CN115216801B - Photo-anode based on cocatalyst and preparation method thereof - Google Patents
Photo-anode based on cocatalyst and preparation method thereof Download PDFInfo
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- CN115216801B CN115216801B CN202210741097.6A CN202210741097A CN115216801B CN 115216801 B CN115216801 B CN 115216801B CN 202210741097 A CN202210741097 A CN 202210741097A CN 115216801 B CN115216801 B CN 115216801B
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Abstract
The invention relates to a photo-anode based on a cocatalystA preparation method, which belongs to the technical field of photoelectrochemistry. The photoanode comprises a conductive substrate, wherein an n-type metal sulfide nano array is arranged on the surface of the conductive substrate; the surface of the n-type metal sulfide nano array is sequentially provided with a zinc oxide film and a titanium dioxide film, and S in the n-type metal sulfide nano array is combined with the zinc oxide film and the titanium dioxide film to obtain a cocatalyst; the cocatalyst is ZnTiO x S y . The invention forms a high-quality photo anode/cocatalyst interface through the ALD process assisted by heat treatment, and constructs a high-efficiency cocatalyst on the surface of the n-type metal sulfide nano-sheet array, so that the PEC performance of the n-type metal sulfide nano-sheet array is obviously improved and is at 1.23V RHE The photocurrent density (J) at the time of measurement was 1.97mAcm ‑2 And an initial potential (V) on ) Is 0.21V RHE 。
Description
Technical Field
The invention belongs to the technical field of photoelectrochemistry, and particularly relates to a photo-anode based on a cocatalyst and a preparation method thereof.
Background
Energy is a core force for promoting the progress of modern society. At present, the global energy supply mainly depends on fossil energy, but the end product is carbon dioxide isothermal chamber gas, which can cause the consequences of the rise of atmospheric temperature, the loss of biological diversity and the like, and the global energy supply conflicts with Paris protocols of the national climate change framework convention. Photoelectrochemistry (PEC) decomposition of water to produce hydrogen is based on a photoelectrocomplementary strategy, and solar energy can be directly converted into hydrogen energy to be stored, so that the hydrogen is one of the most effective schemes for solar energy conversion. Compared with the hydrogen evolution reaction, the Oxygen Evolution Reaction (OER) needs two steps of O-H bond cleavage and O-O bond generation, and is a step of water decomposition reaction. Therefore, the preparation of a photo-anode with excellent performance is a key to achieving high solar-to-hydrogen energy conversion (STH) efficiency. But the poor separation capability of photo-generated electron-hole pairs and slow surface Oxygen Evolution Reaction (OER) kinetics of the photoanode during PEC water decomposition severely limit PEC device development.
For slow OER dynamic reaction, a promoter layer is constructed on the photoelectrode to promote the transfer of holes, reduce the potential barrier of surface catalytic reaction, reduce the impedance of electrochemical reaction and effectively solve the problem. Currently, the usual solution is to cover the photoelectrode surface directly with a layer of co-catalyst. However, this similar cocatalyst preparation scheme introduces a number of defects between the photoelectrode and the cocatalyst, resulting in a severe interfaceAnd (5) compounding. In addition, when the conventional spin coating, hydrothermal means and the like load the cocatalyst on the surface of the photo-anode, a large number of interface defects are introduced at the interface of the photo-anode and the cocatalyst, so that the coverage rate and the content of the cocatalyst cannot be effectively controlled, and serious carrier recombination is caused. Meanwhile, some schemes based on in-situ preparation technology are widely applied. For example by in situ plasma technique, introducing O-S bonds as cocatalysts into SnS 2 And the surface of the base photo-anode. While these efforts can reduce the interfacial recombination of the devices to some extent, they are limited by the choice of materials, often require expensive equipment, and have large limitations on the choice of materials. To date, there are difficulties in preparing high efficiency cocatalysts for high quality interfaces between photoanode and cocatalysts. Generally, the cocatalyst is loaded on the surface of the photo-anode step by step through a two-step method or a multi-step method, so that interface defects are easily introduced, the transmission of photo-generated carriers is not facilitated, and the preparation method based on the in-situ technology can not meet the requirement of universality due to high equipment cost and limitation of material selection.
Disclosure of Invention
Therefore, the technical problem to be solved by the invention is to overcome the problem of preparing the high-efficiency cocatalyst with high quality interface between the photo-anode and the cocatalyst in the prior art.
In order to solve the technical problems, the invention provides a photo-anode based on a cocatalyst and a preparation method thereof. The invention uses a layered structure semiconductor n-type metal sulfide as a substrate, modifies an Atomic Layer Deposition (ALD) modified n-type metal sulfide nano-sheet array (expressed as metal sulfide/ZTA) by a simple air annealing auxiliary strategy, which sequentially deposits a zinc oxide film and a titanium dioxide film on the n-type metal sulfide, thereby obtaining a cocatalyst with a high-quality interface, and well solving the problem of interface recombination. Meanwhile, overflowed S is combined with the deposited zinc oxide film and titanium dioxide film to form a catalyst promoter ZnTiO x S y Greatly increases surface reaction sites, reduces electrochemical impedance and accelerates hole transfer.
It is a first object of the present invention to provideA photo-anode based on a cocatalyst comprises a conductive substrate, wherein an n-type metal sulfide nano array is arranged on the surface of the conductive substrate; the surface of the n-type metal sulfide nano array is sequentially provided with a zinc oxide film and a titanium dioxide film, and S in the n-type metal sulfide nano array is combined with the zinc oxide film and the titanium dioxide film to obtain a cocatalyst; the cocatalyst is ZnTiO x S y 。
In one embodiment of the present invention, the n-type metal sulfide is SnS 2 、In 2 S 3 、ZnIn 2 S 4 And CdIn 2 S 4 One or more of the following.
In one embodiment of the invention, the n-type metal sulfide nanoarray has a thickness of 0.5 μm to 2 μm; the thickness of the zinc oxide film is 0.1nm-10nm; the thickness of the titanium dioxide film is 0.1nm-20nm.
In one embodiment of the invention, the conductive substrate is fluorine doped tin oxide conductive glass (FTO).
A second object of the present invention is to provide a method for preparing the cocatalyst-based photoanode, comprising the steps of,
s1, preparing an n-type metal sulfide nano array on a pretreated conductive substrate to obtain a conductive substrate loaded with the n-type metal sulfide nano array;
s2, sequentially depositing a zinc oxide film and a titanium dioxide film on the conductive substrate loaded with the n-type metal sulfide nano array in the S1 to obtain a photo-anode;
and S3, carrying out annealing treatment on the photo-anode in the S2, and combining the S in the n-type metal sulfide nano array with the zinc oxide film and the titanium dioxide film to form a cocatalyst, so as to obtain the photo-anode based on the cocatalyst.
In one embodiment of the present invention, in S1, the method for preparing the conductive substrate loaded with the n-type metal sulfide nano array includes the steps of:
immersing the pretreated conductive substrate into n-type metal sulfide precursor solution, and reacting for 1-2 h at 70-80 ℃ to obtain the conductive substrate loaded with the n-type metal sulfide nano array; the n-type metal sulfide precursor solution is obtained by dissolving a metal salt and a sulfur source in a solvent.
In one embodiment of the invention, the sulfur source is thioacetamide and/or thiourea.
In one embodiment of the present invention, in S1, the pretreatment is ultrasonic cleaning in acetone, alcohol, and water for 10min-20min, respectively.
In one embodiment of the present invention, in S2, the deposition manner of the zinc oxide thin film and the titanium oxide thin film is one or more of Atomic Layer Deposition (ALD), spin coating, hydrothermal process, and electrodeposition process.
In one embodiment of the invention, in S2, the zinc oxide film is obtained by reacting a zinc source and an oxygen source at 120 ℃ to 200 ℃.
In one embodiment of the invention, the zinc source is dimethyl zinc.
In one embodiment of the present invention, in S2, the titanium oxide film is obtained by reacting a titanium source and an oxygen source at 120 ℃ to 200 ℃.
In one embodiment of the invention, the titanium source is titanium tetra (dimethylamide).
In one embodiment of the invention, the oxygen source is one or more of water, ozone and air.
In one embodiment of the invention, in S3, the annealing is at 150-450 ℃ for 2-10 hours.
Compared with the prior art, the technical scheme of the invention has the following advantages:
(1) The preparation method of the invention uses a simple post-treatment ex-situ strategy to obtain a high-quality photo-anode/cocatalyst interface (few interface defects and high bonding strength) and obtain a high-efficiency cocatalyst. By using a heat treatment annealing strategy, the simple heat treatment is carried out in the air by utilizing the diffusion principle of the S element, so that the interface with high interface bonding strength and few interface defects is successfully obtained, a cocatalyst is obtained, the bulk phase separation of photo-generated electron-hole pairs is promoted, the bulk phase recombination of photo-generated carriers is reduced, and the photoelectrochemical water splitting performance of the composite photo-anode is improved.
(2) The photo-anode based on the cocatalyst disclosed by the invention is effectively combined with a zinc oxide film and a titanium dioxide film due to the overflowing effect of S atoms in the heat treatment process, so that a high-quality photo-anode/cocatalyst interface is constructed, serious interface recombination is avoided, and the service life of carriers is prolonged. The zinc oxide film and the titanium dioxide film effectively avoid a large amount of O doping, inhibit excessive O doping in the heat treatment process and avoid serious degradation of the device performance. Catalyst promoter ZnTiO formed by overflow effect of S in heat treatment process x S y The thin film reduces the overpotential of the surface OER and enhances carrier transfer.
(3) The photo-anode based on the cocatalyst forms a high-quality photo-anode/cocatalyst interface through the ALD process assisted by heat treatment, and constructs an efficient cocatalyst on the surface of the n-type metal sulfide nano-sheet array, so that the PEC performance of the n-type metal sulfide nano-sheet array is obviously improved and is under 1.23V RHE The photocurrent density (J) at the time of measurement was 1.97mA cm -2 And an initial potential (V) on ) Is 0.21V RHE Is superior to the reported metal sulfide-based photoanode.
(4) The preparation method provides a simple and effective strategy, can simultaneously reduce the volume and surface recombination in the photo-anode for PEC water splitting, and also provides a new thought for preparing the high-efficiency cocatalyst through post-treatment or ex-situ preparation strategy to reduce the defects generated by interface recombination.
Drawings
In order that the invention may be more readily understood, a more particular description of the invention will be rendered by reference to specific embodiments thereof which are illustrated in the appended drawings, in which:
FIG. 1 shows SnS of example 1 of the present invention 2 And SnS (sulfur-doped sulfur) 2 SEM of ZTA; wherein a is SnS 2 Is provided; b is SnS 2 Front side of ZTA; c is SnS 2 Is a cross section of (a); d is SnS 2 Section of ZTA.
FIG. 2 shows an embodiment of the present inventionSnS of 1 2 And SnS (sulfur-doped sulfur) 2 J-V plot of/ZTA.
FIG. 3 is a graph of ZnO and TiO for different ALD deposition cycles for example 2 of the present invention 2 J-V plot of (C); wherein a is ZnO; b is TiO 2 。
FIG. 4 is SnS of comparative examples 1-2 of the present invention 2 A and SnS 2 J-V plot of/ZT.
Detailed Description
The present invention will be further described with reference to the accompanying drawings and specific examples, which are not intended to be limiting, so that those skilled in the art will better understand the invention and practice it.
Example 1
A photo-anode based on a cocatalyst and a preparation method thereof specifically comprise the following steps:
(1) Taking FTO as a conductive substrate, respectively ultrasonically cleaning the conductive substrate in an ultrasonic machine for 3 times according to the sequence of acetone, absolute ethyl alcohol and deionized water for 10min each time;
3.16g of tin tetrachloride (SnCl) 4 ) Added to 200mL of absolute ethanol (C) 2 H 5 Stirring for 20min in O). Then, 5.07g of thioacetamide (CH 4 N 2 S, TAA) was mixed into the above solution and vigorously stirred for several minutes to obtain SnS 2 A precursor solution;
the washed conductive substrate was placed with its conductive side facing down in a 15mL glass bottle. 10mL of the precursor solution was added to each vial, and then reacted at 75℃for 90min with sealing. Cooling the glass bottle, taking out, washing with absolute ethyl alcohol, and drying in a vacuum drying oven to obtain the load SnS 2 Conductive substrate of thin film, snS 2 The thickness of the film was about 2 μm.
(2) Placing the conductive substrate treated in the step (1) into an atomic layer deposition cavity, wherein titanium, zinc and oxygen sources are respectively tetra (dimethylamide) titanium, dimethyl zinc and high-purity water, controlling the temperature of the reaction cavity to be 150 ℃, circulating a zinc source 28 times (ZnO circulating 0.14 nm), heating the titanium source to 75 ℃, and circulating the titanium source 54 Times (TiO) 2 One cycle 0.055 nm), at SnS 2 Deposition of ZnO film on surface of filmAnd TiO 2 Film, znO film thickness is 4nm, tiO 2 The thickness of the film was 3nm.
(3) And (3) placing the sample in a muffle furnace for annealing at 350 ℃ for 9 hours to obtain the photo-anode based on the cocatalyst.
The morphology of the cocatalyst-based photoanode is shown in figure 1. From FIG. 1, it can be seen that SnS 2 Vertical FTO growth on nanoplatelets. ALD and heat treatment without altering SnS 2 The appearance of the nano-sheet is beneficial to the ordered transmission of photogenerated carriers.
The above-described co-catalyst based photoanode is assembled into a photoelectrochemical cell, and then water is decomposed by light at different voltages. To serve as a control, snS is loaded 2 The FTO of the film was used as a working electrode and a platinum mesh was used as a counter electrode, and water was photodecomposition under the same conditions, and the results are shown in fig. 2. As can be seen from FIG. 2, at 1.23V RHE The dark current (dotted line in the figure) can be basically ignored, and the photocurrent of the photoelectrode prepared by the method of the embodiment can reach 1.97mA/cm 2 ，V on Negative shift to 0.21V RHE The method comprises the steps of carrying out a first treatment on the surface of the While SnS 2 The photocurrent of the film is only 0.15mA/cm 2 。
Example 2
A photo-anode based on a cocatalyst and a preparation method thereof specifically comprise the following steps:
substantially as in example 1, except that in step (2), znO and TiO of different cycle numbers are deposited by controlling ALD technique 2 Thereby obtaining SnS with different interface quality 2 /ZTA。
The photoelectrodes prepared above were assembled into photoelectrochemical cells, and then water was decomposed by light at different voltages, and the results are shown in fig. 3. As can be seen from FIG. 3, at 1.23V RHE The photocurrent of the photoelectrode prepared by the invention can reach 1.97mA/cm 2 The method comprises the steps of carrying out a first treatment on the surface of the With SnS 2 The photocurrent of the sample as the working electrode was only 0.15mA/cm 2 。
Comparative example 1
Substantially the same as in example 1 except that in step (2), there is noAt SnS 2 The surface is covered with any film (named SnS 2 /A)。
The photoelectrodes prepared above were assembled into photoelectrochemical cells, and then water was decomposed by light at different voltages, and the results are shown in fig. 4. As can be seen from FIG. 4, since S element overflows a lot and a lot of O doping is introduced during annealing, at 1.23V RHE At a voltage which results in a photocurrent of the working electrode of only 0.72mA/cm 2 。
Comparative example 2
Substantially as in example 1, except that in step (3), the sample was not subjected to annealing treatment (designated as SnS 2 /ZT)。
The photoelectrodes prepared above were assembled into photoelectrochemical cells, and then water was decomposed by light at different voltages, and the results are shown in fig. 4. As can be seen from FIG. 4, since S element in the metal sulfide cannot overflow, the metal sulfide is simply coated with the surface film and ZnTiO on the surface x S y The cocatalyst was not formed, thus at 1.23V RHE At a voltage which results in a photocurrent of the working electrode of only 0.26mA/cm 2 。
It is apparent that the above examples are given by way of illustration only and are not limiting of the embodiments. Other variations and modifications of the present invention will be apparent to those of ordinary skill in the art in light of the foregoing description. It is not necessary here nor is it exhaustive of all embodiments. And obvious variations or modifications thereof are contemplated as falling within the scope of the present invention.
Claims (10)
1. The photo-anode based on the cocatalyst comprises a conductive substrate, and is characterized in that an n-type metal sulfide nano array is arranged on the surface of the conductive substrate; the surface of the n-type metal sulfide nano array is sequentially provided with a zinc oxide film and a titanium dioxide film, and S in the n-type metal sulfide nano array is combined with the zinc oxide film and the titanium dioxide film to obtain a cocatalyst; the cocatalyst is ZnTiO x S y 。
2. The promoter-based photoanode of claim 1, wherein the n-type metal sulfide is SnS 2 、In 2 S 3 、ZnIn 2 S 4 And CdIn 2 S 4 One or more of the following.
3. The promoter-based photoanode of claim 1, wherein the thickness of the n-type metal sulfide nanoarray is 0.5 μm-2 μm; the thickness of the zinc oxide film is 0.1nm-10nm; the thickness of the titanium dioxide film is 0.1nm-20nm.
4. The promoter-based photoanode of claim 1, wherein the conductive substrate is fluorine doped tin oxide conductive glass.
5. The method for preparing a cocatalyst-based photoanode according to any one of claims 1 to 4, comprising the steps of,
s1, preparing an n-type metal sulfide nano array on a pretreated conductive substrate to obtain a conductive substrate loaded with the n-type metal sulfide nano array;
s2, sequentially depositing a zinc oxide film and a titanium dioxide film on the conductive substrate loaded with the n-type metal sulfide nano array in the S1 to obtain a photo-anode; the deposition mode is an atomic layer deposition method;
and S3, carrying out annealing treatment on the photo-anode in the S2, and combining the S in the n-type metal sulfide nano array with the zinc oxide film and the titanium dioxide film to form a cocatalyst, so as to obtain the photo-anode based on the cocatalyst.
6. The method of preparing a co-catalyst based photoanode according to claim 5, wherein in S1, the method of preparing an n-type metal sulfide nano-array loaded conductive substrate comprises the steps of:
immersing the pretreated conductive substrate into n-type metal sulfide precursor solution, and reacting for 1-2 h at 70-80 ℃ to obtain the conductive substrate loaded with the n-type metal sulfide nano array; the n-type metal sulfide precursor solution is obtained by dissolving a metal salt and a sulfur source in a solvent.
7. The method of preparing a cocatalyst-based photoanode according to claim 6, characterized in that the sulfur source is thioacetamide and/or thiourea.
8. The method of claim 5, wherein in S2, the zinc oxide film is obtained by reacting a zinc source and an oxygen source at 120 ℃ to 200 ℃.
9. The method of claim 5, wherein in S2, the titanium oxide film is obtained by reacting a titanium source and an oxygen source at 120 ℃ to 200 ℃.
10. The method of claim 5, wherein in S3, the annealing is performed at 150-450 ℃ for 2-10 hours.
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