CN113337833A - Polythiophene compound/carbon fiber cloth water decomposition oxygen generation electrode and preparation method thereof - Google Patents
Polythiophene compound/carbon fiber cloth water decomposition oxygen generation electrode and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a polythiophene compound/carbon fiber cloth water decomposition oxygen generation electrode and a preparation method thereof. In the preparation method, thiophene monomers, lithium perchlorate and carbon fiber cloth are used as raw materials, and an electrochemical deposition method is utilized to obtain the polythiophene compound/carbon fiber cloth composite oxygen generation electrode. The method has the characteristics of simple manufacturing process, environmental protection, safety, low cost and good performance, and can realize industrial production. The product has very wide application potential in numerous fields of electrocatalysis water decomposition, energy conversion, storage and the like.
Description
Technical Field
The invention belongs to the field of electrocatalytic water decomposition of semiconductor polymers, and particularly relates to an oxygen generation electrode by decomposing water with polythiophene compounds/carbon fiber cloth and a preparation method thereof.
Background
Along with the progress of society and the development of science and technology, the living standard of people is greatly improved. Meanwhile, the energy problem caused by social development is more and more prominent. Today, traditional primary energy sources still account for a significant proportion. The environmental problems and resource shortage caused by the energy sources make us compel to develop green novel energy sources capable of sustainable development. Clean energy such as solar energy, wind energy and the like can be directly converted into electric energy, and the storage and conversion of the part of electric energy are worthy of further research. The new way to solve the above problems is to convert electric energy into chemical substances and store them by decomposing water electrically into hydrogen and oxygen. The high-performance catalyst can reduce the activation energy to be overcome in the water decomposition process, and greatly reduce the energy consumption.
For the electrolytic water reaction, the decomposition into two half reactions is generally carried out separately. The cathode generates hydrogen evolution reaction, which relates to the transfer of 2 electrons, and the anode generates oxygen evolution reaction, which relates to the transfer of 4 electrons, so the oxygen evolution reaction is more difficult, and the corresponding overpotential is higher. The search for efficient and practical electrode catalysts to accelerate the kinetic process of oxygen evolution reaction is always a research focus in the electrochemical field for nearly 20 years.
Currently, the most widely studied catalysts are noble metal-based catalysts (e.g., iridium oxide) which have the highest performance, and such metal-based catalysts are subject to environmental and cost problems in practical use. Therefore, it is very necessary to develop a high performance catalyst containing no metal.
Recently, there has been some work on flexible metal-free polymeric materials as functional catalysts for various electrocatalytic reactions, including oxygen evolution reactions. The proper band structure of the polymer can help dissociate water molecules and provide high activity for oxygen evolution reaction, but the electrochemical stability of the polymer electrode remains a major obstacle in practical applications.
Inspired by such research, the application focuses on the conductive polymer, and aims to improve the electrochemical stability of the electrode on the basis of improving the catalytic activity. The synthetic method of the polymer material is simple and cheap, the industrial preparation conditions are mature, and the electrochemical stability is good. The development of the polymer electrocatalysis electrode not only has important application in the fields of chemical industry, energy and the like, but also provides a new visual field for the research of electrocatalysis materials.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides the polythiophene compound/carbon fiber cloth water decomposition oxygen generation electrode with high electrochemical stability and simple synthesis method and the preparation method thereof.
The invention relates to a polythiophene compound/carbon fiber cloth water decomposition oxygen generation electrode, which comprises carbon fiber cloth and a polythiophene compound film formed on the carbon fiber cloth.
Preferably, the polythiophene compound thin film is formed by in-situ polymerization of thiophene monomers on the carbon fiber cloth through an electrochemical deposition reaction.
The thiophene monomer is preferably at least one of thiophene and thiophene in which the 3-position is substituted with an alkyl chain having 1 to 6 carbon atoms.
Preferably, the thickness of the polythiophene compound film is 20-100 nm.
Therefore, the catalysis performance of the polythiophene compound/carbon fiber cloth water decomposition oxygen generation electrode is excellent.
The invention relates to a preparation method of a polythiophene compound/carbon fiber cloth water decomposition oxygen generation electrode, which is characterized by comprising the following steps: preparing acetonitrile solution containing thiophene monomers and lithium perchlorate serving as electrolyte, taking carbon fiber cloth as a working electrode, soaking the carbon fiber cloth in the acetonitrile solution, polymerizing the thiophene monomers on the carbon fiber cloth in situ by using a constant-voltage electrochemical deposition method to form a polythiophene compound film, controlling the electrifying time within the range of 0.5-7 hours, taking out the working electrode after the electrodeposition process is finished, soaking the working electrode in pure water to remove impurities, and naturally drying to obtain the polythiophene compound/carbon fiber cloth water decomposition oxygen generation electrode.
According to the preparation method of the invention, a uniform polymer film can be synthesized, and the polymer electrode has high catalytic activity.
In the preparation method of the polythiophene compound/carbon fiber cloth water decomposition oxygen generation electrode, the carbon fiber cloth is preferably subjected to ultrasonic treatment for 5-10 minutes by using nitric acid with the concentration of 1-2 mol/L.
Therefore, the polymer can be more uniformly formed on the carbon cloth after the nitric acid treatment.
In the preparation method of the polythiophene compound/carbon fiber cloth water decomposition oxygen generation electrode, the concentration of lithium perchlorate in the acetonitrile solution is 0.1-0.2 mol/L; the concentration of the thiophene monomer is 0.005-0.01 mol/L.
This prevents the polymer from falling off the carbon cloth while ensuring the catalytic performance.
In the above method for preparing the electrode by decomposing water with the polythiophene compound/carbon fiber cloth, the deposition time of the constant-voltage electrochemical deposition is preferably 3 h.
Thereby, the catalytic performance can be made excellent.
In the above method for preparing the polythiophene compound/carbon fiber cloth oxygen electrode by decomposing water, preferably, the thiophene monomer is directly polymerized in situ on the surface of the carbon fiber cloth.
The invention also relates to the application of the electrode as an anode in oxygen production by water decomposition.
The polythiophene compound can generate controllable oxidation reaction in the catalytic oxygen evolution reaction process to form oxidized polythiophene with better catalytic performance and more stability.
Effects of the invention
The polythiophene compound/carbon fiber cloth electrode for water decomposition oxygen generation has high activity and good stability, is suitable for being used as an anode in water decomposition oxygen generation, has high shape freedom degree, contributes to miniaturization of a hydrolysis system, is low in cost and is suitable for large-scale production.
The manufacturing method of the polythiophene compound/carbon fiber cloth water decomposition oxygen generation electrode has the advantages of simple process, easy control and low cost, and can realize large-scale production.
Drawings
FIG. 1 is a digital photograph of an oxygen electrode prepared by decomposing water with polythiophene/carbon fiber cloth according to example 1.
FIG. 2 is a scanning electron micrograph of the polythiophene/carbon fiber cloth water-splitting oxygen generation electrode of example 1.
FIG. 3 is a TEM image of the water-splitting oxygen-generating electrode made of polythiophene/carbon fiber cloth of example 1.
FIG. 4 is a linear sweep voltammogram of the electrodes obtained in example 1 and comparative example 1.
Fig. 5 is a graph of current versus time in the potentiostatic stability cycling test over 48 hours for the electrode of example 1.
FIG. 6 is a schematic view showing a production process of the present invention.
Detailed Description
The preparation method of the polythiophene compound/carbon fiber cloth water decomposition oxygen generation electrode comprises the following steps.
First, a thiophene monomer and lithium perchlorate as an electrolyte were dissolved in acetonitrile to prepare an acetonitrile solution. In the embodiment of the invention, the thiophene monomer is selected from at least one of thiophene and thiophene of which the 3-position is substituted by alkyl chain with 1-6 carbon atoms. The concentration of the lithium perchlorate in the acetonitrile solution is 0.1-0.2mol/L, and the concentration of the thiophene monomer is 0.005-0.01 mol/L.
And (2) carrying out ultrasonic treatment on the carbon fiber cloth by using nitric acid, soaking the carbon fiber cloth with a proper area in the acetonitrile solution, taking the carbon fiber cloth as a working electrode, and carrying out in-situ polymerization on thiophene serving as a monomer on the carbon fiber cloth by using a constant-voltage electrochemical deposition method to form a polythiophene compound film, taking out the working electrode after the electrodeposition process is finished, soaking the working electrode in pure water to remove impurities, and naturally drying to obtain the polythiophene/carbon fiber cloth water decomposition oxygen generation electrode. The electrifying time of the constant-voltage electrochemical deposition can be controlled according to the required film thickness, the film thickness is preferably 20-100nm, and the electrifying time is preferably in the range of 0.5-7 hours, and more preferably 3 hours. The soaking time of the working electrode in pure water may be determined according to the film thickness, for example, 30 minutes. The time for the ultrasonic treatment is, for example, 5 to 10 minutes, and the nitric acid concentration is, for example, 1 to 2 mol/L. The carbon fiber cloth can be various types of carbon fiber cloth. The designated area of the carbon fiber cloth can be any area, and the carbon fiber cloth is divided into small pieces for use according to the required area. The thiophene monomers, lithium perchlorate and acetonitrile used in the invention can all adopt general products sold in the market.
Example 1:
a carbon fiber cloth of 0.5cm × 0.5cm (as an actual example, the actual area is described more clearly.) was ultrasonically treated with 1mol/L nitric acid for 5 minutes, and then ultrasonically washed with ethanol and water for use. In acetonitrile solution containing 0.1mol/L of lithium perchlorate and 0.005M of thiophene monomer, carbon fiber cloth treated by nitric acid is taken as a working electrode, a titanium net and a saturated calomel electrode are taken as a counter electrode and a reference electrode to form a three-electrode system, and constant current deposition is carried out for 3 hours under the external voltage of 1.73V, so that the thiophene monomer is polymerized on the carbon fiber cloth in situ to form the polythiophene film. And after the electrodeposition process is finished, taking out the working electrode, soaking the working electrode in pure water for 30 minutes to remove impurities, and naturally drying the electrode to obtain the polythiophene/carbon fiber cloth water decomposition oxygen generation electrode, wherein the thickness of the polythiophene film is 40 nm. The current density of the obtained polythiophene/carbon fiber cloth water-splitting oxygen-generating electrode is measured under the voltage of 1.7V relative to the standard hydrogen electrodeIs 20mA cm-2。
Example 2:
the carbon fiber cloth of 0.5cm multiplied by 0.5cm is treated by ultrasonic with 1mol/L nitric acid for 5 minutes and then cleaned by ultrasonic with ethanol and water for standby. In acetonitrile solution containing 0.1mol/L of lithium perchlorate and 0.005mol/L of thiophene monomer, carbon fiber cloth treated by nitric acid is used as a working electrode, a titanium mesh and a saturated calomel electrode are used as a counter electrode and a reference electrode to form a three-electrode system, and constant current deposition is carried out for 0.5 hour under the applied voltage of 1.73V. And after the electrodeposition process is finished, taking out the working electrode, soaking the working electrode in pure water for 30 minutes to remove impurities, and naturally drying the electrode to obtain the polythiophene/carbon fiber cloth water decomposition oxygen generation electrode, wherein the thickness of the polythiophene film is 20 nm. The current density of the polythiophene/carbon fiber cloth water-decomposing oxygen-generating electrode is 6.4mAcm under the voltage of 1.7V relative to the standard hydrogen electrode-2。
Example 3:
the carbon fiber cloth of 0.5cm multiplied by 0.5cm is treated by ultrasonic with 1mol/L nitric acid for 5 minutes and then cleaned by ultrasonic with ethanol and water for standby. In acetonitrile solution containing 0.1mol/L of lithium perchlorate and 0.005mol/L of thiophene monomer, carbon fiber cloth treated by nitric acid is used as a working electrode, a titanium net and a saturated calomel electrode are used as a counter electrode and a reference electrode to form a three-electrode system, and constant current deposition is carried out for 1 hour under the applied voltage of 1.73V. And after the electrodeposition process is finished, taking out the working electrode, soaking the working electrode in pure water for 30 minutes to remove impurities, and naturally drying the electrode to obtain the polythiophene/carbon fiber cloth water decomposition oxygen generation electrode. The current density of the polythiophene/carbon fiber cloth water decomposition oxygen generation electrode is measured to be 12.9mA cm under the voltage of 1.7V relative to the standard hydrogen electrode-2。
Example 4:
the carbon fiber cloth of 0.5cm multiplied by 0.5cm is treated by ultrasonic with 1mol/L nitric acid for 5 minutes and then cleaned by ultrasonic with ethanol and water for standby. In acetonitrile solution containing 0.1mol/L of lithium perchlorate and 0.005mol/L of thiophene monomer, carbon fiber cloth treated by nitric acid is used as a working electrode, a titanium net and a saturated calomel electrode are used as a counter electrode and a reference electrode to form a three-electrode system, and constant current deposition is carried out for 5 hours under the applied voltage of 1.73V. Electrodeposition processAnd after the operation is finished, taking out the working electrode, soaking the working electrode in pure water for 30 minutes to remove impurities, and naturally drying the working electrode to obtain the polythiophene/carbon fiber cloth water decomposition oxygen generation electrode, wherein the thickness of the polythiophene film is 100 nm. The current density of the polythiophene/carbon fiber cloth water decomposition oxygen generation electrode is measured to be 5.1mA cm under the voltage of 1.7V relative to the standard hydrogen electrode-2。
Example 5:
the carbon fiber cloth of 0.5cm multiplied by 0.5cm is treated by ultrasonic with 1mol/L nitric acid for 5 minutes and then cleaned by ultrasonic with ethanol and water for standby. In acetonitrile solution containing 0.1M of lithium perchlorate and 0.005mol/L of thiophene monomer, carbon fiber cloth treated by nitric acid is used as a working electrode, a titanium mesh and a saturated calomel electrode are used as a counter electrode and a reference electrode to form a three-electrode system, and constant current deposition is carried out for 7 hours under the applied voltage of 1.73V. And after the electrodeposition process is finished, taking out the working electrode, soaking the working electrode in pure water for 30 minutes to remove impurities, and naturally drying the electrode to obtain the polythiophene/carbon fiber cloth water decomposition oxygen generation electrode. The current density of the polythiophene/carbon fiber cloth water decomposition oxygen generation electrode is measured to be 4.8mA cm under the voltage of 1.7V relative to the standard hydrogen electrode-2。
Comparative example 1: preparation of commercial iridium oxide/carbon fiber cloth electrode
The commercialized iridium oxide nano particles purchased from a chemical platform are ground, 5mg of the commercialized iridium oxide nano particles are added into a small sample tube, 0.35mL of ultrapure water, 0.70mL of ethanol and 0.08mL of 5% nafion solution are added, ink is formed by ultrasonic treatment, 0.2mL of ink is dripped on carbon fiber cloth of 1cm x1cm, and the commercialized iridium oxide/carbon fiber cloth electrode is obtained by natural drying. Comparative example an electrode was prepared using a commercial noble metal oxide which is currently being studied more extensively, and performance was compared with examples.
The following observations and evaluations were made on the preparations, especially on the polythiophene compound/carbon fiber cloth obtained, based mainly on example 1.
FIG. 1 is a digital photograph of an oxygen electrode prepared by decomposing water with the polythiophene compound/carbon fiber cloth according to example 1. FIG. 2 is a scanning electron micrograph of the polythiophene compound/carbon fiber cloth water-splitting oxygen generation electrode prepared in example 1. FIG. 3 is a TEM photograph of the polythiophene compound/carbon fiber cloth water-splitting oxygen electrode prepared in example 1. From these photographs, it can be seen that the manner of electrochemical deposition can synthesize a very uniform high quality polymer film.
Fig. 4 is a linear sweep voltammogram measured in an oxygen saturated 0.1M KOH solution (pH 13.0) for a commercial iridium oxide/carbon fiber cloth electrode and polythiophene compound/carbon fiber cloth obtained in example 1 and comparative example 1.
FIG. 5 shows the current versus time plot for the 48 hour potentiostatic test for the electrode of example 1 at an applied voltage of 1.7V versus the standard hydrogen electrode, with no significant decay in the final state current compared to the initial current.
From the data in FIGS. 4-5, it can be seen that the use of the polythiophene/carbon cloth electrodes of the present invention as oxygen generation electrodes resulted in very high current densities with an overpotential of only 430mV at 10mA cm-2. In addition, the electrode has excellent electrocatalytic stability. After the constant voltage stability test for 48 hours, the current density can still be kept high.
Claims (10)
1. An oxygen electrode prepared by decomposing water with polythiophene compound/carbon fiber cloth comprises carbon fiber cloth and a polythiophene compound film formed on the carbon fiber cloth.
2. The polythiophene compound/carbon fiber cloth water splitting oxygen generation electrode of claim 1, wherein the polythiophene compound thin film is formed by in-situ polymerization of thiophene monomers on the carbon fiber cloth through an electrochemical deposition reaction.
3. The polythiophene compound/carbon fiber cloth water splitting oxygen generation electrode according to claim 2, wherein the thiophene monomer is at least one selected from thiophene and thiophene substituted by an alkyl chain having 1-6 carbon atoms at the 3-position.
4. A polythiophene compound/carbon cloth water splitting oxygen generation electrode according to any one of claims 1 to 3, wherein said polythiophene compound thin film has a thickness of 20-100 nm.
5. A preparation method of an oxygen electrode by decomposing water with polythiophene compounds/carbon fiber cloth is characterized by comprising the following steps:
preparing acetonitrile solution containing thiophene monomer and lithium perchlorate as electrolyte,
and (2) taking the carbon fiber cloth as a working electrode, dipping the carbon fiber cloth in the acetonitrile solution, polymerizing a thiophene monomer onto the carbon fiber cloth in situ by using a constant-voltage electrochemical deposition method to form a polythiophene compound film, controlling the electrifying time within the range of 0.5-7 hours, taking out the working electrode after the electrodeposition process is finished, soaking the working electrode in pure water to remove impurities, and naturally drying the working electrode to obtain the polythiophene compound/carbon fiber cloth water decomposition oxygen generation electrode.
6. The method for preparing an oxygen electrode by decomposing water with the polythiophene compound/carbon fiber cloth according to claim 5, wherein the carbon fiber cloth is subjected to ultrasonic treatment for 5-10 minutes by using nitric acid with the concentration of 1-2 mol/L.
7. The preparation method of the polythiophene compound/carbon fiber cloth water-splitting oxygen generation electrode according to claim 5 or 6, wherein the concentration of lithium perchlorate in the acetonitrile solution is 0.1-0.2 mol/L; the concentration of the thiophene monomer is 0.005-0.01 mol/L.
8. The preparation method of the polythiophene compound/carbon fiber cloth water decomposition oxygen generation electrode according to claim 5 or 6, wherein the energization time of the constant-voltage electrochemical deposition is 3 h.
9. The preparation method of the polythiophene compound/carbon fiber cloth water decomposition oxygen generation electrode according to claim 5 or 6, wherein the thiophene monomer is directly polymerized in situ on the surface of the carbon fiber cloth.
10. Use of an electrode according to any one of claims 1 to 4 or obtained by the method of manufacture according to any one of claims 5 to 9 as an anode in the production of oxygen by splitting water.
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| JP2021011260A JP7133661B2 (en) | 2020-02-14 | 2021-01-27 | Polythiophene-based compound/carbon fiber cloth electrode for generating water-splitting oxygen and method for producing the same |
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