CN111740121A - Silicon doping modification method for graphite felt electrode material of vanadium battery - Google Patents
Silicon doping modification method for graphite felt electrode material of vanadium battery Download PDFInfo
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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
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- 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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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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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
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Abstract
The invention provides a silicon doping modification method of a vanadium battery graphite felt electrode material, belonging to the field of green energy materials. After the vanadium battery graphite felt electrode material is subjected to silicon doping modification, the silicon doping amount is 5.5-9.3%, the water absorption rate is improved by 486-578%, the specific surface area is improved by 55-68%, and the doping amount is 200mA/cm2Electricity (D) fromUnder the current density, the energy efficiency of the modified graphite felt used as the vanadium battery electrode can still be kept at 76-88% of the energy efficiency at the use temperature of 10-35 ℃ when the use temperature is 45-47 ℃.
Description
Technical Field
The invention relates to a silicon doping modification method of a graphite felt electrode material of a vanadium battery, belonging to the field of green energy materials.
Background
The rapid development of global economy consumes a large amount of fossil energy, causing the gradual depletion of natural resources, so that renewable energy and clean energy are required to be found as soon as possible, and vanadium batteries have excellent characteristics of high power density, rapid charging and the like, are used as an important support technology for energy reformation, and attract more and more attention of people.
The performance of the vanadium battery is directly influenced by the properties of the electrode material, the graphite felt has the tendency of gradually replacing the traditional metal electrode because of convenient processing and small loss, but the graphite felt electrode has the technical problems of poor wettability with electrolyte, few electrochemical active sites, narrow use temperature range and the like when in use.
Disclosure of Invention
In order to solve the technical problems, the invention provides a silicon doping modification method of a vanadium battery graphite felt electrode material.
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 the graphite felt in an aqueous solution of ethyl silicate and ethylene glycol, ultrasonically oscillating, standing, taking out the graphite felt after gel is formed, calcining in a vacuum furnace, and air cooling to obtain the vanadium battery silicon-doped graphite felt modified electrode material with high electrochemical activity.
The silicon 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 ℃;
(3) preparing an ethyl silicate solution A with the molar concentration of 0.3-0.8 mol/L by using deionized water and an ethyl silicate reagent, and uniformly stirring;
(4) dropwise adding ethylene glycol into the ethyl silicate solution A while performing ultrasonic oscillation to obtain an ethyl silicate mixed solution B;
(5) immersing the dried polyacrylonitrile-based graphite felt into the solution B, continuing ultrasonic oscillation for 5-10 minutes at the temperature of 30-50 ℃, and then standing for 30-60 minutes to obtain a sol C;
(6) and after the sol C is changed into clear and transparent gel, taking out the polyacrylonitrile-based graphite felt, putting the polyacrylonitrile-based graphite felt into a vacuum furnace, preheating for 5-10 minutes at 105 ℃, then calcining for 2-4 hours at 450-600 ℃, and air cooling to obtain the silicon-doped modified graphite felt electrode material for the vanadium battery.
The preferred scheme of the silicon doping modification method of the vanadium battery graphite felt electrode material is that the modified graphite felt is doped with silicon elements, and the mass doping amount is 5.5-9.3%.
The preferable scheme of the silicon 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 486-578% compared with that before modification.
The preferable scheme of the silicon doping modification method of the vanadium battery graphite felt electrode material is that the specific surface area of the modified graphite felt used as the vanadium battery electrode is increased by 55-68% compared with the unmodified graphite felt electrode.
The preferable scheme of the silicon doping modification method of the vanadium battery graphite felt electrode material is that the silicon doping modification method is carried out at 200mA/cm2Under the current density of the modified graphite felt, the energy efficiency of the modified graphite felt used as the vanadium battery electrode can still be kept 76-88% of the energy efficiency at the use temperature of 10-35 ℃ when the use temperature is 45-47 ℃.
The invention has the beneficial effects that:
(1) according to the invention, after silicon doping modification is carried out on the polyacrylonitrile-based graphite felt, a C-O-Si-O bond is formed, and after the polyacrylonitrile-based graphite felt is used as a vanadium battery electrode, the flexibility and the hydrophilicity of the graphite felt electrode are increased, and the use temperature range is enhanced.
(2) According to the invention, a sol-gel method is adopted and an ultrasonic method is combined for modification, so that silicon elements can be uniformly doped into the graphite felt, and after the graphite felt is made into the vanadium battery electrode, the charging and discharging stability of the graphite felt electrode is improved.
(3) The specific surface of the polyacrylonitrile-based graphite felt is greatly improved after silicon doping modification, and the polyacrylonitrile-based graphite felt can improve the energy efficiency of a vanadium battery after being used as an electrode material of the vanadium battery, and has good economic and environmental benefits.
Detailed Description
For further understanding of the present invention, the following describes a method for modifying the silicon 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 silicon 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) preparing ethyl silicate solution A with the molar concentration of 0.5mol/L by using deionized water and an ethyl silicate reagent, and uniformly stirring;
(4) dropwise adding ethylene glycol into the ethyl silicate solution A while performing ultrasonic oscillation to obtain an ethyl silicate mixed solution B;
(5) immersing the dried polyacrylonitrile-based graphite felt into the solution B, continuing ultrasonic oscillation for 5 minutes at the temperature of 30 ℃, and then standing for 30 minutes to obtain a sol C;
(6) and after the sol C is changed into clear and transparent gel, taking out the polyacrylonitrile-based graphite felt, putting the polyacrylonitrile-based graphite felt into a vacuum furnace, preheating for 5 minutes at 105 ℃, calcining for 2 hours at 450 ℃, and air-cooling to obtain the modified graphite felt electrode material with the silicon content doping amount of 5.5 percent for the vanadium battery, wherein the water absorption is improved by 486 percent compared with that before modification, the specific surface area is improved by 55 percent compared with that before modification, and the modified graphite felt electrode material can still keep 80 percent of the energy efficiency at the use temperature of 30 ℃ when being used as the vanadium battery electrode at the use temperature of 45 ℃.
Example 2:
the silicon 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 20 minutes;
(2) taking out the polyacrylonitrile-based graphite felt, and drying in a drying oven at 45 ℃;
(3) preparing ethyl silicate solution A with the molar concentration of 0.8mol/L by using deionized water and an ethyl silicate reagent, and uniformly stirring;
(4) dropwise adding ethylene glycol into the ethyl silicate solution A while performing ultrasonic oscillation to obtain an ethyl silicate mixed solution B;
(5) immersing the dried polyacrylonitrile-based graphite felt into the solution B, continuing ultrasonic oscillation for 10 minutes at the temperature of 45 ℃, and then standing for 60 minutes to obtain a sol C;
(6) and after the sol C is changed into clear and transparent gel, taking out the polyacrylonitrile-based graphite felt, putting the polyacrylonitrile-based graphite felt into a vacuum furnace, preheating for 10 minutes at 105 ℃, calcining for 3 hours at 600 ℃, and air-cooling to obtain the modified graphite felt electrode material with the silicon content doping amount of 9.2 percent for the vanadium battery, wherein the water absorption is improved by 578 percent compared with that before modification, the specific surface area is improved by 68 percent compared with that before modification, and the modified graphite felt electrode material can still keep 78 percent of the energy efficiency at the use temperature of 20 ℃ when being used as the vanadium battery electrode at the use temperature of 47 ℃.
Example 3:
the silicon 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) preparing ethyl silicate solution A with the molar concentration of 0.5mol/L by using deionized water and an ethyl silicate reagent, and uniformly stirring;
(4) dropwise adding ethylene glycol into the ethyl silicate solution A while performing ultrasonic oscillation to obtain an ethyl silicate mixed solution B;
(5) immersing the dried polyacrylonitrile-based graphite felt into the solution B, continuing ultrasonic oscillation for 10 minutes at 40 ℃, and then standing for 50 minutes to obtain a sol C;
(6) and after the sol C is changed into clear and transparent gel, taking out the polyacrylonitrile-based graphite felt, putting the polyacrylonitrile-based graphite felt into a vacuum furnace, preheating for 10 minutes at 105 ℃, calcining for 3 hours at 600 ℃, and air-cooling to obtain the modified graphite felt electrode material with silicon doping amount of 6.7 percent for the vanadium battery, wherein the water absorption is improved by 508 percent compared with that before modification, the specific surface area is improved by 61 percent compared with that before modification, and the modified graphite felt electrode material can still keep 76 percent of the energy efficiency at 25 ℃ when being used as the vanadium battery electrode at 47 ℃.
Example 4:
the silicon 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) preparing ethyl silicate solution A with the molar concentration of 0.5mol/L by using deionized water and an ethyl silicate reagent, and uniformly stirring;
(4) dropwise adding ethylene glycol into the ethyl silicate solution A while performing ultrasonic oscillation to obtain an ethyl silicate mixed solution B;
(5) immersing the dried polyacrylonitrile-based graphite felt into the solution B, continuing ultrasonic oscillation for 10 minutes at 40 ℃, and then standing for 60 minutes to obtain a sol C;
(6) and after the sol C is changed into clear and transparent gel, taking out the polyacrylonitrile-based graphite felt, putting the polyacrylonitrile-based graphite felt into a vacuum furnace, preheating for 10 minutes at 105 ℃, calcining for 2 hours at 600 ℃, and air-cooling to obtain the modified graphite felt electrode material with the silicon content doping amount of 6.2 percent for the vanadium battery, wherein the water absorption is improved by 501 percent compared with that before modification, the specific surface area is improved by 60 percent compared with that before modification, and after the modified graphite felt electrode material is used as the vanadium battery electrode, the energy efficiency can still be kept at 79 percent of that at the use temperature of 25 ℃ when the use temperature is 46 ℃.
Example 5:
the silicon 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 20 minutes;
(2) taking out the polyacrylonitrile-based graphite felt, and drying in a drying oven at 45 ℃;
(3) preparing ethyl silicate solution A with the molar concentration of 0.8mol/L by using deionized water and an ethyl silicate reagent, and uniformly stirring;
(4) dropwise adding ethylene glycol into the ethyl silicate solution A while performing ultrasonic oscillation to obtain an ethyl silicate mixed solution B;
(5) immersing the dried polyacrylonitrile-based graphite felt into the solution B, continuing ultrasonic oscillation for 10 minutes at the temperature of 45 ℃, and then standing for 60 minutes to obtain a sol C;
(6) and after the sol C is changed into clear and transparent gel, taking out the polyacrylonitrile-based graphite felt, putting the polyacrylonitrile-based graphite felt into a vacuum furnace, preheating for 10 minutes at 105 ℃, calcining for 2 hours at 600 ℃, and air-cooling to obtain the modified graphite felt electrode material with the silicon content doping amount of 9.1 percent for the vanadium battery, wherein the water absorption is improved by 570 percent compared with that before modification, the specific surface area is improved by 65 percent compared with that before modification, and the modified graphite felt electrode material can still keep 88 percent of the energy efficiency at the use temperature of 20 ℃ when being used as the vanadium battery electrode at the use temperature of 45 ℃.
Claims (6)
1. A silicon 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 the cleaned polyacrylonitrile-based graphite felt in a drying oven, soaking the graphite felt in an aqueous solution of ethyl silicate and glycol, ultrasonically oscillating the graphite felt, standing the graphite felt, taking out the graphite felt after gel is formed, calcining the graphite felt in a vacuum furnace, and air cooling the graphite felt to obtain the vanadium battery silicon doping graphite felt modified electrode material with high electrochemical activity.
2. The silicon doping modification method of the vanadium battery graphite felt electrode material 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) preparing an ethyl silicate solution A with the molar concentration of 0.3-0.8 mol/L by using deionized water and an ethyl silicate reagent, and uniformly stirring;
(4) dropwise adding ethylene glycol into the ethyl silicate solution A while performing ultrasonic oscillation to obtain an ethyl silicate mixed solution B;
(5) immersing the dried polyacrylonitrile-based graphite felt into the solution B, continuing ultrasonic oscillation for 5-10 minutes at the temperature of 30-50 ℃, and then standing for 30-60 minutes to obtain a sol C;
(6) and after the sol C is changed into clear and transparent gel, taking out the polyacrylonitrile-based graphite felt, putting the polyacrylonitrile-based graphite felt into a vacuum furnace, preheating for 5-10 minutes at 105 ℃, then calcining for 2-4 hours at 450-600 ℃, and air cooling to obtain the silicon-doped modified graphite felt electrode material for the vanadium battery.
3. The silicon 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 silicon element with a mass doping amount of 5.5 to 9.3%.
4. The silicon 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 486 to 578% compared with that before modification.
5. The silicon doping modification method of the graphite felt electrode material of the vanadium battery as claimed in claims 1-2, wherein the specific surface area of the modified graphite felt electrode material is increased by 55-68% compared with that of the unmodified graphite felt electrode material.
6. The silicon doping modification method of the graphite felt electrode material of the vanadium battery as claimed in claims 1-2The method is characterized in that the energy efficiency of the modified graphite felt used as the electrode of the vanadium battery is 200mA/cm2Under the current density of (2), when the using temperature is 45-47 ℃, the energy efficiency of the modified graphite felt used as the vanadium battery electrode can still be kept at 76-88% of the energy efficiency when the using temperature is 10-35 ℃.
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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 |
| CN104987100A (en) * | 2015-07-08 | 2015-10-21 | 赵丽丽 | Infrared reflecting heat-preservation carbon felt manufactured through sol-gel method and application thereof |
| CN107221681A (en) * | 2017-06-14 | 2017-09-29 | 北京航空航天大学 | It is a kind of applied to modified electrode of all-vanadium flow battery and preparation method thereof |
| CN110034305A (en) * | 2019-03-12 | 2019-07-19 | 辽宁科技大学 | A kind of activation method of siderochrome flow battery graphite felt electrode material |
| CN110534757A (en) * | 2019-09-11 | 2019-12-03 | 上海交通大学 | High performance carbon electrode and preparation method thereof |
-
2020
- 2020-07-03 CN CN202010629986.4A patent/CN111740121A/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 |
| CN104987100A (en) * | 2015-07-08 | 2015-10-21 | 赵丽丽 | Infrared reflecting heat-preservation carbon felt manufactured through sol-gel method and application thereof |
| CN107221681A (en) * | 2017-06-14 | 2017-09-29 | 北京航空航天大学 | It is a kind of applied to modified electrode of all-vanadium flow battery and preparation method thereof |
| CN110034305A (en) * | 2019-03-12 | 2019-07-19 | 辽宁科技大学 | A kind of activation method of siderochrome flow battery graphite felt electrode material |
| CN110534757A (en) * | 2019-09-11 | 2019-12-03 | 上海交通大学 | High performance carbon electrode and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| CHEN NA等: "SiO2-decorated graphite felt electrode by silicic acid etching for iron-chromium redox flow battery", 《ELECTROCHIMICA ACTA》 * |
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