ml autoclaves afterwards；
(2) by pretreated FTO electro-conductive glass sheet oblique cutting inside inner liner of reaction kettle, make conducting surface down；
(3) reactor is sealed tightly put into baking oven carries out solvent thermal reaction, 200 DEG C of reaction 7 h, naturally cool to room temperature, will
Electro-conductive glass is dried through deionized water, absolute ethanol washing 100 DEG C, obtains nattierblue thin film；
(4) length of gained has the electro-conductive glass of thin film under air atmosphere is protected, and 550 DEG C of heat treatments are incubated 2 h, obtain yellow
WO3Thin film.
(5) using three-electrode system, long have WO3FTO electro-conductive glass be working electrode, Pt sheet is to electrode, saturated sweet
Mercury electrode is reference electrode, and electrolyte contains 2.181 g Ni (NO3)2·6H2O and 1.784 g Fe (NO3)3·9H2O, and 100
ML water, at WO3Film surface is with-0.10 mA/cm2Electric current density galvanostatic deposition NiFe-LDH, electrodeposition time is 400
S, finally obtains WO3-LDH laminated film.
Embodiment 4
(1) ammonium tungstate weighing 0.5 g is dissolved in 30 ml water, with the pH to 1 of 6 mol/L HCl solution regulation solution, 40 oC
Lower stirring, until forming colourless transparent solution, is transferred in the polytetrafluoroethyllining lining of 50 ml autoclaves afterwards；
(2) by pretreated electro-conductive glass (FTO) sheet oblique cutting inside inner liner of reaction kettle, make conducting surface down；
(3) reactor is sealed tightly put into baking oven carries out solvent thermal reaction, 180 DEG C of reaction 5 h, naturally cool to room temperature, will
Electro-conductive glass is dried through deionized water, absolute ethanol washing and 80 DEG C, obtains nattierblue thin film；
(4) length of gained has the electro-conductive glass of thin film under air atmosphere is protected, and 500 DEG C of isothermal holding 2 h obtain yellow
WO3Thin film.
The WO that the present embodiment is obtained3Thin film (does not deposits the pure WO of LDH3Thin film) as a comparison sample, its scanning electron microscope shines
Sheet as shown in Figure 6, the WO prepared as seen from Figure 63Thin film is by bar-shaped WO3Granule forms.
The WO that embodiment 1 obtains3The WO that-LDH laminated film and embodiment 4 obtain3The XPS collection of illustrative plates of thin film as shown in Figure 4,
From fig. 4, it can be seen that embodiment 1 product WO3Surface is NiFe-LDH, and the valence state composition of embodiment 4 product is strictly WO3。
The photoelectric current of test product, test method particularly includes: test instrunment is CHI660A electrochemical workstation, three electrodes
Test system is that saturated calomel electrode (SCE) is as reference electrode device, and long have WO using Pt sheet as to electrode3And WO3-LDH's
FTO glass is working electrode, and light passes quartz glass electrolyzer, and from FTO back side vertical irradiation, all test area are fixed on
1cm2, the method for selection linear scanning, sweep interval 0 ~ 1.5V(vs. SCE).Electrolyte uses the Na of 0.2 mol/L2SO4Molten
Liquid, pH value is 6.6, and before test, logical nitrogen half an hour, removes dissolved oxygen.Light source uses the 200W xenon lamp of Newport company,
Additional filter plate (λ > 420 nm).Fig. 5 is the photocurrent curve of embodiment 1 and 4, with pure WO3(embodiment 4) is compared, WO3-LDH
The photooxidation water decomposition electric current density of laminated film (embodiment 1) is much larger than the latter, and take-off potential is lower demonstrates preferably
Application prospect.
The above is only used as presently preferred embodiments of the present invention and application, should not be construed as the restriction of the present invention, all
It is that other pro forma amendments of being made of technological thought based on the present invention, the invention replacing and change and realize belong to this
Bright protection domain.The present invention can be done some changing under the premise of not departing from the present invention for those skilled in the art
Entering and modify, these improve and modification is also considered as protection scope of the present invention.
Claims (5)
1. the WO of a photoelectrocatalysis water decomposition3The preparation method of-LDH laminated film, it is characterised in that specifically comprise the following steps that
(1) take the tungstic acid that mass fraction is 0.017g/ml, regulate pH=1, be placed in 40 DEG C of temperature stir to being formed colourless
Clear solution, is transferred in autoclave；
(2) by pretreated FTO electro-conductive glass oblique cutting in a kettle., it is immersed in the solution that step (1) obtains, conducting surface
Downwards；
(3) reactor is placed in 160 ~ 200 DEG C of environment and reacts at least 1h, be cooled to room temperature；Take out FTO electro-conductive glass, successively
It is dried with after deionized water, absolute ethanol washing 20 ~ 100 DEG C；
(4) electro-conductive glass is placed in heat treatment at least 1h in 450-550 DEG C of temperature, it is thus achieved that long have WO3The FTO electro-conductive glass of thin film；
(5) use three-electrode system, have WO with long3The water that FTO electro-conductive glass is working electrode, nickel nitrate and ferric nitrate of thin film
Solution is electrolyte, at WO3Film surface galvanostatic deposition NiFe-LDH, is passed through constant current-0.10 mA/cm2, electro-deposition 50-
400 s, i.e. obtain WO3-LDH laminated film.
The WO of photoelectrocatalysis water decomposition the most according to claim 13The preparation method of-LDH laminated film, it is characterised in that
Described in step (2), pretreated FTO electro-conductive glass is obtained by: respectively with acetone, deionized water and dehydrated alcohol
Ultrasonic cleaning FTO electro-conductive glass 30min, the FTO electro-conductive glass after cleaning is placed in dehydrated alcohol preservation, dries up before using.
The WO of photoelectrocatalysis water decomposition the most according to claim 23The preparation method of-LDH laminated film, it is characterised in that
The aqueous solution of step (5) described nickel nitrate and ferric nitrate is obtained by: by 2.181 g Ni (NO3)2·6H2O and 1.784
g Fe(NO3)3·9H2O adds in 100mL water, i.e. obtains described solution.
The WO of photoelectrocatalysis water decomposition the most according to claim 33The preparation method of-LDH laminated film, it is characterised in that
Step (1) described regulation pH=1 refers to that the HCl so that concentration is 6 mol/L regulates pH value of solution=1.
5. according to the WO of one of claim 1-4 described photoelectrocatalysis water decomposition3The preparation method of-LDH laminated film, it is special
Levying and be, step (5) described three-electrode system refers to, has WO with long3The FTO electro-conductive glass of thin film is working electrode, and Pt sheet is
The system that electrode, saturated calomel electrode are formed by reference electrode.
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