CN107841763B - A kind of optoelectronic pole and preparation method thereof based on the regulation of surface hydrogen-oxygen shell - Google Patents
A kind of optoelectronic pole and preparation method thereof based on the regulation of surface hydrogen-oxygen shell Download PDFInfo
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- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
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- C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
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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
- 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
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- C25B1/00—Electrolytic production of inorganic compounds or non-metals
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- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
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- 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
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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
- 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
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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
Abstract
The invention discloses a kind of optoelectronic poles and preparation method thereof based on the regulation of surface hydrogen-oxygen shell, belong to inorganic photovoltaic pole field of material preparation.The present invention chooses FTO, ITO, the conductive materials such as sheet metal are used as electrode basement, pass through hydro-thermal method, electrochemical deposition, the nano structure membrane of the methods of spin coating lifting growth even compact and well-crystallized, pass through vacuum, inertia or reducing atmosphere calcining introduce Lacking oxygen defect in the electrodes, and the depth distribution regulation of defect is further realized using the electrochemical treatments under light irradiation, finally the processing of electrode surface electroreduction is carried out using electrode system, collaboration plays the surface promoting catalysis of Lacking oxygen layer the separation charge and hydride layer of depth distribution, obtain the raising of electrode photo electrocatalysis activity and operation stability.Electrode photo electrocatalysis activity prepared by the present invention is high, at low cost, is easily achieved stable operation in cycle period, is expected to produce the fields such as new energy in environment remediation and decomposition water and applied.
Description
Technical field
The present invention relates to inorganic photovoltaic pole material and its fabricating technologies, specially a kind of to be based on surface hydrogen-oxygen shell
Photoelectrocatalysielectrode electrode of regulation and preparation method thereof.
Background technique
On the one hand photo-electrocatalytic technology can convert highdensity Hydrogen Energy for the solar energy of low-density, on the other hand may be used
To realize the redox removal of pollutant, therefore in photo-reduction hydrogen production by water decomposition, heavy metal contaminants reduction and organic contamination
The fields such as object oxidative degradation all have important application prospect.
Since raw material is easy to get, stable structure, the metal oxide semiconductors such as titanium oxide, tungsten oxide, iron oxide are standby
A kind of optoelectronic pole material to attract attention, however Carrier recombination is still to restrict its photoelectrocatalysis efficiency, be unable to satisfy and answer on a large scale
With the fundamental factor of demand.
So far, including the multiple technologies such as dye sensitization, heterojunction structure be compound, metal or nonmetal doping are used to
Improve oxide optoelectronic pole photoelectrochemical behaviour.Optoelectronic pole photoelectrocatalysis efficiency is mainly by photochemical catalyst and co-catalyst structure
Influence.With the further investigation to photoelectrocatalysis micro interface mechanism, it has recently been found that photocatalyst surface Lacking oxygen defect is led
Cause high conductivity amorphous shell to be formed, the process for reducing recombination rate inside optoelectronic pole space charge layer, extend electronics with
The service life in hole have great influence [Science, 2011,331,746；Nano Lett.,2016,16,5751].Currently, table
Face promoting catalysis mainly passes through further load NiOOH, IrOx, RuOx, CoOx etc. and realizes that light induced electron/hole is quick
Capture and redox utilize, but still are faced with the problems such as preparation process is complicated, Load Balanced is difficult to control.For how
Control defect density and distribution etc. obtain efficiently separating utilization, how realizing Lacking oxygen layer and co-catalyst association for photogenerated charge
How same-action is further simplified photoelectrocatalysielectrode electrode preparation method etc. and even recognizes by the reconstruct of material microstructure itself
It is insufficient.
Therefore, it is necessary to one kind efficiency light only can be realized by the regulation of photoelectrocatalysimaterial material micro-interface hydrogen-oxygen shell
The effective ways of electrocatalytic reaction.
Summary of the invention
The object of the invention is intended to ask for existing optoelectronic pole photo-generated carrier utilization efficiency during photoelectrocatalysis is low
Topic provides a kind of simple process, easy to operate photoelectrocatalysielectrode electrode and its preparation side based on the regulation of surface hydrogen-oxygen shell
Method can effectively improve optoelectronic pole photoelectric catalytically active.Optoelectronic pole prepared by the present invention is by tungsten oxide, titanium oxide, oxidation
Iron, pucherite etc. are the nanometer semiconductor structure of composition, can be used for the fields such as environment remediation, cracking aquatic products hydrogen.
The technical solution adopted by the present invention to solve the technical problems are as follows:
A kind of optoelectronic pole preparation method based on the regulation of surface hydrogen-oxygen shell, comprising the following steps:
Step 1: the preparation of sull: by nano thin-film preparation method using conductive material as the electrode of substrate
Substrate surface growing oxide film；
Step 2: in electrode Lacking oxygen defect generate: under vacuum, inertia or reducing gas atmosphere to sull into
Row high temperature reduction；
Step 3: electrode Lacking oxygen depth of defect distribution regulation under photoelectric action: being existed using two electrodes or three-electrode system
The Lacking oxygen depth of defect that sull is carried out under radiation source is distributed regulation, applies a timing to prepared optoelectronic pole
Between voltage carry out Lacking oxygen reformation；
Step 4: electrode surface hydride layer generates: applying the electricity of certain time to the optoelectronic pole after the regulation of Lacking oxygen defect
Pressure carries out surface reduction processing, and the photoelectrocatalysis efficiency of electrode is improved using the hydride layer that material surface generates as co-catalyst,
Obtain the optoelectronic pole material regulated and controled based on surface hydrogen-oxygen shell.
As an improvement of the above technical solution, in step 1, the nano thin-film preparation method includes hydro-thermal method, electrochemistry
Oxidation, electrochemical deposition, chemical vapor deposition, spin coating, lifting and other oxide nano-film preparation methods.
As an improvement of the above technical solution, in step 1, the nano thin-film preparation method further includes to electrode basement
The multiple growth of surface growing oxide film progress, surface modification, high-temperature calcination method, to obtain even compact and crystallization
The good nanostructure of property.
As an improvement of the above technical solution, in step 1, the conductive material is electro-conductive glass or sheet metal.
As an improvement of the above technical solution, the conductive material sufficiently cleans it before being used as electrode basement
Processing is to remove surface oxide layer, organic adsorbents.
As an improvement of the above technical solution, in step 2, the high temperature reduction includes using N under high temperature environment2、
Ar、H2Or the gaseous mixture of above several gases, high-temperature calcination is carried out to sull, wherein the gas under the hot environment
Body flow is 10~200sccm, and temperature is 300~500 DEG C, and normal pressure annealing time is 0.5~48 hour.
As an improvement of the above technical solution, in step 3, the radiation source is Xe lamp or high pressure Hg lamp.
As an improvement of the above technical solution, in step 3, to the voltage for the certain time that prepared optoelectronic pole applies
For 1.5~2.5V vs.RHE, the time is 2~24 hours.
As an improvement of the above technical solution, in step 4, the optoelectronic pole after the regulation of Lacking oxygen defect is applied certain
The voltage of time is -0.8V~0.1V vs.RHE, and the time is 10~7200 seconds.
A kind of optoelectronic pole based on the regulation of surface hydrogen-oxygen shell, the optoelectronic pole use any of above-mentioned each technical solution
Item method is prepared.
Bring beneficial effect of the present invention has:
The effect of aquatic products oxygen and degradable organic pollutant is decomposed by comparing photoelectric current, photoelectrocatalysis, it is prepared by the present invention
The photoelectric catalytically active that surface hydrogen-oxygen shell regulates and controls optoelectronic pole is much higher than native oxide optoelectronic pole, and stability obtains
Very big raising, it is easy to accomplish stable operation in cycle period is expected to produce the fields such as new energy in environment remediation and decomposition water
It is applied.
Experimental facilities needed for preparation method of the invention is simple, and operating condition is mild, simple and easy to do, negative without noble metal
Surface promoting catalysis can be realized in load, considerably reduces Electrode treatment cost.
Detailed description of the invention
With reference to the accompanying drawing and specific embodiment the invention will be further described,
Fig. 1 be in embodiment 1 tungsten oxide optoelectronic pole Lacking oxygen generate and depth distribution regulation before high-resolution-ration transmission electric-lens
Photo；
Fig. 2 be in embodiment 1 tungsten oxide optoelectronic pole Lacking oxygen generate and depth distribution regulation after high-resolution-ration transmission electric-lens
Photo；
Fig. 3 is the XPS O 1s spectrum detection that tungsten oxide optoelectronic pole electroreduction front and rear surfaces hydrogenation structure is formed in embodiment 2
As a result；
Fig. 4 be original tungsten oxide in embodiment 1,2,3, the tungsten oxide of Lacking oxygen defect, Lacking oxygen depth regulation oxidation
Photocurrent curve of tungsten oxide optoelectronic pole under the conditions of AM1.5 simulated solar irradiation after tungsten and the regulation of surface hydrogen-oxygen；
Fig. 5 be original titanium oxide in embodiment 4, the titanium oxide of Lacking oxygen defect, Lacking oxygen depth regulation titanium oxide with
And photocurrent curve under the conditions of AM1.5 simulated solar irradiation of the photocatalytic titanium oxide electrode after the regulation of surface hydrogen-oxygen；
Fig. 6 is surface hydrogen-oxygen regulation tungsten oxide optoelectronic pole under AM1.5 simulated solar irradiation, 1.23V vs.RHE voltage
Current versus time curve.
Specific embodiment
Embodiment 1:
A kind of tungsten oxide optoelectronic pole material and preparation method thereof with surface hydriding amorphous layer, this method includes following
Step:
Step 1: using metal leaf as the base material of optoelectronic pole, it is small that it being cleaned by ultrasonic to 1 in 1M NaOH first
When to remove surface oxides, be then successively cleaned by ultrasonic 15 minutes in water, ethyl alcohol, acetone, ethyl alcohol, water, N2Dry up standby
With.
Step 2: growing tungsten oxide nano structure membrane, hydrothermal growth reaction solution on tungsten surface using hydrothermal method
Group becomes the mixed aqueous solution of 1mol/L nitric acid and 4mol/L hydrochloric acid, and the leaf growth after surface treatment is tiltedly placed on down
In reaction kettle, hydro-thermal reaction liquid is added, hydrothermal growth 3 hours under the conditions of 80 DEG C are cooled to room temperature taking-up tungsten to reaction solution
Piece is rinsed well with water, obtains the leaf of surface growth wolframic acid.
Step 3: the leaf of surface growth wolframic acid is placed in Muffle furnace and is annealed, 500 DEG C of temperature, annealing time 2 hours,
5 DEG C/min of heating rate obtains the electrode material that the growth of leaf surface has tungsten oxide nano structure membrane.
Step 4: the leaf for growing tungsten oxide being placed in the reduction of tube furnace high temperature, holding reducing atmosphere is Ar gas, gas
Flow 100sccm, 350 DEG C of annealing temperature, annealing time 1 hour, 5 DEG C/min of heating rate, obtaining had Lacking oxygen defect
Tungsten oxide optoelectronic pole material.
Step 5: in the sodium sulphate electrolyte of 0.2M, using Ag/AgCl as reference electrode, platinum filament is used as to electrode, oxidation
Tungsten nano thin-film applies the voltage of 2V vs.RHE to oxidation tungsten electrode as working electrode, while using Xe lamp source to electricity
Pole applies irradiation, and being kept for the electrode system processing time is 3 hours, obtains the tungsten oxide light of electrode Lacking oxygen depth distribution reconstruct
Electrode material, Fig. 1 and Fig. 2 are the high-resolution-ration transmission electric-lens of the generation of tungsten oxide optoelectronic pole Lacking oxygen and depth distribution regulation front and back
Photo, adjustment (arrow signal lattice defect) is repaired and be distributed to Lacking oxygen after showing regulation.
Step 6: in the sodium sulphate electrolyte of 0.2M, using Ag/AgCl as reference electrode, platinum filament is used as to electrode, oxidation
Tungsten nano thin-film carries out electrochemical reduction processing as working electrode, to the voltage of oxidation tungsten electrode application -0.2V vs.RHE,
It is kept for 30 seconds, obtains the tungsten oxide optoelectronic pole material with surface hydriding amorphous layer.
Embodiment 2:
A kind of tungsten oxide optoelectronic pole material and preparation method thereof with surface hydriding amorphous layer, this method includes following
Step:
Step 1: with (1) step in embodiment 1.
Step 2: with (2) step in embodiment 1.
Step 3: with (3) step in embodiment 1.
Step 4: the leaf for growing tungsten oxide being placed in the reduction of tube furnace high temperature, holding reducing atmosphere is H2Gas, gas
Flow 100sccm, 350 DEG C of annealing temperature, annealing time 1 hour, 5 DEG C/min of heating rate, obtaining had Lacking oxygen defect
Tungsten oxide optoelectronic pole material.
Step 5: with (5) step in embodiment 1.
Step 6: with (6) step in embodiment 1, Fig. 3 is that tungsten oxide optoelectronic pole electroreduction front and rear surfaces hydrogenation structure is formed
XPS testing result, show that hydroxy radical content contained by tungsten oxide surface dramatically increases after electroreduction.
Embodiment 3:
A kind of photocatalytic titanium oxide electrode material and preparation method thereof with the regulation of surface hydrogen-oxygen shell, this method include with
Lower step:
Step 1: using FTO electro-conductive glass as the base material of optoelectronic pole, successively in water, ethyl alcohol, acetone, ethyl alcohol, water
Ultrasonic cleaning 15 minutes, N2It is spare after drying.
Step 2: growing titanium oxide nano structure membrane, hydrothermal growth reaction solution composition on the surface FTO using hydrothermal method
For the mixed aqueous solution of 6mol/L hydrochloric acid and 0.06mol/L butyl titanate, the FTO after surface treatment is faced into oblique be placed on
In reaction kettle, hydro-thermal reaction liquid is added, hydrothermal growth 5 hours under the conditions of 150 DEG C are cooled to room temperature to reaction solution and take out FTO
Electro-conductive glass is rinsed well with water, obtains the FTO electro-conductive glass of surface growth metatitanic acid.
Step 3: the FTO electro-conductive glass of surface growth metatitanic acid is placed in Muffle furnace and is annealed, 500 DEG C of temperature, annealing time
2 hours, 5 DEG C/min of heating rate, obtain the electrode material that the growth of the surface FTO has titanium oxide nano structure membrane.
Step 4: the FTO electro-conductive glass for growing titanium oxide being placed in the reduction of tube furnace high temperature, holding reducing atmosphere is Ar
Gas, gas flow 100sccm, 350 DEG C of annealing temperature, annealing time 1 hour, 5 DEG C/min of heating rate, obtaining had oxygen empty
The photocatalytic titanium oxide electrode material of position defect.
Step 5: in the NaOH electrolyte of 1M, using Ag/AgCl as reference electrode, platinum filament is used as to electrode, oxidation
Titanium nano thin-film applies the voltage of 1.5V vs.RHE to Titanium oxide electrode as working electrode, while using light source to electrode
Apply irradiation, being kept for the electrode system processing time is 3 hours, obtains the titanium oxide photoelectricity of electrode Lacking oxygen depth distribution reconstruct
Pole material.
Step 6: in the sulfuric acid electrolyte of 0.5M, using Ag/AgCl as reference electrode, platinum filament is used as to electrode, titanium oxide
Nano thin-film carries out electrochemical reduction processing as working electrode, to the voltage of Titanium oxide electrode application -0.6V vs.RHE, protects
It holds 30 seconds, obtains the photocatalytic titanium oxide electrode material with the regulation of surface hydrogen-oxygen shell.
Embodiment 4:
A kind of photocatalytic titanium oxide electrode material and preparation method thereof with the regulation of surface hydrogen-oxygen shell, this method include with
Lower step:
Step 1: with (1) step in embodiment 3.
Step 2: with (2) step in embodiment 3.
Step 3: with (3) step in embodiment 3.
Step 4: the FTO electro-conductive glass for growing titanium oxide being placed in the reduction of tube furnace high temperature, holding reducing atmosphere is H2
Gas, gas flow 100sccm, 350 DEG C of annealing temperature, annealing time 1 hour, 5 DEG C/min of heating rate, obtaining had oxygen empty
The photocatalytic titanium oxide electrode material of position defect.
Step 5: with (5) step in embodiment 3.
Step 6: with (6) step in embodiment 3.
Embodiment 5:
Photoelectrolysis water experiment of the invention: in order to prove that hydrogen-oxygen shell regulation in surface proposes electrode photo electrocatalysis performance
Effect is risen, the present invention is simulated the experiment of photoelectric decomposition water oxygen producing under sunlight conditions.
Experiment is using 0.2M sodium sulphate as electrolyte, and using Ag/AgCl as reference electrode, platinum filament is used as to electrode, different surfaces
For the tungsten oxide nanometer thin film of structure as working electrode, light source intensity calibration is AM1.5 (100mW/cm2), in electrochemical operation
By linear volt-ampere curve test evaluation electrode photo electrocatalysis activity on standing, pass through the when m- electricity under 1.23Vvs.RHE voltage
Flow curve evaluates electrode job stability.
It is handled it can be seen from Fig. 4 and Fig. 5 by the regulation of Lacking oxygen depth distribution and surface reduction hydride layer, electrode light
Electrolysis water efficiency obtains nearly 5 times of raising compared with native oxide, while as seen from Figure 6, electrode after the regulation of surface hydrogen-oxygen
Multicycle stable operation can be realized by simple operations, have good stability, and through simple process after operation a period of time
Restore surface texture.
Above describe a variety of different embodiments of the invention, it is obvious to a person skilled in the art that of the invention
It is not limited to the details of above-mentioned exemplary embodiment, the above is only a preferred embodiment of the present invention, should not be construed as limiting
Fixed practical range of the invention.Any changes and modifications in accordance with the scope of the present application should still belong to this hair
Within bright patent covering scope.
Although not each embodiment only includes one simultaneously it should be appreciated that this specification is described according to embodiment
This narrating mode of independent technical solution, this specification is merely for the sake of clarity, and those skilled in the art should will say
As a whole, the technical solutions in the various embodiments may also be suitably combined for bright book, and forming those skilled in the art can be with
The other embodiments of understanding.
Claims (8)
1. a kind of optoelectronic pole preparation method based on the regulation of surface hydrogen-oxygen shell, it is characterised in that: the following steps are included:
Step 1: the preparation of sull: by nano thin-film preparation method using conductive material as the electrode basement table of substrate
Face growing oxide film；
Step 2: Lacking oxygen defect generates in electrode: carrying out under vacuum, inertia or reducing gas atmosphere to sull high
Temperature reduction；
Step 3: electrode Lacking oxygen depth of defect distribution regulation under photoelectric action: using two electrodes or three-electrode system in exposure light
The Lacking oxygen depth of defect that sull is carried out under source is distributed regulation, applies the voltage of certain time to prepared optoelectronic pole
Lacking oxygen reformation is carried out, the voltage to the certain time that prepared optoelectronic pole applies is 1.5~2.5V vs.RHE, time 2
~24 hours；
Step 4: electrode surface hydride layer generates: the voltage for applying certain time to the optoelectronic pole after the regulation of Lacking oxygen defect carries out
Surface reduction processing, the voltage to the certain time that the optoelectronic pole after the regulation of Lacking oxygen defect applies are -0.8V~0.1V
Vs.RHE, time are 10~7200 seconds, and the photoelectrocatalysis of electrode is improved using the hydride layer that material surface generates as co-catalyst
Efficiency obtains the optoelectronic pole material regulated and controled based on surface hydrogen-oxygen shell.
2. a kind of optoelectronic pole preparation method based on the regulation of surface hydrogen-oxygen shell according to claim 1, it is characterised in that:
In step 1, the nano thin-film preparation method includes hydro-thermal method, electrochemical oxidation, electrochemical deposition, chemical vapor deposition, rotation
Painting, lifting and other oxide nano-film preparation methods.
3. a kind of optoelectronic pole preparation method based on the regulation of surface hydrogen-oxygen shell according to claim 2, it is characterised in that:
In step 1, the nano thin-film preparation method further include to electrode basement surface growing oxide film carry out it is multiple grow,
Surface modification, high-temperature calcination method, to obtain even compact and the good nanostructure of crystallinity.
4. a kind of optoelectronic pole preparation method based on the regulation of surface hydrogen-oxygen shell according to claim 3, it is characterised in that:
In step 1, the conductive material is electro-conductive glass or sheet metal.
5. a kind of optoelectronic pole preparation method based on the regulation of surface hydrogen-oxygen shell according to claim 4, it is characterised in that:
The conductive material carries out abundant cleaning treatment to it before being used as electrode basement to remove surface oxide layer, organic adsorbents.
6. a kind of optoelectronic pole preparation method based on the regulation of surface hydrogen-oxygen shell according to claim 1, it is characterised in that:
In step 2, the high temperature reduction includes using N under high temperature environment2、Ar、H2Or the gaseous mixture of above several gases, to oxidation
Object film carries out high-temperature calcination, wherein the gas flow under the hot environment is 10~200sccm, temperature is 300~500
DEG C, normal pressure annealing time is 0.5~48 hour.
7. a kind of optoelectronic pole preparation method based on the regulation of surface hydrogen-oxygen shell according to claim 1, it is characterised in that:
In step 3, the radiation source is Xe lamp or high pressure Hg lamp.
8. a kind of optoelectronic pole based on the regulation of surface hydrogen-oxygen shell, it is characterised in that: the optoelectronic pole uses claim 1~7
Any one method is prepared.
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