CN111155147B - Lanthanum chloride molten salt mediated tantalum nitride photo-anode and preparation method thereof - Google Patents

Lanthanum chloride molten salt mediated tantalum nitride photo-anode and preparation method thereof Download PDF

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CN111155147B
CN111155147B CN202010044387.6A CN202010044387A CN111155147B CN 111155147 B CN111155147 B CN 111155147B CN 202010044387 A CN202010044387 A CN 202010044387A CN 111155147 B CN111155147 B CN 111155147B
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lacl
molten salt
anode
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CN111155147A (en
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朱丽萍
楼子瑞
覃超
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Zhejiang University ZJU
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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
    • C25B11/091—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
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D9/00—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
    • C21D9/46—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for sheet metals
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/02—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working in inert or controlled atmosphere or vacuum
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/16—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of other metals or alloys based thereon
    • C22F1/18—High-melting or refractory metals or alloys based thereon
    • 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
    • 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
    • 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 LaCl3Ta mediated by molten salt3N5A photo-anode and a preparation method thereof. The invention is carried out at low dosage of LaCl3Under the assistance of molten salt, LaCl is prepared by the traditional simple and convenient method of directly oxidizing and nitriding Ta foil3Ta mediated by molten salt3N5The photo-anode successfully improves the performance of photoelectrocatalysis water decomposition. The Ta3N5The photoanode has stronger absorption in solar spectrum, has high-efficiency activity of decomposing water by photoelectrocatalysis, and the performance improvement comes from the doping of La element on the surface and LaTaON2And (4) generation of a phase. The method has the advantages of simple equipment, easy operation, good photo-anode crystallization quality and stable performance, and is beneficial to large-scale popularization and application. LaCl3The introduction of the molten salt brings a new appearance to the traditional preparation method and provides a new method for a large-area, low-cost and high-efficiency photo-anode.

Description

Lanthanum chloride molten salt mediated tantalum nitride photo-anode and preparation method thereof
Technical Field
The invention belongs to the field of photoelectrocatalysis, and particularly relates to LaCl3Ta mediated by molten salt3N5A photo-anode and a preparation method thereof.
Background
Photoelectrochemical (PEC) water splitting as a method of converting solar energyThe strategy of chemical energy in the form of hydrogen and oxygen has attracted people's attention, and provides a feasible technical route for the development of renewable energy sources. In which Ta3N5Has the advantages of good energy band structure matched with hydrogen evolution and oxygen evolution potentials, enough light absorption (2.1 eV), low cost, environmental friendliness and the like, and is a promising candidate material. However, surface/bulk defects and carrier recombination limit performance.
In a recent study, Ta3N5The photo-anode being mainly composed of anodised Ta2O5Nanotube, deposited Ta2O5Nanorods or alkali tantalates are nitrided and a favorable photocurrent is obtained. However, the conventional method of directly oxidizing re-nitrided tantalum metal sheets has hardly developed in a breakthrough manner over the years. This conventional method is most suitable for large-scale industrial production.
Doping and heteroj unction are improvements of Ta3N5Two effective means of photoelectrochemical properties. Doping can effectively suppress Ta by charge compensation3N5While heterojunctions promote photogenerated carrier separation (particularly from various Ta-based perovskite-type oxynitrides) by the potential driving force caused by their band differences. It is very important to combine these measures to improve the conventional TaN oxide metal sheet method to obtain high performance photoelectrode. The invention is through LaCl3Method of molten salt mediation to effect Ta3N5The surface doping and heterojunction modification successfully improve the photoelectric catalytic performance and provide a new idea for the traditional preparation method.
Disclosure of Invention
The invention aims to provide the LaCl with low cost, short preparation period and excellent photoelectric catalytic performance3Ta mediated by molten salt3N5A preparation method of the photo-anode.
LaCl of the invention3Ta mediated by molten salt3N5The preparation method of the photo-anode comprises pre-oxidation and LaCl3Molten salt mediated, Ta3N5Preparing a photo-anode; comprises the following stepsThe method comprises the following steps:
1) pre-oxidation: respectively carrying out ultrasonic cleaning treatment on the Ta foil in acetone, ethanol and deionized water, and then annealing in air to form an oxide layer;
2)LaCl3molten salt mediation: preparation of LaCl3A solution; placing the oxidized Ta foil in the step 1) on a heating plate, and then dropwise adding LaCl on the Ta foil3A solution; when the solvent evaporated, a layer of dense, smooth, translucent LaCl formed on the Ta foil3And (5) film forming to obtain a precursor.
3)Ta3N5Preparing a photo-anode: carrying out heat treatment on the precursor in the step 2) in ammonia atmosphere to obtain LaCl3Ta mediated by molten salt3N5And a photo-anode.
Wherein, the annealing temperature in the step 1) is 450-550 ℃, and the time is 30-120 minutes.
The LaCl in the step 2)3The solvent can be non-aqueous solvent such as methanol, ethanol, acetone, etc., with concentration of 0.1-2M, and the dripping amount is 10-1000 uL.
The reaction temperature of the heat treatment in the step 3) is 900 ℃, the reaction time is 0.5-10 hours, the atmosphere is high-purity ammonia gas, and the purity is at least 99%.
The invention has the beneficial effects that:
1) in the invention, the LaCl with high crystalline quality and excellent photoelectrocatalysis performance is prepared3Ta mediated by molten salt3N5Photoanode, less molten salt treated Ta3N5The performance of the photo-anode is more excellent.
2) In LaCl3Ta can be reacted under the action of molten salt3N5Better crystallization and LaTaON formation on the surface2And La-doped Ta3N5The better heterojunction energy band arrangement is formed, the surface carrier recombination is inhibited, and the surface carrier degree is improved by one order of magnitude.
3) Further loaded with Co3O4After the cocatalyst of (2), in simulated sunlight (AM 1.5G,100mW cm)-2) Irradiated in 1M NaOH electrolyteNow 8.2mA cm-2Photo current of @1.23V vs. rhe. To our knowledge, this is Ta foil prepared by direct oxidation and re-nitridation3N5The highest photocurrent response.
4) The LaCl provided by the invention3Ta mediated by molten salt3N5The photo-anode has the photoelectrochemical properties equivalent to those of a photo-anode with a fine micro-nano structure, so that the production and the manufacture of the photo-anode with large area and low cost can be greatly facilitated.
Drawings
FIG. 1 shows LaCl prepared by the present invention3Ta mediated by molten salt3N5Scanning an electron microscope SEM picture of the surface morphology of the photo-anode;
FIG. 2 shows the preparation of LaCl3Ta mediated by molten salt3N5Photoanode and untreated Ta3N5An XRD spectrum of the photoanode; wherein (a) is the presence/absence of LaCl3Ta mediated by molten salt3N5A photoanode XRD spectrum, (b) is a local enlarged view about 31 degrees;
FIG. 3 shows a LaCl prepared according to the present invention3Ta mediated by molten salt3N5Photoanode and untreated Ta3N5The photoelectrocatalysis decomposition water-based performance curve of the photo-anode is tested in a 1M NaOH solution; wherein (a) is a current-potential curve, and (b) is a photocurrent-time curve at 1.23V vs. rhe;
Detailed Description
The invention will be further described by way of example with reference to the accompanying drawings. It is to be understood that the following examples are illustrative of the present invention and are not to be construed as limiting the scope of the invention, and that certain insubstantial modifications and adaptations of the invention by those skilled in the art in light of the foregoing description are intended to be included within the scope of the invention. The specific process parameters and the like in the following examples are also only an example of suitable ranges, and those skilled in the art can select the appropriate ranges through the description herein, and are not limited to the specific values in the following examples.
Example 1
LaCl3Ta mediated by molten salt3N5And (4) preparing a photo-anode.
1) Pre-oxidation: firstly, cutting a Ta foil into the size of 12mm multiplied by 10mm, then respectively carrying out ultrasonic cleaning treatment on the Ta foil in acetone, ethanol and deionized water, and then annealing for 1h at 500 ℃ in the air to form a gray oxide layer.
2)LaCl3Addition of molten salt: placing the oxidized Ta foil of step 1) on a heating plate, and then dropwise adding 0.5M LaCl on the Ta foil by using a pipette3The solution was 100 uL. When the solvent evaporates, a dense, smooth, translucent layer of LaCl is formed3A film.
3)LaCl3Ta mediated by molten salt3N5Preparation of the photo-anode: carrying out heat treatment on the precursor in the step 2) in ammonia atmosphere, and keeping the temperature at 900 ℃ for 5h to obtain LaCl3Ta mediated by molten salt3N5Photo-anode, named La-Ta3N5. The LaCl3Ta mediated by molten salt3N5The shape of the photo-anode is shown in figure 1, the electrode plate is represented as a red light absorber in a macroscopic manner, the material in a microscopic shape is that nitride is tightly attached to a metal Ta substrate, so that the metal Ta substrate has enough conductivity, the thickness of the nitride is 0.3-10 mu m, and trace La elements exist on the surface of the nitride. FIG. 2 shows the LaCl3Ta mediated by molten salt3N5Photoanode and untreated Ta3N5X-ray diffraction pattern of the photoanode, wherein diffraction peaks in the pattern are all attributed to Ta3N5
(PDF #79-1533) and Ta2N(PDF#26-0985)。Ta2N is considered to be at Ta3N5Conductive phase present in the/Ta interface, and no Ta with poor other conductive phase was found4N5Or Ta5N6It is expected that an interface having better conductivity is advantageous for carrier mobility. In the XRD pattern enlarged view of about 31 degrees, the LaCl3Ta mediated by molten salt3N5The photo-anode has one and Ta3N5(023) A weaker signal peak accompanied by the peak corresponds to the perovskite structure LaTaON2Peak of phase (200) (PDF # 53-0960))。
Example 2
LaCl3Ta mediated by molten salt3N5And testing the performance of the photo-anode.
1) The LaCl obtained in example 1 was added3Ta mediated by molten salt3N5Photoanode with cobalt (Co) oxide3O4) As cocatalyst to Ta3N5The flat photo-anode is optimized by an improved hydrothermal method on Ta3N5Upper hydrothermal deposition of Co3O4And (3) nanoparticles.
2) Testing the photoelectric catalytic performance: we used a standard three-electrode system with chronoamperometric measurements at a potential of 1.23V vs. rhe under AM 1.5G illumination (1 standard sunlight). Testing of La-Ta3N5Photoelectrocatalysis water decomposition performance in 1M NaOH solution (Co cocatalyst is loaded)3O4Is designated as La-Ta3N5-Co). As shown in FIG. 3, in LaCl3With the aid of molten salts, La-Ta3N5The photocurrent of the light source reaches 1.7mA cm-2. In addition, in the case of loading Co3O4After cocatalyst, La-Ta3N5the-Co photo anode reaches 8.2mAcm-2。
Comparative example 1
Untreated Ta3N5And testing the performance of the photo-anode.
1) Ta without molten salt treatment3N5The synthesis of a flat photoanode was similar to the procedure of example 1, but omitting the LaCl3Addition of molten salt to give untreated Ta3N5Photoanode with cobalt (Co) oxide3O4) As cocatalyst to Ta3N5The flat photo-anode is optimized by an improved hydrothermal method on Ta3N5Upper hydrothermal deposition of Co3O4And (3) nanoparticles.
2) Testing the photoelectric catalytic performance: we used a standard three-electrode system with chronoamperometric measurements at a potential of 1.23V vs. rhe under AM 1.5G illumination (1 standard sunlight). Testing Ta3N5In 1M NaOH solutionPhotoelectrocatalysis water decomposition performance in liquid (Co promoter is loaded)3O4Are respectively named Ta3N5-Co). As shown in FIG. 3, Ta without cocatalyst3N5At 1.23VRHEThe photocurrent density at the time of the light irradiation was 0.8mA cm-2This is in contrast to the pure Ta reported in most prior art3N5The performance is equivalent in alkaline solution. Under the load of Co3O4After cocatalyst, Ta3N5the-Co photo anode reaches 4.2mA cm-2。
The invention relates to LaCl3Ta mediated by molten salt3N5A photo-anode and a preparation method thereof. Using low doses of LaCl3Under the assistance of molten salt, LaCl is prepared by the traditional simple and convenient direct oxidation and nitridation method3Ta mediated by molten salt3N5The planar photo-anode successfully improves the performance of photoelectrocatalysis water decomposition. After deposition of the cocatalyst, in the presence/absence of LaCl3With assistance of molten salts, Ta3N5The photo-anode is respectively 8.2mA cm-2And 4.2mA cm-2@1.23V vs.RHE。Ta3N5The surface properties of (A) indicate that in LaCl3The nitriding process can make Ta under the action of molten salt3N5Better crystallization and LaTaON formation on the surface2And La-doped Ta3N5And the surface carrier recombination is inhibited while a better heterojunction energy band arrangement is formed. To our knowledge, this is Ta foil prepared by direct oxidation and re-nitridation3N5The highest photocurrent response. Unlike the published methods, the method utilizes LaCl3Molten salt treatment can greatly improve the traditional Ta3N5The photoelectrocatalysis performance of the photoanode. Although fine micro-nano structures cannot be obtained, LaCl can be used3Ta mediated by molten salt3N5The photoelectrochemical performance of the photoanode is equivalent to that of the reported fine micro-nano structure, so that the photoelectrochemical structure can be possibly applied to the production and the manufacture of the photoanode with large area and low cost.

Claims (3)

1. LaCl3Ta mediated by molten salt3N5The preparation method of the photo-anode is characterized by comprising the following steps:
1) respectively carrying out ultrasonic cleaning treatment on the Ta foil in acetone, ethanol and deionized water, and then annealing in air to form an oxide layer;
2)LaCl3the molten salt adding method comprises the following steps: preparation of LaCl3Solution, placing the Ta foil treated in step 1) on a heating plate, and then dropwise adding LaCl on the Ta foil3Solution, forming a layer of LaCl on the surface of the Ta foil after solvent evaporation3A film to obtain a precursor;
3)LaCl3ta mediated by molten salt3N5Preparation of the photo-anode: carrying out heat treatment on the precursor in the step 2) in ammonia atmosphere to obtain LaCl3Ta mediated by molten salt3N5A photo-anode;
the LaCl in the step 2)3The solution, the solvent is non-aqueous solvent, the concentration is 0.1-2M, and the dropping amount is 10-1000 uL; the reaction temperature of the heat treatment in the step 3) is 900 ℃, and the time is 0.5-10 hours.
2. The LaCl of claim 13Ta mediated by molten salt3N5The preparation method of the photo-anode is characterized by comprising the following steps: the annealing temperature in the step 1) is 450-550 ℃, and the time is 30-120 minutes.
3. LaCl3Ta mediated by molten salt3N5A photoanode, prepared by the method of any one of claims 1 to 2.
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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101862668A (en) * 2010-06-30 2010-10-20 哈尔滨工业大学 Surface gaseous penetration modification method of nanometer titanium dioxide film photocatalyst
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WO2015054656A1 (en) * 2013-10-10 2015-04-16 California Institute Of Technology Protecting the surface of a light absorber in a photoanode
CN106653936A (en) * 2015-11-04 2017-05-10 中国科学院大连化学物理研究所 Ta3N5 photoelectrode and preparation method thereof

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Publication number Priority date Publication date Assignee Title
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CN106637287A (en) * 2016-10-17 2017-05-10 南京大学 Method for preparing tantalic acid lanthanum oxynitride efficient photoelectrode
CN107268020A (en) * 2017-06-06 2017-10-20 中国矿业大学 A kind of Ta3N5The preparation method and Ta of film3N5The application of film

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