CN107268020B - A kind of Ta3N5The preparation method and Ta of film3N5The application of film - Google Patents
A kind of Ta3N5The preparation method and Ta of film3N5The application of film Download PDFInfo
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- CN107268020B CN107268020B CN201710416513.4A CN201710416513A CN107268020B CN 107268020 B CN107268020 B CN 107268020B CN 201710416513 A CN201710416513 A CN 201710416513A CN 107268020 B CN107268020 B CN 107268020B
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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
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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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- 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
Abstract
The invention discloses a kind of Ta3N5The preparation method of film prepares Ta using the method that the chemical attack of metal Ta piece elder generation reoxidizes nitridation3N5Film.The invention also discloses the Ta of preparation3N5The application of film, by the Ta3N5Film is used for decomposing water with solar energy hydrogen manufacturing as light anode.On the one hand the present invention eliminates the oxygen-rich layer on the surface metal Ta by the introducing of chemical attack, to reduce the Ta finally prepared3N5The Carrier recombination center of film surface, reduces photo-generated carrier surface recombination；On the other hand corrosion causes metal Ta surface roughness to increase, to increase the Ta finally prepared3N5The surface roughness and specific surface area of film, increase electrolyte and Ta3N5The contact area of film.The present invention improves Ta3N5Efficiency of light absorption, photo-generated carrier separative efficiency and the carrier transport efficiency of film, Ta3N5The photoelectric current and quantum conversion of light anode greatly improve.
Description
Technical field
The present invention relates to a kind of Ta3N5The preparation method and Ta of film3N5The application of film, belongs to decomposing water with solar energy system
Hydrogen technical field.
Background technique
The fossil energy reserves that the mankind depend on for existence at present are limited, and the use of fossil energy can give off CO2, vulcanization
The pollutants such as object.Therefore, the reproducible cleaning new energy for developing alternative fossil energy is human social
There is an urgent need to.Solar energy is important one of renewable and clean energy resource.Water decomposition, which is carried out, using photoelectrochemical cell produces hydrogen and oxygen,
Solar energy is directly converted into storable cleaning chemistry energy --- Hydrogen Energy has tempting application prospect.Exploitation is had excellent performance
Optoelectronic pole (including light anode and photocathode) material be research and develop efficient photoelectricity treater chemistry solar energy water decompose battery key technology
One of.And the key of optical electro-chemistry hydrogen production by water decomposition is to find efficient N-shaped optical anode material.
Ideal semiconductor optical anode material will have suitable band gap, can utilize most of energy in sunlight, and
And it is strong etc. with high transformation efficiency, corrosion resistance.Up to the present, the optical anode material that can meet above-mentioned condition simultaneously is few
It is again few.Oxide semiconductor light anode such as reports more TiO2、WO3、BiVO4Equal material visible-lights utilization rate is low,
Photoelectric current under 1.23V is both less than 4mA/cm2, solar conversion efficiency is low.Nitride-based semiconductor and the oxidation studied extensively
Object semiconductor, which is compared, has narrower band gap, can become heavy in recent years using the visible light for accounting for most of energy in sunlight
A kind of optical anode material of point concern.
Ta3N5Band gap is 2.1eV, and light absorption band edge is in 600nm；And its valence band location is lower than O2/H2The redox of O
Current potential, conduction band positions are higher than H+/H2Oxidation-reduction potential, if being not required to applying bias, theoretical photoelectric current is reachable
13mAcm2, theoretical solar conversion efficiency is very promising N-shaped optical anode material up to 15.9%.But since light absorption is imitated
The presence for the factors such as rate is low, photo-generated carrier separates, efficiency of transmission is low, the Ta reported at present3N5Photoelectrochemical behaviour it is also remote low
In theoretical value, also many key scientific problems and technology has to be solved.
Summary of the invention
The technical problem to be solved by the present invention is to overcome the deficiencies of existing technologies, a kind of simple, efficient, low cost is provided
Ta3N5The preparation method of film, Ta prepared by the method3N5Film is as light anode, using sun photodegradation aquatic products hydrogen,
Improve Ta3N5Decompose aquatic products hydrogen photoelectric current and quantum conversion.
In order to solve the above technical problems, the present invention provides a kind of Ta3N5The preparation method of film, characterized in that use metal
The chemical attack of Ta piece elder generation reoxidizes the method preparation Ta of nitridation3N5Film.
Further, the preparation method the following steps are included:
(1) metal Ta piece is put into alkaline solution and carries out chemical attack, alkaline solution passes through oil bath heating；
(2) the metal Ta piece after corrosion is taken out, is rinsed with deionized water, and ultrasound is shaken respectively with ethyl alcohol and deionized water
It swings, to remove surface corrosion residue；
(3) above-mentioned steps (1) and (2) are repeated 3 times；
(4) the metal Ta after corrosion is put into batch-type furnace, heats in air atmosphere, obtains Ta2O5/Ta；
(5) obtained Ta2O5/ Ta is put into tube furnace, is heated under ammonia atmosphere, is obtained Ta3N5/Ta。
Further, in above-mentioned steps (1), the alkaline solution be 40% KOH aqueous solution.
Further, in above-mentioned steps (1), the oil bath heating is maintained at 110 DEG C, and etching time is 1 hour.
Further, in above-mentioned steps (2), the ultrasonic vibration time is 30 minutes.
Further, in above-mentioned steps (4), within the temperature range of 550 DEG C~560 DEG C, 30 are heated in air atmosphere
Minute.
Further, it in above-mentioned steps (5), is heated 8 hours under 850 DEG C of ammonia atmosphere.
The present invention also provides a kind of Ta3N5The application of film, characterized in that by the Ta3N5Film is used for as light anode
Decomposing water with solar energy hydrogen manufacturing.
Advantageous effects of the invention: on the one hand the present invention eliminates the surface metal Ta by the introducing of chemical attack
Oxygen-rich layer, to reduce the Ta finally prepared3N5The Carrier recombination center of film surface, reduces photo-generated carrier table
Face is compound；On the other hand corrosion causes metal Ta surface roughness to increase, to increase the Ta finally prepared3N5The table of film
Surface roughness and specific surface area, increase electrolyte and Ta3N5The contact area of film.Above-mentioned two aspects factor improves Ta3N5
Efficiency of light absorption, photo-generated carrier separative efficiency and the carrier transport efficiency of film, final Ta3N5The photoelectric current of light anode and
Quantum conversion greatly improves.Method of the invention is simple, it is at low cost, be easy to large-scale use, be high-efficient.
Detailed description of the invention
Fig. 1 is chemical attack prepared by the present invention-oxidation nitridation Ta3N5(embodiment) and reported simple nitrogen oxide
The Ta of change method preparation3N5The XRD diagram of (comparative example).
Fig. 2 is the photoluminescence spectrum of metal Ta before and after chemical attack of the present invention.
Fig. 3 is chemical attack of the present invention-oxidation nitridation method preparation Ta3N5(embodiment) and simple oxidation nitridation
The Ta of method preparation3N5The photoluminescence spectrum of (comparative example).
Fig. 4 is the surface SEM figure of metal Ta before and after chemical attack；Chemical attack-oxidation nitridation method preparation Ta3N5(implement
Example) and the preparation of simple oxidation nitridation method Ta3N5The surface of (comparative example) and section SEM figure.
Fig. 5 is chemical attack under different scanning speed-oxidation nitridation method preparation Ta3N5(embodiment) and simple nitrogen oxide
The Ta of change method preparation3N5The capacitance current of (comparative example).
Fig. 6 is chemical attack of the present invention-oxidation nitridation method preparation Ta3N5(embodiment) and simple oxidation nitridation
The Ta of method preparation3N5The ultraviolet-visible absorption spectroscopy of (comparative example)；
Fig. 7 is chemical attack of the present invention-oxidation nitridation method preparation Ta3N5(embodiment) and simple oxidation nitridation
The Ta of method preparation3N5The separation of charge efficiency of (comparative example) at different wavelengths；
Fig. 8 is chemical attack of the present invention-oxidation nitridation method preparation Ta3N5(embodiment) and simple oxidation nitridation
The Ta of method preparation3N5The electrochemical impedance spectroscopy of (comparative example).
Fig. 9 is chemical attack of the present invention-oxidation nitridation method preparation Ta3N5(embodiment) and simple oxidation nitridation
The Ta of method preparation3N5Photoelectric current-the potential curve of (comparative example), electrolyte: 1M NaOH aqueous solution, light source: the AM1.5 sun
Optical simulator；
Figure 10 is chemical attack of the present invention-oxidation nitridation method preparation Ta3N5(embodiment) and simple oxidation nitridation
The Ta of method preparation3N5The quantum conversion of (comparative example) at different wavelengths, electrolyte: 1M NaOH aqueous solution, light source:
Full width xenon lamp.
Specific embodiment
The invention will be further described below in conjunction with the accompanying drawings.Following embodiment is only used for clearly illustrating the present invention
Technical solution, and not intended to limit the protection scope of the present invention.
Before experiment, metal Ta piece respectively in ethyl alcohol, acetone, deionized water ultrasound and rinse.
Comparative example
By the Ta piece cleaned in air atmosphere in batch-type furnace 550 DEG C at a temperature of heat 30 minutes, obtain Ta2O5/
Ta；The Ta that will then obtain2O5/ Ta is put into tube furnace, under ammonia atmosphere, is heated 8 hours at 850 DEG C, is obtained specific surface area
Lesser Ta3N5/Ta.This sample is used as chemical attack according to the present invention-oxidation nitridation method preparation Ta3N5Comparative sample
Product, for describing the problem.
Embodiment
The Ta piece cleaned is put into 40% KOH aqueous solution and carries out chemical attack, KOH aqueous temperature passes through oil bath
Heating is maintained at 110 DEG C, and etching time is 1 hour；Metal Ta piece after corrosion is taken out, is rinsed with deionized water, and use second
Pure and mild deionized water is distinguished ultrasonic vibration 30 minutes, to remove surface corrosion residue；Above-mentioned corrosion and cleaning step repeat
3 times；Metal Ta after corrosion is put into batch-type furnace, is heated in air atmosphere within the temperature range of 550 DEG C~560 DEG C
30 minutes, obtain Ta2O5/Ta；The Ta that will finally obtain2O5/ Ta is put into tube furnace, heats 8 under ammonia atmosphere at 850 DEG C
Hour, obtain the Ta of large specific surface area3N5/Ta。
Step more than has obtained the different Ta of specific surface area3N5Film, we have carried out every table to these films
Sign, Fig. 1-10 is to the Ta obtained under different preparation conditions3N5The characterization result of film.Wherein, optical electro-chemistry test using
The three-electrode system of standard, Ta3N5Make anode, platinum Pt makees cathode, and SCE electrode makees reference electrode, AM1.5G solar simulator
Or the xenon lamp as light source of 500W, electric current-potential curve is measured with Shanghai Chen Hua CHI633C electrochemical workstation.Semi-conductor electricity
The quantum conversion (IPCE) of pole is defined as the ratio of light induced electron number Yu incident light subnumber, can be obtained by the following formula:
Wherein IphIt is density of photocurrent, P is light intensity, and λ is the wavelength of incident light.Using light intensity meter (Newport, 840-C)
Light intensity is tested, tests the conversion quantum efficiency (IPCE) under different wave length with monochromatic filter.
It will be seen from figure 1 that (comparison is real for oxidation nitridation after chemical attack-oxidation nitridation (embodiment) and merely for Ta piece
Apply example) after conversion for Ta3N5.And chemical attack-oxidation nitridation method preparation Ta3N5Have no the XRD of metal Ta substrate
Peak, Ta2The peak XRD of N is also than the Ta of simple oxidation nitridation preparation3N5It is much lower.
Fig. 2 gives the photoluminescence spectrum before and after metal Ta piece chemical attack, and Fig. 3 gives chemical attack-oxidation nitridation
The Ta of method preparation3N5(embodiment) and the Ta of simple oxidation nitridation method preparation3N5The photoluminescence spectrum of (comparative example).By Fig. 2
With Fig. 3 it is found that after chemical attack, the Ta that is obtained after metal Ta piece and its oxidation nitridation3N5Luminescence generated by light peak drastically reduce, closely
It disappears.Studies have shown that oxygen-rich layer of this luminescence generated by light peak from the surface metal Ta, and the oxygen impurities conduct in this oxygen-rich layer
Complex centre will cause the compound of a large amount of light induced electrons and hole, and then reduce the decomposing water with solar energy hydrogen manufacturing effect of semiconductive thin film
Rate.Chemical attack of the present invention-oxidation nitridation method preparation Ta3N5The luminescence generated by light peak of film is greatly reduced, and is conducive to mention
The aqueous energy of the decomposition of high film.
Before and after describing chemical attack in Fig. 4, the surface topography of metal Ta piece.Before corrosion, the surface metal Ta is more smooth,
After corrosion, metal Ta modification of surface morphology is significant, rough and uneven in surface, this prepares high-ratio surface Ta to be subsequent3N5Film provides item
Part.Based on the metal Ta for corroding front and back, oxidation nitridation prepares Ta3N5.The Ta of simple oxidation nitridation preparation3N5Film (comparison
Embodiment) smooth surface, and chemical attack-oxidation nitridation method preparation Ta3N5Film (embodiment) surface relief injustice is simultaneously
With hole, rice krispies floral structure is showed.Ta3N5Section SEM structure chart and surface SEM shape appearance figure give identical conclusion.
Fig. 5 gives chemical attack-oxidation nitridation method preparation Ta3N5Film (embodiment) and simple oxidation nitridation legal system
Standby Ta3N5Capacitance current of the film (comparative example) under different scanning speed, size and the film electrification of capacitance current
The size for learning active area is proportional, therefore, chemical attack-oxidation nitridation method preparation Ta3N5The electrochemical surface area of film
It is much greater.Fig. 4 and Fig. 5 shows chemical attack of the present invention-oxidation nitridation method preparation Ta3N5Film has puffed rice
Shape structure, surface roughness, electrochemical surface area, specific surface area are much larger than the Ta of simple oxidation nitridation method preparation3N5It is thin
Film.The structure of semiconductive thin film can have an impact light absorption, solid liquid interface water oxygen, and then influence the sun of semiconductive thin film
It can hydrogen production by water decomposition efficiency.
Fig. 6 gives chemical attack-oxidation nitridation method preparation Ta3N5Film (embodiment) and simple oxidation nitridation legal system
Standby Ta3N5The ultraviolet-visible absorption spectroscopy of film (comparative example) shows chemical attack-nitrogen oxide according to the present invention
The Ta of change method preparation3N5The efficiency of light absorption of film is higher, and light absorption band edge red shift about 15nm, the raising of efficiency of light absorption
Mostly come from the influence of film morphology.
Fig. 7 gives chemical attack-oxidation nitridation method preparation Ta3N5Film (embodiment) and simple oxidation nitridation legal system
Standby Ta3N5The separation of charge efficiency of film (comparative example) shows chemical attack according to the present invention-oxidation nitridation method
The Ta of preparation3N5The main reason for separation of charge of film is more efficient, and separation of charge efficiency improves is also flower-shaped from rice krispies
Large ratio surface structure, this pattern are conducive to the diffusion of electrolyte in the film, reduce hole transport distance.
Fig. 8 gives chemical attack-oxidation nitridation method preparation Ta3N5Film (embodiment) and simple oxidation nitridation legal system
Standby Ta3N5The electrochemical impedance spectroscopy of film (comparative example), impedance ring is smaller, then the electricity of film and electrolyte contacts interface
Lotus efficiency of transmission is higher.Fig. 8 shows chemical attack according to the present invention-oxidation nitridation method preparation Ta3N5The impedance ring of film
Much smaller, i.e. the photo-generated carrier efficiency of transmission of its solid liquid interface is higher.High efficiency of light absorption, separation of charge efficiency and charge
Efficiency of transmission, which favorably has, obtains higher decomposing water with solar energy efficiency.
Fig. 9 and Figure 10 gives co-catalyst Co-Pi and supports rear chemical attack-oxidation nitridation method preparation Ta3N5Film
(embodiment) and the Ta of simple oxidation nitridation method preparation3N5Film (comparative example) is in standard sunlight AM1.5G (100mW/
cm2) photoelectric current and quantum conversion at different wavelengths under irradiation.Show chemical attack-according to the present invention
The Ta of oxidation nitridation method preparation3N5Film at 1.23V photoelectric current up to 6.8mA/cm2, the quantum under the wavelength of 400~450nm
Transformation efficiency can reach 60%.Above-mentioned photocurrent values and quantum conversion are the high values in the light anode reported at present.And
Chemical attack according to the present invention-oxidation nitridation method preparation Ta3N5The photoelectric current of film is simple oxidation nitridation method preparation
Ta3N55 times of film, chemical attack according to the present invention-oxidation nitridation method preparation Ta3N5The quantum conversion of film
It is the Ta of oxidation nitridation method preparation3N56 times of film.
The above analysis illustrates that the method for metal Ta piece chemical attack-oxidation nitridation according to the present invention can be prepared
The rice krispies flower-like structure Ta of high-ratio surface3N5Film, efficiency of light absorption, separation of charge efficiency and the charge transfer efficiency of this film
The Ta prepared compared to simple oxidation nitridation method3N5Film greatly improves, its final decomposing water with solar energy efficiency also substantially mentions
It is high.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, without departing from the technical principles of the invention, several improvement and deformations can also be made, these improvement and deformations
Also it should be regarded as protection scope of the present invention.
Claims (2)
1. a kind of Ta3N5The preparation method of film, characterized in that the method that nitridation is reoxidized using the chemical attack of metal Ta piece elder generation
Prepare Ta3N5Film carries out chemistry corruption specifically includes the following steps: the Ta piece cleaned is put into the KOH aqueous solution of 40 %
Erosion, KOH aqueous temperature are maintained at 110 DEG C by oil bath heating, and etching time is 1 hour；Metal Ta piece after corrosion is taken
Out, it is rinsed with deionized water, and is distinguished ultrasonic vibration 30 minutes with ethyl alcohol and deionized water, to remove surface corrosion residual
Object；Above-mentioned corrosion and cleaning step are repeated 3 times；Metal Ta after corrosion is put into batch-type furnace, in 550 DEG C~560 DEG C of temperature
It is heated in air atmosphere 30 minutes in degree range, obtains Ta2O5/Ta；The Ta that will finally obtain2O5/ Ta is put into tube furnace,
It is heated 8 hours under ammonia atmosphere at 850 DEG C, obtains the Ta of large specific surface area3N5/Ta。
2. utilizing a kind of Ta described in claim 13N5The Ta of the preparation method preparation of film3N5The application of film, characterized in that
By the Ta3N5Film is used for decomposing water with solar energy hydrogen manufacturing as light anode.
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| CN108409332B (en) * | 2018-02-12 | 2020-04-24 | 山东大学 | Preparation method of self-supporting film of endo-growth [153] oriented Ta3N5 |
| CN109374520B (en) * | 2018-11-14 | 2021-01-15 | 中车青岛四方机车车辆股份有限公司 | Electrochemical test system for atmospheric corrosion of metal under flowing thin liquid film |
| CN111155147B (en) * | 2020-01-15 | 2021-05-18 | 浙江大学 | Lanthanum chloride molten salt mediated tantalum nitride photo-anode and preparation method thereof |
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| TW479262B (en) * | 1999-06-09 | 2002-03-11 | Showa Denko Kk | Electrode material for capacitor and capacitor using the same |
| CN102800481A (en) * | 2012-05-04 | 2012-11-28 | 南京大学 | Surface passivation method of iron oxide photoelectrode |
| CN103966623A (en) * | 2013-02-01 | 2014-08-06 | 南京大学 | Ta3N5 photoanode, preparation method and application thereof |
| CN103981558A (en) * | 2014-05-21 | 2014-08-13 | 天津大学 | Tantalum nitride nanotube array electrode and preparation method thereof |
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