CN111682226A - Nickel doping modification method for graphite felt electrode material of vanadium battery - Google Patents
Nickel doping modification method for graphite felt electrode material of vanadium battery Download PDFInfo
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- CN111682226A CN111682226A CN202010629987.9A CN202010629987A CN111682226A CN 111682226 A CN111682226 A CN 111682226A CN 202010629987 A CN202010629987 A CN 202010629987A CN 111682226 A CN111682226 A CN 111682226A
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- graphite felt
- polyacrylonitrile
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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
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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
- 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
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Abstract
The invention provides a nickel doping modification method of a vanadium battery graphite felt electrode material, belonging to the field of green energy materials, wherein a polyacrylonitrile-based graphite felt is activated by concentrated sulfuric acid, then is cleaned by deionized water in an ultrasonic mode, is dried in an oven, is soaked in a mixed solution of nickel acetate and ammonia water, is dropwise added with ethylene glycol to slowly form sol, and when the sol is converted into gel, the graphite felt is taken out, is calcined in a vacuum furnace and is cooled in air to obtain the vanadium battery nickel doping graphite felt modified electrode material. After the graphite felt electrode material of the vanadium battery is subjected to nickel doping modification, the nickel doping amount is 9.8-12.7%, the water absorption is improved by 382-457%, the specific capacitance is improved by 21-32%, and after the graphite felt electrode material is used as a vanadium battery electrode, the nickel doping amount is 250mA/cm2The energy efficiency is improved to 82-90%.
Description
Technical Field
The invention relates to a nickel doping modification method of a graphite felt electrode material of a vanadium battery, belonging to the field of green energy materials.
Background
The vanadium redox battery has the advantages of capability of changing storage capacity, no solid-state reaction, small self-discharge, stable electrode form and the like, so that the vanadium redox battery becomes a future energy storage system and is paid much attention.
The working principle of the vanadium battery is that electrolyte is taken as a main body, and when the electrolyte flows through positive and negative electrodes in the battery, chemical reaction occurs on the electrodes, so that the performance of the vanadium battery is directly influenced by the properties of electrode materials.
One of the key technologies restricting the application of vanadium batteries at present is that when a graphite felt electrode is used, the size of pores is easily reduced because of the application of pretightening force, and after the battery is used for a period of time, the pores of the graphite felt are easily blocked by crystals precipitated from electrolyte.
Disclosure of Invention
In order to solve the technical problems mentioned above, the invention provides a nickel doping modification method for a graphite felt electrode material of a vanadium battery, which comprises the steps of taking a polyacrylonitrile-based graphite felt as a basic electrode material of the vanadium battery, activating the polyacrylonitrile-based graphite felt by concentrated sulfuric acid, soaking the polyacrylonitrile-based graphite felt in a sol formed by nickel acetate and ammonia water, taking out the graphite felt after gel is formed, and calcining the graphite felt in a vacuum furnace to obtain the nickel doping graphite felt modified electrode material of the vanadium battery, which has strong hydrophilicity, high specific capacitance and difficultly blocked pores.
The technical scheme of the invention is as follows:
ultrasonically cleaning a polyacrylonitrile-based graphite felt with deionized water, drying in a drying oven, soaking in a mixed solution of nickel acetate and ammonia water, dropwise adding ethylene glycol to slowly form sol, taking out the graphite felt when the sol is converted into gel, calcining in a vacuum furnace, and air cooling to obtain the nickel-doped graphite felt modified electrode material of the vanadium battery.
The nickel doping modification method of the vanadium battery graphite felt electrode material 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 ℃ to obtain a polyacrylonitrile-based graphite felt A;
(3) soaking the dried polyacrylonitrile-based graphite felt A in concentrated sulfuric acid for 12-24 hours, ultrasonically cleaning the polyacrylonitrile-based graphite felt A with deionized water, and drying to obtain a polyacrylonitrile-based graphite felt B;
(4) preparing a mixed solution C by using deionized water, ammonia water and a nickel acetate reagent, enabling the molar concentration of nickel acetate in the mixed solution C to be 0.3-0.8 mol/L and the molar concentration of ammonia water to be 0.5-1.0 mol/L (in terms of the concentration of ammonium ions), and uniformly stirring by magnetic force;
(5) immersing the polyacrylonitrile-based graphite felt B into the solution C, dropwise adding 5-8 drops of ethylene glycol, continuing to magnetically stir for 5-10 minutes, and then standing for 30-60 minutes to obtain a sol D;
(6) and after the sol D becomes gel, taking out the polyacrylonitrile-based graphite felt B, putting the polyacrylonitrile-based graphite felt B into a vacuum furnace, preheating for 5-10 minutes at 105 ℃, then calcining for 2-4 hours at 400-500 ℃, and air cooling to obtain the nickel-doped modified graphite felt electrode material for the vanadium battery.
The preferred scheme of the nickel doping modification method of the vanadium battery graphite felt electrode material is that the modified graphite felt is doped with nickel elements, and the mass doping amount is 9.8-12.7%.
The preferable scheme of the nickel doping modification method of the vanadium battery graphite felt electrode material is that the water absorption of the modified graphite felt electrode material is improved by 382-457% compared with that before modification.
The preferable scheme of the nickel 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 21-32% compared with that of the unmodified graphite felt electrode.
The preferable scheme of the nickel doping modification method of the vanadium battery graphite felt electrode material is that the energy efficiency of the modified graphite felt used as the vanadium battery electrode is 250mA/cm2The energy efficiency of the graphite felt electrode is improved to 82-90% from 14-18% of the energy efficiency of the graphite felt electrode without modification under the current density of (1).
The invention has the beneficial effects that:
(1) according to the invention, after nickel doping modification is carried out on the polyacrylonitrile-based graphite felt, the rigidity and the hydrophilicity of the graphite felt electrode are increased, and after the graphite felt is used as an electrode material of a vanadium battery, the pores of the graphite felt are not easy to block, so that the cycle life of the battery is prolonged.
(2) According to the invention, after nickel doping modification is carried out on the polyacrylonitrile-based graphite felt, unsaturated carbon atoms at the edge of carbon lattices of the graphite felt are oxidized and etched, so that a groove is formed on carbon fibers, the contact area of vanadium electrolyte and an electrode is increased, and the battery charging and discharging reaction is facilitated.
(3) The invention greatly improves the specific surface after carrying out nickel doping modification on the polyacrylonitrile-based graphite felt, reduces the internal resistance after being used as an electrode material of a vanadium battery, improves the specific capacitance and the energy efficiency, and has good economic and environmental benefits.
Detailed Description
For further understanding of the present invention, the following describes a method for modifying the nickel doping of graphite felt electrode material of a vanadium battery in further 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 nickel 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 ℃ to obtain a polyacrylonitrile-based graphite felt A;
(3) soaking the dried polyacrylonitrile-based graphite felt A in concentrated sulfuric acid for 24 hours, cleaning with deionized water, and drying to obtain a polyacrylonitrile-based graphite felt B;
(4) preparing a mixed solution C by using deionized water, ammonia water and a nickel acetate reagent, enabling the molar concentration of nickel acetate in the mixed solution C to be 0.3mol/L and the molar concentration of ammonia water to be 0.5mol/L (in terms of the concentration of ammonium ions), and uniformly stirring by magnetic force;
(5) immersing the polyacrylonitrile-based graphite felt B into the solution C, dropwise adding 5 drops of ethylene glycol, continuing to magnetically stir for 5 minutes, and then standing for 30 minutes to obtain a sol D;
(6) after the sol D becomes gel, taking out the polyacrylonitrile-based graphite felt B, putting the polyacrylonitrile-based graphite felt B into a vacuum furnace, preheating for 5 minutes at 105 ℃, calcining for 2 hours at 400 ℃, and air cooling to obtain the modified graphite felt electrode material with the nickel doping amount of 9.8 percent for the vanadium battery, wherein the water absorption is improved by 382 percent and the specific capacitance is improved by 21 percent compared with the modified graphite felt electrode material before modification, and the modified graphite felt electrode material is used as the vanadium battery electrode and then is heated to 250mA/cm2The energy efficiency is improved to 82% at the current density of (2).
Example 2:
the nickel 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 ℃ to obtain a polyacrylonitrile-based graphite felt A;
(3) soaking the dried polyacrylonitrile-based graphite felt A in concentrated sulfuric acid for 24 hours, cleaning with deionized water, and drying to obtain a polyacrylonitrile-based graphite felt B;
(4) preparing a mixed solution C by using deionized water, ammonia water and a nickel acetate reagent, enabling the molar concentration of nickel acetate in the mixed solution C to be 0.8mol/L and the molar concentration of ammonia water to be 1.0mol/L (in terms of the concentration of ammonium ions), and uniformly stirring by magnetic force;
(5) immersing the polyacrylonitrile-based graphite felt B into the solution C, dropwise adding 8 drops of ethylene glycol, continuing to magnetically stir for 10 minutes, and standing for 60 minutes to obtain a sol D;
(6) after the sol D becomes gel, taking out the polyacrylonitrile-based graphite felt B, putting the polyacrylonitrile-based graphite felt B into a vacuum furnace, preheating for 10 minutes at 105 ℃, calcining for 4 hours at 500 ℃, and air cooling to obtain the modified graphite felt electrode material with the nickel doping amount of 12.5 percent for the vanadium battery, wherein the water absorption rate is improved by 451 percent compared with that before modification, the specific capacitance is improved by 32 percent, and after the modified graphite felt electrode material is used as the vanadium battery electrode, the polyacrylonitrile-based graphite felt electrode material is subjected to 250mA/cm2The energy efficiency is improved to 89% at the current density of (2).
Example 3:
the nickel 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 25 minutes;
(2) taking out the polyacrylonitrile-based graphite felt, and drying in a drying oven at 45 ℃ to obtain a polyacrylonitrile-based graphite felt A;
(3) soaking the dried polyacrylonitrile-based graphite felt A in concentrated sulfuric acid for 12 hours, cleaning with deionized water, and drying to obtain a polyacrylonitrile-based graphite felt B;
(4) preparing a mixed solution C by using deionized water, ammonia water and a nickel acetate reagent, enabling the molar concentration of nickel acetate in the mixed solution C to be 0.6mol/L and the molar concentration of ammonia water to be 0.8mol/L (in terms of the concentration of ammonium ions), and uniformly stirring by magnetic force;
(5) soaking the polyacrylonitrile-based graphite felt B into the solution C, dropwise adding 5 drops of ethylene glycol into the solution C, continuing to magnetically stir for 5 minutes, and then standing for 60 minutes to obtain a sol D;
(6) after the sol D becomes gel, taking out the polyacrylonitrile-based graphite felt B, putting the polyacrylonitrile-based graphite felt B into a vacuum furnace, preheating for 10 minutes at 105 ℃, calcining for 2 hours at 500 ℃, and air cooling to obtain the modified graphite felt electrode material with the nickel doping amount of 11.6 percent for the vanadium battery, wherein the water absorption is improved by 413 percent and the specific capacitance is improved by 25 percent compared with that before modification, and after the modified graphite felt electrode material is used as the vanadium battery electrode, the polyacrylonitrile-based graphite felt electrode material is subjected to 250mA/cm2The energy efficiency is improved to 86% at the current density of (2).
Claims (6)
1. Activating a polyacrylonitrile-based graphite felt with concentrated sulfuric acid, ultrasonically cleaning the activated polyacrylonitrile-based graphite felt with deionized water, drying the polyacrylonitrile-based graphite felt in a drying oven, soaking the graphite felt in an ammonia water solution of nickel acetate, dropwise adding ethylene glycol, taking out the graphite felt after gel is formed, calcining the graphite felt in a vacuum furnace, and air-cooling to obtain the vanadium battery nickel-doped graphite felt modified electrode material with large specific capacitance and high electrochemical activity.
2. The nickel 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 ℃ to obtain a polyacrylonitrile-based graphite felt A;
(3) soaking the dried polyacrylonitrile-based graphite felt A in concentrated sulfuric acid for 12-24 hours, ultrasonically cleaning the polyacrylonitrile-based graphite felt A with deionized water, and drying to obtain a polyacrylonitrile-based graphite felt B;
(4) preparing a mixed solution C by using deionized water, ammonia water and a nickel acetate reagent, enabling the molar concentration of nickel acetate in the mixed solution C to be 0.3-0.8 mol/L and the molar concentration of ammonia water to be 0.5-1.0 mol/L (in terms of the concentration of ammonium ions), and uniformly stirring by magnetic force;
(5) immersing the polyacrylonitrile-based graphite felt B into the solution C, dropwise adding 5-8 drops of ethylene glycol, continuing to magnetically stir for 5-10 minutes, and then standing for 30-60 minutes to obtain a sol D;
(6) and after the sol D becomes gel, taking out the polyacrylonitrile-based graphite felt B, putting the polyacrylonitrile-based graphite felt B into a vacuum furnace, preheating for 5-10 minutes at 105 ℃, then calcining for 2-4 hours at 400-500 ℃, and air cooling to obtain the nickel-doped modified graphite felt electrode material for the vanadium battery.
3. The method for modifying the nickel doping of the graphite felt electrode material of the vanadium battery as claimed in claims 1 to 2, wherein the modified graphite felt is doped with nickel element, and the mass doping amount is 9.8-12.7%.
4. The nickel doping modification method of the graphite felt electrode material for the vanadium battery as claimed in claims 1 to 2, wherein the water absorption of the modified graphite felt electrode material is improved by 382 to 457% compared with that before modification.
5. The nickel doping modification method of the graphite felt electrode material of the vanadium battery as claimed in claims 1-2, wherein the specific capacitance of the modified graphite felt electrode material is improved by 21-32% compared with that of the unmodified graphite felt electrode material.
6. The nickel doping modification method of the vanadium battery graphite felt electrode material as claimed in claims 1-2, characterized in that the energy efficiency of the modified graphite felt used as the vanadium battery electrode is 250mA/cm2The energy efficiency of the graphite felt electrode is improved to 82-90% from 14-18% of the energy efficiency of the graphite felt electrode without modification under the current density of (1).
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102024954A (en) * | 2009-09-16 | 2011-04-20 | 比亚迪股份有限公司 | Graphite felt electrode of vanadium battery and preparation method thereof and vanadium battery comprising the electrode |
| CN103050713A (en) * | 2011-10-17 | 2013-04-17 | 中国科学院大连化学物理研究所 | Electrode material modified by carbon nanofiber for vanadium redox flow battery and application thereof |
| CN103066287A (en) * | 2012-11-30 | 2013-04-24 | 承德万利通实业集团有限公司 | Treatment method of carbon felt for vanadium batteries |
| CN110534757A (en) * | 2019-09-11 | 2019-12-03 | 上海交通大学 | High performance carbon electrode and preparation method thereof |
| CN111170598A (en) * | 2020-01-21 | 2020-05-19 | 河海大学 | Method for modifying carbon felt anode by manganese dioxide and application |
-
2020
- 2020-07-03 CN CN202010629987.9A patent/CN111682226A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102024954A (en) * | 2009-09-16 | 2011-04-20 | 比亚迪股份有限公司 | Graphite felt electrode of vanadium battery and preparation method thereof and vanadium battery comprising the electrode |
| CN103050713A (en) * | 2011-10-17 | 2013-04-17 | 中国科学院大连化学物理研究所 | Electrode material modified by carbon nanofiber for vanadium redox flow battery and application thereof |
| CN103066287A (en) * | 2012-11-30 | 2013-04-24 | 承德万利通实业集团有限公司 | Treatment method of carbon felt for vanadium batteries |
| CN110534757A (en) * | 2019-09-11 | 2019-12-03 | 上海交通大学 | High performance carbon electrode and preparation method thereof |
| CN111170598A (en) * | 2020-01-21 | 2020-05-19 | 河海大学 | Method for modifying carbon felt anode by manganese dioxide and application |
Non-Patent Citations (1)
| Title |
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| 马奇会: "全钒氧化还原液流电池石墨毡电极的改性研究", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 * |
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