CN111740126A - Chemical doping modification method for graphite felt electrode material of vanadium battery - Google Patents
Chemical doping modification method for graphite felt electrode material of vanadium battery Download PDFInfo
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- CN111740126A CN111740126A CN202010629705.5A CN202010629705A CN111740126A CN 111740126 A CN111740126 A CN 111740126A CN 202010629705 A CN202010629705 A CN 202010629705A CN 111740126 A CN111740126 A CN 111740126A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/96—Carbon-based electrodes
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/88—Processes of manufacture
- H01M4/8878—Treatment steps after deposition of the catalytic active composition or after shaping of the electrode being free-standing body
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/18—Regenerative fuel cells, e.g. redox flow batteries or secondary fuel cells
- H01M8/184—Regeneration by electrochemical means
- H01M8/188—Regeneration by electrochemical means by recharging of redox couples containing fluids; Redox flow type batteries
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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
- Y02E60/50—Fuel cells
Abstract
The invention provides a chemical doping modification method of a vanadium battery graphite felt electrode material, belonging to the field of green energy materials. After the graphite felt electrode material for the vanadium battery is subjected to chemical doping modification, the mass doping amount of iron is 0.2-0.5%, the mass doping amount of nickel is 0.01-0.05%, the water absorption rate is improved by 350-485%, after the graphite felt electrode material is used as a vanadium battery electrode, the specific capacitance is improved by 18-28%, and the energy efficiency is improved to 60-73%.
Description
Technical Field
The invention relates to a chemical doping modification method of a graphite felt electrode material of a vanadium battery, belonging to the field of green energy materials.
Background
With the development of society, the energy crisis is increasingly serious, even the sustainable renewable energy such as solar energy, wind energy or geothermal energy has the problem of non-continuity and unpredictability, in order to solve the problem, the national development and reform committee definitely proposes to research the key problems in high efficiency, energy conservation and energy storage, promotes the diversified development of the national energy structure, and requires the development of a high-capacity energy storage system with stability and reliability.
The all-vanadium redox flow battery has the characteristics of low cost, long service life, high conversion efficiency, support of frequent charging and discharging, environmental protection, no pollution, no noise and the like, and draws more and more attention.
The polyacrylonitrile-based graphite felt electrode has the advantages of large specific surface area, stability, good electrochemical performance and conductive property, and is suitable for being used as an electrode of a vanadium flow battery. However, the graphite felt has the problems of poor wettability, few active sites, low catalytic activity and the like in the electrolyte of the vanadium battery, so how to modify the graphite felt becomes one of the key technologies for the marketization of the vanadium battery.
Disclosure of Invention
Aiming at the technical problems, the invention provides a chemical doping modification method of a graphite felt electrode material of a vanadium battery, which comprises the steps of taking a polyacrylonitrile-based graphite felt as the electrode material of the vanadium battery, ultrasonically dispersing iron-nickel microsphere powder in the graphite felt, and carrying out chemical doping modification on the graphite felt in a potassium permanganate solution medium to obtain the vanadium battery electrode material with strong hydrophilicity, high electrochemical activity, high specific capacitance, small polarization and high energy efficiency.
The technical scheme of the invention is as follows:
ultrasonically cleaning a polyacrylonitrile-based graphite felt with deionized water, drying in an oven, ultrasonically dispersing iron-nickel microsphere powder in the graphite felt, taking out, soaking in a mixed solution of potassium permanganate and sulfuric acid, cleaning with deionized water, and drying in the oven to obtain the vanadium battery iron-nickel doped graphite felt modified electrode material with high electrochemical activity.
The chemical doping modification method of the graphite felt electrode material of the vanadium battery comprises the following steps:
(1) cutting the polyacrylonitrile-based graphite felt into the size of 5cm multiplied by 10cm, washing the polyacrylonitrile-based graphite felt with deionized water once, and then soaking the polyacrylonitrile-based graphite felt in the deionized water for ultrasonic cleaning for 15 to 30 minutes;
(2) taking out the polyacrylonitrile-based graphite felt, and drying in a drying oven at 45 ℃;
(3) putting the iron-nickel microsphere powder into deionized water, and dispersing the iron-nickel microsphere powder into suspension A by ultrasonic waves;
(4) putting the dried polyacrylonitrile-based graphite felt into the suspension A, continuing ultrasonic oscillation for 10-15 minutes to uniformly disperse the iron-nickel microspheres into the pores of the polyacrylonitrile-based graphite felt, and drying in a drying oven at 45 ℃ to obtain a polyacrylonitrile-based graphite felt B deposited with the iron-nickel microspheres;
(5) preparing a mixed solution of potassium permanganate and sulfuric acid, enabling the molar concentration of the potassium permanganate in the mixed solution to be 0.3-0.47 mol/L and the molar concentration of the sulfuric acid to be 0.05-0.1 mol/L, standing for 5-10 minutes, and uniformly mixing to obtain a mixed solution C;
(6) soaking the polyacrylonitrile-based graphite felt B into the mixed solution C for 30-60 minutes to obtain a polyacrylonitrile-based graphite felt D;
(7) and taking out the polyacrylonitrile-based graphite felt D from the mixed solution C, cleaning the polyacrylonitrile-based graphite felt D with deionized water, and drying the polyacrylonitrile-based graphite felt D in a drying oven at the temperature of 45 ℃ to obtain the iron-nickel doped graphite felt electrode material for the vanadium battery.
The preferable scheme of the chemical doping modification method of the vanadium battery graphite felt electrode material is that the modified graphite felt is doped with iron and trace nickel, the mass doping amount of iron is 0.2-0.5%, and the mass doping amount of nickel is 0.01-0.05%.
The preferable scheme of the chemical doping modification method of the vanadium battery graphite felt electrode material is that potassium permanganate under the sulfuric acid condition can not only oxidize and activate the graphite felt, but also oxidize iron microspheres deposited in the graphite felt.
The preferable scheme of the chemical doping modification method of the vanadium battery graphite felt electrode material is that the nickel microspheres can slow down the oxidation speed of the iron microspheres in the graphite felt pores by potassium permanganate, so that iron ions are effectively bonded on the graphite felt, and the electrochemical activity of the graphite felt is improved.
The preferable scheme of the chemical doping modification method of the vanadium battery graphite felt electrode material is that the water absorption of the modified graphite felt is improved by 350-485% compared with that before modification.
The preferable scheme of the chemical doping modification method of the vanadium battery graphite felt electrode material is that the specific capacitance of the modified graphite felt used as the vanadium battery electrode is improved by 18-28% compared with the unmodified graphite felt electrode.
The preferable scheme of the chemical doping modification method of the graphite felt electrode material of the vanadium battery is that the chemical doping modification method is carried out at 200mA/cm2Under the current density of the vanadium battery, the energy efficiency of the modified graphite felt used as the vanadium battery electrode is improved to 60-73% from 13-15% of the energy efficiency of the unmodified graphite felt electrode.
The invention has the beneficial effects that:
the method has simple process and convenient operation, the water absorption and specific capacitance are greatly improved after the polyacrylonitrile-based graphite felt is subjected to chemical doping modification, and after the polyacrylonitrile-based graphite felt is used as an electrode material of a vanadium battery, the charge potential platform of the vanadium battery can be reduced, the discharge potential platform of the vanadium battery is improved, the energy efficiency is greatly improved, and the method has good economic and environmental benefits.
Detailed Description
For further understanding of the present invention, the following describes the chemical doping modification method of graphite felt electrode material of vanadium battery in detail with reference to specific examples, but it should be understood that the scope of protection of the present application is not limited by the specific conditions of these examples.
Example 1:
the chemical doping modification method for the graphite felt electrode material of the vanadium battery comprises the following steps:
(1) cutting the polyacrylonitrile-based graphite felt into the size of 5cm multiplied by 10cm, washing the polyacrylonitrile-based graphite felt with deionized water once, and then soaking the polyacrylonitrile-based graphite felt in the deionized water for ultrasonic cleaning for 15 minutes;
(2) taking out the polyacrylonitrile-based graphite felt, and drying in a drying oven at 45 ℃;
(3) putting the iron-nickel microsphere powder into deionized water, and dispersing the iron-nickel microsphere powder into suspension A by ultrasonic waves;
(4) putting the dried polyacrylonitrile-based graphite felt into the suspension A, continuing to perform ultrasonic oscillation for 10 minutes to uniformly disperse the iron-nickel microspheres into the pores of the polyacrylonitrile-based graphite felt, and then drying in a drying oven at 45 ℃ to obtain a polyacrylonitrile-based graphite felt B deposited with the iron-nickel microspheres;
(5) preparing a mixed solution of potassium permanganate and sulfuric acid, enabling the molar concentration of the potassium permanganate in the mixed solution to be 0.33mol/L and the molar concentration of the sulfuric acid to be 0.1mol/L, standing for 5 minutes, and uniformly mixing to obtain a mixed solution C;
(6) soaking the polyacrylonitrile-based graphite felt B in the mixed solution C for 30 minutes to obtain a polyacrylonitrile-based graphite felt D;
(7) taking out the polyacrylonitrile-based graphite felt D from the mixed solution C, cleaning the polyacrylonitrile-based graphite felt D with deionized water, and drying the polyacrylonitrile-based graphite felt D in a drying oven at 45 ℃ to obtain the iron-nickel doped graphite felt electrode material for the vanadium battery, wherein the iron doping amount is 0.2 percent, the nickel doping amount is 0.03 percent, compared with the unmodified graphite felt electrode material, the water absorption rate is improved by 355 percent, the specific capacitance is improved by 19 percent after the iron-nickel doped graphite felt electrode material is used as the vanadium battery electrode, and the specific capacitance is improved by 200mA/cm2The energy efficiency is improved to 62% at the current density of (2).
Example 2:
the chemical doping modification method for the graphite felt electrode material of the vanadium battery comprises the following steps:
(1) cutting the polyacrylonitrile-based graphite felt into the size of 5cm multiplied by 10cm, washing the polyacrylonitrile-based graphite felt with deionized water once, and then soaking the polyacrylonitrile-based graphite felt in the deionized water for ultrasonic cleaning for 30 minutes;
(2) taking out the polyacrylonitrile-based graphite felt, and drying in a drying oven at 45 ℃;
(3) putting the iron-nickel microsphere powder into deionized water, and dispersing the iron-nickel microsphere powder into suspension A by ultrasonic waves;
(4) putting the dried polyacrylonitrile-based graphite felt into the suspension A, continuing to perform ultrasonic oscillation for 15 minutes to uniformly disperse the iron-nickel microspheres into the pores of the polyacrylonitrile-based graphite felt, and then drying in a drying oven at 45 ℃ to obtain a polyacrylonitrile-based graphite felt B deposited with the iron-nickel microspheres;
(5) preparing a mixed solution of potassium permanganate and sulfuric acid, enabling the molar concentration of the potassium permanganate in the mixed solution to be 0.47mol/L and the molar concentration of the sulfuric acid to be 0.05mol/L, standing for 10 minutes, and uniformly mixing to obtain a mixed solution C;
(6) soaking the polyacrylonitrile-based graphite felt B in the mixed solution C for 60 minutes to obtain a polyacrylonitrile-based graphite felt D;
(7) taking out the polyacrylonitrile-based graphite felt D from the mixed solution C, cleaning the polyacrylonitrile-based graphite felt D with deionized water, and drying the polyacrylonitrile-based graphite felt D in a drying oven at 45 ℃ to obtain the iron-nickel doped graphite felt electrode material for the vanadium battery, wherein the iron mass doping amount of the iron-nickel doped graphite felt electrode material is 0.5 percent and the nickel mass doping amount of the nickel-nickel doped graphite felt electrode material is 0.02 percent, and compared with the unmodified graphite felt electrode material, the iron-nickel doped graphite felt electrode material has the advantages that the water absorption rate is improvedAt 200mA/cm2The energy efficiency is improved to 73% at the current density of (2).
Example 3:
the chemical doping modification method for the graphite felt electrode material of the vanadium battery comprises the following steps:
(1) cutting the polyacrylonitrile-based graphite felt into the size of 5cm multiplied by 10cm, washing the polyacrylonitrile-based graphite felt with deionized water once, and then soaking the polyacrylonitrile-based graphite felt in the deionized water for ultrasonic cleaning for 30 minutes;
(2) taking out the polyacrylonitrile-based graphite felt, and drying in a drying oven at 45 ℃;
(3) putting the iron-nickel microsphere powder into deionized water, and dispersing the iron-nickel microsphere powder into suspension A by ultrasonic waves;
(4) putting the dried polyacrylonitrile-based graphite felt into the suspension A, continuing to perform ultrasonic oscillation for 13 minutes to uniformly disperse the iron-nickel microspheres into the pores of the polyacrylonitrile-based graphite felt, and then drying in a drying oven at 45 ℃ to obtain a polyacrylonitrile-based graphite felt B deposited with the iron-nickel microspheres;
(5) preparing a mixed solution of potassium permanganate and sulfuric acid, enabling the molar concentration of the potassium permanganate in the mixed solution to be 0.35mol/L and the molar concentration of the sulfuric acid to be 0.1mol/L, standing for 10 minutes, and uniformly mixing to obtain a mixed solution C;
(6) soaking the polyacrylonitrile-based graphite felt B in the mixed solution C for 45 minutes to obtain a polyacrylonitrile-based graphite felt D;
(7) taking out the polyacrylonitrile-based graphite felt D from the mixed solution C, cleaning the polyacrylonitrile-based graphite felt D with deionized water, and drying the polyacrylonitrile-based graphite felt D in a drying oven at 45 ℃ to obtain the iron-nickel doped graphite felt electrode material for the vanadium battery, wherein the iron mass doping amount is 0.4% and the nickel doping amount is 0.05%, compared with the unmodified graphite felt electrode, the water absorption rate is improved by 427%, the specific capacitance is improved by 21% after the iron-nickel doped graphite felt electrode material is used as the vanadium battery electrode, and the specific capacitance is improved by 200mA/cm2The energy efficiency is improved to 68% at the current density of (2).
Claims (8)
1. A chemical doping modification method for a vanadium battery graphite felt electrode material is characterized by comprising the steps of ultrasonically cleaning a polyacrylonitrile-based graphite felt with deionized water, drying in an oven, ultrasonically dispersing iron-nickel microsphere powder in the graphite felt, taking out the graphite felt, soaking in a mixed solution of potassium permanganate and sulfuric acid, cleaning with deionized water, and drying in the oven to obtain the vanadium battery iron-nickel doped graphite felt modified electrode material with high electrochemical activity.
2. The chemical doping modification method of the graphite felt electrode material of the vanadium battery as claimed in claim 1, comprising the following steps:
(1) cutting the polyacrylonitrile-based graphite felt into the size of 5cm multiplied by 10cm, washing the polyacrylonitrile-based graphite felt with deionized water once, and then soaking the polyacrylonitrile-based graphite felt in the deionized water for ultrasonic cleaning for 15 to 30 minutes;
(2) taking out the polyacrylonitrile-based graphite felt, and drying in a drying oven at 45 ℃;
(3) putting the iron-nickel microsphere powder into deionized water, and dispersing the iron-nickel microsphere powder into suspension A by ultrasonic waves;
(4) putting the dried polyacrylonitrile-based graphite felt into the suspension A, continuing ultrasonic oscillation for 10-15 minutes to uniformly disperse the iron-nickel microspheres into the pores of the polyacrylonitrile-based graphite felt, and drying in a drying oven at 45 ℃ to obtain a polyacrylonitrile-based graphite felt B deposited with the iron-nickel microspheres;
(5) preparing a mixed solution of potassium permanganate and sulfuric acid, enabling the molar concentration of the potassium permanganate in the mixed solution to be 0.3-0.47 mol/L and the molar concentration of the sulfuric acid to be 0.05-0.1 mol/L, standing for 5-10 minutes, and uniformly mixing to obtain a mixed solution C;
(6) soaking the polyacrylonitrile-based graphite felt B into the mixed solution C for 30-60 minutes to obtain a polyacrylonitrile-based graphite felt D;
(7) and taking out the polyacrylonitrile-based graphite felt D from the mixed solution C, cleaning the polyacrylonitrile-based graphite felt D with deionized water, and drying the polyacrylonitrile-based graphite felt D in a drying oven at the temperature of 45 ℃ to obtain the iron-nickel doped graphite felt electrode material for the vanadium battery.
3. The chemical doping modification method of the graphite felt electrode material of the vanadium battery as claimed in claims 1 to 2, characterized in that the modified graphite felt is doped with iron and trace nickel, the mass doping amount of iron is 0.2 to 0.5%, and the mass doping amount of nickel is 0.01 to 0.05%.
4. The chemical doping modification method of the vanadium battery graphite felt electrode material as claimed in claim 1-2, characterized in that potassium permanganate under sulfuric acid condition can not only oxidize and activate the graphite felt, but also oxidize iron microspheres deposited in the graphite felt.
5. The chemical doping modification method of the vanadium battery graphite felt electrode material as claimed in claim 1-2, characterized in that the nickel microspheres can slow down the oxidation speed of the iron microspheres in the graphite felt pores by potassium permanganate, so that iron ions are effectively bonded on the graphite felt, and the electrochemical activity of the graphite felt is improved.
6. The chemical doping modification method of the graphite felt electrode material for the vanadium battery as claimed in claims 1-2, wherein the water absorption of the modified graphite felt is improved by 350-485% compared with that before modification.
7. The chemical doping modification method of the vanadium battery graphite felt electrode material as claimed in claims 1 to 2, wherein the specific capacitance of the modified graphite felt used as the vanadium battery electrode is improved by 18 to 28% compared with the unmodified graphite felt electrode.
8. The chemical doping modification method of the graphite felt electrode material for the vanadium battery as claimed in claim 1-2, characterized in that the chemical doping modification method is carried out at 200mA/cm2Under the current density of the vanadium battery, the energy efficiency of the modified graphite felt used as the vanadium battery electrode is improved to 60-73% from 13-15% of the energy efficiency of the unmodified graphite felt electrode.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113410478A (en) * | 2021-06-16 | 2021-09-17 | 中国科学技术大学 | Graphite felt composite electrode for zinc-iodine flow battery, and preparation method and application thereof |
| CN114142043A (en) * | 2021-11-30 | 2022-03-04 | 成都先进金属材料产业技术研究院股份有限公司 | Method for improving electrochemical performance of electrode for vanadium battery |
| CN114142048A (en) * | 2021-11-30 | 2022-03-04 | 成都先进金属材料产业技术研究院股份有限公司 | Electrode modification method for vanadium cell |
| CN117638108A (en) * | 2024-01-26 | 2024-03-01 | 杭州德海艾科能源科技有限公司 | High-activity graphite felt electrode for vanadium battery and preparation method thereof |
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Cited By (8)
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| CN113410478A (en) * | 2021-06-16 | 2021-09-17 | 中国科学技术大学 | Graphite felt composite electrode for zinc-iodine flow battery, and preparation method and application thereof |
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| CN117638108A (en) * | 2024-01-26 | 2024-03-01 | 杭州德海艾科能源科技有限公司 | High-activity graphite felt electrode for vanadium battery and preparation method thereof |
| CN117638108B (en) * | 2024-01-26 | 2024-04-23 | 杭州德海艾科能源科技有限公司 | Graphite felt electrode for vanadium battery and preparation method thereof |
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Application publication date: 20201002 |