CN115747861A - Copper bismuth sulfur-based photoelectrochemical cell for hydrogen production by sunlight full-hydrolysis - Google Patents

Copper bismuth sulfur-based photoelectrochemical cell for hydrogen production by sunlight full-hydrolysis Download PDF

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CN115747861A
CN115747861A CN202211444720.8A CN202211444720A CN115747861A CN 115747861 A CN115747861 A CN 115747861A CN 202211444720 A CN202211444720 A CN 202211444720A CN 115747861 A CN115747861 A CN 115747861A
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layer
bis
back electrode
photoelectrochemical cell
electrode layer
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黄定旺
乔梁
王康
李笑玮
夏鹏飞
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Yangtze River Delta Research Institute of UESTC Huzhou
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Yangtze River Delta Research Institute of UESTC Huzhou
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Priority to PCT/CN2023/104645 priority patent/WO2024103785A1/en
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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
    • 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

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Abstract

The invention relates to a copper bismuth sulfenyl photoelectrochemical cell for preparing hydrogen by sunlight full-hydrolysis, which comprises Cu 3 BiS 3 Photocathode and Cu 3 BiS 3 Photoanode, cu 3 BiS 3 The photocathode comprises a first back electrode layer and Cu laminated on the first back electrode layer 3 BiS 3 Absorption layer, cdS/TiO 2 A double buffer layer and a hydrogen evolution promoter layer; cu 3 BiS 3 The photo-anode comprises a second back electrode layer and TiO laminated on the second back electrode layer 2 /CdS double buffer layer, cu 3 BiS 3 An absorption layer and an oxygen evolution promoter layer; the first back electrode layer is connected with the second back electrode layer through a lead.In the photoelectrochemical cell, the photocathode and the photoanode both adopt p-type semiconductor Cu 3 BiS 3 Compared with the traditional p-n series photoelectrochemical cell, the material serving as the light absorption material has the advantage of high light absorption utilization rate, and the light-to-hydrogen conversion efficiency of the cell is improved.

Description

Copper bismuth sulfur-based photoelectrochemical cell for hydrogen production by sunlight full-hydrolysis
Technical Field
The invention relates to the field of hydrogen production by photoelectrochemical water decomposition, in particular to a copper bismuth sulfide-based photoelectrochemical cell for producing hydrogen by sunlight full water decomposition.
Background
Solar energy is increasingly favored as a clean energy source. There are many ways of utilizing solar energy, in which the hydrogen gas is produced by photoelectrochemically decomposing water, and solar energy is stored and reused in the form of hydrogen energy, which is receiving attention from more and more researchers. Through the process, the light abandoning phenomenon existing in the traditional photovoltaic power generation way due to the fluctuation and intermittence of light energy can be effectively solved. In a photoelectrochemical water splitting system, an n-type semiconductor is generally weaker in light absorption capacity when used as a photo-anode, so that the overall efficiency of a photo-electrode is low, the photo-electrode made of the existing single p-type semiconductor often needs to be assisted by an external bias voltage to fully split water to prepare hydrogen, and electric energy still needs to be consumed in the process. Therefore, the realization of the efficient and stable unbiased photoelectrochemical water splitting hydrogen production of the single p-type semiconductor has important significance in the whole water photolysis field.
Disclosure of Invention
In view of the technical problems in the prior art, it is a primary object of the present invention to provide a single p-type semiconductor Cu without external bias 3 BiS 3 Copper bismuth sulfur-based photoelectrochemical cell constructed by materials and used for hydrogen production by sunlight full-hydrolysis and preparation method thereof, wherein p-type semiconductor Cu is selected as the photoelectrochemical cell 3 BiS 3 Material as light absorption layer material to construct Cu 3 BiS 3 A base photo-anode, and a conventional photo-anode made of n-type semiconductor (such as BiVO) 4 、Fe 2 O 3 、Ta 3 N 5 Etc.) as a light absorbing material, the photoanode of the present invention is arranged by a unique structure, compared to Cu 3 BiS 3 Base photocathode series connectionForming a single p-type semiconductor Cu 3 BiS 3 The photoelectrochemical cell for preparing hydrogen by fully hydrolyzing water based on the base material does not need to apply bias voltage, can perform the oxygen evolution half-reaction of the splitting water on the photo-anode, and can perform the hydrogen evolution half-reaction of the splitting water on the photo-cathode simultaneously, thereby improving the light absorption capacity of the photo-anode. Compared with the traditional p-n series photoelectrochemical cell, the photoelectrochemical cell has the advantage of high light absorption utilization rate, and further improves the light-to-hydrogen efficiency of the cell.
Based on the above purpose, the invention at least provides the following technical scheme:
a copper bismuth sulfur-based photoelectrochemical cell for hydrogen production by sunlight full-hydrolysis comprises Cu 3 BiS 3 Photocathode and Cu 3 BiS 3 Photo-anode of said Cu 3 BiS 3 Photocathode and Cu 3 BiS 3 The photo-anodes are connected in series through a lead;
the Cu 3 BiS 3 The photocathode comprises a first back electrode layer and Cu sequentially laminated on the first back electrode layer 3 BiS 3 Absorption layer, cdS/TiO 2 A double buffer layer and a hydrogen evolution promoter layer;
the Cu 3 BiS 3 The photo-anode comprises a second back electrode layer and TiO sequentially laminated on the second back electrode layer 2 /CdS double buffer layer, cu 3 BiS 3 An absorption layer and an oxygen evolution promoter layer;
the first back electrode layer is connected with the second back electrode layer through a lead, the second back electrode layer is made of a transparent conductive substrate, and sunlight irradiates the photoanode along the bottom side of the transparent conductive substrate of the photoanode.
Furthermore, the hydrogen evolution catalyst promoter layer adopts Pt nano particles or MoS x And (3) nanoparticles.
Furthermore, the oxygen evolution promoter layer adopts Co-Pi nano particles or Ni metal film.
Further, the Cu 3 BiS 3 The absorption layer is prepared by a spray pyrolysis method, and the Cu 3 BiS 3 The thickness of the absorption layer is 800-1100nm。
Further, the CdS buffer layer is 70-90 nm thick, and the TiO buffer layer is TiO-doped 2 The thickness of the buffer layer is 40-60 nm.
Further, in the hydrogen evolution promoter layer, the grain size of the Pt nano-particles is 15-25 nm.
Further, in the hydrogen evolution promoter layer, the MoS x The thickness of the nanoparticle layer is 15 to 25nm.
Further, in the oxygen evolution promoter layer, the particle size of the Co-Pi nano particles is 15-25 nm.
Furthermore, in the oxygen evolution promoter layer, the thickness of the Ni metal thin film layer is 2-3 nm.
Further, the first back electrode layer is a Mo electrode layer; and the second back electrode layer is an FTO conductive substrate.
Compared with the prior art, the invention at least has the following beneficial effects:
the photo-anode part of the conventional tandem photoelectrochemical cell is usually selected from n-type semiconductor (such as BiVO) 4 、Fe 2 O 3 、Ta 3 N 5 Etc.) as a light absorbing material, the invention selects p-type semiconductor Cu 3 BiS 3 The material is used as a light absorption layer, and a photoanode is constructed by a special structure arrangement, and Cu 3 BiS 3 The photocathode is serially connected to form the photoelectrochemical cell, so that the light absorption capacity of the photoelectrochemical cell is obviously improved, and the light-to-hydrogen efficiency of the cell is further improved. The photoelectrochemical cell can realize a single p-type semiconductor Cu under the irradiation of sunlight without external bias 3 BiS 3 The hydrogen is produced by efficiently photolyzing water.
On the other hand, the photoelectrochemical cell of the invention adopts single Cu 3 BiS 3 The material is used as a light absorption material, has the characteristics of no toxicity, environmental protection and low cost, is simple in preparation facilities and simple in preparation process, and can realize cleanness, environmental protection, environmental friendliness and regeneration in the process of hydrogen production by photolysis.
Drawings
FIG. 1 shows a schematic view of the present inventionExamples Cu 3 BiS 3 Spray pyrolysis of the absorber layer is a schematic preparation.
FIG. 2 shows Cu in the present invention 3 BiS 3 The structure of each layer of the photocathode is shown schematically.
FIG. 3 shows Cu in the present invention 3 BiS 3 The structure of each layer of the photo-anode is shown schematically.
FIG. 4 shows Cu in the present invention 3 BiS 3 Assembly and operation of the base photoelectrochemical cell.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings of the present invention, and the described embodiments are only a part of the embodiments of the present invention, not all of the embodiments. Other embodiments, which can be obtained by persons skilled in the art without any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention. The experimental methods described in the following examples are all conventional methods unless otherwise specified; the reagents and materials, unless otherwise indicated, are commercially available from a public disclosure.
Spatially relative terms, such as "under," "below," "lower," "over," "above," "upper," and the like, may be used herein to explain the positioning of one element relative to a second element. These terms are intended to encompass different orientations of the device in addition to different orientations than those depicted in the figures.
In addition, terms such as "first", "second", and the like, are used to describe various elements, layers, regions, sections, and the like and are not intended to be limiting. The use of "having," "containing," "including," and the like, are open-ended terms that indicate the presence of stated elements or features, but do not exclude additional elements or features. Unless the context clearly dictates otherwise.
The embodiment of the invention provides a copper bismuth sulfide-based photoelectrochemical cell for hydrogen production by sunlight full-hydrolysis, wherein the photoelectrochemical cell adopts a p-type semiconductor Cu 3 BiS 3 Material as light absorption layer material for constructing Cu 3 BiS 3 Photocathode and Cu 3 BiS 3 The photo-anode, the photo-anode and the photo-cathode are connected in series through a lead to form the photoelectrochemical cell.
The Cu 3 BiS 3 The cathode comprises a first back electrode layer and Cu sequentially stacked on the first back electrode layer 3 BiS 3 Absorption layer, cdS/TiO 2 A double buffer layer and a hydrogen evolution promoter layer. In a preferred embodiment, the first back electrode layer is a Mo electrode layer deposited on the substrate.
Cu 3 BiS 3 The absorption layer is prepared by a spray pyrolysis method, wherein the spray pyrolysis method is used for preparing a spraying precursor liquid. CuCl with the concentration of 1.9-2.3 mol/L and excessive thiourea are dissolved in dimethyl sulfoxide solvent and stirred for 2-3 h until the solution is clear to obtain solution (1), biCl with the concentration of 0.6-0.9 mol/L is added 3 Dissolving excessive thiourea in a dimethyl sulfoxide solvent, stirring for 2-3 h until the solution is clear to obtain a solution (2), and mixing the solution (1) and the solution (2) for 4-5 h to obtain a spray pyrolysis precursor solution.
Then, preparation work before spraying is carried out, and a spray pyrolysis device is set up according to the mode of fig. 1, including cleaning of the Mo-plated substrate, preheating of the heating substrate and assembly of the spray head. The Mo substrate is cut into rectangular slices with a certain size according to actual needs, and is ultrasonically cleaned in alcohol and acetone solvents for 45-60 min respectively; the heating substrate is preheated to 370-400 ℃, and the distance between the spray head and the heating substrate is 15-25 cm. Pouring the precursor liquid into a pre-storage cavity for spraying after the preparation is finished, wherein the gas flow is 17-20L/min during spraying, the spraying time is 300-420 s, and the Cu prepared by spray pyrolysis 3 BiS 3 The layer thickness is 800-1100 nm. Obtaining a structure of Mo/Cu 3 BiS 3 The electrode sheet of (1).
The CdS buffer layer is prepared by chemical water bath deposition method, and 10-13 mmol/L of CdSO is added 4 Dissolving 0.2-0.3 mol/L thiourea and 10-13 mol/L ammonia water in ultrapure water to obtain a chemical water bath reaction solution; then heating the reaction solution to 55-65 ℃; the structure is Mo/Cu 3 BiS 3 The electrode slice is placed in a thermal reaction solution, the chemical water bath time is 12-15 min, and the prepared CThe thickness of the dS layer is 70-90 nm, and the obtained structure is Mo/Cu 3 BiS 3 Electrode sheet of CdS.
TiO 2 The buffer layer is prepared by an atomic layer deposition process and has a Mo/Cu structure 3 BiS 3 The electrode plate of the/CdS is arranged in a vacuum cavity of the atomic layer deposition equipment, the temperature of the cavity is set to be 100-130 ℃, titanium tetra (dimethylamino) is selected as a titanium source, ultrapure water is used as an oxygen source, the number of deposition cycles is set to be 900-1000 cycles, and deposited TiO is deposited 2 The thickness of the layer is 40-60 nm, and the obtained structure is Mo/Cu 3 BiS 3 /CdS/TiO 2 The electrode sheet of (1).
Finally, in the structure Mo/Cu 3 BiS 3 /CdS/TiO 2 Depositing a hydrogen evolution catalyst promoter layer on the electrode sheet to obtain Cu 3 BiS 3 A photocathode. In the preferred embodiment, the hydrogen evolution promoter layer is made of Pt nanoparticles, the Pt nanoparticles are prepared by a photoelectric deposition process, and a photoelectric deposition reaction solution is prepared first. 0.9 to 1.1mol/L of Na 2 SO 4 And 0.95-1.1 mmol/L H 2 PtCl 6 Dissolving in ultrapure water to prepare a reaction solution for photoelectric deposition; then the structure is Mo/Cu 3 BiS 3 /CdS/TiO 2 The electrode slice is used as a working electrode, the Pt slice is used as a counter electrode, ag/AgCl is used as a reference electrode, and the photoelectric deposition with the duration of 26-33 s is carried out by selecting the deposition potential of-0.095-0.11V under the irradiation of simulated sunlight. The thickness of the prepared Pt nano particle layer is 15-25 nm, and the obtained structure is Mo/Cu 3 BiS 3 /CdS/TiO 2 Electrode sheet of-Pt is final Cu 3 BiS 3 The structure diagram of the photocathode is shown in fig. 2.
In another preferred embodiment, the hydrogen evolution promoter layer is a photo-electrodeposited MoS x Nanoparticles, wherein x > 0. Firstly, preparing a photoelectric deposition reaction solution, and adding 2.6-3.2 mmol/L (NH) 4 ) 2 [MoS 4 ]With 0.45 to 0.53mol/L of Na 2 SO 4 Dissolving in ultrapure water to prepare a reaction solution for photoelectric deposition; the structure is Mo/Cu 3 BiS 3 /CdS/TiO 2 The electrode plate of (1) is used as a working electrode, the Pt plate is used as a counter electrode, and Ag/AgCl is used as a referenceAn electrode; selecting a deposition potential of-0.18 to-0.21V under the irradiation of simulated sunlight, and carrying out photoelectric deposition for 15-25 min. Prepared MoS x The thickness of the nano-particle layer is 15-25 nm, and the obtained structure is Mo/Cu 3 BiS 3 /CdS/TiO 2 -MoS x Electrode sheet of (2) is final Cu 3 BiS 3 The schematic structure of the photocathode is shown in fig. 2.
The Cu 3 BiS 3 The base light anode comprises a second back electrode layer and TiO sequentially laminated on the second back electrode layer 2 /CdS double buffer layer, cu 3 BiS 3 An absorption layer and an oxygen evolution promoter layer. The second back electrode layer is a transparent conductive substrate, and in a preferred embodiment, the second back electrode layer is an FTO conductive substrate. The first back electrode layer is connected with the second back electrode layer through a lead.
TiO 2 A buffer layer arranged on the second back electrode layer and a CdS buffer layer arranged on the TiO 2 On the buffer layer, tiO is formed 2 CdS double buffer layer, tiO 2 The thickness of the buffer layer is 40-60nm, the thickness of the CdS buffer layer is 70-90nm, cu is added in the buffer layer, and the buffer layer is made of Cu or Cu alloy 3 BiS 3 The thickness of the absorption layer is 800-1100 nm, wherein, tiO 2 Buffer layer, cdS buffer layer, cu 3 BiS 3 The preparation method and the technological parameters of the absorption layer are the same as those of the Cu 3 BiS 3 The structural layers in the photocathode are the same.
An oxygen evolution promoter layer deposited on the FTO/TiO 2 /CdS/Cu 3 BiS 3 To obtain final Cu on the electrode sheet 3 BiS 3 And (6) a photo-anode. In a preferred embodiment, the oxygen evolution promoter is selected from Co-Pi nanoparticles. The Co-Pi nano particles are obtained by adopting a photoelectric deposition process, firstly preparing a photoelectric deposition reaction solution, and adding 0.85-0.11 mmol/L Co (NO) 3 )·6H 2 O, 0.85-0.11 mol/L NaH 2 PO 4 And 0.85 to 0.11mol/L of Na 2 HPO 4 Dissolving in ultrapure water to obtain reaction solution for photoelectric deposition, and mixing 2 /CdS/Cu 3 BiS 3 The electrode plate of (1) is used as a working electrode, the Pt plate is used as a counter electrode, the Ag/AgCl is used as a reference electrode, and the electrode plate is irradiated by simulated sunlightSelecting a deposition potential of-0.2V to-0.3V, performing photoelectric deposition for 85-95 s to obtain Co-Pi nanoparticles with a thickness of 15-25 nm and an obtained FTO/TiO structure 2 /CdS/Cu 3 BiS 3 The electrode sheet of-Co-Pi is the final Cu 3 BiS 3 The structure schematic diagram of the photo-anode is shown in fig. 3.
In another preferred embodiment, the oxygen evolution promoter is a Ni metal film prepared by a thermal evaporation coating method, and the preparation method comprises the following specific steps: ni metal particles are used as a target material, and the vapor deposition air pressure is controlled to be 0.95 multiplied by 10 -6 ～1.05×10 -6 Pa, the evaporation rate is controlled to be 0.025-0.03 nm/s, the evaporation thickness is set to be 2-3 nm, and the obtained structure is FTO/TiO 2 /CdS/Cu 3 BiS 3 Electrode sheet of-Ni of final Cu 3 BiS 3 The structure diagram of the photo-anode is shown in fig. 3.
Mixing Cu 3 BiS 3 Mo electrode layer and Cu in photocathode 3 BiS 3 FTO electrode layers of the photo-anode are connected in series, cu 3 BiS 3 Photocathode and Cu 3 BiS 3 The photoanodes are packaged in parallel to obtain Cu 3 BiS 3 Base photoelectrochemical cell, as shown in FIG. 4, in Cu 3 BiS 3 When the photoelectrochemical cell works, part of sunlight is from Cu 3 BiS 3 The incident of the hydrogen evolution promoter side of the photocathode is absorbed and utilized, and part of sunlight is absorbed from Cu 3 BiS 3 Incident light from the back electrode side of the photo-anode is absorbed and utilized, cu 3 BiS 3 The photocathode part receives illumination to excite electrons to enter the electrolyte for hydrogen evolution half reaction, and Cu 3 BiS 3 The photoanode part receives illumination to excite a cavity to enter the electrolyte for oxygen evolution half reaction, thereby realizing single Cu 3 BiS 3 The sunlight of the semiconductor is used for decomposing water to produce hydrogen.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.

Claims (10)

1. The copper bismuth sulfur-based photoelectrochemical cell for hydrogen production by sunlight full-hydrolysis is characterized by comprising Cu 3 BiS 3 Photocathode and Cu 3 BiS 3 Photo-anode of said Cu 3 BiS 3 Photocathode and Cu 3 BiS 3 The photo-anodes are connected in series through a lead;
the Cu 3 BiS 3 The photocathode comprises a first back electrode layer and Cu sequentially laminated on the first back electrode layer 3 BiS 3 Absorption layer, cdS/TiO 2 A double buffer layer and a hydrogen evolution promoter layer;
the Cu 3 BiS 3 The photo-anode comprises a second back electrode layer and TiO sequentially laminated on the second back electrode layer 2 /CdS double buffer layer, cu 3 BiS 3 An absorption layer and an oxygen evolution promoter layer;
the first back electrode layer is connected with the second back electrode layer through a wire, the second back electrode layer is made of a transparent conductive substrate, and sunlight irradiates the photo anode along the bottom side of the transparent conductive substrate of the photo anode.
2. The photoelectrochemical cell of claim 1, wherein the hydrogen evolution promoter layer is selected from Pt nanoparticles or MoS x And (3) nanoparticles.
3. The photoelectrochemical cell of claim 1, wherein the oxygen evolution promoter layer is selected from Co-Pi nanoparticles or Ni metal thin films.
4. The photoelectrochemical cell of one of claims 1 to 3, wherein the Cu is 3 BiS 3 The absorption layer is prepared by a spray pyrolysis method, and the Cu 3 BiS 3 The thickness of the absorption layer is 800-1100 nm.
5. According to the claimThe photoelectrochemical cell of any one of claims 1 to 3, wherein the CdS buffer layer has a thickness of 70 to 90nm, and the TiO buffer layer has a thickness of TiO 2 The thickness of the buffer layer is 40-60 nm.
6. The photoelectrochemical cell according to one of claims 1 to 3, wherein the Pt nanoparticles in the hydrogen evolution promoter layer have a particle size of 15 to 25nm.
7. The photoelectrochemical cell according to one of claims 1 to 3, wherein, in the hydrogen evolution promoter layer, the MoS x The thickness of the nanoparticle layer is 15 to 25nm.
8. The photoelectrochemical cell of one of claims 1 to 3, wherein the Co-Pi nanoparticles have a particle size of 15 to 25nm in the oxygen evolution promoter layer.
9. The photoelectrochemical cell according to any one of claims 1 to 3, wherein the Ni metal thin film layer has a thickness of 2 to 3nm in the oxygen evolution promoter layer.
10. The photoelectrochemical cell according to any one of claims 1 to 3, wherein the first back electrode layer is a Mo electrode layer; and the second back electrode layer is an FTO conductive substrate.
CN202211444720.8A 2022-11-18 2022-11-18 Copper bismuth sulfur-based photoelectrochemical cell for hydrogen production by sunlight full-hydrolysis Pending CN115747861A (en)

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CN202211444720.8A CN115747861A (en) 2022-11-18 2022-11-18 Copper bismuth sulfur-based photoelectrochemical cell for hydrogen production by sunlight full-hydrolysis
PCT/CN2023/104645 WO2024103785A1 (en) 2022-11-18 2023-06-30 Copper-bismuth-sulfur-based photoelectrochemical cell for hydrogen production by means of solar overall water splitting

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