CN108642512A - Photoelectrochemical cell optoelectronic pole and its preparation and processing method - Google Patents
Photoelectrochemical cell optoelectronic pole and its preparation and processing method Download PDFInfo
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- CN108642512A CN108642512A CN201810415198.8A CN201810415198A CN108642512A CN 108642512 A CN108642512 A CN 108642512A CN 201810415198 A CN201810415198 A CN 201810415198A CN 108642512 A CN108642512 A CN 108642512A
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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
- C25B1/01—Products
- C25B1/02—Hydrogen or oxygen
- C25B1/04—Hydrogen or oxygen by electrolysis of water
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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
- C25B1/50—Processes
- C25B1/55—Photoelectrolysis
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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
- 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
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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
- 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
- C25B11/077—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of a single catalytic element or catalytic compound the compound being a non-noble metal oxide
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M14/00—Electrochemical current or voltage generators not provided for in groups H01M6/00 - H01M12/00; Manufacture thereof
- H01M14/005—Photoelectrochemical storage cells
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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
- 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
- Y02P20/133—Renewable energy sources, e.g. sunlight
Abstract
The invention discloses a kind of processing methods of optical electro-chemistry water decomposition cell photoelectric pole comprising WO3 compacted zones are deposited between conductive substrates and WO3 nano porous layers；WO3 nano porous layers are modified with ammonium metatungstate methanol solution.Treated, and light anode photoelectric current is handle preceding photoelectric current 19 times.Prepared by the light anode of the present invention and processing method process is simple, is conducive to the separation and transmission of charge, can greatly improve electrode performance；This method is economic and environment-friendly, prepared by the large-scale production that can be applied to optoelectronic pole.
Description
Technical field：
The present invention relates to a kind of photoelectrochemical cell optoelectronic pole and its preparation and processing methods, belong to photoelectrochemical cell field skill
Art field.
Background technology：
With the continuous development of society, the increasingly raising of living standards of the people, what is brought is a large amount of consumption and the environment of the energy
Severe exacerbation.Wherein problem of energy crisis is increasingly severe, countries in the world in order to solve this problem all greatly develop it is novel
Using clean energy resource.Solar energy is maximum clean energy resource so far, and the power of solar radiation is 1000 W/m2, annual to irradiate
It is about can consume energy total amount every year 10000 times to tellurian solar energy.Therefore, it is to solve to work as effectively to utilize solar energy
The optimal path of modern society's energy crisis.
However solar cell is exactly that it diurnally generates electric power, therefore, solar cell there are one very big problem
There is still a need for an effective energy storage modes for large-scale application, wherein effective and feasible one of mode is exactly with chemical energy carrier
Storage.Hydrogen is exactly the advantageous competitor of future source of energy carrier, and hydrogen can be generated by water decomposition, and the product after burning is
Water not will produce any pollution.Therefore, using decomposing water with solar energy production hydrogen be the best mode that stores solar energy it
One.Currently, by using the photocatalysis of semi-conducting material, semiconductor is made to the optoelectronic pole of photochemical cell, to utilize
Sunlight provides new approach to decompose water generation hydrogen.
It can effectively make the photoelectric material of the aquatic hydrogen producing of photodegradation that should have following advantages：1, the effective light of strength is inhaled
The property received；2, stabilization can be kept when there is no light chemically；3, suitable conduction band valence band edge positions, are conducive to the oxygen of water
Change reduction；4, the efficient carrier transmission in semiconductor；5, the global voltage transformation in redox reaction is relatively low；6, it is low at
This.But existing semi-conducting material is difficult to meet above-mentioned all advantages simultaneously, thus improve after meeting certain advantages and be left
Aspect for improve photocatalytic water efficiency be particularly important.
In the prior art, it is directed generally to improve the research of light absorption and efficient carrier transmission, the means usually utilized
Have：1, different particles is adulterated to change the band gap of semiconductor；2, suitable nanostructure is designed to shorten diffusion length, thus
The compound of electron hole pair is reduced, such as one-dimentional structure；3, suitable co-catalyst is introduced in semiconductor surface to promote electronics (empty
Cave) it is reacted with electrolyte；4, hetero-junctions is built to inhibit the compound of electron hole pair, accelerates the separation of carrier.Certainly, it removes
Except above-mentioned means, there are many more other means can be used for improving photodegradation water efficiency.
No matter however, by which kind of means, the specific surface area of optoelectronic pole is limited, and it is weaker to fall into photosensitiveness, limits and electrolyte
Contact area, thus photocatalytic water is less efficient.
Being disclosed in the information of the background technology part, it is only intended to increase understanding of the overall background of the invention, without answering
It has been the prior art well known to persons skilled in the art when being considered as recognizing or imply that the information is constituted in any form.
Invention content：
That the purpose of the present invention is to provide a kind of journeys is simple, conducive to charge transmission, improve transfer efficiency and can be applied to advise greatly
The photoelectrochemical cell optoelectronic pole of mould production, further relates to preparation and the post-processing approach of optoelectronic pole, to overcome above-mentioned existing skill
The defects of art.
To achieve the above object, the present invention provides a kind of photoelectrochemical cell optoelectronic pole, including conductive substrates, further include
Sequence is placed in semiconductor compacted zone, nanometer semiconductor structure layer and semiconductor surface decorative layer in the conductive substrates, institute
Semiconductor compacted zone is stated to be made of compacted zone film, it is compound for inhibiting conductive substrates and electrolyte to occur, enhance conductive liner
Bottom is electrically connected with nanostructured layers；The nanometer semiconductor structure layer is made of nanostructure, is extinction main body, is that photoproduction carries
The main source for flowing son, plays a basic role；The finishing coat is made of nano particle, for improving nanostructured layers and electricity
The charge injection efficiency between liquid is solved, is the decorative layer of nanostructured layers.
The technical solution that the present invention further limits is：
Preferably, in above-mentioned technical proposal, semiconductor TiO2, α-Fe2O3, BiVO4, WO3One such or a variety of mixing half
Conductor material.
Preferably, in above-mentioned technical proposal, the conductive substrates are ITO, AZO or FTO conductive films.
Preferably, in above-mentioned technical proposal, the conductive substrates are opaque electrode metal or metal alloy film.
A kind of preparation of the optoelectronic pole of photoelectrochemical cell and processing method, including step：
S1 prepares WO on conductive substrates3Compacted zone；
S2 prepares the WO of nanostructure3Porous layer；
S3 is to WO3Nano porous layer is surface modified.
The technical solution that the present invention further limits is：
Preferably, in above-mentioned technical proposal, WO is formed by following steps in the S13Compacted zone：
Conductive substrates are cleaned by ultrasonic 20 minutes in acetone, absolute ethyl alcohol, deionized water by S1.1 respectively；
S1.2 takes suitable ammonium metawolframate powder with balance, is dissolved in a small amount of deionized water, with ultrasonic oscillation to thoroughly it is molten
Solution, adds suitable methanol solution, it is ensured that the volume that deionized water volume accounts for total solution is no more than 1/4；
S1.3 takes the drop of the solution in 20 μ l steps S1.2 on conductive substrates, 10 s of spin coating under the rotating speed of 2500 rpm, then
Cabinet-type electric furnace is put it into be warming up to 450 DEG C through 1 h and keep 1 h.
Preferably, in above-mentioned technical proposal, WO is formed by following steps in the S23Nano porous layer：
S2.1, which is weighed in the balance, takes 20 mg WO3Powder and 5 mg elemental iodines are put into the beaker of 50 ml（Reaction vessel）, then to
The acetone of 25 ml is added in beaker, then carry out ultrasonic oscillation reasonable time to make its fully dispersed suspension for stable homogeneous
Liquid；
The conducting surface for the conductive substrates that two panels was cleaned is relatively fixed the positive and negative polarities in D.C. regulated power supply by S2.2, it is ensured that it
Between between be divided into 1 cm.It sets the voltage of D.C. regulated power supply to 25 V again, is inserted by working electrode and to electrode
WO3Suspension in, 150 s are electroplated under voltage stabilizing.
Preferably, in above-mentioned technical proposal, by following steps to WO in the step S33Surface is modified：
S3.1 configures the ammonium metatungstate methanol solution of a concentration of 20 mmol/L of tungsten atom, and 20 μ l solution is taken slowly to drop in film
On, it dries at room temperature, repeats this operation 4 times；
Sample is put into cabinet-type electric furnace by S3.2, and arrange parameter makes to be heated to 450 DEG C in its 1 h, and 1h is kept to anneal.
Preferably, in above-mentioned technical proposal, semiconductor compacted zone equably covers conductive substrates, reduces photo-generated carrier
It is compound, preparation method includes but not limited to solution spin-coating method, sputtering method, vapour deposition method；
Nanometer semiconductor structure layer has the diffusion length that few son is reduced by nanostructure, including but not limited to nanometer rods battle array
The nanostructures such as row, nano-chip arrays and nano-porous film；Nanometer semiconductor structure layer, preparation method include but unlimited
In sol-gal process, anodizing, chemical vapour deposition technique, electrochemical deposition method；Semiconductor surface decorative layer, modification side
Method includes but not limited to chemical bath, chemical vapor deposition, atomic layer deposition.
Compared with prior art, the present invention has the advantages that：The nanometer WO prepared using electrophoretic deposition3It is porous
Structure, the short transmission and dissociation for being conducive to lack son of few sub- diffusion length；The WO of preparation3Compacted zone inhibits the compound of interface；
Surface post-processing increases the electrical connection between particle, greatly strengthens the efficiency of photocatalytic water, the photoelectric current under the voltage of 1.0 V
19 times before being increased to, therefore the method for the present invention is to improve the practicable means of photodegradation water efficiency.
Treated that semiconductor photoelectrode can promote hole to react with electrolyte for method through the invention, has
It is detached conducive to electron hole pair is improved；Simultaneously because inhibit conductive substrates with it is compound at semiconductor material interface, improve
To the utilization ratio of light.Compared with conventional semiconductors electrode, the present invention is overcome by the method for adding compacted zone and post-processing
The disadvantages such as semi-conducting electrode carrier mobility is low are effectively improved photocatalytic water efficiency, and the method preparation process of the present invention
Fairly simple, raw material are sufficient, price is low, are conducive to mass produce, and have huge potential using value.
Description of the drawings：
Fig. 1 is light anode structural schematic diagram prepared by the present invention.
Fig. 2 is the current -voltage curve figure of optoelectronic pole in the embodiment of the present invention.
Specific implementation mode：
Below to the present invention specific implementation mode be described in detail, it is to be understood that protection scope of the present invention not by
The limitation of specific implementation mode.
Unless otherwise explicitly stated, otherwise in entire disclosure and claims, term " comprising " or its change
It changes such as "comprising" or " including " etc. and will be understood to comprise stated element or component, and do not exclude other
Element or other component parts.
The method is conventional method unless otherwise instructed.The raw material unless otherwise instructed can be from open business
Approach and obtain, and without further purification processes.
As shown in Figure 1, optical electro-chemistry optoelectronic pole of the present invention, structure include conductive substrates, can be but unlimited
In the ITO on glass substrate or flexible substrate, FTO and AZO transparent conductive film；Semiconductor compacted zone；Semiconductor nano knot
Structure layer and semiconductor decorative layer.
The present invention provides a kind of preparation of optoelectronic pole of photoelectrochemical cell and post-processing approach, which is to pass through
What the method for electrophoretic deposition was prepared.Specific method is first to choose solvent appropriate to be configured to hang by the powder of semi-conducting material
Turbid connects the positive and negative anodes of D.C. regulated power supply, is closing respectively then by the opposite insertion solution of the conducting surface of two pieces of conductive substrates
Plating a period of time can be obtained optoelectronic pole under suitable voltage.In the present invention, the electrode material of preparation electrode is fabricated to make
For the working electrode of photoelectrochemical cell, platinum electrode is used as to electrode, and electrolyte is the sodium sulphate (Na of 1 M2SO4) aqueous solution, i.e.,
It can be assembled into photoelectrochemical cell.
Specific preparation method：
It will be covered with fluorine element doped stannum oxide（FTO）Substrate of glass successively use water-detergent solution, acetone, absolute ethyl alcohol and
After deionized water supersound washing, the ammonium metatungstate solution of a concentration of 0.15 M of wet method spin coating in substrate, in turning for 2500 rpm
Lower 10 s of spin coating of speed, then anneal at a temperature of 450 DEG C 1 h.
Then the WO of 20 mg is weighed3The iodine of powder and 5 mg are dissolved in the acetone soln of 25 ml, and solution is put into
It is used as reaction vessel in the beaker that specification is 50 ml, then carry out ultrasonic oscillation to make its fully dispersed suspension for stable homogeneous
Liquid.The conducting surface for the conductive substrates that two panels was cleaned then is relatively fixed to the positive and negative polarities in D.C. regulated power supply, it is ensured that it
Between between be divided into 1 cm.It sets the voltage of D.C. regulated power supply to 25 V again, is inserted by working electrode and to electrode
WO3Suspension in, 150 s are electroplated under voltage stabilizing.
Then the ammonium metatungstate methanol solution of a concentration of 20 mM of 20 ul is taken to drop in WO3On electrode, after natural drying, repeat
Sample is finally annealed 1 h at 450 DEG C, obtains the light anode sample of final photoelectrochemical cell by drop 4 times.
The photoelectrochemical cell formed using this optoelectronic pole tests its current curve under applying bias.As shown in Fig. 2,
The WO of the method for the present invention is not used3Photoelectric current of the light anode at 1.0 V only has 0.09 mA/cm2, and processing using the present invention
After method, the photoelectric current at 1.0V has reached 1.71 mA/cm2, photoelectric current is expanded to original 19 times.
The description of the aforementioned specific exemplary embodiment to the present invention is in order to illustrate and illustration purpose.These descriptions
It is not wishing to limit the invention to disclosed precise forms, and it will be apparent that according to the above instruction, can much be changed
And variation.The purpose of selecting and describing the exemplary embodiment is that explaining the specific principle of the present invention and its actually answering
With so that those skilled in the art can realize and utilize the present invention a variety of different exemplary implementation schemes and
Various chooses and changes.The scope of the present invention is intended to be limited by claims and its equivalents.
Claims (9)
1. a kind of photoelectrochemical cell optoelectronic pole, including conductive substrates, it is characterised in that：Further include that sequence is placed in the conductive liner
Semiconductor compacted zone, nanometer semiconductor structure layer on bottom and semiconductor surface decorative layer, the semiconductor compacted zone is by causing
Close layer is made of film, compound for inhibiting conductive substrates and electrolyte to occur, and enhances the electricity of conductive substrates and nanostructured layers
Connection；The nanometer semiconductor structure layer is made of nanostructure, is extinction main body, is the main source of photo-generated carrier, is risen
Basic role；The finishing coat is made of nano particle, for improving the note of the charge between nanostructured layers and electrolyte
Enter efficiency, is the decorative layer of nanostructured layers.
2. the photoelectrochemical cell optoelectronic pole as described in claim 1, which is characterized in that semiconductor TiO2, α-Fe2O3,
BiVO4, WO3One such or a variety of mixed semiconductors material.
3. the photoelectrochemical cell optoelectronic pole as described in claim 1, which is characterized in that the conductive substrates are ITO, AZO
Or FTO conductive films.
4. the photoelectrochemical cell optoelectronic pole as described in claim 1, which is characterized in that the conductive substrates are opaque
Electrode metal or emtal alloy film.
5. preparation and the processing method of a kind of optoelectronic pole of photoelectrochemical cell, including step：
S1 prepares WO on conductive substrates3Compacted zone；
S2 prepares the WO of nanostructure3Porous layer；
S3 is to WO3Nano porous layer is surface modified.
6. preparation and the processing method of the optoelectronic pole of photoelectrochemical cell according to claim 5, it is characterised in that：It is described
In S1 WO is formed by following steps3Compacted zone：
Conductive substrates are cleaned by ultrasonic 20 minutes in acetone, absolute ethyl alcohol, deionized water by S1.1 respectively；
S1.2 takes suitable ammonium metawolframate powder with balance, is dissolved in a small amount of deionized water, with ultrasonic oscillation to thoroughly it is molten
Solution, adds suitable methanol solution, it is ensured that the volume that deionized water volume accounts for total solution is no more than 1/4；
S1.3 takes the drop of the solution in 20 μ l steps S1.2 on conductive substrates, 10 s of spin coating under the rotating speed of 2500 rpm, then
Cabinet-type electric furnace is put it into be warming up to 450 DEG C through 1 h and keep 1 h.
7. preparation and the processing method of the optoelectronic pole of photoelectrochemical cell according to claim 5, it is characterised in that：It is described
In S2 WO is formed by following steps3Nano porous layer：
S2.1, which is weighed in the balance, takes 20 mg WO3Powder and 5 mg elemental iodines are put into the beaker of 50 ml（Reaction vessel）, then to
The acetone of 25 ml is added in beaker, then carry out ultrasonic oscillation reasonable time to make its fully dispersed suspension for stable homogeneous
Liquid；
The conducting surface for the conductive substrates that two panels was cleaned is relatively fixed the positive and negative polarities in D.C. regulated power supply by S2.2, it is ensured that it
Between between be divided into 1 cm；
It sets the voltage of D.C. regulated power supply to 25 V again, WO is inserted by working electrode and to electrode3Suspension in, surely
150 s of pressure plating.
8. preparation and the processing method of the optoelectronic pole of photoelectrochemical cell according to claim 5, it is characterised in that：It is described
By following steps to WO in step S33Surface is modified：
S3.1 configures the ammonium metatungstate methanol solution of a concentration of 20 mmol/L of tungsten atom, and 20 μ l solution is taken slowly to drop in film
On, it dries at room temperature, repeats this operation 4 times；
Sample is put into cabinet-type electric furnace by S3.2, and arrange parameter makes to be heated to 450 DEG C in its 1 h, and 1h is kept to anneal.
9. preparation and the processing method of the optoelectronic pole of photoelectrochemical cell according to claim 5, it is characterised in that：Partly lead
Body compacted zone equably covers conductive substrates, reduces the compound of photo-generated carrier, and preparation method includes but not limited to solution
Spin-coating method, sputtering method, vapour deposition method；
Nanometer semiconductor structure layer has the diffusion length that few son is reduced by nanostructure, including but not limited to nanometer rods battle array
The nanostructures such as row, nano-chip arrays and nano-porous film；Nanometer semiconductor structure layer, preparation method include but unlimited
In sol-gal process, anodizing, chemical vapour deposition technique, electrochemical deposition method；Semiconductor surface decorative layer, modification side
Method includes but not limited to chemical bath, chemical vapor deposition, atomic layer deposition.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115083787A (en) * | 2022-06-23 | 2022-09-20 | 南京邮电大学 | Ultrathin oxide modified semiconductor electrode and preparation method thereof |
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| CN102834929A (en) * | 2010-02-18 | 2012-12-19 | 韩国化学研究院 | Method for manufacturing a nanostructured inorganic/organic heterojunction solar cell |
| CN104711528A (en) * | 2013-12-13 | 2015-06-17 | 中国科学院大连化学物理研究所 | Sheet-like tungsten trioxide photoelectrode and preparation method thereof |
| CN105655488A (en) * | 2016-03-10 | 2016-06-08 | 天津理工大学 | Perovskite solar cell with ferrocene layer and preparation method of perovskite solar cell |
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Patent Citations (4)
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| CN101620939A (en) * | 2008-07-02 | 2010-01-06 | 比亚迪股份有限公司 | Semiconductor electrode, preparation method thereof and solar cell comprising semiconductor electrode |
| CN102834929A (en) * | 2010-02-18 | 2012-12-19 | 韩国化学研究院 | Method for manufacturing a nanostructured inorganic/organic heterojunction solar cell |
| CN104711528A (en) * | 2013-12-13 | 2015-06-17 | 中国科学院大连化学物理研究所 | Sheet-like tungsten trioxide photoelectrode and preparation method thereof |
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| CN115083787A (en) * | 2022-06-23 | 2022-09-20 | 南京邮电大学 | Ultrathin oxide modified semiconductor electrode and preparation method thereof |
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Application publication date: 20181012 |