CN110965074A - Method for preparing composite film photoelectrode - Google Patents
Method for preparing composite film photoelectrode Download PDFInfo
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- CN110965074A CN110965074A CN201911300085.4A CN201911300085A CN110965074A CN 110965074 A CN110965074 A CN 110965074A CN 201911300085 A CN201911300085 A CN 201911300085A CN 110965074 A CN110965074 A CN 110965074A
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
- C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
- C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- 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 method for preparing a composite film photoelectrode, which comprises the following steps: soaking the platinized titanium conductive glass serving as an electrode base material in a hydrogen peroxide solution, washing the electrode base material with water, and performing ultrasonic treatment to form a thin film electrode layer; then placing the mixture into a sodium hydroxide solution for ultrasonic treatment, then repeatedly carrying out ultrasonic cleaning by using deionized water, and drying; finally, in a sodium hypochlorite electrolytic tank, electropolishing and ultrasonically washing to prepare and dry an electrode matrix; pretreatment of an electrode substrate: adding graphene into a mixed solution of sodium carboxymethylcellulose and styrene to obtain a coating solution; spin-coating the coating solution on an electrode substrate, and annealing to obtain an electrode preform; preparing a composite film photoelectrode: preparing an LDH electrode from the electrode preform by using an electrodeposition method, placing the prepared LDH electrode in a muffle furnace, and calcining and air-cooling to prepare an MMO electrode; and preparing the MMO photoelectrode covered by the lead dioxide film by using an electrodeposition method, and washing and drying the MMO photoelectrode by using water.
Description
Technical Field
The invention belongs to the technical field of photoelectrodes, and relates to a method for preparing a composite film photoelectrode.
Background
In order to reduce the consumption of fossil fuels and solve related environmental problems, the utilization rate of clean energy such as solar energy and hydrogen energy needs to be increased urgently, hydrogen production by photoelectrocatalysis and water decomposition can be effectively utilized to generate clean energy hydrogen, the photoelectrode is a new technology which can solve the problems of energy crisis and environmental pollution at the same time, and the photoelectrode is the key of the technology, so that the search for a proper photoelectrocatalysis electrode material and the improvement of a photoelectrode preparation method are very important.
In recent years, semiconductor thin films such as TiO2, SnO2, ZnO, etc., having unique properties and high activity have been in many research fields such as: optical devices, dye-sensitized solar cells (DSSC cells), high-efficiency photocatalysts, and the like have achieved wide applications and have attracted increasing research interest. These semiconductor thin films can be generally formed by a chemical wet process such as a casting method, a doctor blade method, a screen printing method, etc., and various physical methods including a sputtering method, a vapor deposition method, etc. In addition, the porphyrin molecules and the related derivatives thereof are also attracted attention and researched due to the potential application thereof in the fields of optics, photoelectrochemistry, sensing and the like, and the electrode compounded by the photoelectrode and the semiconductor material not only increases the absorption efficiency of light, but also accelerates the transmission and separation of carriers and improves the photoelectric water decomposition performance.
However, the method for preparing the composite thin film photoelectrode adopted in the prior art not only has a complex process, but also has poor surface quality of the prepared electrode, and the surface layer is easy to fall off or wear, so that the service life of the electrode is short.
Disclosure of Invention
The invention aims to provide a method for preparing a composite film photoelectrode, which solves the problems that the process for preparing the composite film photoelectrode is complex, the surface quality of the prepared photoelectrode is poor, and the surface layer is easy to fall off or wear, so that the service life of the photoelectrode is short in the prior art.
The technical scheme adopted by the invention is that the method for preparing the composite film photoelectrode comprises the following steps:
step 1, preparing an electrode substrate: soaking the platinum-plated titanium conductive glass serving as an electrode base material in a 25% hydrogen peroxide solution for 30min, then washing the electrode base material with deionized water, and then putting the electrode base material into an electrolyte for ultrasonic treatment for 30min to form a thin film electrode layer; then placing the mixture into a sodium hydroxide solution for ultrasonic treatment for 10min, then repeatedly carrying out ultrasonic cleaning by using deionized water, and drying; finally, electropolishing for 2-5 minutes in a sodium hypochlorite electrolytic tank at a voltage of 10V by using a metal sheet as an anode and graphite as a cathode, washing with ultrasonic water for more than three times for 5min each time to prepare an electrode substrate, and drying and storing;
step 2, pretreatment of an electrode substrate: adding graphene into a mixed solution of sodium carboxymethylcellulose and styrene to obtain a coating solution; spin-coating at least two layers of the coating solution on the electrode substrate obtained in the step 1, and annealing the electrode substrate to obtain an electrode preform;
step 3, preparing a composite film photoelectrode: preparing the LDH electrode from the electrode preform obtained in the step 2 by using an electrodeposition method, placing the prepared LDH electrode in a muffle furnace, burning the prepared LDH electrode to 800-; and connecting the prepared MMO electrode with a power supply, preparing the MMO photoelectrode covered by the lead dioxide film by using an electrodeposition method, washing with deionized water, and drying.
The invention is also characterized in that:
in the step 1, the electrolyte is prepared by dissolving perchlorate and azobisisobutylimidazoline in deionized water and stirring for 5min at the speed of 80-100 r/min.
In the step 2, adding graphene into the mixture according to the volume ratio of 2: 1, in the mixed solution of sodium carboxymethylcellulose and styrene, the volume ratio of graphene to the mixed solution is 1.5: 1, obtaining a coating solution.
The annealing treatment in the step 2 is to place the coated electrode substrate in an electric heating furnace, burn to 90-110 ℃ and maintain for 1-2 hours, and then air-cool.
The conditions for preparing the LDH electrode by using the electrodeposition method in the step 3 are as follows: and (3) depositing the electrode preform in a sodium hypochlorite electrolytic tank for 12h under the voltage with the deposition potential of-5V, washing with deionized water, performing ultrasonic treatment for three times by using the deionized water, and drying.
The condition for preparing the MMO photoelectrode covered by the lead dioxide film by using the electrodeposition method in the step 3 is as follows: putting lead dioxide into a dispersion medium solution, adding aluminum nitrate, connecting an MMO electrode with a power supply, carrying out electrophoretic deposition for 160-year and 200-second at the voltage of 100V, then washing with deionized water, carrying out ultrasonic treatment for 30min three times with the deionized water, and drying.
The invention has the beneficial effects that: the method solves the problems that the technical process for preparing the composite film photoelectrode is complex, the surface quality of the prepared electrode is poor, and the surface layer is easy to fall off or wear, so that the service life of the electrode is short in the prior art.
Detailed Description
The invention discloses a method for preparing a composite film photoelectrode, which comprises the following steps:
step 1, preparing an electrode substrate: soaking the platinum-plated titanium conductive glass serving as an electrode base material in a 25% hydrogen peroxide solution for 30min, then washing the electrode base material with deionized water, and then putting the electrode base material into an electrolyte for ultrasonic treatment for 30min to form a thin film electrode layer; then placing the mixture into a sodium hydroxide solution for ultrasonic treatment for 10min, then repeatedly carrying out ultrasonic cleaning by using deionized water, and drying; finally, electropolishing for 2-5 minutes in a sodium hypochlorite electrolytic tank at a voltage of 10V by using a metal sheet as an anode and graphite as a cathode, washing with ultrasonic water for more than three times for 5min each time to prepare an electrode substrate, and drying and storing;
step 2, pretreatment of an electrode substrate: adding graphene into a mixed solution of sodium carboxymethylcellulose and styrene to obtain a coating solution; spin-coating at least two layers of the coating solution on the electrode substrate obtained in the step 1, and annealing the electrode substrate to obtain an electrode preform;
step 3, preparing a composite film photoelectrode: preparing the LDH electrode from the electrode preform obtained in the step 2 by using an electrodeposition method, placing the prepared LDH electrode in a muffle furnace, burning the prepared LDH electrode to 800-; and connecting the prepared MMO electrode with a power supply, preparing the MMO photoelectrode covered by the lead dioxide film by using an electrodeposition method, washing with deionized water, and drying.
In the step 1, the electrolyte is prepared by dissolving perchlorate and azobisisobutylimidazoline in deionized water and stirring for 5min at the speed of 80-100 r/min.
In the step 2, adding graphene into the mixture according to the volume ratio of 2: 1, in the mixed solution of sodium carboxymethylcellulose and styrene, the volume ratio of graphene to the mixed solution is 1.5: 1, obtaining a coating solution.
The annealing treatment in the step 2 is to place the coated electrode substrate in an electric heating furnace, burn to 90-110 ℃ and maintain for 1-2 hours, and then air-cool.
The conditions for preparing the LDH electrode by using the electrodeposition method in the step 3 are as follows: and (3) depositing the electrode preform in a sodium hypochlorite electrolytic tank for 12h under the voltage with the deposition potential of-5V, washing with deionized water, performing ultrasonic treatment for three times by using the deionized water, and drying.
The condition for preparing the MMO photoelectrode covered by the lead dioxide film by using the electrodeposition method in the step 3 is as follows: putting lead dioxide into a dispersion medium solution, adding aluminum nitrate, connecting an MMO electrode with a power supply, carrying out electrophoretic deposition for 160-year and 200-second at the voltage of 100V, then washing with deionized water, carrying out ultrasonic treatment for 30min three times with the deionized water, and drying.
The invention discloses a method for preparing a composite film photoelectrode, which has the advantages that: the method solves the problems that the technical process for preparing the composite film photoelectrode is complex, the surface quality of the prepared electrode is poor, and the surface layer is easy to fall off or wear, so that the service life of the electrode is short in the prior art.
Claims (6)
1. A method of making a composite thin film photoelectrode comprising the steps of:
step 1, preparing an electrode substrate: soaking the platinum-plated titanium conductive glass serving as an electrode base material in a 25% hydrogen peroxide solution for 30min, then washing the electrode base material with deionized water, and then putting the electrode base material into an electrolyte for ultrasonic treatment for 30min to form a thin film electrode layer; then placing the mixture into a sodium hydroxide solution for ultrasonic treatment for 10min, then repeatedly carrying out ultrasonic cleaning by using deionized water, and drying; finally, electropolishing for 2-5 minutes in a sodium hypochlorite electrolytic tank at a voltage of 10V by using a metal sheet as an anode and graphite as a cathode, washing with ultrasonic water for more than three times for 5min each time to prepare an electrode substrate, and drying and storing;
step 2, pretreatment of an electrode substrate: adding graphene into a mixed solution of sodium carboxymethylcellulose and styrene to obtain a coating solution; spin-coating at least two layers of the coating solution on the electrode substrate obtained in the step 1, and annealing the electrode substrate to obtain an electrode preform;
step 3, preparing a composite film photoelectrode: preparing the LDH electrode from the electrode preform obtained in the step 2 by using an electrodeposition method, placing the prepared LDH electrode in a muffle furnace, burning the prepared LDH electrode to 800-; and connecting the prepared MMO electrode with a power supply, preparing the MMO photoelectrode covered by the lead dioxide film by using an electrodeposition method, washing with deionized water, and drying.
2. The method of claim 1, wherein the electrolyte in step 1 is prepared by dissolving perchlorate and azobisisobutyrimidazoline in deionized water and stirring at 80-100r/min for 5 min.
3. The method for preparing a composite thin film photoelectrode of claim 1 wherein in step 2, graphene is added to the composite thin film photoelectrode in a volume ratio of 2: 1, in the mixed solution of sodium carboxymethylcellulose and styrene, the volume ratio of graphene to the mixed solution is 1.5: 1, obtaining a coating solution.
4. The method of claim 1, wherein the annealing process in step 2 is carried out by placing the coated electrode substrate in an electric furnace, heating to 90-110 deg.C for 1-2 hours, and air cooling.
5. The method for preparing a composite thin film photoelectrode of claim 1, wherein the conditions for preparing the LDH electrode in step 3 using the electrodeposition method are as follows: and (3) depositing the electrode preform in a sodium hypochlorite electrolytic tank for 12h under the voltage with the deposition potential of-5V, washing with deionized water, performing ultrasonic treatment for three times by using the deionized water, and drying.
6. The method of claim 1, wherein the conditions for preparing the lead dioxide thin film covered MMO photoelectrode by electrodeposition in step 3 are as follows: putting lead dioxide into a dispersion medium solution, adding aluminum nitrate, connecting an MMO electrode with a power supply, carrying out electrophoretic deposition for 160-year and 200-second at the voltage of 100V, then washing with deionized water, carrying out ultrasonic treatment for 30min three times with the deionized water, and drying.
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| CN201911300085.4A CN110965074A (en) | 2019-12-16 | 2019-12-16 | Method for preparing composite film photoelectrode |
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| CN201911300085.4A CN110965074A (en) | 2019-12-16 | 2019-12-16 | Method for preparing composite film photoelectrode |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112251763A (en) * | 2020-08-20 | 2021-01-22 | 西北师范大学 | BiVO4NiOx composite photoelectrode and preparation method thereof |
| CN112981415A (en) * | 2021-02-25 | 2021-06-18 | 浙江大学 | Preparation method and application of layered double-metal hydroxide-based composite film |
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| CN101967017A (en) * | 2010-11-05 | 2011-02-09 | 北京化工大学 | Electrochemical device for wastewater treatment and method for treating wastewater by using same |
| CN104264179A (en) * | 2014-09-17 | 2015-01-07 | 中国科学院山西煤炭化学研究所 | Method for preparing graphene from raw graphite ores through electrolysis |
| CN108842168A (en) * | 2018-06-29 | 2018-11-20 | 太原理工大学 | A kind of two-step electrochemical method preparation g-C3N4/ MMO compound film optoelectronic pole |
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2019
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Patent Citations (3)
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| CN101967017A (en) * | 2010-11-05 | 2011-02-09 | 北京化工大学 | Electrochemical device for wastewater treatment and method for treating wastewater by using same |
| CN104264179A (en) * | 2014-09-17 | 2015-01-07 | 中国科学院山西煤炭化学研究所 | Method for preparing graphene from raw graphite ores through electrolysis |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112251763A (en) * | 2020-08-20 | 2021-01-22 | 西北师范大学 | BiVO4NiOx composite photoelectrode and preparation method thereof |
| CN112981415A (en) * | 2021-02-25 | 2021-06-18 | 浙江大学 | Preparation method and application of layered double-metal hydroxide-based composite film |
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